# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1767 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Professor Malcolm L. H. Green FRS Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR. ; _publ_contact_author_phone '(01865) 272649 ' _publ_contact_author_fax '(01865) 272690 ' _publ_contact_author_email 'Malcolm.Green@chem.ox.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? #========================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #========================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title 'Studies on Ansa-zirconocene-butadiene Derivatives' #============= Material Relevant to Compound(2)===================== data_2 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C34 H40 ZR2' _chemical_formula_structural 'cis-[Zr{Me2C(C5H4)2}(C4H6)]' _chemical_formula_analytical 'C34 H40 ZR2' _chemical_formula_sum 'C34 H40 ZR2' _chemical_formula_weight 631.10 _chemical_melting_point ? _chemical_compound_source ? 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 Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.623(9) _cell_length_b 15.203(15) _cell_length_c 23.029(20) _cell_angle_alpha 90.00 _cell_angle_beta 95.08(7) _cell_angle_gamma 90.00 _cell_volume 2658.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour gold _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method ? _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details 'none' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST TV Area detector' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9781 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.2646 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.28 _reflns_number_total 3916 _reflns_number_observed 2153 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Pflugrath, 1989)' _computing_cell_refinement MADNES _computing_data_reduction 'ABSURD (within MADNES)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 22 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^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 riding _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_number_reflns 3894 _refine_ls_number_parameters 361 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_obs 0.0363 _refine_ls_wR_factor_all 0.0967 _refine_ls_wR_factor_obs 0.0638 _refine_ls_goodness_of_fit_all 0.686 _refine_ls_goodness_of_fit_obs 0.837 _refine_ls_restrained_S_all 1.002 _refine_ls_restrained_S_obs 0.841 _refine_ls_shift/esd_max 0.335 _refine_ls_shift/esd_mean 0.017 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.21644(7) 0.13927(4) 0.11483(3) 0.0137(2) Uani 1 d . . Zr2 Zr 0.70310(7) -0.26042(4) 0.14469(2) 0.0147(2) Uani 1 d . . C1 C 0.2986(7) 0.2838(4) 0.1613(3) 0.022(2) Uani 1 d . . H1 H 0.2605(7) 0.2938(4) 0.1980(3) 0.026 Uiso 1 calc R . C2 C 0.4600(7) 0.2472(4) 0.1502(3) 0.023(2) Uani 1 d . . H2 H 0.5481(7) 0.2300(4) 0.1784(3) 0.028 Uiso 1 calc R . C3 C 0.4684(7) 0.2403(4) 0.0903(3) 0.024(2) Uani 1 d . . H3 H 0.5618(7) 0.2176(4) 0.0716(3) 0.028 Uiso 1 calc R . C4 C 0.3096(7) 0.2742(4) 0.0629(2) 0.0182(15) Uani 1 d . . H4 H 0.2794(7) 0.2771(4) 0.0229(2) 0.022 Uiso 1 calc R . C5 C 0.2029(7) 0.3031(4) 0.1073(3) 0.0154(14) Uani 1 d . . C6 C 0.0086(7) 0.3181(4) 0.0993(3) 0.0168(14) Uani 1 d . . C7 C -0.0452(7) 0.3631(4) 0.0414(2) 0.028(2) Uani 1 d . . H7A H -0.1705(8) 0.3717(20) 0.0374(7) 0.043 Uiso 1 calc R . H7B H -0.0119(39) 0.3269(10) 0.0100(2) 0.043 Uiso 1 calc R . H7C H 0.0128(33) 0.4190(9) 0.0402(6) 0.043 Uiso 1 calc R . C8 C -0.0563(7) 0.3754(4) 0.1481(3) 0.030(2) Uani 1 d . . H8A H -0.1827(7) 0.3755(18) 0.1450(9) 0.045 Uiso 1 calc R . H8B H -0.0142(37) 0.4344(6) 0.1444(9) 0.045 Uiso 1 calc R . H8C H -0.0124(36) 0.3520(13) 0.1853(3) 0.045 Uiso 1 calc R . C9 C -0.0595(6) 0.2237(4) 0.1011(3) 0.0138(14) Uani 1 d . . C10 C -0.0642(6) 0.1632(4) 0.0549(3) 0.0192(15) Uani 1 d . . H10 H -0.0555(6) 0.1768(4) 0.0159(3) 0.023 Uiso 1 calc R . C11 C -0.0843(6) 0.0781(4) 0.0780(3) 0.025(2) Uani 1 d . . H11 H -0.0930(6) 0.0262(4) 0.0566(3) 0.030 Uiso 1 calc R . C12 C -0.0889(6) 0.0844(4) 0.1374(3) 0.0167(15) Uani 1 d U . H12 H -0.1022(6) 0.0380(4) 0.1629(3) 0.020 Uiso 1 calc R . C13 C -0.0698(6) 0.1738(4) 0.1526(3) 0.0172(15) Uani 1 d . . H13 H -0.0648(6) 0.1964(4) 0.1902(3) 0.021 Uiso 1 calc R . C14 C 0.2997(8) 0.0380(4) 0.1865(3) 0.021(2) Uani 1 d . . H14A H 0.2421(64) -0.0104(36) 0.1737(24) 0.023(18) Uiso 1 d . . H14B H 0.2937(59) 0.0217(36) 0.2251(24) 0.026(18) Uiso 1 d . . C15 C 0.4521(7) 0.0391(4) 0.1542(3) 0.0190(15) Uani 1 d U . H15 H 0.5610(7) 0.0417(4) 0.1758(3) 0.023 Uiso 1 calc R . C16 C 0.4540(7) 0.0366(4) 0.0946(3) 0.023(2) Uani 1 d . . H16 H 0.5639(7) 0.0385(4) 0.0800(3) 0.027 Uiso 1 calc R . C17 C 0.3078(8) 0.0314(4) 0.0537(3) 0.020(2) Uani 1 d . . H17A H 0.2279(62) -0.0106(35) 0.0612(22) 0.025(17) Uiso 1 d . . H17B H 0.3367(62) 0.0233(36) 0.0178(25) 0.030(18) Uiso 1 d . . C18 C 0.7859(7) -0.4008(4) 0.1960(3) 0.0207(15) Uani 1 d . . H18 H 0.7455(7) -0.4074(4) 0.2327(3) 0.025 Uiso 1 calc R . C19 C 0.9491(6) -0.3642(4) 0.1842(3) 0.024(2) Uani 1 d U . H19 H 1.0355(6) -0.3442(4) 0.2121(3) 0.028 Uiso 1 calc R . C20 C 0.9605(7) -0.3625(4) 0.1254(3) 0.022(2) Uani 1 d . . H20 H 1.0548(7) -0.3414(4) 0.1065(3) 0.027 Uiso 1 calc R . C21 C 0.8034(7) -0.3987(4) 0.0985(3) 0.0184(15) Uani 1 d . . H21 H 0.7749(7) -0.4042(4) 0.0585(3) 0.022 Uiso 1 calc R . C22 C 0.6956(7) -0.4255(4) 0.1430(3) 0.0129(13) Uani 1 d U . C23 C 0.5010(7) -0.4415(4) 0.1340(2) 0.021(2) Uani 1 d . . C24 C 0.4515(7) -0.4911(4) 0.0785(3) 0.033(2) Uani 1 d . . H24A H 0.3255(7) -0.4937(20) 0.0717(8) 0.049 Uiso 1 calc R . H24B H 0.4982(37) -0.5497(7) 0.0819(6) 0.049 Uiso 1 calc R . H24C H 0.4990(37) -0.4615(12) 0.0466(3) 0.049 Uiso 1 calc R . C25 C 0.4356(7) -0.4923(4) 0.1847(3) 0.026(2) Uani 1 d . . H25A H 0.3102(9) -0.4992(20) 0.1786(8) 0.039 Uiso 1 calc R . H25B H 0.4650(38) -0.4606(11) 0.2203(3) 0.039 Uiso 1 calc R . H25C H 0.4904(34) -0.5492(9) 0.1872(9) 0.039 Uiso 1 calc R . C26 C 0.4305(6) -0.3471(4) 0.1303(2) 0.0157(14) Uani 1 d . . C27 C 0.4293(7) -0.2906(4) 0.0826(3) 0.022(2) Uani 1 d . . H27 H 0.4436(7) -0.3078(4) 0.0446(3) 0.027 Uiso 1 calc R . C28 C 0.4033(7) -0.2045(4) 0.1006(4) 0.035(2) Uani 1 d . . H28 H 0.3949(7) -0.1551(4) 0.0767(4) 0.042 Uiso 1 calc R . C29 C 0.3923(7) -0.2053(4) 0.1597(3) 0.033(2) Uani 1 d . . H29 H 0.3764(7) -0.1563(4) 0.1828(3) 0.040 Uiso 1 calc R . C30 C 0.4091(6) -0.2920(4) 0.1792(3) 0.020(2) Uani 1 d . . H30 H 0.4066(6) -0.3107(4) 0.2176(3) 0.024 Uiso 1 calc R . C31 C 0.7967(8) -0.1539(4) 0.0829(3) 0.024(2) Uani 1 d D . H31A H 0.8061(72) -0.1550(45) 0.0413(13) 0.064(23) Uiso 1 d D . H31B H 0.7000(71) -0.1141(42) 0.0875(36) 0.113(33) Uiso 1 d D . C32 C 0.9390(7) -0.1560(4) 0.1269(3) 0.025(2) Uani 1 d . . H32 H 1.0514(7) -0.1577(4) 0.1142(3) 0.030 Uiso 1 calc R . C33 C 0.9291(7) -0.1559(4) 0.1860(3) 0.025(2) Uani 1 d . . H33 H 1.0356(7) -0.1568(4) 0.2091(3) 0.030 Uiso 1 calc R . C34 C 0.7754(8) -0.1547(4) 0.2157(3) 0.024(2) Uani 1 d . . H34A H 0.6799(63) -0.1153(34) 0.2037(23) 0.026(17) Uiso 1 d . . H34B H 0.7942(57) -0.1518(35) 0.2588(23) 0.022(16) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0110(3) 0.0138(3) 0.0162(4) -0.0017(3) 0.0011(2) -0.0007(3) Zr2 0.0112(3) 0.0148(4) 0.0180(4) 0.0016(3) -0.0001(2) 0.0005(3) C1 0.013(4) 0.023(4) 0.028(4) -0.010(3) -0.000(3) -0.004(3) C2 0.010(3) 0.017(4) 0.042(5) -0.003(4) -0.004(3) -0.008(3) C3 0.014(4) 0.018(4) 0.040(4) -0.005(3) 0.010(3) -0.008(3) C4 0.020(4) 0.022(4) 0.013(4) 0.002(3) 0.007(3) -0.001(3) C5 0.008(3) 0.015(4) 0.023(4) 0.009(3) 0.002(3) 0.001(3) C6 0.023(4) 0.013(4) 0.015(4) 0.002(3) 0.004(3) 0.008(3) C7 0.019(3) 0.040(4) 0.025(4) 0.015(4) -0.004(3) 0.001(3) C8 0.033(4) 0.027(4) 0.031(4) -0.002(3) 0.009(3) 0.002(3) C9 0.007(3) 0.016(4) 0.019(4) 0.001(3) 0.003(3) -0.002(2) C10 0.011(3) 0.024(4) 0.022(4) 0.003(3) -0.001(3) -0.002(3) C11 0.006(3) 0.026(4) 0.040(5) -0.006(3) -0.004(3) -0.003(3) C12 0.003(3) 0.020(3) 0.027(3) 0.008(3) 0.005(2) 0.001(2) C13 0.015(3) 0.023(4) 0.014(4) 0.003(3) 0.006(3) -0.002(3) C14 0.017(4) 0.030(5) 0.017(4) 0.004(3) 0.000(3) 0.001(3) C15 0.010(3) 0.022(4) 0.023(4) 0.000(3) -0.011(3) 0.006(3) C16 0.019(4) 0.020(4) 0.029(5) -0.000(3) 0.006(3) 0.009(3) C17 0.019(4) 0.027(4) 0.016(4) -0.005(3) 0.002(3) 0.005(3) C18 0.015(4) 0.024(4) 0.023(4) 0.012(3) 0.001(3) 0.007(3) C19 0.008(3) 0.028(4) 0.034(4) 0.003(3) -0.006(3) 0.009(3) C20 0.008(4) 0.023(4) 0.035(5) 0.003(4) 0.001(3) 0.006(3) C21 0.020(4) 0.024(4) 0.012(4) 0.004(3) 0.004(3) 0.012(3) C22 0.004(3) 0.020(3) 0.015(3) 0.000(3) 0.003(2) -0.003(2) C23 0.036(4) 0.018(4) 0.008(4) -0.006(3) 0.003(3) -0.005(3) C24 0.028(4) 0.037(5) 0.034(5) -0.007(4) 0.009(3) -0.004(3) C25 0.024(4) 0.022(4) 0.033(4) 0.014(3) 0.006(3) -0.004(3) C26 0.007(3) 0.021(4) 0.019(4) -0.005(3) 0.001(3) -0.002(3) C27 0.018(4) 0.028(4) 0.021(4) 0.009(3) 0.000(3) 0.000(3) C28 0.013(4) 0.025(4) 0.065(6) 0.019(4) -0.014(4) 0.004(3) C29 0.003(4) 0.024(4) 0.072(6) -0.003(4) 0.000(3) -0.002(3) C30 0.008(3) 0.024(4) 0.028(4) -0.004(3) 0.002(3) 0.004(3) C31 0.020(4) 0.031(4) 0.020(4) 0.003(3) -0.000(3) -0.003(3) C32 0.012(4) 0.017(4) 0.047(5) 0.008(3) 0.006(3) -0.008(3) C33 0.025(4) 0.022(4) 0.025(4) -0.003(3) -0.009(3) -0.010(3) C34 0.016(4) 0.032(5) 0.023(4) -0.007(3) -0.000(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix.The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C14 2.305(7) . ? Zr1 C17 2.308(6) . ? Zr1 C9 2.461(5) . ? Zr1 C15 2.466(5) . ? Zr1 C16 2.467(5) . ? Zr1 C10 2.468(5) . ? Zr1 C13 2.476(5) . ? Zr1 C5 2.498(5) . ? Zr1 C4 2.508(5) . ? Zr1 C1 2.500(5) . ? Zr1 C11 2.548(5) . ? Zr1 C2 2.556(5) . ? Zr2 C31 2.311(6) . ? Zr2 C34 2.324(6) . ? Zr2 C32 2.460(5) . ? Zr2 C26 2.458(5) . ? Zr2 C27 2.467(6) . ? Zr2 C33 2.471(5) . ? Zr2 C18 2.494(5) . ? Zr2 C30 2.491(5) . ? Zr2 C21 2.506(5) . ? Zr2 C22 2.511(5) . ? Zr2 C19 2.555(5) . ? Zr2 C28 2.562(6) . ? C1 C2 1.395(7) . ? C1 C5 1.416(8) . ? C2 C3 1.390(7) . ? C3 C4 1.411(7) . ? C4 C5 1.431(7) . ? C5 C6 1.494(7) . ? C6 C9 1.528(7) . ? C6 C7 1.523(7) . ? C6 C8 1.537(7) . ? C9 C10 1.405(7) . ? C9 C13 1.415(7) . ? C10 C11 1.413(8) . ? C11 C12 1.373(7) . ? C12 C13 1.408(8) . ? C14 C15 1.435(8) . ? C15 C16 1.374(7) . ? C16 C17 1.396(8) . ? C18 C22 1.398(7) . ? C18 C19 1.412(7) . ? C19 C20 1.363(7) . ? C20 C21 1.410(7) . ? C21 C22 1.429(7) . ? C22 C23 1.499(7) . ? C23 C24 1.502(7) . ? C23 C25 1.520(7) . ? C23 C26 1.533(8) . ? C26 C27 1.393(7) . ? C26 C30 1.426(7) . ? C27 C28 1.392(8) . ? C28 C29 1.371(8) . ? C29 C30 1.396(8) . ? C31 C32 1.417(8) . ? C32 C33 1.371(7) . ? C33 C34 1.408(7) . ? 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 C14 Zr1 C17 83.3(2) . . ? C14 Zr1 C9 128.2(2) . . ? C17 Zr1 C9 126.4(2) . . ? C14 Zr1 C15 34.8(2) . . ? C17 Zr1 C15 62.3(2) . . ? C9 Zr1 C15 163.0(2) . . ? C14 Zr1 C16 63.4(2) . . ? C17 Zr1 C16 33.8(2) . . ? C9 Zr1 C16 160.0(2) . . ? C15 Zr1 C16 32.3(2) . . ? C14 Zr1 C10 132.0(2) . . ? C17 Zr1 C10 93.3(2) . . ? C9 Zr1 C10 33.1(2) . . ? C15 Zr1 C10 149.7(2) . . ? C16 Zr1 C10 127.0(2) . . ? C14 Zr1 C13 94.9(2) . . ? C17 Zr1 C13 133.4(2) . . ? C9 Zr1 C13 33.3(2) . . ? C15 Zr1 C13 129.6(2) . . ? C16 Zr1 C13 152.3(2) . . ? C10 Zr1 C13 54.4(2) . . ? C14 Zr1 C5 136.3(2) . . ? C17 Zr1 C5 132.8(2) . . ? C9 Zr1 C5 56.1(2) . . ? C15 Zr1 C5 131.7(2) . . ? C16 Zr1 C5 130.1(2) . . ? C10 Zr1 C5 77.6(2) . . ? C13 Zr1 C5 77.3(2) . . ? C14 Zr1 C4 144.7(2) . . ? C17 Zr1 C4 100.2(2) . . ? C9 Zr1 C4 77.7(2) . . ? C15 Zr1 C4 116.9(2) . . ? C16 Zr1 C4 100.6(2) . . ? C10 Zr1 C4 83.2(2) . . ? C13 Zr1 C4 106.8(2) . . ? C5 Zr1 C4 33.2(2) . . ? C14 Zr1 C1 103.8(2) . . ? C17 Zr1 C1 143.9(2) . . ? C9 Zr1 C1 77.0(2) . . ? C15 Zr1 C1 103.8(2) . . ? C16 Zr1 C1 118.5(2) . . ? C10 Zr1 C1 106.4(2) . . ? C13 Zr1 C1 81.9(2) . . ? C5 Zr1 C1 32.9(2) . . ? C4 Zr1 C1 54.2(2) . . ? C14 Zr1 C11 100.2(2) . . ? C17 Zr1 C11 81.3(2) . . ? C9 Zr1 C11 54.1(2) . . ? C15 Zr1 C11 120.1(2) . . ? C16 Zr1 C11 111.1(2) . . ? C10 Zr1 C11 32.7(2) . . ? C13 Zr1 C11 53.1(2) . . ? C5 Zr1 C11 108.1(2) . . ? C4 Zr1 C11 115.1(2) . . ? C1 Zr1 C11 130.3(2) . . ? C14 Zr1 C2 93.1(2) . . ? C17 Zr1 C2 113.6(2) . . ? C9 Zr1 C2 107.1(2) . . ? C15 Zr1 C2 78.1(2) . . ? C16 Zr1 C2 86.7(2) . . ? C10 Zr1 C2 130.7(2) . . ? C13 Zr1 C2 113.0(2) . . ? C5 Zr1 C2 53.6(2) . . ? C4 Zr1 C2 53.0(2) . . ? C1 Zr1 C2 32.0(2) . . ? C11 Zr1 C2 161.2(2) . . ? C31 Zr2 C34 83.2(2) . . ? C31 Zr2 C32 34.4(2) . . ? C34 Zr2 C32 62.6(2) . . ? C31 Zr2 C26 126.6(2) . . ? C34 Zr2 C26 127.6(2) . . ? C32 Zr2 C26 160.9(2) . . ? C31 Zr2 C27 93.7(2) . . ? C34 Zr2 C27 132.3(2) . . ? C32 Zr2 C27 128.1(2) . . ? C26 Zr2 C27 32.9(2) . . ? C31 Zr2 C33 62.9(2) . . ? C34 Zr2 C33 34.0(2) . . ? C32 Zr2 C33 32.3(2) . . ? C26 Zr2 C33 161.6(2) . . ? C27 Zr2 C33 150.3(2) . . ? C31 Zr2 C18 144.4(2) . . ? C34 Zr2 C18 103.0(2) . . ? C32 Zr2 C18 118.2(2) . . ? C26 Zr2 C18 77.3(2) . . ? C27 Zr2 C18 106.3(2) . . ? C33 Zr2 C18 103.2(2) . . ? C31 Zr2 C30 131.9(2) . . ? C34 Zr2 C30 94.2(2) . . ? C32 Zr2 C30 150.4(2) . . ? C26 Zr2 C30 33.5(2) . . ? C27 Zr2 C30 53.8(2) . . ? C33 Zr2 C30 128.1(2) . . ? C18 Zr2 C30 83.2(2) . . ? C31 Zr2 C21 101.8(2) . . ? C34 Zr2 C21 144.7(2) . . ? C32 Zr2 C21 102.4(2) . . ? C26 Zr2 C21 77.2(2) . . ? C27 Zr2 C21 82.7(2) . . ? C33 Zr2 C21 118.3(2) . . ? C18 Zr2 C21 53.8(2) . . ? C30 Zr2 C21 106.9(2) . . ? C31 Zr2 C22 134.3(2) . . ? C34 Zr2 C22 134.9(2) . . ? C32 Zr2 C22 131.2(2) . . ? C26 Zr2 C22 56.2(2) . . ? C27 Zr2 C22 77.8(2) . . ? C33 Zr2 C22 131.5(2) . . ? C18 Zr2 C22 32.4(2) . . ? C30 Zr2 C22 78.0(2) . . ? C21 Zr2 C22 33.1(2) . . ? C31 Zr2 C19 113.2(2) . . ? C34 Zr2 C19 93.2(2) . . ? C32 Zr2 C19 86.2(2) . . ? C26 Zr2 C19 107.6(2) . . ? C27 Zr2 C19 130.4(2) . . ? C33 Zr2 C19 78.2(2) . . ? C18 Zr2 C19 32.4(2) . . ? C30 Zr2 C19 114.8(2) . . ? C21 Zr2 C19 52.5(2) . . ? C22 Zr2 C19 53.4(2) . . ? C31 Zr2 C28 80.6(2) . . ? C34 Zr2 C28 101.4(2) . . ? C32 Zr2 C28 111.1(2) . . ? C26 Zr2 C28 53.9(2) . . ? C27 Zr2 C28 32.1(2) . . ? C33 Zr2 C28 120.4(2) . . ? C18 Zr2 C28 130.6(2) . . ? C30 Zr2 C28 52.7(2) . . ? C21 Zr2 C28 113.9(2) . . ? C22 Zr2 C28 107.9(2) . . ? C19 Zr2 C28 161.2(2) . . ? C2 C1 C5 108.3(5) . . ? C2 C1 Zr1 76.2(3) . . ? C5 C1 Zr1 73.5(3) . . ? C1 C2 C3 109.4(5) . . ? C1 C2 Zr1 71.8(3) . . ? C3 C2 Zr1 74.5(3) . . ? C2 C3 C4 107.6(5) . . ? C2 C3 Zr1 74.0(3) . . ? C4 C3 Zr1 71.7(3) . . ? C3 C4 C5 108.2(5) . . ? C3 C4 Zr1 76.0(3) . . ? C5 C4 Zr1 73.0(3) . . ? C1 C5 C4 106.4(5) . . ? C1 C5 C6 124.7(5) . . ? C4 C5 C6 125.3(5) . . ? C1 C5 Zr1 73.6(3) . . ? C4 C5 Zr1 73.8(3) . . ? C6 C5 Zr1 101.3(3) . . ? C5 C6 C9 100.9(4) . . ? C5 C6 C7 111.4(4) . . ? C9 C6 C7 112.3(5) . . ? C5 C6 C8 112.0(5) . . ? C9 C6 C8 112.3(5) . . ? C7 C6 C8 107.9(5) . . ? C10 C9 C13 106.5(5) . . ? C10 C9 C6 125.4(5) . . ? C13 C9 C6 124.8(5) . . ? C10 C9 Zr1 73.7(3) . . ? C13 C9 Zr1 73.9(3) . . ? C6 C9 Zr1 101.8(3) . . ? C9 C10 C11 108.0(5) . . ? C9 C10 Zr1 73.2(3) . . ? C11 C10 Zr1 76.8(3) . . ? C12 C11 C10 108.9(5) . . ? C12 C11 Zr1 75.2(3) . . ? C10 C11 Zr1 70.5(3) . . ? C11 C12 C13 107.7(5) . . ? C11 C12 Zr1 73.6(3) . . ? C13 C12 Zr1 70.2(3) . . ? C12 C13 C9 108.7(5) . . ? C12 C13 Zr1 77.4(3) . . ? C9 C13 Zr1 72.8(3) . . ? C15 C14 Zr1 78.7(4) . . ? C16 C15 C14 126.8(5) . . ? C16 C15 Zr1 73.9(3) . . ? C14 C15 Zr1 66.5(3) . . ? C15 C16 C17 126.6(6) . . ? C15 C16 Zr1 73.8(3) . . ? C17 C16 Zr1 66.9(3) . . ? C16 C17 Zr1 79.3(4) . . ? C22 C18 C19 108.2(5) . . ? C22 C18 Zr2 74.5(3) . . ? C19 C18 Zr2 76.2(3) . . ? C20 C19 C18 109.5(5) . . ? C20 C19 Zr2 75.2(3) . . ? C18 C19 Zr2 71.4(3) . . ? C19 C20 C21 107.6(5) . . ? C19 C20 Zr2 73.9(3) . . ? C21 C20 Zr2 71.4(3) . . ? C20 C21 C22 108.4(5) . . ? C20 C21 Zr2 76.4(3) . . ? C22 C21 Zr2 73.6(3) . . ? C18 C22 C21 106.2(5) . . ? C18 C22 C23 124.7(5) . . ? C21 C22 C23 124.9(5) . . ? C18 C22 Zr2 73.1(3) . . ? C21 C22 Zr2 73.3(3) . . ? C23 C22 Zr2 100.7(3) . . ? C22 C23 C24 111.7(5) . . ? C22 C23 C25 111.3(5) . . ? C24 C23 C25 108.9(5) . . ? C22 C23 C26 101.2(4) . . ? C24 C23 C26 111.2(5) . . ? C25 C23 C26 112.4(5) . . ? C27 C26 C30 105.5(6) . . ? C27 C26 C23 126.8(5) . . ? C30 C26 C23 124.8(5) . . ? C27 C26 Zr2 73.9(3) . . ? C30 C26 Zr2 74.5(3) . . ? C23 C26 Zr2 101.9(3) . . ? C26 C27 C28 109.7(6) . . ? C26 C27 Zr2 73.2(3) . . ? C28 C27 Zr2 77.7(4) . . ? C29 C28 C27 108.1(6) . . ? C29 C28 Zr2 74.6(3) . . ? C27 C28 Zr2 70.2(3) . . ? C28 C29 C30 108.4(6) . . ? C28 C29 Zr2 74.4(3) . . ? C30 C29 Zr2 71.1(3) . . ? C29 C30 C26 108.3(6) . . ? C29 C30 Zr2 76.9(3) . . ? C26 C30 Zr2 72.0(3) . . ? C32 C31 Zr2 78.6(4) . . ? C33 C32 C31 127.2(5) . . ? C33 C32 Zr2 74.3(3) . . ? C31 C32 Zr2 67.0(3) . . ? C32 C33 C34 127.1(5) . . ? C32 C33 Zr2 73.4(3) . . ? C34 C33 Zr2 67.3(3) . . ? C33 C34 Zr2 78.8(4) . . ? _refine_diff_density_max 0.700 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.108 #==END #=================Material Relevant to Compound (4) ============== data_4 _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic ? _chemical_formula_iupac '[Me2C(C5H4)2 Zr(C4H4Me2)]' _cell_length_a 6.688(2) _cell_angle_alpha 93.686(6) _cell_length_b 7.534(1) _cell_angle_beta 95.980(7) _cell_length_c 16.993(3) _cell_angle_gamma 111.580(2) _cell_volume 786.90(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Zr ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C19 H24 ZR ' _chemical_formula_moiety ' C19 H24 ZR ' _chemical_compound_source ? _chemical_formula_weight 343.60 _cell_measurement_reflns_used 0 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 0 _cell_formula_units_Z 2 _exptl_crystal_description prism _exptl_crystal_colour gold _exptl_crystal_size_min 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_max 0.5 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 350.05 _exptl_absorpt_coefficient_mu 0.68 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_process_details '\y scan' _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 32.10 _diffrn_ambient_temperature 0 _diffrn_reflns_number 4164 _reflns_number_total 3783 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_observed 3214 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.28 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min -9 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -1.14 _refine_diff_density_max 0.66 _refine_ls_number_reflns 3214 _refine_ls_number_parameters 278 _refine_ls_R_factor_obs 0.0346 _refine_ls_wR_factor_obs 0.0342 _refine_ls_goodness_of_fit_obs 1.0237 _refine_ls_shift/esd_max 0.132987 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-nonius CAD4 ' _diffrn_measurement_method 2\q/\w _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial (Carruthers & Watkin, 1979)' _atom_sites_solution_primary 'Direct Methods' _atom_sites_solution_hydrogens 'Geometric' _refine_ls_hydrogen_treatment 'H atoms placed geometrically after each cycle' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type ZR1 0.30734(3) 0.61973(2) 0.76307(1) 0.0303 1.0000 Uani C1 0.1340(3) 0.7680(3) 0.6092(1) 0.0360 1.0000 Uani C2 -0.0938(5) 0.7713(4) 0.5940(2) 0.0525 1.0000 Uani C3 0.2585(6) 0.8462(4) 0.5409(2) 0.0556 1.0000 Uani C4 0.2544(3) 0.8783(3) 0.6897(1) 0.0328 1.0000 Uani C5 0.1595(4) 0.8812(3) 0.7604(1) 0.0394 1.0000 Uani C6 0.3267(5) 0.9512(3) 0.8257(1) 0.0465 1.0000 Uani C7 0.5231(5) 0.9882(3) 0.7966(2) 0.0470 1.0000 Uani C8 0.4808(4) 0.9420(3) 0.7129(2) 0.0417 1.0000 Uani C9 0.1265(3) 0.5674(3) 0.6228(1) 0.0348 1.0000 Uani C10 0.3032(4) 0.5077(3) 0.6202(1) 0.0407 1.0000 Uani C11 0.2563(5) 0.3357(3) 0.6574(2) 0.0484 1.0000 Uani C12 0.0577(5) 0.2927(3) 0.6843(2) 0.0471 1.0000 Uani C13 -0.0228(4) 0.4368(3) 0.6654(1) 0.0414 1.0000 Uani C14 0.5873(4) 0.5385(3) 0.8163(1) 0.0409 1.0000 Uani C15 0.1514(3) 0.4601(3) 0.8652(1) 0.0424 1.0000 Uani C16 0.5545(3) 0.6297(3) 0.8890(1) 0.0369 1.0000 Uani C17 0.3504(3) 0.5914(3) 0.9125(1) 0.0372 1.0000 Uani C18 0.7526(4) 0.7854(4) 0.9363(2) 0.0506 1.0000 Uani C19 0.3255(5) 0.7023(4) 0.9857(1) 0.0495 1.0000 Uani H21 -0.162(6) 0.697(6) 0.548(2) 0.07(1) 1.0000 Uiso H22 -0.18(1) 0.730(9) 0.643(4) 0.15(3) 1.0000 Uiso H23 -0.092(8) 0.900(8) 0.582(3) 0.10(2) 1.0000 Uiso H31 0.19(1) 0.762(9) 0.490(4) 0.13(2) 1.0000 Uiso H32 0.282(7) 0.973(6) 0.536(3) 0.08(1) 1.0000 Uiso H33 0.404(7) 0.845(5) 0.546(2) 0.063(9) 1.0000 Uiso H51 0.001(5) 0.843(4) 0.761(2) 0.048(7) 1.0000 Uiso H61 0.316(6) 0.971(5) 0.874(2) 0.059(9) 1.0000 Uiso H71 0.661(7) 1.036(6) 0.820(3) 0.08(1) 1.0000 Uiso H81 0.579(6) 0.957(6) 0.680(3) 0.07(1) 1.0000 Uiso H101 0.417(6) 0.570(5) 0.595(2) 0.057(8) 1.0000 Uiso H111 0.361(7) 0.268(6) 0.663(2) 0.07(1) 1.0000 Uiso H121 -0.019(5) 0.184(5) 0.707(2) 0.047(8) 1.0000 Uiso H131 -0.160(6) 0.439(6) 0.677(2) 0.07(1) 1.0000 Uiso H141 0.516(6) 0.411(6) 0.808(2) 0.07(1) 1.0000 Uiso H142 0.739(6) 0.565(5) 0.809(2) 0.064(9) 1.0000 Uiso H151 0.019(5) 0.439(4) 0.884(2) 0.048(7) 1.0000 Uiso H152 0.155(5) 0.348(4) 0.842(2) 0.042(7) 1.0000 Uiso H181 0.866(7) 0.818(6) 0.908(2) 0.07(1) 1.0000 Uiso H182 0.787(9) 0.738(8) 0.972(3) 0.11(2) 1.0000 Uiso H183 0.737(7) 0.904(6) 0.953(3) 0.08(1) 1.0000 Uiso H191 0.16(1) 0.684(8) 0.985(3) 0.11(2) 1.0000 Uiso H192 0.372(8) 0.655(7) 1.030(3) 0.10(1) 1.0000 Uiso H193 0.406(7) 0.831(6) 0.991(2) 0.08(1) 1.0000 Uiso 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 0.0322(1) 0.0282(1) 0.0323(1) 0.00487(6) -0.00140(6) 0.01246(6) C1 0.044(1) 0.0380(9) 0.0308(8) 0.0056(7) -0.0031(7) 0.0180(8) C2 0.059(1) 0.060(1) 0.059(1) -0.006(1) -0.023(1) 0.032(1) C3 0.092(2) 0.052(1) 0.039(1) 0.016(1) 0.016(1) 0.019(1) C4 0.0382(9) 0.0294(7) 0.0344(8) 0.0077(6) 0.0009(7) 0.0143(7) C5 0.054(1) 0.0370(9) 0.0384(9) 0.0063(7) 0.0064(8) 0.0252(9) C6 0.085(2) 0.037(1) 0.036(1) -0.0000(8) -0.006(1) 0.028(1) C7 0.057(1) 0.0318(9) 0.060(1) 0.0011(9) -0.023(1) 0.0091(9) C8 0.038(1) 0.0321(9) 0.056(1) 0.0116(8) 0.0011(9) 0.0065(7) C9 0.0368(9) 0.0365(8) 0.0308(8) 0.0027(6) -0.0015(6) 0.0134(7) C10 0.045(1) 0.044(1) 0.0381(9) -0.0054(8) 0.0012(8) 0.0209(8) C11 0.077(2) 0.037(1) 0.050(1) -0.0083(9) -0.012(1) 0.030(1) C12 0.061(1) 0.0291(9) 0.052(1) 0.0012(8) -0.010(1) 0.0056(9) C13 0.0371(9) 0.040(1) 0.041(1) 0.0036(8) -0.0042(8) 0.0037(8) C14 0.0385(9) 0.050(1) 0.045(1) 0.0057(8) 0.0022(8) 0.0256(9) C15 0.038(1) 0.045(1) 0.045(1) 0.0121(9) 0.0072(8) 0.0139(8) C16 0.0369(9) 0.046(1) 0.0384(9) 0.0101(8) -0.0013(7) 0.0219(8) C17 0.043(1) 0.044(1) 0.0345(9) 0.0117(7) 0.0021(7) 0.0218(8) C18 0.041(1) 0.066(2) 0.051(1) 0.003(1) -0.010(1) 0.020(1) C19 0.062(1) 0.062(1) 0.037(1) 0.009(1) 0.005(1) 0.032(1) _refine_ls_extinction_method ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag ZR1 . C4 . 2.491(2) . ZR1 . C5 . 2.509(2) . ZR1 . C6 . 2.604(2) . ZR1 . C7 . 2.606(2) . ZR1 . C8 . 2.523(2) . ZR1 . C9 . 2.496(2) . ZR1 . C10 . 2.512(2) . ZR1 . C11 . 2.600(2) . ZR1 . C12 . 2.595(2) . ZR1 . C13 . 2.497(2) . ZR1 . C14 . 2.293(2) . ZR1 . C15 . 2.296(2) . ZR1 . C16 . 2.544(2) . ZR1 . C17 . 2.557(2) . C1 . C2 . 1.528(3) . C1 . C3 . 1.520(3) . C1 . C4 . 1.530(3) . C1 . C9 . 1.527(3) . C2 . H21 . 0.90(4) . C2 . H22 . 1.06(7) . C2 . H23 . 1.00(6) . C3 . H31 . 0.99(6) . C3 . H32 . 0.92(5) . C3 . H33 . 0.97(4) . C4 . C5 . 1.420(3) . C4 . C8 . 1.413(3) . C5 . C6 . 1.411(3) . C5 . H51 . 0.99(3) . C6 . C7 . 1.390(5) . C6 . H61 . 0.84(4) . C7 . C8 . 1.414(4) . C7 . H71 . 0.89(5) . C8 . H81 . 0.89(4) . C9 . C10 . 1.415(3) . C9 . C13 . 1.417(3) . C10 . C11 . 1.423(4) . C10 . H101 . 0.90(3) . C11 . C12 . 1.381(4) . C11 . H111 . 1.01(4) . C12 . C13 . 1.418(4) . C12 . H121 . 0.93(3) . C13 . H131 . 0.97(4) . C14 . C16 . 1.451(3) . C14 . H141 . 0.90(4) . C14 . H142 . 0.98(4) . C15 . C17 . 1.450(3) . C15 . H151 . 0.94(3) . C15 . H152 . 0.91(3) . C16 . C17 . 1.394(3) . C16 . C18 . 1.514(3) . C17 . C19 . 1.512(3) . C18 . H181 . 0.91(4) . C18 . H182 . 0.78(6) . C18 . H183 . 0.97(5) . C19 . H191 . 1.05(6) . C19 . H192 . 0.93(5) . C19 . H193 . 0.92(4) . loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 . ZR1 . C5 . 32.99(7) . C4 . ZR1 . C6 . 53.62(7) . C5 . ZR1 . C6 . 31.98(8) . C4 . ZR1 . C7 . 53.35(7) . C5 . ZR1 . C7 . 52.48(8) . C6 . ZR1 . C7 . 31.0(1) . C4 . ZR1 . C8 . 32.72(7) . C5 . ZR1 . C8 . 53.69(8) . C6 . ZR1 . C8 . 52.73(9) . C7 . ZR1 . C8 . 31.96(8) . C4 . ZR1 . C9 . 56.05(6) . C5 . ZR1 . C9 . 77.93(7) . C6 . ZR1 . C9 . 107.68(7) . C7 . ZR1 . C9 . 106.82(7) . C8 . ZR1 . C9 . 76.68(7) . C4 . ZR1 . C10 . 76.63(7) . C5 . ZR1 . C10 . 106.20(7) . C6 . ZR1 . C10 . 129.35(8) . C7 . ZR1 . C10 . 112.05(9) . C8 . ZR1 . C10 . 80.96(8) . C4 . ZR1 . C11 . 107.05(7) . C5 . ZR1 . C11 . 131.16(8) . C6 . ZR1 . C11 . 160.66(8) . C7 . ZR1 . C11 . 141.2(1) . C8 . ZR1 . C11 . 112.34(9) . C4 . ZR1 . C12 . 107.64(7) . C5 . ZR1 . C12 . 115.59(8) . C6 . ZR1 . C12 . 145.3(1) . C7 . ZR1 . C12 . 160.35(8) . C8 . ZR1 . C12 . 129.31(8) . C4 . ZR1 . C13 . 77.75(7) . C5 . ZR1 . C13 . 83.90(8) . C6 . ZR1 . C13 . 115.25(9) . C7 . ZR1 . C13 . 130.71(7) . C8 . ZR1 . C13 . 106.09(7) . C4 . ZR1 . C14 . 138.69(8) . C5 . ZR1 . C14 . 144.60(8) . C6 . ZR1 . C14 . 113.03(9) . C7 . ZR1 . C14 . 94.37(8) . C8 . ZR1 . C14 . 106.19(8) . C4 . ZR1 . C15 . 133.46(8) . C5 . ZR1 . C15 . 101.48(8) . C6 . ZR1 . C15 . 93.63(9) . C7 . ZR1 . C15 . 115.94(9) . C8 . ZR1 . C15 . 146.02(9) . C4 . ZR1 . C16 . 132.15(6) . C5 . ZR1 . C16 . 115.96(7) . C6 . ZR1 . C16 . 84.81(7) . C7 . ZR1 . C16 . 78.86(7) . C8 . ZR1 . C16 . 105.11(7) . C4 . ZR1 . C17 . 130.34(7) . C5 . ZR1 . C17 . 100.45(7) . C6 . ZR1 . C17 . 77.02(7) . C7 . ZR1 . C17 . 87.91(8) . C8 . ZR1 . C17 . 119.76(7) . C9 . ZR1 . C10 . 32.81(7) . C9 . ZR1 . C11 . 53.60(7) . C10 . ZR1 . C11 . 32.26(8) . C9 . ZR1 . C12 . 53.54(7) . C10 . ZR1 . C12 . 52.72(8) . C11 . ZR1 . C12 . 30.8(1) . C9 . ZR1 . C13 . 32.99(7) . C10 . ZR1 . C13 . 54.02(8) . C11 . ZR1 . C13 . 52.93(9) . C12 . ZR1 . C13 . 32.26(8) . C9 . ZR1 . C14 . 129.94(7) . C10 . ZR1 . C14 . 97.26(8) . C11 . ZR1 . C14 . 81.54(8) . C12 . ZR1 . C14 . 99.67(9) . C13 . ZR1 . C14 . 131.50(8) . C9 . ZR1 . C15 . 124.80(7) . C10 . ZR1 . C15 . 132.00(8) . C11 . ZR1 . C15 . 101.53(9) . C12 . ZR1 . C15 . 80.11(9) . C13 . ZR1 . C15 . 91.82(8) . C9 . ZR1 . C16 . 164.34(7) . C10 . ZR1 . C16 . 131.57(7) . C11 . ZR1 . C16 . 112.88(8) . C12 . ZR1 . C16 . 120.18(7) . C13 . ZR1 . C16 . 148.78(7) . C9 . ZR1 . C17 . 158.74(7) . C10 . ZR1 . C17 . 152.93(7) . C11 . ZR1 . C17 . 122.10(8) . C12 . ZR1 . C17 . 110.83(8) . C13 . ZR1 . C17 . 125.94(7) . C14 . ZR1 . C15 . 80.75(8) . C14 . ZR1 . C16 . 34.42(7) . C15 . ZR1 . C16 . 61.88(7) . C14 . ZR1 . C17 . 61.82(7) . C15 . ZR1 . C17 . 34.22(7) . C16 . ZR1 . C17 . 31.72(7) . C2 . C1 . C3 . 109.7(2) . C2 . C1 . C4 . 111.3(2) . C3 . C1 . C4 . 111.9(2) . C2 . C1 . C9 . 111.5(2) . C3 . C1 . C9 . 112.2(2) . C4 . C1 . C9 . 100.1(1) . C1 . C2 . H21 . 108.1(26) . C1 . C2 . H22 . 111.2(39) . H21 . C2 . H22 . 113.5(41) . C1 . C2 . H23 . 112.6(30) . H21 . C2 . H23 . 102.3(37) . H22 . C2 . H23 . 108.8(48) . C1 . C3 . H31 . 110.8(35) . C1 . C3 . H32 . 113.8(29) . H31 . C3 . H32 . 112.0(43) . C1 . C3 . H33 . 114.0(22) . H31 . C3 . H33 . 102.0(43) . H32 . C3 . H33 . 103.3(35) . ZR1 . C4 . C1 . 102.0(1) . ZR1 . C4 . C5 . 74.2(1) . C1 . C4 . C5 . 125.6(2) . ZR1 . C4 . C8 . 74.9(1) . C1 . C4 . C8 . 125.0(2) . C5 . C4 . C8 . 106.7(2) . ZR1 . C5 . C4 . 72.8(1) . ZR1 . C5 . C6 . 77.7(1) . C4 . C5 . C6 . 108.7(2) . ZR1 . C5 . H51 . 117.2(18) . C4 . C5 . H51 . 123.6(18) . C6 . C5 . H51 . 127.6(18) . ZR1 . C6 . C5 . 70.3(1) . ZR1 . C6 . C7 . 74.6(1) . C5 . C6 . C7 . 107.8(2) . ZR1 . C6 . H61 . 121.5(25) . C5 . C6 . H61 . 128.4(26) . C7 . C6 . H61 . 123.9(26) . ZR1 . C7 . C6 . 74.4(1) . ZR1 . C7 . C8 . 70.8(1) . C6 . C7 . C8 . 108.6(2) . ZR1 . C7 . H71 . 121.9(28) . C6 . C7 . H71 . 133.0(29) . C8 . C7 . H71 . 118.3(29) . ZR1 . C8 . C4 . 72.4(1) . ZR1 . C8 . C7 . 77.2(1) . C4 . C8 . C7 . 108.2(2) . ZR1 . C8 . H81 . 119.2(26) . C4 . C8 . H81 . 124.9(26) . C7 . C8 . H81 . 126.8(26) . ZR1 . C9 . C1 . 101.9(1) . ZR1 . C9 . C10 . 74.2(1) . C1 . C9 . C10 . 124.8(2) . ZR1 . C9 . C13 . 73.5(1) . C1 . C9 . C13 . 125.1(2) . C10 . C9 . C13 . 106.9(2) . ZR1 . C10 . C9 . 72.9(1) . ZR1 . C10 . C11 . 77.3(1) . C9 . C10 . C11 . 108.3(2) . ZR1 . C10 . H101 . 118.9(22) . C9 . C10 . H101 . 122.1(22) . C11 . C10 . H101 . 129.5(22) . ZR1 . C11 . C10 . 70.5(1) . ZR1 . C11 . C12 . 74.4(1) . C10 . C11 . C12 . 108.0(2) . ZR1 . C11 . H111 . 118.9(23) . C10 . C11 . H111 . 122.0(23) . C12 . C11 . H111 . 129.9(23) . ZR1 . C12 . C11 . 74.8(1) . ZR1 . C12 . C13 . 70.0(1) . C11 . C12 . C13 . 108.6(2) . ZR1 . C12 . H121 . 124.9(20) . C11 . C12 . H121 . 127.1(21) . C13 . C12 . H121 . 124.1(21) . ZR1 . C13 . C9 . 73.5(1) . ZR1 . C13 . C12 . 77.7(1) . C9 . C13 . C12 . 108.1(2) . ZR1 . C13 . H131 . 117.7(23) . C9 . C13 . H131 . 127.0(23) . C12 . C13 . H131 . 124.9(23) . ZR1 . C14 . C16 . 82.3(1) . ZR1 . C14 . H141 . 96.8(25) . C16 . C14 . H141 . 114.7(25) . ZR1 . C14 . H142 . 137.8(22) . C16 . C14 . H142 . 115.7(21) . H141 . C14 . H142 . 107.6(32) . ZR1 . C15 . C17 . 82.8(1) . ZR1 . C15 . H151 . 132.6(19) . C17 . C15 . H151 . 119.2(19) . ZR1 . C15 . H152 . 90.7(19) . C17 . C15 . H152 . 116.5(19) . H151 . C15 . H152 . 111.0(25) . ZR1 . C16 . C14 . 63.3(1) . ZR1 . C16 . C17 . 74.7(1) . C14 . C16 . C17 . 123.1(2) . ZR1 . C16 . C18 . 133.5(2) . C14 . C16 . C18 . 116.7(2) . C17 . C16 . C18 . 120.0(2) . ZR1 . C17 . C15 . 63.0(1) . ZR1 . C17 . C16 . 73.6(1) . C15 . C17 . C16 . 122.8(2) . ZR1 . C17 . C19 . 134.7(1) . C15 . C17 . C19 . 116.4(2) . C16 . C17 . C19 . 120.5(2) . C16 . C18 . H181 . 110.3(25) . C16 . C18 . H182 . 105.7(39) . H181 . C18 . H182 . 105.2(46) . C16 . C18 . H183 . 116.3(28) . H181 . C18 . H183 . 105.9(35) . H182 . C18 . H183 . 113.0(48) . C17 . C19 . H191 . 109.8(31) . C17 . C19 . H192 . 107.9(31) . H191 . C19 . H192 . 110.0(42) . C17 . C19 . H193 . 115.1(26) . H191 . C19 . H193 . 107.7(37) . H192 . C19 . H193 . 106.2(37) . #==END #=================Compound(6)======================== data_6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C30 H38 Cl2 O2 Zr2' _chemical_formula_structural 'C30 H38 ZR2 CL2 O2' _chemical_formula_analytical ? _chemical_formula_sum 'C30 H38 Cl2 O2 Zr2' _chemical_formula_weight 683.94 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.106(3) _cell_length_b 8.853(2) _cell_length_c 21.598(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.83(3) _cell_angle_gamma 90.00 _cell_volume 2977.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour gold _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'mot measured' _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method none _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.967 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'NONIUS FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST TV Area detector' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4573 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4573 _reflns_number_observed 2949 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Pflgrath, 1989)' _computing_cell_refinement MADNES _computing_data_reduction 'ABSURD (within MADNES)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0320P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4571 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_obs 0.0426 _refine_ls_wR_factor_all 0.1342 _refine_ls_wR_factor_obs 0.0985 _refine_ls_goodness_of_fit_all 0.876 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_restrained_S_all 1.154 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.94241(4) 0.45817(7) 0.13263(3) 0.0205(2) Uani 1 d . . Zr2 Zr 0.91436(4) 0.62724(6) 0.29271(3) 0.0194(2) Uani 1 d . . Cl3 Cl 0.75899(10) 0.6777(2) 0.25463(8) 0.0290(4) Uani 1 d . . Cl4 Cl 1.01365(11) 0.6771(2) 0.09784(8) 0.0365(4) Uani 1 d . . O5 O 0.9324(2) 0.5329(4) 0.2158(2) 0.0227(9) Uani 1 d . . C1 C 1.0415(4) 0.7015(7) 0.4278(3) 0.028(2) Uani 1 d . . C2 C 1.1375(4) 0.6629(7) 0.4466(3) 0.038(2) Uani 1 d . . H2A H 1.1709(4) 0.7549(7) 0.4605(3) 0.057 Uiso 1 calc R . H2B H 1.1538(4) 0.6195(7) 0.4096(3) 0.057 Uiso 1 calc R . H2C H 1.1492(4) 0.5895(7) 0.4818(3) 0.057 Uiso 1 calc R . C3 C 1.0172(4) 0.7802(7) 0.4846(3) 0.036(2) Uani 1 d . . H3A H 1.0541(4) 0.8687(7) 0.4978(3) 0.055 Uiso 1 calc R . H3B H 1.0252(4) 0.7096(7) 0.5206(3) 0.055 Uiso 1 calc R . H3C H 0.9570(4) 0.8123(7) 0.4715(3) 0.055 Uiso 1 calc R . C4 C 0.9855(4) 0.5635(6) 0.4058(3) 0.0211(14) Uani 1 d . . C5 C 1.0079(4) 0.4466(6) 0.3660(3) 0.0236(15) Uani 1 d . . H5A H 1.0676(4) 0.4181(6) 0.3650(3) 0.028 Uiso 1 calc R . C6 C 0.9324(4) 0.3591(6) 0.3402(3) 0.0234(15) Uani 1 d . . H6A H 0.9295(4) 0.2628(6) 0.3156(3) 0.028 Uiso 1 calc R . C7 C 0.8637(4) 0.4261(6) 0.3611(3) 0.025(2) Uani 1 d . . H7A H 0.8040(4) 0.3852(6) 0.3534(3) 0.030 Uiso 1 calc R . C8 C 0.8975(4) 0.5515(6) 0.4005(3) 0.0236(14) Uani 1 d . . H8A H 0.8654(4) 0.6108(6) 0.4264(3) 0.028 Uiso 1 calc R . C9 C 1.0161(4) 0.7960(6) 0.3660(3) 0.0234(15) Uani 1 d . . C10 C 0.9398(4) 0.8801(6) 0.3450(3) 0.0238(14) Uani 1 d . . H10A H 0.9059(4) 0.9238(6) 0.3736(3) 0.029 Uiso 1 calc R . C11 C 0.9266(4) 0.9130(6) 0.2798(3) 0.029(2) Uani 1 d . . H11A H 0.8807(4) 0.9802(6) 0.2540(3) 0.034 Uiso 1 calc R . C12 C 0.9937(4) 0.8499(6) 0.2586(3) 0.027(2) Uani 1 d . . H12A H 1.0045(4) 0.8647(6) 0.2155(3) 0.032 Uiso 1 calc R . C13 C 1.0500(4) 0.7753(7) 0.3123(3) 0.028(2) Uani 1 d . . H13A H 1.1080(4) 0.7334(7) 0.3134(3) 0.034 Uiso 1 calc R . C21 C 0.8808(4) 0.1420(7) 0.0685(3) 0.0247(15) Uani 1 d . . C22 C 0.8863(4) 0.0796(7) 0.0032(3) 0.034(2) Uani 1 d . . H22A H 0.9144(4) 0.1542(7) -0.0182(3) 0.050 Uiso 1 calc R . H22B H 0.8283(4) 0.0591(7) -0.0234(3) 0.050 Uiso 1 calc R . H22C H 0.9198(4) -0.0141(7) 0.0096(3) 0.050 Uiso 1 calc R . C23 C 0.8372(4) 0.0239(6) 0.1006(3) 0.032(2) Uani 1 d . . H23A H 0.7819(4) -0.0041(6) 0.0717(3) 0.048 Uiso 1 calc R . H23B H 0.8278(4) 0.0655(6) 0.1403(3) 0.048 Uiso 1 calc R . H23C H 0.8739(4) -0.0658(6) 0.1105(3) 0.048 Uiso 1 calc R . C24 C 0.9675(4) 0.1896(6) 0.1117(3) 0.026(2) Uani 1 d . . C25 C 0.9848(4) 0.2092(6) 0.1782(3) 0.026(2) Uani 1 d . . H25A H 0.9557(4) 0.1530(6) 0.2069(3) 0.032 Uiso 1 calc R . C26 C 1.0625(4) 0.2941(7) 0.1994(3) 0.033(2) Uani 1 d . . H26A H 1.0944(4) 0.3125(7) 0.2449(3) 0.040 Uiso 1 calc R . C27 C 1.0894(4) 0.3342(7) 0.1461(3) 0.031(2) Uani 1 d . . H27A H 1.1440(4) 0.3884(7) 0.1464(3) 0.038 Uiso 1 calc R . C28 C 1.0329(4) 0.2688(7) 0.0917(3) 0.030(2) Uani 1 d . . H28A H 1.0418(4) 0.2671(7) 0.0475(3) 0.036 Uiso 1 calc R . C29 C 0.8332(4) 0.2973(7) 0.0614(3) 0.0242(15) Uani 1 d . . C30 C 0.8494(4) 0.4159(7) 0.0221(3) 0.029(2) Uani 1 d . . H30A H 0.8700(4) 0.4036(7) -0.0175(3) 0.035 Uiso 1 calc R . C31 C 0.8159(4) 0.5521(7) 0.0422(3) 0.030(2) Uani 1 d . . H31A H 0.8124(4) 0.6523(7) 0.0203(3) 0.036 Uiso 1 calc R . C32 C 0.7814(4) 0.5180(7) 0.0932(3) 0.031(2) Uani 1 d . . H32A H 0.7483(4) 0.5887(7) 0.1140(3) 0.037 Uiso 1 calc R . C33 C 0.7929(3) 0.3599(7) 0.1055(3) 0.025(2) Uani 1 d . . H33A H 0.7667(3) 0.3009(7) 0.1351(3) 0.031 Uiso 1 calc R . C101 C 1.2685(6) 0.5002(9) 0.3081(5) 0.085(3) Uani 1 d . . H10I H 1.3124(6) 0.5204(9) 0.2850(5) 0.128 Uiso 1 calc R . H10J H 1.2825(6) 0.5559(9) 0.3487(5) 0.128 Uiso 1 calc R . H10K H 1.2123(6) 0.5328(9) 0.2820(5) 0.128 Uiso 1 calc R . C102 C 1.2662(5) 0.3448(10) 0.3205(4) 0.067(3) Uani 1 d . . H10E H 1.2529(5) 0.2882(10) 0.2796(4) 0.081 Uiso 1 calc R . H10F H 1.3232(5) 0.3113(10) 0.3464(4) 0.081 Uiso 1 calc R . O103 O 1.2037(3) 0.3142(5) 0.3536(2) 0.0463(13) Uani 1 d . . C104 C 1.2010(6) 0.1535(9) 0.3709(4) 0.060(2) Uani 1 d . . H10G H 1.1792(6) 0.0922(9) 0.3318(4) 0.073 Uiso 1 calc R . H10H H 1.2595(6) 0.1180(9) 0.3925(4) 0.073 Uiso 1 calc R . C105 C 1.1450(5) 0.1357(8) 0.4134(5) 0.075(3) Uani 1 d . . H10B H 1.1429(5) 0.0290(8) 0.4250(5) 0.112 Uiso 1 calc R . H10C H 1.0870(5) 0.1703(8) 0.3917(5) 0.112 Uiso 1 calc R . H10D H 1.1671(5) 0.1958(8) 0.4522(5) 0.112 Uiso 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 0.0205(3) 0.0236(4) 0.0183(4) 0.0014(3) 0.0065(3) 0.0010(3) Zr2 0.0202(3) 0.0214(4) 0.0168(3) 0.0021(3) 0.0051(3) 0.0010(3) Cl3 0.0215(9) 0.0357(11) 0.0292(10) 0.0050(7) 0.0052(7) 0.0055(7) Cl4 0.0417(11) 0.0361(11) 0.0358(11) 0.0040(8) 0.0173(9) -0.0073(8) O5 0.026(2) 0.024(2) 0.019(2) -0.001(2) 0.006(2) -0.002(2) C1 0.027(4) 0.027(4) 0.025(4) 0.000(3) -0.004(3) -0.002(3) C2 0.039(4) 0.038(4) 0.030(4) 0.008(3) -0.006(4) -0.005(3) C3 0.048(5) 0.037(4) 0.022(4) -0.001(3) 0.004(4) -0.007(3) C4 0.032(4) 0.018(4) 0.013(3) 0.003(3) 0.004(3) 0.001(3) C5 0.024(4) 0.021(4) 0.025(4) 0.004(3) 0.005(3) 0.001(3) C6 0.033(4) 0.010(3) 0.025(4) 0.000(3) 0.003(3) 0.004(3) C7 0.024(4) 0.033(4) 0.017(4) 0.006(3) 0.005(3) -0.008(3) C8 0.029(4) 0.024(4) 0.019(4) 0.000(3) 0.009(3) 0.004(3) C9 0.030(4) 0.018(4) 0.023(4) -0.001(3) 0.008(3) -0.010(3) C10 0.029(4) 0.015(3) 0.025(4) 0.002(3) 0.003(3) 0.003(3) C11 0.036(4) 0.019(4) 0.028(4) 0.003(3) 0.004(3) 0.001(3) C12 0.037(4) 0.016(4) 0.027(4) 0.007(3) 0.009(3) -0.005(3) C13 0.025(4) 0.025(4) 0.036(4) -0.004(3) 0.010(3) -0.007(3) C21 0.024(4) 0.028(4) 0.023(4) 0.000(3) 0.008(3) -0.002(3) C22 0.038(4) 0.031(4) 0.037(4) -0.006(3) 0.019(4) -0.003(3) C23 0.040(4) 0.031(4) 0.030(4) -0.001(3) 0.017(3) -0.006(3) C24 0.024(4) 0.021(4) 0.032(4) 0.005(3) 0.007(3) 0.004(3) C25 0.030(4) 0.022(4) 0.026(4) 0.000(3) 0.004(3) 0.007(3) C26 0.029(4) 0.029(4) 0.035(5) -0.004(3) -0.005(4) 0.007(3) C27 0.018(4) 0.038(4) 0.039(5) 0.000(3) 0.007(3) 0.000(3) C28 0.028(4) 0.028(4) 0.039(5) -0.003(3) 0.017(4) 0.004(3) C29 0.021(4) 0.030(4) 0.021(4) 0.003(3) 0.003(3) 0.000(3) C30 0.031(4) 0.037(4) 0.017(4) 0.004(3) 0.003(3) 0.000(3) C31 0.026(4) 0.028(4) 0.033(4) 0.006(3) 0.002(3) 0.012(3) C32 0.015(3) 0.049(5) 0.025(4) -0.005(3) -0.003(3) 0.005(3) C33 0.015(3) 0.035(4) 0.027(4) -0.004(3) 0.008(3) -0.003(3) C101 0.103(8) 0.071(7) 0.096(9) -0.010(6) 0.051(7) -0.036(6) C102 0.035(5) 0.101(8) 0.064(6) 0.005(5) 0.010(5) -0.007(5) O103 0.034(3) 0.052(3) 0.053(4) -0.004(3) 0.013(3) -0.003(2) C104 0.083(7) 0.050(6) 0.039(5) 0.004(4) -0.001(5) 0.026(5) C105 0.058(6) 0.037(5) 0.111(9) 0.019(5) -0.010(6) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O5 1.958(4) . ? Zr1 C25 2.439(6) . ? Zr1 Cl4 2.466(2) . ? Zr1 C29 2.470(6) . ? Zr1 C24 2.473(6) . ? Zr1 C33 2.485(6) . ? Zr1 C30 2.500(6) . ? Zr1 C28 2.525(6) . ? Zr1 C26 2.550(6) . ? Zr1 C27 2.558(6) . ? Zr1 C32 2.569(6) . ? Zr1 C31 2.573(6) . ? Zr2 O5 1.947(4) . ? Zr2 Cl3 2.467(2) . ? Zr2 C9 2.469(6) . ? Zr2 C5 2.473(6) . ? Zr2 C4 2.484(6) . ? Zr2 C13 2.489(6) . ? Zr2 C10 2.494(6) . ? Zr2 C8 2.505(6) . ? Zr2 C11 2.558(6) . ? Zr2 C12 2.558(6) . ? Zr2 C6 2.573(6) . ? Zr2 C7 2.576(6) . ? C1 C4 1.521(8) . ? C1 C2 1.534(9) . ? C1 C9 1.539(8) . ? C1 C3 1.546(8) . ? C4 C8 1.397(8) . ? C4 C5 1.449(8) . ? C5 C6 1.430(8) . ? C6 C7 1.426(8) . ? C7 C8 1.420(8) . ? C9 C10 1.409(8) . ? C9 C13 1.415(8) . ? C10 C11 1.401(8) . ? C11 C12 1.393(8) . ? C12 C13 1.436(8) . ? C21 C23 1.521(8) . ? C21 C24 1.527(8) . ? C21 C22 1.538(8) . ? C21 C29 1.563(8) . ? C24 C25 1.402(9) . ? C24 C28 1.421(8) . ? C25 C26 1.432(8) . ? C26 C27 1.377(9) . ? C27 C28 1.413(9) . ? C29 C33 1.397(8) . ? C29 C30 1.415(8) . ? C30 C31 1.433(8) . ? C31 C32 1.387(9) . ? C32 C33 1.428(8) . ? C101 C102 1.404(10) . ? C102 O103 1.402(8) . ? O103 C104 1.474(8) . ? C104 C105 1.450(11) . ? 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 O5 Zr1 C25 90.9(2) . . ? O5 Zr1 Cl4 99.67(12) . . ? C25 Zr1 Cl4 136.8(2) . . ? O5 Zr1 C29 123.6(2) . . ? C25 Zr1 C29 79.1(2) . . ? Cl4 Zr1 C29 125.19(15) . . ? O5 Zr1 C24 123.2(2) . . ? C25 Zr1 C24 33.2(2) . . ? Cl4 Zr1 C24 126.11(15) . . ? C29 Zr1 C24 57.0(2) . . ? O5 Zr1 C33 91.8(2) . . ? C25 Zr1 C33 86.1(2) . . ? Cl4 Zr1 C33 134.6(2) . . ? C29 Zr1 C33 32.8(2) . . ? C24 Zr1 C33 79.3(2) . . ? O5 Zr1 C30 139.1(2) . . ? C25 Zr1 C30 106.7(2) . . ? Cl4 Zr1 C30 92.22(15) . . ? C29 Zr1 C30 33.1(2) . . ? C24 Zr1 C30 76.6(2) . . ? C33 Zr1 C30 54.2(2) . . ? O5 Zr1 C28 137.4(2) . . ? C25 Zr1 C28 54.1(2) . . ? Cl4 Zr1 C28 93.43(15) . . ? C29 Zr1 C28 77.4(2) . . ? C24 Zr1 C28 33.0(2) . . ? C33 Zr1 C28 107.2(2) . . ? C30 Zr1 C28 79.9(2) . . ? O5 Zr1 C26 84.4(2) . . ? C25 Zr1 C26 33.3(2) . . ? Cl4 Zr1 C26 106.0(2) . . ? C29 Zr1 C26 109.9(2) . . ? C24 Zr1 C26 54.5(2) . . ? C33 Zr1 C26 118.9(2) . . ? C30 Zr1 C26 129.6(2) . . ? C28 Zr1 C26 53.0(2) . . ? O5 Zr1 C27 109.4(2) . . ? C25 Zr1 C27 53.9(2) . . ? Cl4 Zr1 C27 83.25(15) . . ? C29 Zr1 C27 108.3(2) . . ? C24 Zr1 C27 54.4(2) . . ? C33 Zr1 C27 133.6(2) . . ? C30 Zr1 C27 110.8(2) . . ? C28 Zr1 C27 32.3(2) . . ? C26 Zr1 C27 31.3(2) . . ? O5 Zr1 C32 85.5(2) . . ? C25 Zr1 C32 118.3(2) . . ? Cl4 Zr1 C32 104.2(2) . . ? C29 Zr1 C32 54.2(2) . . ? C24 Zr1 C32 109.6(2) . . ? C33 Zr1 C32 32.8(2) . . ? C30 Zr1 C32 53.6(2) . . ? C28 Zr1 C32 130.2(2) . . ? C26 Zr1 C32 149.3(2) . . ? C27 Zr1 C32 162.3(2) . . ? O5 Zr1 C31 110.6(2) . . ? C25 Zr1 C31 133.1(2) . . ? Cl4 Zr1 C31 81.6(2) . . ? C29 Zr1 C31 54.2(2) . . ? C24 Zr1 C31 107.9(2) . . ? C33 Zr1 C31 53.3(2) . . ? C30 Zr1 C31 32.8(2) . . ? C28 Zr1 C31 111.4(2) . . ? C26 Zr1 C31 162.2(2) . . ? C27 Zr1 C31 139.0(2) . . ? C32 Zr1 C31 31.3(2) . . ? O5 Zr2 Cl3 98.81(12) . . ? O5 Zr2 C9 126.0(2) . . ? Cl3 Zr2 C9 123.67(15) . . ? O5 Zr2 C5 94.0(2) . . ? Cl3 Zr2 C5 136.95(14) . . ? C9 Zr2 C5 77.6(2) . . ? O5 Zr2 C4 127.6(2) . . ? Cl3 Zr2 C4 122.85(15) . . ? C9 Zr2 C4 56.2(2) . . ? C5 Zr2 C4 34.0(2) . . ? O5 Zr2 C13 93.1(2) . . ? Cl3 Zr2 C13 137.10(15) . . ? C9 Zr2 C13 33.2(2) . . ? C5 Zr2 C13 82.4(2) . . ? C4 Zr2 C13 77.8(2) . . ? O5 Zr2 C10 136.8(2) . . ? Cl3 Zr2 C10 91.33(14) . . ? C9 Zr2 C10 33.0(2) . . ? C5 Zr2 C10 106.7(2) . . ? C4 Zr2 C10 77.2(2) . . ? C13 Zr2 C10 54.2(2) . . ? O5 Zr2 C8 139.0(2) . . ? Cl3 Zr2 C8 90.92(14) . . ? C9 Zr2 C8 77.2(2) . . ? C5 Zr2 C8 54.9(2) . . ? C4 Zr2 C8 32.5(2) . . ? C13 Zr2 C8 106.4(2) . . ? C10 Zr2 C8 82.2(2) . . ? O5 Zr2 C11 107.4(2) . . ? Cl3 Zr2 C11 83.37(15) . . ? C9 Zr2 C11 54.2(2) . . ? C5 Zr2 C11 131.1(2) . . ? C4 Zr2 C11 107.7(2) . . ? C13 Zr2 C11 53.8(2) . . ? C10 Zr2 C11 32.2(2) . . ? C8 Zr2 C11 113.3(2) . . ? O5 Zr2 C12 83.7(2) . . ? Cl3 Zr2 C12 107.67(14) . . ? C9 Zr2 C12 54.5(2) . . ? C5 Zr2 C12 114.5(2) . . ? C4 Zr2 C12 108.6(2) . . ? C13 Zr2 C12 33.0(2) . . ? C10 Zr2 C12 53.3(2) . . ? C8 Zr2 C12 130.9(2) . . ? C11 Zr2 C12 31.6(2) . . ? O5 Zr2 C6 85.3(2) . . ? Cl3 Zr2 C6 107.54(14) . . ? C9 Zr2 C6 108.3(2) . . ? C5 Zr2 C6 32.8(2) . . ? C4 Zr2 C6 54.6(2) . . ? C13 Zr2 C6 114.4(2) . . ? C10 Zr2 C6 131.2(2) . . ? C8 Zr2 C6 53.8(2) . . ? C11 Zr2 C6 162.2(2) . . ? C12 Zr2 C6 144.3(2) . . ? O5 Zr2 C7 109.3(2) . . ? Cl3 Zr2 C7 82.71(14) . . ? C9 Zr2 C7 107.8(2) . . ? C5 Zr2 C7 54.3(2) . . ? C4 Zr2 C7 54.0(2) . . ? C13 Zr2 C7 131.3(2) . . ? C10 Zr2 C7 113.6(2) . . ? C8 Zr2 C7 32.4(2) . . ? C11 Zr2 C7 142.3(2) . . ? C12 Zr2 C7 162.3(2) . . ? C6 Zr2 C7 32.2(2) . . ? Zr2 O5 Zr1 173.1(2) . . ? C4 C1 C2 112.3(5) . . ? C4 C1 C9 99.3(5) . . ? C2 C1 C9 112.1(5) . . ? C4 C1 C3 111.1(5) . . ? C2 C1 C3 109.5(5) . . ? C9 C1 C3 112.3(5) . . ? C8 C4 C5 107.4(5) . . ? C8 C4 C1 126.5(5) . . ? C5 C4 C1 122.8(5) . . ? C8 C4 Zr2 74.6(3) . . ? C5 C4 Zr2 72.6(3) . . ? C1 C4 Zr2 102.2(4) . . ? C6 C5 C4 107.6(5) . . ? C6 C5 Zr2 77.5(3) . . ? C4 C5 Zr2 73.4(3) . . ? C7 C6 C5 107.6(5) . . ? C7 C6 Zr2 74.0(3) . . ? C5 C6 Zr2 69.7(3) . . ? C8 C7 C6 107.8(5) . . ? C8 C7 Zr2 71.0(3) . . ? C6 C7 Zr2 73.8(3) . . ? C4 C8 C7 109.5(5) . . ? C4 C8 Zr2 72.9(3) . . ? C7 C8 Zr2 76.6(3) . . ? C10 C9 C13 107.0(5) . . ? C10 C9 C1 125.6(5) . . ? C13 C9 C1 124.6(6) . . ? C10 C9 Zr2 74.5(3) . . ? C13 C9 Zr2 74.2(3) . . ? C1 C9 Zr2 102.3(3) . . ? C11 C10 C9 109.2(6) . . ? C11 C10 Zr2 76.5(4) . . ? C9 C10 Zr2 72.5(3) . . ? C12 C11 C10 108.4(6) . . ? C12 C11 Zr2 74.2(3) . . ? C10 C11 Zr2 71.4(3) . . ? C11 C12 C13 107.6(6) . . ? C11 C12 Zr2 74.2(3) . . ? C13 C12 Zr2 70.9(3) . . ? C9 C13 C12 107.8(5) . . ? C9 C13 Zr2 72.6(3) . . ? C12 C13 Zr2 76.1(3) . . ? C23 C21 C24 111.6(5) . . ? C23 C21 C22 108.2(5) . . ? C24 C21 C22 113.6(5) . . ? C23 C21 C29 112.2(5) . . ? C24 C21 C29 99.5(4) . . ? C22 C21 C29 111.6(5) . . ? C25 C24 C28 106.4(6) . . ? C25 C24 C21 124.8(6) . . ? C28 C24 C21 125.7(6) . . ? C25 C24 Zr1 72.1(3) . . ? C28 C24 Zr1 75.5(3) . . ? C21 C24 Zr1 102.1(4) . . ? C24 C25 C26 108.7(6) . . ? C24 C25 Zr1 74.8(3) . . ? C26 C25 Zr1 77.6(3) . . ? C27 C26 C25 107.7(6) . . ? C27 C26 Zr1 74.7(4) . . ? C25 C26 Zr1 69.1(3) . . ? C26 C27 C28 108.5(6) . . ? C26 C27 Zr1 74.0(4) . . ? C28 C27 Zr1 72.6(3) . . ? C27 C28 C24 108.6(6) . . ? C27 C28 Zr1 75.1(4) . . ? C24 C28 Zr1 71.5(3) . . ? C33 C29 C30 107.6(5) . . ? C33 C29 C21 125.8(6) . . ? C30 C29 C21 123.4(5) . . ? C33 C29 Zr1 74.2(3) . . ? C30 C29 Zr1 74.6(3) . . ? C21 C29 Zr1 101.2(4) . . ? C29 C30 C31 107.6(6) . . ? C29 C30 Zr1 72.3(4) . . ? C31 C30 Zr1 76.4(4) . . ? C32 C31 C30 108.4(6) . . ? C32 C31 Zr1 74.2(4) . . ? C30 C31 Zr1 70.8(3) . . ? C31 C32 C33 107.5(6) . . ? C31 C32 Zr1 74.5(3) . . ? C33 C32 Zr1 70.4(3) . . ? C29 C33 C32 108.9(5) . . ? C29 C33 Zr1 73.1(3) . . ? C32 C33 Zr1 76.9(3) . . ? O103 C102 C101 110.1(7) . . ? C102 O103 C104 112.8(6) . . ? C105 C104 O103 109.2(6) . . ? _refine_diff_density_max 0.948 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.132 #==END #===================Compound(8)================= data_8 _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_publication_material 'WinGX publication routines (Farrugia,1998)' _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H45 B1 F15 o1 P1 Zr1' _chemical_formula_structural 'C42 H45 B1 F15 o1 P1 ZR1' _chemical_formula_sum 'C42 H45 B1 F15 O1 P1 Zr1' _chemical_formula_weight 983.78 _chemical_compound_source ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.771(2) _cell_length_b 10.379(2) _cell_length_c 24.403(2) _cell_angle_alpha 90 _cell_angle_beta 116.94(5) _cell_angle_gamma 90 _cell_volume 8076.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 _exptl_crystal_description prism _exptl_crystal_colour gold _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method none _exptl_crystal_F_000 4000 _exptl_special_details ; ? ; _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type DIFABS _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 15498 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.1706 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.09 _reflns_number_total 6006 _reflns_number_gt 3580 _reflns_threshold_expression >2sigma(I) _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0628P)^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_extinction_method none _refine_ls_number_reflns 6003 _refine_ls_number_parameters 573 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_gt 0.1274 _refine_ls_wR_factor_all 0.1381 _refine_ls_goodness_of_fit_gt 1.129 _refine_ls_goodness_of_fit_all 0.9 _refine_ls_restrained_S_all 0.917 _refine_ls_restrained_S_obs 1.13 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 1.323 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.113 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.11674(2) 0.24543(5) 0.06894(2) 0.0188(2) Uani 1 d . . P1 P 0.15532(6) 0.1689(2) -0.00064(8) 0.0393(5) Uani 1 d . . F1 F 0.09132(12) 0.5566(3) 0.1936(2) 0.0567(12) Uani 1 d . . F2 F 0.08151(13) 0.8082(3) 0.1914(2) 0.0648(14) Uani 1 d . . F3 F 0.13891(12) 0.9630(3) 0.2794(2) 0.0457(11) Uani 1 d . . F4 F 0.20882(11) 0.8532(3) 0.3719(2) 0.0401(10) Uani 1 d . . F5 F 0.21887(10) 0.6008(3) 0.3771(2) 0.0349(9) Uani 1 d . . F6 F 0.07723(14) 0.3694(5) 0.2802(2) 0.092(2) Uani 1 d . . F7 F 0.0539(2) 0.2952(6) 0.3644(2) 0.110(2) Uani 1 d . . F8 F 0.11136(13) 0.2446(4) 0.4818(2) 0.0588(11) Uani 1 d . . F9 F 0.19325(15) 0.2940(4) 0.5145(2) 0.0698(14) Uani 1 d . . F10 F 0.21835(13) 0.3692(4) 0.4323(2) 0.0566(12) Uani 1 d . . F11 F 0.22649(10) 0.5374(3) 0.2634(2) 0.0330(9) Uani 1 d . . F12 F 0.29942(11) 0.4438(3) 0.2779(2) 0.0400(9) Uani 1 d . . F13 F 0.32912(11) 0.2141(3) 0.3367(2) 0.0453(10) Uani 1 d . . F14 F 0.27982(12) 0.0715(3) 0.3731(2) 0.0504(11) Uani 1 d . . F15 F 0.20482(11) 0.1580(3) 0.3552(2) 0.0383(9) Uani 1 d . . B1 B 0.1627(2) 0.4008(6) 0.2932(3) 0.025(2) Uani 1 d . . C1 C 0.0728(2) 0.1292(5) 0.1079(3) 0.0239(14) Uani 1 d . . H1 H 0.0669(2) 0.1719(5) 0.1366(3) 0.029 Uiso 1 calc R . C2 C 0.1065(2) 0.0430(5) 0.1219(3) 0.028(2) Uani 1 d . . H2 H 0.1262(2) 0.0182(5) 0.1610(3) 0.034 Uiso 1 calc R . C3 C 0.1048(2) 0.0021(5) 0.0667(3) 0.032(2) Uani 1 d . . H3 H 0.1233(2) -0.0554(5) 0.0628(3) 0.038 Uiso 1 calc R . C4 C 0.0700(2) 0.0621(5) 0.0169(3) 0.0275(15) Uani 1 d . . H4 H 0.0622(2) 0.0518(5) -0.0247(3) 0.033 Uiso 1 calc R . C5 C 0.0494(2) 0.1404(5) 0.0429(3) 0.0220(14) Uani 1 d . . C6 C 0.0180(2) 0.2477(5) 0.0094(2) 0.0252(13) Uani 1 d . . C7 C -0.0129(2) 0.2106(6) -0.0578(3) 0.047(2) Uani 1 d . . H7A H -0.0286(9) 0.136(2) -0.0575(3) 0.071 Uiso 1 calc R . H7B H 0.0026(2) 0.192(4) -0.0802(6) 0.071 Uiso 1 calc R . H7C H -0.0317(9) 0.2809(17) -0.0770(7) 0.071 Uiso 1 calc R . C8 C -0.0066(2) 0.2887(6) 0.0448(3) 0.047(2) Uani 1 d . . H8A H -0.0182(11) 0.2137(7) 0.0544(17) 0.071 Uiso 1 calc R . H8B H -0.0288(8) 0.346(3) 0.0198(8) 0.071 Uiso 1 calc R . H8C H 0.0120(3) 0.331(4) 0.0822(10) 0.071 Uiso 1 calc R . C9 C 0.0489(2) 0.3522(5) 0.0103(3) 0.0224(14) Uani 1 d . . C10 C 0.0682(2) 0.3549(5) -0.0289(3) 0.0269(15) Uani 1 d . . H10 H 0.0592(2) 0.3091(5) -0.0654(3) 0.032 Uiso 1 calc R . C11 C 0.1032(2) 0.4380(5) -0.0040(3) 0.034(2) Uani 1 d . . H11 H 0.1213(2) 0.4558(5) -0.0207(3) 0.041 Uiso 1 calc R . C12 C 0.1054(2) 0.4890(5) 0.0510(3) 0.032(2) Uani 1 d . . H12 H 0.1252(2) 0.5481(5) 0.0766(3) 0.038 Uiso 1 calc R . C13 C 0.0725(2) 0.4348(5) 0.0605(3) 0.030(2) Uani 1 d . . H13 H 0.0673(2) 0.4507(5) 0.0939(3) 0.037 Uiso 1 calc R . C14 C 0.1927(2) 0.2676(5) 0.1297(3) 0.0268(14) Uani 1 d . . H14A H 0.2094(2) 0.1970(5) 0.1266(3) 0.032 Uiso 1 calc R . H14B H 0.2042(2) 0.3514(5) 0.1282(3) 0.032 Uiso 1 calc R . C15 C 0.17839(15) 0.2533(5) 0.1742(2) 0.0198(12) Uani 1 d . . H15 H 0.18846(15) 0.1835(5) 0.2008(2) 0.024 Uiso 1 calc R . C16 C 0.1505(2) 0.3349(5) 0.1815(2) 0.0200(13) Uani 1 d . . H16 H 0.1404(2) 0.4049(5) 0.1551(2) 0.024 Uiso 1 calc R . C17 C 0.1351(2) 0.3186(5) 0.2295(3) 0.0234(14) Uani 1 d . . H17A H 0.1360(2) 0.2279(5) 0.2397(3) 0.028 Uiso 1 calc R . H17B H 0.1061(2) 0.3462(5) 0.2122(3) 0.028 Uiso 1 calc R . C18 C 0.1557(2) 0.5594(5) 0.2860(2) 0.0195(13) Uani 1 d . . C19 C 0.1222(2) 0.6240(6) 0.2409(3) 0.033(2) Uani 1 d . . C20 C 0.1158(2) 0.7555(6) 0.2378(3) 0.035(2) Uani 1 d . . C21 C 0.1444(2) 0.8328(6) 0.2816(3) 0.032(2) Uani 1 d . . C22 C 0.1798(2) 0.7773(5) 0.3278(3) 0.0269(15) Uani 1 d . . C23 C 0.1841(2) 0.6461(5) 0.3295(3) 0.0226(14) Uani 1 d . . C24 C 0.1492(2) 0.3617(5) 0.3494(3) 0.032(2) Uani 1 d . . C25 C 0.1084(2) 0.3437(8) 0.3374(3) 0.055(2) Uani 1 d . . C26 C 0.0950(2) 0.3045(8) 0.3795(4) 0.063(2) Uani 1 d . . C27 C 0.1230(3) 0.2838(6) 0.4385(3) 0.042(2) Uani 1 d . . C28 C 0.1643(2) 0.3095(5) 0.4555(3) 0.037(2) Uani 1 d . . C29 C 0.1759(2) 0.3490(5) 0.4105(3) 0.033(2) Uani 1 d . . C30 C 0.2121(2) 0.3566(5) 0.3119(2) 0.0207(13) Uani 1 d . . C31 C 0.2385(2) 0.4207(5) 0.2930(3) 0.0231(14) Uani 1 d . . C32 C 0.2766(2) 0.3750(5) 0.3000(3) 0.0237(14) Uani 1 d . . C33 C 0.2912(2) 0.2583(6) 0.3278(3) 0.0304(15) Uani 1 d . . C34 C 0.2664(2) 0.1881(6) 0.3467(3) 0.032(2) Uani 1 d . . C35 C 0.2279(2) 0.2388(5) 0.3375(2) 0.0255(13) Uani 1 d . . C36 C 0.1212(2) 0.1336(9) -0.0822(3) 0.087(3) Uani 1 d . . H36A H 0.1009(12) 0.069(4) -0.0854(4) 0.13 Uiso 1 calc R . H36B H 0.1379(3) 0.102(5) -0.1010(7) 0.13 Uiso 1 calc R . H36C H 0.1069(15) 0.2108(15) -0.1027(7) 0.13 Uiso 1 calc R . C37 C 0.1865(2) 0.0225(6) 0.0234(4) 0.057(2) Uani 1 d . . H37A H 0.1684(3) -0.0502(8) 0.017(2) 0.086 Uiso 1 calc R . H37B H 0.2059(11) 0.028(2) 0.0663(6) 0.086 Uiso 1 calc R . H37C H 0.2017(12) 0.012(2) -0.0002(15) 0.086 Uiso 1 calc R . C38 C 0.1927(2) 0.2805(6) -0.0063(3) 0.051(2) Uani 1 d . . H38A H 0.2144(8) 0.299(3) 0.0342(4) 0.076 Uiso 1 calc R . H38B H 0.1785(3) 0.3587(17) -0.0256(18) 0.076 Uiso 1 calc R . H38C H 0.2048(10) 0.2422(18) -0.0303(17) 0.076 Uiso 1 calc R . O41 O 0.0299(7) 0.038(3) -0.1776(14) 0.357(16) Uani 0.5 d PDU . C42 C 0.0503(11) -0.036(5) -0.199(3) 0.357(17) Uani 0.5 d PDU . C43 C -0.0220(9) -0.068(2) -0.2459(12) 0.247(9) Uani 1 d U . C44 C -0.0032(10) -0.030(2) -0.1835(17) 0.191(11) Uani 0.5 d PDU . O51 O 0.0304(6) 0.291(2) -0.1821(8) 0.146(8) Uani 0.5 d PD . C52 C 0.0308(10) 0.373(3) -0.2217(14) 0.36(2) Uani 1 d D . C53 C -0.0052(7) 0.357(2) -0.2102(10) 0.215(9) Uani 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0165(3) 0.0198(3) 0.0173(3) 0.0004(3) 0.0050(2) -0.0033(3) P1 0.0286(11) 0.0616(12) 0.0299(11) -0.0138(9) 0.0152(9) -0.0087(9) F1 0.050(3) 0.036(2) 0.043(3) -0.013(2) -0.015(2) 0.010(2) F2 0.070(3) 0.042(2) 0.040(3) -0.003(2) -0.012(2) 0.023(2) F3 0.064(3) 0.025(2) 0.043(3) 0.006(2) 0.019(2) 0.008(2) F4 0.038(2) 0.027(2) 0.046(3) -0.005(2) 0.010(2) -0.008(2) F5 0.025(2) 0.027(2) 0.033(2) -0.0017(15) -0.004(2) 0.0010(15) F6 0.041(3) 0.187(5) 0.051(3) 0.026(3) 0.023(3) 0.007(3) F7 0.061(4) 0.206(6) 0.079(4) 0.026(4) 0.045(3) -0.012(4) F8 0.092(3) 0.056(2) 0.060(3) 0.021(2) 0.062(3) 0.018(2) F9 0.095(4) 0.088(3) 0.028(3) 0.002(2) 0.029(3) -0.025(2) F10 0.061(3) 0.075(3) 0.029(2) -0.008(2) 0.016(2) -0.034(2) F11 0.035(2) 0.029(2) 0.046(2) 0.010(2) 0.027(2) 0.007(2) F12 0.030(2) 0.034(2) 0.066(3) -0.011(2) 0.031(2) -0.004(2) F13 0.028(2) 0.049(2) 0.056(3) -0.008(2) 0.016(2) 0.014(2) F14 0.064(3) 0.026(2) 0.056(3) 0.014(2) 0.024(2) 0.023(2) F15 0.046(2) 0.021(2) 0.052(3) 0.005(2) 0.026(2) 0.001(2) B1 0.027(4) 0.032(4) 0.015(4) 0.000(3) 0.010(3) -0.003(3) C1 0.021(4) 0.027(4) 0.027(4) 0.002(3) 0.015(3) -0.004(3) C2 0.025(4) 0.014(3) 0.037(4) 0.013(3) 0.007(3) -0.008(3) C3 0.031(4) 0.015(3) 0.051(5) -0.002(3) 0.020(4) -0.002(3) C4 0.027(4) 0.023(3) 0.029(4) -0.005(3) 0.010(3) -0.012(3) C5 0.015(3) 0.025(4) 0.020(4) 0.002(3) 0.003(3) -0.005(2) C6 0.019(3) 0.024(3) 0.024(3) 0.000(3) 0.003(3) -0.003(3) C7 0.028(4) 0.053(5) 0.038(4) 0.010(3) -0.006(3) -0.018(3) C8 0.034(4) 0.052(5) 0.058(5) 0.021(3) 0.023(4) 0.012(3) C9 0.017(3) 0.020(3) 0.019(4) 0.005(2) -0.001(3) 0.002(2) C10 0.027(4) 0.027(4) 0.019(3) 0.008(3) 0.004(3) 0.000(3) C11 0.034(4) 0.033(4) 0.028(4) 0.016(3) 0.008(3) -0.005(3) C12 0.028(4) 0.016(3) 0.033(4) 0.010(3) -0.001(3) -0.005(3) C13 0.032(4) 0.022(3) 0.026(4) 0.008(3) 0.003(3) 0.010(3) C14 0.015(3) 0.028(4) 0.032(4) -0.008(3) 0.005(3) -0.004(3) C15 0.012(3) 0.022(3) 0.017(3) -0.001(3) -0.001(2) -0.002(3) C16 0.021(3) 0.023(3) 0.011(3) 0.003(2) 0.003(3) -0.003(3) C17 0.021(3) 0.020(3) 0.027(4) 0.001(3) 0.009(3) 0.001(2) C18 0.021(3) 0.031(4) 0.009(3) 0.004(2) 0.009(3) 0.005(3) C19 0.029(4) 0.038(4) 0.019(4) -0.011(3) -0.001(3) 0.001(3) C20 0.036(4) 0.033(4) 0.018(3) 0.004(3) -0.004(3) 0.011(3) C21 0.044(4) 0.023(4) 0.028(4) 0.000(3) 0.017(4) 0.001(3) C22 0.025(4) 0.034(4) 0.020(4) -0.002(3) 0.009(3) -0.004(3) C23 0.025(4) 0.024(4) 0.019(4) 0.004(3) 0.010(3) -0.001(3) C24 0.044(4) 0.024(4) 0.033(4) 0.011(3) 0.022(4) 0.009(3) C25 0.025(5) 0.113(7) 0.027(5) 0.020(4) 0.013(4) 0.004(4) C26 0.029(5) 0.110(7) 0.059(6) 0.021(5) 0.029(5) 0.002(4) C27 0.067(6) 0.036(4) 0.048(5) 0.013(3) 0.047(5) 0.014(3) C28 0.066(6) 0.021(4) 0.029(4) 0.002(3) 0.025(4) -0.001(3) C29 0.048(5) 0.028(4) 0.028(4) -0.004(3) 0.023(4) -0.006(3) C30 0.019(3) 0.017(3) 0.019(3) -0.004(2) 0.002(3) -0.004(2) C31 0.025(4) 0.020(3) 0.019(3) 0.002(2) 0.006(3) 0.002(3) C32 0.019(4) 0.024(4) 0.027(4) -0.009(3) 0.009(3) -0.005(3) C33 0.022(3) 0.030(4) 0.029(4) -0.012(3) 0.002(3) 0.007(3) C34 0.036(4) 0.025(4) 0.031(4) -0.003(3) 0.010(3) 0.010(3) C35 0.029(3) 0.023(4) 0.022(3) -0.003(3) 0.009(3) -0.005(3) C36 0.044(6) 0.168(9) 0.039(6) -0.038(6) 0.011(5) 0.001(6) C37 0.041(5) 0.053(5) 0.083(6) -0.028(4) 0.032(5) -0.012(4) C38 0.050(5) 0.064(5) 0.051(5) 0.001(4) 0.034(4) -0.005(4) O41 0.138(17) 0.60(4) 0.41(3) -0.43(3) 0.192(18) -0.23(2) C42 0.16(3) 0.49(5) 0.38(5) -0.37(4) 0.09(4) -0.03(4) C43 0.40(3) 0.240(19) 0.25(2) -0.03(2) 0.27(2) -0.04(2) C44 0.28(2) 0.15(3) 0.23(2) 0.12(2) 0.19(3) 0.13(2) O51 0.070(11) 0.27(2) 0.090(13) -0.003(13) 0.027(11) 0.055(14) C52 0.27(4) 0.65(5) 0.16(3) 0.06(3) 0.11(3) -0.17(3) C53 0.16(2) 0.30(3) 0.138(19) 0.055(16) 0.029(18) -0.008(19) _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 C14 2.45(18) . ? Zr1 C5 2.45(16) . ? Zr1 C9 2.45(18) . ? Zr1 C4 2.5(3) . ? Zr1 C13 2.5(3) . ? Zr1 C1 2.49(15) . ? Zr1 C10 2.5(2) . ? Zr1 C15 2.5(2) . ? Zr1 C3 2.6(5) . ? Zr1 C12 2.6(5) . ? Zr1 C11 2.6(3) . ? Zr1 C2 2.6(3) . ? P1 C37 1.8(3) . ? P1 C38 1.82(15) . ? P1 C36 1.84(17) . ? F1 C19 1.37(11) . ? F2 C20 1.35(11) . ? F3 C21 1.4(3) . ? F4 C22 1.36(12) . ? F5 C23 1.34(11) . ? F6 C25 1.36(12) . ? F7 C26 1.35(9) . ? F8 C27 1.36(9) . ? F9 C28 1.35(12) . ? F10 C29 1.38(9) . ? F11 C31 1.4(2) . ? F12 C32 1.37(9) . ? F13 C33 1.35(8) . ? F14 C34 1.4(2) . ? F15 C35 1.38(11) . ? B1 C17 1.65(14) . ? B1 C18 1.7(3) . ? B1 C30 1.67(10) . ? B1 C24 1.70(11) . ? C1 C2 1.41(12) . ? C1 C5 1.42(13) . ? C2 C3 1.39(11) . ? C3 C4 1.43(11) . ? C4 C5 1.43(10) . ? C5 C6 1.53(17) . ? C6 C9 1.54(15) . ? C6 C8 1.55(8) . ? C6 C7 1.55(14) . ? C9 C10 1.41(9) . ? C9 C13 1.42(13) . ? C10 C11 1.41(12) . ? C11 C12 1.41(11) . ? C12 C13 1.41(8) . ? C14 C15 1.40(9) . ? C15 C16 1.38(11) . ? C16 C17 1.51(10) . ? C18 C19 1.38(11) . ? C18 C23 1.41(13) . ? C19 C20 1.4(3) . ? C20 C21 1.36(12) . ? C21 C22 1.38(11) . ? C22 C23 1.4(3) . ? C24 C29 1.36(13) . ? C24 C25 1.36(8) . ? C25 C26 1.38(9) . ? C26 C27 1.35(12) . ? C27 C28 1.37(9) . ? C28 C29 1.40(9) . ? C30 C35 1.4(2) . ? C30 C31 1.39(8) . ? C31 C32 1.38(8) . ? C32 C33 1.4(2) . ? C33 C34 1.38(9) . ? C34 C35 1.39(8) . ? O41 c44 1.33(10) . ? O41 c42 1.33(10) . ? c42 c43 1.30(12) 2_554 ? c43 c42 1.30(12) 2_554 ? c43 c44 1.41(13) . ? c43 c43 1.68(10) 2_554 ? o51 c52 1.29(13) . ? o51 c53 1.33(10) . ? c52 c53 1.44(8) . ? c52 c53 1.50(14) 2_554 ? c52 c52 2.00(17) 2_554 ? c53 c52 1.50(14) 2_554 ? 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 C14 Zr1 C5 153(3) . . ? C14 Zr1 C9 148(6) . . ? C5 Zr1 C9 57(9) . . ? C14 Zr1 C4 134(5) . . ? C5 Zr1 C4 33.6(18) . . ? C9 Zr1 C4 78(10) . . ? C14 Zr1 C13 118(6) . . ? C5 Zr1 C13 79(10) . . ? C9 Zr1 C13 33.5(18) . . ? C4 Zr1 C13 108(10) . . ? C14 Zr1 C1 122(5) . . ? C5 Zr1 C1 34(4) . . ? C9 Zr1 C1 79(7) . . ? C4 Zr1 C1 55(5) . . ? C13 Zr1 C1 86(10) . . ? C14 Zr1 C10 130(5) . . ? C5 Zr1 C10 77(7) . . ? C9 Zr1 C10 33(3) . . ? C4 Zr1 C10 81(10) . . ? C13 Zr1 C10 54(5) . . ? C1 Zr1 C10 107(6) . . ? C14 Zr1 C15 33(3) . . ? C5 Zr1 C15 126(4) . . ? C9 Zr1 C15 139(4) . . ? C4 Zr1 C15 129(5) . . ? C13 Zr1 C15 107(4) . . ? C1 Zr1 C15 92(6) . . ? C10 Zr1 C15 150(5) . . ? C14 Zr1 C3 103.6(7) . . ? C5 Zr1 C3 55(3) . . ? C9 Zr1 C3 109(6) . . ? C4 Zr1 C3 33(5) . . ? C13 Zr1 C3 134(7) . . ? C1 Zr1 C3 53(3) . . ? C10 Zr1 C3 113(6) . . ? C15 Zr1 C3 96.6(10) . . ? C14 Zr1 C12 93(3) . . ? C5 Zr1 C12 110(6) . . ? C9 Zr1 C12 54(3) . . ? C4 Zr1 C12 131(8) . . ? C13 Zr1 C12 33(5) . . ? C1 Zr1 C12 118(5) . . ? C10 Zr1 C12 53(3) . . ? C15 Zr1 C12 98(2) . . ? C3 Zr1 C12 163(3) . . ? C14 Zr1 C11 99(5) . . ? C5 Zr1 C11 108(7) . . ? C9 Zr1 C11 54(4) . . ? C4 Zr1 C11 112(10) . . ? C13 Zr1 C11 54(7) . . ? C1 Zr1 C11 133(4) . . ? C10 Zr1 C11 32.3(17) . . ? C15 Zr1 C11 119(6) . . ? C3 Zr1 C11 141(6) . . ? C12 Zr1 C11 32(4) . . ? C14 Zr1 C2 98(4) . . ? C5 Zr1 C2 55(5) . . ? C9 Zr1 C2 109(6) . . ? C4 Zr1 C2 54(8) . . ? C13 Zr1 C2 117(9) . . ? C1 Zr1 C2 32.3(16) . . ? C10 Zr1 C2 131(4) . . ? C15 Zr1 C2 77(4) . . ? C3 Zr1 C2 31(5) . . ? C12 Zr1 C2 147(5) . . ? C11 Zr1 C2 163(3) . . ? C37 P1 C38 101(10) . . ? C37 P1 C36 101(6) . . ? C38 P1 C36 101(5) . . ? C37 P1 Zr1 117(4) . . ? C38 P1 Zr1 117(8) . . ? C36 P1 Zr1 117(5) . . ? C17 B1 C18 115(7) . . ? C17 B1 C30 103(6) . . ? C18 B1 C30 113.0(17) . . ? C17 B1 C24 112(7) . . ? C18 B1 C24 104(3) . . ? C30 B1 C24 111(5) . . ? C2 C1 C5 109(4) . . ? C2 C1 Zr1 77(9) . . ? C5 C1 Zr1 72(5) . . ? C3 C2 C1 108(5) . . ? C3 C2 Zr1 74(9) . . ? C1 C2 Zr1 70(8) . . ? C2 C3 C4 109(7) . . ? C2 C3 Zr1 75(4) . . ? C4 C3 Zr1 70(6) . . ? C5 C4 C3 107(7) . . ? C5 C4 Zr1 72(8) . . ? C3 C4 Zr1 77(10) . . ? C1 C5 C4 107(5) . . ? C1 C5 C6 125(4) . . ? C4 C5 C6 125(6) . . ? C1 C5 Zr1 75(5) . . ? C4 C5 Zr1 74(8) . . ? C6 C5 Zr1 102(10) . . ? C5 C6 C9 99(10) . . ? C5 C6 C8 112(5) . . ? C9 C6 C8 113(8) . . ? C5 C6 C7 113(8) . . ? C9 C6 C7 111(5) . . ? C8 C6 C7 110(6) . . ? C10 C9 C13 107(5) . . ? C10 C9 C6 125(4) . . ? C13 C9 C6 126(6) . . ? C10 C9 Zr1 75(5) . . ? C13 C9 Zr1 74(9) . . ? C6 C9 Zr1 102(10) . . ? C9 C10 C11 109(5) . . ? C9 C10 Zr1 72(5) . . ? C11 C10 Zr1 77(9) . . ? C12 C11 C10 107(5) . . ? C12 C11 Zr1 74(10) . . ? C10 C11 Zr1 71(9) . . ? C11 C12 C13 108(6) . . ? C11 C12 Zr1 74(6) . . ? C13 C12 Zr1 70(5) . . ? C12 C13 C9 108(6) . . ? C12 C13 Zr1 77(10) . . ? C9 C13 Zr1 73(9) . . ? C15 C14 Zr1 76(6) . . ? C16 C15 C14 125(5) . . ? C16 C15 Zr1 79(5) . . ? C14 C15 Zr1 71(6) . . ? C15 C16 C17 125(5) . . ? C15 C16 Zr1 70(6) . . ? C17 C16 Zr1 128(5) . . ? C16 C17 B1 113(6) . . ? C19 C18 C23 111(10) . . ? C19 C18 B1 127(4) . . ? C23 C18 B1 122(8) . . ? F1 C19 C18 120(10) . . ? F1 C19 C20 114(7) . . ? C18 C19 C20 126(4) . . ? F2 C20 C21 120(10) . . ? F2 C20 C19 121(3) . . ? C21 C20 C19 120(7) . . ? C20 C21 F3 121(7) . . ? C20 C21 C22 119(10) . . ? F3 C21 C22 121(4) . . ? F4 C22 C23 121(7) . . ? F4 C22 C21 120(10) . . ? C23 C22 C21 119(4) . . ? F5 C23 C22 115(3) . . ? F5 C23 C18 120(10) . . ? C22 C23 C18 125(7) . . ? C29 C24 C25 112(5) . . ? C29 C24 B1 126(5) . . ? C25 C24 B1 122(5) . . ? F6 C25 C24 120(5) . . ? F6 C25 C26 115(6) . . ? C24 C25 C26 125(5) . . ? C27 C26 F7 118(5) . . ? C27 C26 C25 120(5) . . ? F7 C26 C25 122(5) . . ? C26 C27 F8 122(5) . . ? C26 C27 C28 118(5) . . ? F8 C27 C28 119(5) . . ? F9 C28 C27 120(5) . . ? F9 C28 C29 121(5) . . ? C27 C28 C29 119(5) . . ? C24 C29 F10 121(5) . . ? C24 C29 C28 125(5) . . ? F10 C29 C28 114(5) . . ? C35 C30 C31 112(6) . . ? C35 C30 B1 122.3(19) . . ? C31 C30 B1 125(7) . . ? F11 C31 C32 115(4) . . ? F11 C31 C30 120(5) . . ? C32 C31 C30 125(8) . . ? F12 C32 C33 120(6) . . ? F12 C32 C31 120(8) . . ? C33 C32 C31 120(3) . . ? F13 C33 C32 121(3) . . ? F13 C33 C34 121(8) . . ? C32 C33 C34 118(6) . . ? F14 C34 C33 119(6) . . ? F14 C34 C35 122(3) . . ? C33 C34 C35 119(8) . . ? C30 C35 F15 120(7) . . ? C30 C35 C34 126(3) . . ? F15 C35 C34 114(9) . . ? c44 o41 c42 106(10) . . ? c43 c42 o41 104(6) 2_554 . ? c42 c43 c44 143(7) 2_554 . ? c42 c43 c43 102(6) 2_554 2_554 ? c44 c43 c43 97(6) . 2_554 ? o41 c44 c43 103(6) . . ? c52 o51 c53 67(6) . . ? o51 c52 c53 58(4) . . ? o51 c52 c53 124(7) . 2_554 ? c53 c52 c53 93(6) . 2_554 ? o51 c52 c52 98(5) . 2_554 ? c53 c52 c52 48(5) . 2_554 ? c53 c52 c52 46(4) 2_554 2_554 ? o51 c53 c52 55(5) . . ? o51 c53 c52 126(4) . 2_554 ? c52 c53 c52 86(7) . 2_554 ? #==END #=============Compound(9)============== data_9 _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic ? _cell_length_a 11.724(2) _cell_angle_alpha 90.000 _cell_length_b 17.331(6) _cell_angle_beta 91.884(2) _cell_length_c 22.963(9) _cell_angle_gamma 90.000 _cell_volume 4663.1(3) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Zr ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C48 H41 ZR N B F15 O2 ' _chemical_formula_moiety ' C48 H41 ZR N B F15 O2 ' _chemical_compound_source ? _chemical_formula_weight 1051.87 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 0 _cell_formula_units_Z 4 _exptl_crystal_description ' box ' _exptl_crystal_colour ' gold ' _exptl_crystal_size_min 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_max 0.5 _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 0.00 _exptl_absorpt_coefficient_mu 0.32 _exptl_absorpt_correction_type 'DIFABS' _exptl_absorpt_process_details 'refined from delta-F' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 11.39 _diffrn_ambient_temperature 0 _diffrn_reflns_number 9452 _reflns_number_total 7288 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 3880 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.28 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.61 _refine_diff_density_max 1.79 _refine_ls_number_reflns 3880 _refine_ls_number_parameters 727 _refine_ls_R_factor_obs 0.0612 _refine_ls_wR_factor_obs 0.0719 _refine_ls_goodness_of_fit_obs 1.6037 _refine_ls_shift/esd_max 2.154581 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-nonius CAD4 ' _diffrn_measurement_method 2\q/\w _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme 'Chebychev polynomial (Carruthers & Watkin, 1979)' _atom_sites_solution_primary 'Direct Methods' _atom_sites_solution_hydrogens 'Geometric' _refine_ls_hydrogen_treatment 'H atoms placed geometrically after each cycle' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type ZR1 0.27276(7) 0.61102(5) 0.66987(4) 0.0517 1.0000 Uani C1 0.200(1) 0.4901(8) 0.7623(5) 0.0915 1.0000 Uani C2 0.140(2) 0.414(1) 0.7475(8) 0.1253 1.0000 Uani C3 0.213(2) 0.496(1) 0.8281(6) 0.1225 1.0000 Uani C4 0.134(1) 0.5577(7) 0.7349(5) 0.0798 1.0000 Uani C5 0.079(1) 0.5588(9) 0.6810(6) 0.0880 1.0000 Uani C6 0.057(1) 0.635(1) 0.6643(7) 0.0943 1.0000 Uani C7 0.100(1) 0.6819(8) 0.7095(7) 0.0932 1.0000 Uani C8 0.148(1) 0.6352(8) 0.7525(5) 0.0878 1.0000 Uani C9 0.312(1) 0.4999(6) 0.7317(5) 0.0761 1.0000 Uani C10 0.395(1) 0.5560(7) 0.7468(5) 0.0752 1.0000 Uani C11 0.469(1) 0.5628(7) 0.7001(6) 0.0799 1.0000 Uani C12 0.434(1) 0.5137(7) 0.6565(5) 0.0823 1.0000 Uani C13 0.336(1) 0.4746(6) 0.6755(5) 0.0817 1.0000 Uani N20 0.3494(7) 0.7337(4) 0.6990(3) 0.0599 1.0000 Uani C21 0.429(1) 0.7440(6) 0.7422(5) 0.0742 1.0000 Uani C22 0.458(1) 0.8160(8) 0.7632(6) 0.0951 1.0000 Uani C23 0.405(2) 0.8790(7) 0.7395(6) 0.0954 1.0000 Uani C24 0.329(1) 0.8703(6) 0.6955(5) 0.0822 1.0000 Uani C25 0.3019(9) 0.7970(6) 0.6757(4) 0.0649 1.0000 Uani C30 0.229(1) 0.5708(6) 0.5742(4) 0.0690 1.0000 Uani C31 0.2627(9) 0.6507(6) 0.5634(4) 0.0608 1.0000 Uani C32 0.3727(8) 0.6757(5) 0.5713(4) 0.0540 1.0000 Uani C33 0.4155(8) 0.7533(5) 0.5566(4) 0.0594 1.0000 Uani B34 0.4908(9) 0.7478(6) 0.4970(4) 0.0545 1.0000 Uani C40 0.5352(7) 0.8358(5) 0.4778(4) 0.0515 1.0000 Uani F41 0.6121(6) 0.8580(4) 0.5728(2) 0.0729 1.0000 Uani C41 0.5934(8) 0.8830(5) 0.5172(4) 0.0575 1.0000 Uani F42 0.6931(6) 0.9960(4) 0.5464(3) 0.0802 1.0000 Uani C42 0.6374(8) 0.9537(6) 0.5049(4) 0.0637 1.0000 Uani F43 0.6674(6) 1.0527(3) 0.4370(3) 0.0831 1.0000 Uani C43 0.6260(8) 0.9829(5) 0.4500(4) 0.0630 1.0000 Uani F44 0.5587(6) 0.9669(4) 0.3540(3) 0.0842 1.0000 Uani C44 0.5710(8) 0.9391(6) 0.4084(4) 0.0613 1.0000 Uani F45 0.4805(5) 0.8291(3) 0.3767(2) 0.0706 1.0000 Uani C45 0.5293(8) 0.8684(5) 0.4223(4) 0.0567 1.0000 Uani C50 0.6110(8) 0.7001(5) 0.5045(4) 0.0577 1.0000 Uani F51 0.6143(5) 0.6885(4) 0.6083(3) 0.0861 1.0000 Uani C51 0.6640(9) 0.6766(6) 0.5566(5) 0.0720 1.0000 Uani F52 0.8117(7) 0.6194(5) 0.6136(4) 0.1092 1.0000 Uani C52 0.767(1) 0.6399(7) 0.5612(7) 0.0838 1.0000 Uani F53 0.9287(7) 0.5918(5) 0.5161(5) 0.1280 1.0000 Uani C53 0.826(1) 0.6258(7) 0.5137(8) 0.0864 1.0000 Uani F54 0.8382(6) 0.6366(5) 0.4112(4) 0.1081 1.0000 Uani C54 0.781(1) 0.6492(7) 0.4596(6) 0.0836 1.0000 Uani F55 0.6355(5) 0.7037(4) 0.4034(2) 0.0789 1.0000 Uani C55 0.6754(8) 0.6840(6) 0.4573(5) 0.0641 1.0000 Uani C60 0.3990(8) 0.7100(5) 0.4492(4) 0.0552 1.0000 Uani F61 0.2924(5) 0.8244(4) 0.4409(3) 0.0819 1.0000 Uani C61 0.3054(9) 0.7494(7) 0.4284(4) 0.0702 1.0000 Uani F62 0.1285(6) 0.7608(5) 0.3759(4) 0.1142 1.0000 Uani C62 0.218(1) 0.7164(8) 0.3945(5) 0.0811 1.0000 Uani F63 0.1361(7) 0.6094(6) 0.3486(4) 0.1214 1.0000 Uani C63 0.221(1) 0.6409(9) 0.3806(6) 0.0851 1.0000 Uani F64 0.3133(7) 0.5214(4) 0.3913(4) 0.1079 1.0000 Uani C64 0.310(1) 0.5977(7) 0.4019(5) 0.0811 1.0000 Uani F65 0.4772(5) 0.5833(3) 0.4565(3) 0.0820 1.0000 Uani C65 0.3952(9) 0.6314(6) 0.4352(4) 0.0656 1.0000 Uani C101 -0.203(2) 0.582(2) 0.762(1) 0.184(9) 1.0000 Uiso C102 -0.229(3) 0.663(2) 0.768(2) 0.22(1) 1.0000 Uiso C103 -0.169(3) 0.679(2) 0.821(2) 0.24(1) 1.0000 Uiso C104 -0.137(3) 0.621(3) 0.845(2) 0.25(2) 1.0000 Uiso O105 -0.155(2) 0.551(2) 0.816(1) 0.27(1) 1.0000 Uiso C201 -0.044(1) 0.833(4) 0.505(1) 0.34(2) 1.0000 Uiso C202 -0.018(3) 0.897(3) 0.521(2) 0.40(3) 1.0000 Uiso C203 0.041(2) 0.892(3) 0.573(2) 0.41(3) 1.0000 Uiso C205 -0.002(3) 0.780(2) 0.547(3) 0.42(3) 1.0000 Uiso O204 0.047(2) 0.817(3) 0.586(1) 0.34(1) 1.0000 Uiso H21 0.1315 0.4059 0.7046 0.1332 1.0000 Uiso H22 0.0647 0.4083 0.7658 0.1332 1.0000 Uiso H23 0.1903 0.3680 0.7634 0.1332 1.0000 Uiso H31 0.2491 0.5466 0.8406 0.1188 1.0000 Uiso H32 0.1355 0.4932 0.8474 0.1188 1.0000 Uiso H33 0.2611 0.4529 0.8450 0.1188 1.0000 Uiso H51 0.0569 0.5114 0.6562 0.0941 1.0000 Uiso H61 0.0199 0.6537 0.6249 0.0990 1.0000 Uiso H71 0.0951 0.7415 0.7116 0.0943 1.0000 Uiso H81 0.1902 0.6537 0.7902 0.0924 1.0000 Uiso H101 0.4014 0.5858 0.7853 0.0814 1.0000 Uiso H111 0.5402 0.6001 0.6999 0.0836 1.0000 Uiso H121 0.4727 0.5068 0.6165 0.0824 1.0000 Uiso H131 0.2913 0.4337 0.6527 0.0819 1.0000 Uiso H211 0.4697 0.6965 0.7594 0.0783 1.0000 Uiso H221 0.5170 0.8232 0.7956 0.1094 1.0000 Uiso H231 0.4223 0.9331 0.7547 0.1026 1.0000 Uiso H241 0.2856 0.9175 0.6772 0.0816 1.0000 Uiso H251 0.2444 0.7907 0.6416 0.0682 1.0000 Uiso H301 0.1436 0.5645 0.5658 0.0708 1.0000 Uiso H303 0.2699 0.5351 0.5477 0.0708 1.0000 Uiso H311 0.2032 0.6897 0.5500 0.0648 1.0000 Uiso H321 0.4320 0.6359 0.5874 0.0561 1.0000 Uiso H331 0.4641 0.7754 0.5899 0.0628 1.0000 Uiso H332 0.3479 0.7893 0.5502 0.0628 1.0000 Uiso H1011 -0.2782 0.5550 0.7474 0.1828 1.0000 Uiso H1012 -0.1511 0.5798 0.7271 0.1828 1.0000 Uiso H1021 -0.3209 0.6760 0.7721 0.2065 1.0000 Uiso H1022 -0.2111 0.7012 0.7344 0.2065 1.0000 Uiso H1031 -0.2194 0.7134 0.8480 0.0500 1.0000 Uiso H1032 -0.1019 0.7134 0.8117 0.0500 1.0000 Uiso H1041 -0.1743 0.6134 0.8899 0.0500 1.0000 Uiso H1042 -0.0486 0.6225 0.8620 0.0500 1.0000 Uiso H2011 -0.1328 0.8407 0.4983 0.0500 1.0000 Uiso H2012 -0.0155 0.8350 0.4621 0.0500 1.0000 Uiso H2021 -0.0832 0.9352 0.5302 0.0500 1.0000 Uiso H2022 0.0353 0.9287 0.4951 0.0500 1.0000 Uiso H2031 0.0036 0.9097 0.6061 0.0500 1.0000 Uiso H2032 0.1219 0.9024 0.5709 0.0500 1.0000 Uiso H2051 -0.0801 0.7545 0.5471 0.0500 1.0000 Uiso H2052 0.0395 0.7513 0.5127 0.0500 1.0000 Uiso 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 0.0631(5) 0.0518(5) 0.0440(4) 0.0010(4) -0.0087(3) -0.0070(5) C1 0.17(1) 0.084(9) 0.063(7) 0.018(6) 0.001(8) -0.037(9) C2 0.22(2) 0.11(1) 0.11(1) 0.033(9) 0.00(1) -0.07(1) C3 0.26(2) 0.16(1) 0.053(7) 0.029(9) 0.00(1) -0.05(2) C4 0.104(9) 0.097(9) 0.058(7) 0.002(6) 0.011(6) -0.035(7) C5 0.093(9) 0.11(1) 0.079(8) -0.001(7) 0.007(7) -0.041(8) C6 0.051(6) 0.16(1) 0.11(1) 0.02(1) 0.004(6) -0.017(7) C7 0.070(8) 0.11(1) 0.12(1) -0.015(9) 0.025(7) 0.001(7) C8 0.101(9) 0.11(1) 0.066(7) 0.001(7) 0.017(6) -0.025(7) C9 0.15(1) 0.054(6) 0.059(6) 0.006(5) -0.020(7) -0.007(7) C10 0.12(1) 0.072(8) 0.061(7) 0.006(5) -0.034(7) 0.017(7) C11 0.084(8) 0.066(7) 0.11(1) 0.003(7) -0.028(7) 0.020(6) C12 0.108(9) 0.065(7) 0.089(8) -0.005(6) -0.010(7) 0.024(7) C13 0.15(1) 0.050(6) 0.076(8) -0.003(5) -0.023(7) -0.005(7) N20 0.073(5) 0.054(5) 0.057(5) -0.004(4) -0.006(4) -0.008(4) C21 0.095(8) 0.075(7) 0.067(6) -0.003(5) -0.026(6) -0.012(6) C22 0.15(1) 0.087(9) 0.093(9) -0.011(7) -0.037(9) -0.045(9) C23 0.17(1) 0.062(8) 0.095(9) -0.009(7) -0.010(9) -0.036(8) C24 0.14(1) 0.052(7) 0.077(7) 0.001(5) 0.007(7) -0.005(6) C25 0.091(7) 0.055(5) 0.055(5) 0.001(5) 0.004(5) -0.003(5) C30 0.093(7) 0.079(7) 0.049(5) -0.002(5) -0.008(5) -0.021(6) C31 0.083(7) 0.070(6) 0.040(5) 0.007(4) -0.004(4) -0.007(5) C32 0.070(6) 0.061(5) 0.038(4) -0.002(4) -0.001(4) -0.009(5) C33 0.073(6) 0.063(6) 0.047(5) -0.003(4) 0.003(4) -0.010(5) B34 0.066(6) 0.060(6) 0.042(5) 0.003(4) -0.003(4) -0.011(5) C40 0.062(5) 0.051(5) 0.044(5) 0.001(4) -0.005(4) -0.007(4) F41 0.114(5) 0.080(4) 0.050(3) 0.003(3) -0.018(3) -0.029(3) C41 0.074(6) 0.060(6) 0.043(4) 0.003(5) -0.002(4) -0.001(5) F42 0.119(5) 0.075(4) 0.072(4) -0.009(3) -0.017(3) -0.035(4) C42 0.074(6) 0.057(6) 0.063(6) -0.006(5) -0.006(5) -0.007(5) F43 0.119(5) 0.065(4) 0.088(4) 0.017(3) -0.006(4) -0.030(4) C43 0.067(6) 0.053(6) 0.072(7) 0.007(5) 0.004(5) -0.005(5) F44 0.130(5) 0.093(4) 0.067(4) 0.033(3) -0.019(3) -0.035(4) C44 0.072(6) 0.061(6) 0.055(6) 0.010(5) -0.006(5) -0.011(5) F45 0.100(4) 0.084(4) 0.049(3) 0.006(3) -0.011(3) -0.032(3) C45 0.061(5) 0.065(6) 0.048(5) -0.002(4) -0.002(4) -0.010(4) C50 0.064(6) 0.056(5) 0.059(6) -0.000(4) -0.012(5) -0.013(4) F51 0.090(4) 0.137(6) 0.058(4) 0.022(4) -0.012(3) -0.019(4) C51 0.068(7) 0.073(7) 0.086(8) -0.002(6) -0.016(6) -0.019(6) F52 0.102(5) 0.138(7) 0.131(6) 0.035(5) -0.057(5) -0.010(5) C52 0.073(8) 0.085(8) 0.11(1) 0.012(7) -0.027(7) -0.009(6) F53 0.085(5) 0.142(7) 0.21(1) -0.028(7) -0.046(6) 0.031(5) C53 0.066(7) 0.083(8) 0.14(1) -0.021(8) -0.030(8) 0.012(6) F54 0.081(4) 0.140(7) 0.133(7) -0.052(5) 0.012(4) 0.005(4) C54 0.076(8) 0.084(8) 0.10(1) -0.028(7) -0.003(7) -0.007(6) F55 0.085(4) 0.100(4) 0.060(3) -0.011(3) 0.005(3) 0.001(3) C55 0.059(6) 0.066(6) 0.073(7) -0.009(5) -0.013(5) -0.007(5) C60 0.064(6) 0.056(5) 0.049(5) 0.004(4) 0.007(4) -0.008(4) F61 0.075(4) 0.070(4) 0.109(5) 0.011(3) -0.012(3) 0.001(3) C61 0.074(7) 0.075(7) 0.064(6) 0.004(5) -0.001(5) -0.012(6) F62 0.089(5) 0.152(7) 0.136(7) 0.031(6) -0.042(5) -0.008(5) C62 0.076(8) 0.10(1) 0.074(7) 0.018(7) -0.010(6) -0.010(7) F63 0.110(6) 0.190(9) 0.138(7) -0.032(7) -0.044(5) -0.058(6) C63 0.083(8) 0.11(1) 0.086(8) -0.015(7) -0.018(7) -0.032(7) F64 0.118(6) 0.093(5) 0.174(8) -0.059(5) -0.008(5) -0.036(4) C64 0.087(8) 0.091(9) 0.080(7) -0.024(6) 0.006(6) -0.027(7) F65 0.084(4) 0.061(3) 0.112(5) -0.017(3) -0.005(4) -0.003(3) C65 0.074(7) 0.071(7) 0.056(5) -0.012(5) 0.001(5) -0.007(5) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag ZR1 . C4 . 2.43(1) . ZR1 . C5 . 2.47(1) . ZR1 . C6 . 2.56(1) . ZR1 . C7 . 2.56(1) . ZR1 . C8 . 2.47(1) . ZR1 . C9 . 2.43(1) . ZR1 . C10 . 2.43(1) . ZR1 . C11 . 2.52(1) . ZR1 . C12 . 2.56(1) . ZR1 . C13 . 2.48(1) . ZR1 . N20 . 2.394(7) . ZR1 . C30 . 2.345(9) . ZR1 . C31 . 2.538(9) . C1 . C2 . 1.53(2) . C1 . C3 . 1.52(2) . C1 . C4 . 1.53(2) . C1 . C9 . 1.51(2) . C2 . H21 . 1.00(2) . C2 . H22 . 1.00(2) . C2 . H23 . 1.05(2) . C3 . H31 . 1.01(2) . C3 . H32 . 1.02(2) . C3 . H33 . 1.00(2) . C4 . C5 . 1.37(2) . C4 . C8 . 1.41(2) . C5 . C6 . 1.39(2) . C5 . H51 . 1.03(1) . C6 . C7 . 1.40(2) . C6 . H61 . 1.04(1) . C7 . C8 . 1.38(2) . C7 . H71 . 1.04(1) . C8 . H81 . 1.04(1) . C9 . C10 . 1.41(2) . C9 . C13 . 1.40(2) . C10 . C11 . 1.40(2) . C10 . H101 . 1.02(1) . C11 . C12 . 1.37(2) . C11 . H111 . 1.06(1) . C12 . C13 . 1.41(2) . C12 . H121 . 1.05(1) . C13 . H131 . 1.02(1) . N20 . C21 . 1.35(1) . N20 . C25 . 1.33(1) . C21 . C22 . 1.37(2) . C21 . H211 . 1.02(1) . C22 . C23 . 1.36(2) . C22 . H221 . 1.01(1) . C23 . C24 . 1.33(2) . C23 . H231 . 1.02(1) . C24 . C25 . 1.38(1) . C24 . H241 . 1.04(1) . C25 . H251 . 1.02(1) . C30 . C31 . 1.46(1) . C30 . H301 . 1.02(1) . C30 . H303 . 1.00(1) . C31 . C32 . 1.37(1) . C31 . H311 . 1.01(1) . C32 . C33 . 1.48(1) . C32 . H321 . 1.038(9) . C33 . B34 . 1.66(1) . C33 . H331 . 1.013(9) . C33 . H332 . 1.02(1) . B34 . C40 . 1.68(1) . B34 . C50 . 1.64(1) . B34 . C60 . 1.65(1) . C40 . C41 . 1.38(1) . C40 . C45 . 1.39(1) . F41 . C41 . 1.36(1) . C41 . C42 . 1.36(1) . F42 . C42 . 1.35(1) . C42 . C43 . 1.36(1) . F43 . C43 . 1.34(1) . C43 . C44 . 1.36(1) . F44 . C44 . 1.34(1) . C44 . C45 . 1.36(1) . F45 . C45 . 1.36(1) . C50 . C51 . 1.39(1) . C50 . C55 . 1.37(1) . F51 . C51 . 1.36(1) . C51 . C52 . 1.37(2) . F52 . C52 . 1.34(1) . C52 . C53 . 1.33(2) . F53 . C53 . 1.34(1) . C53 . C54 . 1.39(2) . F54 . C54 . 1.33(2) . C54 . C55 . 1.38(2) . F55 . C55 . 1.35(1) . C60 . C61 . 1.37(1) . C60 . C65 . 1.40(1) . F61 . C61 . 1.34(1) . C61 . C62 . 1.39(2) . F62 . C62 . 1.36(1) . C62 . C63 . 1.35(2) . F63 . C63 . 1.33(1) . C63 . C64 . 1.36(2) . F64 . C64 . 1.34(1) . C64 . C65 . 1.37(1) . F65 . C65 . 1.35(1) . C101 . C102 . 1.45(3) . C101 . O105 . 1.45(3) . C101 . H1011 . 1.04(3) . C101 . H1012 . 1.02(3) . C102 . C103 . 1.41(4) . C102 . H1021 . 1.11(3) . C102 . H1022 . 1.04(3) . C103 . C104 . 1.20(4) . C103 . H1031 . 1.07(4) . C103 . H1032 . 1.01(4) . C104 . O105 . 1.39(4) . C104 . H1041 . 1.14(4) . C104 . H1042 . 1.09(4) . C201 . C202 . 1.21(3) . C201 . C205 . 1.41(3) . C201 . H2011 . 1.05(2) . C201 . H2012 . 1.06(2) . C202 . C203 . 1.35(3) . C202 . H2021 . 1.03(2) . C202 . H2022 . 1.04(2) . C203 . O204 . 1.33(3) . C203 . H2031 . 0.95(2) . C203 . H2032 . 0.97(2) . C205 . O204 . 1.22(3) . C205 . H2051 . 1.02(3) . C205 . H2052 . 1.07(3) . loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 . ZR1 . C5 . 32.6(4) . C4 . ZR1 . C6 . 53.9(5) . C5 . ZR1 . C6 . 32.1(5) . C4 . ZR1 . C7 . 53.8(5) . C5 . ZR1 . C7 . 52.9(5) . C6 . ZR1 . C7 . 31.8(4) . C4 . ZR1 . C8 . 33.5(4) . C5 . ZR1 . C8 . 53.9(4) . C6 . ZR1 . C8 . 53.2(5) . C7 . ZR1 . C8 . 31.8(4) . C4 . ZR1 . C9 . 57.1(5) . C5 . ZR1 . C9 . 78.8(5) . C6 . ZR1 . C9 . 108.9(5) . C7 . ZR1 . C9 . 108.0(5) . C8 . ZR1 . C9 . 77.9(5) . C4 . ZR1 . C10 . 78.3(5) . C5 . ZR1 . C10 . 107.7(5) . C6 . ZR1 . C10 . 131.1(5) . C7 . ZR1 . C10 . 112.6(5) . C8 . ZR1 . C10 . 82.0(5) . C4 . ZR1 . C11 . 109.2(5) . C5 . ZR1 . C11 . 133.2(5) . C6 . ZR1 . C11 . 163.1(5) . C7 . ZR1 . C11 . 141.7(5) . C8 . ZR1 . C11 . 113.8(5) . C4 . ZR1 . C12 . 109.6(5) . C5 . ZR1 . C12 . 117.1(5) . C6 . ZR1 . C12 . 146.2(5) . C7 . ZR1 . C12 . 162.6(5) . C8 . ZR1 . C12 . 131.5(5) . C4 . ZR1 . C13 . 79.2(5) . C5 . ZR1 . C13 . 85.5(5) . C6 . ZR1 . C13 . 116.8(5) . C7 . ZR1 . C13 . 132.7(5) . C8 . ZR1 . C13 . 107.9(5) . C4 . ZR1 . N20 . 114.8(3) . C5 . ZR1 . N20 . 129.4(4) . C6 . ZR1 . N20 . 103.4(4) . C7 . ZR1 . N20 . 76.6(4) . C8 . ZR1 . N20 . 82.0(4) . C4 . ZR1 . C30 . 109.3(4) . C5 . ZR1 . C30 . 79.3(4) . C6 . ZR1 . C30 . 79.3(5) . C7 . ZR1 . C30 . 108.9(5) . C8 . ZR1 . C30 . 130.7(4) . C4 . ZR1 . C31 . 133.1(4) . C5 . ZR1 . C31 . 100.7(4) . C6 . ZR1 . C31 . 83.9(4) . C7 . ZR1 . C31 . 101.6(4) . C8 . ZR1 . C31 . 133.1(4) . C9 . ZR1 . C10 . 33.8(4) . C9 . ZR1 . C11 . 54.8(5) . C10 . ZR1 . C11 . 32.8(4) . C9 . ZR1 . C12 . 54.7(5) . C10 . ZR1 . C12 . 53.8(4) . C11 . ZR1 . C12 . 31.3(4) . C9 . ZR1 . C13 . 33.2(4) . C10 . ZR1 . C13 . 54.5(4) . C11 . ZR1 . C13 . 53.1(4) . C12 . ZR1 . C13 . 32.4(4) . C9 . ZR1 . N20 . 118.6(3) . C10 . ZR1 . N20 . 86.5(3) . C11 . ZR1 . N20 . 83.5(3) . C12 . ZR1 . N20 . 110.4(4) . C13 . ZR1 . N20 . 136.2(4) . C9 . ZR1 . C30 . 110.1(4) . C10 . ZR1 . C30 . 132.0(4) . C11 . ZR1 . C30 . 109.2(4) . C12 . ZR1 . C30 . 80.3(4) . C13 . ZR1 . C30 . 79.7(4) . C9 . ZR1 . C31 . 141.3(4) . C10 . ZR1 . C31 . 144.3(4) . C11 . ZR1 . C31 . 111.6(4) . C12 . ZR1 . C31 . 94.2(4) . C13 . ZR1 . C31 . 108.2(4) . N20 . ZR1 . C30 . 126.4(3) . N20 . ZR1 . C31 . 91.9(3) . C30 . ZR1 . C31 . 34.6(3) . C2 . C1 . C3 . 107.9(12) . C2 . C1 . C4 . 110.0(13) . C3 . C1 . C4 . 113.1(14) . C2 . C1 . C9 . 113.0(14) . C3 . C1 . C9 . 113.5(13) . C4 . C1 . C9 . 99.2(9) . C1 . C2 . H21 . 112.0(12) . C1 . C2 . H22 . 113.5(18) . H21 . C2 . H22 . 109.7(19) . C1 . C2 . H23 . 109.4(16) . H21 . C2 . H23 . 106.0(19) . H22 . C2 . H23 . 105.7(12) . C1 . C3 . H31 . 111.3(13) . C1 . C3 . H32 . 111.7(16) . H31 . C3 . H32 . 106.5(19) . C1 . C3 . H33 . 111.8(18) . H31 . C3 . H33 . 108.0(18) . H32 . C3 . H33 . 107.3(14) . ZR1 . C4 . C1 . 101.5(8) . ZR1 . C4 . C5 . 75.2(7) . C1 . C4 . C5 . 126.8(12) . ZR1 . C4 . C8 . 74.9(6) . C1 . C4 . C8 . 123.7(11) . C5 . C4 . C8 . 106.9(12) . ZR1 . C5 . C4 . 72.3(7) . ZR1 . C5 . C6 . 77.5(7) . C4 . C5 . C6 . 109.7(12) . ZR1 . C5 . H51 . 116.9(9) . C4 . C5 . H51 . 126.0(15) . C6 . C5 . H51 . 124.3(13) . ZR1 . C6 . C5 . 70.4(7) . ZR1 . C6 . C7 . 74.2(7) . C5 . C6 . C7 . 106.8(13) . ZR1 . C6 . H61 . 118.8(9) . C5 . C6 . H61 . 127.1(16) . C7 . C6 . H61 . 126.0(17) . ZR1 . C7 . C6 . 74.0(7) . ZR1 . C7 . C8 . 70.6(7) . C6 . C7 . C8 . 108.4(13) . ZR1 . C7 . H71 . 122.7(9) . C6 . C7 . H71 . 126.6(16) . C8 . C7 . H71 . 125.0(15) . ZR1 . C8 . C4 . 71.6(7) . ZR1 . C8 . C7 . 77.7(7) . C4 . C8 . C7 . 108.2(11) . ZR1 . C8 . H81 . 114.3(9) . C4 . C8 . H81 . 125.7(13) . C7 . C8 . H81 . 126.1(14) . ZR1 . C9 . C1 . 102.2(8) . ZR1 . C9 . C10 . 73.4(6) . C1 . C9 . C10 . 124.4(12) . ZR1 . C9 . C13 . 75.5(6) . C1 . C9 . C13 . 126.8(12) . C10 . C9 . C13 . 106.1(12) . ZR1 . C10 . C9 . 72.8(6) . ZR1 . C10 . C11 . 77.0(6) . C9 . C10 . C11 . 108.0(11) . ZR1 . C10 . H101 . 116.9(8) . C9 . C10 . H101 . 125.9(14) . C11 . C10 . H101 . 126.0(13) . ZR1 . C11 . C10 . 70.1(6) . ZR1 . C11 . C12 . 75.8(7) . C10 . C11 . C12 . 109.2(12) . ZR1 . C11 . H111 . 120.7(7) . C10 . C11 . H111 . 124.2(13) . C12 . C11 . H111 . 126.6(15) . ZR1 . C12 . C11 . 73.0(6) . ZR1 . C12 . C13 . 70.9(7) . C11 . C12 . C13 . 107.5(12) . ZR1 . C12 . H121 . 121.8(8) . C11 . C12 . H121 . 125.7(14) . C13 . C12 . H121 . 126.9(12) . ZR1 . C13 . C9 . 71.2(6) . ZR1 . C13 . C12 . 76.7(6) . C9 . C13 . C12 . 109.2(11) . ZR1 . C13 . H131 . 119.0(9) . C9 . C13 . H131 . 124.8(15) . C12 . C13 . H131 . 126.0(13) . ZR1 . N20 . C21 . 124.5(7) . ZR1 . N20 . C25 . 118.1(6) . C21 . N20 . C25 . 117.0(8) . N20 . C21 . C22 . 122.3(11) . N20 . C21 . H211 . 118.5(9) . C22 . C21 . H211 . 119.2(10) . C21 . C22 . C23 . 118.9(11) . C21 . C22 . H221 . 121.8(14) . C23 . C22 . H221 . 119.3(13) . C22 . C23 . C24 . 119.9(11) . C22 . C23 . H231 . 121.1(14) . C24 . C23 . H231 . 119.1(15) . C23 . C24 . C25 . 119.4(11) . C23 . C24 . H241 . 121.3(11) . C25 . C24 . H241 . 119.2(12) . N20 . C25 . C24 . 122.5(9) . N20 . C25 . H251 . 118.4(9) . C24 . C25 . H251 . 119.1(10) . ZR1 . C30 . C31 . 79.9(5) . ZR1 . C30 . H301 . 113.2(7) . C31 . C30 . H301 . 109.9(10) . ZR1 . C30 . H303 . 131.1(8) . C31 . C30 . H303 . 110.1(9) . H301 . C30 . H303 . 107.8(9) . ZR1 . C31 . C30 . 65.5(5) . ZR1 . C31 . C32 . 86.9(5) . C30 . C31 . C32 . 122.5(9) . ZR1 . C31 . H311 . 118.9(7) . C30 . C31 . H311 . 119.7(10) . C32 . C31 . H311 . 117.8(9) . C31 . C32 . C33 . 125.7(9) . C31 . C32 . H321 . 117.0(9) . C33 . C32 . H321 . 117.2(8) . C32 . C33 . B34 . 109.3(7) . C32 . C33 . H331 . 111.0(8) . B34 . C33 . H331 . 110.1(8) . C32 . C33 . H332 . 108.9(8) . B34 . C33 . H332 . 110.4(8) . H331 . C33 . H332 . 107.2(8) . C33 . B34 . C40 . 110.1(8) . C33 . B34 . C50 . 115.0(7) . C40 . B34 . C50 . 102.3(7) . C33 . B34 . C60 . 102.7(7) . C40 . B34 . C60 . 112.8(7) . C50 . B34 . C60 . 114.2(8) . B34 . C40 . C41 . 121.2(7) . B34 . C40 . C45 . 127.1(7) . C41 . C40 . C45 . 111.5(8) . C40 . C41 . F41 . 119.1(8) . C40 . C41 . C42 . 125.3(8) . F41 . C41 . C42 . 115.6(8) . C41 . C42 . F42 . 121.1(9) . C41 . C42 . C43 . 120.1(8) . F42 . C42 . C43 . 118.8(9) . C42 . C43 . F43 . 121.1(9) . C42 . C43 . C44 . 118.1(9) . F43 . C43 . C44 . 120.8(9) . C43 . C44 . F44 . 119.0(8) . C43 . C44 . C45 . 120.1(9) . F44 . C44 . C45 . 120.9(8) . C40 . C45 . C44 . 124.9(8) . C40 . C45 . F45 . 120.6(7) . C44 . C45 . F45 . 114.5(8) . B34 . C50 . C51 . 126.7(9) . B34 . C50 . C55 . 120.9(8) . C51 . C50 . C55 . 112.2(9) . C50 . C51 . F51 . 121.1(10) . C50 . C51 . C52 . 124.9(12) . F51 . C51 . C52 . 114.0(10) . C51 . C52 . F52 . 120.7(14) . C51 . C52 . C53 . 120.1(12) . F52 . C52 . C53 . 119.1(12) . C52 . C53 . F53 . 122.4(14) . C52 . C53 . C54 . 119.3(11) . F53 . C53 . C54 . 118.3(15) . C53 . C54 . F54 . 120.9(12) . C53 . C54 . C55 . 118.1(12) . F54 . C54 . C55 . 120.9(12) . C50 . C55 . C54 . 125.3(10) . C50 . C55 . F55 . 119.3(8) . C54 . C55 . F55 . 115.4(10) . B34 . C60 . C61 . 122.3(9) . B34 . C60 . C65 . 123.7(9) . C61 . C60 . C65 . 112.7(9) . C60 . C61 . F61 . 120.4(9) . C60 . C61 . C62 . 124.1(11) . F61 . C61 . C62 . 115.5(10) . C61 . C62 . F62 . 119.4(12) . C61 . C62 . C63 . 120.4(11) . F62 . C62 . C63 . 120.1(11) . C62 . C63 . F63 . 120.2(13) . C62 . C63 . C64 . 118.4(10) . F63 . C63 . C64 . 121.3(13) . C63 . C64 . F64 . 120.3(11) . C63 . C64 . C65 . 120.2(11) . F64 . C64 . C65 . 119.5(12) . C60 . C65 . C64 . 124.1(11) . C60 . C65 . F65 . 120.0(8) . C64 . C65 . F65 . 115.9(10) . C102 . C101 . O105 . 110.3(26) . C102 . C101 . H1011 . 106.8(27) . O105 . C101 . H1011 . 114.6(26) . C102 . C101 . H1012 . 103.6(26) . O105 . C101 . H1012 . 115.5(25) . H1011 . C101 . H1012 . 105.1(24) . C101 . C102 . C103 . 99.8(28) . C101 . C102 . H1021 . 114.4(28) . C103 . C102 . H1021 . 110.3(32) . C101 . C102 . H1022 . 120.3(32) . C103 . C102 . H1022 . 113.8(34) . H1021 . C102 . H1022 . 98.6(26) . C102 . C103 . C104 . 112.5(41) . C102 . C103 . H1031 . 109.9(36) . C104 . C103 . H1031 . 111.4(44) . C102 . C103 . H1032 . 108.0(38) . C104 . C103 . H1032 . 111.2(42) . H1031 . C103 . H1032 . 103.4(33) . C103 . C104 . O105 . 117.3(41) . C103 . C104 . H1041 . 113.5(44) . O105 . C104 . H1041 . 105.8(36) . C103 . C104 . H1042 . 115.0(45) . O105 . C104 . H1042 . 108.4(38) . H1041 . C104 . H1042 . 94.1(30) . C101 . O105 . C104 . 98.2(27) . C202 . C201 . C205 . 107.8(9) . C202 . C201 . H2011 . 100.3(52) . C205 . C201 . H2011 . 120.7(40) . C202 . C201 . H2012 . 100.1(52) . C205 . C201 . H2012 . 122.6(41) . H2011 . C201 . H2012 . 101.4(22) . C201 . C202 . C203 . 108.9(8) . C201 . C202 . H2021 . 117.2(50) . C203 . C202 . H2021 . 103.9(56) . C201 . C202 . H2022 . 117.1(50) . C203 . C202 . H2022 . 104.2(55) . H2021 . C202 . H2022 . 104.1(25) . C202 . C203 . O204 . 106.8(11) . C202 . C203 . H2031 . 116.3(45) . O204 . C203 . H2031 . 98.7(51) . C202 . C203 . H2032 . 115.3(44) . O204 . C203 . H2032 . 98.7(50) . H2031 . C203 . H2032 . 117.0(32) . C201 . C205 . O204 . 107.9(9) . C201 . C205 . H2051 . 89.1(56) . O204 . C205 . H2051 . 128.9(39) . C201 . C205 . H2052 . 87.8(52) . O204 . C205 . H2052 . 125.1(36) . H2051 . C205 . H2052 . 102.7(40) . C203 . O204 . C205 . 108.7(9) . #==END