# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Jean-Cyrille HIERSO' _publ_contact_author_email JEAN-CYRILLE.HIERSO@U-BOURGOGNE.FR _publ_section_title ; Selective formation of a unique diphosphonium-diphosphine from a tetraphosphine double protonation induced by zirconium salts ; loop_ _publ_author_name 'Jean-Cyrille Hierso' 'Helene Cattey' 'Ali Jahel' 'Philippe Meunier' 'Nadine Pirio' 'Philippe Richard' ; N.V.Vologdin ; # Attachment 'CifPubli_HIERSO.cif' data_ali1gr _database_code_depnum_ccdc_archive 'CCDC 685282' _symmetry_space_group_name_hall '-P 1' _audit_update_record ; 2008-04-07 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H64 Fe P4, 2(C4 H8 Cl5 O Zr), 2(C H2 Cl2)' _chemical_formula_sum 'C76 H84 Cl14 Fe O2 P4 Zr2' _chemical_formula_weight 1887.90 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.302(5) _cell_length_b 18.324(5) _cell_length_c 19.112(5) _cell_angle_alpha 75.800(5) _cell_angle_beta 89.510(5) _cell_angle_gamma 87.002(5) _cell_volume 4171(2) _cell_formula_units_Z 2 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 67796 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(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 KappaCCD _diffrn_measurement_method '\f scans (\k = 0) + additional \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36100 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19066 _reflns_number_gt 12486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius,1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett, 1996)' _computing_publication_material 'SHELXL97 and WinGX (Farrugia, 1999)' _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^)+(0.0478P)^2^+0.6629P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19066 _refine_ls_number_parameters 898 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _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 Fe Fe 0.24253(3) 0.44557(2) 0.78696(2) 0.01549(10) Uani 1 1 d . . . P1 P 0.29197(7) 0.36909(4) 0.63138(4) 0.01833(18) Uani 1 1 d . . . P2 P 0.28245(7) 0.25073(5) 0.79928(4) 0.02284(19) Uani 1 1 d . . . HP2 H 0.3598 0.2525 0.7577 0.027 Uiso 1 1 d R . . P3 P 0.50201(7) 0.46614(4) 0.71200(4) 0.01809(18) Uani 1 1 d . . . P4 P 0.32103(7) 0.62431(4) 0.69015(4) 0.01854(18) Uani 1 1 d . . . HP4 H 0.3683 0.6064 0.6378 0.022 Uiso 1 1 d R . . C1 C 0.1263(2) 0.36630(17) 0.81750(15) 0.0180(7) Uani 1 1 d . . . H1 H 0.1083 0.3437 0.8649 0.022 Uiso 1 1 calc R . . C2 C 0.2122(2) 0.34059(17) 0.77698(15) 0.0189(7) Uani 1 1 d . . . C3 C 0.2132(2) 0.39217(16) 0.70569(15) 0.0176(7) Uani 1 1 d . . . C4 C 0.1295(2) 0.44844(16) 0.70586(15) 0.0165(6) Uani 1 1 d . . . H4 H 0.1136 0.4899 0.6676 0.020 Uiso 1 1 calc R . . C5 C 0.0729(2) 0.43233(16) 0.77313(15) 0.0163(6) Uani 1 1 d . . . C6 C 0.4011(2) 0.48085(17) 0.77820(15) 0.0179(7) Uani 1 1 d . . . C7 C 0.3207(2) 0.54412(16) 0.76403(15) 0.0177(7) Uani 1 1 d . . . C8 C 0.2560(2) 0.53911(17) 0.82821(16) 0.0202(7) Uani 1 1 d . . . H8 H 0.1988 0.5725 0.8337 0.024 Uiso 1 1 calc R . . C9 C 0.2944(3) 0.47437(18) 0.88185(15) 0.0220(7) Uani 1 1 d . . . C10 C 0.3809(2) 0.43875(17) 0.85031(15) 0.0192(7) Uani 1 1 d . . . H10 H 0.4190 0.3943 0.8734 0.023 Uiso 1 1 calc R . . C11 C 0.1953(3) 0.18004(17) 0.78637(16) 0.0236(7) Uani 1 1 d . . . C12 C 0.0855(3) 0.18297(19) 0.80404(17) 0.0287(8) Uani 1 1 d . . . H12 H 0.0555 0.2235 0.8202 0.034 Uiso 1 1 calc R . . C13 C 0.0210(3) 0.1249(2) 0.79745(18) 0.0369(9) Uani 1 1 d . . . H13 H -0.0522 0.1262 0.8099 0.044 Uiso 1 1 calc R . . C14 C 0.0649(4) 0.0658(2) 0.77265(18) 0.0414(10) Uani 1 1 d . . . H14 H 0.0214 0.0270 0.7685 0.050 Uiso 1 1 calc R . . C15 C 0.1729(4) 0.0634(2) 0.75386(18) 0.0417(10) Uani 1 1 d . . . H15 H 0.2017 0.0235 0.7362 0.050 Uiso 1 1 calc R . . C16 C 0.2387(3) 0.11971(19) 0.76094(17) 0.0331(9) Uani 1 1 d . . . H16 H 0.3120 0.1175 0.7488 0.040 Uiso 1 1 calc R . . C17 C 0.3402(3) 0.22455(18) 0.88775(18) 0.0291(8) Uani 1 1 d . . . C18 C 0.4511(3) 0.2325(2) 0.8960(2) 0.0452(11) Uani 1 1 d . . . H18 H 0.4941 0.2509 0.8560 0.054 Uiso 1 1 calc R . . C19 C 0.4959(4) 0.2131(3) 0.9636(2) 0.0669(15) Uani 1 1 d . . . H19 H 0.5694 0.2196 0.9698 0.080 Uiso 1 1 calc R . . C20 C 0.4326(4) 0.1839(3) 1.0229(2) 0.0608(14) Uani 1 1 d . . . H20 H 0.4644 0.1695 1.0685 0.073 Uiso 1 1 calc R . . C21 C 0.3226(3) 0.1756(2) 1.0153(2) 0.0468(11) Uani 1 1 d . . . H21 H 0.2804 0.1567 1.0556 0.056 Uiso 1 1 calc R . . C22 C 0.2754(3) 0.19559(18) 0.94742(17) 0.0324(9) Uani 1 1 d . . . H22 H 0.2017 0.1898 0.9416 0.039 Uiso 1 1 calc R . . C23 C 0.1979(3) 0.30240(17) 0.60974(15) 0.0192(7) Uani 1 1 d . . . C24 C 0.2423(3) 0.25137(18) 0.57328(16) 0.0250(7) Uani 1 1 d . . . H24 H 0.3151 0.2535 0.5597 0.030 Uiso 1 1 calc R . . C25 C 0.1791(3) 0.19685(19) 0.55673(17) 0.0322(8) Uani 1 1 d . . . H25 H 0.2092 0.1632 0.5317 0.039 Uiso 1 1 calc R . . C26 C 0.0714(3) 0.19300(19) 0.57773(17) 0.0322(8) Uani 1 1 d . . . H26 H 0.0295 0.1562 0.5673 0.039 Uiso 1 1 calc R . . C27 C 0.0256(3) 0.24346(19) 0.61409(17) 0.0305(8) Uani 1 1 d . . . H27 H -0.0470 0.2408 0.6279 0.037 Uiso 1 1 calc R . . C28 C 0.0884(3) 0.29791(18) 0.62977(16) 0.0256(8) Uani 1 1 d . . . H28 H 0.0573 0.3320 0.6540 0.031 Uiso 1 1 calc R . . C29 C 0.2649(2) 0.45323(17) 0.55677(15) 0.0182(7) Uani 1 1 d . . . C30 C 0.1656(3) 0.47001(18) 0.52005(15) 0.0233(7) Uani 1 1 d . . . H30 H 0.1076 0.4394 0.5347 0.028 Uiso 1 1 calc R . . C31 C 0.1531(3) 0.53207(19) 0.46181(16) 0.0257(8) Uani 1 1 d . . . H31 H 0.0865 0.5431 0.4379 0.031 Uiso 1 1 calc R . . C32 C 0.2392(3) 0.57779(18) 0.43888(16) 0.0259(8) Uani 1 1 d . . . H32 H 0.2301 0.6195 0.3999 0.031 Uiso 1 1 calc R . . C33 C 0.3386(3) 0.56118(18) 0.47402(16) 0.0238(7) Uani 1 1 d . . . H33 H 0.3967 0.5915 0.4585 0.029 Uiso 1 1 calc R . . C34 C 0.3514(3) 0.49909(17) 0.53269(15) 0.0196(7) Uani 1 1 d . . . H34 H 0.4184 0.4880 0.5561 0.024 Uiso 1 1 calc R . . C35 C -0.0343(2) 0.47042(17) 0.78785(15) 0.0190(7) Uani 1 1 d . . . C36 C -0.1148(3) 0.4581(2) 0.73100(17) 0.0321(8) Uani 1 1 d . . . H36A H -0.1863 0.4770 0.7404 0.048 Uiso 1 1 calc R . . H36B H -0.1163 0.4052 0.7334 0.048 Uiso 1 1 calc R . . H36C H -0.0921 0.4844 0.6838 0.048 Uiso 1 1 calc R . . C37 C -0.0774(3) 0.4336(2) 0.86216(16) 0.0297(8) Uani 1 1 d . . . H37A H -0.0278 0.4401 0.8984 0.045 Uiso 1 1 calc R . . H37B H -0.0843 0.3808 0.8662 0.045 Uiso 1 1 calc R . . H37C H -0.1473 0.4566 0.8688 0.045 Uiso 1 1 calc R . . C38 C -0.0262(3) 0.55487(18) 0.7793(2) 0.0359(9) Uani 1 1 d . . . H38A H 0.0199 0.5632 0.8165 0.054 Uiso 1 1 calc R . . H38B H -0.0975 0.5775 0.7830 0.054 Uiso 1 1 calc R . . H38C H 0.0040 0.5770 0.7329 0.054 Uiso 1 1 calc R . . C39 C 0.5883(2) 0.38692(17) 0.76311(16) 0.0206(7) Uani 1 1 d . . . C40 C 0.6337(2) 0.38312(19) 0.83099(16) 0.0242(7) Uani 1 1 d . . . H40 H 0.6164 0.4209 0.8546 0.029 Uiso 1 1 calc R . . C41 C 0.7045(3) 0.32304(19) 0.86290(17) 0.0268(8) Uani 1 1 d . . . H41 H 0.7329 0.3200 0.9085 0.032 Uiso 1 1 calc R . . C42 C 0.7333(3) 0.26766(19) 0.8275(2) 0.0349(9) Uani 1 1 d . . . H42 H 0.7824 0.2284 0.8489 0.042 Uiso 1 1 calc R . . C43 C 0.6894(3) 0.27034(19) 0.76059(19) 0.0339(9) Uani 1 1 d . . . H43 H 0.7086 0.2330 0.7368 0.041 Uiso 1 1 calc R . . C44 C 0.6163(3) 0.32949(18) 0.72909(17) 0.0247(7) Uani 1 1 d . . . H44 H 0.5855 0.3307 0.6845 0.030 Uiso 1 1 calc R . . C45 C 0.5866(2) 0.54626(17) 0.70986(15) 0.0186(7) Uani 1 1 d . . . C46 C 0.6057(3) 0.57681(18) 0.76868(16) 0.0239(7) Uani 1 1 d . . . H46 H 0.5731 0.5567 0.8128 0.029 Uiso 1 1 calc R . . C47 C 0.6726(3) 0.63668(19) 0.76200(18) 0.0290(8) Uani 1 1 d . . . H47 H 0.6855 0.6561 0.8016 0.035 Uiso 1 1 calc R . . C48 C 0.7200(3) 0.66753(19) 0.6963(2) 0.0344(9) Uani 1 1 d . . . H48 H 0.7643 0.7081 0.6915 0.041 Uiso 1 1 calc R . . C49 C 0.7016(3) 0.63821(19) 0.63782(19) 0.0328(9) Uani 1 1 d . . . H49 H 0.7343 0.6588 0.5938 0.039 Uiso 1 1 calc R . . C50 C 0.6349(3) 0.57848(18) 0.64395(17) 0.0264(8) Uani 1 1 d . . . H50 H 0.6222 0.5597 0.6039 0.032 Uiso 1 1 calc R . . C51 C 0.3942(2) 0.69639(17) 0.71437(17) 0.0219(7) Uani 1 1 d . . . C52 C 0.4511(3) 0.74656(18) 0.66203(17) 0.0258(8) Uani 1 1 d . . . H52 H 0.4556 0.7405 0.6152 0.031 Uiso 1 1 calc R . . C53 C 0.5007(3) 0.80503(19) 0.67999(19) 0.0335(9) Uani 1 1 d . . . H53 H 0.5402 0.8378 0.6454 0.040 Uiso 1 1 calc R . . C54 C 0.4923(3) 0.8153(2) 0.7484(2) 0.0385(9) Uani 1 1 d . . . H54 H 0.5245 0.8557 0.7599 0.046 Uiso 1 1 calc R . . C55 C 0.4356(3) 0.7654(2) 0.8005(2) 0.0465(11) Uani 1 1 d . . . H55 H 0.4302 0.7724 0.8470 0.056 Uiso 1 1 calc R . . C56 C 0.3873(3) 0.7058(2) 0.78408(19) 0.0345(9) Uani 1 1 d . . . H56 H 0.3503 0.6720 0.8194 0.041 Uiso 1 1 calc R . . C57 C 0.1874(2) 0.66064(16) 0.65995(15) 0.0188(7) Uani 1 1 d . . . C58 C 0.1309(3) 0.70862(17) 0.69518(16) 0.0230(7) Uani 1 1 d . . . H58 H 0.1613 0.7206 0.7351 0.028 Uiso 1 1 calc R . . C59 C 0.0287(3) 0.73850(17) 0.67030(17) 0.0248(7) Uani 1 1 d . . . H59 H -0.0100 0.7706 0.6936 0.030 Uiso 1 1 calc R . . C60 C -0.0158(3) 0.72066(18) 0.61095(17) 0.0280(8) Uani 1 1 d . . . H60 H -0.0844 0.7409 0.5944 0.034 Uiso 1 1 calc R . . C61 C 0.0407(3) 0.67301(18) 0.57592(17) 0.0272(8) Uani 1 1 d . . . H61 H 0.0099 0.6614 0.5359 0.033 Uiso 1 1 calc R . . C62 C 0.1428(3) 0.64242(17) 0.59996(15) 0.0216(7) Uani 1 1 d . . . H62 H 0.1810 0.6103 0.5766 0.026 Uiso 1 1 calc R . . C63 C 0.2621(3) 0.4557(2) 0.96083(16) 0.0296(8) Uani 1 1 d . . . C64 C 0.2577(4) 0.3710(2) 0.99170(19) 0.0588(13) Uani 1 1 d . . . H64A H 0.2020 0.3519 0.9673 0.088 Uiso 1 1 calc R . . H64B H 0.2414 0.3610 1.0423 0.088 Uiso 1 1 calc R . . H64C H 0.3268 0.3468 0.9851 0.088 Uiso 1 1 calc R . . C65 C 0.1540(3) 0.4942(3) 0.9724(2) 0.0647(15) Uani 1 1 d . . . H65A H 0.1610 0.5477 0.9611 0.097 Uiso 1 1 calc R . . H65B H 0.1324 0.4768 1.0218 0.097 Uiso 1 1 calc R . . H65C H 0.0999 0.4824 0.9415 0.097 Uiso 1 1 calc R . . C66 C 0.3496(3) 0.4871(3) 1.00066(18) 0.0500(12) Uani 1 1 d . . . H66A H 0.4194 0.4637 0.9942 0.075 Uiso 1 1 calc R . . H66B H 0.3327 0.4767 1.0512 0.075 Uiso 1 1 calc R . . H66C H 0.3513 0.5406 0.9815 0.075 Uiso 1 1 calc R . . Zr1 Zr 0.60537(3) 0.136137(18) 0.581749(17) 0.02527(9) Uani 1 1 d . . . O1 O 0.69392(18) 0.09472(12) 0.49654(11) 0.0272(5) Uani 1 1 d . . . Cl5 Cl 0.65158(9) 0.26212(5) 0.51440(5) 0.0440(2) Uani 1 1 d . . . Cl6 Cl 0.50630(8) 0.17905(6) 0.67507(5) 0.0420(2) Uani 1 1 d . . . Cl7 Cl 0.44445(7) 0.14497(5) 0.50656(4) 0.0311(2) Uani 1 1 d . . . Cl8 Cl 0.57656(7) 0.00397(5) 0.63715(4) 0.0324(2) Uani 1 1 d . . . Cl9 Cl 0.78102(7) 0.12431(5) 0.64569(5) 0.0349(2) Uani 1 1 d . . . C69 C 0.7955(3) 0.1226(2) 0.46126(19) 0.0380(9) Uani 1 1 d . . . H69A H 0.8529 0.1189 0.4966 0.046 Uiso 1 1 calc R . . H69B H 0.7850 0.1748 0.4344 0.046 Uiso 1 1 calc R . . C70 C 0.8227(5) 0.0726(4) 0.4117(3) 0.109(3) Uani 1 1 d . . . H70A H 0.8472 0.1024 0.3656 0.131 Uiso 1 1 calc R . . H70B H 0.8808 0.0360 0.4324 0.131 Uiso 1 1 calc R . . C71 C 0.7281(3) 0.0350(2) 0.4016(2) 0.0430(10) Uani 1 1 d . . . H71A H 0.7477 -0.0156 0.3971 0.052 Uiso 1 1 calc R . . H71B H 0.6895 0.0622 0.3582 0.052 Uiso 1 1 calc R . . C72 C 0.6584(3) 0.0325(2) 0.46685(18) 0.0336(9) Uani 1 1 d . . . H72A H 0.5820 0.0400 0.4536 0.040 Uiso 1 1 calc R . . H72B H 0.6696 -0.0156 0.5018 0.040 Uiso 1 1 calc R . . Zr2 Zr 0.07392(3) 0.802476(18) 0.907756(16) 0.02826(9) Uani 1 1 d . . . O2 O 0.16507(19) 0.89339(12) 0.93901(11) 0.0300(6) Uani 1 1 d . . . Cl10 Cl 0.24224(8) 0.72386(5) 0.93922(5) 0.0423(2) Uani 1 1 d . . . Cl11 Cl 0.14340(8) 0.85534(5) 0.78683(4) 0.0341(2) Uani 1 1 d . . . Cl12 Cl -0.07834(8) 0.89702(5) 0.88205(5) 0.0398(2) Uani 1 1 d . . . Cl13 Cl 0.02148(8) 0.76921(5) 1.03540(4) 0.0367(2) Uani 1 1 d . . . Cl14 Cl -0.02111(10) 0.70585(6) 0.87476(5) 0.0535(3) Uani 1 1 d . . . C74 C 0.1220(3) 0.9396(2) 0.9870(2) 0.0411(10) Uani 1 1 d . . . H74A H 0.1319 0.9130 1.0372 0.049 Uiso 1 1 calc R . . H74B H 0.0451 0.9527 0.9779 0.049 Uiso 1 1 calc R . . C75 C 0.1855(4) 1.0076(2) 0.9695(2) 0.0561(12) Uani 1 1 d . . . H75A H 0.1894 1.0297 1.0105 0.067 Uiso 1 1 calc R . . H75B H 0.1536 1.0450 0.9289 0.067 Uiso 1 1 calc R . . C76 C 0.2952(4) 0.9799(2) 0.9510(2) 0.0489(11) Uani 1 1 d . . . H76A H 0.3392 0.9607 0.9941 0.059 Uiso 1 1 calc R . . H76B H 0.3327 1.0199 0.9186 0.059 Uiso 1 1 calc R . . C77 C 0.2729(3) 0.9179(2) 0.9147(2) 0.0407(10) Uani 1 1 d . . . H77A H 0.2740 0.9365 0.8626 0.049 Uiso 1 1 calc R . . H77B H 0.3270 0.8765 0.9287 0.049 Uiso 1 1 calc R . . C67 C 0.8541(3) 0.92190(14) 0.68725(8) 0.0487(13) Uani 0.88 1 d PG A 1 H67A H 0.8129 0.9752 0.6900 0.058 Uiso 0.88 1 d PG A 1 H67B H 0.9325 0.9158 0.7147 0.058 Uiso 0.88 1 d PG A 1 Cl1 Cl 0.77488(10) 0.84913(6) 0.73232(6) 0.0607(4) Uani 0.88 1 d PG A 1 Cl2 Cl 0.87430(12) 0.92061(8) 0.59733(6) 0.0821(5) Uani 0.88 1 d PG A 1 C67B C 0.8555(3) 0.94224(11) 0.66701(11) 0.09(2) Uiso 0.12 1 d PG A 2 H67C H 0.7942 0.9860 0.6713 0.112 Uiso 0.12 1 d PG A 2 H67D H 0.8923 0.9179 0.7198 0.112 Uiso 0.12 1 d PG A 2 Cl1B Cl 0.79090(18) 0.87151(15) 0.63978(6) 0.090(4) Uiso 0.12 1 d PG A 2 Cl2B Cl 0.9555(4) 0.9812(2) 0.60639(12) 0.081(3) Uiso 0.12 1 d PG A 2 C68 C 0.34640(14) -0.00832(15) 1.18778(15) 0.0545(15) Uani 0.80 1 d PG B 1 H68A H 0.3442 -0.0284 1.2464 0.065 Uiso 0.80 1 d PG B 1 H68B H 0.2955 0.0435 1.1711 0.065 Uiso 0.80 1 d PG B 1 Cl3 Cl 0.47978(11) 0.01210(9) 1.16253(9) 0.0867(6) Uani 0.80 1 d PG B 1 Cl4 Cl 0.29779(14) -0.07648(9) 1.14849(8) 0.0910(6) Uani 0.80 1 d PG B 1 C68B C 0.39788(16) -0.04907(11) 1.18986(7) 0.065(7) Uiso 0.20 1 d PG B 2 H68C H 0.3923 -0.0889 1.2424 0.078 Uiso 0.20 1 d PG B 2 H68D H 0.4484 -0.0033 1.1945 0.078 Uiso 0.20 1 d PG B 2 Cl3B Cl 0.46082(18) -0.09611(18) 1.1304(3) 0.106(3) Uiso 0.20 1 d PG B 2 Cl4B Cl 0.26821(10) -0.01247(14) 1.1605(2) 0.118(3) Uiso 0.20 1 d PG B 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 Fe 0.0140(2) 0.0165(2) 0.0164(2) -0.00429(17) 0.00125(17) -0.00403(18) P1 0.0182(4) 0.0183(4) 0.0194(4) -0.0062(3) 0.0026(3) -0.0024(3) P2 0.0193(5) 0.0171(4) 0.0297(5) -0.0011(3) 0.0033(4) -0.0013(4) P3 0.0155(4) 0.0195(4) 0.0191(4) -0.0042(3) 0.0011(3) -0.0029(3) P4 0.0174(4) 0.0168(4) 0.0221(4) -0.0057(3) 0.0028(3) -0.0030(3) C1 0.0165(16) 0.0205(17) 0.0176(15) -0.0038(13) 0.0018(12) -0.0102(13) C2 0.0202(17) 0.0164(16) 0.0201(16) -0.0035(12) -0.0003(13) -0.0050(13) C3 0.0166(17) 0.0141(16) 0.0221(16) -0.0036(12) -0.0013(13) -0.0041(13) C4 0.0183(17) 0.0154(16) 0.0153(15) -0.0020(12) -0.0022(12) -0.0035(13) C5 0.0128(16) 0.0167(16) 0.0210(15) -0.0068(12) 0.0005(12) -0.0047(13) C6 0.0128(16) 0.0192(16) 0.0222(16) -0.0046(13) -0.0010(12) -0.0071(13) C7 0.0161(16) 0.0153(16) 0.0228(16) -0.0058(13) 0.0017(13) -0.0067(13) C8 0.0129(16) 0.0233(17) 0.0293(17) -0.0148(14) 0.0031(13) -0.0068(13) C9 0.0181(17) 0.0319(19) 0.0179(16) -0.0085(14) 0.0005(13) -0.0086(14) C10 0.0164(17) 0.0213(17) 0.0191(16) -0.0017(13) -0.0061(13) -0.0059(13) C11 0.032(2) 0.0132(16) 0.0242(17) -0.0020(13) 0.0045(14) -0.0041(14) C12 0.033(2) 0.0246(19) 0.0312(19) -0.0113(15) 0.0047(16) -0.0073(16) C13 0.043(2) 0.035(2) 0.033(2) -0.0072(17) 0.0069(17) -0.0173(19) C14 0.062(3) 0.035(2) 0.029(2) -0.0076(17) 0.0073(19) -0.024(2) C15 0.071(3) 0.024(2) 0.033(2) -0.0128(16) 0.012(2) -0.009(2) C16 0.046(2) 0.0246(19) 0.0280(19) -0.0045(15) 0.0097(16) -0.0043(17) C17 0.0237(19) 0.0210(18) 0.0358(19) 0.0063(15) -0.0049(15) -0.0012(15) C18 0.030(2) 0.040(2) 0.053(2) 0.0164(19) -0.0090(19) -0.0126(19) C19 0.039(3) 0.074(3) 0.065(3) 0.032(3) -0.026(2) -0.024(2) C20 0.051(3) 0.072(3) 0.043(2) 0.022(2) -0.025(2) -0.024(2) C21 0.045(3) 0.050(3) 0.035(2) 0.0107(18) -0.0057(19) -0.018(2) C22 0.031(2) 0.0245(19) 0.036(2) 0.0056(15) -0.0070(16) -0.0070(16) C23 0.0256(18) 0.0162(16) 0.0155(15) -0.0027(12) -0.0005(13) -0.0040(14) C24 0.0272(19) 0.0217(18) 0.0268(17) -0.0071(14) 0.0000(14) -0.0027(15) C25 0.043(2) 0.0224(19) 0.0339(19) -0.0131(15) -0.0065(17) 0.0019(17) C26 0.040(2) 0.0244(19) 0.0318(19) -0.0034(15) -0.0104(17) -0.0102(17) C27 0.028(2) 0.032(2) 0.0306(19) -0.0039(16) 0.0008(15) -0.0138(16) C28 0.0253(19) 0.0272(19) 0.0265(17) -0.0092(14) 0.0019(14) -0.0089(15) C29 0.0195(17) 0.0217(17) 0.0154(15) -0.0081(13) 0.0045(13) -0.0016(14) C30 0.0182(17) 0.0303(19) 0.0231(17) -0.0090(14) 0.0048(13) -0.0050(15) C31 0.0203(18) 0.034(2) 0.0230(17) -0.0084(15) -0.0056(14) 0.0010(16) C32 0.031(2) 0.0256(19) 0.0186(16) -0.0022(14) 0.0031(14) 0.0023(16) C33 0.0250(19) 0.0219(18) 0.0257(17) -0.0076(14) 0.0063(14) -0.0035(15) C34 0.0176(17) 0.0227(17) 0.0194(16) -0.0069(13) 0.0009(13) 0.0003(14) C35 0.0151(16) 0.0201(17) 0.0232(16) -0.0080(13) -0.0011(13) -0.0018(13) C36 0.0193(19) 0.050(2) 0.0289(18) -0.0129(17) 0.0002(15) 0.0013(17) C37 0.0199(19) 0.047(2) 0.0241(17) -0.0131(16) 0.0035(14) -0.0003(16) C38 0.0201(19) 0.0242(19) 0.065(3) -0.0146(18) 0.0081(17) 0.0003(16) C39 0.0155(17) 0.0208(17) 0.0247(17) -0.0022(13) 0.0023(13) -0.0088(13) C40 0.0166(17) 0.0292(19) 0.0269(17) -0.0056(14) 0.0025(14) -0.0076(15) C41 0.0184(18) 0.031(2) 0.0267(18) 0.0024(15) -0.0028(14) -0.0087(15) C42 0.026(2) 0.0218(19) 0.051(2) 0.0028(17) -0.0061(17) -0.0007(16) C43 0.034(2) 0.0243(19) 0.044(2) -0.0092(16) 0.0001(17) -0.0010(17) C44 0.0250(19) 0.0225(18) 0.0267(17) -0.0056(14) -0.0023(14) -0.0040(15) C45 0.0127(16) 0.0181(16) 0.0237(16) -0.0028(13) 0.0003(13) -0.0006(13) C46 0.0195(18) 0.0265(18) 0.0242(17) -0.0031(14) 0.0022(14) -0.0035(14) C47 0.0203(19) 0.030(2) 0.040(2) -0.0147(16) -0.0023(15) -0.0023(15) C48 0.024(2) 0.0217(19) 0.059(2) -0.0131(17) 0.0120(18) -0.0078(16) C49 0.034(2) 0.027(2) 0.036(2) -0.0062(16) 0.0140(16) -0.0055(17) C50 0.027(2) 0.0226(18) 0.0295(18) -0.0073(14) 0.0061(15) -0.0007(15) C51 0.0134(17) 0.0178(17) 0.0342(19) -0.0058(14) 0.0022(14) -0.0012(13) C52 0.0251(19) 0.0235(18) 0.0284(18) -0.0043(14) -0.0035(14) -0.0052(15) C53 0.033(2) 0.0219(19) 0.043(2) -0.0011(16) 0.0004(17) -0.0122(16) C54 0.034(2) 0.032(2) 0.057(2) -0.0226(18) 0.0076(18) -0.0158(18) C55 0.048(3) 0.054(3) 0.052(2) -0.036(2) 0.018(2) -0.024(2) C56 0.033(2) 0.037(2) 0.041(2) -0.0221(17) 0.0174(17) -0.0167(17) C57 0.0190(17) 0.0146(16) 0.0223(16) -0.0028(13) 0.0042(13) -0.0051(13) C58 0.0243(19) 0.0206(17) 0.0247(17) -0.0058(14) 0.0004(14) -0.0057(14) C59 0.0223(19) 0.0184(17) 0.0336(19) -0.0067(14) 0.0061(15) 0.0008(14) C60 0.0199(18) 0.0264(19) 0.0337(19) 0.0004(15) -0.0044(15) -0.0005(15) C61 0.029(2) 0.029(2) 0.0223(17) -0.0040(14) -0.0036(15) -0.0008(16) C62 0.0277(19) 0.0155(16) 0.0220(16) -0.0055(13) 0.0037(14) -0.0021(14) C63 0.026(2) 0.048(2) 0.0187(17) -0.0133(16) 0.0029(14) -0.0126(17) C64 0.092(4) 0.059(3) 0.024(2) -0.0027(19) 0.014(2) -0.034(3) C65 0.035(3) 0.136(5) 0.031(2) -0.037(3) 0.0098(19) -0.005(3) C66 0.048(3) 0.084(3) 0.0237(19) -0.017(2) -0.0017(18) -0.034(2) Zr1 0.02711(19) 0.02019(18) 0.03029(18) -0.00843(14) 0.00431(14) -0.00742(14) O1 0.0257(13) 0.0249(13) 0.0339(13) -0.0116(10) 0.0059(10) -0.0089(10) Cl5 0.0597(7) 0.0229(5) 0.0492(6) -0.0051(4) 0.0002(5) -0.0174(5) Cl6 0.0368(6) 0.0491(6) 0.0494(6) -0.0291(5) 0.0108(4) -0.0083(5) Cl7 0.0283(5) 0.0274(5) 0.0391(5) -0.0111(4) -0.0004(4) -0.0011(4) Cl8 0.0365(5) 0.0242(5) 0.0353(5) -0.0024(4) -0.0015(4) -0.0115(4) Cl9 0.0302(5) 0.0379(5) 0.0393(5) -0.0122(4) 0.0008(4) -0.0127(4) C69 0.030(2) 0.044(2) 0.042(2) -0.0108(18) 0.0137(17) -0.0158(18) C70 0.093(5) 0.191(7) 0.079(4) -0.088(4) 0.058(3) -0.085(5) C71 0.048(3) 0.041(2) 0.045(2) -0.0198(19) 0.0126(19) 0.000(2) C72 0.031(2) 0.033(2) 0.042(2) -0.0193(17) 0.0033(17) -0.0079(17) Zr2 0.0419(2) 0.02261(18) 0.02124(17) -0.00644(13) 0.00873(15) -0.00693(16) O2 0.0390(15) 0.0271(13) 0.0271(12) -0.0129(10) 0.0067(11) -0.0041(11) Cl10 0.0556(7) 0.0333(5) 0.0347(5) -0.0044(4) 0.0144(4) 0.0073(5) Cl11 0.0534(6) 0.0277(5) 0.0228(4) -0.0079(3) 0.0108(4) -0.0103(4) Cl12 0.0407(6) 0.0415(6) 0.0353(5) -0.0055(4) 0.0053(4) -0.0025(5) Cl13 0.0452(6) 0.0393(5) 0.0231(4) -0.0027(4) 0.0110(4) -0.0042(4) Cl14 0.0819(8) 0.0416(6) 0.0437(6) -0.0178(5) 0.0125(5) -0.0316(6) C74 0.051(3) 0.038(2) 0.042(2) -0.0235(18) 0.0105(19) -0.004(2) C75 0.079(4) 0.041(3) 0.054(3) -0.021(2) 0.002(2) -0.009(2) C76 0.057(3) 0.051(3) 0.045(2) -0.019(2) 0.011(2) -0.024(2) C77 0.036(2) 0.041(2) 0.046(2) -0.0135(18) 0.0051(18) -0.0037(19) C67 0.046(3) 0.035(3) 0.068(3) -0.020(3) -0.011(2) 0.004(2) Cl1 0.0434(7) 0.0360(7) 0.1062(10) -0.0232(7) -0.0179(7) -0.0021(6) Cl2 0.0837(11) 0.0878(11) 0.0681(9) -0.0163(8) -0.0154(8) 0.0454(9) C68 0.040(3) 0.081(4) 0.060(3) -0.047(3) 0.005(3) -0.026(3) Cl3 0.0623(11) 0.0756(12) 0.1045(13) 0.0127(10) 0.0345(9) -0.0132(9) Cl4 0.1527(19) 0.0674(11) 0.0570(9) -0.0158(8) -0.0236(10) -0.0364(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C2 2.033(3) . ? Fe C7 2.040(3) . ? Fe C1 2.069(3) . ? Fe C8 2.069(3) . ? Fe C3 2.072(3) . ? Fe C10 2.078(3) . ? Fe C6 2.080(3) . ? Fe C4 2.081(3) . ? Fe C9 2.121(3) . ? Fe C5 2.139(3) . ? P1 C3 1.834(3) . ? P1 C29 1.843(3) . ? P1 C23 1.846(3) . ? P2 C2 1.776(3) . ? P2 C17 1.784(3) . ? P2 C11 1.787(3) . ? P2 HP2 1.2318 . ? P3 C6 1.822(3) . ? P3 C39 1.830(3) . ? P3 C45 1.835(3) . ? P4 C7 1.771(3) . ? P4 C57 1.787(3) . ? P4 C51 1.789(3) . ? P4 HP4 1.2567 . ? C1 C5 1.427(4) . ? C1 C2 1.431(4) . ? C1 H1 0.9300 . ? C2 C3 1.456(4) . ? C3 C4 1.420(4) . ? C4 C5 1.430(4) . ? C4 H4 0.9300 . ? C5 C35 1.516(4) . ? C6 C10 1.431(4) . ? C6 C7 1.458(4) . ? C7 C8 1.443(4) . ? C8 C9 1.426(4) . ? C8 H8 0.9300 . ? C9 C10 1.425(4) . ? C9 C63 1.518(4) . ? C10 H10 0.9300 . ? C11 C12 1.391(4) . ? C11 C16 1.393(4) . ? C12 C13 1.391(5) . ? C12 H12 0.9300 . ? C13 C14 1.370(5) . ? C13 H13 0.9300 . ? C14 C15 1.375(5) . ? C14 H14 0.9300 . ? C15 C16 1.377(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.394(5) . ? C17 C22 1.396(5) . ? C18 C19 1.366(5) . ? C18 H18 0.9300 . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 C21 1.383(5) . ? C20 H20 0.9300 . ? C21 C22 1.382(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.385(4) . ? C23 C28 1.399(4) . ? C24 C25 1.395(5) . ? C24 H24 0.9300 . ? C25 C26 1.381(5) . ? C25 H25 0.9300 . ? C26 C27 1.382(5) . ? C26 H26 0.9300 . ? C27 C28 1.383(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.395(4) . ? C29 C30 1.396(4) . ? C30 C31 1.385(4) . ? C30 H30 0.9300 . ? C31 C32 1.385(4) . ? C31 H31 0.9300 . ? C32 C33 1.384(4) . ? C32 H32 0.9300 . ? C33 C34 1.391(4) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C37 1.519(4) . ? C35 C38 1.524(4) . ? C35 C36 1.542(4) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C44 1.394(4) . ? C39 C40 1.402(4) . ? C40 C41 1.386(4) . ? C40 H40 0.9300 . ? C41 C42 1.381(5) . ? C41 H41 0.9300 . ? C42 C43 1.381(5) . ? C42 H42 0.9300 . ? C43 C44 1.391(4) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C50 1.396(4) . ? C45 C46 1.400(4) . ? C46 C47 1.386(4) . ? C46 H46 0.9300 . ? C47 C48 1.382(5) . ? C47 H47 0.9300 . ? C48 C49 1.379(5) . ? C48 H48 0.9300 . ? C49 C50 1.383(5) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C56 1.386(4) . ? C51 C52 1.393(4) . ? C52 C53 1.375(4) . ? C52 H52 0.9300 . ? C53 C54 1.369(5) . ? C53 H53 0.9300 . ? C54 C55 1.387(5) . ? C54 H54 0.9300 . ? C55 C56 1.373(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.389(4) . ? C57 C62 1.395(4) . ? C58 C59 1.384(4) . ? C58 H58 0.9300 . ? C59 C60 1.380(4) . ? C59 H59 0.9300 . ? C60 C61 1.382(5) . ? C60 H60 0.9300 . ? C61 C62 1.382(4) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C65 1.513(5) . ? C63 C64 1.522(5) . ? C63 C66 1.538(5) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? Zr1 O1 2.215(2) . ? Zr1 Cl6 2.4157(10) . ? Zr1 Cl7 2.4312(12) . ? Zr1 Cl8 2.4366(11) . ? Zr1 Cl5 2.4446(11) . ? Zr1 Cl9 2.4650(12) . ? O1 C69 1.470(4) . ? O1 C72 1.479(4) . ? C69 C70 1.497(6) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.421(6) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.500(5) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? Zr2 O2 2.255(2) . ? Zr2 Cl14 2.3824(12) . ? Zr2 Cl11 2.4423(10) . ? Zr2 Cl10 2.4514(13) . ? Zr2 Cl12 2.4515(12) . ? Zr2 Cl13 2.4543(10) . ? O2 C77 1.458(4) . ? O2 C74 1.471(4) . ? C74 C75 1.472(5) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.487(6) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 C77 1.507(5) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C67 Cl2 1.7400 . ? C67 Cl1 1.7400 . ? C67 H67A 1.0900 . ? C67 H67B 1.0900 . ? C67 H67C 1.3247 . ? C67 H67D 0.7700 . ? C67B Cl2B 1.7400 . ? C67B Cl1B 1.7400 . ? C67B H67A 0.9631 . ? C67B H67B 1.3096 . ? C67B H67C 1.0900 . ? C67B H67D 1.0900 . ? C68 Cl3 1.7400 . ? C68 Cl4 1.7400 . ? C68 H68A 1.0900 . ? C68 H68B 1.0899 . ? C68 H68D 1.2730 . ? Cl3 H68D 0.7237 . ? C68B Cl4B 1.7400 . ? C68B Cl3B 1.7400 . ? C68B H68A 1.3811 . ? C68B H68C 1.0900 . ? C68B H68D 1.0900 . ? Cl4B H68B 1.1593 . ? 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 C2 Fe C7 154.99(12) . . ? C2 Fe C1 40.83(12) . . ? C7 Fe C1 162.96(12) . . ? C2 Fe C8 162.62(12) . . ? C7 Fe C8 41.10(11) . . ? C1 Fe C8 124.93(12) . . ? C2 Fe C3 41.53(11) . . ? C7 Fe C3 119.96(11) . . ? C1 Fe C3 68.63(11) . . ? C8 Fe C3 153.88(12) . . ? C2 Fe C10 108.89(12) . . ? C7 Fe C10 68.00(12) . . ? C1 Fe C10 119.55(12) . . ? C8 Fe C10 67.13(12) . . ? C3 Fe C10 129.29(12) . . ? C2 Fe C6 119.83(12) . . ? C7 Fe C6 41.45(12) . . ? C1 Fe C6 153.71(12) . . ? C8 Fe C6 68.93(12) . . ? C3 Fe C6 109.24(12) . . ? C10 Fe C6 40.27(11) . . ? C2 Fe C4 67.93(12) . . ? C7 Fe C4 109.14(12) . . ? C1 Fe C4 67.02(11) . . ? C8 Fe C4 119.80(12) . . ? C3 Fe C4 39.98(11) . . ? C10 Fe C4 166.89(11) . . ? C6 Fe C4 129.18(11) . . ? C2 Fe C9 126.44(12) . . ? C7 Fe C9 68.05(12) . . ? C1 Fe C9 107.20(12) . . ? C8 Fe C9 39.78(12) . . ? C3 Fe C9 165.60(12) . . ? C10 Fe C9 39.66(12) . . ? C6 Fe C9 67.99(11) . . ? C4 Fe C9 152.51(12) . . ? C2 Fe C5 67.67(12) . . ? C7 Fe C5 126.94(12) . . ? C1 Fe C5 39.62(11) . . ? C8 Fe C5 107.51(12) . . ? C3 Fe C5 67.49(11) . . ? C10 Fe C5 152.39(11) . . ? C6 Fe C5 165.75(11) . . ? C4 Fe C5 39.57(11) . . ? C9 Fe C5 118.73(11) . . ? C3 P1 C29 102.63(13) . . ? C3 P1 C23 97.24(14) . . ? C29 P1 C23 101.79(14) . . ? C2 P2 C17 114.72(15) . . ? C2 P2 C11 110.15(15) . . ? C17 P2 C11 110.27(15) . . ? C2 P2 HP2 107.9 . . ? C17 P2 HP2 105.6 . . ? C11 P2 HP2 107.9 . . ? C6 P3 C39 102.98(14) . . ? C6 P3 C45 99.70(14) . . ? C39 P3 C45 101.85(14) . . ? C7 P4 C57 113.10(14) . . ? C7 P4 C51 109.52(14) . . ? C57 P4 C51 109.60(14) . . ? C7 P4 HP4 109.0 . . ? C57 P4 HP4 107.0 . . ? C51 P4 HP4 108.6 . . ? C5 C1 C2 108.8(2) . . ? C5 C1 Fe 72.84(17) . . ? C2 C1 Fe 68.23(17) . . ? C5 C1 H1 125.6 . . ? C2 C1 H1 125.6 . . ? Fe C1 H1 124.9 . . ? C1 C2 C3 107.9(3) . . ? C1 C2 P2 126.4(2) . . ? C3 C2 P2 124.0(2) . . ? C1 C2 Fe 70.94(17) . . ? C3 C2 Fe 70.67(17) . . ? P2 C2 Fe 135.64(17) . . ? C4 C3 C2 106.1(2) . . ? C4 C3 P1 131.1(2) . . ? C2 C3 P1 121.5(2) . . ? C4 C3 Fe 70.35(17) . . ? C2 C3 Fe 67.81(16) . . ? P1 C3 Fe 135.76(16) . . ? C3 C4 C5 110.4(2) . . ? C3 C4 Fe 69.67(17) . . ? C5 C4 Fe 72.41(16) . . ? C3 C4 H4 124.8 . . ? C5 C4 H4 124.8 . . ? Fe C4 H4 124.7 . . ? C1 C5 C4 106.6(2) . . ? C1 C5 C35 127.3(3) . . ? C4 C5 C35 125.3(3) . . ? C1 C5 Fe 67.55(16) . . ? C4 C5 Fe 68.01(16) . . ? C35 C5 Fe 137.3(2) . . ? C10 C6 C7 105.7(3) . . ? C10 C6 P3 131.4(2) . . ? C7 C6 P3 122.9(2) . . ? C10 C6 Fe 69.81(16) . . ? C7 C6 Fe 67.84(16) . . ? P3 C6 Fe 126.64(16) . . ? C8 C7 C6 108.0(2) . . ? C8 C7 P4 124.5(2) . . ? C6 C7 P4 126.0(2) . . ? C8 C7 Fe 70.52(16) . . ? C6 C7 Fe 70.72(17) . . ? P4 C7 Fe 135.01(17) . . ? C9 C8 C7 108.6(3) . . ? C9 C8 Fe 72.07(18) . . ? C7 C8 Fe 68.38(16) . . ? C9 C8 H8 125.7 . . ? C7 C8 H8 125.7 . . ? Fe C8 H8 125.4 . . ? C10 C9 C8 107.0(2) . . ? C10 C9 C63 126.6(3) . . ? C8 C9 C63 125.6(3) . . ? C10 C9 Fe 68.54(16) . . ? C8 C9 Fe 68.15(16) . . ? C63 C9 Fe 136.2(2) . . ? C9 C10 C6 110.6(3) . . ? C9 C10 Fe 71.79(17) . . ? C6 C10 Fe 69.92(16) . . ? C9 C10 H10 124.7 . . ? C6 C10 H10 124.7 . . ? Fe C10 H10 125.2 . . ? C12 C11 C16 119.5(3) . . ? C12 C11 P2 120.8(2) . . ? C16 C11 P2 119.6(3) . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120.5(4) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 119.8(4) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C18 C17 C22 120.8(3) . . ? C18 C17 P2 118.9(3) . . ? C22 C17 P2 120.3(3) . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.3(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 119.7(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C17 119.0(3) . . ? C21 C22 H22 120.5 . . ? C17 C22 H22 120.5 . . ? C24 C23 C28 118.6(3) . . ? C24 C23 P1 116.2(2) . . ? C28 C23 P1 125.2(2) . . ? C23 C24 C25 120.7(3) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 119.7(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.5(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 119.6(3) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C23 120.9(3) . . ? C27 C28 H28 119.5 . . ? C23 C28 H28 119.5 . . ? C34 C29 C30 118.7(3) . . ? C34 C29 P1 117.5(2) . . ? C30 C29 P1 123.5(2) . . ? C31 C30 C29 120.3(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 120.5(3) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C31 119.9(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C29 120.7(3) . . ? C33 C34 H34 119.6 . . ? C29 C34 H34 119.6 . . ? C5 C35 C37 111.2(2) . . ? C5 C35 C38 112.4(3) . . ? C37 C35 C38 110.4(3) . . ? C5 C35 C36 105.7(2) . . ? C37 C35 C36 108.1(3) . . ? C38 C35 C36 108.7(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C44 C39 C40 118.5(3) . . ? C44 C39 P3 116.8(2) . . ? C40 C39 P3 124.5(2) . . ? C41 C40 C39 120.0(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 120.3(3) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C44 119.3(3) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C43 C44 C39 121.2(3) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? C50 C45 C46 118.4(3) . . ? C50 C45 P3 116.5(2) . . ? C46 C45 P3 125.1(2) . . ? C47 C46 C45 120.8(3) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C48 C47 C46 119.8(3) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C49 C48 C47 120.0(3) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.6(3) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C49 C50 C45 120.4(3) . . ? C49 C50 H50 119.8 . . ? C45 C50 H50 119.8 . . ? C56 C51 C52 120.0(3) . . ? C56 C51 P4 119.8(2) . . ? C52 C51 P4 120.1(2) . . ? C53 C52 C51 119.7(3) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C55 119.8(3) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C56 C55 C54 120.6(3) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C55 C56 C51 119.4(3) . . ? C55 C56 H56 120.3 . . ? C51 C56 H56 120.3 . . ? C58 C57 C62 120.9(3) . . ? C58 C57 P4 119.4(2) . . ? C62 C57 P4 119.6(2) . . ? C59 C58 C57 119.3(3) . . ? C59 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? C60 C59 C58 120.0(3) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C61 120.6(3) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C60 C61 C62 120.4(3) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? C61 C62 C57 118.8(3) . . ? C61 C62 H62 120.6 . . ? C57 C62 H62 120.6 . . ? C65 C63 C9 111.8(3) . . ? C65 C63 C64 109.6(3) . . ? C9 C63 C64 111.6(3) . . ? C65 C63 C66 107.5(3) . . ? C9 C63 C66 106.3(3) . . ? C64 C63 C66 109.8(3) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O1 Zr1 Cl6 178.77(6) . . ? O1 Zr1 Cl7 86.11(7) . . ? Cl6 Zr1 Cl7 93.29(4) . . ? O1 Zr1 Cl8 85.87(6) . . ? Cl6 Zr1 Cl8 93.08(4) . . ? Cl7 Zr1 Cl8 90.79(3) . . ? O1 Zr1 Cl5 86.08(6) . . ? Cl6 Zr1 Cl5 94.99(4) . . ? Cl7 Zr1 Cl5 89.87(4) . . ? Cl8 Zr1 Cl5 171.86(3) . . ? O1 Zr1 Cl9 87.16(7) . . ? Cl6 Zr1 Cl9 93.47(4) . . ? Cl7 Zr1 Cl9 173.17(3) . . ? Cl8 Zr1 Cl9 89.84(3) . . ? Cl5 Zr1 Cl9 88.55(4) . . ? C69 O1 C72 109.3(2) . . ? C69 O1 Zr1 126.7(2) . . ? C72 O1 Zr1 123.92(18) . . ? O1 C69 C70 104.7(3) . . ? O1 C69 H69A 110.8 . . ? C70 C69 H69A 110.8 . . ? O1 C69 H69B 110.8 . . ? C70 C69 H69B 110.8 . . ? H69A C69 H69B 108.9 . . ? C71 C70 C69 108.6(4) . . ? C71 C70 H70A 110.0 . . ? C69 C70 H70A 110.0 . . ? C71 C70 H70B 110.0 . . ? C69 C70 H70B 110.0 . . ? H70A C70 H70B 108.3 . . ? C70 C71 C72 106.5(3) . . ? C70 C71 H71A 110.4 . . ? C72 C71 H71A 110.4 . . ? C70 C71 H71B 110.4 . . ? C72 C71 H71B 110.4 . . ? H71A C71 H71B 108.6 . . ? O1 C72 C71 104.9(3) . . ? O1 C72 H72A 110.8 . . ? C71 C72 H72A 110.8 . . ? O1 C72 H72B 110.8 . . ? C71 C72 H72B 110.8 . . ? H72A C72 H72B 108.8 . . ? O2 Zr2 Cl14 179.56(7) . . ? O2 Zr2 Cl11 84.76(6) . . ? Cl14 Zr2 Cl11 95.16(4) . . ? O2 Zr2 Cl10 85.56(7) . . ? Cl14 Zr2 Cl10 94.01(5) . . ? Cl11 Zr2 Cl10 90.49(4) . . ? O2 Zr2 Cl12 85.13(7) . . ? Cl14 Zr2 Cl12 95.31(5) . . ? Cl11 Zr2 Cl12 88.76(3) . . ? Cl10 Zr2 Cl12 170.68(4) . . ? O2 Zr2 Cl13 84.25(6) . . ? Cl14 Zr2 Cl13 95.83(4) . . ? Cl11 Zr2 Cl13 169.00(3) . . ? Cl10 Zr2 Cl13 89.24(3) . . ? Cl12 Zr2 Cl13 89.73(3) . . ? C77 O2 C74 108.6(3) . . ? C77 O2 Zr2 127.0(2) . . ? C74 O2 Zr2 124.4(2) . . ? O2 C74 C75 104.8(3) . . ? O2 C74 H74A 110.8 . . ? C75 C74 H74A 110.8 . . ? O2 C74 H74B 110.8 . . ? C75 C74 H74B 110.8 . . ? H74A C74 H74B 108.9 . . ? C74 C75 C76 104.2(3) . . ? C74 C75 H75A 110.9 . . ? C76 C75 H75A 110.9 . . ? C74 C75 H75B 110.9 . . ? C76 C75 H75B 110.9 . . ? H75A C75 H75B 108.9 . . ? C75 C76 C77 104.3(3) . . ? C75 C76 H76A 110.9 . . ? C77 C76 H76A 110.9 . . ? C75 C76 H76B 110.9 . . ? C77 C76 H76B 110.9 . . ? H76A C76 H76B 108.9 . . ? O2 C77 C76 105.6(3) . . ? O2 C77 H77A 110.6 . . ? C76 C77 H77A 110.6 . . ? O2 C77 H77B 110.6 . . ? C76 C77 H77B 110.6 . . ? H77A C77 H77B 108.7 . . ? Cl2 C67 Cl1 112.0 . . ? H67C C67 H67D 113.7 . . ? Cl2B C67B Cl1B 112.0 . . ? Cl2B C67B H67A 118.1 . . ? Cl1B C67B H67A 118.6 . . ? Cl2B C67B H67B 88.4 . . ? Cl1B C67B H67B 112.8 . . ? Cl2B C67B H67C 109.5 . . ? Cl1B C67B H67C 108.2 . . ? Cl2B C67B H67D 109.5 . . ? Cl1B C67B H67D 108.2 . . ? H67C C67B H67D 109.5 . . ? Cl3 C68 Cl4 112.0 . . ? Cl4B C68B Cl3B 112.0 . . ? Cl4B C68B H68A 71.5 . . ? Cl3B C68B H68A 166.7 . . ? Cl4B C68B H68C 109.5 . . ? Cl3B C68B H68C 108.2 . . ? Cl4B C68B H68D 109.5 . . ? Cl3B C68B H68D 108.2 . . ? H68C C68B H68D 109.5 . . ? C68B Cl4B H68B 85.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.302 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.092