# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk6106 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H42 B F10 P Zr' _chemical_formula_weight 893.78 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' B B 0.0013 0.0007 '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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.0134(2) _cell_length_b 20.4685(3) _cell_length_c 16.1406(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7933.40(17) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 15299 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9005 _exptl_absorpt_correction_T_max 0.9502 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46932 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13311 _reflns_number_gt 11762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+13.1929P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(4) _refine_ls_number_reflns 13311 _refine_ls_number_parameters 1044 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 Zr1A Zr 1.37877(2) 1.52667(2) -0.08950(4) 0.05055(14) Uani 1 1 d . . . P1A P 1.35167(5) 1.45319(7) -0.24208(9) 0.0447(3) Uani 1 1 d . . . B1A B 1.4612(3) 1.2910(3) -0.2827(4) 0.0477(14) Uani 1 1 d . . . C1A C 1.3812(2) 1.3691(3) -0.2364(4) 0.0503(13) Uani 1 1 d . . . H1A1 H 1.3784 1.3532 -0.1794 0.060 Uiso 1 1 calc R . . H1A2 H 1.3592 1.3400 -0.2718 0.060 Uiso 1 1 calc R . . C2A C 1.4419(2) 1.3665(3) -0.2637(4) 0.0520(13) Uani 1 1 d . . . H2A1 H 1.4655 1.3849 -0.2201 0.062 Uiso 1 1 calc R . . H2A2 H 1.4467 1.3930 -0.3137 0.062 Uiso 1 1 calc R . . C4A C 1.4530(2) 1.2451(3) -0.2002(4) 0.0532(13) Uani 1 1 d . . . H4A1 H 1.4774 1.2605 -0.1564 0.080 Uiso 1 1 calc R . . H4A2 H 1.4623 1.2002 -0.2137 0.080 Uiso 1 1 calc R . . H4A3 H 1.4147 1.2475 -0.1818 0.080 Uiso 1 1 calc R . . C3A C 1.3149(3) 1.4653(4) -0.0272(5) 0.079(2) Uani 1 1 d . . . H3A1 H 1.3139 1.4758 0.0314 0.119 Uiso 1 1 calc R . . H3A2 H 1.3241 1.4196 -0.0343 0.119 Uiso 1 1 calc R . . H3A3 H 1.2786 1.4740 -0.0515 0.119 Uiso 1 1 calc R . . C31A C 1.2744(2) 1.4522(3) -0.2420(4) 0.0503(13) Uani 1 1 d . . . C32A C 1.2423(2) 1.4003(3) -0.2086(4) 0.0584(14) Uani 1 1 d . . . C33A C 1.1846(3) 1.4031(4) -0.2160(4) 0.0712(19) Uani 1 1 d . . . H33A H 1.1634 1.3681 -0.1953 0.085 Uiso 1 1 calc R . . C34A C 1.1572(3) 1.4547(4) -0.2522(5) 0.0691(19) Uani 1 1 d . . . C35A C 1.1892(2) 1.5060(3) -0.2821(4) 0.0667(17) Uani 1 1 d . . . H35A H 1.1711 1.5422 -0.3059 0.080 Uiso 1 1 calc R . . C36A C 1.2467(2) 1.5057(3) -0.2778(4) 0.0522(13) Uani 1 1 d . . . C37A C 1.2649(3) 1.3406(3) -0.1662(5) 0.079(2) Uani 1 1 d . . . H37A H 1.2360 1.3210 -0.1324 0.118 Uiso 1 1 calc R . . H37B H 1.2961 1.3529 -0.1312 0.118 Uiso 1 1 calc R . . H37C H 1.2773 1.3094 -0.2075 0.118 Uiso 1 1 calc R . . C38A C 1.0944(3) 1.4565(5) -0.2564(6) 0.102(3) Uani 1 1 d . . . H38A H 1.0803 1.4131 -0.2681 0.153 Uiso 1 1 calc R . . H38B H 1.0828 1.4862 -0.2999 0.153 Uiso 1 1 calc R . . H38C H 1.0797 1.4715 -0.2037 0.153 Uiso 1 1 calc R . . C39A C 1.2755(2) 1.5649(3) -0.3162(4) 0.0594(15) Uani 1 1 d . . . H39A H 1.2790 1.5586 -0.3755 0.089 Uiso 1 1 calc R . . H39B H 1.3122 1.5700 -0.2920 0.089 Uiso 1 1 calc R . . H39C H 1.2536 1.6038 -0.3055 0.089 Uiso 1 1 calc R . . C21A C 1.3677(2) 1.4745(3) -0.3502(3) 0.0453(12) Uani 1 1 d . . . C22A C 1.4083(2) 1.5232(3) -0.3680(4) 0.0467(12) Uani 1 1 d . . . C23A C 1.4131(2) 1.5467(3) -0.4484(4) 0.0529(13) Uani 1 1 d . . . H23A H 1.4398 1.5791 -0.4595 0.063 Uiso 1 1 calc R . . C24A C 1.3802(2) 1.5245(3) -0.5128(4) 0.0595(15) Uani 1 1 d . . . C25A C 1.3451(3) 1.4715(3) -0.4969(4) 0.0611(15) Uani 1 1 d . . . H25A H 1.3258 1.4521 -0.5411 0.073 Uiso 1 1 calc R . . C26A C 1.3380(2) 1.4469(3) -0.4173(4) 0.0502(13) Uani 1 1 d . . . C27A C 1.4476(2) 1.5485(3) -0.3042(4) 0.0572(14) Uani 1 1 d . . . H27A H 1.4768 1.5166 -0.2946 0.086 Uiso 1 1 calc R . . H27B H 1.4276 1.5563 -0.2530 0.086 Uiso 1 1 calc R . . H27C H 1.4640 1.5890 -0.3235 0.086 Uiso 1 1 calc R . . C28A C 1.3830(3) 1.5552(4) -0.5975(5) 0.0827(19) Uani 1 1 d . . . H28A H 1.3490 1.5794 -0.6080 0.124 Uiso 1 1 calc R . . H28B H 1.3873 1.5213 -0.6391 0.124 Uiso 1 1 calc R . . H28C H 1.4146 1.5847 -0.6001 0.124 Uiso 1 1 calc R . . C29A C 1.2967(3) 1.3898(3) -0.4099(4) 0.0658(17) Uani 1 1 d . . . H29A H 1.2611 1.4061 -0.3905 0.099 Uiso 1 1 calc R . . H29B H 1.3110 1.3579 -0.3710 0.099 Uiso 1 1 calc R . . H29C H 1.2920 1.3695 -0.4638 0.099 Uiso 1 1 calc R . . C51A C 1.4247(2) 1.2679(3) -0.3654(4) 0.0488(12) Uani 1 1 d . . . C52A C 1.3776(2) 1.2282(3) -0.3640(4) 0.0554(15) Uani 1 1 d . . . F52A F 1.35978(15) 1.20066(19) -0.2948(3) 0.0772(11) Uani 1 1 d . . . C53A C 1.3454(3) 1.2167(3) -0.4343(5) 0.0713(19) Uani 1 1 d . . . F53A F 1.30006(18) 1.1777(2) -0.4279(4) 0.1033(16) Uani 1 1 d . . . C54A C 1.3595(4) 1.2433(4) -0.5082(5) 0.084(2) Uani 1 1 d . . . F54A F 1.3273(2) 1.2326(2) -0.5754(3) 0.1176(19) Uani 1 1 d . . . C55A C 1.4060(4) 1.2811(4) -0.5137(4) 0.081(2) Uani 1 1 d . . . F55A F 1.4204(2) 1.3093(3) -0.5860(3) 0.1310(19) Uani 1 1 d . . . C56A C 1.4364(3) 1.2933(3) -0.4422(4) 0.0641(16) Uani 1 1 d . . . F56A F 1.48114(18) 1.3323(2) -0.4533(3) 0.0902(13) Uani 1 1 d . . . C41A C 1.5288(2) 1.2860(2) -0.3055(3) 0.0451(11) Uani 1 1 d . . . C42A C 1.5690(2) 1.3321(3) -0.2881(4) 0.0548(14) Uani 1 1 d . . . F42A F 1.55587(15) 1.39167(17) -0.2600(3) 0.0842(12) Uani 1 1 d . . . C43A C 1.6262(3) 1.3213(3) -0.2988(4) 0.0624(16) Uani 1 1 d . . . F43A F 1.66214(16) 1.3683(2) -0.2770(4) 0.1057(17) Uani 1 1 d . . . C44A C 1.6449(3) 1.2641(3) -0.3288(4) 0.0619(16) Uani 1 1 d . . . F44A F 1.69979(16) 1.2540(2) -0.3408(3) 0.0937(14) Uani 1 1 d . . . C45A C 1.6075(3) 1.2171(3) -0.3497(5) 0.0647(16) Uani 1 1 d . . . F45A F 1.62477(17) 1.1603(2) -0.3824(3) 0.0971(15) Uani 1 1 d . . . C46A C 1.5514(3) 1.2288(3) -0.3364(4) 0.0582(15) Uani 1 1 d . . . F46A F 1.51677(15) 1.17855(17) -0.3572(3) 0.0882(14) Uani 1 1 d . . . C11A C 1.3020(3) 1.6074(4) -0.1195(5) 0.078(2) Uani 1 1 d . . . H11A H 1.2704 1.5927 -0.1484 0.094 Uiso 1 1 calc R . . C12A C 1.3506(3) 1.6337(3) -0.1543(5) 0.0687(17) Uani 1 1 d . . . H12A H 1.3569 1.6411 -0.2110 0.082 Uiso 1 1 calc R . . C13A C 1.3879(4) 1.6470(3) -0.0905(6) 0.089(2) Uani 1 1 d . . . H13A H 1.4241 1.6637 -0.0970 0.107 Uiso 1 1 calc R . . C14A C 1.3628(6) 1.6316(4) -0.0165(6) 0.113(4) Uani 1 1 d . . . H14A H 1.3786 1.6366 0.0364 0.136 Uiso 1 1 calc R . . C15A C 1.3095(5) 1.6072(5) -0.0339(6) 0.109(4) Uani 1 1 d . . . H15A H 1.2833 1.5930 0.0055 0.131 Uiso 1 1 calc R . . C16A C 1.4321(3) 1.4644(5) 0.0192(5) 0.089(2) Uani 1 1 d . . . H16A H 1.4129 1.4436 0.0626 0.106 Uiso 1 1 calc R . . C17A C 1.4516(3) 1.5272(5) 0.0193(5) 0.092(3) Uani 1 1 d . . . H17A H 1.4471 1.5575 0.0626 0.110 Uiso 1 1 calc R . . C18A C 1.4794(3) 1.5393(4) -0.0562(5) 0.081(2) Uani 1 1 d . . . H18A H 1.4968 1.5784 -0.0725 0.097 Uiso 1 1 calc R . . C19A C 1.4760(2) 1.4820(3) -0.1013(5) 0.0681(17) Uani 1 1 d . . . H19A H 1.4919 1.4754 -0.1539 0.082 Uiso 1 1 calc R . . C20A C 1.4461(3) 1.4364(4) -0.0582(4) 0.0702(18) Uani 1 1 d . . . H20A H 1.4367 1.3943 -0.0766 0.084 Uiso 1 1 calc R . . Zr1B Zr 1.11535(2) 1.49698(3) -0.59659(4) 0.05176(14) Uani 1 1 d . . . P1B P 1.14143(5) 1.43467(6) -0.75491(9) 0.0417(3) Uani 1 1 d . . . B1B B 1.0244(3) 1.2841(3) -0.8284(4) 0.0481(14) Uani 1 1 d . . . C1B C 1.1039(2) 1.3556(2) -0.7653(3) 0.0449(11) Uani 1 1 d . . . H1B1 H 1.1267 1.3261 -0.7989 0.054 Uiso 1 1 calc R . . H1B2 H 1.1004 1.3361 -0.7101 0.054 Uiso 1 1 calc R . . C2B C 1.0457(2) 1.3592(3) -0.8041(4) 0.0524(13) Uani 1 1 d . . . H2B1 H 1.0468 1.3864 -0.8540 0.063 Uiso 1 1 calc R . . H2B2 H 1.0196 1.3791 -0.7648 0.063 Uiso 1 1 calc R . . C4B C 1.0301(2) 1.2346(3) -0.7501(4) 0.0532(13) Uani 1 1 d . . . H4B1 H 1.0164 1.1917 -0.7657 0.080 Uiso 1 1 calc R . . H4B2 H 1.0084 1.2511 -0.7040 0.080 Uiso 1 1 calc R . . H4B3 H 1.0689 1.2313 -0.7339 0.080 Uiso 1 1 calc R . . C3B C 1.1664(3) 1.4151(3) -0.5435(5) 0.0750(19) Uani 1 1 d . . . H3B1 H 1.1674 1.4189 -0.4837 0.112 Uiso 1 1 calc R . . H3B2 H 1.2040 1.4174 -0.5653 0.112 Uiso 1 1 calc R . . H3B3 H 1.1498 1.3735 -0.5587 0.112 Uiso 1 1 calc R . . C31B C 1.2181(2) 1.4208(2) -0.7522(3) 0.0453(11) Uani 1 1 d . . . C32B C 1.2531(2) 1.4731(3) -0.7774(4) 0.0478(12) Uani 1 1 d . . . C33B C 1.3100(2) 1.4653(3) -0.7764(4) 0.0520(13) Uani 1 1 d . . . H33B H 1.3323 1.5004 -0.7939 0.062 Uiso 1 1 calc R . . C34B C 1.3360(2) 1.4085(3) -0.7509(4) 0.0560(14) Uani 1 1 d . . . C35B C 1.3015(2) 1.3578(3) -0.7237(4) 0.0572(15) Uani 1 1 d . . . H35B H 1.3180 1.3192 -0.7041 0.069 Uiso 1 1 calc R . . C36B C 1.2437(2) 1.3624(3) -0.7246(4) 0.0528(13) Uani 1 1 d . . . C37B C 1.2318(2) 1.5391(3) -0.8090(4) 0.0573(15) Uani 1 1 d . . . H37D H 1.2576 1.5732 -0.7931 0.086 Uiso 1 1 calc R . . H37E H 1.1955 1.5480 -0.7851 0.086 Uiso 1 1 calc R . . H37F H 1.2286 1.5377 -0.8689 0.086 Uiso 1 1 calc R . . C38B C 1.3982(3) 1.4011(4) -0.7510(5) 0.079(2) Uani 1 1 d . . . H38D H 1.4088 1.3670 -0.7896 0.118 Uiso 1 1 calc R . . H38E H 1.4107 1.3896 -0.6958 0.118 Uiso 1 1 calc R . . H38F H 1.4152 1.4421 -0.7676 0.118 Uiso 1 1 calc R . . C39B C 1.2135(3) 1.3015(3) -0.6950(5) 0.0702(18) Uani 1 1 d . . . H39D H 1.1971 1.2792 -0.7421 0.105 Uiso 1 1 calc R . . H39E H 1.1843 1.3139 -0.6564 0.105 Uiso 1 1 calc R . . H39F H 1.2397 1.2727 -0.6675 0.105 Uiso 1 1 calc R . . C21B C 1.1297(2) 1.4710(2) -0.8579(3) 0.0421(11) Uani 1 1 d . . . C22B C 1.1557(2) 1.4462(3) -0.9302(4) 0.0489(13) Uani 1 1 d . . . C23B C 1.1512(2) 1.4812(3) -1.0031(4) 0.0581(14) Uani 1 1 d . . . H23B H 1.1678 1.4644 -1.0513 0.070 Uiso 1 1 calc R . . C24B C 1.1229(2) 1.5407(3) -1.0078(4) 0.0574(14) Uani 1 1 d . . . C25B C 1.0942(2) 1.5608(3) -0.9397(4) 0.0534(14) Uani 1 1 d . . . H25B H 1.0717 1.5982 -0.9444 0.064 Uiso 1 1 calc R . . C26B C 1.0963(2) 1.5290(2) -0.8636(3) 0.0450(12) Uani 1 1 d . . . C27B C 1.1892(3) 1.3836(3) -0.9338(4) 0.0577(15) Uani 1 1 d . . . H27D H 1.1914 1.3686 -0.9907 0.087 Uiso 1 1 calc R . . H27E H 1.1712 1.3505 -0.9002 0.087 Uiso 1 1 calc R . . H27F H 1.2265 1.3916 -0.9129 0.087 Uiso 1 1 calc R . . C28B C 1.1232(3) 1.5799(3) -1.0873(5) 0.0752(17) Uani 1 1 d . . . H28D H 1.0924 1.6105 -1.0870 0.113 Uiso 1 1 calc R . . H28E H 1.1195 1.5506 -1.1342 0.113 Uiso 1 1 calc R . . H28F H 1.1581 1.6037 -1.0917 0.113 Uiso 1 1 calc R . . C29B C 1.0627(3) 1.5546(3) -0.7942(4) 0.0614(15) Uani 1 1 d . . . H29D H 1.0556 1.6008 -0.8028 0.092 Uiso 1 1 calc R . . H29E H 1.0829 1.5487 -0.7427 0.092 Uiso 1 1 calc R . . H29F H 1.0276 1.5312 -0.7916 0.092 Uiso 1 1 calc R . . C51B C 0.9573(2) 1.2805(2) -0.8526(4) 0.0481(12) Uani 1 1 d . . . C52B C 0.9164(2) 1.3090(3) -0.8032(4) 0.0553(14) Uani 1 1 d . . . F52B F 0.93181(15) 1.3455(2) -0.7372(3) 0.0856(13) Uani 1 1 d . . . C53B C 0.8596(3) 1.3006(3) -0.8110(5) 0.0638(16) Uani 1 1 d . . . F53B F 0.82411(16) 1.3275(2) -0.7567(3) 0.0870(12) Uani 1 1 d . . . C54B C 0.8395(3) 1.2633(3) -0.8745(5) 0.0665(17) Uani 1 1 d . . . F54B F 0.78466(16) 1.2553(2) -0.8861(3) 0.0992(15) Uani 1 1 d . . . C55B C 0.8770(3) 1.2342(3) -0.9277(5) 0.075(2) Uani 1 1 d . . . F55B F 0.8585(2) 1.1974(3) -0.9909(3) 0.1187(18) Uani 1 1 d . . . C56B C 0.9333(3) 1.2420(3) -0.9135(4) 0.0627(16) Uani 1 1 d . . . F56B F 0.96639(18) 1.2073(2) -0.9664(3) 0.0959(15) Uani 1 1 d . . . C41B C 1.0629(2) 1.2639(3) -0.9102(4) 0.0479(12) Uani 1 1 d . . . C42B C 1.1081(2) 1.2210(3) -0.9113(4) 0.0519(13) Uani 1 1 d . . . F42B F 1.12273(14) 1.18769(17) -0.8428(2) 0.0639(9) Uani 1 1 d . . . C43B C 1.1407(3) 1.2093(3) -0.9796(4) 0.0602(15) Uani 1 1 d . . . F43B F 1.18441(16) 1.16720(19) -0.9754(3) 0.0789(11) Uani 1 1 d . . . C44B C 1.1302(3) 1.2409(3) -1.0533(4) 0.0632(17) Uani 1 1 d . . . F44B F 1.16137(19) 1.2295(2) -1.1209(2) 0.0886(13) Uani 1 1 d . . . C45B C 1.0867(3) 1.2847(3) -1.0561(4) 0.0637(17) Uani 1 1 d . . . F45B F 1.07592(18) 1.3168(2) -1.1271(2) 0.0892(13) Uani 1 1 d . . . C46B C 1.0551(2) 1.2951(3) -0.9860(4) 0.0550(14) Uani 1 1 d . . . F46B F 1.01357(15) 1.33919(18) -0.9943(2) 0.0713(10) Uani 1 1 d . . . C11B C 1.1936(3) 1.5517(4) -0.5212(5) 0.087(2) Uani 1 1 d . . . H11B H 1.2155 1.5266 -0.4849 0.105 Uiso 1 1 calc R . . C12B C 1.1457(4) 1.5844(4) -0.5004(5) 0.093(2) Uani 1 1 d . . . H12B H 1.1297 1.5850 -0.4473 0.111 Uiso 1 1 calc R . . C13B C 1.1242(3) 1.6168(3) -0.5698(5) 0.078(2) Uani 1 1 d . . . H13B H 1.0917 1.6421 -0.5729 0.093 Uiso 1 1 calc R . . C14B C 1.1621(3) 1.6029(3) -0.6340(5) 0.0724(18) Uani 1 1 d . . . H14B H 1.1595 1.6188 -0.6885 0.087 Uiso 1 1 calc R . . C15B C 1.2043(3) 1.5617(3) -0.6043(5) 0.0752(19) Uani 1 1 d . . . H15B H 1.2341 1.5443 -0.6350 0.090 Uiso 1 1 calc R . . C16B C 1.0477(3) 1.4438(4) -0.4986(5) 0.083(2) Uani 1 1 d . . . H16B H 1.0614 1.4219 -0.4516 0.099 Uiso 1 1 calc R . . C17B C 1.0339(3) 1.5100(4) -0.5033(4) 0.0739(19) Uani 1 1 d . . . H17B H 1.0371 1.5410 -0.4606 0.089 Uiso 1 1 calc R . . C18B C 1.0146(2) 1.5213(3) -0.5834(5) 0.0642(15) Uani 1 1 d . . . H18B H 1.0022 1.5617 -0.6044 0.077 Uiso 1 1 calc R . . C19B C 1.0167(3) 1.4632(3) -0.6267(5) 0.0693(18) Uani 1 1 d . . . H19B H 1.0056 1.4572 -0.6820 0.083 Uiso 1 1 calc R . . C20B C 1.0376(3) 1.4159(4) -0.5758(6) 0.081(2) Uani 1 1 d . . . H20B H 1.0440 1.3720 -0.5903 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1A 0.0574(3) 0.0517(3) 0.0425(3) -0.0011(3) 0.0024(3) -0.0001(2) P1A 0.0403(7) 0.0454(7) 0.0483(8) -0.0007(6) -0.0020(6) 0.0009(5) B1A 0.051(3) 0.043(3) 0.049(4) 0.003(3) -0.004(3) -0.003(3) C1A 0.050(3) 0.041(3) 0.060(3) -0.002(2) -0.005(2) 0.005(2) C2A 0.048(3) 0.042(3) 0.066(4) -0.003(3) -0.005(3) 0.000(2) C4A 0.056(3) 0.055(3) 0.048(3) 0.000(3) -0.003(2) 0.008(3) C3A 0.076(5) 0.086(5) 0.076(5) 0.008(4) 0.001(4) -0.008(4) C31A 0.041(3) 0.059(3) 0.052(3) -0.005(3) 0.001(2) -0.004(2) C32A 0.051(3) 0.065(4) 0.059(4) -0.004(3) 0.006(3) -0.014(3) C33A 0.053(4) 0.085(5) 0.075(5) -0.003(4) 0.009(3) -0.019(3) C34A 0.044(3) 0.090(5) 0.074(5) -0.020(4) 0.010(3) -0.004(3) C35A 0.046(3) 0.086(5) 0.068(4) -0.010(3) -0.003(3) 0.012(3) C36A 0.047(3) 0.060(3) 0.049(3) -0.005(3) 0.003(2) 0.001(2) C37A 0.069(4) 0.077(5) 0.090(5) 0.020(4) 0.013(4) -0.024(3) C38A 0.042(4) 0.134(7) 0.129(8) -0.034(6) 0.002(4) -0.003(4) C39A 0.050(3) 0.054(3) 0.074(4) 0.001(3) 0.002(3) 0.010(3) C21A 0.040(3) 0.053(3) 0.043(3) -0.002(2) -0.006(2) 0.008(2) C22A 0.039(3) 0.046(3) 0.055(3) 0.001(2) 0.005(2) 0.010(2) C23A 0.046(3) 0.062(4) 0.050(3) 0.000(3) 0.010(2) 0.005(2) C24A 0.061(4) 0.077(4) 0.041(3) -0.001(3) 0.003(3) 0.014(3) C25A 0.062(4) 0.068(4) 0.053(4) -0.013(3) -0.010(3) 0.013(3) C26A 0.044(3) 0.057(3) 0.049(3) -0.004(3) -0.007(2) 0.006(2) C27A 0.050(3) 0.060(3) 0.061(4) -0.003(3) 0.001(3) -0.008(3) C28A 0.086(5) 0.114(5) 0.048(4) 0.010(5) 0.013(4) 0.019(4) C29A 0.064(4) 0.062(4) 0.071(4) -0.001(3) -0.028(3) 0.000(3) C51A 0.051(3) 0.043(3) 0.052(3) 0.000(2) -0.006(2) 0.003(2) C52A 0.061(4) 0.045(3) 0.061(4) 0.003(3) -0.009(3) 0.003(3) F52A 0.067(2) 0.074(2) 0.090(3) 0.016(2) -0.007(2) -0.0233(18) C53A 0.063(4) 0.054(4) 0.097(6) -0.022(4) -0.024(4) 0.003(3) F53A 0.074(3) 0.084(3) 0.152(5) -0.024(3) -0.044(3) -0.017(2) C54A 0.101(6) 0.076(5) 0.074(5) -0.018(4) -0.041(4) 0.022(4) F54A 0.150(4) 0.105(3) 0.097(4) -0.021(3) -0.078(3) 0.021(3) C55A 0.105(6) 0.092(5) 0.045(4) -0.003(4) -0.016(4) 0.008(5) F55A 0.163(5) 0.177(5) 0.053(3) 0.028(4) -0.022(3) 0.009(4) C56A 0.071(4) 0.068(4) 0.053(4) 0.005(3) -0.008(3) -0.003(3) F56A 0.088(3) 0.113(3) 0.070(3) 0.035(2) -0.004(2) -0.027(2) C41A 0.052(3) 0.043(3) 0.040(3) 0.001(2) -0.005(2) -0.005(2) C42A 0.057(3) 0.052(3) 0.056(3) -0.006(3) -0.003(3) -0.007(3) F42A 0.065(2) 0.058(2) 0.129(4) -0.036(2) 0.004(2) -0.0127(17) C43A 0.056(4) 0.063(4) 0.068(4) -0.004(3) 0.006(3) -0.019(3) F43A 0.057(2) 0.087(3) 0.173(5) -0.027(3) 0.011(3) -0.031(2) C44A 0.059(4) 0.065(4) 0.062(4) 0.000(3) 0.011(3) -0.004(3) F44A 0.053(2) 0.103(3) 0.125(4) -0.006(3) 0.022(2) -0.002(2) C45A 0.057(4) 0.053(3) 0.085(5) -0.010(3) 0.007(3) 0.005(3) F45A 0.079(3) 0.067(3) 0.145(4) -0.035(3) 0.012(3) 0.011(2) C46A 0.059(4) 0.043(3) 0.073(4) -0.004(3) 0.000(3) -0.005(3) F46A 0.059(2) 0.050(2) 0.155(4) -0.030(2) -0.008(2) -0.0055(16) C11A 0.080(5) 0.068(4) 0.086(5) 0.011(4) 0.021(4) 0.026(3) C12A 0.096(5) 0.049(4) 0.062(4) 0.008(3) 0.000(4) 0.007(3) C13A 0.139(7) 0.052(3) 0.077(5) -0.006(4) -0.033(6) -0.016(4) C14A 0.209(13) 0.068(6) 0.063(5) -0.019(4) -0.007(6) 0.041(7) C15A 0.151(9) 0.092(7) 0.084(7) 0.002(5) 0.055(6) 0.047(7) C16A 0.090(6) 0.114(7) 0.061(5) 0.011(4) -0.024(4) 0.015(5) C17A 0.089(6) 0.115(7) 0.073(5) -0.039(5) -0.028(4) 0.013(5) C18A 0.055(4) 0.090(5) 0.098(6) -0.023(4) -0.004(4) -0.001(3) C19A 0.054(3) 0.074(4) 0.076(5) -0.009(4) -0.011(4) 0.001(3) C20A 0.077(4) 0.070(4) 0.063(4) 0.005(3) -0.019(3) 0.011(3) Zr1B 0.0554(3) 0.0561(3) 0.0438(3) -0.0026(3) -0.0032(3) 0.0051(2) P1B 0.0399(7) 0.0396(7) 0.0456(7) -0.0008(6) -0.0025(6) -0.0023(5) B1B 0.046(3) 0.048(3) 0.050(4) -0.001(3) 0.000(3) -0.003(3) C1B 0.048(3) 0.040(3) 0.047(3) -0.001(2) -0.003(2) -0.003(2) C2B 0.047(3) 0.040(3) 0.070(4) -0.007(3) -0.002(3) -0.003(2) C4B 0.061(4) 0.046(3) 0.053(3) 0.002(3) 0.010(3) 0.003(2) C3B 0.073(4) 0.081(5) 0.071(4) 0.015(4) 0.000(3) 0.019(4) C31B 0.039(3) 0.047(3) 0.049(3) 0.002(2) -0.002(2) -0.001(2) C32B 0.041(3) 0.046(3) 0.056(3) -0.001(2) -0.004(2) -0.002(2) C33B 0.041(3) 0.060(3) 0.055(3) -0.005(3) -0.001(2) -0.011(2) C34B 0.036(3) 0.076(4) 0.056(3) -0.008(3) -0.002(3) 0.006(3) C35B 0.052(3) 0.055(4) 0.064(4) 0.003(3) -0.006(3) 0.014(3) C36B 0.051(3) 0.047(3) 0.060(4) 0.006(3) -0.007(2) 0.004(2) C37B 0.051(3) 0.046(3) 0.074(4) -0.001(3) -0.011(3) -0.007(2) C38B 0.041(3) 0.103(6) 0.092(5) 0.004(4) -0.005(3) 0.013(3) C39B 0.060(4) 0.053(4) 0.098(5) 0.016(3) -0.012(3) 0.007(3) C21B 0.039(3) 0.047(3) 0.040(3) -0.002(2) -0.002(2) -0.006(2) C22B 0.045(3) 0.052(3) 0.049(3) -0.004(3) 0.001(2) -0.008(2) C23B 0.061(4) 0.067(4) 0.046(3) -0.006(3) -0.001(3) -0.011(3) C24B 0.062(4) 0.057(4) 0.053(3) 0.002(3) -0.007(3) -0.015(3) C25B 0.049(3) 0.051(3) 0.060(4) 0.004(3) -0.011(3) 0.000(2) C26B 0.039(3) 0.046(3) 0.050(3) 0.000(2) -0.006(2) -0.007(2) C27B 0.065(4) 0.055(4) 0.053(4) -0.008(3) 0.011(3) -0.005(3) C28B 0.090(4) 0.084(4) 0.051(3) 0.010(4) -0.008(4) -0.008(3) C29B 0.061(4) 0.061(4) 0.062(4) 0.001(3) 0.004(3) 0.013(3) C51B 0.051(3) 0.039(3) 0.055(3) 0.004(2) -0.001(3) -0.005(2) C52B 0.046(3) 0.051(3) 0.069(4) -0.007(3) 0.000(3) -0.005(2) F52B 0.061(2) 0.104(3) 0.092(3) -0.048(3) 0.010(2) -0.004(2) C53B 0.058(4) 0.055(4) 0.079(5) 0.007(3) 0.003(3) 0.003(3) F53B 0.060(2) 0.083(3) 0.118(4) -0.011(3) 0.010(2) 0.0107(19) C54B 0.049(4) 0.064(4) 0.086(5) 0.010(4) -0.014(3) -0.012(3) F54B 0.054(2) 0.101(3) 0.143(4) 0.012(3) -0.031(2) -0.017(2) C55B 0.084(5) 0.072(4) 0.068(4) -0.012(4) -0.020(4) -0.028(4) F55B 0.099(3) 0.144(5) 0.112(4) -0.046(3) -0.022(3) -0.045(3) C56B 0.063(4) 0.059(4) 0.067(4) -0.012(3) 0.001(3) -0.014(3) F56B 0.084(3) 0.098(3) 0.106(3) -0.055(3) 0.015(2) -0.032(2) C41B 0.050(3) 0.040(3) 0.054(3) 0.002(2) -0.003(2) -0.005(2) C42B 0.056(3) 0.051(3) 0.048(3) -0.001(3) 0.002(3) -0.007(3) F42B 0.069(2) 0.063(2) 0.059(2) 0.0070(18) 0.0042(17) 0.0187(16) C43B 0.065(4) 0.046(3) 0.070(4) -0.011(3) 0.013(3) -0.008(3) F43B 0.070(2) 0.075(2) 0.092(3) -0.011(2) 0.026(2) 0.0075(19) C44B 0.071(4) 0.073(4) 0.045(3) -0.009(3) 0.017(3) -0.023(3) F44B 0.103(3) 0.101(3) 0.062(3) -0.023(2) 0.033(2) -0.031(2) C45B 0.073(4) 0.073(4) 0.045(3) 0.011(3) -0.001(3) -0.024(3) F45B 0.091(3) 0.118(4) 0.059(2) 0.021(2) -0.002(2) -0.028(2) C46B 0.052(3) 0.056(3) 0.058(4) 0.007(3) -0.001(3) -0.010(3) F46B 0.070(2) 0.074(2) 0.070(2) 0.0215(19) -0.0057(18) 0.0025(18) C11B 0.085(5) 0.107(6) 0.070(5) -0.009(4) -0.026(4) 0.000(5) C12B 0.120(7) 0.094(6) 0.065(5) -0.022(4) -0.007(5) -0.008(5) C13B 0.094(5) 0.053(4) 0.086(6) -0.021(3) -0.011(4) 0.003(3) C14B 0.089(5) 0.060(4) 0.068(4) -0.004(3) -0.011(4) -0.017(4) C15B 0.063(4) 0.078(4) 0.085(6) -0.024(4) -0.017(4) -0.009(3) C16B 0.073(5) 0.105(6) 0.070(5) 0.025(4) 0.020(4) 0.010(4) C17B 0.073(4) 0.100(6) 0.048(4) -0.016(3) 0.008(3) 0.008(4) C18B 0.060(3) 0.071(4) 0.063(4) -0.014(3) -0.001(3) 0.013(3) C19B 0.050(4) 0.076(4) 0.082(5) -0.010(4) 0.000(3) 0.001(3) C20B 0.067(4) 0.065(4) 0.111(7) 0.012(4) 0.033(4) 0.004(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 Zr1A C3A 2.223(7) . ? Zr1A C13A 2.473(6) . ? Zr1A C14A 2.479(8) . ? Zr1A C17A 2.478(7) . ? Zr1A C18A 2.490(7) . ? Zr1A C20A 2.507(6) . ? Zr1A C15A 2.508(8) . ? Zr1A C19A 2.515(6) . ? Zr1A C16A 2.519(7) . ? Zr1A C12A 2.520(6) . ? Zr1A C11A 2.522(7) . ? Zr1A P1A 2.9582(15) . ? P1A C21A 1.839(6) . ? P1A C31A 1.856(5) . ? P1A C1A 1.863(5) . ? B1A C4A 1.641(8) . ? B1A C2A 1.641(8) . ? B1A C51A 1.666(8) . ? B1A C41A 1.670(8) . ? C1A C2A 1.522(7) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C4A H4A3 0.9700 . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C3A H3A3 0.9700 . ? C31A C36A 1.406(8) . ? C31A C32A 1.418(8) . ? C32A C33A 1.392(9) . ? C32A C37A 1.502(9) . ? C33A C34A 1.374(10) . ? C33A H33A 0.9400 . ? C34A C35A 1.388(10) . ? C34A C38A 1.509(9) . ? C35A C36A 1.384(8) . ? C35A H35A 0.9400 . ? C36A C39A 1.526(8) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C37A H37C 0.9700 . ? C38A H38A 0.9700 . ? C38A H38B 0.9700 . ? C38A H38C 0.9700 . ? C39A H39A 0.9700 . ? C39A H39B 0.9700 . ? C39A H39C 0.9700 . ? C21A C26A 1.413(7) . ? C21A C22A 1.424(7) . ? C22A C23A 1.388(8) . ? C22A C27A 1.489(8) . ? C23A C24A 1.382(8) . ? C23A H23A 0.9400 . ? C24A C25A 1.397(9) . ? C24A C28A 1.506(9) . ? C25A C26A 1.391(9) . ? C25A H25A 0.9400 . ? C26A C29A 1.537(8) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C27A H27C 0.9700 . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C28A H28C 0.9700 . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C29A H29C 0.9700 . ? C51A C56A 1.374(8) . ? C51A C52A 1.392(8) . ? C52A F52A 1.323(7) . ? C52A C53A 1.392(9) . ? C53A F53A 1.355(8) . ? C53A C54A 1.355(12) . ? C54A F54A 1.350(8) . ? C54A C55A 1.361(12) . ? C55A F55A 1.348(9) . ? C55A C56A 1.388(9) . ? C56A F56A 1.350(7) . ? C41A C42A 1.377(7) . ? C41A C46A 1.385(8) . ? C42A F42A 1.338(6) . ? C42A C43A 1.403(8) . ? C43A F43A 1.338(7) . ? C43A C44A 1.344(9) . ? C44A F44A 1.349(7) . ? C44A C45A 1.358(9) . ? C45A F45A 1.344(7) . ? C45A C46A 1.385(8) . ? C46A F46A 1.364(6) . ? C11A C15A 1.393(13) . ? C11A C12A 1.402(10) . ? C11A H11A 0.9400 . ? C12A C13A 1.391(11) . ? C12A H12A 0.9400 . ? C13A C14A 1.374(14) . ? C13A H13A 0.9400 . ? C14A C15A 1.403(14) . ? C14A H14A 0.9400 . ? C15A H15A 0.9400 . ? C16A C17A 1.368(11) . ? C16A C20A 1.415(10) . ? C16A H16A 0.9400 . ? C17A C18A 1.413(12) . ? C17A H17A 0.9400 . ? C18A C19A 1.382(10) . ? C18A H18A 0.9400 . ? C19A C20A 1.368(10) . ? C19A H19A 0.9400 . ? C20A H20A 0.9400 . ? Zr1B C3B 2.247(6) . ? Zr1B C12B 2.479(8) . ? Zr1B C18B 2.480(6) . ? Zr1B C17B 2.483(6) . ? Zr1B C13B 2.499(6) . ? Zr1B C11B 2.504(7) . ? Zr1B C16B 2.515(7) . ? Zr1B C19B 2.516(6) . ? Zr1B C14B 2.515(7) . ? Zr1B C15B 2.517(6) . ? Zr1B C20B 2.522(7) . ? Zr1B P1B 2.9239(15) . ? P1B C21B 1.843(5) . ? P1B C1B 1.860(5) . ? P1B C31B 1.864(5) . ? B1B C4B 1.626(9) . ? B1B C51B 1.661(8) . ? B1B C41B 1.664(9) . ? B1B C2B 1.667(8) . ? C1B C2B 1.532(7) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C4B H4B3 0.9700 . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C3B H3B3 0.9700 . ? C31B C36B 1.416(7) . ? C31B C32B 1.420(7) . ? C32B C33B 1.375(7) . ? C32B C37B 1.532(7) . ? C33B C34B 1.383(8) . ? C33B H33B 0.9400 . ? C34B C35B 1.397(9) . ? C34B C38B 1.502(8) . ? C35B C36B 1.391(8) . ? C35B H35B 0.9400 . ? C36B C39B 1.519(8) . ? C37B H37D 0.9700 . ? C37B H37E 0.9700 . ? C37B H37F 0.9700 . ? C38B H38D 0.9700 . ? C38B H38E 0.9700 . ? C38B H38F 0.9700 . ? C39B H39D 0.9700 . ? C39B H39E 0.9700 . ? C39B H39F 0.9700 . ? C21B C22B 1.418(8) . ? C21B C26B 1.435(7) . ? C22B C23B 1.382(8) . ? C22B C27B 1.514(8) . ? C23B C24B 1.397(9) . ? C23B H23B 0.9400 . ? C24B C25B 1.360(9) . ? C24B C28B 1.514(9) . ? C25B C26B 1.392(8) . ? C25B H25B 0.9400 . ? C26B C29B 1.477(8) . ? C27B H27D 0.9700 . ? C27B H27E 0.9700 . ? C27B H27F 0.9700 . ? C28B H28D 0.9700 . ? C28B H28E 0.9700 . ? C28B H28F 0.9700 . ? C29B H29D 0.9700 . ? C29B H29E 0.9700 . ? C29B H29F 0.9700 . ? C51B C56B 1.386(8) . ? C51B C52B 1.391(8) . ? C52B F52B 1.354(7) . ? C52B C53B 1.382(8) . ? C53B F53B 1.340(8) . ? C53B C54B 1.366(10) . ? C54B F54B 1.340(7) . ? C54B C55B 1.380(10) . ? C55B F55B 1.344(8) . ? C55B C56B 1.380(9) . ? C56B F56B 1.366(7) . ? C41B C46B 1.393(8) . ? C41B C42B 1.396(8) . ? C42B F42B 1.346(7) . ? C42B C43B 1.372(8) . ? C43B F43B 1.360(7) . ? C43B C44B 1.376(10) . ? C44B F44B 1.343(7) . ? C44B C45B 1.377(10) . ? C45B F45B 1.348(7) . ? C45B C46B 1.379(9) . ? C46B F46B 1.350(7) . ? C11B C12B 1.373(11) . ? C11B C15B 1.381(11) . ? C11B H11B 0.9400 . ? C12B C13B 1.400(11) . ? C12B H12B 0.9400 . ? C13B C14B 1.408(10) . ? C13B H13B 0.9400 . ? C14B C15B 1.403(10) . ? C14B H14B 0.9400 . ? C15B H15B 0.9400 . ? C16B C20B 1.391(11) . ? C16B C17B 1.398(10) . ? C16B H16B 0.9400 . ? C17B C18B 1.392(10) . ? C17B H17B 0.9400 . ? C18B C19B 1.382(9) . ? C18B H18B 0.9400 . ? C19B C20B 1.366(10) . ? C19B H19B 0.9400 . ? C20B H20B 0.9400 . ? 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 C3A Zr1A C13A 128.8(3) . . ? C3A Zr1A C14A 99.6(4) . . ? C13A Zr1A C14A 32.2(3) . . ? C3A Zr1A C17A 99.7(3) . . ? C13A Zr1A C17A 86.4(3) . . ? C14A Zr1A C17A 76.6(3) . . ? C3A Zr1A C18A 129.1(3) . . ? C13A Zr1A C18A 79.2(3) . . ? C14A Zr1A C18A 87.6(4) . . ? C17A Zr1A C18A 33.0(3) . . ? C3A Zr1A C20A 86.5(3) . . ? C13A Zr1A C20A 132.7(3) . . ? C14A Zr1A C20A 130.0(3) . . ? C17A Zr1A C20A 53.5(3) . . ? C18A Zr1A C20A 53.6(3) . . ? C3A Zr1A C15A 75.6(3) . . ? C13A Zr1A C15A 53.6(4) . . ? C14A Zr1A C15A 32.7(3) . . ? C17A Zr1A C15A 102.2(4) . . ? C18A Zr1A C15A 119.9(4) . . ? C20A Zr1A C15A 147.1(3) . . ? C3A Zr1A C19A 118.1(3) . . ? C13A Zr1A C19A 106.2(3) . . ? C14A Zr1A C19A 119.6(4) . . ? C17A Zr1A C19A 53.2(3) . . ? C18A Zr1A C19A 32.0(2) . . ? C20A Zr1A C19A 31.6(2) . . ? C15A Zr1A C19A 151.9(4) . . ? C3A Zr1A C16A 75.5(3) . . ? C13A Zr1A C16A 117.6(3) . . ? C14A Zr1A C16A 100.7(3) . . ? C17A Zr1A C16A 31.8(3) . . ? C18A Zr1A C16A 53.7(3) . . ? C20A Zr1A C16A 32.7(2) . . ? C15A Zr1A C16A 114.9(3) . . ? C19A Zr1A C16A 52.9(3) . . ? C3A Zr1A C12A 119.6(3) . . ? C13A Zr1A C12A 32.3(2) . . ? C14A Zr1A C12A 53.3(3) . . ? C17A Zr1A C12A 118.6(3) . . ? C18A Zr1A C12A 105.1(3) . . ? C20A Zr1A C12A 153.8(3) . . ? C15A Zr1A C12A 53.1(3) . . ? C19A Zr1A C12A 122.2(2) . . ? C16A Zr1A C12A 149.9(3) . . ? C3A Zr1A C11A 87.3(3) . . ? C13A Zr1A C11A 53.9(3) . . ? C14A Zr1A C11A 53.9(3) . . ? C17A Zr1A C11A 130.4(3) . . ? C18A Zr1A C11A 133.1(3) . . ? C20A Zr1A C11A 173.2(3) . . ? C15A Zr1A C11A 32.2(3) . . ? C19A Zr1A C11A 154.4(2) . . ? C16A Zr1A C11A 146.8(3) . . ? C12A Zr1A C11A 32.3(2) . . ? C3A Zr1A P1A 86.4(2) . . ? C13A Zr1A P1A 121.3(2) . . ? C14A Zr1A P1A 143.3(3) . . ? C17A Zr1A P1A 138.4(2) . . ? C18A Zr1A P1A 116.48(18) . . ? C20A Zr1A P1A 86.29(16) . . ? C15A Zr1A P1A 119.1(3) . . ? C19A Zr1A P1A 87.51(18) . . ? C16A Zr1A P1A 115.8(2) . . ? C12A Zr1A P1A 92.16(17) . . ? C11A Zr1A P1A 90.7(2) . . ? C21A P1A C31A 102.2(2) . . ? C21A P1A C1A 100.7(3) . . ? C31A P1A C1A 111.7(2) . . ? C21A P1A Zr1A 128.55(18) . . ? C31A P1A Zr1A 103.01(18) . . ? C1A P1A Zr1A 110.18(19) . . ? C4A B1A C2A 110.7(5) . . ? C4A B1A C51A 115.1(5) . . ? C2A B1A C51A 105.6(4) . . ? C4A B1A C41A 105.0(4) . . ? C2A B1A C41A 112.0(4) . . ? C51A B1A C41A 108.5(5) . . ? C2A C1A P1A 112.6(4) . . ? C2A C1A H1A1 109.1 . . ? P1A C1A H1A1 109.1 . . ? C2A C1A H1A2 109.1 . . ? P1A C1A H1A2 109.1 . . ? H1A1 C1A H1A2 107.8 . . ? C1A C2A B1A 111.0(4) . . ? C1A C2A H2A1 109.4 . . ? B1A C2A H2A1 109.4 . . ? C1A C2A H2A2 109.4 . . ? B1A C2A H2A2 109.4 . . ? H2A1 C2A H2A2 108.0 . . ? B1A C4A H4A1 109.5 . . ? B1A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? B1A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? Zr1A C3A H3A1 109.5 . . ? Zr1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? Zr1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C36A C31A C32A 118.9(5) . . ? C36A C31A P1A 117.6(4) . . ? C32A C31A P1A 123.5(4) . . ? C33A C32A C31A 118.5(6) . . ? C33A C32A C37A 115.7(6) . . ? C31A C32A C37A 125.9(5) . . ? C34A C33A C32A 123.1(6) . . ? C34A C33A H33A 118.5 . . ? C32A C33A H33A 118.5 . . ? C33A C34A C35A 117.6(6) . . ? C33A C34A C38A 121.1(7) . . ? C35A C34A C38A 121.2(7) . . ? C36A C35A C34A 122.2(6) . . ? C36A C35A H35A 118.9 . . ? C34A C35A H35A 118.9 . . ? C35A C36A C31A 119.7(5) . . ? C35A C36A C39A 115.4(5) . . ? C31A C36A C39A 124.9(5) . . ? C32A C37A H37A 109.5 . . ? C32A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C32A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C34A C38A H38A 109.5 . . ? C34A C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? C34A C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? C36A C39A H39A 109.5 . . ? C36A C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C36A C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? C26A C21A C22A 118.0(5) . . ? C26A C21A P1A 121.8(4) . . ? C22A C21A P1A 120.1(4) . . ? C23A C22A C21A 119.2(5) . . ? C23A C22A C27A 118.3(5) . . ? C21A C22A C27A 122.5(5) . . ? C24A C23A C22A 122.9(6) . . ? C24A C23A H23A 118.6 . . ? C22A C23A H23A 118.6 . . ? C23A C24A C25A 117.4(5) . . ? C23A C24A C28A 121.3(6) . . ? C25A C24A C28A 121.2(6) . . ? C26A C25A C24A 121.7(5) . . ? C26A C25A H25A 119.2 . . ? C24A C25A H25A 119.2 . . ? C25A C26A C21A 120.1(5) . . ? C25A C26A C29A 115.2(5) . . ? C21A C26A C29A 124.8(5) . . ? C22A C27A H27A 109.5 . . ? C22A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C22A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C24A C28A H28A 109.5 . . ? C24A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C24A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C26A C29A H29A 109.5 . . ? C26A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C26A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C56A C51A C52A 113.7(5) . . ? C56A C51A B1A 120.5(5) . . ? C52A C51A B1A 125.5(5) . . ? F52A C52A C53A 116.0(6) . . ? F52A C52A C51A 121.6(5) . . ? C53A C52A C51A 122.4(6) . . ? F53A C53A C54A 120.3(7) . . ? F53A C53A C52A 118.9(7) . . ? C54A C53A C52A 120.8(7) . . ? F54A C54A C53A 119.9(8) . . ? F54A C54A C55A 120.7(8) . . ? C53A C54A C55A 119.3(6) . . ? F55A C55A C54A 120.6(7) . . ? F55A C55A C56A 120.5(8) . . ? C54A C55A C56A 118.7(7) . . ? F56A C56A C51A 120.5(5) . . ? F56A C56A C55A 114.5(6) . . ? C51A C56A C55A 125.0(7) . . ? C42A C41A C46A 112.3(5) . . ? C42A C41A B1A 126.5(5) . . ? C46A C41A B1A 120.8(5) . . ? F42A C42A C41A 121.9(5) . . ? F42A C42A C43A 114.6(5) . . ? C41A C42A C43A 123.6(5) . . ? F43A C43A C44A 120.4(6) . . ? F43A C43A C42A 119.1(6) . . ? C44A C43A C42A 120.5(6) . . ? C43A C44A F44A 120.8(6) . . ? C43A C44A C45A 119.1(6) . . ? F44A C44A C45A 120.1(6) . . ? F45A C45A C44A 120.5(6) . . ? F45A C45A C46A 120.6(6) . . ? C44A C45A C46A 118.9(6) . . ? F46A C46A C41A 119.3(5) . . ? F46A C46A C45A 115.2(5) . . ? C41A C46A C45A 125.5(5) . . ? C15A C11A C12A 107.0(9) . . ? C15A C11A Zr1A 73.4(5) . . ? C12A C11A Zr1A 73.8(4) . . ? C15A C11A H11A 126.5 . . ? C12A C11A H11A 126.5 . . ? Zr1A C11A H11A 118.4 . . ? C13A C12A C11A 108.3(8) . . ? C13A C12A Zr1A 72.0(4) . . ? C11A C12A Zr1A 73.9(4) . . ? C13A C12A H12A 125.8 . . ? C11A C12A H12A 125.8 . . ? Zr1A C12A H12A 120.0 . . ? C14A C13A C12A 108.4(9) . . ? C14A C13A Zr1A 74.1(5) . . ? C12A C13A Zr1A 75.7(4) . . ? C14A C13A H13A 125.8 . . ? C12A C13A H13A 125.8 . . ? Zr1A C13A H13A 116.4 . . ? C13A C14A C15A 108.0(8) . . ? C13A C14A Zr1A 73.6(4) . . ? C15A C14A Zr1A 74.8(5) . . ? C13A C14A H14A 126.0 . . ? C15A C14A H14A 126.0 . . ? Zr1A C14A H14A 117.6 . . ? C11A C15A C14A 108.3(9) . . ? C11A C15A Zr1A 74.5(4) . . ? C14A C15A Zr1A 72.5(5) . . ? C11A C15A H15A 125.9 . . ? C14A C15A H15A 125.9 . . ? Zr1A C15A H15A 119.0 . . ? C17A C16A C20A 107.5(8) . . ? C17A C16A Zr1A 72.5(4) . . ? C20A C16A Zr1A 73.2(4) . . ? C17A C16A H16A 126.3 . . ? C20A C16A H16A 126.3 . . ? Zr1A C16A H16A 119.9 . . ? C16A C17A C18A 109.0(7) . . ? C16A C17A Zr1A 75.8(4) . . ? C18A C17A Zr1A 73.9(4) . . ? C16A C17A H17A 125.5 . . ? C18A C17A H17A 125.5 . . ? Zr1A C17A H17A 116.7 . . ? C19A C18A C17A 106.2(8) . . ? C19A C18A Zr1A 75.0(4) . . ? C17A C18A Zr1A 73.0(4) . . ? C19A C18A H18A 126.9 . . ? C17A C18A H18A 126.9 . . ? Zr1A C18A H18A 117.3 . . ? C20A C19A C18A 110.0(8) . . ? C20A C19A Zr1A 73.8(4) . . ? C18A C19A Zr1A 73.0(4) . . ? C20A C19A H19A 125.0 . . ? C18A C19A H19A 125.0 . . ? Zr1A C19A H19A 119.8 . . ? C19A C20A C16A 107.3(7) . . ? C19A C20A Zr1A 74.5(4) . . ? C16A C20A Zr1A 74.1(4) . . ? C19A C20A H20A 126.3 . . ? C16A C20A H20A 126.3 . . ? Zr1A C20A H20A 117.1 . . ? C3B Zr1B C12B 98.0(3) . . ? C3B Zr1B C18B 130.5(3) . . ? C12B Zr1B C18B 95.1(3) . . ? C3B Zr1B C17B 106.2(3) . . ? C12B Zr1B C17B 77.0(3) . . ? C18B Zr1B C17B 32.6(2) . . ? C3B Zr1B C13B 128.3(3) . . ? C12B Zr1B C13B 32.7(3) . . ? C18B Zr1B C13B 82.6(2) . . ? C17B Zr1B C13B 81.8(3) . . ? C3B Zr1B C11B 74.9(3) . . ? C12B Zr1B C11B 32.0(3) . . ? C18B Zr1B C11B 126.9(3) . . ? C17B Zr1B C11B 104.4(3) . . ? C13B Zr1B C11B 54.1(3) . . ? C3B Zr1B C16B 77.9(3) . . ? C12B Zr1B C16B 96.3(3) . . ? C18B Zr1B C16B 53.3(2) . . ? C17B Zr1B C16B 32.5(2) . . ? C13B Zr1B C16B 111.8(3) . . ? C11B Zr1B C16B 111.9(3) . . ? C3B Zr1B C19B 112.5(3) . . ? C12B Zr1B C19B 126.6(3) . . ? C18B Zr1B C19B 32.1(2) . . ? C17B Zr1B C19B 53.5(2) . . ? C13B Zr1B C19B 112.6(2) . . ? C11B Zr1B C19B 157.5(3) . . ? C16B Zr1B C19B 52.7(3) . . ? C3B Zr1B C14B 119.4(3) . . ? C12B Zr1B C14B 52.9(3) . . ? C18B Zr1B C14B 106.4(2) . . ? C17B Zr1B C14B 113.9(3) . . ? C13B Zr1B C14B 32.6(2) . . ? C11B Zr1B C14B 52.9(3) . . ? C16B Zr1B C14B 144.4(3) . . ? C19B Zr1B C14B 127.7(2) . . ? C3B Zr1B C15B 87.0(3) . . ? C12B Zr1B C15B 53.2(3) . . ? C18B Zr1B C15B 136.6(2) . . ? C17B Zr1B C15B 129.9(2) . . ? C13B Zr1B C15B 54.5(2) . . ? C11B Zr1B C15B 31.9(3) . . ? C16B Zr1B C15B 143.8(3) . . ? C19B Zr1B C15B 159.2(3) . . ? C14B Zr1B C15B 32.4(2) . . ? C3B Zr1B C20B 82.1(3) . . ? C12B Zr1B C20B 127.6(3) . . ? C18B Zr1B C20B 53.0(2) . . ? C17B Zr1B C20B 53.6(3) . . ? C13B Zr1B C20B 133.3(2) . . ? C11B Zr1B C20B 141.8(3) . . ? C16B Zr1B C20B 32.1(3) . . ? C19B Zr1B C20B 31.5(2) . . ? C14B Zr1B C20B 158.5(2) . . ? C15B Zr1B C20B 169.1(2) . . ? C3B Zr1B P1B 83.7(2) . . ? C12B Zr1B P1B 143.1(2) . . ? C18B Zr1B P1B 111.83(16) . . ? C17B Zr1B P1B 138.21(17) . . ? C13B Zr1B P1B 124.12(19) . . ? C11B Zr1B P1B 117.3(2) . . ? C16B Zr1B P1B 119.9(2) . . ? C19B Zr1B P1B 85.01(17) . . ? C14B Zr1B P1B 94.03(17) . . ? C15B Zr1B P1B 90.27(18) . . ? C20B Zr1B P1B 89.3(2) . . ? C21B P1B C1B 101.3(2) . . ? C21B P1B C31B 103.5(2) . . ? C1B P1B C31B 110.4(2) . . ? C21B P1B Zr1B 125.44(17) . . ? C1B P1B Zr1B 110.76(18) . . ? C31B P1B Zr1B 104.95(17) . . ? C4B B1B C51B 103.7(4) . . ? C4B B1B C41B 114.5(5) . . ? C51B B1B C41B 110.0(5) . . ? C4B B1B C2B 111.5(5) . . ? C51B B1B C2B 113.2(5) . . ? C41B B1B C2B 104.2(4) . . ? C2B C1B P1B 115.9(4) . . ? C2B C1B H1B1 108.3 . . ? P1B C1B H1B1 108.3 . . ? C2B C1B H1B2 108.3 . . ? P1B C1B H1B2 108.3 . . ? H1B1 C1B H1B2 107.4 . . ? C1B C2B B1B 109.4(4) . . ? C1B C2B H2B1 109.8 . . ? B1B C2B H2B1 109.8 . . ? C1B C2B H2B2 109.8 . . ? B1B C2B H2B2 109.8 . . ? H2B1 C2B H2B2 108.2 . . ? B1B C4B H4B1 109.5 . . ? B1B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? B1B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? Zr1B C3B H3B1 109.5 . . ? Zr1B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? Zr1B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C36B C31B C32B 118.0(5) . . ? C36B C31B P1B 124.4(4) . . ? C32B C31B P1B 117.6(4) . . ? C33B C32B C31B 119.8(5) . . ? C33B C32B C37B 116.0(5) . . ? C31B C32B C37B 124.2(5) . . ? C32B C33B C34B 123.3(5) . . ? C32B C33B H33B 118.3 . . ? C34B C33B H33B 118.3 . . ? C33B C34B C35B 116.7(5) . . ? C33B C34B C38B 122.2(6) . . ? C35B C34B C38B 121.0(6) . . ? C36B C35B C34B 122.6(5) . . ? C36B C35B H35B 118.7 . . ? C34B C35B H35B 118.7 . . ? C35B C36B C31B 119.5(5) . . ? C35B C36B C39B 114.8(5) . . ? C31B C36B C39B 125.7(5) . . ? C32B C37B H37D 109.5 . . ? C32B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C32B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C34B C38B H38D 109.5 . . ? C34B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C34B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C36B C39B H39D 109.5 . . ? C36B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C36B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C22B C21B C26B 119.3(5) . . ? C22B C21B P1B 122.1(4) . . ? C26B C21B P1B 118.4(4) . . ? C23B C22B C21B 118.7(5) . . ? C23B C22B C27B 116.6(5) . . ? C21B C22B C27B 124.7(5) . . ? C22B C23B C24B 122.5(6) . . ? C22B C23B H23B 118.8 . . ? C24B C23B H23B 118.8 . . ? C25B C24B C23B 117.8(5) . . ? C25B C24B C28B 121.8(6) . . ? C23B C24B C28B 120.3(6) . . ? C24B C25B C26B 123.6(5) . . ? C24B C25B H25B 118.2 . . ? C26B C25B H25B 118.2 . . ? C25B C26B C21B 117.6(5) . . ? C25B C26B C29B 118.9(5) . . ? C21B C26B C29B 123.4(5) . . ? C22B C27B H27D 109.5 . . ? C22B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C22B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C24B C28B H28D 109.5 . . ? C24B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C24B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C26B C29B H29D 109.5 . . ? C26B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C26B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C56B C51B C52B 110.6(5) . . ? C56B C51B B1B 126.5(5) . . ? C52B C51B B1B 122.1(5) . . ? F52B C52B C53B 114.2(5) . . ? F52B C52B C51B 119.4(5) . . ? C53B C52B C51B 126.3(6) . . ? F53B C53B C54B 119.8(6) . . ? F53B C53B C52B 121.2(6) . . ? C54B C53B C52B 119.1(6) . . ? F54B C54B C53B 121.4(7) . . ? F54B C54B C55B 120.1(6) . . ? C53B C54B C55B 118.5(6) . . ? F55B C55B C54B 119.8(6) . . ? F55B C55B C56B 121.0(7) . . ? C54B C55B C56B 119.1(6) . . ? F56B C56B C55B 114.0(6) . . ? F56B C56B C51B 119.9(5) . . ? C55B C56B C51B 126.2(6) . . ? C46B C41B C42B 112.5(5) . . ? C46B C41B B1B 120.5(5) . . ? C42B C41B B1B 126.7(5) . . ? F42B C42B C43B 115.0(5) . . ? F42B C42B C41B 120.7(5) . . ? C43B C42B C41B 124.3(6) . . ? F43B C43B C42B 120.7(6) . . ? F43B C43B C44B 118.8(6) . . ? C42B C43B C44B 120.5(6) . . ? F44B C44B C43B 121.3(6) . . ? F44B C44B C45B 120.5(6) . . ? C43B C44B C45B 118.2(6) . . ? F45B C45B C44B 119.5(6) . . ? F45B C45B C46B 121.1(6) . . ? C44B C45B C46B 119.5(6) . . ? F46B C46B C45B 115.5(5) . . ? F46B C46B C41B 119.5(5) . . ? C45B C46B C41B 125.0(6) . . ? C12B C11B C15B 108.7(7) . . ? C12B C11B Zr1B 73.0(4) . . ? C15B C11B Zr1B 74.6(4) . . ? C12B C11B H11B 125.7 . . ? C15B C11B H11B 125.7 . . ? Zr1B C11B H11B 118.6 . . ? C11B C12B C13B 110.1(8) . . ? C11B C12B Zr1B 75.0(5) . . ? C13B C12B Zr1B 74.4(4) . . ? C11B C12B H12B 124.9 . . ? C13B C12B H12B 124.9 . . ? Zr1B C12B H12B 117.4 . . ? C12B C13B C14B 104.8(7) . . ? C12B C13B Zr1B 72.9(4) . . ? C14B C13B Zr1B 74.3(4) . . ? C12B C13B H13B 127.6 . . ? C14B C13B H13B 127.6 . . ? Zr1B C13B H13B 117.5 . . ? C15B C14B C13B 109.6(7) . . ? C15B C14B Zr1B 73.9(4) . . ? C13B C14B Zr1B 73.0(4) . . ? C15B C14B H14B 125.2 . . ? C13B C14B H14B 125.2 . . ? Zr1B C14B H14B 119.6 . . ? C11B C15B C14B 106.7(7) . . ? C11B C15B Zr1B 73.5(4) . . ? C14B C15B Zr1B 73.7(4) . . ? C11B C15B H15B 126.6 . . ? C14B C15B H15B 126.6 . . ? Zr1B C15B H15B 118.2 . . ? C20B C16B C17B 108.0(7) . . ? C20B C16B Zr1B 74.2(4) . . ? C17B C16B Zr1B 72.5(4) . . ? C20B C16B H16B 126.0 . . ? C17B C16B H16B 126.0 . . ? Zr1B C16B H16B 119.2 . . ? C18B C17B C16B 106.9(6) . . ? C18B C17B Zr1B 73.6(4) . . ? C16B C17B Zr1B 75.0(4) . . ? C18B C17B H17B 126.6 . . ? C16B C17B H17B 126.6 . . ? Zr1B C17B H17B 117.0 . . ? C19B C18B C17B 108.3(6) . . ? C19B C18B Zr1B 75.4(4) . . ? C17B C18B Zr1B 73.8(4) . . ? C19B C18B H18B 125.8 . . ? C17B C18B H18B 125.8 . . ? Zr1B C18B H18B 117.0 . . ? C20B C19B C18B 108.6(7) . . ? C20B C19B Zr1B 74.5(4) . . ? C18B C19B Zr1B 72.5(4) . . ? C20B C19B H19B 125.7 . . ? C18B C19B H19B 125.7 . . ? Zr1B C19B H19B 119.1 . . ? C19B C20B C16B 108.1(7) . . ? C19B C20B Zr1B 74.0(4) . . ? C16B C20B Zr1B 73.7(4) . . ? C19B C20B H20B 125.9 . . ? C16B C20B H20B 125.9 . . ? Zr1B C20B H20B 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3A Zr1A P1A C21A 162.9(3) . . . . ? C13A Zr1A P1A C21A 28.7(3) . . . . ? C14A Zr1A P1A C21A 61.6(6) . . . . ? C17A Zr1A P1A C21A -96.4(4) . . . . ? C18A Zr1A P1A C21A -64.6(3) . . . . ? C20A Zr1A P1A C21A -110.4(3) . . . . ? C15A Zr1A P1A C21A 91.6(3) . . . . ? C19A Zr1A P1A C21A -78.8(3) . . . . ? C16A Zr1A P1A C21A -125.0(3) . . . . ? C12A Zr1A P1A C21A 43.4(3) . . . . ? C11A Zr1A P1A C21A 75.7(3) . . . . ? C3A Zr1A P1A C31A 45.4(3) . . . . ? C13A Zr1A P1A C31A -88.8(3) . . . . ? C14A Zr1A P1A C31A -56.0(6) . . . . ? C17A Zr1A P1A C31A 146.0(4) . . . . ? C18A Zr1A P1A C31A 177.9(3) . . . . ? C20A Zr1A P1A C31A 132.1(3) . . . . ? C15A Zr1A P1A C31A -25.9(3) . . . . ? C19A Zr1A P1A C31A 163.7(3) . . . . ? C16A Zr1A P1A C31A 117.4(3) . . . . ? C12A Zr1A P1A C31A -74.1(3) . . . . ? C11A Zr1A P1A C31A -41.8(3) . . . . ? C3A Zr1A P1A C1A -74.0(3) . . . . ? C13A Zr1A P1A C1A 151.8(3) . . . . ? C14A Zr1A P1A C1A -175.3(6) . . . . ? C17A Zr1A P1A C1A 26.7(4) . . . . ? C18A Zr1A P1A C1A 58.5(3) . . . . ? C20A Zr1A P1A C1A 12.7(3) . . . . ? C15A Zr1A P1A C1A -145.3(3) . . . . ? C19A Zr1A P1A C1A 44.4(3) . . . . ? C16A Zr1A P1A C1A -1.9(3) . . . . ? C12A Zr1A P1A C1A 166.5(3) . . . . ? C11A Zr1A P1A C1A -161.2(3) . . . . ? C21A P1A C1A C2A 53.7(5) . . . . ? C31A P1A C1A C2A 161.7(4) . . . . ? Zr1A P1A C1A C2A -84.4(4) . . . . ? P1A C1A C2A B1A -164.3(4) . . . . ? C4A B1A C2A C1A -58.7(6) . . . . ? C51A B1A C2A C1A 66.6(6) . . . . ? C41A B1A C2A C1A -175.5(5) . . . . ? C21A P1A C31A C36A -48.4(5) . . . . ? C1A P1A C31A C36A -155.4(4) . . . . ? Zr1A P1A C31A C36A 86.4(5) . . . . ? C21A P1A C31A C32A 131.1(5) . . . . ? C1A P1A C31A C32A 24.1(6) . . . . ? Zr1A P1A C31A C32A -94.1(5) . . . . ? C36A C31A C32A C33A 3.0(9) . . . . ? P1A C31A C32A C33A -176.5(5) . . . . ? C36A C31A C32A C37A -178.2(6) . . . . ? P1A C31A C32A C37A 2.3(9) . . . . ? C31A C32A C33A C34A -1.9(10) . . . . ? C37A C32A C33A C34A 179.2(7) . . . . ? C32A C33A C34A C35A -0.3(11) . . . . ? C32A C33A C34A C38A -177.9(7) . . . . ? C33A C34A C35A C36A 1.5(10) . . . . ? C38A C34A C35A C36A 179.1(6) . . . . ? C34A C35A C36A C31A -0.3(10) . . . . ? C34A C35A C36A C39A 177.9(6) . . . . ? C32A C31A C36A C35A -1.9(9) . . . . ? P1A C31A C36A C35A 177.6(4) . . . . ? C32A C31A C36A C39A 180.0(5) . . . . ? P1A C31A C36A C39A -0.5(8) . . . . ? C31A P1A C21A C26A -41.8(5) . . . . ? C1A P1A C21A C26A 73.5(5) . . . . ? Zr1A P1A C21A C26A -159.7(3) . . . . ? C31A P1A C21A C22A 134.0(4) . . . . ? C1A P1A C21A C22A -110.7(4) . . . . ? Zr1A P1A C21A C22A 16.1(5) . . . . ? C26A C21A C22A C23A 7.0(7) . . . . ? P1A C21A C22A C23A -169.0(4) . . . . ? C26A C21A C22A C27A -170.9(5) . . . . ? P1A C21A C22A C27A 13.2(7) . . . . ? C21A C22A C23A C24A -0.5(8) . . . . ? C27A C22A C23A C24A 177.4(5) . . . . ? C22A C23A C24A C25A -6.8(9) . . . . ? C22A C23A C24A C28A 174.6(5) . . . . ? C23A C24A C25A C26A 7.8(9) . . . . ? C28A C24A C25A C26A -173.6(5) . . . . ? C24A C25A C26A C21A -1.4(9) . . . . ? C24A C25A C26A C29A 178.4(5) . . . . ? C22A C21A C26A C25A -6.0(8) . . . . ? P1A C21A C26A C25A 169.9(4) . . . . ? C22A C21A C26A C29A 174.2(5) . . . . ? P1A C21A C26A C29A -9.9(8) . . . . ? C4A B1A C51A C56A -166.3(5) . . . . ? C2A B1A C51A C56A 71.3(7) . . . . ? C41A B1A C51A C56A -48.9(7) . . . . ? C4A B1A C51A C52A 20.7(8) . . . . ? C2A B1A C51A C52A -101.8(6) . . . . ? C41A B1A C51A C52A 138.0(5) . . . . ? C56A C51A C52A F52A -178.8(6) . . . . ? B1A C51A C52A F52A -5.4(9) . . . . ? C56A C51A C52A C53A -0.9(9) . . . . ? B1A C51A C52A C53A 172.6(6) . . . . ? F52A C52A C53A F53A -1.7(9) . . . . ? C51A C52A C53A F53A -179.8(5) . . . . ? F52A C52A C53A C54A 179.2(6) . . . . ? C51A C52A C53A C54A 1.1(10) . . . . ? F53A C53A C54A F54A 2.1(10) . . . . ? C52A C53A C54A F54A -178.8(6) . . . . ? F53A C53A C54A C55A -178.5(7) . . . . ? C52A C53A C54A C55A 0.6(11) . . . . ? F54A C54A C55A F55A 0.7(12) . . . . ? C53A C54A C55A F55A -178.7(7) . . . . ? F54A C54A C55A C56A 177.0(7) . . . . ? C53A C54A C55A C56A -2.4(12) . . . . ? C52A C51A C56A F56A -179.5(6) . . . . ? B1A C51A C56A F56A 6.7(9) . . . . ? C52A C51A C56A C55A -1.0(10) . . . . ? B1A C51A C56A C55A -174.9(6) . . . . ? F55A C55A C56A F56A -2.5(11) . . . . ? C54A C55A C56A F56A -178.8(7) . . . . ? F55A C55A C56A C51A 179.0(7) . . . . ? C54A C55A C56A C51A 2.7(12) . . . . ? C4A B1A C41A C42A -101.6(6) . . . . ? C2A B1A C41A C42A 18.6(8) . . . . ? C51A B1A C41A C42A 134.8(6) . . . . ? C4A B1A C41A C46A 70.4(6) . . . . ? C2A B1A C41A C46A -169.4(5) . . . . ? C51A B1A C41A C46A -53.2(7) . . . . ? C46A C41A C42A F42A 177.9(6) . . . . ? B1A C41A C42A F42A -9.5(9) . . . . ? C46A C41A C42A C43A -1.5(9) . . . . ? B1A C41A C42A C43A 171.0(6) . . . . ? F42A C42A C43A F43A 3.2(9) . . . . ? C41A C42A C43A F43A -177.4(6) . . . . ? F42A C42A C43A C44A -178.2(6) . . . . ? C41A C42A C43A C44A 1.3(10) . . . . ? F43A C43A C44A F44A -2.7(11) . . . . ? C42A C43A C44A F44A 178.6(6) . . . . ? F43A C43A C44A C45A 179.4(7) . . . . ? C42A C43A C44A C45A 0.8(11) . . . . ? C43A C44A C45A F45A 177.8(7) . . . . ? F44A C44A C45A F45A 0.0(11) . . . . ? C43A C44A C45A C46A -2.4(11) . . . . ? F44A C44A C45A C46A 179.8(6) . . . . ? C42A C41A C46A F46A -179.5(6) . . . . ? B1A C41A C46A F46A 7.4(9) . . . . ? C42A C41A C46A C45A -0.2(9) . . . . ? B1A C41A C46A C45A -173.2(6) . . . . ? F45A C45A C46A F46A 1.3(10) . . . . ? C44A C45A C46A F46A -178.5(6) . . . . ? F45A C45A C46A C41A -178.0(6) . . . . ? C44A C45A C46A C41A 2.1(11) . . . . ? C3A Zr1A C11A C15A 66.9(7) . . . . ? C13A Zr1A C11A C15A -77.3(7) . . . . ? C14A Zr1A C11A C15A -37.1(6) . . . . ? C17A Zr1A C11A C15A -33.6(8) . . . . ? C18A Zr1A C11A C15A -78.3(7) . . . . ? C20A Zr1A C11A C15A 89(2) . . . . ? C19A Zr1A C11A C15A -121.0(8) . . . . ? C16A Zr1A C11A C15A 8.9(10) . . . . ? C12A Zr1A C11A C15A -113.8(9) . . . . ? P1A Zr1A C11A C15A 153.3(7) . . . . ? C3A Zr1A C11A C12A -179.3(5) . . . . ? C13A Zr1A C11A C12A 36.5(5) . . . . ? C14A Zr1A C11A C12A 76.7(5) . . . . ? C17A Zr1A C11A C12A 80.3(6) . . . . ? C18A Zr1A C11A C12A 35.6(6) . . . . ? C20A Zr1A C11A C12A -156.7(19) . . . . ? C15A Zr1A C11A C12A 113.8(9) . . . . ? C19A Zr1A C11A C12A -7.2(9) . . . . ? C16A Zr1A C11A C12A 122.7(6) . . . . ? P1A Zr1A C11A C12A -92.9(4) . . . . ? C15A C11A C12A C13A 2.1(8) . . . . ? Zr1A C11A C12A C13A -64.2(5) . . . . ? C15A C11A C12A Zr1A 66.4(6) . . . . ? C3A Zr1A C12A C13A 116.8(6) . . . . ? C14A Zr1A C12A C13A 37.3(6) . . . . ? C17A Zr1A C12A C13A -5.3(7) . . . . ? C18A Zr1A C12A C13A -37.9(6) . . . . ? C20A Zr1A C12A C13A -70.1(8) . . . . ? C15A Zr1A C12A C13A 78.5(7) . . . . ? C19A Zr1A C12A C13A -67.7(6) . . . . ? C16A Zr1A C12A C13A 2.8(9) . . . . ? C11A Zr1A C12A C13A 116.0(8) . . . . ? P1A Zr1A C12A C13A -156.1(5) . . . . ? C3A Zr1A C12A C11A 0.8(6) . . . . ? C13A Zr1A C12A C11A -116.0(8) . . . . ? C14A Zr1A C12A C11A -78.6(6) . . . . ? C17A Zr1A C12A C11A -121.3(5) . . . . ? C18A Zr1A C12A C11A -153.9(5) . . . . ? C20A Zr1A C12A C11A 173.9(5) . . . . ? C15A Zr1A C12A C11A -37.5(6) . . . . ? C19A Zr1A C12A C11A 176.4(5) . . . . ? C16A Zr1A C12A C11A -113.2(6) . . . . ? P1A Zr1A C12A C11A 87.9(5) . . . . ? C11A C12A C13A C14A -2.0(8) . . . . ? Zr1A C12A C13A C14A -67.5(5) . . . . ? C11A C12A C13A Zr1A 65.5(5) . . . . ? C3A Zr1A C13A C14A 29.2(8) . . . . ? C17A Zr1A C13A C14A -70.4(7) . . . . ? C18A Zr1A C13A C14A -102.9(7) . . . . ? C20A Zr1A C13A C14A -100.1(7) . . . . ? C15A Zr1A C13A C14A 37.6(6) . . . . ? C19A Zr1A C13A C14A -120.3(7) . . . . ? C16A Zr1A C13A C14A -64.1(7) . . . . ? C12A Zr1A C13A C14A 114.3(9) . . . . ? C11A Zr1A C13A C14A 77.8(7) . . . . ? P1A Zr1A C13A C14A 142.6(6) . . . . ? C3A Zr1A C13A C12A -85.0(6) . . . . ? C14A Zr1A C13A C12A -114.3(9) . . . . ? C17A Zr1A C13A C12A 175.4(6) . . . . ? C18A Zr1A C13A C12A 142.8(6) . . . . ? C20A Zr1A C13A C12A 145.6(5) . . . . ? C15A Zr1A C13A C12A -76.6(6) . . . . ? C19A Zr1A C13A C12A 125.4(5) . . . . ? C16A Zr1A C13A C12A -178.4(5) . . . . ? C11A Zr1A C13A C12A -36.5(5) . . . . ? P1A Zr1A C13A C12A 28.3(6) . . . . ? C12A C13A C14A C15A 1.1(9) . . . . ? Zr1A C13A C14A C15A -67.5(6) . . . . ? C12A C13A C14A Zr1A 68.6(5) . . . . ? C3A Zr1A C14A C13A -157.3(6) . . . . ? C17A Zr1A C14A C13A 104.9(7) . . . . ? C18A Zr1A C14A C13A 73.4(6) . . . . ? C20A Zr1A C14A C13A 109.2(6) . . . . ? C15A Zr1A C14A C13A -114.4(9) . . . . ? C19A Zr1A C14A C13A 72.5(7) . . . . ? C16A Zr1A C14A C13A 125.8(6) . . . . ? C12A Zr1A C14A C13A -37.4(5) . . . . ? C11A Zr1A C14A C13A -77.9(6) . . . . ? P1A Zr1A C14A C13A -60.3(9) . . . . ? C3A Zr1A C14A C15A -42.9(6) . . . . ? C13A Zr1A C14A C15A 114.4(9) . . . . ? C17A Zr1A C14A C15A -140.7(7) . . . . ? C18A Zr1A C14A C15A -172.2(6) . . . . ? C20A Zr1A C14A C15A -136.3(5) . . . . ? C19A Zr1A C14A C15A -173.1(5) . . . . ? C16A Zr1A C14A C15A -119.8(6) . . . . ? C12A Zr1A C14A C15A 77.0(6) . . . . ? C11A Zr1A C14A C15A 36.5(5) . . . . ? P1A Zr1A C14A C15A 54.2(9) . . . . ? C12A C11A C15A C14A -1.5(10) . . . . ? Zr1A C11A C15A C14A 65.2(6) . . . . ? C12A C11A C15A Zr1A -66.7(5) . . . . ? C13A C14A C15A C11A 0.2(10) . . . . ? Zr1A C14A C15A C11A -66.5(6) . . . . ? C13A C14A C15A Zr1A 66.7(6) . . . . ? C3A Zr1A C15A C11A -108.5(7) . . . . ? C13A Zr1A C15A C11A 78.3(6) . . . . ? C14A Zr1A C15A C11A 115.4(9) . . . . ? C17A Zr1A C15A C11A 154.5(6) . . . . ? C18A Zr1A C15A C11A 124.4(6) . . . . ? C20A Zr1A C15A C11A -167.4(5) . . . . ? C19A Zr1A C15A C11A 128.2(7) . . . . ? C16A Zr1A C15A C11A -174.7(6) . . . . ? C12A Zr1A C15A C11A 37.7(5) . . . . ? P1A Zr1A C15A C11A -31.0(7) . . . . ? C3A Zr1A C15A C14A 136.2(7) . . . . ? C13A Zr1A C15A C14A -37.1(5) . . . . ? C17A Zr1A C15A C14A 39.1(7) . . . . ? C18A Zr1A C15A C14A 9.0(7) . . . . ? C20A Zr1A C15A C14A 77.2(8) . . . . ? C19A Zr1A C15A C14A 12.9(10) . . . . ? C16A Zr1A C15A C14A 70.0(7) . . . . ? C12A Zr1A C15A C14A -77.7(6) . . . . ? C11A Zr1A C15A C14A -115.4(9) . . . . ? P1A Zr1A C15A C14A -146.3(6) . . . . ? C3A Zr1A C16A C17A -138.4(6) . . . . ? C13A Zr1A C16A C17A -11.9(6) . . . . ? C14A Zr1A C16A C17A -41.1(6) . . . . ? C18A Zr1A C16A C17A 37.8(5) . . . . ? C20A Zr1A C16A C17A 115.1(8) . . . . ? C15A Zr1A C16A C17A -72.2(6) . . . . ? C19A Zr1A C16A C17A 78.1(5) . . . . ? C12A Zr1A C16A C17A -13.6(9) . . . . ? C11A Zr1A C16A C17A -77.4(7) . . . . ? P1A Zr1A C16A C17A 142.9(5) . . . . ? C3A Zr1A C16A C20A 106.5(5) . . . . ? C13A Zr1A C16A C20A -127.0(5) . . . . ? C14A Zr1A C16A C20A -156.2(6) . . . . ? C17A Zr1A C16A C20A -115.1(8) . . . . ? C18A Zr1A C16A C20A -77.3(5) . . . . ? C15A Zr1A C16A C20A 172.7(5) . . . . ? C19A Zr1A C16A C20A -37.0(4) . . . . ? C12A Zr1A C16A C20A -128.7(6) . . . . ? C11A Zr1A C16A C20A 167.5(5) . . . . ? P1A Zr1A C16A C20A 27.8(6) . . . . ? C20A C16A C17A C18A -1.8(9) . . . . ? Zr1A C16A C17A C18A -67.1(6) . . . . ? C20A C16A C17A Zr1A 65.3(5) . . . . ? C3A Zr1A C17A C16A 40.7(6) . . . . ? C13A Zr1A C17A C16A 169.5(6) . . . . ? C14A Zr1A C17A C16A 138.4(6) . . . . ? C18A Zr1A C17A C16A -115.0(7) . . . . ? C20A Zr1A C17A C16A -37.5(5) . . . . ? C15A Zr1A C17A C16A 117.9(6) . . . . ? C19A Zr1A C17A C16A -77.2(5) . . . . ? C12A Zr1A C17A C16A 172.3(5) . . . . ? C11A Zr1A C17A C16A 135.4(5) . . . . ? P1A Zr1A C17A C16A -54.9(7) . . . . ? C3A Zr1A C17A C18A 155.7(5) . . . . ? C13A Zr1A C17A C18A -75.6(5) . . . . ? C14A Zr1A C17A C18A -106.6(6) . . . . ? C20A Zr1A C17A C18A 77.5(5) . . . . ? C15A Zr1A C17A C18A -127.1(5) . . . . ? C19A Zr1A C17A C18A 37.8(4) . . . . ? C16A Zr1A C17A C18A 115.0(7) . . . . ? C12A Zr1A C17A C18A -72.7(5) . . . . ? C11A Zr1A C17A C18A -109.6(5) . . . . ? P1A Zr1A C17A C18A 60.1(7) . . . . ? C16A C17A C18A C19A 0.0(9) . . . . ? Zr1A C17A C18A C19A -68.3(5) . . . . ? C16A C17A C18A Zr1A 68.3(6) . . . . ? C3A Zr1A C18A C19A 81.0(6) . . . . ? C13A Zr1A C18A C19A -147.2(6) . . . . ? C14A Zr1A C18A C19A -178.6(6) . . . . ? C17A Zr1A C18A C19A 112.5(8) . . . . ? C20A Zr1A C18A C19A 35.3(5) . . . . ? C15A Zr1A C18A C19A 176.6(5) . . . . ? C16A Zr1A C18A C19A 76.2(5) . . . . ? C12A Zr1A C18A C19A -127.7(5) . . . . ? C11A Zr1A C18A C19A -146.5(5) . . . . ? P1A Zr1A C18A C19A -27.4(6) . . . . ? C3A Zr1A C18A C17A -31.6(6) . . . . ? C13A Zr1A C18A C17A 100.2(6) . . . . ? C14A Zr1A C18A C17A 68.9(6) . . . . ? C20A Zr1A C18A C17A -77.2(5) . . . . ? C15A Zr1A C18A C17A 64.0(6) . . . . ? C19A Zr1A C18A C17A -112.5(8) . . . . ? C16A Zr1A C18A C17A -36.3(5) . . . . ? C12A Zr1A C18A C17A 119.8(5) . . . . ? C11A Zr1A C18A C17A 101.0(6) . . . . ? P1A Zr1A C18A C17A -140.0(5) . . . . ? C17A C18A C19A C20A 1.8(8) . . . . ? Zr1A C18A C19A C20A -65.1(5) . . . . ? C17A C18A C19A Zr1A 66.9(5) . . . . ? C3A Zr1A C19A C20A -2.4(5) . . . . ? C13A Zr1A C19A C20A 151.1(5) . . . . ? C14A Zr1A C19A C20A 119.1(5) . . . . ? C17A Zr1A C19A C20A 78.4(5) . . . . ? C18A Zr1A C19A C20A 117.4(8) . . . . ? C15A Zr1A C19A C20A 111.1(6) . . . . ? C16A Zr1A C19A C20A 38.4(5) . . . . ? C12A Zr1A C19A C20A -177.9(4) . . . . ? C11A Zr1A C19A C20A -173.4(6) . . . . ? P1A Zr1A C19A C20A -87.0(4) . . . . ? C3A Zr1A C19A C18A -119.8(5) . . . . ? C13A Zr1A C19A C18A 33.6(6) . . . . ? C14A Zr1A C19A C18A 1.6(6) . . . . ? C17A Zr1A C19A C18A -39.0(5) . . . . ? C20A Zr1A C19A C18A -117.4(8) . . . . ? C15A Zr1A C19A C18A -6.3(9) . . . . ? C16A Zr1A C19A C18A -79.1(6) . . . . ? C12A Zr1A C19A C18A 64.6(6) . . . . ? C11A Zr1A C19A C18A 69.1(9) . . . . ? P1A Zr1A C19A C18A 155.6(5) . . . . ? C18A C19A C20A C16A -2.9(8) . . . . ? Zr1A C19A C20A C16A -67.4(5) . . . . ? C18A C19A C20A Zr1A 64.5(5) . . . . ? C17A C16A C20A C19A 2.8(8) . . . . ? Zr1A C16A C20A C19A 67.7(5) . . . . ? C17A C16A C20A Zr1A -64.9(5) . . . . ? C3A Zr1A C20A C19A 177.9(5) . . . . ? C13A Zr1A C20A C19A -39.2(6) . . . . ? C14A Zr1A C20A C19A -82.5(6) . . . . ? C17A Zr1A C20A C19A -77.2(5) . . . . ? C18A Zr1A C20A C19A -35.8(5) . . . . ? C15A Zr1A C20A C19A -125.9(7) . . . . ? C16A Zr1A C20A C19A -113.6(7) . . . . ? C12A Zr1A C20A C19A 3.9(8) . . . . ? C11A Zr1A C20A C19A 155(2) . . . . ? P1A Zr1A C20A C19A 91.3(4) . . . . ? C3A Zr1A C20A C16A -68.5(5) . . . . ? C13A Zr1A C20A C16A 74.4(6) . . . . ? C14A Zr1A C20A C16A 31.1(7) . . . . ? C17A Zr1A C20A C16A 36.4(5) . . . . ? C18A Zr1A C20A C16A 77.8(5) . . . . ? C15A Zr1A C20A C16A -12.2(9) . . . . ? C19A Zr1A C20A C16A 113.6(7) . . . . ? C12A Zr1A C20A C16A 117.6(6) . . . . ? C11A Zr1A C20A C16A -91(2) . . . . ? P1A Zr1A C20A C16A -155.1(5) . . . . ? C3B Zr1B P1B C21B -167.8(3) . . . . ? C12B Zr1B P1B C21B -72.8(4) . . . . ? C18B Zr1B P1B C21B 60.9(3) . . . . ? C17B Zr1B P1B C21B 84.8(3) . . . . ? C13B Zr1B P1B C21B -35.1(3) . . . . ? C11B Zr1B P1B C21B -98.5(3) . . . . ? C16B Zr1B P1B C21B 120.1(3) . . . . ? C19B Zr1B P1B C21B 78.9(3) . . . . ? C14B Zr1B P1B C21B -48.6(3) . . . . ? C15B Zr1B P1B C21B -80.8(3) . . . . ? C20B Zr1B P1B C21B 110.1(3) . . . . ? C3B Zr1B P1B C1B 70.4(3) . . . . ? C12B Zr1B P1B C1B 165.4(4) . . . . ? C18B Zr1B P1B C1B -60.9(2) . . . . ? C17B Zr1B P1B C1B -36.9(3) . . . . ? C13B Zr1B P1B C1B -156.8(3) . . . . ? C11B Zr1B P1B C1B 139.8(3) . . . . ? C16B Zr1B P1B C1B -1.7(3) . . . . ? C19B Zr1B P1B C1B -42.9(2) . . . . ? C14B Zr1B P1B C1B -170.4(2) . . . . ? C15B Zr1B P1B C1B 157.4(2) . . . . ? C20B Zr1B P1B C1B -11.7(3) . . . . ? C3B Zr1B P1B C31B -48.7(3) . . . . ? C12B Zr1B P1B C31B 46.3(4) . . . . ? C18B Zr1B P1B C31B 180.0(2) . . . . ? C17B Zr1B P1B C31B -156.1(3) . . . . ? C13B Zr1B P1B C31B 84.0(3) . . . . ? C11B Zr1B P1B C31B 20.6(3) . . . . ? C16B Zr1B P1B C31B -120.8(3) . . . . ? C19B Zr1B P1B C31B -162.0(2) . . . . ? C14B Zr1B P1B C31B 70.5(2) . . . . ? C15B Zr1B P1B C31B 38.3(2) . . . . ? C20B Zr1B P1B C31B -130.8(2) . . . . ? C21B P1B C1B C2B -46.0(5) . . . . ? C31B P1B C1B C2B -155.1(4) . . . . ? Zr1B P1B C1B C2B 89.1(4) . . . . ? P1B C1B C2B B1B 167.2(4) . . . . ? C4B B1B C2B C1B 51.6(6) . . . . ? C51B B1B C2B C1B 168.0(5) . . . . ? C41B B1B C2B C1B -72.5(6) . . . . ? C21B P1B C31B C36B -134.2(5) . . . . ? C1B P1B C31B C36B -26.5(6) . . . . ? Zr1B P1B C31B C36B 92.9(5) . . . . ? C21B P1B C31B C32B 47.7(5) . . . . ? C1B P1B C31B C32B 155.4(4) . . . . ? Zr1B P1B C31B C32B -85.2(4) . . . . ? C36B C31B C32B C33B 1.7(8) . . . . ? P1B C31B C32B C33B 179.9(4) . . . . ? C36B C31B C32B C37B 179.8(5) . . . . ? P1B C31B C32B C37B -2.0(8) . . . . ? C31B C32B C33B C34B -0.7(9) . . . . ? C37B C32B C33B C34B -178.9(6) . . . . ? C32B C33B C34B C35B -1.3(9) . . . . ? C32B C33B C34B C38B 179.6(6) . . . . ? C33B C34B C35B C36B 2.4(9) . . . . ? C38B C34B C35B C36B -178.5(6) . . . . ? C34B C35B C36B C31B -1.4(9) . . . . ? C34B C35B C36B C39B 178.2(6) . . . . ? C32B C31B C36B C35B -0.7(8) . . . . ? P1B C31B C36B C35B -178.7(4) . . . . ? C32B C31B C36B C39B 179.7(6) . . . . ? P1B C31B C36B C39B 1.7(9) . . . . ? C1B P1B C21B C22B -70.6(5) . . . . ? C31B P1B C21B C22B 43.8(5) . . . . ? Zr1B P1B C21B C22B 163.6(3) . . . . ? C1B P1B C21B C26B 113.9(4) . . . . ? C31B P1B C21B C26B -131.7(4) . . . . ? Zr1B P1B C21B C26B -11.9(5) . . . . ? C26B C21B C22B C23B 4.3(7) . . . . ? P1B C21B C22B C23B -171.1(4) . . . . ? C26B C21B C22B C27B -176.4(5) . . . . ? P1B C21B C22B C27B 8.2(7) . . . . ? C21B C22B C23B C24B 1.2(8) . . . . ? C27B C22B C23B C24B -178.2(5) . . . . ? C22B C23B C24B C25B -6.7(8) . . . . ? C22B C23B C24B C28B 174.8(5) . . . . ? C23B C24B C25B C26B 6.9(8) . . . . ? C28B C24B C25B C26B -174.7(5) . . . . ? C24B C25B C26B C21B -1.5(8) . . . . ? C24B C25B C26B C29B -179.0(5) . . . . ? C22B C21B C26B C25B -4.2(7) . . . . ? P1B C21B C26B C25B 171.4(4) . . . . ? C22B C21B C26B C29B 173.1(5) . . . . ? P1B C21B C26B C29B -11.3(7) . . . . ? C4B B1B C51B C56B -96.7(7) . . . . ? C41B B1B C51B C56B 26.3(8) . . . . ? C2B B1B C51B C56B 142.4(6) . . . . ? C4B B1B C51B C52B 72.2(6) . . . . ? C41B B1B C51B C52B -164.9(5) . . . . ? C2B B1B C51B C52B -48.8(7) . . . . ? C56B C51B C52B F52B 176.3(6) . . . . ? B1B C51B C52B F52B 5.8(9) . . . . ? C56B C51B C52B C53B 0.8(9) . . . . ? B1B C51B C52B C53B -169.7(6) . . . . ? F52B C52B C53B F53B 0.4(9) . . . . ? C51B C52B C53B F53B 176.1(6) . . . . ? F52B C52B C53B C54B -178.6(6) . . . . ? C51B C52B C53B C54B -2.9(10) . . . . ? F53B C53B C54B F54B 3.0(10) . . . . ? C52B C53B C54B F54B -178.0(6) . . . . ? F53B C53B C54B C55B -177.6(6) . . . . ? C52B C53B C54B C55B 1.3(10) . . . . ? F54B C54B C55B F55B -0.5(11) . . . . ? C53B C54B C55B F55B -179.8(7) . . . . ? F54B C54B C55B C56B -178.7(6) . . . . ? C53B C54B C55B C56B 2.0(11) . . . . ? F55B C55B C56B F56B -2.7(10) . . . . ? C54B C55B C56B F56B 175.5(6) . . . . ? F55B C55B C56B C51B 177.4(7) . . . . ? C54B C55B C56B C51B -4.4(12) . . . . ? C52B C51B C56B F56B -177.0(6) . . . . ? B1B C51B C56B F56B -7.1(10) . . . . ? C52B C51B C56B C55B 2.9(10) . . . . ? B1B C51B C56B C55B 172.8(6) . . . . ? C4B B1B C41B C46B 168.9(5) . . . . ? C51B B1B C41B C46B 52.6(7) . . . . ? C2B B1B C41B C46B -69.0(6) . . . . ? C4B B1B C41B C42B -17.3(8) . . . . ? C51B B1B C41B C42B -133.6(5) . . . . ? C2B B1B C41B C42B 104.8(6) . . . . ? C46B C41B C42B F42B 178.4(5) . . . . ? B1B C41B C42B F42B 4.1(8) . . . . ? C46B C41B C42B C43B -1.4(8) . . . . ? B1B C41B C42B C43B -175.6(5) . . . . ? F42B C42B C43B F43B -0.5(8) . . . . ? C41B C42B C43B F43B 179.2(5) . . . . ? F42B C42B C43B C44B -179.3(5) . . . . ? C41B C42B C43B C44B 0.4(9) . . . . ? F43B C43B C44B F44B 1.8(9) . . . . ? C42B C43B C44B F44B -179.4(5) . . . . ? F43B C43B C44B C45B -178.2(5) . . . . ? C42B C43B C44B C45B 0.6(9) . . . . ? F44B C44B C45B F45B -0.6(9) . . . . ? C43B C44B C45B F45B 179.4(5) . . . . ? F44B C44B C45B C46B 179.5(5) . . . . ? C43B C44B C45B C46B -0.5(9) . . . . ? F45B C45B C46B F46B -0.3(9) . . . . ? C44B C45B C46B F46B 179.6(5) . . . . ? F45B C45B C46B C41B 179.5(5) . . . . ? C44B C45B C46B C41B -0.6(10) . . . . ? C42B C41B C46B F46B -178.7(5) . . . . ? B1B C41B C46B F46B -4.1(8) . . . . ? C42B C41B C46B C45B 1.5(8) . . . . ? B1B C41B C46B C45B 176.1(5) . . . . ? C3B Zr1B C11B C12B -134.9(6) . . . . ? C18B Zr1B C11B C12B -5.2(7) . . . . ? C17B Zr1B C11B C12B -31.7(6) . . . . ? C13B Zr1B C11B C12B 36.7(5) . . . . ? C16B Zr1B C11B C12B -65.0(6) . . . . ? C19B Zr1B C11B C12B -22.5(10) . . . . ? C14B Zr1B C11B C12B 77.6(6) . . . . ? C15B Zr1B C11B C12B 115.6(8) . . . . ? C20B Zr1B C11B C12B -80.0(7) . . . . ? P1B Zr1B C11B C12B 150.6(5) . . . . ? C3B Zr1B C11B C15B 109.5(5) . . . . ? C12B Zr1B C11B C15B -115.6(8) . . . . ? C18B Zr1B C11B C15B -120.8(5) . . . . ? C17B Zr1B C11B C15B -147.3(5) . . . . ? C13B Zr1B C11B C15B -78.9(5) . . . . ? C16B Zr1B C11B C15B 179.4(5) . . . . ? C19B Zr1B C11B C15B -138.1(6) . . . . ? C14B Zr1B C11B C15B -38.0(4) . . . . ? C20B Zr1B C11B C15B 164.4(4) . . . . ? P1B Zr1B C11B C15B 35.0(5) . . . . ? C15B C11B C12B C13B -0.2(10) . . . . ? Zr1B C11B C12B C13B -66.8(6) . . . . ? C15B C11B C12B Zr1B 66.6(5) . . . . ? C3B Zr1B C12B C11B 43.6(6) . . . . ? C18B Zr1B C12B C11B 175.8(5) . . . . ? C17B Zr1B C12B C11B 148.5(6) . . . . ? C13B Zr1B C12B C11B -116.4(8) . . . . ? C16B Zr1B C12B C11B 122.2(6) . . . . ? C19B Zr1B C12B C11B 169.5(5) . . . . ? C14B Zr1B C12B C11B -77.4(6) . . . . ? C15B Zr1B C12B C11B -36.6(5) . . . . ? C20B Zr1B C12B C11B 129.8(5) . . . . ? P1B Zr1B C12B C11B -46.6(7) . . . . ? C3B Zr1B C12B C13B 160.0(5) . . . . ? C18B Zr1B C12B C13B -67.8(5) . . . . ? C17B Zr1B C12B C13B -95.1(5) . . . . ? C11B Zr1B C12B C13B 116.4(8) . . . . ? C16B Zr1B C12B C13B -121.4(5) . . . . ? C19B Zr1B C12B C13B -74.1(6) . . . . ? C14B Zr1B C12B C13B 39.0(5) . . . . ? C15B Zr1B C12B C13B 79.8(6) . . . . ? C20B Zr1B C12B C13B -113.8(5) . . . . ? P1B Zr1B C12B C13B 69.8(7) . . . . ? C11B C12B C13B C14B -0.9(9) . . . . ? Zr1B C12B C13B C14B -68.1(5) . . . . ? C11B C12B C13B Zr1B 67.1(6) . . . . ? C3B Zr1B C13B C12B -25.5(7) . . . . ? C18B Zr1B C13B C12B 111.6(6) . . . . ? C17B Zr1B C13B C12B 78.7(5) . . . . ? C11B Zr1B C13B C12B -35.9(5) . . . . ? C16B Zr1B C13B C12B 66.0(6) . . . . ? C19B Zr1B C13B C12B 123.3(5) . . . . ? C14B Zr1B C13B C12B -111.3(7) . . . . ? C15B Zr1B C13B C12B -75.5(6) . . . . ? C20B Zr1B C13B C12B 94.7(6) . . . . ? P1B Zr1B C13B C12B -137.1(5) . . . . ? C3B Zr1B C13B C14B 85.8(5) . . . . ? C12B Zr1B C13B C14B 111.3(7) . . . . ? C18B Zr1B C13B C14B -137.1(5) . . . . ? C17B Zr1B C13B C14B -170.0(5) . . . . ? C11B Zr1B C13B C14B 75.5(5) . . . . ? C16B Zr1B C13B C14B 177.4(4) . . . . ? C19B Zr1B C13B C14B -125.4(4) . . . . ? C15B Zr1B C13B C14B 35.9(4) . . . . ? C20B Zr1B C13B C14B -154.0(4) . . . . ? P1B Zr1B C13B C14B -25.7(5) . . . . ? C12B C13B C14B C15B 1.7(8) . . . . ? Zr1B C13B C14B C15B -65.4(5) . . . . ? C12B C13B C14B Zr1B 67.0(5) . . . . ? C3B Zr1B C14B C15B 0.9(5) . . . . ? C12B Zr1B C14B C15B 77.9(5) . . . . ? C18B Zr1B C14B C15B 161.7(4) . . . . ? C17B Zr1B C14B C15B 127.8(4) . . . . ? C13B Zr1B C14B C15B 117.0(6) . . . . ? C11B Zr1B C14B C15B 37.5(5) . . . . ? C16B Zr1B C14B C15B 112.8(6) . . . . ? C19B Zr1B C14B C15B -170.9(4) . . . . ? C20B Zr1B C14B C15B 177.5(7) . . . . ? P1B Zr1B C14B C15B -84.1(4) . . . . ? C3B Zr1B C14B C13B -116.0(5) . . . . ? C12B Zr1B C14B C13B -39.1(5) . . . . ? C18B Zr1B C14B C13B 44.7(5) . . . . ? C17B Zr1B C14B C13B 10.8(5) . . . . ? C11B Zr1B C14B C13B -79.5(5) . . . . ? C16B Zr1B C14B C13B -4.2(7) . . . . ? C19B Zr1B C14B C13B 72.1(5) . . . . ? C15B Zr1B C14B C13B -117.0(6) . . . . ? C20B Zr1B C14B C13B 60.5(9) . . . . ? P1B Zr1B C14B C13B 158.9(4) . . . . ? C12B C11B C15B C14B 1.2(9) . . . . ? Zr1B C11B C15B C14B 66.8(5) . . . . ? C12B C11B C15B Zr1B -65.6(6) . . . . ? C13B C14B C15B C11B -1.8(8) . . . . ? Zr1B C14B C15B C11B -66.6(5) . . . . ? C13B C14B C15B Zr1B 64.8(5) . . . . ? C3B Zr1B C15B C11B -65.7(5) . . . . ? C12B Zr1B C15B C11B 36.6(5) . . . . ? C18B Zr1B C15B C11B 87.5(6) . . . . ? C17B Zr1B C15B C11B 43.1(6) . . . . ? C13B Zr1B C15B C11B 77.3(5) . . . . ? C16B Zr1B C15B C11B -1.0(7) . . . . ? C19B Zr1B C15B C11B 134.1(7) . . . . ? C14B Zr1B C15B C11B 113.5(7) . . . . ? C20B Zr1B C15B C11B -61.6(15) . . . . ? P1B Zr1B C15B C11B -149.4(5) . . . . ? C3B Zr1B C15B C14B -179.2(5) . . . . ? C12B Zr1B C15B C14B -76.9(5) . . . . ? C18B Zr1B C15B C14B -26.0(6) . . . . ? C17B Zr1B C15B C14B -70.4(5) . . . . ? C13B Zr1B C15B C14B -36.2(4) . . . . ? C11B Zr1B C15B C14B -113.5(7) . . . . ? C16B Zr1B C15B C14B -114.5(5) . . . . ? C19B Zr1B C15B C14B 20.6(9) . . . . ? C20B Zr1B C15B C14B -175.1(13) . . . . ? P1B Zr1B C15B C14B 97.1(4) . . . . ? C3B Zr1B C16B C20B -94.4(5) . . . . ? C12B Zr1B C16B C20B 168.7(5) . . . . ? C18B Zr1B C16B C20B 77.0(5) . . . . ? C17B Zr1B C16B C20B 115.2(7) . . . . ? C13B Zr1B C16B C20B 138.9(5) . . . . ? C11B Zr1B C16B C20B -162.4(5) . . . . ? C19B Zr1B C16B C20B 36.5(4) . . . . ? C14B Zr1B C16B C20B 141.4(5) . . . . ? C15B Zr1B C16B C20B -161.9(4) . . . . ? P1B Zr1B C16B C20B -19.1(5) . . . . ? C3B Zr1B C16B C17B 150.4(5) . . . . ? C12B Zr1B C16B C17B 53.5(5) . . . . ? C18B Zr1B C16B C17B -38.2(4) . . . . ? C13B Zr1B C16B C17B 23.7(5) . . . . ? C11B Zr1B C16B C17B 82.4(5) . . . . ? C19B Zr1B C16B C17B -78.7(5) . . . . ? C14B Zr1B C16B C17B 26.2(7) . . . . ? C15B Zr1B C16B C17B 82.9(6) . . . . ? C20B Zr1B C16B C17B -115.2(7) . . . . ? P1B Zr1B C16B C17B -134.3(4) . . . . ? C20B C16B C17B C18B 1.0(8) . . . . ? Zr1B C16B C17B C18B 67.3(5) . . . . ? C20B C16B C17B Zr1B -66.3(5) . . . . ? C3B Zr1B C17B C18B -143.3(4) . . . . ? C12B Zr1B C17B C18B 122.0(5) . . . . ? C13B Zr1B C17B C18B 89.1(4) . . . . ? C11B Zr1B C17B C18B 138.6(4) . . . . ? C16B Zr1B C17B C18B -113.1(7) . . . . ? C19B Zr1B C17B C18B -37.0(4) . . . . ? C14B Zr1B C17B C18B 83.2(5) . . . . ? C15B Zr1B C17B C18B 116.7(4) . . . . ? C20B Zr1B C17B C18B -76.4(5) . . . . ? P1B Zr1B C17B C18B -44.4(6) . . . . ? C3B Zr1B C17B C16B -30.2(5) . . . . ? C12B Zr1B C17B C16B -124.9(5) . . . . ? C18B Zr1B C17B C16B 113.1(7) . . . . ? C13B Zr1B C17B C16B -157.8(5) . . . . ? C11B Zr1B C17B C16B -108.3(5) . . . . ? C19B Zr1B C17B C16B 76.1(5) . . . . ? C14B Zr1B C17B C16B -163.7(5) . . . . ? C15B Zr1B C17B C16B -130.2(5) . . . . ? C20B Zr1B C17B C16B 36.6(5) . . . . ? P1B Zr1B C17B C16B 68.7(5) . . . . ? C16B C17B C18B C19B -0.1(8) . . . . ? Zr1B C17B C18B C19B 68.1(5) . . . . ? C16B C17B C18B Zr1B -68.3(5) . . . . ? C3B Zr1B C18B C19B -65.4(6) . . . . ? C12B Zr1B C18B C19B -170.5(5) . . . . ? C17B Zr1B C18B C19B -114.5(7) . . . . ? C13B Zr1B C18B C19B 159.3(5) . . . . ? C11B Zr1B C18B C19B -167.7(4) . . . . ? C16B Zr1B C18B C19B -76.4(5) . . . . ? C14B Zr1B C18B C19B 136.8(4) . . . . ? C15B Zr1B C18B C19B 150.9(5) . . . . ? C20B Zr1B C18B C19B -36.1(4) . . . . ? P1B Zr1B C18B C19B 35.4(5) . . . . ? C3B Zr1B C18B C17B 49.1(5) . . . . ? C12B Zr1B C18B C17B -56.0(5) . . . . ? C13B Zr1B C18B C17B -86.3(5) . . . . ? C11B Zr1B C18B C17B -53.2(6) . . . . ? C16B Zr1B C18B C17B 38.0(4) . . . . ? C19B Zr1B C18B C17B 114.5(7) . . . . ? C14B Zr1B C18B C17B -108.8(5) . . . . ? C15B Zr1B C18B C17B -94.6(5) . . . . ? C20B Zr1B C18B C17B 78.4(5) . . . . ? P1B Zr1B C18B C17B 149.9(4) . . . . ? C17B C18B C19B C20B -0.8(8) . . . . ? Zr1B C18B C19B C20B 66.3(5) . . . . ? C17B C18B C19B Zr1B -67.1(5) . . . . ? C3B Zr1B C19B C20B 15.8(5) . . . . ? C12B Zr1B C19B C20B -103.9(5) . . . . ? C18B Zr1B C19B C20B -115.8(7) . . . . ? C17B Zr1B C19B C20B -78.2(5) . . . . ? C13B Zr1B C19B C20B -138.1(5) . . . . ? C11B Zr1B C19B C20B -89.3(8) . . . . ? C16B Zr1B C19B C20B -37.3(5) . . . . ? C14B Zr1B C19B C20B -171.9(4) . . . . ? C15B Zr1B C19B C20B 174.4(6) . . . . ? P1B Zr1B C19B C20B 96.9(4) . . . . ? C3B Zr1B C19B C18B 131.6(4) . . . . ? C12B Zr1B C19B C18B 11.9(6) . . . . ? C17B Zr1B C19B C18B 37.6(4) . . . . ? C13B Zr1B C19B C18B -22.3(5) . . . . ? C11B Zr1B C19B C18B 26.5(9) . . . . ? C16B Zr1B C19B C18B 78.5(5) . . . . ? C14B Zr1B C19B C18B -56.1(5) . . . . ? C15B Zr1B C19B C18B -69.8(8) . . . . ? C20B Zr1B C19B C18B 115.8(7) . . . . ? P1B Zr1B C19B C18B -147.3(4) . . . . ? C18B C19B C20B C16B 1.4(8) . . . . ? Zr1B C19B C20B C16B 66.4(5) . . . . ? C18B C19B C20B Zr1B -65.0(5) . . . . ? C17B C16B C20B C19B -1.5(8) . . . . ? Zr1B C16B C20B C19B -66.6(5) . . . . ? C17B C16B C20B Zr1B 65.1(5) . . . . ? C3B Zr1B C20B C19B -165.3(5) . . . . ? C12B Zr1B C20B C19B 100.7(5) . . . . ? C18B Zr1B C20B C19B 36.8(4) . . . . ? C17B Zr1B C20B C19B 77.8(5) . . . . ? C13B Zr1B C20B C19B 57.9(6) . . . . ? C11B Zr1B C20B C19B 141.8(5) . . . . ? C16B Zr1B C20B C19B 114.9(6) . . . . ? C14B Zr1B C20B C19B 17.7(10) . . . . ? C15B Zr1B C20B C19B -169.4(12) . . . . ? P1B Zr1B C20B C19B -81.5(4) . . . . ? C3B Zr1B C20B C16B 79.8(5) . . . . ? C12B Zr1B C20B C16B -14.2(6) . . . . ? C18B Zr1B C20B C16B -78.1(5) . . . . ? C17B Zr1B C20B C16B -37.1(4) . . . . ? C13B Zr1B C20B C16B -57.0(6) . . . . ? C11B Zr1B C20B C16B 26.9(7) . . . . ? C19B Zr1B C20B C16B -114.9(6) . . . . ? C14B Zr1B C20B C16B -97.2(8) . . . . ? C15B Zr1B C20B C16B 75.7(15) . . . . ? P1B Zr1B C20B C16B 163.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.607 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.054 _database_code_depnum_ccdc_archive 'CCDC 950031' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk6888 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H70 B F10 P Zr' _chemical_formula_weight 1126.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.5025(3) _cell_length_b 23.0203(7) _cell_length_c 28.2476(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11381.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4688 _exptl_absorpt_coefficient_mu 2.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5088 _exptl_absorpt_correction_T_max 0.9304 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewsk & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41458 _diffrn_reflns_av_R_equivalents 0.078 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.46 _diffrn_reflns_theta_max 67.01 _reflns_number_total 9865 _reflns_number_gt 6508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogens at C4 atom were refined freely. ; _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^)+(0.0420P)^2^+14.3666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9865 _refine_ls_number_parameters 696 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.027 _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 Zr1 Zr 0.29430(2) 0.132248(14) 0.346961(12) 0.03981(11) Uani 1 1 d . . . P1 P 0.13451(7) 0.15522(5) 0.09478(4) 0.0486(3) Uani 1 1 d . . . B1 B 0.2842(3) 0.0891(2) 0.20169(16) 0.0452(12) Uani 1 1 d . . . C11 C 0.4008(2) 0.14170(18) 0.40678(15) 0.0484(11) Uani 1 1 d . . . C12 C 0.4338(2) 0.11030(18) 0.36865(16) 0.0467(11) Uani 1 1 d . . . C13 C 0.4358(2) 0.14716(18) 0.32892(16) 0.0477(11) Uani 1 1 d . . . C14 C 0.4044(2) 0.20136(18) 0.34190(16) 0.0494(11) Uani 1 1 d . . . C15 C 0.3850(2) 0.19880(17) 0.39053(16) 0.0488(11) Uani 1 1 d . . . C16 C 0.1971(2) 0.1664(2) 0.40766(15) 0.0509(11) Uani 1 1 d . . . C17 C 0.1711(2) 0.11167(19) 0.39175(16) 0.0496(11) Uani 1 1 d . . . C18 C 0.1499(2) 0.11685(17) 0.34370(15) 0.0450(10) Uani 1 1 d . . . C19 C 0.1633(2) 0.17486(18) 0.32942(15) 0.0441(10) Uani 1 1 d . . . C20 C 0.1924(2) 0.20560(18) 0.36880(16) 0.0490(11) Uani 1 1 d . . . C21 C 0.3965(3) 0.1194(2) 0.45673(16) 0.0680(14) Uani 1 1 d . . . H21A H 0.3626 0.0861 0.4579 0.102 Uiso 1 1 calc R . . H21B H 0.3771 0.1497 0.4773 0.102 Uiso 1 1 calc R . . H21C H 0.4471 0.1079 0.4672 0.102 Uiso 1 1 calc R . . C22 C 0.4728(3) 0.05255(19) 0.37221(19) 0.0654(14) Uani 1 1 d . . . H22A H 0.5255 0.0582 0.3819 0.098 Uiso 1 1 calc R . . H22B H 0.4715 0.0334 0.3416 0.098 Uiso 1 1 calc R . . H22C H 0.4467 0.0287 0.3954 0.098 Uiso 1 1 calc R . . C23 C 0.4774(3) 0.1344(2) 0.28359(17) 0.0675(14) Uani 1 1 d . . . H23A H 0.4605 0.1611 0.2592 0.101 Uiso 1 1 calc R . . H23B H 0.4667 0.0948 0.2738 0.101 Uiso 1 1 calc R . . H23C H 0.5319 0.1390 0.2885 0.101 Uiso 1 1 calc R . . C24 C 0.4002(3) 0.2554(2) 0.31133(19) 0.0700(15) Uani 1 1 d . . . H24A H 0.4413 0.2816 0.3199 0.105 Uiso 1 1 calc R . . H24B H 0.3515 0.2745 0.3163 0.105 Uiso 1 1 calc R . . H24C H 0.4051 0.2445 0.2783 0.105 Uiso 1 1 calc R . . C25 C 0.3686(3) 0.2507(2) 0.42142(19) 0.0710(15) Uani 1 1 d . . . H25A H 0.4120 0.2769 0.4207 0.107 Uiso 1 1 calc R . . H25B H 0.3597 0.2379 0.4537 0.107 Uiso 1 1 calc R . . H25C H 0.3236 0.2707 0.4097 0.107 Uiso 1 1 calc R . . C26 C 0.2069(3) 0.1817(2) 0.45912(16) 0.0740(15) Uani 1 1 d . . . H26A H 0.1595 0.1745 0.4759 0.111 Uiso 1 1 calc R . . H26B H 0.2205 0.2224 0.4619 0.111 Uiso 1 1 calc R . . H26C H 0.2472 0.1580 0.4727 0.111 Uiso 1 1 calc R . . C27 C 0.1578(3) 0.0597(2) 0.42305(18) 0.0711(15) Uani 1 1 d . . . H27A H 0.2033 0.0522 0.4416 0.107 Uiso 1 1 calc R . . H27B H 0.1464 0.0261 0.4036 0.107 Uiso 1 1 calc R . . H27C H 0.1151 0.0674 0.4441 0.107 Uiso 1 1 calc R . . C28 C 0.1107(3) 0.07086(19) 0.31443(16) 0.0607(13) Uani 1 1 d . . . H28A H 0.0558 0.0762 0.3162 0.091 Uiso 1 1 calc R . . H28B H 0.1240 0.0327 0.3265 0.091 Uiso 1 1 calc R . . H28C H 0.1272 0.0741 0.2817 0.091 Uiso 1 1 calc R . . C29 C 0.1421(3) 0.2026(2) 0.28315(16) 0.0584(12) Uani 1 1 d . . . H29A H 0.0927 0.2214 0.2862 0.088 Uiso 1 1 calc R . . H29B H 0.1395 0.1731 0.2587 0.088 Uiso 1 1 calc R . . H29C H 0.1804 0.2313 0.2747 0.088 Uiso 1 1 calc R . . C30 C 0.1979(3) 0.2711(2) 0.36983(19) 0.0708(14) Uani 1 1 d . . . H30A H 0.2409 0.2835 0.3506 0.106 Uiso 1 1 calc R . . H30B H 0.2053 0.2840 0.4022 0.106 Uiso 1 1 calc R . . H30C H 0.1512 0.2877 0.3573 0.106 Uiso 1 1 calc R . . C2 C 0.2118(2) 0.11993(18) 0.17591(14) 0.0486(11) Uani 1 1 d . . . H2A H 0.1657 0.1111 0.1942 0.058 Uiso 1 1 calc R . . H2B H 0.2193 0.1621 0.1770 0.058 Uiso 1 1 calc R . . C1 C 0.1980(3) 0.10200(19) 0.12417(14) 0.0504(11) Uani 1 1 d . . . H1A H 0.1745 0.0634 0.1232 0.061 Uiso 1 1 calc R . . H1B H 0.2468 0.1001 0.1073 0.061 Uiso 1 1 calc R . . C3 C 0.2983(3) 0.03413(16) 0.35552(16) 0.0519(11) Uani 1 1 d . . . H3A H 0.3399 0.0185 0.3367 0.078 Uiso 1 1 calc R . . H3B H 0.2504 0.0175 0.3449 0.078 Uiso 1 1 calc R . . H3C H 0.3064 0.0245 0.3886 0.078 Uiso 1 1 calc R . . C4 C 0.2921(3) 0.1138(2) 0.25758(15) 0.0459(10) Uani 1 1 d . . . H4A H 0.341(2) 0.0988(16) 0.2705(14) 0.047(12) Uiso 1 1 d . . . H4B H 0.247(2) 0.1006(14) 0.2725(12) 0.029(10) Uiso 1 1 d . . . H4C H 0.291(2) 0.1570(19) 0.2598(14) 0.059(13) Uiso 1 1 d . . . C31 C 0.1205(2) 0.13793(18) 0.03129(15) 0.0483(10) Uani 1 1 d . . . C32 C 0.1372(3) 0.08549(19) 0.00736(17) 0.0611(13) Uani 1 1 d . . . C33 C 0.1154(3) 0.0787(2) -0.03974(17) 0.0667(14) Uani 1 1 d . . . H33 H 0.1268 0.0433 -0.0549 0.080 Uiso 1 1 calc R . . C34 C 0.0779(3) 0.1210(2) -0.06541(17) 0.0600(13) Uani 1 1 d . . . C35 C 0.0604(3) 0.1721(2) -0.04135(16) 0.0557(12) Uani 1 1 d . . . H35 H 0.0339 0.2015 -0.0576 0.067 Uiso 1 1 calc R . . C36 C 0.0803(2) 0.18134(18) 0.00545(15) 0.0493(11) Uani 1 1 d . . . C37 C 0.1771(4) 0.0344(2) 0.03006(19) 0.091(2) Uani 1 1 d . . . H37A H 0.1860 0.0046 0.0064 0.136 Uiso 1 1 calc R . . H37B H 0.1453 0.0187 0.0552 0.136 Uiso 1 1 calc R . . H37C H 0.2256 0.0470 0.0432 0.136 Uiso 1 1 calc R . . C38 C 0.0559(3) 0.1117(2) -0.11652(18) 0.0828(17) Uani 1 1 d . . . H38A H 0.0381 0.1480 -0.1300 0.124 Uiso 1 1 calc R . . H38B H 0.0155 0.0829 -0.1183 0.124 Uiso 1 1 calc R . . H38C H 0.1000 0.0981 -0.1341 0.124 Uiso 1 1 calc R . . C39 C 0.0548(3) 0.23758(19) 0.02821(16) 0.0580(12) Uani 1 1 d . . . H39A H 0.0210 0.2582 0.0068 0.087 Uiso 1 1 calc R . . H39B H 0.0991 0.2615 0.0350 0.087 Uiso 1 1 calc R . . H39C H 0.0280 0.2291 0.0575 0.087 Uiso 1 1 calc R . . C41 C 0.1980(3) 0.21963(18) 0.09361(14) 0.0489(11) Uani 1 1 d . . . C42 C 0.2646(3) 0.22477(19) 0.06588(15) 0.0515(11) Uani 1 1 d . . . C43 C 0.3080(3) 0.2755(2) 0.06815(16) 0.0634(13) Uani 1 1 d . . . H43 H 0.3532 0.2778 0.0502 0.076 Uiso 1 1 calc R . . C44 C 0.2873(4) 0.3222(2) 0.09549(18) 0.0761(16) Uani 1 1 d . . . C45 C 0.2223(3) 0.3172(2) 0.12266(17) 0.0704(15) Uani 1 1 d . . . H45 H 0.2076 0.3486 0.1418 0.085 Uiso 1 1 calc R . . C46 C 0.1774(3) 0.2670(2) 0.12269(15) 0.0568(12) Uani 1 1 d . . . C47 C 0.2923(3) 0.1776(2) 0.03294(16) 0.0611(12) Uani 1 1 d . . . H47A H 0.2953 0.1411 0.0500 0.092 Uiso 1 1 calc R . . H47B H 0.3425 0.1877 0.0210 0.092 Uiso 1 1 calc R . . H47C H 0.2569 0.1737 0.0067 0.092 Uiso 1 1 calc R . . C48 C 0.3341(4) 0.3773(3) 0.0959(2) 0.119(3) Uani 1 1 d . . . H48A H 0.3673 0.3774 0.1233 0.179 Uiso 1 1 calc R . . H48B H 0.3002 0.4106 0.0972 0.179 Uiso 1 1 calc R . . H48C H 0.3647 0.3793 0.0673 0.179 Uiso 1 1 calc R . . C49 C 0.1078(3) 0.2663(2) 0.15436(17) 0.0697(14) Uani 1 1 d . . . H49A H 0.1065 0.3016 0.1731 0.104 Uiso 1 1 calc R . . H49B H 0.1101 0.2329 0.1752 0.104 Uiso 1 1 calc R . . H49C H 0.0620 0.2641 0.1351 0.104 Uiso 1 1 calc R . . C51 C 0.2777(3) 0.01789(19) 0.21074(14) 0.0520(12) Uani 1 1 d . . . F52 F 0.14350(18) 0.01000(13) 0.19731(10) 0.0794(9) Uani 1 1 d . . . C52 C 0.2109(3) -0.0143(2) 0.21019(16) 0.0613(13) Uani 1 1 d . . . F53 F 0.1382(2) -0.10001(14) 0.22171(12) 0.1154(13) Uani 1 1 d . . . C53 C 0.2065(4) -0.0727(2) 0.22316(19) 0.0795(17) Uani 1 1 d . . . F54 F 0.2661(3) -0.15703(13) 0.25072(13) 0.1346(16) Uani 1 1 d . . . C54 C 0.2703(5) -0.1007(2) 0.2378(2) 0.091(2) Uani 1 1 d . . . F55 F 0.4022(3) -0.09932(14) 0.25322(13) 0.1222(14) Uani 1 1 d . . . C55 C 0.3383(4) -0.0717(2) 0.23920(19) 0.0826(18) Uani 1 1 d . . . F56 F 0.40934(18) 0.01179(13) 0.22860(10) 0.0788(9) Uani 1 1 d . . . C56 C 0.3397(3) -0.0140(2) 0.22579(16) 0.0639(14) Uani 1 1 d . . . C61 C 0.3584(2) 0.10755(18) 0.16862(15) 0.0468(11) Uani 1 1 d . . . F62 F 0.36240(16) 0.01848(11) 0.12629(9) 0.0669(7) Uani 1 1 d . . . C62 C 0.3881(3) 0.0734(2) 0.13265(16) 0.0526(11) Uani 1 1 d . . . F63 F 0.46377(17) 0.05646(14) 0.06436(10) 0.0900(10) Uani 1 1 d . . . C63 C 0.4408(3) 0.0921(2) 0.09946(17) 0.0627(13) Uani 1 1 d . . . C64 C 0.4679(3) 0.1475(3) 0.10197(17) 0.0640(14) Uani 1 1 d . . . F64 F 0.51761(16) 0.16749(15) 0.06902(11) 0.0926(10) Uani 1 1 d . . . F65 F 0.46765(18) 0.23866(13) 0.13940(11) 0.0881(10) Uani 1 1 d . . . C65 C 0.4417(3) 0.1839(2) 0.13642(18) 0.0617(13) Uani 1 1 d . . . F66 F 0.36265(17) 0.20336(11) 0.20002(10) 0.0738(8) Uani 1 1 d . . . C66 C 0.3878(3) 0.1633(2) 0.16838(16) 0.0563(12) Uani 1 1 d . . . C71 C 0.5233(4) -0.0909(2) 0.0824(2) 0.0840(17) Uani 1 1 d U . . C72 C 0.5170(5) -0.0875(2) 0.1310(3) 0.100(2) Uani 1 1 d U . . H72 H 0.4689 -0.0843 0.1455 0.121 Uiso 1 1 calc R . . C73 C 0.5806(6) -0.0890(3) 0.1570(3) 0.121(3) Uani 1 1 d U . . H73 H 0.5763 -0.0871 0.1901 0.145 Uiso 1 1 calc R . . C74 C 0.6507(6) -0.0931(3) 0.1375(4) 0.118(3) Uani 1 1 d U . . H74 H 0.6939 -0.0946 0.1573 0.142 Uiso 1 1 calc R . . C75 C 0.6602(5) -0.0951(3) 0.0880(4) 0.125(3) Uani 1 1 d U . . H75 H 0.7090 -0.0969 0.0741 0.151 Uiso 1 1 calc R . . C76 C 0.5929(5) -0.0944(3) 0.0603(3) 0.100(2) Uani 1 1 d U . . H76 H 0.5959 -0.0962 0.0271 0.120 Uiso 1 1 calc R . . C77 C 0.4509(4) -0.0902(3) 0.0531(3) 0.128(3) Uani 1 1 d U . . H77A H 0.4070 -0.0880 0.0740 0.192 Uiso 1 1 calc R . . H77B H 0.4480 -0.1255 0.0344 0.192 Uiso 1 1 calc R . . H77C H 0.4514 -0.0568 0.0322 0.192 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0429(2) 0.04004(18) 0.03651(18) -0.00222(15) 0.00162(18) -0.00113(17) P1 0.0542(7) 0.0483(6) 0.0434(6) 0.0028(5) 0.0012(6) 0.0012(5) B1 0.061(3) 0.043(3) 0.032(2) 0.0004(19) 0.004(2) -0.002(2) C11 0.047(3) 0.054(3) 0.044(2) -0.003(2) -0.006(2) -0.006(2) C12 0.036(2) 0.047(2) 0.057(3) 0.003(2) -0.002(2) -0.001(2) C13 0.039(2) 0.055(3) 0.049(3) -0.004(2) 0.003(2) -0.005(2) C14 0.046(3) 0.045(2) 0.057(3) 0.004(2) -0.004(2) -0.010(2) C15 0.043(2) 0.043(2) 0.061(3) -0.013(2) -0.007(2) -0.003(2) C16 0.045(3) 0.067(3) 0.040(2) -0.013(2) 0.005(2) 0.002(2) C17 0.045(3) 0.058(3) 0.046(3) 0.003(2) 0.010(2) 0.001(2) C18 0.040(2) 0.051(2) 0.045(3) -0.0061(19) 0.008(2) -0.0051(19) C19 0.038(2) 0.052(2) 0.043(2) -0.007(2) -0.003(2) 0.004(2) C20 0.043(3) 0.050(2) 0.054(3) -0.009(2) 0.003(2) 0.004(2) C21 0.065(3) 0.088(4) 0.052(3) 0.006(3) -0.008(3) -0.002(3) C22 0.052(3) 0.051(3) 0.093(4) 0.006(3) -0.008(3) 0.002(2) C23 0.051(3) 0.087(4) 0.065(3) -0.003(3) 0.012(3) -0.005(3) C24 0.072(3) 0.053(3) 0.085(4) 0.009(3) -0.008(3) -0.007(3) C25 0.070(3) 0.065(3) 0.078(4) -0.023(3) -0.014(3) 0.003(3) C26 0.066(3) 0.109(4) 0.046(3) -0.020(3) 0.001(3) 0.006(3) C27 0.072(3) 0.080(4) 0.061(3) 0.016(3) 0.019(3) -0.003(3) C28 0.060(3) 0.060(3) 0.061(3) -0.007(2) -0.001(3) -0.009(2) C29 0.060(3) 0.061(3) 0.054(3) 0.000(2) -0.003(2) 0.008(2) C30 0.074(3) 0.057(3) 0.081(4) -0.019(3) -0.006(3) 0.006(3) C2 0.057(3) 0.051(3) 0.038(2) -0.0010(18) 0.007(2) 0.000(2) C1 0.057(3) 0.054(2) 0.040(2) -0.001(2) 0.004(2) -0.001(2) C3 0.055(3) 0.037(2) 0.063(3) 0.0052(19) -0.002(2) 0.000(2) C4 0.044(3) 0.054(3) 0.040(2) -0.0004(19) 0.007(2) 0.000(2) C31 0.051(3) 0.048(2) 0.046(2) 0.003(2) 0.000(2) -0.004(2) C32 0.080(4) 0.051(3) 0.052(3) -0.003(2) -0.017(3) 0.000(3) C33 0.091(4) 0.053(3) 0.057(3) -0.009(2) -0.016(3) 0.001(3) C34 0.071(3) 0.063(3) 0.046(3) -0.001(2) -0.010(2) -0.007(3) C35 0.056(3) 0.060(3) 0.052(3) 0.009(2) -0.006(2) -0.004(2) C36 0.049(3) 0.053(3) 0.045(3) 0.003(2) 0.004(2) -0.001(2) C37 0.145(5) 0.058(3) 0.069(4) -0.019(3) -0.033(4) 0.037(3) C38 0.111(5) 0.074(4) 0.063(3) 0.002(3) -0.030(3) -0.014(3) C39 0.061(3) 0.063(3) 0.051(3) 0.011(2) 0.003(2) 0.014(2) C41 0.056(3) 0.051(2) 0.039(2) 0.0058(19) -0.004(2) 0.007(2) C42 0.056(3) 0.061(3) 0.037(2) 0.008(2) -0.002(2) 0.001(2) C43 0.064(3) 0.084(4) 0.042(3) 0.011(2) -0.002(2) -0.021(3) C44 0.112(5) 0.067(3) 0.049(3) 0.002(3) -0.008(3) -0.031(3) C45 0.104(4) 0.056(3) 0.052(3) -0.005(2) 0.003(3) -0.011(3) C46 0.075(3) 0.057(3) 0.039(3) 0.001(2) 0.003(2) 0.001(2) C47 0.059(3) 0.071(3) 0.053(3) 0.004(2) 0.009(3) 0.002(3) C48 0.167(7) 0.099(5) 0.092(5) -0.013(4) 0.017(5) -0.072(5) C49 0.085(4) 0.062(3) 0.062(3) -0.011(3) 0.017(3) 0.010(3) C51 0.071(3) 0.050(2) 0.035(2) -0.0025(19) 0.009(2) 0.002(2) F52 0.078(2) 0.084(2) 0.077(2) 0.0094(16) 0.0058(17) -0.0242(18) C52 0.088(4) 0.056(3) 0.040(3) -0.002(2) 0.009(3) -0.010(3) F53 0.166(4) 0.085(2) 0.095(3) 0.0036(19) 0.026(2) -0.055(3) C53 0.122(5) 0.060(3) 0.056(3) 0.000(3) 0.020(4) -0.030(4) F54 0.247(5) 0.0512(17) 0.106(3) 0.0228(18) 0.030(3) -0.001(3) C54 0.164(7) 0.045(3) 0.062(4) 0.012(3) 0.010(4) 0.004(4) F55 0.178(4) 0.079(2) 0.109(3) 0.020(2) -0.011(3) 0.056(3) C55 0.140(6) 0.055(3) 0.053(3) 0.008(3) -0.003(4) 0.024(4) F56 0.084(2) 0.0746(19) 0.078(2) 0.0045(16) -0.0089(17) 0.0214(17) C56 0.091(4) 0.057(3) 0.044(3) -0.003(2) 0.002(3) 0.009(3) C61 0.047(3) 0.051(2) 0.043(3) 0.006(2) -0.002(2) 0.004(2) F62 0.0817(19) 0.0628(17) 0.0563(17) -0.0067(13) 0.0142(15) 0.0040(15) C62 0.054(3) 0.059(3) 0.046(3) 0.004(2) 0.001(2) 0.008(2) F63 0.091(2) 0.115(3) 0.0638(19) -0.0017(18) 0.0344(18) 0.021(2) C63 0.057(3) 0.083(4) 0.048(3) 0.011(3) 0.011(3) 0.011(3) C64 0.043(3) 0.098(4) 0.051(3) 0.024(3) 0.007(2) 0.003(3) F64 0.069(2) 0.128(3) 0.080(2) 0.043(2) 0.0226(17) -0.0009(19) F65 0.096(2) 0.082(2) 0.086(2) 0.0254(17) -0.0028(18) -0.0309(18) C65 0.058(3) 0.066(3) 0.060(3) 0.022(3) -0.002(3) -0.009(3) F66 0.106(2) 0.0540(16) 0.0613(17) 0.0003(13) 0.0115(17) -0.0103(16) C66 0.065(3) 0.059(3) 0.045(3) 0.008(2) 0.002(2) 0.004(3) C71 0.120(5) 0.054(3) 0.078(4) -0.008(3) -0.015(4) -0.004(3) C72 0.140(6) 0.067(4) 0.095(5) -0.004(3) -0.008(4) -0.008(4) C73 0.182(7) 0.066(4) 0.115(6) 0.007(4) -0.031(6) -0.014(5) C74 0.142(6) 0.055(3) 0.158(7) 0.003(4) -0.057(6) -0.006(4) C75 0.133(6) 0.065(4) 0.178(7) -0.002(5) 0.005(6) 0.000(4) C76 0.130(5) 0.068(4) 0.102(5) -0.015(3) 0.009(5) -0.001(4) C77 0.152(6) 0.106(5) 0.125(6) -0.018(4) -0.017(5) -0.002(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 Zr1 C3 2.273(4) . ? Zr1 C14 2.503(4) . ? Zr1 C11 2.525(4) . ? Zr1 C15 2.526(4) . ? Zr1 C20 2.532(4) . ? Zr1 C16 2.540(4) . ? Zr1 C19 2.543(4) . ? Zr1 C17 2.545(4) . ? Zr1 C13 2.551(4) . ? Zr1 C18 2.553(4) . ? Zr1 C4 2.561(4) . ? Zr1 C12 2.567(4) . ? Zr1 H4B 2.37(3) . ? P1 C1 1.850(4) . ? P1 C41 1.853(4) . ? P1 C31 1.854(4) . ? B1 C2 1.624(6) . ? B1 C61 1.655(6) . ? B1 C51 1.664(6) . ? B1 C4 1.683(6) . ? C11 C15 1.419(6) . ? C11 C12 1.420(6) . ? C11 C21 1.503(6) . ? C12 C13 1.407(6) . ? C12 C22 1.498(6) . ? C13 C14 1.412(6) . ? C13 C23 1.502(6) . ? C14 C15 1.416(6) . ? C14 C24 1.515(6) . ? C15 C25 1.507(6) . ? C16 C17 1.412(6) . ? C16 C20 1.424(6) . ? C16 C26 1.506(6) . ? C17 C18 1.412(6) . ? C17 C27 1.506(6) . ? C18 C19 1.414(6) . ? C18 C28 1.508(6) . ? C19 C20 1.414(6) . ? C19 C29 1.501(6) . ? C20 C30 1.510(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C2 C1 1.538(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.99(4) . ? C4 H4B 0.94(4) . ? C4 H4C 1.00(4) . ? C31 C32 1.414(6) . ? C31 C36 1.423(6) . ? C32 C33 1.393(6) . ? C32 C37 1.512(6) . ? C33 C34 1.381(6) . ? C33 H33 0.9400 . ? C34 C35 1.391(6) . ? C34 C38 1.510(6) . ? C35 C36 1.384(6) . ? C35 H35 0.9400 . ? C36 C39 1.513(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C41 C42 1.409(6) . ? C41 C46 1.413(6) . ? C42 C43 1.396(6) . ? C42 C47 1.510(6) . ? C43 C44 1.371(7) . ? C43 H43 0.9400 . ? C44 C45 1.378(7) . ? C44 C48 1.509(7) . ? C45 C46 1.396(6) . ? C45 H45 0.9400 . ? C46 C49 1.511(6) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C51 C56 1.377(6) . ? C51 C52 1.383(6) . ? F52 C52 1.355(6) . ? C52 C53 1.396(7) . ? F53 C53 1.352(6) . ? C53 C54 1.354(8) . ? F54 C54 1.349(6) . ? C54 C55 1.365(9) . ? F55 C55 1.345(7) . ? C55 C56 1.383(7) . ? F56 C56 1.358(6) . ? C61 C66 1.384(6) . ? C61 C62 1.386(6) . ? F62 C62 1.355(5) . ? C62 C63 1.384(6) . ? F63 C63 1.349(5) . ? C63 C64 1.361(7) . ? C64 F64 1.355(5) . ? C64 C65 1.363(7) . ? F65 C65 1.344(5) . ? C65 C66 1.388(6) . ? F66 C66 1.357(5) . ? C71 C76 1.371(8) . ? C71 C72 1.379(8) . ? C71 C77 1.512(8) . ? C72 C73 1.334(9) . ? C72 H72 0.9400 . ? C73 C74 1.349(10) . ? C73 H73 0.9400 . ? C74 C75 1.409(10) . ? C74 H74 0.9400 . ? C75 C76 1.414(10) . ? C75 H75 0.9400 . ? C76 H76 0.9400 . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C77 H77C 0.9700 . ? 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 C3 Zr1 C14 127.88(15) . . ? C3 Zr1 C11 89.51(15) . . ? C14 Zr1 C11 54.23(14) . . ? C3 Zr1 C15 122.10(15) . . ? C14 Zr1 C15 32.70(13) . . ? C11 Zr1 C15 32.64(13) . . ? C3 Zr1 C20 131.19(15) . . ? C14 Zr1 C20 97.59(14) . . ? C11 Zr1 C20 107.41(14) . . ? C15 Zr1 C20 85.39(14) . . ? C3 Zr1 C16 104.84(15) . . ? C14 Zr1 C16 110.96(15) . . ? C11 Zr1 C16 90.91(14) . . ? C15 Zr1 C16 84.53(14) . . ? C20 Zr1 C16 32.61(14) . . ? C3 Zr1 C19 115.60(15) . . ? C14 Zr1 C19 115.97(14) . . ? C11 Zr1 C19 139.70(13) . . ? C15 Zr1 C19 115.33(13) . . ? C20 Zr1 C19 32.34(13) . . ? C16 Zr1 C19 53.71(14) . . ? C3 Zr1 C17 77.78(15) . . ? C14 Zr1 C17 143.05(15) . . ? C11 Zr1 C17 107.98(14) . . ? C15 Zr1 C17 113.79(15) . . ? C20 Zr1 C17 53.57(14) . . ? C16 Zr1 C17 32.25(13) . . ? C19 Zr1 C17 53.44(14) . . ? C3 Zr1 C13 97.17(15) . . ? C14 Zr1 C13 32.43(13) . . ? C11 Zr1 C13 53.55(14) . . ? C15 Zr1 C13 53.54(14) . . ? C20 Zr1 C13 129.98(14) . . ? C16 Zr1 C13 138.02(14) . . ? C19 Zr1 C13 141.67(14) . . ? C17 Zr1 C13 161.24(14) . . ? C3 Zr1 C18 84.06(14) . . ? C14 Zr1 C18 148.00(14) . . ? C11 Zr1 C18 140.03(14) . . ? C15 Zr1 C18 136.36(13) . . ? C20 Zr1 C18 53.44(13) . . ? C16 Zr1 C18 53.44(13) . . ? C19 Zr1 C18 32.22(13) . . ? C17 Zr1 C18 32.15(13) . . ? C13 Zr1 C18 166.41(14) . . ? C3 Zr1 C4 86.57(15) . . ? C14 Zr1 C4 93.50(16) . . ? C11 Zr1 C4 133.28(16) . . ? C15 Zr1 C4 126.20(16) . . ? C20 Zr1 C4 109.89(15) . . ? C16 Zr1 C4 134.97(16) . . ? C19 Zr1 C4 81.85(15) . . ? C17 Zr1 C4 116.50(16) . . ? C13 Zr1 C4 80.81(16) . . ? C18 Zr1 C4 85.77(15) . . ? C3 Zr1 C12 75.49(14) . . ? C14 Zr1 C12 53.61(13) . . ? C11 Zr1 C12 32.38(13) . . ? C15 Zr1 C12 53.52(13) . . ? C20 Zr1 C12 137.98(14) . . ? C16 Zr1 C12 122.47(14) . . ? C19 Zr1 C12 168.52(13) . . ? C17 Zr1 C12 130.60(14) . . ? C13 Zr1 C12 31.91(13) . . ? C18 Zr1 C12 157.28(14) . . ? C4 Zr1 C12 102.54(16) . . ? C3 Zr1 H4B 78.5(8) . . ? C14 Zr1 H4B 114.3(9) . . ? C11 Zr1 H4B 151.1(9) . . ? C15 Zr1 H4B 146.7(9) . . ? C20 Zr1 H4B 100.1(8) . . ? C16 Zr1 H4B 117.4(9) . . ? C19 Zr1 H4B 68.4(9) . . ? C17 Zr1 H4B 95.1(9) . . ? C13 Zr1 H4B 101.6(9) . . ? C18 Zr1 H4B 65.3(9) . . ? C4 Zr1 H4B 21.6(9) . . ? C12 Zr1 H4B 118.8(9) . . ? C1 P1 C41 100.3(2) . . ? C1 P1 C31 111.82(19) . . ? C41 P1 C31 103.54(19) . . ? C2 B1 C61 104.3(3) . . ? C2 B1 C51 116.5(4) . . ? C61 B1 C51 113.1(4) . . ? C2 B1 C4 109.7(4) . . ? C61 B1 C4 112.2(4) . . ? C51 B1 C4 101.2(3) . . ? C15 C11 C12 107.7(4) . . ? C15 C11 C21 127.6(4) . . ? C12 C11 C21 123.9(4) . . ? C15 C11 Zr1 73.7(2) . . ? C12 C11 Zr1 75.5(2) . . ? C21 C11 Zr1 124.2(3) . . ? C13 C12 C11 107.9(4) . . ? C13 C12 C22 125.3(4) . . ? C11 C12 C22 125.9(4) . . ? C13 C12 Zr1 73.4(2) . . ? C11 C12 Zr1 72.2(2) . . ? C22 C12 Zr1 128.6(3) . . ? C12 C13 C14 108.4(4) . . ? C12 C13 C23 125.0(4) . . ? C14 C13 C23 125.7(4) . . ? C12 C13 Zr1 74.7(2) . . ? C14 C13 Zr1 71.9(2) . . ? C23 C13 Zr1 127.9(3) . . ? C13 C14 C15 107.9(4) . . ? C13 C14 C24 126.6(4) . . ? C15 C14 C24 125.1(4) . . ? C13 C14 Zr1 75.7(2) . . ? C15 C14 Zr1 74.6(2) . . ? C24 C14 Zr1 121.1(3) . . ? C14 C15 C11 107.8(4) . . ? C14 C15 C25 125.0(4) . . ? C11 C15 C25 125.7(4) . . ? C14 C15 Zr1 72.7(2) . . ? C11 C15 Zr1 73.6(2) . . ? C25 C15 Zr1 130.0(3) . . ? C17 C16 C20 107.5(4) . . ? C17 C16 C26 123.6(4) . . ? C20 C16 C26 127.0(4) . . ? C17 C16 Zr1 74.1(2) . . ? C20 C16 Zr1 73.4(2) . . ? C26 C16 Zr1 130.4(3) . . ? C18 C17 C16 108.4(4) . . ? C18 C17 C27 126.2(4) . . ? C16 C17 C27 124.8(4) . . ? C18 C17 Zr1 74.2(2) . . ? C16 C17 Zr1 73.7(2) . . ? C27 C17 Zr1 124.8(3) . . ? C17 C18 C19 108.1(4) . . ? C17 C18 C28 125.9(4) . . ? C19 C18 C28 125.5(4) . . ? C17 C18 Zr1 73.6(2) . . ? C19 C18 Zr1 73.5(2) . . ? C28 C18 Zr1 124.6(3) . . ? C20 C19 C18 107.9(4) . . ? C20 C19 C29 124.1(4) . . ? C18 C19 C29 127.5(4) . . ? C20 C19 Zr1 73.4(2) . . ? C18 C19 Zr1 74.3(2) . . ? C29 C19 Zr1 123.8(3) . . ? C19 C20 C16 108.1(4) . . ? C19 C20 C30 122.5(4) . . ? C16 C20 C30 127.9(4) . . ? C19 C20 Zr1 74.3(2) . . ? C16 C20 Zr1 74.0(2) . . ? C30 C20 Zr1 128.7(3) . . ? C11 C21 H21A 109.5 . . ? C11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C12 C22 H22A 109.5 . . ? C12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C13 C23 H23A 109.5 . . ? C13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C14 C24 H24A 109.5 . . ? C14 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C14 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C15 C25 H25A 109.5 . . ? C15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C15 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C16 C26 H26A 109.5 . . ? C16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C17 C27 H27A 109.5 . . ? C17 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C17 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C29 H29A 109.5 . . ? C19 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C19 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C20 C30 H30A 109.5 . . ? C20 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C20 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C1 C2 B1 115.6(3) . . ? C1 C2 H2A 108.4 . . ? B1 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? B1 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? C2 C1 P1 110.1(3) . . ? C2 C1 H1A 109.6 . . ? P1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? P1 C1 H1B 109.6 . . ? H1A C1 H1B 108.2 . . ? Zr1 C3 H3A 109.5 . . ? Zr1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Zr1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? B1 C4 Zr1 169.1(3) . . ? B1 C4 H4A 107(2) . . ? Zr1 C4 H4A 71(2) . . ? B1 C4 H4B 104(2) . . ? Zr1 C4 H4B 68(2) . . ? H4A C4 H4B 116(3) . . ? B1 C4 H4C 113(2) . . ? Zr1 C4 H4C 77(2) . . ? H4A C4 H4C 110(3) . . ? H4B C4 H4C 106(3) . . ? C32 C31 C36 117.2(4) . . ? C32 C31 P1 128.2(3) . . ? C36 C31 P1 114.3(3) . . ? C33 C32 C31 119.7(4) . . ? C33 C32 C37 116.4(4) . . ? C31 C32 C37 123.9(4) . . ? C34 C33 C32 123.5(4) . . ? C34 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C33 C34 C35 116.4(4) . . ? C33 C34 C38 121.5(5) . . ? C35 C34 C38 122.1(4) . . ? C36 C35 C34 122.8(4) . . ? C36 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C35 C36 C31 120.4(4) . . ? C35 C36 C39 117.6(4) . . ? C31 C36 C39 121.9(4) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C46 118.0(4) . . ? C42 C41 P1 124.9(3) . . ? C46 C41 P1 117.0(3) . . ? C43 C42 C41 119.7(4) . . ? C43 C42 C47 117.1(4) . . ? C41 C42 C47 123.2(4) . . ? C44 C43 C42 122.5(5) . . ? C44 C43 H43 118.7 . . ? C42 C43 H43 118.7 . . ? C43 C44 C45 117.8(5) . . ? C43 C44 C48 121.3(6) . . ? C45 C44 C48 120.9(5) . . ? C44 C45 C46 122.3(5) . . ? C44 C45 H45 118.9 . . ? C46 C45 H45 118.9 . . ? C45 C46 C41 119.6(4) . . ? C45 C46 C49 117.6(4) . . ? C41 C46 C49 122.8(4) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C56 C51 C52 112.6(4) . . ? C56 C51 B1 121.2(4) . . ? C52 C51 B1 125.7(4) . . ? F52 C52 C51 121.2(4) . . ? F52 C52 C53 114.8(5) . . ? C51 C52 C53 124.0(6) . . ? F53 C53 C54 121.2(6) . . ? F53 C53 C52 119.3(6) . . ? C54 C53 C52 119.5(6) . . ? F54 C54 C53 119.7(7) . . ? F54 C54 C55 120.6(7) . . ? C53 C54 C55 119.7(5) . . ? F55 C55 C54 120.2(5) . . ? F55 C55 C56 121.3(7) . . ? C54 C55 C56 118.5(6) . . ? F56 C56 C51 119.5(4) . . ? F56 C56 C55 114.8(5) . . ? C51 C56 C55 125.7(6) . . ? C66 C61 C62 112.5(4) . . ? C66 C61 B1 122.2(4) . . ? C62 C61 B1 124.3(4) . . ? F62 C62 C63 115.0(4) . . ? F62 C62 C61 120.1(4) . . ? C63 C62 C61 124.8(5) . . ? F63 C63 C64 120.3(4) . . ? F63 C63 C62 120.5(5) . . ? C64 C63 C62 119.2(5) . . ? F64 C64 C63 120.4(5) . . ? F64 C64 C65 119.8(5) . . ? C63 C64 C65 119.6(5) . . ? F65 C65 C64 120.5(5) . . ? F65 C65 C66 120.6(5) . . ? C64 C65 C66 118.9(5) . . ? F66 C66 C61 120.4(4) . . ? F66 C66 C65 114.7(4) . . ? C61 C66 C65 124.9(5) . . ? C76 C71 C72 121.8(7) . . ? C76 C71 C77 119.8(6) . . ? C72 C71 C77 118.4(7) . . ? C73 C72 C71 118.7(8) . . ? C73 C72 H72 120.6 . . ? C71 C72 H72 120.6 . . ? C72 C73 C74 122.4(9) . . ? C72 C73 H73 118.8 . . ? C74 C73 H73 118.8 . . ? C73 C74 C75 121.0(9) . . ? C73 C74 H74 119.5 . . ? C75 C74 H74 119.5 . . ? C74 C75 C76 116.8(8) . . ? C74 C75 H75 121.6 . . ? C76 C75 H75 121.6 . . ? C71 C76 C75 119.3(7) . . ? C71 C76 H76 120.3 . . ? C75 C76 H76 120.3 . . ? C71 C77 H77A 109.5 . . ? C71 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C71 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Zr1 C11 C15 176.8(3) . . . . ? C14 Zr1 C11 C15 37.1(2) . . . . ? C20 Zr1 C11 C15 -49.8(3) . . . . ? C16 Zr1 C11 C15 -78.4(3) . . . . ? C19 Zr1 C11 C15 -52.1(3) . . . . ? C17 Zr1 C11 C15 -106.2(3) . . . . ? C13 Zr1 C11 C15 77.5(3) . . . . ? C18 Zr1 C11 C15 -103.1(3) . . . . ? C4 Zr1 C11 C15 92.0(3) . . . . ? C12 Zr1 C11 C15 113.8(4) . . . . ? C3 Zr1 C11 C12 63.0(3) . . . . ? C14 Zr1 C11 C12 -76.8(3) . . . . ? C15 Zr1 C11 C12 -113.8(4) . . . . ? C20 Zr1 C11 C12 -163.6(2) . . . . ? C16 Zr1 C11 C12 167.8(3) . . . . ? C19 Zr1 C11 C12 -165.9(2) . . . . ? C17 Zr1 C11 C12 140.0(2) . . . . ? C13 Zr1 C11 C12 -36.3(2) . . . . ? C18 Zr1 C11 C12 143.1(2) . . . . ? C4 Zr1 C11 C12 -21.9(3) . . . . ? C3 Zr1 C11 C21 -58.4(4) . . . . ? C14 Zr1 C11 C21 161.9(4) . . . . ? C15 Zr1 C11 C21 124.8(5) . . . . ? C20 Zr1 C11 C21 75.0(4) . . . . ? C16 Zr1 C11 C21 46.4(4) . . . . ? C19 Zr1 C11 C21 72.7(4) . . . . ? C17 Zr1 C11 C21 18.6(4) . . . . ? C13 Zr1 C11 C21 -157.7(4) . . . . ? C18 Zr1 C11 C21 21.7(5) . . . . ? C4 Zr1 C11 C21 -143.2(3) . . . . ? C12 Zr1 C11 C21 -121.4(5) . . . . ? C15 C11 C12 C13 -2.1(5) . . . . ? C21 C11 C12 C13 -173.1(4) . . . . ? Zr1 C11 C12 C13 65.2(3) . . . . ? C15 C11 C12 C22 167.5(4) . . . . ? C21 C11 C12 C22 -3.5(7) . . . . ? Zr1 C11 C12 C22 -125.2(4) . . . . ? C15 C11 C12 Zr1 -67.3(3) . . . . ? C21 C11 C12 Zr1 121.7(4) . . . . ? C3 Zr1 C12 C13 131.3(3) . . . . ? C14 Zr1 C12 C13 -36.9(2) . . . . ? C11 Zr1 C12 C13 -115.7(4) . . . . ? C15 Zr1 C12 C13 -77.8(3) . . . . ? C20 Zr1 C12 C13 -91.9(3) . . . . ? C16 Zr1 C12 C13 -130.2(3) . . . . ? C19 Zr1 C12 C13 -63.2(8) . . . . ? C17 Zr1 C12 C13 -169.4(2) . . . . ? C18 Zr1 C12 C13 157.8(3) . . . . ? C4 Zr1 C12 C13 48.2(3) . . . . ? C3 Zr1 C12 C11 -113.1(3) . . . . ? C14 Zr1 C12 C11 78.8(3) . . . . ? C15 Zr1 C12 C11 37.9(2) . . . . ? C20 Zr1 C12 C11 23.8(3) . . . . ? C16 Zr1 C12 C11 -14.5(3) . . . . ? C19 Zr1 C12 C11 52.5(8) . . . . ? C17 Zr1 C12 C11 -53.7(3) . . . . ? C13 Zr1 C12 C11 115.7(4) . . . . ? C18 Zr1 C12 C11 -86.5(4) . . . . ? C4 Zr1 C12 C11 163.9(2) . . . . ? C3 Zr1 C12 C22 9.0(4) . . . . ? C14 Zr1 C12 C22 -159.1(5) . . . . ? C11 Zr1 C12 C22 122.1(5) . . . . ? C15 Zr1 C12 C22 159.9(5) . . . . ? C20 Zr1 C12 C22 145.8(4) . . . . ? C16 Zr1 C12 C22 107.6(4) . . . . ? C19 Zr1 C12 C22 174.6(6) . . . . ? C17 Zr1 C12 C22 68.4(5) . . . . ? C13 Zr1 C12 C22 -122.2(5) . . . . ? C18 Zr1 C12 C22 35.6(6) . . . . ? C4 Zr1 C12 C22 -74.0(4) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C22 C12 C13 C14 -169.6(4) . . . . ? Zr1 C12 C13 C14 64.5(3) . . . . ? C11 C12 C13 C23 169.8(4) . . . . ? C22 C12 C13 C23 0.1(7) . . . . ? Zr1 C12 C13 C23 -125.9(4) . . . . ? C11 C12 C13 Zr1 -64.4(3) . . . . ? C22 C12 C13 Zr1 126.0(4) . . . . ? C3 Zr1 C13 C12 -47.2(3) . . . . ? C14 Zr1 C13 C12 115.8(4) . . . . ? C11 Zr1 C13 C12 36.9(2) . . . . ? C15 Zr1 C13 C12 77.8(3) . . . . ? C20 Zr1 C13 C12 119.2(3) . . . . ? C16 Zr1 C13 C12 74.5(3) . . . . ? C19 Zr1 C13 C12 163.4(2) . . . . ? C17 Zr1 C13 C12 25.8(6) . . . . ? C18 Zr1 C13 C12 -141.6(5) . . . . ? C4 Zr1 C13 C12 -132.5(3) . . . . ? C3 Zr1 C13 C14 -162.9(3) . . . . ? C11 Zr1 C13 C14 -78.9(3) . . . . ? C15 Zr1 C13 C14 -38.0(2) . . . . ? C20 Zr1 C13 C14 3.4(3) . . . . ? C16 Zr1 C13 C14 -41.2(4) . . . . ? C19 Zr1 C13 C14 47.6(4) . . . . ? C17 Zr1 C13 C14 -90.0(5) . . . . ? C18 Zr1 C13 C14 102.7(6) . . . . ? C4 Zr1 C13 C14 111.7(3) . . . . ? C12 Zr1 C13 C14 -115.8(4) . . . . ? C3 Zr1 C13 C23 75.5(4) . . . . ? C14 Zr1 C13 C23 -121.5(5) . . . . ? C11 Zr1 C13 C23 159.6(5) . . . . ? C15 Zr1 C13 C23 -159.5(5) . . . . ? C20 Zr1 C13 C23 -118.1(4) . . . . ? C16 Zr1 C13 C23 -162.8(4) . . . . ? C19 Zr1 C13 C23 -74.0(5) . . . . ? C17 Zr1 C13 C23 148.5(4) . . . . ? C18 Zr1 C13 C23 -18.9(8) . . . . ? C4 Zr1 C13 C23 -9.8(4) . . . . ? C12 Zr1 C13 C23 122.7(5) . . . . ? C12 C13 C14 C15 1.9(5) . . . . ? C23 C13 C14 C15 -167.7(4) . . . . ? Zr1 C13 C14 C15 68.2(3) . . . . ? C12 C13 C14 C24 175.4(4) . . . . ? C23 C13 C14 C24 5.8(7) . . . . ? Zr1 C13 C14 C24 -118.3(4) . . . . ? C12 C13 C14 Zr1 -66.3(3) . . . . ? C23 C13 C14 Zr1 124.1(4) . . . . ? C3 Zr1 C14 C13 21.6(3) . . . . ? C11 Zr1 C14 C13 76.6(3) . . . . ? C15 Zr1 C14 C13 113.6(4) . . . . ? C20 Zr1 C14 C13 -177.4(3) . . . . ? C16 Zr1 C14 C13 151.8(3) . . . . ? C19 Zr1 C14 C13 -149.4(2) . . . . ? C17 Zr1 C14 C13 147.7(3) . . . . ? C18 Zr1 C14 C13 -154.4(3) . . . . ? C4 Zr1 C14 C13 -66.7(3) . . . . ? C12 Zr1 C14 C13 36.3(2) . . . . ? C3 Zr1 C14 C15 -92.0(3) . . . . ? C11 Zr1 C14 C15 -37.0(2) . . . . ? C20 Zr1 C14 C15 69.0(3) . . . . ? C16 Zr1 C14 C15 38.2(3) . . . . ? C19 Zr1 C14 C15 97.0(3) . . . . ? C17 Zr1 C14 C15 34.1(4) . . . . ? C13 Zr1 C14 C15 -113.6(4) . . . . ? C18 Zr1 C14 C15 92.0(3) . . . . ? C4 Zr1 C14 C15 179.7(3) . . . . ? C12 Zr1 C14 C15 -77.3(3) . . . . ? C3 Zr1 C14 C24 146.0(4) . . . . ? C11 Zr1 C14 C24 -159.0(4) . . . . ? C15 Zr1 C14 C24 -122.1(5) . . . . ? C20 Zr1 C14 C24 -53.0(4) . . . . ? C16 Zr1 C14 C24 -83.8(4) . . . . ? C19 Zr1 C14 C24 -25.0(4) . . . . ? C17 Zr1 C14 C24 -88.0(4) . . . . ? C13 Zr1 C14 C24 124.3(5) . . . . ? C18 Zr1 C14 C24 -30.0(5) . . . . ? C4 Zr1 C14 C24 57.6(4) . . . . ? C12 Zr1 C14 C24 160.6(4) . . . . ? C13 C14 C15 C11 -3.2(5) . . . . ? C24 C14 C15 C11 -176.7(4) . . . . ? Zr1 C14 C15 C11 65.8(3) . . . . ? C13 C14 C15 C25 163.9(4) . . . . ? C24 C14 C15 C25 -9.7(7) . . . . ? Zr1 C14 C15 C25 -127.2(4) . . . . ? C13 C14 C15 Zr1 -69.0(3) . . . . ? C24 C14 C15 Zr1 117.5(4) . . . . ? C12 C11 C15 C14 3.2(5) . . . . ? C21 C11 C15 C14 173.8(4) . . . . ? Zr1 C11 C15 C14 -65.2(3) . . . . ? C12 C11 C15 C25 -163.7(4) . . . . ? C21 C11 C15 C25 6.9(7) . . . . ? Zr1 C11 C15 C25 127.9(4) . . . . ? C12 C11 C15 Zr1 68.4(3) . . . . ? C21 C11 C15 Zr1 -121.0(5) . . . . ? C3 Zr1 C15 C14 111.4(3) . . . . ? C11 Zr1 C15 C14 115.2(4) . . . . ? C20 Zr1 C15 C14 -111.8(3) . . . . ? C16 Zr1 C15 C14 -144.5(3) . . . . ? C19 Zr1 C15 C14 -99.2(3) . . . . ? C17 Zr1 C15 C14 -158.4(2) . . . . ? C13 Zr1 C15 C14 37.7(2) . . . . ? C18 Zr1 C15 C14 -129.9(3) . . . . ? C4 Zr1 C15 C14 -0.4(3) . . . . ? C12 Zr1 C15 C14 77.6(3) . . . . ? C3 Zr1 C15 C11 -3.8(3) . . . . ? C14 Zr1 C15 C11 -115.2(4) . . . . ? C20 Zr1 C15 C11 133.0(3) . . . . ? C16 Zr1 C15 C11 100.3(3) . . . . ? C19 Zr1 C15 C11 145.6(2) . . . . ? C17 Zr1 C15 C11 86.4(3) . . . . ? C13 Zr1 C15 C11 -77.5(3) . . . . ? C18 Zr1 C15 C11 114.9(3) . . . . ? C4 Zr1 C15 C11 -115.6(3) . . . . ? C12 Zr1 C15 C11 -37.5(2) . . . . ? C3 Zr1 C15 C25 -127.0(4) . . . . ? C14 Zr1 C15 C25 121.6(5) . . . . ? C11 Zr1 C15 C25 -123.2(6) . . . . ? C20 Zr1 C15 C25 9.8(4) . . . . ? C16 Zr1 C15 C25 -22.9(4) . . . . ? C19 Zr1 C15 C25 22.4(5) . . . . ? C17 Zr1 C15 C25 -36.8(5) . . . . ? C13 Zr1 C15 C25 159.3(5) . . . . ? C18 Zr1 C15 C25 -8.3(5) . . . . ? C4 Zr1 C15 C25 121.2(4) . . . . ? C12 Zr1 C15 C25 -160.8(5) . . . . ? C3 Zr1 C16 C17 -33.9(3) . . . . ? C14 Zr1 C16 C17 -175.3(2) . . . . ? C11 Zr1 C16 C17 -123.6(3) . . . . ? C15 Zr1 C16 C17 -155.7(3) . . . . ? C20 Zr1 C16 C17 114.3(4) . . . . ? C19 Zr1 C16 C17 77.2(3) . . . . ? C13 Zr1 C16 C17 -153.1(3) . . . . ? C18 Zr1 C16 C17 36.9(2) . . . . ? C4 Zr1 C16 C17 66.3(3) . . . . ? C12 Zr1 C16 C17 -115.9(3) . . . . ? C3 Zr1 C16 C20 -148.2(3) . . . . ? C14 Zr1 C16 C20 70.4(3) . . . . ? C11 Zr1 C16 C20 122.0(3) . . . . ? C15 Zr1 C16 C20 90.0(3) . . . . ? C19 Zr1 C16 C20 -37.1(2) . . . . ? C17 Zr1 C16 C20 -114.3(4) . . . . ? C13 Zr1 C16 C20 92.6(3) . . . . ? C18 Zr1 C16 C20 -77.5(3) . . . . ? C4 Zr1 C16 C20 -48.0(3) . . . . ? C12 Zr1 C16 C20 129.7(2) . . . . ? C3 Zr1 C16 C26 87.0(5) . . . . ? C14 Zr1 C16 C26 -54.5(5) . . . . ? C11 Zr1 C16 C26 -2.8(5) . . . . ? C15 Zr1 C16 C26 -34.8(4) . . . . ? C20 Zr1 C16 C26 -124.8(6) . . . . ? C19 Zr1 C16 C26 -162.0(5) . . . . ? C17 Zr1 C16 C26 120.8(6) . . . . ? C13 Zr1 C16 C26 -32.2(5) . . . . ? C18 Zr1 C16 C26 157.7(5) . . . . ? C4 Zr1 C16 C26 -172.8(4) . . . . ? C12 Zr1 C16 C26 4.9(5) . . . . ? C20 C16 C17 C18 -0.4(5) . . . . ? C26 C16 C17 C18 165.1(4) . . . . ? Zr1 C16 C17 C18 -66.7(3) . . . . ? C20 C16 C17 C27 -172.3(4) . . . . ? C26 C16 C17 C27 -6.8(7) . . . . ? Zr1 C16 C17 C27 121.4(4) . . . . ? C20 C16 C17 Zr1 66.3(3) . . . . ? C26 C16 C17 Zr1 -128.2(4) . . . . ? C3 Zr1 C17 C18 -98.4(3) . . . . ? C14 Zr1 C17 C18 122.4(3) . . . . ? C11 Zr1 C17 C18 176.2(2) . . . . ? C15 Zr1 C17 C18 141.7(2) . . . . ? C20 Zr1 C17 C18 77.5(3) . . . . ? C16 Zr1 C17 C18 115.1(4) . . . . ? C19 Zr1 C17 C18 36.9(2) . . . . ? C13 Zr1 C17 C18 -174.5(4) . . . . ? C4 Zr1 C17 C18 -18.5(3) . . . . ? C12 Zr1 C17 C18 -156.8(2) . . . . ? C3 Zr1 C17 C16 146.6(3) . . . . ? C14 Zr1 C17 C16 7.3(4) . . . . ? C11 Zr1 C17 C16 61.1(3) . . . . ? C15 Zr1 C17 C16 26.6(3) . . . . ? C20 Zr1 C17 C16 -37.6(2) . . . . ? C19 Zr1 C17 C16 -78.1(3) . . . . ? C13 Zr1 C17 C16 70.5(5) . . . . ? C18 Zr1 C17 C16 -115.1(4) . . . . ? C4 Zr1 C17 C16 -133.6(3) . . . . ? C12 Zr1 C17 C16 88.1(3) . . . . ? C3 Zr1 C17 C27 25.1(4) . . . . ? C14 Zr1 C17 C27 -114.1(4) . . . . ? C11 Zr1 C17 C27 -60.3(4) . . . . ? C15 Zr1 C17 C27 -94.8(4) . . . . ? C20 Zr1 C17 C27 -159.0(5) . . . . ? C16 Zr1 C17 C27 -121.4(5) . . . . ? C19 Zr1 C17 C27 160.4(5) . . . . ? C13 Zr1 C17 C27 -50.9(7) . . . . ? C18 Zr1 C17 C27 123.5(5) . . . . ? C4 Zr1 C17 C27 105.0(4) . . . . ? C12 Zr1 C17 C27 -33.3(5) . . . . ? C16 C17 C18 C19 0.4(5) . . . . ? C27 C17 C18 C19 172.2(4) . . . . ? Zr1 C17 C18 C19 -65.9(3) . . . . ? C16 C17 C18 C28 -172.5(4) . . . . ? C27 C17 C18 C28 -0.8(7) . . . . ? Zr1 C17 C18 C28 121.1(4) . . . . ? C16 C17 C18 Zr1 66.3(3) . . . . ? C27 C17 C18 Zr1 -121.9(4) . . . . ? C3 Zr1 C18 C17 76.4(3) . . . . ? C14 Zr1 C18 C17 -106.7(3) . . . . ? C11 Zr1 C18 C17 -5.7(3) . . . . ? C15 Zr1 C18 C17 -55.2(3) . . . . ? C20 Zr1 C18 C17 -77.9(3) . . . . ? C16 Zr1 C18 C17 -37.0(2) . . . . ? C19 Zr1 C18 C17 -115.2(4) . . . . ? C13 Zr1 C18 C17 172.4(5) . . . . ? C4 Zr1 C18 C17 163.4(3) . . . . ? C12 Zr1 C18 C17 50.7(5) . . . . ? C3 Zr1 C18 C19 -168.4(3) . . . . ? C14 Zr1 C18 C19 8.4(4) . . . . ? C11 Zr1 C18 C19 109.5(3) . . . . ? C15 Zr1 C18 C19 59.9(3) . . . . ? C20 Zr1 C18 C19 37.2(2) . . . . ? C16 Zr1 C18 C19 78.2(3) . . . . ? C17 Zr1 C18 C19 115.2(4) . . . . ? C13 Zr1 C18 C19 -72.4(6) . . . . ? C4 Zr1 C18 C19 -81.4(3) . . . . ? C12 Zr1 C18 C19 165.8(3) . . . . ? C3 Zr1 C18 C28 -46.2(4) . . . . ? C14 Zr1 C18 C28 130.6(4) . . . . ? C11 Zr1 C18 C28 -128.4(3) . . . . ? C15 Zr1 C18 C28 -177.9(3) . . . . ? C20 Zr1 C18 C28 159.4(4) . . . . ? C16 Zr1 C18 C28 -159.7(4) . . . . ? C19 Zr1 C18 C28 122.1(5) . . . . ? C17 Zr1 C18 C28 -122.7(5) . . . . ? C13 Zr1 C18 C28 49.7(8) . . . . ? C4 Zr1 C18 C28 40.7(4) . . . . ? C12 Zr1 C18 C28 -72.0(5) . . . . ? C17 C18 C19 C20 -0.2(5) . . . . ? C28 C18 C19 C20 172.7(4) . . . . ? Zr1 C18 C19 C20 -66.2(3) . . . . ? C17 C18 C19 C29 -173.2(4) . . . . ? C28 C18 C19 C29 -0.2(7) . . . . ? Zr1 C18 C19 C29 120.8(4) . . . . ? C17 C18 C19 Zr1 66.0(3) . . . . ? C28 C18 C19 Zr1 -121.0(4) . . . . ? C3 Zr1 C19 C20 127.5(3) . . . . ? C14 Zr1 C19 C20 -60.4(3) . . . . ? C11 Zr1 C19 C20 4.1(4) . . . . ? C15 Zr1 C19 C20 -24.0(3) . . . . ? C16 Zr1 C19 C20 37.4(2) . . . . ? C17 Zr1 C19 C20 77.8(3) . . . . ? C13 Zr1 C19 C20 -86.5(3) . . . . ? C18 Zr1 C19 C20 114.7(4) . . . . ? C4 Zr1 C19 C20 -150.3(3) . . . . ? C12 Zr1 C19 C20 -37.0(8) . . . . ? C3 Zr1 C19 C18 12.8(3) . . . . ? C14 Zr1 C19 C18 -175.0(2) . . . . ? C11 Zr1 C19 C18 -110.6(3) . . . . ? C15 Zr1 C19 C18 -138.7(2) . . . . ? C20 Zr1 C19 C18 -114.7(4) . . . . ? C16 Zr1 C19 C18 -77.2(3) . . . . ? C17 Zr1 C19 C18 -36.8(2) . . . . ? C13 Zr1 C19 C18 158.8(2) . . . . ? C4 Zr1 C19 C18 95.0(3) . . . . ? C12 Zr1 C19 C18 -151.6(6) . . . . ? C3 Zr1 C19 C29 -112.2(3) . . . . ? C14 Zr1 C19 C29 60.0(4) . . . . ? C11 Zr1 C19 C29 124.4(3) . . . . ? C15 Zr1 C19 C29 96.4(3) . . . . ? C20 Zr1 C19 C29 120.3(5) . . . . ? C16 Zr1 C19 C29 157.8(4) . . . . ? C17 Zr1 C19 C29 -161.8(4) . . . . ? C13 Zr1 C19 C29 33.8(4) . . . . ? C18 Zr1 C19 C29 -125.0(4) . . . . ? C4 Zr1 C19 C29 -30.0(3) . . . . ? C12 Zr1 C19 C29 83.4(8) . . . . ? C18 C19 C20 C16 0.0(5) . . . . ? C29 C19 C20 C16 173.2(4) . . . . ? Zr1 C19 C20 C16 -66.8(3) . . . . ? C18 C19 C20 C30 -167.0(4) . . . . ? C29 C19 C20 C30 6.2(7) . . . . ? Zr1 C19 C20 C30 126.2(4) . . . . ? C18 C19 C20 Zr1 66.8(3) . . . . ? C29 C19 C20 Zr1 -120.0(4) . . . . ? C17 C16 C20 C19 0.3(5) . . . . ? C26 C16 C20 C19 -164.6(4) . . . . ? Zr1 C16 C20 C19 67.0(3) . . . . ? C17 C16 C20 C30 166.4(4) . . . . ? C26 C16 C20 C30 1.5(8) . . . . ? Zr1 C16 C20 C30 -126.9(5) . . . . ? C17 C16 C20 Zr1 -66.8(3) . . . . ? C26 C16 C20 Zr1 128.4(5) . . . . ? C3 Zr1 C20 C19 -72.0(3) . . . . ? C14 Zr1 C20 C19 128.0(3) . . . . ? C11 Zr1 C20 C19 -177.2(2) . . . . ? C15 Zr1 C20 C19 158.4(3) . . . . ? C16 Zr1 C20 C19 -114.6(4) . . . . ? C17 Zr1 C20 C19 -77.4(3) . . . . ? C13 Zr1 C20 C19 126.1(3) . . . . ? C18 Zr1 C20 C19 -37.1(2) . . . . ? C4 Zr1 C20 C19 31.4(3) . . . . ? C12 Zr1 C20 C19 169.7(2) . . . . ? C3 Zr1 C20 C16 42.6(3) . . . . ? C14 Zr1 C20 C16 -117.5(3) . . . . ? C11 Zr1 C20 C16 -62.7(3) . . . . ? C15 Zr1 C20 C16 -87.1(3) . . . . ? C19 Zr1 C20 C16 114.6(4) . . . . ? C17 Zr1 C20 C16 37.2(2) . . . . ? C13 Zr1 C20 C16 -119.3(3) . . . . ? C18 Zr1 C20 C16 77.5(3) . . . . ? C4 Zr1 C20 C16 146.0(3) . . . . ? C12 Zr1 C20 C16 -75.7(3) . . . . ? C3 Zr1 C20 C30 168.7(4) . . . . ? C14 Zr1 C20 C30 8.6(4) . . . . ? C11 Zr1 C20 C30 63.4(4) . . . . ? C15 Zr1 C20 C30 39.0(4) . . . . ? C16 Zr1 C20 C30 126.1(5) . . . . ? C19 Zr1 C20 C30 -119.3(5) . . . . ? C17 Zr1 C20 C30 163.3(5) . . . . ? C13 Zr1 C20 C30 6.8(5) . . . . ? C18 Zr1 C20 C30 -156.4(5) . . . . ? C4 Zr1 C20 C30 -87.9(4) . . . . ? C12 Zr1 C20 C30 50.4(5) . . . . ? C61 B1 C2 C1 59.0(4) . . . . ? C51 B1 C2 C1 -66.5(5) . . . . ? C4 B1 C2 C1 179.4(4) . . . . ? B1 C2 C1 P1 -163.0(3) . . . . ? C41 P1 C1 C2 67.5(3) . . . . ? C31 P1 C1 C2 176.7(3) . . . . ? C2 B1 C4 Zr1 106.3(18) . . . . ? C61 B1 C4 Zr1 -138.2(17) . . . . ? C51 B1 C4 Zr1 -17(2) . . . . ? C3 Zr1 C4 B1 22.7(18) . . . . ? C14 Zr1 C4 B1 150.5(19) . . . . ? C11 Zr1 C4 B1 108.8(18) . . . . ? C15 Zr1 C4 B1 150.7(18) . . . . ? C20 Zr1 C4 B1 -110.1(18) . . . . ? C16 Zr1 C4 B1 -84.9(19) . . . . ? C19 Zr1 C4 B1 -93.8(19) . . . . ? C17 Zr1 C4 B1 -51.8(19) . . . . ? C13 Zr1 C4 B1 120.5(19) . . . . ? C18 Zr1 C4 B1 -61.6(19) . . . . ? C12 Zr1 C4 B1 97.0(19) . . . . ? C1 P1 C31 C32 15.0(5) . . . . ? C41 P1 C31 C32 122.1(4) . . . . ? C1 P1 C31 C36 -172.3(3) . . . . ? C41 P1 C31 C36 -65.2(4) . . . . ? C36 C31 C32 C33 1.0(7) . . . . ? P1 C31 C32 C33 173.5(4) . . . . ? C36 C31 C32 C37 -178.0(5) . . . . ? P1 C31 C32 C37 -5.5(8) . . . . ? C31 C32 C33 C34 0.4(8) . . . . ? C37 C32 C33 C34 179.5(5) . . . . ? C32 C33 C34 C35 -1.6(8) . . . . ? C32 C33 C34 C38 179.7(5) . . . . ? C33 C34 C35 C36 1.4(7) . . . . ? C38 C34 C35 C36 -179.9(5) . . . . ? C34 C35 C36 C31 0.0(7) . . . . ? C34 C35 C36 C39 -177.3(4) . . . . ? C32 C31 C36 C35 -1.2(6) . . . . ? P1 C31 C36 C35 -174.8(3) . . . . ? C32 C31 C36 C39 176.0(4) . . . . ? P1 C31 C36 C39 2.4(5) . . . . ? C1 P1 C41 C42 68.7(4) . . . . ? C31 P1 C41 C42 -46.9(4) . . . . ? C1 P1 C41 C46 -111.6(4) . . . . ? C31 P1 C41 C46 132.8(3) . . . . ? C46 C41 C42 C43 0.5(6) . . . . ? P1 C41 C42 C43 -179.8(3) . . . . ? C46 C41 C42 C47 -179.3(4) . . . . ? P1 C41 C42 C47 0.4(6) . . . . ? C41 C42 C43 C44 -2.0(7) . . . . ? C47 C42 C43 C44 177.7(5) . . . . ? C42 C43 C44 C45 2.1(8) . . . . ? C42 C43 C44 C48 -177.8(5) . . . . ? C43 C44 C45 C46 -0.6(8) . . . . ? C48 C44 C45 C46 179.3(5) . . . . ? C44 C45 C46 C41 -0.9(8) . . . . ? C44 C45 C46 C49 179.3(5) . . . . ? C42 C41 C46 C45 0.9(6) . . . . ? P1 C41 C46 C45 -178.9(4) . . . . ? C42 C41 C46 C49 -179.3(4) . . . . ? P1 C41 C46 C49 1.0(6) . . . . ? C2 B1 C51 C56 170.3(4) . . . . ? C61 B1 C51 C56 49.4(5) . . . . ? C4 B1 C51 C56 -70.8(5) . . . . ? C2 B1 C51 C52 -18.2(6) . . . . ? C61 B1 C51 C52 -139.1(4) . . . . ? C4 B1 C51 C52 100.7(5) . . . . ? C56 C51 C52 F52 178.6(4) . . . . ? B1 C51 C52 F52 6.5(7) . . . . ? C56 C51 C52 C53 -0.3(7) . . . . ? B1 C51 C52 C53 -172.5(4) . . . . ? F52 C52 C53 F53 0.4(7) . . . . ? C51 C52 C53 F53 179.5(4) . . . . ? F52 C52 C53 C54 -178.3(5) . . . . ? C51 C52 C53 C54 0.7(8) . . . . ? F53 C53 C54 F54 0.7(8) . . . . ? C52 C53 C54 F54 179.5(4) . . . . ? F53 C53 C54 C55 -179.5(5) . . . . ? C52 C53 C54 C55 -0.7(9) . . . . ? F54 C54 C55 F55 0.5(9) . . . . ? C53 C54 C55 F55 -179.3(5) . . . . ? F54 C54 C55 C56 -179.7(5) . . . . ? C53 C54 C55 C56 0.5(9) . . . . ? C52 C51 C56 F56 -179.5(4) . . . . ? B1 C51 C56 F56 -7.0(6) . . . . ? C52 C51 C56 C55 0.1(7) . . . . ? B1 C51 C56 C55 172.6(4) . . . . ? F55 C55 C56 F56 -0.8(7) . . . . ? C54 C55 C56 F56 179.4(5) . . . . ? F55 C55 C56 C51 179.7(5) . . . . ? C54 C55 C56 C51 -0.1(8) . . . . ? C2 B1 C61 C66 72.4(5) . . . . ? C51 B1 C61 C66 -160.1(4) . . . . ? C4 B1 C61 C66 -46.4(5) . . . . ? C2 B1 C61 C62 -95.2(5) . . . . ? C51 B1 C61 C62 32.4(6) . . . . ? C4 B1 C61 C62 146.1(4) . . . . ? C66 C61 C62 F62 -176.6(4) . . . . ? B1 C61 C62 F62 -8.0(7) . . . . ? C66 C61 C62 C63 -0.6(7) . . . . ? B1 C61 C62 C63 168.0(4) . . . . ? F62 C62 C63 F63 -0.7(6) . . . . ? C61 C62 C63 F63 -176.9(4) . . . . ? F62 C62 C63 C64 177.7(4) . . . . ? C61 C62 C63 C64 1.6(7) . . . . ? F63 C63 C64 F64 0.7(7) . . . . ? C62 C63 C64 F64 -177.8(4) . . . . ? F63 C63 C64 C65 177.2(4) . . . . ? C62 C63 C64 C65 -1.3(7) . . . . ? F64 C64 C65 F65 -3.3(7) . . . . ? C63 C64 C65 F65 -179.8(4) . . . . ? F64 C64 C65 C66 176.7(4) . . . . ? C63 C64 C65 C66 0.2(7) . . . . ? C62 C61 C66 F66 177.3(4) . . . . ? B1 C61 C66 F66 8.4(6) . . . . ? C62 C61 C66 C65 -0.6(7) . . . . ? B1 C61 C66 C65 -169.5(4) . . . . ? F65 C65 C66 F66 2.9(6) . . . . ? C64 C65 C66 F66 -177.2(4) . . . . ? F65 C65 C66 C61 -179.1(4) . . . . ? C64 C65 C66 C61 0.8(7) . . . . ? C76 C71 C72 C73 -1.5(9) . . . . ? C77 C71 C72 C73 179.0(6) . . . . ? C71 C72 C73 C74 0.6(11) . . . . ? C72 C73 C74 C75 1.0(12) . . . . ? C73 C74 C75 C76 -1.8(10) . . . . ? C72 C71 C76 C75 0.6(9) . . . . ? C77 C71 C76 C75 -179.8(6) . . . . ? C74 C75 C76 C71 1.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 67.01 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.328 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.060 _database_code_depnum_ccdc_archive 'CCDC 950032' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk6927 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H50 B Cl2 F10 O P Zr' _chemical_formula_weight 1084.82 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' B B 0.0013 0.0007 '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' Zr Zr -2.9673 0.5597 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8875(2) _cell_length_b 17.4300(2) _cell_length_c 19.5656(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.0340(10) _cell_angle_gamma 90.00 _cell_volume 4983.20(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8468 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8350 _exptl_absorpt_correction_T_max 0.9376 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26276 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8562 _reflns_number_gt 7470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One disordered over two positions dichloromethane molecule was found in the asymmetrical unit. Several restraints (SADI, SAME, ISOR and SIMU) were used in order to improve refinement stability. ; _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^)+(0.0441P)^2^+6.6035P] 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 8562 _refine_ls_number_parameters 649 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.094 _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 Zr1 Zr 0.131260(19) 0.848065(18) 0.470467(16) 0.04059(11) Uani 1 1 d . . . P1 P 0.40726(5) 0.73674(4) 0.43379(4) 0.03208(17) Uani 1 1 d . . . B1 B 0.6678(2) 0.75144(19) 0.56548(18) 0.0365(7) Uani 1 1 d . . . O1 O 0.24611(13) 0.79292(11) 0.45984(10) 0.0357(4) Uani 1 1 d . . . C1 C 0.51181(19) 0.70426(17) 0.49078(16) 0.0369(6) Uani 1 1 d . . . H1A H 0.4972 0.6622 0.5201 0.044 Uiso 1 1 calc R . . H1B H 0.5543 0.6845 0.4624 0.044 Uiso 1 1 calc R . . C2 C 0.55831(19) 0.76978(17) 0.53758(16) 0.0384(7) Uani 1 1 d . . . H2A H 0.5281 0.7760 0.5775 0.046 Uiso 1 1 calc R . . H2B H 0.5517 0.8179 0.5112 0.046 Uiso 1 1 calc R . . C4 C 0.6799(2) 0.67131(19) 0.60933(18) 0.0497(8) Uani 1 1 d . . . H4A H 0.6515 0.6762 0.6498 0.075 Uiso 1 1 calc R . . H4B H 0.7445 0.6601 0.6243 0.075 Uiso 1 1 calc R . . H4C H 0.6508 0.6300 0.5800 0.075 Uiso 1 1 calc R . . C3 C 0.1486(3) 0.9520(2) 0.4027(2) 0.0611(10) Uani 1 1 d . . . H3A H 0.1995 0.9830 0.4259 0.092 Uiso 1 1 calc R . . H3B H 0.0930 0.9825 0.3952 0.092 Uiso 1 1 calc R . . H3C H 0.1605 0.9346 0.3582 0.092 Uiso 1 1 calc R . . C5 C 0.32809(19) 0.76298(16) 0.49537(15) 0.0343(6) Uani 1 1 d . . . H5 H 0.3586 0.8020 0.5287 0.041 Uiso 1 1 calc R . . C11 C -0.0289(3) 0.8511(3) 0.3971(3) 0.0736(12) Uani 1 1 d . . . H11 H -0.0579 0.8989 0.3882 0.088 Uiso 1 1 calc R . . C12 C 0.0256(3) 0.8149(3) 0.3558(2) 0.0718(12) Uani 1 1 d . . . H12 H 0.0395 0.8343 0.3142 0.086 Uiso 1 1 calc R . . C13 C 0.0552(3) 0.7464(3) 0.3863(2) 0.0662(11) Uani 1 1 d . . . H13 H 0.0920 0.7105 0.3685 0.079 Uiso 1 1 calc R . . C14 C 0.0220(3) 0.7385(3) 0.4477(2) 0.0674(11) Uani 1 1 d . . . H14 H 0.0335 0.6976 0.4795 0.081 Uiso 1 1 calc R . . C15 C -0.0324(3) 0.8038(3) 0.4533(2) 0.0758(13) Uani 1 1 d . . . H15 H -0.0652 0.8134 0.4889 0.091 Uiso 1 1 calc R . . C16 C 0.0753(3) 0.9200(3) 0.5643(2) 0.0751(13) Uani 1 1 d . . . H16 H 0.0146 0.9380 0.5544 0.090 Uiso 1 1 calc R . . C17 C 0.1023(3) 0.8484(3) 0.5919(2) 0.0731(12) Uani 1 1 d . . . H17 H 0.0641 0.8096 0.6035 0.088 Uiso 1 1 calc R . . C18 C 0.1992(4) 0.8452(4) 0.5991(2) 0.0859(17) Uani 1 1 d . . . H18 H 0.2375 0.8041 0.6167 0.103 Uiso 1 1 calc R . . C19 C 0.2261(3) 0.9152(4) 0.5749(3) 0.0880(16) Uani 1 1 d . . . H19 H 0.2867 0.9291 0.5734 0.106 Uiso 1 1 calc R . . C20 C 0.1511(4) 0.9607(3) 0.5536(3) 0.0835(14) Uani 1 1 d . . . H20 H 0.1511 1.0105 0.5352 0.100 Uiso 1 1 calc R . . C61 C 0.31365(19) 0.69066(17) 0.53551(15) 0.0359(6) Uani 1 1 d . . . C62 C 0.2469(2) 0.63807(19) 0.50767(17) 0.0446(7) Uani 1 1 d . . . H62 H 0.2103 0.6471 0.4636 0.053 Uiso 1 1 calc R . . C63 C 0.2336(3) 0.5723(2) 0.5442(2) 0.0609(10) Uani 1 1 d . . . H63 H 0.1889 0.5364 0.5246 0.073 Uiso 1 1 calc R . . C64 C 0.2862(3) 0.5594(2) 0.6095(2) 0.0716(12) Uani 1 1 d . . . H64 H 0.2773 0.5147 0.6342 0.086 Uiso 1 1 calc R . . C65 C 0.3511(3) 0.6118(2) 0.63821(19) 0.0639(10) Uani 1 1 d . . . H65 H 0.3860 0.6033 0.6829 0.077 Uiso 1 1 calc R . . C66 C 0.3655(2) 0.6772(2) 0.60157(17) 0.0480(8) Uani 1 1 d . . . H66 H 0.4106 0.7127 0.6214 0.058 Uiso 1 1 calc R . . C31 C 0.33974(19) 0.66836(16) 0.37489(14) 0.0334(6) Uani 1 1 d . . . C32 C 0.3478(2) 0.58791(17) 0.38561(16) 0.0396(7) Uani 1 1 d . . . C33 C 0.2851(2) 0.53994(18) 0.34465(16) 0.0426(7) Uani 1 1 d . . . H33 H 0.2898 0.4867 0.3524 0.051 Uiso 1 1 calc R . . C34 C 0.2160(2) 0.56713(19) 0.29295(16) 0.0426(7) Uani 1 1 d . . . C35 C 0.2111(2) 0.64571(18) 0.28167(15) 0.0412(7) Uani 1 1 d . . . H35 H 0.1653 0.6649 0.2459 0.049 Uiso 1 1 calc R . . C36 C 0.2708(2) 0.69719(17) 0.32095(14) 0.0362(6) Uani 1 1 d . . . C37 C 0.4207(2) 0.54952(18) 0.43875(19) 0.0541(9) Uani 1 1 d . . . H37A H 0.4166 0.4943 0.4325 0.081 Uiso 1 1 calc R . . H37B H 0.4119 0.5625 0.4852 0.081 Uiso 1 1 calc R . . H37C H 0.4806 0.5670 0.4327 0.081 Uiso 1 1 calc R . . C38 C 0.1499(3) 0.5127(2) 0.2490(2) 0.0623(10) Uani 1 1 d . . . H38A H 0.0878 0.5259 0.2529 0.093 Uiso 1 1 calc R . . H38B H 0.1631 0.4605 0.2652 0.093 Uiso 1 1 calc R . . H38C H 0.1563 0.5167 0.2007 0.093 Uiso 1 1 calc R . . C39 C 0.2585(2) 0.78072(18) 0.30041(17) 0.0448(7) Uani 1 1 d . . . H39A H 0.3047 0.7954 0.2740 0.067 Uiso 1 1 calc R . . H39B H 0.2649 0.8121 0.3420 0.067 Uiso 1 1 calc R . . H39C H 0.1982 0.7882 0.2721 0.067 Uiso 1 1 calc R . . C21 C 0.4500(2) 0.81168(17) 0.38323(16) 0.0381(7) Uani 1 1 d . . . C22 C 0.4954(2) 0.7869(2) 0.32975(16) 0.0456(8) Uani 1 1 d . . . C23 C 0.5327(2) 0.8425(2) 0.29214(19) 0.0564(9) Uani 1 1 d . . . H23 H 0.5621 0.8265 0.2562 0.068 Uiso 1 1 calc R . . C24 C 0.5283(2) 0.9199(3) 0.3054(2) 0.0621(11) Uani 1 1 d . . . C25 C 0.4854(2) 0.9427(2) 0.3585(2) 0.0559(9) Uani 1 1 d . . . H25 H 0.4824 0.9953 0.3683 0.067 Uiso 1 1 calc R . . C26 C 0.4461(2) 0.89038(18) 0.39835(18) 0.0436(7) Uani 1 1 d . . . C27 C 0.5073(3) 0.7046(2) 0.3089(2) 0.0604(10) Uani 1 1 d . . . H27A H 0.4505 0.6862 0.2808 0.091 Uiso 1 1 calc R . . H27B H 0.5232 0.6732 0.3504 0.091 Uiso 1 1 calc R . . H27C H 0.5557 0.7016 0.2822 0.091 Uiso 1 1 calc R . . C28 C 0.5687(3) 0.9791(3) 0.2636(3) 0.0961(17) Uani 1 1 d . . . H28A H 0.5993 0.9533 0.2304 0.144 Uiso 1 1 calc R . . H28B H 0.6125 1.0103 0.2946 0.144 Uiso 1 1 calc R . . H28C H 0.5202 1.0114 0.2387 0.144 Uiso 1 1 calc R . . C29 C 0.4017(2) 0.92317(18) 0.4551(2) 0.0531(9) Uani 1 1 d . . . H29A H 0.3996 0.9787 0.4514 0.080 Uiso 1 1 calc R . . H29B H 0.4369 0.9086 0.5002 0.080 Uiso 1 1 calc R . . H29C H 0.3399 0.9033 0.4503 0.080 Uiso 1 1 calc R . . C51 C 0.71202(19) 0.75228(17) 0.49360(16) 0.0375(7) Uani 1 1 d . . . F52 F 0.74326(19) 0.61854(12) 0.49084(14) 0.0790(7) Uani 1 1 d . . . C52 C 0.7409(2) 0.6888(2) 0.46086(19) 0.0517(8) Uani 1 1 d . . . F53 F 0.7963(2) 0.62592(17) 0.37019(16) 0.1035(10) Uani 1 1 d . . . C53 C 0.7683(3) 0.6906(3) 0.3975(2) 0.0652(11) Uani 1 1 d . . . F54 F 0.7934(2) 0.76171(19) 0.30021(13) 0.0987(10) Uani 1 1 d . . . C54 C 0.7674(3) 0.7583(3) 0.36230(19) 0.0652(11) Uani 1 1 d . . . F55 F 0.74270(16) 0.89123(15) 0.35932(12) 0.0733(7) Uani 1 1 d . . . C55 C 0.7410(2) 0.8236(2) 0.39200(18) 0.0528(9) Uani 1 1 d . . . F56 F 0.68921(14) 0.88641(11) 0.48114(11) 0.0551(5) Uani 1 1 d . . . C56 C 0.7145(2) 0.81904(19) 0.45589(17) 0.0423(7) Uani 1 1 d . . . C41 C 0.7207(2) 0.81755(17) 0.61965(15) 0.0386(7) Uani 1 1 d . . . F42 F 0.86504(14) 0.77173(18) 0.60440(13) 0.0854(8) Uani 1 1 d . . . C42 C 0.8150(2) 0.8199(2) 0.63691(17) 0.0539(9) Uani 1 1 d . . . F43 F 0.95665(17) 0.8661(2) 0.69891(14) 0.1088(11) Uani 1 1 d U . . C43 C 0.8648(3) 0.8683(3) 0.68559(19) 0.0666(12) Uani 1 1 d . . . F44 F 0.8668(2) 0.96717(16) 0.76762(12) 0.0937(9) Uani 1 1 d . . . C44 C 0.8193(3) 0.9188(2) 0.72073(18) 0.0627(11) Uani 1 1 d . . . F45 F 0.6806(2) 0.96708(16) 0.74169(14) 0.1043(10) Uani 1 1 d . . . C45 C 0.7268(3) 0.9188(2) 0.70715(18) 0.0601(10) Uani 1 1 d . . . F46 F 0.58736(16) 0.87246(15) 0.64999(13) 0.0823(8) Uani 1 1 d . . . C46 C 0.6797(2) 0.8687(2) 0.65803(18) 0.0498(8) Uani 1 1 d . . . C71 C 1.0629(9) 1.0744(7) 0.9176(8) 0.128(4) Uani 0.598(8) 1 d PDU A 1 H71A H 1.1239 1.0816 0.9066 0.153 Uiso 0.598(8) 1 calc PR A 1 H71B H 1.0640 1.0906 0.9657 0.153 Uiso 0.598(8) 1 calc PR A 1 Cl1 Cl 0.9769(8) 1.1265(6) 0.8571(6) 0.258(5) Uani 0.598(8) 1 d PDU A 1 Cl2 Cl 1.0275(3) 0.9805(3) 0.90487(17) 0.145(2) Uani 0.598(8) 1 d PDU A 1 C71A C 1.0519(12) 1.1120(14) 0.8880(13) 0.157(7) Uani 0.402(8) 1 d PDU A 2 H71C H 1.0855 1.0916 0.8535 0.188 Uiso 0.402(8) 1 calc PR A 2 H71D H 1.0876 1.1529 0.9150 0.188 Uiso 0.402(8) 1 calc PR A 2 Cl1A Cl 0.9413(6) 1.1420(6) 0.8501(5) 0.134(2) Uani 0.402(8) 1 d PDU A 2 Cl2A Cl 1.0211(12) 1.0412(12) 0.9405(10) 0.361(10) Uani 0.402(8) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.03301(17) 0.04464(19) 0.04555(19) -0.00315(13) 0.01108(13) 0.00221(13) P1 0.0298(4) 0.0311(4) 0.0350(4) 0.0002(3) 0.0055(3) 0.0001(3) B1 0.0346(17) 0.0328(17) 0.0407(18) -0.0030(14) 0.0035(14) -0.0014(14) O1 0.0322(10) 0.0371(11) 0.0388(11) 0.0038(9) 0.0094(8) 0.0033(8) C1 0.0291(14) 0.0362(15) 0.0431(16) -0.0034(13) 0.0012(12) -0.0001(12) C2 0.0342(15) 0.0380(16) 0.0426(16) -0.0061(13) 0.0067(13) -0.0025(13) C4 0.0495(19) 0.0417(18) 0.054(2) 0.0049(15) 0.0002(15) -0.0048(15) C3 0.057(2) 0.046(2) 0.084(3) 0.0186(19) 0.021(2) 0.0109(17) C5 0.0321(14) 0.0356(15) 0.0350(15) 0.0006(12) 0.0057(12) -0.0018(12) C11 0.044(2) 0.083(3) 0.087(3) -0.004(3) -0.007(2) 0.015(2) C12 0.059(2) 0.100(3) 0.053(2) 0.001(2) 0.0015(19) -0.004(2) C13 0.045(2) 0.075(3) 0.075(3) -0.025(2) 0.0017(19) -0.0027(19) C14 0.054(2) 0.067(3) 0.077(3) 0.003(2) 0.002(2) -0.018(2) C15 0.0363(19) 0.118(4) 0.076(3) -0.024(3) 0.0186(19) -0.016(2) C16 0.062(3) 0.094(3) 0.073(3) -0.030(3) 0.019(2) 0.018(2) C17 0.076(3) 0.102(4) 0.047(2) -0.010(2) 0.025(2) 0.003(3) C18 0.094(4) 0.125(5) 0.036(2) -0.015(2) 0.007(2) 0.049(3) C19 0.063(3) 0.131(5) 0.069(3) -0.048(3) 0.011(2) -0.016(3) C20 0.090(3) 0.073(3) 0.091(3) -0.032(3) 0.027(3) -0.004(3) C61 0.0359(15) 0.0372(16) 0.0350(15) 0.0040(12) 0.0076(12) -0.0015(12) C62 0.0434(17) 0.0467(18) 0.0417(17) 0.0077(14) 0.0035(14) -0.0049(14) C63 0.065(2) 0.051(2) 0.062(2) 0.0141(18) 0.0008(18) -0.0195(18) C64 0.090(3) 0.061(2) 0.060(2) 0.028(2) 0.005(2) -0.013(2) C65 0.070(2) 0.074(3) 0.0424(19) 0.0224(19) -0.0034(18) -0.002(2) C66 0.0485(18) 0.053(2) 0.0394(17) 0.0019(15) 0.0020(14) -0.0053(16) C31 0.0329(14) 0.0333(15) 0.0335(14) -0.0007(12) 0.0050(12) 0.0010(12) C32 0.0385(16) 0.0374(16) 0.0401(16) -0.0040(13) 0.0004(13) 0.0011(13) C33 0.0460(17) 0.0333(15) 0.0467(17) -0.0039(13) 0.0048(14) 0.0028(13) C34 0.0406(16) 0.0488(18) 0.0369(16) -0.0089(14) 0.0037(13) -0.0015(14) C35 0.0392(16) 0.0504(18) 0.0313(15) -0.0022(13) -0.0002(12) 0.0042(14) C36 0.0381(15) 0.0412(16) 0.0305(14) 0.0014(12) 0.0097(12) 0.0051(13) C37 0.056(2) 0.0299(16) 0.066(2) -0.0005(15) -0.0152(17) 0.0011(15) C38 0.060(2) 0.061(2) 0.058(2) -0.0144(18) -0.0099(18) -0.0068(18) C39 0.0445(17) 0.0471(18) 0.0406(17) 0.0110(14) 0.0031(14) 0.0064(14) C21 0.0336(15) 0.0398(16) 0.0410(16) 0.0051(13) 0.0079(12) -0.0042(13) C22 0.0341(16) 0.061(2) 0.0408(17) 0.0050(15) 0.0059(13) -0.0012(15) C23 0.0405(18) 0.085(3) 0.0455(19) 0.0131(19) 0.0120(15) -0.0026(18) C24 0.0443(19) 0.080(3) 0.062(2) 0.030(2) 0.0078(17) -0.0090(19) C25 0.0414(18) 0.049(2) 0.074(2) 0.0207(18) 0.0032(17) -0.0056(15) C26 0.0331(15) 0.0424(17) 0.0549(19) 0.0105(15) 0.0073(14) -0.0011(13) C27 0.058(2) 0.077(3) 0.053(2) -0.0108(19) 0.0257(17) -0.001(2) C28 0.079(3) 0.112(4) 0.100(4) 0.056(3) 0.024(3) -0.021(3) C29 0.051(2) 0.0308(16) 0.080(3) -0.0016(16) 0.0202(18) -0.0052(14) C51 0.0296(14) 0.0372(16) 0.0430(16) -0.0067(13) 0.0004(12) -0.0036(12) F52 0.1063(19) 0.0432(12) 0.0909(17) -0.0140(12) 0.0275(15) 0.0128(12) C52 0.0493(19) 0.0452(19) 0.059(2) -0.0152(16) 0.0062(16) -0.0019(15) F53 0.121(2) 0.096(2) 0.106(2) -0.0538(17) 0.0526(19) -0.0024(18) C53 0.058(2) 0.078(3) 0.062(2) -0.033(2) 0.0170(19) -0.005(2) F54 0.098(2) 0.151(3) 0.0566(14) -0.0286(16) 0.0395(14) -0.0346(19) C54 0.049(2) 0.105(3) 0.044(2) -0.019(2) 0.0142(16) -0.020(2) F55 0.0679(14) 0.0922(17) 0.0599(13) 0.0203(12) 0.0122(11) -0.0223(13) C55 0.0376(17) 0.071(2) 0.0479(19) 0.0042(18) 0.0036(15) -0.0143(17) F56 0.0624(12) 0.0411(10) 0.0637(12) 0.0060(9) 0.0163(10) -0.0007(9) C56 0.0342(15) 0.0465(18) 0.0454(17) -0.0028(14) 0.0055(13) -0.0038(13) C41 0.0428(17) 0.0362(15) 0.0356(15) 0.0030(13) 0.0042(13) -0.0069(13) F42 0.0372(11) 0.144(2) 0.0746(15) -0.0449(16) 0.0103(10) -0.0107(13) C42 0.052(2) 0.071(2) 0.0403(18) -0.0083(17) 0.0124(15) -0.0183(18) F43 0.0580(15) 0.191(3) 0.0778(17) -0.0429(19) 0.0130(13) -0.0598(18) C43 0.051(2) 0.104(3) 0.0432(19) -0.004(2) 0.0048(16) -0.041(2) F44 0.126(2) 0.0944(19) 0.0527(13) -0.0207(13) -0.0040(14) -0.0579(17) C44 0.090(3) 0.059(2) 0.0341(17) -0.0043(16) -0.0013(19) -0.034(2) F45 0.127(2) 0.0886(19) 0.0814(18) -0.0518(15) -0.0210(16) 0.0337(17) C45 0.087(3) 0.046(2) 0.0411(19) -0.0067(16) -0.0031(18) 0.0032(19) F46 0.0608(14) 0.0919(17) 0.0841(16) -0.0475(14) -0.0111(12) 0.0298(13) C46 0.056(2) 0.0439(18) 0.0435(18) -0.0047(15) -0.0045(15) 0.0018(16) C71 0.112(7) 0.143(8) 0.131(7) 0.041(6) 0.029(6) -0.003(6) Cl1 0.257(9) 0.210(7) 0.280(8) -0.039(5) -0.014(6) -0.014(6) Cl2 0.143(3) 0.175(4) 0.098(2) -0.002(2) -0.0225(18) 0.026(2) C71A 0.140(10) 0.166(11) 0.165(11) 0.009(9) 0.031(8) -0.011(9) Cl1A 0.138(5) 0.133(5) 0.128(4) -0.016(3) 0.015(3) -0.022(4) Cl2A 0.353(12) 0.338(13) 0.385(12) 0.025(9) 0.054(9) 0.020(9) _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 Zr1 O1 2.0067(19) . ? Zr1 C3 2.289(4) . ? Zr1 C14 2.493(4) . ? Zr1 C17 2.494(4) . ? Zr1 C16 2.495(4) . ? Zr1 C15 2.516(4) . ? Zr1 C18 2.527(4) . ? Zr1 C20 2.532(4) . ? Zr1 C13 2.535(4) . ? Zr1 C19 2.537(4) . ? Zr1 C11 2.537(4) . ? Zr1 C12 2.548(4) . ? P1 C31 1.821(3) . ? P1 C1 1.823(3) . ? P1 C21 1.825(3) . ? P1 C5 1.896(3) . ? B1 C4 1.631(5) . ? B1 C2 1.649(4) . ? B1 C41 1.659(4) . ? B1 C51 1.663(5) . ? O1 C5 1.386(3) . ? C1 C2 1.543(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C5 C61 1.522(4) . ? C5 H5 0.9900 . ? C11 C15 1.383(7) . ? C11 C12 1.399(6) . ? C11 H11 0.9400 . ? C12 C13 1.369(6) . ? C12 H12 0.9400 . ? C13 C14 1.392(6) . ? C13 H13 0.9400 . ? C14 C15 1.412(6) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C20 1.384(7) . ? C16 C17 1.387(7) . ? C16 H16 0.9400 . ? C17 C18 1.423(7) . ? C17 H17 0.9400 . ? C18 C19 1.395(7) . ? C18 H18 0.9400 . ? C19 C20 1.368(7) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C61 C62 1.385(4) . ? C61 C66 1.393(4) . ? C62 C63 1.385(5) . ? C62 H62 0.9400 . ? C63 C64 1.383(5) . ? C63 H63 0.9400 . ? C64 C65 1.369(6) . ? C64 H64 0.9400 . ? C65 C66 1.386(5) . ? C65 H65 0.9400 . ? C66 H66 0.9400 . ? C31 C36 1.416(4) . ? C31 C32 1.420(4) . ? C32 C33 1.389(4) . ? C32 C37 1.508(4) . ? C33 C34 1.381(4) . ? C33 H33 0.9400 . ? C34 C35 1.387(5) . ? C34 C38 1.512(4) . ? C35 C36 1.388(4) . ? C35 H35 0.9400 . ? C36 C39 1.512(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C21 C26 1.407(4) . ? C21 C22 1.418(4) . ? C22 C23 1.394(5) . ? C22 C27 1.511(5) . ? C23 C24 1.378(6) . ? C23 H23 0.9400 . ? C24 C25 1.377(6) . ? C24 C28 1.511(5) . ? C25 C26 1.398(5) . ? C25 H25 0.9400 . ? C26 C29 1.510(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C51 C56 1.382(4) . ? C51 C52 1.387(4) . ? F52 C52 1.356(4) . ? C52 C53 1.379(5) . ? F53 C53 1.347(5) . ? C53 C54 1.365(6) . ? F54 C54 1.345(4) . ? C54 C55 1.368(6) . ? F55 C55 1.344(4) . ? C55 C56 1.384(5) . ? F56 C56 1.355(4) . ? C41 C46 1.380(5) . ? C41 C42 1.381(5) . ? F42 C42 1.359(4) . ? C42 C43 1.378(5) . ? F43 C43 1.342(5) . ? C43 C44 1.373(6) . ? F44 C44 1.343(4) . ? C44 C45 1.352(6) . ? F45 C45 1.347(5) . ? C45 C46 1.386(5) . ? F46 C46 1.355(4) . ? C71 Cl2 1.723(12) . ? C71 Cl1 1.812(12) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71A Cl2A 1.723(15) . ? C71A Cl1A 1.752(15) . ? C71A H71C 0.9800 . ? C71A H71D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 C3 97.27(11) . . ? O1 Zr1 C14 98.89(12) . . ? C3 Zr1 C14 130.17(15) . . ? O1 Zr1 C17 113.93(12) . . ? C3 Zr1 C17 127.53(16) . . ? C14 Zr1 C17 86.90(16) . . ? O1 Zr1 C16 136.74(12) . . ? C3 Zr1 C16 96.86(16) . . ? C14 Zr1 C16 102.56(16) . . ? C17 Zr1 C16 32.30(15) . . ? O1 Zr1 C15 131.41(13) . . ? C3 Zr1 C15 112.27(16) . . ? C14 Zr1 C15 32.74(15) . . ? C17 Zr1 C15 77.81(15) . . ? C16 Zr1 C15 78.53(15) . . ? O1 Zr1 C18 84.68(12) . . ? C3 Zr1 C18 121.64(19) . . ? C14 Zr1 C18 106.61(19) . . ? C17 Zr1 C18 32.92(15) . . ? C16 Zr1 C18 53.35(15) . . ? C15 Zr1 C18 108.66(18) . . ? O1 Zr1 C20 116.18(14) . . ? C3 Zr1 C20 75.30(18) . . ? C14 Zr1 C20 134.49(16) . . ? C17 Zr1 C20 53.56(17) . . ? C16 Zr1 C20 31.95(15) . . ? C15 Zr1 C20 108.36(16) . . ? C18 Zr1 C20 53.10(18) . . ? O1 Zr1 C13 83.18(11) . . ? C3 Zr1 C13 105.23(16) . . ? C14 Zr1 C13 32.14(14) . . ? C17 Zr1 C13 118.93(16) . . ? C16 Zr1 C13 131.23(15) . . ? C15 Zr1 C13 52.97(14) . . ? C18 Zr1 C13 132.67(19) . . ? C20 Zr1 C13 160.57(15) . . ? O1 Zr1 C19 87.16(13) . . ? C3 Zr1 C19 89.7(2) . . ? C14 Zr1 C19 137.81(18) . . ? C17 Zr1 C19 53.33(17) . . ? C16 Zr1 C19 52.28(15) . . ? C15 Zr1 C19 128.68(15) . . ? C18 Zr1 C19 31.98(17) . . ? C20 Zr1 C19 31.31(17) . . ? C13 Zr1 C19 163.12(19) . . ? O1 Zr1 C11 132.70(12) . . ? C3 Zr1 C11 81.58(16) . . ? C14 Zr1 C11 53.44(15) . . ? C17 Zr1 C11 102.96(16) . . ? C16 Zr1 C11 89.78(15) . . ? C15 Zr1 C11 31.77(15) . . ? C18 Zr1 C11 135.87(17) . . ? C20 Zr1 C11 109.23(16) . . ? C13 Zr1 C11 52.55(14) . . ? C19 Zr1 C11 139.84(16) . . ? O1 Zr1 C12 101.24(12) . . ? C3 Zr1 C12 77.78(16) . . ? C14 Zr1 C12 52.93(15) . . ? C17 Zr1 C12 130.48(15) . . ? C16 Zr1 C12 121.68(15) . . ? C15 Zr1 C12 52.68(15) . . ? C18 Zr1 C12 159.17(19) . . ? C20 Zr1 C12 135.94(17) . . ? C13 Zr1 C12 31.26(14) . . ? C19 Zr1 C12 165.6(2) . . ? C11 Zr1 C12 31.94(14) . . ? C31 P1 C1 119.15(13) . . ? C31 P1 C21 109.44(14) . . ? C1 P1 C21 102.04(14) . . ? C31 P1 C5 103.01(13) . . ? C1 P1 C5 104.37(13) . . ? C21 P1 C5 119.70(14) . . ? C4 B1 C2 110.0(3) . . ? C4 B1 C41 105.5(2) . . ? C2 B1 C41 113.3(2) . . ? C4 B1 C51 115.5(3) . . ? C2 B1 C51 104.2(2) . . ? C41 B1 C51 108.6(2) . . ? C5 O1 Zr1 144.54(18) . . ? C2 C1 P1 111.5(2) . . ? C2 C1 H1A 109.3 . . ? P1 C1 H1A 109.3 . . ? C2 C1 H1B 109.3 . . ? P1 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C1 C2 B1 110.9(2) . . ? C1 C2 H2A 109.5 . . ? B1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? B1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? B1 C4 H4A 109.5 . . ? B1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? B1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Zr1 C3 H3A 109.5 . . ? Zr1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Zr1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O1 C5 C61 111.9(2) . . ? O1 C5 P1 111.54(19) . . ? C61 C5 P1 107.13(19) . . ? O1 C5 H5 108.7 . . ? C61 C5 H5 108.7 . . ? P1 C5 H5 108.7 . . ? C15 C11 C12 107.7(4) . . ? C15 C11 Zr1 73.3(2) . . ? C12 C11 Zr1 74.5(2) . . ? C15 C11 H11 126.1 . . ? C12 C11 H11 126.1 . . ? Zr1 C11 H11 118.1 . . ? C13 C12 C11 108.4(4) . . ? C13 C12 Zr1 73.8(2) . . ? C11 C12 Zr1 73.6(2) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Zr1 C12 H12 118.6 . . ? C12 C13 C14 108.9(4) . . ? C12 C13 Zr1 74.9(2) . . ? C14 C13 Zr1 72.3(2) . . ? C12 C13 H13 125.5 . . ? C14 C13 H13 125.5 . . ? Zr1 C13 H13 119.0 . . ? C13 C14 C15 106.9(4) . . ? C13 C14 Zr1 75.6(2) . . ? C15 C14 Zr1 74.5(2) . . ? C13 C14 H14 126.6 . . ? C15 C14 H14 126.6 . . ? Zr1 C14 H14 115.7 . . ? C11 C15 C14 108.1(4) . . ? C11 C15 Zr1 75.0(2) . . ? C14 C15 Zr1 72.7(2) . . ? C11 C15 H15 126.0 . . ? C14 C15 H15 126.0 . . ? Zr1 C15 H15 118.3 . . ? C20 C16 C17 109.6(4) . . ? C20 C16 Zr1 75.5(2) . . ? C17 C16 Zr1 73.8(2) . . ? C20 C16 H16 125.2 . . ? C17 C16 H16 125.2 . . ? Zr1 C16 H16 117.3 . . ? C16 C17 C18 106.7(5) . . ? C16 C17 Zr1 73.9(2) . . ? C18 C17 Zr1 74.8(2) . . ? C16 C17 H17 126.7 . . ? C18 C17 H17 126.7 . . ? Zr1 C17 H17 116.9 . . ? C19 C18 C17 106.5(4) . . ? C19 C18 Zr1 74.4(3) . . ? C17 C18 Zr1 72.3(2) . . ? C19 C18 H18 126.8 . . ? C17 C18 H18 126.8 . . ? Zr1 C18 H18 118.6 . . ? C20 C19 C18 109.8(5) . . ? C20 C19 Zr1 74.1(3) . . ? C18 C19 Zr1 73.6(3) . . ? C20 C19 H19 125.1 . . ? C18 C19 H19 125.1 . . ? Zr1 C19 H19 118.9 . . ? C19 C20 C16 107.4(5) . . ? C19 C20 Zr1 74.6(3) . . ? C16 C20 Zr1 72.6(2) . . ? C19 C20 H20 126.3 . . ? C16 C20 H20 126.3 . . ? Zr1 C20 H20 118.5 . . ? C62 C61 C66 118.9(3) . . ? C62 C61 C5 120.5(3) . . ? C66 C61 C5 120.7(3) . . ? C61 C62 C63 120.5(3) . . ? C61 C62 H62 119.8 . . ? C63 C62 H62 119.8 . . ? C64 C63 C62 120.0(3) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C65 C64 C63 120.1(3) . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.2(3) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C65 C66 C61 120.3(3) . . ? C65 C66 H66 119.8 . . ? C61 C66 H66 119.8 . . ? C36 C31 C32 119.3(3) . . ? C36 C31 P1 118.2(2) . . ? C32 C31 P1 122.1(2) . . ? C33 C32 C31 118.7(3) . . ? C33 C32 C37 116.5(3) . . ? C31 C32 C37 124.7(3) . . ? C34 C33 C32 122.7(3) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C33 C34 C35 117.7(3) . . ? C33 C34 C38 120.9(3) . . ? C35 C34 C38 121.4(3) . . ? C34 C35 C36 122.8(3) . . ? C34 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? C35 C36 C31 118.7(3) . . ? C35 C36 C39 116.3(3) . . ? C31 C36 C39 125.0(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C26 C21 C22 119.7(3) . . ? C26 C21 P1 123.5(2) . . ? C22 C21 P1 116.6(2) . . ? C23 C22 C21 118.2(3) . . ? C23 C22 C27 116.0(3) . . ? C21 C22 C27 125.8(3) . . ? C24 C23 C22 122.9(4) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C25 C24 C23 118.0(3) . . ? C25 C24 C28 120.1(4) . . ? C23 C24 C28 121.8(4) . . ? C24 C25 C26 122.4(4) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C25 C26 C21 118.7(3) . . ? C25 C26 C29 116.9(3) . . ? C21 C26 C29 124.4(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C56 C51 C52 112.5(3) . . ? C56 C51 B1 120.9(3) . . ? C52 C51 B1 126.2(3) . . ? F52 C52 C53 115.0(3) . . ? F52 C52 C51 120.4(3) . . ? C53 C52 C51 124.7(4) . . ? F53 C53 C54 119.9(4) . . ? F53 C53 C52 120.3(4) . . ? C54 C53 C52 119.8(4) . . ? F54 C54 C53 121.1(4) . . ? F54 C54 C55 120.2(4) . . ? C53 C54 C55 118.7(3) . . ? F55 C55 C54 119.6(3) . . ? F55 C55 C56 121.0(4) . . ? C54 C55 C56 119.4(4) . . ? F56 C56 C51 119.8(3) . . ? F56 C56 C55 115.3(3) . . ? C51 C56 C55 124.9(3) . . ? C46 C41 C42 112.4(3) . . ? C46 C41 B1 126.3(3) . . ? C42 C41 B1 120.9(3) . . ? F42 C42 C43 115.5(3) . . ? F42 C42 C41 119.3(3) . . ? C43 C42 C41 125.1(4) . . ? F43 C43 C44 120.2(3) . . ? F43 C43 C42 120.7(4) . . ? C44 C43 C42 119.1(4) . . ? F44 C44 C45 121.1(4) . . ? F44 C44 C43 120.0(4) . . ? C45 C44 C43 118.9(3) . . ? F45 C45 C44 120.0(3) . . ? F45 C45 C46 120.2(4) . . ? C44 C45 C46 119.8(4) . . ? F46 C46 C41 120.8(3) . . ? F46 C46 C45 114.7(3) . . ? C41 C46 C45 124.5(4) . . ? Cl2 C71 Cl1 102.9(7) . . ? Cl2 C71 H71A 111.2 . . ? Cl1 C71 H71A 111.2 . . ? Cl2 C71 H71B 111.2 . . ? Cl1 C71 H71B 111.2 . . ? H71A C71 H71B 109.1 . . ? Cl2A C71A Cl1A 97.4(11) . . ? Cl2A C71A H71C 112.3 . . ? Cl1A C71A H71C 112.3 . . ? Cl2A C71A H71D 112.3 . . ? Cl1A C71A H71D 112.3 . . ? H71C C71A H71D 109.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Zr1 O1 C5 121.4(3) . . . . ? C14 Zr1 O1 C5 -105.9(3) . . . . ? C17 Zr1 O1 C5 -15.4(3) . . . . ? C16 Zr1 O1 C5 13.2(4) . . . . ? C15 Zr1 O1 C5 -110.2(3) . . . . ? C18 Zr1 O1 C5 0.1(3) . . . . ? C20 Zr1 O1 C5 44.2(3) . . . . ? C13 Zr1 O1 C5 -134.1(3) . . . . ? C19 Zr1 O1 C5 32.1(3) . . . . ? C11 Zr1 O1 C5 -153.4(3) . . . . ? C12 Zr1 O1 C5 -159.7(3) . . . . ? C31 P1 C1 C2 -178.9(2) . . . . ? C21 P1 C1 C2 60.5(2) . . . . ? C5 P1 C1 C2 -64.8(2) . . . . ? P1 C1 C2 B1 -158.1(2) . . . . ? C4 B1 C2 C1 -59.0(3) . . . . ? C41 B1 C2 C1 -176.9(2) . . . . ? C51 B1 C2 C1 65.4(3) . . . . ? Zr1 O1 C5 C61 71.8(4) . . . . ? Zr1 O1 C5 P1 -168.16(18) . . . . ? C31 P1 C5 O1 -58.0(2) . . . . ? C1 P1 C5 O1 176.87(19) . . . . ? C21 P1 C5 O1 63.7(2) . . . . ? C31 P1 C5 C61 64.7(2) . . . . ? C1 P1 C5 C61 -60.4(2) . . . . ? C21 P1 C5 C61 -173.59(18) . . . . ? O1 Zr1 C11 C15 102.7(3) . . . . ? C3 Zr1 C11 C15 -165.2(3) . . . . ? C14 Zr1 C11 C15 37.7(3) . . . . ? C17 Zr1 C11 C15 -38.5(3) . . . . ? C16 Zr1 C11 C15 -68.2(3) . . . . ? C18 Zr1 C11 C15 -37.7(4) . . . . ? C20 Zr1 C11 C15 -94.0(3) . . . . ? C13 Zr1 C11 C15 78.2(3) . . . . ? C19 Zr1 C11 C15 -85.8(4) . . . . ? C12 Zr1 C11 C15 114.4(4) . . . . ? O1 Zr1 C11 C12 -11.8(4) . . . . ? C3 Zr1 C11 C12 80.4(3) . . . . ? C14 Zr1 C11 C12 -76.8(3) . . . . ? C17 Zr1 C11 C12 -152.9(3) . . . . ? C16 Zr1 C11 C12 177.4(3) . . . . ? C15 Zr1 C11 C12 -114.4(4) . . . . ? C18 Zr1 C11 C12 -152.1(3) . . . . ? C20 Zr1 C11 C12 151.5(3) . . . . ? C13 Zr1 C11 C12 -36.2(3) . . . . ? C19 Zr1 C11 C12 159.8(3) . . . . ? C15 C11 C12 C13 -0.1(5) . . . . ? Zr1 C11 C12 C13 66.2(3) . . . . ? C15 C11 C12 Zr1 -66.3(3) . . . . ? O1 Zr1 C12 C13 55.9(3) . . . . ? C3 Zr1 C12 C13 151.0(3) . . . . ? C14 Zr1 C12 C13 -36.8(3) . . . . ? C17 Zr1 C12 C13 -79.6(3) . . . . ? C16 Zr1 C12 C13 -118.4(3) . . . . ? C15 Zr1 C12 C13 -78.3(3) . . . . ? C18 Zr1 C12 C13 -48.9(5) . . . . ? C20 Zr1 C12 C13 -155.7(3) . . . . ? C19 Zr1 C12 C13 -179.2(5) . . . . ? C11 Zr1 C12 C13 -115.3(4) . . . . ? O1 Zr1 C12 C11 171.2(3) . . . . ? C3 Zr1 C12 C11 -93.7(3) . . . . ? C14 Zr1 C12 C11 78.5(3) . . . . ? C17 Zr1 C12 C11 35.7(4) . . . . ? C16 Zr1 C12 C11 -3.1(4) . . . . ? C15 Zr1 C12 C11 37.1(3) . . . . ? C18 Zr1 C12 C11 66.4(6) . . . . ? C20 Zr1 C12 C11 -40.3(4) . . . . ? C13 Zr1 C12 C11 115.3(4) . . . . ? C19 Zr1 C12 C11 -63.9(7) . . . . ? C11 C12 C13 C14 -1.2(5) . . . . ? Zr1 C12 C13 C14 64.8(3) . . . . ? C11 C12 C13 Zr1 -66.0(3) . . . . ? O1 Zr1 C13 C12 -125.1(3) . . . . ? C3 Zr1 C13 C12 -29.4(3) . . . . ? C14 Zr1 C13 C12 116.0(4) . . . . ? C17 Zr1 C13 C12 121.3(3) . . . . ? C16 Zr1 C13 C12 84.4(3) . . . . ? C15 Zr1 C13 C12 77.3(3) . . . . ? C18 Zr1 C13 C12 158.6(3) . . . . ? C20 Zr1 C13 C12 59.5(6) . . . . ? C19 Zr1 C13 C12 179.4(5) . . . . ? C11 Zr1 C13 C12 37.0(3) . . . . ? O1 Zr1 C13 C14 118.9(3) . . . . ? C3 Zr1 C13 C14 -145.4(3) . . . . ? C17 Zr1 C13 C14 5.3(3) . . . . ? C16 Zr1 C13 C14 -31.6(4) . . . . ? C15 Zr1 C13 C14 -38.8(3) . . . . ? C18 Zr1 C13 C14 42.6(3) . . . . ? C20 Zr1 C13 C14 -56.5(6) . . . . ? C19 Zr1 C13 C14 63.3(6) . . . . ? C11 Zr1 C13 C14 -79.0(3) . . . . ? C12 Zr1 C13 C14 -116.0(4) . . . . ? C12 C13 C14 C15 2.0(4) . . . . ? Zr1 C13 C14 C15 68.5(3) . . . . ? C12 C13 C14 Zr1 -66.5(3) . . . . ? O1 Zr1 C14 C13 -61.7(3) . . . . ? C3 Zr1 C14 C13 45.8(3) . . . . ? C17 Zr1 C14 C13 -175.4(3) . . . . ? C16 Zr1 C14 C13 156.2(3) . . . . ? C15 Zr1 C14 C13 112.5(4) . . . . ? C18 Zr1 C14 C13 -148.7(3) . . . . ? C20 Zr1 C14 C13 157.1(3) . . . . ? C19 Zr1 C14 C13 -157.3(3) . . . . ? C11 Zr1 C14 C13 76.0(3) . . . . ? C12 Zr1 C14 C13 35.8(2) . . . . ? O1 Zr1 C14 C15 -174.1(3) . . . . ? C3 Zr1 C14 C15 -66.7(3) . . . . ? C17 Zr1 C14 C15 72.1(3) . . . . ? C16 Zr1 C14 C15 43.7(3) . . . . ? C18 Zr1 C14 C15 98.8(3) . . . . ? C20 Zr1 C14 C15 44.6(4) . . . . ? C13 Zr1 C14 C15 -112.5(4) . . . . ? C19 Zr1 C14 C15 90.3(3) . . . . ? C11 Zr1 C14 C15 -36.5(3) . . . . ? C12 Zr1 C14 C15 -76.7(3) . . . . ? C12 C11 C15 C14 1.3(5) . . . . ? Zr1 C11 C15 C14 -65.8(3) . . . . ? C12 C11 C15 Zr1 67.1(3) . . . . ? C13 C14 C15 C11 -2.0(4) . . . . ? Zr1 C14 C15 C11 67.2(3) . . . . ? C13 C14 C15 Zr1 -69.2(3) . . . . ? O1 Zr1 C15 C11 -107.1(3) . . . . ? C3 Zr1 C15 C11 15.9(3) . . . . ? C14 Zr1 C15 C11 -114.8(4) . . . . ? C17 Zr1 C15 C11 141.7(3) . . . . ? C16 Zr1 C15 C11 108.7(3) . . . . ? C18 Zr1 C15 C11 153.3(3) . . . . ? C20 Zr1 C15 C11 97.1(3) . . . . ? C13 Zr1 C15 C11 -76.8(3) . . . . ? C19 Zr1 C15 C11 124.5(3) . . . . ? C12 Zr1 C15 C11 -37.3(3) . . . . ? O1 Zr1 C15 C14 7.8(3) . . . . ? C3 Zr1 C15 C14 130.7(3) . . . . ? C17 Zr1 C15 C14 -103.5(3) . . . . ? C16 Zr1 C15 C14 -136.5(3) . . . . ? C18 Zr1 C15 C14 -91.9(3) . . . . ? C20 Zr1 C15 C14 -148.1(3) . . . . ? C13 Zr1 C15 C14 38.0(3) . . . . ? C19 Zr1 C15 C14 -120.7(3) . . . . ? C11 Zr1 C15 C14 114.8(4) . . . . ? C12 Zr1 C15 C14 77.5(3) . . . . ? O1 Zr1 C16 C20 60.8(4) . . . . ? C3 Zr1 C16 C20 -47.5(3) . . . . ? C14 Zr1 C16 C20 178.7(3) . . . . ? C17 Zr1 C16 C20 115.9(4) . . . . ? C15 Zr1 C16 C20 -158.9(4) . . . . ? C18 Zr1 C16 C20 77.2(4) . . . . ? C13 Zr1 C16 C20 -164.7(3) . . . . ? C19 Zr1 C16 C20 36.8(3) . . . . ? C11 Zr1 C16 C20 -128.9(3) . . . . ? C12 Zr1 C16 C20 -127.3(3) . . . . ? O1 Zr1 C16 C17 -55.0(4) . . . . ? C3 Zr1 C16 C17 -163.3(3) . . . . ? C14 Zr1 C16 C17 62.9(3) . . . . ? C15 Zr1 C16 C17 85.3(3) . . . . ? C18 Zr1 C16 C17 -38.6(3) . . . . ? C20 Zr1 C16 C17 -115.9(4) . . . . ? C13 Zr1 C16 C17 79.5(3) . . . . ? C19 Zr1 C16 C17 -79.1(3) . . . . ? C11 Zr1 C16 C17 115.2(3) . . . . ? C12 Zr1 C16 C17 116.8(3) . . . . ? C20 C16 C17 C18 0.6(5) . . . . ? Zr1 C16 C17 C18 68.2(3) . . . . ? C20 C16 C17 Zr1 -67.6(3) . . . . ? O1 Zr1 C17 C16 142.1(3) . . . . ? C3 Zr1 C17 C16 21.1(4) . . . . ? C14 Zr1 C17 C16 -119.5(3) . . . . ? C15 Zr1 C17 C16 -87.8(3) . . . . ? C18 Zr1 C17 C16 112.8(5) . . . . ? C20 Zr1 C17 C16 36.3(3) . . . . ? C13 Zr1 C17 C16 -122.3(3) . . . . ? C19 Zr1 C17 C16 75.6(3) . . . . ? C11 Zr1 C17 C16 -68.2(3) . . . . ? C12 Zr1 C17 C16 -86.7(3) . . . . ? O1 Zr1 C17 C18 29.3(4) . . . . ? C3 Zr1 C17 C18 -91.8(4) . . . . ? C14 Zr1 C17 C18 127.6(3) . . . . ? C16 Zr1 C17 C18 -112.8(5) . . . . ? C15 Zr1 C17 C18 159.4(4) . . . . ? C20 Zr1 C17 C18 -76.5(3) . . . . ? C13 Zr1 C17 C18 124.8(3) . . . . ? C19 Zr1 C17 C18 -37.3(3) . . . . ? C11 Zr1 C17 C18 179.0(3) . . . . ? C12 Zr1 C17 C18 160.5(3) . . . . ? C16 C17 C18 C19 -0.5(5) . . . . ? Zr1 C17 C18 C19 67.1(3) . . . . ? C16 C17 C18 Zr1 -67.6(3) . . . . ? O1 Zr1 C18 C19 93.2(3) . . . . ? C3 Zr1 C18 C19 -2.1(3) . . . . ? C14 Zr1 C18 C19 -169.1(3) . . . . ? C17 Zr1 C18 C19 -113.5(4) . . . . ? C16 Zr1 C18 C19 -75.6(3) . . . . ? C15 Zr1 C18 C19 -134.8(3) . . . . ? C20 Zr1 C18 C19 -35.4(3) . . . . ? C13 Zr1 C18 C19 168.8(3) . . . . ? C11 Zr1 C18 C19 -114.9(4) . . . . ? C12 Zr1 C18 C19 -159.0(4) . . . . ? O1 Zr1 C18 C17 -153.3(3) . . . . ? C3 Zr1 C18 C17 111.4(3) . . . . ? C14 Zr1 C18 C17 -55.6(3) . . . . ? C16 Zr1 C18 C17 37.9(3) . . . . ? C15 Zr1 C18 C17 -21.3(4) . . . . ? C20 Zr1 C18 C17 78.1(3) . . . . ? C13 Zr1 C18 C17 -77.7(3) . . . . ? C19 Zr1 C18 C17 113.5(4) . . . . ? C11 Zr1 C18 C17 -1.4(5) . . . . ? C12 Zr1 C18 C17 -45.5(6) . . . . ? C17 C18 C19 C20 0.2(5) . . . . ? Zr1 C18 C19 C20 65.9(3) . . . . ? C17 C18 C19 Zr1 -65.6(3) . . . . ? O1 Zr1 C19 C20 158.7(3) . . . . ? C3 Zr1 C19 C20 61.4(3) . . . . ? C14 Zr1 C19 C20 -101.2(4) . . . . ? C17 Zr1 C19 C20 -78.4(3) . . . . ? C16 Zr1 C19 C20 -37.6(3) . . . . ? C15 Zr1 C19 C20 -57.4(4) . . . . ? C18 Zr1 C19 C20 -116.8(4) . . . . ? C13 Zr1 C19 C20 -146.3(5) . . . . ? C11 Zr1 C19 C20 -15.1(5) . . . . ? C12 Zr1 C19 C20 32.4(8) . . . . ? O1 Zr1 C19 C18 -84.5(3) . . . . ? C3 Zr1 C19 C18 178.2(3) . . . . ? C14 Zr1 C19 C18 15.6(4) . . . . ? C17 Zr1 C19 C18 38.4(3) . . . . ? C16 Zr1 C19 C18 79.3(3) . . . . ? C15 Zr1 C19 C18 59.5(4) . . . . ? C20 Zr1 C19 C18 116.8(4) . . . . ? C13 Zr1 C19 C18 -29.5(7) . . . . ? C11 Zr1 C19 C18 101.7(4) . . . . ? C12 Zr1 C19 C18 149.2(6) . . . . ? C18 C19 C20 C16 0.1(5) . . . . ? Zr1 C19 C20 C16 65.7(3) . . . . ? C18 C19 C20 Zr1 -65.5(3) . . . . ? C17 C16 C20 C19 -0.4(5) . . . . ? Zr1 C16 C20 C19 -67.0(3) . . . . ? C17 C16 C20 Zr1 66.6(3) . . . . ? O1 Zr1 C20 C19 -23.9(4) . . . . ? C3 Zr1 C20 C19 -114.8(4) . . . . ? C14 Zr1 C20 C19 112.6(4) . . . . ? C17 Zr1 C20 C19 77.6(4) . . . . ? C16 Zr1 C20 C19 114.3(5) . . . . ? C15 Zr1 C20 C19 136.2(3) . . . . ? C18 Zr1 C20 C19 36.2(3) . . . . ? C13 Zr1 C20 C19 151.0(5) . . . . ? C11 Zr1 C20 C19 169.8(3) . . . . ? C12 Zr1 C20 C19 -169.0(3) . . . . ? O1 Zr1 C20 C16 -138.2(3) . . . . ? C3 Zr1 C20 C16 130.9(3) . . . . ? C14 Zr1 C20 C16 -1.8(4) . . . . ? C17 Zr1 C20 C16 -36.7(3) . . . . ? C15 Zr1 C20 C16 21.9(4) . . . . ? C18 Zr1 C20 C16 -78.1(3) . . . . ? C13 Zr1 C20 C16 36.7(7) . . . . ? C19 Zr1 C20 C16 -114.3(5) . . . . ? C11 Zr1 C20 C16 55.5(4) . . . . ? C12 Zr1 C20 C16 76.7(4) . . . . ? O1 C5 C61 C62 37.6(4) . . . . ? P1 C5 C61 C62 -85.0(3) . . . . ? O1 C5 C61 C66 -140.7(3) . . . . ? P1 C5 C61 C66 96.8(3) . . . . ? C66 C61 C62 C63 -1.6(5) . . . . ? C5 C61 C62 C63 -179.9(3) . . . . ? C61 C62 C63 C64 1.1(6) . . . . ? C62 C63 C64 C65 0.3(7) . . . . ? C63 C64 C65 C66 -1.1(7) . . . . ? C64 C65 C66 C61 0.6(6) . . . . ? C62 C61 C66 C65 0.8(5) . . . . ? C5 C61 C66 C65 179.1(3) . . . . ? C1 P1 C31 C36 -166.4(2) . . . . ? C21 P1 C31 C36 -49.7(3) . . . . ? C5 P1 C31 C36 78.7(2) . . . . ? C1 P1 C31 C32 20.0(3) . . . . ? C21 P1 C31 C32 136.8(3) . . . . ? C5 P1 C31 C32 -94.9(3) . . . . ? C36 C31 C32 C33 -2.8(4) . . . . ? P1 C31 C32 C33 170.7(2) . . . . ? C36 C31 C32 C37 176.9(3) . . . . ? P1 C31 C32 C37 -9.6(5) . . . . ? C31 C32 C33 C34 1.2(5) . . . . ? C37 C32 C33 C34 -178.5(3) . . . . ? C32 C33 C34 C35 0.9(5) . . . . ? C32 C33 C34 C38 179.2(3) . . . . ? C33 C34 C35 C36 -1.5(5) . . . . ? C38 C34 C35 C36 -179.8(3) . . . . ? C34 C35 C36 C31 -0.1(5) . . . . ? C34 C35 C36 C39 177.8(3) . . . . ? C32 C31 C36 C35 2.2(4) . . . . ? P1 C31 C36 C35 -171.5(2) . . . . ? C32 C31 C36 C39 -175.5(3) . . . . ? P1 C31 C36 C39 10.8(4) . . . . ? C31 P1 C21 C26 134.2(3) . . . . ? C1 P1 C21 C26 -98.7(3) . . . . ? C5 P1 C21 C26 15.7(3) . . . . ? C31 P1 C21 C22 -50.9(3) . . . . ? C1 P1 C21 C22 76.2(3) . . . . ? C5 P1 C21 C22 -169.4(2) . . . . ? C26 C21 C22 C23 -2.0(4) . . . . ? P1 C21 C22 C23 -177.1(2) . . . . ? C26 C21 C22 C27 178.3(3) . . . . ? P1 C21 C22 C27 3.2(4) . . . . ? C21 C22 C23 C24 0.9(5) . . . . ? C27 C22 C23 C24 -179.3(3) . . . . ? C22 C23 C24 C25 0.3(6) . . . . ? C22 C23 C24 C28 -179.6(4) . . . . ? C23 C24 C25 C26 -0.5(5) . . . . ? C28 C24 C25 C26 179.4(4) . . . . ? C24 C25 C26 C21 -0.6(5) . . . . ? C24 C25 C26 C29 179.7(3) . . . . ? C22 C21 C26 C25 1.8(4) . . . . ? P1 C21 C26 C25 176.6(2) . . . . ? C22 C21 C26 C29 -178.5(3) . . . . ? P1 C21 C26 C29 -3.7(4) . . . . ? C4 B1 C51 C56 -173.4(3) . . . . ? C2 B1 C51 C56 65.9(3) . . . . ? C41 B1 C51 C56 -55.1(3) . . . . ? C4 B1 C51 C52 13.6(4) . . . . ? C2 B1 C51 C52 -107.2(3) . . . . ? C41 B1 C51 C52 131.9(3) . . . . ? C56 C51 C52 F52 179.6(3) . . . . ? B1 C51 C52 F52 -6.8(5) . . . . ? C56 C51 C52 C53 -0.7(5) . . . . ? B1 C51 C52 C53 172.9(3) . . . . ? F52 C52 C53 F53 -1.1(5) . . . . ? C51 C52 C53 F53 179.2(3) . . . . ? F52 C52 C53 C54 179.1(3) . . . . ? C51 C52 C53 C54 -0.6(6) . . . . ? F53 C53 C54 F54 0.5(6) . . . . ? C52 C53 C54 F54 -179.7(3) . . . . ? F53 C53 C54 C55 -178.2(3) . . . . ? C52 C53 C54 C55 1.5(6) . . . . ? F54 C54 C55 F55 -1.0(5) . . . . ? C53 C54 C55 F55 177.7(3) . . . . ? F54 C54 C55 C56 -180.0(3) . . . . ? C53 C54 C55 C56 -1.2(5) . . . . ? C52 C51 C56 F56 -179.4(3) . . . . ? B1 C51 C56 F56 6.7(4) . . . . ? C52 C51 C56 C55 1.0(4) . . . . ? B1 C51 C56 C55 -172.9(3) . . . . ? F55 C55 C56 F56 1.3(4) . . . . ? C54 C55 C56 F56 -179.7(3) . . . . ? F55 C55 C56 C51 -179.0(3) . . . . ? C54 C55 C56 C51 -0.1(5) . . . . ? C4 B1 C41 C46 -99.2(4) . . . . ? C2 B1 C41 C46 21.2(4) . . . . ? C51 B1 C41 C46 136.4(3) . . . . ? C4 B1 C41 C42 72.8(4) . . . . ? C2 B1 C41 C42 -166.8(3) . . . . ? C51 B1 C41 C42 -51.6(4) . . . . ? C46 C41 C42 F42 178.8(3) . . . . ? B1 C41 C42 F42 5.8(5) . . . . ? C46 C41 C42 C43 -1.3(5) . . . . ? B1 C41 C42 C43 -174.3(3) . . . . ? F42 C42 C43 F43 -0.3(6) . . . . ? C41 C42 C43 F43 179.8(4) . . . . ? F42 C42 C43 C44 180.0(4) . . . . ? C41 C42 C43 C44 0.1(6) . . . . ? F43 C43 C44 F44 1.2(6) . . . . ? C42 C43 C44 F44 -179.0(3) . . . . ? F43 C43 C44 C45 -178.9(4) . . . . ? C42 C43 C44 C45 0.9(6) . . . . ? F44 C44 C45 F45 -1.1(6) . . . . ? C43 C44 C45 F45 179.0(4) . . . . ? F44 C44 C45 C46 179.4(3) . . . . ? C43 C44 C45 C46 -0.5(6) . . . . ? C42 C41 C46 F46 -177.6(3) . . . . ? B1 C41 C46 F46 -5.0(5) . . . . ? C42 C41 C46 C45 1.8(5) . . . . ? B1 C41 C46 C45 174.3(3) . . . . ? F45 C45 C46 F46 -1.1(5) . . . . ? C44 C45 C46 F46 178.4(3) . . . . ? F45 C45 C46 C41 179.5(3) . . . . ? C44 C45 C46 C41 -1.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.833 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.055 _database_code_depnum_ccdc_archive 'CCDC 950033' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk6936 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H72 B F10 O2 P Zr' _chemical_formula_weight 1148.18 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' B B 0.0013 0.0007 '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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0108(1) _cell_length_b 25.1301(4) _cell_length_c 24.9895(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.229(1) _cell_angle_gamma 90.00 _cell_volume 5654.40(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13245 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 0.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9161 _exptl_absorpt_correction_T_max 0.9709 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54527 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9886 _reflns_number_gt 8382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+6.7868P] 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 9886 _refine_ls_number_parameters 684 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.02723(4) 0.396114(12) 0.360969(13) 0.04075(13) Uani 1 1 d . . . P1 P 0.12554(9) 0.24039(3) 0.46300(3) 0.0353(2) Uani 1 1 d . . . B1 B 0.3511(4) 0.14545(15) 0.34807(15) 0.0405(8) Uani 1 1 d . . . O1 O 0.0402(3) 0.32556(9) 0.40795(9) 0.0444(5) Uani 1 1 d . . . O2 O -0.1318(3) 0.29818(11) 0.46363(13) 0.0632(7) Uani 1 1 d . . . C1 C 0.2108(4) 0.21896(13) 0.40189(13) 0.0411(7) Uani 1 1 d . . . H1A H 0.1317 0.2117 0.3748 0.049 Uiso 1 1 calc R . . H1B H 0.2704 0.2484 0.3886 0.049 Uiso 1 1 calc R . . C2 C 0.3105(4) 0.16939(13) 0.40713(13) 0.0410(7) Uani 1 1 d . . . H2A H 0.2596 0.1419 0.4274 0.049 Uiso 1 1 calc R . . H2B H 0.4025 0.1787 0.4271 0.049 Uiso 1 1 calc R . . C5 C -0.0146(4) 0.29451(13) 0.44270(13) 0.0405(7) Uani 1 1 d . . . C3 C 0.2709(4) 0.38310(15) 0.33555(14) 0.0449(8) Uani 1 1 d . . . H3A H 0.3386 0.3891 0.3661 0.067 Uiso 1 1 calc R . . H3B H 0.2933 0.4079 0.3072 0.067 Uiso 1 1 calc R . . H3C H 0.2823 0.3469 0.3228 0.067 Uiso 1 1 calc R . . C4 C 0.4588(4) 0.18740(15) 0.31802(15) 0.0507(9) Uani 1 1 d . . . H4A H 0.4761 0.1748 0.2821 0.076 Uiso 1 1 calc R . . H4B H 0.5528 0.1903 0.3381 0.076 Uiso 1 1 calc R . . H4C H 0.4114 0.2220 0.3161 0.076 Uiso 1 1 calc R . . C11 C -0.0206(8) 0.49256(17) 0.3860(2) 0.0828(16) Uani 1 1 d U . . C12 C -0.0804(6) 0.4588(2) 0.4272(3) 0.096(2) Uani 1 1 d U . . C13 C 0.0439(9) 0.43695(17) 0.45384(19) 0.0864(18) Uani 1 1 d U . . C14 C 0.1657(7) 0.4537(3) 0.4306(3) 0.0950(19) Uani 1 1 d U . . C15 C 0.1282(7) 0.4865(2) 0.3901(2) 0.0862(17) Uani 1 1 d U . . C21 C -0.1025(13) 0.5362(3) 0.3555(4) 0.200(5) Uani 1 1 d U . . H21A H -0.2086 0.5316 0.3589 0.299 Uiso 1 1 calc R . . H21B H -0.0789 0.5344 0.3180 0.299 Uiso 1 1 calc R . . H21C H -0.0726 0.5705 0.3700 0.299 Uiso 1 1 calc R . . C22 C -0.2394(9) 0.4556(4) 0.4434(5) 0.224(6) Uani 1 1 d U . . H22A H -0.3025 0.4744 0.4175 0.337 Uiso 1 1 calc R . . H22B H -0.2483 0.4716 0.4784 0.337 Uiso 1 1 calc R . . H22C H -0.2697 0.4186 0.4448 0.337 Uiso 1 1 calc R . . C23 C 0.0451(16) 0.4055(3) 0.5050(2) 0.202(5) Uani 1 1 d U . . H23A H -0.0562 0.3977 0.5142 0.303 Uiso 1 1 calc R . . H23B H 0.0936 0.4260 0.5335 0.303 Uiso 1 1 calc R . . H23C H 0.0986 0.3725 0.5002 0.303 Uiso 1 1 calc R . . C24 C 0.3268(10) 0.4440(4) 0.4499(5) 0.226(6) Uani 1 1 d U . . H24A H 0.3289 0.4190 0.4795 0.339 Uiso 1 1 calc R . . H24B H 0.3712 0.4774 0.4617 0.339 Uiso 1 1 calc R . . H24C H 0.3823 0.4295 0.4208 0.339 Uiso 1 1 calc R . . C25 C 0.2388(13) 0.5179(3) 0.3579(4) 0.213(6) Uani 1 1 d U . . H25A H 0.1856 0.5389 0.3308 0.320 Uiso 1 1 calc R . . H25B H 0.3055 0.4935 0.3408 0.320 Uiso 1 1 calc R . . H25C H 0.2957 0.5414 0.3817 0.320 Uiso 1 1 calc R . . C16 C -0.1950(6) 0.4077(2) 0.2971(2) 0.0791(15) Uani 1 1 d U . . C17 C -0.1946(5) 0.3554(2) 0.31316(16) 0.0621(11) Uani 1 1 d U . . C18 C -0.0718(5) 0.33079(16) 0.29134(17) 0.0630(11) Uani 1 1 d U . . C19 C 0.0021(5) 0.3699(3) 0.26227(17) 0.0770(15) Uani 1 1 d U . . C20 C -0.0740(7) 0.4169(2) 0.2670(2) 0.0841(17) Uani 1 1 d U . . C26 C -0.3278(9) 0.4452(4) 0.3004(4) 0.183(5) Uani 1 1 d U . . H26A H -0.3994 0.4302 0.3242 0.274 Uiso 1 1 calc R . . H26B H -0.3740 0.4499 0.2650 0.274 Uiso 1 1 calc R . . H26C H -0.2944 0.4795 0.3141 0.274 Uiso 1 1 calc R . . C27 C -0.3151(7) 0.3289(3) 0.3438(2) 0.125(3) Uani 1 1 d U . . H27A H -0.2891 0.2919 0.3502 0.187 Uiso 1 1 calc R . . H27B H -0.4083 0.3308 0.3231 0.187 Uiso 1 1 calc R . . H27C H -0.3254 0.3469 0.3778 0.187 Uiso 1 1 calc R . . C28 C -0.0397(10) 0.2727(2) 0.2938(3) 0.131(3) Uani 1 1 d U . . H28A H 0.0514 0.2653 0.2757 0.197 Uiso 1 1 calc R . . H28B H -0.1210 0.2532 0.2763 0.197 Uiso 1 1 calc R . . H28C H -0.0287 0.2616 0.3309 0.197 Uiso 1 1 calc R . . C29 C 0.1254(8) 0.3577(5) 0.2244(3) 0.170(4) Uani 1 1 d U . . H29A H 0.1586 0.3213 0.2297 0.255 Uiso 1 1 calc R . . H29B H 0.2078 0.3818 0.2315 0.255 Uiso 1 1 calc R . . H29C H 0.0884 0.3623 0.1877 0.255 Uiso 1 1 calc R . . C30 C -0.0383(13) 0.4656(3) 0.2342(3) 0.184(5) Uani 1 1 d U . . H30A H -0.1041 0.4945 0.2433 0.275 Uiso 1 1 calc R . . H30B H -0.0519 0.4574 0.1964 0.275 Uiso 1 1 calc R . . H30C H 0.0639 0.4762 0.2419 0.275 Uiso 1 1 calc R . . C31 C 0.2371(4) 0.27664(13) 0.51352(13) 0.0400(7) Uani 1 1 d . . . C32 C 0.1699(4) 0.28671(15) 0.56315(14) 0.0502(9) Uani 1 1 d . . . C33 C 0.2507(5) 0.31510(17) 0.60221(15) 0.0617(11) Uani 1 1 d . . . H33 H 0.2067 0.3217 0.6351 0.074 Uiso 1 1 calc R . . C34 C 0.3917(5) 0.33393(17) 0.59510(17) 0.0649(11) Uani 1 1 d . . . C35 C 0.4536(5) 0.32423(16) 0.54610(17) 0.0581(10) Uani 1 1 d . . . H35 H 0.5496 0.3371 0.5404 0.070 Uiso 1 1 calc R . . C36 C 0.3799(4) 0.29628(14) 0.50489(14) 0.0452(8) Uani 1 1 d . . . C37 C 0.0173(5) 0.26871(19) 0.57741(16) 0.0646(11) Uani 1 1 d . . . H37A H 0.0233 0.2334 0.5930 0.097 Uiso 1 1 calc R . . H37B H -0.0470 0.2679 0.5454 0.097 Uiso 1 1 calc R . . H37C H -0.0228 0.2932 0.6031 0.097 Uiso 1 1 calc R . . C38 C 0.4768(7) 0.3639(2) 0.6390(2) 0.0916(17) Uani 1 1 d . . . H38A H 0.4504 0.4013 0.6373 0.137 Uiso 1 1 calc R . . H38B H 0.5826 0.3600 0.6343 0.137 Uiso 1 1 calc R . . H38C H 0.4521 0.3496 0.6736 0.137 Uiso 1 1 calc R . . C39 C 0.4609(4) 0.29205(18) 0.45342(17) 0.0599(10) Uani 1 1 d . . . H39A H 0.4711 0.2549 0.4438 0.090 Uiso 1 1 calc R . . H39B H 0.5586 0.3080 0.4582 0.090 Uiso 1 1 calc R . . H39C H 0.4051 0.3106 0.4252 0.090 Uiso 1 1 calc R . . C41 C 0.0447(4) 0.18048(13) 0.48963(13) 0.0407(7) Uani 1 1 d . . . C42 C 0.1263(4) 0.14968(14) 0.52834(14) 0.0478(8) Uani 1 1 d . . . C43 C 0.0616(5) 0.10347(15) 0.54720(17) 0.0604(11) Uani 1 1 d . . . H43 H 0.1147 0.0834 0.5732 0.072 Uiso 1 1 calc R . . C44 C -0.0769(6) 0.08559(17) 0.52965(18) 0.0664(11) Uani 1 1 d . . . C45 C -0.1503(5) 0.11428(15) 0.49001(17) 0.0588(10) Uani 1 1 d . . . H45 H -0.2429 0.1019 0.4766 0.071 Uiso 1 1 calc R . . C46 C -0.0930(4) 0.16117(14) 0.46885(14) 0.0460(8) Uani 1 1 d . . . C47 C 0.2827(5) 0.16158(17) 0.54897(16) 0.0600(10) Uani 1 1 d . . . H47A H 0.2794 0.1854 0.5794 0.090 Uiso 1 1 calc R . . H47B H 0.3376 0.1782 0.5209 0.090 Uiso 1 1 calc R . . H47C H 0.3314 0.1287 0.5599 0.090 Uiso 1 1 calc R . . C48 C -0.1442(7) 0.0358(2) 0.5525(2) 0.0981(18) Uani 1 1 d . . . H48A H -0.1723 0.0425 0.5890 0.147 Uiso 1 1 calc R . . H48B H -0.0720 0.0072 0.5524 0.147 Uiso 1 1 calc R . . H48C H -0.2314 0.0257 0.5309 0.147 Uiso 1 1 calc R . . C49 C -0.1828(5) 0.18601(17) 0.42301(17) 0.0596(10) Uani 1 1 d . . . H49A H -0.2478 0.2131 0.4368 0.089 Uiso 1 1 calc R . . H49B H -0.2419 0.1588 0.4047 0.089 Uiso 1 1 calc R . . H49C H -0.1162 0.2021 0.3981 0.089 Uiso 1 1 calc R . . C51 C 0.4385(4) 0.08706(13) 0.35352(13) 0.0419(7) Uani 1 1 d . . . F52 F 0.4620(3) 0.08240(10) 0.44893(8) 0.0689(7) Uani 1 1 d . . . C52 C 0.4863(4) 0.06117(14) 0.40026(14) 0.0478(8) Uani 1 1 d . . . C53 C 0.5611(4) 0.01346(15) 0.40183(15) 0.0527(9) Uani 1 1 d . . . F53 F 0.6047(3) -0.00919(11) 0.44872(10) 0.0791(8) Uani 1 1 d . . . F54 F 0.6751(3) -0.05646(9) 0.35544(11) 0.0740(7) Uani 1 1 d . . . C54 C 0.5947(4) -0.01096(14) 0.35498(16) 0.0519(9) Uani 1 1 d . . . F55 F 0.5915(3) -0.00989(10) 0.26092(9) 0.0713(7) Uani 1 1 d . . . C55 C 0.5521(4) 0.01256(15) 0.30725(15) 0.0507(9) Uani 1 1 d . . . F56 F 0.4321(3) 0.07910(9) 0.25882(8) 0.0587(6) Uani 1 1 d . . . C56 C 0.4744(4) 0.05931(14) 0.30803(14) 0.0443(8) Uani 1 1 d . . . C61 C 0.1905(4) 0.13256(13) 0.31610(13) 0.0413(7) Uani 1 1 d . . . F62 F 0.2223(3) 0.18715(10) 0.23984(8) 0.0619(6) Uani 1 1 d . . . C62 C 0.1369(4) 0.15428(14) 0.26767(13) 0.0439(8) Uani 1 1 d . . . F63 F -0.0464(3) 0.16752(12) 0.19880(9) 0.0769(7) Uani 1 1 d . . . C63 C -0.0024(5) 0.14504(16) 0.24594(14) 0.0532(9) Uani 1 1 d . . . F64 F -0.2371(3) 0.10357(12) 0.25007(12) 0.0842(8) Uani 1 1 d . . . C64 C -0.0999(4) 0.11224(17) 0.27150(17) 0.0580(10) Uani 1 1 d . . . F65 F -0.1437(3) 0.05605(12) 0.34412(12) 0.0882(9) Uani 1 1 d . . . C65 C -0.0520(5) 0.08885(16) 0.31824(17) 0.0576(10) Uani 1 1 d . . . F66 F 0.1253(3) 0.07328(10) 0.38514(10) 0.0680(6) Uani 1 1 d . . . C66 C 0.0888(4) 0.09904(14) 0.33880(15) 0.0475(8) Uani 1 1 d . . . C71 C 0.3232(11) -0.2259(4) 0.3564(5) 0.175(4) Uani 1 1 d . . . H71A H 0.2389 -0.2448 0.3393 0.210 Uiso 1 1 calc R . . H71B H 0.3615 -0.2472 0.3868 0.210 Uiso 1 1 calc R . . C72 C 0.4460(11) -0.2174(3) 0.3159(4) 0.141(3) Uani 1 1 d . . . H72A H 0.5396 -0.2335 0.3289 0.170 Uiso 1 1 calc R . . H72B H 0.4172 -0.2332 0.2811 0.170 Uiso 1 1 calc R . . C73 C 0.4606(10) -0.1613(4) 0.3114(3) 0.137(3) Uani 1 1 d . . . H73A H 0.4388 -0.1501 0.2743 0.165 Uiso 1 1 calc R . . H73B H 0.5624 -0.1506 0.3215 0.165 Uiso 1 1 calc R . . C74 C 0.3511(10) -0.1351(3) 0.3488(5) 0.154(4) Uani 1 1 d . . . H74A H 0.4044 -0.1126 0.3752 0.184 Uiso 1 1 calc R . . H74B H 0.2801 -0.1129 0.3282 0.184 Uiso 1 1 calc R . . C75 C 0.2777(13) -0.1756(4) 0.3742(6) 0.219(7) Uani 1 1 d . . . H75A H 0.1704 -0.1717 0.3672 0.263 Uiso 1 1 calc R . . H75B H 0.2974 -0.1729 0.4130 0.263 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0439(2) 0.03173(19) 0.0468(2) 0.00572(13) 0.00417(15) 0.00074(13) P1 0.0418(4) 0.0302(4) 0.0338(4) 0.0014(3) -0.0009(3) 0.0003(3) B1 0.046(2) 0.0364(19) 0.0390(19) 0.0002(15) -0.0004(16) 0.0029(16) O1 0.0548(14) 0.0328(12) 0.0455(13) 0.0058(10) 0.0002(11) 0.0020(10) O2 0.0505(16) 0.0539(16) 0.087(2) 0.0142(14) 0.0205(15) 0.0112(12) C1 0.0518(19) 0.0377(17) 0.0336(16) 0.0010(13) -0.0010(14) 0.0063(15) C2 0.0489(19) 0.0361(17) 0.0375(17) -0.0004(13) -0.0039(14) 0.0080(14) C5 0.048(2) 0.0317(16) 0.0418(18) 0.0002(14) -0.0012(15) 0.0018(14) C3 0.0332(17) 0.057(2) 0.0445(19) 0.0044(16) 0.0046(14) -0.0077(15) C4 0.055(2) 0.0436(19) 0.054(2) 0.0042(16) 0.0054(17) -0.0051(16) C11 0.128(5) 0.032(2) 0.086(3) -0.007(2) -0.024(3) 0.016(3) C12 0.078(3) 0.073(3) 0.141(5) -0.066(4) 0.048(4) -0.020(3) C13 0.174(6) 0.031(2) 0.055(3) -0.0048(18) 0.002(3) 0.004(3) C14 0.097(4) 0.075(4) 0.110(5) -0.041(4) -0.030(4) 0.015(3) C15 0.108(4) 0.052(3) 0.101(4) -0.023(3) 0.030(3) -0.032(3) C21 0.336(12) 0.061(4) 0.190(8) -0.031(4) -0.138(8) 0.079(6) C22 0.129(6) 0.239(10) 0.313(12) -0.204(9) 0.122(7) -0.071(6) C23 0.490(16) 0.060(4) 0.057(3) -0.009(3) 0.030(6) -0.017(6) C24 0.157(7) 0.237(10) 0.274(11) -0.186(9) -0.124(8) 0.083(7) C25 0.288(11) 0.115(6) 0.247(10) -0.064(6) 0.146(9) -0.126(7) C16 0.073(3) 0.070(3) 0.092(4) -0.013(3) -0.028(3) 0.027(3) C17 0.051(2) 0.084(3) 0.051(2) 0.003(2) -0.0001(18) -0.019(2) C18 0.084(3) 0.046(2) 0.056(2) -0.0038(18) -0.028(2) 0.012(2) C19 0.052(2) 0.134(5) 0.045(2) -0.007(3) 0.0075(19) -0.014(3) C20 0.119(4) 0.064(3) 0.067(3) 0.028(2) -0.031(3) -0.029(3) C26 0.121(6) 0.171(8) 0.249(10) -0.096(7) -0.098(6) 0.089(6) C27 0.100(4) 0.193(7) 0.081(4) 0.011(4) 0.003(3) -0.080(5) C28 0.208(7) 0.061(3) 0.118(5) -0.025(3) -0.091(5) 0.043(4) C29 0.098(5) 0.332(12) 0.083(4) -0.062(6) 0.032(4) -0.035(7) C30 0.319(12) 0.120(6) 0.105(5) 0.064(4) -0.081(6) -0.110(7) C31 0.0471(19) 0.0339(16) 0.0388(17) -0.0012(13) -0.0019(14) -0.0032(14) C32 0.061(2) 0.049(2) 0.0416(19) -0.0040(16) 0.0030(17) -0.0070(17) C33 0.083(3) 0.062(3) 0.041(2) -0.0096(18) 0.001(2) -0.011(2) C34 0.083(3) 0.057(2) 0.054(2) -0.0056(19) -0.014(2) -0.014(2) C35 0.054(2) 0.055(2) 0.064(2) 0.0011(19) -0.0096(19) -0.0138(18) C36 0.0455(19) 0.0408(18) 0.049(2) 0.0011(15) -0.0027(16) -0.0030(15) C37 0.072(3) 0.075(3) 0.048(2) -0.012(2) 0.019(2) -0.011(2) C38 0.113(4) 0.094(4) 0.067(3) -0.022(3) -0.019(3) -0.034(3) C39 0.050(2) 0.066(3) 0.065(3) -0.006(2) 0.0085(19) -0.0129(19) C41 0.0505(19) 0.0330(16) 0.0385(17) 0.0037(13) -0.0005(15) -0.0013(14) C42 0.063(2) 0.0386(18) 0.0417(18) 0.0047(15) -0.0031(16) 0.0003(16) C43 0.082(3) 0.043(2) 0.056(2) 0.0190(17) -0.004(2) 0.0008(19) C44 0.087(3) 0.046(2) 0.066(3) 0.013(2) 0.005(2) -0.014(2) C45 0.066(3) 0.046(2) 0.064(2) 0.0032(18) -0.003(2) -0.0141(18) C46 0.050(2) 0.0401(18) 0.0473(19) 0.0018(15) -0.0026(16) -0.0031(15) C47 0.066(3) 0.055(2) 0.058(2) 0.0147(19) -0.018(2) 0.0030(19) C48 0.126(5) 0.060(3) 0.108(4) 0.033(3) -0.003(4) -0.030(3) C49 0.056(2) 0.055(2) 0.066(2) 0.0097(19) -0.017(2) -0.0089(18) C51 0.0442(18) 0.0397(18) 0.0419(18) 0.0023(14) 0.0024(15) 0.0019(14) F52 0.0991(19) 0.0706(15) 0.0371(11) 0.0044(10) 0.0023(11) 0.0382(14) C52 0.056(2) 0.046(2) 0.0414(19) 0.0023(15) 0.0029(16) 0.0103(16) C53 0.059(2) 0.049(2) 0.051(2) 0.0123(17) 0.0011(18) 0.0081(17) F53 0.105(2) 0.0708(16) 0.0614(14) 0.0220(12) 0.0015(14) 0.0382(15) F54 0.0857(17) 0.0518(14) 0.0846(17) -0.0003(12) 0.0036(14) 0.0309(12) C54 0.053(2) 0.0370(19) 0.065(2) 0.0008(17) 0.0003(18) 0.0075(16) F55 0.0810(16) 0.0712(16) 0.0615(14) -0.0240(12) 0.0018(12) 0.0238(13) C55 0.051(2) 0.048(2) 0.053(2) -0.0110(17) 0.0013(17) 0.0054(16) F56 0.0735(15) 0.0640(14) 0.0382(11) -0.0033(10) -0.0044(10) 0.0193(11) C56 0.0454(19) 0.0462(19) 0.0409(18) -0.0005(15) -0.0025(15) 0.0031(15) C61 0.0509(19) 0.0325(17) 0.0406(17) -0.0024(13) 0.0020(15) 0.0035(14) F62 0.0649(14) 0.0728(15) 0.0479(12) 0.0165(11) 0.0000(10) -0.0045(12) C62 0.054(2) 0.0419(18) 0.0359(17) -0.0007(14) 0.0042(15) 0.0035(16) F63 0.0826(17) 0.0942(19) 0.0521(13) 0.0051(13) -0.0218(12) 0.0088(15) C63 0.064(2) 0.053(2) 0.0418(19) -0.0083(17) -0.0075(18) 0.0125(19) F64 0.0554(15) 0.106(2) 0.0893(19) -0.0260(16) -0.0156(13) -0.0100(14) C64 0.049(2) 0.062(2) 0.062(2) -0.020(2) -0.0042(19) -0.0009(18) F65 0.0744(17) 0.090(2) 0.101(2) 0.0053(16) 0.0080(15) -0.0386(15) C65 0.059(2) 0.051(2) 0.063(2) -0.0066(19) 0.007(2) -0.0128(19) F66 0.0762(16) 0.0601(14) 0.0672(15) 0.0242(12) -0.0038(12) -0.0167(12) C66 0.056(2) 0.0376(18) 0.049(2) 0.0026(15) 0.0015(17) -0.0051(15) C71 0.160(8) 0.116(7) 0.256(12) 0.037(8) 0.086(9) 0.010(6) C72 0.160(8) 0.113(6) 0.152(7) -0.017(5) 0.015(6) 0.013(6) C73 0.144(7) 0.149(8) 0.118(6) 0.034(5) -0.005(5) -0.034(6) C74 0.112(6) 0.100(6) 0.250(12) 0.009(7) 0.017(7) 0.000(5) C75 0.194(10) 0.143(9) 0.333(16) -0.068(10) 0.174(11) -0.049(8) _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 Zr1 O1 2.127(2) . ? Zr1 C3 2.333(3) . ? Zr1 C17 2.507(4) . ? Zr1 C12 2.507(4) . ? Zr1 C16 2.529(5) . ? Zr1 C18 2.530(4) . ? Zr1 C13 2.537(5) . ? Zr1 C20 2.541(4) . ? Zr1 C15 2.543(4) . ? Zr1 C11 2.544(4) . ? Zr1 C14 2.552(5) . ? Zr1 C19 2.555(4) . ? P1 C41 1.810(3) . ? P1 C1 1.818(3) . ? P1 C31 1.826(3) . ? P1 C5 1.911(3) . ? B1 C4 1.635(5) . ? B1 C2 1.648(5) . ? B1 C61 1.657(5) . ? B1 C51 1.668(5) . ? O1 C5 1.281(4) . ? O2 C5 1.201(4) . ? C1 C2 1.538(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C11 C15 1.349(8) . ? C11 C12 1.455(8) . ? C11 C21 1.511(8) . ? C12 C13 1.393(9) . ? C12 C22 1.506(8) . ? C13 C14 1.330(9) . ? C13 C23 1.502(8) . ? C14 C15 1.340(9) . ? C14 C24 1.531(9) . ? C15 C25 1.524(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C16 C20 1.368(8) . ? C16 C17 1.375(7) . ? C16 C26 1.529(8) . ? C17 C18 1.397(6) . ? C17 C27 1.508(6) . ? C18 C19 1.405(7) . ? C18 C28 1.490(6) . ? C19 C20 1.375(8) . ? C19 C29 1.518(8) . ? C20 C30 1.514(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C36 1.403(5) . ? C31 C32 1.424(5) . ? C32 C33 1.392(5) . ? C32 C37 1.503(6) . ? C33 C34 1.374(6) . ? C33 H33 0.9400 . ? C34 C35 1.387(6) . ? C34 C38 1.515(6) . ? C35 C36 1.393(5) . ? C35 H35 0.9400 . ? C36 C39 1.507(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C41 C46 1.412(5) . ? C41 C42 1.421(5) . ? C42 C43 1.390(5) . ? C42 C47 1.512(5) . ? C43 C44 1.382(6) . ? C43 H43 0.9400 . ? C44 C45 1.374(6) . ? C44 C48 1.512(6) . ? C45 C46 1.399(5) . ? C45 H45 0.9400 . ? C46 C49 1.511(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C51 C56 1.383(5) . ? C51 C52 1.391(5) . ? F52 C52 1.354(4) . ? C52 C53 1.376(5) . ? C53 F53 1.347(4) . ? C53 C54 1.366(5) . ? F54 C54 1.353(4) . ? C54 C55 1.372(5) . ? F55 C55 1.348(4) . ? C55 C56 1.368(5) . ? F56 C56 1.367(4) . ? C61 C66 1.383(5) . ? C61 C62 1.397(5) . ? F62 C62 1.342(4) . ? C62 C63 1.367(5) . ? F63 C63 1.352(4) . ? C63 C64 1.379(6) . ? F64 C64 1.346(5) . ? C64 C65 1.363(6) . ? F65 C65 1.350(5) . ? C65 C66 1.374(6) . ? F66 C66 1.356(4) . ? C71 C75 1.406(12) . ? C71 C72 1.544(11) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C72 C73 1.422(11) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C73 C74 1.535(11) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C74 C75 1.382(12) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 C3 90.07(11) . . ? O1 Zr1 C17 87.06(13) . . ? C3 Zr1 C17 123.69(14) . . ? O1 Zr1 C12 100.00(19) . . ? C3 Zr1 C12 131.31(15) . . ? C17 Zr1 C12 104.44(17) . . ? O1 Zr1 C16 118.02(16) . . ? C3 Zr1 C16 125.10(17) . . ? C17 Zr1 C16 31.68(16) . . ? C12 Zr1 C16 91.6(2) . . ? O1 Zr1 C18 81.32(11) . . ? C3 Zr1 C18 91.86(15) . . ? C17 Zr1 C18 32.20(15) . . ? C12 Zr1 C18 136.61(17) . . ? C16 Zr1 C18 52.48(14) . . ? O1 Zr1 C13 80.34(12) . . ? C3 Zr1 C13 106.4(2) . . ? C17 Zr1 C13 128.2(2) . . ? C12 Zr1 C13 32.1(2) . . ? C16 Zr1 C13 123.2(2) . . ? C18 Zr1 C13 154.0(2) . . ? O1 Zr1 C20 133.78(13) . . ? C3 Zr1 C20 94.88(19) . . ? C17 Zr1 C20 52.59(15) . . ? C12 Zr1 C20 110.3(3) . . ? C16 Zr1 C20 31.31(19) . . ? C18 Zr1 C20 52.65(15) . . ? C13 Zr1 C20 140.25(19) . . ? O1 Zr1 C15 125.14(18) . . ? C3 Zr1 C15 82.71(17) . . ? C17 Zr1 C15 140.4(2) . . ? C12 Zr1 C15 52.64(17) . . ? C16 Zr1 C15 110.1(2) . . ? C18 Zr1 C15 152.77(18) . . ? C13 Zr1 C15 50.89(17) . . ? C20 Zr1 C15 101.1(2) . . ? O1 Zr1 C11 131.67(14) . . ? C3 Zr1 C11 111.75(19) . . ? C17 Zr1 C11 111.50(18) . . ? C12 Zr1 C11 33.5(2) . . ? C16 Zr1 C11 84.71(17) . . ? C18 Zr1 C11 136.78(15) . . ? C13 Zr1 C11 52.73(16) . . ? C20 Zr1 C11 88.44(18) . . ? C15 Zr1 C11 30.75(18) . . ? O1 Zr1 C14 94.67(19) . . ? C3 Zr1 C14 79.90(18) . . ? C17 Zr1 C14 156.39(19) . . ? C12 Zr1 C14 52.04(19) . . ? C16 Zr1 C14 136.00(17) . . ? C18 Zr1 C14 170.87(17) . . ? C13 Zr1 C14 30.3(2) . . ? C20 Zr1 C14 131.5(2) . . ? C15 Zr1 C14 30.5(2) . . ? C11 Zr1 C14 51.32(18) . . ? O1 Zr1 C19 108.58(16) . . ? C3 Zr1 C19 75.52(14) . . ? C17 Zr1 C19 52.80(14) . . ? C12 Zr1 C19 141.0(2) . . ? C16 Zr1 C19 51.83(17) . . ? C18 Zr1 C19 32.08(16) . . ? C13 Zr1 C19 170.98(18) . . ? C20 Zr1 C19 31.30(18) . . ? C15 Zr1 C19 121.6(2) . . ? C11 Zr1 C19 118.27(19) . . ? C14 Zr1 C19 145.8(2) . . ? C41 P1 C1 104.58(16) . . ? C41 P1 C31 112.29(15) . . ? C1 P1 C31 119.29(16) . . ? C41 P1 C5 114.72(16) . . ? C1 P1 C5 106.52(15) . . ? C31 P1 C5 99.71(15) . . ? C4 B1 C2 109.4(3) . . ? C4 B1 C61 115.3(3) . . ? C2 B1 C61 106.4(3) . . ? C4 B1 C51 108.5(3) . . ? C2 B1 C51 111.6(3) . . ? C61 B1 C51 105.5(3) . . ? C5 O1 Zr1 150.2(2) . . ? C2 C1 P1 115.6(2) . . ? C2 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? C1 C2 B1 111.6(3) . . ? C1 C2 H2A 109.3 . . ? B1 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? B1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O2 C5 O1 128.2(3) . . ? O2 C5 P1 121.5(3) . . ? O1 C5 P1 110.2(2) . . ? Zr1 C3 H3A 109.5 . . ? Zr1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Zr1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? B1 C4 H4A 109.5 . . ? B1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? B1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C15 C11 C12 106.0(5) . . ? C15 C11 C21 125.8(7) . . ? C12 C11 C21 126.4(8) . . ? C15 C11 Zr1 74.6(3) . . ? C12 C11 Zr1 71.9(2) . . ? C21 C11 Zr1 130.6(4) . . ? C13 C12 C11 104.8(5) . . ? C13 C12 C22 127.3(9) . . ? C11 C12 C22 127.2(8) . . ? C13 C12 Zr1 75.1(3) . . ? C11 C12 Zr1 74.6(3) . . ? C22 C12 Zr1 122.7(4) . . ? C14 C13 C12 109.2(5) . . ? C14 C13 C23 124.0(9) . . ? C12 C13 C23 126.3(8) . . ? C14 C13 Zr1 75.5(3) . . ? C12 C13 Zr1 72.8(3) . . ? C23 C13 Zr1 124.3(3) . . ? C13 C14 C15 109.7(5) . . ? C13 C14 C24 126.9(9) . . ? C15 C14 C24 123.0(9) . . ? C13 C14 Zr1 74.2(3) . . ? C15 C14 Zr1 74.4(3) . . ? C24 C14 Zr1 123.8(4) . . ? C14 C15 C11 110.3(5) . . ? C14 C15 C25 124.5(8) . . ? C11 C15 C25 124.8(8) . . ? C14 C15 Zr1 75.1(3) . . ? C11 C15 Zr1 74.7(3) . . ? C25 C15 Zr1 123.1(4) . . ? C11 C21 H21A 109.5 . . ? C11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C12 C22 H22A 109.5 . . ? C12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C13 C23 H23A 109.5 . . ? C13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C14 C24 H24A 109.5 . . ? C14 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C14 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C15 C25 H25A 109.5 . . ? C15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C15 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C16 C17 109.2(4) . . ? C20 C16 C26 124.6(7) . . ? C17 C16 C26 124.6(7) . . ? C20 C16 Zr1 74.8(3) . . ? C17 C16 Zr1 73.3(3) . . ? C26 C16 Zr1 129.7(4) . . ? C16 C17 C18 107.6(4) . . ? C16 C17 C27 125.3(6) . . ? C18 C17 C27 126.8(5) . . ? C16 C17 Zr1 75.1(3) . . ? C18 C17 Zr1 74.8(2) . . ? C27 C17 Zr1 121.0(3) . . ? C17 C18 C19 106.9(4) . . ? C17 C18 C28 125.0(6) . . ? C19 C18 C28 127.7(6) . . ? C17 C18 Zr1 73.0(2) . . ? C19 C18 Zr1 75.0(3) . . ? C28 C18 Zr1 123.0(3) . . ? C20 C19 C18 108.0(4) . . ? C20 C19 C29 127.3(7) . . ? C18 C19 C29 123.7(7) . . ? C20 C19 Zr1 73.8(3) . . ? C18 C19 Zr1 73.0(2) . . ? C29 C19 Zr1 127.9(4) . . ? C16 C20 C19 108.2(4) . . ? C16 C20 C30 128.7(7) . . ? C19 C20 C30 122.1(7) . . ? C16 C20 Zr1 73.9(3) . . ? C19 C20 Zr1 74.9(3) . . ? C30 C20 Zr1 126.2(4) . . ? C16 C26 H26A 109.5 . . ? C16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C17 C27 H27A 109.5 . . ? C17 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C17 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C29 H29A 109.5 . . ? C19 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C19 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C20 C30 H30A 109.5 . . ? C20 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C20 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 119.7(3) . . ? C36 C31 P1 123.6(3) . . ? C32 C31 P1 116.7(3) . . ? C33 C32 C31 118.3(4) . . ? C33 C32 C37 116.5(3) . . ? C31 C32 C37 125.2(3) . . ? C34 C33 C32 123.2(4) . . ? C34 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? C33 C34 C35 117.3(4) . . ? C33 C34 C38 121.5(4) . . ? C35 C34 C38 121.2(4) . . ? C34 C35 C36 123.0(4) . . ? C34 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C31 118.5(3) . . ? C35 C36 C39 115.7(3) . . ? C31 C36 C39 125.7(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C46 C41 C42 119.1(3) . . ? C46 C41 P1 120.7(3) . . ? C42 C41 P1 119.9(3) . . ? C43 C42 C41 118.2(4) . . ? C43 C42 C47 116.6(3) . . ? C41 C42 C47 125.1(3) . . ? C44 C43 C42 123.3(4) . . ? C44 C43 H43 118.3 . . ? C42 C43 H43 118.3 . . ? C45 C44 C43 117.5(4) . . ? C45 C44 C48 121.2(5) . . ? C43 C44 C48 121.3(4) . . ? C44 C45 C46 122.7(4) . . ? C44 C45 H45 118.7 . . ? C46 C45 H45 118.7 . . ? C45 C46 C41 118.9(3) . . ? C45 C46 C49 116.1(3) . . ? C41 C46 C49 125.0(3) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C56 C51 C52 112.3(3) . . ? C56 C51 B1 120.1(3) . . ? C52 C51 B1 127.6(3) . . ? F52 C52 C53 114.5(3) . . ? F52 C52 C51 121.0(3) . . ? C53 C52 C51 124.6(3) . . ? F53 C53 C54 119.3(3) . . ? F53 C53 C52 121.3(3) . . ? C54 C53 C52 119.5(3) . . ? F54 C54 C53 120.6(3) . . ? F54 C54 C55 120.2(3) . . ? C53 C54 C55 119.2(3) . . ? F55 C55 C56 121.6(3) . . ? F55 C55 C54 119.5(3) . . ? C56 C55 C54 118.9(3) . . ? F56 C56 C55 115.1(3) . . ? F56 C56 C51 119.4(3) . . ? C55 C56 C51 125.5(3) . . ? C66 C61 C62 112.4(3) . . ? C66 C61 B1 120.1(3) . . ? C62 C61 B1 127.4(3) . . ? F62 C62 C63 115.8(3) . . ? F62 C62 C61 120.2(3) . . ? C63 C62 C61 124.0(3) . . ? F63 C63 C62 120.6(4) . . ? F63 C63 C64 118.9(4) . . ? C62 C63 C64 120.6(4) . . ? F64 C64 C65 121.8(4) . . ? F64 C64 C63 120.3(4) . . ? C65 C64 C63 117.9(4) . . ? F65 C65 C64 119.7(4) . . ? F65 C65 C66 120.5(4) . . ? C64 C65 C66 119.8(4) . . ? F66 C66 C65 114.8(3) . . ? F66 C66 C61 119.9(3) . . ? C65 C66 C61 125.3(4) . . ? C75 C71 C72 108.0(8) . . ? C75 C71 H71A 110.1 . . ? C72 C71 H71A 110.1 . . ? C75 C71 H71B 110.1 . . ? C72 C71 H71B 110.1 . . ? H71A C71 H71B 108.4 . . ? C73 C72 C71 105.0(7) . . ? C73 C72 H72A 110.7 . . ? C71 C72 H72A 110.7 . . ? C73 C72 H72B 110.7 . . ? C71 C72 H72B 110.7 . . ? H72A C72 H72B 108.8 . . ? C72 C73 C74 108.3(7) . . ? C72 C73 H73A 110.0 . . ? C74 C73 H73A 110.0 . . ? C72 C73 H73B 110.0 . . ? C74 C73 H73B 110.0 . . ? H73A C73 H73B 108.4 . . ? C75 C74 C73 107.1(7) . . ? C75 C74 H74A 110.3 . . ? C73 C74 H74A 110.3 . . ? C75 C74 H74B 110.3 . . ? C73 C74 H74B 110.3 . . ? H74A C74 H74B 108.5 . . ? C74 C75 C71 111.5(8) . . ? C74 C75 H75A 109.3 . . ? C71 C75 H75A 109.3 . . ? C74 C75 H75B 109.3 . . ? C71 C75 H75B 109.3 . . ? H75A C75 H75B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Zr1 O1 C5 170.3(4) . . . . ? C17 Zr1 O1 C5 -65.9(5) . . . . ? C12 Zr1 O1 C5 38.2(5) . . . . ? C16 Zr1 O1 C5 -59.0(5) . . . . ? C18 Zr1 O1 C5 -97.8(5) . . . . ? C13 Zr1 O1 C5 63.7(5) . . . . ? C20 Zr1 O1 C5 -92.8(5) . . . . ? C15 Zr1 O1 C5 89.2(5) . . . . ? C11 Zr1 O1 C5 50.5(5) . . . . ? C14 Zr1 O1 C5 90.4(5) . . . . ? C19 Zr1 O1 C5 -115.0(4) . . . . ? C41 P1 C1 C2 -49.1(3) . . . . ? C31 P1 C1 C2 77.5(3) . . . . ? C5 P1 C1 C2 -170.9(3) . . . . ? P1 C1 C2 B1 167.1(2) . . . . ? C4 B1 C2 C1 68.0(4) . . . . ? C61 B1 C2 C1 -57.2(4) . . . . ? C51 B1 C2 C1 -171.9(3) . . . . ? Zr1 O1 C5 O2 4.0(7) . . . . ? Zr1 O1 C5 P1 -171.7(3) . . . . ? C41 P1 C5 O2 27.3(4) . . . . ? C1 P1 C5 O2 142.5(3) . . . . ? C31 P1 C5 O2 -92.9(3) . . . . ? C41 P1 C5 O1 -156.7(2) . . . . ? C1 P1 C5 O1 -41.5(3) . . . . ? C31 P1 C5 O1 83.2(3) . . . . ? O1 Zr1 C11 C15 90.6(4) . . . . ? C3 Zr1 C11 C15 -20.3(4) . . . . ? C17 Zr1 C11 C15 -163.3(3) . . . . ? C12 Zr1 C11 C15 113.0(5) . . . . ? C16 Zr1 C11 C15 -146.1(4) . . . . ? C18 Zr1 C11 C15 -138.7(3) . . . . ? C13 Zr1 C11 C15 74.3(4) . . . . ? C20 Zr1 C11 C15 -114.9(4) . . . . ? C14 Zr1 C11 C15 35.6(4) . . . . ? C19 Zr1 C11 C15 -105.0(4) . . . . ? O1 Zr1 C11 C12 -22.4(5) . . . . ? C3 Zr1 C11 C12 -133.3(4) . . . . ? C17 Zr1 C11 C12 83.7(4) . . . . ? C16 Zr1 C11 C12 101.0(4) . . . . ? C18 Zr1 C11 C12 108.3(4) . . . . ? C13 Zr1 C11 C12 -38.7(3) . . . . ? C20 Zr1 C11 C12 132.1(4) . . . . ? C15 Zr1 C11 C12 -113.0(5) . . . . ? C14 Zr1 C11 C12 -77.4(4) . . . . ? C19 Zr1 C11 C12 142.0(3) . . . . ? O1 Zr1 C11 C21 -145.1(8) . . . . ? C3 Zr1 C11 C21 103.9(8) . . . . ? C17 Zr1 C11 C21 -39.1(9) . . . . ? C12 Zr1 C11 C21 -122.8(10) . . . . ? C16 Zr1 C11 C21 -21.8(8) . . . . ? C18 Zr1 C11 C21 -14.5(10) . . . . ? C13 Zr1 C11 C21 -161.5(10) . . . . ? C20 Zr1 C11 C21 9.3(9) . . . . ? C15 Zr1 C11 C21 124.2(10) . . . . ? C14 Zr1 C11 C21 159.8(10) . . . . ? C19 Zr1 C11 C21 19.2(9) . . . . ? C15 C11 C12 C13 2.2(5) . . . . ? C21 C11 C12 C13 -162.7(5) . . . . ? Zr1 C11 C12 C13 69.7(3) . . . . ? C15 C11 C12 C22 173.0(5) . . . . ? C21 C11 C12 C22 8.0(9) . . . . ? Zr1 C11 C12 C22 -119.6(6) . . . . ? C15 C11 C12 Zr1 -67.4(3) . . . . ? C21 C11 C12 Zr1 127.6(5) . . . . ? O1 Zr1 C12 C13 53.0(4) . . . . ? C3 Zr1 C12 C13 -46.0(5) . . . . ? C17 Zr1 C12 C13 142.5(4) . . . . ? C16 Zr1 C12 C13 171.8(4) . . . . ? C18 Zr1 C12 C13 140.9(3) . . . . ? C20 Zr1 C12 C13 -162.5(4) . . . . ? C15 Zr1 C12 C13 -74.0(4) . . . . ? C11 Zr1 C12 C13 -110.3(5) . . . . ? C14 Zr1 C12 C13 -35.2(3) . . . . ? C19 Zr1 C12 C13 -169.9(3) . . . . ? O1 Zr1 C12 C11 163.2(3) . . . . ? C3 Zr1 C12 C11 64.2(5) . . . . ? C17 Zr1 C12 C11 -107.2(3) . . . . ? C16 Zr1 C12 C11 -77.9(4) . . . . ? C18 Zr1 C12 C11 -108.9(3) . . . . ? C13 Zr1 C12 C11 110.3(4) . . . . ? C20 Zr1 C12 C11 -52.3(4) . . . . ? C15 Zr1 C12 C11 36.3(3) . . . . ? C14 Zr1 C12 C11 75.1(4) . . . . ? C19 Zr1 C12 C11 -59.7(4) . . . . ? O1 Zr1 C12 C22 -72.1(9) . . . . ? C3 Zr1 C12 C22 -171.1(8) . . . . ? C17 Zr1 C12 C22 17.4(9) . . . . ? C16 Zr1 C12 C22 46.7(9) . . . . ? C18 Zr1 C12 C22 15.8(10) . . . . ? C13 Zr1 C12 C22 -125.1(10) . . . . ? C20 Zr1 C12 C22 72.4(9) . . . . ? C15 Zr1 C12 C22 161.0(10) . . . . ? C11 Zr1 C12 C22 124.6(10) . . . . ? C14 Zr1 C12 C22 -160.3(10) . . . . ? C19 Zr1 C12 C22 65.0(9) . . . . ? C11 C12 C13 C14 -2.0(5) . . . . ? C22 C12 C13 C14 -172.7(5) . . . . ? Zr1 C12 C13 C14 67.3(4) . . . . ? C11 C12 C13 C23 170.4(5) . . . . ? C22 C12 C13 C23 -0.3(8) . . . . ? Zr1 C12 C13 C23 -120.3(5) . . . . ? C11 C12 C13 Zr1 -69.3(3) . . . . ? C22 C12 C13 Zr1 120.0(5) . . . . ? O1 Zr1 C13 C14 117.1(4) . . . . ? C3 Zr1 C13 C14 29.9(4) . . . . ? C17 Zr1 C13 C14 -164.5(4) . . . . ? C12 Zr1 C13 C14 -115.8(5) . . . . ? C16 Zr1 C13 C14 -125.7(4) . . . . ? C18 Zr1 C13 C14 162.8(4) . . . . ? C20 Zr1 C13 C14 -89.7(6) . . . . ? C15 Zr1 C13 C14 -35.9(3) . . . . ? C11 Zr1 C13 C14 -75.3(4) . . . . ? C19 Zr1 C13 C14 -71.4(16) . . . . ? O1 Zr1 C13 C12 -127.1(4) . . . . ? C3 Zr1 C13 C12 145.7(4) . . . . ? C17 Zr1 C13 C12 -48.7(4) . . . . ? C16 Zr1 C13 C12 -9.8(5) . . . . ? C18 Zr1 C13 C12 -81.4(4) . . . . ? C20 Zr1 C13 C12 26.1(6) . . . . ? C15 Zr1 C13 C12 79.9(4) . . . . ? C11 Zr1 C13 C12 40.5(3) . . . . ? C14 Zr1 C13 C12 115.8(5) . . . . ? C19 Zr1 C13 C12 44.4(16) . . . . ? O1 Zr1 C13 C23 -4.5(8) . . . . ? C3 Zr1 C13 C23 -91.7(8) . . . . ? C17 Zr1 C13 C23 74.0(9) . . . . ? C12 Zr1 C13 C23 122.7(10) . . . . ? C16 Zr1 C13 C23 112.8(8) . . . . ? C18 Zr1 C13 C23 41.3(11) . . . . ? C20 Zr1 C13 C23 148.8(8) . . . . ? C15 Zr1 C13 C23 -157.4(10) . . . . ? C11 Zr1 C13 C23 163.2(10) . . . . ? C14 Zr1 C13 C23 -121.5(10) . . . . ? C19 Zr1 C13 C23 167.1(12) . . . . ? C12 C13 C14 C15 1.0(6) . . . . ? C23 C13 C14 C15 -171.6(5) . . . . ? Zr1 C13 C14 C15 66.6(4) . . . . ? C12 C13 C14 C24 173.6(5) . . . . ? C23 C13 C14 C24 1.1(9) . . . . ? Zr1 C13 C14 C24 -120.8(6) . . . . ? C12 C13 C14 Zr1 -65.6(3) . . . . ? C23 C13 C14 Zr1 121.8(5) . . . . ? O1 Zr1 C14 C13 -61.7(4) . . . . ? C3 Zr1 C14 C13 -151.0(4) . . . . ? C17 Zr1 C14 C13 31.6(8) . . . . ? C12 Zr1 C14 C13 37.3(3) . . . . ? C16 Zr1 C14 C13 78.0(5) . . . . ? C18 Zr1 C14 C13 -125.3(12) . . . . ? C20 Zr1 C14 C13 121.4(5) . . . . ? C15 Zr1 C14 C13 116.2(5) . . . . ? C11 Zr1 C14 C13 80.4(4) . . . . ? C19 Zr1 C14 C13 164.7(4) . . . . ? O1 Zr1 C14 C15 -178.0(4) . . . . ? C3 Zr1 C14 C15 92.8(4) . . . . ? C17 Zr1 C14 C15 -84.6(7) . . . . ? C12 Zr1 C14 C15 -78.9(4) . . . . ? C16 Zr1 C14 C15 -38.2(6) . . . . ? C18 Zr1 C14 C15 118.5(13) . . . . ? C13 Zr1 C14 C15 -116.2(5) . . . . ? C20 Zr1 C14 C15 5.2(5) . . . . ? C11 Zr1 C14 C15 -35.9(3) . . . . ? C19 Zr1 C14 C15 48.4(5) . . . . ? O1 Zr1 C14 C24 62.4(9) . . . . ? C3 Zr1 C14 C24 -26.8(8) . . . . ? C17 Zr1 C14 C24 155.8(7) . . . . ? C12 Zr1 C14 C24 161.5(10) . . . . ? C16 Zr1 C14 C24 -157.8(8) . . . . ? C18 Zr1 C14 C24 -1(2) . . . . ? C13 Zr1 C14 C24 124.2(10) . . . . ? C20 Zr1 C14 C24 -114.4(8) . . . . ? C15 Zr1 C14 C24 -119.6(11) . . . . ? C11 Zr1 C14 C24 -155.5(10) . . . . ? C19 Zr1 C14 C24 -71.2(10) . . . . ? C13 C14 C15 C11 0.5(6) . . . . ? C24 C14 C15 C11 -172.4(5) . . . . ? Zr1 C14 C15 C11 67.0(4) . . . . ? C13 C14 C15 C25 173.4(5) . . . . ? C24 C14 C15 C25 0.4(9) . . . . ? Zr1 C14 C15 C25 -120.2(6) . . . . ? C13 C14 C15 Zr1 -66.5(4) . . . . ? C24 C14 C15 Zr1 120.6(6) . . . . ? C12 C11 C15 C14 -1.8(6) . . . . ? C21 C11 C15 C14 163.3(6) . . . . ? Zr1 C11 C15 C14 -67.3(4) . . . . ? C12 C11 C15 C25 -174.5(5) . . . . ? C21 C11 C15 C25 -9.4(9) . . . . ? Zr1 C11 C15 C25 119.9(6) . . . . ? C12 C11 C15 Zr1 65.5(3) . . . . ? C21 C11 C15 Zr1 -129.4(6) . . . . ? O1 Zr1 C15 C14 2.5(5) . . . . ? C3 Zr1 C15 C14 -82.5(4) . . . . ? C17 Zr1 C15 C14 141.3(4) . . . . ? C12 Zr1 C15 C14 76.8(4) . . . . ? C16 Zr1 C15 C14 152.8(4) . . . . ? C18 Zr1 C15 C14 -162.3(4) . . . . ? C13 Zr1 C15 C14 35.7(4) . . . . ? C20 Zr1 C15 C14 -176.0(4) . . . . ? C11 Zr1 C15 C14 116.5(5) . . . . ? C19 Zr1 C15 C14 -150.5(4) . . . . ? O1 Zr1 C15 C11 -114.0(4) . . . . ? C3 Zr1 C15 C11 161.1(4) . . . . ? C17 Zr1 C15 C11 24.8(5) . . . . ? C12 Zr1 C15 C11 -39.7(4) . . . . ? C16 Zr1 C15 C11 36.3(4) . . . . ? C18 Zr1 C15 C11 81.3(5) . . . . ? C13 Zr1 C15 C11 -80.8(4) . . . . ? C20 Zr1 C15 C11 67.5(4) . . . . ? C14 Zr1 C15 C11 -116.5(5) . . . . ? C19 Zr1 C15 C11 93.1(4) . . . . ? O1 Zr1 C15 C25 124.2(8) . . . . ? C3 Zr1 C15 C25 39.3(8) . . . . ? C17 Zr1 C15 C25 -97.0(8) . . . . ? C12 Zr1 C15 C25 -161.5(9) . . . . ? C16 Zr1 C15 C25 -85.5(8) . . . . ? C18 Zr1 C15 C25 -40.5(10) . . . . ? C13 Zr1 C15 C25 157.4(9) . . . . ? C20 Zr1 C15 C25 -54.3(8) . . . . ? C11 Zr1 C15 C25 -121.8(10) . . . . ? C14 Zr1 C15 C25 121.7(10) . . . . ? C19 Zr1 C15 C25 -28.7(9) . . . . ? O1 Zr1 C16 C20 -129.3(3) . . . . ? C3 Zr1 C16 C20 -17.2(4) . . . . ? C17 Zr1 C16 C20 -116.0(4) . . . . ? C12 Zr1 C16 C20 128.5(3) . . . . ? C18 Zr1 C16 C20 -77.9(3) . . . . ? C13 Zr1 C16 C20 133.7(3) . . . . ? C15 Zr1 C16 C20 78.0(3) . . . . ? C11 Zr1 C16 C20 95.7(4) . . . . ? C14 Zr1 C16 C20 97.6(4) . . . . ? C19 Zr1 C16 C20 -37.0(3) . . . . ? O1 Zr1 C16 C17 -13.3(4) . . . . ? C3 Zr1 C16 C17 98.8(3) . . . . ? C12 Zr1 C16 C17 -115.5(3) . . . . ? C18 Zr1 C16 C17 38.1(3) . . . . ? C13 Zr1 C16 C17 -110.3(3) . . . . ? C20 Zr1 C16 C17 116.0(4) . . . . ? C15 Zr1 C16 C17 -166.0(3) . . . . ? C11 Zr1 C16 C17 -148.3(3) . . . . ? C14 Zr1 C16 C17 -146.5(4) . . . . ? C19 Zr1 C16 C17 79.0(3) . . . . ? O1 Zr1 C16 C26 108.1(7) . . . . ? C3 Zr1 C16 C26 -139.9(7) . . . . ? C17 Zr1 C16 C26 121.4(9) . . . . ? C12 Zr1 C16 C26 5.9(8) . . . . ? C18 Zr1 C16 C26 159.4(8) . . . . ? C13 Zr1 C16 C26 11.1(8) . . . . ? C20 Zr1 C16 C26 -122.7(9) . . . . ? C15 Zr1 C16 C26 -44.6(8) . . . . ? C11 Zr1 C16 C26 -26.9(8) . . . . ? C14 Zr1 C16 C26 -25.1(9) . . . . ? C19 Zr1 C16 C26 -159.6(8) . . . . ? C20 C16 C17 C18 -1.6(5) . . . . ? C26 C16 C17 C18 164.6(5) . . . . ? Zr1 C16 C17 C18 -68.3(3) . . . . ? C20 C16 C17 C27 -175.6(5) . . . . ? C26 C16 C17 C27 -9.5(8) . . . . ? Zr1 C16 C17 C27 117.6(5) . . . . ? C20 C16 C17 Zr1 66.8(4) . . . . ? C26 C16 C17 Zr1 -127.1(6) . . . . ? O1 Zr1 C17 C16 168.3(3) . . . . ? C3 Zr1 C17 C16 -103.6(3) . . . . ? C12 Zr1 C17 C16 68.7(4) . . . . ? C18 Zr1 C17 C16 -113.4(4) . . . . ? C13 Zr1 C17 C16 93.0(3) . . . . ? C20 Zr1 C17 C16 -36.0(3) . . . . ? C15 Zr1 C17 C16 20.9(4) . . . . ? C11 Zr1 C17 C16 34.2(4) . . . . ? C14 Zr1 C17 C16 73.3(6) . . . . ? C19 Zr1 C17 C16 -75.7(3) . . . . ? O1 Zr1 C17 C18 -78.3(3) . . . . ? C3 Zr1 C17 C18 9.8(3) . . . . ? C12 Zr1 C17 C18 -177.9(3) . . . . ? C16 Zr1 C17 C18 113.4(4) . . . . ? C13 Zr1 C17 C18 -153.6(2) . . . . ? C20 Zr1 C17 C18 77.4(3) . . . . ? C15 Zr1 C17 C18 134.3(3) . . . . ? C11 Zr1 C17 C18 147.6(3) . . . . ? C14 Zr1 C17 C18 -173.3(5) . . . . ? C19 Zr1 C17 C18 37.7(3) . . . . ? O1 Zr1 C17 C27 45.8(5) . . . . ? C3 Zr1 C17 C27 133.9(5) . . . . ? C12 Zr1 C17 C27 -53.8(6) . . . . ? C16 Zr1 C17 C27 -122.5(6) . . . . ? C18 Zr1 C17 C27 124.1(6) . . . . ? C13 Zr1 C17 C27 -29.5(6) . . . . ? C20 Zr1 C17 C27 -158.5(6) . . . . ? C15 Zr1 C17 C27 -101.6(5) . . . . ? C11 Zr1 C17 C27 -88.2(5) . . . . ? C14 Zr1 C17 C27 -49.1(8) . . . . ? C19 Zr1 C17 C27 161.9(6) . . . . ? C16 C17 C18 C19 0.6(5) . . . . ? C27 C17 C18 C19 174.5(4) . . . . ? Zr1 C17 C18 C19 -67.9(3) . . . . ? C16 C17 C18 C28 -172.7(4) . . . . ? C27 C17 C18 C28 1.2(7) . . . . ? Zr1 C17 C18 C28 118.8(4) . . . . ? C16 C17 C18 Zr1 68.5(3) . . . . ? C27 C17 C18 Zr1 -117.6(5) . . . . ? O1 Zr1 C18 C17 98.3(3) . . . . ? C3 Zr1 C18 C17 -171.9(3) . . . . ? C12 Zr1 C18 C17 2.9(4) . . . . ? C16 Zr1 C18 C17 -37.4(3) . . . . ? C13 Zr1 C18 C17 52.7(5) . . . . ? C20 Zr1 C18 C17 -77.1(3) . . . . ? C15 Zr1 C18 C17 -94.3(5) . . . . ? C11 Zr1 C18 C17 -46.7(4) . . . . ? C14 Zr1 C18 C17 162.8(14) . . . . ? C19 Zr1 C18 C17 -113.4(4) . . . . ? O1 Zr1 C18 C19 -148.3(3) . . . . ? C3 Zr1 C18 C19 -58.5(3) . . . . ? C17 Zr1 C18 C19 113.4(4) . . . . ? C12 Zr1 C18 C19 116.3(4) . . . . ? C16 Zr1 C18 C19 76.0(3) . . . . ? C13 Zr1 C18 C19 166.1(4) . . . . ? C20 Zr1 C18 C19 36.3(3) . . . . ? C15 Zr1 C18 C19 19.1(5) . . . . ? C11 Zr1 C18 C19 66.7(4) . . . . ? C14 Zr1 C18 C19 -83.8(14) . . . . ? O1 Zr1 C18 C28 -22.8(5) . . . . ? C3 Zr1 C18 C28 67.0(6) . . . . ? C17 Zr1 C18 C28 -121.1(7) . . . . ? C12 Zr1 C18 C28 -118.2(6) . . . . ? C16 Zr1 C18 C28 -158.5(6) . . . . ? C13 Zr1 C18 C28 -68.4(7) . . . . ? C20 Zr1 C18 C28 161.7(6) . . . . ? C15 Zr1 C18 C28 144.6(6) . . . . ? C11 Zr1 C18 C28 -167.8(5) . . . . ? C14 Zr1 C18 C28 41.7(16) . . . . ? C19 Zr1 C18 C28 125.5(7) . . . . ? C17 C18 C19 C20 0.5(5) . . . . ? C28 C18 C19 C20 173.6(5) . . . . ? Zr1 C18 C19 C20 -66.0(3) . . . . ? C17 C18 C19 C29 -168.8(5) . . . . ? C28 C18 C19 C29 4.2(8) . . . . ? Zr1 C18 C19 C29 124.6(5) . . . . ? C17 C18 C19 Zr1 66.5(3) . . . . ? C28 C18 C19 Zr1 -120.4(5) . . . . ? O1 Zr1 C19 C20 148.5(3) . . . . ? C3 Zr1 C19 C20 -126.4(4) . . . . ? C17 Zr1 C19 C20 77.3(3) . . . . ? C12 Zr1 C19 C20 13.5(5) . . . . ? C16 Zr1 C19 C20 37.0(3) . . . . ? C18 Zr1 C19 C20 115.2(4) . . . . ? C13 Zr1 C19 C20 -22.8(15) . . . . ? C15 Zr1 C19 C20 -54.7(4) . . . . ? C11 Zr1 C19 C20 -19.2(4) . . . . ? C14 Zr1 C19 C20 -81.1(4) . . . . ? O1 Zr1 C19 C18 33.3(3) . . . . ? C3 Zr1 C19 C18 118.4(3) . . . . ? C17 Zr1 C19 C18 -37.9(3) . . . . ? C12 Zr1 C19 C18 -101.7(4) . . . . ? C16 Zr1 C19 C18 -78.2(3) . . . . ? C13 Zr1 C19 C18 -137.9(13) . . . . ? C20 Zr1 C19 C18 -115.2(4) . . . . ? C15 Zr1 C19 C18 -169.9(3) . . . . ? C11 Zr1 C19 C18 -134.4(3) . . . . ? C14 Zr1 C19 C18 163.7(3) . . . . ? O1 Zr1 C19 C29 -86.6(7) . . . . ? C3 Zr1 C19 C29 -1.5(7) . . . . ? C17 Zr1 C19 C29 -157.7(8) . . . . ? C12 Zr1 C19 C29 138.4(7) . . . . ? C16 Zr1 C19 C29 162.0(8) . . . . ? C18 Zr1 C19 C29 -119.8(9) . . . . ? C13 Zr1 C19 C29 102.2(15) . . . . ? C20 Zr1 C19 C29 125.0(9) . . . . ? C15 Zr1 C19 C29 70.3(8) . . . . ? C11 Zr1 C19 C29 105.7(8) . . . . ? C14 Zr1 C19 C29 43.9(9) . . . . ? C17 C16 C20 C19 1.9(6) . . . . ? C26 C16 C20 C19 -164.2(5) . . . . ? Zr1 C16 C20 C19 67.7(3) . . . . ? C17 C16 C20 C30 170.5(5) . . . . ? C26 C16 C20 C30 4.4(9) . . . . ? Zr1 C16 C20 C30 -123.8(6) . . . . ? C17 C16 C20 Zr1 -65.8(3) . . . . ? C26 C16 C20 Zr1 128.1(6) . . . . ? C18 C19 C20 C16 -1.5(6) . . . . ? C29 C19 C20 C16 167.4(5) . . . . ? Zr1 C19 C20 C16 -67.0(4) . . . . ? C18 C19 C20 C30 -171.0(5) . . . . ? C29 C19 C20 C30 -2.1(9) . . . . ? Zr1 C19 C20 C30 123.6(5) . . . . ? C18 C19 C20 Zr1 65.5(3) . . . . ? C29 C19 C20 Zr1 -125.6(5) . . . . ? O1 Zr1 C20 C16 71.1(4) . . . . ? C3 Zr1 C20 C16 165.9(3) . . . . ? C17 Zr1 C20 C16 36.5(3) . . . . ? C12 Zr1 C20 C16 -56.5(3) . . . . ? C18 Zr1 C20 C16 77.3(3) . . . . ? C13 Zr1 C20 C16 -70.9(4) . . . . ? C15 Zr1 C20 C16 -110.6(3) . . . . ? C11 Zr1 C20 C16 -82.4(4) . . . . ? C14 Zr1 C20 C16 -113.2(3) . . . . ? C19 Zr1 C20 C16 114.5(4) . . . . ? O1 Zr1 C20 C19 -43.4(4) . . . . ? C3 Zr1 C20 C19 51.4(3) . . . . ? C17 Zr1 C20 C19 -78.0(3) . . . . ? C12 Zr1 C20 C19 -171.0(3) . . . . ? C16 Zr1 C20 C19 -114.5(4) . . . . ? C18 Zr1 C20 C19 -37.2(3) . . . . ? C13 Zr1 C20 C19 174.6(4) . . . . ? C15 Zr1 C20 C19 134.9(3) . . . . ? C11 Zr1 C20 C19 163.1(4) . . . . ? C14 Zr1 C20 C19 132.2(3) . . . . ? O1 Zr1 C20 C30 -162.4(7) . . . . ? C3 Zr1 C20 C30 -67.6(8) . . . . ? C17 Zr1 C20 C30 162.9(9) . . . . ? C12 Zr1 C20 C30 70.0(8) . . . . ? C16 Zr1 C20 C30 126.5(9) . . . . ? C18 Zr1 C20 C30 -156.2(9) . . . . ? C13 Zr1 C20 C30 55.5(9) . . . . ? C15 Zr1 C20 C30 15.9(8) . . . . ? C11 Zr1 C20 C30 44.1(8) . . . . ? C14 Zr1 C20 C30 13.2(9) . . . . ? C19 Zr1 C20 C30 -119.0(9) . . . . ? C41 P1 C31 C36 132.8(3) . . . . ? C1 P1 C31 C36 10.0(4) . . . . ? C5 P1 C31 C36 -105.3(3) . . . . ? C41 P1 C31 C32 -49.8(3) . . . . ? C1 P1 C31 C32 -172.6(3) . . . . ? C5 P1 C31 C32 72.1(3) . . . . ? C36 C31 C32 C33 -1.3(5) . . . . ? P1 C31 C32 C33 -178.8(3) . . . . ? C36 C31 C32 C37 179.2(4) . . . . ? P1 C31 C32 C37 1.7(5) . . . . ? C31 C32 C33 C34 0.2(6) . . . . ? C37 C32 C33 C34 179.7(4) . . . . ? C32 C33 C34 C35 0.7(7) . . . . ? C32 C33 C34 C38 -179.0(5) . . . . ? C33 C34 C35 C36 -0.6(7) . . . . ? C38 C34 C35 C36 179.1(4) . . . . ? C34 C35 C36 C31 -0.6(6) . . . . ? C34 C35 C36 C39 176.9(4) . . . . ? C32 C31 C36 C35 1.5(5) . . . . ? P1 C31 C36 C35 178.8(3) . . . . ? C32 C31 C36 C39 -175.6(4) . . . . ? P1 C31 C36 C39 1.7(5) . . . . ? C1 P1 C41 C46 -79.9(3) . . . . ? C31 P1 C41 C46 149.3(3) . . . . ? C5 P1 C41 C46 36.4(3) . . . . ? C1 P1 C41 C42 94.2(3) . . . . ? C31 P1 C41 C42 -36.6(3) . . . . ? C5 P1 C41 C42 -149.5(3) . . . . ? C46 C41 C42 C43 -4.8(5) . . . . ? P1 C41 C42 C43 -178.9(3) . . . . ? C46 C41 C42 C47 171.9(4) . . . . ? P1 C41 C42 C47 -2.2(5) . . . . ? C41 C42 C43 C44 1.0(6) . . . . ? C47 C42 C43 C44 -176.0(4) . . . . ? C42 C43 C44 C45 2.7(7) . . . . ? C42 C43 C44 C48 -178.4(5) . . . . ? C43 C44 C45 C46 -2.6(7) . . . . ? C48 C44 C45 C46 178.4(5) . . . . ? C44 C45 C46 C41 -1.2(6) . . . . ? C44 C45 C46 C49 176.2(4) . . . . ? C42 C41 C46 C45 4.9(5) . . . . ? P1 C41 C46 C45 179.0(3) . . . . ? C42 C41 C46 C49 -172.2(4) . . . . ? P1 C41 C46 C49 1.9(5) . . . . ? C4 B1 C51 C56 -62.9(4) . . . . ? C2 B1 C51 C56 176.4(3) . . . . ? C61 B1 C51 C56 61.2(4) . . . . ? C4 B1 C51 C52 115.5(4) . . . . ? C2 B1 C51 C52 -5.2(5) . . . . ? C61 B1 C51 C52 -120.4(4) . . . . ? C56 C51 C52 F52 179.6(3) . . . . ? B1 C51 C52 F52 1.2(6) . . . . ? C56 C51 C52 C53 0.1(6) . . . . ? B1 C51 C52 C53 -178.4(4) . . . . ? F52 C52 C53 F53 0.2(6) . . . . ? C51 C52 C53 F53 179.7(4) . . . . ? F52 C52 C53 C54 -178.5(4) . . . . ? C51 C52 C53 C54 1.0(6) . . . . ? F53 C53 C54 F54 -2.2(6) . . . . ? C52 C53 C54 F54 176.5(4) . . . . ? F53 C53 C54 C55 -179.1(4) . . . . ? C52 C53 C54 C55 -0.4(6) . . . . ? F54 C54 C55 F55 -0.3(6) . . . . ? C53 C54 C55 F55 176.6(4) . . . . ? F54 C54 C55 C56 -178.3(3) . . . . ? C53 C54 C55 C56 -1.4(6) . . . . ? F55 C55 C56 F56 4.2(5) . . . . ? C54 C55 C56 F56 -177.9(3) . . . . ? F55 C55 C56 C51 -175.2(4) . . . . ? C54 C55 C56 C51 2.8(6) . . . . ? C52 C51 C56 F56 178.7(3) . . . . ? B1 C51 C56 F56 -2.7(5) . . . . ? C52 C51 C56 C55 -2.0(5) . . . . ? B1 C51 C56 C55 176.6(3) . . . . ? C4 B1 C61 C66 -177.8(3) . . . . ? C2 B1 C61 C66 -56.3(4) . . . . ? C51 B1 C61 C66 62.5(4) . . . . ? C4 B1 C61 C62 -1.6(5) . . . . ? C2 B1 C61 C62 119.9(4) . . . . ? C51 B1 C61 C62 -121.4(4) . . . . ? C66 C61 C62 F62 -179.0(3) . . . . ? B1 C61 C62 F62 4.6(5) . . . . ? C66 C61 C62 C63 2.1(5) . . . . ? B1 C61 C62 C63 -174.3(3) . . . . ? F62 C62 C63 F63 1.1(5) . . . . ? C61 C62 C63 F63 -180.0(3) . . . . ? F62 C62 C63 C64 -179.4(3) . . . . ? C61 C62 C63 C64 -0.6(6) . . . . ? F63 C63 C64 F64 -1.0(6) . . . . ? C62 C63 C64 F64 179.6(3) . . . . ? F63 C63 C64 C65 178.3(3) . . . . ? C62 C63 C64 C65 -1.1(6) . . . . ? F64 C64 C65 F65 0.0(6) . . . . ? C63 C64 C65 F65 -179.3(4) . . . . ? F64 C64 C65 C66 -179.7(4) . . . . ? C63 C64 C65 C66 1.0(6) . . . . ? F65 C65 C66 F66 1.0(6) . . . . ? C64 C65 C66 F66 -179.4(4) . . . . ? F65 C65 C66 C61 -178.9(4) . . . . ? C64 C65 C66 C61 0.8(6) . . . . ? C62 C61 C66 F66 177.9(3) . . . . ? B1 C61 C66 F66 -5.4(5) . . . . ? C62 C61 C66 C65 -2.3(5) . . . . ? B1 C61 C66 C65 174.4(4) . . . . ? C75 C71 C72 C73 -1.8(14) . . . . ? C71 C72 C73 C74 0.7(11) . . . . ? C72 C73 C74 C75 0.7(13) . . . . ? C73 C74 C75 C71 -1.9(16) . . . . ? C72 C71 C75 C74 2.4(17) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.798 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 950034' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk7011 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H51 B Cl2 F10 N O P Zr' _chemical_formula_weight 1111.85 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.2150(2) _cell_length_b 12.6017(2) _cell_length_c 22.4162(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.9890(10) _cell_angle_gamma 90.00 _cell_volume 5051.07(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10109 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9302 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30888 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8742 _reflns_number_gt 7126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One Cp group, one methyl group, one C6F5 group and one dichloromethane molecule are disordered over two positions. Several restraints (SADI, SAME ISOR and SIMU) were used in order to improve refinement stability. ; _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^)+(0.0353P)^2^+8.8015P] 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 8742 _refine_ls_number_parameters 777 _refine_ls_number_restraints 380 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.104 _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 Zr1 Zr 0.77669(2) 1.88899(3) 0.852148(16) 0.04182(12) Uani 1 1 d D A . C3 C 0.7783(8) 1.7358(8) 0.7946(6) 0.052(3) Uani 0.543(19) 1 d PDU A 1 H3A H 0.7722 1.7546 0.7519 0.078 Uiso 0.543(19) 1 calc PR A 1 H3B H 0.7378 1.6895 0.8004 0.078 Uiso 0.543(19) 1 calc PR A 1 H3C H 0.8257 1.6995 0.8073 0.078 Uiso 0.543(19) 1 calc PR A 1 C16 C 0.8657(8) 1.9698(14) 0.7909(6) 0.076(4) Uani 0.543(19) 1 d PDU A 1 H16 H 0.8489 1.9784 0.7489 0.091 Uiso 0.543(19) 1 calc PR A 1 C17 C 0.9024(7) 1.8805(11) 0.8195(8) 0.066(4) Uani 0.543(19) 1 d PDU A 1 H17 H 0.9155 1.8199 0.7994 0.079 Uiso 0.543(19) 1 calc PR A 1 C18 C 0.9165(5) 1.8954(13) 0.8822(7) 0.059(3) Uani 0.543(19) 1 d PDU A 1 H18 H 0.9383 1.8467 0.9122 0.071 Uiso 0.543(19) 1 calc PR A 1 C19 C 0.8915(7) 1.9989(13) 0.8912(6) 0.059(3) Uani 0.543(19) 1 d PDU A 1 H19 H 0.8965 2.0326 0.9292 0.071 Uiso 0.543(19) 1 calc PR A 1 C20 C 0.8582(7) 2.0444(8) 0.8361(9) 0.067(3) Uani 0.543(19) 1 d PDU A 1 H20 H 0.8354 2.1114 0.8302 0.080 Uiso 0.543(19) 1 calc PR A 1 C3A C 0.7564(9) 1.7501(10) 0.7853(7) 0.050(4) Uani 0.457(19) 1 d PDU A 2 H3A1 H 0.7555 1.7760 0.7444 0.075 Uiso 0.457(19) 1 calc PR A 2 H3A2 H 0.7089 1.7170 0.7872 0.075 Uiso 0.457(19) 1 calc PR A 2 H3A3 H 0.7963 1.6985 0.7958 0.075 Uiso 0.457(19) 1 calc PR A 2 C16A C 0.8611(9) 1.9923(14) 0.7985(7) 0.073(5) Uani 0.457(19) 1 d PDU A 2 H16A H 0.8384 2.0304 0.7638 0.087 Uiso 0.457(19) 1 calc PR A 2 C17A C 0.8869(9) 1.8883(14) 0.7992(9) 0.072(5) Uani 0.457(19) 1 d PDU A 2 H17A H 0.8850 1.8439 0.7653 0.086 Uiso 0.457(19) 1 calc PR A 2 C18A C 0.9164(7) 1.8616(14) 0.8598(10) 0.072(4) Uani 0.457(19) 1 d PDU A 2 H18A H 0.9369 1.7956 0.8737 0.086 Uiso 0.457(19) 1 calc PR A 2 C19A C 0.9098(8) 1.9502(19) 0.8958(6) 0.068(4) Uani 0.457(19) 1 d PDU A 2 H19A H 0.9265 1.9541 0.9381 0.082 Uiso 0.457(19) 1 calc PR A 2 C20A C 0.8750(9) 2.0312(11) 0.8595(9) 0.064(4) Uani 0.457(19) 1 d PDU A 2 H20A H 0.8628 2.0989 0.8724 0.076 Uiso 0.457(19) 1 calc PR A 2 P1 P 0.77148(5) 1.76263(7) 1.04509(4) 0.0354(2) Uani 1 1 d . A . O1 O 0.78777(14) 1.90766(18) 0.95733(11) 0.0395(6) Uani 1 1 d . A . N1 N 0.77770(17) 1.7468(2) 0.92010(13) 0.0402(7) Uani 1 1 d . A . C1 C 0.8320(2) 1.6473(3) 1.06351(15) 0.0408(8) Uani 1 1 d . . . H1A H 0.8063 1.5852 1.0430 0.049 Uiso 1 1 calc R . . H1B H 0.8775 1.6586 1.0470 0.049 Uiso 1 1 calc R . . C2 C 0.8547(2) 1.6223(3) 1.13149(15) 0.0392(8) Uani 1 1 d . . . H2A H 0.8103 1.6016 1.1474 0.047 Uiso 1 1 calc R . . H2B H 0.8758 1.6861 1.1532 0.047 Uiso 1 1 calc R . . C4 C 0.9940(2) 1.5662(3) 1.12477(19) 0.0519(10) Uani 1 1 d . . . H4A H 0.9854 1.5803 1.0815 0.078 Uiso 1 1 calc R . . H4B H 1.0318 1.5116 1.1348 0.078 Uiso 1 1 calc R . . H4C H 1.0108 1.6306 1.1469 0.078 Uiso 1 1 calc R . . C5 C 0.78092(18) 1.8094(3) 0.96655(15) 0.0357(7) Uani 1 1 d . . . C11 C 0.6729(3) 1.9585(6) 0.7714(2) 0.0850(17) Uani 1 1 d . A . H11 H 0.6805 1.9563 0.7311 0.102 Uiso 1 1 calc R . . C12 C 0.6400(3) 1.8784(5) 0.8011(3) 0.0832(16) Uani 1 1 d . . . H12 H 0.6200 1.8140 0.7842 0.100 Uiso 1 1 calc R A . C13 C 0.6427(2) 1.9128(4) 0.8606(2) 0.0595(11) Uani 1 1 d . A . H13 H 0.6259 1.8747 0.8915 0.071 Uiso 1 1 calc R . . C14 C 0.6746(2) 2.0128(4) 0.8662(2) 0.0600(11) Uani 1 1 d . A . H14 H 0.6831 2.0546 0.9016 0.072 Uiso 1 1 calc R . . C15 C 0.6918(3) 2.0407(4) 0.8116(2) 0.0715(13) Uani 1 1 d . A . H15 H 0.7131 2.1055 0.8029 0.086 Uiso 1 1 calc R . . C21 C 0.6702(2) 1.7471(3) 1.03409(16) 0.0389(8) Uani 1 1 d . . . C22 C 0.6259(2) 1.8389(3) 1.01777(15) 0.0394(8) Uani 1 1 d . A . C23 C 0.5488(2) 1.8276(3) 1.00215(16) 0.0464(9) Uani 1 1 d . . . H23 H 0.5198 1.8878 0.9888 0.056 Uiso 1 1 calc R A . C24 C 0.5133(2) 1.7323(3) 1.00547(19) 0.0525(10) Uani 1 1 d . A . C25 C 0.5570(2) 1.6448(3) 1.02354(19) 0.0545(10) Uani 1 1 d . . . H25 H 0.5331 1.5793 1.0262 0.065 Uiso 1 1 calc R A . C26 C 0.6348(2) 1.6482(3) 1.03804(17) 0.0471(9) Uani 1 1 d . A . C27 C 0.6550(2) 1.9520(3) 1.02062(17) 0.0435(9) Uani 1 1 d . . . H27A H 0.6216 1.9955 0.9916 0.065 Uiso 1 1 calc R A . H27B H 0.7046 1.9529 1.0108 0.065 Uiso 1 1 calc R . . H27C H 0.6572 1.9800 1.0612 0.065 Uiso 1 1 calc R . . C28 C 0.4290(3) 1.7259(4) 0.9908(2) 0.0757(14) Uani 1 1 d . . . H28A H 0.4080 1.7945 0.9976 0.114 Uiso 1 1 calc R A . H28B H 0.4121 1.6734 1.0168 0.114 Uiso 1 1 calc R . . H28C H 0.4129 1.7055 0.9486 0.114 Uiso 1 1 calc R . . C29 C 0.6744(3) 1.5457(3) 1.0578(2) 0.0698(13) Uani 1 1 d . . . H29A H 0.6382 1.4930 1.0650 0.105 Uiso 1 1 calc R A . H29B H 0.7107 1.5572 1.0949 0.105 Uiso 1 1 calc R . . H29C H 0.6998 1.5206 1.0262 0.105 Uiso 1 1 calc R . . C31 C 0.8049(2) 1.8637(3) 1.10145(16) 0.0404(8) Uani 1 1 d . . . C32 C 0.8711(2) 1.9192(3) 1.09765(17) 0.0465(9) Uani 1 1 d . A . C33 C 0.8919(3) 2.0041(3) 1.13682(19) 0.0582(11) Uani 1 1 d . . . H33 H 0.9353 2.0424 1.1338 0.070 Uiso 1 1 calc R A . C34 C 0.8513(3) 2.0342(3) 1.1800(2) 0.0618(12) Uani 1 1 d . A . C35 C 0.7915(3) 1.9723(3) 1.18677(18) 0.0571(11) Uani 1 1 d . . . H35 H 0.7658 1.9890 1.2182 0.068 Uiso 1 1 calc R A . C36 C 0.7668(2) 1.8857(3) 1.14931(16) 0.0441(9) Uani 1 1 d . A . C37 C 0.9259(2) 1.8868(4) 1.0584(2) 0.0668(13) Uani 1 1 d . . . H37A H 0.9460 1.9497 1.0424 0.100 Uiso 1 1 calc R A . H37B H 0.9005 1.8434 1.0250 0.100 Uiso 1 1 calc R . . H37C H 0.9663 1.8465 1.0825 0.100 Uiso 1 1 calc R . . C38 C 0.8754(4) 2.1279(4) 1.2213(2) 0.0918(19) Uani 1 1 d . . . H38A H 0.9004 2.1026 1.2608 0.138 Uiso 1 1 calc R A . H38B H 0.8318 2.1691 1.2258 0.138 Uiso 1 1 calc R . . H38C H 0.9094 2.1722 1.2038 0.138 Uiso 1 1 calc R . . C39 C 0.7041(2) 1.8196(4) 1.16505(18) 0.0568(11) Uani 1 1 d . . . H39A H 0.7003 1.8322 1.2070 0.085 Uiso 1 1 calc R A . H39B H 0.7143 1.7451 1.1595 0.085 Uiso 1 1 calc R . . H39C H 0.6574 1.8390 1.1387 0.085 Uiso 1 1 calc R . . B1 B 0.9165(2) 1.5261(3) 1.14351(18) 0.0388(9) Uani 1 1 d . . . C41 C 0.8791(2) 1.4171(3) 1.10773(16) 0.0448(9) Uani 1 1 d . B . F42 F 0.96585(18) 1.3969(3) 1.04151(13) 0.0866(9) Uani 1 1 d . B . C42 C 0.9048(3) 1.3629(3) 1.0620(2) 0.0641(12) Uani 1 1 d D . . C46 C 0.8163(3) 1.3701(3) 1.1234(2) 0.0594(11) Uani 1 1 d D . . C43 C 0.8627(9) 1.2703(10) 1.0386(7) 0.058(3) Uani 0.54(3) 1 d PDU B 1 F43 F 0.8874(10) 1.2170(9) 0.9936(5) 0.089(3) Uani 0.54(3) 1 d PDU B 1 C44 C 0.7998(9) 1.2332(10) 1.0568(7) 0.059(3) Uani 0.54(3) 1 d PDU B 1 F44 F 0.7638(9) 1.1448(8) 1.0320(6) 0.089(3) Uani 0.54(3) 1 d PDU B 1 C45 C 0.7738(9) 1.2820(10) 1.1034(7) 0.053(3) Uani 0.54(3) 1 d PDU B 1 F45 F 0.7151(6) 1.2476(11) 1.1249(7) 0.077(3) Uani 0.54(3) 1 d PDU B 1 C43A C 0.8855(11) 1.2721(13) 1.0295(9) 0.063(4) Uani 0.46(3) 1 d PDU B 2 F43A F 0.9201(11) 1.2296(12) 0.9884(6) 0.088(4) Uani 0.46(3) 1 d PDU B 2 C44A C 0.8249(10) 1.2269(11) 1.0467(8) 0.058(4) Uani 0.46(3) 1 d PDU B 2 F44A F 0.7958(11) 1.1376(9) 1.0177(6) 0.085(4) Uani 0.46(3) 1 d PDU B 2 C45A C 0.7917(10) 1.2764(12) 1.0896(9) 0.055(4) Uani 0.46(3) 1 d PDU B 2 F45A F 0.7312(8) 1.2280(10) 1.1054(8) 0.075(3) Uani 0.46(3) 1 d PDU B 2 F46 F 0.78630(13) 1.4124(2) 1.16893(12) 0.0666(7) Uani 1 1 d . B . C51 C 0.9385(2) 1.4923(3) 1.21672(16) 0.0420(8) Uani 1 1 d . . . F52 F 1.00824(15) 1.3459(2) 1.19137(12) 0.0693(7) Uani 1 1 d . . . C52 C 0.9846(2) 1.4060(3) 1.23408(18) 0.0514(10) Uani 1 1 d . . . F53 F 1.05399(16) 1.2889(2) 1.30623(13) 0.0867(9) Uani 1 1 d . . . C53 C 1.0106(2) 1.3749(4) 1.2936(2) 0.0609(12) Uani 1 1 d . . . F54 F 1.01814(17) 1.4079(3) 1.39808(12) 0.0956(11) Uani 1 1 d . . . C54 C 0.9910(3) 1.4337(4) 1.3391(2) 0.0644(13) Uani 1 1 d . . . F55 F 0.92586(18) 1.5780(3) 1.37057(11) 0.0892(9) Uani 1 1 d . . . C55 C 0.9454(3) 1.5193(4) 1.32534(18) 0.0593(11) Uani 1 1 d . . . F56 F 0.87157(15) 1.6295(2) 1.25690(10) 0.0666(7) Uani 1 1 d . . . C56 C 0.9192(2) 1.5452(3) 1.26537(17) 0.0494(9) Uani 1 1 d . . . C61 C 0.7649(2) 1.6354(3) 0.91688(16) 0.0398(8) Uani 1 1 d . . . C62 C 0.6928(2) 1.5959(3) 0.90482(19) 0.0515(10) Uani 1 1 d . A . H62 H 0.6520 1.6426 0.9020 0.062 Uiso 1 1 calc R . . C63 C 0.6802(2) 1.4883(3) 0.8969(2) 0.0563(11) Uani 1 1 d . . . H63 H 0.6308 1.4628 0.8888 0.068 Uiso 1 1 calc R A . C64 C 0.7388(2) 1.4172(3) 0.90072(17) 0.0493(10) Uani 1 1 d . A . C65 C 0.8105(2) 1.4580(3) 0.91179(17) 0.0474(9) Uani 1 1 d . . . H65 H 0.8513 1.4113 0.9145 0.057 Uiso 1 1 calc R A . C66 C 0.8239(2) 1.5657(3) 0.91905(17) 0.0444(9) Uani 1 1 d . A . H66 H 0.8732 1.5915 0.9255 0.053 Uiso 1 1 calc R . . C67 C 0.7251(3) 1.2998(3) 0.8923(2) 0.0662(13) Uani 1 1 d . . . H67A H 0.7698 1.2658 0.8840 0.099 Uiso 1 1 calc R A . H67B H 0.6840 1.2881 0.8585 0.099 Uiso 1 1 calc R . . H67C H 0.7126 1.2701 0.9290 0.099 Uiso 1 1 calc R . . C71 C 0.5509(7) 1.3406(11) 1.1935(5) 0.132(4) Uani 0.783(8) 1 d PDU C 1 H71A H 0.6042 1.3423 1.2117 0.159 Uiso 0.783(8) 1 calc PR C 1 H71B H 0.5414 1.2752 1.1696 0.159 Uiso 0.783(8) 1 calc PR C 1 Cl1 Cl 0.4997(3) 1.3366(4) 1.25131(17) 0.1332(15) Uani 0.783(8) 1 d PDU C 1 Cl2 Cl 0.5308(2) 1.4480(4) 1.14500(15) 0.1488(18) Uani 0.783(8) 1 d PDU C 1 C71A C 0.5562(15) 1.355(4) 1.2106(9) 0.096(9) Uani 0.217(8) 1 d PDU C 2 H71C H 0.5753 1.2858 1.2258 0.115 Uiso 0.217(8) 1 calc PR C 2 H71D H 0.5958 1.4089 1.2201 0.115 Uiso 0.217(8) 1 calc PR C 2 Cl1A Cl 0.4760(7) 1.3911(14) 1.2364(8) 0.133(5) Uani 0.217(8) 1 d PDU C 2 Cl2A Cl 0.5159(7) 1.3530(17) 1.1342(7) 0.171(7) Uani 0.217(8) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0519(2) 0.03458(19) 0.0403(2) -0.00138(15) 0.01225(16) -0.00180(17) C3 0.075(7) 0.042(5) 0.034(5) 0.002(4) 0.000(5) 0.006(5) C16 0.080(7) 0.085(8) 0.071(6) 0.018(6) 0.033(5) -0.004(6) C17 0.060(6) 0.077(6) 0.069(8) -0.009(6) 0.031(6) 0.001(5) C18 0.050(5) 0.064(7) 0.066(6) 0.002(5) 0.018(4) -0.009(5) C19 0.050(5) 0.054(6) 0.074(6) -0.013(5) 0.017(5) -0.016(5) C20 0.064(6) 0.055(5) 0.083(8) 0.016(5) 0.016(6) -0.001(4) C3A 0.064(7) 0.044(6) 0.036(6) 0.001(4) -0.008(5) 0.025(5) C16A 0.080(8) 0.071(8) 0.075(8) 0.019(6) 0.035(6) -0.005(6) C17A 0.066(7) 0.086(8) 0.069(7) -0.007(6) 0.028(6) 0.001(6) C18A 0.061(6) 0.078(8) 0.083(8) 0.001(7) 0.027(6) 0.001(5) C19A 0.058(6) 0.073(8) 0.074(6) 0.005(7) 0.017(5) -0.019(7) C20A 0.066(7) 0.054(6) 0.069(8) 0.007(6) 0.009(6) -0.007(5) P1 0.0374(5) 0.0306(4) 0.0370(5) -0.0016(4) 0.0041(4) -0.0004(4) O1 0.0478(15) 0.0286(13) 0.0423(13) -0.0034(10) 0.0091(11) -0.0032(11) N1 0.0464(18) 0.0334(15) 0.0414(16) -0.0022(13) 0.0101(13) -0.0007(13) C1 0.045(2) 0.0360(18) 0.0396(19) -0.0016(15) 0.0045(16) 0.0050(16) C2 0.043(2) 0.0361(18) 0.0367(18) 0.0008(15) 0.0043(15) 0.0017(16) C4 0.045(2) 0.055(2) 0.056(2) 0.003(2) 0.0107(18) 0.0011(19) C5 0.0340(18) 0.0325(18) 0.0397(18) -0.0023(15) 0.0050(14) -0.0008(15) C11 0.085(4) 0.123(5) 0.045(3) 0.015(3) 0.007(3) 0.025(4) C12 0.054(3) 0.090(4) 0.092(4) -0.026(3) -0.018(3) -0.003(3) C13 0.047(2) 0.064(3) 0.066(3) 0.011(2) 0.009(2) 0.004(2) C14 0.061(3) 0.058(3) 0.060(3) 0.006(2) 0.010(2) 0.013(2) C15 0.081(3) 0.064(3) 0.069(3) 0.020(3) 0.014(3) 0.015(3) C21 0.0389(19) 0.0356(18) 0.0413(19) -0.0016(15) 0.0057(15) -0.0041(16) C22 0.042(2) 0.0405(19) 0.0368(18) -0.0001(15) 0.0106(15) 0.0006(17) C23 0.040(2) 0.054(2) 0.044(2) -0.0012(18) 0.0078(16) 0.0024(18) C24 0.039(2) 0.061(3) 0.056(2) -0.010(2) 0.0058(18) -0.007(2) C25 0.048(2) 0.046(2) 0.067(3) -0.003(2) 0.005(2) -0.016(2) C26 0.050(2) 0.039(2) 0.050(2) -0.0027(17) 0.0038(18) -0.0075(18) C27 0.042(2) 0.0377(19) 0.051(2) 0.0002(17) 0.0093(17) 0.0060(17) C28 0.049(3) 0.077(3) 0.098(4) -0.016(3) 0.005(3) -0.016(2) C29 0.063(3) 0.041(2) 0.098(4) 0.012(2) -0.004(3) -0.012(2) C31 0.045(2) 0.0337(18) 0.0408(19) -0.0011(15) 0.0033(16) 0.0019(16) C32 0.047(2) 0.042(2) 0.046(2) 0.0009(17) -0.0017(17) -0.0065(17) C33 0.060(3) 0.049(2) 0.057(3) 0.001(2) -0.010(2) -0.014(2) C34 0.084(3) 0.039(2) 0.054(2) -0.0057(19) -0.009(2) 0.000(2) C35 0.075(3) 0.052(2) 0.042(2) -0.0065(19) 0.006(2) 0.013(2) C36 0.050(2) 0.040(2) 0.0395(19) 0.0006(16) 0.0034(16) 0.0070(18) C37 0.047(2) 0.089(3) 0.064(3) -0.010(3) 0.010(2) -0.019(2) C38 0.136(5) 0.053(3) 0.072(3) -0.020(3) -0.015(3) -0.009(3) C39 0.063(3) 0.067(3) 0.044(2) 0.000(2) 0.018(2) 0.000(2) B1 0.041(2) 0.036(2) 0.039(2) -0.0005(17) 0.0041(17) 0.0042(18) C41 0.048(2) 0.040(2) 0.041(2) 0.0032(16) -0.0045(17) 0.0042(17) F42 0.101(2) 0.091(2) 0.0730(18) -0.0279(16) 0.0312(17) 0.0110(18) C42 0.083(3) 0.049(3) 0.053(3) -0.005(2) -0.003(2) 0.012(2) C46 0.062(3) 0.044(2) 0.063(3) 0.011(2) -0.012(2) -0.002(2) C43 0.070(8) 0.048(5) 0.053(6) -0.014(4) 0.008(5) 0.016(5) F43 0.105(7) 0.071(4) 0.089(5) -0.042(4) 0.014(5) 0.008(5) C44 0.062(7) 0.038(5) 0.068(6) -0.009(4) -0.010(5) 0.000(5) F44 0.100(7) 0.050(4) 0.102(6) -0.017(3) -0.016(5) -0.020(4) C45 0.052(7) 0.042(5) 0.061(6) 0.020(4) -0.001(5) -0.015(5) F45 0.062(4) 0.075(5) 0.089(6) 0.011(4) 0.002(4) -0.029(4) C43A 0.074(8) 0.058(6) 0.057(7) -0.011(5) 0.011(6) 0.015(6) F43A 0.103(8) 0.084(6) 0.077(5) -0.030(4) 0.021(5) 0.011(6) C44A 0.060(8) 0.044(6) 0.061(6) -0.005(5) -0.008(6) 0.008(6) F44A 0.106(8) 0.051(4) 0.086(5) -0.015(4) -0.011(5) -0.012(5) C45A 0.043(6) 0.061(7) 0.059(7) 0.015(6) 0.009(5) -0.005(5) F45A 0.072(6) 0.060(5) 0.089(7) 0.006(4) 0.005(4) -0.023(4) F46 0.0519(14) 0.0677(16) 0.0792(17) 0.0182(14) 0.0097(13) -0.0080(12) C51 0.0361(19) 0.044(2) 0.042(2) 0.0049(16) -0.0011(16) -0.0032(16) F52 0.0723(17) 0.0584(15) 0.0708(16) -0.0009(13) -0.0025(13) 0.0251(13) C52 0.050(2) 0.049(2) 0.051(2) 0.0058(19) -0.0018(18) -0.0020(19) F53 0.0772(19) 0.079(2) 0.092(2) 0.0386(16) -0.0116(15) 0.0133(16) C53 0.047(2) 0.061(3) 0.069(3) 0.025(2) -0.006(2) -0.002(2) F54 0.082(2) 0.144(3) 0.0530(15) 0.0444(18) -0.0058(14) -0.019(2) C54 0.052(3) 0.089(3) 0.046(2) 0.027(2) -0.008(2) -0.019(3) F55 0.103(2) 0.124(3) 0.0432(14) -0.0053(16) 0.0197(14) -0.004(2) C55 0.060(3) 0.078(3) 0.039(2) 0.000(2) 0.0078(19) -0.015(2) F56 0.0830(18) 0.0692(16) 0.0493(13) -0.0064(12) 0.0164(12) 0.0193(14) C56 0.051(2) 0.054(2) 0.043(2) 0.0024(18) 0.0082(18) -0.005(2) C61 0.046(2) 0.0322(18) 0.0407(19) -0.0044(15) 0.0079(16) -0.0023(16) C62 0.047(2) 0.040(2) 0.066(3) -0.0075(19) 0.0065(19) -0.0001(18) C63 0.050(2) 0.046(2) 0.069(3) -0.006(2) 0.003(2) -0.011(2) C64 0.069(3) 0.0337(19) 0.045(2) -0.0041(16) 0.0103(19) -0.0069(19) C65 0.055(2) 0.037(2) 0.050(2) -0.0016(17) 0.0121(18) 0.0056(18) C66 0.043(2) 0.041(2) 0.049(2) -0.0050(17) 0.0083(17) -0.0045(17) C67 0.090(4) 0.037(2) 0.070(3) -0.010(2) 0.010(3) -0.013(2) C71 0.151(7) 0.118(7) 0.116(7) -0.010(6) -0.004(6) 0.051(6) Cl1 0.129(3) 0.144(3) 0.128(2) -0.009(2) 0.028(2) -0.041(2) Cl2 0.177(3) 0.150(4) 0.118(2) 0.025(2) 0.0256(19) 0.037(2) C71A 0.091(11) 0.099(12) 0.096(12) -0.008(9) 0.015(8) 0.009(8) Cl1A 0.095(6) 0.140(8) 0.160(8) -0.009(7) 0.013(5) 0.016(6) Cl2A 0.137(8) 0.196(12) 0.173(9) -0.033(8) 0.013(6) -0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C3A 2.288(10) . ? Zr1 C3 2.326(9) . ? Zr1 O1 2.340(2) . ? Zr1 N1 2.350(3) . ? Zr1 C16A 2.492(12) . ? Zr1 C14 2.493(4) . ? Zr1 C13 2.501(4) . ? Zr1 C18 2.509(10) . ? Zr1 C11 2.514(5) . ? Zr1 C20A 2.517(11) . ? Zr1 C15 2.518(5) . ? Zr1 C17A 2.520(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C16 C17 1.399(12) . ? C16 C20 1.408(14) . ? C16 H16 0.9400 . ? C17 C18 1.394(11) . ? C17 H17 0.9400 . ? C18 C19 1.409(11) . ? C18 H18 0.9400 . ? C19 C20 1.392(11) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C3A H3A3 0.9700 . ? C16A C17A 1.392(13) . ? C16A C20A 1.429(15) . ? C16A H16A 0.9400 . ? C17A C18A 1.402(13) . ? C17A H17A 0.9400 . ? C18A C19A 1.396(12) . ? C18A H18A 0.9400 . ? C19A C20A 1.383(13) . ? C19A H19A 0.9400 . ? C20A H20A 0.9400 . ? P1 C31 1.815(4) . ? P1 C1 1.823(4) . ? P1 C21 1.825(4) . ? P1 C5 1.895(3) . ? O1 C5 1.265(4) . ? N1 C5 1.299(4) . ? N1 C61 1.423(4) . ? C1 C2 1.534(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 B1 1.642(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C4 B1 1.628(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C11 C15 1.373(8) . ? C11 C12 1.405(8) . ? C11 H11 0.9400 . ? C12 C13 1.393(7) . ? C12 H12 0.9400 . ? C13 C14 1.384(6) . ? C13 H13 0.9400 . ? C14 C15 1.367(6) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C21 C26 1.414(5) . ? C21 C22 1.417(5) . ? C22 C23 1.389(5) . ? C22 C27 1.518(5) . ? C23 C24 1.373(6) . ? C23 H23 0.9400 . ? C24 C25 1.376(6) . ? C24 C28 1.509(6) . ? C25 C26 1.393(5) . ? C25 H25 0.9400 . ? C26 C29 1.505(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C31 C32 1.410(5) . ? C31 C36 1.413(5) . ? C32 C33 1.390(5) . ? C32 C37 1.508(6) . ? C33 C34 1.378(6) . ? C33 H33 0.9400 . ? C34 C35 1.372(6) . ? C34 C38 1.514(6) . ? C35 C36 1.398(5) . ? C35 H35 0.9400 . ? C36 C39 1.509(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? B1 C51 1.668(5) . ? B1 C41 1.669(5) . ? C41 C42 1.386(6) . ? C41 C46 1.392(6) . ? F42 C42 1.351(6) . ? C42 C43A 1.365(11) . ? C42 C43 1.438(10) . ? C46 F46 1.355(5) . ? C46 C45 1.378(10) . ? C46 C45A 1.428(11) . ? C43 F43 1.358(11) . ? C43 C44 1.370(11) . ? C44 F44 1.356(10) . ? C44 C45 1.372(11) . ? C45 F45 1.329(11) . ? C43A F43A 1.323(12) . ? C43A C44A 1.362(12) . ? C44A F44A 1.356(11) . ? C44A C45A 1.380(12) . ? C45A F45A 1.364(12) . ? C51 C56 1.380(5) . ? C51 C52 1.383(5) . ? F52 C52 1.354(5) . ? C52 C53 1.384(6) . ? F53 C53 1.339(5) . ? C53 C54 1.363(7) . ? F54 C54 1.360(5) . ? C54 C55 1.360(7) . ? F55 C55 1.356(5) . ? C55 C56 1.377(5) . ? F56 C56 1.362(5) . ? C61 C66 1.382(5) . ? C61 C62 1.382(5) . ? C62 C63 1.381(5) . ? C62 H62 0.9400 . ? C63 C64 1.383(6) . ? C63 H63 0.9400 . ? C64 C65 1.381(6) . ? C64 C67 1.506(5) . ? C65 C66 1.383(5) . ? C65 H65 0.9400 . ? C66 H66 0.9400 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C67 H67C 0.9700 . ? C71 Cl2 1.730(11) . ? C71 Cl1 1.736(10) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71A Cl1A 1.730(16) . ? C71A Cl2A 1.732(17) . ? C71A H71C 0.9800 . ? C71A H71D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3A Zr1 C3 11.2(5) . . ? C3A Zr1 O1 135.2(4) . . ? C3 Zr1 O1 129.4(4) . . ? C3A Zr1 N1 79.7(4) . . ? C3 Zr1 N1 74.2(4) . . ? O1 Zr1 N1 55.59(9) . . ? C3A Zr1 C16A 96.9(6) . . ? C3 Zr1 C16A 95.2(6) . . ? O1 Zr1 C16A 119.4(4) . . ? N1 Zr1 C16A 141.4(4) . . ? C3A Zr1 C14 122.1(4) . . ? C3 Zr1 C14 132.7(4) . . ? O1 Zr1 C14 74.50(12) . . ? N1 Zr1 C14 108.02(13) . . ? C16A Zr1 C14 106.1(5) . . ? C3A Zr1 C13 95.9(4) . . ? C3 Zr1 C13 104.9(4) . . ? O1 Zr1 C13 79.02(12) . . ? N1 Zr1 C13 85.95(13) . . ? C16A Zr1 C13 132.4(4) . . ? C14 Zr1 C13 32.19(14) . . ? C3A Zr1 C18 103.3(5) . . ? C3 Zr1 C18 93.2(5) . . ? O1 Zr1 C18 80.7(4) . . ? N1 Zr1 C18 88.2(3) . . ? C16A Zr1 C18 54.9(5) . . ? C14 Zr1 C18 133.6(5) . . ? C13 Zr1 C18 158.6(4) . . ? C3A Zr1 C11 77.8(4) . . ? C3 Zr1 C11 88.7(4) . . ? O1 Zr1 C11 126.84(14) . . ? N1 Zr1 C11 130.16(18) . . ? C16A Zr1 C11 85.3(4) . . ? C14 Zr1 C11 52.85(17) . . ? C13 Zr1 C11 53.28(16) . . ? C18 Zr1 C11 140.2(3) . . ? C3A Zr1 C20A 127.7(6) . . ? C3 Zr1 C20A 122.9(5) . . ? O1 Zr1 C20A 86.5(5) . . ? N1 Zr1 C20A 125.7(5) . . ? C16A Zr1 C20A 33.1(4) . . ? C14 Zr1 C20A 94.8(4) . . ? C13 Zr1 C20A 127.0(4) . . ? C18 Zr1 C20A 44.5(4) . . ? C11 Zr1 C20A 103.1(6) . . ? C3A Zr1 C15 109.4(4) . . ? C3 Zr1 C15 120.1(4) . . ? O1 Zr1 C15 102.53(13) . . ? N1 Zr1 C15 137.89(14) . . ? C16A Zr1 C15 79.7(4) . . ? C14 Zr1 C15 31.65(15) . . ? C13 Zr1 C15 52.81(16) . . ? C18 Zr1 C15 126.5(3) . . ? C11 Zr1 C15 31.67(18) . . ? C20A Zr1 C15 82.1(5) . . ? C3A Zr1 C17A 74.5(5) . . ? C3 Zr1 C17A 68.9(6) . . ? O1 Zr1 C17A 123.5(5) . . ? N1 Zr1 C17A 113.2(5) . . ? C16A Zr1 C17A 32.2(3) . . ? C14 Zr1 C17A 137.9(5) . . ? C13 Zr1 C17A 155.9(5) . . ? C18 Zr1 C17A 42.9(4) . . ? C11 Zr1 C17A 102.7(5) . . ? C20A Zr1 C17A 54.0(4) . . ? C15 Zr1 C17A 108.8(5) . . ? Zr1 C3 H3A 109.5 . . ? Zr1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Zr1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C17 C16 C20 108.1(10) . . ? C17 C16 Zr1 74.2(6) . . ? C20 C16 Zr1 73.7(6) . . ? C17 C16 H16 125.9 . . ? C20 C16 H16 125.9 . . ? Zr1 C16 H16 118.1 . . ? C18 C17 C16 109.5(10) . . ? C18 C17 Zr1 72.9(6) . . ? C16 C17 Zr1 73.7(6) . . ? C18 C17 H17 125.3 . . ? C16 C17 H17 125.3 . . ? Zr1 C17 H17 119.8 . . ? C17 C18 C19 105.5(9) . . ? C17 C18 Zr1 75.0(6) . . ? C19 C18 Zr1 74.2(6) . . ? C17 C18 H18 127.3 . . ? C19 C18 H18 127.3 . . ? Zr1 C18 H18 116.0 . . ? C20 C19 C18 110.6(10) . . ? C20 C19 Zr1 74.1(6) . . ? C18 C19 Zr1 73.3(5) . . ? C20 C19 H19 124.7 . . ? C18 C19 H19 124.7 . . ? Zr1 C19 H19 119.6 . . ? C19 C20 C16 106.2(10) . . ? C19 C20 Zr1 73.9(6) . . ? C16 C20 Zr1 74.0(6) . . ? C19 C20 H20 126.9 . . ? C16 C20 H20 126.9 . . ? Zr1 C20 H20 117.4 . . ? Zr1 C3A H3A1 109.5 . . ? Zr1 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? Zr1 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C17A C16A C20A 108.4(12) . . ? C17A C16A Zr1 75.0(7) . . ? C20A C16A Zr1 74.4(7) . . ? C17A C16A H16A 125.8 . . ? C20A C16A H16A 125.8 . . ? Zr1 C16A H16A 116.8 . . ? C16A C17A C18A 107.6(12) . . ? C16A C17A Zr1 72.8(7) . . ? C18A C17A Zr1 74.7(7) . . ? C16A C17A H17A 126.2 . . ? C18A C17A H17A 126.2 . . ? Zr1 C17A H17A 118.3 . . ? C19A C18A C17A 108.0(11) . . ? C19A C18A Zr1 74.7(7) . . ? C17A C18A Zr1 73.1(7) . . ? C19A C18A H18A 126.0 . . ? C17A C18A H18A 126.0 . . ? Zr1 C18A H18A 118.2 . . ? C20A C19A C18A 109.3(11) . . ? C20A C19A Zr1 72.6(7) . . ? C18A C19A Zr1 73.5(7) . . ? C20A C19A H19A 125.4 . . ? C18A C19A H19A 125.4 . . ? Zr1 C19A H19A 120.2 . . ? C19A C20A C16A 106.7(11) . . ? C19A C20A Zr1 75.7(7) . . ? C16A C20A Zr1 72.5(7) . . ? C19A C20A H20A 126.7 . . ? C16A C20A H20A 126.7 . . ? Zr1 C20A H20A 117.3 . . ? C31 P1 C1 107.05(17) . . ? C31 P1 C21 111.49(17) . . ? C1 P1 C21 119.78(17) . . ? C31 P1 C5 110.51(16) . . ? C1 P1 C5 107.49(16) . . ? C21 P1 C5 100.16(15) . . ? C5 O1 Zr1 94.2(2) . . ? C5 N1 C61 128.5(3) . . ? C5 N1 Zr1 92.9(2) . . ? C61 N1 Zr1 137.6(2) . . ? C2 C1 P1 115.2(2) . . ? C2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C1 C2 B1 111.2(3) . . ? C1 C2 H2A 109.4 . . ? B1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? B1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? B1 C4 H4A 109.5 . . ? B1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? B1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 N1 117.0(3) . . ? O1 C5 P1 119.0(2) . . ? N1 C5 P1 123.9(3) . . ? O1 C5 Zr1 58.36(17) . . ? N1 C5 Zr1 58.89(18) . . ? P1 C5 Zr1 172.56(17) . . ? C15 C11 C12 107.8(5) . . ? C15 C11 Zr1 74.3(3) . . ? C12 C11 Zr1 74.8(3) . . ? C15 C11 H11 126.1 . . ? C12 C11 H11 126.1 . . ? Zr1 C11 H11 116.9 . . ? C13 C12 C11 106.9(5) . . ? C13 C12 Zr1 72.5(3) . . ? C11 C12 Zr1 72.9(3) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? Zr1 C12 H12 119.9 . . ? C14 C13 C12 107.9(5) . . ? C14 C13 Zr1 73.6(3) . . ? C12 C13 Zr1 75.4(3) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? Zr1 C13 H13 117.0 . . ? C15 C14 C13 108.5(5) . . ? C15 C14 Zr1 75.2(3) . . ? C13 C14 Zr1 74.2(3) . . ? C15 C14 H14 125.8 . . ? C13 C14 H14 125.8 . . ? Zr1 C14 H14 116.8 . . ? C14 C15 C11 108.8(5) . . ? C14 C15 Zr1 73.2(3) . . ? C11 C15 Zr1 74.0(3) . . ? C14 C15 H15 125.6 . . ? C11 C15 H15 125.6 . . ? Zr1 C15 H15 119.0 . . ? C26 C21 C22 119.4(3) . . ? C26 C21 P1 123.2(3) . . ? C22 C21 P1 117.2(3) . . ? C23 C22 C21 118.7(3) . . ? C23 C22 C27 115.7(3) . . ? C21 C22 C27 125.4(3) . . ? C24 C23 C22 122.7(4) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 117.7(4) . . ? C23 C24 C28 120.4(4) . . ? C25 C24 C28 121.9(4) . . ? C24 C25 C26 123.4(4) . . ? C24 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C25 C26 C21 118.0(4) . . ? C25 C26 C29 116.8(4) . . ? C21 C26 C29 125.2(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 119.9(3) . . ? C32 C31 P1 118.9(3) . . ? C36 C31 P1 121.2(3) . . ? C33 C32 C31 118.5(4) . . ? C33 C32 C37 116.5(4) . . ? C31 C32 C37 124.7(4) . . ? C34 C33 C32 122.5(4) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C35 C34 C33 117.8(4) . . ? C35 C34 C38 121.2(5) . . ? C33 C34 C38 120.9(5) . . ? C34 C35 C36 123.2(4) . . ? C34 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C35 C36 C31 117.5(4) . . ? C35 C36 C39 117.5(4) . . ? C31 C36 C39 124.9(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C4 B1 C2 109.2(3) . . ? C4 B1 C51 106.0(3) . . ? C2 B1 C51 112.3(3) . . ? C4 B1 C41 115.2(3) . . ? C2 B1 C41 108.9(3) . . ? C51 B1 C41 105.2(3) . . ? C42 C41 C46 112.8(4) . . ? C42 C41 B1 126.7(4) . . ? C46 C41 B1 120.6(4) . . ? F42 C42 C43A 103.3(8) . . ? F42 C42 C41 120.7(4) . . ? C43A C42 C41 136.0(9) . . ? F42 C42 C43 123.3(8) . . ? C43A C42 C43 20.2(6) . . ? C41 C42 C43 116.0(8) . . ? F46 C46 C45 106.3(8) . . ? F46 C46 C41 119.5(4) . . ? C45 C46 C41 134.2(8) . . ? F46 C46 C45A 126.4(8) . . ? C45 C46 C45A 20.1(6) . . ? C41 C46 C45A 114.1(8) . . ? F43 C43 C44 117.8(9) . . ? F43 C43 C42 116.3(9) . . ? C44 C43 C42 125.9(9) . . ? F44 C44 C43 121.6(10) . . ? F44 C44 C45 118.1(10) . . ? C43 C44 C45 120.2(9) . . ? F45 C45 C44 123.3(9) . . ? F45 C45 C46 125.8(10) . . ? C44 C45 C46 110.9(9) . . ? F43A C43A C44A 123.1(11) . . ? F43A C43A C42 127.0(12) . . ? C44A C43A C42 109.9(10) . . ? F44A C44A C43A 118.4(11) . . ? F44A C44A C45A 121.8(11) . . ? C43A C44A C45A 119.7(10) . . ? F45A C45A C44A 117.5(11) . . ? F45A C45A C46 114.8(10) . . ? C44A C45A C46 127.5(11) . . ? C56 C51 C52 112.9(3) . . ? C56 C51 B1 127.2(3) . . ? C52 C51 B1 119.8(3) . . ? F52 C52 C51 119.9(3) . . ? F52 C52 C53 115.2(4) . . ? C51 C52 C53 124.9(4) . . ? F53 C53 C54 120.7(4) . . ? F53 C53 C52 120.9(5) . . ? C54 C53 C52 118.5(4) . . ? F54 C54 C55 120.2(5) . . ? F54 C54 C53 120.0(5) . . ? C55 C54 C53 119.8(4) . . ? F55 C55 C54 119.9(4) . . ? F55 C55 C56 120.6(4) . . ? C54 C55 C56 119.5(4) . . ? F56 C56 C55 114.5(4) . . ? F56 C56 C51 121.2(3) . . ? C55 C56 C51 124.3(4) . . ? C66 C61 C62 118.8(3) . . ? C66 C61 N1 120.4(3) . . ? C62 C61 N1 120.4(3) . . ? C63 C62 C61 120.4(4) . . ? C63 C62 H62 119.8 . . ? C61 C62 H62 119.8 . . ? C62 C63 C64 121.4(4) . . ? C62 C63 H63 119.3 . . ? C64 C63 H63 119.3 . . ? C65 C64 C63 117.6(3) . . ? C65 C64 C67 121.1(4) . . ? C63 C64 C67 121.3(4) . . ? C64 C65 C66 121.7(4) . . ? C64 C65 H65 119.2 . . ? C66 C65 H65 119.2 . . ? C61 C66 C65 120.1(4) . . ? C61 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? Cl2 C71 Cl1 114.3(6) . . ? Cl2 C71 H71A 108.7 . . ? Cl1 C71 H71A 108.7 . . ? Cl2 C71 H71B 108.7 . . ? Cl1 C71 H71B 108.7 . . ? H71A C71 H71B 107.6 . . ? Cl1A C71A Cl2A 96.3(13) . . ? Cl1A C71A H71C 112.5 . . ? Cl2A C71A H71C 112.5 . . ? Cl1A C71A H71D 112.5 . . ? Cl2A C71A H71D 112.5 . . ? H71C C71A H71D 110.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3A Zr1 C16 C17 -71.0(9) . . . . ? C3 Zr1 C16 C17 -60.0(9) . . . . ? O1 Zr1 C16 C17 77.8(11) . . . . ? N1 Zr1 C16 C17 3.4(13) . . . . ? C16A Zr1 C16 C17 131(5) . . . . ? C14 Zr1 C16 C17 164.1(9) . . . . ? C13 Zr1 C16 C17 -169.2(7) . . . . ? C18 Zr1 C16 C17 35.9(6) . . . . ? C11 Zr1 C16 C17 -148.8(10) . . . . ? C20A Zr1 C16 C17 95.7(10) . . . . ? C15 Zr1 C16 C17 179.5(10) . . . . ? C17A Zr1 C16 C17 -18.8(10) . . . . ? C3A Zr1 C16 C20 174.2(9) . . . . ? C3 Zr1 C16 C20 -174.8(9) . . . . ? O1 Zr1 C16 C20 -37.1(12) . . . . ? N1 Zr1 C16 C20 -111.4(11) . . . . ? C16A Zr1 C16 C20 16(4) . . . . ? C14 Zr1 C16 C20 49.3(10) . . . . ? C13 Zr1 C16 C20 76.0(10) . . . . ? C18 Zr1 C16 C20 -78.9(7) . . . . ? C11 Zr1 C16 C20 96.4(10) . . . . ? C20A Zr1 C16 C20 -19.1(7) . . . . ? C15 Zr1 C16 C20 64.7(10) . . . . ? C17A Zr1 C16 C20 -133.6(15) . . . . ? C20 C16 C17 C18 1.8(14) . . . . ? Zr1 C16 C17 C18 -64.7(8) . . . . ? C20 C16 C17 Zr1 66.4(8) . . . . ? C3A Zr1 C17 C18 -137.0(10) . . . . ? C3 Zr1 C17 C18 -128.2(9) . . . . ? O1 Zr1 C17 C18 -2.1(10) . . . . ? N1 Zr1 C17 C18 -60.7(9) . . . . ? C16A Zr1 C17 C18 107.1(10) . . . . ? C14 Zr1 C17 C18 92.2(12) . . . . ? C13 Zr1 C17 C18 152.0(14) . . . . ? C11 Zr1 C17 C18 151.4(9) . . . . ? C20A Zr1 C17 C18 63.3(7) . . . . ? C15 Zr1 C17 C18 116.4(9) . . . . ? C17A Zr1 C17 C18 162(3) . . . . ? C3A Zr1 C17 C16 106.1(10) . . . . ? C3 Zr1 C17 C16 114.8(10) . . . . ? O1 Zr1 C17 C16 -119.1(10) . . . . ? N1 Zr1 C17 C16 -177.6(9) . . . . ? C16A Zr1 C17 C16 -9.9(10) . . . . ? C14 Zr1 C17 C16 -24.8(14) . . . . ? C13 Zr1 C17 C16 35.1(19) . . . . ? C18 Zr1 C17 C16 -117.0(10) . . . . ? C11 Zr1 C17 C16 34.4(10) . . . . ? C20A Zr1 C17 C16 -53.7(8) . . . . ? C15 Zr1 C17 C16 -0.6(11) . . . . ? C17A Zr1 C17 C16 45(3) . . . . ? C16 C17 C18 C19 -3.4(13) . . . . ? Zr1 C17 C18 C19 -68.5(7) . . . . ? C16 C17 C18 Zr1 65.2(8) . . . . ? C3A Zr1 C18 C17 43.6(10) . . . . ? C3 Zr1 C18 C17 48.6(9) . . . . ? O1 Zr1 C18 C17 178.0(9) . . . . ? N1 Zr1 C18 C17 122.6(9) . . . . ? C16A Zr1 C18 C17 -45.6(8) . . . . ? C14 Zr1 C18 C17 -124.0(9) . . . . ? C13 Zr1 C18 C17 -163.3(8) . . . . ? C11 Zr1 C18 C17 -43.2(13) . . . . ? C20A Zr1 C18 C17 -87.4(9) . . . . ? C15 Zr1 C18 C17 -83.2(11) . . . . ? C17A Zr1 C18 C17 -5.2(10) . . . . ? C3A Zr1 C18 C19 154.9(10) . . . . ? C3 Zr1 C18 C19 159.8(9) . . . . ? O1 Zr1 C18 C19 -70.7(9) . . . . ? N1 Zr1 C18 C19 -126.1(9) . . . . ? C16A Zr1 C18 C19 65.7(8) . . . . ? C14 Zr1 C18 C19 -12.7(11) . . . . ? C13 Zr1 C18 C19 -52.0(11) . . . . ? C11 Zr1 C18 C19 68.0(14) . . . . ? C20A Zr1 C18 C19 23.8(7) . . . . ? C15 Zr1 C18 C19 28.0(12) . . . . ? C17A Zr1 C18 C19 106.0(10) . . . . ? C17 C18 C19 C20 3.8(13) . . . . ? Zr1 C18 C19 C20 -65.3(8) . . . . ? C17 C18 C19 Zr1 69.1(7) . . . . ? C3A Zr1 C19 C20 84.2(12) . . . . ? C3 Zr1 C19 C20 93.5(10) . . . . ? O1 Zr1 C19 C20 -140.7(10) . . . . ? N1 Zr1 C19 C20 175.4(8) . . . . ? C16A Zr1 C19 C20 29.9(9) . . . . ? C14 Zr1 C19 C20 -71.5(9) . . . . ? C13 Zr1 C19 C20 -84.8(8) . . . . ? C18 Zr1 C19 C20 117.9(10) . . . . ? C11 Zr1 C19 C20 -18.1(10) . . . . ? C20A Zr1 C19 C20 -1.0(14) . . . . ? C15 Zr1 C19 C20 -39.8(9) . . . . ? C17A Zr1 C19 C20 68.1(8) . . . . ? C3A Zr1 C19 C18 -33.7(13) . . . . ? C3 Zr1 C19 C18 -24.4(11) . . . . ? O1 Zr1 C19 C18 101.4(10) . . . . ? N1 Zr1 C19 C18 57.5(9) . . . . ? C16A Zr1 C19 C18 -88.0(9) . . . . ? C14 Zr1 C19 C18 170.6(9) . . . . ? C13 Zr1 C19 C18 157.4(6) . . . . ? C11 Zr1 C19 C18 -136.0(9) . . . . ? C20A Zr1 C19 C18 -118.9(16) . . . . ? C15 Zr1 C19 C18 -157.6(9) . . . . ? C17A Zr1 C19 C18 -49.8(7) . . . . ? C18 C19 C20 C16 -2.8(13) . . . . ? Zr1 C19 C20 C16 -67.5(8) . . . . ? C18 C19 C20 Zr1 64.7(8) . . . . ? C17 C16 C20 C19 0.6(13) . . . . ? Zr1 C16 C20 C19 67.4(8) . . . . ? C17 C16 C20 Zr1 -66.8(8) . . . . ? C3A Zr1 C20 C19 -119.4(9) . . . . ? C3 Zr1 C20 C19 -106.6(9) . . . . ? O1 Zr1 C20 C19 37.3(9) . . . . ? N1 Zr1 C20 C19 -6.7(12) . . . . ? C16A Zr1 C20 C19 -117.7(15) . . . . ? C14 Zr1 C20 C19 111.7(9) . . . . ? C13 Zr1 C20 C19 118.8(7) . . . . ? C18 Zr1 C20 C19 -35.8(6) . . . . ? C11 Zr1 C20 C19 164.6(9) . . . . ? C20A Zr1 C20 C19 1(2) . . . . ? C15 Zr1 C20 C19 138.2(10) . . . . ? C17A Zr1 C20 C19 -89.8(8) . . . . ? C3A Zr1 C20 C16 -6.8(11) . . . . ? C3 Zr1 C20 C16 6.0(11) . . . . ? O1 Zr1 C20 C16 149.9(10) . . . . ? N1 Zr1 C20 C16 106.0(11) . . . . ? C16A Zr1 C20 C16 -5.1(14) . . . . ? C14 Zr1 C20 C16 -135.6(10) . . . . ? C13 Zr1 C20 C16 -128.5(8) . . . . ? C18 Zr1 C20 C16 76.9(7) . . . . ? C11 Zr1 C20 C16 -82.8(10) . . . . ? C20A Zr1 C20 C16 114(2) . . . . ? C15 Zr1 C20 C16 -109.2(11) . . . . ? C17A Zr1 C20 C16 22.8(8) . . . . ? C3A Zr1 C16A C17A -45.7(11) . . . . ? C3 Zr1 C16A C17A -34.6(11) . . . . ? O1 Zr1 C16A C17A 107.0(12) . . . . ? N1 Zr1 C16A C17A 36.5(16) . . . . ? C14 Zr1 C16A C17A -172.0(11) . . . . ? C13 Zr1 C16A C17A -150.3(9) . . . . ? C18 Zr1 C16A C17A 55.7(8) . . . . ? C11 Zr1 C16A C17A -122.8(12) . . . . ? C20A Zr1 C16A C17A 114.4(13) . . . . ? C15 Zr1 C16A C17A -154.3(12) . . . . ? C3A Zr1 C16A C20A -160.1(11) . . . . ? C3 Zr1 C16A C20A -149.0(10) . . . . ? O1 Zr1 C16A C20A -7.4(13) . . . . ? N1 Zr1 C16A C20A -77.9(15) . . . . ? C14 Zr1 C16A C20A 73.6(11) . . . . ? C13 Zr1 C16A C20A 95.3(10) . . . . ? C18 Zr1 C16A C20A -58.8(8) . . . . ? C11 Zr1 C16A C20A 122.7(12) . . . . ? C15 Zr1 C16A C20A 91.3(12) . . . . ? C17A Zr1 C16A C20A -114.4(13) . . . . ? C20A C16A C17A C18A 0.3(16) . . . . ? Zr1 C16A C17A C18A -67.2(10) . . . . ? C20A C16A C17A Zr1 67.5(9) . . . . ? C3A Zr1 C17A C16A 132.5(12) . . . . ? C3 Zr1 C17A C16A 142.7(13) . . . . ? O1 Zr1 C17A C16A -93.2(13) . . . . ? N1 Zr1 C17A C16A -156.2(11) . . . . ? C14 Zr1 C17A C16A 11.5(16) . . . . ? C13 Zr1 C17A C16A 63.5(15) . . . . ? C18 Zr1 C17A C16A -97.0(11) . . . . ? C11 Zr1 C17A C16A 59.1(12) . . . . ? C20A Zr1 C17A C16A -38.0(8) . . . . ? C15 Zr1 C17A C16A 26.8(13) . . . . ? C3A Zr1 C17A C18A -113.1(11) . . . . ? C3 Zr1 C17A C18A -102.9(12) . . . . ? O1 Zr1 C17A C18A 21.2(13) . . . . ? N1 Zr1 C17A C18A -41.8(11) . . . . ? C16A Zr1 C17A C18A 114.4(13) . . . . ? C14 Zr1 C17A C18A 125.9(12) . . . . ? C13 Zr1 C17A C18A 177.9(9) . . . . ? C18 Zr1 C17A C18A 17.4(7) . . . . ? C11 Zr1 C17A C18A 173.5(11) . . . . ? C20A Zr1 C17A C18A 76.4(8) . . . . ? C15 Zr1 C17A C18A 141.2(11) . . . . ? C16A C17A C18A C19A -1.2(16) . . . . ? Zr1 C17A C18A C19A -67.1(10) . . . . ? C16A C17A C18A Zr1 65.9(10) . . . . ? C3A Zr1 C18A C19A 177.2(11) . . . . ? C3 Zr1 C18A C19A -177.3(11) . . . . ? O1 Zr1 C18A C19A -47.6(11) . . . . ? N1 Zr1 C18A C19A -103.0(11) . . . . ? C16A Zr1 C18A C19A 77.4(8) . . . . ? C14 Zr1 C18A C19A 18.2(17) . . . . ? C13 Zr1 C18A C19A -59(3) . . . . ? C18 Zr1 C18A C19A -13.3(15) . . . . ? C11 Zr1 C18A C19A 105.9(14) . . . . ? C20A Zr1 C18A C19A 35.7(7) . . . . ? C15 Zr1 C18A C19A 62.1(15) . . . . ? C17A Zr1 C18A C19A 114.8(12) . . . . ? C3A Zr1 C18A C17A 62.4(11) . . . . ? C3 Zr1 C18A C17A 68.0(11) . . . . ? O1 Zr1 C18A C17A -162.4(10) . . . . ? N1 Zr1 C18A C17A 142.2(11) . . . . ? C16A Zr1 C18A C17A -37.3(7) . . . . ? C14 Zr1 C18A C17A -96.6(15) . . . . ? C13 Zr1 C18A C17A -174(2) . . . . ? C18 Zr1 C18A C17A -128(2) . . . . ? C11 Zr1 C18A C17A -8.9(15) . . . . ? C20A Zr1 C18A C17A -79.0(9) . . . . ? C15 Zr1 C18A C17A -52.6(14) . . . . ? C17A C18A C19A C20A 1.7(17) . . . . ? Zr1 C18A C19A C20A -64.4(10) . . . . ? C17A C18A C19A Zr1 66.0(10) . . . . ? C3A Zr1 C19A C20A 113.7(12) . . . . ? C3 Zr1 C19A C20A 119.8(12) . . . . ? O1 Zr1 C19A C20A -114.0(12) . . . . ? N1 Zr1 C19A C20A -165.2(11) . . . . ? C16A Zr1 C19A C20A 39.0(7) . . . . ? C14 Zr1 C19A C20A -52.1(11) . . . . ? C13 Zr1 C19A C20A -74.8(10) . . . . ? C18 Zr1 C19A C20A 128.3(17) . . . . ? C11 Zr1 C19A C20A 10.3(15) . . . . ? C15 Zr1 C19A C20A -17.5(12) . . . . ? C17A Zr1 C19A C20A 79.7(8) . . . . ? C3A Zr1 C19A C18A -3.3(13) . . . . ? C3 Zr1 C19A C18A 2.9(12) . . . . ? O1 Zr1 C19A C18A 129.1(12) . . . . ? N1 Zr1 C19A C18A 77.9(11) . . . . ? C16A Zr1 C19A C18A -77.9(9) . . . . ? C14 Zr1 C19A C18A -169.0(10) . . . . ? C13 Zr1 C19A C18A 168.3(7) . . . . ? C18 Zr1 C19A C18A 11.4(12) . . . . ? C11 Zr1 C19A C18A -106.6(14) . . . . ? C20A Zr1 C19A C18A -116.9(12) . . . . ? C15 Zr1 C19A C18A -134.5(11) . . . . ? C17A Zr1 C19A C18A -37.3(7) . . . . ? C18A C19A C20A C16A -1.4(16) . . . . ? Zr1 C19A C20A C16A -66.4(9) . . . . ? C18A C19A C20A Zr1 64.9(10) . . . . ? C17A C16A C20A C19A 0.7(16) . . . . ? Zr1 C16A C20A C19A 68.6(9) . . . . ? C17A C16A C20A Zr1 -67.9(10) . . . . ? C3A Zr1 C20A C19A -87.8(13) . . . . ? C3 Zr1 C20A C19A -75.4(13) . . . . ? O1 Zr1 C20A C19A 60.5(11) . . . . ? N1 Zr1 C20A C19A 18.3(12) . . . . ? C16A Zr1 C20A C19A -113.0(12) . . . . ? C14 Zr1 C20A C19A 134.6(11) . . . . ? C13 Zr1 C20A C19A 133.9(9) . . . . ? C18 Zr1 C20A C19A -19.7(7) . . . . ? C11 Zr1 C20A C19A -172.5(11) . . . . ? C15 Zr1 C20A C19A 163.7(12) . . . . ? C17A Zr1 C20A C19A -76.1(8) . . . . ? C3A Zr1 C20A C16A 25.2(14) . . . . ? C3 Zr1 C20A C16A 37.6(13) . . . . ? O1 Zr1 C20A C16A 173.5(11) . . . . ? N1 Zr1 C20A C16A 131.4(11) . . . . ? C14 Zr1 C20A C16A -112.4(11) . . . . ? C13 Zr1 C20A C16A -113.0(9) . . . . ? C18 Zr1 C20A C16A 93.3(10) . . . . ? C11 Zr1 C20A C16A -59.4(11) . . . . ? C15 Zr1 C20A C16A -83.3(11) . . . . ? C17A Zr1 C20A C16A 36.9(7) . . . . ? C3A Zr1 O1 C5 2.1(6) . . . . ? C3 Zr1 O1 C5 -10.9(5) . . . . ? N1 Zr1 O1 C5 -3.16(19) . . . . ? C16A Zr1 O1 C5 -137.7(5) . . . . ? C14 Zr1 O1 C5 122.2(2) . . . . ? C13 Zr1 O1 C5 89.5(2) . . . . ? C18 Zr1 O1 C5 -97.4(4) . . . . ? C11 Zr1 O1 C5 114.5(3) . . . . ? C20A Zr1 O1 C5 -141.8(5) . . . . ? C15 Zr1 O1 C5 137.1(2) . . . . ? C17A Zr1 O1 C5 -100.0(5) . . . . ? C3A Zr1 N1 C5 -173.2(5) . . . . ? C3 Zr1 N1 C5 176.9(4) . . . . ? O1 Zr1 N1 C5 3.07(19) . . . . ? C16A Zr1 N1 C5 98.6(8) . . . . ? C14 Zr1 N1 C5 -52.6(2) . . . . ? C13 Zr1 N1 C5 -76.4(2) . . . . ? C18 Zr1 N1 C5 83.0(5) . . . . ? C11 Zr1 N1 C5 -108.8(3) . . . . ? C20A Zr1 N1 C5 57.4(5) . . . . ? C15 Zr1 N1 C5 -65.5(3) . . . . ? C17A Zr1 N1 C5 118.8(5) . . . . ? C3A Zr1 N1 C61 -5.0(5) . . . . ? C3 Zr1 N1 C61 -14.9(5) . . . . ? O1 Zr1 N1 C61 171.3(4) . . . . ? C16A Zr1 N1 C61 -93.2(8) . . . . ? C14 Zr1 N1 C61 115.6(4) . . . . ? C13 Zr1 N1 C61 91.8(4) . . . . ? C18 Zr1 N1 C61 -108.8(6) . . . . ? C11 Zr1 N1 C61 59.4(4) . . . . ? C20A Zr1 N1 C61 -134.4(5) . . . . ? C15 Zr1 N1 C61 102.7(4) . . . . ? C17A Zr1 N1 C61 -73.0(6) . . . . ? C31 P1 C1 C2 39.9(3) . . . . ? C21 P1 C1 C2 -88.2(3) . . . . ? C5 P1 C1 C2 158.6(3) . . . . ? P1 C1 C2 B1 -173.4(3) . . . . ? Zr1 O1 C5 N1 5.3(3) . . . . ? Zr1 O1 C5 P1 -171.92(19) . . . . ? C61 N1 C5 O1 -175.1(3) . . . . ? Zr1 N1 C5 O1 -5.3(3) . . . . ? C61 N1 C5 P1 1.9(5) . . . . ? Zr1 N1 C5 P1 171.8(2) . . . . ? C61 N1 C5 Zr1 -169.9(4) . . . . ? C31 P1 C5 O1 -19.2(3) . . . . ? C1 P1 C5 O1 -135.7(3) . . . . ? C21 P1 C5 O1 98.4(3) . . . . ? C31 P1 C5 N1 163.8(3) . . . . ? C1 P1 C5 N1 47.3(3) . . . . ? C21 P1 C5 N1 -78.6(3) . . . . ? C31 P1 C5 Zr1 -86.7(13) . . . . ? C1 P1 C5 Zr1 156.8(13) . . . . ? C21 P1 C5 Zr1 30.9(14) . . . . ? C3A Zr1 C5 O1 -178.5(5) . . . . ? C3 Zr1 C5 O1 171.4(4) . . . . ? N1 Zr1 C5 O1 174.5(3) . . . . ? C16A Zr1 C5 O1 59.4(7) . . . . ? C14 Zr1 C5 O1 -54.6(2) . . . . ? C13 Zr1 C5 O1 -85.4(2) . . . . ? C18 Zr1 C5 O1 79.2(5) . . . . ? C11 Zr1 C5 O1 -88.6(3) . . . . ? C20A Zr1 C5 O1 40.5(4) . . . . ? C15 Zr1 C5 O1 -51.2(3) . . . . ? C17A Zr1 C5 O1 98.6(5) . . . . ? C3A Zr1 C5 N1 7.0(5) . . . . ? C3 Zr1 C5 N1 -3.1(4) . . . . ? O1 Zr1 C5 N1 -174.5(3) . . . . ? C16A Zr1 C5 N1 -115.1(7) . . . . ? C14 Zr1 C5 N1 130.9(2) . . . . ? C13 Zr1 C5 N1 100.1(2) . . . . ? C18 Zr1 C5 N1 -95.3(5) . . . . ? C11 Zr1 C5 N1 96.9(3) . . . . ? C20A Zr1 C5 N1 -134.0(4) . . . . ? C15 Zr1 C5 N1 134.3(2) . . . . ? C17A Zr1 C5 N1 -75.9(5) . . . . ? C3A Zr1 C5 P1 -106.9(14) . . . . ? C3 Zr1 C5 P1 -117.0(14) . . . . ? O1 Zr1 C5 P1 71.6(13) . . . . ? N1 Zr1 C5 P1 -113.9(14) . . . . ? C16A Zr1 C5 P1 131.0(15) . . . . ? C14 Zr1 C5 P1 17.0(13) . . . . ? C13 Zr1 C5 P1 -13.8(13) . . . . ? C18 Zr1 C5 P1 150.8(14) . . . . ? C11 Zr1 C5 P1 -17.0(14) . . . . ? C20A Zr1 C5 P1 112.1(14) . . . . ? C15 Zr1 C5 P1 20.4(14) . . . . ? C17A Zr1 C5 P1 170.2(14) . . . . ? C3A Zr1 C11 C15 -176.1(6) . . . . ? C3 Zr1 C11 C15 -173.3(5) . . . . ? O1 Zr1 C11 C15 45.7(4) . . . . ? N1 Zr1 C11 C15 118.7(3) . . . . ? C16A Zr1 C11 C15 -78.0(6) . . . . ? C14 Zr1 C11 C15 36.3(3) . . . . ? C13 Zr1 C11 C15 76.9(3) . . . . ? C18 Zr1 C11 C15 -79.9(8) . . . . ? C20A Zr1 C11 C15 -49.8(5) . . . . ? C17A Zr1 C11 C15 -105.3(5) . . . . ? C3A Zr1 C11 C12 69.9(6) . . . . ? C3 Zr1 C11 C12 72.7(5) . . . . ? O1 Zr1 C11 C12 -68.3(4) . . . . ? N1 Zr1 C11 C12 4.8(4) . . . . ? C16A Zr1 C11 C12 168.1(6) . . . . ? C14 Zr1 C11 C12 -77.7(3) . . . . ? C13 Zr1 C11 C12 -37.1(3) . . . . ? C18 Zr1 C11 C12 166.1(7) . . . . ? C20A Zr1 C11 C12 -163.8(5) . . . . ? C15 Zr1 C11 C12 -114.0(5) . . . . ? C17A Zr1 C11 C12 140.7(5) . . . . ? C15 C11 C12 C13 -2.5(6) . . . . ? Zr1 C11 C12 C13 65.1(3) . . . . ? C15 C11 C12 Zr1 -67.6(4) . . . . ? C3A Zr1 C12 C13 144.9(6) . . . . ? C3 Zr1 C12 C13 141.4(5) . . . . ? O1 Zr1 C12 C13 13.0(4) . . . . ? N1 Zr1 C12 C13 69.1(3) . . . . ? C16A Zr1 C12 C13 -127.9(6) . . . . ? C14 Zr1 C12 C13 -37.5(3) . . . . ? C18 Zr1 C12 C13 -167.7(19) . . . . ? C11 Zr1 C12 C13 -114.6(5) . . . . ? C20A Zr1 C12 C13 -92.4(6) . . . . ? C15 Zr1 C12 C13 -77.5(3) . . . . ? C17A Zr1 C12 C13 -164.4(6) . . . . ? C3A Zr1 C12 C11 -100.5(6) . . . . ? C3 Zr1 C12 C11 -104.1(5) . . . . ? O1 Zr1 C12 C11 127.5(3) . . . . ? N1 Zr1 C12 C11 -176.3(3) . . . . ? C16A Zr1 C12 C11 -13.4(7) . . . . ? C14 Zr1 C12 C11 77.1(4) . . . . ? C13 Zr1 C12 C11 114.6(5) . . . . ? C18 Zr1 C12 C11 -53(2) . . . . ? C20A Zr1 C12 C11 22.1(7) . . . . ? C15 Zr1 C12 C11 37.1(3) . . . . ? C17A Zr1 C12 C11 -49.9(6) . . . . ? C11 C12 C13 C14 1.6(6) . . . . ? Zr1 C12 C13 C14 67.0(3) . . . . ? C11 C12 C13 Zr1 -65.3(4) . . . . ? C3A Zr1 C13 C14 -146.8(5) . . . . ? C3 Zr1 C13 C14 -153.5(5) . . . . ? O1 Zr1 C13 C14 78.3(3) . . . . ? N1 Zr1 C13 C14 134.0(3) . . . . ? C16A Zr1 C13 C14 -41.7(7) . . . . ? C18 Zr1 C13 C14 59.5(9) . . . . ? C11 Zr1 C13 C14 -76.7(3) . . . . ? C20A Zr1 C13 C14 1.2(7) . . . . ? C15 Zr1 C13 C14 -36.8(3) . . . . ? C17A Zr1 C13 C14 -82.0(10) . . . . ? C3A Zr1 C13 C12 -32.7(5) . . . . ? C3 Zr1 C13 C12 -39.5(5) . . . . ? O1 Zr1 C13 C12 -167.6(3) . . . . ? N1 Zr1 C13 C12 -111.9(3) . . . . ? C16A Zr1 C13 C12 72.3(7) . . . . ? C14 Zr1 C13 C12 114.1(4) . . . . ? C18 Zr1 C13 C12 173.6(8) . . . . ? C11 Zr1 C13 C12 37.3(3) . . . . ? C20A Zr1 C13 C12 115.3(7) . . . . ? C15 Zr1 C13 C12 77.3(4) . . . . ? C17A Zr1 C13 C12 32.1(10) . . . . ? C12 C13 C14 C15 -0.2(5) . . . . ? Zr1 C13 C14 C15 68.0(3) . . . . ? C12 C13 C14 Zr1 -68.2(3) . . . . ? C3A Zr1 C14 C15 -74.5(6) . . . . ? C3 Zr1 C14 C15 -78.6(6) . . . . ? O1 Zr1 C14 C15 151.5(3) . . . . ? N1 Zr1 C14 C15 -163.5(3) . . . . ? C16A Zr1 C14 C15 34.7(5) . . . . ? C13 Zr1 C14 C15 -114.5(4) . . . . ? C18 Zr1 C14 C15 91.2(5) . . . . ? C11 Zr1 C14 C15 -36.3(3) . . . . ? C20A Zr1 C14 C15 66.5(6) . . . . ? C17A Zr1 C14 C15 28.3(7) . . . . ? C3A Zr1 C14 C13 40.0(6) . . . . ? C3 Zr1 C14 C13 35.9(6) . . . . ? O1 Zr1 C14 C13 -94.0(3) . . . . ? N1 Zr1 C14 C13 -49.0(3) . . . . ? C16A Zr1 C14 C13 149.2(5) . . . . ? C18 Zr1 C14 C13 -154.3(4) . . . . ? C11 Zr1 C14 C13 78.2(3) . . . . ? C20A Zr1 C14 C13 -179.0(6) . . . . ? C15 Zr1 C14 C13 114.5(4) . . . . ? C17A Zr1 C14 C13 142.9(7) . . . . ? C13 C14 C15 C11 -1.4(6) . . . . ? Zr1 C14 C15 C11 66.0(4) . . . . ? C13 C14 C15 Zr1 -67.4(3) . . . . ? C12 C11 C15 C14 2.4(6) . . . . ? Zr1 C11 C15 C14 -65.4(4) . . . . ? C12 C11 C15 Zr1 67.9(4) . . . . ? C3A Zr1 C15 C14 120.0(6) . . . . ? C3 Zr1 C15 C14 123.7(5) . . . . ? O1 Zr1 C15 C14 -28.1(3) . . . . ? N1 Zr1 C15 C14 23.8(4) . . . . ? C16A Zr1 C15 C14 -146.2(6) . . . . ? C13 Zr1 C15 C14 37.5(3) . . . . ? C18 Zr1 C15 C14 -115.7(6) . . . . ? C11 Zr1 C15 C14 116.0(5) . . . . ? C20A Zr1 C15 C14 -112.7(5) . . . . ? C17A Zr1 C15 C14 -160.4(5) . . . . ? C3A Zr1 C15 C11 4.1(6) . . . . ? C3 Zr1 C15 C11 7.7(6) . . . . ? O1 Zr1 C15 C11 -144.1(3) . . . . ? N1 Zr1 C15 C11 -92.2(4) . . . . ? C16A Zr1 C15 C11 97.8(6) . . . . ? C14 Zr1 C15 C11 -116.0(5) . . . . ? C13 Zr1 C15 C11 -78.5(4) . . . . ? C18 Zr1 C15 C11 128.4(6) . . . . ? C20A Zr1 C15 C11 131.3(5) . . . . ? C17A Zr1 C15 C11 83.7(5) . . . . ? C31 P1 C21 C26 -127.2(3) . . . . ? C1 P1 C21 C26 -1.2(4) . . . . ? C5 P1 C21 C26 115.9(3) . . . . ? C31 P1 C21 C22 56.1(3) . . . . ? C1 P1 C21 C22 -177.9(3) . . . . ? C5 P1 C21 C22 -60.8(3) . . . . ? C26 C21 C22 C23 -4.2(5) . . . . ? P1 C21 C22 C23 172.6(3) . . . . ? C26 C21 C22 C27 170.5(3) . . . . ? P1 C21 C22 C27 -12.7(5) . . . . ? C21 C22 C23 C24 4.1(6) . . . . ? C27 C22 C23 C24 -171.1(4) . . . . ? C22 C23 C24 C25 -1.8(6) . . . . ? C22 C23 C24 C28 177.0(4) . . . . ? C23 C24 C25 C26 -0.5(6) . . . . ? C28 C24 C25 C26 -179.3(4) . . . . ? C24 C25 C26 C21 0.2(6) . . . . ? C24 C25 C26 C29 179.2(4) . . . . ? C22 C21 C26 C25 2.1(5) . . . . ? P1 C21 C26 C25 -174.5(3) . . . . ? C22 C21 C26 C29 -176.8(4) . . . . ? P1 C21 C26 C29 6.6(6) . . . . ? C1 P1 C31 C32 74.9(3) . . . . ? C21 P1 C31 C32 -152.4(3) . . . . ? C5 P1 C31 C32 -41.9(3) . . . . ? C1 P1 C31 C36 -103.9(3) . . . . ? C21 P1 C31 C36 28.8(3) . . . . ? C5 P1 C31 C36 139.3(3) . . . . ? C36 C31 C32 C33 -8.1(5) . . . . ? P1 C31 C32 C33 173.1(3) . . . . ? C36 C31 C32 C37 165.3(4) . . . . ? P1 C31 C32 C37 -13.5(5) . . . . ? C31 C32 C33 C34 1.5(6) . . . . ? C37 C32 C33 C34 -172.5(4) . . . . ? C32 C33 C34 C35 4.9(6) . . . . ? C32 C33 C34 C38 -179.3(4) . . . . ? C33 C34 C35 C36 -4.9(6) . . . . ? C38 C34 C35 C36 179.3(4) . . . . ? C34 C35 C36 C31 -1.6(6) . . . . ? C34 C35 C36 C39 175.3(4) . . . . ? C32 C31 C36 C35 8.1(5) . . . . ? P1 C31 C36 C35 -173.2(3) . . . . ? C32 C31 C36 C39 -168.5(4) . . . . ? P1 C31 C36 C39 10.2(5) . . . . ? C1 C2 B1 C4 66.1(4) . . . . ? C1 C2 B1 C51 -176.6(3) . . . . ? C1 C2 B1 C41 -60.5(4) . . . . ? C4 B1 C41 C42 -4.3(5) . . . . ? C2 B1 C41 C42 118.9(4) . . . . ? C51 B1 C41 C42 -120.6(4) . . . . ? C4 B1 C41 C46 174.7(3) . . . . ? C2 B1 C41 C46 -62.1(4) . . . . ? C51 B1 C41 C46 58.4(4) . . . . ? C46 C41 C42 F42 -179.3(4) . . . . ? B1 C41 C42 F42 -0.3(6) . . . . ? C46 C41 C42 C43A -2.9(16) . . . . ? B1 C41 C42 C43A 176.1(15) . . . . ? C46 C41 C42 C43 0.6(10) . . . . ? B1 C41 C42 C43 179.7(9) . . . . ? C42 C41 C46 F46 177.9(3) . . . . ? B1 C41 C46 F46 -1.3(5) . . . . ? C42 C41 C46 C45 -0.4(11) . . . . ? B1 C41 C46 C45 -179.5(10) . . . . ? C42 C41 C46 C45A 0.2(11) . . . . ? B1 C41 C46 C45A -178.9(10) . . . . ? F42 C42 C43 F43 -0.4(19) . . . . ? C43A C42 C43 F43 -7(4) . . . . ? C41 C42 C43 F43 179.7(11) . . . . ? F42 C42 C43 C44 -178.8(13) . . . . ? C43A C42 C43 C44 174(6) . . . . ? C41 C42 C43 C44 1(2) . . . . ? F43 C43 C44 F44 2(3) . . . . ? C42 C43 C44 F44 179.9(13) . . . . ? F43 C43 C44 C45 178.0(16) . . . . ? C42 C43 C44 C45 -4(3) . . . . ? F44 C44 C45 F45 0(3) . . . . ? C43 C44 C45 F45 -177.1(16) . . . . ? F44 C44 C45 C46 180.0(12) . . . . ? C43 C44 C45 C46 3(2) . . . . ? F46 C46 C45 F45 0.4(18) . . . . ? C41 C46 C45 F45 178.8(10) . . . . ? C45A C46 C45 F45 177(6) . . . . ? F46 C46 C45 C44 179.9(11) . . . . ? C41 C46 C45 C44 -1.7(19) . . . . ? C45A C46 C45 C44 -3(3) . . . . ? F42 C42 C43A F43A 0(2) . . . . ? C41 C42 C43A F43A -176.5(13) . . . . ? C43 C42 C43A F43A 174(7) . . . . ? F42 C42 C43A C44A 178.5(15) . . . . ? C41 C42 C43A C44A 2(3) . . . . ? C43 C42 C43A C44A -8(3) . . . . ? F43A C43A C44A F44A -4(3) . . . . ? C42 C43A C44A F44A 177.6(15) . . . . ? F43A C43A C44A C45A -180(2) . . . . ? C42 C43A C44A C45A 2(3) . . . . ? F44A C44A C45A F45A 5(3) . . . . ? C43A C44A C45A F45A -179.9(19) . . . . ? F44A C44A C45A C46 179.9(16) . . . . ? C43A C44A C45A C46 -5(3) . . . . ? F46 C46 C45A F45A 1(2) . . . . ? C45 C46 C45A F45A -3(3) . . . . ? C41 C46 C45A F45A 178.5(12) . . . . ? F46 C46 C45A C44A -174.1(16) . . . . ? C45 C46 C45A C44A -178(6) . . . . ? C41 C46 C45A C44A 3(2) . . . . ? C4 B1 C51 C56 109.2(4) . . . . ? C2 B1 C51 C56 -10.0(5) . . . . ? C41 B1 C51 C56 -128.3(4) . . . . ? C4 B1 C51 C52 -66.8(4) . . . . ? C2 B1 C51 C52 174.0(3) . . . . ? C41 B1 C51 C52 55.7(4) . . . . ? C56 C51 C52 F52 179.9(4) . . . . ? B1 C51 C52 F52 -3.6(6) . . . . ? C56 C51 C52 C53 -1.1(6) . . . . ? B1 C51 C52 C53 175.5(4) . . . . ? F52 C52 C53 F53 -2.2(6) . . . . ? C51 C52 C53 F53 178.7(4) . . . . ? F52 C52 C53 C54 178.0(4) . . . . ? C51 C52 C53 C54 -1.1(7) . . . . ? F53 C53 C54 F54 2.9(7) . . . . ? C52 C53 C54 F54 -177.2(4) . . . . ? F53 C53 C54 C55 -178.4(4) . . . . ? C52 C53 C54 C55 1.4(7) . . . . ? F54 C54 C55 F55 -1.3(6) . . . . ? C53 C54 C55 F55 -180.0(4) . . . . ? F54 C54 C55 C56 179.1(4) . . . . ? C53 C54 C55 C56 0.5(7) . . . . ? F55 C55 C56 F56 -2.3(6) . . . . ? C54 C55 C56 F56 177.3(4) . . . . ? F55 C55 C56 C51 177.5(4) . . . . ? C54 C55 C56 C51 -2.9(7) . . . . ? C52 C51 C56 F56 -177.2(3) . . . . ? B1 C51 C56 F56 6.6(6) . . . . ? C52 C51 C56 C55 3.1(6) . . . . ? B1 C51 C56 C55 -173.1(4) . . . . ? C5 N1 C61 C66 -100.8(5) . . . . ? Zr1 N1 C61 C66 94.3(4) . . . . ? C5 N1 C61 C62 86.3(5) . . . . ? Zr1 N1 C61 C62 -78.5(5) . . . . ? C66 C61 C62 C63 1.9(6) . . . . ? N1 C61 C62 C63 174.9(4) . . . . ? C61 C62 C63 C64 -0.1(7) . . . . ? C62 C63 C64 C65 -1.0(6) . . . . ? C62 C63 C64 C67 179.8(4) . . . . ? C63 C64 C65 C66 0.2(6) . . . . ? C67 C64 C65 C66 179.4(4) . . . . ? C62 C61 C66 C65 -2.7(6) . . . . ? N1 C61 C66 C65 -175.7(3) . . . . ? C64 C65 C66 C61 1.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.746 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.058 #============================================================================= # end of cif data for "erk7011" (compound 8a) #============================================================================= #============================================================================= # end of cif file #============================================================================= _database_code_depnum_ccdc_archive 'CCDC 950035'