# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- BulkyCp-final-121111.cif' _publ_contact_author ; Peter G. Jones Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_phone '049 531 391-5382' _publ_contact_author_fax '049 531 391-5387' _publ_contact_author_email p.jones@tu-bs.de #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; How big is a Cp? Cyloheptatrienyl Zirconium Complexes with Bulky Cyclopentadienyl and Indenyl Ligands. ; loop_ _publ_author_name _publ_author_address A.Glockner ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; H.Bauer ; Fachbereich Chemie Technische Universit\"at Kaiserslautern Erwin-Schroedinger Strasse 67663 Kaiserslautern Germany ; M.Maekawa ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; T.Bannenberg ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; C.G.Daniliuc ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; ; P.G.Jones ; ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; Yu.Sun ; Fachbereich Chemie Technische Universit\"at Kaiserslautern Erwin-Schroedinger Strasse 67663 Kaiserslautern Germany ; H.Sitzmann ; Fachbereich Chemie Technische Universit\"at Kaiserslautern Erwin-Schroedinger Strasse 67663 Kaiserslautern Germany ; M.Tamm ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; M.D.Walter ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_name 'Peter G. Jones' #============================================================================= # cif data for "andyg39" (compound 2) #============================================================================= data_andyg39 _database_code_depnum_ccdc_archive 'CCDC 853653' #TrackingRef '- BulkyCp-final-121111.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H28 Zr' _chemical_formula_weight 359.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3641(2) _cell_length_b 9.9629(2) _cell_length_c 12.1930(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.555(2) _cell_angle_gamma 90.00 _cell_volume 1744.27(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15364 _cell_measurement_theta_min 3.6234 _cell_measurement_theta_max 75.6800 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 5.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81759 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15095 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0104 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 5.40 _diffrn_reflns_theta_max 75.80 _reflns_number_total 3610 _reflns_number_gt 3594 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogens of the seven membered ring and of the C9, C11 and c12 atoms were refined freely. The methyls were refined using a rigid model. ; _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^)+(0.0278P)^2^+1.1348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3610 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.813186(8) 0.584686(11) 0.173838(9) 0.01358(6) Uani 1 1 d . . . C1 C 0.82957(11) 0.78550(16) 0.27167(14) 0.0228(3) Uani 1 1 d . . . H1 H 0.7850(15) 0.845(2) 0.2889(17) 0.030(5) Uiso 1 1 d . . . C2 C 0.84346(12) 0.67832(18) 0.34754(13) 0.0247(3) Uani 1 1 d . . . H2 H 0.8033(16) 0.681(2) 0.4081(19) 0.039(6) Uiso 1 1 d . . . C3 C 0.90113(13) 0.56347(18) 0.33799(14) 0.0259(4) Uani 1 1 d . . . H3 H 0.8967(15) 0.504(2) 0.3935(18) 0.031(5) Uiso 1 1 d . . . C4 C 0.95912(11) 0.52661(17) 0.25026(14) 0.0241(3) Uani 1 1 d . . . H4 H 0.9872(16) 0.446(2) 0.2568(18) 0.031(5) Uiso 1 1 d . . . C5 C 0.97437(11) 0.59624(17) 0.15014(14) 0.0225(3) Uani 1 1 d . . . H5 H 1.0108(16) 0.551(2) 0.1014(18) 0.031(5) Uiso 1 1 d . . . C6 C 0.93423(11) 0.71934(17) 0.11300(13) 0.0215(3) Uani 1 1 d . . . H6 H 0.9466(14) 0.742(2) 0.0434(17) 0.026(5) Uiso 1 1 d . . . C7 C 0.86941(11) 0.80304(16) 0.16677(13) 0.0210(3) Uani 1 1 d . . . H7 H 0.8471(16) 0.873(2) 0.1245(18) 0.033(6) Uiso 1 1 d . . . C8 C 0.64177(10) 0.56764(14) 0.12389(12) 0.0150(3) Uani 1 1 d . . . C9 C 0.66947(10) 0.44163(15) 0.16907(12) 0.0143(3) Uani 1 1 d . . . H9 H 0.6464(14) 0.4082(18) 0.2359(16) 0.017(5) Uiso 1 1 d . . . C10 C 0.73370(10) 0.37809(15) 0.09829(11) 0.0143(3) Uani 1 1 d . . . C11 C 0.74630(10) 0.46735(15) 0.00912(11) 0.0147(3) Uani 1 1 d . . . H11 H 0.7861(13) 0.4515(19) -0.0501(16) 0.017(4) Uiso 1 1 d . . . C12 C 0.69023(11) 0.58284(14) 0.02477(12) 0.0152(3) Uani 1 1 d . . . H12 H 0.6838(13) 0.656(2) -0.0229(15) 0.018(4) Uiso 1 1 d . . . C13 C 0.56730(10) 0.66153(15) 0.16680(12) 0.0174(3) Uani 1 1 d . . . C14 C 0.56885(11) 0.66345(17) 0.29270(13) 0.0219(3) Uani 1 1 d . . . H14A H 0.5572 0.5727 0.3203 0.033 Uiso 1 1 calc R . . H14B H 0.5204 0.7243 0.3182 0.033 Uiso 1 1 calc R . . H14C H 0.6299 0.6945 0.3201 0.033 Uiso 1 1 calc R . . C15 C 0.47185(11) 0.60958(19) 0.12530(15) 0.0275(4) Uani 1 1 d . . . H15A H 0.4695 0.6099 0.0449 0.041 Uiso 1 1 calc R . . H15B H 0.4226 0.6678 0.1527 0.041 Uiso 1 1 calc R . . H15C H 0.4625 0.5179 0.1519 0.041 Uiso 1 1 calc R . . C16 C 0.58099(12) 0.80483(17) 0.12466(14) 0.0268(3) Uani 1 1 d . . . H16A H 0.6418 0.8386 0.1505 0.040 Uiso 1 1 calc R . . H16B H 0.5317 0.8628 0.1522 0.040 Uiso 1 1 calc R . . H16C H 0.5783 0.8048 0.0443 0.040 Uiso 1 1 calc R . . C17 C 0.77383(10) 0.23703(14) 0.10989(12) 0.0162(3) Uani 1 1 d . . . C18 C 0.78383(12) 0.19600(16) 0.23067(13) 0.0245(3) Uani 1 1 d . . . H18A H 0.8237 0.2608 0.2700 0.037 Uiso 1 1 calc R . . H18B H 0.8119 0.1065 0.2359 0.037 Uiso 1 1 calc R . . H18C H 0.7223 0.1945 0.2634 0.037 Uiso 1 1 calc R . . C19 C 0.70684(12) 0.14028(16) 0.04883(15) 0.0265(3) Uani 1 1 d . . . H19A H 0.6454 0.1444 0.0818 0.040 Uiso 1 1 calc R . . H19B H 0.7311 0.0486 0.0545 0.040 Uiso 1 1 calc R . . H19C H 0.7013 0.1663 -0.0286 0.040 Uiso 1 1 calc R . . C20 C 0.86996(11) 0.22843(16) 0.05867(13) 0.0199(3) Uani 1 1 d . . . H20A H 0.8645 0.2515 -0.0194 0.030 Uiso 1 1 calc R . . H20B H 0.8942 0.1369 0.0667 0.030 Uiso 1 1 calc R . . H20C H 0.9126 0.2914 0.0960 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01123(8) 0.01376(8) 0.01566(8) -0.00071(4) -0.00124(5) -0.00137(4) C1 0.0198(7) 0.0200(7) 0.0285(8) -0.0088(6) -0.0003(6) -0.0007(6) C2 0.0225(8) 0.0344(9) 0.0173(7) -0.0061(6) 0.0009(6) -0.0054(7) C3 0.0267(9) 0.0291(8) 0.0215(8) 0.0074(7) -0.0086(6) -0.0058(7) C4 0.0190(7) 0.0208(8) 0.0318(8) 0.0006(6) -0.0098(6) 0.0028(6) C5 0.0115(7) 0.0295(8) 0.0263(8) -0.0053(6) 0.0009(6) 0.0004(6) C6 0.0162(7) 0.0272(8) 0.0211(7) 0.0030(6) 0.0012(6) -0.0068(6) C7 0.0183(7) 0.0160(7) 0.0284(8) 0.0023(6) -0.0036(6) -0.0040(6) C8 0.0111(6) 0.0156(6) 0.0182(7) -0.0021(5) -0.0010(5) -0.0010(5) C9 0.0123(6) 0.0149(6) 0.0160(7) -0.0004(5) 0.0023(5) -0.0017(5) C10 0.0125(6) 0.0141(6) 0.0163(6) -0.0016(5) 0.0006(5) -0.0011(5) C11 0.0129(6) 0.0168(7) 0.0142(6) -0.0015(5) 0.0004(5) -0.0010(5) C12 0.0150(7) 0.0156(7) 0.0151(7) 0.0008(5) -0.0011(5) 0.0000(5) C13 0.0138(7) 0.0174(7) 0.0210(7) -0.0027(5) 0.0011(5) 0.0025(5) C14 0.0200(7) 0.0232(7) 0.0228(8) -0.0044(6) 0.0048(6) 0.0013(6) C15 0.0130(7) 0.0339(9) 0.0356(9) -0.0111(7) -0.0010(6) 0.0049(7) C16 0.0297(9) 0.0191(8) 0.0318(9) 0.0005(6) 0.0056(7) 0.0079(6) C17 0.0158(7) 0.0142(7) 0.0188(7) -0.0002(5) 0.0026(5) 0.0006(5) C18 0.0302(8) 0.0214(8) 0.0221(8) 0.0059(6) 0.0066(6) 0.0077(6) C19 0.0231(8) 0.0156(7) 0.0406(9) -0.0037(7) -0.0025(7) -0.0013(6) C20 0.0180(7) 0.0187(7) 0.0233(7) -0.0013(6) 0.0045(6) 0.0038(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_2 _geom_bond_publ_flag Zr C7 2.3229(15) . ? Zr C6 2.3330(15) . ? Zr C1 2.3380(15) . ? Zr C4 2.3433(15) . ? Zr C5 2.3438(16) . ? Zr C2 2.3441(16) . ? Zr C3 2.3472(16) . ? Zr C11 2.4937(14) . ? Zr C12 2.4999(15) . ? Zr C9 2.5079(14) . ? Zr C10 2.5163(14) . ? Zr C8 2.5261(14) . ? C1 C2 1.423(2) . ? C1 C7 1.426(2) . ? C2 C3 1.419(3) . ? C3 C4 1.422(3) . ? C4 C5 1.426(2) . ? C5 C6 1.424(2) . ? C6 C7 1.423(2) . ? C8 C12 1.419(2) . ? C8 C9 1.423(2) . ? C8 C13 1.524(2) . ? C9 C10 1.4283(19) . ? C10 C11 1.420(2) . ? C10 C17 1.524(2) . ? C11 C12 1.420(2) . ? C13 C16 1.532(2) . ? C13 C14 1.535(2) . ? C13 C15 1.538(2) . ? C17 C18 1.531(2) . ? C17 C20 1.533(2) . ? C17 C19 1.540(2) . ? 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 C7 Zr C6 35.60(6) . . ? C7 Zr C1 35.63(6) . . ? C6 Zr C1 66.71(6) . . ? C7 Zr C4 86.44(6) . . ? C6 Zr C4 66.55(6) . . ? C1 Zr C4 86.09(6) . . ? C7 Zr C5 66.66(6) . . ? C6 Zr C5 35.45(6) . . ? C1 Zr C5 86.26(6) . . ? C4 Zr C5 35.43(6) . . ? C7 Zr C2 66.71(6) . . ? C6 Zr C2 86.38(6) . . ? C1 Zr C2 35.39(6) . . ? C4 Zr C2 66.23(6) . . ? C5 Zr C2 86.11(6) . . ? C7 Zr C3 86.35(6) . . ? C6 Zr C3 86.24(6) . . ? C1 Zr C3 66.27(6) . . ? C4 Zr C3 35.29(6) . . ? C5 Zr C3 66.36(6) . . ? C2 Zr C3 35.22(6) . . ? C7 Zr C11 122.40(5) . . ? C6 Zr C11 106.72(5) . . ? C1 Zr C11 147.49(5) . . ? C4 Zr C11 121.70(5) . . ? C5 Zr C11 106.50(5) . . ? C2 Zr C11 166.46(5) . . ? C3 Zr C11 146.23(6) . . ? C7 Zr C12 102.67(5) . . ? C6 Zr C12 106.92(5) . . ? C1 Zr C12 115.89(5) . . ? C4 Zr C12 153.39(6) . . ? C5 Zr C12 126.26(6) . . ? C2 Zr C12 140.35(6) . . ? C3 Zr C12 166.56(6) . . ? C11 Zr C12 33.05(5) . . ? C7 Zr C9 144.90(5) . . ? C6 Zr C9 159.96(5) . . ? C1 Zr C9 124.72(5) . . ? C4 Zr C9 126.57(5) . . ? C5 Zr C9 147.17(5) . . ? C2 Zr C9 112.30(5) . . ? C3 Zr C9 113.09(5) . . ? C11 Zr C9 54.27(5) . . ? C12 Zr C9 54.13(5) . . ? C7 Zr C10 155.13(5) . . ? C6 Zr C10 133.52(5) . . ? C1 Zr C10 157.69(5) . . ? C4 Zr C10 109.62(5) . . ? C5 Zr C10 115.78(5) . . ? C2 Zr C10 136.68(5) . . ? C3 Zr C10 117.83(6) . . ? C11 Zr C10 32.93(5) . . ? C12 Zr C10 54.77(5) . . ? C9 Zr C10 33.03(4) . . ? C7 Zr C8 113.05(5) . . ? C6 Zr C8 133.78(5) . . ? C1 Zr C8 105.34(5) . . ? C4 Zr C8 159.20(5) . . ? C5 Zr C8 158.94(6) . . ? C2 Zr C8 113.59(5) . . ? C3 Zr C8 134.27(6) . . ? C11 Zr C8 54.73(5) . . ? C12 Zr C8 32.80(5) . . ? C9 Zr C8 32.85(5) . . ? C10 Zr C8 55.05(5) . . ? C2 C1 C7 128.48(15) . . ? C2 C1 Zr 72.54(9) . . ? C7 C1 Zr 71.61(9) . . ? C3 C2 C1 128.57(15) . . ? C3 C2 Zr 72.51(9) . . ? C1 C2 Zr 72.07(9) . . ? C2 C3 C4 128.69(16) . . ? C2 C3 Zr 72.27(9) . . ? C4 C3 Zr 72.21(9) . . ? C3 C4 C5 128.69(15) . . ? C3 C4 Zr 72.50(9) . . ? C5 C4 Zr 72.30(9) . . ? C6 C5 C4 128.38(15) . . ? C6 C5 Zr 71.86(9) . . ? C4 C5 Zr 72.27(9) . . ? C7 C6 C5 128.51(15) . . ? C7 C6 Zr 71.82(9) . . ? C5 C6 Zr 72.69(9) . . ? C6 C7 C1 128.67(15) . . ? C6 C7 Zr 72.59(9) . . ? C1 C7 Zr 72.76(9) . . ? C12 C8 C9 106.58(12) . . ? C12 C8 C13 126.29(13) . . ? C9 C8 C13 126.86(13) . . ? C12 C8 Zr 72.59(8) . . ? C9 C8 Zr 72.87(8) . . ? C13 C8 Zr 124.37(9) . . ? C8 C9 C10 109.60(13) . . ? C8 C9 Zr 74.28(8) . . ? C10 C9 Zr 73.81(8) . . ? C11 C10 C9 106.44(13) . . ? C11 C10 C17 126.35(13) . . ? C9 C10 C17 126.98(13) . . ? C11 C10 Zr 72.66(8) . . ? C9 C10 Zr 73.16(8) . . ? C17 C10 Zr 123.61(9) . . ? C10 C11 C12 108.66(12) . . ? C10 C11 Zr 74.41(8) . . ? C12 C11 Zr 73.71(8) . . ? C8 C12 C11 108.73(12) . . ? C8 C12 Zr 74.62(8) . . ? C11 C12 Zr 73.24(8) . . ? C8 C13 C16 111.05(12) . . ? C8 C13 C14 111.08(12) . . ? C16 C13 C14 108.99(13) . . ? C8 C13 C15 107.94(12) . . ? C16 C13 C15 108.94(14) . . ? C14 C13 C15 108.78(13) . . ? C10 C17 C18 111.15(12) . . ? C10 C17 C20 110.87(12) . . ? C18 C17 C20 108.34(12) . . ? C10 C17 C19 107.61(12) . . ? C18 C17 C19 109.82(13) . . ? C20 C17 C19 109.03(12) . . ? 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 C7 Zr C1 C2 -142.37(14) . . . . ? C6 Zr C1 C2 -119.16(11) . . . . ? C4 Zr C1 C2 -53.04(10) . . . . ? C5 Zr C1 C2 -88.55(10) . . . . ? C3 Zr C1 C2 -22.77(9) . . . . ? C11 Zr C1 C2 156.17(10) . . . . ? C12 Zr C1 C2 142.61(9) . . . . ? C9 Zr C1 C2 79.74(10) . . . . ? C10 Zr C1 C2 83.02(17) . . . . ? C8 Zr C1 C2 109.31(9) . . . . ? C6 Zr C1 C7 23.21(9) . . . . ? C4 Zr C1 C7 89.34(10) . . . . ? C5 Zr C1 C7 53.82(10) . . . . ? C2 Zr C1 C7 142.37(14) . . . . ? C3 Zr C1 C7 119.60(11) . . . . ? C11 Zr C1 C7 -61.46(14) . . . . ? C12 Zr C1 C7 -75.02(10) . . . . ? C9 Zr C1 C7 -137.89(9) . . . . ? C10 Zr C1 C7 -134.60(13) . . . . ? C8 Zr C1 C7 -108.32(9) . . . . ? C7 C1 C2 C3 0.8(3) . . . . ? Zr C1 C2 C3 48.54(16) . . . . ? C7 C1 C2 Zr -47.74(16) . . . . ? C7 Zr C2 C3 -119.31(11) . . . . ? C6 Zr C2 C3 -88.61(10) . . . . ? C1 Zr C2 C3 -142.09(15) . . . . ? C4 Zr C2 C3 -22.67(10) . . . . ? C5 Zr C2 C3 -53.08(10) . . . . ? C11 Zr C2 C3 105.9(2) . . . . ? C12 Zr C2 C3 159.02(10) . . . . ? C9 Zr C2 C3 98.86(10) . . . . ? C10 Zr C2 C3 71.21(12) . . . . ? C8 Zr C2 C3 134.59(10) . . . . ? C7 Zr C2 C1 22.78(9) . . . . ? C6 Zr C2 C1 53.49(10) . . . . ? C4 Zr C2 C1 119.42(11) . . . . ? C5 Zr C2 C1 89.01(10) . . . . ? C3 Zr C2 C1 142.09(15) . . . . ? C11 Zr C2 C1 -112.0(2) . . . . ? C12 Zr C2 C1 -58.88(13) . . . . ? C9 Zr C2 C1 -119.05(9) . . . . ? C10 Zr C2 C1 -146.69(9) . . . . ? C8 Zr C2 C1 -83.31(10) . . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? Zr C2 C3 C4 48.16(17) . . . . ? C1 C2 C3 Zr -48.38(16) . . . . ? C7 Zr C3 C2 53.37(10) . . . . ? C6 Zr C3 C2 89.05(10) . . . . ? C1 Zr C3 C2 22.87(10) . . . . ? C4 Zr C3 C2 142.36(15) . . . . ? C5 Zr C3 C2 119.46(11) . . . . ? C11 Zr C3 C2 -156.10(10) . . . . ? C12 Zr C3 C2 -79.4(3) . . . . ? C9 Zr C3 C2 -96.39(10) . . . . ? C10 Zr C3 C2 -132.73(9) . . . . ? C8 Zr C3 C2 -65.69(12) . . . . ? C7 Zr C3 C4 -88.98(10) . . . . ? C6 Zr C3 C4 -53.31(10) . . . . ? C1 Zr C3 C4 -119.49(11) . . . . ? C5 Zr C3 C4 -22.90(10) . . . . ? C2 Zr C3 C4 -142.36(15) . . . . ? C11 Zr C3 C4 61.54(14) . . . . ? C12 Zr C3 C4 138.2(2) . . . . ? C9 Zr C3 C4 121.25(10) . . . . ? C10 Zr C3 C4 84.91(10) . . . . ? C8 Zr C3 C4 151.95(9) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? Zr C3 C4 C5 48.63(16) . . . . ? C2 C3 C4 Zr -48.19(17) . . . . ? C7 Zr C4 C3 88.72(10) . . . . ? C6 Zr C4 C3 119.29(11) . . . . ? C1 Zr C4 C3 53.01(10) . . . . ? C5 Zr C4 C3 142.06(15) . . . . ? C2 Zr C4 C3 22.64(10) . . . . ? C11 Zr C4 C3 -144.94(9) . . . . ? C12 Zr C4 C3 -159.79(11) . . . . ? C9 Zr C4 C3 -78.29(11) . . . . ? C10 Zr C4 C3 -110.75(10) . . . . ? C8 Zr C4 C3 -71.51(19) . . . . ? C7 Zr C4 C5 -53.34(10) . . . . ? C6 Zr C4 C5 -22.77(9) . . . . ? C1 Zr C4 C5 -89.05(10) . . . . ? C2 Zr C4 C5 -119.42(11) . . . . ? C3 Zr C4 C5 -142.06(15) . . . . ? C11 Zr C4 C5 73.00(11) . . . . ? C12 Zr C4 C5 58.16(16) . . . . ? C9 Zr C4 C5 139.65(9) . . . . ? C10 Zr C4 C5 107.19(10) . . . . ? C8 Zr C4 C5 146.43(14) . . . . ? C3 C4 C5 C6 -0.8(3) . . . . ? Zr C4 C5 C6 47.92(16) . . . . ? C3 C4 C5 Zr -48.71(16) . . . . ? C7 Zr C5 C6 -22.93(9) . . . . ? C1 Zr C5 C6 -53.74(10) . . . . ? C4 Zr C5 C6 -142.25(15) . . . . ? C2 Zr C5 C6 -89.22(10) . . . . ? C3 Zr C5 C6 -119.44(11) . . . . ? C11 Zr C5 C6 95.81(10) . . . . ? C12 Zr C5 C6 65.91(11) . . . . ? C9 Zr C5 C6 144.18(10) . . . . ? C10 Zr C5 C6 129.80(9) . . . . ? C8 Zr C5 C6 70.87(18) . . . . ? C7 Zr C5 C4 119.32(11) . . . . ? C6 Zr C5 C4 142.25(15) . . . . ? C1 Zr C5 C4 88.51(10) . . . . ? C2 Zr C5 C4 53.03(10) . . . . ? C3 Zr C5 C4 22.81(10) . . . . ? C11 Zr C5 C4 -121.94(10) . . . . ? C12 Zr C5 C4 -151.84(9) . . . . ? C9 Zr C5 C4 -73.57(14) . . . . ? C10 Zr C5 C4 -87.95(10) . . . . ? C8 Zr C5 C4 -146.88(14) . . . . ? C4 C5 C6 C7 0.2(3) . . . . ? Zr C5 C6 C7 48.27(15) . . . . ? C4 C5 C6 Zr -48.06(16) . . . . ? C1 Zr C6 C7 -23.24(9) . . . . ? C4 Zr C6 C7 -119.31(10) . . . . ? C5 Zr C6 C7 -142.07(14) . . . . ? C2 Zr C6 C7 -53.69(10) . . . . ? C3 Zr C6 C7 -88.98(10) . . . . ? C11 Zr C6 C7 122.80(9) . . . . ? C12 Zr C6 C7 88.23(9) . . . . ? C9 Zr C6 C7 105.77(16) . . . . ? C10 Zr C6 C7 145.37(9) . . . . ? C8 Zr C6 C7 65.98(11) . . . . ? C7 Zr C6 C5 142.07(14) . . . . ? C1 Zr C6 C5 118.83(11) . . . . ? C4 Zr C6 C5 22.76(9) . . . . ? C2 Zr C6 C5 88.38(10) . . . . ? C3 Zr C6 C5 53.09(10) . . . . ? C11 Zr C6 C5 -95.13(10) . . . . ? C12 Zr C6 C5 -129.70(9) . . . . ? C9 Zr C6 C5 -112.16(16) . . . . ? C10 Zr C6 C5 -72.56(11) . . . . ? C8 Zr C6 C5 -151.95(9) . . . . ? C5 C6 C7 C1 1.0(3) . . . . ? Zr C6 C7 C1 49.54(15) . . . . ? C5 C6 C7 Zr -48.58(16) . . . . ? C2 C1 C7 C6 -1.4(3) . . . . ? Zr C1 C7 C6 -49.48(15) . . . . ? C2 C1 C7 Zr 48.07(16) . . . . ? C1 Zr C7 C6 141.54(14) . . . . ? C4 Zr C7 C6 53.28(10) . . . . ? C5 Zr C7 C6 22.85(9) . . . . ? C2 Zr C7 C6 118.89(10) . . . . ? C3 Zr C7 C6 88.64(10) . . . . ? C11 Zr C7 C6 -72.46(10) . . . . ? C12 Zr C7 C6 -101.43(9) . . . . ? C9 Zr C7 C6 -145.01(9) . . . . ? C10 Zr C7 C6 -78.44(15) . . . . ? C8 Zr C7 C6 -134.22(9) . . . . ? C6 Zr C7 C1 -141.54(14) . . . . ? C4 Zr C7 C1 -88.26(10) . . . . ? C5 Zr C7 C1 -118.69(11) . . . . ? C2 Zr C7 C1 -22.64(9) . . . . ? C3 Zr C7 C1 -52.90(10) . . . . ? C11 Zr C7 C1 146.00(9) . . . . ? C12 Zr C7 C1 117.03(9) . . . . ? C9 Zr C7 C1 73.45(13) . . . . ? C10 Zr C7 C1 140.02(12) . . . . ? C8 Zr C7 C1 84.24(10) . . . . ? C7 Zr C8 C12 77.28(9) . . . . ? C6 Zr C8 C12 41.98(11) . . . . ? C1 Zr C8 C12 114.22(9) . . . . ? C4 Zr C8 C12 -124.25(15) . . . . ? C5 Zr C8 C12 -7.39(19) . . . . ? C2 Zr C8 C12 150.84(9) . . . . ? C3 Zr C8 C12 -174.16(9) . . . . ? C11 Zr C8 C12 -37.07(8) . . . . ? C9 Zr C8 C12 -114.17(12) . . . . ? C10 Zr C8 C12 -77.61(9) . . . . ? C7 Zr C8 C9 -168.55(8) . . . . ? C6 Zr C8 C9 156.16(9) . . . . ? C1 Zr C8 C9 -131.61(9) . . . . ? C4 Zr C8 C9 -10.1(2) . . . . ? C5 Zr C8 C9 106.78(16) . . . . ? C2 Zr C8 C9 -94.99(9) . . . . ? C3 Zr C8 C9 -59.99(11) . . . . ? C11 Zr C8 C9 77.10(9) . . . . ? C12 Zr C8 C9 114.17(12) . . . . ? C10 Zr C8 C9 36.56(8) . . . . ? C7 Zr C8 C13 -45.21(13) . . . . ? C6 Zr C8 C13 -80.50(14) . . . . ? C1 Zr C8 C13 -8.26(13) . . . . ? C4 Zr C8 C13 113.27(17) . . . . ? C5 Zr C8 C13 -129.88(15) . . . . ? C2 Zr C8 C13 28.36(14) . . . . ? C3 Zr C8 C13 63.35(14) . . . . ? C11 Zr C8 C13 -159.56(14) . . . . ? C12 Zr C8 C13 -122.48(16) . . . . ? C9 Zr C8 C13 123.34(16) . . . . ? C10 Zr C8 C13 159.90(14) . . . . ? C12 C8 C9 C10 -0.67(16) . . . . ? C13 C8 C9 C10 173.58(13) . . . . ? Zr C8 C9 C10 -65.94(10) . . . . ? C12 C8 C9 Zr 65.26(10) . . . . ? C13 C8 C9 Zr -120.48(14) . . . . ? C7 Zr C9 C8 18.52(13) . . . . ? C6 Zr C9 C8 -58.41(18) . . . . ? C1 Zr C9 C8 61.32(10) . . . . ? C4 Zr C9 C8 175.57(9) . . . . ? C5 Zr C9 C8 -140.62(11) . . . . ? C2 Zr C9 C8 99.34(9) . . . . ? C3 Zr C9 C8 137.62(9) . . . . ? C11 Zr C9 C8 -78.63(9) . . . . ? C12 Zr C9 C8 -37.57(8) . . . . ? C10 Zr C9 C8 -116.40(12) . . . . ? C7 Zr C9 C10 134.92(10) . . . . ? C6 Zr C9 C10 57.99(18) . . . . ? C1 Zr C9 C10 177.72(8) . . . . ? C4 Zr C9 C10 -68.03(10) . . . . ? C5 Zr C9 C10 -24.22(14) . . . . ? C2 Zr C9 C10 -144.26(9) . . . . ? C3 Zr C9 C10 -105.98(9) . . . . ? C11 Zr C9 C10 37.77(8) . . . . ? C12 Zr C9 C10 78.83(9) . . . . ? C8 Zr C9 C10 116.40(12) . . . . ? C8 C9 C10 C11 0.69(16) . . . . ? Zr C9 C10 C11 -65.55(10) . . . . ? C8 C9 C10 C17 -174.02(13) . . . . ? Zr C9 C10 C17 119.74(14) . . . . ? C8 C9 C10 Zr 66.24(10) . . . . ? C7 Zr C10 C11 9.31(16) . . . . ? C6 Zr C10 C11 -42.54(11) . . . . ? C1 Zr C10 C11 108.89(15) . . . . ? C4 Zr C10 C11 -118.42(9) . . . . ? C5 Zr C10 C11 -80.46(9) . . . . ? C2 Zr C10 C11 165.81(9) . . . . ? C3 Zr C10 C11 -156.07(9) . . . . ? C12 Zr C10 C11 37.12(8) . . . . ? C9 Zr C10 C11 113.84(12) . . . . ? C8 Zr C10 C11 77.49(9) . . . . ? C7 Zr C10 C9 -104.53(14) . . . . ? C6 Zr C10 C9 -156.38(9) . . . . ? C1 Zr C10 C9 -4.95(18) . . . . ? C4 Zr C10 C9 127.75(9) . . . . ? C5 Zr C10 C9 165.70(9) . . . . ? C2 Zr C10 C9 51.97(12) . . . . ? C3 Zr C10 C9 90.09(10) . . . . ? C11 Zr C10 C9 -113.84(12) . . . . ? C12 Zr C10 C9 -76.72(9) . . . . ? C8 Zr C10 C9 -36.35(8) . . . . ? C7 Zr C10 C17 131.87(13) . . . . ? C6 Zr C10 C17 80.01(13) . . . . ? C1 Zr C10 C17 -128.56(15) . . . . ? C4 Zr C10 C17 4.14(12) . . . . ? C5 Zr C10 C17 42.10(13) . . . . ? C2 Zr C10 C17 -71.64(13) . . . . ? C3 Zr C10 C17 -33.51(13) . . . . ? C11 Zr C10 C17 122.56(15) . . . . ? C12 Zr C10 C17 159.68(13) . . . . ? C9 Zr C10 C17 -123.60(15) . . . . ? C8 Zr C10 C17 -159.96(13) . . . . ? C9 C10 C11 C12 -0.44(16) . . . . ? C17 C10 C11 C12 174.32(13) . . . . ? Zr C10 C11 C12 -66.33(10) . . . . ? C9 C10 C11 Zr 65.89(10) . . . . ? C17 C10 C11 Zr -119.36(14) . . . . ? C7 Zr C11 C10 -175.38(8) . . . . ? C6 Zr C11 C10 149.21(8) . . . . ? C1 Zr C11 C10 -138.07(10) . . . . ? C4 Zr C11 C10 76.84(10) . . . . ? C5 Zr C11 C10 112.16(9) . . . . ? C2 Zr C11 C10 -45.9(3) . . . . ? C3 Zr C11 C10 40.19(14) . . . . ? C12 Zr C11 C10 -115.31(12) . . . . ? C9 Zr C11 C10 -37.89(8) . . . . ? C8 Zr C11 C10 -78.53(9) . . . . ? C7 Zr C11 C12 -60.07(10) . . . . ? C6 Zr C11 C12 -95.48(9) . . . . ? C1 Zr C11 C12 -22.76(14) . . . . ? C4 Zr C11 C12 -167.85(9) . . . . ? C5 Zr C11 C12 -132.53(9) . . . . ? C2 Zr C11 C12 69.4(3) . . . . ? C3 Zr C11 C12 155.50(11) . . . . ? C9 Zr C11 C12 77.42(9) . . . . ? C10 Zr C11 C12 115.31(12) . . . . ? C8 Zr C11 C12 36.78(8) . . . . ? C9 C8 C12 C11 0.39(16) . . . . ? C13 C8 C12 C11 -173.91(13) . . . . ? Zr C8 C12 C11 65.85(10) . . . . ? C9 C8 C12 Zr -65.46(10) . . . . ? C13 C8 C12 Zr 120.24(14) . . . . ? C10 C11 C12 C8 0.03(16) . . . . ? Zr C11 C12 C8 -66.76(10) . . . . ? C10 C11 C12 Zr 66.79(10) . . . . ? C7 Zr C12 C8 -113.08(9) . . . . ? C6 Zr C12 C8 -149.69(9) . . . . ? C1 Zr C12 C8 -77.85(9) . . . . ? C4 Zr C12 C8 139.07(12) . . . . ? C5 Zr C12 C8 176.71(8) . . . . ? C2 Zr C12 C8 -44.41(12) . . . . ? C3 Zr C12 C8 18.3(3) . . . . ? C11 Zr C12 C8 115.51(12) . . . . ? C9 Zr C12 C8 37.63(8) . . . . ? C10 Zr C12 C8 78.53(9) . . . . ? C7 Zr C12 C11 131.41(9) . . . . ? C6 Zr C12 C11 94.81(9) . . . . ? C1 Zr C12 C11 166.64(8) . . . . ? C4 Zr C12 C11 23.56(16) . . . . ? C5 Zr C12 C11 61.21(10) . . . . ? C2 Zr C12 C11 -159.91(9) . . . . ? C3 Zr C12 C11 -97.2(3) . . . . ? C9 Zr C12 C11 -77.87(9) . . . . ? C10 Zr C12 C11 -36.98(8) . . . . ? C8 Zr C12 C11 -115.51(12) . . . . ? C12 C8 C13 C16 -27.4(2) . . . . ? C9 C8 C13 C16 159.48(14) . . . . ? Zr C8 C13 C16 65.65(16) . . . . ? C12 C8 C13 C14 -148.82(15) . . . . ? C9 C8 C13 C14 38.0(2) . . . . ? Zr C8 C13 C14 -55.82(16) . . . . ? C12 C8 C13 C15 92.00(18) . . . . ? C9 C8 C13 C15 -81.16(18) . . . . ? Zr C8 C13 C15 -174.99(11) . . . . ? C11 C10 C17 C18 154.69(14) . . . . ? C9 C10 C17 C18 -31.6(2) . . . . ? Zr C10 C17 C18 62.12(15) . . . . ? C11 C10 C17 C20 34.12(19) . . . . ? C9 C10 C17 C20 -152.19(14) . . . . ? Zr C10 C17 C20 -58.46(15) . . . . ? C11 C10 C17 C19 -85.03(17) . . . . ? C9 C10 C17 C19 88.66(17) . . . . ? Zr C10 C17 C19 -177.61(10) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.400 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.058 _iucr_refine_instructions ; TITL andyg39 in P2(1)/c CELL 1.54184 14.3641 9.9629 12.1930 90.000 91.555 90.000 ZERR 4.00 0.0002 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H ZR UNIT 80 112 4 SIZE 0.14 0.10 0.08 TEMP -173 ACTA 145 CONF FMAP 2 PLAN 10 L.S. 4 OMIT 15 0 8 OMIT 5 0 0 OMIT 4 2 1 OMIT 0 2 1 WGHT 0.027800 1.134800 FVAR 5.45048 ZR 3 0.813186 0.584686 0.173838 11.00000 0.01123 0.01376 = 0.01566 -0.00071 -0.00124 -0.00137 C1 1 0.829566 0.785503 0.271674 11.00000 0.01980 0.02005 = 0.02853 -0.00879 -0.00032 -0.00067 H1 2 0.785038 0.845194 0.288930 11.00000 0.03028 C2 1 0.843456 0.678323 0.347538 11.00000 0.02253 0.03435 = 0.01732 -0.00607 0.00090 -0.00537 H2 2 0.803282 0.680907 0.408056 11.00000 0.03866 C3 1 0.901128 0.563467 0.337990 11.00000 0.02674 0.02911 = 0.02150 0.00736 -0.00855 -0.00584 H3 2 0.896729 0.503950 0.393550 11.00000 0.03134 C4 1 0.959118 0.526614 0.250264 11.00000 0.01903 0.02080 = 0.03182 0.00060 -0.00983 0.00279 H4 2 0.987196 0.445584 0.256763 11.00000 0.03064 C5 1 0.974365 0.596240 0.150135 11.00000 0.01154 0.02954 = 0.02633 -0.00525 0.00086 0.00036 H5 2 1.010767 0.550932 0.101355 11.00000 0.03102 C6 1 0.934225 0.719337 0.113001 11.00000 0.01617 0.02721 = 0.02109 0.00295 0.00123 -0.00677 H6 2 0.946604 0.742418 0.043398 11.00000 0.02628 C7 1 0.869405 0.803044 0.166771 11.00000 0.01826 0.01601 = 0.02839 0.00229 -0.00360 -0.00400 H7 2 0.847058 0.873294 0.124496 11.00000 0.03328 C8 1 0.641767 0.567645 0.123887 11.00000 0.01113 0.01558 = 0.01818 -0.00206 -0.00102 -0.00100 C9 1 0.669469 0.441633 0.169069 11.00000 0.01230 0.01486 = 0.01599 -0.00042 0.00233 -0.00173 H9 2 0.646430 0.408177 0.235947 11.00000 0.01735 C10 1 0.733695 0.378089 0.098287 11.00000 0.01253 0.01409 = 0.01627 -0.00158 0.00057 -0.00107 C11 1 0.746302 0.467354 0.009116 11.00000 0.01294 0.01684 = 0.01424 -0.00147 0.00039 -0.00096 H11 2 0.786105 0.451544 -0.050055 11.00000 0.01688 C12 1 0.690227 0.582841 0.024766 11.00000 0.01499 0.01560 = 0.01508 0.00076 -0.00110 -0.00002 H12 2 0.683822 0.655894 -0.022924 11.00000 0.01840 C13 1 0.567302 0.661531 0.166802 11.00000 0.01383 0.01735 = 0.02097 -0.00272 0.00106 0.00255 C14 1 0.568854 0.663450 0.292705 11.00000 0.02005 0.02320 = 0.02279 -0.00437 0.00480 0.00129 AFIX 137 H14A 2 0.557236 0.572742 0.320252 11.00000 -1.50000 H14B 2 0.520407 0.724344 0.318161 11.00000 -1.50000 H14C 2 0.629910 0.694489 0.320093 11.00000 -1.50000 AFIX 0 C15 1 0.471845 0.609576 0.125297 11.00000 0.01301 0.03391 = 0.03559 -0.01108 -0.00098 0.00492 AFIX 137 H15A 2 0.469548 0.609949 0.044895 11.00000 -1.50000 H15B 2 0.422643 0.667824 0.152662 11.00000 -1.50000 H15C 2 0.462534 0.517856 0.151891 11.00000 -1.50000 AFIX 0 C16 1 0.580986 0.804827 0.124658 11.00000 0.02972 0.01913 = 0.03178 0.00048 0.00557 0.00788 AFIX 137 H16A 2 0.641780 0.838602 0.150538 11.00000 -1.50000 H16B 2 0.531682 0.862753 0.152212 11.00000 -1.50000 H16C 2 0.578253 0.804805 0.044261 11.00000 -1.50000 AFIX 0 C17 1 0.773827 0.237032 0.109890 11.00000 0.01576 0.01420 = 0.01885 -0.00020 0.00258 0.00059 C18 1 0.783830 0.196003 0.230668 11.00000 0.03022 0.02138 = 0.02209 0.00587 0.00662 0.00770 AFIX 137 H18A 2 0.823728 0.260797 0.270015 11.00000 -1.50000 H18B 2 0.811899 0.106500 0.235912 11.00000 -1.50000 H18C 2 0.722266 0.194456 0.263371 11.00000 -1.50000 AFIX 0 C19 1 0.706836 0.140279 0.048834 11.00000 0.02315 0.01558 = 0.04056 -0.00367 -0.00248 -0.00129 AFIX 137 H19A 2 0.645422 0.144407 0.081768 11.00000 -1.50000 H19B 2 0.731134 0.048550 0.054450 11.00000 -1.50000 H19C 2 0.701313 0.166296 -0.028581 11.00000 -1.50000 AFIX 0 C20 1 0.869961 0.228426 0.058673 11.00000 0.01799 0.01872 = 0.02327 -0.00128 0.00453 0.00385 AFIX 137 H20A 2 0.864512 0.251464 -0.019376 11.00000 -1.50000 H20B 2 0.894228 0.136914 0.066670 11.00000 -1.50000 H20C 2 0.912586 0.291398 0.095989 11.00000 -1.50000 HKLF 4 ; #============================================================================= # end of cif data for "andyg39" (compound 2) #============================================================================= #============================================================================= # cif data for "andyg32" (compound 3) #============================================================================= data_andyg32 _database_code_depnum_ccdc_archive 'CCDC 853654' #TrackingRef '- BulkyCp-final-121111.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Zr' _chemical_formula_weight 415.75 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 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 10.0111(2) _cell_length_b 21.1152(4) _cell_length_c 10.1725(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.199(2) _cell_angle_gamma 90.00 _cell_volume 2116.35(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 28841 _cell_measurement_theta_min 2.2468 _cell_measurement_theta_max 29.2617 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94880 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87658 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5041 _reflns_number_gt 3857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogens of the seven-membered ring and of the C10 and c12 atoms were refined freely. The methyls were refined using a rigid model. ; _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^)+(0.0214P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5041 _refine_ls_number_parameters 271 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0421 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.770949(12) 0.164940(6) 0.297824(13) 0.01284(4) Uani 1 1 d . . . C1 C 0.89448(15) 0.19920(7) 0.50370(16) 0.0237(3) Uani 1 1 d D . . H1 H 0.9035(14) 0.1795(6) 0.5826(12) 0.025(4) Uiso 1 1 d D . . C2 C 0.98939(14) 0.17934(6) 0.42389(15) 0.0193(3) Uani 1 1 d D . . H2 H 1.0486(13) 0.1493(6) 0.4630(14) 0.023(4) Uiso 1 1 d D . . C3 C 0.99504(14) 0.19484(6) 0.28977(15) 0.0178(3) Uani 1 1 d D . . H3 H 1.0593(12) 0.1728(6) 0.2533(13) 0.014(4) Uiso 1 1 d D . . C4 C 0.90684(14) 0.23477(6) 0.20063(15) 0.0193(3) Uani 1 1 d D . . H4 H 0.9231(14) 0.2357(6) 0.1161(12) 0.021(4) Uiso 1 1 d D . . C5 C 0.79199(15) 0.26905(7) 0.22500(16) 0.0232(3) Uani 1 1 d D . . H5 H 0.7403(13) 0.2875(6) 0.1510(13) 0.026(4) Uiso 1 1 d D . . C6 C 0.73697(15) 0.27195(7) 0.34413(18) 0.0262(4) Uani 1 1 d D . . H6 H 0.6564(12) 0.2910(6) 0.3406(16) 0.030(4) Uiso 1 1 d D . . C7 C 0.78168(16) 0.24098(7) 0.46787(17) 0.0258(4) Uani 1 1 d D . . H7 H 0.7250(14) 0.2455(7) 0.5290(14) 0.028(4) Uiso 1 1 d D . . C8 C 0.72650(12) 0.05142(5) 0.21475(13) 0.0114(3) Uani 1 1 d . . . C9 C 0.66478(12) 0.09328(6) 0.10834(13) 0.0109(3) Uani 1 1 d . . . C10 C 0.55828(12) 0.12600(6) 0.15712(13) 0.0115(3) Uani 1 1 d D . . H10 H 0.5028(12) 0.1551(5) 0.1062(12) 0.009(3) Uiso 1 1 d D . . C11 C 0.55128(12) 0.10683(6) 0.28843(13) 0.0113(3) Uani 1 1 d . . . C12 C 0.65591(13) 0.06160(6) 0.32290(14) 0.0115(3) Uani 1 1 d D . . H12 H 0.6735(12) 0.0416(6) 0.4020(11) 0.011(3) Uiso 1 1 d D . . C13 C 0.83811(12) -0.00023(6) 0.22391(13) 0.0144(3) Uani 1 1 d . . . C14 C 0.98177(13) 0.02756(6) 0.23516(15) 0.0188(3) Uani 1 1 d . . . H14A H 1.0477 -0.0070 0.2388 0.023 Uiso 1 1 calc R . . H14B H 1.0031 0.0531 0.3166 0.023 Uiso 1 1 calc R . . H14C H 0.9860 0.0543 0.1572 0.023 Uiso 1 1 calc R . . C15 C 0.83993(15) -0.04031(7) 0.35034(15) 0.0238(3) Uani 1 1 d . . . H15A H 0.7509 -0.0601 0.3475 0.029 Uiso 1 1 calc R . . H15B H 0.8607 -0.0131 0.4294 0.029 Uiso 1 1 calc R . . H15C H 0.9094 -0.0733 0.3548 0.029 Uiso 1 1 calc R . . C16 C 0.81107(14) -0.04707(6) 0.10597(15) 0.0206(3) Uani 1 1 d . . . H16A H 0.8175 -0.0247 0.0229 0.025 Uiso 1 1 calc R . . H16B H 0.7200 -0.0651 0.0997 0.025 Uiso 1 1 calc R . . H16C H 0.8786 -0.0811 0.1203 0.025 Uiso 1 1 calc R . . C17 C 0.68204(13) 0.10169(6) -0.03787(13) 0.0144(3) Uani 1 1 d . . . C18 C 0.82920(13) 0.09979(6) -0.06093(14) 0.0203(3) Uani 1 1 d . . . H18A H 0.8693 0.0586 -0.0327 0.024 Uiso 1 1 calc R . . H18B H 0.8814 0.1334 -0.0088 0.024 Uiso 1 1 calc R . . H18C H 0.8310 0.1062 -0.1560 0.024 Uiso 1 1 calc R . . C19 C 0.59750(14) 0.05064(6) -0.12279(14) 0.0222(3) Uani 1 1 d . . . H19A H 0.6049 0.0563 -0.2169 0.027 Uiso 1 1 calc R . . H19B H 0.5022 0.0545 -0.1129 0.027 Uiso 1 1 calc R . . H19C H 0.6315 0.0086 -0.0928 0.027 Uiso 1 1 calc R . . C20 C 0.62495(13) 0.16614(6) -0.09175(14) 0.0191(3) Uani 1 1 d . . . H20A H 0.6703 0.2001 -0.0351 0.023 Uiso 1 1 calc R . . H20B H 0.5272 0.1676 -0.0912 0.023 Uiso 1 1 calc R . . H20C H 0.6409 0.1718 -0.1833 0.023 Uiso 1 1 calc R . . C21 C 0.44355(13) 0.12496(6) 0.37043(13) 0.0142(3) Uani 1 1 d . . . C22 C 0.49742(14) 0.11654(6) 0.52002(13) 0.0195(3) Uani 1 1 d . . . H22A H 0.5174 0.0717 0.5392 0.023 Uiso 1 1 calc R . . H22B H 0.4289 0.1310 0.5710 0.023 Uiso 1 1 calc R . . H22C H 0.5805 0.1415 0.5455 0.023 Uiso 1 1 calc R . . C23 C 0.32073(13) 0.08102(6) 0.33041(15) 0.0211(3) Uani 1 1 d . . . H23A H 0.2842 0.0864 0.2351 0.025 Uiso 1 1 calc R . . H23B H 0.2506 0.0917 0.3828 0.025 Uiso 1 1 calc R . . H23C H 0.3491 0.0369 0.3477 0.025 Uiso 1 1 calc R . . C24 C 0.39629(14) 0.19343(6) 0.34302(14) 0.0192(3) Uani 1 1 d . . . H24A H 0.4719 0.2223 0.3739 0.023 Uiso 1 1 calc R . . H24B H 0.3216 0.2025 0.3907 0.023 Uiso 1 1 calc R . . H24C H 0.3651 0.1992 0.2469 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01349(6) 0.01060(6) 0.01375(7) -0.00148(6) 0.00056(4) -0.00233(6) C1 0.0299(9) 0.0229(8) 0.0163(9) -0.0027(7) -0.0014(7) -0.0093(6) C2 0.0191(7) 0.0136(7) 0.0216(8) 0.0016(6) -0.0065(6) -0.0027(5) C3 0.0153(7) 0.0142(7) 0.0233(8) -0.0016(6) 0.0022(6) -0.0044(6) C4 0.0233(8) 0.0160(7) 0.0181(8) 0.0027(6) 0.0022(6) -0.0072(6) C5 0.0236(8) 0.0132(7) 0.0290(10) 0.0040(7) -0.0058(7) -0.0023(6) C6 0.0195(8) 0.0134(8) 0.0449(11) -0.0079(7) 0.0039(7) -0.0003(6) C7 0.0291(9) 0.0223(8) 0.0282(10) -0.0145(7) 0.0108(7) -0.0075(6) C8 0.0109(6) 0.0094(6) 0.0139(7) -0.0009(5) 0.0025(5) -0.0016(5) C9 0.0119(6) 0.0103(6) 0.0107(7) -0.0014(5) 0.0021(5) -0.0015(5) C10 0.0112(6) 0.0114(7) 0.0108(7) -0.0008(5) -0.0009(5) 0.0005(5) C11 0.0112(6) 0.0113(6) 0.0114(7) -0.0025(5) 0.0019(5) -0.0024(5) C12 0.0137(6) 0.0103(6) 0.0105(7) 0.0021(5) 0.0015(5) -0.0010(5) C13 0.0155(7) 0.0120(6) 0.0164(7) 0.0020(6) 0.0051(5) 0.0027(5) C14 0.0144(7) 0.0174(7) 0.0241(9) -0.0008(6) 0.0022(6) 0.0035(5) C15 0.0253(8) 0.0205(8) 0.0274(9) 0.0095(6) 0.0094(7) 0.0111(6) C16 0.0210(7) 0.0124(7) 0.0283(9) -0.0034(6) 0.0040(6) 0.0031(6) C17 0.0178(7) 0.0143(7) 0.0116(7) -0.0007(5) 0.0034(5) 0.0022(5) C18 0.0243(8) 0.0218(7) 0.0174(8) 0.0040(6) 0.0104(6) 0.0051(6) C19 0.0297(8) 0.0227(8) 0.0128(8) -0.0038(6) -0.0002(6) 0.0016(6) C20 0.0238(7) 0.0202(7) 0.0138(7) 0.0034(6) 0.0049(6) 0.0056(6) C21 0.0130(6) 0.0156(7) 0.0146(7) -0.0014(6) 0.0041(5) 0.0009(5) C22 0.0207(7) 0.0231(7) 0.0158(8) -0.0007(6) 0.0062(6) 0.0037(6) C23 0.0152(7) 0.0261(8) 0.0240(8) -0.0058(6) 0.0084(6) -0.0009(6) C24 0.0197(7) 0.0200(7) 0.0198(8) 0.0003(6) 0.0085(6) 0.0047(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_2 _geom_bond_publ_flag Zr C4 2.3407(14) . ? Zr C5 2.3411(14) . ? Zr C6 2.3452(14) . ? Zr C3 2.3459(13) . ? Zr C7 2.3486(15) . ? Zr C1 2.3498(15) . ? Zr C2 2.3508(13) . ? Zr C10 2.4856(12) . ? Zr C12 2.5013(12) . ? Zr C11 2.5054(12) . ? Zr C9 2.5316(12) . ? Zr C8 2.5542(12) . ? C1 C2 1.418(2) . ? C1 C7 1.428(2) . ? C2 C3 1.414(2) . ? C3 C4 1.4245(19) . ? C4 C5 1.417(2) . ? C5 C6 1.418(2) . ? C6 C7 1.419(2) . ? C8 C12 1.4252(18) . ? C8 C9 1.4483(17) . ? C8 C13 1.5523(17) . ? C9 C10 1.4310(17) . ? C9 C17 1.5377(18) . ? C10 C11 1.4093(18) . ? C11 C12 1.4149(17) . ? C11 C21 1.5245(17) . ? C13 C15 1.5370(18) . ? C13 C14 1.5386(18) . ? C13 C16 1.5413(18) . ? C17 C18 1.5328(18) . ? C17 C19 1.5381(18) . ? C17 C20 1.5388(17) . ? C21 C24 1.5313(18) . ? C21 C22 1.5322(19) . ? C21 C23 1.5365(18) . ? 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 C4 Zr C5 35.24(5) . . ? C4 Zr C6 66.03(5) . . ? C5 Zr C6 35.24(5) . . ? C4 Zr C3 35.39(5) . . ? C5 Zr C3 66.18(5) . . ? C6 Zr C3 85.49(5) . . ? C4 Zr C7 85.77(5) . . ? C5 Zr C7 66.18(6) . . ? C6 Zr C7 35.19(6) . . ? C3 Zr C7 85.55(5) . . ? C4 Zr C1 85.93(5) . . ? C5 Zr C1 86.00(5) . . ? C6 Zr C1 66.21(6) . . ? C3 Zr C1 65.96(5) . . ? C7 Zr C1 35.40(5) . . ? C4 Zr C2 66.10(5) . . ? C5 Zr C2 85.64(5) . . ? C6 Zr C2 85.40(5) . . ? C3 Zr C2 35.04(5) . . ? C7 Zr C2 65.98(5) . . ? C1 Zr C2 35.12(5) . . ? C4 Zr C10 117.89(5) . . ? C5 Zr C10 104.14(5) . . ? C6 Zr C10 107.13(5) . . ? C3 Zr C10 142.73(5) . . ? C7 Zr C10 124.97(5) . . ? C1 Zr C10 151.28(5) . . ? C2 Zr C10 167.46(4) . . ? C4 Zr C12 154.84(5) . . ? C5 Zr C12 156.96(5) . . ? C6 Zr C12 137.24(5) . . ? C3 Zr C12 134.33(4) . . ? C7 Zr C12 118.89(5) . . ? C1 Zr C12 110.91(5) . . ? C2 Zr C12 117.25(4) . . ? C10 Zr C12 53.65(4) . . ? C4 Zr C11 149.81(5) . . ? C5 Zr C11 125.13(5) . . ? C6 Zr C11 108.79(5) . . ? C3 Zr C11 165.67(4) . . ? C7 Zr C11 106.76(5) . . ? C1 Zr C11 120.31(5) . . ? C2 Zr C11 144.06(5) . . ? C10 Zr C11 32.80(4) . . ? C12 Zr C11 32.83(4) . . ? C4 Zr C9 104.59(5) . . ? C5 Zr C9 111.69(5) . . ? C6 Zr C9 132.26(5) . . ? C3 Zr C9 114.17(5) . . ? C7 Zr C9 158.08(5) . . ? C1 Zr C9 161.14(5) . . ? C2 Zr C9 135.83(4) . . ? C10 Zr C9 33.13(4) . . ? C12 Zr C9 54.37(4) . . ? C11 Zr C9 55.31(4) . . ? C4 Zr C8 122.11(5) . . ? C5 Zr C8 142.81(5) . . ? C6 Zr C8 161.37(5) . . ? C3 Zr C8 110.65(4) . . ? C7 Zr C8 150.20(5) . . ? C1 Zr C8 128.11(5) . . ? C2 Zr C8 113.12(4) . . ? C10 Zr C8 54.39(4) . . ? C12 Zr C8 32.73(4) . . ? C11 Zr C8 55.07(4) . . ? C9 Zr C8 33.09(4) . . ? C2 C1 C7 128.03(15) . . ? C2 C1 Zr 72.48(8) . . ? C7 C1 Zr 72.25(8) . . ? C3 C2 C1 129.00(13) . . ? C3 C2 Zr 72.29(8) . . ? C1 C2 Zr 72.40(8) . . ? C2 C3 C4 128.68(14) . . ? C2 C3 Zr 72.67(8) . . ? C4 C3 Zr 72.11(8) . . ? C5 C4 C3 128.43(14) . . ? C5 C4 Zr 72.40(8) . . ? C3 C4 Zr 72.50(8) . . ? C4 C5 C6 128.42(14) . . ? C4 C5 Zr 72.36(8) . . ? C6 C5 Zr 72.54(8) . . ? C5 C6 C7 128.96(14) . . ? C5 C6 Zr 72.22(8) . . ? C7 C6 Zr 72.53(8) . . ? C6 C7 C1 128.46(15) . . ? C6 C7 Zr 72.28(9) . . ? C1 C7 Zr 72.35(8) . . ? C12 C8 C9 106.30(11) . . ? C12 C8 C13 120.64(11) . . ? C9 C8 C13 132.91(12) . . ? C12 C8 Zr 71.59(7) . . ? C9 C8 Zr 72.60(7) . . ? C13 C8 Zr 123.92(8) . . ? C10 C9 C8 106.32(11) . . ? C10 C9 C17 119.85(11) . . ? C8 C9 C17 133.42(11) . . ? C10 C9 Zr 71.67(7) . . ? C8 C9 Zr 74.31(7) . . ? C17 C9 Zr 124.29(8) . . ? C11 C10 C9 110.80(11) . . ? C11 C10 Zr 74.37(7) . . ? C9 C10 Zr 75.20(7) . . ? C10 C11 C12 105.65(11) . . ? C10 C11 C21 127.25(11) . . ? C12 C11 C21 126.75(12) . . ? C10 C11 Zr 72.83(7) . . ? C12 C11 Zr 73.43(7) . . ? C21 C11 Zr 123.88(8) . . ? C11 C12 C8 110.92(12) . . ? C11 C12 Zr 73.74(7) . . ? C8 C12 Zr 75.68(7) . . ? C15 C13 C14 105.98(11) . . ? C15 C13 C16 105.81(11) . . ? C14 C13 C16 109.61(11) . . ? C15 C13 C8 109.81(11) . . ? C14 C13 C8 112.95(10) . . ? C16 C13 C8 112.26(10) . . ? C18 C17 C9 114.87(11) . . ? C18 C17 C19 110.11(11) . . ? C9 C17 C19 108.50(10) . . ? C18 C17 C20 105.97(11) . . ? C9 C17 C20 110.40(10) . . ? C19 C17 C20 106.68(11) . . ? C11 C21 C24 111.29(11) . . ? C11 C21 C22 110.83(10) . . ? C24 C21 C22 109.48(11) . . ? C11 C21 C23 108.29(10) . . ? C24 C21 C23 108.36(10) . . ? C22 C21 C23 108.51(11) . . ? 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 C4 Zr C1 C2 -52.78(8) . . . . ? C5 Zr C1 C2 -88.11(9) . . . . ? C6 Zr C1 C2 -118.33(9) . . . . ? C3 Zr C1 C2 -22.45(8) . . . . ? C7 Zr C1 C2 -141.20(13) . . . . ? C10 Zr C1 C2 159.43(9) . . . . ? C12 Zr C1 C2 107.99(8) . . . . ? C11 Zr C1 C2 143.04(8) . . . . ? C9 Zr C1 C2 72.20(17) . . . . ? C8 Zr C1 C2 75.65(10) . . . . ? C4 Zr C1 C7 88.42(9) . . . . ? C5 Zr C1 C7 53.10(9) . . . . ? C6 Zr C1 C7 22.87(9) . . . . ? C3 Zr C1 C7 118.75(10) . . . . ? C2 Zr C1 C7 141.20(13) . . . . ? C10 Zr C1 C7 -59.37(14) . . . . ? C12 Zr C1 C7 -110.81(9) . . . . ? C11 Zr C1 C7 -75.75(10) . . . . ? C9 Zr C1 C7 -146.60(13) . . . . ? C8 Zr C1 C7 -143.15(8) . . . . ? C7 C1 C2 C3 -1.1(2) . . . . ? Zr C1 C2 C3 48.13(13) . . . . ? C7 C1 C2 Zr -49.25(14) . . . . ? C4 Zr C2 C3 -22.91(8) . . . . ? C5 Zr C2 C3 -53.35(8) . . . . ? C6 Zr C2 C3 -88.70(9) . . . . ? C7 Zr C2 C3 -119.18(9) . . . . ? C1 Zr C2 C3 -142.60(12) . . . . ? C10 Zr C2 C3 88.4(2) . . . . ? C12 Zr C2 C3 129.38(8) . . . . ? C11 Zr C2 C3 155.23(8) . . . . ? C9 Zr C2 C3 63.61(10) . . . . ? C8 Zr C2 C3 93.39(8) . . . . ? C4 Zr C2 C1 119.68(9) . . . . ? C5 Zr C2 C1 89.25(9) . . . . ? C6 Zr C2 C1 53.90(9) . . . . ? C3 Zr C2 C1 142.60(12) . . . . ? C7 Zr C2 C1 23.41(9) . . . . ? C10 Zr C2 C1 -129.0(2) . . . . ? C12 Zr C2 C1 -88.02(9) . . . . ? C11 Zr C2 C1 -62.17(11) . . . . ? C9 Zr C2 C1 -153.79(8) . . . . ? C8 Zr C2 C1 -124.02(8) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? Zr C2 C3 C4 48.53(13) . . . . ? C1 C2 C3 Zr -48.17(14) . . . . ? C4 Zr C3 C2 142.08(13) . . . . ? C5 Zr C3 C2 119.01(9) . . . . ? C6 Zr C3 C2 88.42(9) . . . . ? C7 Zr C3 C2 53.12(9) . . . . ? C1 Zr C3 C2 22.49(8) . . . . ? C10 Zr C3 C2 -158.99(8) . . . . ? C12 Zr C3 C2 -73.85(10) . . . . ? C11 Zr C3 C2 -96.6(2) . . . . ? C9 Zr C3 C2 -136.83(8) . . . . ? C8 Zr C3 C2 -101.15(8) . . . . ? C5 Zr C3 C4 -23.06(8) . . . . ? C6 Zr C3 C4 -53.66(9) . . . . ? C7 Zr C3 C4 -88.96(9) . . . . ? C1 Zr C3 C4 -119.58(9) . . . . ? C2 Zr C3 C4 -142.08(13) . . . . ? C10 Zr C3 C4 58.93(11) . . . . ? C12 Zr C3 C4 144.07(8) . . . . ? C11 Zr C3 C4 121.30(18) . . . . ? C9 Zr C3 C4 81.09(9) . . . . ? C8 Zr C3 C4 116.77(8) . . . . ? C2 C3 C4 C5 0.4(2) . . . . ? Zr C3 C4 C5 49.09(13) . . . . ? C2 C3 C4 Zr -48.73(13) . . . . ? C6 Zr C4 C5 -23.10(9) . . . . ? C3 Zr C4 C5 -141.61(13) . . . . ? C7 Zr C4 C5 -53.34(9) . . . . ? C1 Zr C4 C5 -88.83(9) . . . . ? C2 Zr C4 C5 -118.90(10) . . . . ? C10 Zr C4 C5 74.33(10) . . . . ? C12 Zr C4 C5 137.54(11) . . . . ? C11 Zr C4 C5 63.26(13) . . . . ? C9 Zr C4 C5 107.05(9) . . . . ? C8 Zr C4 C5 137.87(8) . . . . ? C5 Zr C4 C3 141.61(13) . . . . ? C6 Zr C4 C3 118.50(10) . . . . ? C7 Zr C4 C3 88.27(9) . . . . ? C1 Zr C4 C3 52.77(9) . . . . ? C2 Zr C4 C3 22.71(8) . . . . ? C10 Zr C4 C3 -144.07(8) . . . . ? C12 Zr C4 C3 -80.85(14) . . . . ? C11 Zr C4 C3 -155.13(9) . . . . ? C9 Zr C4 C3 -111.35(8) . . . . ? C8 Zr C4 C3 -80.52(9) . . . . ? C3 C4 C5 C6 0.0(2) . . . . ? Zr C4 C5 C6 49.16(14) . . . . ? C3 C4 C5 Zr -49.13(13) . . . . ? C6 Zr C5 C4 141.58(13) . . . . ? C3 Zr C5 C4 23.15(8) . . . . ? C7 Zr C5 C4 119.02(10) . . . . ? C1 Zr C5 C4 88.60(9) . . . . ? C2 Zr C5 C4 53.39(9) . . . . ? C10 Zr C5 C4 -118.65(9) . . . . ? C12 Zr C5 C4 -132.83(12) . . . . ? C11 Zr C5 C4 -146.69(8) . . . . ? C9 Zr C5 C4 -84.67(9) . . . . ? C8 Zr C5 C4 -70.04(11) . . . . ? C4 Zr C5 C6 -141.58(13) . . . . ? C3 Zr C5 C6 -118.43(10) . . . . ? C7 Zr C5 C6 -22.56(8) . . . . ? C1 Zr C5 C6 -52.98(9) . . . . ? C2 Zr C5 C6 -88.19(9) . . . . ? C10 Zr C5 C6 99.77(9) . . . . ? C12 Zr C5 C6 85.59(15) . . . . ? C11 Zr C5 C6 71.73(10) . . . . ? C9 Zr C5 C6 133.75(8) . . . . ? C8 Zr C5 C6 148.37(8) . . . . ? C4 C5 C6 C7 -0.8(3) . . . . ? Zr C5 C6 C7 48.34(15) . . . . ? C4 C5 C6 Zr -49.10(14) . . . . ? C4 Zr C6 C5 23.10(8) . . . . ? C3 Zr C6 C5 53.80(9) . . . . ? C7 Zr C6 C5 142.48(13) . . . . ? C1 Zr C6 C5 119.49(9) . . . . ? C2 Zr C6 C5 88.96(9) . . . . ? C10 Zr C6 C5 -90.39(9) . . . . ? C12 Zr C6 C5 -144.92(8) . . . . ? C11 Zr C6 C5 -124.88(8) . . . . ? C9 Zr C6 C5 -65.09(10) . . . . ? C8 Zr C6 C5 -97.05(17) . . . . ? C4 Zr C6 C7 -119.38(10) . . . . ? C5 Zr C6 C7 -142.48(13) . . . . ? C3 Zr C6 C7 -88.68(9) . . . . ? C1 Zr C6 C7 -22.99(9) . . . . ? C2 Zr C6 C7 -53.52(9) . . . . ? C10 Zr C6 C7 127.13(9) . . . . ? C12 Zr C6 C7 72.60(11) . . . . ? C11 Zr C6 C7 92.64(9) . . . . ? C9 Zr C6 C7 152.43(8) . . . . ? C8 Zr C6 C7 120.47(16) . . . . ? C5 C6 C7 C1 0.4(3) . . . . ? Zr C6 C7 C1 48.67(14) . . . . ? C5 C6 C7 Zr -48.23(15) . . . . ? C2 C1 C7 C6 0.7(2) . . . . ? Zr C1 C7 C6 -48.64(14) . . . . ? C2 C1 C7 Zr 49.34(14) . . . . ? C4 Zr C7 C6 52.98(9) . . . . ? C5 Zr C7 C6 22.59(8) . . . . ? C3 Zr C7 C6 88.48(9) . . . . ? C1 Zr C7 C6 141.90(14) . . . . ? C2 Zr C7 C6 118.66(10) . . . . ? C10 Zr C7 C6 -68.40(10) . . . . ? C12 Zr C7 C6 -132.28(9) . . . . ? C11 Zr C7 C6 -99.01(9) . . . . ? C9 Zr C7 C6 -66.56(16) . . . . ? C8 Zr C7 C6 -146.36(9) . . . . ? C4 Zr C7 C1 -88.92(9) . . . . ? C5 Zr C7 C1 -119.31(10) . . . . ? C6 Zr C7 C1 -141.90(14) . . . . ? C3 Zr C7 C1 -53.43(9) . . . . ? C2 Zr C7 C1 -23.24(9) . . . . ? C10 Zr C7 C1 149.70(8) . . . . ? C12 Zr C7 C1 85.82(9) . . . . ? C11 Zr C7 C1 119.09(9) . . . . ? C9 Zr C7 C1 151.54(12) . . . . ? C8 Zr C7 C1 71.73(13) . . . . ? C4 Zr C8 C12 -179.74(7) . . . . ? C5 Zr C8 C12 -139.93(9) . . . . ? C6 Zr C8 C12 -68.62(18) . . . . ? C3 Zr C8 C12 142.64(8) . . . . ? C7 Zr C8 C12 23.21(13) . . . . ? C1 Zr C8 C12 67.57(9) . . . . ? C2 Zr C8 C12 104.87(8) . . . . ? C10 Zr C8 C12 -76.45(8) . . . . ? C11 Zr C8 C12 -36.00(7) . . . . ? C9 Zr C8 C12 -114.47(10) . . . . ? C4 Zr C8 C9 -65.27(8) . . . . ? C5 Zr C8 C9 -25.45(11) . . . . ? C6 Zr C8 C9 45.85(19) . . . . ? C3 Zr C8 C9 -102.89(8) . . . . ? C7 Zr C8 C9 137.69(10) . . . . ? C1 Zr C8 C9 -177.96(7) . . . . ? C2 Zr C8 C9 -140.66(7) . . . . ? C10 Zr C8 C9 38.02(7) . . . . ? C12 Zr C8 C9 114.47(10) . . . . ? C11 Zr C8 C9 78.47(8) . . . . ? C4 Zr C8 C13 65.21(11) . . . . ? C5 Zr C8 C13 105.02(12) . . . . ? C6 Zr C8 C13 176.33(15) . . . . ? C3 Zr C8 C13 27.58(11) . . . . ? C7 Zr C8 C13 -91.84(13) . . . . ? C1 Zr C8 C13 -47.49(12) . . . . ? C2 Zr C8 C13 -10.19(12) . . . . ? C10 Zr C8 C13 168.49(12) . . . . ? C12 Zr C8 C13 -115.05(13) . . . . ? C11 Zr C8 C13 -151.05(12) . . . . ? C9 Zr C8 C13 130.47(14) . . . . ? C12 C8 C9 C10 -0.88(13) . . . . ? C13 C8 C9 C10 174.52(12) . . . . ? Zr C8 C9 C10 -65.00(8) . . . . ? C12 C8 C9 C17 -173.20(12) . . . . ? C13 C8 C9 C17 2.2(2) . . . . ? Zr C8 C9 C17 122.68(14) . . . . ? C12 C8 C9 Zr 64.13(8) . . . . ? C13 C8 C9 Zr -120.48(13) . . . . ? C4 Zr C9 C10 -119.05(8) . . . . ? C5 Zr C9 C10 -82.63(8) . . . . ? C6 Zr C9 C10 -48.36(10) . . . . ? C3 Zr C9 C10 -155.29(7) . . . . ? C7 Zr C9 C10 -2.76(16) . . . . ? C1 Zr C9 C10 118.58(15) . . . . ? C2 Zr C9 C10 170.39(7) . . . . ? C12 Zr C9 C10 76.35(8) . . . . ? C11 Zr C9 C10 35.91(7) . . . . ? C8 Zr C9 C10 113.61(10) . . . . ? C4 Zr C9 C8 127.35(7) . . . . ? C5 Zr C9 C8 163.77(7) . . . . ? C6 Zr C9 C8 -161.96(8) . . . . ? C3 Zr C9 C8 91.10(8) . . . . ? C7 Zr C9 C8 -116.37(14) . . . . ? C1 Zr C9 C8 4.97(18) . . . . ? C2 Zr C9 C8 56.79(10) . . . . ? C10 Zr C9 C8 -113.61(10) . . . . ? C12 Zr C9 C8 -37.26(7) . . . . ? C11 Zr C9 C8 -77.69(7) . . . . ? C4 Zr C9 C17 -4.92(11) . . . . ? C5 Zr C9 C17 31.50(11) . . . . ? C6 Zr C9 C17 65.77(12) . . . . ? C3 Zr C9 C17 -41.16(11) . . . . ? C7 Zr C9 C17 111.37(15) . . . . ? C1 Zr C9 C17 -127.29(15) . . . . ? C2 Zr C9 C17 -75.48(11) . . . . ? C10 Zr C9 C17 114.13(13) . . . . ? C12 Zr C9 C17 -169.53(11) . . . . ? C11 Zr C9 C17 150.04(11) . . . . ? C8 Zr C9 C17 -132.27(13) . . . . ? C8 C9 C10 C11 0.30(14) . . . . ? C17 C9 C10 C11 173.87(11) . . . . ? Zr C9 C10 C11 -66.52(9) . . . . ? C8 C9 C10 Zr 66.81(8) . . . . ? C17 C9 C10 Zr -119.62(10) . . . . ? C4 Zr C10 C11 -169.74(7) . . . . ? C5 Zr C10 C11 -134.78(8) . . . . ? C6 Zr C10 C11 -98.27(8) . . . . ? C3 Zr C10 C11 156.12(8) . . . . ? C7 Zr C10 C11 -64.17(9) . . . . ? C1 Zr C10 C11 -26.71(13) . . . . ? C2 Zr C10 C11 84.7(2) . . . . ? C12 Zr C10 C11 38.38(7) . . . . ? C9 Zr C10 C11 117.09(11) . . . . ? C8 Zr C10 C11 79.12(8) . . . . ? C4 Zr C10 C9 73.18(8) . . . . ? C5 Zr C10 C9 108.13(8) . . . . ? C6 Zr C10 C9 144.64(8) . . . . ? C3 Zr C10 C9 39.03(11) . . . . ? C7 Zr C10 C9 178.74(8) . . . . ? C1 Zr C10 C9 -143.79(10) . . . . ? C2 Zr C10 C9 -32.4(3) . . . . ? C12 Zr C10 C9 -78.71(8) . . . . ? C11 Zr C10 C9 -117.09(11) . . . . ? C8 Zr C10 C9 -37.97(7) . . . . ? C9 C10 C11 C12 0.41(14) . . . . ? Zr C10 C11 C12 -66.63(8) . . . . ? C9 C10 C11 C21 -173.09(11) . . . . ? Zr C10 C11 C21 119.86(12) . . . . ? C9 C10 C11 Zr 67.05(9) . . . . ? C4 Zr C11 C10 18.25(13) . . . . ? C5 Zr C11 C10 57.30(9) . . . . ? C6 Zr C11 C10 92.66(8) . . . . ? C3 Zr C11 C10 -82.0(2) . . . . ? C7 Zr C11 C10 129.62(8) . . . . ? C1 Zr C11 C10 165.51(7) . . . . ? C2 Zr C11 C10 -158.38(8) . . . . ? C12 Zr C11 C10 -112.74(11) . . . . ? C9 Zr C11 C10 -36.28(7) . . . . ? C8 Zr C11 C10 -76.86(8) . . . . ? C4 Zr C11 C12 130.99(10) . . . . ? C5 Zr C11 C12 170.05(8) . . . . ? C6 Zr C11 C12 -154.60(8) . . . . ? C3 Zr C11 C12 30.7(2) . . . . ? C7 Zr C11 C12 -117.64(8) . . . . ? C1 Zr C11 C12 -81.74(9) . . . . ? C2 Zr C11 C12 -45.64(12) . . . . ? C10 Zr C11 C12 112.74(11) . . . . ? C9 Zr C11 C12 76.46(8) . . . . ? C8 Zr C11 C12 35.88(7) . . . . ? C4 Zr C11 C21 -105.50(13) . . . . ? C5 Zr C11 C21 -66.45(12) . . . . ? C6 Zr C11 C21 -31.09(11) . . . . ? C3 Zr C11 C21 154.22(17) . . . . ? C7 Zr C11 C21 5.87(11) . . . . ? C1 Zr C11 C21 41.77(12) . . . . ? C2 Zr C11 C21 77.87(13) . . . . ? C10 Zr C11 C21 -123.75(13) . . . . ? C12 Zr C11 C21 123.51(14) . . . . ? C9 Zr C11 C21 -160.03(12) . . . . ? C8 Zr C11 C21 159.39(12) . . . . ? C10 C11 C12 C8 -1.00(14) . . . . ? C21 C11 C12 C8 172.55(11) . . . . ? Zr C11 C12 C8 -67.21(9) . . . . ? C10 C11 C12 Zr 66.22(8) . . . . ? C21 C11 C12 Zr -120.23(12) . . . . ? C9 C8 C12 C11 1.18(14) . . . . ? C13 C8 C12 C11 -174.90(11) . . . . ? Zr C8 C12 C11 65.99(9) . . . . ? C9 C8 C12 Zr -64.81(8) . . . . ? C13 C8 C12 Zr 119.11(11) . . . . ? C4 Zr C12 C11 -116.76(11) . . . . ? C5 Zr C12 C11 -21.18(17) . . . . ? C6 Zr C12 C11 36.74(12) . . . . ? C3 Zr C12 C11 -169.82(8) . . . . ? C7 Zr C12 C11 75.65(9) . . . . ? C1 Zr C12 C11 113.86(8) . . . . ? C2 Zr C12 C11 151.84(8) . . . . ? C10 Zr C12 C11 -38.34(7) . . . . ? C9 Zr C12 C11 -79.59(8) . . . . ? C8 Zr C12 C11 -117.27(11) . . . . ? C4 Zr C12 C8 0.52(15) . . . . ? C5 Zr C12 C8 96.10(14) . . . . ? C6 Zr C12 C8 154.02(8) . . . . ? C3 Zr C12 C8 -52.55(10) . . . . ? C7 Zr C12 C8 -167.07(8) . . . . ? C1 Zr C12 C8 -128.87(8) . . . . ? C2 Zr C12 C8 -90.89(8) . . . . ? C10 Zr C12 C8 78.94(8) . . . . ? C11 Zr C12 C8 117.27(11) . . . . ? C9 Zr C12 C8 37.68(7) . . . . ? C12 C8 C13 C15 8.05(16) . . . . ? C9 C8 C13 C15 -166.82(13) . . . . ? Zr C8 C13 C15 95.53(12) . . . . ? C12 C8 C13 C14 -110.01(13) . . . . ? C9 C8 C13 C14 75.13(17) . . . . ? Zr C8 C13 C14 -22.53(15) . . . . ? C12 C8 C13 C16 125.45(13) . . . . ? C9 C8 C13 C16 -49.41(18) . . . . ? Zr C8 C13 C16 -147.07(9) . . . . ? C10 C9 C17 C18 145.92(12) . . . . ? C8 C9 C17 C18 -42.59(19) . . . . ? Zr C9 C17 C18 58.64(13) . . . . ? C10 C9 C17 C19 -90.38(13) . . . . ? C8 C9 C17 C19 81.11(16) . . . . ? Zr C9 C17 C19 -177.66(8) . . . . ? C10 C9 C17 C20 26.19(15) . . . . ? C8 C9 C17 C20 -162.32(13) . . . . ? Zr C9 C17 C20 -61.09(13) . . . . ? C10 C11 C21 C24 -36.28(17) . . . . ? C12 C11 C21 C24 151.53(12) . . . . ? Zr C11 C21 C24 57.38(13) . . . . ? C10 C11 C21 C22 -158.36(12) . . . . ? C12 C11 C21 C22 29.45(17) . . . . ? Zr C11 C21 C22 -64.71(13) . . . . ? C10 C11 C21 C23 82.72(15) . . . . ? C12 C11 C21 C23 -89.47(15) . . . . ? Zr C11 C21 C23 176.37(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.330 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.047 _iucr_refine_instructions ; TITL andyg32 in P2(1)/n CELL 0.71073 10.0111 21.1152 10.1725 90.000 100.199 90.000 ZERR 4.00 0.0002 0.0004 0.0002 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H ZR UNIT 96 144 4 SIZE 0.22 0.10 0.05 TEMP -173 SHEL 999 0.76 ACTA CONF FMAP 2 PLAN 10 L.S. 4 SADI c1 H1 C2 H2 C3 H3 C4 H4 C5 H5 C6 H6 C7 H7 C10 H10 C12 H12 OMIT 3 6 2 OMIT -1 1 4 OMIT 0 4 4 OMIT -1 1 5 OMIT 3 7 1 OMIT 4 7 2 WGHT 0.021400 FVAR 2.09313 ZR 3 0.770949 0.164940 0.297824 11.00000 0.01349 0.01060 = 0.01375 -0.00148 0.00056 -0.00233 C1 1 0.894477 0.199199 0.503702 11.00000 0.02985 0.02295 = 0.01627 -0.00275 -0.00144 -0.00926 H1 2 0.903483 0.179523 0.582572 11.00000 0.02547 C2 1 0.989388 0.179340 0.423893 11.00000 0.01909 0.01357 = 0.02158 0.00159 -0.00653 -0.00271 H2 2 1.048638 0.149309 0.463037 11.00000 0.02252 C3 1 0.995041 0.194837 0.289768 11.00000 0.01533 0.01423 = 0.02330 -0.00160 0.00218 -0.00440 H3 2 1.059308 0.172821 0.253290 11.00000 0.01389 C4 1 0.906843 0.234769 0.200627 11.00000 0.02329 0.01603 = 0.01811 0.00272 0.00222 -0.00722 H4 2 0.923097 0.235726 0.116112 11.00000 0.02077 C5 1 0.791992 0.269047 0.225003 11.00000 0.02361 0.01319 = 0.02904 0.00401 -0.00576 -0.00228 H5 2 0.740334 0.287453 0.150969 11.00000 0.02609 C6 1 0.736974 0.271953 0.344126 11.00000 0.01946 0.01341 = 0.04495 -0.00789 0.00385 -0.00028 H6 2 0.656359 0.290963 0.340586 11.00000 0.02985 C7 1 0.781680 0.240978 0.467871 11.00000 0.02912 0.02227 = 0.02820 -0.01452 0.01084 -0.00751 H7 2 0.725006 0.245512 0.529038 11.00000 0.02781 C8 1 0.726504 0.051424 0.214751 11.00000 0.01095 0.00936 = 0.01389 -0.00094 0.00248 -0.00161 C9 1 0.664783 0.093275 0.108344 11.00000 0.01189 0.01028 = 0.01068 -0.00135 0.00208 -0.00153 C10 1 0.558282 0.125998 0.157121 11.00000 0.01119 0.01139 = 0.01079 -0.00084 -0.00086 0.00053 H10 2 0.502831 0.155128 0.106235 11.00000 0.00858 C11 1 0.551275 0.106826 0.288427 11.00000 0.01116 0.01127 = 0.01135 -0.00254 0.00188 -0.00241 C12 1 0.655913 0.061603 0.322897 11.00000 0.01370 0.01026 = 0.01046 0.00210 0.00153 -0.00098 H12 2 0.673503 0.041631 0.401978 11.00000 0.01108 C13 1 0.838110 -0.000229 0.223913 11.00000 0.01551 0.01200 = 0.01636 0.00199 0.00505 0.00268 C14 1 0.981767 0.027556 0.235159 11.00000 0.01443 0.01736 = 0.02415 -0.00077 0.00222 0.00350 AFIX 137 H14A 2 1.047691 -0.006991 0.238806 11.00000 -1.20000 H14B 2 1.003073 0.053097 0.316619 11.00000 -1.20000 H14C 2 0.986037 0.054260 0.157217 11.00000 -1.20000 AFIX 0 C15 1 0.839930 -0.040313 0.350338 11.00000 0.02530 0.02054 = 0.02737 0.00949 0.00942 0.01109 AFIX 137 H15A 2 0.750868 -0.060059 0.347459 11.00000 -1.20000 H15B 2 0.860680 -0.013119 0.429392 11.00000 -1.20000 H15C 2 0.909404 -0.073321 0.354775 11.00000 -1.20000 AFIX 0 C16 1 0.811068 -0.047066 0.105973 11.00000 0.02104 0.01241 = 0.02830 -0.00338 0.00402 0.00310 AFIX 137 H16A 2 0.817462 -0.024728 0.022869 11.00000 -1.20000 H16B 2 0.719977 -0.065120 0.099713 11.00000 -1.20000 H16C 2 0.878570 -0.081130 0.120349 11.00000 -1.20000 AFIX 0 C17 1 0.682038 0.101694 -0.037868 11.00000 0.01776 0.01426 = 0.01158 -0.00072 0.00337 0.00223 C18 1 0.829203 0.099789 -0.060926 11.00000 0.02431 0.02176 = 0.01741 0.00403 0.01043 0.00514 AFIX 137 H18A 2 0.869301 0.058570 -0.032674 11.00000 -1.20000 H18B 2 0.881422 0.133419 -0.008817 11.00000 -1.20000 H18C 2 0.830973 0.106160 -0.156028 11.00000 -1.20000 AFIX 0 C19 1 0.597500 0.050644 -0.122793 11.00000 0.02969 0.02268 = 0.01283 -0.00382 -0.00020 0.00160 AFIX 137 H19A 2 0.604883 0.056334 -0.216850 11.00000 -1.20000 H19B 2 0.502227 0.054463 -0.112887 11.00000 -1.20000 H19C 2 0.631524 0.008607 -0.092754 11.00000 -1.20000 AFIX 0 C20 1 0.624951 0.166144 -0.091748 11.00000 0.02385 0.02017 = 0.01384 0.00340 0.00489 0.00557 AFIX 137 H20A 2 0.670347 0.200107 -0.035076 11.00000 -1.20000 H20B 2 0.527215 0.167576 -0.091159 11.00000 -1.20000 H20C 2 0.640938 0.171793 -0.183323 11.00000 -1.20000 AFIX 0 C21 1 0.443547 0.124956 0.370428 11.00000 0.01302 0.01564 = 0.01464 -0.00144 0.00414 0.00095 C22 1 0.497423 0.116538 0.520023 11.00000 0.02068 0.02306 = 0.01582 -0.00066 0.00621 0.00372 AFIX 137 H22A 2 0.517354 0.071703 0.539212 11.00000 -1.20000 H22B 2 0.428858 0.131039 0.571041 11.00000 -1.20000 H22C 2 0.580517 0.141491 0.545500 11.00000 -1.20000 AFIX 0 C23 1 0.320733 0.081016 0.330410 11.00000 0.01519 0.02607 = 0.02397 -0.00577 0.00836 -0.00089 AFIX 137 H23A 2 0.284166 0.086391 0.235144 11.00000 -1.20000 H23B 2 0.250630 0.091704 0.382835 11.00000 -1.20000 H23C 2 0.349073 0.036930 0.347729 11.00000 -1.20000 AFIX 0 C24 1 0.396293 0.193425 0.343019 11.00000 0.01968 0.02001 = 0.01976 0.00034 0.00845 0.00466 AFIX 137 H24A 2 0.471930 0.222330 0.373924 11.00000 -1.20000 H24B 2 0.321560 0.202526 0.390697 11.00000 -1.20000 H24C 2 0.365148 0.199237 0.246897 11.00000 -1.20000 HKLF 4 ; #============================================================================= # end of cif data for "andyg32" (compound 3) #============================================================================= #============================================================================= # cif data for "andyg99" (compound 4) #============================================================================= data_andyg99 _database_code_depnum_ccdc_archive 'CCDC 853655' #TrackingRef '- BulkyCp-final-121111.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Zr' _chemical_formula_weight 415.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0646(6) _cell_length_b 8.6396(4) _cell_length_c 16.4412(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.047(4) _cell_angle_gamma 90.00 _cell_volume 2139.86(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7590 _cell_measurement_theta_min 3.9750 _cell_measurement_theta_max 62.5859 _exptl_crystal_description needle _exptl_crystal_colour violet _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 4.202 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.4079 _exptl_absorpt_correction_T_max 0.8843 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1399 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14356 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.98 _diffrn_reflns_theta_max 62.68 _reflns_number_total 3422 _reflns_number_gt 3123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was refined as a pseudomerohedral twin (by 180 degree rotation around the a axis. The hydrogens of the seven-membered ring and of the C12 atom were refined freely. The methyls were refined using a rigid model, others riding. ; _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^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3422 _refine_ls_number_parameters 267 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.82672(2) 0.17972(3) 0.19683(2) 0.02731(12) Uani 1 1 d . . . C1 C 0.9359(3) 0.0842(5) 0.1091(3) 0.0403(10) Uani 1 1 d D . . H1 H 0.950(3) 0.100(6) 0.0561(16) 0.055(15) Uiso 1 1 d D . . C2 C 0.8726(3) -0.0355(5) 0.1208(3) 0.0392(10) Uani 1 1 d D . . H2 H 0.849(3) -0.065(5) 0.0723(18) 0.043(13) Uiso 1 1 d D . . C3 C 0.8371(3) -0.0918(4) 0.1951(3) 0.0394(9) Uani 1 1 d D . . H3 H 0.788(2) -0.151(5) 0.191(3) 0.042(12) Uiso 1 1 d D . . C4 C 0.8563(3) -0.0410(5) 0.2753(3) 0.0386(10) Uani 1 1 d D . . H4 H 0.822(2) -0.080(4) 0.3158(18) 0.028(10) Uiso 1 1 d D . . C5 C 0.9144(3) 0.0767(5) 0.3016(3) 0.0431(10) Uani 1 1 d D . . H5 H 0.920(3) 0.088(6) 0.3560(14) 0.049(14) Uiso 1 1 d D . . C6 C 0.9686(3) 0.1750(5) 0.2539(3) 0.0420(11) Uani 1 1 d D . . H6 H 0.993(4) 0.259(5) 0.279(3) 0.071(18) Uiso 1 1 d D . . C7 C 0.9777(3) 0.1784(5) 0.1681(3) 0.0420(11) Uani 1 1 d D . . H7 H 1.010(3) 0.257(4) 0.147(3) 0.048(14) Uiso 1 1 d D . . C8 C 0.7583(2) 0.4003(4) 0.1190(2) 0.0257(8) Uani 1 1 d . . . C9 C 0.6884(2) 0.2913(4) 0.1317(2) 0.0258(8) Uani 1 1 d . . . C10 C 0.6706(3) 0.2841(4) 0.2174(2) 0.0251(7) Uani 1 1 d . . . C11 C 0.7302(3) 0.3890(4) 0.2568(2) 0.0258(8) Uani 1 1 d . . . C12 C 0.7843(3) 0.4571(4) 0.1958(2) 0.0265(7) Uani 1 1 d D . . H12 H 0.827(2) 0.533(4) 0.203(2) 0.021(8) Uiso 1 1 d D . . C13 C 0.7918(3) 0.4615(4) 0.0379(2) 0.0308(9) Uani 1 1 d . . . H13 H 0.7892 0.3755 -0.0027 0.037 Uiso 1 1 calc R . . C14 C 0.7295(3) 0.5913(5) 0.0093(3) 0.0408(10) Uani 1 1 d . . . H14A H 0.7288 0.6744 0.0499 0.061 Uiso 1 1 calc R . . H14B H 0.6694 0.5500 0.0025 0.061 Uiso 1 1 calc R . . H14C H 0.7507 0.6324 -0.0427 0.061 Uiso 1 1 calc R . . C15 C 0.8861(3) 0.5207(5) 0.0416(3) 0.0399(10) Uani 1 1 d . . . H15A H 0.8898 0.6057 0.0809 0.060 Uiso 1 1 calc R . . H15B H 0.9038 0.5581 -0.0123 0.060 Uiso 1 1 calc R . . H15C H 0.9257 0.4367 0.0585 0.060 Uiso 1 1 calc R . . C16 C 0.6356(3) 0.2178(4) 0.0629(2) 0.0292(8) Uani 1 1 d . . . H16 H 0.6670 0.2463 0.0115 0.035 Uiso 1 1 calc R . . C17 C 0.5423(3) 0.2874(5) 0.0563(3) 0.0389(10) Uani 1 1 d . . . H17A H 0.5063 0.2529 0.1025 0.058 Uiso 1 1 calc R . . H17B H 0.5145 0.2532 0.0054 0.058 Uiso 1 1 calc R . . H17C H 0.5463 0.4006 0.0567 0.058 Uiso 1 1 calc R . . C18 C 0.6308(3) 0.0400(5) 0.0640(3) 0.0371(10) Uani 1 1 d . . . H18A H 0.6910 -0.0028 0.0626 0.056 Uiso 1 1 calc R . . H18B H 0.5975 0.0038 0.0164 0.056 Uiso 1 1 calc R . . H18C H 0.6008 0.0057 0.1137 0.056 Uiso 1 1 calc R . . C19 C 0.5963(3) 0.1927(4) 0.2578(2) 0.0292(8) Uani 1 1 d . . . H19 H 0.5666 0.1318 0.2138 0.035 Uiso 1 1 calc R . . C20 C 0.5251(3) 0.2976(5) 0.2945(3) 0.0384(9) Uani 1 1 d . . . H20A H 0.4738 0.2350 0.3107 0.058 Uiso 1 1 calc R . . H20B H 0.5066 0.3744 0.2541 0.058 Uiso 1 1 calc R . . H20C H 0.5494 0.3507 0.3423 0.058 Uiso 1 1 calc R . . C21 C 0.6285(3) 0.0754(5) 0.3211(3) 0.0362(10) Uani 1 1 d . . . H21A H 0.6609 -0.0080 0.2938 0.054 Uiso 1 1 calc R . . H21B H 0.5773 0.0320 0.3500 0.054 Uiso 1 1 calc R . . H21C H 0.6678 0.1271 0.3601 0.054 Uiso 1 1 calc R . . C22 C 0.7280(3) 0.4463(5) 0.3441(2) 0.0332(9) Uani 1 1 d . . . H22 H 0.6922 0.3718 0.3771 0.040 Uiso 1 1 calc R . . C23 C 0.6813(4) 0.6040(5) 0.3457(3) 0.0430(10) Uani 1 1 d . . . H23A H 0.7172 0.6800 0.3162 0.065 Uiso 1 1 calc R . . H23B H 0.6739 0.6378 0.4022 0.065 Uiso 1 1 calc R . . H23C H 0.6229 0.5949 0.3198 0.065 Uiso 1 1 calc R . . C24 C 0.8201(3) 0.4595(6) 0.3824(3) 0.0494(11) Uani 1 1 d . . . H24A H 0.8372 0.3593 0.4057 0.074 Uiso 1 1 calc R . . H24B H 0.8190 0.5378 0.4255 0.074 Uiso 1 1 calc R . . H24C H 0.8632 0.4896 0.3407 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.03024(18) 0.01875(17) 0.03295(18) 0.00205(14) -0.00118(15) 0.00214(14) C1 0.038(2) 0.040(2) 0.043(3) 0.005(2) 0.011(2) 0.0101(19) C2 0.045(2) 0.028(2) 0.045(3) -0.005(2) -0.005(2) 0.008(2) C3 0.040(2) 0.0241(19) 0.055(2) 0.003(2) -0.005(2) 0.0043(18) C4 0.043(3) 0.028(2) 0.045(2) 0.0121(19) 0.0031(19) 0.0078(18) C5 0.044(2) 0.046(3) 0.039(2) 0.008(2) -0.010(2) 0.010(2) C6 0.032(2) 0.038(3) 0.056(3) -0.003(2) -0.010(2) -0.0013(19) C7 0.029(2) 0.040(3) 0.058(3) 0.006(2) 0.0000(19) 0.0003(19) C8 0.032(2) 0.0146(17) 0.031(2) 0.0006(15) 0.0024(16) 0.0027(15) C9 0.027(2) 0.0191(18) 0.0312(19) -0.0011(15) -0.0008(16) 0.0038(15) C10 0.0297(18) 0.0169(16) 0.0286(18) 0.0021(14) 0.0007(16) 0.0000(15) C11 0.033(2) 0.0158(18) 0.028(2) -0.0017(15) -0.0015(16) 0.0028(16) C12 0.0344(19) 0.0129(16) 0.0322(19) -0.0013(17) 0.0012(17) -0.0010(15) C13 0.045(2) 0.0198(19) 0.028(2) 0.0004(16) 0.0048(17) -0.0003(17) C14 0.054(3) 0.030(2) 0.038(2) 0.0081(19) 0.002(2) 0.005(2) C15 0.046(3) 0.033(2) 0.041(2) 0.0067(19) 0.008(2) -0.006(2) C16 0.037(2) 0.029(2) 0.0226(19) -0.0012(16) -0.0003(16) -0.0039(16) C17 0.036(2) 0.042(3) 0.039(2) -0.003(2) -0.0061(19) 0.0021(19) C18 0.042(2) 0.032(2) 0.037(2) -0.0075(19) -0.0005(18) -0.0072(19) C19 0.031(2) 0.026(2) 0.031(2) -0.0005(16) -0.0015(16) -0.0028(16) C20 0.031(2) 0.041(2) 0.043(2) -0.001(2) 0.0062(19) -0.0007(18) C21 0.040(2) 0.031(2) 0.038(2) 0.0052(18) 0.0016(18) -0.0076(18) C22 0.044(2) 0.029(2) 0.027(2) -0.0038(17) 0.0041(17) -0.0070(18) C23 0.064(3) 0.026(2) 0.039(2) -0.0085(18) 0.010(2) -0.002(2) C24 0.056(3) 0.062(3) 0.031(2) -0.008(2) -0.008(2) -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 Zr C7 2.324(5) . ? Zr C6 2.334(4) . ? Zr C1 2.338(4) . ? Zr C2 2.345(4) . ? Zr C4 2.346(4) . ? Zr C5 2.346(4) . ? Zr C3 2.351(4) . ? Zr C12 2.480(3) . ? Zr C8 2.515(4) . ? Zr C11 2.522(4) . ? Zr C9 2.532(4) . ? Zr C10 2.542(4) . ? C1 C7 1.415(7) . ? C1 C2 1.420(7) . ? C1 H1 0.91(2) . ? C2 C3 1.420(7) . ? C2 H2 0.91(2) . ? C3 C4 1.419(7) . ? C3 H3 0.91(2) . ? C4 C5 1.410(7) . ? C4 H4 0.91(2) . ? C5 C6 1.416(7) . ? C5 H5 0.90(2) . ? C6 C7 1.418(7) . ? C6 H6 0.91(2) . ? C7 H7 0.90(2) . ? C8 C12 1.409(6) . ? C8 C9 1.428(5) . ? C8 C13 1.521(5) . ? C9 C10 1.436(5) . ? C9 C16 1.521(5) . ? C10 C11 1.431(5) . ? C10 C19 1.523(5) . ? C11 C12 1.421(6) . ? C11 C22 1.519(5) . ? C12 H12 0.92(2) . ? C13 C15 1.510(6) . ? C13 C14 1.536(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.533(6) . ? C16 C18 1.538(5) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.528(6) . ? C19 C21 1.531(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.527(6) . ? C22 C23 1.534(6) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Zr C6 35.44(18) . . ? C7 Zr C1 35.33(17) . . ? C6 Zr C1 66.28(17) . . ? C7 Zr C2 66.36(16) . . ? C6 Zr C2 86.00(16) . . ? C1 Zr C2 35.29(16) . . ? C7 Zr C4 85.54(16) . . ? C6 Zr C4 65.86(16) . . ? C1 Zr C4 85.35(16) . . ? C2 Zr C4 65.95(15) . . ? C7 Zr C5 66.21(16) . . ? C6 Zr C5 35.22(17) . . ? C1 Zr C5 85.61(17) . . ? C2 Zr C5 85.67(16) . . ? C4 Zr C5 34.97(16) . . ? C7 Zr C3 85.85(16) . . ? C6 Zr C3 85.78(16) . . ? C1 Zr C3 66.02(17) . . ? C2 Zr C3 35.19(17) . . ? C4 Zr C3 35.18(16) . . ? C5 Zr C3 65.97(16) . . ? C7 Zr C12 104.79(15) . . ? C6 Zr C12 104.79(15) . . ? C1 Zr C12 121.19(15) . . ? C2 Zr C12 146.99(15) . . ? C4 Zr C12 146.97(15) . . ? C5 Zr C12 121.10(15) . . ? C3 Zr C12 168.85(14) . . ? C7 Zr C8 107.51(14) . . ? C6 Zr C8 126.32(15) . . ? C1 Zr C8 103.99(14) . . ? C2 Zr C8 116.79(14) . . ? C4 Zr C8 166.77(14) . . ? C5 Zr C8 153.02(15) . . ? C3 Zr C8 141.00(14) . . ? C12 Zr C8 32.76(13) . . ? C7 Zr C11 130.37(15) . . ? C6 Zr C11 112.55(15) . . ? C1 Zr C11 154.19(14) . . ? C2 Zr C11 161.32(15) . . ? C4 Zr C11 118.50(14) . . ? C5 Zr C11 108.02(15) . . ? C3 Zr C11 139.33(15) . . ? C12 Zr C11 33.00(13) . . ? C8 Zr C11 54.51(12) . . ? C7 Zr C9 136.14(14) . . ? C6 Zr C9 158.35(14) . . ? C1 Zr C9 116.88(14) . . ? C2 Zr C9 108.61(14) . . ? C4 Zr C9 134.28(14) . . ? C5 Zr C9 156.59(15) . . ? C3 Zr C9 115.44(14) . . ? C12 Zr C9 54.37(12) . . ? C8 Zr C9 32.87(12) . . ? C11 Zr C9 54.41(12) . . ? C7 Zr C10 159.20(14) . . ? C6 Zr C10 143.12(15) . . ? C1 Zr C10 149.14(14) . . ? C2 Zr C10 128.71(14) . . ? C4 Zr C10 113.00(13) . . ? C5 Zr C10 123.88(14) . . ? C3 Zr C10 114.66(14) . . ? C12 Zr C10 54.53(12) . . ? C8 Zr C10 54.56(11) . . ? C11 Zr C10 32.82(12) . . ? C9 Zr C10 32.88(12) . . ? C7 C1 C2 128.7(4) . . ? C7 C1 Zr 71.8(3) . . ? C2 C1 Zr 72.6(2) . . ? C7 C1 H1 118(3) . . ? C2 C1 H1 114(3) . . ? Zr C1 H1 135(3) . . ? C3 C2 C1 128.3(4) . . ? C3 C2 Zr 72.7(2) . . ? C1 C2 Zr 72.1(2) . . ? C3 C2 H2 121(3) . . ? C1 C2 H2 111(3) . . ? Zr C2 H2 125(3) . . ? C4 C3 C2 128.1(4) . . ? C4 C3 Zr 72.2(2) . . ? C2 C3 Zr 72.2(2) . . ? C4 C3 H3 114(3) . . ? C2 C3 H3 116(3) . . ? Zr C3 H3 121(3) . . ? C5 C4 C3 129.3(4) . . ? C5 C4 Zr 72.5(2) . . ? C3 C4 Zr 72.6(2) . . ? C5 C4 H4 113(3) . . ? C3 C4 H4 117(3) . . ? Zr C4 H4 126(3) . . ? C4 C5 C6 128.4(4) . . ? C4 C5 Zr 72.5(2) . . ? C6 C5 Zr 71.9(3) . . ? C4 C5 H5 116(3) . . ? C6 C5 H5 115(3) . . ? Zr C5 H5 138(3) . . ? C5 C6 C7 128.4(4) . . ? C5 C6 Zr 72.9(2) . . ? C7 C6 Zr 71.9(3) . . ? C5 C6 H6 117(4) . . ? C7 C6 H6 113(4) . . ? Zr C6 H6 123(4) . . ? C1 C7 C6 128.8(4) . . ? C1 C7 Zr 72.9(3) . . ? C6 C7 Zr 72.7(3) . . ? C1 C7 H7 114(3) . . ? C6 C7 H7 117(3) . . ? Zr C7 H7 127(3) . . ? C12 C8 C9 107.7(3) . . ? C12 C8 C13 124.9(3) . . ? C9 C8 C13 127.0(3) . . ? C12 C8 Zr 72.3(2) . . ? C9 C8 Zr 74.2(2) . . ? C13 C8 Zr 125.0(2) . . ? C8 C9 C10 108.0(3) . . ? C8 C9 C16 123.5(3) . . ? C10 C9 C16 127.8(3) . . ? C8 C9 Zr 72.9(2) . . ? C10 C9 Zr 73.9(2) . . ? C16 C9 Zr 125.8(2) . . ? C11 C10 C9 107.4(3) . . ? C11 C10 C19 126.3(3) . . ? C9 C10 C19 126.1(3) . . ? C11 C10 Zr 72.8(2) . . ? C9 C10 Zr 73.2(2) . . ? C19 C10 Zr 123.7(2) . . ? C12 C11 C10 107.6(3) . . ? C12 C11 C22 123.1(3) . . ? C10 C11 C22 128.4(4) . . ? C12 C11 Zr 71.9(2) . . ? C10 C11 Zr 74.4(2) . . ? C22 C11 Zr 128.0(3) . . ? C8 C12 C11 109.2(3) . . ? C8 C12 Zr 75.0(2) . . ? C11 C12 Zr 75.1(2) . . ? C8 C12 H12 123(2) . . ? C11 C12 H12 127(2) . . ? Zr C12 H12 121(2) . . ? C15 C13 C8 113.3(3) . . ? C15 C13 C14 109.8(3) . . ? C8 C13 C14 108.6(3) . . ? C15 C13 H13 108.3 . . ? C8 C13 H13 108.3 . . ? C14 C13 H13 108.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C9 C16 C17 111.6(3) . . ? C9 C16 C18 115.6(3) . . ? C17 C16 C18 110.5(3) . . ? C9 C16 H16 106.1 . . ? C17 C16 H16 106.1 . . ? C18 C16 H16 106.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C10 C19 C20 112.4(3) . . ? C10 C19 C21 114.0(3) . . ? C20 C19 C21 110.2(3) . . ? C10 C19 H19 106.6 . . ? C20 C19 H19 106.6 . . ? C21 C19 H19 106.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C11 C22 C24 113.2(4) . . ? C11 C22 C23 108.4(3) . . ? C24 C22 C23 110.1(4) . . ? C11 C22 H22 108.3 . . ? C24 C22 H22 108.3 . . ? C23 C22 H22 108.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 C6 Zr C1 C7 -23.2(3) . . . . ? C2 Zr C1 C7 -142.5(4) . . . . ? C4 Zr C1 C7 -88.8(3) . . . . ? C5 Zr C1 C7 -53.8(3) . . . . ? C3 Zr C1 C7 -119.4(3) . . . . ? C12 Zr C1 C7 70.2(3) . . . . ? C8 Zr C1 C7 100.7(3) . . . . ? C11 Zr C1 C7 69.8(4) . . . . ? C9 Zr C1 C7 133.1(3) . . . . ? C10 Zr C1 C7 142.2(3) . . . . ? C7 Zr C1 C2 142.5(4) . . . . ? C6 Zr C1 C2 119.3(3) . . . . ? C4 Zr C1 C2 53.6(3) . . . . ? C5 Zr C1 C2 88.7(3) . . . . ? C3 Zr C1 C2 23.1(3) . . . . ? C12 Zr C1 C2 -147.3(2) . . . . ? C8 Zr C1 C2 -116.9(3) . . . . ? C11 Zr C1 C2 -147.7(3) . . . . ? C9 Zr C1 C2 -84.4(3) . . . . ? C10 Zr C1 C2 -75.3(4) . . . . ? C7 C1 C2 C3 -1.3(8) . . . . ? Zr C1 C2 C3 -49.2(4) . . . . ? C7 C1 C2 Zr 47.8(4) . . . . ? C7 Zr C2 C3 118.9(3) . . . . ? C6 Zr C2 C3 88.3(3) . . . . ? C1 Zr C2 C3 141.5(4) . . . . ? C4 Zr C2 C3 23.0(3) . . . . ? C5 Zr C2 C3 53.0(3) . . . . ? C12 Zr C2 C3 -160.4(3) . . . . ? C8 Zr C2 C3 -142.6(2) . . . . ? C11 Zr C2 C3 -85.1(5) . . . . ? C9 Zr C2 C3 -108.0(3) . . . . ? C10 Zr C2 C3 -78.0(3) . . . . ? C7 Zr C2 C1 -22.6(3) . . . . ? C6 Zr C2 C1 -53.2(3) . . . . ? C4 Zr C2 C1 -118.5(3) . . . . ? C5 Zr C2 C1 -88.5(3) . . . . ? C3 Zr C2 C1 -141.5(4) . . . . ? C12 Zr C2 C1 58.1(4) . . . . ? C8 Zr C2 C1 75.8(3) . . . . ? C11 Zr C2 C1 133.4(4) . . . . ? C9 Zr C2 C1 110.5(3) . . . . ? C10 Zr C2 C1 140.5(2) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? Zr C2 C3 C4 -48.6(4) . . . . ? C1 C2 C3 Zr 49.0(4) . . . . ? C7 Zr C3 C4 88.2(3) . . . . ? C6 Zr C3 C4 52.6(3) . . . . ? C1 Zr C3 C4 118.5(3) . . . . ? C2 Zr C3 C4 141.7(4) . . . . ? C5 Zr C3 C4 22.4(3) . . . . ? C12 Zr C3 C4 -109.1(8) . . . . ? C8 Zr C3 C4 -158.9(2) . . . . ? C11 Zr C3 C4 -67.7(3) . . . . ? C9 Zr C3 C4 -131.8(2) . . . . ? C10 Zr C3 C4 -95.5(3) . . . . ? C7 Zr C3 C2 -53.5(3) . . . . ? C6 Zr C3 C2 -89.0(3) . . . . ? C1 Zr C3 C2 -23.2(3) . . . . ? C4 Zr C3 C2 -141.7(4) . . . . ? C5 Zr C3 C2 -119.3(3) . . . . ? C12 Zr C3 C2 109.3(8) . . . . ? C8 Zr C3 C2 59.4(3) . . . . ? C11 Zr C3 C2 150.7(3) . . . . ? C9 Zr C3 C2 86.5(3) . . . . ? C10 Zr C3 C2 122.9(3) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? Zr C3 C4 C5 -48.4(4) . . . . ? C2 C3 C4 Zr 48.6(4) . . . . ? C7 Zr C4 C5 53.5(3) . . . . ? C6 Zr C4 C5 22.9(3) . . . . ? C1 Zr C4 C5 89.0(3) . . . . ? C2 Zr C4 C5 119.6(3) . . . . ? C3 Zr C4 C5 142.6(4) . . . . ? C12 Zr C4 C5 -56.9(4) . . . . ? C8 Zr C4 C5 -135.4(6) . . . . ? C11 Zr C4 C5 -80.7(3) . . . . ? C9 Zr C4 C5 -147.4(3) . . . . ? C10 Zr C4 C5 -116.7(3) . . . . ? C7 Zr C4 C3 -89.1(3) . . . . ? C6 Zr C4 C3 -119.7(3) . . . . ? C1 Zr C4 C3 -53.7(3) . . . . ? C2 Zr C4 C3 -23.0(3) . . . . ? C5 Zr C4 C3 -142.6(4) . . . . ? C12 Zr C4 C3 160.4(3) . . . . ? C8 Zr C4 C3 81.9(7) . . . . ? C11 Zr C4 C3 136.7(2) . . . . ? C9 Zr C4 C3 70.0(3) . . . . ? C10 Zr C4 C3 100.6(3) . . . . ? C3 C4 C5 C6 0.1(8) . . . . ? Zr C4 C5 C6 -48.3(4) . . . . ? C3 C4 C5 Zr 48.5(4) . . . . ? C7 Zr C5 C4 -118.8(3) . . . . ? C6 Zr C5 C4 -142.0(4) . . . . ? C1 Zr C5 C4 -88.2(3) . . . . ? C2 Zr C5 C4 -52.8(3) . . . . ? C3 Zr C5 C4 -22.5(3) . . . . ? C12 Zr C5 C4 147.8(2) . . . . ? C8 Zr C5 C4 159.3(3) . . . . ? C11 Zr C5 C4 114.2(3) . . . . ? C9 Zr C5 C4 76.3(5) . . . . ? C10 Zr C5 C4 82.0(3) . . . . ? C7 Zr C5 C6 23.2(3) . . . . ? C1 Zr C5 C6 53.8(3) . . . . ? C2 Zr C5 C6 89.2(3) . . . . ? C4 Zr C5 C6 142.0(4) . . . . ? C3 Zr C5 C6 119.5(3) . . . . ? C12 Zr C5 C6 -70.3(3) . . . . ? C8 Zr C5 C6 -58.8(5) . . . . ? C11 Zr C5 C6 -103.8(3) . . . . ? C9 Zr C5 C6 -141.7(3) . . . . ? C10 Zr C5 C6 -136.0(3) . . . . ? C4 C5 C6 C7 -0.2(8) . . . . ? Zr C5 C6 C7 -48.8(5) . . . . ? C4 C5 C6 Zr 48.6(4) . . . . ? C7 Zr C6 C5 -141.6(4) . . . . ? C1 Zr C6 C5 -118.5(3) . . . . ? C2 Zr C6 C5 -88.2(3) . . . . ? C4 Zr C6 C5 -22.8(3) . . . . ? C3 Zr C6 C5 -52.9(3) . . . . ? C12 Zr C6 C5 123.5(3) . . . . ? C8 Zr C6 C5 151.2(3) . . . . ? C11 Zr C6 C5 89.6(3) . . . . ? C9 Zr C6 C5 138.1(4) . . . . ? C10 Zr C6 C5 73.9(3) . . . . ? C1 Zr C6 C7 23.1(3) . . . . ? C2 Zr C6 C7 53.5(3) . . . . ? C4 Zr C6 C7 118.9(3) . . . . ? C5 Zr C6 C7 141.6(4) . . . . ? C3 Zr C6 C7 88.8(3) . . . . ? C12 Zr C6 C7 -94.8(3) . . . . ? C8 Zr C6 C7 -67.1(3) . . . . ? C11 Zr C6 C7 -128.8(3) . . . . ? C9 Zr C6 C7 -80.3(5) . . . . ? C10 Zr C6 C7 -144.4(3) . . . . ? C2 C1 C7 C6 1.5(8) . . . . ? Zr C1 C7 C6 49.6(5) . . . . ? C2 C1 C7 Zr -48.1(4) . . . . ? C5 C6 C7 C1 -0.6(8) . . . . ? Zr C6 C7 C1 -49.7(5) . . . . ? C5 C6 C7 Zr 49.1(5) . . . . ? C6 Zr C7 C1 141.5(4) . . . . ? C2 Zr C7 C1 22.6(3) . . . . ? C4 Zr C7 C1 88.2(3) . . . . ? C5 Zr C7 C1 118.5(3) . . . . ? C3 Zr C7 C1 53.0(3) . . . . ? C12 Zr C7 C1 -123.6(3) . . . . ? C8 Zr C7 C1 -89.6(3) . . . . ? C11 Zr C7 C1 -147.6(2) . . . . ? C9 Zr C7 C1 -70.1(3) . . . . ? C10 Zr C7 C1 -117.8(4) . . . . ? C1 Zr C7 C6 -141.5(4) . . . . ? C2 Zr C7 C6 -118.9(3) . . . . ? C4 Zr C7 C6 -53.3(3) . . . . ? C5 Zr C7 C6 -23.0(3) . . . . ? C3 Zr C7 C6 -88.6(3) . . . . ? C12 Zr C7 C6 94.8(3) . . . . ? C8 Zr C7 C6 128.9(3) . . . . ? C11 Zr C7 C6 70.9(3) . . . . ? C9 Zr C7 C6 148.4(2) . . . . ? C10 Zr C7 C6 100.7(4) . . . . ? C7 Zr C8 C12 -90.2(2) . . . . ? C6 Zr C8 C12 -56.2(3) . . . . ? C1 Zr C8 C12 -126.8(2) . . . . ? C2 Zr C8 C12 -162.1(2) . . . . ? C4 Zr C8 C12 99.1(6) . . . . ? C5 Zr C8 C12 -18.4(4) . . . . ? C3 Zr C8 C12 164.1(3) . . . . ? C11 Zr C8 C12 37.3(2) . . . . ? C9 Zr C8 C12 115.0(3) . . . . ? C10 Zr C8 C12 77.9(2) . . . . ? C7 Zr C8 C9 154.8(2) . . . . ? C6 Zr C8 C9 -171.1(2) . . . . ? C1 Zr C8 C9 118.2(2) . . . . ? C2 Zr C8 C9 83.0(2) . . . . ? C4 Zr C8 C9 -15.8(7) . . . . ? C5 Zr C8 C9 -133.4(3) . . . . ? C3 Zr C8 C9 49.2(3) . . . . ? C12 Zr C8 C9 -115.0(3) . . . . ? C11 Zr C8 C9 -77.7(2) . . . . ? C10 Zr C8 C9 -37.1(2) . . . . ? C7 Zr C8 C13 30.3(3) . . . . ? C6 Zr C8 C13 64.4(4) . . . . ? C1 Zr C8 C13 -6.2(3) . . . . ? C2 Zr C8 C13 -41.5(4) . . . . ? C4 Zr C8 C13 -140.3(6) . . . . ? C5 Zr C8 C13 102.1(4) . . . . ? C3 Zr C8 C13 -75.3(4) . . . . ? C12 Zr C8 C13 120.6(4) . . . . ? C11 Zr C8 C13 157.9(4) . . . . ? C9 Zr C8 C13 -124.5(4) . . . . ? C10 Zr C8 C13 -161.5(4) . . . . ? C12 C8 C9 C10 1.1(4) . . . . ? C13 C8 C9 C10 -171.7(3) . . . . ? Zr C8 C9 C10 66.1(3) . . . . ? C12 C8 C9 C16 172.9(3) . . . . ? C13 C8 C9 C16 0.2(6) . . . . ? Zr C8 C9 C16 -122.1(3) . . . . ? C12 C8 C9 Zr -65.0(3) . . . . ? C13 C8 C9 Zr 122.2(4) . . . . ? C7 Zr C9 C8 -35.9(3) . . . . ? C6 Zr C9 C8 19.7(5) . . . . ? C1 Zr C9 C8 -73.4(2) . . . . ? C2 Zr C9 C8 -110.8(2) . . . . ? C4 Zr C9 C8 175.0(2) . . . . ? C5 Zr C9 C8 123.9(4) . . . . ? C3 Zr C9 C8 -148.2(2) . . . . ? C12 Zr C9 C8 37.1(2) . . . . ? C11 Zr C9 C8 78.0(2) . . . . ? C10 Zr C9 C8 115.2(3) . . . . ? C7 Zr C9 C10 -151.1(2) . . . . ? C6 Zr C9 C10 -95.5(4) . . . . ? C1 Zr C9 C10 171.3(2) . . . . ? C2 Zr C9 C10 134.0(2) . . . . ? C4 Zr C9 C10 59.8(3) . . . . ? C5 Zr C9 C10 8.7(5) . . . . ? C3 Zr C9 C10 96.6(2) . . . . ? C12 Zr C9 C10 -78.1(2) . . . . ? C8 Zr C9 C10 -115.2(3) . . . . ? C11 Zr C9 C10 -37.2(2) . . . . ? C7 Zr C9 C16 83.5(4) . . . . ? C6 Zr C9 C16 139.1(4) . . . . ? C1 Zr C9 C16 46.0(3) . . . . ? C2 Zr C9 C16 8.6(3) . . . . ? C4 Zr C9 C16 -65.6(4) . . . . ? C5 Zr C9 C16 -116.7(4) . . . . ? C3 Zr C9 C16 -28.8(4) . . . . ? C12 Zr C9 C16 156.5(4) . . . . ? C8 Zr C9 C16 119.4(4) . . . . ? C11 Zr C9 C16 -162.6(4) . . . . ? C10 Zr C9 C16 -125.4(4) . . . . ? C8 C9 C10 C11 -0.1(4) . . . . ? C16 C9 C10 C11 -171.5(3) . . . . ? Zr C9 C10 C11 65.3(3) . . . . ? C8 C9 C10 C19 174.8(3) . . . . ? C16 C9 C10 C19 3.4(6) . . . . ? Zr C9 C10 C19 -119.8(4) . . . . ? C8 C9 C10 Zr -65.4(2) . . . . ? C16 C9 C10 Zr 123.2(4) . . . . ? C7 Zr C10 C11 -44.3(5) . . . . ? C6 Zr C10 C11 27.4(3) . . . . ? C1 Zr C10 C11 -130.0(3) . . . . ? C2 Zr C10 C11 -175.8(2) . . . . ? C4 Zr C10 C11 107.4(2) . . . . ? C5 Zr C10 C11 69.3(3) . . . . ? C3 Zr C10 C11 145.9(2) . . . . ? C12 Zr C10 C11 -37.3(2) . . . . ? C8 Zr C10 C11 -77.8(2) . . . . ? C9 Zr C10 C11 -114.9(3) . . . . ? C7 Zr C10 C9 70.6(5) . . . . ? C6 Zr C10 C9 142.3(3) . . . . ? C1 Zr C10 C9 -15.2(4) . . . . ? C2 Zr C10 C9 -60.9(3) . . . . ? C4 Zr C10 C9 -137.8(2) . . . . ? C5 Zr C10 C9 -175.8(2) . . . . ? C3 Zr C10 C9 -99.2(2) . . . . ? C12 Zr C10 C9 77.6(2) . . . . ? C8 Zr C10 C9 37.1(2) . . . . ? C11 Zr C10 C9 114.9(3) . . . . ? C7 Zr C10 C19 -166.9(4) . . . . ? C6 Zr C10 C19 -95.2(4) . . . . ? C1 Zr C10 C19 107.4(4) . . . . ? C2 Zr C10 C19 61.6(3) . . . . ? C4 Zr C10 C19 -15.2(3) . . . . ? C5 Zr C10 C19 -53.3(3) . . . . ? C3 Zr C10 C19 23.3(3) . . . . ? C12 Zr C10 C19 -159.9(3) . . . . ? C8 Zr C10 C19 159.6(3) . . . . ? C11 Zr C10 C19 -122.6(4) . . . . ? C9 Zr C10 C19 122.5(4) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C19 C10 C11 C12 -175.7(3) . . . . ? Zr C10 C11 C12 64.7(3) . . . . ? C9 C10 C11 C22 168.0(4) . . . . ? C19 C10 C11 C22 -6.9(6) . . . . ? Zr C10 C11 C22 -126.5(4) . . . . ? C9 C10 C11 Zr -65.5(3) . . . . ? C19 C10 C11 Zr 119.6(4) . . . . ? C7 Zr C11 C12 46.0(3) . . . . ? C6 Zr C11 C12 82.4(3) . . . . ? C1 Zr C11 C12 0.6(4) . . . . ? C2 Zr C11 C12 -104.6(5) . . . . ? C4 Zr C11 C12 156.3(2) . . . . ? C5 Zr C11 C12 119.8(2) . . . . ? C3 Zr C11 C12 -166.4(2) . . . . ? C8 Zr C11 C12 -37.0(2) . . . . ? C9 Zr C11 C12 -77.7(2) . . . . ? C10 Zr C11 C12 -115.0(3) . . . . ? C7 Zr C11 C10 161.0(2) . . . . ? C6 Zr C11 C10 -162.6(2) . . . . ? C1 Zr C11 C10 115.6(4) . . . . ? C2 Zr C11 C10 10.3(5) . . . . ? C4 Zr C11 C10 -88.8(2) . . . . ? C5 Zr C11 C10 -125.3(2) . . . . ? C3 Zr C11 C10 -51.4(3) . . . . ? C12 Zr C11 C10 115.0(3) . . . . ? C8 Zr C11 C10 78.0(2) . . . . ? C9 Zr C11 C10 37.3(2) . . . . ? C7 Zr C11 C22 -72.2(4) . . . . ? C6 Zr C11 C22 -35.8(4) . . . . ? C1 Zr C11 C22 -117.6(4) . . . . ? C2 Zr C11 C22 137.2(4) . . . . ? C4 Zr C11 C22 38.0(4) . . . . ? C5 Zr C11 C22 1.6(4) . . . . ? C3 Zr C11 C22 75.4(4) . . . . ? C12 Zr C11 C22 -118.2(4) . . . . ? C8 Zr C11 C22 -155.2(4) . . . . ? C9 Zr C11 C22 164.1(4) . . . . ? C10 Zr C11 C22 126.8(4) . . . . ? C9 C8 C12 C11 -1.6(4) . . . . ? C13 C8 C12 C11 171.3(3) . . . . ? Zr C8 C12 C11 -68.0(3) . . . . ? C9 C8 C12 Zr 66.3(3) . . . . ? C13 C8 C12 Zr -120.7(4) . . . . ? C10 C11 C12 C8 1.6(4) . . . . ? C22 C11 C12 C8 -168.0(4) . . . . ? Zr C11 C12 C8 67.9(3) . . . . ? C10 C11 C12 Zr -66.3(3) . . . . ? C22 C11 C12 Zr 124.1(4) . . . . ? C7 Zr C12 C8 99.5(2) . . . . ? C6 Zr C12 C8 136.2(2) . . . . ? C1 Zr C12 C8 65.2(3) . . . . ? C2 Zr C12 C8 30.3(4) . . . . ? C4 Zr C12 C8 -155.5(3) . . . . ? C5 Zr C12 C8 170.4(2) . . . . ? C3 Zr C12 C8 -62.7(9) . . . . ? C11 Zr C12 C8 -115.1(3) . . . . ? C9 Zr C12 C8 -37.3(2) . . . . ? C10 Zr C12 C8 -78.0(2) . . . . ? C7 Zr C12 C11 -145.4(2) . . . . ? C6 Zr C12 C11 -108.7(2) . . . . ? C1 Zr C12 C11 -179.7(2) . . . . ? C2 Zr C12 C11 145.3(3) . . . . ? C4 Zr C12 C11 -40.5(4) . . . . ? C5 Zr C12 C11 -74.6(3) . . . . ? C3 Zr C12 C11 52.3(9) . . . . ? C8 Zr C12 C11 115.1(3) . . . . ? C9 Zr C12 C11 77.8(2) . . . . ? C10 Zr C12 C11 37.1(2) . . . . ? C12 C8 C13 C15 31.9(5) . . . . ? C9 C8 C13 C15 -156.6(4) . . . . ? Zr C8 C13 C15 -60.1(4) . . . . ? C12 C8 C13 C14 -90.5(5) . . . . ? C9 C8 C13 C14 81.1(5) . . . . ? Zr C8 C13 C14 177.6(3) . . . . ? C8 C9 C16 C17 -105.3(4) . . . . ? C10 C9 C16 C17 64.9(5) . . . . ? Zr C9 C16 C17 162.3(3) . . . . ? C8 C9 C16 C18 127.3(4) . . . . ? C10 C9 C16 C18 -62.5(5) . . . . ? Zr C9 C16 C18 34.8(5) . . . . ? C11 C10 C19 C20 62.8(5) . . . . ? C9 C10 C19 C20 -111.1(4) . . . . ? Zr C10 C19 C20 155.6(3) . . . . ? C11 C10 C19 C21 -63.6(5) . . . . ? C9 C10 C19 C21 122.5(4) . . . . ? Zr C10 C19 C21 29.3(4) . . . . ? C12 C11 C22 C24 -51.9(5) . . . . ? C10 C11 C22 C24 140.9(4) . . . . ? Zr C11 C22 C24 40.3(5) . . . . ? C12 C11 C22 C23 70.6(5) . . . . ? C10 C11 C22 C23 -96.7(4) . . . . ? Zr C11 C22 C23 162.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 62.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.541 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.077 _iucr_refine_instructions ; TITL andyg99 in P2(1)/c CELL 1.54184 15.0646 8.6396 16.4412 90.000 90.047 90.000 ZERR 4.00 0.0006 0.0004 0.0006 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H ZR UNIT 96 144 4 SIZE 0.26 0.04 0.03 TEMP -123.00 MERG 2 TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 2 SADI c1 H1 C2 H2 C3 H3 C4 H4 C5 H5 C6 H6 C7 H7 C12 H12 FMAP 2 PLAN 10 ACTA CONF BOND $H L.S. 10 OMIT 3 4 0 OMIT 2 3 0 OMIT 1 4 0 OMIT 0 4 0 WGHT 0.063600 BASF 0.17149 FVAR 2.48894 ZR 3 0.826724 0.179721 0.196825 11.00000 0.03024 0.01875 = 0.03295 0.00205 -0.00118 0.00214 C1 1 0.935862 0.084168 0.109110 11.00000 0.03780 0.04040 = 0.04279 0.00493 0.01115 0.01008 H1 2 0.950368 0.099560 0.056088 11.00000 0.05521 C2 1 0.872593 -0.035538 0.120829 11.00000 0.04466 0.02763 = 0.04517 -0.00491 -0.00491 0.00788 H2 2 0.848867 -0.065465 0.072288 11.00000 0.04283 C3 1 0.837123 -0.091825 0.195132 11.00000 0.03950 0.02409 = 0.05458 0.00345 -0.00544 0.00435 H3 2 0.787764 -0.151441 0.191247 11.00000 0.04152 C4 1 0.856318 -0.041038 0.275350 11.00000 0.04294 0.02767 = 0.04508 0.01210 0.00310 0.00779 H4 2 0.821954 -0.079667 0.315834 11.00000 0.02805 C5 1 0.914403 0.076724 0.301638 11.00000 0.04414 0.04606 = 0.03900 0.00847 -0.00974 0.00970 H5 2 0.919990 0.088172 0.355992 11.00000 0.04901 C6 1 0.968576 0.175022 0.253893 11.00000 0.03243 0.03805 = 0.05565 -0.00294 -0.00991 -0.00127 H6 2 0.993030 0.258607 0.279187 11.00000 0.07096 C7 1 0.977742 0.178446 0.168112 11.00000 0.02860 0.03989 = 0.05753 0.00646 0.00001 0.00031 H7 2 1.009691 0.257078 0.146782 11.00000 0.04833 C8 1 0.758344 0.400254 0.119044 11.00000 0.03164 0.01457 = 0.03076 0.00059 0.00241 0.00272 C9 1 0.688421 0.291290 0.131681 11.00000 0.02723 0.01909 = 0.03121 -0.00107 -0.00076 0.00382 C10 1 0.670606 0.284111 0.217386 11.00000 0.02966 0.01689 = 0.02864 0.00211 0.00069 -0.00004 C11 1 0.730202 0.389009 0.256802 11.00000 0.03332 0.01583 = 0.02837 -0.00170 -0.00148 0.00279 C12 1 0.784338 0.457061 0.195766 11.00000 0.03442 0.01289 = 0.03218 -0.00130 0.00120 -0.00100 H12 2 0.826682 0.532798 0.202545 11.00000 0.02121 C13 1 0.791813 0.461494 0.037937 11.00000 0.04477 0.01982 = 0.02793 0.00035 0.00482 -0.00029 AFIX 13 H13 2 0.789212 0.375488 -0.002699 11.00000 -1.20000 AFIX 0 C14 1 0.729530 0.591334 0.009323 11.00000 0.05414 0.02980 = 0.03834 0.00811 0.00214 0.00482 AFIX 137 H14A 2 0.728803 0.674391 0.049913 11.00000 -1.50000 H14B 2 0.669391 0.550027 0.002537 11.00000 -1.50000 H14C 2 0.750656 0.632425 -0.042738 11.00000 -1.50000 AFIX 0 C15 1 0.886075 0.520684 0.041586 11.00000 0.04595 0.03293 = 0.04081 0.00671 0.00817 -0.00566 AFIX 137 H15A 2 0.889811 0.605666 0.080920 11.00000 -1.50000 H15B 2 0.903844 0.558116 -0.012261 11.00000 -1.50000 H15C 2 0.925729 0.436674 0.058465 11.00000 -1.50000 AFIX 0 C16 1 0.635573 0.217820 0.062906 11.00000 0.03660 0.02854 = 0.02256 -0.00115 -0.00035 -0.00389 AFIX 13 H16 2 0.666995 0.246307 0.011486 11.00000 -1.20000 AFIX 0 C17 1 0.542258 0.287411 0.056259 11.00000 0.03553 0.04199 = 0.03930 -0.00271 -0.00614 0.00213 AFIX 137 H17A 2 0.506268 0.252897 0.102454 11.00000 -1.50000 H17B 2 0.514494 0.253216 0.005416 11.00000 -1.50000 H17C 2 0.546349 0.400616 0.056656 11.00000 -1.50000 AFIX 0 C18 1 0.630809 0.039976 0.064010 11.00000 0.04229 0.03193 = 0.03721 -0.00749 -0.00050 -0.00716 AFIX 137 H18A 2 0.691034 -0.002816 0.062580 11.00000 -1.50000 H18B 2 0.597535 0.003760 0.016433 11.00000 -1.50000 H18C 2 0.600824 0.005686 0.113721 11.00000 -1.50000 AFIX 0 C19 1 0.596255 0.192733 0.257820 11.00000 0.03064 0.02586 = 0.03113 -0.00049 -0.00146 -0.00284 AFIX 13 H19 2 0.566590 0.131846 0.213787 11.00000 -1.20000 AFIX 0 C20 1 0.525129 0.297623 0.294549 11.00000 0.03081 0.04121 = 0.04305 -0.00050 0.00617 -0.00071 AFIX 137 H20A 2 0.473848 0.235038 0.310745 11.00000 -1.50000 H20B 2 0.506560 0.374436 0.254111 11.00000 -1.50000 H20C 2 0.549363 0.350663 0.342349 11.00000 -1.50000 AFIX 0 C21 1 0.628479 0.075417 0.321106 11.00000 0.04016 0.03082 = 0.03750 0.00524 0.00159 -0.00757 AFIX 137 H21A 2 0.660923 -0.008004 0.293789 11.00000 -1.50000 H21B 2 0.577320 0.032024 0.349976 11.00000 -1.50000 H21C 2 0.667816 0.127150 0.360055 11.00000 -1.50000 AFIX 0 C22 1 0.728015 0.446301 0.344102 11.00000 0.04392 0.02877 = 0.02677 -0.00375 0.00409 -0.00704 AFIX 13 H22 2 0.692193 0.371779 0.377069 11.00000 -1.20000 AFIX 0 C23 1 0.681266 0.604003 0.345707 11.00000 0.06421 0.02607 = 0.03879 -0.00853 0.01030 -0.00160 AFIX 137 H23A 2 0.717169 0.680045 0.316172 11.00000 -1.50000 H23B 2 0.673863 0.637771 0.402200 11.00000 -1.50000 H23C 2 0.622899 0.594942 0.319776 11.00000 -1.50000 AFIX 0 C24 1 0.820087 0.459455 0.382432 11.00000 0.05559 0.06169 = 0.03080 -0.00847 -0.00836 -0.00744 AFIX 137 H24A 2 0.837182 0.359317 0.405653 11.00000 -1.50000 H24B 2 0.818963 0.537849 0.425499 11.00000 -1.50000 H24C 2 0.863198 0.489639 0.340739 11.00000 -1.50000 HKLF 4 ; #============================================================================= # end of cif data for "andyg99" (compound 4) #============================================================================= #============================================================================= # cif data for "andyg44" (compound 5) #============================================================================= data_andyg44 _database_code_depnum_ccdc_archive 'CCDC 853656' #TrackingRef '- BulkyCp-final-121111.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Zr' _chemical_formula_weight 409.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0987(4) _cell_length_b 14.0383(6) _cell_length_c 15.6547(10) _cell_angle_alpha 66.262(6) _cell_angle_beta 82.216(4) _cell_angle_gamma 84.290(4) _cell_volume 2010.38(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16542 _cell_measurement_theta_min 2.3587 _cell_measurement_theta_max 29.1643 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98753 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63302 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.10 _reflns_number_total 8815 _reflns_number_gt 6070 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogens of the seven-membered ring and of the C9 atom were refined freely. The methyls were refined using a rigid model, others riding. ; _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8815 _refine_ls_number_parameters 511 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0307 _refine_ls_wR_factor_gt 0.0299 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr -0.004332(19) 0.722538(14) 0.125754(13) 0.01538(5) Uani 1 1 d . . . C1 C -0.0061(2) 0.76903(16) -0.03404(13) 0.0252(5) Uani 1 1 d D . . H1 H -0.0685(14) 0.8083(12) -0.0733(10) 0.030 Uiso 1 1 d D . . C2 C 0.0994(2) 0.81985(15) -0.02201(13) 0.0247(5) Uani 1 1 d D . . H2 H 0.0981(16) 0.8923(9) -0.0542(11) 0.030 Uiso 1 1 d D . . C3 C 0.2007(2) 0.77672(15) 0.03920(14) 0.0221(5) Uani 1 1 d D . . H3 H 0.2560(15) 0.8232(11) 0.0431(12) 0.027 Uiso 1 1 d D . . C4 C 0.22164(19) 0.67218(16) 0.10373(14) 0.0229(5) Uani 1 1 d D . . H4 H 0.2870(14) 0.6607(13) 0.1423(10) 0.027 Uiso 1 1 d D . . C5 C 0.1444(2) 0.58556(14) 0.12309(14) 0.0253(5) Uani 1 1 d D . . H5 H 0.1667(17) 0.5273(10) 0.1735(10) 0.030 Uiso 1 1 d D . . C6 C 0.0303(2) 0.58086(15) 0.08133(15) 0.0249(5) Uani 1 1 d D . . H6 H -0.0106(16) 0.5180(10) 0.1101(11) 0.030 Uiso 1 1 d D . . C7 C -0.0360(2) 0.66192(17) 0.01099(15) 0.0253(5) Uani 1 1 d D . . H7 H -0.1143(13) 0.6416(12) 0.0016(12) 0.030 Uiso 1 1 d D . . C8 C -0.22606(17) 0.78662(13) 0.18356(12) 0.0117(4) Uani 1 1 d . . . C9 C -0.12692(19) 0.84722(14) 0.19033(13) 0.0140(5) Uani 1 1 d D . . H9 H -0.1241(15) 0.9176(8) 0.1528(10) 0.017 Uiso 1 1 d D . . C10 C -0.03657(18) 0.78755(13) 0.25564(12) 0.0126(4) Uani 1 1 d . . . C11 C -0.08540(17) 0.68340(13) 0.29687(12) 0.0113(4) Uani 1 1 d . . . C12 C -0.20163(17) 0.68360(13) 0.25188(11) 0.0106(4) Uani 1 1 d . . . C13 C -0.26919(17) 0.58861(13) 0.28137(12) 0.0148(4) Uani 1 1 d . . . H13 H -0.3453 0.5868 0.2526 0.018 Uiso 1 1 calc R . . C14 C -0.22367(18) 0.50128(13) 0.35069(12) 0.0164(5) Uani 1 1 d . . . H14 H -0.2692 0.4387 0.3704 0.020 Uiso 1 1 calc R . . C15 C -0.11000(18) 0.50157(13) 0.39410(12) 0.0168(5) Uani 1 1 d . . . H15 H -0.0810 0.4392 0.4426 0.020 Uiso 1 1 calc R . . C16 C -0.04122(18) 0.58875(13) 0.36820(11) 0.0149(4) Uani 1 1 d . . . H16 H 0.0361 0.5868 0.3974 0.018 Uiso 1 1 calc R . . C17 C -0.34508(18) 0.82902(13) 0.12618(12) 0.0154(4) Uani 1 1 d . . . C18 C -0.32310(18) 0.94134(12) 0.05519(12) 0.0250(5) Uani 1 1 d . . . H18A H -0.3227 0.9869 0.0889 0.037 Uiso 1 1 calc R . . H18B H -0.3954 0.9651 0.0143 0.037 Uiso 1 1 calc R . . H18C H -0.2371 0.9437 0.0171 0.037 Uiso 1 1 calc R . . C19 C -0.37013(18) 0.76503(13) 0.07105(12) 0.0236(5) Uani 1 1 d . . . H19A H -0.2931 0.7681 0.0248 0.035 Uiso 1 1 calc R . . H19B H -0.4506 0.7936 0.0387 0.035 Uiso 1 1 calc R . . H19C H -0.3828 0.6924 0.1144 0.035 Uiso 1 1 calc R . . C20 C -0.47111(17) 0.82932(14) 0.19410(13) 0.0249(5) Uani 1 1 d . . . H20A H -0.4883 0.7577 0.2382 0.037 Uiso 1 1 calc R . . H20B H -0.5481 0.8593 0.1582 0.037 Uiso 1 1 calc R . . H20C H -0.4568 0.8711 0.2290 0.037 Uiso 1 1 calc R . . C21 C 0.06721(18) 0.83340(13) 0.28879(12) 0.0164(5) Uani 1 1 d . . . C22 C 0.11389(18) 0.93634(13) 0.21115(12) 0.0251(5) Uani 1 1 d . . . H22A H 0.1554 0.9237 0.1561 0.038 Uiso 1 1 calc R . . H22B H 0.1793 0.9652 0.2339 0.038 Uiso 1 1 calc R . . H22C H 0.0368 0.9859 0.1938 0.038 Uiso 1 1 calc R . . C23 C 0.19128(18) 0.76151(13) 0.31903(14) 0.0308(6) Uani 1 1 d . . . H23A H 0.1663 0.7004 0.3760 0.046 Uiso 1 1 calc R . . H23B H 0.2579 0.7991 0.3317 0.046 Uiso 1 1 calc R . . H23C H 0.2292 0.7390 0.2688 0.046 Uiso 1 1 calc R . . C24 C -0.00280(19) 0.85575(14) 0.37329(12) 0.0300(5) Uani 1 1 d . . . H24A H -0.0811 0.9034 0.3541 0.045 Uiso 1 1 calc R . . H24B H 0.0597 0.8877 0.3954 0.045 Uiso 1 1 calc R . . H24C H -0.0314 0.7903 0.4240 0.045 Uiso 1 1 calc R . . Zr' Zr 0.502212(19) 0.198986(14) 0.292218(13) 0.01668(5) Uani 1 1 d . . . C1' C 0.5537(2) 0.03173(16) 0.29721(17) 0.0330(6) Uani 1 1 d D . . H1' H 0.6220(15) -0.0117(12) 0.3250(12) 0.040 Uiso 1 1 d D . . C2' C 0.4322(2) 0.02851(15) 0.35541(15) 0.0311(6) Uani 1 1 d D . . H2' H 0.4318(18) -0.0182(12) 0.4175(9) 0.037 Uiso 1 1 d D . . C3' C 0.3161(2) 0.09664(16) 0.33337(15) 0.0279(6) Uani 1 1 d D . . H3' H 0.2539(15) 0.0828(13) 0.3840(10) 0.033 Uiso 1 1 d D . . C4' C 0.2931(2) 0.18308(15) 0.24962(15) 0.0249(5) Uani 1 1 d D . . H4' H 0.2153(13) 0.2225(11) 0.2551(12) 0.030 Uiso 1 1 d D . . C5' C 0.3816(2) 0.22621(16) 0.16643(15) 0.0297(6) Uani 1 1 d D . . H5' H 0.3536(17) 0.2909(10) 0.1239(11) 0.036 Uiso 1 1 d D . . C6' C 0.5131(2) 0.19014(18) 0.14674(15) 0.0319(6) Uani 1 1 d D . . H6' H 0.5583(17) 0.2331(12) 0.0918(10) 0.038 Uiso 1 1 d D . . C7' C 0.5881(2) 0.10367(19) 0.20395(18) 0.0343(6) Uani 1 1 d D . . H7' H 0.6773(13) 0.0961(13) 0.1822(13) 0.041 Uiso 1 1 d D . . C8' C 0.71058(17) 0.25303(13) 0.33045(12) 0.0124(4) Uani 1 1 d . . . C9' C 0.60690(19) 0.25280(14) 0.40152(13) 0.0144(5) Uani 1 1 d D . . H9' H 0.6113(16) 0.2090(10) 0.4626(8) 0.017 Uiso 1 1 d D . . C10' C 0.50428(17) 0.32874(13) 0.36621(12) 0.0123(4) Uani 1 1 d . . . C11' C 0.54571(17) 0.38298(13) 0.26752(12) 0.0117(4) Uani 1 1 d . . . C12' C 0.67404(17) 0.33673(12) 0.24602(12) 0.0118(4) Uani 1 1 d . . . C13' C 0.73585(18) 0.37963(13) 0.15167(12) 0.0158(5) Uani 1 1 d . . . H13' H 0.8201 0.3513 0.1355 0.019 Uiso 1 1 calc R . . C14' C 0.67480(19) 0.46061(13) 0.08511(13) 0.0194(5) Uani 1 1 d . . . H14' H 0.7182 0.4891 0.0230 0.023 Uiso 1 1 calc R . . C15' C 0.54808(18) 0.50370(13) 0.10589(13) 0.0180(5) Uani 1 1 d . . . H15' H 0.5070 0.5595 0.0575 0.022 Uiso 1 1 calc R . . C16' C 0.48438(18) 0.46613(12) 0.19430(13) 0.0160(4) Uani 1 1 d . . . H16' H 0.3990 0.4953 0.2073 0.019 Uiso 1 1 calc R . . C17' C 0.84283(18) 0.18939(13) 0.35042(12) 0.0161(5) Uani 1 1 d . . . C18' C 0.82333(18) 0.08897(12) 0.43861(12) 0.0226(5) Uani 1 1 d . . . H18D H 0.7904 0.1064 0.4926 0.034 Uiso 1 1 calc R . . H18E H 0.9090 0.0489 0.4499 0.034 Uiso 1 1 calc R . . H18F H 0.7582 0.0473 0.4297 0.034 Uiso 1 1 calc R . . C19' C 0.90752(18) 0.15935(14) 0.26989(13) 0.0314(6) Uani 1 1 d . . . H19D H 0.8449 0.1203 0.2554 0.047 Uiso 1 1 calc R . . H19E H 0.9893 0.1160 0.2885 0.047 Uiso 1 1 calc R . . H19F H 0.9298 0.2226 0.2143 0.047 Uiso 1 1 calc R . . C20' C 0.94023(18) 0.25528(13) 0.36819(13) 0.0276(5) Uani 1 1 d . . . H20D H 0.9536 0.3202 0.3126 0.041 Uiso 1 1 calc R . . H20E H 1.0262 0.2161 0.3811 0.041 Uiso 1 1 calc R . . H20F H 0.9030 0.2715 0.4222 0.041 Uiso 1 1 calc R . . C21' C 0.38448(18) 0.35722(13) 0.42430(12) 0.0170(5) Uani 1 1 d . . . C22' C 0.38655(19) 0.28686(15) 0.52827(12) 0.0348(6) Uani 1 1 d . . . H22D H 0.3123 0.3084 0.5649 0.052 Uiso 1 1 calc R . . H22E H 0.4715 0.2926 0.5491 0.052 Uiso 1 1 calc R . . H22F H 0.3772 0.2145 0.5374 0.052 Uiso 1 1 calc R . . C23' C 0.25094(17) 0.34683(13) 0.39375(13) 0.0259(5) Uani 1 1 d . . . H23D H 0.2478 0.3915 0.3271 0.039 Uiso 1 1 calc R . . H23E H 0.1774 0.3682 0.4310 0.039 Uiso 1 1 calc R . . H23F H 0.2420 0.2742 0.4036 0.039 Uiso 1 1 calc R . . C24' C 0.39393(18) 0.47069(13) 0.41300(13) 0.0282(5) Uani 1 1 d . . . H24D H 0.3857 0.5178 0.3475 0.042 Uiso 1 1 calc R . . H24E H 0.4805 0.4787 0.4305 0.042 Uiso 1 1 calc R . . H24F H 0.3216 0.4878 0.4538 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01426(12) 0.01874(12) 0.01126(11) -0.00539(9) 0.00138(9) 0.00162(9) C1 0.0237(14) 0.0379(15) 0.0115(12) -0.0087(11) -0.0018(10) 0.0045(11) C2 0.0278(14) 0.0228(12) 0.0160(12) -0.0020(10) 0.0042(10) -0.0015(11) C3 0.0166(13) 0.0235(13) 0.0251(13) -0.0102(10) 0.0060(10) -0.0045(10) C4 0.0140(12) 0.0294(13) 0.0253(13) -0.0122(11) -0.0019(10) 0.0045(10) C5 0.0221(13) 0.0187(12) 0.0287(14) -0.0049(10) -0.0008(11) 0.0052(10) C6 0.0201(13) 0.0202(13) 0.0333(14) -0.0115(11) 0.0051(11) -0.0028(10) C7 0.0209(14) 0.0364(14) 0.0270(13) -0.0229(11) 0.0025(11) -0.0011(11) C8 0.0103(11) 0.0164(10) 0.0111(10) -0.0088(9) 0.0003(8) -0.0001(8) C9 0.0152(12) 0.0115(10) 0.0135(11) -0.0043(9) 0.0019(9) 0.0001(9) C10 0.0114(11) 0.0158(11) 0.0108(11) -0.0063(9) 0.0010(9) 0.0007(9) C11 0.0090(11) 0.0164(11) 0.0095(10) -0.0074(9) 0.0018(8) 0.0005(8) C12 0.0090(10) 0.0148(10) 0.0084(10) -0.0058(8) 0.0019(8) -0.0005(8) C13 0.0103(11) 0.0218(11) 0.0149(11) -0.0104(9) -0.0001(9) -0.0005(9) C14 0.0177(12) 0.0137(11) 0.0164(11) -0.0054(9) 0.0041(9) -0.0044(9) C15 0.0217(12) 0.0153(11) 0.0114(11) -0.0033(9) -0.0028(9) 0.0008(9) C16 0.0150(11) 0.0218(11) 0.0097(10) -0.0081(9) -0.0015(9) -0.0004(9) C17 0.0117(11) 0.0173(11) 0.0175(11) -0.0073(9) -0.0035(9) 0.0017(9) C18 0.0187(12) 0.0263(12) 0.0267(12) -0.0061(10) -0.0098(10) 0.0042(9) C19 0.0200(12) 0.0288(12) 0.0255(12) -0.0121(10) -0.0139(10) 0.0048(10) C20 0.0156(12) 0.0294(12) 0.0297(13) -0.0125(11) -0.0027(10) 0.0025(10) C21 0.0138(11) 0.0184(11) 0.0170(11) -0.0062(9) -0.0036(9) -0.0020(9) C22 0.0279(13) 0.0248(12) 0.0241(12) -0.0085(10) -0.0038(10) -0.0119(10) C23 0.0191(12) 0.0275(12) 0.0461(15) -0.0111(11) -0.0130(11) -0.0047(10) C24 0.0296(14) 0.0449(14) 0.0240(13) -0.0202(11) -0.0027(11) -0.0115(11) Zr' 0.01751(13) 0.01808(12) 0.01659(12) -0.00898(10) 0.00102(10) -0.00492(9) C1' 0.0258(15) 0.0257(14) 0.0572(18) -0.0255(13) -0.0092(13) 0.0017(11) C2' 0.0306(14) 0.0197(13) 0.0403(15) -0.0089(11) 0.0001(13) -0.0066(11) C3' 0.0210(14) 0.0274(13) 0.0336(15) -0.0113(12) 0.0075(11) -0.0107(11) C4' 0.0198(13) 0.0282(13) 0.0308(13) -0.0153(11) -0.0029(11) -0.0026(10) C5' 0.0316(15) 0.0370(14) 0.0257(14) -0.0145(11) -0.0079(12) -0.0084(12) C6' 0.0309(16) 0.0501(17) 0.0247(14) -0.0235(13) 0.0051(12) -0.0195(13) C7' 0.0205(14) 0.0489(16) 0.0510(17) -0.0396(14) 0.0085(13) -0.0108(13) C8' 0.0107(11) 0.0149(10) 0.0141(11) -0.0089(9) 0.0006(9) -0.0006(8) C9' 0.0180(12) 0.0159(11) 0.0086(11) -0.0045(9) -0.0008(10) -0.0008(9) C10' 0.0109(11) 0.0155(10) 0.0125(11) -0.0077(9) -0.0007(9) -0.0008(9) C11' 0.0114(11) 0.0139(10) 0.0138(11) -0.0089(9) -0.0019(9) -0.0028(8) C12' 0.0103(11) 0.0142(10) 0.0142(11) -0.0085(9) -0.0020(9) -0.0022(8) C13' 0.0121(11) 0.0197(11) 0.0181(12) -0.0105(9) 0.0030(9) -0.0051(9) C14' 0.0255(13) 0.0208(11) 0.0123(11) -0.0068(9) 0.0036(10) -0.0093(10) C15' 0.0241(12) 0.0135(10) 0.0158(11) -0.0029(9) -0.0091(10) -0.0009(9) C16' 0.0122(11) 0.0150(11) 0.0248(12) -0.0113(9) -0.0063(9) 0.0019(9) C17' 0.0122(11) 0.0216(11) 0.0151(11) -0.0089(9) -0.0013(9) 0.0042(9) C18' 0.0180(12) 0.0215(11) 0.0276(12) -0.0090(10) -0.0085(10) 0.0067(9) C19' 0.0258(13) 0.0424(14) 0.0300(13) -0.0214(11) -0.0072(11) 0.0169(11) C20' 0.0127(12) 0.0328(13) 0.0377(14) -0.0147(11) -0.0061(10) 0.0051(10) C21' 0.0116(11) 0.0248(11) 0.0163(11) -0.0114(9) 0.0008(9) 0.0022(9) C22' 0.0265(14) 0.0522(15) 0.0207(13) -0.0154(11) 0.0077(11) 0.0118(11) C23' 0.0125(12) 0.0358(13) 0.0300(13) -0.0160(11) 0.0049(10) -0.0001(10) C24' 0.0193(12) 0.0378(13) 0.0356(14) -0.0266(11) 0.0071(10) 0.0013(10) _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 Zr C1 2.319(2) . ? Zr C2 2.3237(18) . ? Zr C3 2.3290(19) . ? Zr C5 2.3300(19) . ? Zr C6 2.3390(19) . ? Zr C4 2.3427(19) . ? Zr C7 2.344(2) . ? Zr C9 2.5045(18) . ? Zr C10 2.5157(17) . ? Zr C8 2.5195(17) . ? Zr C12 2.5396(16) . ? Zr C11 2.5414(17) . ? C1 C2 1.412(3) . ? C1 C7 1.424(3) . ? C2 C3 1.416(3) . ? C3 C4 1.422(3) . ? C4 C5 1.416(3) . ? C5 C6 1.419(3) . ? C6 C7 1.412(3) . ? C8 C9 1.417(2) . ? C8 C12 1.432(2) . ? C8 C17 1.525(2) . ? C9 C10 1.411(2) . ? C10 C11 1.447(2) . ? C10 C21 1.527(2) . ? C11 C16 1.426(2) . ? C11 C12 1.448(2) . ? C12 C13 1.434(2) . ? C13 C14 1.358(2) . ? C14 C15 1.412(2) . ? C15 C16 1.356(2) . ? C17 C19 1.531(2) . ? C17 C18 1.537(2) . ? C17 C20 1.545(2) . ? C21 C23 1.529(2) . ? C21 C22 1.534(2) . ? C21 C24 1.544(2) . ? Zr' C6' 2.318(2) . ? Zr' C7' 2.321(2) . ? Zr' C1' 2.326(2) . ? Zr' C2' 2.3339(19) . ? Zr' C5' 2.337(2) . ? Zr' C3' 2.3400(19) . ? Zr' C4' 2.355(2) . ? Zr' C9' 2.5111(19) . ? Zr' C10' 2.5245(17) . ? Zr' C8' 2.5271(17) . ? Zr' C11' 2.5278(16) . ? Zr' C12' 2.5446(16) . ? C1' C2' 1.419(3) . ? C1' C7' 1.420(3) . ? C2' C3' 1.425(3) . ? C3' C4' 1.411(3) . ? C4' C5' 1.421(3) . ? C5' C6' 1.413(3) . ? C6' C7' 1.406(3) . ? C8' C9' 1.420(2) . ? C8' C12' 1.435(2) . ? C8' C17' 1.526(2) . ? C9' C10' 1.406(2) . ? C10' C11' 1.443(2) . ? C10' C21' 1.533(2) . ? C11' C16' 1.425(2) . ? C11' C12' 1.451(2) . ? C12' C13' 1.429(2) . ? C13' C14' 1.356(2) . ? C14' C15' 1.415(2) . ? C15' C16' 1.359(2) . ? C17' C19' 1.531(2) . ? C17' C18' 1.532(2) . ? C17' C20' 1.537(2) . ? C21' C22' 1.528(2) . ? C21' C23' 1.529(2) . ? C21' C24' 1.542(2) . ? 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 Zr C2 35.42(7) . . ? C1 Zr C3 66.41(7) . . ? C2 Zr C3 35.44(7) . . ? C1 Zr C5 86.39(7) . . ? C2 Zr C5 86.41(7) . . ? C3 Zr C5 66.42(7) . . ? C1 Zr C6 66.48(7) . . ? C2 Zr C6 86.21(7) . . ? C3 Zr C6 85.97(7) . . ? C5 Zr C6 35.39(7) . . ? C1 Zr C4 86.22(7) . . ? C2 Zr C4 66.57(7) . . ? C3 Zr C4 35.44(6) . . ? C5 Zr C4 35.29(6) . . ? C6 Zr C4 66.22(7) . . ? C1 Zr C7 35.56(7) . . ? C2 Zr C7 66.46(7) . . ? C3 Zr C7 85.85(7) . . ? C5 Zr C7 66.18(8) . . ? C6 Zr C7 35.10(7) . . ? C4 Zr C7 85.72(7) . . ? C1 Zr C9 115.80(7) . . ? C2 Zr C9 107.74(6) . . ? C3 Zr C9 115.04(6) . . ? C5 Zr C9 156.92(7) . . ? C6 Zr C9 158.38(7) . . ? C4 Zr C9 134.15(7) . . ? C7 Zr C9 135.89(7) . . ? C1 Zr C10 145.13(7) . . ? C2 Zr C10 121.89(6) . . ? C3 Zr C10 108.07(6) . . ? C5 Zr C10 124.31(7) . . ? C6 Zr C10 148.24(6) . . ? C4 Zr C10 109.02(6) . . ? C7 Zr C10 164.86(6) . . ? C9 Zr C10 32.64(5) . . ? C1 Zr C8 106.86(6) . . ? C2 Zr C8 120.05(6) . . ? C3 Zr C8 143.40(6) . . ? C5 Zr C8 150.07(6) . . ? C6 Zr C8 125.83(6) . . ? C4 Zr C8 164.73(6) . . ? C7 Zr C8 109.48(6) . . ? C9 Zr C8 32.77(5) . . ? C10 Zr C8 55.72(6) . . ? C1 Zr C12 128.28(7) . . ? C2 Zr C12 152.42(6) . . ? C3 Zr C12 163.04(6) . . ? C5 Zr C12 118.59(6) . . ? C6 Zr C12 107.17(6) . . ? C4 Zr C12 140.76(6) . . ? C7 Zr C12 111.08(6) . . ? C9 Zr C12 53.41(5) . . ? C10 Zr C12 55.23(5) . . ? C8 Zr C12 32.89(5) . . ? C1 Zr C11 160.88(6) . . ? C2 Zr C11 155.01(6) . . ? C3 Zr C11 131.17(7) . . ? C5 Zr C11 106.94(6) . . ? C6 Zr C11 117.02(6) . . ? C4 Zr C11 112.63(6) . . ? C7 Zr C11 138.10(6) . . ? C9 Zr C11 53.48(5) . . ? C10 Zr C11 33.26(5) . . ? C8 Zr C11 55.04(6) . . ? C12 Zr C11 33.11(5) . . ? C2 C1 C7 128.79(19) . . ? C2 C1 Zr 72.46(12) . . ? C7 C1 Zr 73.17(12) . . ? C1 C2 C3 128.33(18) . . ? C1 C2 Zr 72.13(11) . . ? C3 C2 Zr 72.49(11) . . ? C2 C3 C4 128.97(19) . . ? C2 C3 Zr 72.07(11) . . ? C4 C3 Zr 72.81(11) . . ? C5 C4 C3 128.08(19) . . ? C5 C4 Zr 71.87(11) . . ? C3 C4 Zr 71.76(11) . . ? C4 C5 C6 128.78(19) . . ? C4 C5 Zr 72.84(11) . . ? C6 C5 Zr 72.65(12) . . ? C7 C6 C5 128.61(18) . . ? C7 C6 Zr 72.64(11) . . ? C5 C6 Zr 71.96(11) . . ? C6 C7 C1 128.4(2) . . ? C6 C7 Zr 72.25(12) . . ? C1 C7 Zr 71.28(12) . . ? C9 C8 C12 105.43(16) . . ? C9 C8 C17 125.54(16) . . ? C12 C8 C17 128.36(15) . . ? C9 C8 Zr 73.04(10) . . ? C12 C8 Zr 74.33(10) . . ? C17 C8 Zr 124.76(11) . . ? C10 C9 C8 112.62(16) . . ? C10 C9 Zr 74.11(10) . . ? C8 C9 Zr 74.20(10) . . ? C9 C10 C11 105.19(16) . . ? C9 C10 C21 124.41(16) . . ? C11 C10 C21 128.90(16) . . ? C9 C10 Zr 73.24(11) . . ? C11 C10 Zr 74.35(10) . . ? C21 C10 Zr 127.88(12) . . ? C16 C11 C10 132.92(17) . . ? C16 C11 C12 118.99(15) . . ? C10 C11 C12 108.09(15) . . ? C16 C11 Zr 119.74(11) . . ? C10 C11 Zr 72.40(9) . . ? C12 C11 Zr 73.38(9) . . ? C8 C12 C13 132.70(17) . . ? C8 C12 C11 108.57(15) . . ? C13 C12 C11 118.73(15) . . ? C8 C12 Zr 72.78(9) . . ? C13 C12 Zr 120.21(11) . . ? C11 C12 Zr 73.51(9) . . ? C14 C13 C12 119.62(17) . . ? C13 C14 C15 121.36(16) . . ? C16 C15 C14 121.56(17) . . ? C15 C16 C11 119.73(17) . . ? C8 C17 C19 113.38(14) . . ? C8 C17 C18 110.27(14) . . ? C19 C17 C18 107.48(15) . . ? C8 C17 C20 108.21(15) . . ? C19 C17 C20 108.73(15) . . ? C18 C17 C20 108.68(15) . . ? C10 C21 C23 114.05(15) . . ? C10 C21 C22 110.53(15) . . ? C23 C21 C22 107.81(15) . . ? C10 C21 C24 106.79(14) . . ? C23 C21 C24 108.90(15) . . ? C22 C21 C24 108.65(14) . . ? C6' Zr' C7' 35.28(8) . . ? C6' Zr' C1' 66.75(8) . . ? C7' Zr' C1' 35.60(8) . . ? C6' Zr' C2' 86.54(8) . . ? C7' Zr' C2' 66.54(8) . . ? C1' Zr' C2' 35.45(7) . . ? C6' Zr' C5' 35.35(7) . . ? C7' Zr' C5' 66.16(8) . . ? C1' Zr' C5' 86.40(8) . . ? C2' Zr' C5' 86.46(7) . . ? C6' Zr' C3' 85.92(7) . . ? C7' Zr' C3' 85.70(7) . . ? C1' Zr' C3' 66.36(7) . . ? C2' Zr' C3' 35.50(7) . . ? C5' Zr' C3' 66.18(7) . . ? C6' Zr' C4' 66.04(7) . . ? C7' Zr' C4' 85.28(7) . . ? C1' Zr' C4' 85.71(7) . . ? C2' Zr' C4' 66.18(7) . . ? C5' Zr' C4' 35.24(7) . . ? C3' Zr' C4' 34.97(7) . . ? C6' Zr' C9' 148.42(7) . . ? C7' Zr' C9' 131.64(7) . . ? C1' Zr' C9' 118.20(7) . . ? C2' Zr' C9' 115.65(7) . . ? C5' Zr' C9' 155.05(6) . . ? C3' Zr' C9' 125.35(7) . . ? C4' Zr' C9' 142.07(7) . . ? C6' Zr' C10' 141.19(7) . . ? C7' Zr' C10' 156.44(6) . . ? C1' Zr' C10' 149.17(7) . . ? C2' Zr' C10' 130.93(7) . . ? C5' Zr' C10' 123.93(7) . . ? C3' Zr' C10' 117.68(6) . . ? C4' Zr' C10' 115.21(6) . . ? C9' Zr' C10' 32.43(5) . . ? C6' Zr' C8' 116.45(7) . . ? C7' Zr' C8' 102.79(7) . . ? C1' Zr' C8' 105.49(7) . . ? C2' Zr' C8' 124.20(7) . . ? C5' Zr' C8' 141.70(7) . . ? C3' Zr' C8' 151.98(7) . . ? C4' Zr' C8' 168.67(6) . . ? C9' Zr' C8' 32.74(5) . . ? C10' Zr' C8' 55.36(5) . . ? C6' Zr' C11' 108.50(7) . . ? C7' Zr' C11' 129.51(7) . . ? C1' Zr' C11' 156.98(7) . . ? C2' Zr' C11' 163.75(7) . . ? C5' Zr' C11' 102.15(6) . . ? C3' Zr' C11' 136.65(7) . . ? C4' Zr' C11' 113.63(6) . . ? C9' Zr' C11' 53.60(6) . . ? C10' Zr' C11' 33.20(5) . . ? C8' Zr' C11' 55.09(5) . . ? C6' Zr' C12' 96.67(6) . . ? C7' Zr' C12' 102.14(7) . . ? C1' Zr' C12' 123.75(7) . . ? C2' Zr' C12' 154.28(7) . . ? C5' Zr' C12' 110.76(6) . . ? C3' Zr' C12' 169.77(7) . . ? C4' Zr' C12' 138.11(6) . . ? C9' Zr' C12' 53.48(5) . . ? C10' Zr' C12' 55.04(5) . . ? C8' Zr' C12' 32.87(5) . . ? C11' Zr' C12' 33.23(5) . . ? C2' C1' C7' 128.2(2) . . ? C2' C1' Zr' 72.58(12) . . ? C7' C1' Zr' 72.00(12) . . ? C1' C2' C3' 127.8(2) . . ? C1' C2' Zr' 71.97(12) . . ? C3' C2' Zr' 72.49(11) . . ? C4' C3' C2' 129.08(19) . . ? C4' C3' Zr' 73.11(11) . . ? C2' C3' Zr' 72.01(11) . . ? C3' C4' C5' 128.78(19) . . ? C3' C4' Zr' 71.92(12) . . ? C5' C4' Zr' 71.65(12) . . ? C6' C5' C4' 128.0(2) . . ? C6' C5' Zr' 71.59(13) . . ? C4' C5' Zr' 73.10(12) . . ? C7' C6' C5' 128.8(2) . . ? C7' C6' Zr' 72.48(13) . . ? C5' C6' Zr' 73.06(12) . . ? C6' C7' C1' 129.4(2) . . ? C6' C7' Zr' 72.24(12) . . ? C1' C7' Zr' 72.40(12) . . ? C9' C8' C12' 105.67(15) . . ? C9' C8' C17' 123.57(16) . . ? C12' C8' C17' 129.67(16) . . ? C9' C8' Zr' 73.01(11) . . ? C12' C8' Zr' 74.24(10) . . ? C17' C8' Zr' 126.80(11) . . ? C10' C9' C8' 112.26(16) . . ? C10' C9' Zr' 74.31(11) . . ? C8' C9' Zr' 74.25(11) . . ? C9' C10' C11' 105.76(15) . . ? C9' C10' C21' 126.18(16) . . ? C11' C10' C21' 127.52(16) . . ? C9' C10' Zr' 73.27(10) . . ? C11' C10' Zr' 73.53(10) . . ? C21' C10' Zr' 124.72(12) . . ? C16' C11' C10' 132.49(17) . . ? C16' C11' C12' 119.43(16) . . ? C10' C11' C12' 108.07(15) . . ? C16' C11' Zr' 117.59(12) . . ? C10' C11' Zr' 73.27(9) . . ? C12' C11' Zr' 74.02(9) . . ? C13' C12' C8' 133.94(17) . . ? C13' C12' C11' 117.87(16) . . ? C8' C12' C11' 108.19(15) . . ? C13' C12' Zr' 119.78(12) . . ? C8' C12' Zr' 72.89(9) . . ? C11' C12' Zr' 72.75(9) . . ? C14' C13' C12' 120.34(17) . . ? C13' C14' C15' 121.58(17) . . ? C16' C15' C14' 120.75(17) . . ? C15' C16' C11' 120.00(17) . . ? C8' C17' C19' 113.74(15) . . ? C8' C17' C18' 110.68(14) . . ? C19' C17' C18' 107.90(14) . . ? C8' C17' C20' 107.82(14) . . ? C19' C17' C20' 108.31(15) . . ? C18' C17' C20' 108.24(15) . . ? C22' C21' C23' 108.31(15) . . ? C22' C21' C10' 110.38(15) . . ? C23' C21' C10' 112.17(15) . . ? C22' C21' C24' 108.07(15) . . ? C23' C21' C24' 108.85(15) . . ? C10' C21' C24' 108.97(14) . . ? 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 Zr C1 C2 -23.08(11) . . . . ? C5 Zr C1 C2 -88.88(12) . . . . ? C6 Zr C1 C2 -119.19(13) . . . . ? C4 Zr C1 C2 -53.52(12) . . . . ? C7 Zr C1 C2 -141.45(19) . . . . ? C9 Zr C1 C2 84.50(13) . . . . ? C10 Zr C1 C2 64.93(17) . . . . ? C8 Zr C1 C2 118.46(12) . . . . ? C12 Zr C1 C2 146.99(11) . . . . ? C11 Zr C1 C2 135.91(19) . . . . ? C2 Zr C1 C7 141.45(19) . . . . ? C3 Zr C1 C7 118.38(13) . . . . ? C5 Zr C1 C7 52.57(12) . . . . ? C6 Zr C1 C7 22.27(12) . . . . ? C4 Zr C1 C7 87.93(13) . . . . ? C9 Zr C1 C7 -134.05(12) . . . . ? C10 Zr C1 C7 -153.62(12) . . . . ? C8 Zr C1 C7 -100.09(12) . . . . ? C12 Zr C1 C7 -71.56(14) . . . . ? C11 Zr C1 C7 -82.6(2) . . . . ? C7 C1 C2 C3 -1.1(4) . . . . ? Zr C1 C2 C3 48.9(2) . . . . ? C7 C1 C2 Zr -49.9(2) . . . . ? C3 Zr C2 C1 141.72(18) . . . . ? C5 Zr C2 C1 88.82(13) . . . . ? C6 Zr C2 C1 53.35(12) . . . . ? C4 Zr C2 C1 119.03(13) . . . . ? C7 Zr C2 C1 23.28(12) . . . . ? C9 Zr C2 C1 -109.79(12) . . . . ? C10 Zr C2 C1 -142.42(11) . . . . ? C8 Zr C2 C1 -76.40(13) . . . . ? C12 Zr C2 C1 -67.47(18) . . . . ? C11 Zr C2 C1 -147.37(14) . . . . ? C1 Zr C2 C3 -141.72(18) . . . . ? C5 Zr C2 C3 -52.91(13) . . . . ? C6 Zr C2 C3 -88.38(13) . . . . ? C4 Zr C2 C3 -22.69(11) . . . . ? C7 Zr C2 C3 -118.44(13) . . . . ? C9 Zr C2 C3 108.48(12) . . . . ? C10 Zr C2 C3 75.86(13) . . . . ? C8 Zr C2 C3 141.88(11) . . . . ? C12 Zr C2 C3 150.81(13) . . . . ? C11 Zr C2 C3 70.9(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? Zr C2 C3 C4 48.6(2) . . . . ? C1 C2 C3 Zr -48.7(2) . . . . ? C1 Zr C3 C2 23.06(12) . . . . ? C5 Zr C3 C2 119.70(14) . . . . ? C6 Zr C3 C2 89.12(13) . . . . ? C4 Zr C3 C2 142.37(19) . . . . ? C7 Zr C3 C2 53.92(12) . . . . ? C9 Zr C3 C2 -85.61(13) . . . . ? C10 Zr C3 C2 -120.00(12) . . . . ? C8 Zr C3 C2 -63.66(17) . . . . ? C12 Zr C3 C2 -129.3(2) . . . . ? C11 Zr C3 C2 -147.96(11) . . . . ? C1 Zr C3 C4 -119.31(13) . . . . ? C2 Zr C3 C4 -142.37(19) . . . . ? C5 Zr C3 C4 -22.67(12) . . . . ? C6 Zr C3 C4 -53.25(12) . . . . ? C7 Zr C3 C4 -88.45(13) . . . . ? C9 Zr C3 C4 132.02(12) . . . . ? C10 Zr C3 C4 97.63(12) . . . . ? C8 Zr C3 C4 153.96(11) . . . . ? C12 Zr C3 C4 88.4(2) . . . . ? C11 Zr C3 C4 69.66(14) . . . . ? C2 C3 C4 C5 -0.8(4) . . . . ? Zr C3 C4 C5 47.6(2) . . . . ? C2 C3 C4 Zr -48.3(2) . . . . ? C1 Zr C4 C5 -89.10(13) . . . . ? C2 Zr C4 C5 -119.62(14) . . . . ? C3 Zr C4 C5 -142.31(19) . . . . ? C6 Zr C4 C5 -23.17(12) . . . . ? C7 Zr C4 C5 -53.45(13) . . . . ? C9 Zr C4 C5 147.97(12) . . . . ? C10 Zr C4 C5 123.02(12) . . . . ? C8 Zr C4 C5 121.4(2) . . . . ? C12 Zr C4 C5 65.13(16) . . . . ? C11 Zr C4 C5 87.57(13) . . . . ? C1 Zr C4 C3 53.21(12) . . . . ? C2 Zr C4 C3 22.69(12) . . . . ? C5 Zr C4 C3 142.31(19) . . . . ? C6 Zr C4 C3 119.14(13) . . . . ? C7 Zr C4 C3 88.86(13) . . . . ? C9 Zr C4 C3 -69.72(15) . . . . ? C10 Zr C4 C3 -94.67(12) . . . . ? C8 Zr C4 C3 -96.3(3) . . . . ? C12 Zr C4 C3 -152.56(11) . . . . ? C11 Zr C4 C3 -130.12(12) . . . . ? C3 C4 C5 C6 2.0(4) . . . . ? Zr C4 C5 C6 49.6(2) . . . . ? C3 C4 C5 Zr -47.5(2) . . . . ? C1 Zr C5 C4 88.55(13) . . . . ? C2 Zr C5 C4 53.06(13) . . . . ? C3 Zr C5 C4 22.75(12) . . . . ? C6 Zr C5 C4 141.56(19) . . . . ? C7 Zr C5 C4 118.86(13) . . . . ? C9 Zr C5 C4 -76.1(2) . . . . ? C10 Zr C5 C4 -73.67(13) . . . . ? C8 Zr C5 C4 -153.22(12) . . . . ? C12 Zr C5 C4 -139.18(11) . . . . ? C11 Zr C5 C4 -105.41(12) . . . . ? C1 Zr C5 C6 -53.01(12) . . . . ? C2 Zr C5 C6 -88.50(12) . . . . ? C3 Zr C5 C6 -118.81(13) . . . . ? C4 Zr C5 C6 -141.56(19) . . . . ? C7 Zr C5 C6 -22.70(11) . . . . ? C9 Zr C5 C6 142.33(16) . . . . ? C10 Zr C5 C6 144.77(11) . . . . ? C8 Zr C5 C6 65.22(18) . . . . ? C12 Zr C5 C6 79.25(13) . . . . ? C11 Zr C5 C6 113.03(12) . . . . ? C4 C5 C6 C7 -1.1(4) . . . . ? Zr C5 C6 C7 48.6(2) . . . . ? C4 C5 C6 Zr -49.6(2) . . . . ? C1 Zr C6 C7 -22.53(12) . . . . ? C2 Zr C6 C7 -52.99(12) . . . . ? C3 Zr C6 C7 -88.52(12) . . . . ? C5 Zr C6 C7 -142.14(18) . . . . ? C4 Zr C6 C7 -119.03(13) . . . . ? C9 Zr C6 C7 78.4(2) . . . . ? C10 Zr C6 C7 153.00(12) . . . . ? C8 Zr C6 C7 71.83(13) . . . . ? C12 Zr C6 C7 102.41(12) . . . . ? C11 Zr C6 C7 136.66(11) . . . . ? C1 Zr C6 C5 119.61(13) . . . . ? C2 Zr C6 C5 89.14(12) . . . . ? C3 Zr C6 C5 53.62(12) . . . . ? C4 Zr C6 C5 23.11(11) . . . . ? C7 Zr C6 C5 142.14(18) . . . . ? C9 Zr C6 C5 -139.44(17) . . . . ? C10 Zr C6 C5 -64.86(17) . . . . ? C8 Zr C6 C5 -146.03(11) . . . . ? C12 Zr C6 C5 -115.45(11) . . . . ? C11 Zr C6 C5 -81.20(12) . . . . ? C5 C6 C7 C1 -1.4(4) . . . . ? Zr C6 C7 C1 46.9(2) . . . . ? C5 C6 C7 Zr -48.3(2) . . . . ? C2 C1 C7 C6 2.4(4) . . . . ? Zr C1 C7 C6 -47.2(2) . . . . ? C2 C1 C7 Zr 49.7(2) . . . . ? C1 Zr C7 C6 142.83(19) . . . . ? C2 Zr C7 C6 119.64(13) . . . . ? C3 Zr C7 C6 88.89(12) . . . . ? C5 Zr C7 C6 22.87(11) . . . . ? C4 Zr C7 C6 53.36(12) . . . . ? C9 Zr C7 C6 -148.76(11) . . . . ? C10 Zr C7 C6 -113.8(3) . . . . ? C8 Zr C7 C6 -125.20(11) . . . . ? C12 Zr C7 C6 -90.11(12) . . . . ? C11 Zr C7 C6 -66.26(15) . . . . ? C2 Zr C7 C1 -23.20(12) . . . . ? C3 Zr C7 C1 -53.94(13) . . . . ? C5 Zr C7 C1 -119.97(13) . . . . ? C6 Zr C7 C1 -142.83(19) . . . . ? C4 Zr C7 C1 -89.48(13) . . . . ? C9 Zr C7 C1 68.40(15) . . . . ? C10 Zr C7 C1 103.4(3) . . . . ? C8 Zr C7 C1 91.97(12) . . . . ? C12 Zr C7 C1 127.06(12) . . . . ? C11 Zr C7 C1 150.90(11) . . . . ? C1 Zr C8 C9 -111.67(11) . . . . ? C2 Zr C8 C9 -75.62(12) . . . . ? C3 Zr C8 C9 -38.72(16) . . . . ? C5 Zr C8 C9 135.08(14) . . . . ? C6 Zr C8 C9 175.52(11) . . . . ? C4 Zr C8 C9 36.4(3) . . . . ? C7 Zr C8 C9 -149.06(11) . . . . ? C10 Zr C8 C9 34.52(10) . . . . ? C12 Zr C8 C9 111.99(15) . . . . ? C11 Zr C8 C9 75.21(11) . . . . ? C1 Zr C8 C12 136.34(11) . . . . ? C2 Zr C8 C12 172.39(10) . . . . ? C3 Zr C8 C12 -150.71(12) . . . . ? C5 Zr C8 C12 23.09(19) . . . . ? C6 Zr C8 C12 63.53(13) . . . . ? C4 Zr C8 C12 -75.6(3) . . . . ? C7 Zr C8 C12 98.95(11) . . . . ? C9 Zr C8 C12 -111.99(15) . . . . ? C10 Zr C8 C12 -77.47(10) . . . . ? C11 Zr C8 C12 -36.78(9) . . . . ? C1 Zr C8 C17 10.20(15) . . . . ? C2 Zr C8 C17 46.25(16) . . . . ? C3 Zr C8 C17 83.14(17) . . . . ? C5 Zr C8 C17 -103.05(18) . . . . ? C6 Zr C8 C17 -62.62(16) . . . . ? C4 Zr C8 C17 158.3(2) . . . . ? C7 Zr C8 C17 -27.20(15) . . . . ? C9 Zr C8 C17 121.87(18) . . . . ? C10 Zr C8 C17 156.39(16) . . . . ? C12 Zr C8 C17 -126.14(18) . . . . ? C11 Zr C8 C17 -162.92(16) . . . . ? C12 C8 C9 C10 3.1(2) . . . . ? C17 C8 C9 C10 174.25(16) . . . . ? Zr C8 C9 C10 -64.78(14) . . . . ? C12 C8 C9 Zr 67.84(11) . . . . ? C17 C8 C9 Zr -120.97(17) . . . . ? C1 Zr C9 C10 -159.21(11) . . . . ? C2 Zr C9 C10 -121.93(11) . . . . ? C3 Zr C9 C10 -84.56(12) . . . . ? C5 Zr C9 C10 3.7(2) . . . . ? C6 Zr C9 C10 109.8(2) . . . . ? C4 Zr C9 C10 -47.67(14) . . . . ? C7 Zr C9 C10 163.89(11) . . . . ? C8 Zr C9 C10 119.75(15) . . . . ? C12 Zr C9 C10 80.91(11) . . . . ? C11 Zr C9 C10 39.37(10) . . . . ? C1 Zr C9 C8 81.05(12) . . . . ? C2 Zr C9 C8 118.32(11) . . . . ? C3 Zr C9 C8 155.69(11) . . . . ? C5 Zr C9 C8 -116.01(18) . . . . ? C6 Zr C9 C8 -9.9(2) . . . . ? C4 Zr C9 C8 -167.42(10) . . . . ? C7 Zr C9 C8 44.14(14) . . . . ? C10 Zr C9 C8 -119.75(15) . . . . ? C12 Zr C9 C8 -38.84(10) . . . . ? C11 Zr C9 C8 -80.38(11) . . . . ? C8 C9 C10 C11 -3.2(2) . . . . ? Zr C9 C10 C11 -68.05(12) . . . . ? C8 C9 C10 C21 -170.35(16) . . . . ? Zr C9 C10 C21 124.82(17) . . . . ? C8 C9 C10 Zr 64.83(14) . . . . ? C1 Zr C10 C9 33.99(17) . . . . ? C2 Zr C10 C9 72.18(13) . . . . ? C3 Zr C10 C9 108.44(11) . . . . ? C5 Zr C10 C9 -178.23(11) . . . . ? C6 Zr C10 C9 -138.82(13) . . . . ? C4 Zr C10 C9 145.87(11) . . . . ? C7 Zr C10 C9 -47.7(3) . . . . ? C8 Zr C10 C9 -34.66(10) . . . . ? C12 Zr C10 C9 -74.84(11) . . . . ? C11 Zr C10 C9 -111.63(15) . . . . ? C1 Zr C10 C11 145.63(12) . . . . ? C2 Zr C10 C11 -176.19(10) . . . . ? C3 Zr C10 C11 -139.93(11) . . . . ? C5 Zr C10 C11 -66.59(12) . . . . ? C6 Zr C10 C11 -27.19(18) . . . . ? C4 Zr C10 C11 -102.50(11) . . . . ? C7 Zr C10 C11 63.9(3) . . . . ? C9 Zr C10 C11 111.63(15) . . . . ? C8 Zr C10 C11 76.98(11) . . . . ? C12 Zr C10 C11 36.79(9) . . . . ? C1 Zr C10 C21 -86.91(19) . . . . ? C2 Zr C10 C21 -48.72(17) . . . . ? C3 Zr C10 C21 -12.47(16) . . . . ? C5 Zr C10 C21 60.87(16) . . . . ? C6 Zr C10 C21 100.28(17) . . . . ? C4 Zr C10 C21 24.97(16) . . . . ? C7 Zr C10 C21 -168.6(2) . . . . ? C9 Zr C10 C21 -120.90(19) . . . . ? C8 Zr C10 C21 -155.56(17) . . . . ? C12 Zr C10 C21 164.25(17) . . . . ? C11 Zr C10 C21 127.5(2) . . . . ? C9 C10 C11 C16 -178.17(18) . . . . ? C21 C10 C11 C16 -11.8(3) . . . . ? Zr C10 C11 C16 114.6(2) . . . . ? C9 C10 C11 C12 2.06(19) . . . . ? C21 C10 C11 C12 168.40(17) . . . . ? Zr C10 C11 C12 -65.21(12) . . . . ? C9 C10 C11 Zr 67.27(12) . . . . ? C21 C10 C11 Zr -126.39(18) . . . . ? C1 Zr C11 C16 130.4(2) . . . . ? C2 Zr C11 C16 -122.23(18) . . . . ? C3 Zr C11 C16 -75.52(16) . . . . ? C5 Zr C11 C16 -2.32(16) . . . . ? C6 Zr C11 C16 34.43(16) . . . . ? C4 Zr C11 C16 -39.44(16) . . . . ? C7 Zr C11 C16 70.65(17) . . . . ? C9 Zr C11 C16 -168.51(17) . . . . ? C10 Zr C11 C16 -129.91(19) . . . . ? C8 Zr C11 C16 150.86(16) . . . . ? C12 Zr C11 C16 114.33(18) . . . . ? C1 Zr C11 C10 -99.7(2) . . . . ? C2 Zr C11 C10 7.7(2) . . . . ? C3 Zr C11 C10 54.39(13) . . . . ? C5 Zr C11 C10 127.58(11) . . . . ? C6 Zr C11 C10 164.34(11) . . . . ? C4 Zr C11 C10 90.47(11) . . . . ? C7 Zr C11 C10 -159.44(11) . . . . ? C9 Zr C11 C10 -38.60(10) . . . . ? C8 Zr C11 C10 -79.23(11) . . . . ? C12 Zr C11 C10 -115.76(14) . . . . ? C1 Zr C11 C12 16.0(2) . . . . ? C2 Zr C11 C12 123.44(16) . . . . ? C3 Zr C11 C12 170.15(10) . . . . ? C5 Zr C11 C12 -116.66(10) . . . . ? C6 Zr C11 C12 -79.90(11) . . . . ? C4 Zr C11 C12 -153.77(10) . . . . ? C7 Zr C11 C12 -43.68(14) . . . . ? C9 Zr C11 C12 77.16(11) . . . . ? C10 Zr C11 C12 115.76(14) . . . . ? C8 Zr C11 C12 36.53(9) . . . . ? C9 C8 C12 C13 177.55(18) . . . . ? C17 C8 C12 C13 6.7(3) . . . . ? Zr C8 C12 C13 -115.52(19) . . . . ? C9 C8 C12 C11 -1.61(19) . . . . ? C17 C8 C12 C11 -172.47(16) . . . . ? Zr C8 C12 C11 65.32(12) . . . . ? C9 C8 C12 Zr -66.93(12) . . . . ? C17 C8 C12 Zr 122.21(17) . . . . ? C16 C11 C12 C8 179.91(15) . . . . ? C10 C11 C12 C8 -0.28(19) . . . . ? Zr C11 C12 C8 -64.85(12) . . . . ? C16 C11 C12 C13 0.6(2) . . . . ? C10 C11 C12 C13 -179.58(15) . . . . ? Zr C11 C12 C13 115.86(15) . . . . ? C16 C11 C12 Zr -115.25(15) . . . . ? C10 C11 C12 Zr 64.57(12) . . . . ? C1 Zr C12 C8 -57.32(13) . . . . ? C2 Zr C12 C8 -14.33(19) . . . . ? C3 Zr C12 C8 89.9(2) . . . . ? C5 Zr C12 C8 -167.12(11) . . . . ? C6 Zr C12 C8 -130.57(11) . . . . ? C4 Zr C12 C8 156.23(11) . . . . ? C7 Zr C12 C8 -93.56(11) . . . . ? C9 Zr C12 C8 38.68(10) . . . . ? C10 Zr C12 C8 79.11(10) . . . . ? C11 Zr C12 C8 116.07(14) . . . . ? C1 Zr C12 C13 72.55(16) . . . . ? C2 Zr C12 C13 115.54(17) . . . . ? C3 Zr C12 C13 -140.3(2) . . . . ? C5 Zr C12 C13 -37.25(16) . . . . ? C6 Zr C12 C13 -0.69(15) . . . . ? C4 Zr C12 C13 -73.90(17) . . . . ? C7 Zr C12 C13 36.31(16) . . . . ? C9 Zr C12 C13 168.55(17) . . . . ? C10 Zr C12 C13 -151.02(16) . . . . ? C8 Zr C12 C13 129.87(19) . . . . ? C11 Zr C12 C13 -114.06(18) . . . . ? C1 Zr C12 C11 -173.38(10) . . . . ? C2 Zr C12 C11 -130.39(15) . . . . ? C3 Zr C12 C11 -26.2(3) . . . . ? C5 Zr C12 C11 76.81(12) . . . . ? C6 Zr C12 C11 113.37(11) . . . . ? C4 Zr C12 C11 40.16(14) . . . . ? C7 Zr C12 C11 150.37(10) . . . . ? C9 Zr C12 C11 -77.38(11) . . . . ? C10 Zr C12 C11 -36.96(9) . . . . ? C8 Zr C12 C11 -116.07(14) . . . . ? C8 C12 C13 C14 -178.69(18) . . . . ? C11 C12 C13 C14 0.4(2) . . . . ? Zr C12 C13 C14 87.23(19) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C16 -0.3(3) . . . . ? C14 C15 C16 C11 1.3(3) . . . . ? C10 C11 C16 C15 178.77(18) . . . . ? C12 C11 C16 C15 -1.5(2) . . . . ? Zr C11 C16 C15 -88.03(18) . . . . ? C9 C8 C17 C19 136.42(18) . . . . ? C12 C8 C17 C19 -54.4(2) . . . . ? Zr C8 C17 C19 43.03(19) . . . . ? C9 C8 C17 C18 15.9(2) . . . . ? C12 C8 C17 C18 -174.99(16) . . . . ? Zr C8 C17 C18 -77.53(17) . . . . ? C9 C8 C17 C20 -102.88(19) . . . . ? C12 C8 C17 C20 66.3(2) . . . . ? Zr C8 C17 C20 163.72(11) . . . . ? C9 C10 C21 C23 -152.17(17) . . . . ? C11 C10 C21 C23 43.9(3) . . . . ? Zr C10 C21 C23 -57.0(2) . . . . ? C9 C10 C21 C22 -30.5(2) . . . . ? C11 C10 C21 C22 165.51(17) . . . . ? Zr C10 C21 C22 64.65(19) . . . . ? C9 C10 C21 C24 87.5(2) . . . . ? C11 C10 C21 C24 -76.5(2) . . . . ? Zr C10 C21 C24 -177.34(11) . . . . ? C6' Zr' C1' C2' -119.36(15) . . . . ? C7' Zr' C1' C2' -141.5(2) . . . . ? C5' Zr' C1' C2' -88.96(14) . . . . ? C3' Zr' C1' C2' -23.42(13) . . . . ? C4' Zr' C1' C2' -53.63(14) . . . . ? C9' Zr' C1' C2' 95.38(14) . . . . ? C10' Zr' C1' C2' 81.42(18) . . . . ? C8' Zr' C1' C2' 128.05(13) . . . . ? C11' Zr' C1' C2' 158.00(16) . . . . ? C12' Zr' C1' C2' 158.40(12) . . . . ? C6' Zr' C1' C7' 22.15(13) . . . . ? C2' Zr' C1' C7' 141.5(2) . . . . ? C5' Zr' C1' C7' 52.55(14) . . . . ? C3' Zr' C1' C7' 118.09(15) . . . . ? C4' Zr' C1' C7' 87.88(14) . . . . ? C9' Zr' C1' C7' -123.10(13) . . . . ? C10' Zr' C1' C7' -137.07(14) . . . . ? C8' Zr' C1' C7' -90.43(14) . . . . ? C11' Zr' C1' C7' -60.5(2) . . . . ? C12' Zr' C1' C7' -60.09(15) . . . . ? C7' C1' C2' C3' 0.4(4) . . . . ? Zr' C1' C2' C3' 49.2(2) . . . . ? C7' C1' C2' Zr' -48.8(2) . . . . ? C6' Zr' C2' C1' 53.34(14) . . . . ? C7' Zr' C2' C1' 23.26(14) . . . . ? C5' Zr' C2' C1' 88.76(15) . . . . ? C3' Zr' C2' C1' 141.2(2) . . . . ? C4' Zr' C2' C1' 118.63(15) . . . . ? C9' Zr' C2' C1' -103.25(14) . . . . ? C10' Zr' C2' C1' -137.87(13) . . . . ? C8' Zr' C2' C1' -66.56(16) . . . . ? C11' Zr' C2' C1' -148.4(2) . . . . ? C12' Zr' C2' C1' -44.9(2) . . . . ? C6' Zr' C2' C3' -87.82(14) . . . . ? C7' Zr' C2' C3' -117.90(15) . . . . ? C1' Zr' C2' C3' -141.2(2) . . . . ? C5' Zr' C2' C3' -52.40(13) . . . . ? C4' Zr' C2' C3' -22.53(12) . . . . ? C9' Zr' C2' C3' 115.59(13) . . . . ? C10' Zr' C2' C3' 80.97(15) . . . . ? C8' Zr' C2' C3' 152.28(11) . . . . ? C11' Zr' C2' C3' 70.4(3) . . . . ? C12' Zr' C2' C3' 173.98(14) . . . . ? C1' C2' C3' C4' -0.1(4) . . . . ? Zr' C2' C3' C4' 48.9(2) . . . . ? C1' C2' C3' Zr' -49.0(2) . . . . ? C6' Zr' C3' C4' -52.53(13) . . . . ? C7' Zr' C3' C4' -87.91(13) . . . . ? C1' Zr' C3' C4' -118.91(14) . . . . ? C2' Zr' C3' C4' -142.3(2) . . . . ? C5' Zr' C3' C4' -22.11(12) . . . . ? C9' Zr' C3' C4' 132.31(12) . . . . ? C10' Zr' C3' C4' 95.11(13) . . . . ? C8' Zr' C3' C4' 162.74(12) . . . . ? C11' Zr' C3' C4' 60.28(16) . . . . ? C12' Zr' C3' C4' 52.5(4) . . . . ? C6' Zr' C3' C2' 89.77(14) . . . . ? C7' Zr' C3' C2' 54.39(14) . . . . ? C1' Zr' C3' C2' 23.39(13) . . . . ? C5' Zr' C3' C2' 120.19(14) . . . . ? C4' Zr' C3' C2' 142.3(2) . . . . ? C9' Zr' C3' C2' -85.39(14) . . . . ? C10' Zr' C3' C2' -122.59(13) . . . . ? C8' Zr' C3' C2' -55.0(2) . . . . ? C11' Zr' C3' C2' -157.42(12) . . . . ? C12' Zr' C3' C2' -165.2(3) . . . . ? C2' C3' C4' C5' -1.9(4) . . . . ? Zr' C3' C4' C5' 46.6(2) . . . . ? C2' C3' C4' Zr' -48.5(2) . . . . ? C6' Zr' C4' C3' 119.96(14) . . . . ? C7' Zr' C4' C3' 89.25(13) . . . . ? C1' Zr' C4' C3' 53.53(13) . . . . ? C2' Zr' C4' C3' 22.84(12) . . . . ? C5' Zr' C4' C3' 143.37(19) . . . . ? C9' Zr' C4' C3' -78.90(15) . . . . ? C10' Zr' C4' C3' -102.87(12) . . . . ? C8' Zr' C4' C3' -134.8(3) . . . . ? C11' Zr' C4' C3' -139.40(12) . . . . ? C12' Zr' C4' C3' -167.81(11) . . . . ? C6' Zr' C4' C5' -23.40(12) . . . . ? C7' Zr' C4' C5' -54.12(13) . . . . ? C1' Zr' C4' C5' -89.83(13) . . . . ? C2' Zr' C4' C5' -120.53(13) . . . . ? C3' Zr' C4' C5' -143.37(19) . . . . ? C9' Zr' C4' C5' 137.74(12) . . . . ? C10' Zr' C4' C5' 113.76(12) . . . . ? C8' Zr' C4' C5' 81.9(4) . . . . ? C11' Zr' C4' C5' 77.23(13) . . . . ? C12' Zr' C4' C5' 48.83(16) . . . . ? C3' C4' C5' C6' 2.3(4) . . . . ? Zr' C4' C5' C6' 49.0(2) . . . . ? C3' C4' C5' Zr' -46.7(2) . . . . ? C7' Zr' C5' C6' -23.14(12) . . . . ? C1' Zr' C5' C6' -53.49(13) . . . . ? C2' Zr' C5' C6' -89.00(13) . . . . ? C3' Zr' C5' C6' -119.19(14) . . . . ? C4' Zr' C5' C6' -141.15(19) . . . . ? C9' Zr' C5' C6' 117.41(18) . . . . ? C10' Zr' C5' C6' 132.44(12) . . . . ? C8' Zr' C5' C6' 57.13(17) . . . . ? C11' Zr' C5' C6' 104.91(13) . . . . ? C12' Zr' C5' C6' 71.36(13) . . . . ? C6' Zr' C5' C4' 141.15(19) . . . . ? C7' Zr' C5' C4' 118.01(13) . . . . ? C1' Zr' C5' C4' 87.66(13) . . . . ? C2' Zr' C5' C4' 52.14(12) . . . . ? C3' Zr' C5' C4' 21.95(11) . . . . ? C9' Zr' C5' C4' -101.44(18) . . . . ? C10' Zr' C5' C4' -86.41(13) . . . . ? C8' Zr' C5' C4' -161.72(11) . . . . ? C11' Zr' C5' C4' -113.94(12) . . . . ? C12' Zr' C5' C4' -147.49(11) . . . . ? C4' C5' C6' C7' 0.0(4) . . . . ? Zr' C5' C6' C7' 49.6(2) . . . . ? C4' C5' C6' Zr' -49.6(2) . . . . ? C1' Zr' C6' C7' -22.33(12) . . . . ? C2' Zr' C6' C7' -52.76(13) . . . . ? C5' Zr' C6' C7' -141.52(19) . . . . ? C3' Zr' C6' C7' -88.33(13) . . . . ? C4' Zr' C6' C7' -118.18(14) . . . . ? C9' Zr' C6' C7' 84.12(17) . . . . ? C10' Zr' C6' C7' 140.80(12) . . . . ? C8' Zr' C6' C7' 74.03(13) . . . . ? C11' Zr' C6' C7' 133.53(12) . . . . ? C12' Zr' C6' C7' 101.62(12) . . . . ? C7' Zr' C6' C5' 141.52(19) . . . . ? C1' Zr' C6' C5' 119.19(14) . . . . ? C2' Zr' C6' C5' 88.76(13) . . . . ? C3' Zr' C6' C5' 53.19(13) . . . . ? C4' Zr' C6' C5' 23.34(12) . . . . ? C9' Zr' C6' C5' -134.36(14) . . . . ? C10' Zr' C6' C5' -77.68(16) . . . . ? C8' Zr' C6' C5' -144.45(11) . . . . ? C11' Zr' C6' C5' -84.95(13) . . . . ? C12' Zr' C6' C5' -116.86(12) . . . . ? C5' C6' C7' C1' -2.1(4) . . . . ? Zr' C6' C7' C1' 47.7(2) . . . . ? C5' C6' C7' Zr' -49.8(2) . . . . ? C2' C1' C7' C6' 1.4(4) . . . . ? Zr' C1' C7' C6' -47.6(2) . . . . ? C2' C1' C7' Zr' 49.0(2) . . . . ? C1' Zr' C7' C6' 143.1(2) . . . . ? C2' Zr' C7' C6' 119.98(14) . . . . ? C5' Zr' C7' C6' 23.18(12) . . . . ? C3' Zr' C7' C6' 89.00(13) . . . . ? C4' Zr' C7' C6' 53.92(13) . . . . ? C9' Zr' C7' C6' -135.81(12) . . . . ? C10' Zr' C7' C6' -97.7(2) . . . . ? C8' Zr' C7' C6' -118.03(12) . . . . ? C11' Zr' C7' C6' -63.03(15) . . . . ? C12' Zr' C7' C6' -84.35(13) . . . . ? C6' Zr' C7' C1' -143.1(2) . . . . ? C2' Zr' C7' C1' -23.17(13) . . . . ? C5' Zr' C7' C1' -119.97(15) . . . . ? C3' Zr' C7' C1' -54.14(14) . . . . ? C4' Zr' C7' C1' -89.22(14) . . . . ? C9' Zr' C7' C1' 81.05(15) . . . . ? C10' Zr' C7' C1' 119.15(19) . . . . ? C8' Zr' C7' C1' 98.82(13) . . . . ? C11' Zr' C7' C1' 153.83(12) . . . . ? C12' Zr' C7' C1' 132.50(13) . . . . ? C6' Zr' C8' C9' 170.24(11) . . . . ? C7' Zr' C8' C9' -155.05(12) . . . . ? C1' Zr' C8' C9' -118.40(12) . . . . ? C2' Zr' C8' C9' -84.89(12) . . . . ? C5' Zr' C8' C9' 137.37(12) . . . . ? C3' Zr' C8' C9' -49.80(18) . . . . ? C4' Zr' C8' C9' 70.2(4) . . . . ? C10' Zr' C8' C9' 34.67(10) . . . . ? C11' Zr' C8' C9' 75.37(11) . . . . ? C12' Zr' C8' C9' 112.31(15) . . . . ? C6' Zr' C8' C12' 57.93(12) . . . . ? C7' Zr' C8' C12' 92.64(12) . . . . ? C1' Zr' C8' C12' 129.29(11) . . . . ? C2' Zr' C8' C12' 162.80(10) . . . . ? C5' Zr' C8' C12' 25.06(16) . . . . ? C3' Zr' C8' C12' -162.11(13) . . . . ? C4' Zr' C8' C12' -42.1(4) . . . . ? C9' Zr' C8' C12' -112.31(15) . . . . ? C10' Zr' C8' C12' -77.64(10) . . . . ? C11' Zr' C8' C12' -36.94(9) . . . . ? C6' Zr' C8' C17' -70.18(16) . . . . ? C7' Zr' C8' C17' -35.47(16) . . . . ? C1' Zr' C8' C17' 1.18(16) . . . . ? C2' Zr' C8' C17' 34.69(17) . . . . ? C5' Zr' C8' C17' -103.06(16) . . . . ? C3' Zr' C8' C17' 69.8(2) . . . . ? C4' Zr' C8' C17' -170.2(3) . . . . ? C9' Zr' C8' C17' 119.58(19) . . . . ? C10' Zr' C8' C17' 154.25(17) . . . . ? C11' Zr' C8' C17' -165.05(17) . . . . ? C12' Zr' C8' C17' -128.11(19) . . . . ? C12' C8' C9' C10' 2.4(2) . . . . ? C17' C8' C9' C10' 171.47(16) . . . . ? Zr' C8' C9' C10' -65.22(14) . . . . ? C12' C8' C9' Zr' 67.62(12) . . . . ? C17' C8' C9' Zr' -123.30(16) . . . . ? C6' Zr' C9' C10' 102.37(16) . . . . ? C7' Zr' C9' C10' 152.61(12) . . . . ? C1' Zr' C9' C10' -166.66(11) . . . . ? C2' Zr' C9' C10' -126.83(11) . . . . ? C5' Zr' C9' C10' 23.7(2) . . . . ? C3' Zr' C9' C10' -86.88(12) . . . . ? C4' Zr' C9' C10' -43.29(15) . . . . ? C8' Zr' C9' C10' 119.22(15) . . . . ? C11' Zr' C9' C10' 38.90(9) . . . . ? C12' Zr' C9' C10' 80.55(11) . . . . ? C6' Zr' C9' C8' -16.84(19) . . . . ? C7' Zr' C9' C8' 33.40(15) . . . . ? C1' Zr' C9' C8' 74.12(12) . . . . ? C2' Zr' C9' C8' 113.95(11) . . . . ? C5' Zr' C9' C8' -95.56(19) . . . . ? C3' Zr' C9' C8' 153.90(10) . . . . ? C4' Zr' C9' C8' -162.51(11) . . . . ? C10' Zr' C9' C8' -119.22(15) . . . . ? C11' Zr' C9' C8' -80.32(11) . . . . ? C12' Zr' C9' C8' -38.66(9) . . . . ? C8' C9' C10' C11' -1.7(2) . . . . ? Zr' C9' C10' C11' -66.89(12) . . . . ? C8' C9' C10' C21' -173.68(16) . . . . ? Zr' C9' C10' C21' 121.13(17) . . . . ? C8' C9' C10' Zr' 65.18(14) . . . . ? C6' Zr' C10' C9' -125.29(13) . . . . ? C7' Zr' C10' C9' -59.3(2) . . . . ? C1' Zr' C10' C9' 23.37(18) . . . . ? C2' Zr' C10' C9' 72.75(13) . . . . ? C5' Zr' C10' C9' -168.23(11) . . . . ? C3' Zr' C10' C9' 113.11(11) . . . . ? C4' Zr' C10' C9' 152.23(11) . . . . ? C8' Zr' C10' C9' -35.01(10) . . . . ? C11' Zr' C10' C9' -112.62(15) . . . . ? C12' Zr' C10' C9' -75.32(11) . . . . ? C6' Zr' C10' C11' -12.67(17) . . . . ? C7' Zr' C10' C11' 53.3(2) . . . . ? C1' Zr' C10' C11' 135.99(14) . . . . ? C2' Zr' C10' C11' -174.63(11) . . . . ? C5' Zr' C10' C11' -55.61(13) . . . . ? C3' Zr' C10' C11' -134.27(11) . . . . ? C4' Zr' C10' C11' -95.15(11) . . . . ? C9' Zr' C10' C11' 112.62(15) . . . . ? C8' Zr' C10' C11' 77.61(11) . . . . ? C12' Zr' C10' C11' 37.30(10) . . . . ? C6' Zr' C10' C21' 111.92(16) . . . . ? C7' Zr' C10' C21' 177.88(19) . . . . ? C1' Zr' C10' C21' -99.42(18) . . . . ? C2' Zr' C10' C21' -50.04(18) . . . . ? C5' Zr' C10' C21' 68.98(16) . . . . ? C3' Zr' C10' C21' -9.68(17) . . . . ? C4' Zr' C10' C21' 29.44(16) . . . . ? C9' Zr' C10' C21' -122.79(19) . . . . ? C8' Zr' C10' C21' -157.80(17) . . . . ? C11' Zr' C10' C21' 124.59(19) . . . . ? C12' Zr' C10' C21' 161.89(17) . . . . ? C9' C10' C11' C16' 179.08(18) . . . . ? C21' C10' C11' C16' -9.1(3) . . . . ? Zr' C10' C11' C16' 112.4(2) . . . . ? C9' C10' C11' C12' 0.3(2) . . . . ? C21' C10' C11' C12' 172.15(16) . . . . ? Zr' C10' C11' C12' -66.39(12) . . . . ? C9' C10' C11' Zr' 66.71(12) . . . . ? C21' C10' C11' Zr' -121.46(18) . . . . ? C6' Zr' C11' C16' 41.96(15) . . . . ? C7' Zr' C11' C16' 74.84(16) . . . . ? C1' Zr' C11' C16' 115.9(2) . . . . ? C2' Zr' C11' C16' -115.1(3) . . . . ? C5' Zr' C11' C16' 5.84(15) . . . . ? C3' Zr' C11' C16' -62.22(17) . . . . ? C4' Zr' C11' C16' -29.31(16) . . . . ? C9' Zr' C11' C16' -167.65(16) . . . . ? C10' Zr' C11' C16' -129.70(19) . . . . ? C8' Zr' C11' C16' 151.80(16) . . . . ? C12' Zr' C11' C16' 115.27(18) . . . . ? C6' Zr' C11' C10' 171.66(11) . . . . ? C7' Zr' C11' C10' -155.46(12) . . . . ? C1' Zr' C11' C10' -114.42(19) . . . . ? C2' Zr' C11' C10' 14.6(3) . . . . ? C5' Zr' C11' C10' 135.54(11) . . . . ? C3' Zr' C11' C10' 67.48(14) . . . . ? C4' Zr' C11' C10' 100.39(11) . . . . ? C9' Zr' C11' C10' -37.95(10) . . . . ? C8' Zr' C11' C10' -78.50(11) . . . . ? C12' Zr' C11' C10' -115.02(15) . . . . ? C6' Zr' C11' C12' -73.31(12) . . . . ? C7' Zr' C11' C12' -40.44(14) . . . . ? C1' Zr' C11' C12' 0.6(2) . . . . ? C2' Zr' C11' C12' 129.7(2) . . . . ? C5' Zr' C11' C12' -109.44(11) . . . . ? C3' Zr' C11' C12' -177.50(11) . . . . ? C4' Zr' C11' C12' -144.59(10) . . . . ? C9' Zr' C11' C12' 77.07(11) . . . . ? C10' Zr' C11' C12' 115.02(15) . . . . ? C8' Zr' C11' C12' 36.52(9) . . . . ? C9' C8' C12' C13' 178.07(19) . . . . ? C17' C8' C12' C13' 9.9(3) . . . . ? Zr' C8' C12' C13' -115.2(2) . . . . ? C9' C8' C12' C11' -2.09(19) . . . . ? C17' C8' C12' C11' -170.26(17) . . . . ? Zr' C8' C12' C11' 64.67(12) . . . . ? C9' C8' C12' Zr' -66.77(12) . . . . ? C17' C8' C12' Zr' 125.07(18) . . . . ? C16' C11' C12' C13' 2.0(2) . . . . ? C10' C11' C12' C13' -179.00(15) . . . . ? Zr' C11' C12' C13' 115.10(15) . . . . ? C16' C11' C12' C8' -177.82(15) . . . . ? C10' C11' C12' C8' 1.13(19) . . . . ? Zr' C11' C12' C8' -64.77(12) . . . . ? C16' C11' C12' Zr' -113.06(15) . . . . ? C10' C11' C12' Zr' 65.90(12) . . . . ? C6' Zr' C12' C13' 1.13(15) . . . . ? C7' Zr' C12' C13' 36.49(16) . . . . ? C1' Zr' C12' C13' 67.56(16) . . . . ? C2' Zr' C12' C13' 97.0(2) . . . . ? C5' Zr' C12' C13' -32.37(16) . . . . ? C3' Zr' C12' C13' -103.0(4) . . . . ? C4' Zr' C12' C13' -60.05(17) . . . . ? C9' Zr' C12' C13' 169.83(17) . . . . ? C10' Zr' C12' C13' -149.97(16) . . . . ? C8' Zr' C12' C13' 131.33(19) . . . . ? C11' Zr' C12' C13' -112.72(18) . . . . ? C6' Zr' C12' C8' -130.20(11) . . . . ? C7' Zr' C12' C8' -94.84(12) . . . . ? C1' Zr' C12' C8' -63.76(13) . . . . ? C2' Zr' C12' C8' -34.3(2) . . . . ? C5' Zr' C12' C8' -163.70(10) . . . . ? C3' Zr' C12' C8' 125.7(4) . . . . ? C4' Zr' C12' C8' 168.62(11) . . . . ? C9' Zr' C12' C8' 38.50(10) . . . . ? C10' Zr' C12' C8' 78.70(11) . . . . ? C11' Zr' C12' C8' 115.95(15) . . . . ? C6' Zr' C12' C11' 113.85(12) . . . . ? C7' Zr' C12' C11' 149.21(11) . . . . ? C1' Zr' C12' C11' -179.72(11) . . . . ? C2' Zr' C12' C11' -150.25(15) . . . . ? C5' Zr' C12' C11' 80.35(12) . . . . ? C3' Zr' C12' C11' 9.7(4) . . . . ? C4' Zr' C12' C11' 52.67(14) . . . . ? C9' Zr' C12' C11' -77.45(11) . . . . ? C10' Zr' C12' C11' -37.26(10) . . . . ? C8' Zr' C12' C11' -115.95(15) . . . . ? C8' C12' C13' C14' 179.47(18) . . . . ? C11' C12' C13' C14' -0.4(3) . . . . ? Zr' C12' C13' C14' 84.83(19) . . . . ? C12' C13' C14' C15' -1.3(3) . . . . ? C13' C14' C15' C16' 1.2(3) . . . . ? C14' C15' C16' C11' 0.5(3) . . . . ? C10' C11' C16' C15' 179.20(18) . . . . ? C12' C11' C16' C15' -2.1(3) . . . . ? Zr' C11' C16' C15' -88.60(18) . . . . ? C9' C8' C17' C19' 152.26(17) . . . . ? C12' C8' C17' C19' -41.5(3) . . . . ? Zr' C8' C17' C19' 58.90(19) . . . . ? C9' C8' C17' C18' 30.6(2) . . . . ? C12' C8' C17' C18' -163.12(17) . . . . ? Zr' C8' C17' C18' -62.77(19) . . . . ? C9' C8' C17' C20' -87.6(2) . . . . ? C12' C8' C17' C20' 78.7(2) . . . . ? Zr' C8' C17' C20' 179.02(11) . . . . ? C9' C10' C21' C22' -3.0(3) . . . . ? C11' C10' C21' C22' -173.20(17) . . . . ? Zr' C10' C21' C22' 91.22(17) . . . . ? C9' C10' C21' C23' -123.83(19) . . . . ? C11' C10' C21' C23' 65.9(2) . . . . ? Zr' C10' C21' C23' -29.7(2) . . . . ? C9' C10' C21' C24' 115.57(19) . . . . ? C11' C10' C21' C24' -54.7(2) . . . . ? Zr' C10' C21' C24' -150.25(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.748 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.060 _iucr_refine_instructions ; TITL andyg44 in P-1 CELL 0.71073 10.0987 14.0383 15.6547 66.262 82.216 84.290 ZERR 4.00 0.0004 0.0006 0.0010 0.006 0.004 0.004 LATT 1 SFAC C H ZR UNIT 96 120 4 SIZE 0.14 0.09 0.05 TEMP -173 SHEL 999 0.78 ACTA CONF FMAP 2 PLAN 10 L.S. 4 SADI c1 H1 C2 H2 C3 H3 C4 H4 C5 H5 C6 H6 C7 H7 C9 H9 c1' H1' C2' H2' C3' H3' = C4' H4' C5' H5' C6' H6' C7' H7' C9' H9' OMIT 3 3 4 OMIT 0 -1 6 OMIT 1 4 2 OMIT 0 -3 6 OMIT -1 -3 3 OMIT 3 -3 5 OMIT 0 -1 2 OMIT -2 2 3 OMIT 2 -4 4 OMIT 4 0 3 OMIT -1 -4 3 WGHT 0.000000 FVAR 1.65845 ZR 3 -0.004332 0.722538 0.125754 11.00000 0.01426 0.01874 = 0.01126 -0.00539 0.00138 0.00162 C1 1 -0.006109 0.769028 -0.034043 11.00000 0.02369 0.03789 = 0.01154 -0.00873 -0.00175 0.00448 H1 2 -0.068511 0.808349 -0.073328 11.00000 -1.20000 C2 1 0.099430 0.819854 -0.022013 11.00000 0.02776 0.02284 = 0.01600 -0.00200 0.00418 -0.00146 H2 2 0.098108 0.892264 -0.054160 11.00000 -1.20000 C3 1 0.200674 0.776719 0.039196 11.00000 0.01661 0.02352 = 0.02510 -0.01021 0.00599 -0.00453 H3 2 0.255954 0.823234 0.043121 11.00000 -1.20000 C4 1 0.221637 0.672185 0.103732 11.00000 0.01396 0.02936 = 0.02533 -0.01222 -0.00185 0.00450 H4 2 0.287027 0.660670 0.142343 11.00000 -1.20000 C5 1 0.144434 0.585563 0.123087 11.00000 0.02212 0.01872 = 0.02874 -0.00486 -0.00076 0.00524 H5 2 0.166747 0.527339 0.173487 11.00000 -1.20000 C6 1 0.030279 0.580859 0.081334 11.00000 0.02007 0.02017 = 0.03329 -0.01147 0.00510 -0.00280 H6 2 -0.010586 0.517964 0.110084 11.00000 -1.20000 C7 1 -0.035990 0.661921 0.010992 11.00000 0.02086 0.03644 = 0.02700 -0.02289 0.00247 -0.00107 H7 2 -0.114324 0.641593 0.001607 11.00000 -1.20000 C8 1 -0.226062 0.786617 0.183561 11.00000 0.01028 0.01645 = 0.01109 -0.00880 0.00029 -0.00014 C9 1 -0.126918 0.847220 0.190331 11.00000 0.01523 0.01149 = 0.01354 -0.00426 0.00195 0.00013 H9 2 -0.124149 0.917641 0.152823 11.00000 -1.20000 C10 1 -0.036567 0.787546 0.255640 11.00000 0.01140 0.01579 = 0.01076 -0.00627 0.00097 0.00068 C11 1 -0.085398 0.683400 0.296873 11.00000 0.00900 0.01641 = 0.00949 -0.00737 0.00183 0.00053 C12 1 -0.201631 0.683598 0.251884 11.00000 0.00904 0.01484 = 0.00838 -0.00584 0.00191 -0.00050 C13 1 -0.269190 0.588609 0.281366 11.00000 0.01032 0.02176 = 0.01492 -0.01042 -0.00009 -0.00051 AFIX 43 H13 2 -0.345341 0.586795 0.252560 11.00000 -1.20000 AFIX 0 C14 1 -0.223673 0.501279 0.350695 11.00000 0.01769 0.01374 = 0.01637 -0.00539 0.00408 -0.00445 AFIX 43 H14 2 -0.269241 0.438700 0.370400 11.00000 -1.20000 AFIX 0 C15 1 -0.110002 0.501569 0.394102 11.00000 0.02171 0.01531 = 0.01136 -0.00334 -0.00276 0.00080 AFIX 43 H15 2 -0.081042 0.439203 0.442600 11.00000 -1.20000 AFIX 0 C16 1 -0.041217 0.588748 0.368202 11.00000 0.01499 0.02182 = 0.00966 -0.00813 -0.00153 -0.00040 AFIX 43 H16 2 0.036100 0.586793 0.397449 11.00000 -1.20000 AFIX 0 C17 1 -0.345084 0.829015 0.126177 11.00000 0.01173 0.01730 = 0.01754 -0.00730 -0.00350 0.00168 C18 1 -0.323098 0.941336 0.055186 11.00000 0.01870 0.02627 = 0.02674 -0.00613 -0.00975 0.00423 AFIX 137 H18A 2 -0.322722 0.986914 0.088881 11.00000 -1.50000 H18B 2 -0.395437 0.965050 0.014326 11.00000 -1.50000 H18C 2 -0.237117 0.943655 0.017090 11.00000 -1.50000 AFIX 0 C19 1 -0.370132 0.765027 0.071051 11.00000 0.02002 0.02880 = 0.02548 -0.01211 -0.01394 0.00484 AFIX 137 H19A 2 -0.293097 0.768053 0.024805 11.00000 -1.50000 H19B 2 -0.450579 0.793628 0.038709 11.00000 -1.50000 H19C 2 -0.382753 0.692441 0.114353 11.00000 -1.50000 AFIX 0 C20 1 -0.471114 0.829320 0.194104 11.00000 0.01558 0.02938 = 0.02972 -0.01249 -0.00269 0.00246 AFIX 137 H20A 2 -0.488317 0.757722 0.238176 11.00000 -1.50000 H20B 2 -0.548129 0.859289 0.158221 11.00000 -1.50000 H20C 2 -0.456845 0.871141 0.229006 11.00000 -1.50000 AFIX 0 C21 1 0.067211 0.833398 0.288790 11.00000 0.01378 0.01842 = 0.01704 -0.00615 -0.00358 -0.00202 C22 1 0.113886 0.936340 0.211151 11.00000 0.02793 0.02479 = 0.02405 -0.00851 -0.00380 -0.01191 AFIX 137 H22A 2 0.155389 0.923657 0.156119 11.00000 -1.50000 H22B 2 0.179255 0.965234 0.233900 11.00000 -1.50000 H22C 2 0.036828 0.985882 0.193843 11.00000 -1.50000 AFIX 0 C23 1 0.191282 0.761511 0.319028 11.00000 0.01911 0.02755 = 0.04611 -0.01106 -0.01301 -0.00467 AFIX 137 H23A 2 0.166308 0.700427 0.375979 11.00000 -1.50000 H23B 2 0.257870 0.799059 0.331710 11.00000 -1.50000 H23C 2 0.229207 0.738961 0.268781 11.00000 -1.50000 AFIX 0 C24 1 -0.002796 0.855751 0.373286 11.00000 0.02962 0.04492 = 0.02395 -0.02020 -0.00273 -0.01153 AFIX 137 H24A 2 -0.081111 0.903385 0.354067 11.00000 -1.50000 H24B 2 0.059651 0.887730 0.395438 11.00000 -1.50000 H24C 2 -0.031357 0.790325 0.423976 11.00000 -1.50000 AFIX 0 ZR' 3 0.502212 0.198986 0.292218 11.00000 0.01751 0.01808 = 0.01659 -0.00898 0.00102 -0.00492 C1' 1 0.553713 0.031729 0.297212 11.00000 0.02577 0.02571 = 0.05721 -0.02554 -0.00919 0.00175 H1' 2 0.622048 -0.011684 0.325028 11.00000 -1.20000 C2' 1 0.432229 0.028505 0.355410 11.00000 0.03062 0.01970 = 0.04028 -0.00890 0.00007 -0.00663 H2' 2 0.431827 -0.018240 0.417512 11.00000 -1.20000 C3' 1 0.316099 0.096644 0.333370 11.00000 0.02097 0.02745 = 0.03358 -0.01132 0.00747 -0.01074 H3' 2 0.253890 0.082796 0.383972 11.00000 -1.20000 C4' 1 0.293120 0.183079 0.249624 11.00000 0.01977 0.02819 = 0.03076 -0.01533 -0.00286 -0.00263 H4' 2 0.215349 0.222458 0.255122 11.00000 -1.20000 C5' 1 0.381561 0.226211 0.166432 11.00000 0.03158 0.03696 = 0.02568 -0.01453 -0.00789 -0.00842 H5' 2 0.353639 0.290913 0.123910 11.00000 -1.20000 C6' 1 0.513106 0.190144 0.146736 11.00000 0.03091 0.05007 = 0.02475 -0.02351 0.00508 -0.01953 H6' 2 0.558277 0.233140 0.091846 11.00000 -1.20000 C7' 1 0.588146 0.103668 0.203951 11.00000 0.02053 0.04893 = 0.05097 -0.03960 0.00845 -0.01076 H7' 2 0.677308 0.096067 0.182230 11.00000 -1.20000 C8' 1 0.710583 0.253029 0.330450 11.00000 0.01066 0.01492 = 0.01411 -0.00892 0.00060 -0.00060 C9' 1 0.606896 0.252803 0.401518 11.00000 0.01804 0.01593 = 0.00864 -0.00447 -0.00084 -0.00079 H9' 2 0.611335 0.208979 0.462634 11.00000 -1.20000 C10' 1 0.504278 0.328743 0.366208 11.00000 0.01090 0.01549 = 0.01254 -0.00771 -0.00071 -0.00083 C11' 1 0.545714 0.382980 0.267517 11.00000 0.01142 0.01390 = 0.01378 -0.00893 -0.00194 -0.00275 C12' 1 0.674036 0.336734 0.246019 11.00000 0.01033 0.01420 = 0.01417 -0.00854 -0.00203 -0.00223 C13' 1 0.735854 0.379629 0.151669 11.00000 0.01214 0.01970 = 0.01814 -0.01053 0.00299 -0.00510 AFIX 43 H13' 2 0.820144 0.351267 0.135501 11.00000 -1.20000 AFIX 0 C14' 1 0.674795 0.460609 0.085112 11.00000 0.02552 0.02075 = 0.01233 -0.00683 0.00362 -0.00928 AFIX 43 H14' 2 0.718164 0.489079 0.023046 11.00000 -1.20000 AFIX 0 C15' 1 0.548076 0.503700 0.105889 11.00000 0.02406 0.01351 = 0.01584 -0.00291 -0.00911 -0.00092 AFIX 43 H15' 2 0.507050 0.559535 0.057482 11.00000 -1.20000 AFIX 0 C16' 1 0.484376 0.466134 0.194296 11.00000 0.01222 0.01500 = 0.02481 -0.01129 -0.00626 0.00189 AFIX 43 H16' 2 0.398952 0.495294 0.207305 11.00000 -1.20000 AFIX 0 C17' 1 0.842828 0.189394 0.350419 11.00000 0.01220 0.02160 = 0.01509 -0.00892 -0.00131 0.00420 C18' 1 0.823334 0.088966 0.438606 11.00000 0.01800 0.02150 = 0.02761 -0.00897 -0.00853 0.00672 AFIX 137 H18D 2 0.790353 0.106446 0.492612 11.00000 -1.50000 H18E 2 0.908984 0.048890 0.449880 11.00000 -1.50000 H18F 2 0.758194 0.047320 0.429741 11.00000 -1.50000 AFIX 0 C19' 1 0.907521 0.159351 0.269893 11.00000 0.02576 0.04242 = 0.03002 -0.02145 -0.00720 0.01692 AFIX 137 H19D 2 0.844891 0.120309 0.255367 11.00000 -1.50000 H19E 2 0.989315 0.115950 0.288476 11.00000 -1.50000 H19F 2 0.929765 0.222563 0.214291 11.00000 -1.50000 AFIX 0 C20' 1 0.940226 0.255276 0.368186 11.00000 0.01274 0.03283 = 0.03771 -0.01473 -0.00606 0.00509 AFIX 137 H20D 2 0.953575 0.320197 0.312584 11.00000 -1.50000 H20E 2 1.026244 0.216145 0.381093 11.00000 -1.50000 H20F 2 0.902961 0.271492 0.422208 11.00000 -1.50000 AFIX 0 C21' 1 0.384475 0.357222 0.424296 11.00000 0.01157 0.02485 = 0.01632 -0.01140 0.00084 0.00220 C22' 1 0.386550 0.286856 0.528266 11.00000 0.02649 0.05220 = 0.02072 -0.01541 0.00766 0.01175 AFIX 137 H22D 2 0.312299 0.308410 0.564879 11.00000 -1.50000 H22E 2 0.471517 0.292576 0.549149 11.00000 -1.50000 H22F 2 0.377165 0.214465 0.537435 11.00000 -1.50000 AFIX 0 C23' 1 0.250941 0.346832 0.393754 11.00000 0.01250 0.03579 = 0.03003 -0.01601 0.00494 -0.00005 AFIX 137 H23D 2 0.247807 0.391476 0.327126 11.00000 -1.50000 H23E 2 0.177390 0.368193 0.430982 11.00000 -1.50000 H23F 2 0.242048 0.274170 0.403579 11.00000 -1.50000 AFIX 0 C24' 1 0.393931 0.470690 0.413003 11.00000 0.01926 0.03779 = 0.03558 -0.02662 0.00711 0.00128 AFIX 137 H24D 2 0.385725 0.517760 0.347550 11.00000 -1.50000 H24E 2 0.480468 0.478685 0.430496 11.00000 -1.50000 H24F 2 0.321610 0.487756 0.453784 11.00000 -1.50000 HKLF 4 ; #============================================================================= # end of cif data for "andyg44" (compound 5) #============================================================================= #============================================================================= # cif data for "andyg47" (compound 6) #============================================================================= data_andyg47 _database_code_depnum_ccdc_archive 'CCDC 853657' #TrackingRef '- BulkyCp-final-121111.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 Zr' _chemical_formula_weight 461.77 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 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6123(8) _cell_length_b 21.0921(12) _cell_length_c 16.3638(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.805(6) _cell_angle_gamma 90.00 _cell_volume 4497.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13257 _cell_measurement_theta_min 2.2993 _cell_measurement_theta_max 29.3086 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92357 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 140503 _diffrn_reflns_av_R_equivalents 0.1569 _diffrn_reflns_av_sigmaI/netI 0.1694 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9188 _reflns_number_gt 4557 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogens of the two seven-membered rings were refined freely. The hydrogens of the C9 and C9'atoms were refined freely, others riding. ; _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9188 _refine_ls_number_parameters 571 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.48631(3) 0.26957(2) 0.59234(3) 0.02244(12) Uani 1 1 d . . . C1 C 0.4630(4) 0.3611(2) 0.6658(3) 0.0438(14) Uani 1 1 d D . . H1 H 0.484(3) 0.3998(11) 0.662(3) 0.053 Uiso 1 1 d D . . C2 C 0.3673(4) 0.3452(2) 0.6081(3) 0.0346(13) Uani 1 1 d D . . H2 H 0.349(3) 0.3792(13) 0.581(2) 0.041 Uiso 1 1 d D . . C3 C 0.3159(4) 0.2870(3) 0.5923(3) 0.0415(14) Uani 1 1 d D . . H3 H 0.264(2) 0.285(2) 0.5473(18) 0.050 Uiso 1 1 d D . . C4 C 0.3481(5) 0.2285(3) 0.6285(4) 0.0591(17) Uani 1 1 d D . . H4 H 0.313(3) 0.1952(16) 0.606(3) 0.071 Uiso 1 1 d D . . C5 C 0.4411(6) 0.2130(3) 0.6965(5) 0.0631(19) Uani 1 1 d D . . H5 H 0.453(4) 0.1729(10) 0.706(3) 0.076 Uiso 1 1 d D . . C6 C 0.5221(5) 0.2548(3) 0.7373(3) 0.0529(18) Uani 1 1 d D . . H6 H 0.573(2) 0.235(2) 0.771(2) 0.064 Uiso 1 1 d D . . C7 C 0.5321(4) 0.3190(3) 0.7247(3) 0.0474(15) Uani 1 1 d D . . H7 H 0.5942(18) 0.334(2) 0.746(3) 0.057 Uiso 1 1 d D . . C8 C 0.6109(3) 0.28921(18) 0.5093(2) 0.0181(10) Uani 1 1 d . . . C9 C 0.5318(3) 0.25119(19) 0.4580(3) 0.0185(11) Uani 1 1 d D . . H9 H 0.486(2) 0.2635(17) 0.4120(15) 0.022 Uiso 1 1 d D . . C10 C 0.5290(3) 0.19051(19) 0.4934(3) 0.0205(11) Uani 1 1 d . . . C11 C 0.6135(3) 0.1891(2) 0.5703(3) 0.0241(11) Uani 1 1 d . . . C12 C 0.6637(3) 0.24910(18) 0.5795(3) 0.0201(11) Uani 1 1 d . . . C13 C 0.7513(3) 0.2597(2) 0.6524(3) 0.0276(11) Uani 1 1 d . . . H13 H 0.7846 0.2997 0.6612 0.033 Uiso 1 1 calc R . . C14 C 0.7852(3) 0.2118(2) 0.7081(3) 0.0308(12) Uani 1 1 d . . . H14 H 0.8432 0.2186 0.7561 0.037 Uiso 1 1 calc R . . C15 C 0.7369(3) 0.1525(2) 0.6968(3) 0.0298(12) Uani 1 1 d . . . H15 H 0.7640 0.1200 0.7373 0.036 Uiso 1 1 calc R . . C16 C 0.6537(3) 0.13959(19) 0.6308(3) 0.0224(11) Uani 1 1 d . . . H16 H 0.6226 0.0989 0.6244 0.027 Uiso 1 1 calc R . . C17 C 0.6409(3) 0.35529(18) 0.4924(3) 0.0202(10) Uani 1 1 d . . . H17 H 0.6759 0.3750 0.5489 0.024 Uiso 1 1 calc R . . C18 C 0.5496(3) 0.39715(19) 0.4488(3) 0.0309(12) Uani 1 1 d . . . H18A H 0.5118 0.3779 0.3935 0.037 Uiso 1 1 calc R . . H18B H 0.5024 0.3991 0.4849 0.037 Uiso 1 1 calc R . . C19 C 0.5813(3) 0.4638(2) 0.4334(3) 0.0380(13) Uani 1 1 d . . . H19A H 0.6131 0.4848 0.4888 0.046 Uiso 1 1 calc R . . H19B H 0.5197 0.4885 0.4028 0.046 Uiso 1 1 calc R . . C20 C 0.6571(3) 0.4634(2) 0.3810(3) 0.0302(12) Uani 1 1 d . . . H20A H 0.6801 0.5072 0.3750 0.036 Uiso 1 1 calc R . . H20B H 0.6233 0.4466 0.3232 0.036 Uiso 1 1 calc R . . C21 C 0.7494(3) 0.4222(2) 0.4246(3) 0.0302(12) Uani 1 1 d . . . H21A H 0.7963 0.4201 0.3884 0.036 Uiso 1 1 calc R . . H21B H 0.7872 0.4417 0.4798 0.036 Uiso 1 1 calc R . . C22 C 0.7166(3) 0.35574(19) 0.4402(3) 0.0222(11) Uani 1 1 d . . . H22A H 0.6848 0.3349 0.3846 0.027 Uiso 1 1 calc R . . H22B H 0.7780 0.3309 0.4705 0.027 Uiso 1 1 calc R . . C23 C 0.4585(3) 0.13581(19) 0.4593(3) 0.0215(11) Uani 1 1 d . . . H23 H 0.4481 0.1126 0.5095 0.026 Uiso 1 1 calc R . . C24 C 0.5049(3) 0.08939(18) 0.4102(3) 0.0204(10) Uani 1 1 d . . . H24A H 0.5716 0.0741 0.4475 0.024 Uiso 1 1 calc R . . H24B H 0.5179 0.1114 0.3608 0.024 Uiso 1 1 calc R . . C25 C 0.4348(3) 0.03300(19) 0.3784(3) 0.0266(11) Uani 1 1 d . . . H25A H 0.4287 0.0080 0.4279 0.032 Uiso 1 1 calc R . . H25B H 0.4657 0.0053 0.3436 0.032 Uiso 1 1 calc R . . C26 C 0.3281(3) 0.0533(2) 0.3249(3) 0.0288(12) Uani 1 1 d . . . H26A H 0.3327 0.0729 0.2712 0.035 Uiso 1 1 calc R . . H26B H 0.2833 0.0155 0.3100 0.035 Uiso 1 1 calc R . . C27 C 0.2817(3) 0.1001(2) 0.3732(3) 0.0329(12) Uani 1 1 d . . . H27A H 0.2690 0.0788 0.4231 0.039 Uiso 1 1 calc R . . H27B H 0.2150 0.1152 0.3357 0.039 Uiso 1 1 calc R . . C28 C 0.3525(3) 0.1565(2) 0.4035(3) 0.0304(12) Uani 1 1 d . . . H28A H 0.3213 0.1855 0.4364 0.036 Uiso 1 1 calc R . . H28B H 0.3602 0.1799 0.3533 0.036 Uiso 1 1 calc R . . Zr' Zr 0.11410(3) 0.38128(2) 0.26384(3) 0.02517(13) Uani 1 1 d . . . C1' C 0.1246(8) 0.3826(4) 0.4063(4) 0.078(2) Uani 1 1 d D . . H1' H 0.092(4) 0.409(2) 0.428(3) 0.093 Uiso 1 1 d D . . C2' C 0.0598(5) 0.3331(4) 0.3703(4) 0.0590(18) Uani 1 1 d D . . H2' H 0.002(2) 0.333(2) 0.382(3) 0.071 Uiso 1 1 d D . . C3' C 0.0750(4) 0.2857(3) 0.3205(4) 0.0469(15) Uani 1 1 d D . . H3' H 0.030(3) 0.2569(16) 0.304(3) 0.056 Uiso 1 1 d D . . C4' C 0.1580(5) 0.2741(3) 0.2905(3) 0.0474(15) Uani 1 1 d D . . H4' H 0.139(3) 0.2437(15) 0.257(2) 0.057 Uiso 1 1 d D . . C5' C 0.2471(6) 0.3074(4) 0.3017(5) 0.070(2) Uani 1 1 d D . . H5' H 0.281(4) 0.292(2) 0.270(3) 0.084 Uiso 1 1 d D . . C6' C 0.2781(5) 0.3640(5) 0.3498(7) 0.099(4) Uani 1 1 d D . . H6' H 0.329(3) 0.371(3) 0.331(4) 0.119 Uiso 1 1 d D . . C7' C 0.2218(9) 0.3966(4) 0.3977(5) 0.110(4) Uani 1 1 d D . . H7' H 0.254(4) 0.4318(17) 0.412(4) 0.132 Uiso 1 1 d D . . C8' C 0.0645(3) 0.49662(19) 0.2414(3) 0.0211(11) Uani 1 1 d . . . C9' C -0.0098(3) 0.4624(2) 0.1790(3) 0.0213(11) Uani 1 1 d D . . H9' H -0.0721(15) 0.4602(18) 0.179(2) 0.026 Uiso 1 1 d D . . C10' C 0.0353(3) 0.43176(19) 0.1224(3) 0.0205(10) Uani 1 1 d . . . C11' C 0.1402(3) 0.45110(19) 0.1460(3) 0.0212(11) Uani 1 1 d . . . C12' C 0.1606(3) 0.4880(2) 0.2203(3) 0.0242(11) Uani 1 1 d . . . C13' C 0.2579(3) 0.5170(2) 0.2557(3) 0.0274(12) Uani 1 1 d . . . H13' H 0.2700 0.5448 0.3033 0.033 Uiso 1 1 calc R . . C14' C 0.3332(3) 0.5033(2) 0.2187(3) 0.0329(12) Uani 1 1 d . . . H14' H 0.3997 0.5206 0.2426 0.040 Uiso 1 1 calc R . . C15' C 0.3152(3) 0.4638(2) 0.1455(3) 0.0333(12) Uani 1 1 d . . . H15' H 0.3692 0.4558 0.1208 0.040 Uiso 1 1 calc R . . C16' C 0.2218(3) 0.43747(19) 0.1108(3) 0.0275(11) Uani 1 1 d . . . H16' H 0.2108 0.4100 0.0630 0.033 Uiso 1 1 calc R . . C17' C 0.0444(3) 0.53802(19) 0.3102(3) 0.0204(11) Uani 1 1 d . . . H17' H 0.1041 0.5327 0.3623 0.025 Uiso 1 1 calc R . . C18' C -0.0507(3) 0.5201(2) 0.3344(3) 0.0268(11) Uani 1 1 d . . . H18C H -0.0449 0.4754 0.3535 0.032 Uiso 1 1 calc R . . H18D H -0.1110 0.5235 0.2833 0.032 Uiso 1 1 calc R . . C19' C -0.0679(3) 0.5618(2) 0.4048(3) 0.0313(12) Uani 1 1 d . . . H19C H -0.1331 0.5495 0.4159 0.038 Uiso 1 1 calc R . . H19D H -0.0115 0.5548 0.4580 0.038 Uiso 1 1 calc R . . C20' C -0.0720(3) 0.63130(19) 0.3811(3) 0.0257(11) Uani 1 1 d . . . H20C H -0.0763 0.6573 0.4303 0.031 Uiso 1 1 calc R . . H20D H -0.1341 0.6396 0.3330 0.031 Uiso 1 1 calc R . . C21' C 0.0229(3) 0.65005(19) 0.3555(3) 0.0251(11) Uani 1 1 d . . . H21C H 0.0157 0.6945 0.3352 0.030 Uiso 1 1 calc R . . H21D H 0.0838 0.6476 0.4062 0.030 Uiso 1 1 calc R . . C22' C 0.0392(3) 0.60777(18) 0.2862(3) 0.0240(11) Uani 1 1 d . . . H22C H 0.1038 0.6201 0.2742 0.029 Uiso 1 1 calc R . . H22D H -0.0177 0.6143 0.2333 0.029 Uiso 1 1 calc R . . C23' C -0.0194(3) 0.39383(19) 0.0434(3) 0.0227(11) Uani 1 1 d . . . H23' H 0.0139 0.4046 -0.0018 0.027 Uiso 1 1 calc R . . C24' C -0.0096(4) 0.3230(2) 0.0571(3) 0.0456(14) Uani 1 1 d . . . H24C H -0.0408 0.3108 0.1024 0.055 Uiso 1 1 calc R . . H24D H 0.0640 0.3114 0.0766 0.055 Uiso 1 1 calc R . . C25' C -0.0626(4) 0.2859(2) -0.0253(3) 0.0515(15) Uani 1 1 d . . . H25C H -0.0257 0.2937 -0.0684 0.062 Uiso 1 1 calc R . . H25D H -0.0594 0.2399 -0.0127 0.062 Uiso 1 1 calc R . . C26' C -0.1725(4) 0.3057(2) -0.0609(3) 0.0413(14) Uani 1 1 d . . . H26C H -0.2029 0.2837 -0.1158 0.050 Uiso 1 1 calc R . . H26D H -0.2113 0.2928 -0.0210 0.050 Uiso 1 1 calc R . . C27' C -0.1826(4) 0.3749(2) -0.0746(3) 0.0492(15) Uani 1 1 d . . . H27C H -0.2561 0.3864 -0.0950 0.059 Uiso 1 1 calc R . . H27D H -0.1500 0.3874 -0.1190 0.059 Uiso 1 1 calc R . . C28' C -0.1310(3) 0.4106(2) 0.0089(3) 0.0429(14) Uani 1 1 d . . . H28C H -0.1378 0.4568 -0.0018 0.051 Uiso 1 1 calc R . . H28D H -0.1667 0.4000 0.0519 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.0251(3) 0.0236(3) 0.0190(3) -0.0008(2) 0.0069(2) -0.0007(2) C1 0.061(4) 0.030(4) 0.040(4) -0.011(3) 0.013(3) 0.008(3) C2 0.049(4) 0.034(4) 0.018(3) 0.002(2) 0.005(3) 0.009(3) C3 0.035(3) 0.056(4) 0.035(4) -0.006(3) 0.012(3) 0.002(3) C4 0.054(4) 0.041(4) 0.095(5) -0.004(4) 0.042(4) -0.013(4) C5 0.081(5) 0.051(5) 0.082(5) 0.037(4) 0.062(4) 0.027(4) C6 0.065(5) 0.083(6) 0.019(3) 0.024(3) 0.024(3) 0.038(4) C7 0.046(4) 0.069(5) 0.025(3) -0.019(3) 0.006(3) 0.013(4) C8 0.019(2) 0.019(3) 0.016(3) -0.002(2) 0.005(2) -0.001(2) C9 0.021(3) 0.019(3) 0.016(3) -0.002(2) 0.007(2) 0.005(2) C10 0.022(3) 0.021(3) 0.021(3) -0.003(2) 0.010(2) -0.003(2) C11 0.021(3) 0.029(3) 0.020(3) 0.009(2) 0.001(2) -0.008(2) C12 0.024(3) 0.015(3) 0.022(3) -0.005(2) 0.008(2) -0.001(2) C13 0.023(3) 0.026(3) 0.032(3) -0.006(2) 0.005(2) -0.006(2) C14 0.022(3) 0.039(3) 0.027(3) 0.004(2) 0.000(2) 0.003(2) C15 0.031(3) 0.029(3) 0.028(3) 0.007(2) 0.007(2) 0.007(2) C16 0.026(3) 0.017(3) 0.026(3) 0.002(2) 0.008(2) 0.002(2) C17 0.024(3) 0.021(3) 0.014(3) 0.000(2) 0.004(2) -0.008(2) C18 0.028(3) 0.025(3) 0.044(3) -0.002(2) 0.017(2) 0.001(2) C19 0.025(3) 0.031(3) 0.055(4) 0.011(3) 0.008(3) 0.005(2) C20 0.037(3) 0.021(3) 0.028(3) 0.007(2) 0.002(2) -0.011(2) C21 0.032(3) 0.030(3) 0.031(3) -0.005(2) 0.012(2) -0.012(2) C22 0.016(2) 0.027(3) 0.020(3) -0.006(2) 0.000(2) -0.005(2) C23 0.024(3) 0.022(3) 0.019(3) 0.004(2) 0.006(2) -0.002(2) C24 0.021(2) 0.020(2) 0.019(2) 0.001(2) 0.003(2) -0.004(2) C25 0.028(3) 0.026(3) 0.026(3) -0.005(2) 0.009(2) 0.001(2) C26 0.028(3) 0.025(3) 0.028(3) -0.006(2) -0.001(2) -0.011(2) C27 0.021(3) 0.030(3) 0.042(3) -0.005(2) 0.001(2) -0.003(2) C28 0.027(3) 0.023(3) 0.040(3) -0.004(2) 0.009(2) 0.003(2) Zr' 0.0261(3) 0.0274(3) 0.0202(3) 0.0031(2) 0.0039(2) -0.0003(2) C1' 0.177(9) 0.043(5) 0.010(3) 0.006(3) 0.023(5) 0.043(5) C2' 0.073(5) 0.067(5) 0.053(5) 0.033(4) 0.045(4) 0.018(4) C3' 0.036(4) 0.042(4) 0.055(4) 0.019(3) 0.001(3) -0.007(3) C4' 0.076(5) 0.032(4) 0.026(3) -0.008(3) 0.002(3) 0.007(4) C5' 0.054(5) 0.095(6) 0.072(6) 0.053(5) 0.034(4) 0.044(4) C6' 0.026(4) 0.125(9) 0.116(9) 0.093(7) -0.028(5) -0.009(5) C7' 0.147(10) 0.060(6) 0.055(6) 0.034(5) -0.078(6) -0.052(7) C8' 0.024(3) 0.017(3) 0.017(3) 0.000(2) -0.001(2) 0.000(2) C9' 0.011(2) 0.033(3) 0.019(3) 0.006(2) 0.002(2) 0.001(2) C10' 0.028(3) 0.018(3) 0.015(3) 0.001(2) 0.007(2) 0.001(2) C11' 0.020(3) 0.022(3) 0.023(3) 0.007(2) 0.009(2) 0.001(2) C12' 0.017(3) 0.046(3) 0.011(3) -0.008(2) 0.007(2) -0.023(2) C13' 0.035(3) 0.024(3) 0.025(3) 0.003(2) 0.012(2) 0.004(2) C14' 0.021(3) 0.035(3) 0.042(3) -0.004(3) 0.008(3) -0.010(2) C15' 0.025(3) 0.037(3) 0.045(3) -0.001(3) 0.021(3) -0.001(2) C16' 0.035(3) 0.022(3) 0.025(3) 0.000(2) 0.009(2) -0.003(2) C17' 0.014(2) 0.027(3) 0.017(3) -0.005(2) 0.000(2) 0.001(2) C18' 0.029(3) 0.028(3) 0.023(3) -0.007(2) 0.006(2) -0.007(2) C19' 0.024(3) 0.042(3) 0.028(3) -0.004(2) 0.009(2) -0.008(2) C20' 0.025(3) 0.033(3) 0.018(3) -0.006(2) 0.003(2) 0.001(2) C21' 0.024(3) 0.021(3) 0.027(3) -0.001(2) 0.002(2) 0.003(2) C22' 0.024(3) 0.024(3) 0.026(3) -0.004(2) 0.011(2) -0.004(2) C23' 0.027(3) 0.027(3) 0.016(3) -0.002(2) 0.008(2) -0.001(2) C24' 0.064(4) 0.032(3) 0.029(3) -0.010(3) -0.006(3) 0.010(3) C25' 0.076(4) 0.031(4) 0.039(4) -0.007(3) 0.003(3) 0.006(3) C26' 0.051(4) 0.049(4) 0.023(3) -0.011(3) 0.009(3) -0.014(3) C27' 0.055(3) 0.047(4) 0.028(3) -0.012(3) -0.015(3) -0.004(3) C28' 0.050(3) 0.035(3) 0.032(3) -0.011(3) -0.007(3) 0.008(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 Zr C4 2.299(5) . ? Zr C6 2.300(5) . ? Zr C5 2.304(5) . ? Zr C7 2.322(5) . ? Zr C1 2.344(5) . ? Zr C2 2.340(5) . ? Zr C3 2.348(5) . ? Zr C9 2.481(4) . ? Zr C8 2.495(4) . ? Zr C10 2.507(4) . ? Zr C11 2.524(4) . ? Zr C12 2.521(4) . ? C1 C2 1.411(7) . ? C1 C7 1.441(7) . ? C2 C3 1.401(7) . ? C3 C4 1.384(8) . ? C4 C5 1.460(9) . ? C5 C6 1.418(9) . ? C6 C7 1.382(8) . ? C8 C9 1.408(5) . ? C8 C12 1.440(5) . ? C8 C17 1.501(5) . ? C9 C10 1.410(5) . ? C10 C11 1.438(5) . ? C10 C23 1.502(5) . ? C11 C12 1.425(5) . ? C11 C16 1.434(5) . ? C12 C13 1.439(5) . ? C13 C14 1.348(5) . ? C14 C15 1.401(5) . ? C15 C16 1.348(5) . ? C17 C22 1.517(5) . ? C17 C18 1.523(5) . ? C18 C19 1.514(5) . ? C19 C20 1.520(5) . ? C20 C21 1.524(5) . ? C21 C22 1.516(5) . ? C23 C24 1.516(5) . ? C23 C28 1.531(5) . ? C24 C25 1.520(5) . ? C25 C26 1.524(5) . ? C26 C27 1.512(5) . ? C27 C28 1.520(5) . ? Zr' C7' 2.280(6) . ? Zr' C1' 2.294(5) . ? Zr' C6' 2.298(6) . ? Zr' C2' 2.314(5) . ? Zr' C5' 2.333(6) . ? Zr' C3' 2.344(5) . ? Zr' C4' 2.346(5) . ? Zr' C10' 2.491(4) . ? Zr' C12' 2.497(4) . ? Zr' C9' 2.519(4) . ? Zr' C8' 2.523(4) . ? Zr' C11' 2.531(4) . ? C1' C2' 1.384(10) . ? C1' C7' 1.401(12) . ? C2' C3' 1.343(8) . ? C3' C4' 1.378(8) . ? C4' C5' 1.367(9) . ? C5' C6' 1.427(12) . ? C6' C7' 1.421(12) . ? C8' C9' 1.411(5) . ? C8' C12' 1.458(5) . ? C8' C17' 1.511(5) . ? C9' C10' 1.408(5) . ? C10' C11' 1.427(5) . ? C10' C23' 1.520(5) . ? C11' C12' 1.401(5) . ? C11' C16' 1.422(5) . ? C12' C13' 1.421(5) . ? C13' C14' 1.364(5) . ? C14' C15' 1.420(6) . ? C15' C16' 1.353(5) . ? C17' C18' 1.508(5) . ? C17' C22' 1.519(5) . ? C18' C19' 1.520(5) . ? C19' C20' 1.514(5) . ? C20' C21' 1.520(5) . ? C21' C22' 1.509(5) . ? C23' C28' 1.502(5) . ? C23' C24' 1.511(5) . ? C24' C25' 1.545(6) . ? C25' C26' 1.500(6) . ? C26' C27' 1.476(6) . ? C27' C28' 1.540(5) . ? 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 C4 Zr C6 68.2(2) . . ? C4 Zr C5 37.0(2) . . ? C6 Zr C5 35.9(2) . . ? C4 Zr C7 87.0(2) . . ? C6 Zr C7 34.8(2) . . ? C5 Zr C7 66.4(2) . . ? C4 Zr C1 86.3(2) . . ? C6 Zr C1 66.6(2) . . ? C5 Zr C1 86.7(2) . . ? C7 Zr C1 35.97(18) . . ? C4 Zr C2 65.5(2) . . ? C6 Zr C2 85.75(17) . . ? C5 Zr C2 86.02(18) . . ? C7 Zr C2 66.32(18) . . ? C1 Zr C2 35.05(17) . . ? C4 Zr C3 34.64(19) . . ? C6 Zr C3 86.35(19) . . ? C5 Zr C3 66.8(2) . . ? C7 Zr C3 85.91(17) . . ? C1 Zr C3 65.89(19) . . ? C2 Zr C3 34.78(17) . . ? C4 Zr C9 127.01(19) . . ? C6 Zr C9 149.30(16) . . ? C5 Zr C9 139.72(19) . . ? C7 Zr C9 145.97(17) . . ? C1 Zr C9 133.53(16) . . ? C2 Zr C9 124.19(15) . . ? C3 Zr C9 121.59(16) . . ? C4 Zr C8 159.79(18) . . ? C6 Zr C8 127.54(18) . . ? C5 Zr C8 149.02(18) . . ? C7 Zr C8 113.10(17) . . ? C1 Zr C8 110.89(16) . . ? C2 Zr C8 123.19(15) . . ? C3 Zr C8 143.18(17) . . ? C9 Zr C8 32.88(12) . . ? C4 Zr C10 105.98(17) . . ? C6 Zr C10 123.81(18) . . ? C5 Zr C10 107.14(18) . . ? C7 Zr C10 148.42(17) . . ? C1 Zr C10 165.99(16) . . ? C2 Zr C10 145.25(16) . . ? C3 Zr C10 121.13(16) . . ? C9 Zr C10 32.84(12) . . ? C8 Zr C10 55.79(12) . . ? C4 Zr C11 115.44(19) . . ? C6 Zr C11 96.15(16) . . ? C5 Zr C11 95.66(16) . . ? C7 Zr C11 115.20(17) . . ? C1 Zr C11 145.84(17) . . ? C2 Zr C11 178.09(15) . . ? C3 Zr C11 145.43(18) . . ? C9 Zr C11 53.89(13) . . ? C8 Zr C11 55.35(12) . . ? C10 Zr C11 33.23(12) . . ? C4 Zr C12 146.3(2) . . ? C6 Zr C12 98.07(17) . . ? C5 Zr C12 116.10(19) . . ? C7 Zr C12 98.62(16) . . ? C1 Zr C12 117.31(16) . . ? C2 Zr C12 146.71(17) . . ? C3 Zr C12 175.30(16) . . ? C9 Zr C12 53.74(13) . . ? C8 Zr C12 33.37(12) . . ? C10 Zr C12 54.95(13) . . ? C11 Zr C12 32.82(11) . . ? C2 C1 C7 126.8(5) . . ? C2 C1 Zr 72.3(3) . . ? C7 C1 Zr 71.1(3) . . ? C3 C2 C1 130.3(5) . . ? C3 C2 Zr 72.9(3) . . ? C1 C2 Zr 72.6(3) . . ? C4 C3 C2 128.6(5) . . ? C4 C3 Zr 70.8(3) . . ? C2 C3 Zr 72.3(3) . . ? C3 C4 C5 128.5(5) . . ? C3 C4 Zr 74.6(3) . . ? C5 C4 Zr 71.7(3) . . ? C6 C5 C4 127.2(5) . . ? C6 C5 Zr 71.9(3) . . ? C4 C5 Zr 71.3(3) . . ? C7 C6 C5 129.4(5) . . ? C7 C6 Zr 73.4(3) . . ? C5 C6 Zr 72.2(3) . . ? C6 C7 C1 129.0(5) . . ? C6 C7 Zr 71.7(3) . . ? C1 C7 Zr 72.9(3) . . ? C9 C8 C12 105.1(3) . . ? C9 C8 C17 128.4(4) . . ? C12 C8 C17 126.4(4) . . ? C9 C8 Zr 73.0(2) . . ? C12 C8 Zr 74.3(2) . . ? C17 C8 Zr 121.3(3) . . ? C8 C9 C10 112.3(4) . . ? C8 C9 Zr 74.1(2) . . ? C10 C9 Zr 74.6(2) . . ? C9 C10 C11 105.5(4) . . ? C9 C10 C23 129.4(4) . . ? C11 C10 C23 125.0(4) . . ? C9 C10 Zr 72.6(2) . . ? C11 C10 Zr 74.0(2) . . ? C23 C10 Zr 120.6(2) . . ? C12 C11 C10 108.2(4) . . ? C12 C11 C16 119.9(4) . . ? C10 C11 C16 131.9(4) . . ? C12 C11 Zr 73.5(2) . . ? C10 C11 Zr 72.7(2) . . ? C16 C11 Zr 122.1(3) . . ? C11 C12 C8 108.9(4) . . ? C11 C12 C13 118.8(4) . . ? C8 C12 C13 132.3(4) . . ? C11 C12 Zr 73.7(2) . . ? C8 C12 Zr 72.3(2) . . ? C13 C12 Zr 119.2(3) . . ? C14 C13 C12 118.9(4) . . ? C13 C14 C15 121.6(4) . . ? C16 C15 C14 122.6(4) . . ? C15 C16 C11 118.1(4) . . ? C8 C17 C22 112.0(3) . . ? C8 C17 C18 113.3(3) . . ? C22 C17 C18 109.2(3) . . ? C19 C18 C17 112.5(3) . . ? C18 C19 C20 111.2(4) . . ? C19 C20 C21 109.9(3) . . ? C22 C21 C20 111.3(3) . . ? C17 C22 C21 112.4(3) . . ? C10 C23 C24 111.9(3) . . ? C10 C23 C28 113.2(3) . . ? C24 C23 C28 109.4(3) . . ? C23 C24 C25 111.7(3) . . ? C24 C25 C26 112.1(3) . . ? C27 C26 C25 110.9(3) . . ? C26 C27 C28 111.1(3) . . ? C27 C28 C23 111.8(3) . . ? C7' Zr' C1' 35.7(3) . . ? C7' Zr' C6' 36.2(3) . . ? C1' Zr' C6' 67.4(3) . . ? C7' Zr' C2' 66.1(3) . . ? C1' Zr' C2' 35.0(3) . . ? C6' Zr' C2' 86.3(3) . . ? C7' Zr' C5' 66.8(3) . . ? C1' Zr' C5' 85.6(2) . . ? C6' Zr' C5' 35.9(3) . . ? C2' Zr' C5' 84.2(2) . . ? C7' Zr' C3' 84.1(2) . . ? C1' Zr' C3' 64.1(3) . . ? C6' Zr' C3' 85.0(2) . . ? C2' Zr' C3' 33.5(2) . . ? C5' Zr' C3' 64.4(2) . . ? C7' Zr' C4' 84.2(2) . . ? C1' Zr' C4' 83.4(2) . . ? C6' Zr' C4' 65.4(3) . . ? C2' Zr' C4' 63.7(2) . . ? C5' Zr' C4' 34.0(2) . . ? C3' Zr' C4' 34.17(19) . . ? C7' Zr' C10' 144.8(2) . . ? C1' Zr' C10' 145.33(19) . . ? C6' Zr' C10' 135.9(2) . . ? C2' Zr' C10' 137.85(18) . . ? C5' Zr' C10' 128.70(18) . . ? C3' Zr' C10' 130.49(17) . . ? C4' Zr' C10' 127.05(15) . . ? C7' Zr' C12' 90.1(2) . . ? C1' Zr' C12' 109.4(2) . . ? C6' Zr' C12' 92.1(2) . . ? C2' Zr' C12' 140.6(2) . . ? C5' Zr' C12' 115.9(2) . . ? C3' Zr' C12' 173.51(19) . . ? C4' Zr' C12' 148.1(2) . . ? C10' Zr' C12' 54.97(13) . . ? C7' Zr' C9' 125.1(3) . . ? C1' Zr' C9' 112.75(19) . . ? C6' Zr' C9' 145.3(3) . . ? C2' Zr' C9' 113.83(17) . . ? C5' Zr' C9' 160.88(17) . . ? C3' Zr' C9' 127.56(16) . . ? C4' Zr' C9' 148.26(18) . . ? C10' Zr' C9' 32.63(12) . . ? C12' Zr' C9' 54.23(13) . . ? C7' Zr' C8' 94.2(2) . . ? C1' Zr' C8' 94.10(19) . . ? C6' Zr' C8' 114.4(3) . . ? C2' Zr' C8' 113.7(2) . . ? C5' Zr' C8' 146.9(3) . . ? C3' Zr' C8' 143.63(19) . . ? C4' Zr' C8' 177.39(17) . . ? C10' Zr' C8' 55.06(13) . . ? C12' Zr' C8' 33.77(12) . . ? C9' Zr' C8' 32.50(12) . . ? C7' Zr' C11' 117.2(3) . . ? C1' Zr' C11' 141.8(3) . . ? C6' Zr' C11' 103.5(2) . . ? C2' Zr' C11' 166.95(18) . . ? C5' Zr' C11' 108.80(18) . . ? C3' Zr' C11' 154.12(19) . . ? C4' Zr' C11' 128.15(18) . . ? C10' Zr' C11' 32.99(12) . . ? C12' Zr' C11' 32.34(12) . . ? C9' Zr' C11' 53.44(13) . . ? C8' Zr' C11' 54.45(13) . . ? C2' C1' C7' 128.3(7) . . ? C2' C1' Zr' 73.3(3) . . ? C7' C1' Zr' 71.6(4) . . ? C3' C2' C1' 129.0(6) . . ? C3' C2' Zr' 74.5(3) . . ? C1' C2' Zr' 71.7(3) . . ? C2' C3' C4' 129.4(5) . . ? C2' C3' Zr' 72.0(3) . . ? C4' C3' Zr' 73.0(3) . . ? C5' C4' C3' 130.4(6) . . ? C5' C4' Zr' 72.5(4) . . ? C3' C4' Zr' 72.8(3) . . ? C4' C5' C6' 127.9(7) . . ? C4' C5' Zr' 73.5(3) . . ? C6' C5' Zr' 70.7(4) . . ? C7' C6' C5' 126.1(7) . . ? C7' C6' Zr' 71.2(4) . . ? C5' C6' Zr' 73.4(4) . . ? C1' C7' C6' 129.0(7) . . ? C1' C7' Zr' 72.7(4) . . ? C6' C7' Zr' 72.6(4) . . ? C9' C8' C12' 105.6(4) . . ? C9' C8' C17' 126.1(4) . . ? C12' C8' C17' 128.1(4) . . ? C9' C8' Zr' 73.6(2) . . ? C12' C8' Zr' 72.1(2) . . ? C17' C8' Zr' 123.2(3) . . ? C8' C9' C10' 110.6(4) . . ? C8' C9' Zr' 73.9(2) . . ? C10' C9' Zr' 72.6(2) . . ? C9' C10' C11' 106.5(4) . . ? C9' C10' C23' 127.0(4) . . ? C11' C10' C23' 125.9(4) . . ? C9' C10' Zr' 74.8(2) . . ? C11' C10' Zr' 75.1(2) . . ? C23' C10' Zr' 122.6(3) . . ? C12' C11' C16' 118.8(4) . . ? C12' C11' C10' 109.0(3) . . ? C16' C11' C10' 132.1(4) . . ? C12' C11' Zr' 72.5(2) . . ? C16' C11' Zr' 119.3(3) . . ? C10' C11' Zr' 72.0(2) . . ? C11' C12' C13' 121.4(4) . . ? C11' C12' C8' 108.0(3) . . ? C13' C12' C8' 130.0(4) . . ? C11' C12' Zr' 75.2(2) . . ? C13' C12' Zr' 123.7(3) . . ? C8' C12' Zr' 74.1(2) . . ? C14' C13' C12' 117.3(4) . . ? C13' C14' C15' 122.1(4) . . ? C16' C15' C14' 120.4(4) . . ? C15' C16' C11' 119.8(4) . . ? C18' C17' C8' 113.9(3) . . ? C18' C17' C22' 109.3(3) . . ? C8' C17' C22' 111.9(3) . . ? C17' C18' C19' 112.7(3) . . ? C20' C19' C18' 111.6(3) . . ? C19' C20' C21' 110.6(3) . . ? C22' C21' C20' 112.0(3) . . ? C21' C22' C17' 112.6(3) . . ? C28' C23' C24' 109.0(4) . . ? C28' C23' C10' 112.9(3) . . ? C24' C23' C10' 113.2(3) . . ? C23' C24' C25' 111.8(4) . . ? C26' C25' C24' 111.0(4) . . ? C27' C26' C25' 111.9(4) . . ? C26' C27' C28' 110.5(4) . . ? C23' C28' C27' 111.7(4) . . ? 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 C4 Zr C1 C2 -50.7(3) . . . . ? C6 Zr C1 C2 -118.5(4) . . . . ? C5 Zr C1 C2 -87.8(3) . . . . ? C7 Zr C1 C2 -140.7(5) . . . . ? C3 Zr C1 C2 -21.7(3) . . . . ? C9 Zr C1 C2 89.7(3) . . . . ? C8 Zr C1 C2 118.4(3) . . . . ? C10 Zr C1 C2 101.3(7) . . . . ? C11 Zr C1 C2 177.0(3) . . . . ? C12 Zr C1 C2 154.4(3) . . . . ? C4 Zr C1 C7 89.9(4) . . . . ? C6 Zr C1 C7 22.1(3) . . . . ? C5 Zr C1 C7 52.9(3) . . . . ? C2 Zr C1 C7 140.7(5) . . . . ? C3 Zr C1 C7 118.9(4) . . . . ? C9 Zr C1 C7 -129.6(3) . . . . ? C8 Zr C1 C7 -100.9(3) . . . . ? C10 Zr C1 C7 -118.0(7) . . . . ? C11 Zr C1 C7 -42.3(5) . . . . ? C12 Zr C1 C7 -64.9(3) . . . . ? C7 C1 C2 C3 -0.5(9) . . . . ? Zr C1 C2 C3 48.0(5) . . . . ? C7 C1 C2 Zr -48.5(5) . . . . ? C4 Zr C2 C3 -21.8(3) . . . . ? C6 Zr C2 C3 -89.7(3) . . . . ? C5 Zr C2 C3 -53.7(3) . . . . ? C7 Zr C2 C3 -119.7(3) . . . . ? C1 Zr C2 C3 -143.7(5) . . . . ? C9 Zr C2 C3 97.6(3) . . . . ? C8 Zr C2 C3 137.3(3) . . . . ? C10 Zr C2 C3 61.0(4) . . . . ? C11 Zr C2 C3 98(5) . . . . ? C12 Zr C2 C3 172.0(3) . . . . ? C4 Zr C2 C1 121.9(4) . . . . ? C6 Zr C2 C1 53.9(3) . . . . ? C5 Zr C2 C1 89.9(4) . . . . ? C7 Zr C2 C1 24.0(3) . . . . ? C3 Zr C2 C1 143.7(5) . . . . ? C9 Zr C2 C1 -118.8(3) . . . . ? C8 Zr C2 C1 -79.0(3) . . . . ? C10 Zr C2 C1 -155.4(3) . . . . ? C11 Zr C2 C1 -119(5) . . . . ? C12 Zr C2 C1 -44.3(4) . . . . ? C1 C2 C3 C4 -2.1(9) . . . . ? Zr C2 C3 C4 45.8(5) . . . . ? C1 C2 C3 Zr -47.9(5) . . . . ? C6 Zr C3 C4 -55.8(4) . . . . ? C5 Zr C3 C4 -24.6(4) . . . . ? C7 Zr C3 C4 -90.6(4) . . . . ? C1 Zr C3 C4 -121.7(4) . . . . ? C2 Zr C3 C4 -143.6(5) . . . . ? C9 Zr C3 C4 110.7(4) . . . . ? C8 Zr C3 C4 145.2(3) . . . . ? C10 Zr C3 C4 72.0(4) . . . . ? C11 Zr C3 C4 39.8(5) . . . . ? C12 Zr C3 C4 105(2) . . . . ? C4 Zr C3 C2 143.6(5) . . . . ? C6 Zr C3 C2 87.8(3) . . . . ? C5 Zr C3 C2 118.9(4) . . . . ? C7 Zr C3 C2 52.9(3) . . . . ? C1 Zr C3 C2 21.9(3) . . . . ? C9 Zr C3 C2 -105.7(3) . . . . ? C8 Zr C3 C2 -71.2(4) . . . . ? C10 Zr C3 C2 -144.4(3) . . . . ? C11 Zr C3 C2 -176.7(3) . . . . ? C12 Zr C3 C2 -112(2) . . . . ? C2 C3 C4 C5 4.2(10) . . . . ? Zr C3 C4 C5 50.6(5) . . . . ? C2 C3 C4 Zr -46.4(5) . . . . ? C6 Zr C4 C3 117.3(4) . . . . ? C5 Zr C4 C3 140.5(5) . . . . ? C7 Zr C4 C3 87.1(4) . . . . ? C1 Zr C4 C3 51.1(3) . . . . ? C2 Zr C4 C3 21.9(3) . . . . ? C9 Zr C4 C3 -93.6(3) . . . . ? C8 Zr C4 C3 -98.3(6) . . . . ? C10 Zr C4 C3 -122.1(3) . . . . ? C11 Zr C4 C3 -156.3(3) . . . . ? C12 Zr C4 C3 -171.8(3) . . . . ? C6 Zr C4 C5 -23.2(3) . . . . ? C7 Zr C4 C5 -53.3(4) . . . . ? C1 Zr C4 C5 -89.3(4) . . . . ? C2 Zr C4 C5 -118.6(4) . . . . ? C3 Zr C4 C5 -140.5(5) . . . . ? C9 Zr C4 C5 125.9(3) . . . . ? C8 Zr C4 C5 121.2(6) . . . . ? C10 Zr C4 C5 97.4(4) . . . . ? C11 Zr C4 C5 63.2(4) . . . . ? C12 Zr C4 C5 47.7(5) . . . . ? C3 C4 C5 C6 -3.6(10) . . . . ? Zr C4 C5 C6 48.0(5) . . . . ? C3 C4 C5 Zr -51.7(6) . . . . ? C4 Zr C5 C6 -141.5(5) . . . . ? C7 Zr C5 C6 -22.4(3) . . . . ? C1 Zr C5 C6 -53.1(3) . . . . ? C2 Zr C5 C6 -88.3(3) . . . . ? C3 Zr C5 C6 -118.3(4) . . . . ? C9 Zr C5 C6 129.6(3) . . . . ? C8 Zr C5 C6 73.6(5) . . . . ? C10 Zr C5 C6 124.6(3) . . . . ? C11 Zr C5 C6 92.7(3) . . . . ? C12 Zr C5 C6 65.8(4) . . . . ? C6 Zr C5 C4 141.5(5) . . . . ? C7 Zr C5 C4 119.1(4) . . . . ? C1 Zr C5 C4 88.3(4) . . . . ? C2 Zr C5 C4 53.2(4) . . . . ? C3 Zr C5 C4 23.2(3) . . . . ? C9 Zr C5 C4 -88.9(4) . . . . ? C8 Zr C5 C4 -145.0(3) . . . . ? C10 Zr C5 C4 -94.0(3) . . . . ? C11 Zr C5 C4 -125.9(3) . . . . ? C12 Zr C5 C4 -152.8(3) . . . . ? C4 C5 C6 C7 1.6(10) . . . . ? Zr C5 C6 C7 49.4(6) . . . . ? C4 C5 C6 Zr -47.8(6) . . . . ? C4 Zr C6 C7 -118.5(4) . . . . ? C5 Zr C6 C7 -142.3(5) . . . . ? C1 Zr C6 C7 -22.8(3) . . . . ? C2 Zr C6 C7 -53.2(3) . . . . ? C3 Zr C6 C7 -88.1(3) . . . . ? C9 Zr C6 C7 114.9(4) . . . . ? C8 Zr C6 C7 76.2(4) . . . . ? C10 Zr C6 C7 146.4(3) . . . . ? C11 Zr C6 C7 126.5(3) . . . . ? C12 Zr C6 C7 93.5(3) . . . . ? C4 Zr C6 C5 23.8(3) . . . . ? C7 Zr C6 C5 142.3(5) . . . . ? C1 Zr C6 C5 119.5(4) . . . . ? C2 Zr C6 C5 89.1(3) . . . . ? C3 Zr C6 C5 54.2(3) . . . . ? C9 Zr C6 C5 -102.8(4) . . . . ? C8 Zr C6 C5 -141.5(3) . . . . ? C10 Zr C6 C5 -71.3(3) . . . . ? C11 Zr C6 C5 -91.2(3) . . . . ? C12 Zr C6 C5 -124.2(3) . . . . ? C5 C6 C7 C1 -0.7(10) . . . . ? Zr C6 C7 C1 48.2(5) . . . . ? C5 C6 C7 Zr -48.9(6) . . . . ? C2 C1 C7 C6 1.1(9) . . . . ? Zr C1 C7 C6 -47.8(5) . . . . ? C2 C1 C7 Zr 49.0(5) . . . . ? C4 Zr C7 C6 54.8(3) . . . . ? C5 Zr C7 C6 23.0(3) . . . . ? C1 Zr C7 C6 142.7(5) . . . . ? C2 Zr C7 C6 119.3(4) . . . . ? C3 Zr C7 C6 89.5(3) . . . . ? C9 Zr C7 C6 -124.2(4) . . . . ? C8 Zr C7 C6 -123.1(3) . . . . ? C10 Zr C7 C6 -61.4(5) . . . . ? C11 Zr C7 C6 -62.0(4) . . . . ? C12 Zr C7 C6 -91.8(3) . . . . ? C4 Zr C7 C1 -87.9(3) . . . . ? C6 Zr C7 C1 -142.7(5) . . . . ? C5 Zr C7 C1 -119.7(4) . . . . ? C2 Zr C7 C1 -23.4(3) . . . . ? C3 Zr C7 C1 -53.2(3) . . . . ? C9 Zr C7 C1 93.1(4) . . . . ? C8 Zr C7 C1 94.1(3) . . . . ? C10 Zr C7 C1 155.9(3) . . . . ? C11 Zr C7 C1 155.3(3) . . . . ? C12 Zr C7 C1 125.5(3) . . . . ? C4 Zr C8 C9 7.0(7) . . . . ? C6 Zr C8 C9 144.0(3) . . . . ? C5 Zr C8 C9 98.8(5) . . . . ? C7 Zr C8 C9 -179.0(3) . . . . ? C1 Zr C8 C9 -140.1(3) . . . . ? C2 Zr C8 C9 -103.0(3) . . . . ? C3 Zr C8 C9 -62.8(4) . . . . ? C10 Zr C8 C9 34.9(2) . . . . ? C11 Zr C8 C9 75.5(2) . . . . ? C12 Zr C8 C9 111.6(3) . . . . ? C4 Zr C8 C12 -104.7(6) . . . . ? C6 Zr C8 C12 32.4(3) . . . . ? C5 Zr C8 C12 -12.8(5) . . . . ? C7 Zr C8 C12 69.4(3) . . . . ? C1 Zr C8 C12 108.3(3) . . . . ? C2 Zr C8 C12 145.4(2) . . . . ? C3 Zr C8 C12 -174.4(3) . . . . ? C9 Zr C8 C12 -111.6(3) . . . . ? C10 Zr C8 C12 -76.7(2) . . . . ? C11 Zr C8 C12 -36.1(2) . . . . ? C4 Zr C8 C17 132.0(6) . . . . ? C6 Zr C8 C17 -91.0(4) . . . . ? C5 Zr C8 C17 -136.2(5) . . . . ? C7 Zr C8 C17 -53.9(4) . . . . ? C1 Zr C8 C17 -15.1(4) . . . . ? C2 Zr C8 C17 22.0(4) . . . . ? C3 Zr C8 C17 62.2(4) . . . . ? C9 Zr C8 C17 125.0(4) . . . . ? C10 Zr C8 C17 160.0(4) . . . . ? C11 Zr C8 C17 -159.5(4) . . . . ? C12 Zr C8 C17 -123.4(4) . . . . ? C12 C8 C9 C10 2.5(5) . . . . ? C17 C8 C9 C10 177.8(4) . . . . ? Zr C8 C9 C10 -65.5(3) . . . . ? C12 C8 C9 Zr 68.0(3) . . . . ? C17 C8 C9 Zr -116.7(4) . . . . ? C4 Zr C9 C8 -177.0(3) . . . . ? C6 Zr C9 C8 -66.0(5) . . . . ? C5 Zr C9 C8 -128.1(4) . . . . ? C7 Zr C9 C8 1.7(4) . . . . ? C1 Zr C9 C8 55.7(3) . . . . ? C2 Zr C9 C8 99.7(3) . . . . ? C3 Zr C9 C8 141.3(3) . . . . ? C10 Zr C9 C8 -119.2(4) . . . . ? C11 Zr C9 C8 -80.3(2) . . . . ? C12 Zr C9 C8 -39.4(2) . . . . ? C4 Zr C9 C10 -57.8(3) . . . . ? C6 Zr C9 C10 53.2(5) . . . . ? C5 Zr C9 C10 -9.0(4) . . . . ? C7 Zr C9 C10 120.8(4) . . . . ? C1 Zr C9 C10 174.8(3) . . . . ? C2 Zr C9 C10 -141.2(3) . . . . ? C3 Zr C9 C10 -99.6(3) . . . . ? C8 Zr C9 C10 119.2(4) . . . . ? C11 Zr C9 C10 38.8(2) . . . . ? C12 Zr C9 C10 79.8(3) . . . . ? C8 C9 C10 C11 -2.1(5) . . . . ? Zr C9 C10 C11 -67.3(3) . . . . ? C8 C9 C10 C23 -179.2(4) . . . . ? Zr C9 C10 C23 115.6(4) . . . . ? C8 C9 C10 Zr 65.2(3) . . . . ? C4 Zr C10 C9 135.3(3) . . . . ? C6 Zr C10 C9 -150.5(3) . . . . ? C5 Zr C10 C9 173.9(3) . . . . ? C7 Zr C10 C9 -113.4(4) . . . . ? C1 Zr C10 C9 -15.6(8) . . . . ? C2 Zr C10 C9 65.5(4) . . . . ? C3 Zr C10 C9 101.1(3) . . . . ? C8 Zr C10 C9 -35.0(2) . . . . ? C11 Zr C10 C9 -112.4(3) . . . . ? C12 Zr C10 C9 -75.8(3) . . . . ? C4 Zr C10 C11 -112.2(3) . . . . ? C6 Zr C10 C11 -38.1(3) . . . . ? C5 Zr C10 C11 -73.6(3) . . . . ? C7 Zr C10 C11 -1.0(5) . . . . ? C1 Zr C10 C11 96.8(7) . . . . ? C2 Zr C10 C11 177.9(3) . . . . ? C3 Zr C10 C11 -146.5(3) . . . . ? C9 Zr C10 C11 112.4(3) . . . . ? C8 Zr C10 C11 77.5(2) . . . . ? C12 Zr C10 C11 36.6(2) . . . . ? C4 Zr C10 C23 9.3(4) . . . . ? C6 Zr C10 C23 83.5(4) . . . . ? C5 Zr C10 C23 48.0(4) . . . . ? C7 Zr C10 C23 120.6(4) . . . . ? C1 Zr C10 C23 -141.6(7) . . . . ? C2 Zr C10 C23 -60.5(4) . . . . ? C3 Zr C10 C23 -24.9(4) . . . . ? C9 Zr C10 C23 -126.0(4) . . . . ? C8 Zr C10 C23 -161.0(4) . . . . ? C11 Zr C10 C23 121.6(4) . . . . ? C12 Zr C10 C23 158.2(4) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C23 C10 C11 C12 178.1(4) . . . . ? Zr C10 C11 C12 -65.5(3) . . . . ? C9 C10 C11 C16 -175.8(4) . . . . ? C23 C10 C11 C16 1.5(7) . . . . ? Zr C10 C11 C16 118.0(5) . . . . ? C9 C10 C11 Zr 66.2(3) . . . . ? C23 C10 C11 Zr -116.4(4) . . . . ? C4 Zr C11 C12 -164.1(3) . . . . ? C6 Zr C11 C12 -95.4(3) . . . . ? C5 Zr C11 C12 -131.4(3) . . . . ? C7 Zr C11 C12 -64.9(3) . . . . ? C1 Zr C11 C12 -39.0(4) . . . . ? C2 Zr C11 C12 77(5) . . . . ? C3 Zr C11 C12 172.1(3) . . . . ? C9 Zr C11 C12 77.3(3) . . . . ? C8 Zr C11 C12 36.7(2) . . . . ? C10 Zr C11 C12 115.7(3) . . . . ? C4 Zr C11 C10 80.2(3) . . . . ? C6 Zr C11 C10 149.0(3) . . . . ? C5 Zr C11 C10 112.9(3) . . . . ? C7 Zr C11 C10 179.4(3) . . . . ? C1 Zr C11 C10 -154.7(3) . . . . ? C2 Zr C11 C10 -38(5) . . . . ? C3 Zr C11 C10 56.5(4) . . . . ? C9 Zr C11 C10 -38.3(2) . . . . ? C8 Zr C11 C10 -78.9(2) . . . . ? C12 Zr C11 C10 -115.7(3) . . . . ? C4 Zr C11 C16 -48.8(4) . . . . ? C6 Zr C11 C16 19.9(4) . . . . ? C5 Zr C11 C16 -16.2(4) . . . . ? C7 Zr C11 C16 50.4(4) . . . . ? C1 Zr C11 C16 76.3(4) . . . . ? C2 Zr C11 C16 -168(5) . . . . ? C3 Zr C11 C16 -72.6(4) . . . . ? C9 Zr C11 C16 -167.4(4) . . . . ? C8 Zr C11 C16 152.0(4) . . . . ? C10 Zr C11 C16 -129.1(5) . . . . ? C12 Zr C11 C16 115.3(4) . . . . ? C10 C11 C12 C8 0.7(5) . . . . ? C16 C11 C12 C8 177.8(4) . . . . ? Zr C11 C12 C8 -64.2(3) . . . . ? C10 C11 C12 C13 179.7(3) . . . . ? C16 C11 C12 C13 -3.3(6) . . . . ? Zr C11 C12 C13 114.7(3) . . . . ? C10 C11 C12 Zr 65.0(3) . . . . ? C16 C11 C12 Zr -118.0(4) . . . . ? C9 C8 C12 C11 -1.9(4) . . . . ? C17 C8 C12 C11 -177.3(4) . . . . ? Zr C8 C12 C11 65.1(3) . . . . ? C9 C8 C12 C13 179.3(4) . . . . ? C17 C8 C12 C13 3.9(7) . . . . ? Zr C8 C12 C13 -113.7(4) . . . . ? C9 C8 C12 Zr -67.0(3) . . . . ? C17 C8 C12 Zr 117.6(4) . . . . ? C4 Zr C12 C11 26.4(4) . . . . ? C6 Zr C12 C11 88.8(3) . . . . ? C5 Zr C12 C11 56.2(3) . . . . ? C7 Zr C12 C11 124.0(3) . . . . ? C1 Zr C12 C11 156.6(3) . . . . ? C2 Zr C12 C11 -176.6(3) . . . . ? C3 Zr C12 C11 -71(2) . . . . ? C9 Zr C12 C11 -77.8(3) . . . . ? C8 Zr C12 C11 -116.5(3) . . . . ? C10 Zr C12 C11 -37.1(2) . . . . ? C4 Zr C12 C8 143.0(4) . . . . ? C6 Zr C12 C8 -154.6(3) . . . . ? C5 Zr C12 C8 172.7(3) . . . . ? C7 Zr C12 C8 -119.4(3) . . . . ? C1 Zr C12 C8 -86.9(3) . . . . ? C2 Zr C12 C8 -60.0(4) . . . . ? C3 Zr C12 C8 45(2) . . . . ? C9 Zr C12 C8 38.7(2) . . . . ? C10 Zr C12 C8 79.4(2) . . . . ? C11 Zr C12 C8 116.5(3) . . . . ? C4 Zr C12 C13 -87.9(4) . . . . ? C6 Zr C12 C13 -25.5(4) . . . . ? C5 Zr C12 C13 -58.2(4) . . . . ? C7 Zr C12 C13 9.7(4) . . . . ? C1 Zr C12 C13 42.2(4) . . . . ? C2 Zr C12 C13 69.1(4) . . . . ? C3 Zr C12 C13 174(2) . . . . ? C9 Zr C12 C13 167.9(4) . . . . ? C8 Zr C12 C13 129.1(4) . . . . ? C10 Zr C12 C13 -151.4(4) . . . . ? C11 Zr C12 C13 -114.3(4) . . . . ? C11 C12 C13 C14 2.3(6) . . . . ? C8 C12 C13 C14 -179.0(4) . . . . ? Zr C12 C13 C14 88.9(4) . . . . ? C12 C13 C14 C15 -0.4(6) . . . . ? C13 C14 C15 C16 -0.7(7) . . . . ? C14 C15 C16 C11 -0.3(6) . . . . ? C12 C11 C16 C15 2.2(6) . . . . ? C10 C11 C16 C15 178.5(4) . . . . ? Zr C11 C16 C15 -86.3(4) . . . . ? C9 C8 C17 C22 -87.0(5) . . . . ? C12 C8 C17 C22 87.4(5) . . . . ? Zr C8 C17 C22 -179.5(2) . . . . ? C9 C8 C17 C18 37.1(6) . . . . ? C12 C8 C17 C18 -148.5(4) . . . . ? Zr C8 C17 C18 -55.4(4) . . . . ? C8 C17 C18 C19 179.2(4) . . . . ? C22 C17 C18 C19 -55.1(5) . . . . ? C17 C18 C19 C20 56.6(5) . . . . ? C18 C19 C20 C21 -55.6(5) . . . . ? C19 C20 C21 C22 55.7(5) . . . . ? C8 C17 C22 C21 -178.6(3) . . . . ? C18 C17 C22 C21 55.0(4) . . . . ? C20 C21 C22 C17 -56.7(5) . . . . ? C9 C10 C23 C24 95.3(5) . . . . ? C11 C10 C23 C24 -81.4(5) . . . . ? Zr C10 C23 C24 -172.7(3) . . . . ? C9 C10 C23 C28 -29.0(6) . . . . ? C11 C10 C23 C28 154.4(4) . . . . ? Zr C10 C23 C28 63.1(4) . . . . ? C10 C23 C24 C25 178.0(3) . . . . ? C28 C23 C24 C25 -55.6(4) . . . . ? C23 C24 C25 C26 55.3(5) . . . . ? C24 C25 C26 C27 -54.1(5) . . . . ? C25 C26 C27 C28 54.7(5) . . . . ? C26 C27 C28 C23 -57.1(5) . . . . ? C10 C23 C28 C27 -177.5(3) . . . . ? C24 C23 C28 C27 56.9(4) . . . . ? C7' Zr' C1' C2' -141.4(7) . . . . ? C6' Zr' C1' C2' -118.2(5) . . . . ? C5' Zr' C1' C2' -86.2(4) . . . . ? C3' Zr' C1' C2' -22.6(3) . . . . ? C4' Zr' C1' C2' -52.2(4) . . . . ? C10' Zr' C1' C2' 101.9(4) . . . . ? C12' Zr' C1' C2' 157.9(4) . . . . ? C9' Zr' C1' C2' 99.5(4) . . . . ? C8' Zr' C1' C2' 127.0(4) . . . . ? C11' Zr' C1' C2' 158.7(3) . . . . ? C6' Zr' C1' C7' 23.2(5) . . . . ? C2' Zr' C1' C7' 141.4(7) . . . . ? C5' Zr' C1' C7' 55.2(5) . . . . ? C3' Zr' C1' C7' 118.8(5) . . . . ? C4' Zr' C1' C7' 89.3(5) . . . . ? C10' Zr' C1' C7' -116.7(5) . . . . ? C12' Zr' C1' C7' -60.7(5) . . . . ? C9' Zr' C1' C7' -119.1(5) . . . . ? C8' Zr' C1' C7' -91.6(5) . . . . ? C11' Zr' C1' C7' -59.9(6) . . . . ? C7' C1' C2' C3' 2.0(11) . . . . ? Zr' C1' C2' C3' 50.9(6) . . . . ? C7' C1' C2' Zr' -49.0(6) . . . . ? C7' Zr' C2' C3' -117.8(5) . . . . ? C1' Zr' C2' C3' -141.2(6) . . . . ? C6' Zr' C2' C3' -86.6(5) . . . . ? C5' Zr' C2' C3' -50.7(4) . . . . ? C4' Zr' C2' C3' -22.3(3) . . . . ? C10' Zr' C2' C3' 94.8(4) . . . . ? C12' Zr' C2' C3' -175.3(3) . . . . ? C9' Zr' C2' C3' 122.7(3) . . . . ? C8' Zr' C2' C3' 158.3(3) . . . . ? C11' Zr' C2' C3' 134.6(9) . . . . ? C7' Zr' C2' C1' 23.4(5) . . . . ? C6' Zr' C2' C1' 54.6(5) . . . . ? C5' Zr' C2' C1' 90.5(4) . . . . ? C3' Zr' C2' C1' 141.2(6) . . . . ? C4' Zr' C2' C1' 118.9(4) . . . . ? C10' Zr' C2' C1' -124.0(4) . . . . ? C12' Zr' C2' C1' -34.1(5) . . . . ? C9' Zr' C2' C1' -96.1(4) . . . . ? C8' Zr' C2' C1' -60.5(4) . . . . ? C11' Zr' C2' C1' -84.2(10) . . . . ? C1' C2' C3' C4' -1.5(11) . . . . ? Zr' C2' C3' C4' 48.4(6) . . . . ? C1' C2' C3' Zr' -49.9(6) . . . . ? C7' Zr' C3' C2' 54.4(5) . . . . ? C1' Zr' C3' C2' 23.5(4) . . . . ? C6' Zr' C3' C2' 90.8(5) . . . . ? C5' Zr' C3' C2' 121.4(4) . . . . ? C4' Zr' C3' C2' 142.8(5) . . . . ? C10' Zr' C3' C2' -118.4(4) . . . . ? C12' Zr' C3' C2' 27.4(17) . . . . ? C9' Zr' C3' C2' -76.2(4) . . . . ? C8' Zr' C3' C2' -34.8(5) . . . . ? C11' Zr' C3' C2' -158.4(4) . . . . ? C7' Zr' C3' C4' -88.4(5) . . . . ? C1' Zr' C3' C4' -119.3(4) . . . . ? C6' Zr' C3' C4' -52.0(4) . . . . ? C2' Zr' C3' C4' -142.8(5) . . . . ? C5' Zr' C3' C4' -21.4(3) . . . . ? C10' Zr' C3' C4' 98.8(3) . . . . ? C12' Zr' C3' C4' -115.3(16) . . . . ? C9' Zr' C3' C4' 141.0(3) . . . . ? C8' Zr' C3' C4' -177.6(3) . . . . ? C11' Zr' C3' C4' 58.8(5) . . . . ? C2' C3' C4' C5' -0.7(11) . . . . ? Zr' C3' C4' C5' 47.4(6) . . . . ? C2' C3' C4' Zr' -48.1(6) . . . . ? C7' Zr' C4' C5' -55.9(5) . . . . ? C1' Zr' C4' C5' -91.8(4) . . . . ? C6' Zr' C4' C5' -23.7(4) . . . . ? C2' Zr' C4' C5' -122.1(4) . . . . ? C3' Zr' C4' C5' -144.0(5) . . . . ? C10' Zr' C4' C5' 106.3(4) . . . . ? C12' Zr' C4' C5' 24.9(5) . . . . ? C9' Zr' C4' C5' 144.6(4) . . . . ? C8' Zr' C4' C5' -111(4) . . . . ? C11' Zr' C4' C5' 64.4(4) . . . . ? C7' Zr' C4' C3' 88.1(4) . . . . ? C1' Zr' C4' C3' 52.2(4) . . . . ? C6' Zr' C4' C3' 120.3(4) . . . . ? C2' Zr' C4' C3' 21.9(3) . . . . ? C5' Zr' C4' C3' 144.0(5) . . . . ? C10' Zr' C4' C3' -109.7(3) . . . . ? C12' Zr' C4' C3' 168.8(3) . . . . ? C9' Zr' C4' C3' -71.4(4) . . . . ? C8' Zr' C4' C3' 33(4) . . . . ? C11' Zr' C4' C3' -151.6(3) . . . . ? C3' C4' C5' C6' 0.7(11) . . . . ? Zr' C4' C5' C6' 48.2(6) . . . . ? C3' C4' C5' Zr' -47.5(6) . . . . ? C7' Zr' C5' C4' 116.2(4) . . . . ? C1' Zr' C5' C4' 84.8(4) . . . . ? C6' Zr' C5' C4' 141.4(6) . . . . ? C2' Zr' C5' C4' 49.7(4) . . . . ? C3' Zr' C5' C4' 21.5(3) . . . . ? C10' Zr' C5' C4' -101.1(3) . . . . ? C12' Zr' C5' C4' -165.7(3) . . . . ? C9' Zr' C5' C4' -111.4(7) . . . . ? C8' Zr' C5' C4' 175.5(3) . . . . ? C11' Zr' C5' C4' -131.5(3) . . . . ? C7' Zr' C5' C6' -25.2(5) . . . . ? C1' Zr' C5' C6' -56.6(5) . . . . ? C2' Zr' C5' C6' -91.7(5) . . . . ? C3' Zr' C5' C6' -119.9(5) . . . . ? C4' Zr' C5' C6' -141.4(6) . . . . ? C10' Zr' C5' C6' 117.5(4) . . . . ? C12' Zr' C5' C6' 52.9(5) . . . . ? C9' Zr' C5' C6' 107.2(8) . . . . ? C8' Zr' C5' C6' 34.1(6) . . . . ? C11' Zr' C5' C6' 87.1(5) . . . . ? C4' C5' C6' C7' 1.5(12) . . . . ? Zr' C5' C6' C7' 50.8(7) . . . . ? C4' C5' C6' Zr' -49.3(6) . . . . ? C1' Zr' C6' C7' -22.9(4) . . . . ? C2' Zr' C6' C7' -53.3(5) . . . . ? C5' Zr' C6' C7' -138.6(7) . . . . ? C3' Zr' C6' C7' -86.9(5) . . . . ? C4' Zr' C6' C7' -116.0(5) . . . . ? C10' Zr' C6' C7' 125.3(4) . . . . ? C12' Zr' C6' C7' 87.3(5) . . . . ? C9' Zr' C6' C7' 74.8(6) . . . . ? C8' Zr' C6' C7' 61.1(5) . . . . ? C11' Zr' C6' C7' 117.9(5) . . . . ? C7' Zr' C6' C5' 138.6(7) . . . . ? C1' Zr' C6' C5' 115.7(5) . . . . ? C2' Zr' C6' C5' 85.3(5) . . . . ? C3' Zr' C6' C5' 51.7(4) . . . . ? C4' Zr' C6' C5' 22.5(4) . . . . ? C10' Zr' C6' C5' -96.1(4) . . . . ? C12' Zr' C6' C5' -134.1(4) . . . . ? C9' Zr' C6' C5' -146.6(4) . . . . ? C8' Zr' C6' C5' -160.3(4) . . . . ? C11' Zr' C6' C5' -103.5(4) . . . . ? C2' C1' C7' C6' 0.5(12) . . . . ? Zr' C1' C7' C6' -49.1(7) . . . . ? C2' C1' C7' Zr' 49.6(6) . . . . ? C5' C6' C7' C1' -2.5(13) . . . . ? Zr' C6' C7' C1' 49.2(7) . . . . ? C5' C6' C7' Zr' -51.7(7) . . . . ? C6' Zr' C7' C1' -142.0(7) . . . . ? C2' Zr' C7' C1' -23.0(4) . . . . ? C5' Zr' C7' C1' -117.0(5) . . . . ? C3' Zr' C7' C1' -52.4(5) . . . . ? C4' Zr' C7' C1' -86.7(5) . . . . ? C10' Zr' C7' C1' 118.2(5) . . . . ? C12' Zr' C7' C1' 124.7(5) . . . . ? C9' Zr' C7' C1' 80.2(4) . . . . ? C8' Zr' C7' C1' 91.1(5) . . . . ? C11' Zr' C7' C1' 143.0(4) . . . . ? C1' Zr' C7' C6' 142.0(7) . . . . ? C2' Zr' C7' C6' 119.0(5) . . . . ? C5' Zr' C7' C6' 25.0(5) . . . . ? C3' Zr' C7' C6' 89.6(5) . . . . ? C4' Zr' C7' C6' 55.2(5) . . . . ? C10' Zr' C7' C6' -99.9(6) . . . . ? C12' Zr' C7' C6' -93.4(5) . . . . ? C9' Zr' C7' C6' -137.8(4) . . . . ? C8' Zr' C7' C6' -126.9(5) . . . . ? C11' Zr' C7' C6' -75.0(5) . . . . ? C7' Zr' C8' C9' -163.3(4) . . . . ? C1' Zr' C8' C9' -127.5(4) . . . . ? C6' Zr' C8' C9' 165.5(4) . . . . ? C2' Zr' C8' C9' -97.5(3) . . . . ? C5' Zr' C8' C9' 144.3(4) . . . . ? C3' Zr' C8' C9' -77.4(4) . . . . ? C4' Zr' C8' C9' -109(4) . . . . ? C10' Zr' C8' C9' 35.4(2) . . . . ? C12' Zr' C8' C9' 113.0(3) . . . . ? C11' Zr' C8' C9' 76.1(3) . . . . ? C7' Zr' C8' C12' 83.7(4) . . . . ? C1' Zr' C8' C12' 119.5(4) . . . . ? C6' Zr' C8' C12' 52.5(4) . . . . ? C2' Zr' C8' C12' 149.5(3) . . . . ? C5' Zr' C8' C12' 31.4(4) . . . . ? C3' Zr' C8' C12' 169.6(3) . . . . ? C4' Zr' C8' C12' 138(4) . . . . ? C10' Zr' C8' C12' -77.6(2) . . . . ? C9' Zr' C8' C12' -113.0(3) . . . . ? C11' Zr' C8' C12' -36.9(2) . . . . ? C7' Zr' C8' C17' -40.6(5) . . . . ? C1' Zr' C8' C17' -4.8(4) . . . . ? C6' Zr' C8' C17' -71.8(4) . . . . ? C2' Zr' C8' C17' 25.2(4) . . . . ? C5' Zr' C8' C17' -93.0(5) . . . . ? C3' Zr' C8' C17' 45.3(5) . . . . ? C4' Zr' C8' C17' 14(4) . . . . ? C10' Zr' C8' C17' 158.1(4) . . . . ? C12' Zr' C8' C17' -124.3(4) . . . . ? C9' Zr' C8' C17' 122.7(4) . . . . ? C11' Zr' C8' C17' -161.2(4) . . . . ? C12' C8' C9' C10' 1.7(5) . . . . ? C17' C8' C9' C10' 176.8(4) . . . . ? Zr' C8' C9' C10' -63.8(3) . . . . ? C12' C8' C9' Zr' 65.5(3) . . . . ? C17' C8' C9' Zr' -119.4(4) . . . . ? C7' Zr' C9' C8' 20.5(5) . . . . ? C1' Zr' C9' C8' 59.1(4) . . . . ? C6' Zr' C9' C8' -23.6(6) . . . . ? C2' Zr' C9' C8' 97.2(3) . . . . ? C5' Zr' C9' C8' -103.3(9) . . . . ? C3' Zr' C9' C8' 133.1(3) . . . . ? C4' Zr' C9' C8' 175.3(4) . . . . ? C10' Zr' C9' C8' -118.3(4) . . . . ? C12' Zr' C9' C8' -39.1(2) . . . . ? C11' Zr' C9' C8' -79.5(3) . . . . ? C7' Zr' C9' C10' 138.9(5) . . . . ? C1' Zr' C9' C10' 177.4(4) . . . . ? C6' Zr' C9' C10' 94.7(6) . . . . ? C2' Zr' C9' C10' -144.4(3) . . . . ? C5' Zr' C9' C10' 15.0(9) . . . . ? C3' Zr' C9' C10' -108.5(3) . . . . ? C4' Zr' C9' C10' -66.3(4) . . . . ? C12' Zr' C9' C10' 79.2(3) . . . . ? C8' Zr' C9' C10' 118.3(4) . . . . ? C11' Zr' C9' C10' 38.9(2) . . . . ? C8' C9' C10' C11' -4.3(5) . . . . ? Zr' C9' C10' C11' -68.9(3) . . . . ? C8' C9' C10' C23' -175.7(4) . . . . ? Zr' C9' C10' C23' 119.6(4) . . . . ? C8' C9' C10' Zr' 64.6(3) . . . . ? C7' Zr' C10' C9' -68.8(7) . . . . ? C1' Zr' C10' C9' -4.2(6) . . . . ? C6' Zr' C10' C9' -125.5(5) . . . . ? C2' Zr' C10' C9' 52.5(4) . . . . ? C5' Zr' C10' C9' -173.8(4) . . . . ? C3' Zr' C10' C9' 98.8(3) . . . . ? C4' Zr' C10' C9' 142.9(3) . . . . ? C12' Zr' C10' C9' -76.7(3) . . . . ? C8' Zr' C10' C9' -35.2(2) . . . . ? C11' Zr' C10' C9' -112.1(4) . . . . ? C7' Zr' C10' C11' 43.3(7) . . . . ? C1' Zr' C10' C11' 108.0(6) . . . . ? C6' Zr' C10' C11' -13.3(6) . . . . ? C2' Zr' C10' C11' 164.6(4) . . . . ? C5' Zr' C10' C11' -61.6(4) . . . . ? C3' Zr' C10' C11' -149.0(3) . . . . ? C4' Zr' C10' C11' -105.0(3) . . . . ? C12' Zr' C10' C11' 35.4(2) . . . . ? C9' Zr' C10' C11' 112.1(4) . . . . ? C8' Zr' C10' C11' 76.9(2) . . . . ? C7' Zr' C10' C23' 166.7(7) . . . . ? C1' Zr' C10' C23' -128.6(6) . . . . ? C6' Zr' C10' C23' 110.1(6) . . . . ? C2' Zr' C10' C23' -72.0(5) . . . . ? C5' Zr' C10' C23' 61.8(5) . . . . ? C3' Zr' C10' C23' -25.6(4) . . . . ? C4' Zr' C10' C23' 18.4(4) . . . . ? C12' Zr' C10' C23' 158.8(4) . . . . ? C9' Zr' C10' C23' -124.5(4) . . . . ? C8' Zr' C10' C23' -159.7(4) . . . . ? C11' Zr' C10' C23' 123.4(4) . . . . ? C9' C10' C11' C12' 5.3(5) . . . . ? C23' C10' C11' C12' 176.9(4) . . . . ? Zr' C10' C11' C12' -63.4(3) . . . . ? C9' C10' C11' C16' -177.7(4) . . . . ? C23' C10' C11' C16' -6.1(7) . . . . ? Zr' C10' C11' C16' 113.6(5) . . . . ? C9' C10' C11' Zr' 68.7(3) . . . . ? C23' C10' C11' Zr' -119.7(4) . . . . ? C7' Zr' C11' C12' -36.1(5) . . . . ? C1' Zr' C11' C12' -1.5(5) . . . . ? C6' Zr' C11' C12' -72.0(4) . . . . ? C2' Zr' C11' C12' 65.6(11) . . . . ? C5' Zr' C11' C12' -109.0(4) . . . . ? C3' Zr' C11' C12' -178.8(4) . . . . ? C4' Zr' C11' C12' -141.1(3) . . . . ? C10' Zr' C11' C12' 117.5(3) . . . . ? C9' Zr' C11' C12' 79.1(3) . . . . ? C8' Zr' C11' C12' 38.6(2) . . . . ? C7' Zr' C11' C16' 77.7(5) . . . . ? C1' Zr' C11' C16' 112.2(5) . . . . ? C6' Zr' C11' C16' 41.8(5) . . . . ? C2' Zr' C11' C16' 179.3(10) . . . . ? C5' Zr' C11' C16' 4.8(4) . . . . ? C3' Zr' C11' C16' -65.1(5) . . . . ? C4' Zr' C11' C16' -27.4(4) . . . . ? C10' Zr' C11' C16' -128.8(5) . . . . ? C12' Zr' C11' C16' 113.7(4) . . . . ? C9' Zr' C11' C16' -167.2(4) . . . . ? C8' Zr' C11' C16' 152.3(4) . . . . ? C7' Zr' C11' C10' -153.6(4) . . . . ? C1' Zr' C11' C10' -119.1(4) . . . . ? C6' Zr' C11' C10' 170.5(4) . . . . ? C2' Zr' C11' C10' -52.0(11) . . . . ? C5' Zr' C11' C10' 133.5(3) . . . . ? C3' Zr' C11' C10' 63.7(5) . . . . ? C4' Zr' C11' C10' 101.4(3) . . . . ? C12' Zr' C11' C10' -117.5(3) . . . . ? C9' Zr' C11' C10' -38.4(2) . . . . ? C8' Zr' C11' C10' -78.9(2) . . . . ? C16' C11' C12' C13' 6.3(6) . . . . ? C10' C11' C12' C13' -176.2(4) . . . . ? Zr' C11' C12' C13' 120.7(4) . . . . ? C16' C11' C12' C8' 178.2(4) . . . . ? C10' C11' C12' C8' -4.3(5) . . . . ? Zr' C11' C12' C8' -67.4(3) . . . . ? C16' C11' C12' Zr' -114.4(4) . . . . ? C10' C11' C12' Zr' 63.1(3) . . . . ? C9' C8' C12' C11' 1.7(5) . . . . ? C17' C8' C12' C11' -173.3(4) . . . . ? Zr' C8' C12' C11' 68.2(3) . . . . ? C9' C8' C12' C13' 172.6(4) . . . . ? C17' C8' C12' C13' -2.4(7) . . . . ? Zr' C8' C12' C13' -120.9(5) . . . . ? C9' C8' C12' Zr' -66.5(3) . . . . ? C17' C8' C12' Zr' 118.5(4) . . . . ? C7' Zr' C12' C11' 148.4(4) . . . . ? C1' Zr' C12' C11' 179.0(3) . . . . ? C6' Zr' C12' C11' 112.3(4) . . . . ? C2' Zr' C12' C11' -161.1(3) . . . . ? C5' Zr' C12' C11' 84.4(3) . . . . ? C3' Zr' C12' C11' 175.3(15) . . . . ? C4' Zr' C12' C11' 69.3(4) . . . . ? C10' Zr' C12' C11' -36.1(2) . . . . ? C9' Zr' C12' C11' -76.4(3) . . . . ? C8' Zr' C12' C11' -114.0(3) . . . . ? C7' Zr' C12' C13' 30.3(5) . . . . ? C1' Zr' C12' C13' 60.9(4) . . . . ? C6' Zr' C12' C13' -5.8(5) . . . . ? C2' Zr' C12' C13' 80.8(4) . . . . ? C5' Zr' C12' C13' -33.7(4) . . . . ? C3' Zr' C12' C13' 57.1(16) . . . . ? C4' Zr' C12' C13' -48.8(5) . . . . ? C10' Zr' C12' C13' -154.3(4) . . . . ? C9' Zr' C12' C13' 165.4(4) . . . . ? C8' Zr' C12' C13' 127.9(5) . . . . ? C11' Zr' C12' C13' -118.1(5) . . . . ? C7' Zr' C12' C8' -97.6(4) . . . . ? C1' Zr' C12' C8' -67.0(3) . . . . ? C6' Zr' C12' C8' -133.7(4) . . . . ? C2' Zr' C12' C8' -47.1(4) . . . . ? C5' Zr' C12' C8' -161.6(3) . . . . ? C3' Zr' C12' C8' -70.7(16) . . . . ? C4' Zr' C12' C8' -176.7(3) . . . . ? C10' Zr' C12' C8' 77.9(2) . . . . ? C9' Zr' C12' C8' 37.6(2) . . . . ? C11' Zr' C12' C8' 114.0(3) . . . . ? C11' C12' C13' C14' -5.2(6) . . . . ? C8' C12' C13' C14' -175.1(4) . . . . ? Zr' C12' C13' C14' 87.4(4) . . . . ? C12' C13' C14' C15' 2.5(6) . . . . ? C13' C14' C15' C16' -1.1(7) . . . . ? C14' C15' C16' C11' 2.1(6) . . . . ? C12' C11' C16' C15' -4.7(6) . . . . ? C10' C11' C16' C15' 178.5(4) . . . . ? Zr' C11' C16' C15' -89.8(4) . . . . ? C9' C8' C17' C18' 25.4(6) . . . . ? C12' C8' C17' C18' -160.6(4) . . . . ? Zr' C8' C17' C18' -67.9(4) . . . . ? C9' C8' C17' C22' -99.2(5) . . . . ? C12' C8' C17' C22' 74.8(5) . . . . ? Zr' C8' C17' C22' 167.5(3) . . . . ? C8' C17' C18' C19' 178.9(3) . . . . ? C22' C17' C18' C19' -55.1(5) . . . . ? C17' C18' C19' C20' 55.9(5) . . . . ? C18' C19' C20' C21' -53.6(5) . . . . ? C19' C20' C21' C22' 53.7(4) . . . . ? C20' C21' C22' C17' -55.4(4) . . . . ? C18' C17' C22' C21' 54.9(4) . . . . ? C8' C17' C22' C21' -178.0(3) . . . . ? C9' C10' C23' C28' 22.2(6) . . . . ? C11' C10' C23' C28' -147.7(4) . . . . ? Zr' C10' C23' C28' 117.4(3) . . . . ? C9' C10' C23' C24' -102.2(5) . . . . ? C11' C10' C23' C24' 87.9(5) . . . . ? Zr' C10' C23' C24' -7.0(5) . . . . ? C28' C23' C24' C25' 55.6(5) . . . . ? C10' C23' C24' C25' -177.8(4) . . . . ? C23' C24' C25' C26' -54.6(5) . . . . ? C24' C25' C26' C27' 54.6(5) . . . . ? C25' C26' C27' C28' -56.0(5) . . . . ? C24' C23' C28' C27' -57.3(5) . . . . ? C10' C23' C28' C27' 176.0(4) . . . . ? C26' C27' C28' C23' 58.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.405 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.082 _iucr_refine_instructions ; TITL andyg47 in P2(1)/c CELL 0.71073 13.6123 21.0921 16.3638 90.000 106.805 90.000 ZERR 8.00 0.0008 0.0012 0.0010 0.000 0.006 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H ZR UNIT 224 272 8 SIZE 0.11 0.09 0.05 TEMP -173 SHEL 999 0.8 ACTA CONF FMAP 2 PLAN 10 L.S. 8 SADI C1 H1 C2 H2 C3 H3 C4 H4 C5 H5 C6 H6 C7 H7 C9 H9 C1' H1' C2' H2' C3' H3' = C4' H4' C5' H5' C6' H6' C7' H7' C9' H9' OMIT -2 0 2 OMIT 1 1 3 OMIT 0 1 2 OMIT 1 4 4 OMIT 2 1 5 OMIT 2 1 6 OMIT 1 3 1 OMIT 0 2 2 OMIT 1 1 2 OMIT 1 0 2 OMIT 0 0 6 OMIT 1 3 0 OMIT 0 3 2 OMIT 0 2 3 OMIT 2 1 4 WGHT 0.020000 FVAR 0.87985 ZR 3 0.486312 0.269573 0.592343 11.00000 0.02512 0.02355 = 0.01900 -0.00082 0.00692 -0.00070 C1 1 0.463004 0.361130 0.665832 11.00000 0.06052 0.02979 = 0.04000 -0.01148 0.01294 0.00803 H1 2 0.484404 0.399760 0.661502 11.00000 -1.20000 C2 1 0.367341 0.345249 0.608056 11.00000 0.04926 0.03362 = 0.01777 0.00190 0.00477 0.00919 H2 2 0.348926 0.379199 0.581036 11.00000 -1.20000 C3 1 0.315912 0.286963 0.592270 11.00000 0.03516 0.05569 = 0.03469 -0.00560 0.01164 0.00195 H3 2 0.264369 0.284642 0.547310 11.00000 -1.20000 C4 1 0.348092 0.228471 0.628549 11.00000 0.05441 0.04145 = 0.09462 -0.00445 0.04220 -0.01257 H4 2 0.312716 0.195235 0.606361 11.00000 -1.20000 C5 1 0.441140 0.213043 0.696491 11.00000 0.08086 0.05096 = 0.08168 0.03668 0.06196 0.02729 H5 2 0.453009 0.172928 0.705539 11.00000 -1.20000 C6 1 0.522113 0.254839 0.737272 11.00000 0.06460 0.08282 = 0.01890 0.02370 0.02399 0.03820 H6 2 0.573313 0.235324 0.770596 11.00000 -1.20000 C7 1 0.532065 0.319047 0.724725 11.00000 0.04579 0.06857 = 0.02508 -0.01880 0.00608 0.01256 H7 2 0.594210 0.333970 0.746437 11.00000 -1.20000 C8 1 0.610867 0.289215 0.509298 11.00000 0.01882 0.01895 = 0.01649 -0.00244 0.00482 -0.00056 C9 1 0.531836 0.251190 0.458004 11.00000 0.02070 0.01942 = 0.01645 -0.00244 0.00719 0.00509 H9 2 0.485548 0.263488 0.412022 11.00000 -1.20000 C10 1 0.529004 0.190511 0.493418 11.00000 0.02240 0.02056 = 0.02094 -0.00280 0.01030 -0.00269 C11 1 0.613501 0.189113 0.570276 11.00000 0.02071 0.02874 = 0.01966 0.00907 0.00087 -0.00805 C12 1 0.663731 0.249100 0.579484 11.00000 0.02356 0.01529 = 0.02222 -0.00455 0.00784 -0.00063 C13 1 0.751260 0.259672 0.652437 11.00000 0.02305 0.02609 = 0.03186 -0.00598 0.00529 -0.00619 AFIX 43 H13 2 0.784606 0.299721 0.661227 11.00000 -1.20000 AFIX 0 C14 1 0.785150 0.211844 0.708074 11.00000 0.02249 0.03899 = 0.02679 0.00435 0.00048 0.00339 AFIX 43 H14 2 0.843162 0.218558 0.756105 11.00000 -1.20000 AFIX 0 C15 1 0.736943 0.152466 0.696828 11.00000 0.03127 0.02949 = 0.02768 0.00716 0.00701 0.00679 AFIX 43 H15 2 0.763954 0.120006 0.737342 11.00000 -1.20000 AFIX 0 C16 1 0.653721 0.139594 0.630757 11.00000 0.02559 0.01668 = 0.02550 0.00192 0.00825 0.00156 AFIX 43 H16 2 0.622602 0.098873 0.624443 11.00000 -1.20000 AFIX 0 C17 1 0.640870 0.355294 0.492368 11.00000 0.02351 0.02149 = 0.01443 -0.00026 0.00353 -0.00809 AFIX 13 H17 2 0.675900 0.375002 0.548867 11.00000 -1.20000 AFIX 0 C18 1 0.549573 0.397155 0.448845 11.00000 0.02779 0.02481 = 0.04447 -0.00201 0.01748 0.00075 AFIX 23 H18A 2 0.511792 0.377851 0.393542 11.00000 -1.20000 H18B 2 0.502421 0.399072 0.484877 11.00000 -1.20000 AFIX 0 C19 1 0.581292 0.463840 0.433367 11.00000 0.02513 0.03144 = 0.05485 0.01103 0.00760 0.00501 AFIX 23 H19A 2 0.613052 0.484827 0.488846 11.00000 -1.20000 H19B 2 0.519749 0.488509 0.402840 11.00000 -1.20000 AFIX 0 C20 1 0.657110 0.463403 0.380989 11.00000 0.03665 0.02092 = 0.02807 0.00678 0.00156 -0.01128 AFIX 23 H20A 2 0.680147 0.507221 0.374963 11.00000 -1.20000 H20B 2 0.623280 0.446620 0.323189 11.00000 -1.20000 AFIX 0 C21 1 0.749372 0.422238 0.424636 11.00000 0.03242 0.02955 = 0.03062 -0.00487 0.01227 -0.01159 AFIX 23 H21A 2 0.796297 0.420150 0.388418 11.00000 -1.20000 H21B 2 0.787190 0.441720 0.479804 11.00000 -1.20000 AFIX 0 C22 1 0.716585 0.355737 0.440195 11.00000 0.01567 0.02731 = 0.02034 -0.00572 0.00002 -0.00522 AFIX 23 H22A 2 0.684832 0.334924 0.384589 11.00000 -1.20000 H22B 2 0.777992 0.330869 0.470504 11.00000 -1.20000 AFIX 0 C23 1 0.458459 0.135815 0.459300 11.00000 0.02405 0.02157 = 0.01860 0.00398 0.00560 -0.00163 AFIX 13 H23 2 0.448137 0.112582 0.509450 11.00000 -1.20000 AFIX 0 C24 1 0.504905 0.089385 0.410151 11.00000 0.02061 0.02001 = 0.01864 0.00139 0.00262 -0.00364 AFIX 23 H24A 2 0.571563 0.074137 0.447542 11.00000 -1.20000 H24B 2 0.517900 0.111361 0.360830 11.00000 -1.20000 AFIX 0 C25 1 0.434760 0.033001 0.378377 11.00000 0.02797 0.02614 = 0.02636 -0.00505 0.00906 0.00055 AFIX 23 H25A 2 0.428725 0.008045 0.427939 11.00000 -1.20000 H25B 2 0.465681 0.005329 0.343604 11.00000 -1.20000 AFIX 0 C26 1 0.328111 0.053288 0.324935 11.00000 0.02806 0.02523 = 0.02759 -0.00589 -0.00068 -0.01054 AFIX 23 H26A 2 0.332675 0.072940 0.271212 11.00000 -1.20000 H26B 2 0.283252 0.015544 0.309989 11.00000 -1.20000 AFIX 0 C27 1 0.281708 0.100113 0.373202 11.00000 0.02125 0.02986 = 0.04212 -0.00468 0.00053 -0.00289 AFIX 23 H27A 2 0.269008 0.078774 0.423075 11.00000 -1.20000 H27B 2 0.214990 0.115170 0.335691 11.00000 -1.20000 AFIX 0 C28 1 0.352504 0.156485 0.403450 11.00000 0.02704 0.02313 = 0.04021 -0.00425 0.00864 0.00330 AFIX 23 H28A 2 0.321271 0.185546 0.436416 11.00000 -1.20000 H28B 2 0.360220 0.179937 0.353261 11.00000 -1.20000 AFIX 0 ZR' 3 0.114098 0.381275 0.263837 11.00000 0.02609 0.02743 = 0.02019 0.00313 0.00387 -0.00031 C1' 1 0.124631 0.382617 0.406280 11.00000 0.17735 0.04307 = 0.00967 0.00575 0.02305 0.04318 H1' 2 0.092361 0.408783 0.428348 11.00000 -1.20000 C2' 1 0.059800 0.333114 0.370253 11.00000 0.07337 0.06731 = 0.05328 0.03283 0.04533 0.01789 H2' 2 0.002470 0.332972 0.382349 11.00000 -1.20000 C3' 1 0.075008 0.285686 0.320520 11.00000 0.03610 0.04151 = 0.05531 0.01854 0.00092 -0.00730 H3' 2 0.029777 0.256898 0.304130 11.00000 -1.20000 C4' 1 0.157967 0.274118 0.290455 11.00000 0.07577 0.03213 = 0.02600 -0.00762 0.00175 0.00720 H4' 2 0.139081 0.243661 0.257081 11.00000 -1.20000 C5' 1 0.247098 0.307353 0.301724 11.00000 0.05409 0.09503 = 0.07161 0.05315 0.03444 0.04381 H5' 2 0.281312 0.291898 0.270151 11.00000 -1.20000 C6' 1 0.278089 0.364035 0.349830 11.00000 0.02574 0.12534 = 0.11612 0.09310 -0.02793 -0.00914 H6' 2 0.329340 0.370768 0.330740 11.00000 -1.20000 C7' 1 0.221792 0.396579 0.397732 11.00000 0.14742 0.06042 = 0.05545 0.03404 -0.07800 -0.05224 H7' 2 0.254434 0.431760 0.411690 11.00000 -1.20000 C8' 1 0.064495 0.496619 0.241381 11.00000 0.02401 0.01718 = 0.01743 0.00036 -0.00145 -0.00043 C9' 1 -0.009839 0.462366 0.179023 11.00000 0.01063 0.03283 = 0.01881 0.00561 0.00162 0.00126 H9' 2 -0.072125 0.460241 0.178747 11.00000 -1.20000 C10' 1 0.035298 0.431764 0.122418 11.00000 0.02837 0.01828 = 0.01506 0.00095 0.00669 0.00104 C11' 1 0.140184 0.451098 0.146036 11.00000 0.02023 0.02165 = 0.02333 0.00715 0.00898 0.00058 C12' 1 0.160617 0.487964 0.220257 11.00000 0.01681 0.04637 = 0.01099 -0.00815 0.00650 -0.02300 C13' 1 0.257866 0.516974 0.255727 11.00000 0.03548 0.02352 = 0.02543 0.00329 0.01212 0.00432 AFIX 43 H13' 2 0.269953 0.544776 0.303283 11.00000 -1.20000 AFIX 0 C14' 1 0.333161 0.503251 0.218662 11.00000 0.02069 0.03506 = 0.04239 -0.00350 0.00808 -0.01018 AFIX 43 H14' 2 0.399674 0.520644 0.242554 11.00000 -1.20000 AFIX 0 C15' 1 0.315248 0.463795 0.145508 11.00000 0.02494 0.03695 = 0.04471 -0.00055 0.02085 -0.00123 AFIX 43 H15' 2 0.369195 0.455827 0.120808 11.00000 -1.20000 AFIX 0 C16' 1 0.221803 0.437473 0.110757 11.00000 0.03494 0.02247 = 0.02520 -0.00011 0.00897 -0.00325 AFIX 43 H16' 2 0.210784 0.409989 0.062958 11.00000 -1.20000 AFIX 0 C17' 1 0.044429 0.538016 0.310163 11.00000 0.01403 0.02719 = 0.01727 -0.00503 0.00011 0.00138 AFIX 13 H17' 2 0.104076 0.532721 0.362346 11.00000 -1.20000 AFIX 0 C18' 1 -0.050707 0.520098 0.334374 11.00000 0.02897 0.02802 = 0.02285 -0.00716 0.00645 -0.00689 AFIX 23 H18C 2 -0.044928 0.475373 0.353530 11.00000 -1.20000 H18D 2 -0.111032 0.523460 0.283346 11.00000 -1.20000 AFIX 0 C19' 1 -0.067854 0.561766 0.404813 11.00000 0.02422 0.04226 = 0.02813 -0.00416 0.00892 -0.00759 AFIX 23 H19C 2 -0.133060 0.549548 0.415888 11.00000 -1.20000 H19D 2 -0.011525 0.554811 0.457954 11.00000 -1.20000 AFIX 0 C20' 1 -0.071952 0.631299 0.381078 11.00000 0.02451 0.03300 = 0.01759 -0.00634 0.00294 0.00066 AFIX 23 H20C 2 -0.076256 0.657300 0.430294 11.00000 -1.20000 H20D 2 -0.134106 0.639581 0.333017 11.00000 -1.20000 AFIX 0 C21' 1 0.022876 0.650050 0.355533 11.00000 0.02351 0.02136 = 0.02716 -0.00120 0.00197 0.00288 AFIX 23 H21C 2 0.015669 0.694498 0.335226 11.00000 -1.20000 H21D 2 0.083819 0.647632 0.406179 11.00000 -1.20000 AFIX 0 C22' 1 0.039177 0.607766 0.286201 11.00000 0.02435 0.02384 = 0.02598 -0.00373 0.01051 -0.00358 AFIX 23 H22C 2 0.103819 0.620060 0.274192 11.00000 -1.20000 H22D 2 -0.017743 0.614291 0.233334 11.00000 -1.20000 AFIX 0 C23' 1 -0.019437 0.393829 0.043388 11.00000 0.02676 0.02665 = 0.01619 -0.00155 0.00849 -0.00066 AFIX 13 H23' 2 0.013921 0.404586 -0.001849 11.00000 -1.20000 AFIX 0 C24' 1 -0.009617 0.323009 0.057087 11.00000 0.06392 0.03156 = 0.02896 -0.01003 -0.00632 0.00981 AFIX 23 H24C 2 -0.040828 0.310804 0.102447 11.00000 -1.20000 H24D 2 0.063974 0.311430 0.076586 11.00000 -1.20000 AFIX 0 C25' 1 -0.062577 0.285919 -0.025331 11.00000 0.07585 0.03070 = 0.03921 -0.00702 0.00268 0.00575 AFIX 23 H25C 2 -0.025661 0.293670 -0.068377 11.00000 -1.20000 H25D 2 -0.059386 0.239934 -0.012712 11.00000 -1.20000 AFIX 0 C26' 1 -0.172529 0.305735 -0.060904 11.00000 0.05127 0.04850 = 0.02276 -0.01100 0.00863 -0.01373 AFIX 23 H26C 2 -0.202902 0.283712 -0.115847 11.00000 -1.20000 H26D 2 -0.211308 0.292783 -0.020958 11.00000 -1.20000 AFIX 0 C27' 1 -0.182554 0.374863 -0.074617 11.00000 0.05522 0.04702 = 0.02819 -0.01225 -0.01508 -0.00406 AFIX 23 H27C 2 -0.256110 0.386426 -0.094954 11.00000 -1.20000 H27D 2 -0.150039 0.387419 -0.119025 11.00000 -1.20000 AFIX 0 C28' 1 -0.131025 0.410582 0.008870 11.00000 0.05004 0.03483 = 0.03159 -0.01134 -0.00742 0.00841 AFIX 23 H28C 2 -0.137758 0.456804 -0.001802 11.00000 -1.20000 H28D 2 -0.166687 0.400007 0.051945 11.00000 -1.20000 HKLF 4 ; #============================================================================= # end of cif data for "andyg47" (compound 6) #============================================================================= #============================================================================= # cif data for "mwal01" #============================================================================= data_mwal01 _database_code_depnum_ccdc_archive 'CCDC 853658' #TrackingRef '- BulkyCp-final-121111.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H38' _chemical_formula_weight 362.57 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' _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 11.5611(4) _cell_length_b 13.3654(4) _cell_length_c 13.8835(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.061(2) _cell_angle_gamma 90.00 _cell_volume 2133.27(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17273 _cell_measurement_theta_min 2.3320 _cell_measurement_theta_max 29.1825 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69085 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4355 _reflns_number_gt 3017 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0516P)^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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4355 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.26596(10) 0.44863(9) 0.68208(8) 0.0182(3) Uani 1 1 d . . . C2 C 0.37298(10) 0.38239(9) 0.68745(8) 0.0186(3) Uani 1 1 d . . . H2 H 0.3726 0.3139 0.7058 0.022 Uiso 1 1 calc R . . C3 C 0.46763(10) 0.42974(9) 0.66390(8) 0.0182(3) Uani 1 1 d . . . C4 C 0.43394(10) 0.53339(8) 0.63617(8) 0.0188(3) Uani 1 1 d . . . C5 C 0.49834(11) 0.61170(9) 0.60312(8) 0.0241(3) Uani 1 1 d . . . H5 H 0.5790 0.6038 0.5972 0.029 Uiso 1 1 calc R . . C6 C 0.44285(12) 0.70150(9) 0.57890(9) 0.0268(3) Uani 1 1 d . . . H6 H 0.4862 0.7561 0.5575 0.032 Uiso 1 1 calc R . . C7 C 0.32507(12) 0.71259(9) 0.58547(9) 0.0268(3) Uani 1 1 d . . . H7 H 0.2880 0.7742 0.5671 0.032 Uiso 1 1 calc R . . C8 C 0.26015(11) 0.63468(9) 0.61865(8) 0.0229(3) Uani 1 1 d . . . H8 H 0.1791 0.6426 0.6227 0.028 Uiso 1 1 calc R . . C9 C 0.31506(10) 0.54535(8) 0.64571(8) 0.0183(3) Uani 1 1 d . . . C10 C 0.16601(10) 0.40802(9) 0.60800(8) 0.0185(3) Uani 1 1 d . . . H10 H 0.1024 0.4590 0.6035 0.022 Uiso 1 1 calc R . . C11 C 0.20397(11) 0.39644(9) 0.50610(8) 0.0212(3) Uani 1 1 d . . . H11A H 0.2346 0.4612 0.4851 0.025 Uiso 1 1 calc R . . H11B H 0.2675 0.3466 0.5078 0.025 Uiso 1 1 calc R . . C12 C 0.10359(11) 0.36308(9) 0.43292(9) 0.0243(3) Uani 1 1 d . . . H12A H 0.0423 0.4151 0.4275 0.029 Uiso 1 1 calc R . . H12B H 0.1318 0.3550 0.3685 0.029 Uiso 1 1 calc R . . C13 C 0.05257(11) 0.26468(9) 0.46356(9) 0.0252(3) Uani 1 1 d . . . H13A H 0.1115 0.2111 0.4625 0.030 Uiso 1 1 calc R . . H13B H -0.0151 0.2465 0.4172 0.030 Uiso 1 1 calc R . . C14 C 0.01448(11) 0.27319(10) 0.56508(9) 0.0264(3) Uani 1 1 d . . . H14A H -0.0128 0.2070 0.5854 0.032 Uiso 1 1 calc R . . H14B H -0.0516 0.3205 0.5638 0.032 Uiso 1 1 calc R . . C15 C 0.11329(11) 0.30944(9) 0.63900(9) 0.0224(3) Uani 1 1 d . . . H15A H 0.1748 0.2577 0.6468 0.027 Uiso 1 1 calc R . . H15B H 0.0831 0.3188 0.7025 0.027 Uiso 1 1 calc R . . C16 C 0.22790(10) 0.46068(9) 0.78635(8) 0.0220(3) Uani 1 1 d . . . H16 H 0.2111 0.3918 0.8093 0.026 Uiso 1 1 calc R . . C17 C 0.11680(11) 0.52190(10) 0.79204(9) 0.0272(3) Uani 1 1 d . . . H17A H 0.1296 0.5912 0.7704 0.033 Uiso 1 1 calc R . . H17B H 0.0529 0.4925 0.7479 0.033 Uiso 1 1 calc R . . C18 C 0.08157(12) 0.52390(10) 0.89527(9) 0.0313(3) Uani 1 1 d . . . H18A H 0.0108 0.5653 0.8967 0.038 Uiso 1 1 calc R . . H18B H 0.0629 0.4551 0.9151 0.038 Uiso 1 1 calc R . . C19 C 0.17786(12) 0.56609(10) 0.96646(10) 0.0351(4) Uani 1 1 d . . . H19A H 0.1541 0.5629 1.0329 0.042 Uiso 1 1 calc R . . H19B H 0.1912 0.6371 0.9508 0.042 Uiso 1 1 calc R . . C20 C 0.29016(12) 0.50713(10) 0.96230(9) 0.0322(3) Uani 1 1 d . . . H20A H 0.2794 0.4382 0.9858 0.039 Uiso 1 1 calc R . . H20B H 0.3532 0.5388 1.0056 0.039 Uiso 1 1 calc R . . C21 C 0.32537(11) 0.50317(10) 0.85911(9) 0.0271(3) Uani 1 1 d . . . H21A H 0.3957 0.4610 0.8584 0.033 Uiso 1 1 calc R . . H21B H 0.3452 0.5715 0.8387 0.033 Uiso 1 1 calc R . . C22 C 0.58961(10) 0.39116(9) 0.66564(8) 0.0207(3) Uani 1 1 d . . . H22 H 0.6172 0.4065 0.6014 0.025 Uiso 1 1 calc R . . C23 C 0.59740(11) 0.27801(9) 0.68052(9) 0.0249(3) Uani 1 1 d . . . H23A H 0.5672 0.2606 0.7425 0.030 Uiso 1 1 calc R . . H23B H 0.5480 0.2443 0.6277 0.030 Uiso 1 1 calc R . . C24 C 0.72188(12) 0.24016(11) 0.68202(10) 0.0330(3) Uani 1 1 d . . . H24A H 0.7238 0.1676 0.6962 0.040 Uiso 1 1 calc R . . H24B H 0.7487 0.2499 0.6173 0.040 Uiso 1 1 calc R . . C25 C 0.80424(12) 0.29433(11) 0.75755(10) 0.0376(4) Uani 1 1 d . . . H25A H 0.7840 0.2774 0.8231 0.045 Uiso 1 1 calc R . . H25B H 0.8850 0.2718 0.7526 0.045 Uiso 1 1 calc R . . C26 C 0.79670(11) 0.40679(11) 0.74292(10) 0.0358(4) Uani 1 1 d . . . H26A H 0.8250 0.4243 0.6802 0.043 Uiso 1 1 calc R . . H26B H 0.8474 0.4405 0.7950 0.043 Uiso 1 1 calc R . . C27 C 0.67244(11) 0.44368(10) 0.74404(9) 0.0288(3) Uani 1 1 d . . . H27A H 0.6698 0.5168 0.7328 0.035 Uiso 1 1 calc R . . H27B H 0.6462 0.4307 0.8085 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0199(7) 0.0163(6) 0.0183(6) 0.0014(5) 0.0022(5) 0.0011(5) C2 0.0230(7) 0.0148(6) 0.0173(6) 0.0003(5) -0.0015(5) 0.0007(5) C3 0.0205(7) 0.0193(6) 0.0141(6) -0.0020(5) -0.0010(5) 0.0001(5) C4 0.0235(7) 0.0187(6) 0.0135(6) -0.0022(5) -0.0006(5) -0.0030(5) C5 0.0289(7) 0.0258(7) 0.0175(6) -0.0022(5) 0.0019(5) -0.0076(6) C6 0.0426(9) 0.0192(7) 0.0180(6) 0.0006(5) 0.0005(6) -0.0112(6) C7 0.0460(9) 0.0149(6) 0.0185(6) -0.0002(5) -0.0014(6) 0.0005(6) C8 0.0310(7) 0.0203(7) 0.0171(6) -0.0030(5) 0.0012(5) 0.0042(6) C9 0.0242(7) 0.0175(6) 0.0128(6) -0.0008(5) 0.0002(5) -0.0011(5) C10 0.0167(6) 0.0181(6) 0.0207(6) -0.0003(5) 0.0015(5) 0.0029(5) C11 0.0239(7) 0.0194(6) 0.0205(6) 0.0004(5) 0.0029(5) 0.0019(5) C12 0.0285(7) 0.0227(7) 0.0211(6) -0.0032(5) 0.0002(5) 0.0067(6) C13 0.0233(7) 0.0241(7) 0.0272(7) -0.0064(6) -0.0013(5) 0.0021(6) C14 0.0227(7) 0.0253(7) 0.0314(7) -0.0029(6) 0.0031(6) -0.0026(6) C15 0.0227(7) 0.0224(7) 0.0222(6) -0.0010(5) 0.0034(5) -0.0011(5) C16 0.0280(7) 0.0188(7) 0.0193(6) 0.0009(5) 0.0030(5) -0.0033(5) C17 0.0291(8) 0.0275(7) 0.0259(7) -0.0019(6) 0.0067(6) -0.0019(6) C18 0.0384(8) 0.0281(7) 0.0294(7) -0.0052(6) 0.0140(6) -0.0077(6) C19 0.0485(9) 0.0334(8) 0.0258(7) -0.0086(6) 0.0149(6) -0.0138(7) C20 0.0453(9) 0.0275(8) 0.0230(7) -0.0045(6) -0.0011(6) -0.0101(7) C21 0.0320(8) 0.0246(7) 0.0243(7) -0.0024(6) 0.0011(6) -0.0027(6) C22 0.0200(7) 0.0254(7) 0.0165(6) -0.0001(5) 0.0005(5) -0.0009(5) C23 0.0240(7) 0.0276(7) 0.0228(6) 0.0050(5) 0.0014(5) 0.0040(6) C24 0.0308(8) 0.0384(8) 0.0306(7) 0.0106(6) 0.0064(6) 0.0121(7) C25 0.0219(7) 0.0628(10) 0.0283(8) 0.0160(7) 0.0034(6) 0.0109(7) C26 0.0233(7) 0.0597(10) 0.0234(7) 0.0037(7) -0.0030(6) -0.0043(7) C27 0.0243(7) 0.0396(8) 0.0216(7) -0.0027(6) -0.0009(5) -0.0033(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_2 _geom_bond_publ_flag C1 C2 1.5168(16) . ? C1 C9 1.5195(16) . ? C1 C10 1.5610(15) . ? C1 C16 1.5652(16) . ? C2 C3 1.3343(16) . ? C3 C4 1.4790(16) . ? C3 C22 1.4993(16) . ? C4 C5 1.3902(16) . ? C4 C9 1.4036(17) . ? C5 C6 1.3855(17) . ? C6 C7 1.3822(19) . ? C7 C8 1.3903(18) . ? C8 C9 1.3853(16) . ? C10 C15 1.5323(16) . ? C10 C11 1.5327(16) . ? C11 C12 1.5260(16) . ? C12 C13 1.5204(17) . ? C13 C14 1.5246(18) . ? C14 C15 1.5315(16) . ? C16 C17 1.5319(17) . ? C16 C21 1.5403(16) . ? C17 C18 1.5310(18) . ? C18 C19 1.5171(18) . ? C19 C20 1.525(2) . ? C20 C21 1.5311(18) . ? C22 C23 1.5277(16) . ? C22 C27 1.5408(16) . ? C23 C24 1.5235(18) . ? C24 C25 1.5230(19) . ? C25 C26 1.5180(19) . ? C26 C27 1.5205(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C9 100.46(9) . . ? C2 C1 C10 111.88(9) . . ? C9 C1 C10 110.70(9) . . ? C2 C1 C16 108.79(9) . . ? C9 C1 C16 111.79(9) . . ? C10 C1 C16 112.60(9) . . ? C3 C2 C1 113.38(10) . . ? C2 C3 C4 107.93(10) . . ? C2 C3 C22 128.84(11) . . ? C4 C3 C22 123.21(10) . . ? C5 C4 C9 120.61(11) . . ? C5 C4 C3 130.97(11) . . ? C9 C4 C3 108.41(10) . . ? C6 C5 C4 118.81(12) . . ? C7 C6 C5 120.73(12) . . ? C6 C7 C8 120.77(12) . . ? C9 C8 C7 119.17(12) . . ? C8 C9 C4 119.85(11) . . ? C8 C9 C1 130.29(11) . . ? C4 C9 C1 109.77(10) . . ? C15 C10 C11 109.48(9) . . ? C15 C10 C1 113.75(9) . . ? C11 C10 C1 112.27(9) . . ? C12 C11 C10 111.86(10) . . ? C13 C12 C11 110.90(10) . . ? C12 C13 C14 110.65(10) . . ? C13 C14 C15 112.04(11) . . ? C14 C15 C10 111.99(10) . . ? C17 C16 C21 109.18(10) . . ? C17 C16 C1 114.95(9) . . ? C21 C16 C1 112.76(10) . . ? C18 C17 C16 111.41(10) . . ? C19 C18 C17 111.53(11) . . ? C18 C19 C20 110.63(11) . . ? C19 C20 C21 111.40(11) . . ? C20 C21 C16 112.21(11) . . ? C3 C22 C23 112.62(10) . . ? C3 C22 C27 111.59(10) . . ? C23 C22 C27 109.39(10) . . ? C24 C23 C22 111.88(11) . . ? C25 C24 C23 111.87(12) . . ? C26 C25 C24 110.83(11) . . ? C25 C26 C27 111.14(11) . . ? C26 C27 C22 111.25(11) . . ? 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 C9 C1 C2 C3 2.44(12) . . . . ? C10 C1 C2 C3 119.92(11) . . . . ? C16 C1 C2 C3 -115.05(11) . . . . ? C1 C2 C3 C4 -2.09(13) . . . . ? C1 C2 C3 C22 176.50(11) . . . . ? C2 C3 C4 C5 -177.72(12) . . . . ? C22 C3 C4 C5 3.59(19) . . . . ? C2 C3 C4 C9 0.77(13) . . . . ? C22 C3 C4 C9 -177.91(10) . . . . ? C9 C4 C5 C6 -0.59(16) . . . . ? C3 C4 C5 C6 177.74(11) . . . . ? C4 C5 C6 C7 -1.34(17) . . . . ? C5 C6 C7 C8 1.50(18) . . . . ? C6 C7 C8 C9 0.31(17) . . . . ? C7 C8 C9 C4 -2.23(17) . . . . ? C7 C8 C9 C1 -178.64(11) . . . . ? C5 C4 C9 C8 2.39(16) . . . . ? C3 C4 C9 C8 -176.29(10) . . . . ? C5 C4 C9 C1 179.49(10) . . . . ? C3 C4 C9 C1 0.81(12) . . . . ? C2 C1 C9 C8 174.85(11) . . . . ? C10 C1 C9 C8 56.51(16) . . . . ? C16 C1 C9 C8 -69.89(15) . . . . ? C2 C1 C9 C4 -1.85(11) . . . . ? C10 C1 C9 C4 -120.19(10) . . . . ? C16 C1 C9 C4 113.41(10) . . . . ? C2 C1 C10 C15 67.92(13) . . . . ? C9 C1 C10 C15 179.08(10) . . . . ? C16 C1 C10 C15 -54.97(13) . . . . ? C2 C1 C10 C11 -57.10(13) . . . . ? C9 C1 C10 C11 54.05(13) . . . . ? C16 C1 C10 C11 180.00(9) . . . . ? C15 C10 C11 C12 56.30(13) . . . . ? C1 C10 C11 C12 -176.36(9) . . . . ? C10 C11 C12 C13 -57.88(13) . . . . ? C11 C12 C13 C14 55.95(14) . . . . ? C12 C13 C14 C15 -54.60(14) . . . . ? C13 C14 C15 C10 54.56(14) . . . . ? C11 C10 C15 C14 -54.36(13) . . . . ? C1 C10 C15 C14 179.14(10) . . . . ? C2 C1 C16 C17 -177.18(10) . . . . ? C9 C1 C16 C17 72.78(13) . . . . ? C10 C1 C16 C17 -52.57(14) . . . . ? C2 C1 C16 C21 56.79(13) . . . . ? C9 C1 C16 C21 -53.24(13) . . . . ? C10 C1 C16 C21 -178.60(9) . . . . ? C21 C16 C17 C18 -55.99(13) . . . . ? C1 C16 C17 C18 176.16(10) . . . . ? C16 C17 C18 C19 57.65(14) . . . . ? C17 C18 C19 C20 -56.11(15) . . . . ? C18 C19 C20 C21 54.85(14) . . . . ? C19 C20 C21 C16 -55.41(14) . . . . ? C17 C16 C21 C20 55.27(14) . . . . ? C1 C16 C21 C20 -175.66(10) . . . . ? C2 C3 C22 C23 11.02(17) . . . . ? C4 C3 C22 C23 -170.60(10) . . . . ? C2 C3 C22 C27 -112.47(14) . . . . ? C4 C3 C22 C27 65.92(14) . . . . ? C3 C22 C23 C24 179.96(10) . . . . ? C27 C22 C23 C24 -55.34(14) . . . . ? C22 C23 C24 C25 55.10(14) . . . . ? C23 C24 C25 C26 -54.48(15) . . . . ? C24 C25 C26 C27 55.82(15) . . . . ? C25 C26 C27 C22 -57.69(14) . . . . ? C3 C22 C27 C26 -177.97(10) . . . . ? C23 C22 C27 C26 56.73(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.249 _refine_diff_density_min -0.168 _refine_diff_density_rms 0.032 _iucr_refine_instructions ; TITL mwal01 in P2(1)/n CELL 0.71073 11.5611 13.3654 13.8835 90.000 96.061 90.000 ZERR 4.00 0.0004 0.0004 0.0004 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H UNIT 108 152 SIZE 0.27 0.22 0.20 TEMP -173 SHEL 999 0.8 ACTA CONF FMAP 2 PLAN 10 L.S. 4 OMIT 5 2 1 OMIT 4 3 4 OMIT -1 2 3 OMIT 5 3 1 OMIT 5 0 1 WGHT 0.051600 FVAR 4.01760 C1 1 0.265963 0.448632 0.682079 11.00000 0.01988 0.01631 = 0.01831 0.00142 0.00221 0.00108 C2 1 0.372977 0.382387 0.687447 11.00000 0.02295 0.01483 = 0.01729 0.00034 -0.00150 0.00067 AFIX 43 H2 2 0.372645 0.313912 0.705770 11.00000 -1.20000 AFIX 0 C3 1 0.467630 0.429743 0.663902 11.00000 0.02052 0.01932 = 0.01411 -0.00203 -0.00103 0.00008 C4 1 0.433936 0.533389 0.636170 11.00000 0.02354 0.01870 = 0.01353 -0.00221 -0.00065 -0.00301 C5 1 0.498336 0.611703 0.603120 11.00000 0.02886 0.02584 = 0.01751 -0.00216 0.00190 -0.00761 AFIX 43 H5 2 0.578951 0.603788 0.597247 11.00000 -1.20000 AFIX 0 C6 1 0.442847 0.701502 0.578901 11.00000 0.04264 0.01924 = 0.01799 0.00060 0.00051 -0.01121 AFIX 43 H6 2 0.486227 0.756057 0.557545 11.00000 -1.20000 AFIX 0 C7 1 0.325068 0.712593 0.585466 11.00000 0.04603 0.01492 = 0.01846 -0.00016 -0.00143 0.00055 AFIX 43 H7 2 0.288049 0.774169 0.567093 11.00000 -1.20000 AFIX 0 C8 1 0.260151 0.634679 0.618646 11.00000 0.03103 0.02030 = 0.01714 -0.00297 0.00119 0.00415 AFIX 43 H8 2 0.179149 0.642595 0.622709 11.00000 -1.20000 AFIX 0 C9 1 0.315064 0.545353 0.645708 11.00000 0.02417 0.01748 = 0.01284 -0.00085 0.00018 -0.00115 C10 1 0.166007 0.408016 0.608002 11.00000 0.01668 0.01812 = 0.02066 -0.00029 0.00154 0.00292 AFIX 13 H10 2 0.102400 0.459037 0.603540 11.00000 -1.20000 AFIX 0 C11 1 0.203971 0.396437 0.506101 11.00000 0.02392 0.01941 = 0.02046 0.00041 0.00285 0.00186 AFIX 23 H11A 2 0.234580 0.461154 0.485110 11.00000 -1.20000 H11B 2 0.267499 0.346592 0.507828 11.00000 -1.20000 AFIX 0 C12 1 0.103592 0.363080 0.432920 11.00000 0.02854 0.02267 = 0.02114 -0.00321 0.00023 0.00668 AFIX 23 H12A 2 0.042304 0.415113 0.427508 11.00000 -1.20000 H12B 2 0.131842 0.354998 0.368494 11.00000 -1.20000 AFIX 0 C13 1 0.052570 0.264680 0.463560 11.00000 0.02333 0.02413 = 0.02721 -0.00635 -0.00127 0.00214 AFIX 23 H13A 2 0.111501 0.211061 0.462504 11.00000 -1.20000 H13B 2 -0.015124 0.246467 0.417170 11.00000 -1.20000 AFIX 0 C14 1 0.014479 0.273187 0.565076 11.00000 0.02270 0.02526 = 0.03139 -0.00287 0.00314 -0.00265 AFIX 23 H14A 2 -0.012791 0.207018 0.585420 11.00000 -1.20000 H14B 2 -0.051552 0.320497 0.563827 11.00000 -1.20000 AFIX 0 C15 1 0.113290 0.309438 0.638997 11.00000 0.02271 0.02242 = 0.02218 -0.00096 0.00338 -0.00111 AFIX 23 H15A 2 0.174828 0.257684 0.646827 11.00000 -1.20000 H15B 2 0.083125 0.318833 0.702519 11.00000 -1.20000 AFIX 0 C16 1 0.227896 0.460681 0.786347 11.00000 0.02796 0.01876 = 0.01926 0.00093 0.00299 -0.00335 AFIX 13 H16 2 0.211117 0.391801 0.809327 11.00000 -1.20000 AFIX 0 C17 1 0.116801 0.521901 0.792039 11.00000 0.02905 0.02748 = 0.02592 -0.00190 0.00673 -0.00187 AFIX 23 H17A 2 0.129581 0.591216 0.770357 11.00000 -1.20000 H17B 2 0.052881 0.492513 0.747912 11.00000 -1.20000 AFIX 0 C18 1 0.081573 0.523904 0.895274 11.00000 0.03844 0.02813 = 0.02943 -0.00524 0.01403 -0.00773 AFIX 23 H18A 2 0.010755 0.565289 0.896703 11.00000 -1.20000 H18B 2 0.062910 0.455103 0.915060 11.00000 -1.20000 AFIX 0 C19 1 0.177863 0.566086 0.966465 11.00000 0.04850 0.03338 = 0.02578 -0.00864 0.01494 -0.01380 AFIX 23 H19A 2 0.154116 0.562930 1.032852 11.00000 -1.20000 H19B 2 0.191224 0.637140 0.950802 11.00000 -1.20000 AFIX 0 C20 1 0.290159 0.507129 0.962303 11.00000 0.04529 0.02745 = 0.02298 -0.00446 -0.00110 -0.01010 AFIX 23 H20A 2 0.279380 0.438166 0.985799 11.00000 -1.20000 H20B 2 0.353238 0.538834 1.005596 11.00000 -1.20000 AFIX 0 C21 1 0.325368 0.503173 0.859111 11.00000 0.03204 0.02456 = 0.02433 -0.00244 0.00113 -0.00267 AFIX 23 H21A 2 0.395668 0.460992 0.858428 11.00000 -1.20000 H21B 2 0.345231 0.571483 0.838726 11.00000 -1.20000 AFIX 0 C22 1 0.589607 0.391160 0.665640 11.00000 0.01996 0.02545 = 0.01649 -0.00005 0.00046 -0.00086 AFIX 13 H22 2 0.617232 0.406489 0.601383 11.00000 -1.20000 AFIX 0 C23 1 0.597402 0.278010 0.680521 11.00000 0.02401 0.02762 = 0.02283 0.00500 0.00137 0.00398 AFIX 23 H23A 2 0.567174 0.260564 0.742487 11.00000 -1.20000 H23B 2 0.547959 0.244268 0.627663 11.00000 -1.20000 AFIX 0 C24 1 0.721879 0.240155 0.682023 11.00000 0.03076 0.03838 = 0.03056 0.01057 0.00636 0.01212 AFIX 23 H24A 2 0.723801 0.167552 0.696231 11.00000 -1.20000 H24B 2 0.748685 0.249933 0.617272 11.00000 -1.20000 AFIX 0 C25 1 0.804241 0.294328 0.757552 11.00000 0.02191 0.06284 = 0.02829 0.01601 0.00336 0.01089 AFIX 23 H25A 2 0.783997 0.277415 0.823142 11.00000 -1.20000 H25B 2 0.884978 0.271784 0.752646 11.00000 -1.20000 AFIX 0 C26 1 0.796698 0.406790 0.742916 11.00000 0.02330 0.05965 = 0.02340 0.00367 -0.00296 -0.00435 AFIX 23 H26A 2 0.824959 0.424305 0.680187 11.00000 -1.20000 H26B 2 0.847421 0.440543 0.794965 11.00000 -1.20000 AFIX 0 C27 1 0.672435 0.443679 0.744035 11.00000 0.02432 0.03963 = 0.02159 -0.00270 -0.00090 -0.00330 AFIX 23 H27A 2 0.669808 0.516824 0.732771 11.00000 -1.20000 H27B 2 0.646236 0.430666 0.808494 11.00000 -1.20000 HKLF 4 ; #============================================================================= # end of cif data for "mwal01" #============================================================================= #============================================================================= # end of cif file #=============================================================================