#------------------------------------------------------------------------------ #$Date: 2021-10-29 02:53:16 +0300 (Fri, 29 Oct 2021) $ #$Revision: 270128 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708642.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7708642 loop_ _publ_author_name 'Suzuki, Noriyuki' 'Ban, Sayaka' 'Mochizuki, Ayari' 'Ito, Saki' _publ_section_title ; Reactions of Five-Membered Zirconacycloalkynes And Zirconacycloallenes with Cp2Zr(H)Cl; Formal Hydrogenation by Metal Hydrides ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03313A _journal_year 2021 _chemical_formula_moiety 'C23 H36 Si2 Zr' _chemical_formula_sum 'C23 H36 Si2 Zr' _chemical_formula_weight 459.93 _chemical_name_systematic 1,1-bis(\h5-cyclopentadienyl)-2-triethylsilyl-5-trimethylsilyl-1-zirconacyclopenta-2,3-diene _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_update_record ; 2021-08-22 deposited with the CCDC. 2021-10-26 downloaded from the CCDC. ; _cell_angle_alpha 90.0000 _cell_angle_beta 91.5834(12) _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 7.55776(9) _cell_length_b 23.9500(6) _cell_length_c 13.75372(17) _cell_measurement_reflns_used 13675 _cell_measurement_temperature 213 _cell_measurement_theta_max 76.04 _cell_measurement_theta_min 3.67 _cell_volume 2488.59(8) _computing_cell_refinement 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_molecular_graphics 'CrystalStructure 4.2.5' _computing_publication_material 'CrystalStructure 4.2.5 (Rigaku, 2017)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _diffrn_ambient_temperature 213 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku XtaLAB P100' _diffrn_measurement_method \w _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_Laue_measured_fraction_full 0.000 _diffrn_reflns_Laue_measured_fraction_max 0.000 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 33855 _diffrn_reflns_point_group_measured_fraction_full 0.000 _diffrn_reflns_point_group_measured_fraction_max 0.000 _diffrn_reflns_theta_full 68.400 _diffrn_reflns_theta_max 68.400 _diffrn_reflns_theta_min 3.691 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.675 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_correction_T_min 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 968.00 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: hexane' _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.030 _refine_diff_density_max 1.51 _refine_diff_density_min -0.79 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 229 _refine_ls_number_reflns 4571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0789 _refine_ls_shift/su_max 0.022 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1251P)^2^+8.0709P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2303 _refine_ls_wR_factor_ref 0.2341 _reflns_d_resolution_high 0.8292 _reflns_number_gt 4135 _reflns_number_total 4571 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file d1dt03313a2.cif _cod_data_source_block ns399ar _cod_database_code 7708642 _shelx_title ' xcalibur' _shelx_refln_list_code 4 _shelx_f_calc_maximum 272.75 _shelx_f_squared_multiplier 1.000 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 -1/2+X,-1/2-Y,-1/2+Z 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.60537(7) 0.23619(3) 0.67406(4) 0.0591(3) Uani 1 1 d . . . Si1 Si 0.3840(5) 0.08263(12) 0.6812(2) 0.1080(10) Uani 1 1 d . . . Si2 Si 0.3290(4) 0.37460(11) 0.6609(2) 0.0878(7) Uani 1 1 d . . . C1 C 0.4176(11) 0.1582(4) 0.6930(6) 0.079(2) Uani 1 1 d . . . C2 C 0.3262(9) 0.2012(4) 0.7042(7) 0.075(2) Uani 1 1 d . . . C3 C 0.3053(9) 0.2585(3) 0.7165(7) 0.072(2) Uani 1 1 d . . . H3 H 0.2858 0.2723 0.7832 0.087 Uiso 1 1 calc R . . C4 C 0.3622(9) 0.2988(3) 0.6448(6) 0.072(2) Uani 1 1 d . . . H4 H 0.3057 0.2883 0.5816 0.087 Uiso 1 1 calc R . . C5 C 0.5356 0.0381 0.7434 0.56(4) Uani 1 1 d . . . H5A H 0.6062 0.0642 0.7832 0.676 Uiso 1 1 calc R . . H5B H 0.4605 0.0186 0.7895 0.676 Uiso 1 1 calc R . . C6 C 0.6572 -0.0021 0.7200 0.53(5) Uani 1 1 d . . . H6A H 0.7462 0.0141 0.6791 0.638 Uiso 1 1 calc R . . H6B H 0.5977 -0.0323 0.6853 0.638 Uiso 1 1 calc R . . H6C H 0.7135 -0.0165 0.7791 0.638 Uiso 1 1 calc R . . C7 C 0.203(3) 0.0631(6) 0.7595(17) 0.226(12) Uani 1 1 d . . . H7A H 0.0928 0.0773 0.7294 0.272 Uiso 1 1 calc R . . H7B H 0.1948 0.0223 0.7594 0.272 Uiso 1 1 calc R . . C8 C 0.209(5) 0.0811(9) 0.8579(16) 0.32(2) Uani 1 1 d . . . H8A H 0.2234 0.1213 0.8602 0.385 Uiso 1 1 calc R . . H8B H 0.3088 0.0635 0.8919 0.385 Uiso 1 1 calc R . . H8C H 0.1004 0.0707 0.8889 0.385 Uiso 1 1 calc R . . C9 C 0.335(3) 0.0603(8) 0.5543(13) 0.188(8) Uani 1 1 d . . . H9A H 0.4384 0.0688 0.5156 0.225 Uiso 1 1 calc R . . H9B H 0.3206 0.0196 0.5541 0.225 Uiso 1 1 calc R . . C10 C 0.189(3) 0.0831(8) 0.5081(13) 0.183(8) Uani 1 1 d . . . H10A H 0.2003 0.1235 0.5072 0.219 Uiso 1 1 calc R . . H10B H 0.0835 0.0728 0.5424 0.219 Uiso 1 1 calc R . . H10C H 0.1800 0.0693 0.4418 0.219 Uiso 1 1 calc R . . C11 C 0.132(2) 0.3998(6) 0.5874(11) 0.172(8) Uani 1 1 d . . . H11A H 0.0270 0.3801 0.6075 0.207 Uiso 1 1 calc R . . H11B H 0.1504 0.3928 0.5190 0.207 Uiso 1 1 calc R . . H11C H 0.1165 0.4395 0.5978 0.207 Uiso 1 1 calc R . . C12 C 0.2889(17) 0.3925(5) 0.7894(8) 0.114(4) Uani 1 1 d . . . H12A H 0.2425 0.4302 0.7930 0.136 Uiso 1 1 calc R . . H12B H 0.3992 0.3901 0.8269 0.136 Uiso 1 1 calc R . . H12C H 0.2040 0.3665 0.8156 0.136 Uiso 1 1 calc R . . C13 C 0.517(2) 0.4139(6) 0.6105(17) 0.208(10) Uani 1 1 d . . . H13A H 0.5259 0.4055 0.5417 0.249 Uiso 1 1 calc R . . H13B H 0.6261 0.4030 0.6443 0.249 Uiso 1 1 calc R . . H13C H 0.4981 0.4536 0.6190 0.249 Uiso 1 1 calc R . . C14 C 0.6220(17) 0.2690(7) 0.8497(7) 0.115(4) Uani 1 1 d . . . H14 H 0.5187 0.2789 0.8821 0.138 Uiso 1 1 calc R . . C15 C 0.7185(15) 0.3050(6) 0.8005(7) 0.107(3) Uani 1 1 d . . . H15 H 0.6928 0.3429 0.7892 0.129 Uiso 1 1 calc R . . C16 C 0.8608(11) 0.2766(5) 0.7698(6) 0.084(3) Uani 1 1 d . . . H16 H 0.9539 0.2929 0.7359 0.101 Uiso 1 1 calc R . . C17 C 0.8536(13) 0.2220(5) 0.7937(7) 0.094(3) Uani 1 1 d . . . H17 H 0.9356 0.1939 0.7787 0.113 Uiso 1 1 calc R . . C18 C 0.689(2) 0.2157(7) 0.8483(7) 0.130(5) Uani 1 1 d . . . H18 H 0.6416 0.1832 0.8755 0.156 Uiso 1 1 calc R . . C19 C 0.5896(11) 0.2117(5) 0.4957(5) 0.083(2) Uani 1 1 d . . . H19 H 0.4796 0.2018 0.4672 0.100 Uiso 1 1 calc R . . C20 C 0.7127(18) 0.1758(5) 0.5370(6) 0.103(3) Uani 1 1 d . . . H20 H 0.7007 0.1369 0.5436 0.123 Uiso 1 1 calc R . . C21 C 0.8576(15) 0.2075(8) 0.5668(6) 0.118(5) Uani 1 1 d . . . H21 H 0.9614 0.1939 0.5978 0.142 Uiso 1 1 calc R . . C22 C 0.8235(19) 0.2617(7) 0.5435(8) 0.124(5) Uani 1 1 d . . . H22 H 0.9020 0.2917 0.5531 0.149 Uiso 1 1 calc R . . C23 C 0.6581(19) 0.2650(5) 0.5042(7) 0.103(4) Uani 1 1 d . . . H23 H 0.5993 0.2981 0.4858 0.124 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0372(3) 0.1037(5) 0.0366(3) -0.0098(2) 0.0043(2) 0.0008(2) Si1 0.140(3) 0.0828(16) 0.101(2) -0.0155(14) 0.0155(18) 0.0095(16) Si2 0.0911(17) 0.0785(14) 0.0947(17) -0.0126(12) 0.0200(13) -0.0031(12) C1 0.069(5) 0.087(5) 0.080(5) -0.006(4) 0.012(4) 0.007(4) C2 0.037(3) 0.093(6) 0.094(6) -0.009(4) 0.002(3) -0.009(3) C3 0.038(3) 0.081(5) 0.098(6) -0.011(4) 0.002(4) -0.002(3) C4 0.049(4) 0.089(5) 0.080(5) -0.014(4) -0.004(3) 0.002(3) C5 1.01(11) 0.22(3) 0.45(6) -0.09(3) -0.26(7) 0.37(5) C6 0.21(3) 1.20(15) 0.19(3) -0.09(6) -0.03(2) 0.21(5) C7 0.34(3) 0.090(9) 0.26(2) -0.033(12) 0.16(2) -0.060(13) C8 0.63(6) 0.157(16) 0.18(2) -0.037(15) 0.23(3) -0.09(3) C9 0.25(2) 0.150(13) 0.155(15) -0.041(11) -0.053(15) 0.013(14) C10 0.207(18) 0.186(16) 0.152(15) -0.008(12) -0.061(13) 0.052(14) C11 0.27(2) 0.102(8) 0.144(13) -0.009(8) -0.068(13) 0.049(11) C12 0.143(10) 0.096(7) 0.101(8) -0.029(6) 0.005(7) 0.020(7) C13 0.206(17) 0.125(11) 0.30(2) -0.060(14) 0.150(18) -0.061(11) C14 0.101(8) 0.205(14) 0.038(4) -0.021(6) 0.000(5) -0.023(8) C15 0.097(7) 0.151(10) 0.073(6) -0.038(6) -0.014(5) -0.003(7) C16 0.053(4) 0.154(9) 0.045(4) -0.011(5) -0.005(3) -0.008(5) C17 0.074(6) 0.144(9) 0.064(5) -0.006(6) -0.019(4) 0.013(6) C18 0.176(14) 0.156(11) 0.056(5) 0.038(7) -0.049(7) -0.070(10) C19 0.069(5) 0.134(8) 0.047(4) -0.017(4) -0.008(3) 0.004(5) C20 0.140(10) 0.120(8) 0.051(4) -0.010(5) 0.031(5) 0.040(7) C21 0.084(7) 0.228(15) 0.042(4) -0.017(7) 0.015(4) 0.053(9) C22 0.091(8) 0.225(16) 0.059(6) -0.039(7) 0.042(6) -0.049(9) C23 0.141(11) 0.123(8) 0.048(5) 0.003(4) 0.055(6) 0.014(7) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Si Si 0.2541 0.3302 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Zr Zr -0.1862 2.2449 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Zr1 C1 31.0(3) . . ? C2 Zr1 C4 63.8(3) . . ? C1 Zr1 C4 93.0(3) . . ? C2 Zr1 C3 34.1(3) . . ? C1 Zr1 C3 65.0(3) . . ? C4 Zr1 C3 35.1(3) . . ? C2 Zr1 C23 116.1(4) . . ? C1 Zr1 C23 115.9(4) . . ? C4 Zr1 C23 79.0(4) . . ? C3 Zr1 C23 110.0(4) . . ? C2 Zr1 C17 120.4(4) . . ? C1 Zr1 C17 105.3(4) . . ? C4 Zr1 C17 139.3(3) . . ? C3 Zr1 C17 124.5(3) . . ? C23 Zr1 C17 121.6(5) . . ? C2 Zr1 C16 137.6(3) . . ? C1 Zr1 C16 134.8(3) . . ? C4 Zr1 C16 115.1(3) . . ? C3 Zr1 C16 120.2(3) . . ? C23 Zr1 C16 104.3(4) . . ? C17 Zr1 C16 31.4(3) . . ? C2 Zr1 C18 88.0(4) . . ? C1 Zr1 C18 82.9(4) . . ? C4 Zr1 C18 117.0(5) . . ? C3 Zr1 C18 91.5(5) . . ? C23 Zr1 C18 155.7(5) . . ? C17 Zr1 C18 34.5(4) . . ? C16 Zr1 C18 53.3(4) . . ? C2 Zr1 C19 94.1(3) . . ? C1 Zr1 C19 84.9(3) . . ? C4 Zr1 C19 88.1(3) . . ? C3 Zr1 C19 105.5(3) . . ? C23 Zr1 C19 32.1(4) . . ? C17 Zr1 C19 128.8(3) . . ? C16 Zr1 C19 128.1(3) . . ? C18 Zr1 C19 152.5(5) . . ? C2 Zr1 C15 113.9(4) . . ? C1 Zr1 C15 129.2(4) . . ? C4 Zr1 C15 87.2(3) . . ? C3 Zr1 C15 89.5(3) . . ? C23 Zr1 C15 114.0(4) . . ? C17 Zr1 C15 53.0(4) . . ? C16 Zr1 C15 31.1(3) . . ? C18 Zr1 C15 53.0(4) . . ? C19 Zr1 C15 145.8(4) . . ? C2 Zr1 C20 103.8(4) . . ? C1 Zr1 C20 80.6(4) . . ? C4 Zr1 C20 119.5(3) . . ? C3 Zr1 C20 129.0(4) . . ? C23 Zr1 C20 52.6(3) . . ? C17 Zr1 C20 99.4(4) . . ? C16 Zr1 C20 110.8(4) . . ? C18 Zr1 C20 121.5(5) . . ? C19 Zr1 C20 31.7(3) . . ? C15 Zr1 C20 141.0(4) . . ? C2 Zr1 C14 87.9(4) . . ? C1 Zr1 C14 98.8(4) . . ? C4 Zr1 C14 89.1(4) . . ? C3 Zr1 C14 74.0(4) . . ? C23 Zr1 C14 143.6(5) . . ? C17 Zr1 C14 52.8(4) . . ? C16 Zr1 C14 50.4(3) . . ? C18 Zr1 C14 31.5(4) . . ? C19 Zr1 C14 175.4(5) . . ? C15 Zr1 C14 30.4(4) . . ? C20 Zr1 C14 151.4(4) . . ? C5 Si1 C1 117.8(3) . . ? C5 Si1 C7 92.7(8) . . ? C1 Si1 C7 107.8(5) . . ? C5 Si1 C9 113.0(6) . . ? C1 Si1 C9 113.1(7) . . ? C7 Si1 C9 110.3(11) . . ? C12 Si2 C13 112.8(8) . . ? C12 Si2 C4 111.6(5) . . ? C13 Si2 C4 110.2(6) . . ? C12 Si2 C11 106.9(7) . . ? C13 Si2 C11 104.0(10) . . ? C4 Si2 C11 111.1(5) . . ? C2 C1 Si1 138.3(7) . . ? C2 C1 Zr1 72.5(5) . . ? Si1 C1 Zr1 148.4(4) . . ? C1 C2 C3 152.9(7) . . ? C1 C2 Zr1 76.5(5) . . ? C3 C2 Zr1 76.8(4) . . ? C2 C3 C4 122.3(8) . . ? C2 C3 Zr1 69.0(4) . . ? C4 C3 Zr1 71.7(4) . . ? C2 C3 H3 117.5 . . ? C4 C3 H3 117.5 . . ? Zr1 C3 H3 117.5 . . ? C3 C4 Si2 121.8(6) . . ? C3 C4 Zr1 73.2(4) . . ? Si2 C4 Zr1 134.5(4) . . ? C3 C4 H4 107.4 . . ? Si2 C4 H4 107.4 . . ? Zr1 C4 H4 107.4 . . ? C6 C5 Si1 137.51(10) . . ? C6 C5 H5A 102.7 . . ? Si1 C5 H5A 102.7 . . ? C6 C5 H5B 102.7 . . ? Si1 C5 H5B 102.7 . . ? H5A C5 H5B 105.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 Si1 118.5(18) . . ? C8 C7 H7A 107.7 . . ? Si1 C7 H7A 107.7 . . ? C8 C7 H7B 107.7 . . ? Si1 C7 H7B 107.7 . . ? H7A C7 H7B 107.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Si1 117.3(15) . . ? C10 C9 H9A 108.0 . . ? Si1 C9 H9A 108.0 . . ? C10 C9 H9B 108.0 . . ? Si1 C9 H9B 108.0 . . ? H9A C9 H9B 107.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C18 112.9(12) . . ? C15 C14 Zr1 74.3(6) . . ? C18 C14 Zr1 73.0(6) . . ? C15 C14 H14 123.5 . . ? C18 C14 H14 123.6 . . ? Zr1 C14 H14 120.6 . . ? C14 C15 C16 106.6(13) . . ? C14 C15 Zr1 75.3(6) . . ? C16 C15 Zr1 73.4(5) . . ? C14 C15 H15 126.7 . . ? C16 C15 H15 126.7 . . ? Zr1 C15 H15 116.8 . . ? C15 C16 C17 112.0(10) . . ? C15 C16 Zr1 75.5(5) . . ? C17 C16 Zr1 73.6(5) . . ? C15 C16 H16 124.0 . . ? C17 C16 H16 124.0 . . ? Zr1 C16 H16 118.5 . . ? C16 C17 C18 105.2(10) . . ? C16 C17 Zr1 75.0(5) . . ? C18 C17 Zr1 73.7(5) . . ? C16 C17 H17 127.4 . . ? C18 C17 H17 127.4 . . ? Zr1 C17 H17 116.3 . . ? C14 C18 C17 103.2(10) . . ? C14 C18 Zr1 75.4(6) . . ? C17 C18 Zr1 71.8(5) . . ? C14 C18 H18 128.4 . . ? C17 C18 H18 128.4 . . ? Zr1 C18 H18 117.0 . . ? C20 C19 C23 107.1(10) . . ? C20 C19 Zr1 74.4(5) . . ? C23 C19 Zr1 72.3(5) . . ? C20 C19 H19 126.4 . . ? C23 C19 H19 126.4 . . ? Zr1 C19 H19 118.9 . . ? C21 C20 C19 107.4(11) . . ? C21 C20 Zr1 74.5(5) . . ? C19 C20 Zr1 73.9(5) . . ? C21 C20 H20 126.3 . . ? C19 C20 H20 126.3 . . ? Zr1 C20 H20 117.4 . . ? C20 C21 C22 108.1(10) . . ? C20 C21 Zr1 73.8(5) . . ? C22 C21 Zr1 74.8(6) . . ? C20 C21 H21 126.0 . . ? C22 C21 H21 126.0 . . ? Zr1 C21 H21 117.5 . . ? C23 C22 C21 108.6(12) . . ? C23 C22 Zr1 71.7(5) . . ? C21 C22 Zr1 74.2(6) . . ? C23 C22 H22 125.7 . . ? C21 C22 H22 125.7 . . ? Zr1 C22 H22 120.2 . . ? C22 C23 C19 108.6(11) . . ? C22 C23 Zr1 77.2(6) . . ? C19 C23 Zr1 75.7(5) . . ? C22 C23 H23 125.7 . . ? C19 C23 H23 125.7 . . ? Zr1 C23 H23 113.7 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C2 2.318(7) . ? Zr1 C1 2.364(9) . ? Zr1 C4 2.397(8) . ? Zr1 C3 2.418(7) . ? Zr1 C23 2.478(8) . ? Zr1 C17 2.484(9) . ? Zr1 C16 2.502(8) . ? Zr1 C18 2.510(9) . ? Zr1 C19 2.521(7) . ? Zr1 C15 2.527(9) . ? Zr1 C20 2.528(8) . ? Zr1 C14 2.540(9) . ? Si1 C5 1.768(4) . ? Si1 C1 1.835(9) . ? Si1 C7 1.825(17) . ? Si1 C9 1.855(16) . ? Si2 C12 1.852(11) . ? Si2 C13 1.855(13) . ? Si2 C4 1.848(8) . ? Si2 C11 1.877(15) . ? C1 C2 1.251(11) . ? C2 C3 1.394(12) . ? C3 C4 1.453(12) . ? C3 H3 0.9900 . ? C4 H4 0.9900 . ? C5 C6 1.3753 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.42(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.37(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.327(17) . ? C14 C18 1.372(19) . ? C14 H14 0.9400 . ? C15 C16 1.350(14) . ? C15 H15 0.9400 . ? C16 C17 1.350(15) . ? C16 H16 0.9400 . ? C17 C18 1.479(18) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.378(14) . ? C19 C23 1.381(15) . ? C19 H19 0.9400 . ? C20 C21 1.385(17) . ? C20 H20 0.9400 . ? C21 C22 1.359(19) . ? C21 H21 0.9400 . ? C22 C23 1.351(18) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? 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 C5 Si1 C1 C2 -138.5(11) . . . . ? C7 Si1 C1 C2 -35.5(16) . . . . ? C9 Si1 C1 C2 86.7(14) . . . . ? C5 Si1 C1 Zr1 57.3(10) . . . . ? C7 Si1 C1 Zr1 160.3(12) . . . . ? C9 Si1 C1 Zr1 -77.5(12) . . . . ? C4 Zr1 C1 C2 -18.9(6) . . . . ? C3 Zr1 C1 C2 3.0(6) . . . . ? C23 Zr1 C1 C2 -98.2(7) . . . . ? C17 Zr1 C1 C2 124.4(6) . . . . ? C16 Zr1 C1 C2 111.6(6) . . . . ? C18 Zr1 C1 C2 98.0(7) . . . . ? C19 Zr1 C1 C2 -106.7(6) . . . . ? C15 Zr1 C1 C2 70.0(7) . . . . ? C20 Zr1 C1 C2 -138.3(7) . . . . ? C14 Zr1 C1 C2 70.6(7) . . . . ? C2 Zr1 C1 Si1 169.0(14) . . . . ? C4 Zr1 C1 Si1 150.1(10) . . . . ? C3 Zr1 C1 Si1 172.0(11) . . . . ? C23 Zr1 C1 Si1 70.9(10) . . . . ? C17 Zr1 C1 Si1 -66.6(10) . . . . ? C16 Zr1 C1 Si1 -79.3(10) . . . . ? C18 Zr1 C1 Si1 -93.0(10) . . . . ? C19 Zr1 C1 Si1 62.3(9) . . . . ? C15 Zr1 C1 Si1 -121.0(9) . . . . ? C20 Zr1 C1 Si1 30.7(9) . . . . ? C14 Zr1 C1 Si1 -120.3(10) . . . . ? Si1 C1 C2 C3 178.2(14) . . . . ? Zr1 C1 C2 C3 -10(2) . . . . ? Si1 C1 C2 Zr1 -171.4(11) . . . . ? C4 Zr1 C2 C1 158.9(7) . . . . ? C3 Zr1 C2 C1 -175.2(9) . . . . ? C23 Zr1 C2 C1 97.4(6) . . . . ? C17 Zr1 C2 C1 -67.4(7) . . . . ? C16 Zr1 C2 C1 -101.8(7) . . . . ? C18 Zr1 C2 C1 -79.5(7) . . . . ? C19 Zr1 C2 C1 73.0(6) . . . . ? C15 Zr1 C2 C1 -127.2(6) . . . . ? C20 Zr1 C2 C1 42.5(7) . . . . ? C14 Zr1 C2 C1 -111.1(7) . . . . ? C1 Zr1 C2 C3 175.2(9) . . . . ? C4 Zr1 C2 C3 -26.0(5) . . . . ? C23 Zr1 C2 C3 -87.5(6) . . . . ? C17 Zr1 C2 C3 107.8(6) . . . . ? C16 Zr1 C2 C3 73.3(7) . . . . ? C18 Zr1 C2 C3 95.6(7) . . . . ? C19 Zr1 C2 C3 -111.8(6) . . . . ? C15 Zr1 C2 C3 48.0(6) . . . . ? C20 Zr1 C2 C3 -142.4(5) . . . . ? C14 Zr1 C2 C3 64.1(6) . . . . ? C1 C2 C3 C4 61(2) . . . . ? Zr1 C2 C3 C4 50.1(7) . . . . ? C1 C2 C3 Zr1 10.4(19) . . . . ? C1 Zr1 C3 C2 -2.7(5) . . . . ? C4 Zr1 C3 C2 136.9(8) . . . . ? C23 Zr1 C3 C2 107.3(6) . . . . ? C17 Zr1 C3 C2 -94.6(6) . . . . ? C16 Zr1 C3 C2 -131.6(5) . . . . ? C18 Zr1 C3 C2 -84.2(6) . . . . ? C19 Zr1 C3 C2 73.9(6) . . . . ? C15 Zr1 C3 C2 -137.2(6) . . . . ? C20 Zr1 C3 C2 49.7(7) . . . . ? C14 Zr1 C3 C2 -110.8(6) . . . . ? C2 Zr1 C3 C4 -136.9(8) . . . . ? C1 Zr1 C3 C4 -139.7(6) . . . . ? C23 Zr1 C3 C4 -29.6(6) . . . . ? C17 Zr1 C3 C4 128.5(6) . . . . ? C16 Zr1 C3 C4 91.4(6) . . . . ? C18 Zr1 C3 C4 138.9(6) . . . . ? C19 Zr1 C3 C4 -63.0(5) . . . . ? C15 Zr1 C3 C4 85.9(6) . . . . ? C20 Zr1 C3 C4 -87.2(6) . . . . ? C14 Zr1 C3 C4 112.3(6) . . . . ? C2 C3 C4 Si2 178.6(6) . . . . ? Zr1 C3 C4 Si2 -132.4(6) . . . . ? C2 C3 C4 Zr1 -49.0(6) . . . . ? C12 Si2 C4 C3 18.8(8) . . . . ? C13 Si2 C4 C3 144.9(10) . . . . ? C11 Si2 C4 C3 -100.5(9) . . . . ? C12 Si2 C4 Zr1 -78.8(7) . . . . ? C13 Si2 C4 Zr1 47.3(11) . . . . ? C11 Si2 C4 Zr1 162.0(8) . . . . ? C2 Zr1 C4 C3 25.3(5) . . . . ? C1 Zr1 C4 C3 36.0(5) . . . . ? C23 Zr1 C4 C3 151.8(6) . . . . ? C17 Zr1 C4 C3 -81.8(7) . . . . ? C16 Zr1 C4 C3 -107.4(5) . . . . ? C18 Zr1 C4 C3 -47.6(6) . . . . ? C19 Zr1 C4 C3 120.8(5) . . . . ? C15 Zr1 C4 C3 -93.1(6) . . . . ? C20 Zr1 C4 C3 116.9(6) . . . . ? C14 Zr1 C4 C3 -62.8(6) . . . . ? C2 Zr1 C4 Si2 143.6(7) . . . . ? C1 Zr1 C4 Si2 154.3(6) . . . . ? C3 Zr1 C4 Si2 118.3(9) . . . . ? C23 Zr1 C4 Si2 -89.9(7) . . . . ? C17 Zr1 C4 Si2 36.6(9) . . . . ? C16 Zr1 C4 Si2 10.9(7) . . . . ? C18 Zr1 C4 Si2 70.8(7) . . . . ? C19 Zr1 C4 Si2 -120.9(6) . . . . ? C15 Zr1 C4 Si2 25.2(7) . . . . ? C20 Zr1 C4 Si2 -124.8(6) . . . . ? C14 Zr1 C4 Si2 55.6(7) . . . . ? C1 Si1 C5 C6 -117.5(3) . . . . ? C7 Si1 C5 C6 130.8(6) . . . . ? C9 Si1 C5 C6 17.4(8) . . . . ? C5 Si1 C7 C8 70(2) . . . . ? C1 Si1 C7 C8 -51(2) . . . . ? C9 Si1 C7 C8 -175(2) . . . . ? C5 Si1 C9 C10 164.3(16) . . . . ? C1 Si1 C9 C10 -59(2) . . . . ? C7 Si1 C9 C10 62(2) . . . . ? C2 Zr1 C14 C15 -149.9(9) . . . . ? C1 Zr1 C14 C15 -178.9(8) . . . . ? C4 Zr1 C14 C15 -86.0(8) . . . . ? C3 Zr1 C14 C15 -118.2(9) . . . . ? C23 Zr1 C14 C15 -16.0(13) . . . . ? C17 Zr1 C14 C15 78.5(9) . . . . ? C16 Zr1 C14 C15 38.2(7) . . . . ? C18 Zr1 C14 C15 120.5(13) . . . . ? C19 Zr1 C14 C15 -34(5) . . . . ? C20 Zr1 C14 C15 94.6(13) . . . . ? C2 Zr1 C14 C18 89.6(9) . . . . ? C1 Zr1 C14 C18 60.5(9) . . . . ? C4 Zr1 C14 C18 153.4(9) . . . . ? C3 Zr1 C14 C18 121.3(9) . . . . ? C23 Zr1 C14 C18 -136.6(10) . . . . ? C17 Zr1 C14 C18 -42.0(8) . . . . ? C16 Zr1 C14 C18 -82.3(9) . . . . ? C19 Zr1 C14 C18 -155(4) . . . . ? C15 Zr1 C14 C18 -120.5(13) . . . . ? C20 Zr1 C14 C18 -26.0(14) . . . . ? C18 C14 C15 C16 -3.9(12) . . . . ? Zr1 C14 C15 C16 -67.3(6) . . . . ? C18 C14 C15 Zr1 63.4(8) . . . . ? C2 Zr1 C15 C14 33.3(9) . . . . ? C1 Zr1 C15 C14 1.4(10) . . . . ? C4 Zr1 C15 C14 93.0(9) . . . . ? C3 Zr1 C15 C14 57.9(9) . . . . ? C23 Zr1 C15 C14 169.7(9) . . . . ? C17 Zr1 C15 C14 -77.8(9) . . . . ? C16 Zr1 C15 C14 -112.7(12) . . . . ? C18 Zr1 C15 C14 -34.3(9) . . . . ? C19 Zr1 C15 C14 175.4(8) . . . . ? C20 Zr1 C15 C14 -130.7(9) . . . . ? C2 Zr1 C15 C16 146.0(7) . . . . ? C1 Zr1 C15 C16 114.1(7) . . . . ? C4 Zr1 C15 C16 -154.3(8) . . . . ? C3 Zr1 C15 C16 170.6(8) . . . . ? C23 Zr1 C15 C16 -77.6(8) . . . . ? C17 Zr1 C15 C16 34.9(6) . . . . ? C18 Zr1 C15 C16 78.4(8) . . . . ? C19 Zr1 C15 C16 -71.9(10) . . . . ? C20 Zr1 C15 C16 -18.0(11) . . . . ? C14 Zr1 C15 C16 112.7(12) . . . . ? C14 C15 C16 C17 3.4(11) . . . . ? Zr1 C15 C16 C17 -65.2(7) . . . . ? C14 C15 C16 Zr1 68.6(7) . . . . ? C2 Zr1 C16 C15 -49.3(10) . . . . ? C1 Zr1 C16 C15 -94.5(9) . . . . ? C4 Zr1 C16 C15 28.6(8) . . . . ? C3 Zr1 C16 C15 -10.9(9) . . . . ? C23 Zr1 C16 C15 113.0(8) . . . . ? C17 Zr1 C16 C15 -118.7(10) . . . . ? C18 Zr1 C16 C15 -77.5(9) . . . . ? C19 Zr1 C16 C15 137.2(7) . . . . ? C20 Zr1 C16 C15 168.0(7) . . . . ? C14 Zr1 C16 C15 -37.2(7) . . . . ? C2 Zr1 C16 C17 69.3(8) . . . . ? C1 Zr1 C16 C17 24.2(8) . . . . ? C4 Zr1 C16 C17 147.2(6) . . . . ? C3 Zr1 C16 C17 107.8(6) . . . . ? C23 Zr1 C16 C17 -128.4(6) . . . . ? C18 Zr1 C16 C17 41.2(7) . . . . ? C19 Zr1 C16 C17 -104.1(7) . . . . ? C15 Zr1 C16 C17 118.7(10) . . . . ? C20 Zr1 C16 C17 -73.3(6) . . . . ? C14 Zr1 C16 C17 81.4(7) . . . . ? C15 C16 C17 C18 -1.7(10) . . . . ? Zr1 C16 C17 C18 -68.1(6) . . . . ? C15 C16 C17 Zr1 66.4(7) . . . . ? C2 Zr1 C17 C16 -133.0(6) . . . . ? C1 Zr1 C17 C16 -162.5(5) . . . . ? C4 Zr1 C17 C16 -48.8(8) . . . . ? C3 Zr1 C17 C16 -92.5(6) . . . . ? C23 Zr1 C17 C16 63.1(7) . . . . ? C18 Zr1 C17 C16 -111.1(10) . . . . ? C19 Zr1 C17 C16 101.7(7) . . . . ? C15 Zr1 C17 C16 -34.6(6) . . . . ? C20 Zr1 C17 C16 114.8(6) . . . . ? C14 Zr1 C17 C16 -72.9(7) . . . . ? C2 Zr1 C17 C18 -21.9(9) . . . . ? C1 Zr1 C17 C18 -51.4(9) . . . . ? C4 Zr1 C17 C18 62.3(11) . . . . ? C3 Zr1 C17 C18 18.6(10) . . . . ? C23 Zr1 C17 C18 174.3(8) . . . . ? C16 Zr1 C17 C18 111.1(10) . . . . ? C19 Zr1 C17 C18 -147.2(8) . . . . ? C15 Zr1 C17 C18 76.5(8) . . . . ? C20 Zr1 C17 C18 -134.1(8) . . . . ? C14 Zr1 C17 C18 38.2(7) . . . . ? C15 C14 C18 C17 2.8(11) . . . . ? Zr1 C14 C18 C17 66.9(6) . . . . ? C15 C14 C18 Zr1 -64.1(8) . . . . ? C16 C17 C18 C14 -0.6(10) . . . . ? Zr1 C17 C18 C14 -69.6(7) . . . . ? C16 C17 C18 Zr1 69.0(6) . . . . ? C2 Zr1 C18 C14 -89.2(9) . . . . ? C1 Zr1 C18 C14 -119.9(9) . . . . ? C4 Zr1 C18 C14 -30.1(9) . . . . ? C3 Zr1 C18 C14 -55.3(8) . . . . ? C23 Zr1 C18 C14 97.5(15) . . . . ? C17 Zr1 C18 C14 109.5(10) . . . . ? C16 Zr1 C18 C14 72.2(8) . . . . ? C19 Zr1 C18 C14 175.8(7) . . . . ? C15 Zr1 C18 C14 33.0(7) . . . . ? C20 Zr1 C18 C14 165.8(8) . . . . ? C2 Zr1 C18 C17 161.2(8) . . . . ? C1 Zr1 C18 C17 130.6(8) . . . . ? C4 Zr1 C18 C17 -139.6(8) . . . . ? C3 Zr1 C18 C17 -164.8(8) . . . . ? C23 Zr1 C18 C17 -12.0(17) . . . . ? C16 Zr1 C18 C17 -37.3(6) . . . . ? C19 Zr1 C18 C17 66.3(11) . . . . ? C15 Zr1 C18 C17 -76.5(7) . . . . ? C20 Zr1 C18 C17 56.2(9) . . . . ? C14 Zr1 C18 C17 -109.5(10) . . . . ? C2 Zr1 C19 C20 -109.9(8) . . . . ? C1 Zr1 C19 C20 -80.3(8) . . . . ? C4 Zr1 C19 C20 -173.5(8) . . . . ? C3 Zr1 C19 C20 -142.7(7) . . . . ? C23 Zr1 C19 C20 114.2(10) . . . . ? C17 Zr1 C19 C20 25.2(9) . . . . ? C16 Zr1 C19 C20 65.7(9) . . . . ? C18 Zr1 C19 C20 -16.5(12) . . . . ? C15 Zr1 C19 C20 104.3(9) . . . . ? C14 Zr1 C19 C20 135(4) . . . . ? C2 Zr1 C19 C23 135.9(7) . . . . ? C1 Zr1 C19 C23 165.5(7) . . . . ? C4 Zr1 C19 C23 72.3(7) . . . . ? C3 Zr1 C19 C23 103.1(7) . . . . ? C17 Zr1 C19 C23 -89.0(9) . . . . ? C16 Zr1 C19 C23 -48.6(9) . . . . ? C18 Zr1 C19 C23 -130.7(10) . . . . ? C15 Zr1 C19 C23 -9.9(10) . . . . ? C20 Zr1 C19 C23 -114.2(10) . . . . ? C14 Zr1 C19 C23 21(5) . . . . ? C23 C19 C20 C21 -2.2(9) . . . . ? Zr1 C19 C20 C21 -67.5(6) . . . . ? C23 C19 C20 Zr1 65.4(5) . . . . ? C2 Zr1 C20 C21 -171.3(8) . . . . ? C1 Zr1 C20 C21 -150.6(8) . . . . ? C4 Zr1 C20 C21 121.2(8) . . . . ? C3 Zr1 C20 C21 162.6(8) . . . . ? C23 Zr1 C20 C21 76.3(8) . . . . ? C17 Zr1 C20 C21 -46.6(9) . . . . ? C16 Zr1 C20 C21 -16.2(9) . . . . ? C18 Zr1 C20 C21 -75.0(9) . . . . ? C19 Zr1 C20 C21 113.8(10) . . . . ? C15 Zr1 C20 C21 -6.3(11) . . . . ? C14 Zr1 C20 C21 -59.5(12) . . . . ? C2 Zr1 C20 C19 75.0(7) . . . . ? C1 Zr1 C20 C19 95.6(7) . . . . ? C4 Zr1 C20 C19 7.5(9) . . . . ? C3 Zr1 C20 C19 48.8(8) . . . . ? C23 Zr1 C20 C19 -37.5(7) . . . . ? C17 Zr1 C20 C19 -160.3(7) . . . . ? C16 Zr1 C20 C19 -129.9(7) . . . . ? C18 Zr1 C20 C19 171.2(7) . . . . ? C15 Zr1 C20 C19 -120.1(8) . . . . ? C14 Zr1 C20 C19 -173.2(8) . . . . ? C19 C20 C21 C22 -0.4(10) . . . . ? Zr1 C20 C21 C22 -67.5(6) . . . . ? C19 C20 C21 Zr1 67.1(6) . . . . ? C2 Zr1 C21 C20 12.1(10) . . . . ? C1 Zr1 C21 C20 30.6(8) . . . . ? C4 Zr1 C21 C20 -80.5(10) . . . . ? C3 Zr1 C21 C20 -37.9(18) . . . . ? C23 Zr1 C21 C20 -78.4(7) . . . . ? C17 Zr1 C21 C20 132.8(9) . . . . ? C16 Zr1 C21 C20 164.7(8) . . . . ? C18 Zr1 C21 C20 119.3(7) . . . . ? C19 Zr1 C21 C20 -37.4(6) . . . . ? C15 Zr1 C21 C20 175.8(7) . . . . ? C14 Zr1 C21 C20 148.3(7) . . . . ? C2 Zr1 C21 C22 126.5(10) . . . . ? C1 Zr1 C21 C22 145.1(8) . . . . ? C4 Zr1 C21 C22 33.9(11) . . . . ? C3 Zr1 C21 C22 76.6(17) . . . . ? C23 Zr1 C21 C22 36.1(7) . . . . ? C17 Zr1 C21 C22 -112.8(9) . . . . ? C16 Zr1 C21 C22 -80.9(9) . . . . ? C18 Zr1 C21 C22 -126.2(8) . . . . ? C19 Zr1 C21 C22 77.0(8) . . . . ? C15 Zr1 C21 C22 -69.8(9) . . . . ? C20 Zr1 C21 C22 114.4(10) . . . . ? C14 Zr1 C21 C22 -97.2(9) . . . . ? C20 C21 C22 C23 2.9(10) . . . . ? Zr1 C21 C22 C23 -63.9(7) . . . . ? C20 C21 C22 Zr1 66.8(6) . . . . ? C2 Zr1 C22 C23 25.8(14) . . . . ? C1 Zr1 C22 C23 69.2(12) . . . . ? C4 Zr1 C22 C23 -38.0(9) . . . . ? C3 Zr1 C22 C23 -30.0(11) . . . . ? C17 Zr1 C22 C23 -179.6(9) . . . . ? C16 Zr1 C22 C23 -151.0(10) . . . . ? C18 Zr1 C22 C23 -175.8(8) . . . . ? C19 Zr1 C22 C23 38.2(7) . . . . ? C15 Zr1 C22 C23 -126.8(9) . . . . ? C20 Zr1 C22 C23 78.8(8) . . . . ? C14 Zr1 C22 C23 -137.0(8) . . . . ? C2 Zr1 C22 C21 -90.5(12) . . . . ? C1 Zr1 C22 C21 -47.1(11) . . . . ? C4 Zr1 C22 C21 -154.3(8) . . . . ? C3 Zr1 C22 C21 -146.3(8) . . . . ? C23 Zr1 C22 C21 -116.3(11) . . . . ? C17 Zr1 C22 C21 64.1(9) . . . . ? C16 Zr1 C22 C21 92.7(9) . . . . ? C18 Zr1 C22 C21 67.9(10) . . . . ? C19 Zr1 C22 C21 -78.0(8) . . . . ? C15 Zr1 C22 C21 117.0(9) . . . . ? C20 Zr1 C22 C21 -37.5(7) . . . . ? C14 Zr1 C22 C21 106.7(9) . . . . ? C21 C22 C23 C19 -4.3(10) . . . . ? Zr1 C22 C23 C19 -69.8(6) . . . . ? C21 C22 C23 Zr1 65.5(7) . . . . ? C20 C19 C23 C22 4.0(9) . . . . ? Zr1 C19 C23 C22 70.8(6) . . . . ? C20 C19 C23 Zr1 -66.8(6) . . . . ? C2 Zr1 C23 C22 -164.0(9) . . . . ? C1 Zr1 C23 C22 -129.5(9) . . . . ? C4 Zr1 C23 C22 142.5(9) . . . . ? C3 Zr1 C23 C22 159.3(9) . . . . ? C17 Zr1 C23 C22 0.5(10) . . . . ? C16 Zr1 C23 C22 29.2(9) . . . . ? C18 Zr1 C23 C22 8.4(16) . . . . ? C19 Zr1 C23 C22 -113.4(11) . . . . ? C15 Zr1 C23 C22 60.6(9) . . . . ? C20 Zr1 C23 C22 -76.3(8) . . . . ? C14 Zr1 C23 C22 69.4(11) . . . . ? C2 Zr1 C23 C19 -50.7(8) . . . . ? C1 Zr1 C23 C19 -16.1(8) . . . . ? C4 Zr1 C23 C19 -104.2(7) . . . . ? C3 Zr1 C23 C19 -87.3(7) . . . . ? C17 Zr1 C23 C19 113.8(8) . . . . ? C16 Zr1 C23 C19 142.5(7) . . . . ? C18 Zr1 C23 C19 121.8(12) . . . . ? C15 Zr1 C23 C19 173.9(6) . . . . ? C20 Zr1 C23 C19 37.0(6) . . . . ? C14 Zr1 C23 C19 -177.3(7) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 9300.17 10443.20 146.95 o 4 0 0 21585.13 22619.04 608.40 o 6 0 0 362.91 420.35 21.37 o 8 0 0 267.76 499.69 20.16 o 1 1 0 1835.13 1601.72 80.70 o 2 1 0 2681.37 3352.83 78.23 o 3 1 0 8.67 2.43 4.23 o 4 1 0 5445.70 6175.56 219.98 o 5 1 0 626.76 564.32 21.98 o 6 1 0 1431.85 1479.13 38.83 o 7 1 0 5.86 2.99 3.66 o 8 1 0 1391.19 1519.92 30.45 o 9 1 0 9.03 3.06 4.44 o 0 2 0 68081.92 65655.30 3478.80 o 1 2 0 221.75 1064.86 38.71 o 2 2 0 157.88 179.18 10.62 o 3 2 0 98.71 84.43 6.48 o 4 2 0 11107.33 10191.12 247.29 o 5 2 0 167.85 102.34 10.23 o 6 2 0 749.05 832.67 20.49 o 7 2 0 3.36 7.71 4.13 o 8 2 0 296.22 481.05 15.52 o 9 2 0 0.26 -3.41 3.41 o 1 3 0 4.52 50.19 3.21 o 2 3 0 13294.77 10055.82 219.54 o 3 3 0 535.91 453.64 14.04 o 4 3 0 3055.60 2684.65 64.09 o 5 3 0 705.20 738.91 23.03 o 6 3 0 1904.60 1775.38 30.68 o 7 3 0 54.20 55.22 4.17 o 8 3 0 999.86 1062.84 21.93 o 9 3 0 33.32 27.11 3.55 o 0 4 0 22193.21 21644.94 1149.22 o 1 4 0 13095.76 9357.63 311.37 o 2 4 0 461.85 438.25 12.09 o 3 4 0 2612.20 2446.94 69.83 o 4 4 0 6896.37 5955.34 137.84 o 5 4 0 165.97 215.29 12.87 o 6 4 0 996.51 883.26 21.10 o 7 4 0 368.23 331.32 8.21 o 8 4 0 349.39 449.87 9.99 o 9 4 0 0.67 0.24 2.66 o 1 5 0 3211.74 2554.03 80.13 o 2 5 0 10288.92 13615.55 362.02 o 3 5 0 389.95 316.30 18.95 o 4 5 0 1854.40 1885.32 51.93 o 5 5 0 76.44 66.64 10.40 o 6 5 0 1268.53 1230.32 27.29 o 7 5 0 33.61 38.13 3.42 o 8 5 0 580.78 620.80 16.71 o 0 6 0 74391.94 74064.08 3926.36 o 1 6 0 596.73 127.85 6.16 o 2 6 0 10.25 8.50 5.67 o 3 6 0 3685.01 3650.82 119.27 o 4 6 0 6933.07 6941.47 221.66 o 5 6 0 33.94 30.73 14.86 o 6 6 0 555.00 438.97 13.53 o 7 6 0 812.58 778.46 14.13 o 8 6 0 235.88 234.26 9.11 o 1 7 0 2429.87 2050.60 148.76 o 2 7 0 4610.60 3271.81 100.56 o 3 7 0 1467.75 1400.58 63.85 o 4 7 0 2728.02 2393.07 83.31 o 5 7 0 1118.25 1004.91 20.46 o 6 7 0 1297.77 1365.72 23.24 o 7 7 0 3.08 14.05 3.73 o 8 7 0 330.35 351.09 15.96 o 0 8 0 1736.94 1201.63 70.05 o 1 8 0 931.50 444.08 37.63 o 2 8 0 62.94 82.38 6.82 o 3 8 0 2095.81 1773.83 102.55 o 4 8 0 2487.19 2028.48 88.46 o 5 8 0 4.47 15.73 3.15 o 6 8 0 220.59 211.84 8.89 o 7 8 0 596.00 624.87 12.91 o 8 8 0 71.91 67.15 4.30 o 1 9 0 554.17 370.80 20.76 o 2 9 0 3821.10 3631.06 123.24 o 3 9 0 32.48 47.76 7.08 o 4 9 0 1093.59 938.67 28.88 o 5 9 0 1682.67 1636.18 24.14 o 6 9 0 1144.31 990.99 18.82 o 7 9 0 7.47 18.05 4.25 o 8 9 0 134.39 133.67 8.68 o 0 10 0 32.67 58.03 12.20 o 1 10 0 10601.64 9701.79 444.45 o 2 10 0 256.84 250.69 14.31 o 3 10 0 3682.27 3647.85 89.01 o 4 10 0 749.50 540.41 25.14 o 5 10 0 249.08 257.35 5.82 o 6 10 0 338.35 335.32 8.43 o 7 10 0 444.67 393.27 8.43 o 8 10 0 44.74 61.48 4.49 o 1 11 0 1224.73 1246.59 73.43 o 2 11 0 2622.63 2269.61 78.63 o 3 11 0 24.21 21.49 5.45 o 4 11 0 54.00 58.63 7.97 o 5 11 0 1190.15 1106.62 18.73 o 6 11 0 313.81 324.71 8.44 o 7 11 0 13.10 17.88 3.31 o 8 11 0 17.32 24.46 4.00 o 0 12 0 783.67 637.35 42.10 o 1 12 0 193.20 173.78 11.70 o 2 12 0 471.76 378.56 15.44 o 3 12 0 1676.42 1553.05 63.19 o 4 12 0 387.12 387.69 13.51 o 5 12 0 10.33 24.55 3.69 o 6 12 0 372.32 381.86 10.04 o 7 12 0 394.30 385.64 8.85 o 8 12 0 33.89 32.91 4.59 o 1 13 0 3086.90 2867.86 78.81 o 2 13 0 1312.72 1173.50 48.88 o 3 13 0 1256.18 1176.44 41.10 o 4 13 0 24.72 22.84 3.30 o 5 13 0 1341.80 1285.97 29.89 o 6 13 0 144.32 148.58 6.22 o 7 13 0 0.58 9.88 3.57 o 8 13 0 3.42 11.28 5.35 o 0 14 0 31.29 55.13 10.64 o 1 14 0 2.59 15.08 7.21 o 2 14 0 8.03 19.07 5.13 o 3 14 0 346.40 339.08 32.61 o 4 14 0 0.90 22.17 3.64 o 5 14 0 4.34 6.56 3.75 o 6 14 0 44.26 57.54 5.00 o 7 14 0 329.31 349.50 7.86 o 1 15 0 1983.26 1678.67 52.58 o 2 15 0 319.90 312.70 16.96 o 3 15 0 457.90 412.04 11.50 o 4 15 0 213.05 227.30 8.79 o 5 15 0 798.27 790.14 15.11 o 6 15 0 109.54 123.69 5.84 o 7 15 0 0.34 5.38 3.90 o 0 16 0 88.47 83.46 10.25 o 1 16 0 1766.05 2042.41 72.56 o 2 16 0 301.99 297.02 17.94 o 3 16 0 976.12 990.31 24.13 o 4 16 0 1.23 6.21 4.56 o 5 16 0 17.86 28.22 4.63 o 6 16 0 16.09 23.82 4.62 o 7 16 0 209.05 205.16 8.20 o 1 17 0 182.30 276.03 17.34 o 2 17 0 180.97 207.38 7.17 o 3 17 0 1.11 5.63 3.71 o 4 17 0 48.10 45.14 5.08 o 5 17 0 510.41 576.44 12.97 o 6 17 0 1.12 6.40 4.36 o 7 17 0 0.34 5.69 5.12 o 0 18 0 113.04 64.24 12.60 o 1 18 0 564.77 512.50 37.25 o 2 18 0 8.13 8.21 4.44 o 3 18 0 381.56 349.45 10.79 o 4 18 0 13.59 14.79 4.87 o 5 18 0 9.72 14.88 4.64 o 6 18 0 4.35 12.42 5.05 o 7 18 0 88.17 78.73 5.78 o 1 19 0 238.57 210.51 14.43 o 2 19 0 6.82 14.06 4.87 o 3 19 0 13.75 8.51 3.87 o 4 19 0 3.24 13.19 5.24 o 5 19 0 413.69 484.71 16.61 o 6 19 0 2.22 4.76 4.20 o 0 20 0 177.73 187.58 19.08 o 1 20 0 76.03 88.15 8.22 o 2 20 0 3.02 13.63 5.13 o 3 20 0 158.54 190.79 6.08 o 4 20 0 25.38 26.63 4.73 o 5 20 0 1.01 2.22 4.20 o 6 20 0 0.05 7.57 3.68 o 1 21 0 185.49 229.92 10.00 o 2 21 0 2.16 5.43 4.67 o 3 21 0 69.72 88.34 4.87 o 4 21 0 2.76 7.05 4.32 o 5 21 0 120.23 127.30 7.23 o 6 21 0 0.02 1.85 3.38 o 0 22 0 12.51 39.73 17.82 o 1 22 0 35.99 57.32 6.91 o 2 22 0 9.60 8.74 5.35 o 3 22 0 214.18 258.35 9.07 o 4 22 0 12.69 3.75 4.22 o 5 22 0 0.09 5.03 4.59 o 1 23 0 55.39 87.88 6.91 o 2 23 0 181.74 176.72 7.96 o 3 23 0 7.43 15.77 4.15 o 4 23 0 0.47 3.93 4.53 o 5 23 0 46.21 60.40 4.44 o 0 24 0 22.81 27.90 10.98 o 1 24 0 13.11 34.15 6.64 o 2 24 0 2.69 8.00 5.04 o 3 24 0 34.88 43.65 4.96 o 4 24 0 0.14 -1.16 4.66 o 5 24 0 0.03 9.10 5.44 o 1 25 0 39.06 56.47 7.51 o 2 25 0 61.20 73.04 5.54 o 3 25 0 0.19 0.95 4.78 o 4 25 0 0.02 7.86 4.07 o 0 26 0 37.13 49.45 13.38 o 1 26 0 20.97 32.61 4.77 o 2 26 0 5.12 9.46 4.12 o 3 26 0 6.13 9.52 3.83 o 1 27 0 2.59 14.07 3.94 o 2 27 0 2.31 5.29 3.31 o 3 27 0 0.30 6.41 3.10 o 0 28 0 61.62 59.32 7.10 o 1 28 0 15.43 23.07 3.86 o 2 28 0 0.00 3.15 3.15 o -9 0 1 71.57 147.41 8.73 o -7 0 1 2530.12 2738.09 75.24 o -5 0 1 1481.64 1310.91 181.91 o -3 0 1 2878.07 2701.96 76.01 o -1 0 1 12122.12 19395.71 1031.02 o 1 0 1 11966.44 11165.62 418.33 o 3 0 1 14337.08 13942.81 375.75 o 5 0 1 1070.31 1602.18 73.78 o 7 0 1 2123.26 2399.80 53.94 o 9 0 1 160.85 170.85 7.68 o -9 1 1 646.67 582.38 11.59 o -8 1 1 1.57 -2.71 3.36 o -7 1 1 196.41 382.51 26.76 o -6 1 1 36.80 26.97 4.21 o -5 1 1 2709.28 2597.70 89.51 o -4 1 1 754.30 731.38 31.99 o -3 1 1 17190.72 17262.30 373.86 o -2 1 1 27.64 86.86 6.81 o -1 1 1 17522.83 21663.95 970.24 o 0 1 1 828.60 1231.17 43.99 o 1 1 1 36267.49 40010.10 1547.56 o 2 1 1 670.41 990.52 24.04 o 3 1 1 1849.29 2135.35 65.39 o 4 1 1 129.42 108.76 6.92 o 5 1 1 2209.64 2175.85 119.65 o 6 1 1 50.57 43.20 4.38 o 7 1 1 1015.64 1339.63 35.93 o 8 1 1 2.08 2.59 3.12 o 9 1 1 244.48 318.32 8.39 o -9 2 1 65.96 108.20 3.84 o -8 2 1 23.45 20.66 3.75 o -7 2 1 2446.80 2490.66 43.63 o -6 2 1 264.37 249.34 6.63 o -5 2 1 2641.39 2701.04 93.06 o -4 2 1 99.63 136.98 8.50 o -3 2 1 6274.36 5262.26 127.56 o -2 2 1 566.44 262.84 9.06 o -1 2 1 35602.25 33623.20 721.25 o 0 2 1 844.09 2193.76 215.43 o 1 2 1 9238.44 7755.85 239.70 o 2 2 1 800.84 455.03 12.77 o 3 2 1 14845.17 14445.37 346.28 o 4 2 1 1236.92 1116.46 49.77 o 5 2 1 346.21 335.56 18.31 o 6 2 1 214.63 214.67 6.44 o 7 2 1 1790.92 1962.56 40.41 o 8 2 1 0.64 3.19 3.33 o 9 2 1 183.97 210.97 6.84 o -9 3 1 659.32 678.57 16.09 o -8 3 1 6.84 3.72 3.73 o -7 3 1 99.03 172.92 11.87 o -6 3 1 525.15 492.87 10.28 o -5 3 1 1296.54 1366.14 40.43 o -4 3 1 33.77 46.61 5.73 o -3 3 1 8004.20 7014.72 157.43 o -2 3 1 926.40 540.88 14.54 o -1 3 1 4150.70 3887.48 122.70 o 0 3 1 400.82 213.03 47.64 o 1 3 1 22839.00 21331.42 655.03 o 2 3 1 90.72 26.85 3.65 o 3 3 1 1291.55 1586.18 38.32 o 4 3 1 0.99 8.32 5.22 o 5 3 1 3886.75 3941.46 103.30 o 6 3 1 0.09 5.83 3.17 o 7 3 1 788.21 836.33 20.41 o 8 3 1 40.46 48.20 3.58 o 9 3 1 256.66 291.93 7.88 o -9 4 1 52.34 64.09 4.95 o -8 4 1 54.64 67.70 4.36 o -7 4 1 1629.87 1544.22 31.41 o -6 4 1 1.36 9.35 3.02 o -5 4 1 3705.88 3405.61 91.80 o -4 4 1 441.73 298.43 14.99 o -3 4 1 9526.68 10522.84 232.13 o -2 4 1 576.49 369.00 11.34 o -1 4 1 41047.09 38498.76 1737.82 o 0 4 1 430.20 638.35 19.21 o 1 4 1 18621.50 19856.60 609.57 o 2 4 1 5333.27 5217.35 139.94 o 3 4 1 12594.23 12599.61 302.67 o 4 4 1 11.71 -2.68 6.53 o 5 4 1 51.33 55.01 11.26 o 6 4 1 271.07 301.11 8.70 o 7 4 1 1158.29 1142.04 22.38 o 8 4 1 26.74 24.73 3.63 o -8 5 1 102.96 77.90 4.45 o -7 5 1 99.70 119.62 4.68 o -6 5 1 846.95 784.75 13.30 o -5 5 1 1903.97 1882.52 54.10 o -4 5 1 516.20 565.29 22.46 o -3 5 1 3416.53 3770.20 85.50 o -2 5 1 3519.32 3839.80 110.43 o -1 5 1 2199.79 2329.57 84.54 o 0 5 1 3980.42 4477.10 128.20 o 1 5 1 11152.39 12955.98 450.04 o 2 5 1 516.30 742.89 34.16 o 3 5 1 536.41 385.10 16.81 o 4 5 1 1973.70 2068.95 63.79 o 5 5 1 3287.43 2962.73 117.53 o 6 5 1 261.60 225.20 8.37 o 7 5 1 457.24 475.62 11.15 o 8 5 1 167.89 171.93 7.83 o -8 6 1 145.50 168.52 6.06 o -7 6 1 1055.34 1068.85 18.49 o -6 6 1 28.03 35.67 5.17 o -5 6 1 1479.43 1138.61 44.90 o -4 6 1 3580.13 3453.70 155.96 o -3 6 1 5990.06 5038.05 124.79 o -2 6 1 1488.15 1920.38 60.30 o -1 6 1 2130.18 1720.07 51.84 o 0 6 1 16788.02 19007.44 679.75 o 1 6 1 1368.64 1664.39 54.35 o 2 6 1 6.74 4.44 5.62 o 3 6 1 6774.72 6353.66 246.44 o 4 6 1 64.34 90.99 10.97 o 5 6 1 292.05 280.41 18.61 o 6 6 1 177.44 154.85 4.73 o 7 6 1 935.41 996.73 18.24 o 8 6 1 38.52 40.78 5.72 o -8 7 1 117.02 110.10 5.39 o -7 7 1 130.82 146.92 6.10 o -6 7 1 644.27 609.64 12.79 o -5 7 1 1161.97 1022.76 25.80 o -4 7 1 0.15 44.82 10.53 o -3 7 1 5049.82 4270.43 118.75 o -2 7 1 961.40 836.66 28.15 o -1 7 1 3127.68 2676.81 65.97 o 0 7 1 2490.15 1855.85 51.20 o 1 7 1 5742.36 4436.83 137.85 o 2 7 1 170.92 209.02 20.74 o 3 7 1 40.45 17.38 9.61 o 4 7 1 3174.72 2724.63 97.40 o 5 7 1 1430.12 1509.45 25.13 o 6 7 1 50.81 63.24 3.65 o 7 7 1 348.43 378.81 10.68 o 8 7 1 327.96 305.28 11.68 o -8 8 1 272.99 242.20 10.24 o -7 8 1 935.37 908.81 18.56 o -6 8 1 40.56 38.31 4.78 o -5 8 1 569.28 632.04 12.04 o -4 8 1 3352.76 3050.11 101.81 o -3 8 1 2869.53 2445.74 81.87 o -2 8 1 40.26 5.93 3.74 o -1 8 1 1836.58 1723.71 44.14 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