data_PhaseII_RT _audit_creation_date 2014-02-08 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ; _chemical_name_common ? _chemical_name_systematic 'Lithium zirconium oxalate dimethiyammonium hydrate' _chemical_formula_moiety 'C16 H2 Li4 O33 Zr2, 4(C2 H8 N)' _chemical_formula_sum 'C24 H34 Li4 N4 O33 Zr2' _chemical_formula_weight 1116.75 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'Zr Li2 N2 C12 O16.5 H17' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'triclinic' _space_group_IT_number 1 _space_group_name_H-M_alt 'P 1' _space_group_name_Hall 'P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' _cell_length_a 8.5302(6) _cell_length_b 8.5902(6) _cell_length_c 16.1582(12) _cell_angle_alpha 89.309(6) _cell_angle_beta 78.004(6) _cell_angle_gamma 68.812(6) _cell_volume 1077.27(13) _cell_formula_units_Z 1 _cell_measurement_reflns_used 5462 _cell_measurement_temperature 299(6) _cell_measurement_theta_max 67.5100 _cell_measurement_theta_min 2.7800 _exptl_absorpt_coefficient_mu 4.969 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_correction_T_min 0.478 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 562 _exptl_crystal_size_max 0.1923 _exptl_crystal_size_mid 0.0796 _exptl_crystal_size_min 0.0537 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0428 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10149 _diffrn_reflns_theta_full 67.75 _diffrn_reflns_theta_max 67.75 _diffrn_reflns_theta_min 2.80 _diffrn_ambient_temperature 299(6) _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1692972000 _diffrn_orient_matrix_UB_12 -0.0014702000 _diffrn_orient_matrix_UB_13 0.0559568000 _diffrn_orient_matrix_UB_21 -0.0992942000 _diffrn_orient_matrix_UB_22 0.1706439000 _diffrn_orient_matrix_UB_23 -0.0307708000 _diffrn_orient_matrix_UB_31 -0.0295563000 _diffrn_orient_matrix_UB_32 -0.0897321000 _diffrn_orient_matrix_UB_33 -0.0739476000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4885 _reflns_number_total 5380 _reflns_odcompleteness_completeness 97.37 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 1.005 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.112 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.33(3) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 613 _refine_ls_number_reflns 5380 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0423 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+0.7458P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1136 _refine_ls_wR_factor_ref 0.1186 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C47) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3.a Rotating group: O2(H2A,H2B) 3.b Secondary CH2 refined with riding coordinates: N46(H46A,H46B), N2(H2F,H2G), N7(H7A,H7B), N1(H1A,H1B) 3.c Idealised Me refined as rotating group: C49(H49A,H49B,H49C), C61(H61A,H61B,H61C), C2(H2C,H2D,H2E), C10(H10A,H10B, H10C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C12(H12A, H12B,H12C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Li3 Li 0.825(3) 0.185(3) 0.3220(17) 0.034(6) Uani 1 1 d . . . . Li6 Li 1.148(3) 0.218(3) 0.3787(15) 0.032(6) Uani 1 1 d . . . . Li8 Li 0.477(7) 1.205(8) 0.850(4) 0.078(6) Uani 1 1 d . . . . Li11 Li 0.4692(19) 1.242(2) 1.3778(10) 0.052(4) Uani 1 1 d . . . . C29 C 0.6531(18) 0.952(2) 0.7084(10) 0.037(4) Uani 1 1 d . . . U C31 C 0.6452(18) 0.9629(18) 0.4410(8) 0.028(3) Uani 1 1 d . . . U C32 C 0.3356(18) 1.4207(16) 0.9802(8) 0.027(3) Uani 1 1 d . . . U C34 C 0.3215(18) 1.4392(16) 1.2563(10) 0.029(3) Uani 1 1 d . . . . C35 C 0.0343(18) 1.9400(18) 1.1893(9) 0.026(3) Uani 1 1 d . . . U C36 C 0.9416(18) 0.4535(19) 0.5089(10) 0.029(3) Uani 1 1 d . . . U C37 C 0.816(2) 0.4375(19) 0.4604(10) 0.032(3) Uani 1 1 d . . . U C38 C 0.1658(17) 1.9610(18) 1.2390(9) 0.025(3) Uani 1 1 d . . . U C39 C 0.5115(17) 1.4316(17) 1.2490(9) 0.023(3) Uani 1 1 d . . . U C40 C 0.462(2) 0.9676(18) 0.4501(10) 0.029(3) Uani 1 1 d . . . U C41 C 0.495(3) 1.853(3) 0.9714(13) 0.059(5) Uani 1 1 d . . . U C43 C 0.525(2) 1.366(2) 0.9737(10) 0.035(4) Uani 1 1 d . . . U C47 C 0.446(2) 1.0171(19) 0.7187(10) 0.032(4) Uani 1 1 d . . . U C50 C 0.3383(19) 0.5759(18) 0.6743(9) 0.031(3) Uani 1 1 d . . . U C51 C 0.633(3) 1.802(2) 1.0234(13) 0.052(5) Uani 1 1 d . . . U C55 C 0.491(2) 0.520(2) 0.7205(11) 0.041(4) Uani 1 1 d . . . U O1 O 0.6033(16) 1.7298(17) 1.0887(8) 0.033(2) Uani 1 1 d . . . . O2 O 0.4266(8) 1.3468(9) 1.4886(4) 0.0606(19) Uani 1 1 d . . . . H2A H 0.4439 1.2728 1.5288 0.091 Uiso 1 1 d . . GR . H2B H 0.3180 1.4201 1.5058 0.091 Uiso 1 1 d . . GR . O3 O 0.8683(16) 0.3205(16) 0.4021(8) 0.043(3) Uani 1 1 d . . . . O4 O 0.1087(15) 2.0680(15) 1.2953(8) 0.037(3) Uani 1 1 d . . . . O5 O 0.6234(15) 1.2629(15) 0.9218(8) 0.054(4) Uani 1 1 d . . . . O6 O 0.3497(15) 1.1341(14) 0.7736(7) 0.042(3) Uani 1 1 d . . . . O7 O 0.7044(15) 1.0420(15) 0.3885(8) 0.044(3) Uani 1 1 d . . . . O8 O 0.2703(14) 1.3553(14) 1.3098(8) 0.039(3) Uani 1 1 d . . . . O9 O 0.0970(10) 1.8191(11) 1.1330(6) 0.029(2) Uani 1 1 d . . . . O10 O 0.4054(12) 0.9400(13) 0.6702(6) 0.034(3) Uani 1 1 d . . . . O11 O 0.5671(14) 1.4498(13) 1.0303(8) 0.048(3) Uani 1 1 d . . . . O12 O 0.6604(13) 0.5373(13) 0.4841(7) 0.036(3) Uani 1 1 d . . . . O13 O 0.8746(13) 0.5758(12) 0.5659(6) 0.032(2) Uani 1 1 d . . . . O14 O 0.3175(14) 1.8538(13) 1.2141(7) 0.033(2) Uani 1 1 d . . . . O15 O 0.6062(14) 0.5772(13) 0.6906(7) 0.038(3) Uani 1 1 d . . . . O16 O 0.3623(15) 1.8143(15) 1.0078(7) 0.042(3) Uani 1 1 d . . . . O17 O 0.6023(14) 1.3417(13) 1.2923(7) 0.034(3) Uani 1 1 d . . . . O18 O 0.2407(13) 1.5556(14) 1.0415(7) 0.040(3) Uani 1 1 d . . . . O19 O 0.2422(14) 1.5314(14) 1.2058(7) 0.034(3) Uani 1 1 d . . . . O20 O 0.7295(11) 0.8422(12) 0.6604(7) 0.032(2) Uani 1 1 d . . . . O21 O 0.4205(13) 0.8751(14) 0.5042(7) 0.036(3) Uani 1 1 d . . . . O22 O 0.7260(12) 0.8625(14) 0.4900(7) 0.035(3) Uani 1 1 d . . . . O23 O 0.5527(11) 1.5237(13) 1.1945(6) 0.028(2) Uani 1 1 d . . . . O24 O -0.1149(13) 2.0357(14) 1.2070(8) 0.047(3) Uani 1 1 d . . . . O25 O 1.0902(13) 0.3544(13) 0.4903(7) 0.037(3) Uani 1 1 d . . . . O26 O 0.3719(14) 1.0590(13) 0.4047(7) 0.034(3) Uani 1 1 d . . . . O27 O 0.6988(14) 1.0389(17) 0.7551(8) 0.057(4) Uani 1 1 d . . . . O28 O 0.2706(15) 1.3577(13) 0.9396(7) 0.048(3) Uani 1 1 d . . . . O30 O 0.5029(18) 1.928(2) 0.9086(9) 0.134(8) Uani 1 1 d . . . . O33B O 0.4946(19) 0.4354(16) 0.7785(10) 0.083(4) Uani 1 1 d . 2 . . O42 O 0.7722(16) 1.8338(19) 0.9991(10) 0.088(5) Uani 1 1 d . . . . O44 O 0.2166(14) 0.5472(18) 0.6959(7) 0.067(4) Uani 1 1 d . . . . O60 O 0.3735(16) 0.6582(17) 0.6100(8) 0.031(2) Uani 1 1 d . . . . Zr1 Zr 0.59693(5) 0.73780(5) 0.58595(3) 0.0229(3) Uani 1 1 d . . . . Zr2 Zr 0.37781(5) 1.65760(5) 1.11165(3) 0.0226(2) Uani 1 1 d . . . . C49 C 0.005(2) 0.992(2) 0.5588(14) 0.071(6) Uani 1 1 d . . . . H49A H 0.0820 1.0422 0.5292 0.106 Uiso 1 1 calc . . GR . H49B H -0.0106 1.0111 0.6188 0.106 Uiso 1 1 calc . . GR . H49C H -0.1048 1.0406 0.5432 0.106 Uiso 1 1 calc . . GR . C61 C 0.138(2) 0.755(3) 0.4454(11) 0.062(6) Uani 1 1 d . . . . H61A H 0.0516 0.8171 0.4153 0.094 Uiso 1 1 calc . . GR . H61B H 0.1598 0.6377 0.4378 0.094 Uiso 1 1 calc . . GR . H61C H 0.2423 0.7747 0.4237 0.094 Uiso 1 1 calc . . GR . N46 N 0.0774(15) 0.8085(16) 0.5356(9) 0.037(3) Uani 1 1 d . . . . H46A H 0.1663 0.7619 0.5610 0.045 Uiso 1 1 calc . . R . H46B H -0.0036 0.7664 0.5574 0.045 Uiso 1 1 calc . . R . C2 C -0.030(3) 0.308(3) 0.7313(17) 0.105(9) Uani 1 1 d . . . . H2C H -0.0321 0.2883 0.6731 0.158 Uiso 1 1 calc . . GR . H2D H -0.1104 0.2681 0.7676 0.158 Uiso 1 1 calc . . GR . H2E H 0.0835 0.2489 0.7403 0.158 Uiso 1 1 calc . . GR . C10 C -0.104(3) 0.518(3) 0.8376(14) 0.095(9) Uani 1 1 d . . . . H10A H -0.1155 0.6323 0.8452 0.143 Uiso 1 1 calc . . GR . H10B H -0.0085 0.4467 0.8597 0.143 Uiso 1 1 calc . . GR . H10C H -0.2078 0.5042 0.8673 0.143 Uiso 1 1 calc . . GR . N2 N -0.0756(18) 0.4733(17) 0.7494(7) 0.042(3) Uani 1 1 d . . . . H2F H -0.1723 0.5291 0.7311 0.050 Uiso 1 1 calc . . R . H2G H 0.0082 0.5062 0.7207 0.050 Uiso 1 1 calc . . R . C13 C 0.835(2) 1.636(2) 1.2516(11) 0.056(5) Uani 1 1 d . . . . H13A H 0.7703 1.7537 1.2618 0.084 Uiso 1 1 calc . . GR . H13B H 0.9340 1.6066 1.2765 0.084 Uiso 1 1 calc . . GR . H13C H 0.7642 1.5751 1.2764 0.084 Uiso 1 1 calc . . GR . C18 C 0.9640(19) 1.408(2) 1.1413(13) 0.060(6) Uani 1 1 d . . . . H18A H 1.0060 1.3814 1.0813 0.089 Uiso 1 1 calc . . GR . H18B H 0.8753 1.3641 1.1615 0.089 Uiso 1 1 calc . . GR . H18C H 1.0569 1.3594 1.1698 0.089 Uiso 1 1 calc . . GR . N7 N 0.8926(18) 1.5921(18) 1.1587(9) 0.043(4) Uani 1 1 d . . . . H7A H 0.8028 1.6376 1.1338 0.052 Uiso 1 1 calc . . R . H7B H 0.9735 1.6343 1.1368 0.052 Uiso 1 1 calc . . R . C9 C 0.014(2) 1.098(2) 0.9660(12) 0.059(4) Uani 1 1 d . . . . H9A H 0.1104 1.1300 0.9425 0.088 Uiso 1 1 calc . . GR . H9B H -0.0166 1.1216 1.0264 0.088 Uiso 1 1 calc . . GR . H9C H -0.0821 1.1608 0.9419 0.088 Uiso 1 1 calc . . GR . C12 C 0.095(3) 0.864(3) 0.8542(12) 0.095(8) Uani 1 1 d . . . . H12A H 0.1417 0.9372 0.8216 0.142 Uiso 1 1 calc . . GR . H12B H -0.0119 0.8735 0.8397 0.142 Uiso 1 1 calc . . GR . H12C H 0.1746 0.7505 0.8419 0.142 Uiso 1 1 calc . . GR . N1 N 0.063(2) 0.911(2) 0.9454(11) 0.063(5) Uani 1 1 d . . . . H1A H 0.1586 0.8538 0.9644 0.076 Uiso 1 1 calc . . R . H1B H -0.0222 0.8794 0.9735 0.076 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 Li3 0.012(9) 0.042(13) 0.040(13) -0.009(10) -0.008(8) 0.002(8) Li6 0.052(13) 0.027(10) 0.026(11) -0.001(8) -0.009(9) -0.026(9) Li8 0.045(10) 0.102(14) 0.073(10) -0.068(9) 0.006(8) -0.021(10) Li11 0.042(8) 0.067(11) 0.062(10) 0.033(8) -0.036(8) -0.025(8) C29 0.032(6) 0.055(7) 0.035(6) 0.004(5) -0.017(5) -0.024(5) C31 0.022(6) 0.038(6) 0.023(6) 0.012(5) -0.006(5) -0.010(5) C32 0.034(5) 0.020(4) 0.020(5) -0.009(4) 0.011(4) -0.012(4) C34 0.024(6) 0.020(5) 0.043(8) -0.010(5) -0.005(6) -0.011(5) C35 0.028(6) 0.026(6) 0.025(6) 0.003(5) -0.005(5) -0.010(5) C36 0.023(6) 0.032(6) 0.030(6) 0.003(5) -0.005(5) -0.008(5) C37 0.039(6) 0.028(6) 0.028(6) 0.004(5) -0.005(5) -0.011(5) C38 0.022(5) 0.032(6) 0.026(5) -0.001(4) -0.004(4) -0.017(4) C39 0.020(5) 0.025(5) 0.022(5) 0.002(4) -0.005(4) -0.006(4) C40 0.030(6) 0.026(5) 0.032(6) -0.002(5) -0.009(5) -0.012(5) C41 0.053(7) 0.078(9) 0.060(8) 0.023(6) -0.023(6) -0.034(6) C43 0.038(6) 0.039(6) 0.033(6) -0.003(5) -0.016(5) -0.014(5) C47 0.031(6) 0.029(6) 0.032(6) 0.000(5) 0.000(5) -0.011(5) C50 0.030(5) 0.035(5) 0.034(5) 0.018(4) -0.006(4) -0.020(4) C51 0.053(7) 0.051(7) 0.058(8) -0.007(6) -0.013(6) -0.024(6) C55 0.042(6) 0.043(6) 0.039(6) 0.017(5) -0.003(4) -0.020(5) O1 0.026(5) 0.046(5) 0.040(6) 0.017(4) -0.009(4) -0.027(4) O2 0.038(3) 0.075(4) 0.072(4) -0.037(4) 0.008(3) -0.034(3) O3 0.040(7) 0.043(7) 0.044(7) -0.016(6) -0.002(6) -0.017(6) O4 0.033(6) 0.038(7) 0.036(6) -0.012(5) -0.011(5) -0.004(5) O5 0.038(6) 0.060(7) 0.061(8) -0.040(6) -0.009(6) -0.012(6) O6 0.042(6) 0.040(6) 0.035(6) 0.000(5) -0.006(5) -0.004(5) O7 0.034(6) 0.052(7) 0.052(8) 0.031(6) -0.011(5) -0.022(6) O8 0.030(6) 0.043(7) 0.046(7) 0.015(5) -0.009(5) -0.017(5) O9 0.006(4) 0.033(5) 0.042(6) -0.014(4) -0.008(4) 0.002(3) O10 0.022(5) 0.053(7) 0.034(5) -0.006(5) -0.013(4) -0.015(4) O11 0.034(6) 0.035(6) 0.060(8) -0.025(5) -0.010(5) 0.006(5) O12 0.017(5) 0.041(6) 0.042(6) -0.016(5) -0.009(4) -0.001(4) O13 0.045(6) 0.033(5) 0.023(5) 0.005(4) -0.012(4) -0.017(4) O14 0.034(6) 0.038(6) 0.035(6) -0.003(5) -0.014(5) -0.018(5) O15 0.034(6) 0.043(6) 0.046(6) 0.018(5) -0.022(5) -0.020(5) O16 0.038(6) 0.065(8) 0.029(6) 0.030(5) -0.010(5) -0.025(6) O17 0.029(6) 0.035(6) 0.036(6) 0.010(5) -0.013(5) -0.005(4) O18 0.038(6) 0.062(7) 0.032(5) -0.008(5) -0.012(4) -0.033(5) O19 0.035(6) 0.045(6) 0.030(6) 0.017(5) -0.013(5) -0.023(5) O20 0.015(4) 0.033(5) 0.038(5) -0.022(4) 0.003(4) 0.000(4) O21 0.035(6) 0.039(6) 0.037(6) 0.019(5) -0.006(5) -0.020(5) O22 0.017(5) 0.043(6) 0.049(7) 0.022(5) -0.012(5) -0.013(4) O23 0.018(5) 0.040(6) 0.035(6) 0.015(4) -0.018(4) -0.014(4) O24 0.019(5) 0.048(7) 0.057(8) 0.000(6) 0.000(5) 0.003(5) O25 0.030(5) 0.044(6) 0.037(6) -0.018(5) -0.011(5) -0.009(5) O26 0.029(6) 0.038(6) 0.039(7) 0.015(5) -0.013(5) -0.014(5) O27 0.030(6) 0.090(9) 0.056(8) -0.005(7) -0.002(5) -0.032(6) O28 0.052(7) 0.057(7) 0.035(6) -0.033(5) -0.005(5) -0.023(5) O30 0.081(8) 0.29(2) 0.091(9) 0.144(12) -0.059(7) -0.123(11) O33B 0.099(9) 0.073(6) 0.095(9) 0.050(6) -0.042(7) -0.042(6) O42 0.050(7) 0.101(10) 0.116(11) 0.028(9) 0.013(6) -0.049(7) O44 0.049(6) 0.119(10) 0.067(7) 0.055(7) -0.039(6) -0.060(7) O60 0.024(4) 0.042(5) 0.029(5) 0.007(4) -0.008(4) -0.013(4) Zr1 0.0203(5) 0.0263(6) 0.0233(6) 0.0026(4) -0.0057(4) -0.0094(4) Zr2 0.0191(5) 0.0272(6) 0.0228(6) 0.0024(4) -0.0062(4) -0.0092(4) C49 0.050(10) 0.054(10) 0.087(15) 0.004(9) 0.000(9) -0.003(7) C61 0.055(11) 0.093(14) 0.049(11) -0.022(9) -0.002(8) -0.042(11) N46 0.024(6) 0.043(7) 0.052(9) 0.016(6) -0.015(6) -0.018(5) C2 0.090(16) 0.084(16) 0.12(2) 0.037(14) -0.022(15) -0.008(12) C10 0.129(19) 0.123(18) 0.077(16) 0.010(13) -0.017(13) -0.099(16) N2 0.049(7) 0.054(8) 0.032(6) 0.018(5) -0.015(5) -0.028(6) C13 0.041(9) 0.079(13) 0.059(12) 0.022(9) -0.017(8) -0.034(9) C18 0.037(8) 0.056(10) 0.099(14) -0.011(9) 0.002(8) -0.041(7) N7 0.043(8) 0.053(8) 0.044(8) 0.010(7) -0.021(7) -0.024(7) C9 0.057(9) 0.046(8) 0.080(12) 0.006(8) -0.034(9) -0.018(7) C12 0.092(14) 0.15(2) 0.038(10) -0.017(11) 0.008(9) -0.056(14) N1 0.037(7) 0.086(12) 0.076(11) 0.014(9) -0.015(7) -0.032(7) _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 Li3 Li6 3.175(15) . ? Li3 Li11 2.84(3) 1_544 ? Li3 O3 1.92(3) . ? Li3 O4 2.20(2) 1_634 ? Li3 O7 2.04(3) 1_545 ? Li3 O17 2.04(2) 1_544 ? Li3 O24 2.14(3) 1_634 ? Li6 Li11 2.82(3) 1_644 ? Li6 C36 2.76(3) . ? Li6 O3 2.17(3) . ? Li6 O4 2.03(3) 1_634 ? Li6 O8 2.03(3) 1_644 ? Li6 O25 2.03(3) . ? Li6 O26 2.03(3) 1_645 ? Li8 C32 2.59(4) . ? Li8 C43 2.62(5) . ? Li8 O5 2.05(5) . ? Li8 O6 2.03(5) . ? Li8 O27 2.21(4) . ? Li8 O28 2.06(4) . ? Li8 O30 2.50(7) 1_545 ? Li8 O33B 2.32(7) 1_565 ? Li11 Li3 2.84(3) 1_566 ? Li11 Li6 2.82(3) 1_466 ? Li11 C31 2.65(2) 1_556 ? Li11 C34 2.78(2) . ? Li11 C39 2.68(2) . ? Li11 C40 2.63(2) 1_556 ? Li11 O2 1.920(18) . ? Li11 O7 2.155(19) 1_556 ? Li11 O8 2.144(18) . ? Li11 O17 1.990(19) . ? Li11 O26 2.028(19) 1_556 ? C29 C47 1.624(19) . ? C29 O20 1.131(18) . ? C29 O27 1.275(19) . ? C31 Li11 2.65(2) 1_554 ? C31 C40 1.53(2) . ? C31 O7 1.222(17) . ? C31 O22 1.275(16) . ? C32 C43 1.49(2) . ? C32 O18 1.413(15) . ? C32 O28 1.185(18) . ? C34 C39 1.578(19) . ? C34 O8 1.230(18) . ? C34 O19 1.255(18) . ? C35 C38 1.57(2) . ? C35 O9 1.270(16) . ? C35 O24 1.215(17) . ? C36 C37 1.50(2) . ? C36 O13 1.285(17) . ? C36 O25 1.220(17) . ? C37 O3 1.273(19) . ? C37 O12 1.270(17) . ? C38 O4 1.192(18) . ? C38 O14 1.271(16) . ? C39 O17 1.210(17) . ? C39 O23 1.258(16) . ? C40 Li11 2.63(2) 1_554 ? C40 O21 1.255(18) . ? C40 O26 1.236(18) . ? C41 C51 1.52(3) . ? C41 O16 1.31(2) . ? C41 O30 1.20(2) . ? C43 O5 1.175(18) . ? C43 O11 1.351(18) . ? C47 O6 1.261(17) . ? C47 O10 1.208(18) . ? C50 C55 1.56(2) . ? C50 O44 1.137(17) . ? C50 O60 1.293(18) . ? C51 O1 1.24(2) . ? C51 O42 1.30(2) . ? C55 O15 1.255(18) . ? C55 O33B 1.180(19) . ? O1 Zr2 2.187(12) . ? O4 Li3 2.20(2) 1_476 ? O4 Li6 2.03(3) 1_476 ? O7 Li3 2.04(3) 1_565 ? O7 Li11 2.155(19) 1_554 ? O8 Li6 2.03(3) 1_466 ? O9 Zr2 2.247(7) . ? O10 Zr1 2.149(10) . ? O11 Zr2 2.148(9) . ? O12 Zr1 2.235(10) . ? O13 Zr1 2.227(10) . ? O14 Zr2 2.221(11) . ? O15 Zr1 2.165(11) . ? O16 Zr2 2.134(10) . ? O17 Li3 2.04(2) 1_566 ? O18 Zr2 2.177(10) . ? O19 Zr2 2.228(10) . ? O20 Zr1 2.203(10) . ? O21 Zr1 2.216(10) . ? O22 Zr1 2.207(10) . ? O23 Zr2 2.212(9) . ? O24 Li3 2.14(3) 1_476 ? O26 Li6 2.03(3) 1_465 ? O26 Li11 2.028(19) 1_554 ? O30 Li8 2.50(7) 1_565 ? O33B Li8 2.32(7) 1_545 ? O60 Zr1 2.209(13) . ? C49 N46 1.49(2) . ? C61 N46 1.46(2) . ? C2 N2 1.35(3) . ? C10 N2 1.43(2) . ? C13 N7 1.48(2) . ? C18 N7 1.48(2) . ? C9 N1 1.53(2) . ? C12 N1 1.48(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 Li11 Li3 Li6 143.7(7) 1_544 . ? O3 Li3 Li6 42.1(7) . . ? O3 Li3 Li11 104.0(10) . 1_544 ? O3 Li3 O4 81.4(9) . 1_634 ? O3 Li3 O7 108.0(13) . 1_545 ? O3 Li3 O17 103.5(11) . 1_544 ? O3 Li3 O24 155.0(13) . 1_634 ? O4 Li3 Li6 39.4(7) 1_634 . ? O4 Li3 Li11 162.4(13) 1_634 1_544 ? O7 Li3 Li6 118.8(8) 1_545 . ? O7 Li3 Li11 49.0(6) 1_545 1_544 ? O7 Li3 O4 113.5(12) 1_545 1_634 ? O7 Li3 O17 92.1(10) 1_545 1_544 ? O7 Li3 O24 92.1(12) 1_545 1_634 ? O17 Li3 Li6 137.5(10) 1_544 . ? O17 Li3 Li11 44.4(6) 1_544 1_544 ? O17 Li3 O4 151.4(15) 1_544 1_634 ? O17 Li3 O24 90.1(11) 1_544 1_634 ? O24 Li3 Li6 115.1(7) 1_634 . ? O24 Li3 Li11 100.4(10) 1_634 1_544 ? O24 Li3 O4 76.8(8) 1_634 1_634 ? Li11 Li6 Li3 163.4(7) 1_644 . ? C36 Li6 Li3 92.5(7) . . ? C36 Li6 Li11 100.0(9) . 1_644 ? O3 Li6 Li3 36.4(7) . . ? O3 Li6 Li11 152.7(11) . 1_644 ? O3 Li6 C36 56.4(7) . . ? O4 Li6 Li3 43.5(7) 1_634 . ? O4 Li6 Li11 124.3(12) 1_634 1_644 ? O4 Li6 C36 135.6(12) 1_634 . ? O4 Li6 O3 79.9(10) 1_634 . ? O4 Li6 O25 154.4(14) 1_634 . ? O4 Li6 O26 100.1(11) 1_634 1_645 ? O8 Li6 Li3 118.1(9) 1_644 . ? O8 Li6 Li11 49.2(7) 1_644 1_644 ? O8 Li6 C36 99.3(9) 1_644 . ? O8 Li6 O3 116.0(12) 1_644 . ? O8 Li6 O4 107.2(12) 1_644 1_634 ? O8 Li6 O25 95.3(11) 1_644 . ? O8 Li6 O26 91.5(11) 1_644 1_645 ? O25 Li6 Li3 114.7(9) . . ? O25 Li6 Li11 79.6(9) . 1_644 ? O25 Li6 C36 23.9(5) . . ? O25 Li6 O3 79.4(9) . . ? O26 Li6 Li3 136.7(8) 1_645 . ? O26 Li6 Li11 45.9(7) 1_645 1_644 ? O26 Li6 C36 114.4(11) 1_645 . ? O26 Li6 O3 151.5(13) 1_645 . ? O26 Li6 O25 91.1(11) 1_645 . ? C32 Li8 C43 33.2(7) . . ? O5 Li8 C32 58.8(12) . . ? O5 Li8 C43 25.6(7) . . ? O5 Li8 O27 95(2) . . ? O5 Li8 O28 84.8(17) . . ? O5 Li8 O30 96(3) . 1_545 ? O5 Li8 O33B 84(2) . 1_565 ? O6 Li8 C32 126(2) . . ? O6 Li8 C43 159(2) . . ? O6 Li8 O5 175(2) . . ? O6 Li8 O27 80.3(16) . . ? O6 Li8 O28 100(2) . . ? O6 Li8 O30 82(2) . 1_545 ? O6 Li8 O33B 97(3) . 1_565 ? O27 Li8 C32 154(3) . . ? O27 Li8 C43 121(2) . . ? O27 Li8 O30 80.1(19) . 1_545 ? O27 Li8 O33B 90(2) . 1_565 ? O28 Li8 C32 26.5(7) . . ? O28 Li8 C43 59.4(12) . . ? O28 Li8 O27 179(4) . . ? O28 Li8 O30 99(3) . 1_545 ? O28 Li8 O33B 91(2) . 1_565 ? O30 Li8 C32 105(2) 1_545 . ? O30 Li8 C43 103(2) 1_545 . ? O33B Li8 C32 83.6(17) 1_565 . ? O33B Li8 C43 82.0(18) 1_565 . ? O33B Li8 O30 170(2) 1_565 1_545 ? Li6 Li11 Li3 158.6(11) 1_466 1_566 ? C31 Li11 Li3 72.3(7) 1_556 1_566 ? C31 Li11 Li6 105.0(8) 1_556 1_466 ? C31 Li11 C34 156.6(9) 1_556 . ? C31 Li11 C39 139.8(8) 1_556 . ? C34 Li11 Li3 103.2(8) . 1_566 ? C34 Li11 Li6 70.5(7) . 1_466 ? C39 Li11 Li3 70.6(7) . 1_566 ? C39 Li11 Li6 103.8(7) . 1_466 ? C39 Li11 C34 33.6(4) . . ? C40 Li11 Li3 104.8(8) 1_556 1_566 ? C40 Li11 Li6 71.6(7) 1_556 1_466 ? C40 Li11 C31 33.6(5) 1_556 1_556 ? C40 Li11 C34 137.3(7) 1_556 . ? C40 Li11 C39 156.3(9) 1_556 . ? O2 Li11 Li3 99.7(8) . 1_566 ? O2 Li11 Li6 101.3(8) . 1_466 ? O2 Li11 C31 85.9(6) . 1_556 ? O2 Li11 C34 117.5(8) . . ? O2 Li11 C39 115.0(8) . . ? O2 Li11 C40 88.6(7) . 1_556 ? O2 Li11 O7 95.4(7) . 1_556 ? O2 Li11 O8 114.3(9) . . ? O2 Li11 O17 110.2(9) . . ? O2 Li11 O26 101.5(8) . 1_556 ? O7 Li11 Li3 45.6(7) 1_556 1_566 ? O7 Li11 Li6 127.4(9) 1_556 1_466 ? O7 Li11 C31 27.1(4) 1_556 1_556 ? O7 Li11 C34 139.9(9) 1_556 . ? O7 Li11 C39 113.3(8) 1_556 . ? O7 Li11 C40 59.2(6) 1_556 1_556 ? O8 Li11 Li3 126.7(9) . 1_566 ? O8 Li11 Li6 45.7(6) . 1_466 ? O8 Li11 C31 145.4(9) . 1_556 ? O8 Li11 C34 24.9(4) . . ? O8 Li11 C39 58.4(5) . . ? O8 Li11 C40 115.3(8) . 1_556 ? O8 Li11 O7 150.1(11) . 1_556 ? O17 Li11 Li3 45.9(7) . 1_566 ? O17 Li11 Li6 127.9(8) . 1_466 ? O17 Li11 C31 117.4(8) . 1_556 ? O17 Li11 C34 58.4(6) . . ? O17 Li11 C39 25.0(5) . . ? O17 Li11 C40 146.2(9) . 1_556 ? O17 Li11 O7 90.3(8) . 1_556 ? O17 Li11 O8 83.2(7) . . ? O17 Li11 O26 147.9(12) . 1_556 ? O26 Li11 Li3 124.8(9) 1_556 1_566 ? O26 Li11 Li6 46.1(7) 1_556 1_466 ? O26 Li11 C31 59.2(6) 1_556 1_556 ? O26 Li11 C34 110.7(7) 1_556 . ? O26 Li11 C39 137.8(8) 1_556 . ? O26 Li11 C40 27.0(5) 1_556 1_556 ? O26 Li11 O7 81.9(7) 1_556 1_556 ? O26 Li11 O8 88.3(7) 1_556 . ? O20 C29 C47 115.0(13) . . ? O20 C29 O27 132.2(14) . . ? O27 C29 C47 112.8(14) . . ? C40 C31 Li11 72.6(9) . 1_554 ? O7 C31 Li11 53.4(9) . 1_554 ? O7 C31 C40 121.4(14) . . ? O7 C31 O22 126.2(14) . . ? O22 C31 Li11 161.6(12) . 1_554 ? O22 C31 C40 112.2(12) . . ? C43 C32 Li8 74.4(14) . . ? O18 C32 Li8 169.9(19) . . ? O18 C32 C43 112.3(12) . . ? O28 C32 Li8 50.6(14) . . ? O28 C32 C43 124.4(12) . . ? O28 C32 O18 123.3(13) . . ? C39 C34 Li11 69.6(8) . . ? O8 C34 Li11 47.2(9) . . ? O8 C34 C39 116.7(14) . . ? O8 C34 O19 128.5(15) . . ? O19 C34 Li11 175.0(12) . . ? O19 C34 C39 114.8(13) . . ? O9 C35 C38 114.9(12) . . ? O24 C35 C38 119.5(14) . . ? O24 C35 O9 125.5(15) . . ? C37 C36 Li6 76.8(10) . . ? O13 C36 Li6 166.7(12) . . ? O13 C36 C37 113.1(13) . . ? O25 C36 Li6 42.6(9) . . ? O25 C36 C37 118.5(14) . . ? O25 C36 O13 128.4(15) . . ? O3 C37 C36 118.5(14) . . ? O12 C37 C36 116.8(14) . . ? O12 C37 O3 124.5(16) . . ? O4 C38 C35 116.4(13) . . ? O4 C38 O14 130.3(15) . . ? O14 C38 C35 113.2(13) . . ? C34 C39 Li11 76.9(9) . . ? O17 C39 Li11 44.0(8) . . ? O17 C39 C34 120.5(14) . . ? O17 C39 O23 126.6(14) . . ? O23 C39 Li11 169.4(11) . . ? O23 C39 C34 112.8(12) . . ? C31 C40 Li11 73.8(9) . 1_554 ? O21 C40 Li11 159.7(12) . 1_554 ? O21 C40 C31 114.6(14) . . ? O26 C40 Li11 48.2(8) . 1_554 ? O26 C40 C31 118.0(14) . . ? O26 C40 O21 127.4(15) . . ? O16 C41 C51 111.0(17) . . ? O30 C41 C51 123.8(18) . . ? O30 C41 O16 124.9(18) . . ? C32 C43 Li8 72.4(14) . . ? O5 C43 Li8 49.0(13) . . ? O5 C43 C32 121.2(15) . . ? O5 C43 O11 125.3(16) . . ? O11 C43 Li8 172.7(17) . . ? O11 C43 C32 113.4(13) . . ? O6 C47 C29 119.3(15) . . ? O10 C47 C29 111.8(12) . . ? O10 C47 O6 128.9(15) . . ? O44 C50 C55 123.7(13) . . ? O44 C50 O60 127.2(15) . . ? O60 C50 C55 109.1(13) . . ? O1 C51 C41 116.3(18) . . ? O1 C51 O42 123.4(18) . . ? O42 C51 C41 120.2(18) . . ? O15 C55 C50 113.3(13) . . ? O33B C55 C50 122.2(15) . . ? O33B C55 O15 124.5(18) . . ? C51 O1 Zr2 118.5(13) . . ? Li3 O3 Li6 101.6(10) . . ? C37 O3 Li3 151.3(13) . . ? C37 O3 Li6 107.2(12) . . ? Li6 O4 Li3 97.1(11) 1_476 1_476 ? C38 O4 Li3 113.1(12) . 1_476 ? C38 O4 Li6 149.5(13) . 1_476 ? C43 O5 Li8 105.4(16) . . ? C47 O6 Li8 114.1(17) . . ? Li3 O7 Li11 85.3(8) 1_565 1_554 ? C31 O7 Li3 167.3(14) . 1_565 ? C31 O7 Li11 99.5(11) . 1_554 ? Li6 O8 Li11 85.1(10) 1_466 . ? C34 O8 Li6 166.0(14) . 1_466 ? C34 O8 Li11 107.9(11) . . ? C35 O9 Zr2 119.3(9) . . ? C47 O10 Zr1 121.1(9) . . ? C43 O11 Zr2 122.0(10) . . ? C37 O12 Zr1 118.6(10) . . ? C36 O13 Zr1 120.6(10) . . ? C38 O14 Zr2 121.2(10) . . ? C55 O15 Zr1 124.4(11) . . ? C41 O16 Zr2 120.4(12) . . ? Li11 O17 Li3 89.7(10) . 1_566 ? C39 O17 Li3 157.1(13) . 1_566 ? C39 O17 Li11 111.1(11) . . ? C32 O18 Zr2 119.2(9) . . ? C34 O19 Zr2 119.5(10) . . ? C29 O20 Zr1 120.3(9) . . ? C40 O21 Zr1 120.9(10) . . ? C31 O22 Zr1 121.8(9) . . ? C39 O23 Zr2 121.1(9) . . ? C35 O24 Li3 112.5(12) . 1_476 ? C36 O25 Li6 113.5(12) . . ? Li11 O26 Li6 88.0(9) 1_554 1_465 ? C40 O26 Li6 154.6(13) . 1_465 ? C40 O26 Li11 104.8(11) . 1_554 ? C29 O27 Li8 111.6(18) . . ? C32 O28 Li8 102.9(18) . . ? C41 O30 Li8 146(2) . 1_565 ? C55 O33B Li8 156(2) . 1_545 ? C50 O60 Zr1 123.4(11) . . ? O10 Zr1 O12 148.8(4) . . ? O10 Zr1 O13 140.0(4) . . ? O10 Zr1 O15 88.8(4) . . ? O10 Zr1 O20 71.8(3) . . ? O10 Zr1 O21 76.9(4) . . ? O10 Zr1 O22 104.2(4) . . ? O10 Zr1 O60 78.0(4) . . ? O13 Zr1 O12 70.6(4) . . ? O15 Zr1 O12 96.3(4) . . ? O15 Zr1 O13 76.3(4) . . ? O15 Zr1 O20 80.8(4) . . ? O15 Zr1 O21 140.5(4) . . ? O15 Zr1 O22 149.6(4) . . ? O15 Zr1 O60 69.2(4) . . ? O20 Zr1 O12 139.4(3) . . ? O20 Zr1 O13 69.3(3) . . ? O20 Zr1 O21 126.8(4) . . ? O20 Zr1 O22 77.6(4) . . ? O20 Zr1 O60 137.5(4) . . ? O21 Zr1 O12 79.9(4) . . ? O21 Zr1 O13 135.9(4) . . ? O22 Zr1 O12 86.7(4) . . ? O22 Zr1 O13 76.3(3) . . ? O22 Zr1 O21 69.8(4) . . ? O22 Zr1 O60 139.8(5) . . ? O60 Zr1 O12 75.2(4) . . ? O60 Zr1 O13 127.6(4) . . ? O60 Zr1 O21 71.8(4) . . ? O1 Zr2 O9 129.5(4) . . ? O1 Zr2 O14 75.7(5) . . ? O1 Zr2 O19 140.5(5) . . ? O1 Zr2 O23 70.3(4) . . ? O11 Zr2 O1 78.3(5) . . ? O11 Zr2 O9 140.1(4) . . ? O11 Zr2 O14 148.5(4) . . ? O11 Zr2 O18 72.7(4) . . ? O11 Zr2 O19 102.2(5) . . ? O11 Zr2 O23 76.6(4) . . ? O14 Zr2 O9 71.3(4) . . ? O14 Zr2 O19 87.3(4) . . ? O16 Zr2 O1 72.1(5) . . ? O16 Zr2 O9 75.8(4) . . ? O16 Zr2 O11 90.6(5) . . ? O16 Zr2 O14 97.8(4) . . ? O16 Zr2 O18 80.2(5) . . ? O16 Zr2 O19 146.5(5) . . ? O16 Zr2 O23 142.0(4) . . ? O18 Zr2 O1 139.3(4) . . ? O18 Zr2 O9 68.1(4) . . ? O18 Zr2 O14 138.5(4) . . ? O18 Zr2 O19 74.4(4) . . ? O18 Zr2 O23 127.3(4) . . ? O19 Zr2 O9 74.6(4) . . ? O23 Zr2 O9 134.9(4) . . ? O23 Zr2 O14 78.2(4) . . ? O23 Zr2 O19 71.5(4) . . ? C61 N46 C49 117.2(15) . . ? C2 N2 C10 113.6(17) . . ? C18 N7 C13 110.3(14) . . ? C12 N1 C9 113.9(17) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 3 3 8 0.0392 3.0000 3.0000 8.0000 -0.0646 -0.0321 -0.9494 -3 -3 -8 0.0362 -3.0000 -3.0000 -8.0000 0.0646 0.0321 0.9494 2 4 -7 0.0938 2.0000 4.0000 -7.0001 -0.7362 0.6994 0.0996 -2 -4 7 0.0758 -2.0000 -4.0000 7.0001 0.7362 -0.6994 -0.0996 3 -2 -5 0.0259 3.0000 -2.0000 -5.0001 -0.7847 -0.4853 0.4605 -3 2 5 0.0279 -3.0000 2.0000 5.0001 0.7847 0.4853 -0.4605 5 2 6 0.0390 5.0000 2.0000 6.0000 -0.5137 -0.3398 -0.7709 -5 -2 -6 0.0380 -5.0000 -2.0000 -6.0000 0.5137 0.3398 0.7709