# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1708 #******************************************************************** data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42H41LIO2Zr' _chemical_formula_weight 675.91 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' 'Li' 'Li' -0.0003 0.0001 '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 14.9859(18) _cell_length_b 10.4594(8) _cell_length_c 22.028(2) _cell_angle_beta 102.073(11) _cell_volume 3376.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5000 _cell_measurement_2theta_min 4.1 _cell_measurement_2theta_max 47.9 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.361 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _absorpt_process_ref ; [X-Shape a Crystal Optimisation for Numerical Absorption Corrections Revision 1.01 July 1996 STOE and Cie GMBH 1996] ; _exptl_absorpt_process_details ; .Absorption corrections were applied on the data by using a set of symmetry equivalent reflections selected with the criterion [I>3((I)] such that all directions of the reciprocal space are equally represented. ; _exptl_special_details ; The data was collected at low temperature (T=160K) on a STOE imaging plate diffraction system (I.P.D.S), equipped with an Oxford cryosystems cooler device, the crystal-to-detector distance was 80mm, 208 exposures were obtained with 0<(<250 and with the crystal rotated through 1.2 in (. Coverage of the unique set has been 97% complete to at least 24.2. Crystal decay was monitored by measuring 200 reflections by image. The final unit cell parameters was obtained by the least-squares refinement of 5000 reflections. Any significant fluctuations in the intensity monitors were during the data collection. ; _diffrn_ambient_temperature 160(2)K _diffrn_radiation_wavelength 0.710733 _diffrn_radiation_type MoK\( _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany' _diffrn_measurement_method 'rotation en (' _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23132 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4701 _reflns_number_gt 4225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe and Cie (1996) IPDS Manual. Version 2.75 Stoe and Cie, Darmstadt, Germany' _computing_cell_refinement 'Stoe and Cie (1996) IPDS Manual. Version 2.75 Stoe and Cie, Darmstadt, Germany' _computing_data_reduction 'Stoe and Cie (1996) IPDS Manual. Version 2.75 Stoe and Cie, Darmstadt, Germany' _computing_structure_solution ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods.J. Appl. Cryst. (27), 435 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zsolnai,L.(1997). ZORTEP.Molecular Graphics Program.University of Heidelberg, Germany.' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Structure has been solved by Direct Methods using SIR92, and refined by least-squares procedures on a F2 with the aid of SHELXL97 by minimizing the function : (w(Fo2-Fc2)2, where Fo and Fc are respectively the observed and calculated structure factors. The Atomic Scattering Factors were taken from International tables for X-Ray crystallography. All hydrogen atoms were located on a difference Fourier maps, and refined with a riding model. Non-hydrogens atom were anisotropically refined, and in the last cycles of refinement a weighting scheme was used.Refinement of F2 against.ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement R-factors based on F2 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^)+(0.0528P)^2^+0.9754P] 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 4701 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _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 0.796693(12) 0.113904(17) 0.562538(7) 0.01974(9) Uani 1 1 d . . . C1 C 0.94498(14) 0.2283(2) 0.61058(10) 0.0359(5) Uani 1 1 d . . . H1 H 0.9580 0.2413 0.6542 0.043 Uiso 1 1 calc R . . C2 C 0.96854(14) 0.1203(2) 0.57949(11) 0.0341(5) Uani 1 1 d . . . H2 H 1.0009 0.0475 0.5983 0.041 Uiso 1 1 calc R . . C3 C 0.93592(15) 0.1389(2) 0.51590(10) 0.0340(5) Uani 1 1 d . . . H3 H 0.9418 0.0806 0.4839 0.041 Uiso 1 1 calc R . . C4 C 0.89283(15) 0.2589(2) 0.50754(10) 0.0352(5) Uani 1 1 d . . . H4 H 0.8646 0.2959 0.4689 0.042 Uiso 1 1 calc R . . C5 C 0.89875(15) 0.3139(2) 0.56560(11) 0.0365(5) Uani 1 1 d . . . H5 H 0.8756 0.3954 0.5735 0.044 Uiso 1 1 calc R . . C6 C 0.70627(18) 0.0965(2) 0.45146(10) 0.0410(6) Uani 1 1 d . . . H6 H 0.7172 0.1585 0.4223 0.049 Uiso 1 1 calc R . . C7 C 0.64037(16) 0.1043(2) 0.48775(10) 0.0370(6) Uani 1 1 d . . . H7 H 0.5986 0.1727 0.4875 0.044 Uiso 1 1 calc R . . C8 C 0.64650(15) -0.0063(2) 0.52458(9) 0.0333(5) Uani 1 1 d . . . H8 H 0.6103 -0.0252 0.5540 0.040 Uiso 1 1 calc R . . C9 C 0.71568(16) -0.0838(2) 0.51017(9) 0.0329(5) Uani 1 1 d . . . H9 H 0.7336 -0.1654 0.5275 0.040 Uiso 1 1 calc R . . C10 C 0.75370(17) -0.0197(2) 0.46576(9) 0.0382(6) Uani 1 1 d . . . H10 H 0.8028 -0.0493 0.4484 0.046 Uiso 1 1 calc R . . C11 C 0.84265(13) -0.04189(19) 0.62934(8) 0.0216(4) Uani 1 1 d . . . C12 C 0.79518(13) 0.03119(18) 0.66104(8) 0.0210(4) Uani 1 1 d . . . C13 C 0.78123(13) 0.01162(19) 0.72185(9) 0.0225(4) Uani 1 1 d . . . C14 C 0.76943(13) 0.0004(2) 0.77429(9) 0.0244(4) Uani 1 1 d . . . C15 C 0.71481(13) 0.2879(2) 0.58600(9) 0.0252(4) Uani 1 1 d . . . C16 C 0.67761(14) 0.38888(19) 0.59387(9) 0.0248(5) Uani 1 1 d . . . C111 C 0.89277(12) -0.1623(2) 0.64301(8) 0.0214(4) Uani 1 1 d . . . C112 C 0.91027(13) -0.2195(2) 0.70204(9) 0.0271(5) Uani 1 1 d . . . H112 H 0.8908 -0.1779 0.7354 0.032 Uiso 1 1 calc R . . C113 C 0.95538(14) -0.3354(2) 0.71229(10) 0.0321(5) Uani 1 1 d . . . H113 H 0.9665 -0.3726 0.7525 0.038 Uiso 1 1 calc R . . C114 C 0.98453(14) -0.3978(2) 0.66425(11) 0.0324(5) Uani 1 1 d . . . H114 H 1.0148 -0.4779 0.6713 0.039 Uiso 1 1 calc R . . C115 C 0.96915(14) -0.3425(2) 0.60628(10) 0.0318(5) Uani 1 1 d . . . H115 H 0.9894 -0.3841 0.5733 0.038 Uiso 1 1 calc R . . C116 C 0.92420(13) -0.2264(2) 0.59603(9) 0.0267(5) Uani 1 1 d . . . H116 H 0.9145 -0.1892 0.5558 0.032 Uiso 1 1 calc R . . C121 C 0.77132(13) -0.0252(2) 0.83856(8) 0.0237(4) Uani 1 1 d . . . C122 C 0.71943(15) 0.0441(2) 0.87289(9) 0.0317(5) Uani 1 1 d . . . H122 H 0.6798 0.1096 0.8533 0.038 Uiso 1 1 calc R . . C123 C 0.72518(15) 0.0182(2) 0.93545(9) 0.0338(5) Uani 1 1 d . . . H123 H 0.6888 0.0654 0.9581 0.041 Uiso 1 1 calc R . . C124 C 0.78304(15) -0.0751(2) 0.96491(9) 0.0325(5) Uani 1 1 d . . . H124 H 0.7868 -0.0922 1.0077 0.039 Uiso 1 1 calc R . . C125 C 0.83579(16) -0.1439(2) 0.93173(10) 0.0362(5) Uani 1 1 d . . . H125 H 0.8766 -0.2075 0.9521 0.043 Uiso 1 1 calc R . . C126 C 0.82937(15) -0.1205(2) 0.86935(10) 0.0306(5) Uani 1 1 d . . . H126 H 0.8649 -0.1698 0.8469 0.037 Uiso 1 1 calc R . . C131 C 0.63998(13) 0.51107(19) 0.60423(8) 0.0235(4) Uani 1 1 d . . . C132 C 0.69721(14) 0.6113(2) 0.62942(10) 0.0285(5) Uani 1 1 d . . . H132 H 0.7614 0.5988 0.6385 0.034 Uiso 1 1 calc R . . C133 C 0.66200(16) 0.7288(2) 0.64143(10) 0.0369(5) Uani 1 1 d . . . H133 H 0.7021 0.7959 0.6588 0.044 Uiso 1 1 calc R . . C134 C 0.56929(16) 0.7488(2) 0.62835(11) 0.0410(6) Uani 1 1 d . . . H134 H 0.5452 0.8294 0.6368 0.049 Uiso 1 1 calc R . . C135 C 0.51173(16) 0.6518(3) 0.60301(13) 0.0443(6) Uani 1 1 d . . . H135 H 0.4477 0.6657 0.5939 0.053 Uiso 1 1 calc R . . C136 C 0.54599(15) 0.5344(2) 0.59066(11) 0.0387(5) Uani 1 1 d . . . H136 H 0.5052 0.4686 0.5727 0.046 Uiso 1 1 calc R . . O100 O 0.73210(10) 0.31173(16) 0.74337(7) 0.0396(4) Uani 1 1 d . . . C101 C 0.82980(17) 0.3290(3) 0.75905(15) 0.0593(8) Uani 1 1 d . . . H10A H 0.8522 0.3634 0.7231 0.071 Uiso 1 1 calc R . . H10B H 0.8608 0.2468 0.7716 0.071 Uiso 1 1 calc R . . C102 C 0.84729(19) 0.4215(3) 0.81152(12) 0.0514(7) Uani 1 1 d . . . H10C H 0.9054 0.4680 0.8136 0.062 Uiso 1 1 calc R . . H10D H 0.8485 0.3784 0.8517 0.062 Uiso 1 1 calc R . . C103 C 0.7664(2) 0.5095(3) 0.79435(11) 0.0503(7) Uani 1 1 d . . . H10E H 0.7761 0.5739 0.7634 0.060 Uiso 1 1 calc R . . H10F H 0.7538 0.5539 0.8313 0.060 Uiso 1 1 calc R . . C104 C 0.68961(16) 0.4184(2) 0.76696(10) 0.0389(5) Uani 1 1 d . . . H10G H 0.6569 0.3900 0.7992 0.047 Uiso 1 1 calc R . . H10H H 0.6455 0.4605 0.7332 0.047 Uiso 1 1 calc R . . O200 O 0.56599(10) 0.14958(18) 0.66735(7) 0.0431(4) Uani 1 1 d . . . C201 C 0.52471(19) 0.1469(4) 0.72010(13) 0.0717(10) Uani 1 1 d . . . H20A H 0.5686 0.1748 0.7578 0.086 Uiso 1 1 calc R . . H20B H 0.5035 0.0595 0.7270 0.086 Uiso 1 1 calc R . . C202 C 0.4466(2) 0.2365(4) 0.70546(15) 0.0790(11) Uani 1 1 d . . . H20C H 0.4659 0.3248 0.7181 0.095 Uiso 1 1 calc R . . H20D H 0.3973 0.2107 0.7266 0.095 Uiso 1 1 calc R . . C203 C 0.41594(19) 0.2271(4) 0.63707(13) 0.0652(9) Uani 1 1 d . . . H20E H 0.4034 0.3131 0.6184 0.078 Uiso 1 1 calc R . . H20F H 0.3598 0.1749 0.6261 0.078 Uiso 1 1 calc R . . C204 C 0.49277(15) 0.1647(3) 0.61460(10) 0.0426(6) Uani 1 1 d . . . H20G H 0.4734 0.0804 0.5960 0.051 Uiso 1 1 calc R . . H20H H 0.5123 0.2186 0.5828 0.051 Uiso 1 1 calc R . . Li1 Li 0.6924(2) 0.3016(3) 0.17178(15) 0.0304(8) Uani 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 0.02259(13) 0.01870(14) 0.01801(13) 0.00031(6) 0.00445(8) 0.00234(7) C1 0.0263(11) 0.0450(15) 0.0366(12) -0.0005(10) 0.0069(9) -0.0142(10) C2 0.0204(11) 0.0357(15) 0.0469(13) 0.0126(10) 0.0087(10) 0.0040(9) C3 0.0305(12) 0.0381(15) 0.0383(12) 0.0029(10) 0.0186(10) 0.0061(10) C4 0.0293(12) 0.0394(15) 0.0398(12) 0.0162(10) 0.0142(9) 0.0035(10) C5 0.0285(12) 0.0250(14) 0.0611(15) 0.0009(10) 0.0207(10) -0.0035(9) C6 0.0596(16) 0.0382(15) 0.0201(10) 0.0012(9) -0.0035(10) -0.0020(11) C7 0.0364(13) 0.0361(15) 0.0299(12) -0.0062(9) -0.0127(10) 0.0061(10) C8 0.0294(12) 0.0372(14) 0.0289(11) -0.0060(9) -0.0040(9) -0.0058(10) C9 0.0434(13) 0.0248(13) 0.0252(11) -0.0061(9) -0.0050(9) -0.0002(10) C10 0.0496(14) 0.0409(15) 0.0231(10) -0.0111(9) 0.0054(10) 0.0017(11) C11 0.0238(10) 0.0198(11) 0.0207(9) -0.0001(7) 0.0038(8) -0.0023(8) C12 0.0235(10) 0.0197(11) 0.0189(9) -0.0004(7) 0.0024(7) -0.0025(8) C13 0.0212(10) 0.0186(11) 0.0266(11) -0.0032(8) 0.0029(8) 0.0033(8) C14 0.0243(10) 0.0255(12) 0.0237(11) -0.0010(8) 0.0055(8) 0.0019(8) C15 0.0245(10) 0.0239(12) 0.0268(10) 0.0008(8) 0.0047(8) 0.0003(9) C16 0.0232(11) 0.0260(13) 0.0251(10) 0.0013(8) 0.0047(8) -0.0009(9) C111 0.0178(9) 0.0216(11) 0.0242(9) -0.0009(8) 0.0033(7) -0.0033(8) C112 0.0274(11) 0.0272(13) 0.0268(10) 0.0000(8) 0.0063(8) 0.0026(9) C113 0.0301(11) 0.0300(13) 0.0336(11) 0.0078(9) 0.0010(9) 0.0029(10) C114 0.0233(11) 0.0225(13) 0.0494(14) -0.0011(9) 0.0032(10) 0.0037(8) C115 0.0282(11) 0.0294(13) 0.0397(12) -0.0091(10) 0.0111(9) 0.0013(9) C116 0.0260(11) 0.0269(12) 0.0283(10) -0.0005(8) 0.0082(8) 0.0006(9) C121 0.0214(10) 0.0267(12) 0.0231(10) -0.0012(8) 0.0052(8) -0.0034(8) C122 0.0306(11) 0.0389(14) 0.0252(10) -0.0002(9) 0.0049(8) 0.0096(9) C123 0.0338(12) 0.0455(15) 0.0237(11) -0.0074(9) 0.0100(9) 0.0013(10) C124 0.0380(12) 0.0376(14) 0.0210(10) 0.0027(9) 0.0042(9) -0.0092(10) C125 0.0393(13) 0.0348(14) 0.0335(12) 0.0101(10) 0.0051(10) 0.0057(10) C126 0.0298(12) 0.0335(14) 0.0302(11) 0.0039(8) 0.0103(9) 0.0073(9) C131 0.0238(10) 0.0230(12) 0.0245(9) 0.0036(8) 0.0065(8) 0.0025(8) C132 0.0223(11) 0.0300(13) 0.0337(11) -0.0008(8) 0.0069(9) -0.0009(8) C133 0.0405(13) 0.0246(13) 0.0477(13) -0.0058(10) 0.0143(10) -0.0051(10) C134 0.0451(14) 0.0230(14) 0.0620(15) 0.0041(10) 0.0271(12) 0.0089(10) C135 0.0249(12) 0.0352(15) 0.0749(17) 0.0084(12) 0.0150(11) 0.0080(11) C136 0.0257(12) 0.0281(14) 0.0600(14) 0.0021(10) 0.0035(10) -0.0029(9) O100 0.0245(8) 0.0416(11) 0.0491(9) -0.0163(7) -0.0005(7) 0.0047(7) C101 0.0284(13) 0.060(2) 0.083(2) -0.0279(16) -0.0019(13) 0.0006(12) C102 0.0516(16) 0.0519(18) 0.0448(14) -0.0007(12) -0.0037(12) -0.0078(13) C103 0.0726(18) 0.0383(16) 0.0376(13) -0.0091(11) 0.0058(12) 0.0033(13) C104 0.0419(13) 0.0433(15) 0.0321(12) -0.0010(10) 0.0095(10) 0.0138(11) O200 0.0213(8) 0.0624(12) 0.0434(9) 0.0136(8) 0.0017(7) -0.0018(7) C201 0.0384(15) 0.130(3) 0.0436(15) 0.0290(17) 0.0026(12) -0.0201(17) C202 0.0454(17) 0.122(3) 0.073(2) -0.039(2) 0.0203(15) -0.0113(19) C203 0.0425(16) 0.090(3) 0.0646(18) 0.0142(16) 0.0139(14) 0.0191(15) C204 0.0300(12) 0.0537(17) 0.0394(13) -0.0057(11) -0.0032(10) -0.0037(11) Li1 0.0255(17) 0.033(2) 0.0326(17) 0.0022(14) 0.0049(14) -0.0018(14) _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 C11 2.2070(19) . ? Zr1 C15 2.313(2) . ? Zr1 C12 2.3405(18) . ? Zr1 C10 2.517(2) . ? Zr1 C3 2.525(2) . ? Zr1 C2 2.525(2) . ? Zr1 C6 2.543(2) . ? Zr1 C9 2.548(2) . ? Zr1 C1 2.551(2) . ? Zr1 C8 2.561(2) . ? Zr1 C4 2.564(2) . ? Zr1 C7 2.569(2) . ? C1 C2 1.404(3) . ? C1 C5 1.406(3) . ? C2 C3 1.397(3) . ? C3 C4 1.406(3) . ? C4 C5 1.388(3) . ? C6 C7 1.397(4) . ? C6 C10 1.410(4) . ? C7 C8 1.405(3) . ? C8 C9 1.404(3) . ? C9 C10 1.402(3) . ? C11 C12 1.336(3) . ? C11 C111 1.465(3) . ? C12 C13 1.413(3) . ? C12 Li1 2.374(4) 4_566 ? C13 C14 1.210(3) . ? C13 Li1 2.487(4) 4_566 ? C14 C121 1.435(3) . ? C15 C16 1.223(3) . ? C15 Li1 2.197(4) 4_566 ? C16 C131 1.434(3) . ? C16 Li1 2.609(4) 4_566 ? C111 C116 1.395(3) . ? C111 C112 1.405(3) . ? C112 C113 1.383(3) . ? C113 C114 1.390(3) . ? C114 C115 1.377(3) . ? C115 C116 1.384(3) . ? C121 C122 1.396(3) . ? C121 C126 1.401(3) . ? C122 C123 1.389(3) . ? C123 C124 1.375(3) . ? C124 C125 1.385(3) . ? C125 C126 1.379(3) . ? C131 C132 1.394(3) . ? C131 C136 1.399(3) . ? C132 C133 1.385(3) . ? C133 C134 1.375(3) . ? C134 C135 1.373(4) . ? C135 C136 1.380(4) . ? O100 C104 1.435(3) . ? O100 C101 1.444(3) . ? O100 Li1 1.963(4) 4_566 ? C101 C102 1.488(4) . ? C102 C103 1.506(4) . ? C103 C104 1.519(4) . ? O200 C201 1.426(3) . ? O200 C204 1.430(3) . ? O200 Li1 1.945(4) 4_566 ? C201 C202 1.482(5) . ? C202 C203 1.484(4) . ? C203 C204 1.495(4) . ? Li1 O200 1.945(4) 4_565 ? Li1 O100 1.963(4) 4_565 ? Li1 C15 2.197(4) 4_565 ? Li1 C12 2.374(4) 4_565 ? Li1 C13 2.488(4) 4_565 ? Li1 C16 2.609(4) 4_565 ? Li1 Zr1 3.253(3) 4_565 ? 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 C11 Zr1 C15 122.55(7) . . ? C11 Zr1 C12 34.02(7) . . ? C15 Zr1 C12 88.58(7) . . ? C11 Zr1 C10 98.27(7) . . ? C15 Zr1 C10 124.90(7) . . ? C12 Zr1 C10 121.98(7) . . ? C11 Zr1 C3 100.29(7) . . ? C15 Zr1 C3 122.11(7) . . ? C12 Zr1 C3 125.78(7) . . ? C10 Zr1 C3 78.45(8) . . ? C11 Zr1 C2 75.79(7) . . ? C15 Zr1 C2 121.23(7) . . ? C12 Zr1 C2 94.59(7) . . ? C10 Zr1 C2 102.26(8) . . ? C3 Zr1 C2 32.13(7) . . ? C11 Zr1 C6 128.15(8) . . ? C15 Zr1 C6 94.04(7) . . ? C12 Zr1 C6 139.37(8) . . ? C10 Zr1 C6 32.34(8) . . ? C3 Zr1 C6 86.29(8) . . ? C2 Zr1 C6 117.77(8) . . ? C11 Zr1 C9 75.84(7) . . ? C15 Zr1 C9 120.98(7) . . ? C12 Zr1 C9 91.36(7) . . ? C10 Zr1 C9 32.12(8) . . ? C3 Zr1 C9 104.83(8) . . ? C2 Zr1 C9 117.59(8) . . ? C6 Zr1 C9 53.06(8) . . ? C11 Zr1 C1 86.94(7) . . ? C15 Zr1 C1 89.71(8) . . ? C12 Zr1 C1 88.01(7) . . ? C10 Zr1 C1 131.16(8) . . ? C3 Zr1 C1 52.98(7) . . ? C2 Zr1 C1 32.12(8) . . ? C6 Zr1 C1 132.48(8) . . ? C9 Zr1 C1 149.29(8) . . ? C11 Zr1 C8 89.18(7) . . ? C15 Zr1 C8 89.32(7) . . ? C12 Zr1 C8 86.73(7) . . ? C10 Zr1 C8 53.08(8) . . ? C3 Zr1 C8 131.51(7) . . ? C2 Zr1 C8 149.43(8) . . ? C6 Zr1 C8 52.82(8) . . ? C9 Zr1 C8 31.89(7) . . ? C1 Zr1 C8 174.68(7) . . ? C11 Zr1 C4 128.61(7) . . ? C15 Zr1 C4 90.97(7) . . ? C12 Zr1 C4 140.54(7) . . ? C10 Zr1 C4 89.87(8) . . ? C3 Zr1 C4 32.06(7) . . ? C2 Zr1 C4 52.96(7) . . ? C6 Zr1 C4 80.02(8) . . ? C9 Zr1 C4 121.85(7) . . ? C1 Zr1 C4 52.53(7) . . ? C8 Zr1 C4 132.72(7) . . ? C11 Zr1 C7 120.95(7) . . ? C15 Zr1 C7 73.67(7) . . ? C12 Zr1 C7 113.32(7) . . ? C10 Zr1 C7 52.96(8) . . ? C3 Zr1 C7 117.62(8) . . ? C2 Zr1 C7 149.45(8) . . ? C6 Zr1 C7 31.71(8) . . ? C9 Zr1 C7 52.68(7) . . ? C1 Zr1 C7 152.00(8) . . ? C8 Zr1 C7 31.79(8) . . ? C4 Zr1 C7 104.32(8) . . ? C2 C1 C5 107.81(19) . . ? C2 C1 Zr1 72.91(12) . . ? C5 C1 Zr1 75.42(13) . . ? C3 C2 C1 107.8(2) . . ? C3 C2 Zr1 73.93(12) . . ? C1 C2 Zr1 74.97(12) . . ? C2 C3 C4 108.1(2) . . ? C2 C3 Zr1 73.93(12) . . ? C4 C3 Zr1 75.51(12) . . ? C5 C4 C3 108.1(2) . . ? C5 C4 Zr1 75.17(12) . . ? C3 C4 Zr1 72.43(12) . . ? C4 C5 C1 108.2(2) . . ? C4 C5 Zr1 73.55(13) . . ? C1 C5 Zr1 72.81(13) . . ? C7 C6 C10 107.8(2) . . ? C7 C6 Zr1 75.14(12) . . ? C10 C6 Zr1 72.81(12) . . ? C6 C7 C8 108.3(2) . . ? C6 C7 Zr1 73.15(13) . . ? C8 C7 Zr1 73.80(12) . . ? C9 C8 C7 107.9(2) . . ? C9 C8 Zr1 73.56(13) . . ? C7 C8 Zr1 74.41(13) . . ? C10 C9 C8 108.0(2) . . ? C10 C9 Zr1 72.72(13) . . ? C8 C9 Zr1 74.54(12) . . ? C9 C10 C6 108.0(2) . . ? C9 C10 Zr1 75.16(12) . . ? C6 C10 Zr1 74.85(12) . . ? C12 C11 C111 133.66(17) . . ? C12 C11 Zr1 78.47(12) . . ? C111 C11 Zr1 147.87(13) . . ? C11 C12 C13 127.80(18) . . ? C11 C12 Zr1 67.51(11) . . ? C13 C12 Zr1 164.66(15) . . ? C11 C12 Li1 154.23(16) . 4_566 ? C13 C12 Li1 77.56(14) . 4_566 ? Zr1 C12 Li1 87.27(10) . 4_566 ? C14 C13 C12 177.2(2) . . ? C14 C13 Li1 109.15(16) . 4_566 ? C12 C13 Li1 68.74(13) . 4_566 ? C13 C14 C121 169.4(2) . . ? C16 C15 Li1 95.18(17) . 4_566 ? C16 C15 Zr1 171.76(17) . . ? Li1 C15 Zr1 92.30(12) 4_566 . ? C15 C16 C131 176.1(2) . . ? C15 C16 Li1 56.99(14) . 4_566 ? C131 C16 Li1 123.94(15) . 4_566 ? C116 C111 C112 117.10(19) . . ? C116 C111 C11 119.91(17) . . ? C112 C111 C11 122.98(17) . . ? C113 C112 C111 120.93(19) . . ? C112 C113 C114 120.55(19) . . ? C115 C114 C113 119.4(2) . . ? C114 C115 C116 120.09(19) . . ? C115 C116 C111 121.93(19) . . ? C122 C121 C126 117.84(18) . . ? C122 C121 C14 122.63(19) . . ? C126 C121 C14 119.50(18) . . ? C123 C122 C121 120.7(2) . . ? C124 C123 C122 120.6(2) . . ? C123 C124 C125 119.54(18) . . ? C126 C125 C124 120.3(2) . . ? C125 C126 C121 121.0(2) . . ? C132 C131 C136 117.53(19) . . ? C132 C131 C16 120.25(18) . . ? C136 C131 C16 122.22(19) . . ? C133 C132 C131 121.1(2) . . ? C134 C133 C132 120.3(2) . . ? C135 C134 C133 119.6(2) . . ? C134 C135 C136 120.7(2) . . ? C135 C136 C131 120.8(2) . . ? C104 O100 C101 108.70(18) . . ? C104 O100 Li1 132.68(17) . 4_566 ? C101 O100 Li1 112.92(17) . 4_566 ? O100 C101 C102 105.8(2) . . ? C101 C102 C103 101.6(2) . . ? C102 C103 C104 102.7(2) . . ? O100 C104 C103 105.96(19) . . ? C201 O200 C204 105.92(18) . . ? C201 O200 Li1 123.25(18) . 4_566 ? C204 O200 Li1 125.85(17) . 4_566 ? O200 C201 C202 105.5(2) . . ? C201 C202 C203 104.0(3) . . ? C202 C203 C204 105.6(2) . . ? O200 C204 C203 107.0(2) . . ? O200 Li1 O100 109.07(17) 4_565 4_565 ? O200 Li1 C15 113.02(17) 4_565 4_565 ? O100 Li1 C15 111.00(18) 4_565 4_565 ? O200 Li1 C12 116.56(18) 4_565 4_565 ? O100 Li1 C12 115.55(16) 4_565 4_565 ? C15 Li1 C12 90.55(14) 4_565 4_565 ? O200 Li1 C13 103.97(16) 4_565 4_565 ? O100 Li1 C13 94.25(14) 4_565 4_565 ? C15 Li1 C13 123.55(16) 4_565 4_565 ? C12 Li1 C13 33.70(8) 4_565 4_565 ? O200 Li1 C16 102.66(15) 4_565 4_565 ? O100 Li1 C16 92.11(15) 4_565 4_565 ? C15 Li1 C16 27.84(8) 4_565 4_565 ? C12 Li1 C16 117.70(14) 4_565 4_565 ? C13 Li1 C16 148.82(16) 4_565 4_565 ? O200 Li1 Zr1 120.35(15) 4_565 4_565 ? O100 Li1 Zr1 130.29(15) 4_565 4_565 ? C15 Li1 Zr1 45.27(8) 4_565 4_565 ? C12 Li1 Zr1 45.94(7) 4_565 4_565 ? C13 Li1 Zr1 79.62(10) 4_565 4_565 ? C16 Li1 Zr1 73.07(9) 4_565 4_565 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.545 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.053