# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Helen Aspinall' _publ_contact_author_email HCA@LIV.AC.UK _publ_section_title ; Deposition of zirconium dioxide and hafnium dioxide thin films by liquid injection MOCVD and ALD using ansa-metallocene zirconium and hafnium precursors ; loop_ _publ_author_name 'H. Aspinall' 'John Bacsa' 'Kate Black' 'P. Chalker' 'Simon Elliott' 'Peter N. Heys' ; A.C.Jones ; 'Katarzyna Przybylak' 'Stephen Taylor' 'Ce Zhou Zhao.' 'Aleksandra Zydor' # Attachment 'B807205A.cif' data_KP23 _database_code_depnum_ccdc_archive 'CCDC 686525' # start Validation Reply Form #_vrf_PLAT029_KP23 #; #PROBLEM: _diffrn_measured_fraction_theta_full #RESPONSE: The data set is 99% complete to 25 degrees, 93 % to 27 degrees. #The structure is well-refined with low esd's on the bond distances and #angles #; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common KP23 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 O Zr' _chemical_formula_weight 307.53 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' 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_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 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 7.6566(7) _cell_length_b 14.2184(13) _cell_length_c 12.4639(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.546(2) _cell_angle_gamma 90.00 _cell_volume 1356.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7434 _cell_measurement_theta_min 0.93 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6927 _exptl_absorpt_correction_T_max 0.7969 _exptl_absorpt_process_details 'SADABS-2007/4 (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 diffractometer with APEX detector' _diffrn_measurement_method '\w scans with a narrow frame width' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7252 _diffrn_reflns_av_R_equivalents 0.0111 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2892 _reflns_number_gt 2706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v.5.632 (Bruker, 2005)' _computing_cell_refinement 'SAINT v6.45a (Bruker, 2005)' _computing_data_reduction 'SAINT v6.45a (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.6236P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2892 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0496 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Zr1 Zr Uani 0.14329(2) 0.70675(1) 0.45735(1) 1.000 0.0131(1) . . O1 O Uani 0.20966(14) 0.60858(7) 0.35953(9) 1.000 0.0198(3) . . C1 C Uani -0.1504(2) 0.68073(13) 0.46391(15) 1.000 0.0242(5) . . C2 C Uani 0.3098(3) 0.53426(13) 0.32172(17) 1.000 0.0334(6) . . C3 C Uani 0.26127(19) 0.86968(9) 0.47686(12) 1.000 0.0165(4) . . C4 C Uani 0.0808(2) 0.88194(10) 0.45587(13) 1.000 0.0186(4) . . C5 C Uani 0.0410(2) 0.85226(10) 0.34906(13) 1.000 0.0207(4) . . C6 C Uani 0.1964(2) 0.82206(11) 0.30368(12) 1.000 0.0202(4) . . C7 C Uani 0.3325(2) 0.83076(10) 0.38219(12) 1.000 0.0179(4) . . C8 C Uani 0.3490(2) 0.86438(10) 0.58899(12) 1.000 0.0181(4) . . C9 C Uani 0.5467(2) 0.87812(12) 0.58503(14) 1.000 0.0232(5) . . C10 C Uani 0.2739(3) 0.93669(12) 0.66559(14) 1.000 0.0270(5) . . C11 C Uani 0.30246(19) 0.76343(11) 0.62107(11) 1.000 0.0172(4) . . C12 C Uani 0.1385(2) 0.73412(12) 0.65791(12) 1.000 0.0205(4) . . C13 C Uani 0.1263(2) 0.63501(12) 0.64754(12) 1.000 0.0221(4) . . C14 C Uani 0.2811(2) 0.60258(11) 0.60399(13) 1.000 0.0205(4) . . C15 C Uani 0.3899(2) 0.68120(11) 0.58538(12) 1.000 0.0175(4) . . H1A H Uiso -0.198(3) 0.7156(14) 0.5185(19) 1.000 0.038(6) . . H1B H Uiso -0.214(3) 0.6952(13) 0.3960(18) 1.000 0.030(5) . . H1C H Uiso -0.169(3) 0.6135(16) 0.4811(17) 1.000 0.038(6) . . H2 H Uiso 0.600(3) 0.8366(14) 0.5346(16) 1.000 0.027(5) . . H2A H Uiso 0.419(4) 0.554(2) 0.307(2) 1.000 0.073(9) . . H2B H Uiso 0.263(4) 0.511(2) 0.257(2) 1.000 0.075(9) . . H2C H Uiso 0.322(3) 0.4870(17) 0.373(2) 1.000 0.052(7) . . H4 H Uiso 0.005(3) 0.9031(13) 0.5058(16) 1.000 0.024(5) . . H5 H Uiso -0.068(2) 0.8539(12) 0.3160(15) 1.000 0.021(4) . . H6 H Uiso 0.203(3) 0.7976(12) 0.2343(18) 1.000 0.024(5) . . H7 H Uiso 0.451(3) 0.8131(13) 0.3727(15) 1.000 0.022(5) . . H9A H Uiso 0.571(3) 0.9410(15) 0.5649(15) 1.000 0.029(5) . . H10A H Uiso 0.326(3) 0.9288(14) 0.7355(17) 1.000 0.033(5) . . H10B H Uiso 0.306(3) 1.0013(15) 0.6410(17) 1.000 0.036(6) . . H10C H Uiso 0.150(3) 0.9333(13) 0.6720(15) 1.000 0.026(5) . . H12 H Uiso 0.056(3) 0.7689(14) 0.6827(17) 1.000 0.027(5) . . H13 H Uiso 0.030(3) 0.5979(13) 0.6655(15) 1.000 0.026(5) . . H14 H Uiso 0.309(2) 0.5410(14) 0.5901(15) 1.000 0.024(5) . . H15 H Uiso 0.500(3) 0.6800(13) 0.5555(15) 1.000 0.021(4) . . H19 H Uiso 0.595(3) 0.8688(14) 0.6538(17) 1.000 0.029(5) . . 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 0.0126(1) 0.0127(1) 0.0141(1) 0.0001(1) -0.0005(1) 0.0007(1) O1 0.0214(5) 0.0170(5) 0.0211(5) -0.0033(4) 0.0004(4) 0.0046(4) C1 0.0164(7) 0.0287(8) 0.0276(9) -0.0002(7) 0.0011(6) -0.0006(6) C2 0.0436(11) 0.0254(9) 0.0317(10) 0.0006(8) 0.0092(8) 0.0165(8) C3 0.0213(7) 0.0107(6) 0.0175(7) 0.0007(5) -0.0012(6) -0.0008(5) C4 0.0200(7) 0.0134(7) 0.0223(8) 0.0008(6) 0.0006(6) 0.0039(6) C5 0.0227(8) 0.0156(7) 0.0233(8) 0.0041(6) -0.0072(6) 0.0011(6) C6 0.0284(8) 0.0180(7) 0.0140(7) 0.0025(6) -0.0001(6) -0.0032(6) C7 0.0192(7) 0.0168(7) 0.0179(7) 0.0024(6) 0.0021(6) -0.0025(5) C8 0.0217(7) 0.0166(7) 0.0158(7) -0.0008(6) -0.0019(5) -0.0002(5) C9 0.0237(8) 0.0199(8) 0.0255(8) 0.0025(7) -0.0072(7) -0.0044(6) C10 0.0390(10) 0.0215(8) 0.0204(8) -0.0048(7) -0.0004(7) 0.0020(7) C11 0.0200(7) 0.0188(7) 0.0125(7) 0.0002(6) -0.0034(5) 0.0003(6) C12 0.0221(8) 0.0246(8) 0.0149(7) 0.0015(6) 0.0022(6) 0.0014(6) C13 0.0238(8) 0.0249(8) 0.0176(7) 0.0070(6) -0.0014(6) -0.0053(6) C14 0.0248(8) 0.0166(7) 0.0196(7) 0.0036(6) -0.0073(6) -0.0001(6) C15 0.0161(7) 0.0192(7) 0.0169(7) 0.0023(6) -0.0044(6) 0.0010(6) _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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 1.9305(11) . . yes Zr1 C1 2.2825(16) . . yes Zr1 C3 2.4960(13) . . yes Zr1 C4 2.5364(15) . . yes Zr1 C5 2.5804(15) . . yes Zr1 C6 2.5620(15) . . yes Zr1 C7 2.4816(15) . . yes Zr1 C11 2.4828(14) . . yes Zr1 C12 2.5311(15) . . yes Zr1 C13 2.5871(16) . . yes Zr1 C14 2.5581(16) . . yes Zr1 C15 2.4660(15) . . yes O1 C2 1.395(2) . . yes C3 C4 1.410(2) . . no C3 C7 1.425(2) . . no C3 C8 1.536(2) . . no C4 C5 1.422(2) . . no C5 C6 1.399(2) . . no C6 C7 1.416(2) . . no C8 C9 1.528(2) . . no C8 C10 1.526(2) . . no C8 C11 1.535(2) . . no C11 C12 1.411(2) . . no C11 C15 1.425(2) . . no C12 C13 1.418(2) . . no C13 C14 1.395(2) . . no C14 C15 1.417(2) . . no C1 H1A 0.93(2) . . no C1 H1B 0.99(2) . . no C1 H1C 0.99(2) . . no C2 H2A 0.91(3) . . no C2 H2B 0.93(3) . . no C2 H2C 0.93(2) . . no C4 H4 0.91(2) . . no C5 H5 0.921(16) . . no C6 H6 0.94(2) . . no C7 H7 0.95(2) . . no C9 H2 0.96(2) . . no C9 H9A 0.95(2) . . no C9 H19 0.93(2) . . no C10 H10A 0.96(2) . . no C10 H10B 1.00(2) . . no C10 H10C 0.96(2) . . no C12 H12 0.87(2) . . no C13 H13 0.94(2) . . no C14 H14 0.92(2) . . no C15 H15 0.93(2) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 C1 100.47(6) . . . yes O1 Zr1 C3 129.19(5) . . . yes O1 Zr1 C4 139.32(5) . . . yes O1 Zr1 C5 109.31(5) . . . yes O1 Zr1 C6 86.60(5) . . . yes O1 Zr1 C7 96.26(5) . . . yes O1 Zr1 C11 128.46(5) . . . yes O1 Zr1 C12 138.25(5) . . . yes O1 Zr1 C13 108.31(5) . . . yes O1 Zr1 C14 85.53(5) . . . yes O1 Zr1 C15 95.29(5) . . . yes C1 Zr1 C3 120.09(6) . . . yes C1 Zr1 C4 88.49(6) . . . yes C1 Zr1 C5 82.14(6) . . . yes C1 Zr1 C6 107.87(6) . . . yes C1 Zr1 C7 135.60(6) . . . yes C1 Zr1 C11 119.04(6) . . . yes C1 Zr1 C12 87.08(6) . . . yes C1 Zr1 C13 80.17(6) . . . yes C1 Zr1 C14 105.57(6) . . . yes C1 Zr1 C15 133.70(6) . . . yes C3 Zr1 C4 32.54(5) . . . yes C3 Zr1 C5 53.90(5) . . . yes C3 Zr1 C6 54.17(5) . . . yes C3 Zr1 C7 33.27(5) . . . yes C3 Zr1 C11 56.66(5) . . . yes C3 Zr1 C12 77.05(5) . . . yes C3 Zr1 C13 107.68(5) . . . yes C3 Zr1 C14 109.06(5) . . . yes C3 Zr1 C15 78.75(5) . . . yes C4 Zr1 C5 32.25(5) . . . yes C4 Zr1 C6 53.12(5) . . . yes C4 Zr1 C7 53.94(5) . . . yes C4 Zr1 C11 77.03(5) . . . yes C4 Zr1 C12 81.28(5) . . . yes C4 Zr1 C13 112.32(5) . . . yes C4 Zr1 C14 130.39(5) . . . yes C4 Zr1 C15 106.88(5) . . . yes C5 Zr1 C6 31.56(5) . . . yes C5 Zr1 C7 53.48(5) . . . yes C5 Zr1 C11 107.76(5) . . . yes C5 Zr1 C12 112.40(5) . . . yes C5 Zr1 C13 140.66(5) . . . yes C5 Zr1 C14 162.08(5) . . . yes C5 Zr1 C15 132.29(5) . . . yes C6 Zr1 C7 32.55(5) . . . yes C6 Zr1 C11 108.81(5) . . . yes C6 Zr1 C12 130.30(5) . . . yes C6 Zr1 C13 161.85(5) . . . yes C6 Zr1 C14 146.51(5) . . . yes C6 Zr1 C15 116.35(5) . . . yes C7 Zr1 C11 78.52(5) . . . yes C7 Zr1 C12 106.72(5) . . . yes C7 Zr1 C13 132.09(5) . . . yes C7 Zr1 C14 116.57(5) . . . yes C7 Zr1 C15 84.51(5) . . . yes C11 Zr1 C12 32.68(5) . . . yes C11 Zr1 C13 53.89(5) . . . yes C11 Zr1 C14 54.33(5) . . . yes C11 Zr1 C15 33.46(5) . . . yes C12 Zr1 C13 32.14(5) . . . yes C12 Zr1 C14 53.14(5) . . . yes C12 Zr1 C15 54.18(5) . . . yes C13 Zr1 C14 31.46(5) . . . yes C13 Zr1 C15 53.53(5) . . . yes C14 Zr1 C15 32.70(5) . . . yes Zr1 O1 C2 156.57(12) . . . yes Zr1 C3 C4 75.31(8) . . . yes Zr1 C3 C7 72.81(8) . . . yes Zr1 C3 C8 101.03(8) . . . yes C4 C3 C7 106.82(13) . . . no C4 C3 C8 125.25(13) . . . no C7 C3 C8 124.51(13) . . . no Zr1 C4 C3 72.16(8) . . . yes Zr1 C4 C5 75.58(8) . . . yes C3 C4 C5 108.74(13) . . . no Zr1 C5 C4 72.17(8) . . . yes Zr1 C5 C6 73.49(9) . . . yes C4 C5 C6 107.85(13) . . . no Zr1 C6 C5 74.94(9) . . . yes Zr1 C6 C7 70.60(8) . . . yes C5 C6 C7 108.18(13) . . . no Zr1 C7 C3 73.92(8) . . . yes Zr1 C7 C6 76.85(9) . . . yes C3 C7 C6 108.38(13) . . . no C3 C8 C9 111.93(13) . . . no C3 C8 C10 111.92(13) . . . no C3 C8 C11 100.61(11) . . . no C9 C8 C10 108.92(14) . . . no C9 C8 C11 111.42(12) . . . no C10 C8 C11 111.91(13) . . . no Zr1 C11 C8 101.64(9) . . . yes Zr1 C11 C12 75.54(9) . . . yes Zr1 C11 C15 72.62(8) . . . yes C8 C11 C12 125.16(14) . . . no C8 C11 C15 124.89(13) . . . no C12 C11 C15 106.79(14) . . . no Zr1 C12 C11 71.78(8) . . . yes Zr1 C12 C13 76.11(9) . . . yes C11 C12 C13 108.71(14) . . . no Zr1 C13 C12 71.75(9) . . . yes Zr1 C13 C14 73.12(9) . . . yes C12 C13 C14 108.02(14) . . . no Zr1 C14 C13 75.42(9) . . . yes Zr1 C14 C15 70.08(9) . . . yes C13 C14 C15 108.20(14) . . . no Zr1 C15 C11 73.92(8) . . . yes Zr1 C15 C14 77.23(9) . . . yes C11 C15 C14 108.24(13) . . . no Zr1 C1 H1A 110.4(14) . . . no Zr1 C1 H1B 113.5(13) . . . no Zr1 C1 H1C 108.2(13) . . . no H1A C1 H1B 108.9(19) . . . no H1A C1 H1C 107.2(18) . . . no H1B C1 H1C 108.4(17) . . . no O1 C2 H2A 110.7(18) . . . no O1 C2 H2B 111.0(18) . . . no O1 C2 H2C 111.2(15) . . . no H2A C2 H2B 106(2) . . . no H2A C2 H2C 107(2) . . . no H2B C2 H2C 112(2) . . . no Zr1 C4 H4 116.2(12) . . . no C3 C4 H4 123.5(14) . . . no C5 C4 H4 127.7(14) . . . no Zr1 C5 H5 120.9(11) . . . no C4 C5 H5 125.5(11) . . . no C6 C5 H5 126.7(11) . . . no Zr1 C6 H6 117.9(11) . . . no C5 C6 H6 123.8(14) . . . no C7 C6 H6 128.0(14) . . . no Zr1 C7 H7 115.3(11) . . . no C3 C7 H7 126.4(11) . . . no C6 C7 H7 125.3(11) . . . no C8 C9 H2 112.4(13) . . . no C8 C9 H9A 109.3(14) . . . no C8 C9 H19 108.7(14) . . . no H2 C9 H9A 108.4(17) . . . no H2 C9 H19 110.4(18) . . . no H9A C9 H19 107.5(17) . . . no C8 C10 H10A 109.7(13) . . . no C8 C10 H10B 109.1(13) . . . no C8 C10 H10C 114.2(11) . . . no H10A C10 H10B 106.7(18) . . . no H10A C10 H10C 108.0(18) . . . no H10B C10 H10C 108.9(17) . . . no Zr1 C12 H12 118.1(14) . . . no C11 C12 H12 127.7(14) . . . no C13 C12 H12 123.6(14) . . . no Zr1 C13 H13 120.0(12) . . . no C12 C13 H13 126.0(12) . . . no C14 C13 H13 126.0(12) . . . no Zr1 C14 H14 120.7(12) . . . no C13 C14 H14 126.3(10) . . . no C15 C14 H14 125.5(10) . . . no Zr1 C15 H15 115.5(12) . . . no C11 C15 H15 125.3(12) . . . no C14 C15 H15 126.4(11) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Zr1 O1 C2 -134.4(3) . . . . no C3 Zr1 O1 C2 81.7(3) . . . . no C4 Zr1 O1 C2 125.6(3) . . . . no C5 Zr1 O1 C2 140.4(3) . . . . no C6 Zr1 O1 C2 118.1(3) . . . . no C7 Zr1 O1 C2 86.9(3) . . . . no C11 Zr1 O1 C2 6.6(3) . . . . no C12 Zr1 O1 C2 -37.0(3) . . . . no C13 Zr1 O1 C2 -51.4(3) . . . . no C14 Zr1 O1 C2 -29.4(3) . . . . no C15 Zr1 O1 C2 1.9(3) . . . . no O1 Zr1 C3 C4 122.77(9) . . . . no O1 Zr1 C3 C7 9.55(11) . . . . no O1 Zr1 C3 C8 -113.40(9) . . . . no C1 Zr1 C3 C4 -15.25(11) . . . . no C1 Zr1 C3 C7 -128.47(9) . . . . no C1 Zr1 C3 C8 108.58(10) . . . . no C4 Zr1 C3 C7 -113.22(13) . . . . no C4 Zr1 C3 C8 123.83(14) . . . . no C5 Zr1 C3 C4 36.58(9) . . . . no C5 Zr1 C3 C7 -76.64(9) . . . . no C5 Zr1 C3 C8 160.41(11) . . . . no C6 Zr1 C3 C4 75.85(10) . . . . no C6 Zr1 C3 C7 -37.37(8) . . . . no C6 Zr1 C3 C8 -160.32(11) . . . . no C7 Zr1 C3 C4 113.22(13) . . . . no C7 Zr1 C3 C8 -122.95(13) . . . . no C11 Zr1 C3 C4 -122.13(10) . . . . no C11 Zr1 C3 C7 124.66(10) . . . . no C11 Zr1 C3 C8 1.70(8) . . . . no C12 Zr1 C3 C4 -94.09(9) . . . . no C12 Zr1 C3 C7 152.70(9) . . . . no C12 Zr1 C3 C8 29.74(9) . . . . no C13 Zr1 C3 C4 -103.97(9) . . . . no C13 Zr1 C3 C7 142.81(8) . . . . no C13 Zr1 C3 C8 19.86(10) . . . . no C14 Zr1 C3 C4 -137.14(9) . . . . no C14 Zr1 C3 C7 109.64(9) . . . . no C14 Zr1 C3 C8 -13.31(10) . . . . no C15 Zr1 C3 C4 -149.58(10) . . . . no C15 Zr1 C3 C7 97.20(9) . . . . no C15 Zr1 C3 C8 -25.75(9) . . . . no O1 Zr1 C4 C3 -88.79(11) . . . . no O1 Zr1 C4 C5 26.76(12) . . . . no C1 Zr1 C4 C3 166.84(10) . . . . no C1 Zr1 C4 C5 -77.62(10) . . . . no C3 Zr1 C4 C5 115.55(13) . . . . no C5 Zr1 C4 C3 -115.55(13) . . . . no C6 Zr1 C4 C3 -79.36(10) . . . . no C6 Zr1 C4 C5 36.19(9) . . . . no C7 Zr1 C4 C3 -38.58(9) . . . . no C7 Zr1 C4 C5 76.96(10) . . . . no C11 Zr1 C4 C3 46.55(9) . . . . no C11 Zr1 C4 C5 162.10(10) . . . . no C12 Zr1 C4 C3 79.56(9) . . . . no C12 Zr1 C4 C5 -164.89(9) . . . . no C13 Zr1 C4 C3 88.11(9) . . . . no C13 Zr1 C4 C5 -156.35(9) . . . . no C14 Zr1 C4 C3 57.57(11) . . . . no C14 Zr1 C4 C5 173.12(8) . . . . no C15 Zr1 C4 C3 31.26(10) . . . . no C15 Zr1 C4 C5 146.81(9) . . . . no O1 Zr1 C5 C4 -161.88(8) . . . . no O1 Zr1 C5 C6 -46.34(10) . . . . no C1 Zr1 C5 C4 99.72(10) . . . . no C1 Zr1 C5 C6 -144.74(10) . . . . no C3 Zr1 C5 C4 -36.91(9) . . . . no C3 Zr1 C5 C6 78.63(10) . . . . no C4 Zr1 C5 C6 115.54(13) . . . . no C6 Zr1 C5 C4 -115.54(13) . . . . no C7 Zr1 C5 C4 -78.53(9) . . . . no C7 Zr1 C5 C6 37.02(9) . . . . no C11 Zr1 C5 C4 -18.34(10) . . . . no C11 Zr1 C5 C6 97.21(9) . . . . no C12 Zr1 C5 C4 16.18(10) . . . . no C12 Zr1 C5 C6 131.73(9) . . . . no C13 Zr1 C5 C4 35.83(12) . . . . no C13 Zr1 C5 C6 151.37(9) . . . . no C15 Zr1 C5 C4 -45.09(11) . . . . no C15 Zr1 C5 C6 70.46(11) . . . . no O1 Zr1 C6 C5 136.85(9) . . . . no O1 Zr1 C6 C7 -107.22(9) . . . . no C1 Zr1 C6 C5 36.94(10) . . . . no C1 Zr1 C6 C7 152.87(9) . . . . no C3 Zr1 C6 C5 -77.70(9) . . . . no C3 Zr1 C6 C7 38.24(8) . . . . no C4 Zr1 C6 C5 -37.01(9) . . . . no C4 Zr1 C6 C7 78.93(9) . . . . no C5 Zr1 C6 C7 115.93(13) . . . . no C7 Zr1 C6 C5 -115.93(13) . . . . no C11 Zr1 C6 C5 -93.50(9) . . . . no C11 Zr1 C6 C7 22.43(10) . . . . no C12 Zr1 C6 C5 -64.79(11) . . . . no C12 Zr1 C6 C7 51.14(11) . . . . no C14 Zr1 C6 C5 -146.52(10) . . . . no C14 Zr1 C6 C7 -30.59(14) . . . . no C15 Zr1 C6 C5 -128.93(9) . . . . no C15 Zr1 C6 C7 -13.00(10) . . . . no O1 Zr1 C7 C3 -172.57(8) . . . . no O1 Zr1 C7 C6 73.58(9) . . . . no C1 Zr1 C7 C3 75.51(11) . . . . no C1 Zr1 C7 C6 -38.34(12) . . . . no C3 Zr1 C7 C6 -113.85(13) . . . . no C4 Zr1 C7 C3 37.69(8) . . . . no C4 Zr1 C7 C6 -76.16(9) . . . . no C5 Zr1 C7 C3 77.99(9) . . . . no C5 Zr1 C7 C6 -35.86(9) . . . . no C6 Zr1 C7 C3 113.85(13) . . . . no C11 Zr1 C7 C3 -44.52(9) . . . . no C11 Zr1 C7 C6 -158.37(9) . . . . no C12 Zr1 C7 C3 -27.83(9) . . . . no C12 Zr1 C7 C6 -141.68(9) . . . . no C13 Zr1 C7 C3 -50.90(11) . . . . no C13 Zr1 C7 C6 -164.75(8) . . . . no C14 Zr1 C7 C3 -84.45(9) . . . . no C14 Zr1 C7 C6 161.70(8) . . . . no C15 Zr1 C7 C3 -77.83(9) . . . . no C15 Zr1 C7 C6 168.32(9) . . . . no O1 Zr1 C11 C8 114.61(9) . . . . no O1 Zr1 C11 C12 -121.75(9) . . . . no O1 Zr1 C11 C15 -8.58(11) . . . . no C1 Zr1 C11 C8 -110.43(10) . . . . no C1 Zr1 C11 C12 13.21(12) . . . . no C1 Zr1 C11 C15 126.38(9) . . . . no C3 Zr1 C11 C8 -1.71(8) . . . . no C3 Zr1 C11 C12 121.94(11) . . . . no C3 Zr1 C11 C15 -124.90(10) . . . . no C4 Zr1 C11 C8 -29.57(9) . . . . no C4 Zr1 C11 C12 94.08(10) . . . . no C4 Zr1 C11 C15 -152.76(9) . . . . no C5 Zr1 C11 C8 -19.65(10) . . . . no C5 Zr1 C11 C12 103.99(10) . . . . no C5 Zr1 C11 C15 -142.84(9) . . . . no C6 Zr1 C11 C8 13.62(10) . . . . no C6 Zr1 C11 C12 137.27(9) . . . . no C6 Zr1 C11 C15 -109.57(9) . . . . no C7 Zr1 C11 C8 25.71(9) . . . . no C7 Zr1 C11 C12 149.36(10) . . . . no C7 Zr1 C11 C15 -97.48(9) . . . . no C12 Zr1 C11 C8 -123.65(14) . . . . no C12 Zr1 C11 C15 113.16(13) . . . . no C13 Zr1 C11 C8 -160.14(11) . . . . no C13 Zr1 C11 C12 -36.50(9) . . . . no C13 Zr1 C11 C15 76.66(9) . . . . no C14 Zr1 C11 C8 160.75(11) . . . . no C14 Zr1 C11 C12 -75.60(10) . . . . no C14 Zr1 C11 C15 37.56(9) . . . . no C15 Zr1 C11 C8 123.19(13) . . . . no C15 Zr1 C11 C12 -113.16(13) . . . . no O1 Zr1 C12 C11 89.06(11) . . . . no O1 Zr1 C12 C13 -26.37(12) . . . . no C1 Zr1 C12 C11 -168.46(10) . . . . no C1 Zr1 C12 C13 76.12(10) . . . . no C3 Zr1 C12 C11 -46.67(9) . . . . no C3 Zr1 C12 C13 -162.10(10) . . . . no C4 Zr1 C12 C11 -79.54(10) . . . . no C4 Zr1 C12 C13 165.04(9) . . . . no C5 Zr1 C12 C11 -88.19(10) . . . . no C5 Zr1 C12 C13 156.38(9) . . . . no C6 Zr1 C12 C11 -57.38(11) . . . . no C6 Zr1 C12 C13 -172.81(8) . . . . no C7 Zr1 C12 C11 -31.44(10) . . . . no C7 Zr1 C12 C13 -146.86(9) . . . . no C11 Zr1 C12 C13 -115.43(13) . . . . no C13 Zr1 C12 C11 115.43(13) . . . . no C14 Zr1 C12 C11 79.57(10) . . . . no C14 Zr1 C12 C13 -35.85(9) . . . . no C15 Zr1 C12 C11 38.69(9) . . . . no C15 Zr1 C12 C13 -76.74(10) . . . . no O1 Zr1 C13 C12 161.85(9) . . . . no O1 Zr1 C13 C14 45.72(10) . . . . no C1 Zr1 C13 C12 -100.28(10) . . . . no C1 Zr1 C13 C14 143.59(10) . . . . no C3 Zr1 C13 C12 18.33(10) . . . . no C3 Zr1 C13 C14 -97.80(10) . . . . no C4 Zr1 C13 C12 -16.02(10) . . . . no C4 Zr1 C13 C14 -132.15(9) . . . . no C5 Zr1 C13 C12 -35.75(12) . . . . no C5 Zr1 C13 C14 -151.88(9) . . . . no C7 Zr1 C13 C12 44.87(11) . . . . no C7 Zr1 C13 C14 -71.26(11) . . . . no C11 Zr1 C13 C12 37.13(9) . . . . no C11 Zr1 C13 C14 -79.01(10) . . . . no C12 Zr1 C13 C14 -116.13(13) . . . . no C14 Zr1 C13 C12 116.13(13) . . . . no C15 Zr1 C13 C12 78.97(10) . . . . no C15 Zr1 C13 C14 -37.16(9) . . . . no O1 Zr1 C14 C13 -137.02(10) . . . . no O1 Zr1 C14 C15 107.03(9) . . . . no C1 Zr1 C14 C13 -37.38(11) . . . . no C1 Zr1 C14 C15 -153.33(9) . . . . no C3 Zr1 C14 C13 92.92(10) . . . . no C3 Zr1 C14 C15 -23.03(10) . . . . no C4 Zr1 C14 C13 64.22(11) . . . . no C4 Zr1 C14 C15 -51.73(11) . . . . no C6 Zr1 C14 C13 146.03(10) . . . . no C6 Zr1 C14 C15 30.09(14) . . . . no C7 Zr1 C14 C13 128.21(9) . . . . no C7 Zr1 C14 C15 12.26(11) . . . . no C11 Zr1 C14 C13 77.47(10) . . . . no C11 Zr1 C14 C15 -38.47(9) . . . . no C12 Zr1 C14 C13 36.66(9) . . . . no C12 Zr1 C14 C15 -79.29(10) . . . . no C13 Zr1 C14 C15 -115.95(14) . . . . no C15 Zr1 C14 C13 115.95(14) . . . . no O1 Zr1 C15 C11 173.26(9) . . . . no O1 Zr1 C15 C14 -73.20(9) . . . . no C1 Zr1 C15 C11 -76.81(11) . . . . no C1 Zr1 C15 C14 36.74(13) . . . . no C3 Zr1 C15 C11 44.31(9) . . . . no C3 Zr1 C15 C14 157.86(10) . . . . no C4 Zr1 C15 C11 27.78(10) . . . . no C4 Zr1 C15 C14 141.32(9) . . . . no C5 Zr1 C15 C11 51.04(11) . . . . no C5 Zr1 C15 C14 164.58(9) . . . . no C6 Zr1 C15 C11 84.44(9) . . . . no C6 Zr1 C15 C14 -162.02(9) . . . . no C7 Zr1 C15 C11 77.46(9) . . . . no C7 Zr1 C15 C14 -169.00(9) . . . . no C11 Zr1 C15 C14 113.54(13) . . . . no C12 Zr1 C15 C11 -37.75(9) . . . . no C12 Zr1 C15 C14 75.80(10) . . . . no C13 Zr1 C15 C11 -77.84(9) . . . . no C13 Zr1 C15 C14 35.71(9) . . . . no C14 Zr1 C15 C11 -113.54(13) . . . . no Zr1 C3 C4 C5 -67.33(10) . . . . no C7 C3 C4 Zr1 66.52(9) . . . . no C7 C3 C4 C5 -0.80(16) . . . . no C8 C3 C4 Zr1 -93.27(13) . . . . no C8 C3 C4 C5 -160.59(13) . . . . no Zr1 C3 C7 C6 69.80(11) . . . . no C4 C3 C7 Zr1 -68.23(10) . . . . no C4 C3 C7 C6 1.57(16) . . . . no C8 C3 C7 Zr1 91.74(13) . . . . no C8 C3 C7 C6 161.54(13) . . . . no Zr1 C3 C8 C9 116.07(11) . . . . no Zr1 C3 C8 C10 -121.32(12) . . . . no Zr1 C3 C8 C11 -2.34(11) . . . . no C4 C3 C8 C9 -164.22(13) . . . . no C4 C3 C8 C10 -41.61(19) . . . . no C4 C3 C8 C11 77.37(16) . . . . no C7 C3 C8 C9 39.45(19) . . . . no C7 C3 C8 C10 162.06(14) . . . . no C7 C3 C8 C11 -78.97(16) . . . . no Zr1 C4 C5 C6 -65.35(11) . . . . no C3 C4 C5 Zr1 65.08(10) . . . . no C3 C4 C5 C6 -0.26(17) . . . . no Zr1 C5 C6 C7 -63.23(11) . . . . no C4 C5 C6 Zr1 64.47(10) . . . . no C4 C5 C6 C7 1.24(17) . . . . no Zr1 C6 C7 C3 -67.83(10) . . . . no C5 C6 C7 Zr1 66.08(11) . . . . no C5 C6 C7 C3 -1.75(17) . . . . no C3 C8 C11 Zr1 2.36(11) . . . . no C3 C8 C11 C12 -78.04(17) . . . . no C3 C8 C11 C15 79.17(17) . . . . no C9 C8 C11 Zr1 -116.43(11) . . . . no C9 C8 C11 C12 163.16(14) . . . . no C9 C8 C11 C15 -39.6(2) . . . . no C10 C8 C11 Zr1 121.35(12) . . . . no C10 C8 C11 C12 40.9(2) . . . . no C10 C8 C11 C15 -161.84(15) . . . . no Zr1 C11 C12 C13 67.77(11) . . . . no C8 C11 C12 Zr1 94.20(13) . . . . no C8 C11 C12 C13 161.96(14) . . . . no C15 C11 C12 Zr1 -66.42(10) . . . . no C15 C11 C12 C13 1.34(17) . . . . no Zr1 C11 C15 C14 -70.29(11) . . . . no C8 C11 C15 Zr1 -92.26(13) . . . . no C8 C11 C15 C14 -162.55(14) . . . . no C12 C11 C15 Zr1 68.43(10) . . . . no C12 C11 C15 C14 -1.86(17) . . . . no Zr1 C12 C13 C14 64.61(11) . . . . no C11 C12 C13 Zr1 -64.92(10) . . . . no C11 C12 C13 C14 -0.31(17) . . . . no Zr1 C13 C14 C15 62.86(11) . . . . no C12 C13 C14 Zr1 -63.72(11) . . . . no C12 C13 C14 C15 -0.86(18) . . . . no Zr1 C14 C15 C11 68.05(10) . . . . no C13 C14 C15 Zr1 -66.36(11) . . . . no C13 C14 C15 C11 1.70(18) . . . . no _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.389 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.058 #===END data_KP24 _database_code_depnum_ccdc_archive 'CCDC 686526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common KP24 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 Hf' _chemical_formula_weight 378.80 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' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.1700(14) _cell_length_b 9.0530(18) _cell_length_c 10.385(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.14(3) _cell_angle_gamma 90.00 _cell_volume 674.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 211(2) _cell_measurement_reflns_used 3099 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 23.2 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 7.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.090 _exptl_absorpt_correction_T_max 0.411 _exptl_absorpt_process_details 'SORTAV (R.H. Blessing, (1989)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 211(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '200\% f scan, \f-incr 2.0 \%, 100 exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4194 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 24.03 _reflns_number_total 1122 _reflns_number_gt 985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe & Cie, 1996)' _computing_cell_refinement 'IPDS (Stoe & Cie, 1996)' _computing_data_reduction 'IPDS (Stoe & Cie, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1122 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Hf1 Hf Uani 0.18694(5) 0.25000 0.18166(3) 1.000 0.0279(1) . . C1 C Uani 0.3159(16) 0.25000 -0.0112(9) 1.000 0.057(4) . . C2 C Uani -0.1136(14) 0.25000 0.1164(11) 1.000 0.058(4) . . C3 C Uani 0.3129(8) 0.1209(6) 0.3726(6) 1.000 0.0297(17) . . C4 C Uani 0.4126(9) 0.0666(6) 0.2662(6) 1.000 0.0348(19) . . C5 C Uani 0.2943(11) -0.0184(7) 0.1877(8) 1.000 0.051(3) . . C6 C Uani 0.1172(11) -0.0174(7) 0.2416(7) 1.000 0.048(3) . . C7 C Uani 0.1261(9) 0.0700(7) 0.3537(6) 1.000 0.039(2) . . C8 C Uani 0.3675(12) 0.25000 0.4569(8) 1.000 0.031(3) . . C9 C Uani 0.2695(16) 0.25000 0.5851(9) 1.000 0.049(3) . . C10 C Uani 0.5820(13) 0.25000 0.4844(9) 1.000 0.042(3) . . H1A H Uiso 0.25410 0.17720 -0.06570 0.500 0.0850 calc . H1B H Uiso 0.44720 0.22570 -0.00210 0.500 0.0850 calc . H1C H Uiso 0.30250 0.34710 -0.04980 0.500 0.0850 calc . H2A H Uiso -0.15290 0.35040 0.09770 0.500 0.0870 calc . H2B H Uiso -0.18990 0.20950 0.18400 0.500 0.0870 calc . H2C H Uiso -0.12790 0.19010 0.03940 0.500 0.0870 calc . H4 H Uiso 0.53920 0.08490 0.25080 1.000 0.0420 calc R H5 H Uiso 0.32780 -0.06760 0.11200 1.000 0.0620 calc R H6 H Uiso 0.01090 -0.06640 0.20870 1.000 0.0570 calc R H7 H Uiso 0.02540 0.09120 0.40720 1.000 0.0470 calc R H9A H Uiso 0.13580 0.25710 0.57030 0.500 0.0740 calc . H9B H Uiso 0.31200 0.33370 0.63610 0.500 0.0740 calc . H9C H Uiso 0.29820 0.15920 0.63100 0.500 0.0740 calc . H10A H Uiso 0.61420 0.33170 0.54110 0.500 0.0640 calc . H10B H Uiso 0.64730 0.26060 0.40400 0.500 0.0640 calc . H10C H Uiso 0.61800 0.15770 0.52530 0.500 0.0640 calc . 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 Hf1 0.0194(2) 0.0379(2) 0.0264(2) 0.0000 0.0023(1) 0.0000 C1 0.052(7) 0.089(8) 0.031(5) 0.0000 0.021(5) 0.0000 C2 0.028(6) 0.089(9) 0.058(7) 0.0000 -0.005(5) 0.0000 C3 0.034(3) 0.022(3) 0.033(3) 0.006(2) -0.001(2) -0.001(3) C4 0.029(3) 0.026(3) 0.049(4) -0.004(3) -0.006(3) 0.009(3) C5 0.065(5) 0.030(4) 0.059(5) -0.019(3) 0.004(4) 0.006(3) C6 0.047(4) 0.035(4) 0.062(5) -0.006(3) -0.004(3) -0.017(3) C7 0.031(4) 0.037(3) 0.048(4) 0.008(3) 0.005(3) -0.006(3) C8 0.027(5) 0.037(5) 0.029(4) 0.0000 -0.005(4) 0.0000 C9 0.062(7) 0.055(6) 0.031(5) 0.0000 0.009(5) 0.0000 C10 0.034(6) 0.048(6) 0.044(5) 0.0000 -0.012(4) 0.0000 _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 Hf1 C1 2.222(9) . ? Hf1 C2 2.246(10) . ? Hf1 C3 2.458(6) 4_565 ? Hf1 C3 2.458(6) . ? Hf1 C7 2.463(6) 4_565 ? Hf1 C7 2.463(6) . ? Hf1 C4 2.468(6) 4_565 ? Hf1 C4 2.468(6) . ? Hf1 C5 2.549(7) . ? Hf1 C5 2.549(7) 4_565 ? Hf1 C6 2.551(7) 4_565 ? Hf1 C6 2.551(7) . ? C8 C3 1.507(8) . ? C8 C3 1.507(8) 4_565 ? C8 C9 1.518(12) . ? C8 C10 1.559(12) . ? C3 C4 1.416(9) . ? C3 C7 1.427(9) . ? C4 C5 1.395(10) . ? C4 H4 0.9400 . ? C7 C6 1.408(10) . ? C7 H7 0.9400 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C10 H10A 0.9712 . ? C10 H10B 0.9712 . ? C10 H10C 0.9712 . ? C6 C5 1.397(11) . ? C6 H6 0.9400 . ? C9 H9A 0.9723 . ? C9 H9B 0.9723 . ? C9 H9C 0.9723 . ? C5 H5 0.9400 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Hf1 C2 98.2(4) . . ? C1 Hf1 C3 125.0(3) . 4_565 ? C2 Hf1 C3 125.3(3) . 4_565 ? C1 Hf1 C3 125.0(3) . . ? C2 Hf1 C3 125.3(3) . . ? C3 Hf1 C3 56.8(3) 4_565 . ? C1 Hf1 C7 137.41(17) . 4_565 ? C2 Hf1 C7 92.1(3) . 4_565 ? C3 Hf1 C7 33.7(2) 4_565 4_565 ? C3 Hf1 C7 78.3(2) . 4_565 ? C1 Hf1 C7 137.42(17) . . ? C2 Hf1 C7 92.1(3) . . ? C3 Hf1 C7 78.3(2) 4_565 . ? C3 Hf1 C7 33.7(2) . . ? C7 Hf1 C7 82.8(3) 4_565 . ? C1 Hf1 C4 92.2(3) . 4_565 ? C2 Hf1 C4 136.52(16) . 4_565 ? C3 Hf1 C4 33.4(2) 4_565 4_565 ? C3 Hf1 C4 78.8(2) . 4_565 ? C7 Hf1 C4 54.6(2) 4_565 4_565 ? C7 Hf1 C4 108.1(2) . 4_565 ? C1 Hf1 C4 92.2(3) . . ? C2 Hf1 C4 136.52(16) . . ? C3 Hf1 C4 78.8(2) 4_565 . ? C3 Hf1 C4 33.4(2) . . ? C7 Hf1 C4 108.1(2) 4_565 . ? C7 Hf1 C4 54.6(2) . . ? C4 Hf1 C4 84.6(3) 4_565 . ? C1 Hf1 C5 83.77(19) . . ? C2 Hf1 C5 107.15(18) . . ? C3 Hf1 C5 109.1(2) 4_565 . ? C3 Hf1 C5 54.6(2) . . ? C7 Hf1 C5 132.1(2) 4_565 . ? C7 Hf1 C5 53.8(2) . . ? C4 Hf1 C5 115.9(2) 4_565 . ? C4 Hf1 C5 32.3(2) . . ? C1 Hf1 C5 83.8(2) . 4_565 ? C2 Hf1 C5 107.15(18) . 4_565 ? C3 Hf1 C5 54.6(2) 4_565 4_565 ? C3 Hf1 C5 109.1(2) . 4_565 ? C7 Hf1 C5 53.8(2) 4_565 4_565 ? C7 Hf1 C5 132.1(2) . 4_565 ? C4 Hf1 C5 32.3(2) 4_565 4_565 ? C4 Hf1 C5 115.9(2) . 4_565 ? C5 Hf1 C5 144.8(4) . 4_565 ? C1 Hf1 C6 107.87(17) . 4_565 ? C2 Hf1 C6 83.2(2) . 4_565 ? C3 Hf1 C6 54.8(2) 4_565 4_565 ? C3 Hf1 C6 109.0(2) . 4_565 ? C7 Hf1 C6 32.5(2) 4_565 4_565 ? C7 Hf1 C6 114.4(2) . 4_565 ? C4 Hf1 C6 53.5(2) 4_565 4_565 ? C4 Hf1 C6 133.0(2) . 4_565 ? C5 Hf1 C6 163.5(2) . 4_565 ? C5 Hf1 C6 31.8(2) 4_565 4_565 ? C1 Hf1 C6 107.87(17) . . ? C2 Hf1 C6 83.2(2) . . ? C3 Hf1 C6 109.0(2) 4_565 . ? C3 Hf1 C6 54.8(2) . . ? C7 Hf1 C6 114.4(2) 4_565 . ? C7 Hf1 C6 32.5(2) . . ? C4 Hf1 C6 133.0(2) 4_565 . ? C4 Hf1 C6 53.5(2) . . ? C5 Hf1 C6 31.8(2) . . ? C5 Hf1 C6 163.5(2) 4_565 . ? C6 Hf1 C6 143.2(3) 4_565 . ? C3 C8 C3 101.7(7) . 4_565 ? C3 C8 C9 113.0(5) . . ? C3 C8 C9 113.0(5) 4_565 . ? C3 C8 C10 110.5(5) . . ? C3 C8 C10 110.5(5) 4_565 . ? C9 C8 C10 108.1(8) . . ? C4 C3 C7 105.5(5) . . ? C4 C3 C8 126.4(6) . . ? C7 C3 C8 124.3(6) . . ? C4 C3 Hf1 73.7(3) . . ? C7 C3 Hf1 73.4(3) . . ? C8 C3 Hf1 100.8(4) . . ? C5 C4 C3 109.7(6) . . ? C5 C4 Hf1 77.1(4) . . ? C3 C4 Hf1 72.9(3) . . ? C5 C4 H4 125.2 . . ? C3 C4 H4 125.2 . . ? Hf1 C4 H4 116.7 . . ? C6 C7 C3 108.8(6) . . ? C6 C7 Hf1 77.2(4) . . ? C3 C7 Hf1 72.9(3) . . ? C6 C7 H7 125.6 . . ? C3 C7 H7 125.6 . . ? Hf1 C7 H7 116.3 . . ? Hf1 C1 H1A 109.5 . . ? Hf1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Hf1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C8 C10 H10A 109.6 . . ? C8 C10 H10B 109.6 . . ? H10A C10 H10B 109.4 . . ? C8 C10 H10C 109.6 . . ? H10A C10 H10C 109.4 . . ? H10B C10 H10C 109.4 . . ? C5 C6 C7 107.9(6) . . ? C5 C6 Hf1 74.0(4) . . ? C7 C6 Hf1 70.3(4) . . ? C5 C6 H6 126.0 . . ? C7 C6 H6 126.0 . . ? Hf1 C6 H6 121.4 . . ? C8 C9 H9A 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 109.2 . . ? C8 C9 H9C 109.7 . . ? H9A C9 H9C 109.2 . . ? H9B C9 H9C 109.2 . . ? C4 C5 C6 108.0(6) . . ? C4 C5 Hf1 70.7(4) . . ? C6 C5 Hf1 74.2(4) . . ? C4 C5 H5 126.0 . . ? C6 C5 H5 126.0 . . ? Hf1 C5 H5 120.9 . . ? Hf1 C2 H2A 109.5 . . ? Hf1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Hf1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C8 C3 C4 77.2(8) 4_565 . . . ? C9 C8 C3 C4 -161.4(7) . . . . ? C10 C8 C3 C4 -40.2(8) . . . . ? C3 C8 C3 C7 -77.5(8) 4_565 . . . ? C9 C8 C3 C7 43.9(9) . . . . ? C10 C8 C3 C7 165.2(6) . . . . ? C3 C8 C3 Hf1 -0.4(7) 4_565 . . . ? C9 C8 C3 Hf1 121.0(6) . . . . ? C10 C8 C3 Hf1 -117.7(5) . . . . ? C1 Hf1 C3 C4 -12.5(4) . . . . ? C2 Hf1 C3 C4 122.7(4) . . . . ? C3 Hf1 C3 C4 -124.8(3) 4_565 . . . ? C7 Hf1 C3 C4 -153.1(4) 4_565 . . . ? C7 Hf1 C3 C4 112.2(5) . . . . ? C4 Hf1 C3 C4 -97.3(4) 4_565 . . . ? C5 Hf1 C3 C4 36.2(4) . . . . ? C5 Hf1 C3 C4 -108.4(4) 4_565 . . . ? C6 Hf1 C3 C4 -142.1(4) 4_565 . . . ? C6 Hf1 C3 C4 75.4(4) . . . . ? C1 Hf1 C3 C7 -124.7(4) . . . . ? C2 Hf1 C3 C7 10.5(5) . . . . ? C3 Hf1 C3 C7 123.0(3) 4_565 . . . ? C7 Hf1 C3 C7 94.7(5) 4_565 . . . ? C4 Hf1 C3 C7 150.5(4) 4_565 . . . ? C4 Hf1 C3 C7 -112.2(5) . . . . ? C5 Hf1 C3 C7 -76.0(4) . . . . ? C5 Hf1 C3 C7 139.4(4) 4_565 . . . ? C6 Hf1 C3 C7 105.7(4) 4_565 . . . ? C6 Hf1 C3 C7 -36.8(4) . . . . ? C1 Hf1 C3 C8 112.5(5) . . . . ? C2 Hf1 C3 C8 -112.2(5) . . . . ? C3 Hf1 C3 C8 0.3(5) 4_565 . . . ? C7 Hf1 C3 C8 -28.1(4) 4_565 . . . ? C7 Hf1 C3 C8 -122.8(6) . . . . ? C4 Hf1 C3 C8 27.7(4) 4_565 . . . ? C4 Hf1 C3 C8 125.0(6) . . . . ? C5 Hf1 C3 C8 161.2(5) . . . . ? C5 Hf1 C3 C8 16.6(5) 4_565 . . . ? C6 Hf1 C3 C8 -17.1(5) 4_565 . . . ? C6 Hf1 C3 C8 -159.6(5) . . . . ? C7 C3 C4 C5 -2.0(7) . . . . ? C8 C3 C4 C5 -160.5(6) . . . . ? Hf1 C3 C4 C5 -69.0(5) . . . . ? C7 C3 C4 Hf1 67.0(4) . . . . ? C8 C3 C4 Hf1 -91.5(6) . . . . ? C1 Hf1 C4 C5 -74.6(5) . . . . ? C2 Hf1 C4 C5 29.8(7) . . . . ? C3 Hf1 C4 C5 160.1(5) 4_565 . . . ? C3 Hf1 C4 C5 115.6(6) . . . . ? C7 Hf1 C4 C5 143.4(4) 4_565 . . . ? C7 Hf1 C4 C5 76.6(5) . . . . ? C4 Hf1 C4 C5 -166.6(4) 4_565 . . . ? C5 Hf1 C4 C5 -158.8(6) 4_565 . . . ? C6 Hf1 C4 C5 168.2(4) 4_565 . . . ? C6 Hf1 C4 C5 36.1(4) . . . . ? C1 Hf1 C4 C3 169.8(4) . . . . ? C2 Hf1 C4 C3 -85.8(6) . . . . ? C3 Hf1 C4 C3 44.5(3) 4_565 . . . ? C7 Hf1 C4 C3 27.8(4) 4_565 . . . ? C7 Hf1 C4 C3 -39.1(3) . . . . ? C4 Hf1 C4 C3 77.8(4) 4_565 . . . ? C5 Hf1 C4 C3 -115.6(6) . . . . ? C5 Hf1 C4 C3 85.6(4) 4_565 . . . ? C6 Hf1 C4 C3 52.6(5) 4_565 . . . ? C6 Hf1 C4 C3 -79.5(4) . . . . ? C4 C3 C7 C6 2.3(7) . . . . ? C8 C3 C7 C6 161.4(6) . . . . ? Hf1 C3 C7 C6 69.5(5) . . . . ? C4 C3 C7 Hf1 -67.2(4) . . . . ? C8 C3 C7 Hf1 91.9(5) . . . . ? C1 Hf1 C7 C6 -30.4(7) . . . . ? C2 Hf1 C7 C6 74.0(5) . . . . ? C3 Hf1 C7 C6 -160.3(4) 4_565 . . . ? C3 Hf1 C7 C6 -114.6(6) . . . . ? C7 Hf1 C7 C6 165.8(3) 4_565 . . . ? C4 Hf1 C7 C6 -145.1(4) 4_565 . . . ? C4 Hf1 C7 C6 -75.9(4) . . . . ? C5 Hf1 C7 C6 -35.8(4) . . . . ? C5 Hf1 C7 C6 -170.5(4) 4_565 . . . ? C6 Hf1 C7 C6 157.5(5) 4_565 . . . ? C1 Hf1 C7 C3 84.1(6) . . . . ? C2 Hf1 C7 C3 -171.4(4) . . . . ? C3 Hf1 C7 C3 -45.7(3) 4_565 . . . ? C7 Hf1 C7 C3 -79.6(4) 4_565 . . . ? C4 Hf1 C7 C3 -30.5(4) 4_565 . . . ? C4 Hf1 C7 C3 38.7(3) . . . . ? C5 Hf1 C7 C3 78.7(4) . . . . ? C5 Hf1 C7 C3 -55.9(5) 4_565 . . . ? C6 Hf1 C7 C3 -87.9(4) 4_565 . . . ? C6 Hf1 C7 C3 114.6(6) . . . . ? C3 C7 C6 C5 -1.8(8) . . . . ? Hf1 C7 C6 C5 64.9(6) . . . . ? C3 C7 C6 Hf1 -66.7(4) . . . . ? C1 Hf1 C6 C5 42.6(6) . . . . ? C2 Hf1 C6 C5 139.0(6) . . . . ? C3 Hf1 C6 C5 -95.9(5) 4_565 . . . ? C3 Hf1 C6 C5 -78.1(5) . . . . ? C7 Hf1 C6 C5 -131.8(5) 4_565 . . . ? C7 Hf1 C6 C5 -116.3(7) . . . . ? C4 Hf1 C6 C5 -68.3(6) 4_565 . . . ? C4 Hf1 C6 C5 -36.6(5) . . . . ? C5 Hf1 C6 C5 -90.8(10) 4_565 . . . ? C6 Hf1 C6 C5 -151.9(4) 4_565 . . . ? C1 Hf1 C6 C7 158.9(5) . . . . ? C2 Hf1 C6 C7 -104.7(5) . . . . ? C3 Hf1 C6 C7 20.4(5) 4_565 . . . ? C3 Hf1 C6 C7 38.2(4) . . . . ? C7 Hf1 C6 C7 -15.5(4) 4_565 . . . ? C4 Hf1 C6 C7 48.0(5) 4_565 . . . ? C4 Hf1 C6 C7 79.7(4) . . . . ? C5 Hf1 C6 C7 116.3(7) . . . . ? C5 Hf1 C6 C7 25.5(11) 4_565 . . . ? C6 Hf1 C6 C7 -35.6(8) 4_565 . . . ? C3 C4 C5 C6 1.0(8) . . . . ? Hf1 C4 C5 C6 -65.3(6) . . . . ? C3 C4 C5 Hf1 66.3(4) . . . . ? C7 C6 C5 C4 0.5(9) . . . . ? Hf1 C6 C5 C4 63.0(5) . . . . ? C7 C6 C5 Hf1 -62.5(5) . . . . ? C1 Hf1 C5 C4 104.3(5) . . . . ? C2 Hf1 C5 C4 -159.1(5) . . . . ? C3 Hf1 C5 C4 -20.7(5) 4_565 . . . ? C3 Hf1 C5 C4 -37.5(4) . . . . ? C7 Hf1 C5 C4 -49.8(6) 4_565 . . . ? C7 Hf1 C5 C4 -79.4(5) . . . . ? C4 Hf1 C5 C4 14.8(4) 4_565 . . . ? C5 Hf1 C5 C4 34.4(9) 4_565 . . . ? C6 Hf1 C5 C4 -31.6(11) 4_565 . . . ? C6 Hf1 C5 C4 -116.1(7) . . . . ? C1 Hf1 C5 C6 -139.6(6) . . . . ? C2 Hf1 C5 C6 -43.0(6) . . . . ? C3 Hf1 C5 C6 95.4(5) 4_565 . . . ? C3 Hf1 C5 C6 78.6(5) . . . . ? C7 Hf1 C5 C6 66.3(6) 4_565 . . . ? C7 Hf1 C5 C6 36.7(4) . . . . ? C4 Hf1 C5 C6 130.9(5) 4_565 . . . ? C4 Hf1 C5 C6 116.1(7) . . . . ? C5 Hf1 C5 C6 150.5(4) 4_565 . . . ? C6 Hf1 C5 C6 84.5(10) 4_565 . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.03 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.508 _refine_diff_density_min -1.644 _refine_diff_density_rms 0.144