# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Fu-Chen Liu' _publ_contact_author_email fcliu@mail.ndhu.edu.tw loop_ _publ_author_name 'Hsueh-Hui Yang' 'Chung-Hsien ChienChien' 'Chien-Chan Yang' 'Fu-Chen Liu' 'Agnes Chang' 'Gene-Hsiang Lee' 'Shie-Ming Peng' data_ic14382 _database_code_depnum_ccdc_archive 'CCDC 890534' #TrackingRef '42.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H84 Cl2 Zr4' _chemical_formula_weight 1168.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5114(2) _cell_length_b 15.0165(3) _cell_length_c 27.4482(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.0312(8) _cell_angle_gamma 90.00 _cell_volume 5569.07(16) _cell_formula_units_Z 4 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 32076 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour ornge-red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32076 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12772 _reflns_number_gt 8397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Two phenyl rings from the toluene solvents are fitted to a regular hexagon (AFIX 63) and two distance restrains are applied for C41-C47 and C48-C54. The FLAT command was used to two toluene solvents to be coplanar. ; _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^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12772 _refine_ls_number_parameters 458 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 0.15189(3) 1.39073(3) 0.771741(15) 0.03224(12) Uani 1 1 d . . . Zr2 Zr 0.23446(3) 1.54519(3) 0.860914(15) 0.03020(12) Uani 1 1 d . . . Zr3 Zr 0.27049(3) 1.34415(3) 0.862991(15) 0.03152(12) Uani 1 1 d . . . Zr4 Zr 0.34741(3) 1.49266(3) 0.769058(15) 0.03088(12) Uani 1 1 d . . . H1 H 0.234(3) 1.297(3) 0.7949(16) 0.046 Uiso 1 1 d . . . H2 H 0.142(3) 1.346(3) 0.8207(15) 0.046 Uiso 1 1 d . . . H3 H 0.175(3) 1.433(3) 0.8897(17) 0.046 Uiso 1 1 d . . . H4 H 0.326(3) 1.458(3) 0.8862(17) 0.046 Uiso 1 1 d . . . H5 H 0.360(3) 1.551(3) 0.8275(17) 0.046 Uiso 1 1 d . . . H6 H 0.269(3) 1.590(3) 0.7949(16) 0.046 Uiso 1 1 d . . . H7 H 0.213(3) 1.503(3) 0.7419(16) 0.046 Uiso 1 1 d . . . H8 H 0.282(3) 1.387(3) 0.7343(16) 0.046 Uiso 1 1 d . . . Cl1 Cl 0.06484(8) 1.52368(8) 0.81632(4) 0.0395(3) Uani 1 1 d . . . Cl2 Cl 0.43733(8) 1.36269(8) 0.81518(4) 0.0387(3) Uani 1 1 d . . . C1 C 0.1000(3) 1.2571(3) 0.72350(17) 0.0391(11) Uani 1 1 d . . . C2 C 0.1159(3) 1.3261(3) 0.68942(17) 0.0421(12) Uani 1 1 d . . . C3 C 0.0427(4) 1.3925(3) 0.6975(2) 0.0485(13) Uani 1 1 d . . . C4 C -0.0182(3) 1.3648(4) 0.73537(19) 0.0463(13) Uani 1 1 d . . . C5 C 0.0157(3) 1.2807(3) 0.75166(17) 0.0410(12) Uani 1 1 d . . . C6 C 0.1535(4) 1.1695(4) 0.7242(2) 0.0595(15) Uani 1 1 d . . . H6A H 0.2200 1.1775 0.7116 0.089 Uiso 1 1 calc R . . H6B H 0.1182 1.1270 0.7040 0.089 Uiso 1 1 calc R . . H6C H 0.1569 1.1475 0.7573 0.089 Uiso 1 1 calc R . . C7 C 0.1885(4) 1.3211(4) 0.6482(2) 0.0702(19) Uani 1 1 d . . . H7A H 0.1549 1.3014 0.6189 0.105 Uiso 1 1 calc R . . H7B H 0.2406 1.2792 0.6564 0.105 Uiso 1 1 calc R . . H7C H 0.2172 1.3795 0.6428 0.105 Uiso 1 1 calc R . . C8 C 0.0257(5) 1.4735(4) 0.6669(3) 0.084(2) Uani 1 1 d . . . H8A H -0.0091 1.5181 0.6859 0.127 Uiso 1 1 calc R . . H8B H -0.0136 1.4577 0.6387 0.127 Uiso 1 1 calc R . . H8C H 0.0889 1.4974 0.6564 0.127 Uiso 1 1 calc R . . C9 C -0.1104(4) 1.4101(4) 0.7539(3) 0.076(2) Uani 1 1 d . . . H9A H -0.0982 1.4337 0.7862 0.114 Uiso 1 1 calc R . . H9B H -0.1642 1.3673 0.7552 0.114 Uiso 1 1 calc R . . H9C H -0.1282 1.4583 0.7320 0.114 Uiso 1 1 calc R . . C10 C -0.0343(4) 1.2201(4) 0.7872(2) 0.0686(18) Uani 1 1 d . . . H10A H -0.0763 1.1785 0.7697 0.103 Uiso 1 1 calc R . . H10B H -0.0744 1.2551 0.8094 0.103 Uiso 1 1 calc R . . H10C H 0.0152 1.1875 0.8055 0.103 Uiso 1 1 calc R . . C11 C 0.2339(4) 1.7101(3) 0.88068(17) 0.0416(12) Uani 1 1 d . . . C12 C 0.1443(4) 1.6750(3) 0.90003(18) 0.0448(12) Uani 1 1 d . . . C13 C 0.1691(3) 1.6155(3) 0.93804(16) 0.0390(11) Uani 1 1 d . . . C14 C 0.2737(3) 1.6143(3) 0.94193(16) 0.0374(11) Uani 1 1 d . . . C15 C 0.3126(4) 1.6724(3) 0.90741(16) 0.0398(11) Uani 1 1 d . . . C16 C 0.2405(5) 1.7830(4) 0.8436(2) 0.075(2) Uani 1 1 d . . . H16A H 0.2280 1.8398 0.8592 0.112 Uiso 1 1 calc R . . H16B H 0.1916 1.7730 0.8183 0.112 Uiso 1 1 calc R . . H16C H 0.3061 1.7833 0.8293 0.112 Uiso 1 1 calc R . . C17 C 0.0422(4) 1.7065(4) 0.8862(2) 0.0715(19) Uani 1 1 d . . . H17A H 0.0362 1.7080 0.8510 0.107 Uiso 1 1 calc R . . H17B H 0.0314 1.7658 0.8992 0.107 Uiso 1 1 calc R . . H17C H -0.0068 1.6661 0.8995 0.107 Uiso 1 1 calc R . . C18 C 0.0935(4) 1.5716(4) 0.9710(2) 0.0628(16) Uani 1 1 d . . . H18A H 0.0710 1.6142 0.9951 0.094 Uiso 1 1 calc R . . H18B H 0.1236 1.5211 0.9873 0.094 Uiso 1 1 calc R . . H18C H 0.0377 1.5515 0.9517 0.094 Uiso 1 1 calc R . . C19 C 0.3317(4) 1.5700(4) 0.98144(19) 0.0578(15) Uani 1 1 d . . . H19A H 0.2926 1.5225 0.9957 0.087 Uiso 1 1 calc R . . H19B H 0.3481 1.6133 1.0064 0.087 Uiso 1 1 calc R . . H19C H 0.3921 1.5454 0.9679 0.087 Uiso 1 1 calc R . . C20 C 0.4211(4) 1.7000(4) 0.9042(2) 0.0641(17) Uani 1 1 d . . . H20A H 0.4629 1.6478 0.9076 0.096 Uiso 1 1 calc R . . H20B H 0.4361 1.7419 0.9300 0.096 Uiso 1 1 calc R . . H20C H 0.4334 1.7278 0.8728 0.096 Uiso 1 1 calc R . . C21 C 0.1957(4) 1.2200(4) 0.9129(2) 0.0550(15) Uani 1 1 d . . . C22 C 0.2383(4) 1.2804(4) 0.94639(18) 0.0486(13) Uani 1 1 d . . . C23 C 0.3414(4) 1.2785(3) 0.93938(18) 0.0464(13) Uani 1 1 d . . . C24 C 0.3616(4) 1.2167(4) 0.90247(18) 0.0489(14) Uani 1 1 d . . . C25 C 0.2716(5) 1.1811(3) 0.88616(19) 0.0540(14) Uani 1 1 d . . . C26 C 0.0875(5) 1.1941(5) 0.9118(3) 0.107(3) Uani 1 1 d . . . H26A H 0.0661 1.1780 0.9443 0.160 Uiso 1 1 calc R . . H26B H 0.0785 1.1436 0.8901 0.160 Uiso 1 1 calc R . . H26C H 0.0484 1.2439 0.9001 0.160 Uiso 1 1 calc R . . C27 C 0.1824(6) 1.3263(5) 0.9861(2) 0.096(3) Uani 1 1 d . . . H27A H 0.1792 1.2879 1.0144 0.143 Uiso 1 1 calc R . . H27B H 0.1158 1.3395 0.9749 0.143 Uiso 1 1 calc R . . H27C H 0.2158 1.3813 0.9946 0.143 Uiso 1 1 calc R . . C28 C 0.4199(5) 1.3235(5) 0.9701(2) 0.086(2) Uani 1 1 d . . . H28A H 0.4694 1.3499 0.9489 0.130 Uiso 1 1 calc R . . H28B H 0.4510 1.2799 0.9911 0.130 Uiso 1 1 calc R . . H28C H 0.3895 1.3697 0.9898 0.130 Uiso 1 1 calc R . . C29 C 0.4646(5) 1.1845(5) 0.8877(3) 0.098(3) Uani 1 1 d . . . H29A H 0.4593 1.1463 0.8593 0.147 Uiso 1 1 calc R . . H29B H 0.4939 1.1513 0.9144 0.147 Uiso 1 1 calc R . . H29C H 0.5060 1.2353 0.8800 0.147 Uiso 1 1 calc R . . C30 C 0.2625(7) 1.1049(4) 0.8499(3) 0.124(4) Uani 1 1 d . . . H30A H 0.2806 1.0495 0.8657 0.186 Uiso 1 1 calc R . . H30B H 0.3063 1.1156 0.8226 0.186 Uiso 1 1 calc R . . H30C H 0.1948 1.1012 0.8384 0.186 Uiso 1 1 calc R . . C31 C 0.4829(3) 1.6016(3) 0.74561(17) 0.0378(11) Uani 1 1 d . . . C32 C 0.5143(4) 1.5153(3) 0.72923(19) 0.0454(13) Uani 1 1 d . . . C33 C 0.4497(4) 1.4867(3) 0.69223(18) 0.0424(12) Uani 1 1 d . . . C34 C 0.3785(4) 1.5541(3) 0.68452(17) 0.0433(12) Uani 1 1 d . . . C35 C 0.3976(3) 1.6244(3) 0.71845(17) 0.0366(11) Uani 1 1 d . . . C36 C 0.5383(4) 1.6624(4) 0.77956(19) 0.0564(15) Uani 1 1 d . . . H36A H 0.5865 1.6966 0.7612 0.085 Uiso 1 1 calc R . . H36B H 0.5719 1.6273 0.8041 0.085 Uiso 1 1 calc R . . H36C H 0.4920 1.7027 0.7952 0.085 Uiso 1 1 calc R . . C37 C 0.6078(4) 1.4675(4) 0.7450(3) 0.074(2) Uani 1 1 d . . . H37A H 0.6018 1.4045 0.7377 0.111 Uiso 1 1 calc R . . H37B H 0.6173 1.4753 0.7798 0.111 Uiso 1 1 calc R . . H37C H 0.6641 1.4920 0.7277 0.111 Uiso 1 1 calc R . . C38 C 0.4648(5) 1.4044(4) 0.6627(2) 0.077(2) Uani 1 1 d . . . H38A H 0.4735 1.3538 0.6843 0.116 Uiso 1 1 calc R . . H38B H 0.5233 1.4112 0.6426 0.116 Uiso 1 1 calc R . . H38C H 0.4075 1.3946 0.6421 0.116 Uiso 1 1 calc R . . C39 C 0.3032(5) 1.5589(4) 0.6444(2) 0.0658(18) Uani 1 1 d . . . H39A H 0.3357 1.5752 0.6141 0.099 Uiso 1 1 calc R . . H39B H 0.2537 1.6032 0.6524 0.099 Uiso 1 1 calc R . . H39C H 0.2717 1.5012 0.6406 0.099 Uiso 1 1 calc R . . C40 C 0.3461(2) 1.7121(2) 0.71847(10) 0.0552(15) Uani 1 1 d . . . H40A H 0.2790 1.7046 0.7066 0.083 Uiso 1 1 calc R . . H40B H 0.3813 1.7532 0.6975 0.083 Uiso 1 1 calc R . . H40C H 0.3445 1.7356 0.7514 0.083 Uiso 1 1 calc R . . C41 C 0.2307(2) 1.6049(2) 1.10764(10) 0.165(4) Uiso 1 1 d RD . . C42 C 0.1694(2) 1.5309(2) 1.10389(10) 0.107(3) Uiso 1 1 d RD . . H42A H 0.1006 1.5384 1.1008 0.128 Uiso 1 1 calc R . . C43 C 0.2098(2) 1.4458(2) 1.10467(10) 0.161(4) Uiso 1 1 d RD . . H43A H 0.1684 1.3957 1.1021 0.193 Uiso 1 1 calc R . . C44 C 0.3116(2) 1.4347(2) 1.10920(10) 0.117(3) Uiso 1 1 d RD . . H44A H 0.3389 1.3772 1.1097 0.141 Uiso 1 1 calc R . . C45 C 0.3729(2) 1.5087(2) 1.11296(10) 0.123(3) Uiso 1 1 d RD . . H45A H 0.4416 1.5013 1.1160 0.148 Uiso 1 1 calc R . . C46 C 0.3324(2) 1.5938(2) 1.11217(10) 0.090(2) Uiso 1 1 d RD . . H46A H 0.3739 1.6439 1.1147 0.108 Uiso 1 1 calc R . . C47 C 0.1825(4) 1.6857(4) 1.10475(15) 0.164(4) Uiso 1 1 d D . . H47A H 0.1117 1.6758 1.1026 0.246 Uiso 1 1 calc R . . H47B H 0.2048 1.7175 1.0760 0.246 Uiso 1 1 calc R . . H47C H 0.1972 1.7207 1.1336 0.246 Uiso 1 1 calc R . . C48 C 0.2698(4) 1.0227(4) 1.00326(15) 0.256(8) Uiso 1 1 d RD . . C49 C 0.1689(4) 1.0231(4) 1.01308(15) 0.334(8) Uiso 1 1 d RD . . H49A H 0.1377 1.0761 1.0230 0.401 Uiso 1 1 calc R . . C50 C 0.1142(4) 0.9452(4) 1.00828(15) 0.334(8) Uiso 1 1 d RD . . H50A H 0.0459 0.9455 1.0149 0.401 Uiso 1 1 calc R . . C51 C 0.1603(4) 0.8670(4) 0.99366(15) 0.294(9) Uiso 1 1 d RD . . H51A H 0.1233 0.8143 0.9904 0.353 Uiso 1 1 calc R . . C52 C 0.2612(4) 0.8665(4) 0.98384(15) 0.255(8) Uiso 1 1 d RD . . H52A H 0.2924 0.8136 0.9740 0.306 Uiso 1 1 calc R . . C53 C 0.3160(4) 0.9444(4) 0.98865(15) 0.296(10) Uiso 1 1 d RD . . H53A H 0.3842 0.9441 0.9820 0.355 Uiso 1 1 calc R . . C54 C 0.3360(9) 1.0892(9) 1.0066(3) 0.310(10) Uiso 1 1 d D . . H54A H 0.3026 1.1434 1.0165 0.464 Uiso 1 1 calc R . . H54B H 0.3671 1.0983 0.9751 0.464 Uiso 1 1 calc R . . H54C H 0.3861 1.0738 1.0305 0.464 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 0.0305(2) 0.0307(2) 0.0356(2) -0.00285(19) -0.00461(19) -0.00158(18) Zr2 0.0302(2) 0.0297(2) 0.0307(2) -0.00130(18) -0.00202(18) 0.00050(18) Zr3 0.0305(2) 0.0301(2) 0.0340(2) 0.00245(18) -0.00050(19) 0.00052(18) Zr4 0.0303(2) 0.0298(2) 0.0326(2) 0.00133(18) 0.00076(18) -0.00123(18) Cl1 0.0325(6) 0.0394(6) 0.0467(7) -0.0066(5) -0.0066(5) 0.0041(5) Cl2 0.0332(6) 0.0392(6) 0.0436(6) 0.0044(5) 0.0026(5) 0.0037(5) C1 0.037(3) 0.034(3) 0.046(3) -0.009(2) -0.012(2) -0.002(2) C2 0.041(3) 0.044(3) 0.041(3) -0.008(2) -0.005(2) -0.011(2) C3 0.055(3) 0.032(3) 0.058(3) -0.005(2) -0.031(3) -0.002(2) C4 0.030(3) 0.051(3) 0.058(3) -0.022(3) -0.015(2) 0.004(2) C5 0.033(3) 0.043(3) 0.047(3) -0.009(2) -0.005(2) -0.010(2) C6 0.062(4) 0.042(3) 0.075(4) -0.019(3) -0.018(3) 0.008(3) C7 0.067(4) 0.086(5) 0.058(4) -0.020(3) 0.009(3) -0.027(4) C8 0.112(6) 0.050(4) 0.091(5) 0.003(3) -0.063(4) -0.001(4) C9 0.040(3) 0.076(5) 0.111(5) -0.045(4) -0.020(3) 0.016(3) C10 0.058(4) 0.081(5) 0.067(4) -0.006(3) 0.003(3) -0.035(3) C11 0.058(3) 0.030(3) 0.037(3) -0.003(2) -0.004(2) 0.003(2) C12 0.048(3) 0.042(3) 0.044(3) -0.014(2) -0.009(2) 0.013(2) C13 0.041(3) 0.041(3) 0.035(2) -0.010(2) 0.001(2) 0.001(2) C14 0.041(3) 0.038(3) 0.033(2) -0.008(2) -0.005(2) 0.007(2) C15 0.046(3) 0.038(3) 0.036(3) -0.009(2) 0.000(2) -0.004(2) C16 0.136(6) 0.035(3) 0.054(4) 0.003(3) -0.004(4) 0.000(4) C17 0.055(4) 0.075(4) 0.084(4) -0.027(4) -0.024(3) 0.027(3) C18 0.058(4) 0.066(4) 0.065(4) -0.010(3) 0.025(3) -0.001(3) C19 0.070(4) 0.065(4) 0.038(3) -0.004(3) -0.011(3) 0.013(3) C20 0.055(3) 0.070(4) 0.068(4) -0.021(3) -0.001(3) -0.018(3) C21 0.048(3) 0.052(3) 0.064(4) 0.026(3) -0.010(3) -0.010(3) C22 0.056(3) 0.053(3) 0.038(3) 0.015(2) 0.014(2) 0.021(3) C23 0.051(3) 0.042(3) 0.046(3) 0.015(2) -0.012(2) -0.005(2) C24 0.055(3) 0.048(3) 0.043(3) 0.020(3) 0.014(3) 0.018(3) C25 0.085(4) 0.035(3) 0.042(3) 0.006(2) -0.009(3) 0.002(3) C26 0.057(4) 0.131(7) 0.131(7) 0.075(6) -0.027(4) -0.035(4) C27 0.156(7) 0.080(5) 0.051(4) 0.022(3) 0.042(4) 0.048(5) C28 0.103(6) 0.081(5) 0.075(4) 0.022(4) -0.045(4) -0.012(4) C29 0.080(5) 0.106(6) 0.107(6) 0.056(5) 0.037(4) 0.058(4) C30 0.263(11) 0.034(4) 0.075(5) -0.002(3) -0.052(6) 0.002(5) C31 0.035(3) 0.039(3) 0.040(3) 0.003(2) 0.004(2) -0.007(2) C32 0.040(3) 0.044(3) 0.053(3) 0.016(2) 0.014(2) 0.007(2) C33 0.052(3) 0.030(3) 0.045(3) 0.002(2) 0.017(3) -0.003(2) C34 0.046(3) 0.047(3) 0.037(3) 0.007(2) -0.001(2) -0.009(2) C35 0.029(2) 0.033(3) 0.047(3) 0.006(2) 0.002(2) -0.0020(19) C36 0.048(3) 0.066(4) 0.055(3) -0.001(3) 0.001(3) -0.022(3) C37 0.040(3) 0.087(5) 0.095(5) 0.045(4) 0.023(3) 0.025(3) C38 0.105(5) 0.051(4) 0.076(4) -0.014(3) 0.043(4) -0.009(4) C39 0.073(4) 0.082(5) 0.042(3) 0.017(3) -0.011(3) -0.033(3) C40 0.053(3) 0.037(3) 0.075(4) 0.012(3) 0.020(3) 0.005(2) _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 C1 2.504(4) . ? Zr1 C2 2.507(5) . ? Zr1 C3 2.515(5) . ? Zr1 C5 2.533(4) . ? Zr1 C4 2.536(5) . ? Zr1 Cl1 2.6206(12) . ? Zr1 Zr3 3.0539(6) . ? Zr1 Zr4 3.0541(6) . ? Zr1 Zr2 3.5514(6) . ? Zr1 H1 1.90(5) . ? Zr1 H2 1.51(4) . ? Zr1 H7 2.06(4) . ? Zr1 H8 2.04(4) . ? Zr2 C14 2.510(4) . ? Zr2 C13 2.525(4) . ? Zr2 C15 2.527(5) . ? Zr2 C11 2.534(5) . ? Zr2 C12 2.537(5) . ? Zr2 Cl1 2.6176(12) . ? Zr2 Zr4 3.0516(6) . ? Zr2 Zr3 3.0585(6) . ? Zr2 H3 2.03(4) . ? Zr2 H4 1.93(5) . ? Zr2 H5 1.93(4) . ? Zr2 H6 1.99(4) . ? Zr3 C23 2.507(5) . ? Zr3 C24 2.520(5) . ? Zr3 C22 2.520(5) . ? Zr3 C21 2.524(5) . ? Zr3 C25 2.530(5) . ? Zr3 Cl2 2.6239(12) . ? Zr3 Zr4 3.5643(6) . ? Zr3 H1 2.06(4) . ? Zr3 H2 2.09(5) . ? Zr3 H3 2.00(4) . ? Zr3 H4 1.97(5) . ? Zr4 C35 2.511(4) . ? Zr4 C33 2.524(4) . ? Zr4 C32 2.530(5) . ? Zr4 C34 2.532(5) . ? Zr4 C31 2.539(4) . ? Zr4 Cl2 2.6241(12) . ? Zr4 H5 1.84(5) . ? Zr4 H6 1.95(4) . ? Zr4 H7 1.96(5) . ? Zr4 H8 2.05(5) . ? C1 C2 1.412(7) . ? C1 C5 1.421(6) . ? C1 C6 1.501(7) . ? C2 C3 1.422(7) . ? C2 C7 1.499(7) . ? C3 C4 1.390(7) . ? C3 C8 1.496(8) . ? C4 C5 1.416(7) . ? C4 C9 1.508(7) . ? C5 C10 1.496(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C15 1.409(7) . ? C11 C12 1.424(7) . ? C11 C16 1.498(7) . ? C12 C13 1.414(7) . ? C12 C17 1.507(7) . ? C13 C14 1.417(6) . ? C13 C18 1.515(7) . ? C14 C15 1.391(7) . ? C14 C19 1.494(7) . ? C15 C20 1.527(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 C25 1.390(8) . ? C21 C22 1.414(8) . ? C21 C26 1.513(8) . ? C22 C23 1.407(7) . ? C22 C27 1.494(7) . ? C23 C24 1.401(7) . ? C23 C28 1.512(8) . ? C24 C25 1.401(8) . ? C24 C29 1.529(7) . ? C25 C30 1.520(8) . ? 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 C35 1.414(6) . ? C31 C32 1.436(7) . ? C31 C36 1.504(7) . ? C32 C33 1.407(7) . ? C32 C37 1.516(7) . ? C33 C34 1.412(7) . ? C33 C38 1.491(7) . ? C34 C35 1.432(7) . ? C34 C39 1.501(7) . ? C35 C40 1.489(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? 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 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 C47 1.379(7) . ? C41 C42 1.3899 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 H42A 0.9400 . ? C43 C44 1.3900 . ? C43 H43A 0.9400 . ? C44 C45 1.3899 . ? C44 H44A 0.9400 . ? C45 C46 1.3900 . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 C54 1.343(11) . ? C48 C53 1.3898 . ? C48 C49 1.3901 . ? C49 C50 1.3900 . ? C49 H49A 0.9400 . ? C50 C51 1.3900 . ? C50 H50A 0.9400 . ? C51 C52 1.3900 . ? C51 H51A 0.9400 . ? C52 C53 1.3901 . ? C52 H52A 0.9400 . ? C53 H53A 0.9400 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 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 C1 Zr1 C2 32.74(15) . . ? C1 Zr1 C3 54.27(16) . . ? C2 Zr1 C3 32.90(16) . . ? C1 Zr1 C5 32.76(15) . . ? C2 Zr1 C5 53.89(15) . . ? C3 Zr1 C5 53.49(16) . . ? C1 Zr1 C4 54.20(15) . . ? C2 Zr1 C4 53.86(15) . . ? C3 Zr1 C4 31.95(17) . . ? C5 Zr1 C4 32.44(16) . . ? C1 Zr1 Cl1 137.03(11) . . ? C2 Zr1 Cl1 128.98(12) . . ? C3 Zr1 Cl1 96.15(12) . . ? C5 Zr1 Cl1 105.81(11) . . ? C4 Zr1 Cl1 83.92(11) . . ? C1 Zr1 Zr3 113.38(11) . . ? C2 Zr1 Zr3 138.76(12) . . ? C3 Zr1 Zr3 166.94(12) . . ? C5 Zr1 Zr3 114.19(12) . . ? C4 Zr1 Zr3 139.71(13) . . ? Cl1 Zr1 Zr3 91.55(3) . . ? C1 Zr1 Zr4 129.12(11) . . ? C2 Zr1 Zr4 109.86(11) . . ? C3 Zr1 Zr4 118.83(13) . . ? C5 Zr1 Zr4 161.75(11) . . ? C4 Zr1 Zr4 148.38(14) . . ? Cl1 Zr1 Zr4 91.03(3) . . ? Zr3 Zr1 Zr4 71.402(15) . . ? C1 Zr1 Zr2 167.31(11) . . ? C2 Zr1 Zr2 159.22(11) . . ? C3 Zr1 Zr2 137.34(12) . . ? C5 Zr1 Zr2 143.50(11) . . ? C4 Zr1 Zr2 131.01(11) . . ? Cl1 Zr1 Zr2 47.28(3) . . ? Zr3 Zr1 Zr2 54.538(13) . . ? Zr4 Zr1 Zr2 54.400(12) . . ? C1 Zr1 H1 75.3(14) . . ? C2 Zr1 H1 97.3(13) . . ? C3 Zr1 H1 128.3(14) . . ? C5 Zr1 H1 90.7(14) . . ? C4 Zr1 H1 123.1(14) . . ? Cl1 Zr1 H1 132.1(13) . . ? Zr3 Zr1 H1 41.5(13) . . ? Zr4 Zr1 H1 82.8(13) . . ? Zr2 Zr1 H1 94.1(14) . . ? C1 Zr1 H2 95.2(17) . . ? C2 Zr1 H2 127.9(17) . . ? C3 Zr1 H2 132.4(17) . . ? C5 Zr1 H2 80.7(17) . . ? C4 Zr1 H2 101.6(17) . . ? Cl1 Zr1 H2 83.2(17) . . ? Zr3 Zr1 H2 38.2(17) . . ? Zr4 Zr1 H2 108.8(17) . . ? Zr2 Zr1 H2 72.8(17) . . ? H1 Zr1 H2 55(2) . . ? C1 Zr1 H7 124.2(13) . . ? C2 Zr1 H7 92.2(13) . . ? C3 Zr1 H7 84.6(13) . . ? C5 Zr1 H7 138.1(13) . . ? C4 Zr1 H7 109.7(13) . . ? Cl1 Zr1 H7 74.9(12) . . ? Zr3 Zr1 H7 107.6(13) . . ? Zr4 Zr1 H7 39.5(13) . . ? Zr2 Zr1 H7 67.0(13) . . ? H1 Zr1 H7 120.5(18) . . ? H2 Zr1 H7 139(2) . . ? C1 Zr1 H8 87.3(13) . . ? C2 Zr1 H8 72.6(13) . . ? C3 Zr1 H8 95.6(13) . . ? C5 Zr1 H8 120.0(13) . . ? C4 Zr1 H8 125.4(13) . . ? Cl1 Zr1 H8 130.0(13) . . ? Zr3 Zr1 H8 87.5(13) . . ? Zr4 Zr1 H8 41.8(13) . . ? Zr2 Zr1 H8 95.4(13) . . ? H1 Zr1 H8 69.3(18) . . ? H2 Zr1 H8 121(2) . . ? H7 Zr1 H8 58.1(18) . . ? C14 Zr2 C13 32.68(14) . . ? C14 Zr2 C15 32.05(15) . . ? C13 Zr2 C15 53.63(15) . . ? C14 Zr2 C11 53.64(15) . . ? C13 Zr2 C11 53.94(16) . . ? C15 Zr2 C11 32.33(15) . . ? C14 Zr2 C12 53.75(15) . . ? C13 Zr2 C12 32.44(16) . . ? C15 Zr2 C12 53.58(16) . . ? C11 Zr2 C12 32.61(16) . . ? C14 Zr2 Cl1 130.50(11) . . ? C13 Zr2 Cl1 97.88(11) . . ? C15 Zr2 Cl1 133.99(12) . . ? C11 Zr2 Cl1 102.60(12) . . ? C12 Zr2 Cl1 82.66(12) . . ? C14 Zr2 Zr4 137.17(11) . . ? C13 Zr2 Zr4 167.40(11) . . ? C15 Zr2 Zr4 113.81(11) . . ? C11 Zr2 Zr4 115.52(11) . . ? C12 Zr2 Zr4 142.06(12) . . ? Cl1 Zr2 Zr4 91.14(3) . . ? C14 Zr2 Zr3 110.99(11) . . ? C13 Zr2 Zr3 116.91(12) . . ? C15 Zr2 Zr3 132.07(11) . . ? C11 Zr2 Zr3 163.88(11) . . ? C12 Zr2 Zr3 145.78(12) . . ? Cl1 Zr2 Zr3 91.50(3) . . ? Zr4 Zr2 Zr3 71.374(14) . . ? C14 Zr2 Zr1 161.20(11) . . ? C13 Zr2 Zr1 137.80(11) . . ? C15 Zr2 Zr1 166.51(11) . . ? C11 Zr2 Zr1 141.68(11) . . ? C12 Zr2 Zr1 129.99(11) . . ? Cl1 Zr2 Zr1 47.35(3) . . ? Zr4 Zr2 Zr1 54.466(12) . . ? Zr3 Zr2 Zr1 54.418(13) . . ? C14 Zr2 H3 94.7(13) . . ? C13 Zr2 H3 83.2(13) . . ? C15 Zr2 H3 126.7(13) . . ? C11 Zr2 H3 136.6(13) . . ? C12 Zr2 H3 106.3(13) . . ? Cl1 Zr2 H3 74.4(13) . . ? Zr4 Zr2 H3 107.9(12) . . ? Zr3 Zr2 H3 40.2(12) . . ? Zr1 Zr2 H3 66.5(13) . . ? C14 Zr2 H4 80.2(14) . . ? C13 Zr2 H4 102.0(14) . . ? C15 Zr2 H4 93.8(14) . . ? C11 Zr2 H4 126.1(14) . . ? C12 Zr2 H4 132.7(14) . . ? Cl1 Zr2 H4 130.0(14) . . ? Zr4 Zr2 H4 78.5(13) . . ? Zr3 Zr2 H4 38.7(14) . . ? Zr1 Zr2 H4 90.2(14) . . ? H3 Zr2 H4 63.3(18) . . ? C14 Zr2 H5 102.5(14) . . ? C13 Zr2 H5 133.4(14) . . ? C15 Zr2 H5 80.7(14) . . ? C11 Zr2 H5 93.4(13) . . ? C12 Zr2 H5 126.0(13) . . ? Cl1 Zr2 H5 123.5(14) . . ? Zr4 Zr2 H5 34.8(14) . . ? Zr3 Zr2 H5 85.1(13) . . ? Zr1 Zr2 H5 88.7(14) . . ? H3 Zr2 H5 125.0(18) . . ? H4 Zr2 H5 68.9(19) . . ? C14 Zr2 H6 128.1(14) . . ? C13 Zr2 H6 134.6(13) . . ? C15 Zr2 H6 96.0(14) . . ? C11 Zr2 H6 82.1(13) . . ? C12 Zr2 H6 103.6(13) . . ? Cl1 Zr2 H6 79.7(13) . . ? Zr4 Zr2 H6 38.7(13) . . ? Zr3 Zr2 H6 108.5(13) . . ? Zr1 Zr2 H6 70.6(13) . . ? H3 Zr2 H6 137.0(19) . . ? H4 Zr2 H6 114.2(19) . . ? H5 Zr2 H6 49.2(18) . . ? C23 Zr3 C24 32.36(17) . . ? C23 Zr3 C22 32.52(16) . . ? C24 Zr3 C22 53.49(15) . . ? C23 Zr3 C21 53.79(17) . . ? C24 Zr3 C21 53.24(17) . . ? C22 Zr3 C21 32.56(18) . . ? C23 Zr3 C25 53.63(17) . . ? C24 Zr3 C25 32.22(18) . . ? C22 Zr3 C25 53.47(17) . . ? C21 Zr3 C25 31.93(18) . . ? C23 Zr3 Cl2 97.57(12) . . ? C24 Zr3 Cl2 82.89(11) . . ? C22 Zr3 Cl2 130.06(12) . . ? C21 Zr3 Cl2 133.95(14) . . ? C25 Zr3 Cl2 102.91(15) . . ? C23 Zr3 Zr1 167.50(12) . . ? C24 Zr3 Zr1 141.50(14) . . ? C22 Zr3 Zr1 137.85(13) . . ? C21 Zr3 Zr1 113.82(13) . . ? C25 Zr3 Zr1 115.53(13) . . ? Cl2 Zr3 Zr1 90.92(3) . . ? C23 Zr3 Zr2 117.67(13) . . ? C24 Zr3 Zr2 146.65(14) . . ? C22 Zr3 Zr2 111.38(12) . . ? C21 Zr3 Zr2 132.48(14) . . ? C25 Zr3 Zr2 163.94(13) . . ? Cl2 Zr3 Zr2 91.30(3) . . ? Zr1 Zr3 Zr2 71.044(15) . . ? C23 Zr3 Zr4 137.69(12) . . ? C24 Zr3 Zr4 130.08(11) . . ? C22 Zr3 Zr4 161.02(14) . . ? C21 Zr3 Zr4 166.25(14) . . ? C25 Zr3 Zr4 141.79(13) . . ? Cl2 Zr3 Zr4 47.22(3) . . ? Zr1 Zr3 Zr4 54.302(12) . . ? Zr2 Zr3 Zr4 54.223(12) . . ? C23 Zr3 H1 135.8(13) . . ? C24 Zr3 H1 104.3(13) . . ? C22 Zr3 H1 130.8(13) . . ? C21 Zr3 H1 98.2(13) . . ? C25 Zr3 H1 84.1(13) . . ? Cl2 Zr3 H1 77.8(12) . . ? Zr1 Zr3 H1 37.6(13) . . ? Zr2 Zr3 H1 106.5(13) . . ? Zr4 Zr3 H1 68.2(12) . . ? C23 Zr3 H2 142.0(12) . . ? C24 Zr3 H2 131.0(13) . . ? C22 Zr3 H2 111.5(12) . . ? C21 Zr3 H2 88.8(12) . . ? C25 Zr3 H2 99.1(13) . . ? Cl2 Zr3 H2 115.8(11) . . ? Zr1 Zr3 H2 26.5(12) . . ? Zr2 Zr3 H2 80.9(12) . . ? Zr4 Zr3 H2 80.3(12) . . ? H1 Zr3 H2 45.6(16) . . ? C23 Zr3 H3 101.7(13) . . ? C24 Zr3 H3 131.7(13) . . ? C22 Zr3 H3 78.9(13) . . ? C21 Zr3 H3 92.0(13) . . ? C25 Zr3 H3 123.9(13) . . ? Cl2 Zr3 H3 132.0(13) . . ? Zr1 Zr3 H3 78.9(13) . . ? Zr2 Zr3 H3 41.0(13) . . ? Zr4 Zr3 H3 92.1(13) . . ? H1 Zr3 H3 113.9(18) . . ? H2 Zr3 H3 69.8(18) . . ? C23 Zr3 H4 85.7(14) . . ? C24 Zr3 H4 109.5(14) . . ? C22 Zr3 H4 95.8(14) . . ? C21 Zr3 H4 128.1(13) . . ? C25 Zr3 H4 139.0(14) . . ? Cl2 Zr3 H4 75.1(13) . . ? Zr1 Zr3 H4 105.5(14) . . ? Zr2 Zr3 H4 38.0(13) . . ? Zr4 Zr3 H4 65.2(14) . . ? H1 Zr3 H4 133.0(19) . . ? H2 Zr3 H4 118.9(18) . . ? H3 Zr3 H4 63.3(18) . . ? C35 Zr4 C33 54.38(15) . . ? C35 Zr4 C32 54.10(15) . . ? C33 Zr4 C32 32.33(17) . . ? C35 Zr4 C34 32.98(15) . . ? C33 Zr4 C34 32.43(16) . . ? C32 Zr4 C34 53.60(16) . . ? C35 Zr4 C31 32.51(15) . . ? C33 Zr4 C31 54.25(15) . . ? C32 Zr4 C31 32.91(16) . . ? C34 Zr4 C31 54.04(15) . . ? C35 Zr4 Cl2 136.69(11) . . ? C33 Zr4 Cl2 97.07(12) . . ? C32 Zr4 Cl2 84.03(11) . . ? C34 Zr4 Cl2 129.48(12) . . ? C31 Zr4 Cl2 105.54(11) . . ? C35 Zr4 Zr2 112.88(11) . . ? C33 Zr4 Zr2 166.90(11) . . ? C32 Zr4 Zr2 140.22(13) . . ? C34 Zr4 Zr2 138.27(12) . . ? C31 Zr4 Zr2 113.82(11) . . ? Cl2 Zr4 Zr2 91.45(3) . . ? C35 Zr4 Zr1 129.96(11) . . ? C33 Zr4 Zr1 118.45(12) . . ? C32 Zr4 Zr1 148.13(13) . . ? C34 Zr4 Zr1 110.41(11) . . ? C31 Zr4 Zr1 162.38(11) . . ? Cl2 Zr4 Zr1 90.91(3) . . ? Zr2 Zr4 Zr1 71.133(14) . . ? C35 Zr4 Zr3 166.44(11) . . ? C33 Zr4 Zr3 137.92(11) . . ? C32 Zr4 Zr3 131.08(11) . . ? C34 Zr4 Zr3 159.94(11) . . ? C31 Zr4 Zr3 142.87(11) . . ? Cl2 Zr4 Zr3 47.22(3) . . ? Zr2 Zr4 Zr3 54.403(12) . . ? Zr1 Zr4 Zr3 54.296(12) . . ? C35 Zr4 H5 94.7(14) . . ? C33 Zr4 H5 134.1(14) . . ? C32 Zr4 H5 103.3(14) . . ? C34 Zr4 H5 127.7(14) . . ? C31 Zr4 H5 81.2(14) . . ? Cl2 Zr4 H5 83.7(14) . . ? Zr2 Zr4 H5 37.0(14) . . ? Zr1 Zr4 H5 107.4(14) . . ? Zr3 Zr4 H5 72.2(14) . . ? C35 Zr4 H6 75.9(13) . . ? C33 Zr4 H6 129.1(13) . . ? C32 Zr4 H6 122.9(13) . . ? C34 Zr4 H6 98.7(13) . . ? C31 Zr4 H6 90.1(13) . . ? Cl2 Zr4 H6 129.6(13) . . ? Zr2 Zr4 H6 39.7(13) . . ? Zr1 Zr4 H6 84.0(14) . . ? Zr3 Zr4 H6 92.8(13) . . ? H5 Zr4 H6 51.1(19) . . ? C35 Zr4 H7 88.5(13) . . ? C33 Zr4 H7 101.0(13) . . ? C32 Zr4 H7 130.3(13) . . ? C34 Zr4 H7 77.1(13) . . ? C31 Zr4 H7 121.0(13) . . ? Cl2 Zr4 H7 132.1(13) . . ? Zr2 Zr4 H7 80.2(13) . . ? Zr1 Zr4 H7 41.7(13) . . ? Zr3 Zr4 H7 93.2(13) . . ? H5 Zr4 H7 112.1(19) . . ? H6 Zr4 H7 64.7(19) . . ? C35 Zr4 H8 117.9(12) . . ? C33 Zr4 H8 79.7(12) . . ? C32 Zr4 H8 106.8(12) . . ? C34 Zr4 H8 85.8(12) . . ? C31 Zr4 H8 133.8(12) . . ? Cl2 Zr4 H8 81.3(13) . . ? Zr2 Zr4 H8 111.6(12) . . ? Zr1 Zr4 H8 41.4(12) . . ? Zr3 Zr4 H8 74.1(12) . . ? H5 Zr4 H8 144.6(19) . . ? H6 Zr4 H8 121.1(18) . . ? H7 Zr4 H8 59.3(18) . . ? Zr2 Cl1 Zr1 85.37(3) . . ? Zr3 Cl2 Zr4 85.56(3) . . ? C2 C1 C5 107.5(4) . . ? C2 C1 C6 125.2(5) . . ? C5 C1 C6 126.7(5) . . ? C2 C1 Zr1 73.7(3) . . ? C5 C1 Zr1 74.8(3) . . ? C6 C1 Zr1 124.1(3) . . ? C1 C2 C3 107.7(4) . . ? C1 C2 C7 124.3(5) . . ? C3 C2 C7 127.5(5) . . ? C1 C2 Zr1 73.5(3) . . ? C3 C2 Zr1 73.9(3) . . ? C7 C2 Zr1 124.9(3) . . ? C4 C3 C2 108.6(5) . . ? C4 C3 C8 124.9(5) . . ? C2 C3 C8 126.1(6) . . ? C4 C3 Zr1 74.9(3) . . ? C2 C3 Zr1 73.2(3) . . ? C8 C3 Zr1 123.6(4) . . ? C3 C4 C5 108.1(4) . . ? C3 C4 C9 127.3(5) . . ? C5 C4 C9 124.3(5) . . ? C3 C4 Zr1 73.2(3) . . ? C5 C4 Zr1 73.7(3) . . ? C9 C4 Zr1 123.2(3) . . ? C4 C5 C1 108.1(4) . . ? C4 C5 C10 127.0(5) . . ? C1 C5 C10 124.5(5) . . ? C4 C5 Zr1 73.9(3) . . ? C1 C5 Zr1 72.5(2) . . ? C10 C5 Zr1 125.7(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 107.4(4) . . ? C15 C11 C16 127.1(5) . . ? C12 C11 C16 125.1(5) . . ? C15 C11 Zr2 73.6(3) . . ? C12 C11 Zr2 73.8(3) . . ? C16 C11 Zr2 124.6(3) . . ? C13 C12 C11 107.9(4) . . ? C13 C12 C17 126.9(5) . . ? C11 C12 C17 124.7(5) . . ? C13 C12 Zr2 73.3(3) . . ? C11 C12 Zr2 73.6(3) . . ? C17 C12 Zr2 125.1(3) . . ? C12 C13 C14 107.4(4) . . ? C12 C13 C18 123.8(5) . . ? C14 C13 C18 128.5(5) . . ? C12 C13 Zr2 74.2(3) . . ? C14 C13 Zr2 73.1(2) . . ? C18 C13 Zr2 123.7(3) . . ? C15 C14 C13 108.6(4) . . ? C15 C14 C19 125.1(5) . . ? C13 C14 C19 125.7(5) . . ? C15 C14 Zr2 74.6(3) . . ? C13 C14 Zr2 74.2(3) . . ? C19 C14 Zr2 124.7(3) . . ? C14 C15 C11 108.8(4) . . ? C14 C15 C20 125.0(5) . . ? C11 C15 C20 125.8(5) . . ? C14 C15 Zr2 73.3(3) . . ? C11 C15 Zr2 74.1(3) . . ? C20 C15 Zr2 125.2(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 108.2(5) . . ? C25 C21 C26 126.5(6) . . ? C22 C21 C26 124.8(6) . . ? C25 C21 Zr3 74.3(3) . . ? C22 C21 Zr3 73.5(3) . . ? C26 C21 Zr3 124.5(4) . . ? C23 C22 C21 107.5(5) . . ? C23 C22 C27 127.6(6) . . ? C21 C22 C27 124.4(6) . . ? C23 C22 Zr3 73.2(3) . . ? C21 C22 Zr3 73.9(3) . . ? C27 C22 Zr3 125.0(4) . . ? C24 C23 C22 107.7(5) . . ? C24 C23 C28 124.2(5) . . ? C22 C23 C28 127.5(5) . . ? C24 C23 Zr3 74.3(3) . . ? C22 C23 Zr3 74.2(3) . . ? C28 C23 Zr3 123.9(4) . . ? C25 C24 C23 108.4(5) . . ? C25 C24 C29 125.8(6) . . ? C23 C24 C29 125.3(6) . . ? C25 C24 Zr3 74.3(3) . . ? C23 C24 Zr3 73.3(3) . . ? C29 C24 Zr3 124.8(3) . . ? C21 C25 C24 108.1(5) . . ? C21 C25 C30 127.0(7) . . ? C24 C25 C30 124.5(6) . . ? C21 C25 Zr3 73.8(3) . . ? C24 C25 Zr3 73.5(3) . . ? C30 C25 Zr3 124.3(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C35 C31 C32 107.1(4) . . ? C35 C31 C36 125.8(5) . . ? C32 C31 C36 126.5(5) . . ? C35 C31 Zr4 72.7(3) . . ? C32 C31 Zr4 73.2(3) . . ? C36 C31 Zr4 126.4(3) . . ? C33 C32 C31 108.6(4) . . ? C33 C32 C37 125.3(5) . . ? C31 C32 C37 125.8(5) . . ? C33 C32 Zr4 73.6(3) . . ? C31 C32 Zr4 73.9(3) . . ? C37 C32 Zr4 123.7(3) . . ? C32 C33 C34 108.1(4) . . ? C32 C33 C38 124.1(5) . . ? C34 C33 C38 127.3(5) . . ? C32 C33 Zr4 74.1(3) . . ? C34 C33 Zr4 74.1(3) . . ? C38 C33 Zr4 123.9(3) . . ? C33 C34 C35 108.0(4) . . ? C33 C34 C39 127.2(5) . . ? C35 C34 C39 124.4(5) . . ? C33 C34 Zr4 73.4(3) . . ? C35 C34 Zr4 72.7(3) . . ? C39 C34 Zr4 125.3(3) . . ? C31 C35 C34 108.1(4) . . ? C31 C35 C40 126.5(4) . . ? C34 C35 C40 124.6(4) . . ? C31 C35 Zr4 74.8(3) . . ? C34 C35 Zr4 74.3(3) . . ? C40 C35 Zr4 124.7(3) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? 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 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C47 C41 C42 114.7(3) . . ? C47 C41 C46 125.2(3) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C54 C48 C53 110.5(7) . . ? C54 C48 C49 129.5(7) . . ? C53 C48 C49 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C51 C50 C49 120.0 . . ? C51 C50 H50A 120.0 . . ? C49 C50 H50A 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C48 C53 C52 120.0 . . ? C48 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C48 C54 H54A 109.5 . . ? C48 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C48 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.378 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.238 # =============================================== END data_ic14461 _database_code_depnum_ccdc_archive 'CCDC 890536' #TrackingRef '42.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H66 Zr4' _chemical_formula_weight 911.81 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' Zr Zr -2.9673 0.5597 '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 11.3501(7) _cell_length_b 11.4160(7) _cell_length_c 18.7944(12) _cell_angle_alpha 82.9518(16) _cell_angle_beta 82.0425(14) _cell_angle_gamma 65.2804(13) _cell_volume 2185.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2539 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 22.81 _exptl_crystal_description plate _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8706 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23159 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7712 _reflns_number_gt 6038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0355P)^2^+12.2434P] 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 7712 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1523 _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_restrained_S_all 1.210 _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 0.76179(9) 0.67951(8) 0.18059(5) 0.0235(2) Uani 1 1 d . . . Zr2 Zr 0.69000(9) 0.94735(8) 0.23190(5) 0.0234(2) Uani 1 1 d . . . Zr3 Zr 0.73182(9) 0.71378(9) 0.34158(5) 0.0252(2) Uani 1 1 d . . . Zr4 Zr 0.48964(9) 0.82639(9) 0.25646(5) 0.0251(2) Uani 1 1 d . . . H1 H 0.763(8) 0.845(8) 0.154(4) 0.030 Uiso 1 1 d . . . H2 H 0.843(8) 0.577(8) 0.267(4) 0.030 Uiso 1 1 d . . . H3 H 0.576(8) 0.746(8) 0.171(4) 0.030 Uiso 1 1 d . . . H4 H 0.750(8) 0.899(8) 0.343(4) 0.030 Uiso 1 1 d . . . H5 H 0.509(8) 0.992(8) 0.236(4) 0.030 Uiso 1 1 d . . . H6 H 0.529(8) 0.724(8) 0.368(4) 0.030 Uiso 1 1 d . . . C1 C 0.8900(12) 0.4591(10) 0.1389(6) 0.048(3) Uani 1 1 d . . . C2 C 0.9691(11) 0.5262(12) 0.1224(7) 0.050(3) Uani 1 1 d . . . C3 C 0.9132(15) 0.6234(12) 0.0682(7) 0.061(4) Uani 1 1 d . . . C4 C 0.7973(14) 0.6163(11) 0.0547(6) 0.054(3) Uani 1 1 d . . . C5 C 0.7856(11) 0.5119(11) 0.0979(6) 0.045(3) Uani 1 1 d . . . C6 C 0.917(2) 0.3393(11) 0.1906(8) 0.113(7) Uani 1 1 d . . . H6A H 0.8356 0.3308 0.2077 0.170 Uiso 1 1 calc R . . H6B H 0.9573 0.3473 0.2318 0.170 Uiso 1 1 calc R . . H6C H 0.9771 0.2626 0.1657 0.170 Uiso 1 1 calc R . . C7 C 1.0974(15) 0.493(2) 0.1509(11) 0.160(11) Uani 1 1 d . . . H7A H 1.0996 0.4460 0.1983 0.240 Uiso 1 1 calc R . . H7B H 1.1080 0.5727 0.1553 0.240 Uiso 1 1 calc R . . H7C H 1.1684 0.4387 0.1177 0.240 Uiso 1 1 calc R . . C8 C 0.974(2) 0.7120(16) 0.0284(10) 0.139(10) Uani 1 1 d . . . H8A H 1.0120 0.6821 -0.0196 0.209 Uiso 1 1 calc R . . H8B H 1.0425 0.7107 0.0555 0.209 Uiso 1 1 calc R . . H8C H 0.9069 0.8004 0.0237 0.209 Uiso 1 1 calc R . . C9 C 0.706(2) 0.7044(16) 0.0004(7) 0.143(10) Uani 1 1 d . . . H9A H 0.7555 0.7355 -0.0384 0.214 Uiso 1 1 calc R . . H9B H 0.6380 0.7782 0.0242 0.214 Uiso 1 1 calc R . . H9C H 0.6660 0.6564 -0.0199 0.214 Uiso 1 1 calc R . . C10 C 0.6835(14) 0.4635(16) 0.0956(11) 0.123(8) Uani 1 1 d . . . H10A H 0.6578 0.4360 0.1445 0.184 Uiso 1 1 calc R . . H10B H 0.7178 0.3900 0.0654 0.184 Uiso 1 1 calc R . . H10C H 0.6074 0.5327 0.0753 0.184 Uiso 1 1 calc R . . C11 C 0.6041(10) 1.1881(9) 0.1981(7) 0.040(3) Uani 1 1 d . . . C12 C 0.6993(13) 1.1248(10) 0.1434(6) 0.048(3) Uani 1 1 d . . . C13 C 0.8178(11) 1.0695(10) 0.1706(7) 0.047(3) Uani 1 1 d . . . C14 C 0.8004(11) 1.0908(10) 0.2439(7) 0.044(3) Uani 1 1 d . . . C15 C 0.6670(11) 1.1643(9) 0.2605(6) 0.039(3) Uani 1 1 d . . . C16 C 0.4614(14) 1.2710(12) 0.1893(10) 0.099(6) Uani 1 1 d . . . H16A H 0.4501 1.3597 0.1732 0.148 Uiso 1 1 calc R . . H16B H 0.4096 1.2708 0.2355 0.148 Uiso 1 1 calc R . . H16C H 0.4325 1.2359 0.1534 0.148 Uiso 1 1 calc R . . C17 C 0.671(2) 1.1358(15) 0.0656(7) 0.105(7) Uani 1 1 d . . . H17A H 0.7315 1.0575 0.0423 0.158 Uiso 1 1 calc R . . H17B H 0.6819 1.2113 0.0400 0.158 Uiso 1 1 calc R . . H17C H 0.5813 1.1456 0.0643 0.158 Uiso 1 1 calc R . . C18 C 0.9516(14) 1.0035(13) 0.1270(10) 0.102(7) Uani 1 1 d . . . H18A H 0.9401 0.9688 0.0845 0.153 Uiso 1 1 calc R . . H18B H 1.0103 0.9329 0.1572 0.153 Uiso 1 1 calc R . . H18C H 0.9890 1.0670 0.1117 0.153 Uiso 1 1 calc R . . C19 C 0.9120(15) 1.0500(13) 0.2927(9) 0.099(7) Uani 1 1 d . . . H19A H 0.9511 1.1131 0.2848 0.149 Uiso 1 1 calc R . . H19B H 0.9784 0.9645 0.2811 0.149 Uiso 1 1 calc R . . H19C H 0.8772 1.0466 0.3433 0.149 Uiso 1 1 calc R . . C20 C 0.6028(17) 1.2192(13) 0.3323(7) 0.085(5) Uani 1 1 d . . . H20A H 0.5954 1.3080 0.3314 0.128 Uiso 1 1 calc R . . H20B H 0.6556 1.1660 0.3708 0.128 Uiso 1 1 calc R . . H20C H 0.5157 1.2190 0.3410 0.128 Uiso 1 1 calc R . . C21 C 0.9090(11) 0.5521(12) 0.4128(6) 0.047(3) Uani 1 1 d . . . C22 C 0.8755(13) 0.6751(12) 0.4388(6) 0.050(3) Uani 1 1 d . . . C23 C 0.7483(12) 0.7181(11) 0.4717(5) 0.044(3) Uani 1 1 d . . . C24 C 0.7010(12) 0.6238(12) 0.4673(5) 0.045(3) Uani 1 1 d . . . C25 C 0.7990(11) 0.5240(10) 0.4313(5) 0.039(3) Uani 1 1 d . . . C26 C 1.0424(13) 0.4666(14) 0.3785(7) 0.086(5) Uani 1 1 d . . . H26A H 1.0952 0.4088 0.4159 0.130 Uiso 1 1 calc R . . H26B H 1.0857 0.5208 0.3537 0.130 Uiso 1 1 calc R . . H26C H 1.0323 0.4150 0.3436 0.130 Uiso 1 1 calc R . . C27 C 0.9656(17) 0.7434(17) 0.4360(9) 0.110(7) Uani 1 1 d . . . H27A H 0.9147 0.8328 0.4486 0.165 Uiso 1 1 calc R . . H27B H 1.0094 0.7431 0.3872 0.165 Uiso 1 1 calc R . . H27C H 1.0308 0.6984 0.4703 0.165 Uiso 1 1 calc R . . C28 C 0.6706(18) 0.8442(13) 0.5094(7) 0.098(6) Uani 1 1 d . . . H28A H 0.6726 0.8258 0.5617 0.147 Uiso 1 1 calc R . . H28B H 0.5802 0.8811 0.4976 0.147 Uiso 1 1 calc R . . H28C H 0.7097 0.9061 0.4931 0.147 Uiso 1 1 calc R . . C29 C 0.5682(14) 0.6267(14) 0.5002(7) 0.074(4) Uani 1 1 d . . . H29A H 0.5344 0.5903 0.4675 0.110 Uiso 1 1 calc R . . H29B H 0.5071 0.7162 0.5077 0.110 Uiso 1 1 calc R . . H29C H 0.5785 0.5753 0.5465 0.110 Uiso 1 1 calc R . . C30 C 0.7892(15) 0.3999(12) 0.4168(7) 0.073(4) Uani 1 1 d . . . H30A H 0.7864 0.3489 0.4625 0.110 Uiso 1 1 calc R . . H30B H 0.8652 0.3494 0.3850 0.110 Uiso 1 1 calc R . . H30C H 0.7096 0.4216 0.3937 0.110 Uiso 1 1 calc R . . C31 C 0.2578(9) 0.9784(10) 0.2762(6) 0.036(2) Uani 1 1 d . . . C32 C 0.2692(10) 0.8657(11) 0.3215(6) 0.041(3) Uani 1 1 d . . . C33 C 0.3000(11) 0.7649(10) 0.2783(7) 0.045(3) Uani 1 1 d . . . C34 C 0.3031(10) 0.8118(11) 0.2047(6) 0.043(3) Uani 1 1 d . . . C35 C 0.2785(10) 0.9436(10) 0.2042(6) 0.038(3) Uani 1 1 d . . . C36 C 0.2159(11) 1.1107(10) 0.3015(7) 0.052(3) Uani 1 1 d . . . H36A H 0.1215 1.1477 0.3146 0.079 Uiso 1 1 calc R . . H36B H 0.2378 1.1661 0.2628 0.079 Uiso 1 1 calc R . . H36C H 0.2608 1.1047 0.3436 0.079 Uiso 1 1 calc R . . C37 C 0.2453(13) 0.8617(15) 0.4030(6) 0.075(4) Uani 1 1 d . . . H37A H 0.2770 0.7715 0.4228 0.112 Uiso 1 1 calc R . . H37B H 0.1516 0.9057 0.4172 0.112 Uiso 1 1 calc R . . H37C H 0.2916 0.9052 0.4217 0.112 Uiso 1 1 calc R . . C38 C 0.3212(14) 0.6254(13) 0.3036(9) 0.081(5) Uani 1 1 d . . . H38A H 0.3448 0.6068 0.3533 0.122 Uiso 1 1 calc R . . H38B H 0.3917 0.5660 0.2723 0.122 Uiso 1 1 calc R . . H38C H 0.2409 0.6140 0.3015 0.122 Uiso 1 1 calc R . . C39 C 0.3221(13) 0.7375(15) 0.1401(7) 0.075(4) Uani 1 1 d . . . H39A H 0.3655 0.6446 0.1532 0.112 Uiso 1 1 calc R . . H39B H 0.3760 0.7626 0.1012 0.112 Uiso 1 1 calc R . . H39C H 0.2371 0.7569 0.1237 0.112 Uiso 1 1 calc R . . C40 C 0.2686(11) 1.0343(12) 0.1381(6) 0.058(4) Uani 1 1 d . . . H40A H 0.3473 0.9976 0.1049 0.088 Uiso 1 1 calc R . . H40B H 0.2600 1.1178 0.1518 0.088 Uiso 1 1 calc R . . H40C H 0.1922 1.0466 0.1145 0.088 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 0.0276(5) 0.0183(5) 0.0245(5) 0.0001(4) -0.0032(4) -0.0096(4) Zr2 0.0234(5) 0.0193(5) 0.0296(5) 0.0003(4) -0.0054(4) -0.0105(4) Zr3 0.0261(5) 0.0269(5) 0.0243(5) 0.0015(4) -0.0038(4) -0.0131(4) Zr4 0.0227(5) 0.0253(5) 0.0294(5) 0.0027(4) -0.0060(4) -0.0121(4) C1 0.051(7) 0.021(6) 0.048(7) -0.007(5) 0.001(6) 0.007(5) C2 0.030(6) 0.059(8) 0.060(8) -0.027(7) 0.010(6) -0.018(6) C3 0.099(11) 0.048(8) 0.051(8) -0.032(6) 0.052(8) -0.056(8) C4 0.082(10) 0.041(7) 0.021(6) -0.004(5) -0.019(6) -0.005(7) C5 0.041(7) 0.042(7) 0.062(8) -0.022(6) 0.000(6) -0.022(6) C6 0.21(2) 0.016(6) 0.062(10) -0.005(6) 0.011(11) -0.003(9) C7 0.053(10) 0.25(3) 0.17(2) -0.17(2) 0.015(12) -0.012(13) C8 0.20(2) 0.105(14) 0.137(16) -0.084(12) 0.128(16) -0.114(15) C9 0.22(2) 0.086(13) 0.038(9) -0.016(8) -0.050(12) 0.031(14) C10 0.061(10) 0.122(15) 0.22(2) -0.138(15) 0.056(12) -0.060(10) C11 0.028(6) 0.020(5) 0.077(9) 0.005(5) -0.022(6) -0.011(5) C12 0.080(9) 0.031(6) 0.042(7) 0.012(5) -0.013(7) -0.033(7) C13 0.045(7) 0.035(6) 0.066(8) -0.017(6) 0.026(6) -0.028(6) C14 0.044(7) 0.031(6) 0.077(9) 0.013(6) -0.028(6) -0.032(5) C15 0.058(7) 0.024(5) 0.042(6) -0.016(5) 0.012(6) -0.025(5) C16 0.070(10) 0.038(8) 0.191(19) 0.034(10) -0.061(12) -0.020(7) C17 0.23(2) 0.091(12) 0.053(9) 0.036(8) -0.065(11) -0.113(14) C18 0.086(11) 0.054(9) 0.170(17) -0.056(10) 0.078(11) -0.047(9) C19 0.115(13) 0.071(10) 0.158(16) 0.057(10) -0.119(12) -0.070(10) C20 0.144(15) 0.071(10) 0.059(9) -0.030(8) 0.033(9) -0.068(11) C21 0.044(7) 0.058(8) 0.031(6) 0.015(5) -0.013(5) -0.014(6) C22 0.071(9) 0.064(8) 0.036(7) 0.019(6) -0.034(6) -0.047(7) C23 0.059(8) 0.044(7) 0.020(5) -0.008(5) -0.003(5) -0.011(6) C24 0.066(8) 0.064(8) 0.016(5) 0.007(5) -0.005(5) -0.040(7) C25 0.058(7) 0.033(6) 0.032(6) 0.013(5) -0.011(5) -0.027(6) C26 0.063(10) 0.088(11) 0.060(9) 0.021(8) -0.003(8) 0.008(8) C27 0.135(15) 0.158(17) 0.103(13) 0.064(12) -0.077(12) -0.125(15) C28 0.184(19) 0.062(10) 0.051(9) -0.015(7) -0.037(10) -0.041(11) C29 0.092(11) 0.085(11) 0.044(8) 0.013(7) -0.004(8) -0.041(9) C30 0.112(12) 0.044(8) 0.071(10) 0.013(7) -0.031(9) -0.037(8) C31 0.025(5) 0.044(6) 0.041(6) -0.012(5) -0.001(5) -0.014(5) C32 0.034(6) 0.047(7) 0.050(7) 0.002(5) 0.003(5) -0.026(5) C33 0.040(7) 0.037(6) 0.069(8) -0.004(6) 0.009(6) -0.030(6) C34 0.034(6) 0.058(8) 0.050(7) -0.010(6) -0.010(5) -0.030(6) C35 0.027(6) 0.042(6) 0.047(7) 0.011(5) -0.021(5) -0.014(5) C36 0.033(6) 0.037(7) 0.087(10) -0.021(6) -0.004(6) -0.010(5) C37 0.067(9) 0.119(13) 0.043(8) -0.015(8) 0.028(7) -0.051(9) C38 0.067(10) 0.056(9) 0.123(14) 0.011(9) 0.004(9) -0.036(8) C39 0.049(8) 0.109(12) 0.069(10) -0.020(9) -0.017(7) -0.028(8) C40 0.047(7) 0.076(9) 0.048(7) 0.023(6) -0.031(6) -0.020(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 C2 2.472(11) . ? Zr1 C1 2.484(10) . ? Zr1 C4 2.488(10) . ? Zr1 C3 2.497(10) . ? Zr1 C5 2.516(10) . ? Zr1 Zr3 3.0525(13) . ? Zr1 Zr2 3.0603(12) . ? Zr1 Zr4 3.0694(13) . ? Zr1 H1 1.90(8) . ? Zr1 H2 1.98(8) . ? Zr1 H3 1.95(8) . ? Zr2 C12 2.487(10) . ? Zr2 C14 2.488(9) . ? Zr2 C13 2.493(10) . ? Zr2 C15 2.498(9) . ? Zr2 C11 2.532(9) . ? Zr2 Zr3 3.0737(12) . ? Zr2 Zr4 3.0774(12) . ? Zr2 H1 1.87(8) . ? Zr2 H4 2.21(8) . ? Zr2 H5 1.89(8) . ? Zr3 C23 2.486(10) . ? Zr3 C25 2.489(9) . ? Zr3 C22 2.493(10) . ? Zr3 C24 2.497(10) . ? Zr3 C21 2.506(10) . ? Zr3 Zr4 3.0864(13) . ? Zr3 H2 2.10(8) . ? Zr3 H4 2.21(8) . ? Zr3 H6 2.24(8) . ? Zr4 C31 2.478(10) . ? Zr4 C35 2.479(9) . ? Zr4 C33 2.499(10) . ? Zr4 C32 2.510(10) . ? Zr4 C34 2.522(10) . ? Zr4 H3 1.88(8) . ? Zr4 H5 1.98(8) . ? Zr4 H6 2.28(8) . ? C1 C5 1.379(15) . ? C1 C2 1.389(16) . ? C1 C6 1.521(16) . ? C2 C3 1.408(18) . ? C2 C7 1.503(19) . ? C3 C4 1.409(18) . ? C3 C8 1.521(17) . ? C4 C5 1.401(16) . ? C4 C9 1.516(17) . ? C5 C10 1.485(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.396(15) . ? C11 C12 1.404(16) . ? C11 C16 1.516(16) . ? C12 C13 1.368(16) . ? C12 C17 1.519(16) . ? C13 C14 1.401(16) . ? C13 C18 1.547(16) . ? C14 C15 1.402(15) . ? C14 C19 1.545(14) . ? C15 C20 1.515(15) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.404(15) . ? C21 C22 1.423(16) . ? C21 C26 1.520(16) . ? C22 C23 1.393(16) . ? C22 C27 1.516(16) . ? C23 C24 1.403(15) . ? C23 C28 1.540(16) . ? C24 C25 1.383(15) . ? C24 C29 1.537(17) . ? C25 C30 1.527(15) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C35 1.417(14) . ? C31 C32 1.421(14) . ? C31 C36 1.498(14) . ? C32 C33 1.386(15) . ? C32 C37 1.517(15) . ? C33 C34 1.422(15) . ? C33 C38 1.531(15) . ? C34 C35 1.410(14) . ? C34 C39 1.507(16) . ? C35 C40 1.501(14) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 C2 Zr1 C1 32.6(4) . . ? C2 Zr1 C4 54.5(4) . . ? C1 Zr1 C4 53.5(4) . . ? C2 Zr1 C3 32.9(4) . . ? C1 Zr1 C3 53.7(4) . . ? C4 Zr1 C3 32.8(4) . . ? C2 Zr1 C5 54.1(4) . . ? C1 Zr1 C5 32.0(4) . . ? C4 Zr1 C5 32.5(4) . . ? C3 Zr1 C5 54.0(4) . . ? C2 Zr1 Zr3 120.5(3) . . ? C1 Zr1 Zr3 118.2(3) . . ? C4 Zr1 Zr3 171.4(3) . . ? C3 Zr1 Zr3 146.8(4) . . ? C5 Zr1 Zr3 139.3(3) . . ? C2 Zr1 Zr2 130.4(3) . . ? C1 Zr1 Zr2 161.9(3) . . ? C4 Zr1 Zr2 128.2(3) . . ? C3 Zr1 Zr2 116.3(2) . . ? C5 Zr1 Zr2 158.6(3) . . ? Zr3 Zr1 Zr2 60.37(3) . . ? C2 Zr1 Zr4 169.2(3) . . ? C1 Zr1 Zr4 136.6(3) . . ? C4 Zr1 Zr4 122.8(3) . . ? C3 Zr1 Zr4 150.4(4) . . ? C5 Zr1 Zr4 117.2(3) . . ? Zr3 Zr1 Zr4 60.55(3) . . ? Zr2 Zr1 Zr4 60.27(3) . . ? C2 Zr1 H1 105(3) . . ? C1 Zr1 H1 135(3) . . ? C4 Zr1 H1 95(2) . . ? C3 Zr1 H1 82(2) . . ? C5 Zr1 H1 127(2) . . ? Zr3 Zr1 H1 94(2) . . ? Zr2 Zr1 H1 35(2) . . ? Zr4 Zr1 H1 86(3) . . ? C2 Zr1 H2 80(2) . . ? C1 Zr1 H2 76(2) . . ? C4 Zr1 H2 129(2) . . ? C3 Zr1 H2 113(2) . . ? C5 Zr1 H2 104(2) . . ? Zr3 Zr1 H2 43(2) . . ? Zr2 Zr1 H2 97(2) . . ? Zr4 Zr1 H2 97(2) . . ? H1 Zr1 H2 121(3) . . ? C2 Zr1 H3 139(2) . . ? C1 Zr1 H3 114(2) . . ? C4 Zr1 H3 87(2) . . ? C3 Zr1 H3 118(2) . . ? C5 Zr1 H3 86(2) . . ? Zr3 Zr1 H3 95(2) . . ? Zr2 Zr1 H3 83(2) . . ? Zr4 Zr1 H3 36(2) . . ? H1 Zr1 H3 91(4) . . ? H2 Zr1 H3 123(3) . . ? C12 Zr2 C14 53.9(4) . . ? C12 Zr2 C13 31.9(4) . . ? C14 Zr2 C13 32.7(4) . . ? C12 Zr2 C15 53.7(4) . . ? C14 Zr2 C15 32.7(4) . . ? C13 Zr2 C15 53.6(3) . . ? C12 Zr2 C11 32.5(4) . . ? C14 Zr2 C11 53.8(3) . . ? C13 Zr2 C11 53.2(4) . . ? C15 Zr2 C11 32.2(3) . . ? C12 Zr2 Zr1 119.6(3) . . ? C14 Zr2 Zr1 138.1(3) . . ? C13 Zr2 Zr1 116.5(2) . . ? C15 Zr2 Zr1 169.9(2) . . ? C11 Zr2 Zr1 146.1(3) . . ? C12 Zr2 Zr3 169.6(3) . . ? C14 Zr2 Zr3 118.7(3) . . ? C13 Zr2 Zr3 137.8(3) . . ? C15 Zr2 Zr3 125.2(3) . . ? C11 Zr2 Zr3 152.2(3) . . ? Zr1 Zr2 Zr3 59.69(3) . . ? C12 Zr2 Zr4 129.5(3) . . ? C14 Zr2 Zr4 160.7(3) . . ? C13 Zr2 Zr4 159.6(3) . . ? C15 Zr2 Zr4 129.8(3) . . ? C11 Zr2 Zr4 116.9(2) . . ? Zr1 Zr2 Zr4 60.01(3) . . ? Zr3 Zr2 Zr4 60.23(3) . . ? C12 Zr2 H1 84(3) . . ? C14 Zr2 H1 113(3) . . ? C13 Zr2 H1 84(3) . . ? C15 Zr2 H1 135(3) . . ? C11 Zr2 H1 114(3) . . ? Zr1 Zr2 H1 36(3) . . ? Zr3 Zr2 H1 94(3) . . ? Zr4 Zr2 H1 86(3) . . ? C12 Zr2 H4 129(2) . . ? C14 Zr2 H4 76(2) . . ? C13 Zr2 H4 105(2) . . ? C15 Zr2 H4 81(2) . . ? C11 Zr2 H4 112(2) . . ? Zr1 Zr2 H4 102(2) . . ? Zr3 Zr2 H4 46(2) . . ? Zr4 Zr2 H4 96(2) . . ? H1 Zr2 H4 127(3) . . ? C12 Zr2 H5 98(3) . . ? C14 Zr2 H5 128(3) . . ? C13 Zr2 H5 129(3) . . ? C15 Zr2 H5 95(3) . . ? C11 Zr2 H5 79(3) . . ? Zr1 Zr2 H5 93(3) . . ? Zr3 Zr2 H5 93(3) . . ? Zr4 Zr2 H5 38(3) . . ? H1 Zr2 H5 105(4) . . ? H4 Zr2 H5 109(3) . . ? C23 Zr3 C25 53.6(4) . . ? C23 Zr3 C22 32.5(4) . . ? C25 Zr3 C22 53.9(4) . . ? C23 Zr3 C24 32.7(4) . . ? C25 Zr3 C24 32.2(4) . . ? C22 Zr3 C24 54.1(4) . . ? C23 Zr3 C21 54.4(4) . . ? C25 Zr3 C21 32.6(3) . . ? C22 Zr3 C21 33.1(4) . . ? C24 Zr3 C21 54.3(4) . . ? C23 Zr3 Zr1 170.1(3) . . ? C25 Zr3 Zr1 121.3(3) . . ? C22 Zr3 Zr1 137.9(3) . . ? C24 Zr3 Zr1 147.5(3) . . ? C21 Zr3 Zr1 116.4(3) . . ? C23 Zr3 Zr2 123.6(3) . . ? C25 Zr3 Zr2 171.3(3) . . ? C22 Zr3 Zr2 118.8(3) . . ? C24 Zr3 Zr2 150.1(3) . . ? C21 Zr3 Zr2 138.7(3) . . ? Zr1 Zr3 Zr2 59.94(3) . . ? C23 Zr3 Zr4 129.8(3) . . ? C25 Zr3 Zr4 128.6(3) . . ? C22 Zr3 Zr4 160.9(3) . . ? C24 Zr3 Zr4 116.1(3) . . ? C21 Zr3 Zr4 159.0(3) . . ? Zr1 Zr3 Zr4 60.00(3) . . ? Zr2 Zr3 Zr4 59.94(3) . . ? C23 Zr3 H2 131(2) . . ? C25 Zr3 H2 84(2) . . ? C22 Zr3 H2 105(2) . . ? C24 Zr3 H2 115(2) . . ? C21 Zr3 H2 77(2) . . ? Zr1 Zr3 H2 40(2) . . ? Zr2 Zr3 H2 94(2) . . ? Zr4 Zr3 H2 94(2) . . ? C23 Zr3 H4 79(2) . . ? C25 Zr3 H4 128(2) . . ? C22 Zr3 H4 76(2) . . ? C24 Zr3 H4 110(2) . . ? C21 Zr3 H4 105(2) . . ? Zr1 Zr3 H4 102(2) . . ? Zr2 Zr3 H4 46(2) . . ? Zr4 Zr3 H4 96(2) . . ? H2 Zr3 H4 123(3) . . ? C23 Zr3 H6 90(2) . . ? C25 Zr3 H6 86(2) . . ? C22 Zr3 H6 121(2) . . ? C24 Zr3 H6 69(2) . . ? C21 Zr3 H6 118(2) . . ? Zr1 Zr3 H6 99(2) . . ? Zr2 Zr3 H6 102(2) . . ? Zr4 Zr3 H6 48(2) . . ? H2 Zr3 H6 112(3) . . ? H4 Zr3 H6 115(3) . . ? C31 Zr4 C35 33.2(3) . . ? C31 Zr4 C33 54.4(3) . . ? C35 Zr4 C33 54.2(4) . . ? C31 Zr4 C32 33.1(3) . . ? C35 Zr4 C32 54.4(4) . . ? C33 Zr4 C32 32.1(3) . . ? C31 Zr4 C34 54.8(3) . . ? C35 Zr4 C34 32.7(3) . . ? C33 Zr4 C34 32.9(4) . . ? C32 Zr4 C34 54.1(4) . . ? C31 Zr4 Zr1 160.8(2) . . ? C35 Zr4 Zr1 129.3(3) . . ? C33 Zr4 Zr1 128.9(3) . . ? C32 Zr4 Zr1 159.2(3) . . ? C34 Zr4 Zr1 115.8(3) . . ? C31 Zr4 Zr2 116.3(2) . . ? C35 Zr4 Zr2 118.7(2) . . ? C33 Zr4 Zr2 170.7(3) . . ? C32 Zr4 Zr2 140.1(3) . . ? C34 Zr4 Zr2 144.3(3) . . ? Zr1 Zr4 Zr2 59.72(3) . . ? C31 Zr4 Zr3 137.3(2) . . ? C35 Zr4 Zr3 170.2(3) . . ? C33 Zr4 Zr3 126.0(3) . . ? C32 Zr4 Zr3 119.6(3) . . ? C34 Zr4 Zr3 153.0(3) . . ? Zr1 Zr4 Zr3 59.45(3) . . ? Zr2 Zr4 Zr3 59.82(3) . . ? C31 Zr4 H3 127(3) . . ? C35 Zr4 H3 94(3) . . ? C33 Zr4 H3 102(3) . . ? C32 Zr4 H3 132(3) . . ? C34 Zr4 H3 80(3) . . ? Zr1 Zr4 H3 37(3) . . ? Zr2 Zr4 H3 84(3) . . ? Zr3 Zr4 H3 96(3) . . ? C31 Zr4 H5 81(2) . . ? C35 Zr4 H5 85(2) . . ? C33 Zr4 H5 135(2) . . ? C32 Zr4 H5 110(2) . . ? C34 Zr4 H5 116(2) . . ? Zr1 Zr4 H5 91(2) . . ? Zr2 Zr4 H5 36(2) . . ? Zr3 Zr4 H5 91(2) . . ? H3 Zr4 H5 100(3) . . ? C31 Zr4 H6 102(2) . . ? C35 Zr4 H6 129(2) . . ? C33 Zr4 H6 82(2) . . ? C32 Zr4 H6 75(2) . . ? C34 Zr4 H6 114(2) . . ? Zr1 Zr4 H6 97(2) . . ? Zr2 Zr4 H6 101(2) . . ? Zr3 Zr4 H6 46(2) . . ? H3 Zr4 H6 123(3) . . ? H5 Zr4 H6 118(3) . . ? C5 C1 C2 110.0(10) . . ? C5 C1 C6 124.2(13) . . ? C2 C1 C6 125.7(13) . . ? C5 C1 Zr1 75.3(6) . . ? C2 C1 Zr1 73.2(6) . . ? C6 C1 Zr1 121.3(8) . . ? C1 C2 C3 107.0(10) . . ? C1 C2 C7 126.6(16) . . ? C3 C2 C7 126.1(15) . . ? C1 C2 Zr1 74.2(6) . . ? C3 C2 Zr1 74.5(6) . . ? C7 C2 Zr1 121.8(8) . . ? C2 C3 C4 107.5(9) . . ? C2 C3 C8 125.3(16) . . ? C4 C3 C8 127.1(16) . . ? C2 C3 Zr1 72.6(6) . . ? C4 C3 Zr1 73.2(6) . . ? C8 C3 Zr1 123.1(8) . . ? C5 C4 C3 108.1(10) . . ? C5 C4 C9 127.0(15) . . ? C3 C4 C9 124.8(15) . . ? C5 C4 Zr1 74.9(6) . . ? C3 C4 Zr1 73.9(6) . . ? C9 C4 Zr1 119.1(8) . . ? C1 C5 C4 107.3(10) . . ? C1 C5 C10 127.1(13) . . ? C4 C5 C10 125.5(14) . . ? C1 C5 Zr1 72.7(6) . . ? C4 C5 Zr1 72.6(6) . . ? C10 C5 Zr1 123.1(8) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 107.0(9) . . ? C15 C11 C16 127.1(12) . . ? C12 C11 C16 125.8(12) . . ? C15 C11 Zr2 72.6(5) . . ? C12 C11 Zr2 72.0(6) . . ? C16 C11 Zr2 122.7(7) . . ? C13 C12 C11 108.6(10) . . ? C13 C12 C17 128.0(14) . . ? C11 C12 C17 123.0(13) . . ? C13 C12 Zr2 74.3(6) . . ? C11 C12 Zr2 75.5(6) . . ? C17 C12 Zr2 122.8(8) . . ? C12 C13 C14 109.0(10) . . ? C12 C13 C18 126.0(13) . . ? C14 C13 C18 124.8(13) . . ? C12 C13 Zr2 73.8(6) . . ? C14 C13 Zr2 73.4(6) . . ? C18 C13 Zr2 122.7(7) . . ? C13 C14 C15 106.7(10) . . ? C13 C14 C19 124.7(13) . . ? C15 C14 C19 128.3(13) . . ? C13 C14 Zr2 73.9(6) . . ? C15 C14 Zr2 74.1(5) . . ? C19 C14 Zr2 121.8(7) . . ? C11 C15 C14 108.6(9) . . ? C11 C15 C20 125.3(12) . . ? C14 C15 C20 126.0(12) . . ? C11 C15 Zr2 75.2(6) . . ? C14 C15 Zr2 73.3(5) . . ? C20 C15 Zr2 121.7(7) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 106.0(10) . . ? C25 C21 C26 128.4(12) . . ? C22 C21 C26 125.4(12) . . ? C25 C21 Zr3 73.1(6) . . ? C22 C21 Zr3 73.0(6) . . ? C26 C21 Zr3 123.1(7) . . ? C23 C22 C21 108.2(10) . . ? C23 C22 C27 125.7(13) . . ? C21 C22 C27 125.9(14) . . ? C23 C22 Zr3 73.5(6) . . ? C21 C22 Zr3 74.0(6) . . ? C27 C22 Zr3 121.9(8) . . ? C22 C23 C24 108.5(10) . . ? C22 C23 C28 127.4(13) . . ? C24 C23 C28 124.1(12) . . ? C22 C23 Zr3 74.0(6) . . ? C24 C23 Zr3 74.1(6) . . ? C28 C23 Zr3 119.6(8) . . ? C25 C24 C23 107.3(10) . . ? C25 C24 C29 126.1(11) . . ? C23 C24 C29 126.5(11) . . ? C25 C24 Zr3 73.6(6) . . ? C23 C24 Zr3 73.2(6) . . ? C29 C24 Zr3 121.5(8) . . ? C24 C25 C21 110.0(10) . . ? C24 C25 C30 124.4(11) . . ? C21 C25 C30 125.6(11) . . ? C24 C25 Zr3 74.2(6) . . ? C21 C25 Zr3 74.3(6) . . ? C30 C25 Zr3 120.0(7) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C35 C31 C32 106.8(9) . . ? C35 C31 C36 127.6(10) . . ? C32 C31 C36 125.2(10) . . ? C35 C31 Zr4 73.4(6) . . ? C32 C31 Zr4 74.7(6) . . ? C36 C31 Zr4 122.9(7) . . ? C33 C32 C31 108.3(10) . . ? C33 C32 C37 127.1(11) . . ? C31 C32 C37 124.5(11) . . ? C33 C32 Zr4 73.5(6) . . ? C31 C32 Zr4 72.2(6) . . ? C37 C32 Zr4 122.2(8) . . ? C32 C33 C34 109.3(9) . . ? C32 C33 C38 126.8(12) . . ? C34 C33 C38 123.9(11) . . ? C32 C33 Zr4 74.4(6) . . ? C34 C33 Zr4 74.4(6) . . ? C38 C33 Zr4 119.9(8) . . ? C35 C34 C33 106.4(9) . . ? C35 C34 C39 126.6(11) . . ? C33 C34 C39 126.9(11) . . ? C35 C34 Zr4 72.0(5) . . ? C33 C34 Zr4 72.7(6) . . ? C39 C34 Zr4 122.8(8) . . ? C34 C35 C31 109.1(9) . . ? C34 C35 C40 125.4(11) . . ? C31 C35 C40 125.4(10) . . ? C34 C35 Zr4 75.3(6) . . ? C31 C35 Zr4 73.3(6) . . ? C40 C35 Zr4 120.2(7) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? 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 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.762 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.142