# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1525 data_POB9704 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H66 N2 O8 Zr2' _chemical_formula_weight 741.27 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1455(9) _cell_length_b 12.4123(11) _cell_length_c 17.585(2) _cell_angle_alpha 104.847(9) _cell_angle_beta 92.927(10) _cell_angle_gamma 113.762(8) _cell_volume 1929.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.32 _cell_measurement_theta_max 12.49 _exptl_crystal_description blocks _exptl_crystal_colour Clear _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.83 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method ? _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 12.05 _diffrn_reflns_number 7067 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6656 _reflns_number_observed 5164 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.8241P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6654 _refine_ls_number_parameters 451 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_obs 0.0380 _refine_ls_wR_factor_all 0.0949 _refine_ls_wR_factor_obs 0.0850 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.19184(4) -0.11469(3) 0.23505(2) 0.03127(10) Uani 1 d . . Zr2 Zr 0.27382(4) 0.17783(3) 0.25658(2) 0.03640(11) Uani 1 d . . N1 N 0.2595(4) -0.1819(3) 0.1029(2) 0.0461(8) Uani 1 d . . C2 C 0.4125(5) -0.0919(4) 0.1078(3) 0.0511(10) Uani 1 d . . H2A H 0.4387(5) -0.1035(4) 0.0544(3) 0.061 Uiso 1 calc R . H2B H 0.4788(5) -0.1065(4) 0.1420(3) 0.061 Uiso 1 calc R . C3 C 0.4299(4) 0.0383(4) 0.1413(2) 0.0468(9) Uani 1 d . . H3A H 0.3774(4) 0.0577(4) 0.1016(2) 0.056 Uiso 1 calc R . O4 O 0.3649(3) 0.0439(2) 0.21069(15) 0.0376(6) Uani 1 d . . C5 C 0.5899(5) 0.1310(4) 0.1615(3) 0.0646(13) Uani 1 d . . H5A H 0.5971(5) 0.2138(4) 0.1829(3) 0.097 Uiso 1 calc R . H5B H 0.6331(5) 0.1253(4) 0.1135(3) 0.097 Uiso 1 calc R . H5C H 0.6416(5) 0.1131(4) 0.2009(3) 0.097 Uiso 1 calc R . C7 C 0.2547(6) -0.3066(4) 0.0853(3) 0.0627(12) Uani 1 d . . H7A H 0.3191(6) -0.3081(4) 0.1273(3) 0.094 Uiso 1 calc R . H7B H 0.2864(6) -0.3271(4) 0.0346(3) 0.094 Uiso 1 calc R . H7C H 0.1555(6) -0.3665(4) 0.0823(3) 0.094 Uiso 1 calc R . C8 C 0.1617(5) -0.1804(5) 0.0389(2) 0.0605(12) Uani 1 d . . H8A H 0.1644(5) -0.0988(5) 0.0502(2) 0.091 Uiso 1 calc R . H8B H 0.0625(5) -0.2405(5) 0.0360(2) 0.091 Uiso 1 calc R . H8C H 0.1935(5) -0.2011(5) -0.0117(2) 0.091 Uiso 1 calc R . N11 N 0.0917(4) -0.1573(3) 0.3591(2) 0.0471(8) Uani 1 d . . C12 C 0.1947(5) -0.0527(4) 0.4261(2) 0.0498(10) Uani 1 d . . H12A H 0.2872(5) -0.0594(4) 0.4334(2) 0.060 Uiso 1 calc R . H12B H 0.1541(5) -0.0543(4) 0.4754(2) 0.060 Uiso 1 calc R . C13 C 0.2221(5) 0.0678(4) 0.4096(2) 0.0461(9) Uani 1 d . . H13A H 0.1323(5) 0.0810(4) 0.4120(2) 0.055 Uiso 1 calc R . O14 O 0.2529(3) 0.0545(2) 0.33108(14) 0.0387(6) Uani 1 d . . C15 C 0.3465(6) 0.1755(4) 0.4700(3) 0.0714(14) Uani 1 d . . H15A H 0.3617(6) 0.2513(4) 0.4580(3) 0.107 Uiso 1 calc R . H15B H 0.4350(6) 0.1633(4) 0.4676(3) 0.107 Uiso 1 calc R . H15C H 0.3225(6) 0.1810(4) 0.5231(3) 0.107 Uiso 1 calc R . C17 C -0.0572(5) -0.1628(5) 0.3591(3) 0.0688(14) Uani 1 d . . H17A H -0.1248(5) -0.2319(5) 0.3148(3) 0.103 Uiso 1 calc R . H17B H -0.0558(5) -0.0866(5) 0.3535(3) 0.103 Uiso 1 calc R . H17C H -0.0884(5) -0.1735(5) 0.4089(3) 0.103 Uiso 1 calc R . C18 C 0.0876(6) -0.2729(4) 0.3689(3) 0.0630(13) Uani 1 d . . H18A H 0.0198(6) -0.3423(4) 0.3248(3) 0.095 Uiso 1 calc R . H18B H 0.0557(6) -0.2823(4) 0.4188(3) 0.095 Uiso 1 calc R . H18C H 0.1845(6) -0.2703(4) 0.3695(3) 0.095 Uiso 1 calc R . O21 O 0.3357(2) -0.1640(2) 0.27415(15) 0.0430(6) Uani 1 d D . C22 C 0.4795(4) -0.1499(6) 0.2908(4) 0.052(2) Uani 0.55 d PD 1 H22A H 0.5240(4) -0.1436(6) 0.2424(4) 0.063 Uiso 0.55 calc PR 1 C23 C 0.5700(9) -0.0341(8) 0.3577(9) 0.082(7) Uani 0.55 d PD 1 H23A H 0.5679(9) 0.0363(8) 0.3443(9) 0.123 Uiso 0.55 calc PR 1 H23B H 0.6701(9) -0.0240(8) 0.3657(9) 0.123 Uiso 0.55 calc PR 1 H23C H 0.5304(9) -0.0398(8) 0.4063(9) 0.123 Uiso 0.55 calc PR 1 C24 C 0.4821(10) -0.2595(8) 0.3111(8) 0.086(4) Uani 0.55 d PDU 1 H24A H 0.4235(10) -0.3341(8) 0.2676(8) 0.130 Uiso 0.55 calc PR 1 H24B H 0.4424(10) -0.2655(8) 0.3596(8) 0.130 Uiso 0.55 calc PR 1 H24C H 0.5821(10) -0.2498(8) 0.3190(8) 0.130 Uiso 0.55 calc PR 1 C22' C 0.4530(6) -0.1557(8) 0.3249(4) 0.060(3) Uiso 0.45 d PD 2 H22B H 0.4183(6) -0.1719(8) 0.3742(4) 0.072 Uiso 0.45 calc PR 2 C23' C 0.5774(9) -0.0290(10) 0.3478(11) 0.076(8) Uiso 0.45 d PD 2 H23D H 0.5429(9) 0.0319(10) 0.3722(11) 0.114 Uiso 0.45 calc PR 2 H23E H 0.6158(9) -0.0126(10) 0.3005(11) 0.114 Uiso 0.45 calc PR 2 H23F H 0.6541(9) -0.0244(10) 0.3856(11) 0.114 Uiso 0.45 calc PR 2 C24' C 0.5061(13) -0.2501(12) 0.2871(9) 0.085(5) Uiso 0.45 d PDU 2 H24D H 0.4255(13) -0.3319(12) 0.2723(9) 0.128 Uiso 0.45 calc PR 2 H24E H 0.5827(13) -0.2457(12) 0.3248(9) 0.128 Uiso 0.45 calc PR 2 H24F H 0.5444(13) -0.2339(12) 0.2398(9) 0.128 Uiso 0.45 calc PR 2 O25 O 0.0154(3) -0.2716(2) 0.1862(2) 0.0457(6) Uani 1 d D . C26 C -0.0915(7) -0.3840(5) 0.1356(4) 0.061(3) Uani 0.50 d PD 1 H26A H -0.0694(7) -0.3920(5) 0.0808(4) 0.073 Uiso 0.50 calc PR 1 C27 C -0.0896(19) -0.4918(3) 0.1586(11) 0.098(10) Uani 0.50 d PD 1 H27A H 0.0076(19) -0.4887(3) 0.1595(11) 0.147 Uiso 0.50 calc PR 1 H27B H -0.1595(19) -0.5681(3) 0.1200(11) 0.147 Uiso 0.50 calc PR 1 H27C H -0.1157(19) -0.4883(3) 0.2112(11) 0.147 Uiso 0.50 calc PR 1 C28 C -0.2415(4) -0.3884(14) 0.1342(8) 0.093(5) Uani 0.50 d PD 1 H28A H -0.2423(4) -0.3186(14) 0.1193(8) 0.140 Uiso 0.50 calc PR 1 H28B H -0.2677(4) -0.3848(14) 0.1868(8) 0.140 Uiso 0.50 calc PR 1 H28C H -0.3115(4) -0.4646(14) 0.0956(8) 0.140 Uiso 0.50 calc PR 1 C26' C -0.1096(7) -0.3839(5) 0.1685(5) 0.063(3) Uani 0.50 d PD 2 H26B H -0.1655(7) -0.3789(5) 0.2128(5) 0.076 Uiso 0.50 calc PR 2 C27' C -0.0709(20) -0.4901(4) 0.1623(11) 0.081(8) Uani 0.50 d PD 2 H27D H -0.0082(20) -0.4742(4) 0.2112(11) 0.121 Uiso 0.50 calc PR 2 H27E H -0.0199(20) -0.4994(4) 0.1176(11) 0.121 Uiso 0.50 calc PR 2 H27F H -0.1595(20) -0.5653(4) 0.1539(11) 0.121 Uiso 0.50 calc PR 2 C28' C -0.2066(10) -0.4081(12) 0.0929(8) 0.105(6) Uani 0.50 d PD 2 H28D H -0.2315(10) -0.3393(12) 0.0971(8) 0.157 Uiso 0.50 calc PR 2 H28E H -0.2953(10) -0.4832(12) 0.0845(8) 0.157 Uiso 0.50 calc PR 2 H28F H -0.1557(10) -0.4173(12) 0.0482(8) 0.157 Uiso 0.50 calc PR 2 O29 O 0.0868(2) -0.0124(2) 0.19283(14) 0.0405(6) Uani 1 d D . C30 C -0.0503(3) -0.0475(3) 0.1479(2) 0.0459(9) Uani 1 d D . H30A H -0.0767(3) -0.1275(3) 0.1067(2) 0.055 Uiso 1 calc R . C31 C -0.1665(3) -0.0650(5) 0.1992(3) 0.078(2) Uani 1 d D . H31A H -0.1685(3) -0.1246(5) 0.2262(3) 0.118 Uiso 1 calc R . H31B H -0.2609(3) -0.0950(5) 0.1660(3) 0.118 Uiso 1 calc R . H31C H -0.1452(3) 0.0133(5) 0.2386(3) 0.118 Uiso 1 calc R . C32 C -0.0473(4) 0.0446(4) 0.1063(3) 0.0691(14) Uani 1 d D . H32A H 0.0278(4) 0.0560(4) 0.0732(3) 0.104 Uiso 1 calc R . H32B H -0.0260(4) 0.1228(4) 0.1457(3) 0.104 Uiso 1 calc R . H32C H -0.1417(4) 0.0146(4) 0.0731(3) 0.104 Uiso 1 calc R . O33 O 0.1385(3) 0.2369(2) 0.3061(2) 0.0531(7) Uani 1 d D . C34 C 0.0612(6) 0.3029(5) 0.3402(3) 0.073(2) Uani 0.75 d PDU 1 H34A H -0.0280(6) 0.2773(5) 0.3013(3) 0.087 Uiso 0.75 calc PR 1 C35 C 0.1497(11) 0.4395(4) 0.3578(6) 0.118(4) Uani 0.75 d PD 1 H35A H 0.1797(11) 0.4574(4) 0.3093(6) 0.177 Uiso 0.75 calc PR 1 H35B H 0.2357(11) 0.4671(4) 0.3976(6) 0.177 Uiso 0.75 calc PR 1 H35C H 0.0911(11) 0.4821(4) 0.3781(6) 0.177 Uiso 0.75 calc PR 1 C36 C 0.0150(12) 0.2754(9) 0.4153(5) 0.098(4) Uani 0.75 d PDU 1 H36A H -0.0422(12) 0.1872(9) 0.4040(5) 0.148 Uiso 0.75 calc PR 1 H36B H -0.0436(12) 0.3182(9) 0.4355(5) 0.148 Uiso 0.75 calc PR 1 H36C H 0.1011(12) 0.3031(9) 0.4550(5) 0.148 Uiso 0.75 calc PR 1 C34' C 0.0926(20) 0.3199(14) 0.3536(8) 0.158(16) Uiso 0.25 d PDU 2 H34B H 0.1769(20) 0.3831(14) 0.3950(8) 0.189 Uiso 0.25 calc PR 2 C35' C 0.0423(28) 0.3842(19) 0.3054(16) 0.103(9) Uiso 0.25 d PD 2 H35D H 0.1201(28) 0.4254(19) 0.2786(16) 0.155 Uiso 0.25 calc PR 2 H35E H 0.0173(28) 0.4448(19) 0.3404(16) 0.155 Uiso 0.25 calc PR 2 H35F H -0.0430(28) 0.3241(19) 0.2658(16) 0.155 Uiso 0.25 calc PR 2 C36' C -0.0278(38) 0.2563(33) 0.3950(20) 0.116(11) Uiso 0.25 d PDU 2 H36D H 0.0046(38) 0.2146(33) 0.4262(20) 0.174 Uiso 0.25 calc PR 2 H36E H -0.1131(38) 0.1963(33) 0.3554(20) 0.174 Uiso 0.25 calc PR 2 H36F H -0.0527(38) 0.3169(33) 0.4300(20) 0.174 Uiso 0.25 calc PR 2 O37 O 0.2910(3) 0.2298(3) 0.1597(2) 0.0564(8) Uani 1 d D . C38 C 0.2871(8) 0.2827(6) 0.0984(3) 0.050(2) Uani 0.50 d PDU 1 H38A H 0.1890(8) 0.2364(6) 0.0645(3) 0.060 Uiso 0.50 calc PR 1 C39 C 0.3994(14) 0.2757(11) 0.0475(6) 0.058(4) Uani 0.50 d PDU 1 H39A H 0.3821(14) 0.1902(11) 0.0253(6) 0.087 Uiso 0.50 calc PR 1 H39B H 0.4963(14) 0.3226(11) 0.0798(6) 0.087 Uiso 0.50 calc PR 1 H39C H 0.3925(14) 0.3099(11) 0.0044(6) 0.087 Uiso 0.50 calc PR 1 C40 C 0.3141(21) 0.4153(9) 0.1327(8) 0.140(7) Uani 0.50 d PDU 1 H40A H 0.2416(21) 0.4199(9) 0.1657(8) 0.210 Uiso 0.50 calc PR 1 H40B H 0.3071(21) 0.4493(9) 0.0896(8) 0.210 Uiso 0.50 calc PR 1 H40C H 0.4110(21) 0.4622(9) 0.1650(8) 0.210 Uiso 0.50 calc PR 1 C38' C 0.3542(9) 0.3328(5) 0.1321(5) 0.071(3) Uani 0.50 d PDU 2 H38B H 0.4409(9) 0.3960(5) 0.1720(5) 0.086 Uiso 0.50 calc PR 2 C39' C 0.4031(20) 0.3000(15) 0.0540(8) 0.127(9) Uani 0.50 d PDU 2 H39D H 0.4715(20) 0.2650(15) 0.0598(8) 0.190 Uiso 0.50 calc PR 2 H39E H 0.4504(20) 0.3738(15) 0.0379(8) 0.190 Uiso 0.50 calc PR 2 H39F H 0.3189(20) 0.2401(15) 0.0137(8) 0.190 Uiso 0.50 calc PR 2 C40' C 0.2483(18) 0.3873(12) 0.1235(9) 0.113(5) Uani 0.50 d PDU 2 H40D H 0.2169(18) 0.4083(12) 0.1742(9) 0.169 Uiso 0.50 calc PR 2 H40E H 0.1640(18) 0.3276(12) 0.0832(9) 0.169 Uiso 0.50 calc PR 2 H40F H 0.2956(18) 0.4612(12) 0.1076(9) 0.169 Uiso 0.50 calc PR 2 O41 O 0.4555(3) 0.3077(2) 0.3218(2) 0.0639(8) Uani 1 d D . C42 C 0.5721(5) 0.4044(4) 0.3788(3) 0.065(2) Uani 0.60 d PD 1 H42A H 0.5361(5) 0.4218(4) 0.4297(3) 0.078 Uiso 0.60 calc PR 1 C43 C 0.6266(11) 0.5195(5) 0.3537(7) 0.112(5) Uani 0.60 d PD 1 H43A H 0.5465(11) 0.5410(5) 0.3447(7) 0.169 Uiso 0.60 calc PR 1 H43B H 0.6656(11) 0.5052(5) 0.3048(7) 0.169 Uiso 0.60 calc PR 1 H43C H 0.7029(11) 0.5866(5) 0.3955(7) 0.169 Uiso 0.60 calc PR 1 C44 C 0.6949(8) 0.3701(9) 0.3929(9) 0.131(6) Uani 0.60 d PDU 1 H44A H 0.6587(8) 0.2956(9) 0.4091(9) 0.196 Uiso 0.60 calc PR 1 H44B H 0.7714(8) 0.4368(9) 0.4347(9) 0.196 Uiso 0.60 calc PR 1 H44C H 0.7339(8) 0.3555(9) 0.3441(9) 0.196 Uiso 0.60 calc PR 1 C42' C 0.5944(6) 0.4064(7) 0.3365(6) 0.078(4) Uiso 0.40 d PD 2 H42B H 0.6191(6) 0.4193(7) 0.2848(6) 0.094 Uiso 0.40 calc PR 2 C43' C 0.5959(16) 0.5232(6) 0.3892(10) 0.097(7) Uiso 0.40 d PD 2 H43D H 0.5218(16) 0.5405(6) 0.3648(10) 0.145 Uiso 0.40 calc PR 2 H43E H 0.6913(16) 0.5911(6) 0.3959(10) 0.145 Uiso 0.40 calc PR 2 H43F H 0.5756(16) 0.5134(6) 0.4410(10) 0.145 Uiso 0.40 calc PR 2 C44' C 0.7090(10) 0.3795(16) 0.3742(15) 0.147(8) Uiso 0.40 d PDU 2 H44D H 0.7080(10) 0.3041(16) 0.3401(15) 0.220 Uiso 0.40 calc PR 2 H44E H 0.6886(10) 0.3697(16) 0.4259(15) 0.220 Uiso 0.40 calc PR 2 H44F H 0.8044(10) 0.4474(16) 0.3810(15) 0.220 Uiso 0.40 calc PR 2 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 0.0322(2) 0.0342(2) 0.0300(2) 0.01128(14) 0.00649(14) 0.01570(15) Zr2 0.0377(2) 0.0352(2) 0.0410(2) 0.0146(2) 0.0121(2) 0.0179(2) N1 0.058(2) 0.049(2) 0.037(2) 0.0115(15) 0.014(2) 0.030(2) C2 0.055(3) 0.064(3) 0.051(2) 0.022(2) 0.026(2) 0.037(2) C3 0.047(2) 0.058(2) 0.049(2) 0.026(2) 0.024(2) 0.028(2) O4 0.0375(13) 0.0404(14) 0.0428(14) 0.0174(11) 0.0175(11) 0.0202(11) C5 0.046(3) 0.070(3) 0.082(3) 0.029(3) 0.033(2) 0.022(2) C7 0.082(3) 0.055(3) 0.056(3) 0.008(2) 0.023(2) 0.038(3) C8 0.075(3) 0.077(3) 0.034(2) 0.014(2) 0.013(2) 0.038(3) N11 0.051(2) 0.050(2) 0.042(2) 0.021(2) 0.015(2) 0.019(2) C12 0.067(3) 0.058(2) 0.033(2) 0.019(2) 0.015(2) 0.030(2) C13 0.056(2) 0.052(2) 0.034(2) 0.013(2) 0.013(2) 0.026(2) O14 0.051(2) 0.0384(13) 0.0300(12) 0.0115(10) 0.0091(11) 0.0212(12) C15 0.097(4) 0.059(3) 0.037(2) 0.005(2) 0.002(2) 0.021(3) C17 0.053(3) 0.085(4) 0.063(3) 0.025(3) 0.025(2) 0.021(3) C18 0.086(4) 0.054(3) 0.055(3) 0.032(2) 0.022(2) 0.026(3) O21 0.0422(15) 0.048(2) 0.0468(15) 0.0176(12) 0.0034(12) 0.0253(13) C22 0.042(4) 0.080(6) 0.057(5) 0.030(4) 0.019(4) 0.041(4) C23 0.041(6) 0.081(9) 0.094(11) 0.005(6) -0.032(6) 0.014(5) C24 0.089(7) 0.081(6) 0.111(9) 0.019(6) -0.022(6) 0.068(6) O25 0.0420(15) 0.0379(14) 0.046(2) 0.0087(12) 0.0011(12) 0.0098(12) C26 0.064(7) 0.053(6) 0.057(7) 0.012(5) 0.009(6) 0.019(5) C27 0.097(15) 0.081(19) 0.072(15) 0.011(12) 0.005(12) 0.004(12) C28 0.059(8) 0.064(9) 0.106(12) 0.012(8) -0.008(7) -0.012(6) C26' 0.054(6) 0.039(6) 0.073(9) 0.010(5) 0.012(6) 0.001(5) C27' 0.100(14) 0.019(8) 0.114(20) 0.018(10) 0.005(12) 0.020(8) C28' 0.088(10) 0.057(8) 0.121(14) 0.012(9) -0.048(9) 0.001(8) O29 0.0345(14) 0.0419(14) 0.0463(15) 0.0137(12) 0.0007(11) 0.0184(12) C30 0.040(2) 0.051(2) 0.047(2) 0.013(2) -0.001(2) 0.022(2) C31 0.046(3) 0.116(5) 0.093(4) 0.049(4) 0.022(3) 0.043(3) C32 0.065(3) 0.085(4) 0.064(3) 0.031(3) -0.009(2) 0.036(3) O33 0.059(2) 0.058(2) 0.057(2) 0.0166(14) 0.0239(14) 0.038(2) C34 0.108(6) 0.082(5) 0.081(5) 0.042(4) 0.058(4) 0.078(5) C35 0.178(11) 0.070(5) 0.142(9) 0.042(6) 0.085(8) 0.078(7) C36 0.132(9) 0.144(8) 0.092(7) 0.060(6) 0.072(7) 0.109(8) O37 0.071(2) 0.063(2) 0.063(2) 0.042(2) 0.031(2) 0.040(2) C38 0.065(5) 0.049(5) 0.045(5) 0.024(4) 0.017(4) 0.028(4) C39 0.089(9) 0.059(6) 0.048(6) 0.044(5) 0.044(6) 0.033(6) C40 0.227(15) 0.108(10) 0.137(10) 0.067(8) 0.073(10) 0.100(10) C38' 0.092(7) 0.062(6) 0.053(5) 0.021(5) 0.004(5) 0.023(5) C39' 0.116(15) 0.155(16) 0.134(15) 0.065(12) 0.029(12) 0.069(12) C40' 0.194(14) 0.096(8) 0.121(9) 0.081(7) 0.072(9) 0.099(9) O41 0.051(2) 0.039(2) 0.084(2) 0.009(2) -0.001(2) 0.0096(14) C42 0.053(5) 0.049(4) 0.069(6) 0.013(4) -0.005(4) 0.005(4) C43 0.119(10) 0.039(5) 0.132(12) 0.024(6) -0.014(9) -0.006(5) C44 0.054(6) 0.110(8) 0.190(13) -0.006(8) -0.046(7) 0.038(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O21 1.953(2) . ? Zr1 O25 1.978(2) . ? Zr1 O14 2.161(2) . ? Zr1 O29 2.189(2) . ? Zr1 O4 2.206(2) . ? Zr1 N1 2.490(3) . ? Zr1 N11 2.540(3) . ? Zr1 Zr2 3.2936(6) . ? Zr2 O41 1.937(3) . ? Zr2 O33 1.946(2) . ? Zr2 O37 1.964(2) . ? Zr2 O4 2.212(2) . ? Zr2 O14 2.214(2) . ? Zr2 O29 2.291(2) . ? N1 C8 1.471(5) . ? N1 C7 1.479(5) . ? N1 C2 1.484(5) . ? C2 C3 1.504(6) . ? C3 O4 1.415(4) . ? C3 C5 1.521(6) . ? N11 C12 1.471(5) . ? N11 C18 1.473(5) . ? N11 C17 1.485(5) . ? C12 C13 1.515(5) . ? C13 O14 1.413(4) . ? C13 C15 1.511(6) . ? O21 C22' 1.402(2) . ? O21 C22 1.403(2) . ? C22 C23 1.500(2) . ? C22 C24 1.501(2) . ? C22' C24' 1.501(2) . ? C22' C23' 1.501(2) . ? O25 C26 1.400(2) . ? O25 C26' 1.400(2) . ? C26 C28 1.499(2) . ? C26 C27 1.500(2) . ? C26' C28' 1.500(2) . ? C26' C27' 1.500(2) . ? O29 C30 1.403(2) . ? C30 C32 1.500(2) . ? C30 C31 1.501(2) . ? O33 C34 1.399(2) . ? O33 C34' 1.400(2) . ? C34 C36 1.499(2) . ? C34 C35 1.500(2) . ? C34' C36' 1.500(2) . ? C34' C35' 1.501(2) . ? O37 C38' 1.403(2) . ? O37 C38 1.403(2) . ? C38 C39 1.501(2) . ? C38 C40 1.502(2) . ? C38' C39' 1.499(2) . ? C38' C40' 1.502(2) . ? O41 C42' 1.401(2) . ? O41 C42 1.402(2) . ? C42 C44 1.499(2) . ? C42 C43 1.500(2) . ? C42' C44' 1.500(2) . ? C42' C43' 1.501(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 O21 Zr1 O25 104.57(10) . . ? O21 Zr1 O14 97.55(10) . . ? O25 Zr1 O14 137.70(10) . . ? O21 Zr1 O29 163.63(9) . . ? O25 Zr1 O29 90.72(9) . . ? O14 Zr1 O29 74.03(9) . . ? O21 Zr1 O4 91.40(10) . . ? O25 Zr1 O4 144.57(10) . . ? O14 Zr1 O4 68.31(9) . . ? O29 Zr1 O4 72.52(9) . . ? O21 Zr1 N1 84.01(11) . . ? O25 Zr1 N1 80.62(11) . . ? O14 Zr1 N1 137.97(10) . . ? O29 Zr1 N1 92.93(10) . . ? O4 Zr1 N1 69.67(10) . . ? O21 Zr1 N11 81.77(11) . . ? O25 Zr1 N11 79.39(11) . . ? O14 Zr1 N11 68.55(10) . . ? O29 Zr1 N11 107.22(10) . . ? O4 Zr1 N11 134.91(10) . . ? N1 Zr1 N11 151.63(11) . . ? O21 Zr1 Zr2 121.05(7) . . ? O25 Zr1 Zr2 134.37(8) . . ? O14 Zr1 Zr2 41.77(6) . . ? O29 Zr1 Zr2 43.89(6) . . ? O4 Zr1 Zr2 41.88(6) . . ? N1 Zr1 Zr2 102.21(8) . . ? N11 Zr1 Zr2 106.16(8) . . ? O41 Zr2 O33 98.85(13) . . ? O41 Zr2 O37 97.85(14) . . ? O33 Zr2 O37 103.56(11) . . ? O41 Zr2 O4 95.67(11) . . ? O33 Zr2 O4 156.82(10) . . ? O37 Zr2 O4 92.18(10) . . ? O41 Zr2 O14 93.81(12) . . ? O33 Zr2 O14 93.71(10) . . ? O37 Zr2 O14 157.34(10) . . ? O4 Zr2 O14 67.28(9) . . ? O41 Zr2 O29 162.38(10) . . ? O33 Zr2 O29 91.35(10) . . ? O37 Zr2 O29 93.65(11) . . ? O4 Zr2 O29 70.48(8) . . ? O14 Zr2 O29 71.09(8) . . ? O41 Zr2 Zr1 120.89(9) . . ? O33 Zr2 Zr1 115.12(8) . . ? O37 Zr2 Zr1 117.28(9) . . ? O4 Zr2 Zr1 41.72(6) . . ? O14 Zr2 Zr1 40.57(6) . . ? O29 Zr2 Zr1 41.49(5) . . ? C8 N1 C7 109.2(3) . . ? C8 N1 C2 110.6(3) . . ? C7 N1 C2 108.5(3) . . ? C8 N1 Zr1 110.3(2) . . ? C7 N1 Zr1 112.5(2) . . ? C2 N1 Zr1 105.8(2) . . ? N1 C2 C3 110.7(3) . . ? O4 C3 C2 107.3(3) . . ? O4 C3 C5 110.5(3) . . ? C2 C3 C5 111.6(3) . . ? C3 O4 Zr1 125.2(2) . . ? C3 O4 Zr2 123.5(2) . . ? Zr1 O4 Zr2 96.40(9) . . ? C12 N11 C18 109.1(3) . . ? C12 N11 C17 109.7(3) . . ? C18 N11 C17 108.6(4) . . ? C12 N11 Zr1 104.8(2) . . ? C18 N11 Zr1 112.3(3) . . ? C17 N11 Zr1 112.2(3) . . ? N11 C12 C13 109.9(3) . . ? O14 C13 C15 111.7(3) . . ? O14 C13 C12 106.6(3) . . ? C15 C13 C12 111.2(4) . . ? C13 O14 Zr1 127.9(2) . . ? C13 O14 Zr2 128.9(2) . . ? Zr1 O14 Zr2 97.66(9) . . ? C22' O21 Zr1 157.7(4) . . ? C22 O21 Zr1 152.2(3) . . ? O21 C22 C23 111.3(2) . . ? O21 C22 C24 111.2(2) . . ? C23 C22 C24 109.9(3) . . ? O21 C22' C24' 111.4(2) . . ? O21 C22' C23' 111.4(2) . . ? C24' C22' C23' 109.6(3) . . ? C26 O25 Zr1 165.9(4) . . ? C26' O25 Zr1 167.7(4) . . ? O25 C26 C28 111.7(2) . . ? O25 C26 C27 111.7(2) . . ? C28 C26 C27 109.7(3) . . ? O25 C26' C28' 111.6(2) . . ? O25 C26' C27' 111.6(2) . . ? C28' C26' C27' 109.7(3) . . ? C30 O29 Zr1 133.5(2) . . ? C30 O29 Zr2 131.7(2) . . ? Zr1 O29 Zr2 94.62(7) . . ? O29 C30 C32 111.8(2) . . ? O29 C30 C31 111.4(2) . . ? C32 C30 C31 109.4(2) . . ? C34 O33 Zr2 168.1(3) . . ? C34' O33 Zr2 157.7(8) . . ? O33 C34 C36 111.5(3) . . ? O33 C34 C35 111.5(3) . . ? C36 C34 C35 109.3(3) . . ? O33 C34' C36' 111.5(3) . . ? O33 C34' C35' 111.4(3) . . ? C36' C34' C35' 109.4(3) . . ? C38' O37 Zr2 143.1(4) . . ? C38 O37 Zr2 167.1(3) . . ? O37 C38 C39 110.8(3) . . ? O37 C38 C40 110.6(3) . . ? C39 C38 C40 109.4(3) . . ? O37 C38' C39' 111.5(3) . . ? O37 C38' C40' 110.5(3) . . ? C39' C38' C40' 109.7(3) . . ? C42' O41 Zr2 155.6(5) . . ? C42 O41 Zr2 170.2(4) . . ? O41 C42 C44 111.4(3) . . ? O41 C42 C43 110.8(3) . . ? C44 C42 C43 110.0(3) . . ? O41 C42' C44' 111.4(3) . . ? O41 C42' C43' 111.0(3) . . ? C44' C42' C43' 109.5(3) . . ? _refine_diff_density_max 0.483 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.064 data_POB9701 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H76 N4 O8 Zr2' _chemical_formula_weight 827.41 _chemical_melting_point ? _chemical_compound_source ? 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.0660(15) _cell_length_b 12.3385(9) _cell_length_c 32.591(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.162(7) _cell_angle_gamma 90.00 _cell_volume 8705.5(12) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 14.88 _cell_measurement_theta_max 37.94 _exptl_crystal_description Rhombs _exptl_crystal_colour Clear _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.90 _exptl_crystal_size_min 0.73 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method ? _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 4.287 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 9.20 _diffrn_reflns_number 7139 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 62.49 _reflns_number_total 6937 _reflns_number_observed 5510 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+28.6676P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00058(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6934 _refine_ls_number_parameters 428 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_obs 0.0537 _refine_ls_wR_factor_all 0.1480 _refine_ls_wR_factor_obs 0.1363 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_restrained_S_all 1.054 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max -0.105 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.26260(2) 0.96784(3) 0.117236(12) 0.0175(2) Uani 1 d . . Zr2 Zr 0.13537(2) 0.97448(3) 0.155710(12) 0.0189(2) Uani 1 d . . N1 N 0.2647(2) 0.7734(4) 0.09575(15) 0.0294(11) Uani 1 d . . C2 C 0.2045(3) 0.7515(5) 0.0689(2) 0.0309(13) Uani 1 d . . H2A H 0.1996(3) 0.6732(5) 0.0644(2) 0.037 Uiso 1 calc R . H2B H 0.2027(3) 0.7861(5) 0.0417(2) 0.037 Uiso 1 calc R . C3 C 0.1526(2) 0.7931(4) 0.0882(2) 0.0239(11) Uani 1 d . . H3A H 0.1494(2) 0.7477(4) 0.1127(2) 0.029 Uiso 1 calc R . O4 O 0.1683(2) 0.9007(3) 0.10200(10) 0.0195(7) Uani 1 d . . C5 C 0.0903(3) 0.7951(5) 0.0586(2) 0.0356(14) Uani 1 d . . H5A H 0.0607(3) 0.8334(5) 0.0722(2) 0.043 Uiso 1 calc R . H5B H 0.0943(3) 0.8361(5) 0.0335(2) 0.043 Uiso 1 calc R . N6 N 0.0661(2) 0.6876(4) 0.0461(2) 0.0374(12) Uani 1 d . . C7 C 0.3137(3) 0.7521(6) 0.0719(2) 0.047(2) Uani 1 d . . H7A H 0.3080(3) 0.7990(6) 0.0475(2) 0.070 Uiso 1 calc R . H7B H 0.3117(3) 0.6770(6) 0.0629(2) 0.070 Uiso 1 calc R . H7C H 0.3536(3) 0.7664(6) 0.0894(2) 0.070 Uiso 1 calc R . C8 C 0.2741(3) 0.7019(5) 0.1323(2) 0.044(2) Uani 1 d . . H8A H 0.3140(3) 0.7170(5) 0.1499(2) 0.065 Uiso 1 calc R . H8B H 0.2728(3) 0.6270(5) 0.1232(2) 0.065 Uiso 1 calc R . H8C H 0.2417(3) 0.7144(5) 0.1481(2) 0.065 Uiso 1 calc R . C9 C 0.0687(4) 0.6627(6) 0.0031(2) 0.062(2) Uani 1 d . . H9A H 0.1107(4) 0.6719(6) -0.0012(2) 0.093 Uiso 1 calc R . H9B H 0.0415(4) 0.7113(6) -0.0154(2) 0.093 Uiso 1 calc R . H9C H 0.0557(4) 0.5884(6) -0.0030(2) 0.093 Uiso 1 calc R . C10 C 0.0037(4) 0.6737(8) 0.0520(3) 0.082(3) Uani 1 d . . H10A H 0.0014(4) 0.6902(8) 0.0807(3) 0.122 Uiso 1 calc R . H10B H -0.0092(4) 0.5994(8) 0.0457(3) 0.122 Uiso 1 calc R . H10C H -0.0234(4) 0.7223(8) 0.0334(3) 0.122 Uiso 1 calc R . N11 N 0.3069(2) 1.1563(4) 0.12554(15) 0.0306(11) Uani 1 d . . C12 C 0.2550(3) 1.2280(4) 0.1084(2) 0.0303(13) Uani 1 d . . H12A H 0.2443(3) 1.2197(4) 0.0780(2) 0.036 Uiso 1 calc R . H12B H 0.2667(3) 1.3037(4) 0.1147(2) 0.036 Uiso 1 calc R . C13 C 0.2000(2) 1.1991(4) 0.1277(2) 0.0263(12) Uani 1 d . . H13A H 0.2075(2) 1.2251(4) 0.1569(2) 0.032 Uiso 1 calc R . O14 O 0.1945(2) 1.0859(3) 0.12740(11) 0.0253(8) Uani 1 d . . C15 C 0.1413(3) 1.2504(4) 0.1037(2) 0.0309(13) Uani 1 d . . H15A H 0.1294(3) 1.2142(4) 0.0766(2) 0.037 Uiso 1 calc R . H15B H 0.1080(3) 1.2393(4) 0.1192(2) 0.037 Uiso 1 calc R . N16 N 0.1481(2) 1.3666(4) 0.0968(2) 0.0335(11) Uani 1 d . . C17 C 0.3307(3) 1.1851(6) 0.1698(2) 0.050(2) Uani 1 d . . H17A H 0.3650(3) 1.1379(6) 0.1812(2) 0.075 Uiso 1 calc R . H17B H 0.2981(3) 1.1765(6) 0.1856(2) 0.075 Uiso 1 calc R . H17C H 0.3446(3) 1.2598(6) 0.1715(2) 0.075 Uiso 1 calc R . C18 C 0.3575(3) 1.1745(6) 0.1025(2) 0.049(2) Uani 1 d . . H18A H 0.3920(3) 1.1274(6) 0.1136(2) 0.074 Uiso 1 calc R . H18B H 0.3708(3) 1.2495(6) 0.1056(2) 0.074 Uiso 1 calc R . H18C H 0.3429(3) 1.1586(6) 0.0730(2) 0.074 Uiso 1 calc R . C19 C 0.1527(4) 1.4303(6) 0.1342(3) 0.059(2) Uani 1 d . . H19A H 0.1879(4) 1.4060(6) 0.1548(3) 0.088 Uiso 1 calc R . H19B H 0.1153(4) 1.4218(6) 0.1454(3) 0.088 Uiso 1 calc R . H19C H 0.1581(4) 1.5060(6) 0.1277(3) 0.088 Uiso 1 calc R . C20 C 0.0950(3) 1.4039(6) 0.0660(2) 0.053(2) Uani 1 d . . H20A H 0.0916(3) 1.3612(6) 0.0407(2) 0.080 Uiso 1 calc R . H20B H 0.1005(3) 1.4796(6) 0.0597(2) 0.080 Uiso 1 calc R . H20C H 0.0577(3) 1.3955(6) 0.0773(2) 0.080 Uiso 1 calc R . O21 O 0.2616(2) 0.9958(3) 0.05819(11) 0.0292(9) Uani 1 d . . C22 C 0.2382(4) 1.0035(6) 0.0150(2) 0.048(2) Uani 1 d . . H22A H 0.2331(4) 0.9285(6) 0.0041(2) 0.058 Uiso 1 calc R . C23 C 0.1762(4) 1.0551(8) 0.0059(2) 0.075(3) Uani 1 d . . H23A H 0.1485(4) 1.0163(8) 0.0204(2) 0.112 Uiso 1 calc R . H23B H 0.1601(4) 1.0529(8) -0.0240(2) 0.112 Uiso 1 calc R . H23C H 0.1796(4) 1.1299(8) 0.0152(2) 0.112 Uiso 1 calc R . C24 C 0.2845(5) 1.0587(8) -0.0064(2) 0.077(3) Uani 1 d . . H24A H 0.3239(5) 1.0217(8) 0.0007(2) 0.115 Uiso 1 calc R . H24B H 0.2894(5) 1.1336(8) 0.0027(2) 0.115 Uiso 1 calc R . H24C H 0.2699(5) 1.0564(8) -0.0365(2) 0.115 Uiso 1 calc R . O25 O 0.3497(2) 0.9368(3) 0.14129(11) 0.0286(9) Uani 1 d . . C26 C 0.4092(3) 0.8933(6) 0.1560(2) 0.0393(15) Uani 1 d . . H26A H 0.4047(3) 0.8142(6) 0.1594(2) 0.047 Uiso 1 calc R . C27 C 0.4503(3) 0.9109(7) 0.1235(3) 0.058(2) Uani 1 d . . H27A H 0.4301(3) 0.8808(7) 0.0968(3) 0.086 Uiso 1 calc R . H27B H 0.4897(3) 0.8752(7) 0.1328(3) 0.086 Uiso 1 calc R . H27C H 0.4569(3) 0.9880(7) 0.1203(3) 0.086 Uiso 1 calc R . C28 C 0.4391(3) 0.9390(7) 0.1977(2) 0.055(2) Uani 1 d . . H28A H 0.4125(3) 0.9270(7) 0.2177(2) 0.082 Uiso 1 calc R . H28B H 0.4457(3) 1.0162(7) 0.1950(2) 0.082 Uiso 1 calc R . H28C H 0.4785(3) 0.9035(7) 0.2074(2) 0.082 Uiso 1 calc R . O29 O 0.2360(2) 0.9229(3) 0.17583(10) 0.0215(8) Uani 1 d . . C30 C 0.2711(3) 0.8885(5) 0.2150(2) 0.0303(13) Uani 1 d . . H30A H 0.3084(3) 0.8507(5) 0.2098(2) 0.036 Uiso 1 calc R . C31 C 0.2914(3) 0.9838(6) 0.2433(2) 0.051(2) Uani 1 d . . H31A H 0.3148(3) 1.0338(6) 0.2294(2) 0.076 Uiso 1 calc R . H31B H 0.3172(3) 0.9585(6) 0.2690(2) 0.076 Uiso 1 calc R . H31C H 0.2554(3) 1.0204(6) 0.2495(2) 0.076 Uiso 1 calc R . C32 C 0.2348(3) 0.8107(6) 0.2364(2) 0.047(2) Uani 1 d . . H32A H 0.2217(3) 0.7495(6) 0.2182(2) 0.071 Uiso 1 calc R . H32B H 0.1987(3) 0.8473(6) 0.2427(2) 0.071 Uiso 1 calc R . H32C H 0.2605(3) 0.7853(6) 0.2622(2) 0.071 Uiso 1 calc R . O33 O 0.1398(2) 1.0629(4) 0.20552(13) 0.0399(10) Uani 1 d . . C34 C 0.1226(4) 1.1211(7) 0.2384(3) 0.071(3) Uani 1 d . . H34A H 0.1601(4) 1.1602(7) 0.2524(3) 0.085 Uiso 1 calc R . C35 C 0.1054(6) 1.0506(11) 0.2698(3) 0.117(5) Uani 1 d . . H35A H 0.1382(6) 0.9987(11) 0.2790(3) 0.175 Uiso 1 calc R . H35B H 0.0677(6) 1.0123(11) 0.2580(3) 0.175 Uiso 1 calc R . H35C H 0.0989(6) 1.0936(11) 0.2935(3) 0.175 Uiso 1 calc R . C36 C 0.0767(6) 1.2068(9) 0.2207(4) 0.115(5) Uani 1 d . . H36A H 0.0928(6) 1.2490(9) 0.2001(4) 0.173 Uiso 1 calc R . H36B H 0.0693(6) 1.2540(9) 0.2431(4) 0.173 Uiso 1 calc R . H36C H 0.0382(6) 1.1727(9) 0.2076(4) 0.173 Uiso 1 calc R . O37 O 0.1033(2) 0.8379(3) 0.17298(13) 0.0347(9) Uani 1 d . . C38 C 0.0721(4) 0.7670(6) 0.1955(3) 0.060(2) Uani 1 d . . H38A H 0.0892(4) 0.7786(6) 0.2256(3) 0.072 Uiso 1 calc R . C39 C 0.0836(5) 0.6534(7) 0.1861(4) 0.101(4) Uani 1 d . . H39A H 0.1278(5) 0.6403(7) 0.1911(4) 0.151 Uiso 1 calc R . H39B H 0.0660(5) 0.6383(7) 0.1571(4) 0.151 Uiso 1 calc R . H39C H 0.0648(5) 0.6065(7) 0.2040(4) 0.151 Uiso 1 calc R . C40 C 0.0056(4) 0.7941(8) 0.1887(4) 0.093(3) Uani 1 d . . H40A H 0.0008(4) 0.8699(8) 0.1953(4) 0.139 Uiso 1 calc R . H40B H -0.0144(4) 0.7493(8) 0.2066(4) 0.139 Uiso 1 calc R . H40C H -0.0132(4) 0.7810(8) 0.1597(4) 0.139 Uiso 1 calc R . O41 O 0.0581(2) 1.0285(3) 0.12285(14) 0.0392(10) Uani 1 d D . C42 C 0.0025(4) 1.0762(10) 0.1016(3) 0.047(3) Uani 0.55 d PDU 1 H42A H 0.0023(4) 1.1552(10) 0.1069(3) 0.057 Uiso 0.55 calc PR 1 C43 C -0.0510(7) 1.0212(15) 0.1158(5) 0.074(4) Uani 0.55 d PDU 1 H43A H -0.0488(7) 1.0349(15) 0.1454(5) 0.112 Uiso 0.55 calc PR 1 H43B H -0.0490(7) 0.9437(15) 0.1111(5) 0.112 Uiso 0.55 calc PR 1 H43C H -0.0895(7) 1.0495(15) 0.1001(5) 0.112 Uiso 0.55 calc PR 1 C44 C -0.0025(9) 1.0526(14) 0.0553(4) 0.061(4) Uani 0.55 d PDU 1 H44A H 0.0314(9) 1.0873(14) 0.0454(4) 0.091 Uiso 0.55 calc PR 1 H44B H -0.0414(9) 1.0805(14) 0.0400(4) 0.091 Uiso 0.55 calc PR 1 H44C H -0.0008(9) 0.9749(14) 0.0511(4) 0.091 Uiso 0.55 calc PR 1 C42' C -0.0024(5) 1.0222(14) 0.1000(4) 0.051(3) Uiso 0.45 d PDU 2 H42B H -0.0151(5) 0.9458(14) 0.0946(4) 0.062 Uiso 0.45 calc PR 2 C43' C -0.0440(9) 1.0786(17) 0.1245(6) 0.072(4) Uiso 0.45 d PDU 2 H43D H -0.0424(9) 1.0413(17) 0.1509(6) 0.107 Uiso 0.45 calc PR 2 H43E H -0.0860(9) 1.0780(17) 0.1087(6) 0.107 Uiso 0.45 calc PR 2 H43F H -0.0303(9) 1.1529(17) 0.1299(6) 0.107 Uiso 0.45 calc PR 2 C44' C -0.0081(12) 1.0838(18) 0.0600(5) 0.069(5) Uiso 0.45 d PDU 2 H44D H 0.0181(12) 1.0508(18) 0.0428(5) 0.104 Uiso 0.45 calc PR 2 H44E H 0.0047(12) 1.1583(18) 0.0660(5) 0.104 Uiso 0.45 calc PR 2 H44F H -0.0507(12) 1.0824(18) 0.0452(5) 0.104 Uiso 0.45 calc PR 2 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 0.0189(3) 0.0198(3) 0.0122(2) -0.0001(2) -0.0012(2) -0.0003(2) Zr2 0.0190(3) 0.0189(3) 0.0174(2) 0.0005(2) 0.0001(2) 0.0001(2) N1 0.027(2) 0.026(2) 0.032(3) -0.008(2) -0.002(2) 0.004(2) C2 0.041(3) 0.023(3) 0.025(3) -0.010(2) -0.003(2) 0.001(2) C3 0.027(3) 0.019(3) 0.021(3) -0.004(2) -0.005(2) -0.004(2) O4 0.026(2) 0.017(2) 0.014(2) -0.0054(14) -0.0011(13) -0.0021(14) C5 0.036(3) 0.023(3) 0.039(3) -0.005(3) -0.016(3) -0.003(2) N6 0.040(3) 0.030(3) 0.036(3) -0.006(2) -0.008(2) -0.010(2) C7 0.040(4) 0.048(4) 0.053(4) -0.018(3) 0.012(3) 0.008(3) C8 0.042(4) 0.028(3) 0.052(4) 0.005(3) -0.013(3) 0.005(3) C9 0.099(7) 0.041(4) 0.041(4) -0.013(3) -0.001(4) -0.005(4) C10 0.072(6) 0.071(6) 0.103(7) -0.030(6) 0.021(5) -0.039(5) N11 0.024(2) 0.031(3) 0.034(3) -0.002(2) -0.001(2) -0.004(2) C12 0.034(3) 0.017(3) 0.037(3) 0.005(2) -0.001(2) -0.005(2) C13 0.030(3) 0.017(3) 0.031(3) 0.000(2) 0.004(2) -0.003(2) O14 0.026(2) 0.021(2) 0.029(2) 0.002(2) 0.005(2) 0.002(2) C15 0.031(3) 0.022(3) 0.038(3) 0.005(2) 0.002(2) 0.004(2) N16 0.037(3) 0.020(2) 0.042(3) 0.009(2) 0.002(2) 0.003(2) C17 0.040(4) 0.045(4) 0.057(4) -0.013(3) -0.011(3) -0.003(3) C18 0.033(4) 0.047(4) 0.070(5) 0.003(4) 0.015(3) -0.011(3) C19 0.074(5) 0.030(4) 0.071(5) -0.012(4) 0.009(4) -0.003(4) C20 0.042(4) 0.050(4) 0.065(5) 0.027(4) 0.005(3) 0.012(3) O21 0.037(2) 0.034(2) 0.016(2) -0.001(2) 0.005(2) -0.004(2) C22 0.083(5) 0.045(4) 0.015(3) 0.005(3) 0.007(3) 0.001(4) C23 0.074(6) 0.101(7) 0.037(4) 0.011(4) -0.021(4) -0.001(5) C24 0.107(8) 0.094(7) 0.039(4) 0.030(5) 0.037(5) 0.019(6) O25 0.027(2) 0.035(2) 0.022(2) 0.006(2) 0.000(2) 0.006(2) C26 0.019(3) 0.052(4) 0.044(4) 0.005(3) -0.002(2) 0.006(3) C27 0.026(3) 0.078(6) 0.072(5) -0.010(4) 0.018(3) 0.002(4) C28 0.027(3) 0.082(6) 0.050(4) 0.013(4) -0.009(3) 0.004(3) O29 0.021(2) 0.028(2) 0.012(2) 0.0054(15) -0.0045(13) 0.003(2) C30 0.024(3) 0.043(3) 0.018(3) 0.012(2) -0.009(2) 0.004(2) C31 0.051(4) 0.063(5) 0.031(3) -0.005(3) -0.012(3) -0.009(4) C32 0.046(4) 0.057(4) 0.037(4) 0.024(3) 0.002(3) 0.003(3) O33 0.039(2) 0.051(3) 0.030(2) -0.014(2) 0.008(2) 0.001(2) C34 0.092(7) 0.069(6) 0.062(5) -0.045(5) 0.041(5) -0.020(5) C35 0.159(12) 0.147(12) 0.065(7) 0.001(7) 0.075(8) 0.018(9) C36 0.152(12) 0.085(8) 0.121(10) -0.011(7) 0.059(9) 0.058(8) O37 0.033(2) 0.034(2) 0.039(2) 0.009(2) 0.009(2) -0.006(2) C38 0.056(5) 0.046(4) 0.085(6) 0.018(4) 0.029(4) -0.013(4) C39 0.092(8) 0.037(5) 0.176(12) 0.022(6) 0.033(8) -0.006(5) C40 0.055(6) 0.085(7) 0.149(10) 0.008(7) 0.046(6) -0.013(5) O41 0.024(2) 0.045(3) 0.044(2) 0.005(2) -0.005(2) 0.008(2) C42 0.038(5) 0.039(5) 0.056(5) -0.002(5) -0.013(4) 0.010(4) C43 0.072(4) 0.075(4) 0.076(4) -0.001(2) 0.013(2) 0.001(2) C44 0.061(4) 0.060(4) 0.060(4) 0.000(2) 0.007(2) 0.003(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 O21 1.951(4) . ? Zr1 O25 1.967(4) . ? Zr1 O14 2.165(4) . ? Zr1 O29 2.176(3) . ? Zr1 O4 2.204(3) . ? Zr1 N1 2.502(4) . ? Zr1 N11 2.516(5) . ? Zr1 Zr2 3.2900(6) . ? Zr2 O33 1.943(4) . ? Zr2 O41 1.946(4) . ? Zr2 O37 1.953(4) . ? Zr2 O14 2.216(4) . ? Zr2 O4 2.217(3) . ? Zr2 O29 2.280(3) . ? N1 C8 1.465(8) . ? N1 C2 1.467(7) . ? N1 C7 1.473(8) . ? C2 C3 1.498(8) . ? C3 O4 1.423(6) . ? C3 C5 1.519(7) . ? C5 N6 1.459(7) . ? N6 C10 1.436(10) . ? N6 C9 1.449(8) . ? N11 C12 1.470(7) . ? N11 C17 1.478(8) . ? N11 C18 1.480(8) . ? C12 C13 1.512(8) . ? C13 O14 1.402(6) . ? C13 C15 1.516(7) . ? C15 N16 1.463(7) . ? N16 C19 1.437(9) . ? N16 C20 1.462(8) . ? O21 C22 1.404(7) . ? C22 C23 1.485(11) . ? C22 C24 1.508(11) . ? O25 C26 1.415(6) . ? C26 C28 1.503(9) . ? C26 C27 1.537(9) . ? O29 C30 1.423(6) . ? C30 C32 1.506(8) . ? C30 C31 1.507(9) . ? O33 C34 1.403(8) . ? C34 C35 1.448(13) . ? C34 C36 1.500(13) . ? O37 C38 1.405(8) . ? C38 C39 1.468(12) . ? C38 C40 1.478(11) . ? O41 C42' 1.400(9) . ? O41 C42 1.415(8) . ? C42 C43 1.511(9) . ? C42 C44 1.519(9) . ? C42' C44' 1.494(10) . ? C42' C43' 1.499(9) . ? 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 O21 Zr1 O25 104.5(2) . . ? O21 Zr1 O14 99.0(2) . . ? O25 Zr1 O14 136.35(15) . . ? O21 Zr1 O29 163.24(15) . . ? O25 Zr1 O29 90.54(14) . . ? O14 Zr1 O29 73.96(13) . . ? O21 Zr1 O4 90.84(14) . . ? O25 Zr1 O4 145.39(15) . . ? O14 Zr1 O4 68.54(13) . . ? O29 Zr1 O4 72.47(12) . . ? O21 Zr1 N1 83.7(2) . . ? O25 Zr1 N1 81.7(2) . . ? O14 Zr1 N1 137.65(14) . . ? O29 Zr1 N1 91.38(15) . . ? O4 Zr1 N1 69.16(14) . . ? O21 Zr1 N11 82.7(2) . . ? O25 Zr1 N11 78.9(2) . . ? O14 Zr1 N11 68.19(14) . . ? O29 Zr1 N11 107.83(15) . . ? O4 Zr1 N11 134.52(14) . . ? N1 Zr1 N11 152.7(2) . . ? O21 Zr1 Zr2 121.62(12) . . ? O25 Zr1 Zr2 133.84(11) . . ? O14 Zr1 Zr2 41.90(10) . . ? O29 Zr1 Zr2 43.66(9) . . ? O4 Zr1 Zr2 42.06(8) . . ? N1 Zr1 Zr2 101.16(11) . . ? N11 Zr1 Zr2 106.16(11) . . ? O33 Zr2 O41 99.5(2) . . ? O33 Zr2 O37 101.9(2) . . ? O41 Zr2 O37 97.3(2) . . ? O33 Zr2 O14 93.5(2) . . ? O41 Zr2 O14 94.7(2) . . ? O37 Zr2 O14 158.6(2) . . ? O33 Zr2 O4 156.8(2) . . ? O41 Zr2 O4 95.3(2) . . ? O37 Zr2 O4 93.8(2) . . ? O14 Zr2 O4 67.44(13) . . ? O33 Zr2 O29 91.6(2) . . ? O41 Zr2 O29 162.5(2) . . ? O37 Zr2 O29 93.65(15) . . ? O14 Zr2 O29 70.98(12) . . ? O4 Zr2 O29 70.28(12) . . ? O33 Zr2 Zr1 115.10(13) . . ? O41 Zr2 Zr1 121.30(13) . . ? O37 Zr2 Zr1 118.19(12) . . ? O14 Zr2 Zr1 40.73(9) . . ? O4 Zr2 Zr1 41.77(9) . . ? O29 Zr2 Zr1 41.19(8) . . ? C8 N1 C2 110.1(5) . . ? C8 N1 C7 108.6(5) . . ? C2 N1 C7 109.0(5) . . ? C8 N1 Zr1 110.9(4) . . ? C2 N1 Zr1 106.3(3) . . ? C7 N1 Zr1 111.9(4) . . ? N1 C2 C3 111.3(4) . . ? O4 C3 C2 107.1(4) . . ? O4 C3 C5 108.7(4) . . ? C2 C3 C5 114.2(5) . . ? C3 O4 Zr1 125.6(3) . . ? C3 O4 Zr2 122.4(3) . . ? Zr1 O4 Zr2 96.17(12) . . ? N6 C5 C3 113.6(5) . . ? C10 N6 C9 108.8(6) . . ? C10 N6 C5 112.4(6) . . ? C9 N6 C5 112.4(5) . . ? C12 N11 C17 109.2(5) . . ? C12 N11 C18 108.9(5) . . ? C17 N11 C18 107.4(5) . . ? C12 N11 Zr1 104.9(3) . . ? C17 N11 Zr1 112.6(4) . . ? C18 N11 Zr1 113.7(4) . . ? N11 C12 C13 109.2(4) . . ? O14 C13 C12 108.0(4) . . ? O14 C13 C15 110.3(4) . . ? C12 C13 C15 111.2(5) . . ? C13 O14 Zr1 127.5(3) . . ? C13 O14 Zr2 132.4(3) . . ? Zr1 O14 Zr2 97.36(14) . . ? N16 C15 C13 112.7(5) . . ? C19 N16 C20 109.0(6) . . ? C19 N16 C15 113.4(5) . . ? C20 N16 C15 108.7(5) . . ? C22 O21 Zr1 158.6(4) . . ? O21 C22 C23 112.1(6) . . ? O21 C22 C24 110.0(6) . . ? C23 C22 C24 113.1(7) . . ? C26 O25 Zr1 168.7(4) . . ? O25 C26 C28 112.4(5) . . ? O25 C26 C27 110.2(5) . . ? C28 C26 C27 110.9(6) . . ? C30 O29 Zr1 132.1(3) . . ? C30 O29 Zr2 132.2(3) . . ? Zr1 O29 Zr2 95.15(12) . . ? O29 C30 C32 111.1(5) . . ? O29 C30 C31 111.2(5) . . ? C32 C30 C31 109.6(5) . . ? C34 O33 Zr2 161.7(5) . . ? O33 C34 C35 112.3(8) . . ? O33 C34 C36 109.2(7) . . ? C35 C34 C36 116.4(9) . . ? C38 O37 Zr2 158.4(5) . . ? O37 C38 C39 111.3(7) . . ? O37 C38 C40 110.6(7) . . ? C39 C38 C40 113.1(8) . . ? C42' O41 Zr2 156.5(8) . . ? C42 O41 Zr2 174.6(6) . . ? O41 C42 C43 108.6(10) . . ? O41 C42 C44 107.2(10) . . ? C43 C42 C44 107.8(11) . . ? O41 C42' C44' 110.2(14) . . ? O41 C42' C43' 108.1(12) . . ? C44' C42' C43' 105.9(13) . . ? _refine_diff_density_max 0.778 _refine_diff_density_min -1.621 _refine_diff_density_rms 0.113 data_POB9706 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H96 N8 O8 Zr2' _chemical_formula_weight 999.69 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.949(2) _cell_length_b 12.276(2) _cell_length_c 23.485(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.494(7) _cell_angle_gamma 90.00 _cell_volume 5619.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.88 _cell_measurement_theta_max 12.55 _exptl_crystal_description 'blocky plates' _exptl_crystal_colour Clear _exptl_crystal_size_max 0.83 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method ? _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.418 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10.22 _diffrn_reflns_number 10156 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9871 _reflns_number_observed 7323 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+1.7315P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00028(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9871 _refine_ls_number_parameters 528 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_obs 0.0454 _refine_ls_wR_factor_all 0.1083 _refine_ls_wR_factor_obs 0.0950 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.074 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.74069(2) 0.85483(3) 0.033668(15) 0.02189(9) Uani 1 d . . Zr2 Zr 0.66023(2) 0.71615(3) -0.09106(2) 0.02514(9) Uani 1 d . . O O 0.66232(14) 0.7347(2) 0.00440(12) 0.0305(6) Uani 1 d D . H H 0.6386(21) 0.7229(46) 0.0289(18) 0.052(15) Uiso 1 d D . N1 N 0.8385(2) 0.7333(3) 0.0903(2) 0.0385(8) Uani 1 d . . C2 C 0.8762(2) 0.7135(4) 0.0492(2) 0.0363(9) Uani 1 d . . H2A H 0.9105(2) 0.6562(4) 0.0663(2) 0.044 Uiso 1 calc R . H2B H 0.9002(2) 0.7801(4) 0.0454(2) 0.044 Uiso 1 calc R . C3 C 0.8262(2) 0.6791(3) -0.0135(2) 0.0299(8) Uani 1 d . . H3A H 0.8128(2) 0.6021(3) -0.0120(2) 0.036 Uiso 1 calc R . O4 O 0.76763(13) 0.7463(2) -0.02838(12) 0.0279(5) Uani 1 d . . C5 C 0.8579(2) 0.6919(4) -0.0623(2) 0.0365(9) Uani 1 d . . H5A H 0.8246(2) 0.6681(4) -0.1019(2) 0.044 Uiso 1 calc R . H5B H 0.8677(2) 0.7691(4) -0.0659(2) 0.044 Uiso 1 calc R . N6 N 0.9212(2) 0.6289(4) -0.0481(2) 0.0463(9) Uani 1 d . . C7 C 0.8861(3) 0.7800(6) 0.1481(2) 0.062(2) Uani 1 d . . H7A H 0.8618(3) 0.7934(6) 0.1755(2) 0.093 Uiso 1 calc R . H7B H 0.9045(3) 0.8481(6) 0.1398(2) 0.093 Uiso 1 calc R . H7C H 0.9234(3) 0.7294(6) 0.1671(2) 0.093 Uiso 1 calc R . C8 C 0.8112(3) 0.6286(5) 0.1030(3) 0.0583(14) Uani 1 d . . H8A H 0.7863(3) 0.6412(5) 0.1300(3) 0.087 Uiso 1 calc R . H8B H 0.8489(3) 0.5788(5) 0.1225(3) 0.087 Uiso 1 calc R . H8C H 0.7805(3) 0.5971(5) 0.0649(3) 0.087 Uiso 1 calc R . C9 C 0.9074(3) 0.5145(5) -0.0630(4) 0.080(2) Uani 1 d . . H9A H 0.8797(3) 0.4856(5) -0.0413(4) 0.120 Uiso 1 calc R . H9B H 0.9503(3) 0.4748(5) -0.0510(4) 0.120 Uiso 1 calc R . H9C H 0.8829(3) 0.5066(5) -0.1067(4) 0.120 Uiso 1 calc R . C10 C 0.9627(3) 0.6732(6) -0.0804(3) 0.074(2) Uani 1 d . . H10A H 0.9717(3) 0.7496(6) -0.0702(3) 0.111 Uiso 1 calc R . H10B H 0.9383(3) 0.6656(6) -0.1241(3) 0.111 Uiso 1 calc R . H10C H 1.0058(3) 0.6339(6) -0.0684(3) 0.111 Uiso 1 calc R . N11 N 0.6618(2) 1.0136(3) 0.02013(14) 0.0277(6) Uani 1 d . . C12 C 0.6577(2) 1.0667(3) -0.0377(2) 0.0291(7) Uani 1 d . . H12A H 0.7014(2) 1.1022(3) -0.0324(2) 0.035 Uiso 1 calc R . H12B H 0.6217(2) 1.1224(3) -0.0492(2) 0.035 Uiso 1 calc R . C13 C 0.6416(2) 0.9809(3) -0.0874(2) 0.0270(7) Uani 1 d . . H13A H 0.5930(2) 0.9587(3) -0.0998(2) 0.032 Uiso 1 calc R . O14 O 0.68427(13) 0.8898(2) -0.06329(11) 0.0256(5) Uani 1 d . . C15 C 0.6550(2) 1.0219(3) -0.1436(2) 0.0349(8) Uani 1 d . . H15A H 0.7039(2) 1.0393(3) -0.1314(2) 0.042 Uiso 1 calc R . H15B H 0.6445(2) 0.9633(3) -0.1740(2) 0.042 Uiso 1 calc R . N16 N 0.6150(2) 1.1176(3) -0.1718(2) 0.0424(9) Uani 1 d . . C17 C 0.5929(2) 0.9769(4) 0.0153(2) 0.0373(9) Uani 1 d . . H17A H 0.5757(2) 0.9242(4) -0.0176(2) 0.056 Uiso 1 calc R . H17B H 0.5621(2) 1.0389(4) 0.0067(2) 0.056 Uiso 1 calc R . H17C H 0.5957(2) 0.9434(4) 0.0535(2) 0.056 Uiso 1 calc R . C18 C 0.6874(2) 1.0939(3) 0.0704(2) 0.0383(9) Uani 1 d . . H18A H 0.7327(2) 1.1185(3) 0.0740(2) 0.057 Uiso 1 calc R . H18B H 0.6899(2) 1.0601(3) 0.1085(2) 0.057 Uiso 1 calc R . H18C H 0.6564(2) 1.1556(3) 0.0617(2) 0.057 Uiso 1 calc R . C19 C 0.5424(3) 1.0901(6) -0.2022(3) 0.076(2) Uani 1 d . . H19A H 0.5254(3) 1.0579(6) -0.1728(3) 0.114 Uiso 1 calc R . H19B H 0.5371(3) 1.0386(6) -0.2349(3) 0.114 Uiso 1 calc R . H19C H 0.5165(3) 1.1557(6) -0.2190(3) 0.114 Uiso 1 calc R . C20 C 0.6412(4) 1.1661(5) -0.2154(3) 0.065(2) Uani 1 d . . H20A H 0.6140(4) 1.2298(5) -0.2338(3) 0.097 Uiso 1 calc R . H20B H 0.6383(4) 1.1135(5) -0.2470(3) 0.097 Uiso 1 calc R . H20C H 0.6886(4) 1.1875(5) -0.1944(3) 0.097 Uiso 1 calc R . N21 N 0.7121(2) 0.8590(4) 0.2651(2) 0.0446(9) Uani 1 d . . C22 C 0.7457(2) 0.8533(4) 0.2208(2) 0.0420(10) Uani 1 d . . H22A H 0.7793(2) 0.7939(4) 0.2322(2) 0.050 Uiso 1 calc R . H22B H 0.7707(2) 0.9214(4) 0.2222(2) 0.050 Uiso 1 calc R . C23 C 0.6952(2) 0.8345(3) 0.1551(2) 0.0317(8) Uani 1 d . . H23A H 0.6587(2) 0.8903(3) 0.1459(2) 0.038 Uiso 1 calc R . O24 O 0.72927(14) 0.8494(2) 0.11423(12) 0.0328(6) Uani 1 d . . C25 C 0.6617(2) 0.7231(4) 0.1495(2) 0.0403(9) Uani 1 d . . H25A H 0.6951(2) 0.6675(4) 0.1490(2) 0.048 Uiso 1 calc R . H25B H 0.6505(2) 0.7105(4) 0.1860(2) 0.048 Uiso 1 calc R . N26 N 0.5991(2) 0.7083(3) 0.0951(2) 0.0418(8) Uani 1 d . . C27 C 0.6765(4) 0.9602(6) 0.2616(3) 0.084(2) Uani 1 d . . H27A H 0.6443(4) 0.9712(6) 0.2202(3) 0.126 Uiso 1 calc R . H27B H 0.7094(4) 1.0195(6) 0.2729(3) 0.126 Uiso 1 calc R . H27C H 0.6519(4) 0.9583(6) 0.2895(3) 0.126 Uiso 1 calc R . C28 C 0.7605(4) 0.8403(8) 0.3263(2) 0.092(3) Uani 1 d . . H28A H 0.7839(4) 0.7717(8) 0.3277(2) 0.138 Uiso 1 calc R . H28B H 0.7363(4) 0.8377(8) 0.3545(2) 0.138 Uiso 1 calc R . H28C H 0.7938(4) 0.8990(8) 0.3379(2) 0.138 Uiso 1 calc R . C29 C 0.5411(3) 0.7628(5) 0.1028(3) 0.0601(14) Uani 1 d . . H29A H 0.5504(3) 0.8402(5) 0.1086(3) 0.090 Uiso 1 calc R . H29B H 0.5340(3) 0.7332(5) 0.1383(3) 0.090 Uiso 1 calc R . H29C H 0.5002(3) 0.7512(5) 0.0667(3) 0.090 Uiso 1 calc R . C30 C 0.5844(3) 0.5920(5) 0.0865(3) 0.064(2) Uani 1 d . . H30A H 0.6228(3) 0.5550(5) 0.0813(3) 0.095 Uiso 1 calc R . H30B H 0.5434(3) 0.5809(5) 0.0504(3) 0.095 Uiso 1 calc R . H30C H 0.5772(3) 0.5629(5) 0.1220(3) 0.095 Uiso 1 calc R . N31 N 0.8791(3) 1.1494(5) 0.1373(2) 0.071(2) Uani 1 d . . C32 C 0.9038(3) 1.0970(5) 0.0944(2) 0.0535(13) Uani 1 d . . H32A H 0.9329(3) 1.0354(5) 0.1149(2) 0.064 Uiso 1 calc R . H32B H 0.9326(3) 1.1488(5) 0.0829(2) 0.064 Uiso 1 calc R . C33 C 0.8487(2) 1.0561(4) 0.0371(2) 0.0441(10) Uani 1 d . . H33A H 0.8159(2) 1.1170(4) 0.0213(2) 0.053 Uiso 1 calc R . O34 O 0.81085(13) 0.9687(2) 0.04710(12) 0.0302(6) Uani 1 d . . C35 C 0.8727(2) 1.0248(4) -0.0138(2) 0.0453(11) Uani 1 d . . H35A H 0.9003(2) 0.9583(4) -0.0017(2) 0.054 Uiso 1 calc R . H35B H 0.8324(2) 1.0073(4) -0.0502(2) 0.054 Uiso 1 calc R . N36 N 0.9130(2) 1.1071(3) -0.0304(2) 0.0431(9) Uani 1 d . . C37 C 0.8653(3) 1.0745(6) 0.1793(3) 0.073(2) Uani 1 d . . H37A H 0.8489(3) 1.1150(6) 0.2067(3) 0.109 Uiso 1 calc R . H37B H 0.9071(3) 1.0362(6) 0.2029(3) 0.109 Uiso 1 calc R . H37C H 0.8306(3) 1.0224(6) 0.1563(3) 0.109 Uiso 1 calc R . C38 C 0.9251(5) 1.2343(9) 0.1713(5) 0.132(5) Uani 1 d . . H38A H 0.9070(5) 1.2677(9) 0.1996(5) 0.197 Uiso 1 calc R . H38B H 0.9295(5) 1.2890(9) 0.1431(5) 0.197 Uiso 1 calc R . H38C H 0.9699(5) 1.2031(9) 0.1939(5) 0.197 Uiso 1 calc R . C39 C 0.9395(3) 1.0577(6) -0.0735(3) 0.0630(15) Uani 1 d . . H39A H 0.9644(3) 0.9918(6) -0.0558(3) 0.095 Uiso 1 calc R . H39B H 0.9701(3) 1.1085(6) -0.0824(3) 0.095 Uiso 1 calc R . H39C H 0.9017(3) 1.0399(6) -0.1111(3) 0.095 Uiso 1 calc R . C40 C 0.8760(4) 1.2047(6) -0.0566(4) 0.080(2) Uani 1 d . . H40A H 0.8583(4) 1.2376(6) -0.0278(4) 0.120 Uiso 1 calc R . H40B H 0.8382(4) 1.1869(6) -0.0941(4) 0.120 Uiso 1 calc R . H40C H 0.9066(4) 1.2554(6) -0.0655(4) 0.120 Uiso 1 calc R . O41 O 0.56077(14) 0.7435(3) -0.12290(14) 0.0404(7) Uani 1 d . . C42 C 0.4900(2) 0.7288(4) -0.1368(2) 0.0373(9) Uani 1 d . . C43 C 0.4792(3) 0.6918(5) -0.0794(2) 0.0553(13) Uani 1 d . . H43A H 0.5023(3) 0.6227(5) -0.0658(2) 0.083 Uiso 1 calc R . H43B H 0.4305(3) 0.6830(5) -0.0881(2) 0.083 Uiso 1 calc R . H43C H 0.4978(3) 0.7458(5) -0.0474(2) 0.083 Uiso 1 calc R . C44 C 0.4629(2) 0.6422(5) -0.1864(2) 0.0524(12) Uani 1 d . . H44A H 0.4864(2) 0.5738(5) -0.1717(2) 0.079 Uiso 1 calc R . H44B H 0.4711(2) 0.6651(5) -0.2227(2) 0.079 Uiso 1 calc R . H44C H 0.4141(2) 0.6326(5) -0.1964(2) 0.079 Uiso 1 calc R . C45 C 0.4542(3) 0.8365(5) -0.1586(3) 0.069(2) Uani 1 d . . H45A H 0.4614(3) 0.8595(5) -0.1953(3) 0.103 Uiso 1 calc R . H45B H 0.4728(3) 0.8910(5) -0.1268(3) 0.103 Uiso 1 calc R . H45C H 0.4054(3) 0.8282(5) -0.1675(3) 0.103 Uiso 1 calc R . O46 O 0.6767(2) 0.7314(3) -0.16724(14) 0.0433(7) Uani 1 d . . C47 C 0.6736(3) 0.7246(5) -0.2280(2) 0.0536(13) Uani 1 d . . C48 C 0.7243(4) 0.8064(6) -0.2362(3) 0.084(2) Uani 1 d . . H48A H 0.7704(4) 0.7881(6) -0.2088(3) 0.126 Uiso 1 calc R . H48B H 0.7128(4) 0.8791(6) -0.2268(3) 0.126 Uiso 1 calc R . H48C H 0.7221(4) 0.8042(6) -0.2781(3) 0.126 Uiso 1 calc R . C49 C 0.6947(4) 0.6110(5) -0.2392(3) 0.073(2) Uani 1 d . . H49A H 0.7412(4) 0.5968(5) -0.2113(3) 0.109 Uiso 1 calc R . H49B H 0.6925(4) 0.6053(5) -0.2810(3) 0.109 Uiso 1 calc R . H49C H 0.6639(4) 0.5581(5) -0.2323(3) 0.109 Uiso 1 calc R . C50 C 0.6018(4) 0.7511(8) -0.2700(3) 0.095(3) Uani 1 d . . H50A H 0.5901(4) 0.8243(8) -0.2615(3) 0.142 Uiso 1 calc R . H50B H 0.5701(4) 0.6995(8) -0.2633(3) 0.142 Uiso 1 calc R . H50C H 0.5987(4) 0.7467(8) -0.3121(3) 0.142 Uiso 1 calc R . O51 O 0.6684(2) 0.5585(2) -0.0814(2) 0.0482(8) Uani 1 d . . C52 C 0.6639(3) 0.4445(4) -0.0778(3) 0.0524(12) Uani 1 d . . C53 C 0.6495(6) 0.4149(7) -0.0214(4) 0.118(3) Uani 1 d U . H53A H 0.6079(6) 0.4509(7) -0.0226(4) 0.177 Uiso 1 calc R . H53B H 0.6876(6) 0.4380(7) 0.0147(4) 0.177 Uiso 1 calc R . H53C H 0.6438(6) 0.3366(7) -0.0201(4) 0.177 Uiso 1 calc R . C54 C 0.7258(4) 0.3942(6) -0.0804(5) 0.104(3) Uani 1 d U . H54A H 0.7320(4) 0.4166(6) -0.1177(5) 0.155 Uiso 1 calc R . H54B H 0.7214(4) 0.3156(6) -0.0801(5) 0.155 Uiso 1 calc R . H54C H 0.7651(4) 0.4170(6) -0.0453(5) 0.155 Uiso 1 calc R . C55 C 0.6021(4) 0.4056(5) -0.1317(4) 0.087(2) Uani 1 d U . H55A H 0.5609(4) 0.4391(5) -0.1300(4) 0.130 Uiso 1 calc R . H55B H 0.5984(4) 0.3271(5) -0.1299(4) 0.130 Uiso 1 calc R . H55C H 0.6074(4) 0.4260(5) -0.1696(4) 0.130 Uiso 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 0.0207(2) 0.0238(2) 0.0208(2) -0.00067(13) 0.00714(12) -0.00285(13) Zr2 0.0236(2) 0.0236(2) 0.0265(2) -0.00464(14) 0.00724(13) -0.00232(13) O 0.0321(13) 0.0329(14) 0.0284(13) -0.0026(11) 0.0135(11) -0.0128(11) N1 0.037(2) 0.047(2) 0.030(2) 0.007(2) 0.0106(14) 0.009(2) C2 0.025(2) 0.046(2) 0.036(2) 0.005(2) 0.009(2) 0.006(2) C3 0.022(2) 0.029(2) 0.040(2) 0.004(2) 0.013(2) 0.0045(14) O4 0.0213(12) 0.0288(12) 0.0327(13) -0.0023(10) 0.0089(10) 0.0020(10) C5 0.032(2) 0.039(2) 0.041(2) -0.002(2) 0.017(2) 0.002(2) N6 0.034(2) 0.052(2) 0.061(2) -0.004(2) 0.026(2) 0.003(2) C7 0.045(3) 0.098(4) 0.028(2) -0.007(3) -0.005(2) 0.023(3) C8 0.066(3) 0.060(3) 0.061(3) 0.035(3) 0.038(3) 0.029(3) C9 0.052(3) 0.059(4) 0.138(7) -0.020(4) 0.046(4) 0.010(3) C10 0.055(3) 0.095(5) 0.093(5) 0.004(4) 0.052(3) 0.003(3) N11 0.028(2) 0.029(2) 0.029(2) -0.0021(13) 0.0129(12) -0.0010(12) C12 0.030(2) 0.026(2) 0.032(2) 0.0001(15) 0.0126(15) 0.0011(14) C13 0.025(2) 0.026(2) 0.028(2) 0.0028(14) 0.0084(14) 0.0008(14) O14 0.0290(12) 0.0219(12) 0.0240(12) 0.0013(9) 0.0077(10) -0.0008(10) C15 0.041(2) 0.036(2) 0.028(2) 0.005(2) 0.013(2) 0.005(2) N16 0.057(2) 0.037(2) 0.037(2) 0.014(2) 0.022(2) 0.012(2) C17 0.027(2) 0.048(2) 0.040(2) 0.008(2) 0.016(2) 0.003(2) C18 0.047(2) 0.034(2) 0.035(2) -0.006(2) 0.018(2) 0.000(2) C19 0.057(3) 0.082(4) 0.073(4) 0.038(4) 0.006(3) 0.027(3) C20 0.096(4) 0.058(3) 0.053(3) 0.027(3) 0.041(3) 0.014(3) N21 0.043(2) 0.063(2) 0.029(2) -0.001(2) 0.014(2) 0.001(2) C22 0.037(2) 0.059(3) 0.027(2) 0.000(2) 0.009(2) -0.006(2) C23 0.033(2) 0.039(2) 0.024(2) 0.001(2) 0.011(2) -0.002(2) O24 0.0405(15) 0.0365(15) 0.0243(12) -0.0012(11) 0.0153(11) -0.0063(12) C25 0.045(2) 0.042(2) 0.036(2) 0.006(2) 0.019(2) -0.004(2) N26 0.042(2) 0.046(2) 0.041(2) -0.003(2) 0.019(2) -0.016(2) C27 0.114(6) 0.085(5) 0.061(4) -0.014(3) 0.042(4) 0.020(4) C28 0.075(4) 0.169(9) 0.031(3) 0.014(4) 0.018(3) 0.007(5) C29 0.043(3) 0.067(3) 0.078(4) 0.009(3) 0.032(3) -0.011(2) C30 0.075(4) 0.056(3) 0.060(3) -0.001(3) 0.026(3) -0.029(3) N31 0.074(3) 0.089(4) 0.063(3) -0.036(3) 0.039(3) -0.046(3) C32 0.044(2) 0.070(3) 0.051(3) -0.021(2) 0.021(2) -0.031(2) C33 0.044(2) 0.050(3) 0.042(2) -0.010(2) 0.020(2) -0.021(2) O34 0.0274(12) 0.0328(14) 0.0308(13) -0.0037(11) 0.0110(11) -0.0085(11) C35 0.044(2) 0.053(3) 0.042(2) -0.005(2) 0.019(2) -0.013(2) N36 0.035(2) 0.052(2) 0.044(2) 0.009(2) 0.016(2) -0.005(2) C37 0.076(4) 0.102(5) 0.045(3) -0.013(3) 0.027(3) -0.021(4) C38 0.132(8) 0.138(9) 0.158(9) -0.099(8) 0.092(8) -0.075(7) C39 0.056(3) 0.084(4) 0.052(3) 0.011(3) 0.025(3) 0.014(3) C40 0.098(5) 0.065(4) 0.092(5) 0.024(4) 0.052(4) 0.018(4) O41 0.0247(14) 0.051(2) 0.042(2) -0.0039(13) 0.0072(12) -0.0043(12) C42 0.023(2) 0.040(2) 0.043(2) 0.001(2) 0.005(2) -0.006(2) C43 0.051(3) 0.069(3) 0.048(3) -0.006(2) 0.021(2) -0.015(3) C44 0.038(2) 0.070(3) 0.040(2) -0.009(2) 0.004(2) -0.013(2) C45 0.037(2) 0.057(3) 0.100(5) 0.019(3) 0.010(3) 0.004(2) O46 0.045(2) 0.056(2) 0.0314(15) -0.0113(14) 0.0178(13) -0.0069(15) C47 0.063(3) 0.072(3) 0.030(2) -0.005(2) 0.021(2) 0.007(3) C48 0.122(6) 0.079(4) 0.087(5) 0.001(4) 0.081(5) 0.002(4) C49 0.099(5) 0.071(4) 0.057(3) -0.024(3) 0.040(3) -0.004(4) C50 0.081(5) 0.155(8) 0.035(3) -0.016(4) 0.006(3) 0.030(5) O51 0.051(2) 0.0227(15) 0.066(2) -0.0046(14) 0.017(2) -0.0047(13) C52 0.056(3) 0.023(2) 0.076(4) -0.006(2) 0.023(3) -0.005(2) C53 0.172(8) 0.077(5) 0.115(6) -0.001(4) 0.064(6) -0.027(5) C54 0.062(4) 0.051(3) 0.192(8) -0.017(4) 0.040(4) 0.007(3) C55 0.073(4) 0.044(3) 0.127(6) -0.018(3) 0.017(4) -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 O34 1.968(3) . ? Zr1 O24 1.993(3) . ? Zr1 O 2.125(3) . ? Zr1 O14 2.190(2) . ? Zr1 O4 2.195(3) . ? Zr1 N1 2.488(4) . ? Zr1 N11 2.499(3) . ? Zr1 Zr2 3.2714(6) . ? Zr2 O51 1.948(3) . ? Zr2 O46 1.951(3) . ? Zr2 O41 1.968(3) . ? Zr2 O4 2.222(3) . ? Zr2 O14 2.232(3) . ? Zr2 O 2.238(3) . ? N1 C2 1.474(5) . ? N1 C7 1.476(6) . ? N1 C8 1.481(7) . ? C2 C3 1.522(5) . ? C3 O4 1.413(4) . ? C3 C5 1.526(5) . ? C5 N6 1.466(5) . ? N6 C10 1.450(6) . ? N6 C9 1.451(7) . ? N11 C17 1.476(5) . ? N11 C18 1.479(5) . ? N11 C12 1.480(5) . ? C12 C13 1.517(5) . ? C13 O14 1.414(4) . ? C13 C15 1.531(5) . ? C15 N16 1.455(5) . ? N16 C20 1.455(6) . ? N16 C19 1.463(7) . ? N21 C27 1.435(8) . ? N21 C28 1.442(7) . ? N21 C22 1.457(5) . ? C22 C23 1.535(5) . ? C23 O24 1.401(4) . ? C23 C25 1.521(6) . ? C25 N26 1.469(6) . ? N26 C29 1.456(7) . ? N26 C30 1.458(6) . ? N31 C32 1.444(7) . ? N31 C38 1.445(8) . ? N31 C37 1.452(8) . ? C32 C33 1.503(6) . ? C33 O34 1.404(5) . ? C33 C35 1.506(6) . ? C35 N36 1.459(6) . ? N36 C40 1.436(7) . ? N36 C39 1.454(7) . ? O41 C42 1.408(5) . ? C42 C45 1.513(7) . ? C42 C43 1.518(6) . ? C42 C44 1.525(6) . ? O46 C47 1.407(5) . ? C47 C50 1.501(8) . ? C47 C49 1.515(8) . ? C47 C48 1.524(9) . ? O51 C52 1.408(5) . ? C52 C54 1.456(8) . ? C52 C53 1.506(10) . ? C52 C55 1.519(8) . ? 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 O34 Zr1 O24 102.37(11) . . ? O34 Zr1 O 171.02(11) . . ? O24 Zr1 O 86.36(11) . . ? O34 Zr1 O14 96.56(10) . . ? O24 Zr1 O14 141.90(11) . . ? O Zr1 O14 74.99(10) . . ? O34 Zr1 O4 100.30(10) . . ? O24 Zr1 O4 139.39(11) . . ? O Zr1 O4 73.76(10) . . ? O14 Zr1 O4 66.47(9) . . ? O34 Zr1 N1 85.42(12) . . ? O24 Zr1 N1 80.47(12) . . ? O Zr1 N1 98.27(12) . . ? O14 Zr1 N1 134.27(11) . . ? O4 Zr1 N1 68.24(11) . . ? O34 Zr1 N11 83.48(11) . . ? O24 Zr1 N11 80.99(11) . . ? O Zr1 N11 95.96(11) . . ? O14 Zr1 N11 68.59(10) . . ? O4 Zr1 N11 135.04(10) . . ? N1 Zr1 N11 155.78(11) . . ? O34 Zr1 Zr2 128.50(8) . . ? O24 Zr1 Zr2 129.10(8) . . ? O Zr1 Zr2 42.75(7) . . ? O14 Zr1 Zr2 42.79(7) . . ? O4 Zr1 Zr2 42.55(7) . . ? N1 Zr1 Zr2 102.67(9) . . ? N11 Zr1 Zr2 101.09(7) . . ? O51 Zr2 O46 99.5(2) . . ? O51 Zr2 O41 104.42(14) . . ? O46 Zr2 O41 98.84(13) . . ? O51 Zr2 O4 93.67(12) . . ? O46 Zr2 O4 96.60(12) . . ? O41 Zr2 O4 153.82(11) . . ? O51 Zr2 O14 156.00(13) . . ? O46 Zr2 O14 94.56(12) . . ? O41 Zr2 O14 92.43(12) . . ? O4 Zr2 O14 65.29(9) . . ? O51 Zr2 O 90.89(13) . . ? O46 Zr2 O 164.51(11) . . ? O41 Zr2 O 89.58(12) . . ? O4 Zr2 O 71.10(10) . . ? O14 Zr2 O 71.98(9) . . ? O51 Zr2 Zr1 114.71(11) . . ? O46 Zr2 Zr1 124.39(10) . . ? O41 Zr2 Zr1 112.21(9) . . ? O4 Zr2 Zr1 41.90(7) . . ? O14 Zr2 Zr1 41.78(6) . . ? O Zr2 Zr1 40.14(6) . . ? Zr1 O Zr2 97.12(10) . . ? C2 N1 C7 108.8(4) . . ? C2 N1 C8 109.2(4) . . ? C7 N1 C8 109.4(4) . . ? C2 N1 Zr1 106.4(2) . . ? C7 N1 Zr1 113.9(3) . . ? C8 N1 Zr1 109.0(3) . . ? N1 C2 C3 109.6(3) . . ? O4 C3 C2 107.7(3) . . ? O4 C3 C5 109.3(3) . . ? C2 C3 C5 111.3(3) . . ? C3 O4 Zr1 127.0(2) . . ? C3 O4 Zr2 130.0(2) . . ? Zr1 O4 Zr2 95.55(10) . . ? N6 C5 C3 112.4(4) . . ? C10 N6 C9 110.0(5) . . ? C10 N6 C5 110.5(4) . . ? C9 N6 C5 111.8(4) . . ? C17 N11 C18 108.9(3) . . ? C17 N11 C12 109.7(3) . . ? C18 N11 C12 108.8(3) . . ? C17 N11 Zr1 110.7(2) . . ? C18 N11 Zr1 112.9(2) . . ? C12 N11 Zr1 105.9(2) . . ? N11 C12 C13 108.8(3) . . ? O14 C13 C12 108.1(3) . . ? O14 C13 C15 108.5(3) . . ? C12 C13 C15 112.1(3) . . ? C13 O14 Zr1 126.4(2) . . ? C13 O14 Zr2 126.6(2) . . ? Zr1 O14 Zr2 95.43(9) . . ? N16 C15 C13 113.6(3) . . ? C20 N16 C15 110.3(4) . . ? C20 N16 C19 110.1(5) . . ? C15 N16 C19 111.1(4) . . ? C27 N21 C28 110.8(5) . . ? C27 N21 C22 112.2(5) . . ? C28 N21 C22 110.9(4) . . ? N21 C22 C23 113.0(3) . . ? O24 C23 C25 113.1(3) . . ? O24 C23 C22 109.4(3) . . ? C25 C23 C22 110.3(3) . . ? C23 O24 Zr1 157.3(2) . . ? N26 C25 C23 115.0(4) . . ? C29 N26 C30 108.9(4) . . ? C29 N26 C25 110.8(4) . . ? C30 N26 C25 108.5(4) . . ? C32 N31 C38 111.6(5) . . ? C32 N31 C37 113.8(6) . . ? C38 N31 C37 109.9(6) . . ? N31 C32 C33 114.8(4) . . ? O34 C33 C32 113.6(4) . . ? O34 C33 C35 108.1(4) . . ? C32 C33 C35 115.1(4) . . ? C33 O34 Zr1 161.8(3) . . ? N36 C35 C33 115.4(4) . . ? C40 N36 C39 109.5(5) . . ? C40 N36 C35 114.8(4) . . ? C39 N36 C35 107.7(4) . . ? C42 O41 Zr2 160.9(3) . . ? O41 C42 C45 108.5(4) . . ? O41 C42 C43 108.6(4) . . ? C45 C42 C43 110.1(5) . . ? O41 C42 C44 109.4(4) . . ? C45 C42 C44 110.6(4) . . ? C43 C42 C44 109.6(4) . . ? C47 O46 Zr2 165.1(3) . . ? O46 C47 C50 108.4(4) . . ? O46 C47 C49 108.8(5) . . ? C50 C47 C49 111.8(6) . . ? O46 C47 C48 108.2(5) . . ? C50 C47 C48 110.6(6) . . ? C49 C47 C48 108.9(5) . . ? C52 O51 Zr2 171.8(3) . . ? O51 C52 C54 109.8(5) . . ? O51 C52 C53 109.4(5) . . ? C54 C52 C53 113.8(7) . . ? O51 C52 C55 108.5(5) . . ? C54 C52 C55 109.4(6) . . ? C53 C52 C55 105.8(6) . . ? _refine_diff_density_max 0.807 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.086 data_POB9708 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H96 N8 O8 Zr2' _chemical_formula_weight 999.69 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5887(14) _cell_length_b 14.147(2) _cell_length_c 17.0623(13) _cell_angle_alpha 86.483(8) _cell_angle_beta 70.620(8) _cell_angle_gamma 85.225(11) _cell_volume 2854.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 4.71 _cell_measurement_theta_max 12.53 _exptl_crystal_description prisms _exptl_crystal_colour Clear _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method ? _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 14.28 _diffrn_reflns_number 10017 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.1056 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9526 _reflns_number_observed 5785 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0535P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9523 _refine_ls_number_parameters 571 _refine_ls_number_restraints 155 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_obs 0.0561 _refine_ls_wR_factor_all 0.1427 _refine_ls_wR_factor_obs 0.1136 _refine_ls_goodness_of_fit_all 1.009 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max 0.034 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.49751(5) 0.21597(4) 0.28567(3) 0.0355(2) Uani 1 d . . Zr2 Zr 0.72916(5) 0.31434(4) 0.17473(4) 0.0402(2) Uani 1 d . . O O 0.5613(4) 0.3527(3) 0.2682(3) 0.0521(11) Uani 1 d D . H H 0.5044(38) 0.3982(34) 0.2808(42) 0.057(20) Uiso 1 d D . N1 N 0.3811(5) 0.2282(4) 0.1925(4) 0.0506(13) Uani 1 d . . C2 C 0.4498(6) 0.1815(5) 0.1160(4) 0.053(2) Uani 1 d . . H2A H 0.4134(6) 0.1937(5) 0.0733(4) 0.064 Uiso 1 calc R . H2B H 0.4557(6) 0.1127(5) 0.1268(4) 0.064 Uiso 1 calc R . C3 C 0.5674(6) 0.2187(5) 0.0846(4) 0.050(2) Uani 1 d . . H3A H 0.5638(6) 0.2824(5) 0.0578(4) 0.060 Uiso 1 calc R . O4 O 0.6017(4) 0.2262(3) 0.1557(2) 0.0444(10) Uani 1 d . . C5 C 0.6529(7) 0.1547(5) 0.0245(4) 0.061(2) Uani 1 d . . H5A H 0.7248(7) 0.1849(5) 0.0043(4) 0.073 Uiso 1 calc R . H5B H 0.6647(7) 0.0952(5) 0.0540(4) 0.073 Uiso 1 calc R . N6 N 0.6207(7) 0.1324(5) -0.0475(4) 0.076(2) Uani 1 d . . C7 C 0.2737(6) 0.1822(6) 0.2295(5) 0.065(2) Uani 1 d . . H7A H 0.2288(6) 0.2135(6) 0.2801(5) 0.097 Uiso 1 calc R . H7B H 0.2892(6) 0.1158(6) 0.2425(5) 0.097 Uiso 1 calc R . H7C H 0.2324(6) 0.1870(6) 0.1903(5) 0.097 Uiso 1 calc R . C8 C 0.3559(7) 0.3295(5) 0.1731(5) 0.066(2) Uani 1 d . . H8A H 0.3105(7) 0.3603(5) 0.2237(5) 0.099 Uiso 1 calc R . H8B H 0.3148(7) 0.3339(5) 0.1338(5) 0.099 Uiso 1 calc R . H8C H 0.4260(7) 0.3605(5) 0.1490(5) 0.099 Uiso 1 calc R . C9 C 0.6314(11) 0.2128(8) -0.1054(6) 0.109(4) Uani 1 d . . H9A H 0.5840(11) 0.2664(8) -0.0774(6) 0.164 Uiso 1 calc R . H9B H 0.6079(11) 0.1967(8) -0.1514(6) 0.164 Uiso 1 calc R . H9C H 0.7094(11) 0.2291(8) -0.1264(6) 0.164 Uiso 1 calc R . C10 C 0.6918(12) 0.0510(8) -0.0891(7) 0.120(4) Uani 1 d . . H10A H 0.6842(12) -0.0026(8) -0.0499(7) 0.179 Uiso 1 calc R . H10B H 0.7700(12) 0.0670(8) -0.1100(7) 0.179 Uiso 1 calc R . H10C H 0.6685(12) 0.0346(8) -0.1350(7) 0.179 Uiso 1 calc R . N11 N 0.5298(5) 0.1813(4) 0.4206(3) 0.0466(12) Uani 1 d . . C12 C 0.6365(6) 0.1205(5) 0.4016(4) 0.050(2) Uani 1 d . . H12A H 0.6237(6) 0.0570(5) 0.3882(4) 0.060 Uiso 1 calc R . H12B H 0.6614(6) 0.1144(5) 0.4504(4) 0.060 Uiso 1 calc R . C13 C 0.7271(6) 0.1634(4) 0.3288(4) 0.0488(15) Uani 1 d . . H13A H 0.7544(6) 0.2187(4) 0.3475(4) 0.059 Uiso 1 calc R . O14 O 0.6776(3) 0.1944(3) 0.2677(2) 0.0421(9) Uani 1 d . . C15 C 0.8246(6) 0.0939(6) 0.2925(5) 0.067(2) Uani 1 d . . H15A H 0.7976(6) 0.0400(6) 0.2728(5) 0.081 Uiso 1 calc R . H15B H 0.8790(6) 0.1242(6) 0.2443(5) 0.081 Uiso 1 calc R . N16 N 0.8828(6) 0.0580(6) 0.3516(5) 0.087(2) Uani 1 d . . C17 C 0.5438(7) 0.2699(5) 0.4576(5) 0.067(2) Uani 1 d . . H17A H 0.6030(7) 0.3044(5) 0.4176(5) 0.101 Uiso 1 calc R . H17B H 0.5641(7) 0.2540(5) 0.5071(5) 0.101 Uiso 1 calc R . H17C H 0.4736(7) 0.3091(5) 0.4721(5) 0.101 Uiso 1 calc R . C18 C 0.4400(6) 0.1296(5) 0.4816(4) 0.056(2) Uani 1 d . . H18A H 0.3694(6) 0.1682(5) 0.4948(4) 0.084 Uiso 1 calc R . H18B H 0.4594(6) 0.1156(5) 0.5317(4) 0.084 Uiso 1 calc R . H18C H 0.4319(6) 0.0707(5) 0.4584(4) 0.084 Uiso 1 calc R . C19 C 0.9551(9) 0.1270(9) 0.3612(9) 0.123(4) Uani 1 d . . H19A H 0.9111(9) 0.1862(9) 0.3787(9) 0.184 Uiso 1 calc R . H19B H 1.0142(9) 0.1376(9) 0.3086(9) 0.184 Uiso 1 calc R . H19C H 0.9887(9) 0.1036(9) 0.4029(9) 0.184 Uiso 1 calc R . C20 C 0.9468(12) -0.0284(9) 0.3261(11) 0.157(6) Uani 1 d . . H20A H 0.8980(12) -0.0747(9) 0.3197(11) 0.236 Uiso 1 calc R . H20B H 0.9805(12) -0.0518(9) 0.3678(11) 0.236 Uiso 1 calc R . H20C H 1.0059(12) -0.0178(9) 0.2735(11) 0.236 Uiso 1 calc R . N21 N 0.0947(6) 0.3524(5) 0.5253(5) 0.079(2) Uani 1 d D . C22 C 0.1629(10) 0.3048(9) 0.4488(9) 0.065(4) Uani 0.55 d PD 1 H22A H 0.1219(10) 0.3121(9) 0.4088(9) 0.078 Uiso 0.55 calc PR 1 H22B H 0.1721(10) 0.2368(9) 0.4619(9) 0.078 Uiso 0.55 calc PR 1 C22' C 0.1916(13) 0.3019(13) 0.4819(10) 0.069(6) Uiso 0.45 d PD 2 H22C H 0.1685(13) 0.2450(13) 0.4636(10) 0.082 Uiso 0.45 calc PR 2 H22D H 0.2297(13) 0.2802(13) 0.5220(10) 0.082 Uiso 0.45 calc PR 2 C23 C 0.2786(6) 0.3422(5) 0.4085(5) 0.057(2) Uani 1 d D . H23A H 0.3062(6) 0.3465(5) 0.4560(5) 0.069 Uiso 0.55 calc PR 1 H23B H 0.2333(6) 0.3600(5) 0.3737(5) 0.069 Uiso 0.45 d PR 2 O24 O 0.3546(4) 0.2778(3) 0.3597(3) 0.0512(11) Uani 1 d . . C25 C 0.2751(11) 0.4414(8) 0.3771(10) 0.073(4) Uani 0.55 d PD 1 H25A H 0.2464(11) 0.4430(8) 0.3302(10) 0.088 Uiso 0.55 calc PR 1 H25B H 0.2199(11) 0.4784(8) 0.4210(10) 0.088 Uiso 0.55 calc PR 1 C25' C 0.3148(18) 0.4374(12) 0.4214(11) 0.079(5) Uiso 0.45 d PD 2 H25C H 0.2466(18) 0.4771(12) 0.4494(11) 0.095 Uiso 0.45 calc PR 2 H25D H 0.3584(18) 0.4274(12) 0.4596(11) 0.095 Uiso 0.45 calc PR 2 N26 N 0.3805(6) 0.4902(4) 0.3497(5) 0.087(2) Uani 1 d D . C27 C 0.1237(16) 0.2946(13) 0.5949(9) 0.100(6) Uani 0.55 d PD 1 H27A H 0.2037(16) 0.2962(13) 0.5863(9) 0.150 Uiso 0.55 calc PR 1 H27B H 0.1053(16) 0.2294(13) 0.5947(9) 0.150 Uiso 0.55 calc PR 1 H27C H 0.0806(16) 0.3214(13) 0.6481(9) 0.150 Uiso 0.55 calc PR 1 C28 C -0.0235(12) 0.3486(19) 0.5397(15) 0.135(8) Uani 0.55 d PDU 1 H28A H -0.0660(12) 0.3806(19) 0.5905(15) 0.203 Uiso 0.55 calc PR 1 H28B H -0.0424(12) 0.2829(19) 0.5451(15) 0.203 Uiso 0.55 calc PR 1 H28C H -0.0424(12) 0.3798(19) 0.4934(15) 0.203 Uiso 0.55 calc PR 1 C29 C 0.4056(19) 0.5277(12) 0.4193(12) 0.122(8) Uani 0.55 d PD 1 H29A H 0.4756(19) 0.5593(12) 0.3985(12) 0.182 Uiso 0.55 calc PR 1 H29B H 0.4130(19) 0.4759(12) 0.4575(12) 0.182 Uiso 0.55 calc PR 1 H29C H 0.3447(19) 0.5727(12) 0.4481(12) 0.182 Uiso 0.55 calc PR 1 C30 C 0.3704(19) 0.5696(11) 0.2916(11) 0.117(7) Uani 0.55 d PDU 1 H30A H 0.3538(19) 0.5454(11) 0.2453(11) 0.175 Uiso 0.55 calc PR 1 H30B H 0.4408(19) 0.6006(11) 0.2711(11) 0.175 Uiso 0.55 calc PR 1 H30C H 0.3099(19) 0.6149(11) 0.3203(11) 0.175 Uiso 0.55 calc PR 1 C27' C 0.0310(20) 0.3220(18) 0.6082(10) 0.105(7) Uiso 0.45 d PD 2 H27D H -0.0348(20) 0.3656(18) 0.6297(10) 0.158 Uiso 0.45 calc PR 2 H27E H 0.0776(20) 0.3211(18) 0.6435(10) 0.158 Uiso 0.45 calc PR 2 H27F H 0.0070(20) 0.2588(18) 0.6074(10) 0.158 Uiso 0.45 calc PR 2 C28' C 0.0124(20) 0.3727(20) 0.4776(16) 0.119(9) Uiso 0.45 d PD 2 H28D H -0.0542(20) 0.4086(20) 0.5117(16) 0.178 Uiso 0.45 calc PR 2 H28E H -0.0090(20) 0.3133(20) 0.4637(16) 0.178 Uiso 0.45 calc PR 2 H28F H 0.0479(20) 0.4093(20) 0.4270(16) 0.178 Uiso 0.45 calc PR 2 C29' C 0.4477(25) 0.5574(20) 0.3720(20) 0.146(14) Uiso 0.45 d PD 2 H29D H 0.4910(25) 0.5919(20) 0.3224(20) 0.220 Uiso 0.45 calc PR 2 H29E H 0.4986(25) 0.5229(20) 0.3973(20) 0.220 Uiso 0.45 calc PR 2 H29F H 0.3978(25) 0.6017(20) 0.4111(20) 0.220 Uiso 0.45 calc PR 2 C30' C 0.3066(22) 0.5463(19) 0.3083(16) 0.114(9) Uiso 0.45 d PD 2 H30D H 0.3530(22) 0.5813(19) 0.2601(16) 0.171 Uiso 0.45 calc PR 2 H30E H 0.2557(22) 0.5905(19) 0.3471(16) 0.171 Uiso 0.45 calc PR 2 H30F H 0.2630(22) 0.5036(19) 0.2908(16) 0.171 Uiso 0.45 calc PR 2 N31 N 0.3138(6) -0.0762(5) 0.3960(4) 0.051(2) Uani 0.75 d PD 1 N31' N 0.2816(17) -0.0593(14) 0.3432(14) 0.063(6) Uiso 0.25 d PD 2 C32 C 0.3903(7) -0.0748(4) 0.3141(4) 0.061(2) Uani 1 d D . H32A H 0.3460(7) -0.0546(4) 0.2776(4) 0.073 Uiso 0.75 calc PR 1 H32B H 0.4180(7) -0.1408(4) 0.3013(4) 0.073 Uiso 0.75 calc PR 1 H32C H 0.4026(7) -0.1120(4) 0.2663(4) 0.073 Uiso 0.25 d PR 2 H32D H 0.4026(7) -0.1191(4) 0.3557(4) 0.073 Uiso 0.25 d PR 2 C33 C 0.4904(6) -0.0181(4) 0.2876(5) 0.062(2) Uani 1 d . . H33A H 0.5241(6) -0.0345(4) 0.3319(5) 0.074 Uiso 1 calc R . O34 O 0.4695(3) 0.0792(3) 0.2936(2) 0.0401(9) Uani 1 d . . C35 C 0.5818(8) -0.0446(5) 0.2137(6) 0.084(3) Uani 1 d . . H35A H 0.6474(8) -0.0114(5) 0.2129(6) 0.101 Uiso 1 calc R . H35B H 0.5604(8) -0.0199(5) 0.1658(6) 0.101 Uiso 1 calc R . N36 N 0.6179(7) -0.1435(5) 0.2008(5) 0.086(2) Uani 1 d . . C37 C 0.2366(6) 0.0086(5) 0.4140(5) 0.068(2) Uani 1 d D . H37A H 0.1861(6) 0.0039(5) 0.4709(5) 0.102 Uiso 0.75 calc PR 1 H37B H 0.1930(6) 0.0139(5) 0.3764(5) 0.102 Uiso 0.75 calc PR 1 H37C H 0.2796(6) 0.0642(5) 0.4066(5) 0.102 Uiso 0.75 calc PR 1 H37D H 0.2736(6) 0.0666(5) 0.3966(5) 0.102 Uiso 0.25 d PR 2 H37E H 0.1564(6) 0.0219(5) 0.4304(5) 0.102 Uiso 0.25 d PR 2 H37F H 0.2563(6) -0.0203(5) 0.4601(5) 0.102 Uiso 0.25 d PR 2 C38 C 0.2459(10) -0.1602(7) 0.4134(7) 0.079(3) Uani 0.75 d PD 1 H38A H 0.1942(10) -0.1591(7) 0.4701(7) 0.118 Uiso 0.75 calc PR 1 H38B H 0.2955(10) -0.2176(7) 0.4063(7) 0.118 Uiso 0.75 calc PR 1 H38C H 0.2032(10) -0.1591(7) 0.3753(7) 0.118 Uiso 0.75 calc PR 1 C38' C 0.2181(23) -0.1467(18) 0.3684(22) 0.082(10) Uiso 0.25 d PD 2 H38D H 0.1378(23) -0.1292(18) 0.3894(22) 0.124 Uiso 0.25 calc PR 2 H38E H 0.2409(23) -0.1819(18) 0.4115(22) 0.124 Uiso 0.25 calc PR 2 H38F H 0.2344(23) -0.1860(18) 0.3206(22) 0.124 Uiso 0.25 calc PR 2 C39 C 0.6642(11) -0.1580(9) 0.1129(7) 0.124(4) Uani 1 d . . H39A H 0.6083(11) -0.1367(9) 0.0868(7) 0.186 Uiso 1 calc R . H39B H 0.6850(11) -0.2249(9) 0.1034(7) 0.186 Uiso 1 calc R . H39C H 0.7306(11) -0.1221(9) 0.0891(7) 0.186 Uiso 1 calc R . C40 C 0.6964(15) -0.1736(10) 0.2424(10) 0.162(7) Uani 1 d . . H40A H 0.6622(15) -0.1627(10) 0.3014(10) 0.244 Uiso 1 calc R . H40B H 0.7631(15) -0.1378(10) 0.2200(10) 0.244 Uiso 1 calc R . H40C H 0.7175(15) -0.2407(10) 0.2343(10) 0.244 Uiso 1 calc R . O41 O 0.8064(4) 0.3773(4) 0.2376(3) 0.0651(13) Uani 1 d D . C42 C 0.8438(7) 0.4473(5) 0.2748(5) 0.076(2) Uani 1 d D . C43 C 0.7402(16) 0.5216(12) 0.3069(16) 0.150(11) Uani 0.55 d PD 1 H43A H 0.6785(16) 0.4912(12) 0.3483(16) 0.225 Uiso 0.55 calc PR 1 H43B H 0.7161(16) 0.5459(12) 0.2606(16) 0.225 Uiso 0.55 calc PR 1 H43C H 0.7620(16) 0.5736(12) 0.3315(16) 0.225 Uiso 0.55 calc PR 1 C44 C 0.9364(15) 0.4948(13) 0.2124(10) 0.098(5) Uani 0.55 d PDU 1 H44A H 0.9114(15) 0.5202(13) 0.1669(10) 0.147 Uiso 0.55 calc PR 1 H44B H 1.0004(15) 0.4494(13) 0.1915(10) 0.147 Uiso 0.55 calc PR 1 H44C H 0.9583(15) 0.5461(13) 0.2378(10) 0.147 Uiso 0.55 calc PR 1 C45 C 0.8725(21) 0.4054(14) 0.3481(11) 0.128(8) Uani 0.55 d PDU 1 H45A H 0.8077(21) 0.3755(14) 0.3863(11) 0.192 Uiso 0.55 calc PR 1 H45B H 0.8932(21) 0.4551(14) 0.3759(11) 0.192 Uiso 0.55 calc PR 1 H45C H 0.9354(21) 0.3584(14) 0.3297(11) 0.192 Uiso 0.55 calc PR 1 C43' C 0.8340(24) 0.5418(12) 0.2346(16) 0.132(10) Uiso 0.45 d PD 2 H43D H 0.8698(24) 0.5378(12) 0.1749(16) 0.198 Uiso 0.45 calc PR 2 H43E H 0.8710(24) 0.5870(12) 0.2555(16) 0.198 Uiso 0.45 calc PR 2 H43F H 0.7550(24) 0.5624(12) 0.2469(16) 0.198 Uiso 0.45 calc PR 2 C44' C 0.9745(13) 0.4191(16) 0.2556(15) 0.108(8) Uiso 0.45 d PD 2 H44D H 1.0126(13) 0.4222(16) 0.1959(15) 0.162 Uiso 0.45 calc PR 2 H44E H 0.9844(13) 0.3551(16) 0.2770(15) 0.162 Uiso 0.45 calc PR 2 H44F H 1.0063(13) 0.4629(16) 0.2819(15) 0.162 Uiso 0.45 calc PR 2 C45' C 0.7937(19) 0.4410(16) 0.3658(9) 0.092(7) Uiso 0.45 d PD 2 H45D H 0.8055(19) 0.3765(16) 0.3855(9) 0.139 Uiso 0.45 calc PR 2 H45E H 0.7134(19) 0.4584(16) 0.3817(9) 0.139 Uiso 0.45 calc PR 2 H45F H 0.8292(19) 0.4838(16) 0.3902(9) 0.139 Uiso 0.45 calc PR 2 O46 O 0.8597(4) 0.2438(3) 0.1014(3) 0.0615(13) Uani 1 d . . C47 C 0.9680(7) 0.2141(5) 0.0485(5) 0.071(2) Uani 1 d . . C48 C 0.9707(10) 0.1113(7) 0.0334(9) 0.125(5) Uani 1 d . . H48A H 0.9141(10) 0.1009(7) 0.0083(9) 0.187 Uiso 1 calc R . H48B H 0.9550(10) 0.0753(7) 0.0859(9) 0.187 Uiso 1 calc R . H48C H 1.0447(10) 0.0906(7) -0.0037(9) 0.187 Uiso 1 calc R . C49 C 0.9883(9) 0.2717(9) -0.0338(6) 0.105(4) Uani 1 d . . H49A H 0.9865(9) 0.3387(9) -0.0237(6) 0.158 Uiso 1 calc R . H49B H 0.9298(9) 0.2612(9) -0.0570(6) 0.158 Uiso 1 calc R . H49C H 1.0614(9) 0.2517(9) -0.0726(6) 0.158 Uiso 1 calc R . C50 C 1.0569(8) 0.2320(8) 0.0881(6) 0.092(3) Uani 1 d . . H50A H 1.0543(8) 0.2992(8) 0.0976(6) 0.138 Uiso 1 calc R . H50B H 1.1312(8) 0.2117(8) 0.0512(6) 0.138 Uiso 1 calc R . H50C H 1.0416(8) 0.1965(8) 0.1407(6) 0.138 Uiso 1 calc R . O51 O 0.7078(4) 0.4135(3) 0.0966(3) 0.0650(13) Uani 1 d . . C52 C 0.7035(8) 0.4892(5) 0.0410(6) 0.078(2) Uani 1 d . . C53 C 0.5994(11) 0.5493(9) 0.0764(9) 0.149(6) Uani 1 d . . H53A H 0.5347(11) 0.5115(9) 0.0880(9) 0.223 Uiso 1 calc R . H53B H 0.5949(11) 0.6006(9) 0.0370(9) 0.223 Uiso 1 calc R . H53C H 0.5998(11) 0.5754(9) 0.1275(9) 0.223 Uiso 1 calc R . C54 C 0.7031(15) 0.4478(8) -0.0394(7) 0.150(7) Uani 1 d . . H54A H 0.7719(15) 0.4081(8) -0.0626(7) 0.225 Uiso 1 calc R . H54B H 0.6986(15) 0.4990(8) -0.0789(7) 0.225 Uiso 1 calc R . H54C H 0.6384(15) 0.4099(8) -0.0278(7) 0.225 Uiso 1 calc R . C55 C 0.8026(12) 0.5453(9) 0.0230(9) 0.152(6) Uani 1 d . . H55A H 0.8708(12) 0.5048(9) -0.0003(9) 0.228 Uiso 1 calc R . H55B H 0.8037(12) 0.5714(9) 0.0739(9) 0.228 Uiso 1 calc R . H55C H 0.7989(12) 0.5966(9) -0.0167(9) 0.228 Uiso 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 0.0361(4) 0.0300(3) 0.0404(3) 0.0034(2) -0.0128(3) -0.0051(2) Zr2 0.0413(4) 0.0353(3) 0.0440(4) 0.0041(2) -0.0131(3) -0.0109(3) O 0.045(3) 0.031(2) 0.067(3) -0.001(2) -0.003(2) -0.002(2) N1 0.047(3) 0.048(3) 0.061(3) 0.014(2) -0.024(3) -0.008(2) C2 0.056(4) 0.056(4) 0.060(4) 0.016(3) -0.035(3) -0.021(3) C3 0.066(5) 0.049(3) 0.042(3) 0.004(3) -0.024(3) -0.018(3) O4 0.050(3) 0.049(2) 0.036(2) -0.001(2) -0.013(2) -0.015(2) C5 0.078(5) 0.062(4) 0.047(4) -0.007(3) -0.024(4) -0.021(4) N6 0.104(6) 0.079(4) 0.056(4) -0.011(3) -0.033(4) -0.030(4) C7 0.054(5) 0.074(5) 0.077(5) 0.027(4) -0.036(4) -0.023(4) C8 0.080(6) 0.052(4) 0.068(5) 0.022(3) -0.031(4) 0.002(4) C9 0.168(12) 0.115(8) 0.062(5) -0.001(5) -0.057(7) -0.028(8) C10 0.189(13) 0.099(7) 0.089(7) -0.038(6) -0.065(8) -0.008(8) N11 0.048(3) 0.052(3) 0.041(3) 0.002(2) -0.016(2) -0.008(2) C12 0.053(4) 0.054(3) 0.050(3) 0.015(3) -0.026(3) -0.009(3) C13 0.049(4) 0.043(3) 0.063(4) 0.008(3) -0.029(3) -0.008(3) O14 0.036(2) 0.042(2) 0.049(2) 0.011(2) -0.016(2) -0.005(2) C15 0.050(4) 0.071(5) 0.070(5) 0.015(4) -0.011(4) 0.009(4) N16 0.063(5) 0.095(5) 0.107(6) 0.037(4) -0.041(4) 0.003(4) C17 0.081(6) 0.071(5) 0.061(4) -0.012(4) -0.033(4) -0.019(4) C18 0.059(4) 0.068(4) 0.041(3) 0.006(3) -0.017(3) -0.012(3) C19 0.079(8) 0.142(10) 0.179(13) 0.021(9) -0.088(8) -0.015(7) C20 0.138(12) 0.126(11) 0.229(18) -0.004(11) -0.106(12) 0.057(9) N21 0.054(4) 0.075(4) 0.089(5) -0.025(4) 0.006(4) -0.003(3) C22 0.036(7) 0.059(8) 0.093(11) -0.019(7) -0.010(8) 0.003(6) C23 0.049(4) 0.053(4) 0.062(4) -0.005(3) -0.007(3) -0.006(3) O24 0.045(3) 0.042(2) 0.058(3) 0.002(2) -0.007(2) 0.000(2) C25 0.069(10) 0.050(7) 0.086(11) 0.002(7) -0.010(8) 0.013(7) N26 0.074(5) 0.047(3) 0.112(6) -0.007(4) 0.006(4) -0.002(3) C27 0.099(15) 0.105(14) 0.078(12) -0.004(10) -0.001(10) -0.026(11) C28 0.071(12) 0.173(17) 0.135(15) 0.002(14) -0.001(11) -0.004(12) C29 0.158(21) 0.051(9) 0.137(19) -0.044(11) -0.017(17) -0.005(11) C30 0.132(15) 0.059(9) 0.120(13) 0.008(9) 0.005(12) 0.007(10) N31 0.053(5) 0.048(4) 0.058(4) 0.014(3) -0.028(4) -0.018(3) C32 0.073(5) 0.041(3) 0.061(4) -0.002(3) -0.009(4) -0.016(3) C33 0.063(5) 0.026(3) 0.092(5) 0.004(3) -0.020(4) -0.008(3) O34 0.042(2) 0.031(2) 0.048(2) 0.004(2) -0.015(2) -0.006(2) C35 0.077(6) 0.053(4) 0.098(6) -0.014(4) 0.007(5) -0.016(4) N36 0.103(6) 0.047(3) 0.086(5) -0.010(3) -0.003(4) 0.004(4) C37 0.044(4) 0.072(5) 0.082(5) 0.003(4) -0.012(4) -0.010(4) C38 0.079(8) 0.077(7) 0.090(8) 0.028(6) -0.037(7) -0.047(6) C39 0.120(10) 0.129(10) 0.097(8) -0.035(7) 0.005(7) -0.010(8) C40 0.213(18) 0.126(11) 0.155(14) 0.003(10) -0.082(13) 0.041(12) O41 0.070(3) 0.067(3) 0.067(3) -0.009(2) -0.027(3) -0.027(3) C42 0.094(7) 0.071(5) 0.076(5) -0.005(4) -0.036(5) -0.043(5) C43 0.138(21) 0.099(15) 0.203(27) -0.095(18) -0.025(20) -0.018(14) C44 0.103(9) 0.108(9) 0.088(8) -0.018(7) -0.025(7) -0.052(7) C45 0.169(17) 0.126(14) 0.123(14) -0.012(11) -0.081(13) -0.050(13) O46 0.047(3) 0.060(3) 0.065(3) -0.011(2) 0.001(2) -0.010(2) C47 0.052(5) 0.060(4) 0.082(5) -0.009(4) 0.003(4) -0.009(3) C48 0.108(9) 0.070(6) 0.175(12) -0.042(7) -0.015(8) 0.007(6) C49 0.071(7) 0.149(10) 0.076(6) 0.007(6) 0.000(5) -0.008(6) C50 0.056(6) 0.117(8) 0.093(7) -0.006(6) -0.008(5) -0.016(5) O51 0.068(3) 0.057(3) 0.071(3) 0.028(2) -0.026(3) -0.021(2) C52 0.097(7) 0.053(4) 0.084(6) 0.033(4) -0.031(5) -0.023(4) C53 0.117(11) 0.127(10) 0.162(13) 0.050(9) -0.014(9) 0.038(8) C54 0.309(21) 0.080(7) 0.102(8) 0.033(6) -0.121(12) -0.043(10) C55 0.167(13) 0.136(10) 0.177(13) 0.102(10) -0.089(11) -0.091(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O34 1.984(4) . ? Zr1 O24 1.991(5) . ? Zr1 O 2.123(4) . ? Zr1 O4 2.173(4) . ? Zr1 O14 2.182(4) . ? Zr1 N11 2.481(5) . ? Zr1 N1 2.485(5) . ? Zr1 Zr2 3.2731(9) . ? Zr2 O51 1.939(4) . ? Zr2 O46 1.943(5) . ? Zr2 O41 1.959(5) . ? Zr2 O4 2.228(4) . ? Zr2 O 2.232(4) . ? Zr2 O14 2.233(4) . ? N1 C2 1.467(9) . ? N1 C7 1.476(8) . ? N1 C8 1.483(8) . ? C2 C3 1.526(9) . ? C3 O4 1.427(7) . ? C3 C5 1.500(10) . ? C5 N6 1.474(9) . ? N6 C9 1.444(12) . ? N6 C10 1.463(13) . ? N11 C18 1.470(8) . ? N11 C12 1.484(8) . ? N11 C17 1.486(8) . ? C12 C13 1.515(9) . ? C13 O14 1.413(7) . ? C13 C15 1.492(10) . ? C15 N16 1.475(10) . ? N16 C20 1.414(14) . ? N16 C19 1.440(13) . ? N21 C22' 1.366(15) . ? N21 C28 1.431(15) . ? N21 C27' 1.43(2) . ? N21 C22 1.471(12) . ? N21 C28' 1.52(2) . ? N21 C27 1.528(15) . ? C22 C23 1.514(12) . ? C22' C23 1.48(2) . ? C23 O24 1.363(8) . ? C23 C25 1.473(12) . ? C23 C25' 1.51(2) . ? C25 N26 1.468(13) . ? C25' N26 1.43(2) . ? N26 C29 1.466(15) . ? N26 C29' 1.47(2) . ? N26 C30 1.477(14) . ? N26 C30' 1.50(2) . ? N31 C32 1.410(10) . ? N31 C37 1.459(10) . ? N31 C38 1.480(10) . ? N31' C32 1.30(2) . ? N31' C38' 1.49(2) . ? N31' C37 1.52(2) . ? C32 C33 1.477(9) . ? C33 O34 1.384(7) . ? C33 C35 1.441(11) . ? C35 N36 1.442(10) . ? N36 C40 1.42(2) . ? N36 C39 1.439(12) . ? O41 C42 1.401(8) . ? C42 C44 1.470(13) . ? C42 C45' 1.469(15) . ? C42 C43' 1.48(2) . ? C42 C45 1.489(15) . ? C42 C43 1.57(2) . ? C42 C44' 1.59(2) . ? O46 C47 1.410(9) . ? C47 C48 1.489(12) . ? C47 C50 1.532(13) . ? C47 C49 1.535(13) . ? O51 C52 1.397(8) . ? C52 C53 1.468(14) . ? C52 C55 1.470(13) . ? C52 C54 1.527(14) . ? 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 O34 Zr1 O24 104.5(2) . . ? O34 Zr1 O 168.8(2) . . ? O24 Zr1 O 86.1(2) . . ? O34 Zr1 O4 99.0(2) . . ? O24 Zr1 O4 137.6(2) . . ? O Zr1 O4 74.5(2) . . ? O34 Zr1 O14 95.8(2) . . ? O24 Zr1 O14 142.1(2) . . ? O Zr1 O14 73.3(2) . . ? O4 Zr1 O14 67.2(2) . . ? O34 Zr1 N11 83.7(2) . . ? O24 Zr1 N11 81.5(2) . . ? O Zr1 N11 94.6(2) . . ? O4 Zr1 N11 136.4(2) . . ? O14 Zr1 N11 69.2(2) . . ? O34 Zr1 N1 84.1(2) . . ? O24 Zr1 N1 79.4(2) . . ? O Zr1 N1 101.6(2) . . ? O4 Zr1 N1 68.5(2) . . ? O14 Zr1 N1 135.1(2) . . ? N11 Zr1 N1 153.9(2) . . ? O34 Zr1 Zr2 126.92(12) . . ? O24 Zr1 Zr2 128.53(13) . . ? O Zr1 Zr2 42.54(12) . . ? O4 Zr1 Zr2 42.60(11) . . ? O14 Zr1 Zr2 42.76(10) . . ? N11 Zr1 Zr2 102.08(12) . . ? N1 Zr1 Zr2 103.70(12) . . ? O51 Zr2 O46 99.2(2) . . ? O51 Zr2 O41 103.0(2) . . ? O46 Zr2 O41 98.2(2) . . ? O51 Zr2 O4 93.1(2) . . ? O46 Zr2 O4 95.6(2) . . ? O41 Zr2 O4 156.8(2) . . ? O51 Zr2 O 92.2(2) . . ? O46 Zr2 O 163.2(2) . . ? O41 Zr2 O 91.2(2) . . ? O4 Zr2 O 71.4(2) . . ? O51 Zr2 O14 155.4(2) . . ? O46 Zr2 O14 94.9(2) . . ? O41 Zr2 O14 94.9(2) . . ? O4 Zr2 O14 65.36(15) . . ? O Zr2 O14 70.32(15) . . ? O51 Zr2 Zr1 114.2(2) . . ? O46 Zr2 Zr1 123.24(14) . . ? O41 Zr2 Zr1 115.77(15) . . ? O4 Zr2 Zr1 41.32(10) . . ? O Zr2 Zr1 40.03(10) . . ? O14 Zr2 Zr1 41.56(10) . . ? Zr1 O Zr2 97.4(2) . . ? C2 N1 C7 110.1(6) . . ? C2 N1 C8 109.5(5) . . ? C7 N1 C8 108.8(6) . . ? C2 N1 Zr1 106.2(4) . . ? C7 N1 Zr1 112.5(4) . . ? C8 N1 Zr1 109.7(4) . . ? N1 C2 C3 110.2(5) . . ? O4 C3 C5 108.7(6) . . ? O4 C3 C2 106.9(5) . . ? C5 C3 C2 113.2(6) . . ? C3 O4 Zr1 127.4(4) . . ? C3 O4 Zr2 130.5(3) . . ? Zr1 O4 Zr2 96.1(2) . . ? N6 C5 C3 114.0(7) . . ? C9 N6 C10 110.0(8) . . ? C9 N6 C5 111.2(6) . . ? C10 N6 C5 109.5(8) . . ? C18 N11 C12 108.2(5) . . ? C18 N11 C17 109.0(5) . . ? C12 N11 C17 108.9(5) . . ? C18 N11 Zr1 113.6(4) . . ? C12 N11 Zr1 105.9(4) . . ? C17 N11 Zr1 111.0(4) . . ? N11 C12 C13 110.2(5) . . ? O14 C13 C15 109.5(6) . . ? O14 C13 C12 107.6(5) . . ? C15 C13 C12 112.1(5) . . ? C13 O14 Zr1 126.6(4) . . ? C13 O14 Zr2 126.5(3) . . ? Zr1 O14 Zr2 95.68(15) . . ? N16 C15 C13 113.6(7) . . ? C20 N16 C19 109.6(9) . . ? C20 N16 C15 111.5(9) . . ? C19 N16 C15 110.9(7) . . ? C22' N21 C27' 120.3(12) . . ? C28 N21 C22 111.6(12) . . ? C22' N21 C28' 113.5(12) . . ? C27' N21 C28' 107.3(14) . . ? C28 N21 C27 108.2(12) . . ? C22 N21 C27 104.6(10) . . ? N21 C22 C23 114.1(9) . . ? N21 C22' C23 123.0(13) . . ? O24 C23 C25 118.6(8) . . ? O24 C23 C22' 115.6(8) . . ? O24 C23 C25' 120.4(10) . . ? C22' C23 C25' 114.6(11) . . ? O24 C23 C22 113.0(7) . . ? C25 C23 C22 113.6(9) . . ? C23 O24 Zr1 162.0(4) . . ? N26 C25 C23 118.2(10) . . ? N26 C25' C23 118.1(13) . . ? C29 N26 C25 112.3(11) . . ? C25' N26 C29' 111.4(13) . . ? C29 N26 C30 108.9(11) . . ? C25 N26 C30 108.7(11) . . ? C25' N26 C30' 111.2(13) . . ? C29' N26 C30' 107.4(15) . . ? C32 N31 C37 112.9(6) . . ? C32 N31 C38 111.5(7) . . ? C37 N31 C38 108.2(8) . . ? C32 N31' C38' 114.5(18) . . ? C32 N31' C37 116.3(14) . . ? C38' N31' C37 107.8(17) . . ? N31' C32 C33 137.4(10) . . ? N31 C32 C33 122.8(7) . . ? O34 C33 C35 112.6(6) . . ? O34 C33 C32 116.2(6) . . ? C35 C33 C32 118.2(6) . . ? C33 O34 Zr1 160.0(4) . . ? C33 C35 N36 119.3(7) . . ? C40 N36 C39 112.0(10) . . ? C40 N36 C35 111.1(10) . . ? C39 N36 C35 108.8(8) . . ? C42 O41 Zr2 161.9(5) . . ? O41 C42 C44 109.9(8) . . ? O41 C42 C45' 111.3(9) . . ? O41 C42 C43' 111.2(11) . . ? C45' C42 C43' 116.4(12) . . ? O41 C42 C45 109.9(9) . . ? C44 C42 C45 114.3(11) . . ? O41 C42 C43 105.6(8) . . ? C44 C42 C43 108.7(11) . . ? C45 C42 C43 108.2(11) . . ? O41 C42 C44' 104.4(10) . . ? C45' C42 C44' 105.5(11) . . ? C43' C42 C44' 107.2(12) . . ? C47 O46 Zr2 165.3(5) . . ? O46 C47 C48 109.0(7) . . ? O46 C47 C50 110.0(7) . . ? C48 C47 C50 110.3(9) . . ? O46 C47 C49 107.1(7) . . ? C48 C47 C49 109.7(9) . . ? C50 C47 C49 110.6(7) . . ? C52 O51 Zr2 173.4(5) . . ? O51 C52 C53 109.4(8) . . ? O51 C52 C55 110.8(8) . . ? C53 C52 C55 110.3(10) . . ? O51 C52 C54 107.6(7) . . ? C53 C52 C54 109.6(11) . . ? C55 C52 C54 109.1(10) . . ? _refine_diff_density_max 0.479 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.076