# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(C6H4)(ArO)2TiCl(dme) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H42 Cl O4 Ti' _chemical_formula_sum 'C32 H42 Cl O4 Ti' _chemical_formula_weight 574.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 26.4628(17) _cell_length_b 11.6059(6) _cell_length_c 19.5905(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6016.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10777 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9158 _exptl_absorpt_correction_T_max 0.9452 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Mercury375R CCD (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 13.6612 _diffrn_reflns_number 41404 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13770 _reflns_number_gt 8939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2009)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2009)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(3) _refine_ls_number_reflns 13770 _refine_ls_number_parameters 705 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Ti1 Ti 0.80006(3) 0.10035(8) 0.82019(4) 0.0196(2) Uani 1 1 d . . . Cl1 Cl 0.79661(5) -0.08258(11) 0.76356(6) 0.0266(3) Uani 1 1 d . . . O1 O 0.86759(12) 0.0860(3) 0.84777(16) 0.0223(8) Uani 1 1 d . . . O2 O 0.73012(12) 0.1295(3) 0.81333(16) 0.0207(7) Uani 1 1 d . . . C1 C 0.83267(19) 0.0489(4) 0.9753(2) 0.0220(11) Uani 1 1 d . . . C2 C 0.80209(18) -0.0280(4) 0.9389(3) 0.0211(12) Uani 1 1 d . . . H1 H 0.8158 -0.0983 0.9225 0.025 Uiso 1 1 calc R . . C3 C 0.7520(2) -0.0016(4) 0.9269(2) 0.0248(11) Uani 1 1 d . . . H2 H 0.7315 -0.0545 0.9024 0.030 Uiso 1 1 calc R . . C4 C 0.73068(18) 0.1023(4) 0.9503(2) 0.0211(10) Uani 1 1 d . . . C5 C 0.75896(19) 0.1671(4) 0.9959(2) 0.0239(11) Uani 1 1 d . . . H3 H 0.7436 0.2295 1.0194 0.029 Uiso 1 1 calc R . . C6 C 0.80961(19) 0.1415(4) 1.0075(3) 0.0222(11) Uani 1 1 d . . . H4 H 0.8287 0.1882 1.0379 0.027 Uiso 1 1 calc R . . C7 C 0.90376(19) 0.0626(4) 0.8959(3) 0.0236(11) Uani 1 1 d . . . C8 C 0.95540(19) 0.0588(4) 0.8790(3) 0.0220(11) Uani 1 1 d . . . C9 C 0.98910(19) 0.0328(4) 0.9320(2) 0.0236(11) Uani 1 1 d . . . H5 H 1.0241 0.0282 0.9215 0.028 Uiso 1 1 calc R . . C10 C 0.9741(2) 0.0132(4) 0.9995(3) 0.0260(12) Uani 1 1 d . . . C11 C 0.92307(18) 0.0188(4) 1.0149(3) 0.0241(11) Uani 1 1 d . . . H6 H 0.9121 0.0062 1.0604 0.029 Uiso 1 1 calc R . . C12 C 0.8878(2) 0.0426(4) 0.9645(3) 0.0220(12) Uani 1 1 d . . . C13 C 0.68479(19) 0.1507(4) 0.8453(2) 0.0217(11) Uani 1 1 d . . . C14 C 0.68384(18) 0.1430(4) 0.9174(2) 0.0200(11) Uani 1 1 d . . . C15 C 0.64072(17) 0.1757(4) 0.9527(2) 0.0198(10) Uani 1 1 d . . . H7 H 0.6405 0.1732 1.0012 0.024 Uiso 1 1 calc R . . C16 C 0.59751(18) 0.2124(4) 0.9174(3) 0.0246(11) Uani 1 1 d . . . C17 C 0.59898(18) 0.2103(4) 0.8460(3) 0.0239(11) Uani 1 1 d . . . H8 H 0.5692 0.2307 0.8219 0.029 Uiso 1 1 calc R . . C18 C 0.64173(19) 0.1798(4) 0.8082(2) 0.0224(11) Uani 1 1 d . . . C19 C 0.97445(19) 0.0783(4) 0.8054(2) 0.0231(11) Uani 1 1 d . . . C20 C 0.9545(2) -0.0190(4) 0.7594(3) 0.0303(12) Uani 1 1 d . . . H9 H 0.9665 -0.0070 0.7126 0.045 Uiso 1 1 calc R . . H10 H 0.9175 -0.0186 0.7599 0.045 Uiso 1 1 calc R . . H11 H 0.9668 -0.0933 0.7763 0.045 Uiso 1 1 calc R . . C21 C 0.9559(2) 0.1950(4) 0.7782(3) 0.0312(13) Uani 1 1 d . . . H12 H 0.9690 0.2570 0.8072 0.047 Uiso 1 1 calc R . . H13 H 0.9188 0.1966 0.7788 0.047 Uiso 1 1 calc R . . H14 H 0.9679 0.2057 0.7313 0.047 Uiso 1 1 calc R . . C22 C 1.0323(2) 0.0806(5) 0.8005(3) 0.0317(14) Uani 1 1 d . . . H15 H 1.0423 0.0930 0.7529 0.048 Uiso 1 1 calc R . . H16 H 1.0460 0.0070 0.8165 0.048 Uiso 1 1 calc R . . H17 H 1.0455 0.1433 0.8288 0.048 Uiso 1 1 calc R . . C23 C 1.01248(19) -0.0140(5) 1.0549(3) 0.0316(13) Uani 1 1 d . . . H18 H 1.0138 0.0497 1.0877 0.047 Uiso 1 1 calc R . . H19 H 1.0459 -0.0245 1.0342 0.047 Uiso 1 1 calc R . . H20 H 1.0025 -0.0849 1.0786 0.047 Uiso 1 1 calc R . . C24 C 0.6409(2) 0.1776(4) 0.7292(2) 0.0243(11) Uani 1 1 d . . . C25 C 0.6549(2) 0.0558(4) 0.7047(3) 0.0319(13) Uani 1 1 d . . . H21 H 0.6886 0.0356 0.7216 0.048 Uiso 1 1 calc R . . H22 H 0.6548 0.0538 0.6547 0.048 Uiso 1 1 calc R . . H23 H 0.6301 0.0004 0.7222 0.048 Uiso 1 1 calc R . . C26 C 0.6785(2) 0.2645(5) 0.7012(3) 0.0352(14) Uani 1 1 d . . . H24 H 0.7130 0.2385 0.7111 0.053 Uiso 1 1 calc R . . H25 H 0.6728 0.3396 0.7227 0.053 Uiso 1 1 calc R . . H26 H 0.6741 0.2715 0.6517 0.053 Uiso 1 1 calc R . . C27 C 0.5887(2) 0.2085(5) 0.7007(3) 0.0348(14) Uani 1 1 d . . . H27 H 0.5897 0.2065 0.6507 0.052 Uiso 1 1 calc R . . H28 H 0.5792 0.2860 0.7160 0.052 Uiso 1 1 calc R . . H29 H 0.5637 0.1527 0.7172 0.052 Uiso 1 1 calc R . . C28 C 0.55161(18) 0.2557(4) 0.9547(3) 0.0295(12) Uani 1 1 d . . . H30 H 0.5404 0.3284 0.9343 0.044 Uiso 1 1 calc R . . H31 H 0.5601 0.2684 1.0029 0.044 Uiso 1 1 calc R . . H32 H 0.5245 0.1985 0.9514 0.044 Uiso 1 1 calc R . . O3 O 0.81518(13) 0.1965(3) 0.73021(17) 0.0264(8) Uani 1 1 d . . . O4 O 0.80592(12) 0.2862(3) 0.85573(16) 0.0220(8) Uani 1 1 d . . . C29 C 0.8316(2) 0.1526(5) 0.6645(3) 0.0413(15) Uani 1 1 d . . . H33 H 0.8115 0.1882 0.6282 0.062 Uiso 1 1 calc R . . H34 H 0.8271 0.0689 0.6633 0.062 Uiso 1 1 calc R . . H35 H 0.8674 0.1712 0.6577 0.062 Uiso 1 1 calc R . . C30 C 0.8191(2) 0.3207(4) 0.7353(3) 0.0281(12) Uani 1 1 d . . . H36 H 0.8043 0.3576 0.6944 0.034 Uiso 1 1 calc R . . H37 H 0.8550 0.3440 0.7387 0.034 Uiso 1 1 calc R . . C31 C 0.79058(18) 0.3571(4) 0.7987(2) 0.0231(11) Uani 1 1 d . . . H38 H 0.7977 0.4391 0.8088 0.028 Uiso 1 1 calc R . . H39 H 0.7538 0.3487 0.7910 0.028 Uiso 1 1 calc R . . C32 C 0.85018(18) 0.3329(4) 0.8897(3) 0.0273(12) Uani 1 1 d . . . H40 H 0.8778 0.3403 0.8567 0.041 Uiso 1 1 calc R . . H41 H 0.8605 0.2811 0.9267 0.041 Uiso 1 1 calc R . . H42 H 0.8421 0.4089 0.9086 0.041 Uiso 1 1 calc R . . Ti2 Ti 0.67006(3) 0.60679(8) 1.01408(4) 0.0194(2) Uani 1 1 d . . . Cl2 Cl 0.67314(5) 0.42223(11) 1.06814(6) 0.0285(3) Uani 1 1 d . . . O5 O 0.60200(12) 0.5924(3) 0.98575(16) 0.0199(7) Uani 1 1 d . . . O6 O 0.73975(12) 0.6356(3) 1.02151(16) 0.0213(8) Uani 1 1 d . . . C33 C 0.6378(2) 0.5555(4) 0.8590(2) 0.0224(12) Uani 1 1 d . . . C34 C 0.66800(18) 0.4780(4) 0.8958(3) 0.0230(12) Uani 1 1 d . . . H43 H 0.6537 0.4080 0.9120 0.028 Uiso 1 1 calc R . . C35 C 0.71794(19) 0.5018(4) 0.9086(2) 0.0203(11) Uani 1 1 d . . . H44 H 0.7379 0.4488 0.9339 0.024 Uiso 1 1 calc R . . C36 C 0.73963(19) 0.6060(4) 0.8841(2) 0.0230(10) Uani 1 1 d . . . C37 C 0.7123(2) 0.6725(5) 0.8385(2) 0.0258(12) Uani 1 1 d . . . H45 H 0.7281 0.7353 0.8158 0.031 Uiso 1 1 calc R . . C38 C 0.66122(19) 0.6473(4) 0.8258(3) 0.0237(11) Uani 1 1 d . . . H46 H 0.6426 0.6930 0.7945 0.028 Uiso 1 1 calc R . . C39 C 0.56598(19) 0.5688(4) 0.9383(2) 0.0183(11) Uani 1 1 d . . . C40 C 0.51490(18) 0.5637(4) 0.9540(2) 0.0201(10) Uani 1 1 d . . . C41 C 0.48098(18) 0.5382(4) 0.9011(2) 0.0214(10) Uani 1 1 d . . . H47 H 0.4460 0.5339 0.9115 0.026 Uiso 1 1 calc R . . C42 C 0.49625(19) 0.5188(4) 0.8337(2) 0.0219(11) Uani 1 1 d . . . C43 C 0.54686(19) 0.5252(4) 0.8195(3) 0.0237(12) Uani 1 1 d . . . H48 H 0.5581 0.5124 0.7741 0.028 Uiso 1 1 calc R . . C44 C 0.58205(19) 0.5499(4) 0.8698(2) 0.0210(11) Uani 1 1 d . . . C45 C 0.78475(18) 0.6540(4) 0.9897(3) 0.0217(11) Uani 1 1 d . . . C46 C 0.78690(18) 0.6451(4) 0.9173(2) 0.0209(11) Uani 1 1 d . . . C47 C 0.83005(18) 0.6740(4) 0.8823(2) 0.0225(11) Uani 1 1 d . . . H49 H 0.8304 0.6692 0.8339 0.027 Uiso 1 1 calc R . . C48 C 0.87318(19) 0.7102(4) 0.9164(2) 0.0212(11) Uani 1 1 d . . . C49 C 0.87189(18) 0.7125(4) 0.9878(2) 0.0228(11) Uani 1 1 d . . . H50 H 0.9018 0.7344 1.0114 0.027 Uiso 1 1 calc R . . C50 C 0.82894(19) 0.6844(4) 1.0265(2) 0.0223(11) Uani 1 1 d . . . C51 C 0.4958(2) 0.5818(4) 1.0277(3) 0.0231(12) Uani 1 1 d . . . C52 C 0.51545(19) 0.4843(4) 1.0732(3) 0.0291(12) Uani 1 1 d . . . H51 H 0.5524 0.4803 1.0697 0.044 Uiso 1 1 calc R . . H52 H 0.5008 0.4110 1.0584 0.044 Uiso 1 1 calc R . . H53 H 0.5058 0.4993 1.1207 0.044 Uiso 1 1 calc R . . C53 C 0.51311(19) 0.6985(4) 1.0558(3) 0.0281(12) Uani 1 1 d . . . H54 H 0.4987 0.7102 1.1013 0.042 Uiso 1 1 calc R . . H55 H 0.5017 0.7601 1.0253 0.042 Uiso 1 1 calc R . . H56 H 0.5501 0.6997 1.0587 0.042 Uiso 1 1 calc R . . C54 C 0.4377(2) 0.5834(5) 1.0318(3) 0.0333(13) Uani 1 1 d . . . H57 H 0.4272 0.5960 1.0792 0.050 Uiso 1 1 calc R . . H58 H 0.4243 0.5095 1.0157 0.050 Uiso 1 1 calc R . . H59 H 0.4245 0.6457 1.0031 0.050 Uiso 1 1 calc R . . C55 C 0.45814(19) 0.4903(5) 0.7781(2) 0.0305(13) Uani 1 1 d . . . H60 H 0.4558 0.5549 0.7461 0.046 Uiso 1 1 calc R . . H61 H 0.4250 0.4766 0.7988 0.046 Uiso 1 1 calc R . . H62 H 0.4691 0.4210 0.7537 0.046 Uiso 1 1 calc R . . C56 C 0.83030(19) 0.6862(4) 1.1049(2) 0.0237(11) Uani 1 1 d . . . C57 C 0.81737(19) 0.5640(4) 1.1313(2) 0.0287(12) Uani 1 1 d . . . H63 H 0.7832 0.5430 1.1166 0.043 Uiso 1 1 calc R . . H64 H 0.8191 0.5631 1.1813 0.043 Uiso 1 1 calc R . . H65 H 0.8417 0.5085 1.1128 0.043 Uiso 1 1 calc R . . C58 C 0.8832(2) 0.7161(5) 1.1319(3) 0.0368(15) Uani 1 1 d . . . H66 H 0.9077 0.6602 1.1144 0.055 Uiso 1 1 calc R . . H67 H 0.8830 0.7137 1.1819 0.055 Uiso 1 1 calc R . . H68 H 0.8926 0.7936 1.1165 0.055 Uiso 1 1 calc R . . C59 C 0.7928(2) 0.7729(4) 1.1345(3) 0.0297(12) Uani 1 1 d . . . H69 H 0.7994 0.8494 1.1153 0.044 Uiso 1 1 calc R . . H70 H 0.7965 0.7756 1.1842 0.044 Uiso 1 1 calc R . . H71 H 0.7583 0.7492 1.1229 0.044 Uiso 1 1 calc R . . C60 C 0.91998(18) 0.7486(4) 0.8787(3) 0.0287(12) Uani 1 1 d . . . H72 H 0.9127 0.7532 0.8297 0.043 Uiso 1 1 calc R . . H73 H 0.9473 0.6931 0.8865 0.043 Uiso 1 1 calc R . . H74 H 0.9304 0.8246 0.8953 0.043 Uiso 1 1 calc R . . O7 O 0.65362(13) 0.7000(3) 1.10503(16) 0.0223(7) Uani 1 1 d . . . O8 O 0.66357(12) 0.7933(3) 0.98065(16) 0.0223(8) Uani 1 1 d . . . C61 C 0.6368(2) 0.6547(5) 1.1693(2) 0.0389(15) Uani 1 1 d . . . H75 H 0.6596 0.6804 1.2056 0.058 Uiso 1 1 calc R . . H76 H 0.6368 0.5703 1.1674 0.058 Uiso 1 1 calc R . . H77 H 0.6025 0.6823 1.1788 0.058 Uiso 1 1 calc R . . C62 C 0.6488(2) 0.8238(4) 1.1012(2) 0.0267(12) Uani 1 1 d . . . H78 H 0.6627 0.8602 1.1429 0.032 Uiso 1 1 calc R . . H79 H 0.6128 0.8459 1.0969 0.032 Uiso 1 1 calc R . . C63 C 0.67785(19) 0.8622(4) 1.0393(2) 0.0238(11) Uani 1 1 d . . . H80 H 0.6707 0.9445 1.0300 0.029 Uiso 1 1 calc R . . H81 H 0.7145 0.8540 1.0479 0.029 Uiso 1 1 calc R . . C64 C 0.61992(19) 0.8390(5) 0.9463(3) 0.0315(13) Uani 1 1 d . . . H82 H 0.5914 0.8419 0.9781 0.047 Uiso 1 1 calc R . . H83 H 0.6113 0.7894 0.9075 0.047 Uiso 1 1 calc R . . H84 H 0.6274 0.9169 0.9298 0.047 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 Ti1 0.0221(5) 0.0217(5) 0.0149(4) 0.0007(4) 0.0004(4) -0.0005(4) Cl1 0.0363(8) 0.0220(6) 0.0215(6) -0.0027(5) 0.0027(5) -0.0018(5) O1 0.0197(19) 0.026(2) 0.0211(17) -0.0008(15) 0.0026(14) -0.0017(15) O2 0.0196(18) 0.0263(19) 0.0162(17) 0.0034(14) 0.0004(14) -0.0014(14) C1 0.020(3) 0.028(3) 0.018(2) 0.001(2) 0.003(2) 0.001(2) C2 0.025(3) 0.022(3) 0.017(3) 0.003(2) 0.004(2) 0.007(2) C3 0.030(3) 0.024(3) 0.021(2) 0.006(2) 0.003(2) -0.002(2) C4 0.022(3) 0.026(3) 0.015(2) 0.005(2) 0.002(2) -0.002(2) C5 0.029(3) 0.028(3) 0.015(2) 0.0022(19) 0.004(2) 0.002(2) C6 0.024(3) 0.030(3) 0.012(2) -0.006(2) 0.002(2) 0.000(2) C7 0.024(3) 0.022(3) 0.025(3) -0.002(2) 0.000(2) 0.002(2) C8 0.026(3) 0.017(3) 0.024(3) -0.001(2) 0.002(2) -0.002(2) C9 0.025(3) 0.021(3) 0.025(3) 0.003(2) 0.000(2) 0.004(2) C10 0.029(3) 0.022(3) 0.026(3) -0.002(2) 0.001(2) -0.001(2) C11 0.027(3) 0.024(3) 0.021(2) 0.001(2) -0.005(2) 0.000(2) C12 0.027(3) 0.022(3) 0.018(3) 0.002(2) 0.004(2) 0.006(2) C13 0.027(3) 0.019(3) 0.019(2) -0.002(2) 0.002(2) -0.002(2) C14 0.023(3) 0.016(3) 0.021(2) 0.003(2) 0.001(2) 0.001(2) C15 0.017(3) 0.020(3) 0.022(2) 0.001(2) 0.001(2) 0.001(2) C16 0.022(3) 0.025(3) 0.027(3) -0.001(2) 0.004(2) 0.001(2) C17 0.022(3) 0.022(3) 0.027(3) 0.002(2) -0.005(2) -0.004(2) C18 0.031(3) 0.022(3) 0.014(2) -0.0041(19) -0.002(2) -0.001(2) C19 0.023(3) 0.025(3) 0.021(3) -0.001(2) 0.002(2) -0.002(2) C20 0.039(3) 0.031(3) 0.021(3) -0.003(2) 0.000(2) 0.000(2) C21 0.033(3) 0.029(3) 0.031(3) 0.008(2) 0.006(2) 0.002(2) C22 0.027(3) 0.040(4) 0.028(3) 0.007(3) 0.010(2) 0.001(3) C23 0.032(3) 0.031(3) 0.032(3) -0.002(2) -0.005(2) 0.000(2) C24 0.031(3) 0.024(3) 0.018(2) -0.002(2) -0.004(2) 0.006(2) C25 0.042(4) 0.029(3) 0.024(3) -0.008(2) -0.006(2) -0.002(3) C26 0.048(4) 0.030(3) 0.027(3) 0.005(2) -0.008(3) -0.001(3) C27 0.032(3) 0.042(4) 0.031(3) 0.003(3) -0.010(2) 0.010(3) C28 0.024(3) 0.031(3) 0.033(3) 0.000(2) 0.004(2) 0.000(2) O3 0.039(2) 0.0206(19) 0.0196(17) -0.0004(14) 0.0043(16) 0.0022(16) O4 0.028(2) 0.0195(19) 0.0186(18) 0.0033(14) -0.0022(14) -0.0017(14) C29 0.069(5) 0.035(3) 0.019(3) -0.003(2) 0.018(3) 0.005(3) C30 0.045(3) 0.017(3) 0.022(2) 0.003(2) 0.007(2) 0.000(2) C31 0.028(3) 0.021(3) 0.020(2) 0.003(2) 0.000(2) 0.004(2) C32 0.030(3) 0.030(3) 0.022(2) -0.002(2) -0.003(2) -0.003(2) Ti2 0.0223(5) 0.0217(5) 0.0142(4) 0.0009(4) 0.0007(4) -0.0009(4) Cl2 0.0412(8) 0.0235(7) 0.0208(6) 0.0046(5) -0.0002(5) 0.0008(5) O5 0.0225(19) 0.0216(18) 0.0155(15) -0.0001(14) -0.0027(14) -0.0015(14) O6 0.0188(19) 0.0293(19) 0.0159(17) 0.0039(15) 0.0025(14) 0.0059(15) C33 0.023(3) 0.027(3) 0.017(2) -0.007(2) 0.000(2) -0.005(2) C34 0.027(3) 0.021(3) 0.021(3) -0.005(2) 0.003(2) -0.004(2) C35 0.022(3) 0.023(3) 0.016(2) -0.003(2) 0.001(2) -0.003(2) C36 0.030(3) 0.026(3) 0.013(2) -0.002(2) 0.003(2) -0.003(2) C37 0.033(3) 0.028(3) 0.016(3) 0.005(2) 0.004(2) -0.004(2) C38 0.030(3) 0.029(3) 0.012(2) -0.002(2) -0.005(2) -0.002(2) C39 0.021(3) 0.019(3) 0.015(2) -0.0052(19) 0.000(2) -0.003(2) C40 0.024(3) 0.016(2) 0.020(2) -0.0013(19) 0.000(2) -0.001(2) C41 0.020(3) 0.023(3) 0.022(2) -0.001(2) -0.002(2) 0.002(2) C42 0.025(3) 0.019(3) 0.022(3) -0.002(2) -0.004(2) 0.001(2) C43 0.031(3) 0.020(3) 0.020(2) -0.006(2) 0.001(2) -0.002(2) C44 0.025(3) 0.017(2) 0.021(2) 0.002(2) 0.000(2) -0.003(2) C45 0.020(3) 0.025(3) 0.020(2) 0.002(2) 0.005(2) 0.001(2) C46 0.023(3) 0.020(3) 0.019(2) -0.001(2) 0.000(2) 0.001(2) C47 0.030(3) 0.021(3) 0.017(2) -0.001(2) 0.002(2) 0.001(2) C48 0.030(3) 0.015(3) 0.018(2) -0.0007(19) 0.003(2) 0.001(2) C49 0.026(3) 0.022(3) 0.021(2) 0.001(2) 0.001(2) -0.005(2) C50 0.022(3) 0.021(3) 0.024(3) 0.003(2) 0.001(2) 0.004(2) C51 0.023(3) 0.025(3) 0.022(3) 0.000(2) 0.002(2) -0.004(2) C52 0.033(3) 0.030(3) 0.025(3) 0.002(2) 0.003(2) 0.002(2) C53 0.030(3) 0.028(3) 0.026(3) -0.008(2) 0.000(2) -0.006(2) C54 0.026(3) 0.042(4) 0.032(3) -0.006(3) 0.001(2) -0.002(3) C55 0.035(3) 0.035(3) 0.021(3) -0.003(2) -0.009(2) -0.004(2) C56 0.020(3) 0.030(3) 0.021(2) 0.002(2) -0.002(2) 0.003(2) C57 0.027(3) 0.041(3) 0.019(2) 0.008(2) 0.001(2) 0.003(2) C58 0.038(4) 0.052(4) 0.021(3) 0.005(3) -0.008(2) -0.003(3) C59 0.038(3) 0.031(3) 0.020(3) -0.004(2) -0.003(2) 0.009(2) C60 0.027(3) 0.031(3) 0.028(3) 0.000(2) 0.000(2) -0.006(2) O7 0.033(2) 0.0217(19) 0.0127(16) 0.0008(13) 0.0050(14) -0.0029(15) O8 0.026(2) 0.0223(19) 0.0185(18) 0.0018(15) -0.0042(14) 0.0003(15) C61 0.065(4) 0.034(3) 0.018(3) 0.006(2) 0.007(3) -0.008(3) C62 0.038(3) 0.022(3) 0.020(2) -0.002(2) 0.002(2) -0.003(2) C63 0.033(3) 0.016(3) 0.022(2) -0.0007(19) -0.005(2) -0.004(2) C64 0.036(3) 0.034(3) 0.024(3) 0.001(2) -0.006(2) 0.010(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 Ti1 O1 1.874(3) . ? Ti1 O2 1.886(3) . ? Ti1 O3 2.124(3) . ? Ti1 O4 2.271(3) . ? Ti1 Cl1 2.3972(15) . ? Ti1 C3 2.719(5) . ? O1 C7 1.371(6) . ? O2 C13 1.375(6) . ? C1 C6 1.387(7) . ? C1 C2 1.399(7) . ? C1 C12 1.477(6) . ? C2 C3 1.381(6) . ? C2 H1 0.9500 . ? C3 C4 1.408(6) . ? C3 H2 0.9500 . ? C4 C5 1.386(6) . ? C4 C14 1.475(6) . ? C5 C6 1.391(6) . ? C5 H3 0.9500 . ? C6 H4 0.9500 . ? C7 C8 1.407(6) . ? C7 C12 1.426(7) . ? C8 C9 1.401(7) . ? C8 C19 1.545(7) . ? C9 C10 1.400(7) . ? C9 H5 0.9500 . ? C10 C11 1.385(7) . ? C10 C23 1.520(7) . ? C11 C12 1.386(7) . ? C11 H6 0.9500 . ? C13 C18 1.394(7) . ? C13 C14 1.415(6) . ? C14 C15 1.388(6) . ? C15 C16 1.403(6) . ? C15 H7 0.9500 . ? C16 C17 1.399(7) . ? C16 C28 1.504(6) . ? C17 C18 1.398(6) . ? C17 H8 0.9500 . ? C18 C24 1.548(6) . ? C19 C22 1.534(6) . ? C19 C21 1.536(7) . ? C19 C20 1.538(7) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 H18 0.9800 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C24 C26 1.520(7) . ? C24 C27 1.533(7) . ? C24 C25 1.538(7) . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? O3 C30 1.449(6) . ? O3 C29 1.451(6) . ? O4 C31 1.446(5) . ? O4 C32 1.452(5) . ? C29 H33 0.9800 . ? C29 H34 0.9800 . ? C29 H35 0.9800 . ? C30 C31 1.513(6) . ? C30 H36 0.9900 . ? C30 H37 0.9900 . ? C31 H38 0.9900 . ? C31 H39 0.9900 . ? C32 H40 0.9800 . ? C32 H41 0.9800 . ? C32 H42 0.9800 . ? Ti2 O6 1.880(3) . ? Ti2 O5 1.892(3) . ? Ti2 O7 2.130(3) . ? Ti2 O8 2.268(3) . ? Ti2 Cl2 2.3908(16) . ? Ti2 C35 2.712(5) . ? O5 C39 1.359(5) . ? O6 C45 1.361(5) . ? C33 C38 1.394(7) . ? C33 C34 1.403(7) . ? C33 C44 1.491(6) . ? C34 C35 1.373(6) . ? C34 H43 0.9500 . ? C35 C36 1.422(6) . ? C35 H44 0.9500 . ? C36 C37 1.384(7) . ? C36 C46 1.482(6) . ? C37 C38 1.406(6) . ? C37 H45 0.9500 . ? C38 H46 0.9500 . ? C39 C40 1.387(6) . ? C39 C44 1.424(7) . ? C40 C41 1.402(6) . ? C40 C51 1.544(7) . ? C41 C42 1.398(6) . ? C41 H47 0.9500 . ? C42 C43 1.370(6) . ? C42 C55 1.521(6) . ? C43 C44 1.386(7) . ? C43 H48 0.9500 . ? C45 C50 1.419(7) . ? C45 C46 1.423(7) . ? C46 C47 1.374(6) . ? C47 C48 1.387(7) . ? C47 H49 0.9500 . ? C48 C49 1.400(6) . ? C48 C60 1.510(6) . ? C49 C50 1.405(7) . ? C49 H50 0.9500 . ? C50 C56 1.535(6) . ? C51 C52 1.532(7) . ? C51 C53 1.533(7) . ? C51 C54 1.539(6) . ? C52 H51 0.9800 . ? C52 H52 0.9800 . ? C52 H53 0.9800 . ? C53 H54 0.9800 . ? C53 H55 0.9800 . ? C53 H56 0.9800 . ? C54 H57 0.9800 . ? C54 H58 0.9800 . ? C54 H59 0.9800 . ? C55 H60 0.9800 . ? C55 H61 0.9800 . ? C55 H62 0.9800 . ? C56 C59 1.528(7) . ? C56 C58 1.536(7) . ? C56 C57 1.549(7) . ? C57 H63 0.9800 . ? C57 H64 0.9800 . ? C57 H65 0.9800 . ? C58 H66 0.9800 . ? C58 H67 0.9800 . ? C58 H68 0.9800 . ? C59 H69 0.9800 . ? C59 H70 0.9800 . ? C59 H71 0.9800 . ? C60 H72 0.9800 . ? C60 H73 0.9800 . ? C60 H74 0.9800 . ? O7 C61 1.435(5) . ? O7 C62 1.445(5) . ? O8 C64 1.439(5) . ? O8 C63 1.451(5) . ? C61 H75 0.9800 . ? C61 H76 0.9800 . ? C61 H77 0.9800 . ? C62 C63 1.504(7) . ? C62 H78 0.9900 . ? C62 H79 0.9900 . ? C63 H80 0.9900 . ? C63 H81 0.9900 . ? C64 H82 0.9800 . ? C64 H83 0.9800 . ? C64 H84 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 O1 Ti1 O2 166.40(14) . . ? O1 Ti1 O3 96.11(14) . . ? O2 Ti1 O3 91.81(14) . . ? O1 Ti1 O4 86.04(13) . . ? O2 Ti1 O4 85.34(13) . . ? O3 Ti1 O4 75.09(12) . . ? O1 Ti1 Cl1 95.22(11) . . ? O2 Ti1 Cl1 95.07(10) . . ? O3 Ti1 Cl1 95.07(10) . . ? O4 Ti1 Cl1 170.17(9) . . ? O1 Ti1 C3 100.70(15) . . ? O2 Ti1 C3 70.95(14) . . ? O3 Ti1 C3 162.75(15) . . ? O4 Ti1 C3 102.08(14) . . ? Cl1 Ti1 C3 87.29(11) . . ? C7 O1 Ti1 151.8(3) . . ? C13 O2 Ti1 148.8(3) . . ? C6 C1 C2 118.1(5) . . ? C6 C1 C12 122.6(4) . . ? C2 C1 C12 117.8(4) . . ? C3 C2 C1 120.0(5) . . ? C3 C2 H1 120.0 . . ? C1 C2 H1 120.0 . . ? C2 C3 C4 121.3(5) . . ? C2 C3 Ti1 77.2(3) . . ? C4 C3 Ti1 93.7(3) . . ? C2 C3 H2 119.4 . . ? C4 C3 H2 119.4 . . ? Ti1 C3 H2 99.2 . . ? C5 C4 C3 117.2(5) . . ? C5 C4 C14 124.2(4) . . ? C3 C4 C14 117.9(4) . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H3 119.7 . . ? C6 C5 H3 119.7 . . ? C1 C6 C5 121.0(5) . . ? C1 C6 H4 119.5 . . ? C5 C6 H4 119.5 . . ? O1 C7 C8 121.5(4) . . ? O1 C7 C12 118.3(4) . . ? C8 C7 C12 120.2(5) . . ? C9 C8 C7 116.8(5) . . ? C9 C8 C19 121.0(4) . . ? C7 C8 C19 122.2(5) . . ? C10 C9 C8 123.6(5) . . ? C10 C9 H5 118.2 . . ? C8 C9 H5 118.2 . . ? C11 C10 C9 118.3(5) . . ? C11 C10 C23 120.4(5) . . ? C9 C10 C23 121.3(5) . . ? C10 C11 C12 120.7(5) . . ? C10 C11 H6 119.6 . . ? C12 C11 H6 119.6 . . ? C11 C12 C7 120.3(5) . . ? C11 C12 C1 125.0(5) . . ? C7 C12 C1 114.8(4) . . ? O2 C13 C18 121.2(4) . . ? O2 C13 C14 117.3(4) . . ? C18 C13 C14 121.5(5) . . ? C15 C14 C13 119.7(5) . . ? C15 C14 C4 124.1(4) . . ? C13 C14 C4 116.2(4) . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H7 119.7 . . ? C16 C15 H7 119.7 . . ? C17 C16 C15 117.7(5) . . ? C17 C16 C28 121.0(5) . . ? C15 C16 C28 121.3(5) . . ? C18 C17 C16 123.9(4) . . ? C18 C17 H8 118.1 . . ? C16 C17 H8 118.1 . . ? C13 C18 C17 116.5(4) . . ? C13 C18 C24 122.0(4) . . ? C17 C18 C24 121.5(4) . . ? C22 C19 C21 106.4(4) . . ? C22 C19 C20 108.6(4) . . ? C21 C19 C20 109.5(4) . . ? C22 C19 C8 112.8(4) . . ? C21 C19 C8 110.4(4) . . ? C20 C19 C8 109.2(4) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C10 C23 H18 109.5 . . ? C10 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? C10 C23 H20 109.5 . . ? H18 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C26 C24 C27 107.7(4) . . ? C26 C24 C25 109.9(4) . . ? C27 C24 C25 108.6(4) . . ? C26 C24 C18 109.9(4) . . ? C27 C24 C18 111.9(4) . . ? C25 C24 C18 108.9(4) . . ? C24 C25 H21 109.5 . . ? C24 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C26 H24 109.5 . . ? C24 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C24 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C16 C28 H30 109.5 . . ? C16 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C16 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C30 O3 C29 112.9(4) . . ? C30 O3 Ti1 118.6(3) . . ? C29 O3 Ti1 127.5(3) . . ? C31 O4 C32 111.6(3) . . ? C31 O4 Ti1 106.5(3) . . ? C32 O4 Ti1 123.4(3) . . ? O3 C29 H33 109.5 . . ? O3 C29 H34 109.5 . . ? H33 C29 H34 109.5 . . ? O3 C29 H35 109.5 . . ? H33 C29 H35 109.5 . . ? H34 C29 H35 109.5 . . ? O3 C30 C31 107.4(4) . . ? O3 C30 H36 110.2 . . ? C31 C30 H36 110.2 . . ? O3 C30 H37 110.2 . . ? C31 C30 H37 110.2 . . ? H36 C30 H37 108.5 . . ? O4 C31 C30 109.6(4) . . ? O4 C31 H38 109.8 . . ? C30 C31 H38 109.8 . . ? O4 C31 H39 109.8 . . ? C30 C31 H39 109.8 . . ? H38 C31 H39 108.2 . . ? O4 C32 H40 109.5 . . ? O4 C32 H41 109.5 . . ? H40 C32 H41 109.5 . . ? O4 C32 H42 109.5 . . ? H40 C32 H42 109.5 . . ? H41 C32 H42 109.5 . . ? O6 Ti2 O5 166.49(14) . . ? O6 Ti2 O7 92.59(14) . . ? O5 Ti2 O7 95.50(13) . . ? O6 Ti2 O8 85.82(13) . . ? O5 Ti2 O8 85.85(13) . . ? O7 Ti2 O8 75.00(12) . . ? O6 Ti2 Cl2 95.24(10) . . ? O5 Ti2 Cl2 94.77(10) . . ? O7 Ti2 Cl2 95.25(10) . . ? O8 Ti2 Cl2 170.24(10) . . ? O6 Ti2 C35 71.37(14) . . ? O5 Ti2 C35 100.47(14) . . ? O7 Ti2 C35 163.92(15) . . ? O8 Ti2 C35 104.14(14) . . ? Cl2 Ti2 C35 85.34(11) . . ? C39 O5 Ti2 152.4(3) . . ? C45 O6 Ti2 148.3(3) . . ? C38 C33 C34 118.4(5) . . ? C38 C33 C44 122.7(5) . . ? C34 C33 C44 117.6(4) . . ? C35 C34 C33 120.9(5) . . ? C35 C34 H43 119.6 . . ? C33 C34 H43 119.6 . . ? C34 C35 C36 119.8(5) . . ? C34 C35 Ti2 77.3(3) . . ? C36 C35 Ti2 93.7(3) . . ? C34 C35 H44 120.1 . . ? C36 C35 H44 120.1 . . ? Ti2 C35 H44 98.9 . . ? C37 C36 C35 118.8(5) . . ? C37 C36 C46 123.6(4) . . ? C35 C36 C46 116.9(4) . . ? C36 C37 C38 120.0(5) . . ? C36 C37 H45 120.0 . . ? C38 C37 H45 120.0 . . ? C33 C38 C37 120.3(5) . . ? C33 C38 H46 119.8 . . ? C37 C38 H46 119.8 . . ? O5 C39 C40 122.7(4) . . ? O5 C39 C44 117.8(4) . . ? C40 C39 C44 119.5(4) . . ? C39 C40 C41 118.0(4) . . ? C39 C40 C51 121.4(4) . . ? C41 C40 C51 120.6(4) . . ? C42 C41 C40 123.1(5) . . ? C42 C41 H47 118.4 . . ? C40 C41 H47 118.4 . . ? C43 C42 C41 117.8(5) . . ? C43 C42 C55 121.0(4) . . ? C41 C42 C55 121.3(4) . . ? C42 C43 C44 121.6(5) . . ? C42 C43 H48 119.2 . . ? C44 C43 H48 119.2 . . ? C43 C44 C39 120.1(5) . . ? C43 C44 C33 124.9(4) . . ? C39 C44 C33 115.0(4) . . ? O6 C45 C50 121.8(5) . . ? O6 C45 C46 118.7(4) . . ? C50 C45 C46 119.5(4) . . ? C47 C46 C45 120.9(5) . . ? C47 C46 C36 123.9(4) . . ? C45 C46 C36 115.3(4) . . ? C46 C47 C48 121.2(5) . . ? C46 C47 H49 119.4 . . ? C48 C47 H49 119.4 . . ? C47 C48 C49 117.8(5) . . ? C47 C48 C60 122.0(4) . . ? C49 C48 C60 120.2(5) . . ? C48 C49 C50 123.7(5) . . ? C48 C49 H50 118.2 . . ? C50 C49 H50 118.2 . . ? C49 C50 C45 116.7(5) . . ? C49 C50 C56 121.2(4) . . ? C45 C50 C56 122.1(4) . . ? C52 C51 C53 109.9(4) . . ? C52 C51 C54 108.5(4) . . ? C53 C51 C54 105.6(4) . . ? C52 C51 C40 109.4(4) . . ? C53 C51 C40 111.0(4) . . ? C54 C51 C40 112.3(4) . . ? C51 C52 H51 109.5 . . ? C51 C52 H52 109.5 . . ? H51 C52 H52 109.5 . . ? C51 C52 H53 109.5 . . ? H51 C52 H53 109.5 . . ? H52 C52 H53 109.5 . . ? C51 C53 H54 109.5 . . ? C51 C53 H55 109.5 . . ? H54 C53 H55 109.5 . . ? C51 C53 H56 109.5 . . ? H54 C53 H56 109.5 . . ? H55 C53 H56 109.5 . . ? C51 C54 H57 109.5 . . ? C51 C54 H58 109.5 . . ? H57 C54 H58 109.5 . . ? C51 C54 H59 109.5 . . ? H57 C54 H59 109.5 . . ? H58 C54 H59 109.5 . . ? C42 C55 H60 109.5 . . ? C42 C55 H61 109.5 . . ? H60 C55 H61 109.5 . . ? C42 C55 H62 109.5 . . ? H60 C55 H62 109.5 . . ? H61 C55 H62 109.5 . . ? C59 C56 C50 111.9(4) . . ? C59 C56 C58 108.2(5) . . ? C50 C56 C58 111.6(4) . . ? C59 C56 C57 109.4(4) . . ? C50 C56 C57 108.5(4) . . ? C58 C56 C57 107.0(4) . . ? C56 C57 H63 109.5 . . ? C56 C57 H64 109.5 . . ? H63 C57 H64 109.5 . . ? C56 C57 H65 109.5 . . ? H63 C57 H65 109.5 . . ? H64 C57 H65 109.5 . . ? C56 C58 H66 109.5 . . ? C56 C58 H67 109.5 . . ? H66 C58 H67 109.5 . . ? C56 C58 H68 109.5 . . ? H66 C58 H68 109.5 . . ? H67 C58 H68 109.5 . . ? C56 C59 H69 109.5 . . ? C56 C59 H70 109.5 . . ? H69 C59 H70 109.5 . . ? C56 C59 H71 109.5 . . ? H69 C59 H71 109.5 . . ? H70 C59 H71 109.5 . . ? C48 C60 H72 109.5 . . ? C48 C60 H73 109.5 . . ? H72 C60 H73 109.5 . . ? C48 C60 H74 109.5 . . ? H72 C60 H74 109.5 . . ? H73 C60 H74 109.5 . . ? C61 O7 C62 112.5(4) . . ? C61 O7 Ti2 127.6(3) . . ? C62 O7 Ti2 118.7(3) . . ? C64 O8 C63 112.1(4) . . ? C64 O8 Ti2 123.2(3) . . ? C63 O8 Ti2 106.2(3) . . ? O7 C61 H75 109.5 . . ? O7 C61 H76 109.5 . . ? H75 C61 H76 109.5 . . ? O7 C61 H77 109.5 . . ? H75 C61 H77 109.5 . . ? H76 C61 H77 109.5 . . ? O7 C62 C63 106.9(4) . . ? O7 C62 H78 110.3 . . ? C63 C62 H78 110.3 . . ? O7 C62 H79 110.3 . . ? C63 C62 H79 110.3 . . ? H78 C62 H79 108.6 . . ? O8 C63 C62 110.0(4) . . ? O8 C63 H80 109.7 . . ? C62 C63 H80 109.7 . . ? O8 C63 H81 109.7 . . ? C62 C63 H81 109.7 . . ? H80 C63 H81 108.2 . . ? O8 C64 H82 109.5 . . ? O8 C64 H83 109.5 . . ? H82 C64 H83 109.5 . . ? O8 C64 H84 109.5 . . ? H82 C64 H84 109.5 . . ? H83 C64 H84 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 O2 Ti1 O1 C7 38.1(10) . . . . ? O3 Ti1 O1 C7 163.4(6) . . . . ? O4 Ti1 O1 C7 88.9(7) . . . . ? Cl1 Ti1 O1 C7 -100.9(6) . . . . ? C3 Ti1 O1 C7 -12.7(7) . . . . ? O1 Ti1 O2 C13 -18.8(10) . . . . ? O3 Ti1 O2 C13 -144.5(6) . . . . ? O4 Ti1 O2 C13 -69.6(6) . . . . ? Cl1 Ti1 O2 C13 120.3(5) . . . . ? C3 Ti1 O2 C13 34.9(5) . . . . ? C6 C1 C2 C3 9.9(7) . . . . ? C12 C1 C2 C3 -156.5(4) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C1 C2 C3 Ti1 86.9(4) . . . . ? O1 Ti1 C3 C2 -10.2(3) . . . . ? O2 Ti1 C3 C2 -179.1(3) . . . . ? O3 Ti1 C3 C2 -177.0(4) . . . . ? O4 Ti1 C3 C2 -98.4(3) . . . . ? Cl1 Ti1 C3 C2 84.6(3) . . . . ? O1 Ti1 C3 C4 111.0(3) . . . . ? O2 Ti1 C3 C4 -57.8(3) . . . . ? O3 Ti1 C3 C4 -55.8(6) . . . . ? O4 Ti1 C3 C4 22.8(3) . . . . ? Cl1 Ti1 C3 C4 -154.2(3) . . . . ? C2 C3 C4 C5 -11.2(7) . . . . ? Ti1 C3 C4 C5 -88.5(4) . . . . ? C2 C3 C4 C14 159.9(5) . . . . ? Ti1 C3 C4 C14 82.6(4) . . . . ? C3 C4 C5 C6 11.9(7) . . . . ? C14 C4 C5 C6 -158.6(5) . . . . ? C2 C1 C6 C5 -9.3(7) . . . . ? C12 C1 C6 C5 156.4(4) . . . . ? C4 C5 C6 C1 -1.8(7) . . . . ? Ti1 O1 C7 C8 174.3(5) . . . . ? Ti1 O1 C7 C12 -6.1(9) . . . . ? O1 C7 C8 C9 -179.3(4) . . . . ? C12 C7 C8 C9 1.1(7) . . . . ? O1 C7 C8 C19 -1.2(7) . . . . ? C12 C7 C8 C19 179.2(5) . . . . ? C7 C8 C9 C10 -1.3(7) . . . . ? C19 C8 C9 C10 -179.4(5) . . . . ? C8 C9 C10 C11 0.6(8) . . . . ? C8 C9 C10 C23 -179.7(5) . . . . ? C9 C10 C11 C12 0.3(7) . . . . ? C23 C10 C11 C12 -179.4(5) . . . . ? C10 C11 C12 C7 -0.5(7) . . . . ? C10 C11 C12 C1 179.2(4) . . . . ? O1 C7 C12 C11 -179.9(4) . . . . ? C8 C7 C12 C11 -0.3(7) . . . . ? O1 C7 C12 C1 0.4(6) . . . . ? C8 C7 C12 C1 -180.0(4) . . . . ? C6 C1 C12 C11 74.7(7) . . . . ? C2 C1 C12 C11 -119.5(6) . . . . ? C6 C1 C12 C7 -105.6(6) . . . . ? C2 C1 C12 C7 60.1(6) . . . . ? Ti1 O2 C13 C18 172.7(4) . . . . ? Ti1 O2 C13 C14 -6.6(8) . . . . ? O2 C13 C14 C15 172.9(4) . . . . ? C18 C13 C14 C15 -6.3(8) . . . . ? O2 C13 C14 C4 -5.5(7) . . . . ? C18 C13 C14 C4 175.2(4) . . . . ? C5 C4 C14 C15 -60.2(7) . . . . ? C3 C4 C14 C15 129.3(5) . . . . ? C5 C4 C14 C13 118.1(5) . . . . ? C3 C4 C14 C13 -52.3(6) . . . . ? C13 C14 C15 C16 2.3(7) . . . . ? C4 C14 C15 C16 -179.4(5) . . . . ? C14 C15 C16 C17 2.5(7) . . . . ? C14 C15 C16 C28 -175.9(5) . . . . ? C15 C16 C17 C18 -3.7(8) . . . . ? C28 C16 C17 C18 174.8(5) . . . . ? O2 C13 C18 C17 -174.1(4) . . . . ? C14 C13 C18 C17 5.2(7) . . . . ? O2 C13 C18 C24 6.5(7) . . . . ? C14 C13 C18 C24 -174.3(5) . . . . ? C16 C17 C18 C13 -0.2(7) . . . . ? C16 C17 C18 C24 179.3(5) . . . . ? C9 C8 C19 C22 -7.0(6) . . . . ? C7 C8 C19 C22 175.0(4) . . . . ? C9 C8 C19 C21 -125.9(5) . . . . ? C7 C8 C19 C21 56.1(6) . . . . ? C9 C8 C19 C20 113.7(5) . . . . ? C7 C8 C19 C20 -64.3(6) . . . . ? C13 C18 C24 C26 -62.6(6) . . . . ? C17 C18 C24 C26 118.0(5) . . . . ? C13 C18 C24 C27 177.7(4) . . . . ? C17 C18 C24 C27 -1.7(7) . . . . ? C13 C18 C24 C25 57.8(6) . . . . ? C17 C18 C24 C25 -121.7(5) . . . . ? O1 Ti1 O3 C30 -86.7(3) . . . . ? O2 Ti1 O3 C30 82.3(3) . . . . ? O4 Ti1 O3 C30 -2.4(3) . . . . ? Cl1 Ti1 O3 C30 177.5(3) . . . . ? C3 Ti1 O3 C30 80.3(6) . . . . ? O1 Ti1 O3 C29 80.8(4) . . . . ? O2 Ti1 O3 C29 -110.3(4) . . . . ? O4 Ti1 O3 C29 165.0(4) . . . . ? Cl1 Ti1 O3 C29 -15.0(4) . . . . ? C3 Ti1 O3 C29 -112.3(6) . . . . ? O1 Ti1 O4 C31 125.9(3) . . . . ? O2 Ti1 O4 C31 -64.6(3) . . . . ? O3 Ti1 O4 C31 28.5(3) . . . . ? C3 Ti1 O4 C31 -134.0(3) . . . . ? O1 Ti1 O4 C32 -5.0(3) . . . . ? O2 Ti1 O4 C32 164.5(3) . . . . ? O3 Ti1 O4 C32 -102.4(3) . . . . ? C3 Ti1 O4 C32 95.1(3) . . . . ? C29 O3 C30 C31 167.8(4) . . . . ? Ti1 O3 C30 C31 -23.0(5) . . . . ? C32 O4 C31 C30 87.0(5) . . . . ? Ti1 O4 C31 C30 -50.2(4) . . . . ? O3 C30 C31 O4 48.7(5) . . . . ? O6 Ti2 O5 C39 38.6(10) . . . . ? O7 Ti2 O5 C39 165.2(6) . . . . ? O8 Ti2 O5 C39 90.7(6) . . . . ? Cl2 Ti2 O5 C39 -99.1(6) . . . . ? C35 Ti2 O5 C39 -12.9(7) . . . . ? O5 Ti2 O6 C45 -20.8(10) . . . . ? O7 Ti2 O6 C45 -147.6(6) . . . . ? O8 Ti2 O6 C45 -72.9(6) . . . . ? Cl2 Ti2 O6 C45 116.8(6) . . . . ? C35 Ti2 O6 C45 33.6(6) . . . . ? C38 C33 C34 C35 10.9(7) . . . . ? C44 C33 C34 C35 -156.3(4) . . . . ? C33 C34 C35 C36 -0.4(7) . . . . ? C33 C34 C35 Ti2 86.5(4) . . . . ? O6 Ti2 C35 C34 -177.8(3) . . . . ? O5 Ti2 C35 C34 -9.0(3) . . . . ? O7 Ti2 C35 C34 177.9(5) . . . . ? O8 Ti2 C35 C34 -97.3(3) . . . . ? Cl2 Ti2 C35 C34 85.0(3) . . . . ? O6 Ti2 C35 C36 -58.1(3) . . . . ? O5 Ti2 C35 C36 110.8(3) . . . . ? O7 Ti2 C35 C36 -62.4(6) . . . . ? O8 Ti2 C35 C36 22.5(3) . . . . ? Cl2 Ti2 C35 C36 -155.2(3) . . . . ? C34 C35 C36 C37 -10.3(7) . . . . ? Ti2 C35 C36 C37 -87.7(4) . . . . ? C34 C35 C36 C46 160.6(4) . . . . ? Ti2 C35 C36 C46 83.1(4) . . . . ? C35 C36 C37 C38 10.4(7) . . . . ? C46 C36 C37 C38 -159.8(5) . . . . ? C34 C33 C38 C37 -10.7(7) . . . . ? C44 C33 C38 C37 155.8(5) . . . . ? C36 C37 C38 C33 0.1(7) . . . . ? Ti2 O5 C39 C40 173.2(4) . . . . ? Ti2 O5 C39 C44 -7.4(9) . . . . ? O5 C39 C40 C41 -179.7(4) . . . . ? C44 C39 C40 C41 0.9(7) . . . . ? O5 C39 C40 C51 -1.6(7) . . . . ? C44 C39 C40 C51 179.1(5) . . . . ? C39 C40 C41 C42 -0.6(7) . . . . ? C51 C40 C41 C42 -178.7(4) . . . . ? C40 C41 C42 C43 0.1(7) . . . . ? C40 C41 C42 C55 179.4(5) . . . . ? C41 C42 C43 C44 0.0(7) . . . . ? C55 C42 C43 C44 -179.3(5) . . . . ? C42 C43 C44 C39 0.3(7) . . . . ? C42 C43 C44 C33 178.4(4) . . . . ? O5 C39 C44 C43 179.8(4) . . . . ? C40 C39 C44 C43 -0.8(7) . . . . ? O5 C39 C44 C33 1.6(6) . . . . ? C40 C39 C44 C33 -179.0(4) . . . . ? C38 C33 C44 C43 74.5(6) . . . . ? C34 C33 C44 C43 -118.8(5) . . . . ? C38 C33 C44 C39 -107.3(5) . . . . ? C34 C33 C44 C39 59.3(6) . . . . ? Ti2 O6 C45 C50 173.4(4) . . . . ? Ti2 O6 C45 C46 -5.1(9) . . . . ? O6 C45 C46 C47 173.5(4) . . . . ? C50 C45 C46 C47 -5.1(7) . . . . ? O6 C45 C46 C36 -5.0(7) . . . . ? C50 C45 C46 C36 176.4(4) . . . . ? C37 C36 C46 C47 -61.2(7) . . . . ? C35 C36 C46 C47 128.4(5) . . . . ? C37 C36 C46 C45 117.2(5) . . . . ? C35 C36 C46 C45 -53.1(6) . . . . ? C45 C46 C47 C48 1.6(8) . . . . ? C36 C46 C47 C48 179.9(4) . . . . ? C46 C47 C48 C49 2.1(7) . . . . ? C46 C47 C48 C60 -176.5(5) . . . . ? C47 C48 C49 C50 -2.4(8) . . . . ? C60 C48 C49 C50 176.3(4) . . . . ? C48 C49 C50 C45 -1.0(7) . . . . ? C48 C49 C50 C56 178.7(5) . . . . ? O6 C45 C50 C49 -173.8(4) . . . . ? C46 C45 C50 C49 4.6(7) . . . . ? O6 C45 C50 C56 6.5(7) . . . . ? C46 C45 C50 C56 -175.0(5) . . . . ? C39 C40 C51 C52 -64.7(6) . . . . ? C41 C40 C51 C52 113.4(5) . . . . ? C39 C40 C51 C53 56.8(6) . . . . ? C41 C40 C51 C53 -125.1(5) . . . . ? C39 C40 C51 C54 174.7(4) . . . . ? C41 C40 C51 C54 -7.2(6) . . . . ? C49 C50 C56 C59 119.0(5) . . . . ? C45 C50 C56 C59 -61.3(6) . . . . ? C49 C50 C56 C58 -2.5(7) . . . . ? C45 C50 C56 C58 177.2(5) . . . . ? C49 C50 C56 C57 -120.2(5) . . . . ? C45 C50 C56 C57 59.5(6) . . . . ? O6 Ti2 O7 C61 -110.2(4) . . . . ? O5 Ti2 O7 C61 80.6(4) . . . . ? O8 Ti2 O7 C61 164.8(4) . . . . ? Cl2 Ti2 O7 C61 -14.7(4) . . . . ? C35 Ti2 O7 C61 -106.2(6) . . . . ? O6 Ti2 O7 C62 83.0(3) . . . . ? O5 Ti2 O7 C62 -86.2(3) . . . . ? O8 Ti2 O7 C62 -2.0(3) . . . . ? Cl2 Ti2 O7 C62 178.5(3) . . . . ? C35 Ti2 O7 C62 87.1(6) . . . . ? O6 Ti2 O8 C64 163.2(3) . . . . ? O5 Ti2 O8 C64 -6.2(3) . . . . ? O7 Ti2 O8 C64 -103.0(3) . . . . ? C35 Ti2 O8 C64 93.6(3) . . . . ? O6 Ti2 O8 C63 -65.7(3) . . . . ? O5 Ti2 O8 C63 125.0(3) . . . . ? O7 Ti2 O8 C63 28.2(3) . . . . ? C35 Ti2 O8 C63 -135.3(3) . . . . ? C61 O7 C62 C63 167.6(4) . . . . ? Ti2 O7 C62 C63 -23.7(5) . . . . ? C64 O8 C63 C62 86.5(5) . . . . ? Ti2 O8 C63 C62 -50.7(4) . . . . ? O7 C62 C63 O8 49.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.447 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 962315' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[(C6H4)(ArO)2Ti(pyridine)2]2(N2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H84 N6 O4 Ti2' _chemical_formula_sum 'C76 H84 N6 O4 Ti2' _chemical_formula_weight 1241.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 22.533(5) _cell_length_b 50.714(11) _cell_length_c 11.285(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12896(5) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7289 _cell_measurement_theta_min 3.0129 _cell_measurement_theta_max 27.4546 _exptl_crystal_description Platelet _exptl_crystal_colour Purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5264 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9418 _exptl_absorpt_correction_T_max 0.9909 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Saturn CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 26369 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 65 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.44 _reflns_number_total 7372 _reflns_number_gt 5196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+9.5508P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(4) _refine_ls_number_reflns 7372 _refine_ls_number_parameters 405 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.22824(3) 0.203214(15) 0.39992(7) 0.02587(19) Uani 1 1 d . . . N1 N 0.24496(14) 0.23774(6) 0.3955(3) 0.0261(8) Uani 1 1 d . . . O1 O 0.16817(14) 0.19952(6) 0.5197(3) 0.0293(7) Uani 1 1 d . . . O2 O 0.27984(13) 0.18799(6) 0.2797(3) 0.0274(7) Uani 1 1 d . . . N2 N 0.29496(16) 0.19136(7) 0.5376(3) 0.0259(8) Uani 1 1 d . . . N3 N 0.15352(16) 0.20499(7) 0.2667(4) 0.0293(9) Uani 1 1 d . . . C1 C 0.16124(19) 0.14631(8) 0.5271(4) 0.0269(10) Uani 1 1 d . . . C2 C 0.2141(2) 0.13517(8) 0.5669(4) 0.0291(10) Uani 1 1 d . . . H1 H 0.2181 0.1304 0.6479 0.035 Uiso 1 1 calc R . . C3 C 0.2612(2) 0.13087(8) 0.4892(4) 0.0289(11) Uani 1 1 d . . . H2 H 0.2967 0.1229 0.5171 0.035 Uiso 1 1 calc R . . C4 C 0.2563(2) 0.13825(9) 0.3706(4) 0.0297(11) Uani 1 1 d . . . C5 C 0.1992(2) 0.14458(9) 0.3285(4) 0.0302(11) Uani 1 1 d . . . H3 H 0.1927 0.1461 0.2457 0.036 Uiso 1 1 calc R . . C6 C 0.15296(18) 0.14856(8) 0.4051(4) 0.0289(10) Uani 1 1 d . . . H4 H 0.1149 0.1529 0.3748 0.035 Uiso 1 1 calc R . . C7 C 0.13001(18) 0.18963(9) 0.6007(4) 0.0265(10) Uani 1 1 d . . . C8 C 0.09883(19) 0.20618(8) 0.6794(4) 0.0271(10) Uani 1 1 d . . . C9 C 0.05961(19) 0.19456(9) 0.7567(4) 0.0280(10) Uani 1 1 d . . . H5 H 0.0376 0.2058 0.8078 0.034 Uiso 1 1 calc R . . C10 C 0.04969(19) 0.16745(9) 0.7657(4) 0.0281(10) Uani 1 1 d . . . C11 C 0.08207(19) 0.15117(9) 0.6898(4) 0.0312(11) Uani 1 1 d . . . H6 H 0.0768 0.1326 0.6935 0.037 Uiso 1 1 calc R . . C12 C 0.12223(18) 0.16192(9) 0.6081(4) 0.0285(10) Uani 1 1 d . . . C13 C 0.31641(19) 0.16828(8) 0.2448(4) 0.0268(10) Uani 1 1 d . . . C14 C 0.30853(19) 0.14252(9) 0.2931(4) 0.0272(10) Uani 1 1 d . . . C15 C 0.34998(19) 0.12265(9) 0.2699(4) 0.0296(10) Uani 1 1 d . . . H7 H 0.3458 0.1059 0.3071 0.035 Uiso 1 1 calc R . . C16 C 0.3972(2) 0.12701(9) 0.1933(4) 0.0305(11) Uani 1 1 d . . . C17 C 0.40258(19) 0.15179(8) 0.1428(4) 0.0293(10) Uani 1 1 d . . . H8 H 0.4337 0.1544 0.0873 0.035 Uiso 1 1 calc R . . C18 C 0.36513(18) 0.17335(8) 0.1680(4) 0.0269(10) Uani 1 1 d . . . C19 C 0.10810(19) 0.23640(8) 0.6780(4) 0.0305(11) Uani 1 1 d . . . C20 C 0.1733(2) 0.24310(10) 0.7037(5) 0.0411(13) Uani 1 1 d . . . H9 H 0.1982 0.2368 0.6384 0.062 Uiso 1 1 calc R . . H10 H 0.1856 0.2345 0.7776 0.062 Uiso 1 1 calc R . . H11 H 0.1778 0.2622 0.7115 0.062 Uiso 1 1 calc R . . C21 C 0.0710(2) 0.24986(9) 0.7751(5) 0.0427(13) Uani 1 1 d . . . H12 H 0.0786 0.2689 0.7739 0.064 Uiso 1 1 calc R . . H13 H 0.0821 0.2427 0.8526 0.064 Uiso 1 1 calc R . . H14 H 0.0288 0.2466 0.7606 0.064 Uiso 1 1 calc R . . C22 C 0.0895(2) 0.24803(9) 0.5579(5) 0.0414(13) Uani 1 1 d . . . H15 H 0.0918 0.2673 0.5614 0.062 Uiso 1 1 calc R . . H16 H 0.0488 0.2427 0.5397 0.062 Uiso 1 1 calc R . . H17 H 0.1163 0.2415 0.4959 0.062 Uiso 1 1 calc R . . C23 C 0.0060(2) 0.15701(9) 0.8536(4) 0.0302(10) Uani 1 1 d . . . H18 H 0.0013 0.1380 0.8422 0.045 Uiso 1 1 calc R . . H19 H -0.0323 0.1658 0.8423 0.045 Uiso 1 1 calc R . . H20 H 0.0205 0.1604 0.9341 0.045 Uiso 1 1 calc R . . C24 C 0.3787(2) 0.20108(9) 0.1202(4) 0.0285(10) Uani 1 1 d . . . C25 C 0.3938(2) 0.21976(9) 0.2248(4) 0.0369(12) Uani 1 1 d . . . H21 H 0.4042 0.2372 0.1938 0.055 Uiso 1 1 calc R . . H22 H 0.4274 0.2126 0.2694 0.055 Uiso 1 1 calc R . . H23 H 0.3593 0.2213 0.2771 0.055 Uiso 1 1 calc R . . C26 C 0.3255(2) 0.21296(11) 0.0555(5) 0.0440(13) Uani 1 1 d . . . H24 H 0.3098 0.2001 -0.0013 0.066 Uiso 1 1 calc R . . H25 H 0.3380 0.2289 0.0132 0.066 Uiso 1 1 calc R . . H26 H 0.2946 0.2175 0.1131 0.066 Uiso 1 1 calc R . . C27 C 0.4321(2) 0.20084(10) 0.0350(4) 0.0419(13) Uani 1 1 d . . . H27 H 0.4238 0.1890 -0.0315 0.063 Uiso 1 1 calc R . . H28 H 0.4675 0.1947 0.0773 0.063 Uiso 1 1 calc R . . H29 H 0.4391 0.2187 0.0050 0.063 Uiso 1 1 calc R . . C28 C 0.4414(2) 0.10539(9) 0.1668(5) 0.0365(12) Uani 1 1 d . . . H30 H 0.4770 0.1131 0.1307 0.055 Uiso 1 1 calc R . . H31 H 0.4236 0.0927 0.1120 0.055 Uiso 1 1 calc R . . H32 H 0.4523 0.0964 0.2406 0.055 Uiso 1 1 calc R . . C29 C 0.2795(2) 0.18743(8) 0.6524(4) 0.0316(10) Uani 1 1 d . . . H33 H 0.2403 0.1918 0.6761 0.038 Uiso 1 1 calc R . . C30 C 0.3182(2) 0.17739(10) 0.7375(5) 0.0381(12) Uani 1 1 d . . . H34 H 0.3052 0.1750 0.8168 0.046 Uiso 1 1 calc R . . C31 C 0.3753(2) 0.17103(9) 0.7055(5) 0.0370(12) Uani 1 1 d . . . H35 H 0.4024 0.1642 0.7622 0.044 Uiso 1 1 calc R . . C32 C 0.3923(2) 0.17482(9) 0.5901(4) 0.0361(12) Uani 1 1 d . . . H36 H 0.4313 0.1704 0.5652 0.043 Uiso 1 1 calc R . . C33 C 0.35125(19) 0.18525(9) 0.5097(4) 0.0288(10) Uani 1 1 d . . . H37 H 0.3640 0.1882 0.4305 0.035 Uiso 1 1 calc R . . C34 C 0.1651(2) 0.20569(9) 0.1480(5) 0.0374(11) Uani 1 1 d . . . H38 H 0.2054 0.2059 0.1231 0.045 Uiso 1 1 calc R . . C35 C 0.1215(2) 0.20614(11) 0.0626(5) 0.0450(14) Uani 1 1 d . . . H39 H 0.1315 0.2067 -0.0191 0.054 Uiso 1 1 calc R . . C36 C 0.0633(2) 0.20579(10) 0.0979(5) 0.0414(13) Uani 1 1 d . . . H40 H 0.0323 0.2061 0.0408 0.050 Uiso 1 1 calc R . . C37 C 0.0503(2) 0.20492(10) 0.2156(5) 0.0427(13) Uani 1 1 d . . . H41 H 0.0102 0.2045 0.2415 0.051 Uiso 1 1 calc R . . C38 C 0.09608(19) 0.20464(9) 0.2970(5) 0.0327(11) Uani 1 1 d . . . H42 H 0.0863 0.2042 0.3788 0.039 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 Ti1 0.0242(4) 0.0234(4) 0.0299(4) -0.0010(4) 0.0010(4) 0.0007(3) N1 0.0201(17) 0.0262(17) 0.0319(19) 0.0003(18) 0.0037(19) 0.0000(14) O1 0.0264(17) 0.0269(16) 0.0348(19) -0.0008(15) 0.0020(15) -0.0024(13) O2 0.0251(16) 0.0284(16) 0.0288(17) -0.0011(14) 0.0017(14) 0.0046(13) N2 0.028(2) 0.0247(19) 0.026(2) -0.0021(16) 0.0042(17) -0.0009(16) N3 0.024(2) 0.025(2) 0.039(2) -0.0011(18) -0.0006(18) -0.0009(16) C1 0.027(2) 0.019(2) 0.035(3) -0.001(2) 0.001(2) -0.0032(18) C2 0.035(3) 0.026(2) 0.027(2) 0.003(2) 0.000(2) 0.0004(19) C3 0.030(2) 0.017(2) 0.039(3) -0.002(2) -0.002(2) 0.0032(18) C4 0.029(2) 0.023(2) 0.037(3) -0.002(2) 0.000(2) -0.0066(18) C5 0.033(3) 0.023(2) 0.034(3) -0.005(2) 0.000(2) -0.0010(19) C6 0.023(2) 0.023(2) 0.040(3) -0.005(2) 0.001(2) -0.0002(17) C7 0.020(2) 0.029(2) 0.030(2) 0.001(2) 0.0022(19) 0.0003(18) C8 0.026(2) 0.020(2) 0.036(3) 0.001(2) -0.004(2) -0.0013(17) C9 0.027(2) 0.024(2) 0.033(3) -0.005(2) 0.002(2) 0.0044(19) C10 0.021(2) 0.029(2) 0.034(3) 0.000(2) -0.002(2) -0.0021(18) C11 0.028(2) 0.028(2) 0.038(3) 0.003(2) -0.002(2) -0.0042(19) C12 0.017(2) 0.032(2) 0.037(3) -0.001(2) 0.000(2) 0.0008(18) C13 0.027(2) 0.023(2) 0.030(2) -0.004(2) -0.002(2) 0.0018(18) C14 0.027(2) 0.025(2) 0.029(2) -0.002(2) -0.002(2) -0.0050(18) C15 0.031(2) 0.027(2) 0.031(3) -0.004(2) -0.003(2) 0.0000(19) C16 0.030(2) 0.030(2) 0.031(3) -0.008(2) 0.000(2) 0.004(2) C17 0.029(2) 0.032(2) 0.028(2) -0.006(2) -0.001(2) 0.0044(18) C18 0.025(2) 0.028(2) 0.028(2) -0.001(2) -0.001(2) -0.0014(18) C19 0.025(2) 0.024(2) 0.042(3) -0.003(2) 0.008(2) -0.0018(18) C20 0.034(3) 0.032(3) 0.057(3) -0.013(2) 0.009(2) -0.005(2) C21 0.042(3) 0.026(3) 0.060(4) -0.007(3) 0.008(3) 0.004(2) C22 0.051(3) 0.019(2) 0.055(3) 0.003(2) 0.011(3) 0.003(2) C23 0.030(2) 0.031(2) 0.030(2) 0.005(2) 0.000(2) 0.000(2) C24 0.029(2) 0.028(2) 0.028(3) 0.002(2) 0.000(2) 0.0016(19) C25 0.041(3) 0.029(3) 0.041(3) -0.002(2) 0.000(2) -0.001(2) C26 0.035(3) 0.052(3) 0.045(3) 0.014(3) 0.000(3) 0.005(2) C27 0.041(3) 0.050(3) 0.035(3) 0.012(3) 0.010(2) 0.001(2) C28 0.036(3) 0.035(3) 0.038(3) -0.005(2) 0.006(2) 0.007(2) C29 0.037(2) 0.030(2) 0.028(2) -0.002(2) 0.004(2) -0.0011(19) C30 0.048(3) 0.035(3) 0.031(3) 0.006(2) 0.001(2) -0.008(2) C31 0.045(3) 0.025(2) 0.040(3) 0.005(2) -0.011(3) 0.003(2) C32 0.033(3) 0.034(3) 0.041(3) -0.003(2) -0.006(2) 0.009(2) C33 0.026(2) 0.032(3) 0.029(2) -0.002(2) 0.003(2) 0.0029(19) C34 0.034(3) 0.037(3) 0.042(3) -0.003(3) -0.001(3) 0.001(2) C35 0.042(3) 0.052(3) 0.041(3) -0.002(3) -0.009(3) 0.006(3) C36 0.038(3) 0.032(3) 0.055(4) -0.012(3) -0.019(3) 0.003(2) C37 0.030(3) 0.039(3) 0.059(4) -0.011(3) -0.008(3) 0.007(2) C38 0.023(2) 0.030(3) 0.045(3) -0.006(2) -0.004(2) 0.0013(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 1.792(3) . ? Ti1 O1 1.922(3) . ? Ti1 O2 1.947(3) . ? Ti1 N2 2.244(4) . ? Ti1 N3 2.259(4) . ? N1 N1 1.264(6) 14 ? O1 C7 1.351(5) . ? O2 C13 1.354(5) . ? N2 C33 1.343(5) . ? N2 C29 1.355(6) . ? N3 C38 1.339(6) . ? N3 C34 1.365(6) . ? C1 C2 1.392(6) . ? C1 C6 1.394(7) . ? C1 C12 1.495(6) . ? C2 C3 1.393(6) . ? C2 H1 0.9500 . ? C3 C4 1.394(6) . ? C3 H2 0.9500 . ? C4 C5 1.408(6) . ? C4 C14 1.482(6) . ? C5 C6 1.369(6) . ? C5 H3 0.9500 . ? C6 H4 0.9500 . ? C7 C8 1.410(6) . ? C7 C12 1.418(6) . ? C8 C9 1.375(6) . ? C8 C19 1.547(6) . ? C9 C10 1.397(6) . ? C9 H5 0.9500 . ? C10 C11 1.396(6) . ? C10 C23 1.494(6) . ? C11 C12 1.402(6) . ? C11 H6 0.9500 . ? C13 C18 1.422(6) . ? C13 C14 1.427(6) . ? C14 C15 1.399(6) . ? C15 C16 1.388(6) . ? C15 H7 0.9500 . ? C16 C17 1.385(6) . ? C16 C28 1.512(6) . ? C17 C18 1.410(5) . ? C17 H8 0.9500 . ? C18 C24 1.537(6) . ? C19 C22 1.536(7) . ? C19 C20 1.537(6) . ? C19 C21 1.537(6) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 H18 0.9800 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C24 C26 1.528(6) . ? C24 C27 1.541(6) . ? C24 C25 1.551(6) . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? C29 C30 1.393(7) . ? C29 H33 0.9500 . ? C30 C31 1.374(7) . ? C30 H34 0.9500 . ? C31 C32 1.371(7) . ? C31 H35 0.9500 . ? C32 C33 1.400(6) . ? C32 H36 0.9500 . ? C33 H37 0.9500 . ? C34 C35 1.377(7) . ? C34 H38 0.9500 . ? C35 C36 1.371(7) . ? C35 H39 0.9500 . ? C36 C37 1.361(7) . ? C36 H40 0.9500 . ? C37 C38 1.381(7) . ? C37 H41 0.9500 . ? C38 H42 0.9500 . ? 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 N1 Ti1 O1 105.25(15) . . ? N1 Ti1 O2 104.04(15) . . ? O1 Ti1 O2 150.71(13) . . ? N1 Ti1 N2 98.08(15) . . ? O1 Ti1 N2 87.61(14) . . ? O2 Ti1 N2 88.65(12) . . ? N1 Ti1 N3 95.68(15) . . ? O1 Ti1 N3 86.98(13) . . ? O2 Ti1 N3 89.83(13) . . ? N2 Ti1 N3 166.12(14) . . ? N1 N1 Ti1 177.6(3) 14 . ? C7 O1 Ti1 163.7(3) . . ? C13 O2 Ti1 149.2(3) . . ? C33 N2 C29 115.6(4) . . ? C33 N2 Ti1 122.1(3) . . ? C29 N2 Ti1 122.0(3) . . ? C38 N3 C34 115.9(4) . . ? C38 N3 Ti1 123.4(3) . . ? C34 N3 Ti1 120.7(3) . . ? C2 C1 C6 117.8(4) . . ? C2 C1 C12 121.4(4) . . ? C6 C1 C12 118.8(4) . . ? C1 C2 C3 120.8(4) . . ? C1 C2 H1 119.6 . . ? C3 C2 H1 119.6 . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H2 119.9 . . ? C4 C3 H2 119.9 . . ? C3 C4 C5 117.1(4) . . ? C3 C4 C14 122.9(4) . . ? C5 C4 C14 119.6(4) . . ? C6 C5 C4 121.1(4) . . ? C6 C5 H3 119.4 . . ? C4 C5 H3 119.4 . . ? C5 C6 C1 120.6(4) . . ? C5 C6 H4 119.7 . . ? C1 C6 H4 119.7 . . ? O1 C7 C8 121.5(4) . . ? O1 C7 C12 119.1(4) . . ? C8 C7 C12 119.4(4) . . ? C9 C8 C7 117.7(4) . . ? C9 C8 C19 121.2(4) . . ? C7 C8 C19 121.1(4) . . ? C8 C9 C10 124.8(4) . . ? C8 C9 H5 117.6 . . ? C10 C9 H5 117.6 . . ? C11 C10 C9 117.0(4) . . ? C11 C10 C23 122.8(4) . . ? C9 C10 C23 120.2(4) . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H6 119.6 . . ? C12 C11 H6 119.6 . . ? C11 C12 C7 120.2(4) . . ? C11 C12 C1 125.1(4) . . ? C7 C12 C1 114.6(4) . . ? O2 C13 C18 120.9(4) . . ? O2 C13 C14 119.3(4) . . ? C18 C13 C14 119.6(4) . . ? C15 C14 C13 120.3(4) . . ? C15 C14 C4 122.4(4) . . ? C13 C14 C4 117.3(4) . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H7 119.6 . . ? C14 C15 H7 119.6 . . ? C17 C16 C15 117.9(4) . . ? C17 C16 C28 121.2(4) . . ? C15 C16 C28 120.8(4) . . ? C16 C17 C18 124.6(4) . . ? C16 C17 H8 117.7 . . ? C18 C17 H8 117.7 . . ? C17 C18 C13 116.4(4) . . ? C17 C18 C24 121.3(4) . . ? C13 C18 C24 122.2(4) . . ? C22 C19 C20 110.0(4) . . ? C22 C19 C21 108.1(4) . . ? C20 C19 C21 106.7(4) . . ? C22 C19 C8 110.7(4) . . ? C20 C19 C8 110.2(4) . . ? C21 C19 C8 111.0(4) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C10 C23 H18 109.5 . . ? C10 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? C10 C23 H20 109.5 . . ? H18 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C26 C24 C18 111.9(4) . . ? C26 C24 C27 108.5(4) . . ? C18 C24 C27 111.6(4) . . ? C26 C24 C25 107.1(4) . . ? C18 C24 C25 109.6(4) . . ? C27 C24 C25 108.0(4) . . ? C24 C25 H21 109.5 . . ? C24 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C26 H24 109.5 . . ? C24 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C24 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C16 C28 H30 109.5 . . ? C16 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C16 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? N2 C29 C30 123.5(4) . . ? N2 C29 H33 118.3 . . ? C30 C29 H33 118.3 . . ? C31 C30 C29 119.4(5) . . ? C31 C30 H34 120.3 . . ? C29 C30 H34 120.3 . . ? C32 C31 C30 118.5(5) . . ? C32 C31 H35 120.7 . . ? C30 C31 H35 120.7 . . ? C31 C32 C33 119.0(5) . . ? C31 C32 H36 120.5 . . ? C33 C32 H36 120.5 . . ? N2 C33 C32 123.9(4) . . ? N2 C33 H37 118.0 . . ? C32 C33 H37 118.0 . . ? N3 C34 C35 123.4(5) . . ? N3 C34 H38 118.3 . . ? C35 C34 H38 118.3 . . ? C36 C35 C34 118.6(5) . . ? C36 C35 H39 120.7 . . ? C34 C35 H39 120.7 . . ? C37 C36 C35 119.3(5) . . ? C37 C36 H40 120.3 . . ? C35 C36 H40 120.3 . . ? C36 C37 C38 119.3(5) . . ? C36 C37 H41 120.4 . . ? C38 C37 H41 120.4 . . ? N3 C38 C37 123.5(5) . . ? N3 C38 H42 118.2 . . ? C37 C38 H42 118.2 . . ? 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 N1 Ti1 O1 C7 -166.5(10) . . . . ? O2 Ti1 O1 C7 14.2(12) . . . . ? N2 Ti1 O1 C7 -68.8(10) . . . . ? N3 Ti1 O1 C7 98.4(10) . . . . ? N1 Ti1 O2 C13 139.4(5) . . . . ? O1 Ti1 O2 C13 -41.3(7) . . . . ? N2 Ti1 O2 C13 41.4(5) . . . . ? N3 Ti1 O2 C13 -124.8(5) . . . . ? N1 Ti1 N2 C33 -86.3(3) . . . . ? O1 Ti1 N2 C33 168.6(3) . . . . ? O2 Ti1 N2 C33 17.7(3) . . . . ? N3 Ti1 N2 C33 101.5(6) . . . . ? N1 Ti1 N2 C29 100.3(3) . . . . ? O1 Ti1 N2 C29 -4.8(3) . . . . ? O2 Ti1 N2 C29 -155.7(3) . . . . ? N3 Ti1 N2 C29 -71.9(7) . . . . ? N1 Ti1 N3 C38 -101.7(3) . . . . ? O1 Ti1 N3 C38 3.3(3) . . . . ? O2 Ti1 N3 C38 154.2(3) . . . . ? N2 Ti1 N3 C38 70.5(7) . . . . ? N1 Ti1 N3 C34 80.3(4) . . . . ? O1 Ti1 N3 C34 -174.6(3) . . . . ? O2 Ti1 N3 C34 -23.8(3) . . . . ? N2 Ti1 N3 C34 -107.4(6) . . . . ? C6 C1 C2 C3 11.4(6) . . . . ? C12 C1 C2 C3 -152.2(4) . . . . ? C1 C2 C3 C4 1.4(6) . . . . ? C2 C3 C4 C5 -13.4(6) . . . . ? C2 C3 C4 C14 159.5(4) . . . . ? C3 C4 C5 C6 13.0(6) . . . . ? C14 C4 C5 C6 -160.2(4) . . . . ? C4 C5 C6 C1 -0.3(6) . . . . ? C2 C1 C6 C5 -11.9(6) . . . . ? C12 C1 C6 C5 152.1(4) . . . . ? Ti1 O1 C7 C8 169.1(8) . . . . ? Ti1 O1 C7 C12 -9.5(13) . . . . ? O1 C7 C8 C9 178.2(4) . . . . ? C12 C7 C8 C9 -3.2(6) . . . . ? O1 C7 C8 C19 -1.3(6) . . . . ? C12 C7 C8 C19 177.3(4) . . . . ? C7 C8 C9 C10 2.2(7) . . . . ? C19 C8 C9 C10 -178.4(4) . . . . ? C8 C9 C10 C11 -0.3(7) . . . . ? C8 C9 C10 C23 179.7(4) . . . . ? C9 C10 C11 C12 -0.5(6) . . . . ? C23 C10 C11 C12 179.5(4) . . . . ? C10 C11 C12 C7 -0.7(7) . . . . ? C10 C11 C12 C1 176.8(4) . . . . ? O1 C7 C12 C11 -178.8(4) . . . . ? C8 C7 C12 C11 2.6(6) . . . . ? O1 C7 C12 C1 3.5(6) . . . . ? C8 C7 C12 C1 -175.2(4) . . . . ? C2 C1 C12 C11 -80.3(6) . . . . ? C6 C1 C12 C11 116.3(5) . . . . ? C2 C1 C12 C7 97.3(5) . . . . ? C6 C1 C12 C7 -66.1(5) . . . . ? Ti1 O2 C13 C18 -148.1(4) . . . . ? Ti1 O2 C13 C14 27.1(8) . . . . ? O2 C13 C14 C15 -172.1(4) . . . . ? C18 C13 C14 C15 3.1(6) . . . . ? O2 C13 C14 C4 6.0(6) . . . . ? C18 C13 C14 C4 -178.8(4) . . . . ? C3 C4 C14 C15 59.8(6) . . . . ? C5 C4 C14 C15 -127.5(5) . . . . ? C3 C4 C14 C13 -118.3(5) . . . . ? C5 C4 C14 C13 54.5(6) . . . . ? C13 C14 C15 C16 -4.5(7) . . . . ? C4 C14 C15 C16 177.5(4) . . . . ? C14 C15 C16 C17 1.4(6) . . . . ? C14 C15 C16 C28 -179.0(4) . . . . ? C15 C16 C17 C18 3.1(7) . . . . ? C28 C16 C17 C18 -176.4(4) . . . . ? C16 C17 C18 C13 -4.4(7) . . . . ? C16 C17 C18 C24 172.3(4) . . . . ? O2 C13 C18 C17 176.3(4) . . . . ? C14 C13 C18 C17 1.1(6) . . . . ? O2 C13 C18 C24 -0.3(6) . . . . ? C14 C13 C18 C24 -175.5(4) . . . . ? C9 C8 C19 C22 -117.3(5) . . . . ? C7 C8 C19 C22 62.2(5) . . . . ? C9 C8 C19 C20 120.8(5) . . . . ? C7 C8 C19 C20 -59.8(6) . . . . ? C9 C8 C19 C21 2.8(6) . . . . ? C7 C8 C19 C21 -177.8(4) . . . . ? C17 C18 C24 C26 127.8(5) . . . . ? C13 C18 C24 C26 -55.8(6) . . . . ? C17 C18 C24 C27 6.0(6) . . . . ? C13 C18 C24 C27 -177.6(4) . . . . ? C17 C18 C24 C25 -113.6(5) . . . . ? C13 C18 C24 C25 62.9(5) . . . . ? C33 N2 C29 C30 -0.9(6) . . . . ? Ti1 N2 C29 C30 172.9(3) . . . . ? N2 C29 C30 C31 0.2(7) . . . . ? C29 C30 C31 C32 0.0(7) . . . . ? C30 C31 C32 C33 0.7(7) . . . . ? C29 N2 C33 C32 1.6(6) . . . . ? Ti1 N2 C33 C32 -172.2(4) . . . . ? C31 C32 C33 N2 -1.6(7) . . . . ? C38 N3 C34 C35 0.3(7) . . . . ? Ti1 N3 C34 C35 178.4(4) . . . . ? N3 C34 C35 C36 -0.3(7) . . . . ? C34 C35 C36 C37 -0.2(8) . . . . ? C35 C36 C37 C38 0.5(8) . . . . ? C34 N3 C38 C37 0.1(6) . . . . ? Ti1 N3 C38 C37 -178.0(3) . . . . ? C36 C37 C38 N3 -0.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.503 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 962316' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(C6H4)(ArO)2ZrBn2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H46 O2 Zr' _chemical_formula_sum 'C42 H46 O2 Zr' _chemical_formula_weight 674.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.1726(15) _cell_length_b 21.898(3) _cell_length_c 15.189(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.409(6) _cell_angle_gamma 90.00 _cell_volume 3382.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4612 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9513 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Mercury375R CCD (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 13.6612 _diffrn_reflns_number 35970 _diffrn_reflns_av_R_equivalents 0.1139 _diffrn_reflns_av_sigmaI/netI 0.0934 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7752 _reflns_number_gt 4374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2009)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2009)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+2.7803P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7752 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1492 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Zr1 Zr 0.32571(5) 0.56569(2) 0.81655(3) 0.01996(14) Uani 1 1 d . . . O1 O 0.2684(3) 0.48242(14) 0.7795(2) 0.0191(8) Uani 1 1 d . . . O2 O 0.3464(3) 0.65663(14) 0.8178(2) 0.0191(8) Uani 1 1 d . . . C1 C 0.1398(5) 0.5332(2) 0.6421(3) 0.0204(11) Uani 1 1 d . . . C2 C 0.2624(5) 0.5592(2) 0.6240(3) 0.0199(11) Uani 1 1 d . . . H1 H 0.3304 0.5346 0.6009 0.024 Uiso 1 1 calc R . . C3 C 0.2843(5) 0.6206(2) 0.6397(3) 0.0197(11) Uani 1 1 d . . . H2 H 0.3672 0.6380 0.6268 0.024 Uiso 1 1 calc R . . C4 C 0.1855(5) 0.6574(2) 0.6745(3) 0.0190(11) Uani 1 1 d . . . C5 C 0.0583(5) 0.6330(2) 0.6797(3) 0.0204(11) Uani 1 1 d . . . H3 H -0.0133 0.6586 0.6944 0.024 Uiso 1 1 calc R . . C6 C 0.0375(5) 0.5711(2) 0.6635(3) 0.0225(11) Uani 1 1 d . . . H4 H -0.0487 0.5548 0.6672 0.027 Uiso 1 1 calc R . . C7 C 0.2011(5) 0.4416(2) 0.7269(3) 0.0200(11) Uani 1 1 d . . . C8 C 0.1939(5) 0.3788(2) 0.7460(3) 0.0206(11) Uani 1 1 d . . . C9 C 0.1192(5) 0.3428(2) 0.6880(3) 0.0246(12) Uani 1 1 d . . . H5 H 0.1153 0.3001 0.6990 0.029 Uiso 1 1 calc R . . C10 C 0.0496(5) 0.3655(2) 0.6145(3) 0.0263(12) Uani 1 1 d . . . C11 C 0.0564(5) 0.4281(2) 0.5980(3) 0.0243(12) Uani 1 1 d . . . H6 H 0.0095 0.4451 0.5491 0.029 Uiso 1 1 calc R . . C12 C 0.1324(5) 0.4657(2) 0.6537(3) 0.0234(12) Uani 1 1 d . . . C13 C 0.3101(5) 0.7134(2) 0.7891(3) 0.0198(11) Uani 1 1 d . . . C14 C 0.2240(5) 0.7167(2) 0.7154(3) 0.0190(11) Uani 1 1 d . . . C15 C 0.1768(5) 0.7728(2) 0.6853(3) 0.0206(11) Uani 1 1 d . . . H7 H 0.1165 0.7740 0.6366 0.025 Uiso 1 1 calc R . . C16 C 0.2163(5) 0.8266(2) 0.7252(3) 0.0214(11) Uani 1 1 d . . . C17 C 0.3014(5) 0.8222(2) 0.7982(3) 0.0236(12) Uani 1 1 d . . . H8 H 0.3259 0.8590 0.8272 0.028 Uiso 1 1 calc R . . C18 C 0.3536(5) 0.7676(2) 0.8321(3) 0.0200(11) Uani 1 1 d . . . C19 C 0.2616(5) 0.3511(2) 0.8284(3) 0.0221(11) Uani 1 1 d . . . C20 C 0.4114(5) 0.3596(2) 0.8235(4) 0.0280(13) Uani 1 1 d . . . H9 H 0.4439 0.3376 0.7722 0.042 Uiso 1 1 calc R . . H10 H 0.4539 0.3434 0.8772 0.042 Uiso 1 1 calc R . . H11 H 0.4318 0.4031 0.8179 0.042 Uiso 1 1 calc R . . C21 C 0.2364(6) 0.2815(2) 0.8366(3) 0.0311(13) Uani 1 1 d . . . H12 H 0.1428 0.2743 0.8461 0.047 Uiso 1 1 calc R . . H13 H 0.2882 0.2652 0.8865 0.047 Uiso 1 1 calc R . . H14 H 0.2624 0.2611 0.7823 0.047 Uiso 1 1 calc R . . C22 C 0.2132(5) 0.3809(2) 0.9118(3) 0.0261(12) Uani 1 1 d . . . H15 H 0.2328 0.4247 0.9105 0.039 Uiso 1 1 calc R . . H16 H 0.2576 0.3622 0.9631 0.039 Uiso 1 1 calc R . . H17 H 0.1181 0.3749 0.9156 0.039 Uiso 1 1 calc R . . C23 C -0.0294(6) 0.3233(2) 0.5544(3) 0.0324(14) Uani 1 1 d . . . H18 H -0.0931 0.3472 0.5194 0.049 Uiso 1 1 calc R . . H19 H -0.0761 0.2934 0.5900 0.049 Uiso 1 1 calc R . . H20 H 0.0300 0.3019 0.5150 0.049 Uiso 1 1 calc R . . C24 C 0.4472(5) 0.7672(2) 0.9120(3) 0.0236(12) Uani 1 1 d . . . C25 C 0.5735(5) 0.7307(2) 0.8927(3) 0.0284(13) Uani 1 1 d . . . H21 H 0.5503 0.6884 0.8782 0.043 Uiso 1 1 calc R . . H22 H 0.6323 0.7313 0.9448 0.043 Uiso 1 1 calc R . . H23 H 0.6181 0.7494 0.8429 0.043 Uiso 1 1 calc R . . C26 C 0.3802(5) 0.7391(2) 0.9918(3) 0.0279(13) Uani 1 1 d . . . H24 H 0.2962 0.7598 1.0010 0.042 Uiso 1 1 calc R . . H25 H 0.4372 0.7440 1.0442 0.042 Uiso 1 1 calc R . . H26 H 0.3643 0.6956 0.9810 0.042 Uiso 1 1 calc R . . C27 C 0.4911(6) 0.8322(2) 0.9384(4) 0.0356(15) Uani 1 1 d . . . H27 H 0.5344 0.8517 0.8888 0.053 Uiso 1 1 calc R . . H28 H 0.5527 0.8300 0.9889 0.053 Uiso 1 1 calc R . . H29 H 0.4141 0.8563 0.9544 0.053 Uiso 1 1 calc R . . C28 C 0.1688(5) 0.8881(2) 0.6932(3) 0.0269(12) Uani 1 1 d . . . H30 H 0.1156 0.8829 0.6390 0.040 Uiso 1 1 calc R . . H31 H 0.2446 0.9142 0.6813 0.040 Uiso 1 1 calc R . . H32 H 0.1153 0.9071 0.7384 0.040 Uiso 1 1 calc R . . C29 C 0.2616(5) 0.5590(2) 0.9565(3) 0.0211(11) Uani 1 1 d . . . H33 H 0.2677 0.5172 0.9809 0.025 Uiso 1 1 calc R . . H34 H 0.3062 0.5887 0.9964 0.025 Uiso 1 1 calc R . . C30 C 0.1258(5) 0.5772(2) 0.9303(3) 0.0226(12) Uani 1 1 d . . . C31 C 0.0885(5) 0.6392(2) 0.9273(3) 0.0267(12) Uani 1 1 d . . . H35 H 0.1498 0.6696 0.9457 0.032 Uiso 1 1 calc R . . C32 C -0.0361(5) 0.6565(2) 0.8980(3) 0.0271(13) Uani 1 1 d . . . H36 H -0.0588 0.6985 0.8964 0.032 Uiso 1 1 calc R . . C33 C -0.1274(5) 0.6134(2) 0.8712(3) 0.0271(13) Uani 1 1 d . . . H37 H -0.2132 0.6254 0.8523 0.033 Uiso 1 1 calc R . . C34 C -0.0926(5) 0.5529(3) 0.8721(3) 0.0313(14) Uani 1 1 d . . . H38 H -0.1549 0.5231 0.8531 0.038 Uiso 1 1 calc R . . C35 C 0.0322(5) 0.5343(2) 0.9003(3) 0.0249(12) Uani 1 1 d . . . H39 H 0.0544 0.4922 0.8994 0.030 Uiso 1 1 calc R . . C36 C 0.5344(5) 0.5416(2) 0.8481(3) 0.0255(12) Uani 1 1 d . . . H40 H 0.5778 0.5714 0.8883 0.031 Uiso 1 1 calc R . . H41 H 0.5442 0.4997 0.8721 0.031 Uiso 1 1 calc R . . C37 C 0.5800(5) 0.5467(2) 0.7559(3) 0.0223(12) Uani 1 1 d . . . C38 C 0.5816(5) 0.4962(2) 0.6988(4) 0.0283(13) Uani 1 1 d . . . H42 H 0.5519 0.4579 0.7199 0.034 Uiso 1 1 calc R . . C39 C 0.6243(6) 0.4998(3) 0.6134(4) 0.0352(14) Uani 1 1 d . . . H43 H 0.6253 0.4643 0.5776 0.042 Uiso 1 1 calc R . . C40 C 0.6664(6) 0.5562(2) 0.5792(4) 0.0331(14) Uani 1 1 d . . . H44 H 0.6977 0.5594 0.5210 0.040 Uiso 1 1 calc R . . C41 C 0.6606(5) 0.6066(2) 0.6334(4) 0.0284(13) Uani 1 1 d . . . H45 H 0.6874 0.6452 0.6115 0.034 Uiso 1 1 calc R . . C42 C 0.6170(5) 0.6027(2) 0.7188(3) 0.0264(12) Uani 1 1 d . . . H46 H 0.6118 0.6389 0.7531 0.032 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 0.0222(3) 0.0184(3) 0.0192(3) 0.0011(2) -0.00252(19) 0.0002(2) O1 0.0202(19) 0.0162(19) 0.0208(19) 0.0011(14) -0.0007(15) 0.0002(14) O2 0.027(2) 0.0132(17) 0.0171(17) -0.0005(14) 0.0006(15) 0.0023(14) C1 0.019(3) 0.023(3) 0.019(3) 0.003(2) -0.001(2) -0.001(2) C2 0.024(3) 0.022(3) 0.013(2) 0.000(2) 0.000(2) 0.003(2) C3 0.023(3) 0.021(3) 0.016(3) 0.003(2) -0.001(2) -0.001(2) C4 0.026(3) 0.022(3) 0.009(2) 0.003(2) 0.000(2) 0.006(2) C5 0.017(3) 0.023(3) 0.021(3) 0.005(2) -0.004(2) 0.004(2) C6 0.020(3) 0.021(3) 0.026(3) 0.000(2) -0.004(2) 0.000(2) C7 0.020(3) 0.023(3) 0.017(3) 0.001(2) 0.004(2) 0.002(2) C8 0.023(3) 0.022(3) 0.017(3) -0.002(2) 0.000(2) -0.003(2) C9 0.034(3) 0.013(3) 0.027(3) 0.002(2) 0.001(2) 0.000(2) C10 0.031(3) 0.030(3) 0.018(3) -0.001(2) 0.004(2) -0.006(2) C11 0.028(3) 0.027(3) 0.018(3) 0.002(2) -0.004(2) 0.000(2) C12 0.029(3) 0.018(3) 0.023(3) 0.004(2) 0.000(2) -0.001(2) C13 0.019(3) 0.018(3) 0.022(3) 0.001(2) 0.003(2) 0.002(2) C14 0.016(3) 0.022(3) 0.019(3) 0.000(2) 0.003(2) -0.001(2) C15 0.024(3) 0.019(3) 0.019(3) 0.005(2) -0.002(2) -0.001(2) C16 0.023(3) 0.016(3) 0.026(3) 0.004(2) 0.008(2) 0.001(2) C17 0.023(3) 0.022(3) 0.026(3) 0.000(2) 0.005(2) -0.003(2) C18 0.027(3) 0.018(3) 0.015(3) -0.003(2) 0.001(2) -0.001(2) C19 0.026(3) 0.015(3) 0.025(3) 0.002(2) 0.005(2) 0.001(2) C20 0.027(3) 0.025(3) 0.033(3) 0.007(2) 0.007(3) 0.006(2) C21 0.044(4) 0.020(3) 0.029(3) 0.004(2) -0.005(3) 0.001(3) C22 0.030(3) 0.028(3) 0.021(3) 0.006(2) 0.003(2) 0.006(2) C23 0.046(4) 0.026(3) 0.024(3) 0.001(2) -0.009(3) -0.010(3) C24 0.031(3) 0.018(3) 0.022(3) -0.005(2) -0.005(2) -0.001(2) C25 0.023(3) 0.035(3) 0.027(3) 0.000(2) -0.006(2) 0.004(2) C26 0.031(3) 0.035(3) 0.017(3) 0.003(2) -0.001(2) -0.001(3) C27 0.043(4) 0.026(3) 0.037(3) 0.001(3) -0.011(3) -0.013(3) C28 0.029(3) 0.021(3) 0.031(3) 0.002(2) -0.005(2) -0.002(2) C29 0.023(3) 0.018(3) 0.023(3) 0.002(2) 0.001(2) -0.001(2) C30 0.024(3) 0.027(3) 0.017(3) 0.001(2) 0.002(2) 0.003(2) C31 0.028(3) 0.023(3) 0.030(3) -0.002(2) 0.001(2) -0.005(2) C32 0.031(3) 0.025(3) 0.026(3) 0.003(2) 0.007(3) 0.007(2) C33 0.023(3) 0.034(3) 0.024(3) -0.002(2) 0.002(2) -0.002(2) C34 0.027(3) 0.036(4) 0.031(3) -0.004(2) -0.001(3) -0.006(3) C35 0.024(3) 0.024(3) 0.027(3) -0.003(2) -0.001(2) -0.001(2) C36 0.025(3) 0.025(3) 0.026(3) 0.005(2) -0.004(2) 0.002(2) C37 0.018(3) 0.021(3) 0.029(3) 0.004(2) -0.004(2) 0.001(2) C38 0.031(3) 0.018(3) 0.036(3) 0.002(2) 0.001(3) 0.001(2) C39 0.049(4) 0.022(3) 0.036(3) -0.002(3) 0.009(3) 0.004(3) C40 0.041(4) 0.029(3) 0.030(3) 0.005(2) 0.005(3) 0.004(3) C41 0.029(3) 0.019(3) 0.036(3) 0.004(2) -0.005(3) -0.002(2) C42 0.024(3) 0.025(3) 0.030(3) -0.003(2) -0.011(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 1.991(3) . ? Zr1 O2 2.003(3) . ? Zr1 C36 2.228(5) . ? Zr1 C29 2.243(5) . ? Zr1 C30 2.712(5) . ? Zr1 C37 2.799(5) . ? O1 C7 1.370(6) . ? O2 C13 1.366(5) . ? C1 C6 1.377(7) . ? C1 C2 1.405(7) . ? C1 C12 1.489(7) . ? C2 C3 1.382(6) . ? C2 H1 0.9500 . ? C3 C4 1.402(7) . ? C3 H2 0.9500 . ? C4 C5 1.405(7) . ? C4 C14 1.488(6) . ? C5 C6 1.392(7) . ? C5 H3 0.9500 . ? C6 H4 0.9500 . ? C7 C12 1.402(6) . ? C7 C8 1.409(7) . ? C8 C9 1.393(7) . ? C8 C19 1.538(7) . ? C9 C10 1.399(7) . ? C9 H5 0.9500 . ? C10 C11 1.394(7) . ? C10 C23 1.516(7) . ? C11 C12 1.401(7) . ? C11 H6 0.9500 . ? C13 C14 1.407(7) . ? C13 C18 1.420(6) . ? C14 C15 1.391(6) . ? C15 C16 1.381(6) . ? C15 H7 0.9500 . ? C16 C17 1.393(7) . ? C16 C28 1.506(6) . ? C17 C18 1.401(7) . ? C17 H8 0.9500 . ? C18 C24 1.525(7) . ? C19 C22 1.516(7) . ? C19 C20 1.539(7) . ? C19 C21 1.551(7) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 H18 0.9800 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C24 C26 1.533(7) . ? C24 C27 1.543(7) . ? C24 C25 1.547(7) . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? C29 C30 1.483(7) . ? C29 H33 0.9900 . ? C29 H34 0.9900 . ? C30 C35 1.406(7) . ? C30 C31 1.409(7) . ? C31 C32 1.385(7) . ? C31 H35 0.9500 . ? C32 C33 1.379(7) . ? C32 H36 0.9500 . ? C33 C34 1.372(7) . ? C33 H37 0.9500 . ? C34 C35 1.390(7) . ? C34 H38 0.9500 . ? C35 H39 0.9500 . ? C36 C37 1.491(7) . ? C36 H40 0.9900 . ? C36 H41 0.9900 . ? C37 C42 1.405(7) . ? C37 C38 1.405(7) . ? C38 C39 1.380(7) . ? C38 H42 0.9500 . ? C39 C40 1.410(7) . ? C39 H43 0.9500 . ? C40 C41 1.379(7) . ? C40 H44 0.9500 . ? C41 C42 1.383(7) . ? C41 H45 0.9500 . ? C42 H46 0.9500 . ? 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 O1 Zr1 O2 160.60(13) . . ? O1 Zr1 C36 96.57(17) . . ? O2 Zr1 C36 97.71(17) . . ? O1 Zr1 C29 96.83(16) . . ? O2 Zr1 C29 95.08(16) . . ? C36 Zr1 C29 94.49(18) . . ? O1 Zr1 C30 92.68(15) . . ? O2 Zr1 C30 88.96(14) . . ? C36 Zr1 C30 127.62(17) . . ? C29 Zr1 C30 33.14(15) . . ? O1 Zr1 C37 92.15(14) . . ? O2 Zr1 C37 93.01(14) . . ? C36 Zr1 C37 32.02(16) . . ? C29 Zr1 C37 126.50(16) . . ? C30 Zr1 C37 159.59(15) . . ? C7 O1 Zr1 154.2(3) . . ? C13 O2 Zr1 151.0(3) . . ? C6 C1 C2 118.7(5) . . ? C6 C1 C12 122.0(5) . . ? C2 C1 C12 118.3(4) . . ? C3 C2 C1 120.1(5) . . ? C3 C2 H1 120.0 . . ? C1 C2 H1 120.0 . . ? C2 C3 C4 120.7(5) . . ? C2 C3 H2 119.7 . . ? C4 C3 H2 119.7 . . ? C3 C4 C5 118.2(5) . . ? C3 C4 C14 118.4(5) . . ? C5 C4 C14 122.8(4) . . ? C6 C5 C4 119.8(5) . . ? C6 C5 H3 120.1 . . ? C4 C5 H3 120.1 . . ? C1 C6 C5 121.1(5) . . ? C1 C6 H4 119.4 . . ? C5 C6 H4 119.4 . . ? O1 C7 C12 116.7(4) . . ? O1 C7 C8 123.0(4) . . ? C12 C7 C8 120.2(4) . . ? C9 C8 C7 116.9(4) . . ? C9 C8 C19 121.2(4) . . ? C7 C8 C19 121.8(4) . . ? C8 C9 C10 124.1(5) . . ? C8 C9 H5 117.9 . . ? C10 C9 H5 117.9 . . ? C11 C10 C9 117.8(5) . . ? C11 C10 C23 121.3(5) . . ? C9 C10 C23 120.9(5) . . ? C10 C11 C12 120.0(5) . . ? C10 C11 H6 120.0 . . ? C12 C11 H6 120.0 . . ? C11 C12 C7 121.0(5) . . ? C11 C12 C1 122.7(5) . . ? C7 C12 C1 116.2(4) . . ? O2 C13 C14 117.3(4) . . ? O2 C13 C18 122.4(4) . . ? C14 C13 C18 120.3(4) . . ? C15 C14 C13 120.7(5) . . ? C15 C14 C4 123.2(4) . . ? C13 C14 C4 116.1(4) . . ? C16 C15 C14 121.0(5) . . ? C16 C15 H7 119.5 . . ? C14 C15 H7 119.5 . . ? C15 C16 C17 117.3(5) . . ? C15 C16 C28 122.3(5) . . ? C17 C16 C28 120.5(4) . . ? C16 C17 C18 125.1(5) . . ? C16 C17 H8 117.5 . . ? C18 C17 H8 117.5 . . ? C17 C18 C13 115.7(4) . . ? C17 C18 C24 121.4(4) . . ? C13 C18 C24 122.8(4) . . ? C22 C19 C8 111.3(4) . . ? C22 C19 C20 109.3(4) . . ? C8 C19 C20 109.7(4) . . ? C22 C19 C21 107.3(4) . . ? C8 C19 C21 112.4(4) . . ? C20 C19 C21 106.7(4) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C10 C23 H18 109.5 . . ? C10 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? C10 C23 H20 109.5 . . ? H18 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C18 C24 C26 110.5(4) . . ? C18 C24 C27 111.9(4) . . ? C26 C24 C27 107.2(4) . . ? C18 C24 C25 111.0(4) . . ? C26 C24 C25 109.3(4) . . ? C27 C24 C25 106.8(4) . . ? C24 C25 H21 109.5 . . ? C24 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C26 H24 109.5 . . ? C24 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C24 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C16 C28 H30 109.5 . . ? C16 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C16 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C30 C29 Zr1 91.0(3) . . ? C30 C29 H33 113.5 . . ? Zr1 C29 H33 113.5 . . ? C30 C29 H34 113.5 . . ? Zr1 C29 H34 113.5 . . ? H33 C29 H34 110.8 . . ? C35 C30 C31 116.9(5) . . ? C35 C30 C29 121.8(5) . . ? C31 C30 C29 121.0(5) . . ? C35 C30 Zr1 104.2(3) . . ? C31 C30 Zr1 106.0(3) . . ? C29 C30 Zr1 55.8(2) . . ? C32 C31 C30 121.2(5) . . ? C32 C31 H35 119.4 . . ? C30 C31 H35 119.4 . . ? C33 C32 C31 120.8(5) . . ? C33 C32 H36 119.6 . . ? C31 C32 H36 119.6 . . ? C34 C33 C32 119.1(5) . . ? C34 C33 H37 120.5 . . ? C32 C33 H37 120.5 . . ? C33 C34 C35 121.3(5) . . ? C33 C34 H38 119.4 . . ? C35 C34 H38 119.4 . . ? C34 C35 C30 120.7(5) . . ? C34 C35 H39 119.6 . . ? C30 C35 H39 119.6 . . ? C37 C36 Zr1 95.6(3) . . ? C37 C36 H40 112.6 . . ? Zr1 C36 H40 112.6 . . ? C37 C36 H41 112.6 . . ? Zr1 C36 H41 112.6 . . ? H40 C36 H41 110.1 . . ? C42 C37 C38 115.6(5) . . ? C42 C37 C36 122.4(5) . . ? C38 C37 C36 121.9(5) . . ? C42 C37 Zr1 105.1(3) . . ? C38 C37 Zr1 110.1(3) . . ? C36 C37 Zr1 52.4(2) . . ? C39 C38 C37 122.9(5) . . ? C39 C38 H42 118.5 . . ? C37 C38 H42 118.5 . . ? C38 C39 C40 120.1(5) . . ? C38 C39 H43 119.9 . . ? C40 C39 H43 119.9 . . ? C41 C40 C39 117.6(5) . . ? C41 C40 H44 121.2 . . ? C39 C40 H44 121.2 . . ? C40 C41 C42 122.0(5) . . ? C40 C41 H45 119.0 . . ? C42 C41 H45 119.0 . . ? C41 C42 C37 121.6(5) . . ? C41 C42 H46 119.2 . . ? C37 C42 H46 119.2 . . ? 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 O2 Zr1 O1 C7 -2.1(10) . . . . ? C36 Zr1 O1 C7 -139.3(7) . . . . ? C29 Zr1 O1 C7 125.4(7) . . . . ? C30 Zr1 O1 C7 92.3(7) . . . . ? C37 Zr1 O1 C7 -107.5(7) . . . . ? O1 Zr1 O2 C13 13.0(9) . . . . ? C36 Zr1 O2 C13 150.1(6) . . . . ? C29 Zr1 O2 C13 -114.7(6) . . . . ? C30 Zr1 O2 C13 -82.1(6) . . . . ? C37 Zr1 O2 C13 118.3(6) . . . . ? C6 C1 C2 C3 9.1(7) . . . . ? C12 C1 C2 C3 -159.6(4) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C2 C3 C4 C5 -9.9(7) . . . . ? C2 C3 C4 C14 161.6(4) . . . . ? C3 C4 C5 C6 9.7(7) . . . . ? C14 C4 C5 C6 -161.4(4) . . . . ? C2 C1 C6 C5 -9.3(7) . . . . ? C12 C1 C6 C5 158.9(5) . . . . ? C4 C5 C6 C1 -0.1(7) . . . . ? Zr1 O1 C7 C12 3.9(10) . . . . ? Zr1 O1 C7 C8 -172.9(5) . . . . ? O1 C7 C8 C9 178.4(4) . . . . ? C12 C7 C8 C9 1.6(7) . . . . ? O1 C7 C8 C19 0.2(7) . . . . ? C12 C7 C8 C19 -176.6(5) . . . . ? C7 C8 C9 C10 -1.7(8) . . . . ? C19 C8 C9 C10 176.5(5) . . . . ? C8 C9 C10 C11 0.5(8) . . . . ? C8 C9 C10 C23 179.9(5) . . . . ? C9 C10 C11 C12 0.7(8) . . . . ? C23 C10 C11 C12 -178.7(5) . . . . ? C10 C11 C12 C7 -0.7(8) . . . . ? C10 C11 C12 C1 -177.5(5) . . . . ? O1 C7 C12 C11 -177.5(4) . . . . ? C8 C7 C12 C11 -0.5(8) . . . . ? O1 C7 C12 C1 -0.5(7) . . . . ? C8 C7 C12 C1 176.5(4) . . . . ? C6 C1 C12 C11 74.0(7) . . . . ? C2 C1 C12 C11 -117.7(6) . . . . ? C6 C1 C12 C7 -103.0(6) . . . . ? C2 C1 C12 C7 65.3(6) . . . . ? Zr1 O2 C13 C14 -11.5(9) . . . . ? Zr1 O2 C13 C18 167.0(4) . . . . ? O2 C13 C14 C15 176.4(4) . . . . ? C18 C13 C14 C15 -2.2(7) . . . . ? O2 C13 C14 C4 -2.1(7) . . . . ? C18 C13 C14 C4 179.3(4) . . . . ? C3 C4 C14 C15 120.0(5) . . . . ? C5 C4 C14 C15 -68.9(7) . . . . ? C3 C4 C14 C13 -61.5(6) . . . . ? C5 C4 C14 C13 109.6(5) . . . . ? C13 C14 C15 C16 2.1(8) . . . . ? C4 C14 C15 C16 -179.5(5) . . . . ? C14 C15 C16 C17 -2.1(7) . . . . ? C14 C15 C16 C28 178.9(5) . . . . ? C15 C16 C17 C18 2.5(8) . . . . ? C28 C16 C17 C18 -178.5(5) . . . . ? C16 C17 C18 C13 -2.6(8) . . . . ? C16 C17 C18 C24 179.5(5) . . . . ? O2 C13 C18 C17 -176.1(4) . . . . ? C14 C13 C18 C17 2.3(7) . . . . ? O2 C13 C18 C24 1.7(8) . . . . ? C14 C13 C18 C24 -179.8(5) . . . . ? C9 C8 C19 C22 -120.1(5) . . . . ? C7 C8 C19 C22 58.0(6) . . . . ? C9 C8 C19 C20 118.8(5) . . . . ? C7 C8 C19 C20 -63.1(6) . . . . ? C9 C8 C19 C21 0.3(7) . . . . ? C7 C8 C19 C21 178.4(5) . . . . ? C17 C18 C24 C26 110.4(5) . . . . ? C13 C18 C24 C26 -67.4(6) . . . . ? C17 C18 C24 C27 -9.1(7) . . . . ? C13 C18 C24 C27 173.2(5) . . . . ? C17 C18 C24 C25 -128.2(5) . . . . ? C13 C18 C24 C25 54.0(7) . . . . ? O1 Zr1 C29 C30 -84.4(3) . . . . ? O2 Zr1 C29 C30 80.2(3) . . . . ? C36 Zr1 C29 C30 178.4(3) . . . . ? C37 Zr1 C29 C30 177.8(3) . . . . ? Zr1 C29 C30 C35 85.8(5) . . . . ? Zr1 C29 C30 C31 -88.8(4) . . . . ? O1 Zr1 C30 C35 -20.7(3) . . . . ? O2 Zr1 C30 C35 140.0(3) . . . . ? C36 Zr1 C30 C35 -121.1(3) . . . . ? C29 Zr1 C30 C35 -119.1(5) . . . . ? C37 Zr1 C30 C35 -124.2(4) . . . . ? O1 Zr1 C30 C31 -144.6(3) . . . . ? O2 Zr1 C30 C31 16.1(3) . . . . ? C36 Zr1 C30 C31 115.0(4) . . . . ? C29 Zr1 C30 C31 117.0(5) . . . . ? C37 Zr1 C30 C31 111.9(5) . . . . ? O1 Zr1 C30 C29 98.4(3) . . . . ? O2 Zr1 C30 C29 -100.9(3) . . . . ? C36 Zr1 C30 C29 -2.0(4) . . . . ? C37 Zr1 C30 C29 -5.1(6) . . . . ? C35 C30 C31 C32 1.4(7) . . . . ? C29 C30 C31 C32 176.3(5) . . . . ? Zr1 C30 C31 C32 116.9(5) . . . . ? C30 C31 C32 C33 0.3(8) . . . . ? C31 C32 C33 C34 -1.3(8) . . . . ? C32 C33 C34 C35 0.6(8) . . . . ? C33 C34 C35 C30 1.1(8) . . . . ? C31 C30 C35 C34 -2.0(7) . . . . ? C29 C30 C35 C34 -176.9(5) . . . . ? Zr1 C30 C35 C34 -118.6(5) . . . . ? O1 Zr1 C36 C37 83.5(3) . . . . ? O2 Zr1 C36 C37 -83.3(3) . . . . ? C29 Zr1 C36 C37 -179.1(3) . . . . ? C30 Zr1 C36 C37 -178.0(3) . . . . ? Zr1 C36 C37 C42 84.4(5) . . . . ? Zr1 C36 C37 C38 -91.9(5) . . . . ? O1 Zr1 C37 C42 141.5(3) . . . . ? O2 Zr1 C37 C42 -19.8(3) . . . . ? C36 Zr1 C37 C42 -119.5(5) . . . . ? C29 Zr1 C37 C42 -118.3(3) . . . . ? C30 Zr1 C37 C42 -114.9(5) . . . . ? O1 Zr1 C37 C38 16.4(4) . . . . ? O2 Zr1 C37 C38 -144.9(4) . . . . ? C36 Zr1 C37 C38 115.3(5) . . . . ? C29 Zr1 C37 C38 116.5(4) . . . . ? C30 Zr1 C37 C38 120.0(5) . . . . ? O1 Zr1 C37 C36 -99.0(3) . . . . ? O2 Zr1 C37 C36 99.7(3) . . . . ? C29 Zr1 C37 C36 1.2(4) . . . . ? C30 Zr1 C37 C36 4.6(6) . . . . ? C42 C37 C38 C39 4.0(8) . . . . ? C36 C37 C38 C39 -179.5(5) . . . . ? Zr1 C37 C38 C39 123.0(5) . . . . ? C37 C38 C39 C40 -1.3(9) . . . . ? C38 C39 C40 C41 -1.2(8) . . . . ? C39 C40 C41 C42 0.8(8) . . . . ? C40 C41 C42 C37 2.1(8) . . . . ? C38 C37 C42 C41 -4.3(7) . . . . ? C36 C37 C42 C41 179.2(5) . . . . ? Zr1 C37 C42 C41 -126.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.104 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.122 _database_code_depnum_ccdc_archive 'CCDC 962317' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(C6H4)(ArO)2ZrCl2(thf) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Cl2 O3 Zr' _chemical_formula_sum 'C32 H40 Cl2 O3 Zr' _chemical_formula_weight 634.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 15.032(2) _cell_length_b 9.1927(15) _cell_length_c 22.154(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.733(3) _cell_angle_gamma 90.00 _cell_volume 3061.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8077 _cell_measurement_theta_min 3.1729 _cell_measurement_theta_max 27.4816 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9354 _exptl_absorpt_correction_T_max 0.9616 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Mercury375R CCD (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 13.6612 _diffrn_reflns_number 24316 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6957 _reflns_number_gt 5714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2009)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2009)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6957 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Zr1 Zr 0.235924(17) 0.39122(3) 0.453819(11) 0.01840(11) Uani 1 1 d . . . Cl1 Cl 0.10774(5) 0.29598(9) 0.50357(3) 0.03168(19) Uani 1 1 d . . . Cl2 Cl 0.31348(5) 0.16128(8) 0.45360(4) 0.03221(19) Uani 1 1 d . . . O1 O 0.19651(13) 0.3829(2) 0.36862(9) 0.0215(4) Uani 1 1 d . . . O2 O 0.30255(12) 0.4739(2) 0.52272(8) 0.0209(4) Uani 1 1 d . . . C1 C 0.32004(19) 0.5804(3) 0.33468(12) 0.0216(6) Uani 1 1 d . . . C2 C 0.37366(18) 0.4845(3) 0.36813(13) 0.0231(6) Uani 1 1 d . . . H1 H 0.3866 0.3909 0.3522 0.028 Uiso 1 1 calc R . . C3 C 0.40792(17) 0.5237(3) 0.42365(13) 0.0220(6) Uani 1 1 d . . . H2 H 0.4456 0.4585 0.4453 0.026 Uiso 1 1 calc R . . C4 C 0.38717(18) 0.6601(3) 0.44835(12) 0.0210(6) Uani 1 1 d . . . C5 C 0.34534(19) 0.7627(3) 0.41133(13) 0.0238(6) Uani 1 1 d . . . H3 H 0.3398 0.8604 0.4247 0.029 Uiso 1 1 calc R . . C6 C 0.31177(19) 0.7229(3) 0.35501(12) 0.0237(6) Uani 1 1 d . . . H4 H 0.2830 0.7934 0.3302 0.028 Uiso 1 1 calc R . . C7 C 0.19625(19) 0.4159(3) 0.30884(12) 0.0202(6) Uani 1 1 d . . . C8 C 0.1336(2) 0.3552(3) 0.26809(13) 0.0227(6) Uani 1 1 d . . . C9 C 0.1401(2) 0.3967(3) 0.20751(13) 0.0224(6) Uani 1 1 d . . . H5 H 0.0992 0.3554 0.1793 0.027 Uiso 1 1 calc R . . C10 C 0.2030(2) 0.4947(3) 0.18598(13) 0.0253(6) Uani 1 1 d . . . C11 C 0.2614(2) 0.5562(3) 0.22738(13) 0.0247(6) Uani 1 1 d . . . H6 H 0.3035 0.6260 0.2142 0.030 Uiso 1 1 calc R . . C12 C 0.25946(19) 0.5174(3) 0.28798(13) 0.0229(6) Uani 1 1 d . . . C13 C 0.35618(18) 0.5731(3) 0.55069(13) 0.0201(6) Uani 1 1 d . . . C14 C 0.39794(18) 0.6800(3) 0.51438(12) 0.0210(6) Uani 1 1 d . . . C15 C 0.44214(19) 0.7956(3) 0.54118(14) 0.0263(6) Uani 1 1 d . . . H7 H 0.4676 0.8688 0.5165 0.032 Uiso 1 1 calc R . . C16 C 0.44986(19) 0.8064(3) 0.60408(14) 0.0254(6) Uani 1 1 d . . . C17 C 0.41471(18) 0.6930(3) 0.63785(13) 0.0239(6) Uani 1 1 d . . . H8 H 0.4236 0.6959 0.6804 0.029 Uiso 1 1 calc R . . C18 C 0.36747(19) 0.5756(3) 0.61391(13) 0.0218(6) Uani 1 1 d . . . C19 C 0.06144(19) 0.2485(3) 0.28861(13) 0.0249(6) Uani 1 1 d . . . C20 C 0.1053(2) 0.1096(3) 0.31349(15) 0.0324(7) Uani 1 1 d . . . H9 H 0.1420 0.0654 0.2822 0.049 Uiso 1 1 calc R . . H10 H 0.0592 0.0407 0.3256 0.049 Uiso 1 1 calc R . . H11 H 0.1428 0.1341 0.3485 0.049 Uiso 1 1 calc R . . C21 C 0.0034(2) 0.3155(4) 0.33820(14) 0.0303(7) Uani 1 1 d . . . H12 H 0.0402 0.3347 0.3742 0.045 Uiso 1 1 calc R . . H13 H -0.0443 0.2476 0.3484 0.045 Uiso 1 1 calc R . . H14 H -0.0226 0.4069 0.3235 0.045 Uiso 1 1 calc R . . C22 C -0.0016(2) 0.2059(4) 0.23630(14) 0.0339(7) Uani 1 1 d . . . H15 H -0.0299 0.2936 0.2197 0.051 Uiso 1 1 calc R . . H16 H -0.0474 0.1396 0.2512 0.051 Uiso 1 1 calc R . . H17 H 0.0324 0.1575 0.2046 0.051 Uiso 1 1 calc R . . C23 C 0.2059(2) 0.5320(4) 0.12019(14) 0.0333(7) Uani 1 1 d . . . H18 H 0.2535 0.6029 0.1134 0.050 Uiso 1 1 calc R . . H19 H 0.1488 0.5738 0.1074 0.050 Uiso 1 1 calc R . . H20 H 0.2176 0.4437 0.0968 0.050 Uiso 1 1 calc R . . C24 C 0.3289(2) 0.4544(3) 0.65419(13) 0.0260(6) Uani 1 1 d . . . C25 C 0.3645(2) 0.3059(3) 0.63371(15) 0.0335(7) Uani 1 1 d . . . H21 H 0.3406 0.2294 0.6597 0.050 Uiso 1 1 calc R . . H22 H 0.4296 0.3057 0.6365 0.050 Uiso 1 1 calc R . . H23 H 0.3458 0.2879 0.5918 0.050 Uiso 1 1 calc R . . C26 C 0.3567(3) 0.4742(4) 0.72036(15) 0.0406(8) Uani 1 1 d . . . H24 H 0.3293 0.5628 0.7363 0.061 Uiso 1 1 calc R . . H25 H 0.4216 0.4824 0.7234 0.061 Uiso 1 1 calc R . . H26 H 0.3369 0.3901 0.7438 0.061 Uiso 1 1 calc R . . C27 C 0.2275(2) 0.4575(4) 0.65064(15) 0.0343(7) Uani 1 1 d . . . H27 H 0.2061 0.5534 0.6632 0.051 Uiso 1 1 calc R . . H28 H 0.2034 0.3827 0.6774 0.051 Uiso 1 1 calc R . . H29 H 0.2079 0.4383 0.6090 0.051 Uiso 1 1 calc R . . C28 C 0.4953(2) 0.9330(4) 0.63407(15) 0.0346(7) Uani 1 1 d . . . H30 H 0.4583 0.9691 0.6670 0.052 Uiso 1 1 calc R . . H31 H 0.5040 1.0107 0.6044 0.052 Uiso 1 1 calc R . . H32 H 0.5531 0.9019 0.6504 0.052 Uiso 1 1 calc R . . O3 O 0.16505(13) 0.6069(2) 0.45388(9) 0.0210(4) Uani 1 1 d . . . C29 C 0.1497(2) 0.6945(4) 0.50777(14) 0.0360(8) Uani 1 1 d . . . H33 H 0.2057 0.7076 0.5311 0.043 Uiso 1 1 calc R . . H34 H 0.1054 0.6471 0.5340 0.043 Uiso 1 1 calc R . . C30 C 0.1149(2) 0.8403(4) 0.48499(14) 0.0319(7) Uani 1 1 d . . . H35 H 0.1618 0.9158 0.4877 0.038 Uiso 1 1 calc R . . H36 H 0.0631 0.8724 0.5087 0.038 Uiso 1 1 calc R . . C31 C 0.0880(2) 0.8126(4) 0.41945(14) 0.0311(7) Uani 1 1 d . . . H37 H 0.0263 0.8459 0.4116 0.037 Uiso 1 1 calc R . . H38 H 0.1283 0.8644 0.3918 0.037 Uiso 1 1 calc R . . C32 C 0.0953(2) 0.6494(3) 0.41085(13) 0.0267(6) Uani 1 1 d . . . H39 H 0.0384 0.6005 0.4201 0.032 Uiso 1 1 calc R . . H40 H 0.1123 0.6253 0.3690 0.032 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 0.01919(17) 0.01859(17) 0.01739(16) 0.00137(9) -0.00071(11) -0.00161(10) Cl1 0.0267(4) 0.0387(4) 0.0297(4) 0.0064(3) 0.0035(3) -0.0078(3) Cl2 0.0341(4) 0.0213(4) 0.0412(4) 0.0004(3) 0.0002(3) 0.0045(3) O1 0.0251(11) 0.0214(10) 0.0181(10) 0.0008(7) -0.0012(8) -0.0017(8) O2 0.0217(10) 0.0210(10) 0.0201(9) 0.0010(7) -0.0022(8) -0.0030(8) C1 0.0229(14) 0.0255(14) 0.0165(13) 0.0024(10) 0.0049(11) -0.0053(12) C2 0.0210(14) 0.0254(15) 0.0230(14) -0.0007(11) 0.0035(11) -0.0025(11) C3 0.0147(12) 0.0264(15) 0.0248(14) 0.0024(11) -0.0001(11) -0.0002(11) C4 0.0185(13) 0.0217(14) 0.0229(13) 0.0022(11) -0.0006(11) -0.0066(11) C5 0.0290(15) 0.0192(14) 0.0233(14) 0.0002(11) 0.0028(11) -0.0036(12) C6 0.0283(15) 0.0227(14) 0.0201(13) 0.0052(11) 0.0025(11) -0.0043(12) C7 0.0217(14) 0.0224(13) 0.0166(13) -0.0011(10) 0.0015(11) 0.0003(11) C8 0.0268(15) 0.0195(13) 0.0218(14) 0.0018(11) 0.0000(12) 0.0012(12) C9 0.0274(15) 0.0223(15) 0.0173(13) -0.0020(10) -0.0035(11) 0.0012(11) C10 0.0312(16) 0.0271(15) 0.0176(13) 0.0001(11) 0.0015(12) 0.0053(13) C11 0.0292(15) 0.0251(15) 0.0197(14) 0.0018(11) 0.0069(12) -0.0001(13) C12 0.0235(14) 0.0245(14) 0.0208(13) -0.0037(11) 0.0006(11) -0.0003(12) C13 0.0170(13) 0.0206(13) 0.0227(14) -0.0014(11) -0.0009(11) 0.0012(11) C14 0.0173(13) 0.0238(14) 0.0219(13) 0.0008(11) 0.0013(11) -0.0009(11) C15 0.0237(15) 0.0244(15) 0.0308(16) 0.0001(12) -0.0003(12) -0.0018(12) C16 0.0229(14) 0.0256(15) 0.0276(15) -0.0047(12) 0.0019(12) -0.0002(12) C17 0.0222(14) 0.0277(15) 0.0219(13) -0.0046(11) -0.0004(11) 0.0037(12) C18 0.0201(14) 0.0240(14) 0.0212(14) 0.0009(11) -0.0006(11) 0.0026(11) C19 0.0284(15) 0.0211(14) 0.0251(14) 0.0010(11) -0.0042(12) -0.0073(12) C20 0.043(2) 0.0229(16) 0.0310(17) 0.0034(12) -0.0051(14) -0.0066(13) C21 0.0238(15) 0.0342(17) 0.0329(16) 0.0002(13) 0.0018(13) -0.0075(13) C22 0.0396(18) 0.0334(18) 0.0284(16) 0.0029(13) -0.0112(14) -0.0138(14) C23 0.0382(18) 0.0398(19) 0.0220(15) 0.0029(13) 0.0000(13) -0.0005(15) C24 0.0321(16) 0.0258(15) 0.0200(14) 0.0032(11) -0.0021(12) 0.0009(13) C25 0.0435(19) 0.0266(16) 0.0305(16) 0.0070(13) -0.0038(14) -0.0002(14) C26 0.054(2) 0.045(2) 0.0227(15) 0.0062(14) -0.0074(15) -0.0076(18) C27 0.0345(17) 0.0396(19) 0.0290(17) 0.0056(14) 0.0059(14) -0.0027(15) C28 0.0369(18) 0.0343(18) 0.0325(17) -0.0115(14) -0.0008(14) -0.0083(15) O3 0.0234(10) 0.0223(10) 0.0174(10) -0.0016(7) -0.0035(8) 0.0032(8) C29 0.047(2) 0.0402(19) 0.0202(14) -0.0107(13) -0.0063(13) 0.0212(16) C30 0.0392(18) 0.0253(16) 0.0310(16) -0.0054(13) -0.0060(14) 0.0016(14) C31 0.0339(17) 0.0299(17) 0.0295(16) 0.0049(12) -0.0028(13) 0.0080(14) C32 0.0288(15) 0.0288(15) 0.0224(14) -0.0032(12) -0.0075(12) 0.0077(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O2 1.9678(19) . ? Zr1 O1 1.973(2) . ? Zr1 O3 2.2508(19) . ? Zr1 Cl1 2.3976(8) . ? Zr1 Cl2 2.4140(8) . ? O1 C7 1.359(3) . ? O2 C13 1.361(3) . ? C1 C6 1.392(4) . ? C1 C2 1.400(4) . ? C1 C12 1.487(4) . ? C2 C3 1.375(4) . ? C3 C4 1.405(4) . ? C4 C5 1.394(4) . ? C4 C14 1.481(4) . ? C5 C6 1.389(4) . ? C7 C8 1.411(4) . ? C7 C12 1.414(4) . ? C8 C9 1.400(4) . ? C8 C19 1.536(4) . ? C9 C10 1.394(4) . ? C10 C11 1.383(4) . ? C10 C23 1.498(4) . ? C11 C12 1.390(4) . ? C13 C18 1.409(4) . ? C13 C14 1.421(4) . ? C14 C15 1.383(4) . ? C15 C16 1.400(4) . ? C16 C17 1.391(4) . ? C16 C28 1.500(4) . ? C17 C18 1.393(4) . ? C18 C24 1.545(4) . ? C19 C20 1.536(4) . ? C19 C22 1.538(4) . ? C19 C21 1.540(4) . ? C24 C27 1.526(4) . ? C24 C26 1.530(4) . ? C24 C25 1.536(4) . ? O3 C29 1.461(3) . ? O3 C32 1.461(3) . ? C29 C30 1.523(4) . ? C30 C31 1.524(4) . ? C31 C32 1.516(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 O2 Zr1 O1 154.27(8) . . ? O2 Zr1 O3 83.99(8) . . ? O1 Zr1 O3 84.15(7) . . ? O2 Zr1 Cl1 100.87(6) . . ? O1 Zr1 Cl1 101.10(6) . . ? O3 Zr1 Cl1 86.46(6) . . ? O2 Zr1 Cl2 95.68(6) . . ? O1 Zr1 Cl2 95.94(6) . . ? O3 Zr1 Cl2 179.37(6) . . ? Cl1 Zr1 Cl2 94.14(3) . . ? C7 O1 Zr1 157.13(18) . . ? C13 O2 Zr1 154.77(18) . . ? C6 C1 C2 118.3(3) . . ? C6 C1 C12 122.4(3) . . ? C2 C1 C12 117.8(3) . . ? C3 C2 C1 121.0(3) . . ? C2 C3 C4 120.0(3) . . ? C5 C4 C3 118.4(3) . . ? C5 C4 C14 122.7(3) . . ? C3 C4 C14 118.2(3) . . ? C6 C5 C4 120.4(3) . . ? C5 C6 C1 120.4(3) . . ? O1 C7 C8 121.9(3) . . ? O1 C7 C12 118.2(2) . . ? C8 C7 C12 119.9(3) . . ? C9 C8 C7 116.8(3) . . ? C9 C8 C19 121.1(3) . . ? C7 C8 C19 122.1(3) . . ? C10 C9 C8 124.1(3) . . ? C11 C10 C9 117.7(3) . . ? C11 C10 C23 121.6(3) . . ? C9 C10 C23 120.7(3) . . ? C10 C11 C12 121.0(3) . . ? C11 C12 C7 120.5(3) . . ? C11 C12 C1 123.5(3) . . ? C7 C12 C1 116.0(2) . . ? O2 C13 C18 121.8(2) . . ? O2 C13 C14 118.0(2) . . ? C18 C13 C14 120.2(3) . . ? C15 C14 C13 120.1(3) . . ? C15 C14 C4 124.4(3) . . ? C13 C14 C4 115.5(2) . . ? C14 C15 C16 121.0(3) . . ? C17 C16 C15 117.1(3) . . ? C17 C16 C28 121.1(3) . . ? C15 C16 C28 121.8(3) . . ? C16 C17 C18 124.8(3) . . ? C17 C18 C13 116.4(3) . . ? C17 C18 C24 122.1(3) . . ? C13 C18 C24 121.4(3) . . ? C8 C19 C20 109.6(2) . . ? C8 C19 C22 111.7(2) . . ? C20 C19 C22 108.5(3) . . ? C8 C19 C21 111.4(2) . . ? C20 C19 C21 108.7(3) . . ? C22 C19 C21 106.9(3) . . ? C27 C24 C26 107.9(3) . . ? C27 C24 C25 110.6(3) . . ? C26 C24 C25 107.3(3) . . ? C27 C24 C18 109.8(2) . . ? C26 C24 C18 111.6(3) . . ? C25 C24 C18 109.6(2) . . ? C29 O3 C32 105.4(2) . . ? C29 O3 Zr1 124.44(17) . . ? C32 O3 Zr1 124.82(16) . . ? O3 C29 C30 105.7(2) . . ? C29 C30 C31 104.7(2) . . ? C32 C31 C30 105.5(2) . . ? O3 C32 C31 103.6(2) . . ? 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 O2 Zr1 O1 C7 12.4(6) . . . . ? O3 Zr1 O1 C7 75.4(5) . . . . ? Cl1 Zr1 O1 C7 160.6(5) . . . . ? Cl2 Zr1 O1 C7 -104.0(5) . . . . ? O1 Zr1 O2 C13 4.0(5) . . . . ? O3 Zr1 O2 C13 -59.0(4) . . . . ? Cl1 Zr1 O2 C13 -144.2(4) . . . . ? Cl2 Zr1 O2 C13 120.4(4) . . . . ? C6 C1 C2 C3 8.4(4) . . . . ? C12 C1 C2 C3 -158.0(3) . . . . ? C1 C2 C3 C4 1.8(4) . . . . ? C2 C3 C4 C5 -11.3(4) . . . . ? C2 C3 C4 C14 159.4(3) . . . . ? C3 C4 C5 C6 10.6(4) . . . . ? C14 C4 C5 C6 -159.6(3) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C2 C1 C6 C5 -9.1(4) . . . . ? C12 C1 C6 C5 156.7(3) . . . . ? Zr1 O1 C7 C8 -178.3(3) . . . . ? Zr1 O1 C7 C12 -0.1(6) . . . . ? O1 C7 C8 C9 -179.7(2) . . . . ? C12 C7 C8 C9 2.2(4) . . . . ? O1 C7 C8 C19 0.3(4) . . . . ? C12 C7 C8 C19 -177.9(3) . . . . ? C7 C8 C9 C10 -1.1(4) . . . . ? C19 C8 C9 C10 178.9(3) . . . . ? C8 C9 C10 C11 -1.1(4) . . . . ? C8 C9 C10 C23 179.4(3) . . . . ? C9 C10 C11 C12 2.3(4) . . . . ? C23 C10 C11 C12 -178.2(3) . . . . ? C10 C11 C12 C7 -1.3(4) . . . . ? C10 C11 C12 C1 -179.6(3) . . . . ? O1 C7 C12 C11 -179.3(3) . . . . ? C8 C7 C12 C11 -1.1(4) . . . . ? O1 C7 C12 C1 -0.8(4) . . . . ? C8 C7 C12 C1 177.4(3) . . . . ? C6 C1 C12 C11 71.7(4) . . . . ? C2 C1 C12 C11 -122.5(3) . . . . ? C6 C1 C12 C7 -106.7(3) . . . . ? C2 C1 C12 C7 59.1(3) . . . . ? Zr1 O2 C13 C18 168.3(3) . . . . ? Zr1 O2 C13 C14 -8.8(6) . . . . ? O2 C13 C14 C15 170.4(2) . . . . ? C18 C13 C14 C15 -6.8(4) . . . . ? O2 C13 C14 C4 -7.4(4) . . . . ? C18 C13 C14 C4 175.5(3) . . . . ? C5 C4 C14 C15 -58.6(4) . . . . ? C3 C4 C14 C15 131.1(3) . . . . ? C5 C4 C14 C13 119.0(3) . . . . ? C3 C4 C14 C13 -51.2(3) . . . . ? C13 C14 C15 C16 2.7(4) . . . . ? C4 C14 C15 C16 -179.7(3) . . . . ? C14 C15 C16 C17 2.7(4) . . . . ? C14 C15 C16 C28 -178.2(3) . . . . ? C15 C16 C17 C18 -4.6(4) . . . . ? C28 C16 C17 C18 176.4(3) . . . . ? C16 C17 C18 C13 0.7(4) . . . . ? C16 C17 C18 C24 -179.0(3) . . . . ? O2 C13 C18 C17 -172.1(2) . . . . ? C14 C13 C18 C17 5.0(4) . . . . ? O2 C13 C18 C24 7.7(4) . . . . ? C14 C13 C18 C24 -175.3(3) . . . . ? C9 C8 C19 C20 116.7(3) . . . . ? C7 C8 C19 C20 -63.3(4) . . . . ? C9 C8 C19 C22 -3.6(4) . . . . ? C7 C8 C19 C22 176.5(3) . . . . ? C9 C8 C19 C21 -123.0(3) . . . . ? C7 C8 C19 C21 57.1(4) . . . . ? C17 C18 C24 C27 114.4(3) . . . . ? C13 C18 C24 C27 -65.3(4) . . . . ? C17 C18 C24 C26 -5.2(4) . . . . ? C13 C18 C24 C26 175.1(3) . . . . ? C17 C18 C24 C25 -123.9(3) . . . . ? C13 C18 C24 C25 56.4(4) . . . . ? O2 Zr1 O3 C29 -30.9(2) . . . . ? O1 Zr1 O3 C29 172.0(2) . . . . ? Cl1 Zr1 O3 C29 70.4(2) . . . . ? O2 Zr1 O3 C32 178.6(2) . . . . ? O1 Zr1 O3 C32 21.5(2) . . . . ? Cl1 Zr1 O3 C32 -80.0(2) . . . . ? C32 O3 C29 C30 -34.5(3) . . . . ? Zr1 O3 C29 C30 170.30(19) . . . . ? O3 C29 C30 C31 15.4(4) . . . . ? C29 C30 C31 C32 8.4(4) . . . . ? C29 O3 C32 C31 39.5(3) . . . . ? Zr1 O3 C32 C31 -165.42(18) . . . . ? C30 C31 C32 O3 -29.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.554 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 962318' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(C6H4)(ArO)2Zr(thf)3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H56 O5 Zr, C4 H8 O' _chemical_formula_sum 'C44 H64 O6 Zr' _chemical_formula_weight 780.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 24.091(6) _cell_length_b 9.788(2) _cell_length_c 16.906(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.277(5) _cell_angle_gamma 90.00 _cell_volume 3962.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8044 _cell_measurement_theta_min 3.0244 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.324 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9380 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Saturn CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 30136 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.1153 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9065 _reflns_number_gt 5588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+5.5681P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9065 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1821 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Zr1 Zr 0.766338(17) 0.25727(4) 0.17404(3) 0.01716(13) Uani 1 1 d . . . O1 O 0.84067(13) 0.3587(3) 0.21341(18) 0.0212(7) Uani 1 1 d . . . O2 O 0.69149(12) 0.2340(3) 0.10006(18) 0.0201(7) Uani 1 1 d . . . C1 C 0.81880(19) 0.1254(5) 0.2847(3) 0.0206(10) Uani 1 1 d . . . C2 C 0.76503(19) 0.1623(5) 0.3067(3) 0.0216(10) Uani 1 1 d . . . H1 H 0.7608 0.2192 0.3511 0.026 Uiso 1 1 calc R . . C3 C 0.71994(19) 0.1101(4) 0.2594(3) 0.0201(10) Uani 1 1 d . . . H2 H 0.6825 0.1252 0.2698 0.024 Uiso 1 1 calc R . . C4 C 0.7346(2) 0.0289(5) 0.1912(3) 0.0224(10) Uani 1 1 d . . . C5 C 0.78003(19) -0.0698(5) 0.2143(3) 0.0229(10) Uani 1 1 d . . . H3 H 0.7783 -0.1625 0.1976 0.027 Uiso 1 1 calc R . . C6 C 0.82397(19) -0.0183(4) 0.2607(3) 0.0212(10) Uani 1 1 d . . . H4 H 0.8563 -0.0712 0.2769 0.025 Uiso 1 1 calc R . . C7 C 0.87798(19) 0.3269(5) 0.2769(3) 0.0203(10) Uani 1 1 d . . . C8 C 0.9253(2) 0.4091(5) 0.3008(3) 0.0227(10) Uani 1 1 d . . . C9 C 0.9594(2) 0.3683(5) 0.3682(3) 0.0239(10) Uani 1 1 d . . . H5 H 0.9903 0.4247 0.3865 0.029 Uiso 1 1 calc R . . C10 C 0.95094(18) 0.2501(5) 0.4104(3) 0.0227(10) Uani 1 1 d . . . C11 C 0.90512(19) 0.1677(5) 0.3838(3) 0.0232(10) Uani 1 1 d . . . H6 H 0.8989 0.0849 0.4109 0.028 Uiso 1 1 calc R . . C12 C 0.86865(18) 0.2057(5) 0.3183(3) 0.0204(10) Uani 1 1 d . . . C13 C 0.66561(19) 0.1108(4) 0.0848(3) 0.0194(10) Uani 1 1 d . . . C14 C 0.68757(19) -0.0020(4) 0.1288(3) 0.0196(10) Uani 1 1 d . . . C15 C 0.6658(2) -0.1309(4) 0.1117(3) 0.0232(10) Uani 1 1 d . . . H7 H 0.6812 -0.2071 0.1412 0.028 Uiso 1 1 calc R . . C16 C 0.6214(2) -0.1514(5) 0.0521(3) 0.0245(11) Uani 1 1 d . . . C17 C 0.6005(2) -0.0379(5) 0.0100(3) 0.0250(11) Uani 1 1 d . . . H8 H 0.5705 -0.0510 -0.0305 0.030 Uiso 1 1 calc R . . C18 C 0.62097(18) 0.0950(5) 0.0235(3) 0.0187(10) Uani 1 1 d . . . C19 C 0.9404(2) 0.5337(5) 0.2512(3) 0.0263(11) Uani 1 1 d . . . C20 C 0.9531(2) 0.4824(6) 0.1695(3) 0.0362(13) Uani 1 1 d . . . H9 H 0.9869 0.4261 0.1757 0.054 Uiso 1 1 calc R . . H10 H 0.9588 0.5606 0.1351 0.054 Uiso 1 1 calc R . . H11 H 0.9216 0.4276 0.1454 0.054 Uiso 1 1 calc R . . C21 C 0.9935(2) 0.6049(6) 0.2881(3) 0.0422(15) Uani 1 1 d . . . H12 H 0.9872 0.6424 0.3401 0.063 Uiso 1 1 calc R . . H13 H 1.0030 0.6791 0.2531 0.063 Uiso 1 1 calc R . . H14 H 1.0242 0.5388 0.2947 0.063 Uiso 1 1 calc R . . C22 C 0.8934(2) 0.6372(5) 0.2411(4) 0.0474(16) Uani 1 1 d . . . H15 H 0.8586 0.5913 0.2206 0.071 Uiso 1 1 calc R . . H16 H 0.9022 0.7081 0.2035 0.071 Uiso 1 1 calc R . . H17 H 0.8889 0.6791 0.2926 0.071 Uiso 1 1 calc R . . C23 C 0.9904(2) 0.2122(6) 0.4843(3) 0.0310(12) Uani 1 1 d . . . H18 H 1.0280 0.1967 0.4691 0.047 Uiso 1 1 calc R . . H19 H 0.9770 0.1287 0.5080 0.047 Uiso 1 1 calc R . . H20 H 0.9914 0.2868 0.5231 0.047 Uiso 1 1 calc R . . C24 C 0.59646(19) 0.2174(5) -0.0253(3) 0.0235(11) Uani 1 1 d . . . C25 C 0.6432(2) 0.2817(5) -0.0687(3) 0.0325(13) Uani 1 1 d . . . H21 H 0.6763 0.2967 -0.0307 0.049 Uiso 1 1 calc R . . H22 H 0.6303 0.3693 -0.0921 0.049 Uiso 1 1 calc R . . H23 H 0.6526 0.2200 -0.1109 0.049 Uiso 1 1 calc R . . C26 C 0.5731(2) 0.3215(5) 0.0304(3) 0.0282(11) Uani 1 1 d . . . H24 H 0.5454 0.2770 0.0600 0.042 Uiso 1 1 calc R . . H25 H 0.5555 0.3970 -0.0011 0.042 Uiso 1 1 calc R . . H26 H 0.6037 0.3571 0.0678 0.042 Uiso 1 1 calc R . . C27 C 0.5488(2) 0.1763(5) -0.0883(3) 0.0292(12) Uani 1 1 d . . . H27 H 0.5625 0.1089 -0.1245 0.044 Uiso 1 1 calc R . . H28 H 0.5352 0.2572 -0.1186 0.044 Uiso 1 1 calc R . . H29 H 0.5183 0.1363 -0.0621 0.044 Uiso 1 1 calc R . . C28 C 0.5981(2) -0.2923(5) 0.0347(3) 0.0334(13) Uani 1 1 d . . . H30 H 0.5601 -0.2849 0.0077 0.050 Uiso 1 1 calc R . . H31 H 0.5973 -0.3425 0.0847 0.050 Uiso 1 1 calc R . . H32 H 0.6217 -0.3411 0.0004 0.050 Uiso 1 1 calc R . . O3 O 0.77151(13) 0.4309(3) 0.07649(19) 0.0233(7) Uani 1 1 d . . . C29 C 0.7306(2) 0.5385(5) 0.0635(3) 0.0326(12) Uani 1 1 d . . . H33 H 0.7340 0.6033 0.1088 0.039 Uiso 1 1 calc R . . H34 H 0.6923 0.5002 0.0574 0.039 Uiso 1 1 calc R . . C30 C 0.7431(2) 0.6097(6) -0.0126(3) 0.0395(14) Uani 1 1 d . . . H35 H 0.7235 0.5649 -0.0602 0.047 Uiso 1 1 calc R . . H36 H 0.7325 0.7074 -0.0124 0.047 Uiso 1 1 calc R . . C31 C 0.8048(2) 0.5926(5) -0.0093(4) 0.0405(14) Uani 1 1 d . . . H37 H 0.8248 0.6605 0.0268 0.049 Uiso 1 1 calc R . . H38 H 0.8175 0.6012 -0.0628 0.049 Uiso 1 1 calc R . . C32 C 0.8138(2) 0.4485(5) 0.0230(3) 0.0317(12) Uani 1 1 d . . . H39 H 0.8092 0.3806 -0.0206 0.038 Uiso 1 1 calc R . . H40 H 0.8517 0.4386 0.0518 0.038 Uiso 1 1 calc R . . O4 O 0.72227(13) 0.4335(3) 0.23288(19) 0.0226(7) Uani 1 1 d . . . C33 C 0.66234(19) 0.4431(5) 0.2361(3) 0.0270(11) Uani 1 1 d . . . H41 H 0.6487 0.3632 0.2641 0.032 Uiso 1 1 calc R . . H42 H 0.6424 0.4469 0.1818 0.032 Uiso 1 1 calc R . . C34 C 0.6530(2) 0.5740(5) 0.2812(3) 0.0343(13) Uani 1 1 d . . . H43 H 0.6476 0.6530 0.2447 0.041 Uiso 1 1 calc R . . H44 H 0.6202 0.5659 0.3114 0.041 Uiso 1 1 calc R . . C35 C 0.7059(2) 0.5877(6) 0.3361(3) 0.0424(15) Uani 1 1 d . . . H45 H 0.7041 0.5332 0.3851 0.051 Uiso 1 1 calc R . . H46 H 0.7132 0.6844 0.3510 0.051 Uiso 1 1 calc R . . C36 C 0.7502(2) 0.5334(5) 0.2882(3) 0.0322(13) Uani 1 1 d . . . H47 H 0.7663 0.6083 0.2587 0.039 Uiso 1 1 calc R . . H48 H 0.7805 0.4893 0.3234 0.039 Uiso 1 1 calc R . . O5 O 0.81544(13) 0.1535(3) 0.08221(18) 0.0227(7) Uani 1 1 d . . . C37 C 0.87531(19) 0.1273(5) 0.0970(3) 0.0268(11) Uani 1 1 d . . . H49 H 0.8865 0.1119 0.1544 0.032 Uiso 1 1 calc R . . H50 H 0.8969 0.2053 0.0790 0.032 Uiso 1 1 calc R . . C38 C 0.8851(2) 0.0006(5) 0.0497(3) 0.0302(12) Uani 1 1 d . . . H51 H 0.8806 -0.0832 0.0812 0.036 Uiso 1 1 calc R . . H52 H 0.9228 0.0011 0.0315 0.036 Uiso 1 1 calc R . . C39 C 0.8395(2) 0.0116(5) -0.0205(3) 0.0271(11) Uani 1 1 d . . . H53 H 0.8504 0.0755 -0.0615 0.032 Uiso 1 1 calc R . . H54 H 0.8309 -0.0787 -0.0452 0.032 Uiso 1 1 calc R . . C40 C 0.7914(2) 0.0651(5) 0.0176(3) 0.0254(11) Uani 1 1 d . . . H55 H 0.7660 0.1176 -0.0211 0.030 Uiso 1 1 calc R . . H56 H 0.7702 -0.0108 0.0387 0.030 Uiso 1 1 calc R . . O6 O 0.50418(16) 0.5638(4) 0.2576(2) 0.0425(10) Uani 1 1 d . . . C41 C 0.5134(2) 0.4619(6) 0.1995(3) 0.0388(14) Uani 1 1 d . . . H57 H 0.5406 0.3930 0.2226 0.047 Uiso 1 1 calc R . . H58 H 0.5282 0.5043 0.1530 0.047 Uiso 1 1 calc R . . C42 C 0.4579(2) 0.3961(6) 0.1750(3) 0.0374(13) Uani 1 1 d . . . H59 H 0.4624 0.2988 0.1610 0.045 Uiso 1 1 calc R . . H60 H 0.4376 0.4442 0.1291 0.045 Uiso 1 1 calc R . . C43 C 0.4275(2) 0.4105(6) 0.2492(4) 0.0408(14) Uani 1 1 d . . . H61 H 0.4372 0.3354 0.2874 0.049 Uiso 1 1 calc R . . H62 H 0.3865 0.4131 0.2355 0.049 Uiso 1 1 calc R . . C44 C 0.4500(2) 0.5481(6) 0.2820(3) 0.0377(13) Uani 1 1 d . . . H63 H 0.4253 0.6234 0.2606 0.045 Uiso 1 1 calc R . . H64 H 0.4518 0.5491 0.3408 0.045 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 0.0176(2) 0.0161(2) 0.0174(2) 0.00028(18) 0.00050(16) 0.00020(19) O1 0.0196(16) 0.0216(16) 0.0214(17) 0.0023(14) -0.0021(14) -0.0017(13) O2 0.0196(16) 0.0188(16) 0.0210(16) 0.0038(13) -0.0019(13) -0.0003(13) C1 0.020(2) 0.020(2) 0.022(2) -0.0002(19) 0.0012(19) -0.0001(19) C2 0.023(2) 0.021(2) 0.020(2) 0.001(2) 0.003(2) -0.0017(19) C3 0.018(2) 0.018(2) 0.024(2) 0.0062(19) 0.0017(19) -0.0040(18) C4 0.026(3) 0.017(2) 0.024(3) 0.000(2) 0.003(2) 0.0011(19) C5 0.028(3) 0.015(2) 0.026(3) -0.0032(19) 0.003(2) -0.0014(19) C6 0.022(2) 0.017(2) 0.025(2) -0.0006(19) -0.001(2) 0.0012(19) C7 0.020(2) 0.023(2) 0.017(2) -0.0046(19) 0.0007(19) -0.001(2) C8 0.026(3) 0.021(2) 0.021(2) -0.004(2) 0.003(2) 0.001(2) C9 0.022(2) 0.028(3) 0.022(2) -0.007(2) 0.002(2) -0.005(2) C10 0.017(2) 0.030(3) 0.021(2) -0.002(2) 0.0017(18) 0.004(2) C11 0.027(3) 0.025(2) 0.017(2) 0.002(2) 0.000(2) 0.003(2) C12 0.015(2) 0.020(2) 0.025(3) -0.0057(19) 0.0010(19) 0.0003(18) C13 0.024(2) 0.015(2) 0.020(2) -0.0052(18) 0.006(2) -0.0008(18) C14 0.022(2) 0.017(2) 0.020(2) -0.0034(19) 0.0027(19) -0.0013(19) C15 0.031(3) 0.013(2) 0.026(3) 0.0018(19) 0.004(2) 0.002(2) C16 0.025(3) 0.022(2) 0.026(3) 0.000(2) 0.005(2) -0.001(2) C17 0.022(2) 0.028(3) 0.024(3) -0.002(2) -0.001(2) -0.001(2) C18 0.019(2) 0.023(2) 0.014(2) -0.0053(19) -0.0004(18) -0.0005(19) C19 0.022(2) 0.028(3) 0.029(3) -0.003(2) 0.002(2) -0.006(2) C20 0.046(3) 0.038(3) 0.025(3) 0.002(2) 0.004(3) -0.012(3) C21 0.051(4) 0.034(3) 0.040(3) 0.005(3) -0.005(3) -0.024(3) C22 0.050(4) 0.021(3) 0.074(5) 0.012(3) 0.016(3) 0.003(3) C23 0.026(3) 0.043(3) 0.023(3) 0.004(2) -0.004(2) 0.002(2) C24 0.018(2) 0.031(3) 0.021(2) -0.004(2) -0.0023(19) 0.001(2) C25 0.043(3) 0.037(3) 0.018(3) 0.010(2) 0.004(2) 0.001(2) C26 0.028(3) 0.030(3) 0.027(3) 0.002(2) 0.001(2) 0.006(2) C27 0.028(3) 0.030(3) 0.028(3) -0.004(2) -0.004(2) 0.007(2) C28 0.033(3) 0.024(3) 0.041(3) -0.003(2) -0.005(3) -0.004(2) O3 0.0253(18) 0.0213(17) 0.0233(17) 0.0069(14) 0.0022(14) 0.0053(14) C29 0.039(3) 0.027(3) 0.032(3) 0.007(2) 0.006(2) 0.014(2) C30 0.054(4) 0.033(3) 0.033(3) 0.019(3) 0.010(3) 0.010(3) C31 0.050(4) 0.031(3) 0.042(3) 0.012(3) 0.013(3) -0.004(3) C32 0.034(3) 0.033(3) 0.031(3) 0.010(2) 0.015(2) 0.007(2) O4 0.0188(16) 0.0204(16) 0.0281(18) -0.0091(14) 0.0004(14) 0.0003(14) C33 0.017(2) 0.035(3) 0.029(3) -0.008(2) 0.004(2) 0.000(2) C34 0.033(3) 0.026(3) 0.045(3) -0.005(2) 0.013(3) 0.003(2) C35 0.043(3) 0.043(3) 0.041(3) -0.025(3) 0.005(3) 0.001(3) C36 0.032(3) 0.024(3) 0.038(3) -0.012(2) -0.006(2) 0.004(2) O5 0.0232(18) 0.0240(17) 0.0208(17) -0.0053(14) 0.0023(14) 0.0040(14) C37 0.014(2) 0.038(3) 0.028(3) -0.004(2) 0.001(2) 0.006(2) C38 0.029(3) 0.029(3) 0.033(3) -0.002(2) 0.005(2) 0.013(2) C39 0.034(3) 0.024(2) 0.025(3) -0.009(2) 0.008(2) 0.002(2) C40 0.028(3) 0.026(3) 0.022(3) -0.009(2) 0.004(2) -0.004(2) O6 0.036(2) 0.036(2) 0.056(3) -0.013(2) 0.007(2) -0.0073(18) C41 0.044(3) 0.036(3) 0.038(3) -0.006(3) 0.013(3) 0.009(3) C42 0.044(3) 0.031(3) 0.036(3) -0.003(3) 0.000(3) 0.007(3) C43 0.037(3) 0.035(3) 0.052(4) 0.002(3) 0.008(3) 0.001(3) C44 0.039(3) 0.035(3) 0.041(3) 0.001(3) 0.015(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 2.092(3) . ? Zr1 O2 2.091(3) . ? Zr1 O5 2.290(3) . ? Zr1 O4 2.307(3) . ? Zr1 O3 2.380(3) . ? Zr1 C4 2.391(5) . ? Zr1 C3 2.400(4) . ? Zr1 C2 2.431(5) . ? Zr1 C1 2.499(5) . ? O1 C7 1.358(5) . ? O2 C13 1.369(5) . ? C1 C2 1.432(6) . ? C1 C6 1.474(6) . ? C1 C12 1.494(6) . ? C2 C3 1.374(6) . ? C2 H1 0.9500 . ? C3 C4 1.475(6) . ? C3 H2 0.9500 . ? C4 C5 1.481(6) . ? C4 C14 1.492(6) . ? C5 C6 1.344(6) . ? C5 H3 0.9500 . ? C6 H4 0.9500 . ? C7 C12 1.407(6) . ? C7 C8 1.418(6) . ? C8 C9 1.389(6) . ? C8 C19 1.546(7) . ? C9 C10 1.386(6) . ? C9 H5 0.9500 . ? C10 C11 1.401(6) . ? C10 C23 1.530(6) . ? C11 C12 1.388(6) . ? C11 H6 0.9500 . ? C13 C14 1.402(6) . ? C13 C18 1.419(6) . ? C14 C15 1.385(6) . ? C15 C16 1.401(6) . ? C15 H7 0.9500 . ? C16 C17 1.383(6) . ? C16 C28 1.506(6) . ? C17 C18 1.401(6) . ? C17 H8 0.9500 . ? C18 C24 1.535(6) . ? C19 C22 1.516(7) . ? C19 C21 1.527(7) . ? C19 C20 1.531(7) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 H18 0.9800 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C24 C27 1.532(6) . ? C24 C26 1.535(7) . ? C24 C25 1.543(7) . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? O3 C29 1.443(5) . ? O3 C32 1.445(6) . ? C29 C30 1.521(7) . ? C29 H33 0.9900 . ? C29 H34 0.9900 . ? C30 C31 1.493(8) . ? C30 H35 0.9900 . ? C30 H36 0.9900 . ? C31 C32 1.519(7) . ? C31 H37 0.9900 . ? C31 H38 0.9900 . ? C32 H39 0.9900 . ? C32 H40 0.9900 . ? O4 C33 1.454(5) . ? O4 C36 1.464(5) . ? C33 C34 1.520(7) . ? C33 H41 0.9900 . ? C33 H42 0.9900 . ? C34 C35 1.498(7) . ? C34 H43 0.9900 . ? C34 H44 0.9900 . ? C35 C36 1.505(7) . ? C35 H45 0.9900 . ? C35 H46 0.9900 . ? C36 H47 0.9900 . ? C36 H48 0.9900 . ? O5 C37 1.459(5) . ? O5 C40 1.463(5) . ? C37 C38 1.508(6) . ? C37 H49 0.9900 . ? C37 H50 0.9900 . ? C38 C39 1.531(7) . ? C38 H51 0.9900 . ? C38 H52 0.9900 . ? C39 C40 1.480(6) . ? C39 H53 0.9900 . ? C39 H54 0.9900 . ? C40 H55 0.9900 . ? C40 H56 0.9900 . ? O6 C44 1.420(6) . ? O6 C41 1.435(6) . ? C41 C42 1.501(8) . ? C41 H57 0.9900 . ? C41 H58 0.9900 . ? C42 C43 1.525(8) . ? C42 H59 0.9900 . ? C42 H60 0.9900 . ? C43 C44 1.532(8) . ? C43 H61 0.9900 . ? C43 H62 0.9900 . ? C44 H63 0.9900 . ? C44 H64 0.9900 . ? 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 O1 Zr1 O2 153.40(12) . . ? O1 Zr1 O5 86.48(12) . . ? O2 Zr1 O5 91.25(12) . . ? O1 Zr1 O4 85.77(11) . . ? O2 Zr1 O4 86.10(11) . . ? O5 Zr1 O4 156.95(12) . . ? O1 Zr1 O3 76.92(11) . . ? O2 Zr1 O3 76.74(11) . . ? O5 Zr1 O3 77.11(11) . . ? O4 Zr1 O3 80.01(11) . . ? O1 Zr1 C4 132.81(14) . . ? O2 Zr1 C4 72.80(14) . . ? O5 Zr1 C4 82.17(14) . . ? O4 Zr1 C4 118.56(14) . . ? O3 Zr1 C4 142.49(14) . . ? O1 Zr1 C3 122.16(14) . . ? O2 Zr1 C3 82.33(14) . . ? O5 Zr1 C3 116.79(14) . . ? O4 Zr1 C3 85.57(14) . . ? O3 Zr1 C3 155.24(13) . . ? C4 Zr1 C3 35.85(15) . . ? O1 Zr1 C2 89.14(14) . . ? O2 Zr1 C2 114.37(14) . . ? O5 Zr1 C2 121.03(14) . . ? O4 Zr1 C2 80.52(14) . . ? O3 Zr1 C2 156.77(14) . . ? C4 Zr1 C2 59.58(16) . . ? C3 Zr1 C2 33.05(14) . . ? O1 Zr1 C1 70.22(13) . . ? O2 Zr1 C1 136.36(13) . . ? O5 Zr1 C1 91.27(13) . . ? O4 Zr1 C1 106.38(13) . . ? O3 Zr1 C1 145.76(13) . . ? C4 Zr1 C1 64.45(15) . . ? C3 Zr1 C1 58.03(15) . . ? C2 Zr1 C1 33.73(14) . . ? C7 O1 Zr1 127.7(3) . . ? C13 O2 Zr1 123.6(3) . . ? C2 C1 C6 114.7(4) . . ? C2 C1 C12 118.8(4) . . ? C6 C1 C12 121.2(4) . . ? C2 C1 Zr1 70.5(3) . . ? C6 C1 Zr1 109.7(3) . . ? C12 C1 Zr1 109.4(3) . . ? C3 C2 C1 115.8(4) . . ? C3 C2 Zr1 72.2(3) . . ? C1 C2 Zr1 75.8(3) . . ? C3 C2 H1 122.1 . . ? C1 C2 H1 122.1 . . ? Zr1 C2 H1 121.2 . . ? C2 C3 C4 114.4(4) . . ? C2 C3 Zr1 74.7(3) . . ? C4 C3 Zr1 71.7(2) . . ? C2 C3 H2 122.8 . . ? C4 C3 H2 122.8 . . ? Zr1 C3 H2 122.2 . . ? C3 C4 C5 112.3(4) . . ? C3 C4 C14 115.8(4) . . ? C5 C4 C14 122.5(4) . . ? C3 C4 Zr1 72.4(2) . . ? C5 C4 Zr1 113.9(3) . . ? C14 C4 Zr1 109.4(3) . . ? C6 C5 C4 115.0(4) . . ? C6 C5 H3 122.5 . . ? C4 C5 H3 122.5 . . ? C5 C6 C1 115.7(4) . . ? C5 C6 H4 122.2 . . ? C1 C6 H4 122.2 . . ? O1 C7 C12 117.3(4) . . ? O1 C7 C8 122.5(4) . . ? C12 C7 C8 120.2(4) . . ? C9 C8 C7 117.1(4) . . ? C9 C8 C19 121.3(4) . . ? C7 C8 C19 121.5(4) . . ? C10 C9 C8 123.8(4) . . ? C10 C9 H5 118.1 . . ? C8 C9 H5 118.1 . . ? C9 C10 C11 118.1(4) . . ? C9 C10 C23 120.6(4) . . ? C11 C10 C23 121.3(4) . . ? C12 C11 C10 120.6(4) . . ? C12 C11 H6 119.7 . . ? C10 C11 H6 119.7 . . ? C11 C12 C7 120.1(4) . . ? C11 C12 C1 125.0(4) . . ? C7 C12 C1 114.8(4) . . ? O2 C13 C14 117.1(4) . . ? O2 C13 C18 121.8(4) . . ? C14 C13 C18 121.0(4) . . ? C15 C14 C13 119.6(4) . . ? C15 C14 C4 125.0(4) . . ? C13 C14 C4 115.4(4) . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H7 119.3 . . ? C16 C15 H7 119.3 . . ? C17 C16 C15 117.5(4) . . ? C17 C16 C28 121.8(4) . . ? C15 C16 C28 120.7(4) . . ? C16 C17 C18 124.1(4) . . ? C16 C17 H8 118.0 . . ? C18 C17 H8 118.0 . . ? C17 C18 C13 116.4(4) . . ? C17 C18 C24 122.0(4) . . ? C13 C18 C24 121.6(4) . . ? C22 C19 C21 108.8(4) . . ? C22 C19 C20 109.7(5) . . ? C21 C19 C20 106.2(4) . . ? C22 C19 C8 111.8(4) . . ? C21 C19 C8 112.0(4) . . ? C20 C19 C8 108.2(4) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C10 C23 H18 109.5 . . ? C10 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? C10 C23 H20 109.5 . . ? H18 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C27 C24 C18 112.5(4) . . ? C27 C24 C26 107.7(4) . . ? C18 C24 C26 109.5(4) . . ? C27 C24 C25 107.9(4) . . ? C18 C24 C25 108.4(4) . . ? C26 C24 C25 110.8(4) . . ? C24 C25 H21 109.5 . . ? C24 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C26 H24 109.5 . . ? C24 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C24 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C16 C28 H30 109.5 . . ? C16 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C16 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C29 O3 C32 109.5(3) . . ? C29 O3 Zr1 122.7(3) . . ? C32 O3 Zr1 127.8(3) . . ? O3 C29 C30 105.5(4) . . ? O3 C29 H33 110.6 . . ? C30 C29 H33 110.6 . . ? O3 C29 H34 110.6 . . ? C30 C29 H34 110.6 . . ? H33 C29 H34 108.8 . . ? C31 C30 C29 101.8(4) . . ? C31 C30 H35 111.4 . . ? C29 C30 H35 111.4 . . ? C31 C30 H36 111.4 . . ? C29 C30 H36 111.4 . . ? H35 C30 H36 109.3 . . ? C30 C31 C32 102.7(4) . . ? C30 C31 H37 111.2 . . ? C32 C31 H37 111.2 . . ? C30 C31 H38 111.2 . . ? C32 C31 H38 111.2 . . ? H37 C31 H38 109.1 . . ? O3 C32 C31 104.7(4) . . ? O3 C32 H39 110.8 . . ? C31 C32 H39 110.8 . . ? O3 C32 H40 110.8 . . ? C31 C32 H40 110.8 . . ? H39 C32 H40 108.9 . . ? C33 O4 C36 108.7(3) . . ? C33 O4 Zr1 124.8(3) . . ? C36 O4 Zr1 125.0(3) . . ? O4 C33 C34 106.0(4) . . ? O4 C33 H41 110.5 . . ? C34 C33 H41 110.5 . . ? O4 C33 H42 110.5 . . ? C34 C33 H42 110.5 . . ? H41 C33 H42 108.7 . . ? C35 C34 C33 102.9(4) . . ? C35 C34 H43 111.2 . . ? C33 C34 H43 111.2 . . ? C35 C34 H44 111.2 . . ? C33 C34 H44 111.2 . . ? H43 C34 H44 109.1 . . ? C34 C35 C36 103.9(4) . . ? C34 C35 H45 111.0 . . ? C36 C35 H45 111.0 . . ? C34 C35 H46 111.0 . . ? C36 C35 H46 111.0 . . ? H45 C35 H46 109.0 . . ? O4 C36 C35 106.1(4) . . ? O4 C36 H47 110.5 . . ? C35 C36 H47 110.5 . . ? O4 C36 H48 110.5 . . ? C35 C36 H48 110.5 . . ? H47 C36 H48 108.7 . . ? C37 O5 C40 109.1(3) . . ? C37 O5 Zr1 122.4(3) . . ? C40 O5 Zr1 125.3(3) . . ? O5 C37 C38 105.2(4) . . ? O5 C37 H49 110.7 . . ? C38 C37 H49 110.7 . . ? O5 C37 H50 110.7 . . ? C38 C37 H50 110.7 . . ? H49 C37 H50 108.8 . . ? C37 C38 C39 102.3(4) . . ? C37 C38 H51 111.3 . . ? C39 C38 H51 111.3 . . ? C37 C38 H52 111.3 . . ? C39 C38 H52 111.3 . . ? H51 C38 H52 109.2 . . ? C40 C39 C38 102.5(4) . . ? C40 C39 H53 111.3 . . ? C38 C39 H53 111.3 . . ? C40 C39 H54 111.3 . . ? C38 C39 H54 111.3 . . ? H53 C39 H54 109.2 . . ? O5 C40 C39 105.7(4) . . ? O5 C40 H55 110.6 . . ? C39 C40 H55 110.6 . . ? O5 C40 H56 110.6 . . ? C39 C40 H56 110.6 . . ? H55 C40 H56 108.7 . . ? C44 O6 C41 109.8(4) . . ? O6 C41 C42 106.7(4) . . ? O6 C41 H57 110.4 . . ? C42 C41 H57 110.4 . . ? O6 C41 H58 110.4 . . ? C42 C41 H58 110.4 . . ? H57 C41 H58 108.6 . . ? C41 C42 C43 103.1(4) . . ? C41 C42 H59 111.1 . . ? C43 C42 H59 111.1 . . ? C41 C42 H60 111.1 . . ? C43 C42 H60 111.1 . . ? H59 C42 H60 109.1 . . ? C42 C43 C44 101.3(5) . . ? C42 C43 H61 111.5 . . ? C44 C43 H61 111.5 . . ? C42 C43 H62 111.5 . . ? C44 C43 H62 111.5 . . ? H61 C43 H62 109.3 . . ? O6 C44 C43 106.9(4) . . ? O6 C44 H63 110.3 . . ? C43 C44 H63 110.3 . . ? O6 C44 H64 110.3 . . ? C43 C44 H64 110.3 . . ? H63 C44 H64 108.6 . . ? 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 O2 Zr1 O1 C7 175.2(3) . . . . ? O5 Zr1 O1 C7 -99.1(3) . . . . ? O4 Zr1 O1 C7 102.6(4) . . . . ? O3 Zr1 O1 C7 -176.7(4) . . . . ? C4 Zr1 O1 C7 -23.2(4) . . . . ? C3 Zr1 O1 C7 20.5(4) . . . . ? C2 Zr1 O1 C7 22.1(4) . . . . ? C1 Zr1 O1 C7 -6.5(3) . . . . ? O1 Zr1 O2 C13 155.5(3) . . . . ? O5 Zr1 O2 C13 70.9(3) . . . . ? O4 Zr1 O2 C13 -132.0(3) . . . . ? O3 Zr1 O2 C13 147.4(3) . . . . ? C4 Zr1 O2 C13 -10.5(3) . . . . ? C3 Zr1 O2 C13 -45.9(3) . . . . ? C2 Zr1 O2 C13 -54.2(4) . . . . ? C1 Zr1 O2 C13 -22.2(4) . . . . ? O1 Zr1 C1 C2 120.7(3) . . . . ? O2 Zr1 C1 C2 -60.4(3) . . . . ? O5 Zr1 C1 C2 -153.6(3) . . . . ? O4 Zr1 C1 C2 41.5(3) . . . . ? O3 Zr1 C1 C2 137.8(3) . . . . ? C4 Zr1 C1 C2 -72.9(3) . . . . ? C3 Zr1 C1 C2 -32.4(3) . . . . ? O1 Zr1 C1 C6 -129.2(3) . . . . ? O2 Zr1 C1 C6 49.7(4) . . . . ? O5 Zr1 C1 C6 -43.4(3) . . . . ? O4 Zr1 C1 C6 151.6(3) . . . . ? O3 Zr1 C1 C6 -112.1(3) . . . . ? C4 Zr1 C1 C6 37.3(3) . . . . ? C3 Zr1 C1 C6 77.8(3) . . . . ? C2 Zr1 C1 C6 110.2(4) . . . . ? O1 Zr1 C1 C12 6.0(3) . . . . ? O2 Zr1 C1 C12 -175.1(3) . . . . ? O5 Zr1 C1 C12 91.8(3) . . . . ? O4 Zr1 C1 C12 -73.2(3) . . . . ? O3 Zr1 C1 C12 23.1(4) . . . . ? C4 Zr1 C1 C12 172.5(4) . . . . ? C3 Zr1 C1 C12 -147.0(4) . . . . ? C2 Zr1 C1 C12 -114.7(4) . . . . ? C6 C1 C2 C3 -41.5(6) . . . . ? C12 C1 C2 C3 163.8(4) . . . . ? Zr1 C1 C2 C3 61.8(4) . . . . ? C6 C1 C2 Zr1 -103.4(4) . . . . ? C12 C1 C2 Zr1 102.0(4) . . . . ? O1 Zr1 C2 C3 -177.7(3) . . . . ? O2 Zr1 C2 C3 15.2(3) . . . . ? O5 Zr1 C2 C3 -92.3(3) . . . . ? O4 Zr1 C2 C3 96.5(3) . . . . ? O3 Zr1 C2 C3 129.8(3) . . . . ? C4 Zr1 C2 C3 -34.8(3) . . . . ? C1 Zr1 C2 C3 -123.6(4) . . . . ? O1 Zr1 C2 C1 -54.1(3) . . . . ? O2 Zr1 C2 C1 138.8(2) . . . . ? O5 Zr1 C2 C1 31.3(3) . . . . ? O4 Zr1 C2 C1 -139.9(3) . . . . ? O3 Zr1 C2 C1 -106.6(4) . . . . ? C4 Zr1 C2 C1 88.8(3) . . . . ? C3 Zr1 C2 C1 123.6(4) . . . . ? C1 C2 C3 C4 -2.5(6) . . . . ? Zr1 C2 C3 C4 61.2(3) . . . . ? C1 C2 C3 Zr1 -63.8(4) . . . . ? O1 Zr1 C3 C2 2.8(3) . . . . ? O2 Zr1 C3 C2 -166.1(3) . . . . ? O5 Zr1 C3 C2 106.4(3) . . . . ? O4 Zr1 C3 C2 -79.4(3) . . . . ? O3 Zr1 C3 C2 -133.7(3) . . . . ? C4 Zr1 C3 C2 122.8(4) . . . . ? C1 Zr1 C3 C2 33.0(3) . . . . ? O1 Zr1 C3 C4 -120.0(3) . . . . ? O2 Zr1 C3 C4 71.1(3) . . . . ? O5 Zr1 C3 C4 -16.4(3) . . . . ? O4 Zr1 C3 C4 157.8(3) . . . . ? O3 Zr1 C3 C4 103.5(4) . . . . ? C2 Zr1 C3 C4 -122.8(4) . . . . ? C1 Zr1 C3 C4 -89.8(3) . . . . ? C2 C3 C4 C5 46.3(5) . . . . ? Zr1 C3 C4 C5 109.2(4) . . . . ? C2 C3 C4 C14 -166.4(4) . . . . ? Zr1 C3 C4 C14 -103.5(4) . . . . ? C2 C3 C4 Zr1 -62.9(3) . . . . ? O1 Zr1 C4 C3 87.5(3) . . . . ? O2 Zr1 C4 C3 -100.9(3) . . . . ? O5 Zr1 C4 C3 165.3(3) . . . . ? O4 Zr1 C4 C3 -25.4(3) . . . . ? O3 Zr1 C4 C3 -138.0(2) . . . . ? C2 Zr1 C4 C3 32.1(2) . . . . ? C1 Zr1 C4 C3 70.1(3) . . . . ? O1 Zr1 C4 C5 -19.6(4) . . . . ? O2 Zr1 C4 C5 151.9(4) . . . . ? O5 Zr1 C4 C5 58.2(3) . . . . ? O4 Zr1 C4 C5 -132.5(3) . . . . ? O3 Zr1 C4 C5 114.9(3) . . . . ? C3 Zr1 C4 C5 -107.1(4) . . . . ? C2 Zr1 C4 C5 -75.0(3) . . . . ? C1 Zr1 C4 C5 -37.0(3) . . . . ? O1 Zr1 C4 C14 -160.6(3) . . . . ? O2 Zr1 C4 C14 10.9(3) . . . . ? O5 Zr1 C4 C14 -82.9(3) . . . . ? O4 Zr1 C4 C14 86.5(3) . . . . ? O3 Zr1 C4 C14 -26.2(4) . . . . ? C3 Zr1 C4 C14 111.8(4) . . . . ? C2 Zr1 C4 C14 144.0(4) . . . . ? C1 Zr1 C4 C14 -178.1(4) . . . . ? C3 C4 C5 C6 -46.5(6) . . . . ? C14 C4 C5 C6 168.7(4) . . . . ? Zr1 C4 C5 C6 33.4(5) . . . . ? C4 C5 C6 C1 3.2(6) . . . . ? C2 C1 C6 C5 41.5(6) . . . . ? C12 C1 C6 C5 -164.5(4) . . . . ? Zr1 C1 C6 C5 -35.5(5) . . . . ? Zr1 O1 C7 C12 5.4(6) . . . . ? Zr1 O1 C7 C8 -175.8(3) . . . . ? O1 C7 C8 C9 177.9(4) . . . . ? C12 C7 C8 C9 -3.3(7) . . . . ? O1 C7 C8 C19 -5.8(7) . . . . ? C12 C7 C8 C19 173.0(4) . . . . ? C7 C8 C9 C10 3.0(7) . . . . ? C19 C8 C9 C10 -173.4(4) . . . . ? C8 C9 C10 C11 -0.5(7) . . . . ? C8 C9 C10 C23 -180.0(4) . . . . ? C9 C10 C11 C12 -1.6(7) . . . . ? C23 C10 C11 C12 177.8(4) . . . . ? C10 C11 C12 C7 1.1(7) . . . . ? C10 C11 C12 C1 179.7(4) . . . . ? O1 C7 C12 C11 -179.8(4) . . . . ? C8 C7 C12 C11 1.4(7) . . . . ? O1 C7 C12 C1 1.5(6) . . . . ? C8 C7 C12 C1 -177.3(4) . . . . ? C2 C1 C12 C11 97.7(6) . . . . ? C6 C1 C12 C11 -55.3(7) . . . . ? Zr1 C1 C12 C11 175.5(4) . . . . ? C2 C1 C12 C7 -83.7(5) . . . . ? C6 C1 C12 C7 123.3(5) . . . . ? Zr1 C1 C12 C7 -5.8(5) . . . . ? Zr1 O2 C13 C14 7.6(5) . . . . ? Zr1 O2 C13 C18 -168.1(3) . . . . ? O2 C13 C14 C15 -175.2(4) . . . . ? C18 C13 C14 C15 0.6(7) . . . . ? O2 C13 C14 C4 4.0(6) . . . . ? C18 C13 C14 C4 179.7(4) . . . . ? C3 C4 C14 C15 -112.9(5) . . . . ? C5 C4 C14 C15 30.8(7) . . . . ? Zr1 C4 C14 C15 167.8(4) . . . . ? C3 C4 C14 C13 68.0(5) . . . . ? C5 C4 C14 C13 -148.4(4) . . . . ? Zr1 C4 C14 C13 -11.3(5) . . . . ? C13 C14 C15 C16 -1.0(7) . . . . ? C4 C14 C15 C16 179.9(4) . . . . ? C14 C15 C16 C17 0.7(7) . . . . ? C14 C15 C16 C28 -179.7(5) . . . . ? C15 C16 C17 C18 0.0(8) . . . . ? C28 C16 C17 C18 -179.6(5) . . . . ? C16 C17 C18 C13 -0.4(7) . . . . ? C16 C17 C18 C24 179.6(5) . . . . ? O2 C13 C18 C17 175.7(4) . . . . ? C14 C13 C18 C17 0.1(7) . . . . ? O2 C13 C18 C24 -4.4(7) . . . . ? C14 C13 C18 C24 -179.9(4) . . . . ? C9 C8 C19 C22 -125.4(5) . . . . ? C7 C8 C19 C22 58.4(6) . . . . ? C9 C8 C19 C21 -3.0(7) . . . . ? C7 C8 C19 C21 -179.2(5) . . . . ? C9 C8 C19 C20 113.7(5) . . . . ? C7 C8 C19 C20 -62.5(6) . . . . ? C17 C18 C24 C27 -0.2(6) . . . . ? C13 C18 C24 C27 179.8(4) . . . . ? C17 C18 C24 C26 119.5(5) . . . . ? C13 C18 C24 C26 -60.4(6) . . . . ? C17 C18 C24 C25 -119.5(5) . . . . ? C13 C18 C24 C25 60.6(6) . . . . ? O1 Zr1 O3 C29 -116.9(3) . . . . ? O2 Zr1 O3 C29 59.4(3) . . . . ? O5 Zr1 O3 C29 153.8(4) . . . . ? O4 Zr1 O3 C29 -28.9(3) . . . . ? C4 Zr1 O3 C29 95.7(4) . . . . ? C3 Zr1 O3 C29 26.4(5) . . . . ? C2 Zr1 O3 C29 -62.3(5) . . . . ? C1 Zr1 O3 C29 -133.4(4) . . . . ? O1 Zr1 O3 C32 62.4(4) . . . . ? O2 Zr1 O3 C32 -121.4(4) . . . . ? O5 Zr1 O3 C32 -27.0(4) . . . . ? O4 Zr1 O3 C32 150.3(4) . . . . ? C4 Zr1 O3 C32 -85.1(4) . . . . ? C3 Zr1 O3 C32 -154.4(4) . . . . ? C2 Zr1 O3 C32 116.9(5) . . . . ? C1 Zr1 O3 C32 45.8(5) . . . . ? C32 O3 C29 C30 11.0(5) . . . . ? Zr1 O3 C29 C30 -169.7(3) . . . . ? O3 C29 C30 C31 -31.5(6) . . . . ? C29 C30 C31 C32 39.1(6) . . . . ? C29 O3 C32 C31 13.8(5) . . . . ? Zr1 O3 C32 C31 -165.5(3) . . . . ? C30 C31 C32 O3 -33.4(6) . . . . ? O1 Zr1 O4 C33 -177.8(4) . . . . ? O2 Zr1 O4 C33 27.6(3) . . . . ? O5 Zr1 O4 C33 111.6(4) . . . . ? O3 Zr1 O4 C33 104.8(3) . . . . ? C4 Zr1 O4 C33 -40.4(4) . . . . ? C3 Zr1 O4 C33 -55.0(4) . . . . ? C2 Zr1 O4 C33 -87.9(4) . . . . ? C1 Zr1 O4 C33 -109.8(4) . . . . ? O1 Zr1 O4 C36 -13.3(4) . . . . ? O2 Zr1 O4 C36 -167.9(4) . . . . ? O5 Zr1 O4 C36 -83.9(5) . . . . ? O3 Zr1 O4 C36 -90.7(4) . . . . ? C4 Zr1 O4 C36 124.1(4) . . . . ? C3 Zr1 O4 C36 109.5(4) . . . . ? C2 Zr1 O4 C36 76.5(4) . . . . ? C1 Zr1 O4 C36 54.7(4) . . . . ? C36 O4 C33 C34 12.5(5) . . . . ? Zr1 O4 C33 C34 179.2(3) . . . . ? O4 C33 C34 C35 -29.7(5) . . . . ? C33 C34 C35 C36 35.1(6) . . . . ? C33 O4 C36 C35 9.7(5) . . . . ? Zr1 O4 C36 C35 -156.9(3) . . . . ? C34 C35 C36 O4 -28.3(6) . . . . ? O1 Zr1 O5 C37 29.5(3) . . . . ? O2 Zr1 O5 C37 -177.1(3) . . . . ? O4 Zr1 O5 C37 100.0(4) . . . . ? O3 Zr1 O5 C37 106.8(3) . . . . ? C4 Zr1 O5 C37 -104.6(3) . . . . ? C3 Zr1 O5 C37 -95.0(3) . . . . ? C2 Zr1 O5 C37 -57.4(4) . . . . ? C1 Zr1 O5 C37 -40.6(3) . . . . ? O1 Zr1 O5 C40 -173.2(3) . . . . ? O2 Zr1 O5 C40 -19.7(3) . . . . ? O4 Zr1 O5 C40 -102.7(4) . . . . ? O3 Zr1 O5 C40 -95.8(3) . . . . ? C4 Zr1 O5 C40 52.7(3) . . . . ? C3 Zr1 O5 C40 62.3(4) . . . . ? C2 Zr1 O5 C40 100.0(3) . . . . ? C1 Zr1 O5 C40 116.7(3) . . . . ? C40 O5 C37 C38 -10.5(5) . . . . ? Zr1 O5 C37 C38 150.1(3) . . . . ? O5 C37 C38 C39 30.3(5) . . . . ? C37 C38 C39 C40 -38.9(5) . . . . ? C37 O5 C40 C39 -14.6(5) . . . . ? Zr1 O5 C40 C39 -174.5(3) . . . . ? C38 C39 C40 O5 33.0(5) . . . . ? C44 O6 C41 C42 11.2(6) . . . . ? O6 C41 C42 C43 -29.0(6) . . . . ? C41 C42 C43 C44 34.2(5) . . . . ? C41 O6 C44 C43 11.4(6) . . . . ? C42 C43 C44 O6 -28.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.493 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.116 _database_code_depnum_ccdc_archive 'CCDC 962319' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_{[(C6H3)(ArO)2]2[(C6H4)(ArO)2]2Zr4(H)2(thf)2}2(toluene)2(pentane) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C120 H144 O10 Zr4, 2(C7 H8), 2(C5 H12)' _chemical_formula_sum 'C144 H184 O10 Zr4' _chemical_formula_weight 2439.79 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 31.709(6) _cell_length_b 15.741(3) _cell_length_c 25.572(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12763(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 23515 _cell_measurement_theta_min 3.0062 _cell_measurement_theta_max 27.4662 _exptl_crystal_description Platelet _exptl_crystal_colour Brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5152 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9528 _exptl_absorpt_correction_T_max 0.9670 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Saturn CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 83954 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14603 _reflns_number_gt 12326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+24.9085P] 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 14603 _refine_ls_number_parameters 711 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2015 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.208 _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 Zr1 Zr 0.070125(14) 0.75762(3) 0.330954(16) 0.03082(13) Uani 1 1 d . A . Zr2 Zr 0.052981(13) 0.92892(3) 0.227734(15) 0.02778(12) Uani 1 1 d . . . H1 H 0.0755(16) 0.822(3) 0.263(2) 0.045(14) Uiso 1 1 d . . . O1 O 0.03425(10) 0.6517(2) 0.34661(12) 0.0356(7) Uani 1 1 d . . . O2 O 0.06277(10) 1.0464(2) 0.24924(11) 0.0324(7) Uani 1 1 d . . . O3 O 0.11850(10) 0.7389(2) 0.37989(12) 0.0367(7) Uani 1 1 d . . . O4 O 0.08887(10) 0.9325(2) 0.16501(11) 0.0325(7) Uani 1 1 d . . . C1 C 0.00306(14) 0.7993(3) 0.37124(15) 0.0292(9) Uani 1 1 d . . . C2 C 0.00333(14) 0.8269(3) 0.31640(16) 0.0288(9) Uani 1 1 d . . . H2 H -0.012(2) 0.789(4) 0.295(2) 0.069(19) Uiso 1 1 d . . . C3 C 0.00987(14) 0.9202(3) 0.30727(15) 0.0286(9) Uani 1 1 d . . . C4 C 0.04072(14) 0.9553(3) 0.33849(15) 0.0291(9) Uani 1 1 d . . . C5 C 0.06248(15) 0.8959(3) 0.37348(16) 0.0322(9) Uani 1 1 d . . . H3 H 0.0862(15) 0.918(3) 0.3943(18) 0.030(12) Uiso 1 1 d . . . C6 C 0.03435(15) 0.8363(3) 0.40057(16) 0.0309(9) Uani 1 1 d . . . H4 H 0.040(2) 0.823(4) 0.434(3) 0.08(2) Uiso 1 1 d . . . C7 C -0.00165(15) 0.6468(3) 0.37568(16) 0.0341(10) Uani 1 1 d . . . C8 C -0.01985(16) 0.5689(3) 0.39162(17) 0.0373(10) Uani 1 1 d . . . C9 C -0.05776(16) 0.5737(3) 0.41852(18) 0.0403(11) Uani 1 1 d . . . H5 H -0.0702 0.5222 0.4301 0.048 Uiso 1 1 calc R . . C10 C -0.07867(16) 0.6496(3) 0.42953(18) 0.0399(11) Uani 1 1 d . . . C11 C -0.05978(15) 0.7253(3) 0.41446(17) 0.0353(10) Uani 1 1 d . . . H6 H -0.0732 0.7780 0.4217 0.042 Uiso 1 1 calc R . . C12 C -0.02128(15) 0.7237(3) 0.38886(17) 0.0336(9) Uani 1 1 d . . . C13 C 0.06057(14) 1.0920(3) 0.29447(16) 0.0305(9) Uani 1 1 d . . . C14 C 0.05009(14) 1.0480(3) 0.34043(16) 0.0306(9) Uani 1 1 d . . . C15 C 0.04948(15) 1.0918(3) 0.38740(17) 0.0351(10) Uani 1 1 d . . . H7 H 0.0430 1.0623 0.4188 0.042 Uiso 1 1 calc R . . C16 C 0.05822(17) 1.1782(3) 0.38936(18) 0.0394(11) Uani 1 1 d . . . C17 C 0.06860(16) 1.2202(3) 0.34334(18) 0.0374(10) Uani 1 1 d . . . H8 H 0.0746 1.2793 0.3449 0.045 Uiso 1 1 calc R . . C18 C 0.07067(14) 1.1791(3) 0.29479(17) 0.0324(9) Uani 1 1 d . . . C19 C 0.00135(18) 0.4843(3) 0.3785(2) 0.0433(12) Uani 1 1 d . . . C20 C 0.0036(2) 0.4735(3) 0.3187(2) 0.0528(14) Uani 1 1 d . . . H9 H -0.0250 0.4686 0.3045 0.079 Uiso 1 1 calc R . . H10 H 0.0196 0.4220 0.3103 0.079 Uiso 1 1 calc R . . H11 H 0.0176 0.5229 0.3032 0.079 Uiso 1 1 calc R . . C21 C -0.0227(2) 0.4075(3) 0.4005(3) 0.0583(15) Uani 1 1 d . . . H12 H -0.0238 0.4114 0.4387 0.087 Uiso 1 1 calc R . . H13 H -0.0083 0.3551 0.3903 0.087 Uiso 1 1 calc R . . H14 H -0.0515 0.4072 0.3865 0.087 Uiso 1 1 calc R . . C22 C 0.04602(18) 0.4812(3) 0.4024(2) 0.0526(14) Uani 1 1 d . . . H15 H 0.0622 0.5307 0.3906 0.079 Uiso 1 1 calc R . . H16 H 0.0603 0.4291 0.3912 0.079 Uiso 1 1 calc R . . H17 H 0.0439 0.4820 0.4407 0.079 Uiso 1 1 calc R . . C23 C -0.12138(18) 0.6499(4) 0.4570(2) 0.0529(14) Uani 1 1 d . . . H18 H -0.1390 0.6043 0.4428 0.079 Uiso 1 1 calc R . . H19 H -0.1353 0.7047 0.4513 0.079 Uiso 1 1 calc R . . H20 H -0.1173 0.6409 0.4946 0.079 Uiso 1 1 calc R . . C24 C 0.08398(16) 1.2256(3) 0.24443(18) 0.0375(10) Uani 1 1 d . . . C25 C 0.04874(17) 1.2210(3) 0.2030(2) 0.0443(12) Uani 1 1 d . . . H21 H 0.0244 1.2542 0.2148 0.066 Uiso 1 1 calc R . . H22 H 0.0403 1.1617 0.1979 0.066 Uiso 1 1 calc R . . H23 H 0.0591 1.2443 0.1698 0.066 Uiso 1 1 calc R . . C26 C 0.12441(16) 1.1839(3) 0.22187(19) 0.0426(11) Uani 1 1 d . . . H24 H 0.1338 1.2158 0.1911 0.064 Uiso 1 1 calc R . . H25 H 0.1183 1.1251 0.2118 0.064 Uiso 1 1 calc R . . H26 H 0.1467 1.1845 0.2485 0.064 Uiso 1 1 calc R . . C27 C 0.09354(18) 1.3190(3) 0.2534(2) 0.0473(12) Uani 1 1 d . . . H27 H 0.0685 1.3472 0.2678 0.071 Uiso 1 1 calc R . . H28 H 0.1013 1.3457 0.2201 0.071 Uiso 1 1 calc R . . H29 H 0.1170 1.3244 0.2781 0.071 Uiso 1 1 calc R . . C28 C 0.0571(2) 1.2250(4) 0.4411(2) 0.0555(15) Uani 1 1 d . . . H30 H 0.0659 1.2840 0.4358 0.083 Uiso 1 1 calc R . . H31 H 0.0763 1.1973 0.4659 0.083 Uiso 1 1 calc R . . H32 H 0.0284 1.2238 0.4552 0.083 Uiso 1 1 calc R . . C29 C 0.16748(15) 0.8547(3) 0.32565(17) 0.0379(10) Uani 1 1 d . . . C30 C 0.15498(15) 0.9314(3) 0.30307(18) 0.0369(10) Uani 1 1 d . . . H33 H 0.1485 0.9787 0.3247 0.044 Uiso 1 1 calc R . . C31 C 0.15200(14) 0.9388(3) 0.24909(18) 0.0349(10) Uani 1 1 d . . . H34 H 0.1437 0.9915 0.2343 0.042 Uiso 1 1 calc R . . C32 C 0.16103(15) 0.8697(3) 0.21563(17) 0.0379(10) Uani 1 1 d . . . C33 C 0.17433(15) 0.7950(3) 0.23857(19) 0.0402(11) Uani 1 1 d . . . H35 H 0.1816 0.7480 0.2170 0.048 Uiso 1 1 calc R . . C34 C 0.17730(16) 0.7870(3) 0.29249(19) 0.0423(11) Uani 1 1 d . . . H36 H 0.1862 0.7346 0.3071 0.051 Uiso 1 1 calc R . . C35 C 0.14839(15) 0.7794(3) 0.40816(17) 0.0366(10) Uani 1 1 d . . . C36 C 0.15632(15) 0.7581(3) 0.46150(18) 0.0374(11) Uani 1 1 d . . . C37 C 0.18625(15) 0.8073(3) 0.48720(17) 0.0406(11) Uani 1 1 d . . . H37 H 0.1921 0.7947 0.5228 0.049 Uiso 1 1 calc R . . C38 C 0.20812(16) 0.8738(3) 0.46410(19) 0.0432(11) Uani 1 1 d . . . C39 C 0.20103(16) 0.8895(3) 0.41162(18) 0.0421(11) Uani 1 1 d . . . H38 H 0.2163 0.9335 0.3947 0.051 Uiso 1 1 calc R . . C40 C 0.17225(15) 0.8428(3) 0.38338(16) 0.0359(10) Uani 1 1 d . . . C41 C 0.12334(14) 0.9195(3) 0.13439(16) 0.0321(9) Uani 1 1 d . . . C42 C 0.15830(14) 0.8797(3) 0.15790(17) 0.0344(10) Uani 1 1 d . . . C43 C 0.19119(16) 0.8522(3) 0.12643(19) 0.0431(11) Uani 1 1 d . . . H39 H 0.2144 0.8234 0.1419 0.052 Uiso 1 1 calc R . . C44 C 0.19096(16) 0.8660(4) 0.07252(19) 0.0462(12) Uani 1 1 d . . . C45 C 0.15793(16) 0.9134(3) 0.05168(18) 0.0416(11) Uani 1 1 d . . . H40 H 0.1587 0.9267 0.0154 0.050 Uiso 1 1 calc R . . C46 C 0.12380(15) 0.9427(3) 0.08107(16) 0.0344(10) Uani 1 1 d . . . C47 C 0.13454(17) 0.6820(4) 0.48761(19) 0.0465(12) Uani 1 1 d . . . C48 C 0.08639(17) 0.6893(4) 0.4870(2) 0.0523(14) Uani 1 1 d . . . H41 H 0.0779 0.7419 0.5046 0.078 Uiso 1 1 calc R . . H42 H 0.0741 0.6405 0.5053 0.078 Uiso 1 1 calc R . . H43 H 0.0764 0.6900 0.4508 0.078 Uiso 1 1 calc R . . C49 C 0.14739(19) 0.6728(4) 0.5457(2) 0.0577(15) Uani 1 1 d . . . H44 H 0.1781 0.6681 0.5482 0.087 Uiso 1 1 calc R . . H45 H 0.1343 0.6217 0.5604 0.087 Uiso 1 1 calc R . . H46 H 0.1379 0.7228 0.5652 0.087 Uiso 1 1 calc R . . C50 C 0.1484(2) 0.6002(4) 0.4591(2) 0.0565(14) Uani 1 1 d . . . H47 H 0.1392 0.6027 0.4225 0.085 Uiso 1 1 calc R . . H48 H 0.1356 0.5508 0.4762 0.085 Uiso 1 1 calc R . . H49 H 0.1792 0.5953 0.4605 0.085 Uiso 1 1 calc R . . C51 C 0.23980(19) 0.9255(4) 0.4952(2) 0.0581(15) Uani 1 1 d . . . H50 H 0.2515 0.9704 0.4729 0.087 Uiso 1 1 calc R . . H51 H 0.2626 0.8884 0.5072 0.087 Uiso 1 1 calc R . . H52 H 0.2257 0.9512 0.5254 0.087 Uiso 1 1 calc R . . C52 C 0.09027(15) 1.0019(3) 0.05764(17) 0.0352(10) Uani 1 1 d . . . C53 C 0.08892(19) 1.0849(3) 0.08926(19) 0.0463(12) Uani 1 1 d . . . H53 H 0.1170 1.1108 0.0896 0.069 Uiso 1 1 calc R . . H54 H 0.0801 1.0726 0.1252 0.069 Uiso 1 1 calc R . . H55 H 0.0688 1.1242 0.0731 0.069 Uiso 1 1 calc R . . C54 C 0.04639(15) 0.9605(3) 0.05806(18) 0.0381(10) Uani 1 1 d . . . H56 H 0.0258 0.9998 0.0430 0.057 Uiso 1 1 calc R . . H57 H 0.0384 0.9471 0.0941 0.057 Uiso 1 1 calc R . . H58 H 0.0471 0.9081 0.0373 0.057 Uiso 1 1 calc R . . C55 C 0.10042(17) 1.0253(3) 0.00104(17) 0.0436(12) Uani 1 1 d . . . H59 H 0.1279 1.0538 -0.0004 0.065 Uiso 1 1 calc R . . H60 H 0.0786 1.0635 -0.0125 0.065 Uiso 1 1 calc R . . H61 H 0.1013 0.9736 -0.0203 0.065 Uiso 1 1 calc R . . C56 C 0.22590(19) 0.8329(5) 0.0383(2) 0.0627(17) Uani 1 1 d . . . H62 H 0.2414 0.8807 0.0231 0.094 Uiso 1 1 calc R . . H63 H 0.2139 0.7980 0.0103 0.094 Uiso 1 1 calc R . . H64 H 0.2452 0.7983 0.0594 0.094 Uiso 1 1 calc R . . O5 O 0.09878(11) 0.6637(2) 0.27404(12) 0.0403(8) Uani 1 1 d . . . C57 C 0.1238(5) 0.5925(8) 0.2959(5) 0.042(3) Uiso 0.54(2) 1 d P A 1 C58 C 0.1199(5) 0.5290(8) 0.2496(4) 0.056(4) Uiso 0.54(2) 1 d P A 1 C59 C 0.1137(5) 0.5738(9) 0.2008(5) 0.046(3) Uiso 0.54(2) 1 d P A 1 C60 C 0.0948(4) 0.6631(8) 0.2163(4) 0.037(3) Uiso 0.54(2) 1 d P A 1 C61 C 0.1129(5) 0.5789(8) 0.2916(5) 0.030(3) Uiso 0.46(2) 1 d P A 2 C62 C 0.1423(4) 0.5518(7) 0.2474(4) 0.038(4) Uiso 0.46(2) 1 d P A 2 C63 C 0.1237(5) 0.5897(10) 0.1984(5) 0.039(4) Uiso 0.46(2) 1 d P A 2 C64 C 0.0855(5) 0.6465(9) 0.2186(5) 0.036(3) Uiso 0.46(2) 1 d P A 2 C65 C 0.2562(6) 0.6209(12) 0.1463(8) 0.132(6) Uiso 0.708(12) 1 d PD B 1 C66 C 0.2374(3) 0.5314(7) 0.1690(4) 0.072(3) Uiso 0.708(12) 1 d PD B 1 C67 C 0.2500(4) 0.5110(9) 0.2177(5) 0.084(4) Uiso 0.708(12) 1 d PD B 1 C68 C 0.2378(4) 0.4332(7) 0.2437(4) 0.075(3) Uiso 0.708(12) 1 d PD B 1 C69 C 0.2120(3) 0.3780(6) 0.2164(4) 0.064(3) Uiso 0.708(12) 1 d PD B 1 C70 C 0.1969(4) 0.4023(8) 0.1656(5) 0.070(3) Uiso 0.708(12) 1 d PD B 1 C71 C 0.2094(3) 0.4739(8) 0.1430(4) 0.071(3) Uiso 0.708(12) 1 d PD B 1 C72 C 0.1994(11) 0.371(3) 0.1785(15) 0.103(12) Uiso 0.292(12) 1 d PD B 2 C73 C 0.2236(9) 0.470(2) 0.1814(14) 0.123(13) Uiso 0.292(12) 1 d PD B 2 C74 C 0.2189(8) 0.5178(17) 0.1372(10) 0.075(7) Uiso 0.292(12) 1 d PD B 2 C75 C 0.2372(9) 0.6055(16) 0.1395(10) 0.069(7) Uiso 0.292(12) 1 d PD B 2 C76 C 0.2585(12) 0.624(3) 0.1847(17) 0.158(19) Uiso 0.292(12) 1 d PD B 2 C77 C 0.2626(13) 0.577(3) 0.2313(17) 0.160(19) Uiso 0.292(12) 1 d PD B 2 C78 C 0.2426(11) 0.486(3) 0.2296(16) 0.125(17) Uiso 0.292(12) 1 d PD B 2 C79 C 0.1718(4) 0.3890(7) 0.3819(5) 0.123(4) Uiso 1 1 d D . . C80 C 0.1927(6) 0.3023(11) 0.3603(7) 0.205(7) Uiso 1 1 d D . . C81 C 0.1812(6) 0.2512(10) 0.4020(7) 0.185(6) Uiso 1 1 d D . . C82 C 0.1947(5) 0.1544(10) 0.3839(6) 0.180(6) Uiso 1 1 d D . . C83 C 0.2384(6) 0.1364(12) 0.3650(7) 0.205(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0320(3) 0.0349(2) 0.0255(2) 0.00294(16) 0.00089(16) 0.00381(17) Zr2 0.0283(2) 0.0336(2) 0.02149(19) 0.00042(15) 0.00039(15) -0.00048(17) O1 0.0354(18) 0.0352(16) 0.0361(16) 0.0012(13) 0.0047(13) 0.0030(14) O2 0.0371(18) 0.0382(16) 0.0218(14) 0.0007(12) 0.0011(12) -0.0006(13) O3 0.0348(18) 0.0450(18) 0.0303(16) 0.0046(13) 0.0003(13) 0.0033(14) O4 0.0298(16) 0.0429(18) 0.0249(14) 0.0017(12) 0.0009(12) 0.0023(13) C1 0.030(2) 0.033(2) 0.0241(19) 0.0023(16) 0.0052(16) 0.0045(18) C2 0.034(2) 0.032(2) 0.0212(18) -0.0031(16) -0.0006(16) -0.0006(18) C3 0.030(2) 0.034(2) 0.0217(18) 0.0025(16) 0.0009(16) 0.0022(17) C4 0.027(2) 0.036(2) 0.0234(18) 0.0012(16) 0.0018(16) 0.0015(18) C5 0.034(2) 0.037(2) 0.025(2) 0.0031(17) -0.0012(17) 0.0025(19) C6 0.036(2) 0.033(2) 0.024(2) 0.0038(16) -0.0012(17) 0.0026(18) C7 0.040(3) 0.038(2) 0.024(2) 0.0019(17) 0.0034(18) -0.003(2) C8 0.046(3) 0.036(2) 0.030(2) 0.0023(18) -0.001(2) -0.001(2) C9 0.049(3) 0.039(3) 0.033(2) 0.0057(19) 0.005(2) -0.011(2) C10 0.043(3) 0.046(3) 0.030(2) 0.0004(19) 0.008(2) -0.008(2) C11 0.040(3) 0.038(2) 0.028(2) -0.0019(18) 0.0028(18) -0.002(2) C12 0.036(3) 0.036(2) 0.028(2) 0.0015(17) -0.0032(18) -0.0027(19) C13 0.032(2) 0.035(2) 0.0240(19) -0.0017(16) -0.0012(16) 0.0006(18) C14 0.032(2) 0.034(2) 0.0256(19) -0.0002(16) -0.0015(17) -0.0021(18) C15 0.044(3) 0.036(2) 0.025(2) 0.0007(17) -0.0061(18) 0.001(2) C16 0.053(3) 0.035(2) 0.030(2) -0.0056(18) -0.006(2) 0.003(2) C17 0.049(3) 0.030(2) 0.033(2) 0.0003(18) -0.004(2) -0.003(2) C18 0.032(2) 0.035(2) 0.030(2) 0.0016(17) -0.0022(17) 0.0007(18) C19 0.053(3) 0.034(2) 0.043(3) 0.003(2) 0.008(2) 0.000(2) C20 0.069(4) 0.042(3) 0.047(3) -0.008(2) 0.009(3) 0.002(3) C21 0.066(4) 0.037(3) 0.072(4) 0.005(3) 0.009(3) 0.000(3) C22 0.056(4) 0.041(3) 0.061(3) 0.011(2) 0.002(3) 0.006(2) C23 0.053(3) 0.055(3) 0.051(3) -0.003(3) 0.018(3) -0.011(3) C24 0.043(3) 0.037(2) 0.033(2) 0.0045(18) 0.005(2) -0.001(2) C25 0.048(3) 0.046(3) 0.039(3) 0.008(2) 0.002(2) -0.001(2) C26 0.046(3) 0.042(3) 0.040(3) 0.004(2) 0.003(2) -0.004(2) C27 0.058(4) 0.036(3) 0.048(3) 0.004(2) 0.005(2) -0.007(2) C28 0.090(5) 0.045(3) 0.032(3) -0.007(2) -0.003(3) -0.002(3) C29 0.031(2) 0.053(3) 0.030(2) 0.008(2) -0.0019(18) 0.001(2) C30 0.032(2) 0.046(3) 0.033(2) 0.0030(19) -0.0014(18) 0.000(2) C31 0.031(2) 0.041(3) 0.032(2) 0.0037(18) -0.0004(18) 0.0013(19) C32 0.030(2) 0.053(3) 0.031(2) 0.005(2) 0.0012(18) 0.000(2) C33 0.034(3) 0.049(3) 0.038(2) 0.003(2) 0.0055(19) 0.005(2) C34 0.038(3) 0.051(3) 0.038(2) 0.009(2) 0.001(2) 0.006(2) C35 0.035(3) 0.046(3) 0.029(2) 0.0005(19) -0.0051(18) 0.009(2) C36 0.034(3) 0.047(3) 0.030(2) 0.0095(19) 0.0041(18) 0.013(2) C37 0.038(3) 0.057(3) 0.027(2) 0.008(2) -0.0027(19) 0.011(2) C38 0.041(3) 0.054(3) 0.035(2) 0.000(2) -0.002(2) 0.006(2) C39 0.037(3) 0.054(3) 0.035(2) 0.003(2) 0.000(2) 0.003(2) C40 0.035(3) 0.049(3) 0.024(2) 0.0046(18) -0.0011(17) 0.003(2) C41 0.032(2) 0.038(2) 0.027(2) -0.0011(17) 0.0055(17) -0.0026(18) C42 0.032(2) 0.042(2) 0.029(2) 0.0030(18) 0.0027(17) 0.000(2) C43 0.035(3) 0.055(3) 0.039(3) 0.004(2) 0.002(2) 0.006(2) C44 0.039(3) 0.064(3) 0.035(2) 0.000(2) 0.008(2) 0.002(2) C45 0.038(3) 0.059(3) 0.028(2) 0.002(2) 0.0048(19) -0.001(2) C46 0.033(2) 0.044(3) 0.026(2) 0.0034(18) -0.0019(17) -0.005(2) C47 0.045(3) 0.057(3) 0.037(3) 0.009(2) -0.002(2) 0.011(2) C48 0.046(3) 0.073(4) 0.038(3) 0.018(3) -0.001(2) 0.004(3) C49 0.051(3) 0.080(4) 0.042(3) 0.020(3) -0.003(2) 0.007(3) C50 0.063(4) 0.049(3) 0.057(3) 0.011(3) -0.001(3) 0.008(3) C51 0.052(4) 0.077(4) 0.045(3) -0.004(3) -0.009(3) -0.003(3) C52 0.038(3) 0.041(2) 0.026(2) 0.0050(18) 0.0009(18) -0.005(2) C53 0.065(4) 0.043(3) 0.031(2) 0.000(2) -0.003(2) -0.003(2) C54 0.036(3) 0.046(3) 0.032(2) 0.005(2) -0.0009(19) -0.001(2) C55 0.049(3) 0.057(3) 0.025(2) 0.009(2) -0.0008(19) -0.005(2) C56 0.049(3) 0.097(5) 0.043(3) 0.009(3) 0.015(3) 0.021(3) O5 0.049(2) 0.0409(18) 0.0314(16) 0.0016(13) 0.0046(14) 0.0119(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O3 2.001(3) . ? Zr1 O1 2.058(3) . ? Zr1 O5 2.265(3) . ? Zr1 C2 2.411(4) . ? Zr1 C5 2.445(5) . ? Zr1 C6 2.447(4) . ? Zr1 C1 2.452(4) . ? Zr1 H1 2.02(5) . ? Zr2 O2 1.954(3) . ? Zr2 O4 1.967(3) . ? Zr2 C3 2.189(4) 4 ? Zr2 C3 2.454(4) . ? Zr2 C2 2.654(4) 4 ? Zr2 Zr2 3.5477(10) 4 ? Zr2 H1 2.03(5) . ? O1 C7 1.362(5) . ? O2 C13 1.363(5) . ? O3 C35 1.351(6) . ? O4 C41 1.360(5) . ? C1 C6 1.374(6) . ? C1 C2 1.468(5) . ? C1 C12 1.488(6) . ? C2 C3 1.502(6) . ? C2 Zr2 2.654(4) 4 ? C2 H2 0.95(7) . ? C3 C4 1.378(6) . ? C3 Zr2 2.189(4) 4 ? C4 C5 1.467(6) . ? C4 C14 1.491(6) . ? C5 C6 1.468(6) . ? C5 H3 0.98(5) . ? C6 H4 0.89(7) . ? C7 C12 1.403(6) . ? C7 C8 1.414(6) . ? C8 C9 1.387(7) . ? C8 C19 1.529(7) . ? C9 C10 1.394(7) . ? C9 H5 0.9500 . ? C10 C11 1.389(7) . ? C10 C23 1.526(7) . ? C11 C12 1.385(6) . ? C11 H6 0.9500 . ? C13 C14 1.404(6) . ? C13 C18 1.409(6) . ? C14 C15 1.385(6) . ? C15 C16 1.388(6) . ? C15 H7 0.9500 . ? C16 C17 1.389(7) . ? C16 C28 1.516(6) . ? C17 C18 1.401(6) . ? C17 H8 0.9500 . ? C18 C24 1.540(6) . ? C19 C21 1.536(7) . ? C19 C20 1.540(7) . ? C19 C22 1.544(8) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 H18 0.9800 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C24 C27 1.518(7) . ? C24 C25 1.542(7) . ? C24 C26 1.551(7) . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? C29 C30 1.395(7) . ? C29 C34 1.397(7) . ? C29 C40 1.496(6) . ? C30 C31 1.389(6) . ? C30 H33 0.9500 . ? C31 C32 1.412(7) . ? C31 H34 0.9500 . ? C32 C33 1.381(7) . ? C32 C42 1.487(6) . ? C33 C34 1.388(7) . ? C33 H35 0.9500 . ? C34 H36 0.9500 . ? C35 C40 1.404(7) . ? C35 C36 1.427(6) . ? C36 C37 1.390(7) . ? C36 C47 1.536(7) . ? C37 C38 1.387(7) . ? C37 H37 0.9500 . ? C38 C39 1.383(7) . ? C38 C51 1.518(7) . ? C39 C40 1.377(7) . ? C39 H38 0.9500 . ? C41 C42 1.408(6) . ? C41 C46 1.412(6) . ? C42 C43 1.387(7) . ? C43 C44 1.395(7) . ? C43 H39 0.9500 . ? C44 C45 1.393(7) . ? C44 C56 1.505(7) . ? C45 C46 1.396(7) . ? C45 H40 0.9500 . ? C46 C52 1.536(7) . ? C47 C48 1.531(8) . ? C47 C50 1.543(8) . ? C47 C49 1.546(7) . ? C48 H41 0.9800 . ? C48 H42 0.9800 . ? C48 H43 0.9800 . ? C49 H44 0.9800 . ? C49 H45 0.9800 . ? C49 H46 0.9800 . ? C50 H47 0.9800 . ? C50 H48 0.9800 . ? C50 H49 0.9800 . ? C51 H50 0.9800 . ? C51 H51 0.9800 . ? C51 H52 0.9800 . ? C52 C55 1.528(6) . ? C52 C53 1.537(7) . ? C52 C54 1.537(6) . ? C53 H53 0.9800 . ? C53 H54 0.9800 . ? C53 H55 0.9800 . ? C54 H56 0.9800 . ? C54 H57 0.9800 . ? C54 H58 0.9800 . ? C55 H59 0.9800 . ? C55 H60 0.9800 . ? C55 H61 0.9800 . ? C56 H62 0.9800 . ? C56 H63 0.9800 . ? C56 H64 0.9800 . ? O5 C61 1.478(12) . ? O5 C60 1.482(11) . ? O5 C57 1.483(12) . ? O5 C64 1.503(13) . ? C57 C58 1.556(18) . ? C58 C59 1.445(17) . ? C59 C60 1.579(17) . ? C61 C62 1.525(17) . ? C62 C63 1.508(17) . ? C63 C64 1.59(2) . ? C65 C66 1.64(2) . ? C66 C67 1.345(16) . ? C66 C71 1.433(16) . ? C67 C68 1.447(19) . ? C68 C69 1.381(14) . ? C69 C70 1.439(16) . ? C70 C71 1.326(16) . ? C72 C73 1.73(5) . ? C73 C74 1.37(4) . ? C73 C78 1.40(4) . ? C74 C75 1.50(3) . ? C75 C76 1.37(5) . ? C76 C77 1.41(5) . ? C77 C78 1.58(5) . ? C79 C80 1.614(14) . ? C80 C81 1.386(15) . ? C81 C82 1.649(14) . ? C82 C83 1.50(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 O3 Zr1 O1 100.54(13) . . ? O3 Zr1 O5 89.90(13) . . ? O1 Zr1 O5 79.51(12) . . ? O3 Zr1 C2 146.76(13) . . ? O1 Zr1 C2 84.89(14) . . ? O5 Zr1 C2 123.26(13) . . ? O3 Zr1 C5 85.92(14) . . ? O1 Zr1 C5 125.44(14) . . ? O5 Zr1 C5 155.04(14) . . ? C2 Zr1 C5 65.11(15) . . ? O3 Zr1 C6 88.56(14) . . ? O1 Zr1 C6 90.70(14) . . ? O5 Zr1 C6 169.64(13) . . ? C2 Zr1 C6 58.42(14) . . ? C5 Zr1 C6 34.92(15) . . ? O3 Zr1 C1 116.19(13) . . ? O1 Zr1 C1 69.85(13) . . ? O5 Zr1 C1 142.41(14) . . ? C2 Zr1 C1 35.13(13) . . ? C5 Zr1 C1 59.28(15) . . ? C6 Zr1 C1 32.56(15) . . ? O3 Zr1 H1 123.2(14) . . ? O1 Zr1 H1 128.4(15) . . ? O5 Zr1 H1 75.0(15) . . ? C2 Zr1 H1 73.4(14) . . ? C5 Zr1 H1 86.8(15) . . ? C6 Zr1 H1 114.3(15) . . ? C1 Zr1 H1 107.5(14) . . ? O2 Zr2 O4 96.32(13) . . ? O2 Zr2 C3 108.58(14) . 4 ? O4 Zr2 C3 101.25(14) . 4 ? O2 Zr2 C3 84.71(13) . . ? O4 Zr2 C3 177.89(13) . . ? C3 Zr2 C3 80.11(15) 4 . ? O2 Zr2 C2 143.06(13) . 4 ? O4 Zr2 C2 93.45(13) . 4 ? C3 Zr2 C2 34.48(14) 4 4 ? C3 Zr2 C2 86.79(14) . 4 ? O2 Zr2 Zr2 93.44(9) . 4 ? O4 Zr2 Zr2 144.05(9) . 4 ? C3 Zr2 Zr2 43.03(10) 4 4 ? C3 Zr2 Zr2 37.49(10) . 4 ? C2 Zr2 Zr2 59.95(9) 4 4 ? O2 Zr2 H1 127.0(15) . . ? O4 Zr2 H1 100.4(15) . . ? C3 Zr2 H1 116.6(14) 4 . ? C3 Zr2 H1 77.5(15) . . ? C2 Zr2 H1 85.6(14) 4 . ? Zr2 Zr2 H1 101.0(14) 4 . ? C7 O1 Zr1 127.9(3) . . ? C13 O2 Zr2 136.8(3) . . ? C35 O3 Zr1 143.4(3) . . ? C41 O4 Zr2 158.4(3) . . ? C6 C1 C2 113.1(4) . . ? C6 C1 C12 123.3(4) . . ? C2 C1 C12 121.9(4) . . ? C6 C1 Zr1 73.5(3) . . ? C2 C1 Zr1 70.9(2) . . ? C12 C1 Zr1 111.3(3) . . ? C1 C2 C3 116.0(3) . . ? C1 C2 Zr1 74.0(2) . . ? C3 C2 Zr1 110.2(3) . . ? C1 C2 Zr2 125.6(3) . 4 ? C3 C2 Zr2 55.6(2) . 4 ? Zr1 C2 Zr2 158.51(19) . 4 ? C1 C2 H2 111(4) . . ? C3 C2 H2 127(4) . . ? Zr1 C2 H2 105(4) . . ? Zr2 C2 H2 78(4) 4 . ? C4 C3 C2 113.5(4) . . ? C4 C3 Zr2 149.1(3) . 4 ? C2 C3 Zr2 89.9(3) . 4 ? C4 C3 Zr2 93.6(3) . . ? C2 C3 Zr2 105.1(3) . . ? Zr2 C3 Zr2 99.49(15) 4 . ? C3 C4 C5 115.6(4) . . ? C3 C4 C14 123.5(4) . . ? C5 C4 C14 120.7(4) . . ? C4 C5 C6 114.2(4) . . ? C4 C5 Zr1 110.0(3) . . ? C6 C5 Zr1 72.6(3) . . ? C4 C5 H3 118(3) . . ? C6 C5 H3 116(3) . . ? Zr1 C5 H3 118(3) . . ? C1 C6 C5 116.9(4) . . ? C1 C6 Zr1 73.9(2) . . ? C5 C6 Zr1 72.4(2) . . ? C1 C6 H4 124(4) . . ? C5 C6 H4 119(4) . . ? Zr1 C6 H4 119(4) . . ? O1 C7 C12 116.9(4) . . ? O1 C7 C8 123.2(4) . . ? C12 C7 C8 119.8(4) . . ? C9 C8 C7 116.7(4) . . ? C9 C8 C19 122.5(4) . . ? C7 C8 C19 120.8(4) . . ? C8 C9 C10 124.0(4) . . ? C8 C9 H5 118.0 . . ? C10 C9 H5 118.0 . . ? C11 C10 C9 118.3(4) . . ? C11 C10 C23 120.5(5) . . ? C9 C10 C23 121.2(4) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H6 120.2 . . ? C10 C11 H6 120.2 . . ? C11 C12 C7 121.4(4) . . ? C11 C12 C1 125.8(4) . . ? C7 C12 C1 112.8(4) . . ? O2 C13 C14 117.6(4) . . ? O2 C13 C18 120.4(4) . . ? C14 C13 C18 121.9(4) . . ? C15 C14 C13 118.9(4) . . ? C15 C14 C4 120.9(4) . . ? C13 C14 C4 120.1(4) . . ? C14 C15 C16 121.1(4) . . ? C14 C15 H7 119.5 . . ? C16 C15 H7 119.5 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 C28 120.2(4) . . ? C17 C16 C28 120.9(4) . . ? C16 C17 C18 122.8(4) . . ? C16 C17 H8 118.6 . . ? C18 C17 H8 118.6 . . ? C17 C18 C13 116.3(4) . . ? C17 C18 C24 122.3(4) . . ? C13 C18 C24 121.3(4) . . ? C8 C19 C21 112.7(4) . . ? C8 C19 C20 109.6(4) . . ? C21 C19 C20 107.4(5) . . ? C8 C19 C22 110.1(4) . . ? C21 C19 C22 106.6(4) . . ? C20 C19 C22 110.4(5) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C10 C23 H18 109.5 . . ? C10 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? C10 C23 H20 109.5 . . ? H18 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C27 C24 C18 112.8(4) . . ? C27 C24 C25 107.1(4) . . ? C18 C24 C25 110.8(4) . . ? C27 C24 C26 107.5(4) . . ? C18 C24 C26 109.7(4) . . ? C25 C24 C26 108.9(4) . . ? C24 C25 H21 109.5 . . ? C24 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C26 H24 109.5 . . ? C24 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C24 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C16 C28 H30 109.5 . . ? C16 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C16 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C30 C29 C34 118.2(4) . . ? C30 C29 C40 123.1(5) . . ? C34 C29 C40 118.7(4) . . ? C31 C30 C29 120.2(5) . . ? C31 C30 H33 119.9 . . ? C29 C30 H33 119.9 . . ? C30 C31 C32 121.6(4) . . ? C30 C31 H34 119.2 . . ? C32 C31 H34 119.2 . . ? C33 C32 C31 117.4(4) . . ? C33 C32 C42 122.0(5) . . ? C31 C32 C42 120.5(4) . . ? C32 C33 C34 121.3(5) . . ? C32 C33 H35 119.4 . . ? C34 C33 H35 119.4 . . ? C33 C34 C29 121.3(5) . . ? C33 C34 H36 119.4 . . ? C29 C34 H36 119.4 . . ? O3 C35 C40 118.1(4) . . ? O3 C35 C36 121.7(4) . . ? C40 C35 C36 120.2(4) . . ? C37 C36 C35 116.2(4) . . ? C37 C36 C47 122.4(4) . . ? C35 C36 C47 121.3(5) . . ? C38 C37 C36 124.1(4) . . ? C38 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? C39 C38 C37 117.8(5) . . ? C39 C38 C51 121.3(5) . . ? C37 C38 C51 120.8(5) . . ? C40 C39 C38 121.4(5) . . ? C40 C39 H38 119.3 . . ? C38 C39 H38 119.3 . . ? C39 C40 C35 120.0(4) . . ? C39 C40 C29 121.2(4) . . ? C35 C40 C29 118.7(4) . . ? O4 C41 C42 117.0(4) . . ? O4 C41 C46 121.7(4) . . ? C42 C41 C46 121.3(4) . . ? C43 C42 C41 118.9(4) . . ? C43 C42 C32 120.0(4) . . ? C41 C42 C32 121.1(4) . . ? C42 C43 C44 121.4(5) . . ? C42 C43 H39 119.3 . . ? C44 C43 H39 119.3 . . ? C45 C44 C43 117.7(4) . . ? C45 C44 C56 121.2(5) . . ? C43 C44 C56 121.1(5) . . ? C44 C45 C46 123.6(4) . . ? C44 C45 H40 118.2 . . ? C46 C45 H40 118.2 . . ? C45 C46 C41 116.3(4) . . ? C45 C46 C52 121.8(4) . . ? C41 C46 C52 121.8(4) . . ? C48 C47 C36 112.7(4) . . ? C48 C47 C50 110.0(5) . . ? C36 C47 C50 108.5(4) . . ? C48 C47 C49 106.2(4) . . ? C36 C47 C49 111.8(5) . . ? C50 C47 C49 107.5(5) . . ? C47 C48 H41 109.5 . . ? C47 C48 H42 109.5 . . ? H41 C48 H42 109.5 . . ? C47 C48 H43 109.5 . . ? H41 C48 H43 109.5 . . ? H42 C48 H43 109.5 . . ? C47 C49 H44 109.5 . . ? C47 C49 H45 109.5 . . ? H44 C49 H45 109.5 . . ? C47 C49 H46 109.5 . . ? H44 C49 H46 109.5 . . ? H45 C49 H46 109.5 . . ? C47 C50 H47 109.5 . . ? C47 C50 H48 109.5 . . ? H47 C50 H48 109.5 . . ? C47 C50 H49 109.5 . . ? H47 C50 H49 109.5 . . ? H48 C50 H49 109.5 . . ? C38 C51 H50 109.5 . . ? C38 C51 H51 109.5 . . ? H50 C51 H51 109.5 . . ? C38 C51 H52 109.5 . . ? H50 C51 H52 109.5 . . ? H51 C51 H52 109.5 . . ? C55 C52 C46 111.7(4) . . ? C55 C52 C53 107.4(4) . . ? C46 C52 C53 109.3(4) . . ? C55 C52 C54 107.4(4) . . ? C46 C52 C54 111.5(4) . . ? C53 C52 C54 109.4(4) . . ? C52 C53 H53 109.5 . . ? C52 C53 H54 109.5 . . ? H53 C53 H54 109.5 . . ? C52 C53 H55 109.5 . . ? H53 C53 H55 109.5 . . ? H54 C53 H55 109.5 . . ? C52 C54 H56 109.5 . . ? C52 C54 H57 109.5 . . ? H56 C54 H57 109.5 . . ? C52 C54 H58 109.5 . . ? H56 C54 H58 109.5 . . ? H57 C54 H58 109.5 . . ? C52 C55 H59 109.5 . . ? C52 C55 H60 109.5 . . ? H59 C55 H60 109.5 . . ? C52 C55 H61 109.5 . . ? H59 C55 H61 109.5 . . ? H60 C55 H61 109.5 . . ? C44 C56 H62 109.5 . . ? C44 C56 H63 109.5 . . ? H62 C56 H63 109.5 . . ? C44 C56 H64 109.5 . . ? H62 C56 H64 109.5 . . ? H63 C56 H64 109.5 . . ? C61 O5 C60 108.8(7) . . ? C60 O5 C57 114.6(7) . . ? C61 O5 C64 102.0(8) . . ? C57 O5 C64 111.6(8) . . ? C61 O5 Zr1 121.1(5) . . ? C60 O5 Zr1 127.7(5) . . ? C57 O5 Zr1 117.8(5) . . ? C64 O5 Zr1 127.7(5) . . ? O5 C57 C58 99.0(9) . . ? C59 C58 C57 110.8(10) . . ? C58 C59 C60 105.6(10) . . ? O5 C60 C59 102.9(8) . . ? O5 C61 C62 102.3(8) . . ? C63 C62 C61 105.4(10) . . ? C62 C63 C64 104.4(10) . . ? O5 C64 C63 101.3(10) . . ? C67 C66 C71 117.6(11) . . ? C67 C66 C65 115.2(12) . . ? C71 C66 C65 127.2(12) . . ? C66 C67 C68 123.2(12) . . ? C69 C68 C67 117.4(10) . . ? C68 C69 C70 119.1(10) . . ? C71 C70 C69 121.3(11) . . ? C70 C71 C66 121.3(11) . . ? C74 C73 C78 132(3) . . ? C74 C73 C72 114(3) . . ? C78 C73 C72 113(3) . . ? C73 C74 C75 116(3) . . ? C76 C75 C74 115(2) . . ? C75 C76 C77 130(3) . . ? C76 C77 C78 115(3) . . ? C73 C78 C77 111(3) . . ? C81 C80 C79 96.9(13) . . ? C80 C81 C82 104.6(14) . . ? C83 C82 C81 120.4(15) . . ? 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 O3 Zr1 O1 C7 103.3(3) . . . . ? O5 Zr1 O1 C7 -168.8(4) . . . . ? C2 Zr1 O1 C7 -43.6(3) . . . . ? C5 Zr1 O1 C7 10.8(4) . . . . ? C6 Zr1 O1 C7 14.6(4) . . . . ? C1 Zr1 O1 C7 -10.9(3) . . . . ? O4 Zr2 O2 C13 -156.9(4) . . . . ? C3 Zr2 O2 C13 99.0(4) 4 . . . ? C3 Zr2 O2 C13 21.3(4) . . . . ? C2 Zr2 O2 C13 98.7(4) 4 . . . ? Zr2 Zr2 O2 C13 57.8(4) 4 . . . ? O1 Zr1 O3 C35 -152.2(5) . . . . ? O5 Zr1 O3 C35 128.5(5) . . . . ? C2 Zr1 O3 C35 -55.4(6) . . . . ? C5 Zr1 O3 C35 -26.9(5) . . . . ? C6 Zr1 O3 C35 -61.7(5) . . . . ? C1 Zr1 O3 C35 -79.6(5) . . . . ? O2 Zr2 O4 C41 101.9(8) . . . . ? C3 Zr2 O4 C41 -147.7(8) 4 . . . ? C2 Zr2 O4 C41 -113.8(8) 4 . . . ? Zr2 Zr2 O4 C41 -153.3(7) 4 . . . ? O3 Zr1 C1 C6 34.7(3) . . . . ? O1 Zr1 C1 C6 126.8(3) . . . . ? O5 Zr1 C1 C6 164.2(2) . . . . ? C2 Zr1 C1 C6 -122.3(4) . . . . ? C5 Zr1 C1 C6 -32.7(2) . . . . ? O3 Zr1 C1 C2 157.0(2) . . . . ? O1 Zr1 C1 C2 -110.9(3) . . . . ? O5 Zr1 C1 C2 -73.5(3) . . . . ? C5 Zr1 C1 C2 89.6(3) . . . . ? C6 Zr1 C1 C2 122.3(4) . . . . ? O3 Zr1 C1 C12 -85.2(3) . . . . ? O1 Zr1 C1 C12 6.9(3) . . . . ? O5 Zr1 C1 C12 44.3(4) . . . . ? C2 Zr1 C1 C12 117.8(4) . . . . ? C5 Zr1 C1 C12 -152.6(3) . . . . ? C6 Zr1 C1 C12 -119.9(4) . . . . ? C6 C1 C2 C3 -43.3(5) . . . . ? C12 C1 C2 C3 151.3(4) . . . . ? Zr1 C1 C2 C3 -105.0(4) . . . . ? C6 C1 C2 Zr1 61.7(3) . . . . ? C12 C1 C2 Zr1 -103.7(4) . . . . ? C6 C1 C2 Zr2 -108.2(4) . . . 4 ? C12 C1 C2 Zr2 86.3(5) . . . 4 ? Zr1 C1 C2 Zr2 -169.9(3) . . . 4 ? O3 Zr1 C2 C1 -39.7(4) . . . . ? O1 Zr1 C2 C1 61.7(2) . . . . ? O5 Zr1 C2 C1 135.6(2) . . . . ? C5 Zr1 C2 C1 -71.4(2) . . . . ? C6 Zr1 C2 C1 -32.3(2) . . . . ? O3 Zr1 C2 C3 72.7(4) . . . . ? O1 Zr1 C2 C3 174.1(3) . . . . ? O5 Zr1 C2 C3 -112.0(3) . . . . ? C5 Zr1 C2 C3 41.0(3) . . . . ? C6 Zr1 C2 C3 80.1(3) . . . . ? C1 Zr1 C2 C3 112.4(4) . . . . ? O3 Zr1 C2 Zr2 117.4(5) . . . 4 ? O1 Zr1 C2 Zr2 -141.1(5) . . . 4 ? O5 Zr1 C2 Zr2 -67.2(6) . . . 4 ? C5 Zr1 C2 Zr2 85.8(5) . . . 4 ? C6 Zr1 C2 Zr2 124.9(6) . . . 4 ? C1 Zr1 C2 Zr2 157.1(7) . . . 4 ? C1 C2 C3 C4 42.6(5) . . . . ? Zr1 C2 C3 C4 -38.9(4) . . . . ? Zr2 C2 C3 C4 159.4(4) 4 . . . ? C1 C2 C3 Zr2 -116.7(4) . . . 4 ? Zr1 C2 C3 Zr2 161.78(17) . . . 4 ? C1 C2 C3 Zr2 143.5(3) . . . . ? Zr1 C2 C3 Zr2 62.0(3) . . . . ? Zr2 C2 C3 Zr2 -99.81(19) 4 . . . ? O2 Zr2 C3 C4 -49.3(3) . . . . ? C3 Zr2 C3 C4 -159.2(2) 4 . . . ? C2 Zr2 C3 C4 166.7(3) 4 . . . ? Zr2 Zr2 C3 C4 -151.9(4) 4 . . . ? O2 Zr2 C3 C2 -164.8(3) . . . . ? C3 Zr2 C3 C2 85.3(3) 4 . . . ? C2 Zr2 C3 C2 51.2(3) 4 . . . ? Zr2 Zr2 C3 C2 92.5(3) 4 . . . ? O2 Zr2 C3 Zr2 102.69(16) . . . 4 ? C3 Zr2 C3 Zr2 -7.2(2) 4 . . 4 ? C2 Zr2 C3 Zr2 -41.32(16) 4 . . 4 ? C2 C3 C4 C5 1.9(5) . . . . ? Zr2 C3 C4 C5 138.5(5) 4 . . . ? Zr2 C3 C4 C5 -106.3(3) . . . . ? C2 C3 C4 C14 -173.8(4) . . . . ? Zr2 C3 C4 C14 -37.3(8) 4 . . . ? Zr2 C3 C4 C14 78.0(4) . . . . ? C3 C4 C5 C6 -44.1(5) . . . . ? C14 C4 C5 C6 131.7(4) . . . . ? C3 C4 C5 Zr1 35.2(4) . . . . ? C14 C4 C5 Zr1 -148.9(3) . . . . ? O3 Zr1 C5 C4 156.6(3) . . . . ? O1 Zr1 C5 C4 -103.3(3) . . . . ? O5 Zr1 C5 C4 75.7(5) . . . . ? C2 Zr1 C5 C4 -40.1(3) . . . . ? C6 Zr1 C5 C4 -110.0(4) . . . . ? C1 Zr1 C5 C4 -79.5(3) . . . . ? O3 Zr1 C5 C6 -93.3(3) . . . . ? O1 Zr1 C5 C6 6.7(3) . . . . ? O5 Zr1 C5 C6 -174.3(3) . . . . ? C2 Zr1 C5 C6 69.9(3) . . . . ? C1 Zr1 C5 C6 30.5(2) . . . . ? C2 C1 C6 C5 -0.1(6) . . . . ? C12 C1 C6 C5 165.1(4) . . . . ? Zr1 C1 C6 C5 60.1(4) . . . . ? C2 C1 C6 Zr1 -60.2(3) . . . . ? C12 C1 C6 Zr1 105.0(4) . . . . ? C4 C5 C6 C1 43.8(6) . . . . ? Zr1 C5 C6 C1 -60.9(4) . . . . ? C4 C5 C6 Zr1 104.7(4) . . . . ? O3 Zr1 C6 C1 -149.3(3) . . . . ? O1 Zr1 C6 C1 -48.8(3) . . . . ? O5 Zr1 C6 C1 -67.7(8) . . . . ? C2 Zr1 C6 C1 34.8(2) . . . . ? C5 Zr1 C6 C1 125.8(4) . . . . ? O3 Zr1 C6 C5 84.9(3) . . . . ? O1 Zr1 C6 C5 -174.5(3) . . . . ? O5 Zr1 C6 C5 166.5(7) . . . . ? C2 Zr1 C6 C5 -91.0(3) . . . . ? C1 Zr1 C6 C5 -125.8(4) . . . . ? Zr1 O1 C7 C12 12.9(6) . . . . ? Zr1 O1 C7 C8 -168.6(3) . . . . ? O1 C7 C8 C9 -176.4(4) . . . . ? C12 C7 C8 C9 2.1(7) . . . . ? O1 C7 C8 C19 2.5(7) . . . . ? C12 C7 C8 C19 -179.0(4) . . . . ? C7 C8 C9 C10 1.2(7) . . . . ? C19 C8 C9 C10 -177.7(5) . . . . ? C8 C9 C10 C11 -2.5(8) . . . . ? C8 C9 C10 C23 177.0(5) . . . . ? C9 C10 C11 C12 0.4(7) . . . . ? C23 C10 C11 C12 -179.0(4) . . . . ? C10 C11 C12 C7 2.8(7) . . . . ? C10 C11 C12 C1 -178.9(4) . . . . ? O1 C7 C12 C11 174.4(4) . . . . ? C8 C7 C12 C11 -4.2(7) . . . . ? O1 C7 C12 C1 -4.1(6) . . . . ? C8 C7 C12 C1 177.3(4) . . . . ? C6 C1 C12 C11 94.2(6) . . . . ? C2 C1 C12 C11 -101.8(5) . . . . ? Zr1 C1 C12 C11 178.0(4) . . . . ? C6 C1 C12 C7 -87.4(5) . . . . ? C2 C1 C12 C7 76.6(5) . . . . ? Zr1 C1 C12 C7 -3.6(4) . . . . ? Zr2 O2 C13 C14 2.7(6) . . . . ? Zr2 O2 C13 C18 179.6(3) . . . . ? O2 C13 C14 C15 177.1(4) . . . . ? C18 C13 C14 C15 0.3(7) . . . . ? O2 C13 C14 C4 -1.6(6) . . . . ? C18 C13 C14 C4 -178.4(4) . . . . ? C3 C4 C14 C15 124.8(5) . . . . ? C5 C4 C14 C15 -50.7(6) . . . . ? C3 C4 C14 C13 -56.5(6) . . . . ? C5 C4 C14 C13 128.0(5) . . . . ? C13 C14 C15 C16 1.3(7) . . . . ? C4 C14 C15 C16 179.9(4) . . . . ? C14 C15 C16 C17 -1.4(7) . . . . ? C14 C15 C16 C28 179.6(5) . . . . ? C15 C16 C17 C18 0.0(8) . . . . ? C28 C16 C17 C18 178.9(5) . . . . ? C16 C17 C18 C13 1.5(7) . . . . ? C16 C17 C18 C24 -177.4(5) . . . . ? O2 C13 C18 C17 -178.3(4) . . . . ? C14 C13 C18 C17 -1.6(7) . . . . ? O2 C13 C18 C24 0.6(7) . . . . ? C14 C13 C18 C24 177.3(4) . . . . ? C9 C8 C19 C21 -2.8(7) . . . . ? C7 C8 C19 C21 178.5(5) . . . . ? C9 C8 C19 C20 116.8(5) . . . . ? C7 C8 C19 C20 -62.0(6) . . . . ? C9 C8 C19 C22 -121.6(5) . . . . ? C7 C8 C19 C22 59.6(6) . . . . ? C17 C18 C24 C27 -1.0(7) . . . . ? C13 C18 C24 C27 -179.9(4) . . . . ? C17 C18 C24 C25 -121.0(5) . . . . ? C13 C18 C24 C25 60.1(6) . . . . ? C17 C18 C24 C26 118.8(5) . . . . ? C13 C18 C24 C26 -60.1(6) . . . . ? C34 C29 C30 C31 0.8(7) . . . . ? C40 C29 C30 C31 178.7(4) . . . . ? C29 C30 C31 C32 0.6(7) . . . . ? C30 C31 C32 C33 -2.1(7) . . . . ? C30 C31 C32 C42 -178.9(4) . . . . ? C31 C32 C33 C34 2.2(7) . . . . ? C42 C32 C33 C34 179.0(5) . . . . ? C32 C33 C34 C29 -0.8(8) . . . . ? C30 C29 C34 C33 -0.7(7) . . . . ? C40 C29 C34 C33 -178.7(5) . . . . ? Zr1 O3 C35 C40 -48.0(7) . . . . ? Zr1 O3 C35 C36 133.0(4) . . . . ? O3 C35 C36 C37 -176.6(4) . . . . ? C40 C35 C36 C37 4.3(7) . . . . ? O3 C35 C36 C47 6.6(7) . . . . ? C40 C35 C36 C47 -172.5(4) . . . . ? C35 C36 C37 C38 -0.2(7) . . . . ? C47 C36 C37 C38 176.6(5) . . . . ? C36 C37 C38 C39 -3.0(8) . . . . ? C36 C37 C38 C51 178.9(5) . . . . ? C37 C38 C39 C40 2.1(8) . . . . ? C51 C38 C39 C40 -179.9(5) . . . . ? C38 C39 C40 C35 2.0(8) . . . . ? C38 C39 C40 C29 -174.5(5) . . . . ? O3 C35 C40 C39 175.6(4) . . . . ? C36 C35 C40 C39 -5.3(7) . . . . ? O3 C35 C40 C29 -7.8(7) . . . . ? C36 C35 C40 C29 171.2(4) . . . . ? C30 C29 C40 C39 -61.8(7) . . . . ? C34 C29 C40 C39 116.1(6) . . . . ? C30 C29 C40 C35 121.7(5) . . . . ? C34 C29 C40 C35 -60.5(6) . . . . ? Zr2 O4 C41 C42 -2.5(10) . . . . ? Zr2 O4 C41 C46 175.9(6) . . . . ? O4 C41 C42 C43 169.2(4) . . . . ? C46 C41 C42 C43 -9.3(7) . . . . ? O4 C41 C42 C32 -12.9(7) . . . . ? C46 C41 C42 C32 168.6(4) . . . . ? C33 C32 C42 C43 -45.6(7) . . . . ? C31 C32 C42 C43 131.1(5) . . . . ? C33 C32 C42 C41 136.5(5) . . . . ? C31 C32 C42 C41 -46.8(7) . . . . ? C41 C42 C43 C44 2.4(8) . . . . ? C32 C42 C43 C44 -175.5(5) . . . . ? C42 C43 C44 C45 4.3(8) . . . . ? C42 C43 C44 C56 -177.5(5) . . . . ? C43 C44 C45 C46 -4.6(8) . . . . ? C56 C44 C45 C46 177.2(5) . . . . ? C44 C45 C46 C41 -1.8(8) . . . . ? C44 C45 C46 C52 174.1(5) . . . . ? O4 C41 C46 C45 -169.6(4) . . . . ? C42 C41 C46 C45 8.8(7) . . . . ? O4 C41 C46 C52 14.5(7) . . . . ? C42 C41 C46 C52 -167.0(4) . . . . ? C37 C36 C47 C48 124.1(5) . . . . ? C35 C36 C47 C48 -59.3(6) . . . . ? C37 C36 C47 C50 -113.8(5) . . . . ? C35 C36 C47 C50 62.8(6) . . . . ? C37 C36 C47 C49 4.5(7) . . . . ? C35 C36 C47 C49 -178.8(5) . . . . ? C45 C46 C52 C55 -2.1(6) . . . . ? C41 C46 C52 C55 173.6(4) . . . . ? C45 C46 C52 C53 -120.8(5) . . . . ? C41 C46 C52 C53 54.8(6) . . . . ? C45 C46 C52 C54 118.1(5) . . . . ? C41 C46 C52 C54 -66.2(6) . . . . ? O3 Zr1 O5 C61 49.7(8) . . . . ? O1 Zr1 O5 C61 -51.0(7) . . . . ? C2 Zr1 O5 C61 -127.8(7) . . . . ? C5 Zr1 O5 C61 129.8(8) . . . . ? C6 Zr1 O5 C61 -31.7(12) . . . . ? C1 Zr1 O5 C61 -86.5(8) . . . . ? O3 Zr1 O5 C60 -150.3(8) . . . . ? O1 Zr1 O5 C60 109.0(8) . . . . ? C2 Zr1 O5 C60 32.3(8) . . . . ? C5 Zr1 O5 C60 -70.2(8) . . . . ? C6 Zr1 O5 C60 128.3(10) . . . . ? C1 Zr1 O5 C60 73.5(8) . . . . ? O3 Zr1 O5 C57 31.2(7) . . . . ? O1 Zr1 O5 C57 -69.5(7) . . . . ? C2 Zr1 O5 C57 -146.2(7) . . . . ? C5 Zr1 O5 C57 111.3(7) . . . . ? C6 Zr1 O5 C57 -50.2(11) . . . . ? C1 Zr1 O5 C57 -104.9(7) . . . . ? O3 Zr1 O5 C64 -169.7(9) . . . . ? O1 Zr1 O5 C64 89.6(9) . . . . ? C2 Zr1 O5 C64 12.8(9) . . . . ? C5 Zr1 O5 C64 -89.6(9) . . . . ? C6 Zr1 O5 C64 108.9(11) . . . . ? C1 Zr1 O5 C64 54.1(9) . . . . ? C61 O5 C57 C58 51(3) . . . . ? C60 O5 C57 C58 -21.7(15) . . . . ? C64 O5 C57 C58 -5.3(15) . . . . ? Zr1 O5 C57 C58 156.9(7) . . . . ? O5 C57 C58 C59 27.3(14) . . . . ? C57 C58 C59 C60 -23.1(14) . . . . ? C61 O5 C60 C59 -7.2(15) . . . . ? C57 O5 C60 C59 9.3(16) . . . . ? C64 O5 C60 C59 -73(3) . . . . ? Zr1 O5 C60 C59 -169.2(7) . . . . ? C58 C59 C60 O5 8.7(14) . . . . ? C60 O5 C61 C62 35.1(15) . . . . ? C57 O5 C61 C62 -78(3) . . . . ? C64 O5 C61 C62 49.4(14) . . . . ? Zr1 O5 C61 C62 -161.5(7) . . . . ? O5 C61 C62 C63 -33.6(13) . . . . ? C61 C62 C63 C64 5.7(14) . . . . ? C61 O5 C64 C63 -44.9(15) . . . . ? C60 O5 C64 C63 73(3) . . . . ? C57 O5 C64 C63 -31.0(16) . . . . ? Zr1 O5 C64 C63 168.9(8) . . . . ? C62 C63 C64 O5 23.6(14) . . . . ? C71 C66 C67 C68 2.3(16) . . . . ? C65 C66 C67 C68 -178.0(10) . . . . ? C66 C67 C68 C69 0.1(17) . . . . ? C67 C68 C69 C70 -3.4(15) . . . . ? C68 C69 C70 C71 4.5(16) . . . . ? C69 C70 C71 C66 -2.1(16) . . . . ? C67 C66 C71 C70 -1.3(14) . . . . ? C65 C66 C71 C70 179.1(10) . . . . ? C78 C73 C74 C75 0(3) . . . . ? C72 C73 C74 C75 176.5(19) . . . . ? C73 C74 C75 C76 4(4) . . . . ? C74 C75 C76 C77 -7(5) . . . . ? C75 C76 C77 C78 5(4) . . . . ? C74 C73 C78 C77 -1(2) . . . . ? C72 C73 C78 C77 -177.7(15) . . . . ? C76 C77 C78 C73 -1.3(19) . . . . ? C79 C80 C81 C82 173.0(12) . . . . ? C80 C81 C82 C83 52(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.258 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 962320' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(C6H4)2(CO2)(ArO)4Zr2(thf)4]2.5(thf) _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C73 H85 O10 Zr2, 2.5(C4 H8 O)' _chemical_formula_sum 'C83 H105 O12.50 Zr2' _chemical_formula_weight 1485.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.785(2) _cell_length_b 14.4383(19) _cell_length_c 29.830(4) _cell_angle_alpha 90 _cell_angle_beta 95.8792(19) _cell_angle_gamma 90 _cell_volume 7619.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11744 _cell_measurement_theta_min 3.0477 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.295 _exptl_crystal_F_000 3132 _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.334 _shelx_estimated_absorpt_T_min 0.971 _shelx_estimated_absorpt_T_max 0.990 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9705 _exptl_absorpt_correction_T_max 0.9900 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Saturn CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 92813 _diffrn_reflns_av_unetI/netI 0.0946 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.048 _diffrn_reflns_theta_max 27.513 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 17461 _reflns_number_gt 11882 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1460P)^2^+16.7935P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 17461 _refine_ls_number_parameters 819 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.2712 _refine_ls_wR_factor_gt 0.2322 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.10325(3) 0.46092(4) 0.20936(2) 0.02917(15) Uani 1 1 d . . . . . O1 O 0.1869(2) 0.4840(3) 0.26238(13) 0.0322(8) Uani 1 1 d . . . . . O2 O 0.0093(2) 0.4885(3) 0.16194(13) 0.0368(9) Uani 1 1 d . . . . . C1 C 0.1497(3) 0.3065(4) 0.25194(18) 0.0313(11) Uani 1 1 d . . . . . C2 C 0.1812(3) 0.2849(4) 0.21357(18) 0.0321(11) Uani 1 1 d . . . . . H1 H 0.2335 0.2701 0.2167 0.039 Uiso 1 1 calc R U . . . C3 C 0.1409(3) 0.2820(4) 0.16641(18) 0.0306(11) Uani 1 1 d . . . . . H2 H 0.1443 0.2191 0.1527 0.037 Uiso 1 1 calc R U . . . C4 C 0.0590(3) 0.3104(4) 0.16908(18) 0.0303(11) Uani 1 1 d . . . . . C5 C 0.0272(3) 0.3152(4) 0.20929(19) 0.0340(12) Uani 1 1 d . . . . . H3 H -0.0263 0.3116 0.2084 0.041 Uiso 1 1 calc R U . . . C6 C 0.0699(3) 0.3252(4) 0.25215(18) 0.0316(11) Uani 1 1 d . . . . . H4 H 0.0479 0.3428 0.2786 0.038 Uiso 1 1 calc R U . . . C7 C 0.2204(3) 0.4277(4) 0.29477(18) 0.0321(12) Uani 1 1 d . . . . . C8 C 0.2729(3) 0.4605(4) 0.32987(19) 0.0366(13) Uani 1 1 d . . . . . C9 C 0.3010(3) 0.3958(5) 0.3622(2) 0.0405(14) Uani 1 1 d . . . . . H5 H 0.3358 0.4170 0.3863 0.049 Uiso 1 1 calc R U . . . C10 C 0.2814(3) 0.3023(4) 0.36145(19) 0.0375(13) Uani 1 1 d . . . . . C11 C 0.2307(3) 0.2719(4) 0.3253(2) 0.0378(13) Uani 1 1 d . . . . . H6 H 0.2166 0.2084 0.3234 0.045 Uiso 1 1 calc R U . . . C12 C 0.2014(3) 0.3324(4) 0.29284(18) 0.0316(11) Uani 1 1 d . . . . . C13 C -0.0095(3) 0.4340(4) 0.12555(19) 0.0323(12) Uani 1 1 d . . . . . C14 C 0.0104(3) 0.3396(4) 0.12781(18) 0.0322(12) Uani 1 1 d . . . . . C15 C -0.0126(3) 0.2795(4) 0.09260(19) 0.0348(12) Uani 1 1 d . . . . . H7 H -0.0011 0.2154 0.0957 0.042 Uiso 1 1 calc R U . . . C16 C -0.0518(3) 0.3109(5) 0.0534(2) 0.0416(14) Uani 1 1 d . . . . . C17 C -0.0664(3) 0.4059(5) 0.0500(2) 0.0407(14) Uani 1 1 d . . . . . H8 H -0.0917 0.4284 0.0226 0.049 Uiso 1 1 calc R U . . . C18 C -0.0461(3) 0.4703(4) 0.0846(2) 0.0363(13) Uani 1 1 d . . . . . C19 C 0.3024(4) 0.5606(5) 0.3305(2) 0.0448(15) Uani 1 1 d . . . . . C20 C 0.3465(4) 0.5751(5) 0.2890(2) 0.0497(16) Uani 1 1 d . . . . . H9 H 0.3920 0.5365 0.2919 0.075 Uiso 1 1 calc R U . . . H10 H 0.3609 0.6404 0.2871 0.075 Uiso 1 1 calc R U . . . H11 H 0.3144 0.5576 0.2616 0.075 Uiso 1 1 calc R U . . . C21 C 0.2362(4) 0.6305(5) 0.3289(3) 0.0575(19) Uani 1 1 d . . . . . H12 H 0.2018 0.6199 0.3015 0.086 Uiso 1 1 calc R U . . . H13 H 0.2562 0.6937 0.3286 0.086 Uiso 1 1 calc R U . . . H14 H 0.2088 0.6221 0.3554 0.086 Uiso 1 1 calc R U . . . C22 C 0.3555(5) 0.5825(6) 0.3723(3) 0.063(2) Uani 1 1 d . . . . . H15 H 0.3284 0.5760 0.3991 0.095 Uiso 1 1 calc R U . . . H16 H 0.3741 0.6461 0.3704 0.095 Uiso 1 1 calc R U . . . H17 H 0.3983 0.5394 0.3743 0.095 Uiso 1 1 calc R U . . . C23 C 0.3095(4) 0.2379(5) 0.3989(2) 0.0509(16) Uani 1 1 d . . . . . H18 H 0.3458 0.2706 0.4203 0.076 Uiso 1 1 calc R U . . . H19 H 0.3343 0.1846 0.3864 0.076 Uiso 1 1 calc R U . . . H20 H 0.2668 0.2165 0.4145 0.076 Uiso 1 1 calc R U . . . C24 C -0.0587(4) 0.5745(4) 0.0779(2) 0.0428(14) Uani 1 1 d . . . . . C25 C 0.0195(4) 0.6223(5) 0.0840(2) 0.0478(15) Uani 1 1 d . . . . . H21 H 0.0444 0.6086 0.1141 0.072 Uiso 1 1 calc R U . . . H22 H 0.0130 0.6894 0.0805 0.072 Uiso 1 1 calc R U . . . H23 H 0.0507 0.5992 0.0611 0.072 Uiso 1 1 calc R U . . . C26 C -0.1082(4) 0.6140(5) 0.1122(2) 0.0532(17) Uani 1 1 d . . . . . H24 H -0.1584 0.5854 0.1079 0.080 Uiso 1 1 calc R U . . . H25 H -0.1130 0.6811 0.1081 0.080 Uiso 1 1 calc R U . . . H26 H -0.0849 0.6007 0.1428 0.080 Uiso 1 1 calc R U . . . C27 C -0.0946(4) 0.5984(5) 0.0307(2) 0.0546(18) Uani 1 1 d . . . . . H27 H -0.0629 0.5745 0.0083 0.082 Uiso 1 1 calc R U . . . H28 H -0.0991 0.6658 0.0276 0.082 Uiso 1 1 calc R U . . . H29 H -0.1449 0.5703 0.0258 0.082 Uiso 1 1 calc R U . . . C28 C -0.0730(4) 0.2475(5) 0.0145(2) 0.0536(17) Uani 1 1 d . . . . . H30 H -0.0272 0.2271 0.0017 0.080 Uiso 1 1 calc R U . . . H31 H -0.1060 0.2804 -0.0085 0.080 Uiso 1 1 calc R U . . . H32 H -0.0996 0.1935 0.0249 0.080 Uiso 1 1 calc R U . . . Zr2 Zr 0.33917(3) 0.35410(3) 0.10511(2) 0.02741(15) Uani 1 1 d . . . . . O3 O 0.3791(2) 0.4903(3) 0.11230(13) 0.0331(8) Uani 1 1 d . . . . . O4 O 0.3464(2) 0.2077(2) 0.10790(13) 0.0323(8) Uani 1 1 d . . . . . C29 C 0.2615(3) 0.4707(4) 0.05012(19) 0.0326(12) Uani 1 1 d . . . . . C30 C 0.2028(3) 0.4541(4) 0.07526(18) 0.0302(11) Uani 1 1 d . . . . . H33 H 0.1794 0.5067 0.0869 0.036 Uiso 1 1 calc R U . . . C31 C 0.1715(3) 0.3608(3) 0.08638(17) 0.0275(11) Uani 1 1 d . . . . . H34 H 0.1167 0.3553 0.0752 0.033 Uiso 1 1 calc R U . . . C32 C 0.2187(3) 0.2877(4) 0.06519(18) 0.0305(11) Uani 1 1 d . . . . . C33 C 0.2669(3) 0.3079(4) 0.03227(19) 0.0338(12) Uani 1 1 d . . . . . H35 H 0.2804 0.2597 0.0129 0.041 Uiso 1 1 calc R U . . . C34 C 0.2959(3) 0.3968(4) 0.02689(18) 0.0337(12) Uani 1 1 d . . . . . H36 H 0.3361 0.4080 0.0089 0.040 Uiso 1 1 calc R U . . . C35 C 0.3589(3) 0.5687(4) 0.0900(2) 0.0325(12) Uani 1 1 d . . . . . C36 C 0.3952(3) 0.6545(4) 0.0996(2) 0.0364(13) Uani 1 1 d . . . . . C37 C 0.3682(4) 0.7296(4) 0.0752(2) 0.0459(16) Uani 1 1 d . . . . . H37 H 0.3914 0.7878 0.0822 0.055 Uiso 1 1 calc R U . . . C38 C 0.3088(3) 0.7270(4) 0.0407(3) 0.0474(16) Uani 1 1 d . . . . . C39 C 0.2752(4) 0.6422(4) 0.0306(2) 0.0461(15) Uani 1 1 d . . . . . H38 H 0.2352 0.6377 0.0070 0.055 Uiso 1 1 calc R U . . . C40 C 0.2996(3) 0.5639(4) 0.0546(2) 0.0353(12) Uani 1 1 d . . . . . C41 C 0.2840(3) 0.1541(3) 0.10377(19) 0.0303(11) Uani 1 1 d . . . . . C42 C 0.2171(3) 0.1887(4) 0.07940(18) 0.0310(11) Uani 1 1 d . . . . . C43 C 0.1549(3) 0.1315(4) 0.06980(18) 0.0343(12) Uani 1 1 d . . . . . H39 H 0.1106 0.1559 0.0535 0.041 Uiso 1 1 calc R U . . . C44 C 0.1556(4) 0.0388(4) 0.0835(2) 0.0389(13) Uani 1 1 d . . . . . C45 C 0.2186(3) 0.0092(4) 0.1117(2) 0.0378(13) Uani 1 1 d . . . . . H40 H 0.2181 -0.0519 0.1235 0.045 Uiso 1 1 calc R U . . . C46 C 0.2823(3) 0.0641(4) 0.12340(19) 0.0343(12) Uani 1 1 d . . . . . C47 C 0.4583(4) 0.6625(4) 0.1390(2) 0.0459(15) Uani 1 1 d . . . . . C48 C 0.4225(4) 0.6443(5) 0.1839(2) 0.0565(18) Uani 1 1 d . . . . . H41 H 0.3956 0.5850 0.1819 0.085 Uiso 1 1 calc R U . . . H42 H 0.3870 0.6943 0.1889 0.085 Uiso 1 1 calc R U . . . H43 H 0.4625 0.6423 0.2090 0.085 Uiso 1 1 calc R U . . . C49 C 0.4939(4) 0.7595(5) 0.1427(3) 0.0567(19) Uani 1 1 d . . . . . H44 H 0.5335 0.7609 0.1681 0.085 Uiso 1 1 calc R U . . . H45 H 0.4550 0.8053 0.1476 0.085 Uiso 1 1 calc R U . . . H46 H 0.5161 0.7741 0.1148 0.085 Uiso 1 1 calc R U . . . C50 C 0.5214(4) 0.5932(4) 0.1354(2) 0.0482(16) Uani 1 1 d . . . . . H47 H 0.5407 0.5992 0.1059 0.072 Uiso 1 1 calc R U . . . H48 H 0.5020 0.5303 0.1388 0.072 Uiso 1 1 calc R U . . . H49 H 0.5624 0.6052 0.1593 0.072 Uiso 1 1 calc R U . . . C51 C 0.2829(4) 0.8139(5) 0.0155(3) 0.075(3) Uani 1 1 d . . . . . H50 H 0.2390 0.8396 0.0285 0.113 Uiso 1 1 calc R U . . . H51 H 0.2691 0.7990 -0.0163 0.113 Uiso 1 1 calc R U . . . H52 H 0.3240 0.8595 0.0180 0.113 Uiso 1 1 calc R U . . . C52 C 0.3471(4) 0.0327(4) 0.1577(2) 0.0425(14) Uani 1 1 d . . . . . C53 C 0.3559(4) 0.1020(5) 0.1968(2) 0.0513(17) Uani 1 1 d . . . . . H53 H 0.3605 0.1648 0.1849 0.077 Uiso 1 1 calc R U . . . H54 H 0.4013 0.0869 0.2169 0.077 Uiso 1 1 calc R U . . . H55 H 0.3114 0.0988 0.2136 0.077 Uiso 1 1 calc R U . . . C54 C 0.4213(4) 0.0245(5) 0.1362(3) 0.0579(19) Uani 1 1 d . . . . . H56 H 0.4153 -0.0207 0.1116 0.087 Uiso 1 1 calc R U . . . H57 H 0.4615 0.0041 0.1590 0.087 Uiso 1 1 calc R U . . . H58 H 0.4345 0.0850 0.1243 0.087 Uiso 1 1 calc R U . . . C55 C 0.3317(4) -0.0625(5) 0.1780(3) 0.0561(19) Uani 1 1 d . . . . . H59 H 0.2833 -0.0608 0.1910 0.084 Uiso 1 1 calc R U . . . H60 H 0.3723 -0.0777 0.2015 0.084 Uiso 1 1 calc R U . . . H61 H 0.3295 -0.1097 0.1543 0.084 Uiso 1 1 calc R U . . . C56 C 0.0919(4) -0.0270(4) 0.0690(2) 0.0506(17) Uani 1 1 d . . . . . H62 H 0.0434 0.0035 0.0720 0.076 Uiso 1 1 calc R U . . . H63 H 0.0964 -0.0824 0.0880 0.076 Uiso 1 1 calc R U . . . H64 H 0.0944 -0.0447 0.0374 0.076 Uiso 1 1 calc R U . . . C57 C 0.1844(3) 0.3572(4) 0.13970(17) 0.0274(11) Uani 1 1 d . . . . . O5 O 0.1632(2) 0.4420(2) 0.15800(12) 0.0282(8) Uani 1 1 d . . . . . O6 O 0.2630(2) 0.3463(3) 0.14915(12) 0.0297(8) Uani 1 1 d . . . . . O7 O 0.1336(2) 0.6133(3) 0.19713(14) 0.0368(9) Uani 1 1 d . . . . . C58 C 0.2057(4) 0.6400(5) 0.1826(3) 0.0532(18) Uani 1 1 d . . . . . H65 H 0.2280 0.5881 0.1668 0.064 Uiso 1 1 calc R U . . . H66 H 0.2414 0.6580 0.2088 0.064 Uiso 1 1 calc R U . . . C59 C 0.1906(6) 0.7181(6) 0.1524(4) 0.092(3) Uani 1 1 d . . . . . H67 H 0.1725 0.6973 0.1215 0.111 Uiso 1 1 calc R U . . . H68 H 0.2361 0.7572 0.1512 0.111 Uiso 1 1 calc R U . . . C60 C 0.1272(5) 0.7711(5) 0.1746(4) 0.075(3) Uani 1 1 d . . . . . H69 H 0.1491 0.8195 0.1956 0.090 Uiso 1 1 calc R U . . . H70 H 0.0909 0.8004 0.1514 0.090 Uiso 1 1 calc R U . . . C61 C 0.0889(4) 0.6955(4) 0.1999(3) 0.0526(17) Uani 1 1 d . . . . . H71 H 0.0868 0.7135 0.2318 0.063 Uiso 1 1 calc R U . . . H72 H 0.0367 0.6848 0.1859 0.063 Uiso 1 1 calc R U . . . O8 O 0.0200(2) 0.5373(3) 0.25308(13) 0.0387(9) Uani 1 1 d . . . . . C62 C -0.0612(4) 0.5493(8) 0.2435(3) 0.079(3) Uani 1 1 d . . . . . H73 H -0.0720 0.6107 0.2294 0.094 Uiso 1 1 calc R U . . . H74 H -0.0817 0.5012 0.2220 0.094 Uiso 1 1 calc R U . . . C63 C -0.0963(4) 0.5427(6) 0.2836(3) 0.063(2) Uani 1 1 d . . . . . H75 H -0.1290 0.4871 0.2829 0.075 Uiso 1 1 calc R U . . . H76 H -0.1280 0.5980 0.2873 0.075 Uiso 1 1 calc R U . . . C64 C -0.0348(4) 0.5361(6) 0.3220(2) 0.064(2) Uani 1 1 d . . . . . H77 H -0.0334 0.4735 0.3355 0.076 Uiso 1 1 calc R U . . . H78 H -0.0426 0.5823 0.3456 0.076 Uiso 1 1 calc R U . . . C65 C 0.0370(4) 0.5558(5) 0.3008(2) 0.0452(15) Uani 1 1 d . . . . . H79 H 0.0525 0.6212 0.3058 0.054 Uiso 1 1 calc R U . . . H80 H 0.0784 0.5153 0.3139 0.054 Uiso 1 1 calc R U . . . O9 O 0.4213(2) 0.3416(3) 0.16903(13) 0.0366(9) Uani 1 1 d . . . . . C66 C 0.4968(4) 0.3040(5) 0.1739(2) 0.0495(16) Uani 1 1 d . . . . . H81 H 0.5298 0.3392 0.1553 0.059 Uiso 1 1 calc R U . . . H82 H 0.4962 0.2383 0.1643 0.059 Uiso 1 1 calc R U . . . C67 C 0.5249(5) 0.3120(6) 0.2227(2) 0.066(2) Uani 1 1 d . . . . . H83 H 0.5796 0.3264 0.2266 0.079 Uiso 1 1 calc R U . . . H84 H 0.5159 0.2540 0.2390 0.079 Uiso 1 1 calc R U . . . C68 C 0.4782(4) 0.3924(5) 0.2393(2) 0.0566(18) Uani 1 1 d . . . . . H85 H 0.4737 0.3876 0.2720 0.068 Uiso 1 1 calc R U . . . H86 H 0.5005 0.4532 0.2328 0.068 Uiso 1 1 calc R U . . . C69 C 0.4024(4) 0.3783(5) 0.2119(2) 0.0500(16) Uani 1 1 d . . . . . H87 H 0.3708 0.3339 0.2270 0.060 Uiso 1 1 calc R U . . . H88 H 0.3748 0.4377 0.2075 0.060 Uiso 1 1 calc R U . . . O10 O 0.4544(2) 0.3294(3) 0.07364(13) 0.0350(9) Uani 1 1 d . . . . . C70 C 0.4863(7) 0.2436(8) 0.0607(4) 0.035(3) Uiso 0.60(2) 1 d . . P A 1 C71 C 0.5490(7) 0.2627(9) 0.0325(4) 0.054(4) Uiso 0.60(2) 1 d . . P A 1 C72 C 0.5364(9) 0.3643(9) 0.0179(5) 0.057(4) Uiso 0.60(2) 1 d . . P A 1 C73 C 0.5020(9) 0.4054(11) 0.0581(5) 0.047(5) Uiso 0.60(2) 1 d . . P A 1 C74 C 0.4675(11) 0.2374(12) 0.0483(7) 0.037(4) Uiso 0.40(2) 1 d . . P A 2 C75 C 0.4997(13) 0.2607(15) 0.0099(8) 0.070(7) Uiso 0.40(2) 1 d . . P A 2 C76 C 0.5066(12) 0.3645(12) 0.0048(6) 0.042(4) Uiso 0.40(2) 1 d . . P A 2 C77 C 0.4887(10) 0.4057(12) 0.0494(6) 0.023(4) Uiso 0.40(2) 1 d . . P A 2 O11 O 0.1021(5) 0.4976(7) 0.4027(3) 0.127(3) Uiso 1 1 d . . . . . C78 C 0.1032(5) 0.3972(7) 0.4012(3) 0.078(2) Uiso 1 1 d . . . . . C79 C 0.1457(6) 0.3708(7) 0.4482(3) 0.084(3) Uiso 1 1 d . . . . . C80 C 0.2015(6) 0.4523(8) 0.4617(4) 0.092(3) Uiso 1 1 d . . . . . C81 C 0.1588(8) 0.5318(10) 0.4404(5) 0.125(4) Uiso 1 1 d . . . . . O12 O 0.3272(8) 0.8797(10) 0.3673(5) 0.202(5) Uiso 1 1 d . . . . . C82 C 0.2482(10) 0.8711(12) 0.3899(6) 0.156(6) Uiso 1 1 d . . . . . C83 C 0.1967(9) 0.8829(10) 0.3456(5) 0.133(5) Uiso 1 1 d . . . . . C84 C 0.2357(13) 0.9100(16) 0.3061(8) 0.204(8) Uiso 1 1 d . . . . . C85 C 0.3014(12) 0.9480(14) 0.3312(7) 0.180(7) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0296(3) 0.0273(3) 0.0316(3) 0.0004(2) 0.0076(2) -0.0001(2) O1 0.0298(19) 0.0310(19) 0.036(2) 0.0001(16) 0.0034(16) 0.0014(16) O2 0.038(2) 0.035(2) 0.037(2) -0.0002(17) 0.0023(17) 0.0041(17) C1 0.036(3) 0.026(3) 0.033(3) 0.004(2) 0.010(2) -0.002(2) C2 0.034(3) 0.028(3) 0.035(3) 0.004(2) 0.007(2) 0.001(2) C3 0.035(3) 0.025(3) 0.033(3) 0.000(2) 0.006(2) -0.005(2) C4 0.030(3) 0.028(3) 0.034(3) -0.001(2) 0.008(2) -0.005(2) C5 0.031(3) 0.030(3) 0.042(3) 0.001(2) 0.005(2) -0.007(2) C6 0.035(3) 0.034(3) 0.027(3) 0.002(2) 0.010(2) -0.001(2) C7 0.032(3) 0.037(3) 0.028(3) 0.001(2) 0.005(2) 0.000(2) C8 0.037(3) 0.041(3) 0.032(3) -0.003(2) 0.007(2) -0.002(2) C9 0.035(3) 0.049(4) 0.037(3) -0.002(3) 0.001(2) 0.004(3) C10 0.033(3) 0.046(3) 0.033(3) 0.004(3) 0.001(2) 0.004(3) C11 0.032(3) 0.037(3) 0.046(3) 0.003(3) 0.010(2) 0.007(2) C12 0.024(3) 0.038(3) 0.033(3) 0.001(2) 0.005(2) 0.000(2) C13 0.026(3) 0.035(3) 0.036(3) -0.004(2) 0.006(2) 0.002(2) C14 0.032(3) 0.032(3) 0.033(3) -0.001(2) 0.004(2) -0.003(2) C15 0.037(3) 0.033(3) 0.034(3) 0.001(2) 0.004(2) -0.003(2) C16 0.039(3) 0.046(4) 0.040(3) -0.004(3) -0.001(3) -0.006(3) C17 0.034(3) 0.050(4) 0.036(3) -0.009(3) -0.004(2) -0.001(3) C18 0.024(3) 0.046(3) 0.038(3) 0.006(3) -0.001(2) 0.003(2) C19 0.042(3) 0.049(4) 0.043(3) -0.007(3) 0.001(3) -0.009(3) C20 0.053(4) 0.051(4) 0.046(4) 0.000(3) 0.007(3) -0.015(3) C21 0.066(5) 0.042(4) 0.064(5) -0.018(3) 0.006(4) -0.003(3) C22 0.075(5) 0.061(5) 0.051(4) -0.005(4) -0.008(4) -0.016(4) C23 0.043(4) 0.066(5) 0.042(3) 0.011(3) -0.002(3) 0.000(3) C24 0.042(3) 0.044(3) 0.041(3) 0.001(3) -0.003(3) 0.009(3) C25 0.046(4) 0.045(4) 0.053(4) 0.004(3) 0.007(3) 0.003(3) C26 0.049(4) 0.059(4) 0.051(4) -0.001(3) 0.002(3) 0.018(3) C27 0.056(4) 0.054(4) 0.051(4) 0.012(3) -0.008(3) 0.016(3) C28 0.062(4) 0.049(4) 0.046(4) -0.014(3) -0.008(3) -0.004(3) Zr2 0.0283(3) 0.0245(3) 0.0299(3) 0.0015(2) 0.0054(2) 0.00105(19) O3 0.034(2) 0.0279(19) 0.038(2) -0.0007(16) 0.0072(16) 0.0002(16) O4 0.034(2) 0.0240(18) 0.040(2) 0.0000(16) 0.0063(16) -0.0009(15) C29 0.031(3) 0.034(3) 0.034(3) 0.010(2) 0.004(2) 0.006(2) C30 0.031(3) 0.027(3) 0.033(3) 0.007(2) 0.004(2) 0.004(2) C31 0.028(3) 0.025(2) 0.029(3) 0.003(2) 0.000(2) -0.002(2) C32 0.029(3) 0.027(3) 0.035(3) -0.005(2) 0.003(2) -0.003(2) C33 0.031(3) 0.039(3) 0.031(3) 0.002(2) 0.002(2) 0.002(2) C34 0.031(3) 0.039(3) 0.032(3) 0.001(2) 0.005(2) 0.003(2) C35 0.027(3) 0.025(3) 0.047(3) 0.003(2) 0.009(2) 0.003(2) C36 0.034(3) 0.028(3) 0.050(3) 0.000(2) 0.016(3) -0.001(2) C37 0.040(3) 0.027(3) 0.074(5) 0.004(3) 0.022(3) -0.006(2) C38 0.034(3) 0.031(3) 0.078(5) 0.020(3) 0.013(3) 0.005(2) C39 0.043(4) 0.041(3) 0.055(4) 0.020(3) 0.012(3) 0.006(3) C40 0.032(3) 0.028(3) 0.048(3) 0.009(2) 0.012(2) 0.001(2) C41 0.035(3) 0.022(2) 0.036(3) -0.002(2) 0.010(2) 0.000(2) C42 0.034(3) 0.030(3) 0.030(3) 0.000(2) 0.008(2) -0.002(2) C43 0.038(3) 0.038(3) 0.028(3) -0.007(2) 0.011(2) -0.009(2) C44 0.045(3) 0.036(3) 0.037(3) -0.009(3) 0.011(3) -0.011(3) C45 0.047(3) 0.025(3) 0.045(3) -0.003(2) 0.021(3) -0.002(2) C46 0.038(3) 0.028(3) 0.038(3) -0.004(2) 0.011(2) 0.002(2) C47 0.043(4) 0.037(3) 0.060(4) -0.002(3) 0.019(3) -0.004(3) C48 0.060(5) 0.055(4) 0.056(4) -0.012(3) 0.014(3) -0.014(3) C49 0.048(4) 0.041(4) 0.082(5) -0.014(4) 0.010(4) -0.007(3) C50 0.043(4) 0.034(3) 0.067(4) -0.007(3) 0.007(3) -0.002(3) C51 0.055(5) 0.044(4) 0.128(8) 0.040(5) 0.008(5) 0.000(3) C52 0.045(4) 0.031(3) 0.052(4) 0.010(3) 0.007(3) 0.006(3) C53 0.061(4) 0.042(4) 0.050(4) 0.013(3) -0.002(3) 0.001(3) C54 0.050(4) 0.041(4) 0.085(6) 0.018(4) 0.014(4) 0.003(3) C55 0.048(4) 0.041(4) 0.079(5) 0.026(4) 0.006(4) 0.001(3) C56 0.058(4) 0.037(3) 0.057(4) -0.008(3) 0.011(3) -0.018(3) C57 0.029(3) 0.027(3) 0.027(2) -0.001(2) 0.006(2) 0.000(2) O5 0.0308(19) 0.0207(17) 0.0343(19) 0.0015(15) 0.0091(15) 0.0008(14) O6 0.0267(18) 0.034(2) 0.0292(18) 0.0008(15) 0.0061(15) 0.0008(15) O7 0.038(2) 0.0249(19) 0.049(2) 0.0006(17) 0.0072(18) -0.0016(16) C58 0.048(4) 0.041(4) 0.074(5) 0.011(3) 0.022(4) -0.002(3) C59 0.088(7) 0.060(5) 0.138(9) 0.036(6) 0.055(6) -0.001(5) C60 0.069(5) 0.035(4) 0.126(8) 0.023(4) 0.035(5) 0.010(3) C61 0.061(4) 0.034(3) 0.066(4) 0.001(3) 0.020(4) 0.014(3) O8 0.035(2) 0.046(2) 0.036(2) -0.0031(18) 0.0069(17) 0.0061(18) C62 0.030(4) 0.150(9) 0.057(5) -0.023(5) 0.012(3) 0.010(4) C63 0.047(4) 0.078(6) 0.066(5) 0.003(4) 0.021(4) -0.002(4) C64 0.064(5) 0.086(6) 0.045(4) -0.006(4) 0.025(4) -0.004(4) C65 0.046(4) 0.058(4) 0.033(3) -0.011(3) 0.010(3) 0.002(3) O9 0.032(2) 0.041(2) 0.036(2) 0.0010(18) -0.0032(16) 0.0041(17) C66 0.037(3) 0.057(4) 0.053(4) 0.004(3) -0.003(3) 0.006(3) C67 0.064(5) 0.077(5) 0.052(4) 0.007(4) -0.019(4) 0.018(4) C68 0.053(4) 0.062(5) 0.051(4) -0.004(4) -0.013(3) 0.007(3) C69 0.055(4) 0.058(4) 0.036(3) -0.005(3) 0.001(3) 0.002(3) O10 0.035(2) 0.032(2) 0.041(2) 0.0071(17) 0.0147(17) 0.0065(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O5 1.973(4) . ? Zr1 O1 2.085(4) . ? Zr1 O2 2.114(4) . ? Zr1 O7 2.303(4) . ? Zr1 O8 2.346(4) . ? Zr1 C6 2.444(5) . ? Zr1 C5 2.501(5) . ? Zr1 C4 2.568(5) . ? Zr1 C1 2.656(5) . ? O1 C7 1.353(6) . ? O2 C13 1.354(7) . ? C1 C2 1.361(7) . ? C1 C6 1.445(8) . ? C1 C12 1.498(8) . ? C2 C3 1.512(8) . ? C2 H1 0.9500 . ? C3 C4 1.523(7) . ? C3 C57 1.593(7) . ? C3 H2 1.0000 . ? C4 C5 1.379(7) . ? C4 C14 1.491(8) . ? C5 C6 1.426(8) . ? C5 H3 0.9500 . ? C6 H4 0.9500 . ? C7 C8 1.412(8) . ? C7 C12 1.416(8) . ? C8 C9 1.396(8) . ? C8 C19 1.538(9) . ? C9 C10 1.395(9) . ? C9 H5 0.9500 . ? C10 C11 1.403(8) . ? C10 C23 1.499(8) . ? C11 C12 1.367(8) . ? C11 H6 0.9500 . ? C13 C14 1.408(8) . ? C13 C18 1.425(8) . ? C14 C15 1.392(8) . ? C15 C16 1.374(8) . ? C15 H7 0.9500 . ? C16 C17 1.397(9) . ? C16 C28 1.495(8) . ? C17 C18 1.408(8) . ? C17 H8 0.9500 . ? C18 C24 1.532(9) . ? C19 C22 1.518(9) . ? C19 C21 1.548(10) . ? C19 C20 1.545(9) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 H18 0.9800 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C24 C26 1.528(9) . ? C24 C27 1.525(9) . ? C24 C25 1.546(9) . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? Zr2 O6 1.984(4) . ? Zr2 O3 2.094(4) . ? Zr2 O4 2.119(4) . ? Zr2 O9 2.287(4) . ? Zr2 O10 2.367(4) . ? Zr2 C34 2.459(5) . ? Zr2 C33 2.499(6) . ? Zr2 C32 2.530(5) . ? Zr2 C29 2.640(5) . ? O3 C35 1.344(6) . ? O4 C41 1.348(6) . ? C29 C30 1.367(7) . ? C29 C34 1.443(8) . ? C29 C40 1.506(8) . ? C30 C31 1.507(7) . ? C30 H33 0.9500 . ? C31 C32 1.526(7) . ? C31 C57 1.584(7) . ? C31 H34 1.0000 . ? C32 C33 1.399(7) . ? C32 C42 1.492(7) . ? C33 C34 1.399(8) . ? C33 H35 0.9500 . ? C34 H36 0.9500 . ? C35 C40 1.415(8) . ? C35 C36 1.413(8) . ? C36 C37 1.366(8) . ? C36 C47 1.542(9) . ? C37 C38 1.398(10) . ? C37 H37 0.9500 . ? C38 C39 1.381(9) . ? C38 C51 1.510(9) . ? C39 C40 1.384(8) . ? C39 H38 0.9500 . ? C41 C42 1.420(8) . ? C41 C46 1.427(7) . ? C42 C43 1.388(8) . ? C43 C44 1.399(8) . ? C43 H39 0.9500 . ? C44 C45 1.396(9) . ? C44 C56 1.508(8) . ? C45 C46 1.398(8) . ? C45 H40 0.9500 . ? C46 C52 1.529(8) . ? C47 C50 1.515(9) . ? C47 C49 1.537(9) . ? C47 C48 1.563(9) . ? C48 H41 0.9800 . ? C48 H42 0.9800 . ? C48 H43 0.9800 . ? C49 H44 0.9800 . ? C49 H45 0.9800 . ? C49 H46 0.9800 . ? C50 H47 0.9800 . ? C50 H48 0.9800 . ? C50 H49 0.9800 . ? C51 H50 0.9800 . ? C51 H51 0.9800 . ? C51 H52 0.9800 . ? C52 C54 1.529(9) . ? C52 C53 1.533(9) . ? C52 C55 1.537(8) . ? C53 H53 0.9800 . ? C53 H54 0.9800 . ? C53 H55 0.9800 . ? C54 H56 0.9800 . ? C54 H57 0.9800 . ? C54 H58 0.9800 . ? C55 H59 0.9800 . ? C55 H60 0.9800 . ? C55 H61 0.9800 . ? C56 H62 0.9800 . ? C56 H63 0.9800 . ? C56 H64 0.9800 . ? C57 O6 1.406(6) . ? C57 O5 1.407(6) . ? O7 C61 1.436(7) . ? O7 C58 1.447(7) . ? C58 C59 1.453(11) . ? C58 H65 0.9900 . ? C58 H66 0.9900 . ? C59 C60 1.565(12) . ? C59 H67 0.9900 . ? C59 H68 0.9900 . ? C60 C61 1.527(10) . ? C60 H69 0.9900 . ? C60 H70 0.9900 . ? C61 H71 0.9900 . ? C61 H72 0.9900 . ? O8 C65 1.449(7) . ? O8 C62 1.454(8) . ? C62 C63 1.410(10) . ? C62 H73 0.9900 . ? C62 H74 0.9900 . ? C63 C64 1.502(11) . ? C63 H75 0.9900 . ? C63 H76 0.9900 . ? C64 C65 1.510(9) . ? C64 H77 0.9900 . ? C64 H78 0.9900 . ? C65 H79 0.9900 . ? C65 H80 0.9900 . ? O9 C66 1.442(7) . ? O9 C69 1.455(7) . ? C66 C67 1.493(9) . ? C66 H81 0.9900 . ? C66 H82 0.9900 . ? C67 C68 1.539(11) . ? C67 H83 0.9900 . ? C67 H84 0.9900 . ? C68 C69 1.517(9) . ? C68 H85 0.9900 . ? C68 H86 0.9900 . ? C69 H87 0.9900 . ? C69 H88 0.9900 . ? O10 C70 1.432(12) . ? O10 C77 1.483(17) . ? O10 C73 1.489(16) . ? O10 C74 1.557(19) . ? C70 C71 1.488(16) . ? C71 C72 1.541(18) . ? C72 C73 1.52(2) . ? C74 C75 1.38(3) . ? C75 C76 1.51(3) . ? C76 C77 1.52(2) . ? O11 C78 1.451(12) . ? O11 C81 1.514(15) . ? C78 C79 1.570(13) . ? C79 C80 1.565(14) . ? C80 C81 1.484(16) . ? O12 C85 1.50(2) . ? O12 C82 1.623(19) . ? C82 C83 1.54(2) . ? C83 C84 1.48(2) . ? C84 C85 1.43(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zr1 O1 102.15(15) . . ? O5 Zr1 O2 87.70(15) . . ? O1 Zr1 O2 158.72(15) . . ? O5 Zr1 O7 81.68(14) . . ? O1 Zr1 O7 78.85(15) . . ? O2 Zr1 O7 84.07(15) . . ? O5 Zr1 O8 156.76(14) . . ? O1 Zr1 O8 86.86(14) . . ? O2 Zr1 O8 77.46(15) . . ? O7 Zr1 O8 79.10(14) . . ? O5 Zr1 C6 118.26(16) . . ? O1 Zr1 C6 85.66(17) . . ? O2 Zr1 C6 106.43(17) . . ? O7 Zr1 C6 157.17(17) . . ? O8 Zr1 C6 83.44(16) . . ? O5 Zr1 C5 102.60(17) . . ? O1 Zr1 C5 118.63(17) . . ? O2 Zr1 C5 76.53(17) . . ? O7 Zr1 C5 159.87(17) . . ? O8 Zr1 C5 91.35(17) . . ? C6 Zr1 C5 33.50(18) . . ? O5 Zr1 C4 71.56(15) . . ? O1 Zr1 C4 130.63(16) . . ? O2 Zr1 C4 70.28(17) . . ? O7 Zr1 C4 143.13(16) . . ? O8 Zr1 C4 118.50(16) . . ? C6 Zr1 C4 59.12(17) . . ? C5 Zr1 C4 31.54(17) . . ? O5 Zr1 C1 95.07(15) . . ? O1 Zr1 C1 66.95(16) . . ? O2 Zr1 C1 131.60(16) . . ? O7 Zr1 C1 144.21(16) . . ? O8 Zr1 C1 108.17(15) . . ? C6 Zr1 C1 32.59(17) . . ? C5 Zr1 C1 55.66(18) . . ? C4 Zr1 C1 65.07(17) . . ? C7 O1 Zr1 132.3(3) . . ? C13 O2 Zr1 122.7(3) . . ? C2 C1 C6 122.4(5) . . ? C2 C1 C12 118.1(5) . . ? C6 C1 C12 118.1(5) . . ? C2 C1 Zr1 85.7(3) . . ? C6 C1 Zr1 65.6(3) . . ? C12 C1 Zr1 108.3(3) . . ? C1 C2 C3 126.3(5) . . ? C1 C2 H1 116.8 . . ? C3 C2 H1 116.8 . . ? C2 C3 C4 108.0(4) . . ? C2 C3 C57 103.8(4) . . ? C4 C3 C57 111.1(4) . . ? C2 C3 H2 111.2 . . ? C4 C3 H2 111.2 . . ? C57 C3 H2 111.2 . . ? C5 C4 C14 116.7(5) . . ? C5 C4 C3 122.6(5) . . ? C14 C4 C3 120.6(5) . . ? C5 C4 Zr1 71.6(3) . . ? C14 C4 Zr1 105.7(3) . . ? C3 C4 Zr1 90.2(3) . . ? C4 C5 C6 123.8(5) . . ? C4 C5 Zr1 76.9(3) . . ? C6 C5 Zr1 71.0(3) . . ? C4 C5 H3 118.1 . . ? C6 C5 H3 118.1 . . ? Zr1 C5 H3 125.8 . . ? C5 C6 C1 114.2(5) . . ? C5 C6 Zr1 75.5(3) . . ? C1 C6 Zr1 81.8(3) . . ? C5 C6 H4 122.9 . . ? C1 C6 H4 122.9 . . ? Zr1 C6 H4 111.3 . . ? O1 C7 C8 122.5(5) . . ? O1 C7 C12 118.0(5) . . ? C8 C7 C12 119.5(5) . . ? C9 C8 C7 116.8(5) . . ? C9 C8 C19 121.5(5) . . ? C7 C8 C19 121.6(5) . . ? C8 C9 C10 124.4(6) . . ? C8 C9 H5 117.8 . . ? C10 C9 H5 117.8 . . ? C11 C10 C9 117.1(5) . . ? C11 C10 C23 121.2(6) . . ? C9 C10 C23 121.6(6) . . ? C12 C11 C10 120.8(6) . . ? C12 C11 H6 119.6 . . ? C10 C11 H6 119.6 . . ? C11 C12 C7 121.3(5) . . ? C11 C12 C1 125.1(5) . . ? C7 C12 C1 113.5(5) . . ? O2 C13 C14 118.9(5) . . ? O2 C13 C18 121.9(5) . . ? C14 C13 C18 119.1(5) . . ? C15 C14 C13 121.0(5) . . ? C15 C14 C4 123.2(5) . . ? C13 C14 C4 115.8(5) . . ? C16 C15 C14 121.3(6) . . ? C16 C15 H7 119.3 . . ? C14 C15 H7 119.3 . . ? C15 C16 C17 117.4(5) . . ? C15 C16 C28 121.6(6) . . ? C17 C16 C28 120.9(6) . . ? C16 C17 C18 124.3(6) . . ? C16 C17 H8 117.8 . . ? C18 C17 H8 117.8 . . ? C17 C18 C13 116.5(5) . . ? C17 C18 C24 122.1(5) . . ? C13 C18 C24 121.4(5) . . ? C22 C19 C8 112.8(6) . . ? C22 C19 C21 107.3(6) . . ? C8 C19 C21 110.8(5) . . ? C22 C19 C20 107.9(6) . . ? C8 C19 C20 108.5(5) . . ? C21 C19 C20 109.4(6) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C10 C23 H18 109.5 . . ? C10 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? C10 C23 H20 109.5 . . ? H18 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C18 C24 C26 111.4(6) . . ? C18 C24 C27 112.6(5) . . ? C26 C24 C27 108.6(5) . . ? C18 C24 C25 107.8(5) . . ? C26 C24 C25 109.1(6) . . ? C27 C24 C25 107.1(6) . . ? C24 C25 H21 109.5 . . ? C24 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C26 H24 109.5 . . ? C24 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C24 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C16 C28 H30 109.5 . . ? C16 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C16 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? O6 Zr2 O3 103.45(15) . . ? O6 Zr2 O4 87.71(15) . . ? O3 Zr2 O4 156.11(15) . . ? O6 Zr2 O9 82.21(15) . . ? O3 Zr2 O9 78.95(15) . . ? O4 Zr2 O9 81.80(14) . . ? O6 Zr2 O10 158.66(14) . . ? O3 Zr2 O10 83.33(14) . . ? O4 Zr2 O10 79.29(14) . . ? O9 Zr2 O10 79.26(14) . . ? O6 Zr2 C34 118.30(17) . . ? O3 Zr2 C34 86.06(17) . . ? O4 Zr2 C34 107.41(17) . . ? O9 Zr2 C34 157.17(17) . . ? O10 Zr2 C34 82.00(16) . . ? O6 Zr2 C33 103.62(17) . . ? O3 Zr2 C33 118.58(17) . . ? O4 Zr2 C33 77.95(17) . . ? O9 Zr2 C33 158.62(17) . . ? O10 Zr2 C33 90.22(16) . . ? C34 Zr2 C33 32.77(18) . . ? O6 Zr2 C32 71.80(16) . . ? O3 Zr2 C32 131.73(16) . . ? O4 Zr2 C32 71.65(16) . . ? O9 Zr2 C32 143.11(16) . . ? O10 Zr2 C32 118.82(16) . . ? C34 Zr2 C32 58.76(18) . . ? C33 Zr2 C32 32.29(17) . . ? O6 Zr2 C29 95.63(16) . . ? O3 Zr2 C29 67.36(16) . . ? O4 Zr2 C29 133.34(16) . . ? O9 Zr2 C29 144.82(17) . . ? O10 Zr2 C29 105.61(15) . . ? C34 Zr2 C29 32.62(17) . . ? C33 Zr2 C29 55.97(18) . . ? C32 Zr2 C29 65.50(18) . . ? C35 O3 Zr2 132.1(3) . . ? C41 O4 Zr2 121.6(3) . . ? C30 C29 C34 121.3(5) . . ? C30 C29 C40 118.1(5) . . ? C34 C29 C40 119.5(5) . . ? C30 C29 Zr2 85.8(3) . . ? C34 C29 Zr2 66.8(3) . . ? C40 C29 Zr2 108.2(4) . . ? C29 C30 C31 126.7(5) . . ? C29 C30 H33 116.6 . . ? C31 C30 H33 116.6 . . ? C30 C31 C32 107.2(4) . . ? C30 C31 C57 103.4(4) . . ? C32 C31 C57 111.3(4) . . ? C30 C31 H34 111.5 . . ? C32 C31 H34 111.5 . . ? C57 C31 H34 111.5 . . ? C33 C32 C42 115.5(5) . . ? C33 C32 C31 123.3(5) . . ? C42 C32 C31 121.2(5) . . ? C33 C32 Zr2 72.6(3) . . ? C42 C32 Zr2 105.6(3) . . ? C31 C32 Zr2 91.0(3) . . ? C32 C33 C34 122.1(5) . . ? C32 C33 Zr2 75.1(3) . . ? C34 C33 Zr2 72.0(3) . . ? C32 C33 H35 119.0 . . ? C34 C33 H35 119.0 . . ? Zr2 C33 H35 125.7 . . ? C33 C34 C29 116.3(5) . . ? C33 C34 Zr2 75.2(3) . . ? C29 C34 Zr2 80.6(3) . . ? C33 C34 H36 121.8 . . ? C29 C34 H36 121.8 . . ? Zr2 C34 H36 113.4 . . ? O3 C35 C40 118.0(5) . . ? O3 C35 C36 122.9(5) . . ? C40 C35 C36 119.1(5) . . ? C37 C36 C35 117.3(6) . . ? C37 C36 C47 122.3(5) . . ? C35 C36 C47 120.2(5) . . ? C36 C37 C38 124.6(6) . . ? C36 C37 H37 117.7 . . ? C38 C37 H37 117.7 . . ? C39 C38 C37 117.5(6) . . ? C39 C38 C51 121.6(7) . . ? C37 C38 C51 120.8(6) . . ? C38 C39 C40 120.4(6) . . ? C38 C39 H38 119.8 . . ? C40 C39 H38 119.8 . . ? C39 C40 C35 121.0(6) . . ? C39 C40 C29 124.8(6) . . ? C35 C40 C29 113.9(5) . . ? O4 C41 C42 118.9(5) . . ? O4 C41 C46 122.5(5) . . ? C42 C41 C46 118.6(5) . . ? C43 C42 C41 120.3(5) . . ? C43 C42 C32 123.3(5) . . ? C41 C42 C32 116.3(5) . . ? C42 C43 C44 121.7(6) . . ? C42 C43 H39 119.1 . . ? C44 C43 H39 119.1 . . ? C43 C44 C45 116.9(5) . . ? C43 C44 C56 122.2(6) . . ? C45 C44 C56 120.9(6) . . ? C46 C45 C44 123.8(5) . . ? C46 C45 H40 118.1 . . ? C44 C45 H40 118.1 . . ? C45 C46 C41 117.6(5) . . ? C45 C46 C52 122.4(5) . . ? C41 C46 C52 119.9(5) . . ? C50 C47 C49 107.7(5) . . ? C50 C47 C36 112.6(5) . . ? C49 C47 C36 112.7(6) . . ? C50 C47 C48 108.6(6) . . ? C49 C47 C48 106.9(6) . . ? C36 C47 C48 108.2(5) . . ? C47 C48 H41 109.5 . . ? C47 C48 H42 109.5 . . ? H41 C48 H42 109.5 . . ? C47 C48 H43 109.5 . . ? H41 C48 H43 109.5 . . ? H42 C48 H43 109.5 . . ? C47 C49 H44 109.5 . . ? C47 C49 H45 109.5 . . ? H44 C49 H45 109.5 . . ? C47 C49 H46 109.5 . . ? H44 C49 H46 109.5 . . ? H45 C49 H46 109.5 . . ? C47 C50 H47 109.5 . . ? C47 C50 H48 109.5 . . ? H47 C50 H48 109.5 . . ? C47 C50 H49 109.5 . . ? H47 C50 H49 109.5 . . ? H48 C50 H49 109.5 . . ? C38 C51 H50 109.5 . . ? C38 C51 H51 109.5 . . ? H50 C51 H51 109.5 . . ? C38 C51 H52 109.5 . . ? H50 C51 H52 109.5 . . ? H51 C51 H52 109.5 . . ? C54 C52 C46 111.4(5) . . ? C54 C52 C53 110.1(6) . . ? C46 C52 C53 109.1(5) . . ? C54 C52 C55 107.0(5) . . ? C46 C52 C55 112.0(5) . . ? C53 C52 C55 107.1(6) . . ? C52 C53 H53 109.5 . . ? C52 C53 H54 109.5 . . ? H53 C53 H54 109.5 . . ? C52 C53 H55 109.5 . . ? H53 C53 H55 109.5 . . ? H54 C53 H55 109.5 . . ? C52 C54 H56 109.5 . . ? C52 C54 H57 109.5 . . ? H56 C54 H57 109.5 . . ? C52 C54 H58 109.5 . . ? H56 C54 H58 109.5 . . ? H57 C54 H58 109.5 . . ? C52 C55 H59 109.5 . . ? C52 C55 H60 109.5 . . ? H59 C55 H60 109.5 . . ? C52 C55 H61 109.5 . . ? H59 C55 H61 109.5 . . ? H60 C55 H61 109.5 . . ? C44 C56 H62 109.5 . . ? C44 C56 H63 109.5 . . ? H62 C56 H63 109.5 . . ? C44 C56 H64 109.5 . . ? H62 C56 H64 109.5 . . ? H63 C56 H64 109.5 . . ? O6 C57 O5 108.7(4) . . ? O6 C57 C31 104.1(4) . . ? O5 C57 C31 110.1(4) . . ? O6 C57 C3 110.3(4) . . ? O5 C57 C3 103.6(4) . . ? C31 C57 C3 119.8(4) . . ? C57 O5 Zr1 127.5(3) . . ? C57 O6 Zr2 126.4(3) . . ? C61 O7 C58 108.1(5) . . ? C61 O7 Zr1 129.8(4) . . ? C58 O7 Zr1 122.1(3) . . ? O7 C58 C59 106.2(6) . . ? O7 C58 H65 110.5 . . ? C59 C58 H65 110.5 . . ? O7 C58 H66 110.5 . . ? C59 C58 H66 110.5 . . ? H65 C58 H66 108.7 . . ? C58 C59 C60 102.2(7) . . ? C58 C59 H67 111.3 . . ? C60 C59 H67 111.3 . . ? C58 C59 H68 111.3 . . ? C60 C59 H68 111.3 . . ? H67 C59 H68 109.2 . . ? C61 C60 C59 103.7(6) . . ? C61 C60 H69 111.0 . . ? C59 C60 H69 111.0 . . ? C61 C60 H70 111.0 . . ? C59 C60 H70 111.0 . . ? H69 C60 H70 109.0 . . ? O7 C61 C60 106.6(5) . . ? O7 C61 H71 110.4 . . ? C60 C61 H71 110.4 . . ? O7 C61 H72 110.4 . . ? C60 C61 H72 110.4 . . ? H71 C61 H72 108.6 . . ? C65 O8 C62 105.9(5) . . ? C65 O8 Zr1 123.6(3) . . ? C62 O8 Zr1 128.1(4) . . ? C63 C62 O8 110.0(6) . . ? C63 C62 H73 109.7 . . ? O8 C62 H73 109.7 . . ? C63 C62 H74 109.7 . . ? O8 C62 H74 109.7 . . ? H73 C62 H74 108.2 . . ? C62 C63 C64 107.5(6) . . ? C62 C63 H75 110.2 . . ? C64 C63 H75 110.2 . . ? C62 C63 H76 110.2 . . ? C64 C63 H76 110.2 . . ? H75 C63 H76 108.5 . . ? C63 C64 C65 104.5(6) . . ? C63 C64 H77 110.9 . . ? C65 C64 H77 110.9 . . ? C63 C64 H78 110.9 . . ? C65 C64 H78 110.9 . . ? H77 C64 H78 108.9 . . ? O8 C65 C64 106.0(5) . . ? O8 C65 H79 110.5 . . ? C64 C65 H79 110.5 . . ? O8 C65 H80 110.5 . . ? C64 C65 H80 110.5 . . ? H79 C65 H80 108.7 . . ? C66 O9 C69 110.2(5) . . ? C66 O9 Zr2 128.5(4) . . ? C69 O9 Zr2 121.2(3) . . ? O9 C66 C67 106.6(6) . . ? O9 C66 H81 110.4 . . ? C67 C66 H81 110.4 . . ? O9 C66 H82 110.4 . . ? C67 C66 H82 110.4 . . ? H81 C66 H82 108.6 . . ? C66 C67 C68 103.6(6) . . ? C66 C67 H83 111.0 . . ? C68 C67 H83 111.0 . . ? C66 C67 H84 111.0 . . ? C68 C67 H84 111.0 . . ? H83 C67 H84 109.0 . . ? C69 C68 C67 101.8(6) . . ? C69 C68 H85 111.4 . . ? C67 C68 H85 111.4 . . ? C69 C68 H86 111.4 . . ? C67 C68 H86 111.4 . . ? H85 C68 H86 109.3 . . ? O9 C69 C68 104.5(5) . . ? O9 C69 H87 110.9 . . ? C68 C69 H87 110.9 . . ? O9 C69 H88 110.9 . . ? C68 C69 H88 110.9 . . ? H87 C69 H88 108.9 . . ? C70 O10 C73 107.4(8) . . ? C77 O10 C74 107.9(9) . . ? C70 O10 Zr2 128.3(5) . . ? C77 O10 Zr2 119.9(7) . . ? C73 O10 Zr2 123.8(7) . . ? C74 O10 Zr2 119.9(7) . . ? O10 C70 C71 109.4(9) . . ? C70 C71 C72 103.9(10) . . ? C73 C72 C71 101.9(11) . . ? O10 C73 C72 104.2(11) . . ? C75 C74 O10 107.0(14) . . ? C74 C75 C76 111.7(18) . . ? C75 C76 C77 106.0(15) . . ? O10 C77 C76 105.7(12) . . ? C78 O11 C81 109.9(9) . . ? O11 C78 C79 102.7(8) . . ? C78 C79 C80 106.5(8) . . ? C81 C80 C79 100.8(9) . . ? C80 C81 O11 109.8(11) . . ? C85 O12 C82 97.8(13) . . ? C83 C82 O12 95.7(12) . . ? C84 C83 C82 115.3(15) . . ? C85 C84 C83 96.3(18) . . ? C84 C85 O12 107.2(18) . . ? 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 C1 C2 C3 3.4(9) . . . . ? C12 C1 C2 C3 -162.5(5) . . . . ? Zr1 C1 C2 C3 -54.0(5) . . . . ? C1 C2 C3 C4 1.6(7) . . . . ? C1 C2 C3 C57 119.5(6) . . . . ? C2 C3 C4 C5 -13.5(7) . . . . ? C57 C3 C4 C5 -126.7(5) . . . . ? C2 C3 C4 C14 162.9(5) . . . . ? C57 C3 C4 C14 49.7(6) . . . . ? C2 C3 C4 Zr1 54.5(4) . . . . ? C57 C3 C4 Zr1 -58.7(4) . . . . ? C14 C4 C5 C6 -154.9(5) . . . . ? C3 C4 C5 C6 21.7(8) . . . . ? Zr1 C4 C5 C6 -56.1(5) . . . . ? C14 C4 C5 Zr1 -98.7(4) . . . . ? C3 C4 C5 Zr1 77.9(5) . . . . ? C4 C5 C6 C1 -15.1(8) . . . . ? Zr1 C5 C6 C1 -73.8(4) . . . . ? C4 C5 C6 Zr1 58.8(5) . . . . ? C2 C1 C6 C5 2.6(8) . . . . ? C12 C1 C6 C5 168.6(5) . . . . ? Zr1 C1 C6 C5 69.9(4) . . . . ? C2 C1 C6 Zr1 -67.4(5) . . . . ? C12 C1 C6 Zr1 98.6(4) . . . . ? Zr1 O1 C7 C8 -175.2(4) . . . . ? Zr1 O1 C7 C12 4.9(7) . . . . ? O1 C7 C8 C9 177.5(5) . . . . ? C12 C7 C8 C9 -2.6(8) . . . . ? O1 C7 C8 C19 -7.1(8) . . . . ? C12 C7 C8 C19 172.8(5) . . . . ? C7 C8 C9 C10 0.9(9) . . . . ? C19 C8 C9 C10 -174.5(6) . . . . ? C8 C9 C10 C11 0.9(9) . . . . ? C8 C9 C10 C23 -175.7(6) . . . . ? C9 C10 C11 C12 -1.0(8) . . . . ? C23 C10 C11 C12 175.6(6) . . . . ? C10 C11 C12 C7 -0.7(8) . . . . ? C10 C11 C12 C1 177.2(5) . . . . ? O1 C7 C12 C11 -177.5(5) . . . . ? C8 C7 C12 C11 2.6(8) . . . . ? O1 C7 C12 C1 4.3(7) . . . . ? C8 C7 C12 C1 -175.5(5) . . . . ? C2 C1 C12 C11 -91.5(7) . . . . ? C6 C1 C12 C11 102.0(7) . . . . ? Zr1 C1 C12 C11 173.5(4) . . . . ? C2 C1 C12 C7 86.6(6) . . . . ? C6 C1 C12 C7 -80.0(6) . . . . ? Zr1 C1 C12 C7 -8.4(5) . . . . ? Zr1 O2 C13 C14 27.6(7) . . . . ? Zr1 O2 C13 C18 -150.0(4) . . . . ? O2 C13 C14 C15 175.1(5) . . . . ? C18 C13 C14 C15 -7.2(8) . . . . ? O2 C13 C14 C4 -6.9(7) . . . . ? C18 C13 C14 C4 170.8(5) . . . . ? C5 C4 C14 C15 -115.9(6) . . . . ? C3 C4 C14 C15 67.4(7) . . . . ? Zr1 C4 C14 C15 167.2(4) . . . . ? C5 C4 C14 C13 66.1(7) . . . . ? C3 C4 C14 C13 -110.6(6) . . . . ? Zr1 C4 C14 C13 -10.8(5) . . . . ? C13 C14 C15 C16 3.7(9) . . . . ? C4 C14 C15 C16 -174.1(5) . . . . ? C14 C15 C16 C17 1.1(9) . . . . ? C14 C15 C16 C28 176.6(6) . . . . ? C15 C16 C17 C18 -2.3(9) . . . . ? C28 C16 C17 C18 -178.0(6) . . . . ? C16 C17 C18 C13 -1.1(9) . . . . ? C16 C17 C18 C24 175.7(6) . . . . ? O2 C13 C18 C17 -176.6(5) . . . . ? C14 C13 C18 C17 5.8(8) . . . . ? O2 C13 C18 C24 6.6(8) . . . . ? C14 C13 C18 C24 -171.0(5) . . . . ? C9 C8 C19 C22 -7.5(9) . . . . ? C7 C8 C19 C22 177.3(6) . . . . ? C9 C8 C19 C21 -127.9(6) . . . . ? C7 C8 C19 C21 57.0(8) . . . . ? C9 C8 C19 C20 112.0(6) . . . . ? C7 C8 C19 C20 -63.2(7) . . . . ? C17 C18 C24 C26 122.3(6) . . . . ? C13 C18 C24 C26 -61.1(7) . . . . ? C17 C18 C24 C27 -0.1(8) . . . . ? C13 C18 C24 C27 176.6(6) . . . . ? C17 C18 C24 C25 -118.0(6) . . . . ? C13 C18 C24 C25 58.6(7) . . . . ? C34 C29 C30 C31 6.5(9) . . . . ? C40 C29 C30 C31 -161.4(5) . . . . ? Zr2 C29 C30 C31 -53.0(5) . . . . ? C29 C30 C31 C32 1.3(7) . . . . ? C29 C30 C31 C57 119.0(6) . . . . ? C30 C31 C32 C33 -15.3(7) . . . . ? C57 C31 C32 C33 -127.7(5) . . . . ? C30 C31 C32 C42 163.5(5) . . . . ? C57 C31 C32 C42 51.1(6) . . . . ? C30 C31 C32 Zr2 54.5(4) . . . . ? C57 C31 C32 Zr2 -57.9(4) . . . . ? C42 C32 C33 C34 -156.5(5) . . . . ? C31 C32 C33 C34 22.4(8) . . . . ? Zr2 C32 C33 C34 -57.1(5) . . . . ? C42 C32 C33 Zr2 -99.4(4) . . . . ? C31 C32 C33 Zr2 79.4(5) . . . . ? C32 C33 C34 C29 -12.9(8) . . . . ? Zr2 C33 C34 C29 -71.4(4) . . . . ? C32 C33 C34 Zr2 58.5(5) . . . . ? C30 C29 C34 C33 -1.1(8) . . . . ? C40 C29 C34 C33 166.7(5) . . . . ? Zr2 C29 C34 C33 68.2(4) . . . . ? C30 C29 C34 Zr2 -69.3(5) . . . . ? C40 C29 C34 Zr2 98.5(5) . . . . ? Zr2 O3 C35 C40 0.4(7) . . . . ? Zr2 O3 C35 C36 -178.1(4) . . . . ? O3 C35 C36 C37 -178.4(5) . . . . ? C40 C35 C36 C37 3.1(8) . . . . ? O3 C35 C36 C47 -3.5(8) . . . . ? C40 C35 C36 C47 178.0(5) . . . . ? C35 C36 C37 C38 -2.0(9) . . . . ? C47 C36 C37 C38 -176.8(6) . . . . ? C36 C37 C38 C39 0.0(10) . . . . ? C36 C37 C38 C51 -179.8(7) . . . . ? C37 C38 C39 C40 0.9(10) . . . . ? C51 C38 C39 C40 -179.3(7) . . . . ? C38 C39 C40 C35 0.3(9) . . . . ? C38 C39 C40 C29 172.6(6) . . . . ? O3 C35 C40 C39 179.1(5) . . . . ? C36 C35 C40 C39 -2.3(8) . . . . ? O3 C35 C40 C29 6.0(7) . . . . ? C36 C35 C40 C29 -175.4(5) . . . . ? C30 C29 C40 C39 -85.5(8) . . . . ? C34 C29 C40 C39 106.3(7) . . . . ? Zr2 C29 C40 C39 179.4(5) . . . . ? C30 C29 C40 C35 87.3(6) . . . . ? C34 C29 C40 C35 -80.9(7) . . . . ? Zr2 C29 C40 C35 -7.8(6) . . . . ? Zr2 O4 C41 C42 26.4(6) . . . . ? Zr2 O4 C41 C46 -152.9(4) . . . . ? O4 C41 C42 C43 172.1(5) . . . . ? C46 C41 C42 C43 -8.5(8) . . . . ? O4 C41 C42 C32 -7.7(7) . . . . ? C46 C41 C42 C32 171.7(5) . . . . ? C33 C32 C42 C43 -111.5(6) . . . . ? C31 C32 C42 C43 69.6(7) . . . . ? Zr2 C32 C42 C43 170.7(4) . . . . ? C33 C32 C42 C41 68.3(6) . . . . ? C31 C32 C42 C41 -110.6(6) . . . . ? Zr2 C32 C42 C41 -9.6(5) . . . . ? C41 C42 C43 C44 -0.1(8) . . . . ? C32 C42 C43 C44 179.7(5) . . . . ? C42 C43 C44 C45 7.1(8) . . . . ? C42 C43 C44 C56 -173.0(5) . . . . ? C43 C44 C45 C46 -5.6(9) . . . . ? C56 C44 C45 C46 174.5(6) . . . . ? C44 C45 C46 C41 -2.8(8) . . . . ? C44 C45 C46 C52 174.2(5) . . . . ? O4 C41 C46 C45 -170.9(5) . . . . ? C42 C41 C46 C45 9.8(8) . . . . ? O4 C41 C46 C52 12.0(8) . . . . ? C42 C41 C46 C52 -167.3(5) . . . . ? C37 C36 C47 C50 -130.4(6) . . . . ? C35 C36 C47 C50 54.9(7) . . . . ? C37 C36 C47 C49 -8.3(8) . . . . ? C35 C36 C47 C49 177.0(5) . . . . ? C37 C36 C47 C48 109.7(7) . . . . ? C35 C36 C47 C48 -65.0(7) . . . . ? C45 C46 C52 C54 117.9(6) . . . . ? C41 C46 C52 C54 -65.1(7) . . . . ? C45 C46 C52 C53 -120.3(6) . . . . ? C41 C46 C52 C53 56.7(7) . . . . ? C45 C46 C52 C55 -1.9(8) . . . . ? C41 C46 C52 C55 175.0(6) . . . . ? C30 C31 C57 O6 -71.8(5) . . . . ? C32 C31 C57 O6 42.9(5) . . . . ? C30 C31 C57 O5 44.5(5) . . . . ? C32 C31 C57 O5 159.3(4) . . . . ? C30 C31 C57 C3 164.4(4) . . . . ? C32 C31 C57 C3 -80.8(6) . . . . ? C2 C3 C57 O6 46.0(5) . . . . ? C4 C3 C57 O6 161.8(4) . . . . ? C2 C3 C57 O5 -70.1(5) . . . . ? C4 C3 C57 O5 45.6(5) . . . . ? C2 C3 C57 C31 166.7(4) . . . . ? C4 C3 C57 C31 -77.5(6) . . . . ? O6 C57 O5 Zr1 -111.1(4) . . . . ? C31 C57 O5 Zr1 135.5(4) . . . . ? C3 C57 O5 Zr1 6.2(5) . . . . ? O5 C57 O6 Zr2 -108.8(4) . . . . ? C31 C57 O6 Zr2 8.5(5) . . . . ? C3 C57 O6 Zr2 138.2(3) . . . . ? C61 O7 C58 C59 -33.5(8) . . . . ? Zr1 O7 C58 C59 144.2(6) . . . . ? O7 C58 C59 C60 36.5(9) . . . . ? C58 C59 C60 C61 -26.6(10) . . . . ? C58 O7 C61 C60 14.9(8) . . . . ? Zr1 O7 C61 C60 -162.6(5) . . . . ? C59 C60 C61 O7 7.5(10) . . . . ? C65 O8 C62 C63 -19.9(10) . . . . ? Zr1 O8 C62 C63 142.8(6) . . . . ? O8 C62 C63 C64 6.2(11) . . . . ? C62 C63 C64 C65 9.3(10) . . . . ? C62 O8 C65 C64 25.1(8) . . . . ? Zr1 O8 C65 C64 -138.6(5) . . . . ? C63 C64 C65 O8 -21.2(8) . . . . ? C69 O9 C66 C67 3.7(8) . . . . ? Zr2 O9 C66 C67 -179.6(5) . . . . ? O9 C66 C67 C68 -24.8(8) . . . . ? C66 C67 C68 C69 35.6(8) . . . . ? C66 O9 C69 C68 19.4(7) . . . . ? Zr2 O9 C69 C68 -157.6(4) . . . . ? C67 C68 C69 O9 -33.5(7) . . . . ? C77 O10 C70 C71 7.4(14) . . . . ? C73 O10 C70 C71 -6.1(13) . . . . ? C74 O10 C70 C71 99(3) . . . . ? Zr2 O10 C70 C71 166.3(6) . . . . ? O10 C70 C71 C72 -16.6(14) . . . . ? C70 C71 C72 C73 31.8(14) . . . . ? C70 O10 C73 C72 26.7(13) . . . . ? C77 O10 C73 C72 -70(5) . . . . ? C74 O10 C73 C72 8.1(14) . . . . ? Zr2 O10 C73 C72 -146.1(8) . . . . ? C71 C72 C73 O10 -35.7(13) . . . . ? C70 O10 C74 C75 -101(3) . . . . ? C77 O10 C74 C75 -5.8(19) . . . . ? C73 O10 C74 C75 -19.0(19) . . . . ? Zr2 O10 C74 C75 136.4(13) . . . . ? O10 C74 C75 C76 -3(2) . . . . ? C74 C75 C76 C77 11(2) . . . . ? C70 O10 C77 C76 30.8(15) . . . . ? C73 O10 C77 C76 119(6) . . . . ? C74 O10 C77 C76 12.0(16) . . . . ? Zr2 O10 C77 C76 -130.1(11) . . . . ? C75 C76 C77 O10 -13.6(19) . . . . ? C81 O11 C78 C79 16.1(11) . . . . ? O11 C78 C79 C80 -29.9(10) . . . . ? C78 C79 C80 C81 31.6(11) . . . . ? C79 C80 C81 O11 -21.8(13) . . . . ? C78 O11 C81 C80 3.9(14) . . . . ? C85 O12 C82 C83 34.2(15) . . . . ? O12 C82 C83 C84 -9.0(19) . . . . ? C82 C83 C84 C85 -22(2) . . . . ? C83 C84 C85 O12 47(2) . . . . ? C82 O12 C85 C84 -54.7(19) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 138 25 ' ' 2 0.337 0.029 0.431 13 1 ' ' 3 0.500 0.500 0.500 138 25 ' ' 4 0.337 0.471 0.931 13 1 ' ' 5 0.663 0.529 0.069 13 1 ' ' 6 0.663 0.971 0.569 13 1 ' ' _platon_squeeze_details ; ; _refine_diff_density_max 1.579 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.114 _database_code_depnum_ccdc_archive 'CCDC 962321' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_{[(C6H4)(ArO)2Zr]2(C2S4)(thf)2}4(toluene) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H80 O6 S4 Zr2, 4(C7 H8)' _chemical_formula_sum 'C94 H112 O6 S4 Zr2' _chemical_formula_weight 1648.52 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 9.498(3) _cell_length_b 14.156(5) _cell_length_c 16.469(5) _cell_angle_alpha 77.889(15) _cell_angle_beta 80.28(2) _cell_angle_gamma 80.586(14) _cell_volume 2114.9(12) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5127 _cell_measurement_theta_min 3.0006 _cell_measurement_theta_max 27.4468 _exptl_crystal_description Platelet _exptl_crystal_colour Blue _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9247 _exptl_absorpt_correction_T_max 0.9247 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Saturn CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 26318 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1033 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9639 _reflns_number_gt 6469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+3.0523P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9639 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1647 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.33297(5) 0.06874(3) 0.34232(3) 0.02434(14) Uani 1 1 d . . . O1 O 0.4293(3) -0.0552(2) 0.30744(19) 0.0260(7) Uani 1 1 d . . . O2 O 0.2234(3) 0.2017(2) 0.32140(19) 0.0275(7) Uani 1 1 d . . . C1 C 0.4309(5) 0.0255(3) 0.1431(3) 0.0245(10) Uani 1 1 d . . . C2 C 0.4974(5) 0.0956(3) 0.1675(3) 0.0249(10) Uani 1 1 d . . . H1 H 0.5916 0.0797 0.1794 0.030 Uiso 1 1 calc R . . C3 C 0.4249(5) 0.1873(3) 0.1738(3) 0.0262(10) Uani 1 1 d . . . H2 H 0.4694 0.2320 0.1911 0.031 Uiso 1 1 calc R . . C4 C 0.2835(5) 0.2126(3) 0.1540(3) 0.0246(10) Uani 1 1 d . . . C5 C 0.2252(5) 0.1492(3) 0.1193(3) 0.0268(10) Uani 1 1 d . . . H3 H 0.1367 0.1687 0.0997 0.032 Uiso 1 1 calc R . . C6 C 0.2983(5) 0.0564(3) 0.1135(3) 0.0253(10) Uani 1 1 d . . . H4 H 0.2585 0.0148 0.0897 0.030 Uiso 1 1 calc R . . C7 C 0.4813(5) -0.1174(3) 0.2522(3) 0.0239(9) Uani 1 1 d . . . C8 C 0.5283(5) -0.2171(3) 0.2797(3) 0.0251(10) Uani 1 1 d . . . C9 C 0.5687(5) -0.2751(3) 0.2181(3) 0.0263(10) Uani 1 1 d . . . H5 H 0.5970 -0.3414 0.2353 0.032 Uiso 1 1 calc R . . C10 C 0.5688(5) -0.2390(3) 0.1328(3) 0.0265(10) Uani 1 1 d . . . C11 C 0.5267(5) -0.1398(3) 0.1072(3) 0.0260(10) Uani 1 1 d . . . H6 H 0.5265 -0.1139 0.0504 0.031 Uiso 1 1 calc R . . C12 C 0.4847(5) -0.0786(3) 0.1659(3) 0.0255(10) Uani 1 1 d . . . C13 C 0.1587(5) 0.2831(3) 0.2748(3) 0.0245(10) Uani 1 1 d . . . C14 C 0.1885(5) 0.2946(3) 0.1865(3) 0.0272(10) Uani 1 1 d . . . C15 C 0.1227(5) 0.3733(3) 0.1361(3) 0.0291(11) Uani 1 1 d . . . H7 H 0.1443 0.3799 0.0782 0.035 Uiso 1 1 calc R . . C16 C 0.0236(5) 0.4440(3) 0.1705(3) 0.0307(11) Uani 1 1 d . . . C17 C -0.0043(5) 0.4322(3) 0.2575(3) 0.0293(11) Uani 1 1 d . . . H8 H -0.0691 0.4794 0.2807 0.035 Uiso 1 1 calc R . . C18 C 0.0594(5) 0.3534(3) 0.3122(3) 0.0265(10) Uani 1 1 d . . . C19 C 0.5382(5) -0.2604(3) 0.3729(3) 0.0270(10) Uani 1 1 d . . . C20 C 0.6419(5) -0.2060(3) 0.4026(3) 0.0338(11) Uani 1 1 d . . . H9 H 0.6371 -0.2236 0.4625 0.051 Uiso 1 1 calc R . . H10 H 0.6148 -0.1369 0.3870 0.051 Uiso 1 1 calc R . . H11 H 0.7385 -0.2235 0.3769 0.051 Uiso 1 1 calc R . . C21 C 0.5973(6) -0.3688(3) 0.3867(3) 0.0339(11) Uani 1 1 d . . . H12 H 0.6902 -0.3780 0.3536 0.051 Uiso 1 1 calc R . . H13 H 0.5326 -0.4044 0.3701 0.051 Uiso 1 1 calc R . . H14 H 0.6063 -0.3922 0.4449 0.051 Uiso 1 1 calc R . . C22 C 0.3907(5) -0.2498(4) 0.4264(3) 0.0337(11) Uani 1 1 d . . . H15 H 0.3237 -0.2775 0.4037 0.050 Uiso 1 1 calc R . . H16 H 0.3573 -0.1819 0.4261 0.050 Uiso 1 1 calc R . . H17 H 0.3984 -0.2831 0.4829 0.050 Uiso 1 1 calc R . . C23 C 0.6138(6) -0.3054(4) 0.0688(3) 0.0356(12) Uani 1 1 d . . . H18 H 0.7109 -0.2985 0.0428 0.053 Uiso 1 1 calc R . . H19 H 0.5505 -0.2878 0.0267 0.053 Uiso 1 1 calc R . . H20 H 0.6085 -0.3718 0.0963 0.053 Uiso 1 1 calc R . . C24 C 0.0294(5) 0.3477(4) 0.4075(3) 0.0315(11) Uani 1 1 d . . . C25 C 0.1682(6) 0.3605(4) 0.4374(3) 0.0422(14) Uani 1 1 d . . . H21 H 0.2425 0.3087 0.4251 0.063 Uiso 1 1 calc R . . H22 H 0.1510 0.3588 0.4968 0.063 Uiso 1 1 calc R . . H23 H 0.1981 0.4220 0.4091 0.063 Uiso 1 1 calc R . . C26 C -0.0222(6) 0.2507(4) 0.4538(3) 0.0455(15) Uani 1 1 d . . . H24 H -0.1068 0.2422 0.4328 0.068 Uiso 1 1 calc R . . H25 H -0.0445 0.2513 0.5127 0.068 Uiso 1 1 calc R . . H26 H 0.0525 0.1979 0.4446 0.068 Uiso 1 1 calc R . . C27 C -0.0897(6) 0.4290(4) 0.4324(3) 0.0374(12) Uani 1 1 d . . . H27 H -0.0597 0.4915 0.4076 0.056 Uiso 1 1 calc R . . H28 H -0.1064 0.4224 0.4923 0.056 Uiso 1 1 calc R . . H29 H -0.1770 0.4236 0.4126 0.056 Uiso 1 1 calc R . . C28 C -0.0524(6) 0.5295(4) 0.1161(3) 0.0431(14) Uani 1 1 d . . . H30 H -0.1212 0.5073 0.0903 0.065 Uiso 1 1 calc R . . H31 H 0.0168 0.5599 0.0734 0.065 Uiso 1 1 calc R . . H32 H -0.1015 0.5758 0.1499 0.065 Uiso 1 1 calc R . . S1 S 0.26632(12) 0.00812(9) 0.49410(7) 0.0263(3) Uani 1 1 d . . . S2 S 0.46086(12) -0.12062(8) 0.60798(7) 0.0265(3) Uani 1 1 d . . . C29 C 0.4433(5) -0.0238(3) 0.5217(3) 0.0251(10) Uani 1 1 d . . . O3 O 0.1283(3) 0.0248(2) 0.3149(2) 0.0258(7) Uani 1 1 d . . . C30 C -0.0115(5) 0.0862(4) 0.3055(3) 0.0318(11) Uani 1 1 d . . . H33 H 0.0013 0.1476 0.2677 0.038 Uiso 1 1 calc R . . H34 H -0.0614 0.0992 0.3593 0.038 Uiso 1 1 calc R . . C31 C -0.0934(6) 0.0253(4) 0.2693(4) 0.0408(13) Uani 1 1 d . . . H35 H -0.1967 0.0429 0.2820 0.049 Uiso 1 1 calc R . . H36 H -0.0669 0.0325 0.2090 0.049 Uiso 1 1 calc R . . C32 C -0.0459(5) -0.0766(4) 0.3130(4) 0.0389(13) Uani 1 1 d . . . H37 H -0.0603 -0.1245 0.2818 0.047 Uiso 1 1 calc R . . H38 H -0.0978 -0.0902 0.3693 0.047 Uiso 1 1 calc R . . C33 C 0.1129(6) -0.0759(4) 0.3148(4) 0.0400(13) Uani 1 1 d . . . H39 H 0.1435 -0.1186 0.3647 0.048 Uiso 1 1 calc R . . H40 H 0.1704 -0.0974 0.2658 0.048 Uiso 1 1 calc R . . C34 C 0.3878(8) 0.4927(5) 0.2212(6) 0.078(2) Uani 1 1 d . . . H41 H 0.4028 0.5592 0.1989 0.117 Uiso 1 1 calc R . . H42 H 0.3739 0.4822 0.2814 0.117 Uiso 1 1 calc R . . H43 H 0.3041 0.4794 0.2023 0.117 Uiso 1 1 calc R . . C35 C 0.5149(6) 0.4270(4) 0.1921(4) 0.0451(14) Uani 1 1 d . . . C36 C 0.6015(7) 0.3714(5) 0.2496(4) 0.0559(17) Uani 1 1 d . . . H44 H 0.5794 0.3744 0.3063 0.067 Uiso 1 1 calc R . . C37 C 0.7195(8) 0.3122(5) 0.2209(7) 0.079(3) Uani 1 1 d . . . H45 H 0.7770 0.2746 0.2595 0.095 Uiso 1 1 calc R . . C38 C 0.7571(8) 0.3056(6) 0.1392(7) 0.083(3) Uani 1 1 d . . . H46 H 0.8385 0.2645 0.1219 0.100 Uiso 1 1 calc R . . C39 C 0.6704(10) 0.3623(6) 0.0811(5) 0.077(2) Uani 1 1 d . . . H47 H 0.6941 0.3600 0.0244 0.092 Uiso 1 1 calc R . . C40 C 0.5503(8) 0.4214(5) 0.1090(4) 0.0607(18) Uani 1 1 d . . . H48 H 0.4917 0.4583 0.0707 0.073 Uiso 1 1 calc R . . C41 C 0.0755(8) 0.6822(5) 0.2616(5) 0.069(2) Uani 1 1 d . . . H49 H -0.0188 0.6842 0.2937 0.104 Uiso 1 1 calc R . . H50 H 0.1397 0.7039 0.2909 0.104 Uiso 1 1 calc R . . H51 H 0.1105 0.6166 0.2540 0.104 Uiso 1 1 calc R . . C42 C 0.0681(7) 0.7475(5) 0.1777(5) 0.0521(16) Uani 1 1 d . . . C43 C 0.1945(6) 0.7687(5) 0.1253(5) 0.0564(17) Uani 1 1 d . . . H52 H 0.2831 0.7420 0.1427 0.068 Uiso 1 1 calc R . . C44 C 0.1898(7) 0.8281(5) 0.0489(5) 0.0590(18) Uani 1 1 d . . . H53 H 0.2757 0.8407 0.0147 0.071 Uiso 1 1 calc R . . C45 C 0.0610(8) 0.8701(6) 0.0208(5) 0.0655(19) Uani 1 1 d . . . H54 H 0.0595 0.9100 -0.0318 0.079 Uiso 1 1 calc R . . C46 C -0.0648(8) 0.8515(6) 0.0723(5) 0.073(2) Uani 1 1 d . . . H55 H -0.1529 0.8802 0.0551 0.087 Uiso 1 1 calc R . . C47 C -0.0617(7) 0.7905(5) 0.1496(4) 0.0570(18) Uani 1 1 d . . . H56 H -0.1480 0.7779 0.1834 0.068 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 0.0236(3) 0.0240(2) 0.0241(2) -0.00513(18) -0.00441(18) 0.00269(17) O1 0.0275(18) 0.0232(16) 0.0269(17) -0.0081(13) -0.0017(13) -0.0001(13) O2 0.0267(18) 0.0267(17) 0.0269(18) -0.0031(14) -0.0056(14) 0.0024(13) C1 0.026(2) 0.027(2) 0.018(2) -0.0015(18) -0.0007(18) -0.0023(19) C2 0.021(2) 0.025(2) 0.025(2) -0.0024(18) -0.0016(18) 0.0016(18) C3 0.020(2) 0.030(3) 0.029(2) -0.008(2) -0.0035(19) -0.0003(19) C4 0.025(2) 0.026(2) 0.021(2) -0.0021(18) -0.0031(18) 0.0002(18) C5 0.022(2) 0.032(3) 0.026(2) -0.0059(19) -0.0023(19) 0.0001(19) C6 0.030(3) 0.027(2) 0.018(2) -0.0065(18) -0.0009(18) -0.0019(19) C7 0.019(2) 0.026(2) 0.026(2) -0.0092(18) -0.0006(18) 0.0021(18) C8 0.018(2) 0.024(2) 0.031(3) -0.0030(19) 0.0001(19) -0.0022(18) C9 0.024(2) 0.027(2) 0.026(2) -0.0071(19) -0.0007(19) 0.0008(19) C10 0.021(2) 0.027(2) 0.033(3) -0.010(2) -0.0020(19) -0.0018(18) C11 0.028(3) 0.030(2) 0.020(2) -0.0071(19) -0.0015(18) -0.0019(19) C12 0.019(2) 0.026(2) 0.030(3) -0.0067(19) -0.0005(19) 0.0014(18) C13 0.024(2) 0.025(2) 0.023(2) -0.0039(18) -0.0056(18) 0.0032(18) C14 0.027(3) 0.024(2) 0.029(3) -0.0064(19) -0.003(2) 0.0016(19) C15 0.037(3) 0.023(2) 0.026(2) -0.0046(19) -0.008(2) 0.000(2) C16 0.036(3) 0.021(2) 0.036(3) -0.006(2) -0.014(2) 0.006(2) C17 0.030(3) 0.028(3) 0.033(3) -0.009(2) -0.015(2) 0.002(2) C18 0.022(2) 0.026(2) 0.029(3) -0.0053(19) -0.0023(19) 0.0015(18) C19 0.032(3) 0.023(2) 0.025(2) -0.0064(18) -0.002(2) 0.0029(19) C20 0.034(3) 0.027(3) 0.038(3) -0.004(2) -0.007(2) 0.004(2) C21 0.040(3) 0.026(3) 0.034(3) -0.002(2) -0.010(2) -0.001(2) C22 0.034(3) 0.032(3) 0.028(3) 0.003(2) 0.003(2) -0.003(2) C23 0.042(3) 0.029(3) 0.034(3) -0.012(2) 0.000(2) 0.003(2) C24 0.033(3) 0.030(3) 0.028(3) -0.008(2) -0.004(2) 0.009(2) C25 0.044(3) 0.050(3) 0.034(3) -0.018(2) -0.015(2) 0.014(3) C26 0.057(4) 0.033(3) 0.035(3) -0.005(2) 0.014(3) 0.007(3) C27 0.042(3) 0.033(3) 0.032(3) -0.010(2) 0.000(2) 0.009(2) C28 0.056(4) 0.028(3) 0.043(3) -0.007(2) -0.017(3) 0.014(2) S1 0.0225(6) 0.0307(6) 0.0236(6) -0.0034(5) -0.0024(4) -0.0001(5) S2 0.0248(6) 0.0278(6) 0.0258(6) -0.0021(5) -0.0052(5) -0.0023(5) C29 0.024(2) 0.028(2) 0.025(2) -0.0080(19) -0.0066(18) 0.0003(18) O3 0.0188(16) 0.0190(16) 0.0380(19) -0.0015(13) -0.0055(14) -0.0014(12) C30 0.018(2) 0.032(3) 0.042(3) -0.003(2) -0.006(2) 0.0017(19) C31 0.027(3) 0.057(4) 0.043(3) -0.014(3) -0.010(2) -0.007(2) C32 0.035(3) 0.039(3) 0.048(3) -0.021(3) 0.000(2) -0.006(2) C33 0.034(3) 0.025(3) 0.063(4) -0.007(2) -0.014(3) -0.003(2) C34 0.063(5) 0.061(5) 0.114(7) -0.029(5) -0.001(5) -0.014(4) C35 0.047(4) 0.031(3) 0.058(4) -0.009(3) -0.008(3) -0.007(3) C36 0.067(5) 0.047(4) 0.063(4) -0.017(3) -0.018(4) -0.015(3) C37 0.060(5) 0.059(5) 0.136(8) -0.032(5) -0.051(5) -0.001(4) C38 0.046(5) 0.066(5) 0.145(9) -0.051(6) 0.015(5) -0.019(4) C39 0.096(6) 0.057(5) 0.075(5) -0.026(4) 0.033(5) -0.035(4) C40 0.088(5) 0.037(3) 0.058(4) -0.004(3) -0.014(4) -0.014(3) C41 0.059(5) 0.043(4) 0.106(6) -0.023(4) 0.000(4) -0.008(3) C42 0.039(3) 0.046(4) 0.081(5) -0.039(3) 0.001(3) -0.007(3) C43 0.032(3) 0.048(4) 0.090(5) -0.023(4) -0.002(3) -0.003(3) C44 0.043(4) 0.062(4) 0.075(5) -0.031(4) 0.006(3) -0.009(3) C45 0.061(5) 0.091(6) 0.055(4) -0.034(4) -0.006(4) -0.013(4) C46 0.045(4) 0.121(7) 0.064(5) -0.050(5) -0.014(4) 0.002(4) C47 0.033(3) 0.084(5) 0.065(5) -0.046(4) 0.004(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O2 1.989(3) . ? Zr1 O1 1.992(3) . ? Zr1 O3 2.276(3) . ? Zr1 S1 2.4755(15) . ? Zr1 S2 2.5116(14) 2_656 ? O1 C7 1.373(5) . ? O2 C13 1.361(5) . ? C1 C6 1.398(6) . ? C1 C2 1.414(6) . ? C1 C12 1.469(6) . ? C2 C3 1.382(6) . ? C2 H1 0.9300 . ? C3 C4 1.407(6) . ? C3 H2 0.9300 . ? C4 C5 1.387(6) . ? C4 C14 1.484(6) . ? C5 C6 1.396(6) . ? C5 H3 0.9300 . ? C6 H4 0.9300 . ? C7 C12 1.409(6) . ? C7 C8 1.411(6) . ? C8 C9 1.401(6) . ? C8 C19 1.542(6) . ? C9 C10 1.390(6) . ? C9 H5 0.9300 . ? C10 C11 1.391(6) . ? C10 C23 1.520(6) . ? C11 C12 1.398(6) . ? C11 H6 0.9300 . ? C13 C14 1.414(6) . ? C13 C18 1.418(6) . ? C14 C15 1.371(6) . ? C15 C16 1.398(6) . ? C15 H7 0.9300 . ? C16 C17 1.392(7) . ? C16 C28 1.506(6) . ? C17 C18 1.402(6) . ? C17 H8 0.9300 . ? C18 C24 1.535(6) . ? C19 C22 1.526(6) . ? C19 C21 1.529(6) . ? C19 C20 1.541(7) . ? C20 H9 0.9600 . ? C20 H10 0.9600 . ? C20 H11 0.9600 . ? C21 H12 0.9600 . ? C21 H13 0.9600 . ? C21 H14 0.9600 . ? C22 H15 0.9600 . ? C22 H16 0.9600 . ? C22 H17 0.9600 . ? C23 H18 0.9600 . ? C23 H19 0.9600 . ? C23 H20 0.9600 . ? C24 C25 1.533(7) . ? C24 C26 1.538(7) . ? C24 C27 1.544(6) . ? C25 H21 0.9600 . ? C25 H22 0.9600 . ? C25 H23 0.9600 . ? C26 H24 0.9600 . ? C26 H25 0.9600 . ? C26 H26 0.9600 . ? C27 H27 0.9600 . ? C27 H28 0.9600 . ? C27 H29 0.9600 . ? C28 H30 0.9600 . ? C28 H31 0.9600 . ? C28 H32 0.9600 . ? S1 C29 1.778(4) . ? S2 C29 1.764(5) . ? S2 Zr1 2.5116(14) 2_656 ? C29 C29 1.378(9) 2_656 ? O3 C33 1.457(6) . ? O3 C30 1.475(5) . ? C30 C31 1.515(7) . ? C30 H33 0.9700 . ? C30 H34 0.9700 . ? C31 C32 1.504(7) . ? C31 H35 0.9700 . ? C31 H36 0.9700 . ? C32 C33 1.516(7) . ? C32 H37 0.9700 . ? C32 H38 0.9700 . ? C33 H39 0.9700 . ? C33 H40 0.9700 . ? C34 C35 1.475(9) . ? C34 H41 0.9600 . ? C34 H42 0.9600 . ? C34 H43 0.9600 . ? C35 C40 1.369(9) . ? C35 C36 1.390(8) . ? C36 C37 1.364(10) . ? C36 H44 0.9300 . ? C37 C38 1.352(12) . ? C37 H45 0.9300 . ? C38 C39 1.402(12) . ? C38 H46 0.9300 . ? C39 C40 1.373(10) . ? C39 H47 0.9300 . ? C40 H48 0.9300 . ? C41 C42 1.499(10) . ? C41 H49 0.9600 . ? C41 H50 0.9600 . ? C41 H51 0.9600 . ? C42 C43 1.390(9) . ? C42 C47 1.391(9) . ? C43 C44 1.363(9) . ? C43 H52 0.9300 . ? C44 C45 1.378(9) . ? C44 H53 0.9300 . ? C45 C46 1.373(10) . ? C45 H54 0.9300 . ? C46 C47 1.382(10) . ? C46 H55 0.9300 . ? C47 H56 0.9300 . ? 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 O2 Zr1 O1 153.04(13) . . ? O2 Zr1 O3 82.71(12) . . ? O1 Zr1 O3 84.98(12) . . ? O2 Zr1 S1 104.34(10) . . ? O1 Zr1 S1 99.63(10) . . ? O3 Zr1 S1 90.43(9) . . ? O2 Zr1 S2 95.13(10) . 2_656 ? O1 Zr1 S2 100.06(10) . 2_656 ? O3 Zr1 S2 171.97(9) . 2_656 ? S1 Zr1 S2 82.59(5) . 2_656 ? C7 O1 Zr1 155.9(3) . . ? C13 O2 Zr1 156.0(3) . . ? C6 C1 C2 117.7(4) . . ? C6 C1 C12 121.3(4) . . ? C2 C1 C12 119.7(4) . . ? C3 C2 C1 121.2(4) . . ? C3 C2 H1 119.4 . . ? C1 C2 H1 119.4 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H2 120.1 . . ? C4 C3 H2 120.1 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 C14 119.8(4) . . ? C3 C4 C14 119.7(4) . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H3 119.7 . . ? C6 C5 H3 119.7 . . ? C5 C6 C1 120.6(4) . . ? C5 C6 H4 119.7 . . ? C1 C6 H4 119.7 . . ? O1 C7 C12 117.7(4) . . ? O1 C7 C8 122.1(4) . . ? C12 C7 C8 120.3(4) . . ? C9 C8 C7 117.0(4) . . ? C9 C8 C19 121.2(4) . . ? C7 C8 C19 121.7(4) . . ? C10 C9 C8 123.7(4) . . ? C10 C9 H5 118.2 . . ? C8 C9 H5 118.2 . . ? C9 C10 C11 118.1(4) . . ? C9 C10 C23 121.4(4) . . ? C11 C10 C23 120.5(4) . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H6 119.7 . . ? C12 C11 H6 119.7 . . ? C11 C12 C7 120.1(4) . . ? C11 C12 C1 123.1(4) . . ? C7 C12 C1 116.6(4) . . ? O2 C13 C14 118.0(4) . . ? O2 C13 C18 122.0(4) . . ? C14 C13 C18 120.0(4) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 C4 123.5(4) . . ? C13 C14 C4 115.5(4) . . ? C14 C15 C16 121.1(4) . . ? C14 C15 H7 119.4 . . ? C16 C15 H7 119.4 . . ? C17 C16 C15 117.7(4) . . ? C17 C16 C28 120.6(4) . . ? C15 C16 C28 121.8(5) . . ? C16 C17 C18 123.9(4) . . ? C16 C17 H8 118.1 . . ? C18 C17 H8 118.1 . . ? C17 C18 C13 116.7(4) . . ? C17 C18 C24 121.0(4) . . ? C13 C18 C24 122.2(4) . . ? C22 C19 C21 107.5(4) . . ? C22 C19 C20 109.8(4) . . ? C21 C19 C20 108.1(4) . . ? C22 C19 C8 111.4(4) . . ? C21 C19 C8 112.1(4) . . ? C20 C19 C8 108.0(4) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C10 C23 H18 109.5 . . ? C10 C23 H19 109.5 . . ? H18 C23 H19 109.5 . . ? C10 C23 H20 109.5 . . ? H18 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C25 C24 C18 108.2(4) . . ? C25 C24 C26 110.2(4) . . ? C18 C24 C26 112.0(4) . . ? C25 C24 C27 108.1(4) . . ? C18 C24 C27 112.0(4) . . ? C26 C24 C27 106.3(4) . . ? C24 C25 H21 109.5 . . ? C24 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C24 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C24 C26 H24 109.5 . . ? C24 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C24 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C24 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C16 C28 H30 109.5 . . ? C16 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C16 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C29 S1 Zr1 98.00(16) . . ? C29 S2 Zr1 96.99(15) . 2_656 ? C29 C29 S2 123.4(5) 2_656 . ? C29 C29 S1 122.0(5) 2_656 . ? S2 C29 S1 114.6(3) . . ? C33 O3 C30 109.2(3) . . ? C33 O3 Zr1 122.6(3) . . ? C30 O3 Zr1 127.8(3) . . ? O3 C30 C31 103.6(4) . . ? O3 C30 H33 111.0 . . ? C31 C30 H33 111.0 . . ? O3 C30 H34 111.0 . . ? C31 C30 H34 111.0 . . ? H33 C30 H34 109.0 . . ? C32 C31 C30 102.5(4) . . ? C32 C31 H35 111.3 . . ? C30 C31 H35 111.3 . . ? C32 C31 H36 111.3 . . ? C30 C31 H36 111.3 . . ? H35 C31 H36 109.2 . . ? C31 C32 C33 102.9(4) . . ? C31 C32 H37 111.2 . . ? C33 C32 H37 111.2 . . ? C31 C32 H38 111.2 . . ? C33 C32 H38 111.2 . . ? H37 C32 H38 109.1 . . ? O3 C33 C32 105.7(4) . . ? O3 C33 H39 110.6 . . ? C32 C33 H39 110.6 . . ? O3 C33 H40 110.6 . . ? C32 C33 H40 110.6 . . ? H39 C33 H40 108.7 . . ? C35 C34 H41 109.5 . . ? C35 C34 H42 109.5 . . ? H41 C34 H42 109.5 . . ? C35 C34 H43 109.5 . . ? H41 C34 H43 109.5 . . ? H42 C34 H43 109.5 . . ? C40 C35 C36 119.5(6) . . ? C40 C35 C34 120.9(6) . . ? C36 C35 C34 119.6(6) . . ? C37 C36 C35 118.5(7) . . ? C37 C36 H44 120.8 . . ? C35 C36 H44 120.8 . . ? C38 C37 C36 123.2(8) . . ? C38 C37 H45 118.4 . . ? C36 C37 H45 118.4 . . ? C37 C38 C39 118.3(8) . . ? C37 C38 H46 120.8 . . ? C39 C38 H46 120.8 . . ? C40 C39 C38 119.2(8) . . ? C40 C39 H47 120.4 . . ? C38 C39 H47 120.4 . . ? C35 C40 C39 121.2(7) . . ? C35 C40 H48 119.4 . . ? C39 C40 H48 119.4 . . ? C42 C41 H49 109.5 . . ? C42 C41 H50 109.5 . . ? H49 C41 H50 109.5 . . ? C42 C41 H51 109.5 . . ? H49 C41 H51 109.5 . . ? H50 C41 H51 109.5 . . ? C43 C42 C47 117.6(7) . . ? C43 C42 C41 119.9(6) . . ? C47 C42 C41 122.6(6) . . ? C44 C43 C42 120.7(6) . . ? C44 C43 H52 119.7 . . ? C42 C43 H52 119.7 . . ? C43 C44 C45 121.8(7) . . ? C43 C44 H53 119.1 . . ? C45 C44 H53 119.1 . . ? C46 C45 C44 118.3(7) . . ? C46 C45 H54 120.8 . . ? C44 C45 H54 120.8 . . ? C45 C46 C47 120.5(7) . . ? C45 C46 H55 119.7 . . ? C47 C46 H55 119.7 . . ? C46 C47 C42 121.1(6) . . ? C46 C47 H56 119.4 . . ? C42 C47 H56 119.4 . . ? 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 O2 Zr1 O1 C7 6.8(9) . . . . ? O3 Zr1 O1 C7 69.8(7) . . . . ? S1 Zr1 O1 C7 159.4(7) . . . . ? S2 Zr1 O1 C7 -116.5(7) 2_656 . . . ? O1 Zr1 O2 C13 -5.3(9) . . . . ? O3 Zr1 O2 C13 -68.8(7) . . . . ? S1 Zr1 O2 C13 -157.4(7) . . . . ? S2 Zr1 O2 C13 119.0(7) 2_656 . . . ? C6 C1 C2 C3 9.5(6) . . . . ? C12 C1 C2 C3 -157.5(4) . . . . ? C1 C2 C3 C4 -1.5(7) . . . . ? C2 C3 C4 C5 -7.3(7) . . . . ? C2 C3 C4 C14 159.6(4) . . . . ? C3 C4 C5 C6 7.8(7) . . . . ? C14 C4 C5 C6 -159.1(4) . . . . ? C4 C5 C6 C1 0.5(7) . . . . ? C2 C1 C6 C5 -9.0(6) . . . . ? C12 C1 C6 C5 157.8(4) . . . . ? Zr1 O1 C7 C12 9.8(9) . . . . ? Zr1 O1 C7 C8 -169.4(5) . . . . ? O1 C7 C8 C9 175.2(4) . . . . ? C12 C7 C8 C9 -3.9(6) . . . . ? O1 C7 C8 C19 -6.1(7) . . . . ? C12 C7 C8 C19 174.8(4) . . . . ? C7 C8 C9 C10 2.0(7) . . . . ? C19 C8 C9 C10 -176.7(4) . . . . ? C8 C9 C10 C11 0.1(7) . . . . ? C8 C9 C10 C23 180.0(4) . . . . ? C9 C10 C11 C12 -0.4(7) . . . . ? C23 C10 C11 C12 179.8(4) . . . . ? C10 C11 C12 C7 -1.5(7) . . . . ? C10 C11 C12 C1 -176.2(4) . . . . ? O1 C7 C12 C11 -175.4(4) . . . . ? C8 C7 C12 C11 3.8(7) . . . . ? O1 C7 C12 C1 -0.4(6) . . . . ? C8 C7 C12 C1 178.8(4) . . . . ? C6 C1 C12 C11 67.9(6) . . . . ? C2 C1 C12 C11 -125.5(5) . . . . ? C6 C1 C12 C7 -106.9(5) . . . . ? C2 C1 C12 C7 59.7(6) . . . . ? Zr1 O2 C13 C14 -13.3(10) . . . . ? Zr1 O2 C13 C18 164.1(5) . . . . ? O2 C13 C14 C15 177.7(4) . . . . ? C18 C13 C14 C15 0.2(7) . . . . ? O2 C13 C14 C4 2.9(6) . . . . ? C18 C13 C14 C4 -174.6(4) . . . . ? C5 C4 C14 C15 -69.0(7) . . . . ? C3 C4 C14 C15 124.2(5) . . . . ? C5 C4 C14 C13 105.7(5) . . . . ? C3 C4 C14 C13 -61.1(6) . . . . ? C13 C14 C15 C16 -0.5(7) . . . . ? C4 C14 C15 C16 173.9(5) . . . . ? C14 C15 C16 C17 0.9(7) . . . . ? C14 C15 C16 C28 -178.4(5) . . . . ? C15 C16 C17 C18 -0.9(7) . . . . ? C28 C16 C17 C18 178.4(5) . . . . ? C16 C17 C18 C13 0.6(7) . . . . ? C16 C17 C18 C24 176.9(4) . . . . ? O2 C13 C18 C17 -177.6(4) . . . . ? C14 C13 C18 C17 -0.2(7) . . . . ? O2 C13 C18 C24 6.1(7) . . . . ? C14 C13 C18 C24 -176.5(4) . . . . ? C9 C8 C19 C22 -119.5(5) . . . . ? C7 C8 C19 C22 61.8(6) . . . . ? C9 C8 C19 C21 0.9(6) . . . . ? C7 C8 C19 C21 -177.8(4) . . . . ? C9 C8 C19 C20 119.8(5) . . . . ? C7 C8 C19 C20 -58.8(5) . . . . ? C17 C18 C24 C25 -111.5(5) . . . . ? C13 C18 C24 C25 64.6(6) . . . . ? C17 C18 C24 C26 126.8(5) . . . . ? C13 C18 C24 C26 -57.1(6) . . . . ? C17 C18 C24 C27 7.5(7) . . . . ? C13 C18 C24 C27 -176.4(5) . . . . ? O2 Zr1 S1 C29 -126.25(18) . . . . ? O1 Zr1 S1 C29 66.19(18) . . . . ? O3 Zr1 S1 C29 151.17(17) . . . . ? S2 Zr1 S1 C29 -32.82(15) 2_656 . . . ? Zr1 S2 C29 C29 28.8(5) 2_656 . . 2_656 ? Zr1 S2 C29 S1 -151.4(2) 2_656 . . . ? Zr1 S1 C29 C29 29.0(5) . . . 2_656 ? Zr1 S1 C29 S2 -150.8(2) . . . . ? O2 Zr1 O3 C33 178.6(4) . . . . ? O1 Zr1 O3 C33 22.6(4) . . . . ? S1 Zr1 O3 C33 -77.0(4) . . . . ? O2 Zr1 O3 C30 -9.6(3) . . . . ? O1 Zr1 O3 C30 -165.6(4) . . . . ? S1 Zr1 O3 C30 94.8(3) . . . . ? C33 O3 C30 C31 -19.5(5) . . . . ? Zr1 O3 C30 C31 167.8(3) . . . . ? O3 C30 C31 C32 36.5(5) . . . . ? C30 C31 C32 C33 -39.5(5) . . . . ? C30 O3 C33 C32 -5.1(6) . . . . ? Zr1 O3 C33 C32 168.0(3) . . . . ? C31 C32 C33 O3 27.9(6) . . . . ? C40 C35 C36 C37 -0.2(9) . . . . ? C34 C35 C36 C37 -179.1(6) . . . . ? C35 C36 C37 C38 0.5(11) . . . . ? C36 C37 C38 C39 0.0(11) . . . . ? C37 C38 C39 C40 -0.7(11) . . . . ? C36 C35 C40 C39 -0.6(9) . . . . ? C34 C35 C40 C39 178.3(6) . . . . ? C38 C39 C40 C35 1.1(10) . . . . ? C47 C42 C43 C44 -1.1(9) . . . . ? C41 C42 C43 C44 -179.9(6) . . . . ? C42 C43 C44 C45 0.6(10) . . . . ? C43 C44 C45 C46 0.6(10) . . . . ? C44 C45 C46 C47 -1.4(11) . . . . ? C45 C46 C47 C42 0.9(10) . . . . ? C43 C42 C47 C46 0.3(9) . . . . ? C41 C42 C47 C46 179.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.147 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.113 #===END _database_code_depnum_ccdc_archive 'CCDC 962322'