Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #============================================================================== _audit_creation_date 26-08-98 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; _journal_coden_Cambridge 186 loop_ _publ_author_name 'Rothwell, Ian' 'Fanwick, P.' 'Lee, Jongtaik' 'Thorn, Matt G.' _publ_contact_author_name 'Prof Ian Rothwell' _publ_contact_author_address ; Department of Chemistry Purdue University 1393 Brown Building West Lafayette IN 47907-1393 UNITED STATES OF AMERICA ; _publ_contact_author_email 'fanwick@.xray.chem.purdue.edu' _publ_contact_author_fax '1(765)4940239' _publ_contact_author_phone '1(765)4944572' _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_section_title ; Synthesis, Structure and Molecular Dynamics of 2-Imnoacyl Compounds [Cp(ArO)Zr( 2-ButNCCH2Ph)] and [Cp(ArO)Zr( 2-ButNCCH2Ph)2] ; _publ_section_references ; P. T. Beurskens, G. Admirall, G. Beurskens, W. P. Bosman S. Garcia-Granda, R. O. Gould, J. M. M. Smits, '& C. Smykalla (1992). The DIRDIF92 Program System, 'Technical Report. Crystallography Laboratory, Univ. of Nijmegen, The Netherlands. Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Hall S.R. & du Boulay, D. (1995) Editors U. of Western Aurtralia Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1996). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of Gottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; data_MT50G _database_code_CSD 182088 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C49 H62 N2 O1 Zr1' _chemical_formula_structural ? _chemical_formula_weight 786.27 _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 12.1678(4) _cell_length_b 12.3408(4) _cell_length_c 15.8545(3) _cell_angle_alpha 82.1531(18) _cell_angle_beta 88.5042(17) _cell_angle_gamma 63.8531(12) _cell_volume 2115.53(15) _cell_measurement_reflns_used 22831 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.23 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.290 _cell_measurement_temperature 203 _exptl_crystal_F_000 836 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.7584 _exptl_absorpt_correction_T_max 0.9368 _diffrn_reflns_number 22831 _reflns_number_total 10661 _reflns_number_gt 7934 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 30.54 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 21 # 7. REFINEMENT DATA _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_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.101 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 10661 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.4862P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.44 _refine_diff_density_min -0.72 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.99E-02 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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_calc_flag Zr 0.204432(18) 0.115537(19) 0.185367(12) 0.02667(8) Uani ? O(10) 0.18396(13) -0.04231(13) 0.21101(9) 0.0303(5) Uani ? N(5) 0.26064(16) 0.08564(16) 0.32355(11) 0.0297(6) Uani ? N(7) 0.10166(16) 0.31340(16) 0.20593(11) 0.0297(6) Uani ? C(1) 0.1603(2) 0.1272(3) 0.02338(15) 0.0533(11) Uani ? C(2) 0.1698(3) 0.2327(3) 0.03218(15) 0.0585(11) Uani ? C(3) 0.2900(3) 0.2003(3) 0.05965(16) 0.0526(11) Uani ? C(4) 0.3545(2) 0.0736(2) 0.06681(15) 0.0411(9) Uani ? C(5) 0.2747(2) 0.0286(2) 0.04371(14) 0.0419(9) Uani ? C(6) 0.3508(2) 0.0865(2) 0.28120(14) 0.0324(7) Uani ? C(8) 0.0212(2) 0.2759(2) 0.19572(14) 0.0319(7) Uani ? C(11) 0.19373(19) -0.13738(19) 0.26878(13) 0.0281(7) Uani ? C(12) 0.31125(19) -0.2256(2) 0.30135(14) 0.0304(7) Uani ? C(13) 0.3221(2) -0.3150(2) 0.36893(14) 0.0329(7) Uani ? C(14) 0.2205(2) -0.3245(2) 0.40507(14) 0.0312(7) Uani ? C(15) 0.10733(19) -0.2450(2) 0.36627(14) 0.0311(7) Uani ? C(16) 0.08955(19) -0.15316(19) 0.29832(14) 0.0291(7) Uani ? C(51) 0.2405(2) 0.0752(2) 0.41762(14) 0.0350(8) Uani ? C(52) 0.2479(3) 0.1810(2) 0.45260(16) 0.0469(10) Uani ? C(53) 0.1127(2) 0.0828(3) 0.42756(16) 0.0464(10) Uani ? C(54) 0.3339(2) -0.0469(2) 0.46412(16) 0.0453(9) Uani ? C(60) 0.4766(2) 0.0648(2) 0.31312(17) 0.0426(9) Uani ? C(61) 0.5157(2) 0.1579(2) 0.26887(16) 0.0393(8) Uani ? C(62) 0.5116(2) 0.2504(3) 0.3103(2) 0.0523(10) Uani ? C(63) 0.5379(3) 0.3419(3) 0.2693(3) 0.0783(16) Uani ? C(64) 0.5699(3) 0.3397(5) 0.1855(4) 0.098(2) Uani ? C(65) 0.5788(3) 0.2462(5) 0.1442(3) 0.095(2) Uani ? C(66) 0.5530(2) 0.1538(3) 0.18600(19) 0.0607(14) Uani ? C(71) 0.0882(2) 0.4378(2) 0.21516(15) 0.0359(8) Uani ? C(72) 0.2170(2) 0.4231(2) 0.23259(18) 0.0471(10) Uani ? C(73) 0.0332(3) 0.5238(2) 0.13222(17) 0.0476(10) Uani ? C(74) 0.0097(3) 0.4873(2) 0.29012(17) 0.0487(10) Uani ? C(80) -0.1180(2) 0.3497(2) 0.19083(16) 0.0385(8) Uani ? C(81) -0.1725(2) 0.3598(2) 0.10338(16) 0.0368(8) Uani ? C(82) -0.1476(2) 0.2582(2) 0.06431(17) 0.0415(8) Uani ? C(83) -0.2032(2) 0.2687(3) -0.01375(18) 0.0497(10) Uani ? C(84) -0.2859(3) 0.3819(3) -0.0529(2) 0.0584(12) Uani ? C(85) -0.3116(3) 0.4829(3) -0.0147(2) 0.0594(12) Uani ? C(86) -0.2548(2) 0.4730(2) 0.06244(19) 0.0471(9) Uani ? C(121) 0.4267(2) -0.2294(2) 0.26390(15) 0.0343(7) Uani ? C(122) 0.4422(2) -0.2258(2) 0.17685(17) 0.0442(9) Uani ? C(123) 0.5509(3) -0.2347(3) 0.1414(2) 0.0561(11) Uani ? C(124) 0.6478(2) -0.2504(3) 0.1936(2) 0.0595(10) Uani ? C(125) 0.6359(2) -0.2577(3) 0.2798(2) 0.0540(10) Uani ? C(126) 0.5260(2) -0.2469(2) 0.31528(18) 0.0446(9) Uani ? C(141) 0.2363(2) -0.4187(2) 0.48326(15) 0.0372(8) Uani ? C(142) 0.2753(4) -0.3817(3) 0.56053(19) 0.0673(13) Uani ? C(143) 0.3330(3) -0.5448(2) 0.4674(2) 0.0578(11) Uani ? C(144) 0.1183(3) -0.4314(3) 0.50256(19) 0.0543(11) Uani ? C(161) -0.0399(2) -0.0744(2) 0.25750(14) 0.0317(7) Uani ? C(162) -0.0358(2) -0.0744(2) 0.16069(15) 0.0417(9) Uani ? C(163) -0.0908(2) 0.0559(2) 0.27889(16) 0.0381(8) Uani ? C(164) -0.1317(2) -0.1242(2) 0.28894(18) 0.0455(9) Uani ? H(1) 0.0899 0.1227 0.0068 0.0690 Uiso calc H(2) 0.1071 0.3116 0.0217 0.0760 Uiso calc H(3) 0.3212 0.2535 0.0711 0.0680 Uiso calc H(4) 0.4365 0.0274 0.0840 0.0530 Uiso calc H(5) 0.2941 -0.0529 0.0421 0.0540 Uiso calc H(13) 0.3999 -0.3703 0.3907 0.0430 Uiso calc H(15) 0.0388 -0.2534 0.3868 0.0400 Uiso calc H(62) 0.4907 0.2513 0.3671 0.0680 Uiso calc H(63) 0.5339 0.4043 0.2980 0.1020 Uiso calc H(64) 0.5857 0.4021 0.1569 0.1270 Uiso calc H(65) 0.6021 0.2443 0.0879 0.1230 Uiso calc H(66) 0.5610 0.0893 0.1581 0.0790 Uiso calc H(82) -0.0927 0.1817 0.0908 0.0540 Uiso calc H(83) -0.1848 0.1997 -0.0395 0.0650 Uiso calc H(84) -0.3238 0.3894 -0.1050 0.0760 Uiso calc H(85) -0.3678 0.5591 -0.0408 0.0770 Uiso calc H(86) -0.2718 0.5427 0.0870 0.0610 Uiso calc H(122) 0.3784 -0.2171 0.1414 0.0570 Uiso calc H(123) 0.5586 -0.2302 0.0827 0.0730 Uiso calc H(124) 0.7206 -0.2560 0.1700 0.0770 Uiso calc H(125) 0.7015 -0.2699 0.3150 0.0700 Uiso calc H(126) 0.5189 -0.2514 0.3741 0.0580 Uiso calc H(14A) 0.2888 -0.4426 0.6089 0.0880 Uiso calc H(14B) 0.2121 -0.3049 0.5723 0.0880 Uiso calc H(14C) 0.3497 -0.3741 0.5493 0.0880 Uiso calc H(14D) 0.3098 -0.5661 0.4170 0.0750 Uiso calc H(14E) 0.3390 -0.6041 0.5153 0.0750 Uiso calc H(14F) 0.4109 -0.5433 0.4600 0.0750 Uiso calc H(14G) 0.0927 -0.4545 0.4540 0.0710 Uiso calc H(14H) 0.0553 -0.3549 0.5149 0.0710 Uiso calc H(14I) 0.1329 -0.4927 0.5509 0.0710 Uiso calc H(16A) -0.1163 -0.0248 0.1353 0.0540 Uiso calc H(16B) -0.0077 -0.1564 0.1485 0.0540 Uiso calc H(16C) 0.0193 -0.0423 0.1377 0.0540 Uiso calc H(16D) -0.0997 0.0548 0.3393 0.0500 Uiso calc H(16E) -0.1693 0.1046 0.2502 0.0500 Uiso calc H(16F) -0.0355 0.0901 0.2606 0.0500 Uiso calc H(16G) -0.1428 -0.1196 0.3487 0.0590 Uiso calc H(16H) -0.1007 -0.2076 0.2794 0.0590 Uiso calc H(16I) -0.2088 -0.0766 0.2583 0.0590 Uiso calc H(52A) 0.3290 0.1750 0.4459 0.0610 Uiso calc H(52B) 0.2299 0.1778 0.5119 0.0610 Uiso calc H(52C) 0.1896 0.2566 0.4220 0.0610 Uiso calc H(53A) 0.0538 0.1584 0.3971 0.0600 Uiso calc H(53B) 0.0943 0.0789 0.4868 0.0600 Uiso calc H(53C) 0.1092 0.0160 0.4050 0.0600 Uiso calc H(54A) 0.3296 -0.1123 0.4400 0.0590 Uiso calc H(54B) 0.3160 -0.0531 0.5234 0.0590 Uiso calc H(54C) 0.4148 -0.0522 0.4582 0.0590 Uiso calc H(60A) 0.4752 0.0680 0.3740 0.0550 Uiso calc H(60B) 0.5363 -0.0160 0.3037 0.0550 Uiso calc H(72A) 0.2504 0.3693 0.2848 0.0610 Uiso calc H(72B) 0.2136 0.5012 0.2373 0.0610 Uiso calc H(72C) 0.2680 0.3894 0.1866 0.0610 Uiso calc H(73A) 0.0849 0.4920 0.0861 0.0620 Uiso calc H(73B) 0.0272 0.6028 0.1375 0.0620 Uiso calc H(73C) -0.0469 0.5307 0.1210 0.0620 Uiso calc H(74A) -0.0746 0.5106 0.2757 0.0630 Uiso calc H(74B) 0.0184 0.5570 0.3029 0.0630 Uiso calc H(74C) 0.0360 0.4254 0.3390 0.0630 Uiso calc H(80A) -0.1534 0.3111 0.2332 0.0500 Uiso calc H(80B) -0.1391 0.4308 0.2041 0.0500 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr 0.02654(12) 0.02886(12) 0.02230(12) -0.01096(8) 0.00002(7) -0.00047(8) O(10) 0.0305(8) 0.0287(8) 0.0303(8) -0.0127(6) 0.0002(6) -0.0003(6) N(5) 0.0341(10) 0.0294(9) 0.0232(9) -0.0131(8) -0.0021(7) 0.0011(7) N(7) 0.0328(9) 0.0273(9) 0.0247(9) -0.0103(8) -0.0001(7) 0.0002(7) C(1) 0.0426(15) 0.086(2) 0.0244(12) -0.0210(15) -0.0019(10) -0.0113(13) C(2) 0.072(2) 0.0491(16) 0.0212(12) 0.0007(14) 0.0062(12) 0.0040(11) C(3) 0.081(2) 0.0505(16) 0.0342(14) -0.0372(15) 0.0206(14) -0.0058(12) C(4) 0.0379(13) 0.0519(15) 0.0333(12) -0.0191(12) 0.0087(10) -0.0091(11) C(5) 0.0533(15) 0.0456(14) 0.0282(12) -0.0222(12) 0.0073(10) -0.0096(10) C(6) 0.0318(11) 0.0325(11) 0.0324(12) -0.0149(9) -0.0052(9) 0.0010(9) C(8) 0.0323(11) 0.0315(11) 0.0286(11) -0.0118(9) 0.0026(9) -0.0015(9) C(11) 0.0303(11) 0.0278(10) 0.0268(10) -0.0129(9) 0.0020(8) -0.0054(8) C(12) 0.0248(10) 0.0314(11) 0.0346(12) -0.0119(9) 0.0007(8) -0.0047(9) C(13) 0.0267(11) 0.0297(11) 0.0385(12) -0.0099(9) -0.0017(9) -0.0010(9) C(14) 0.0315(11) 0.0304(11) 0.0317(11) -0.0138(9) 0.0011(9) -0.0037(9) C(15) 0.0270(10) 0.0331(11) 0.0330(12) -0.0137(9) 0.0020(9) -0.0028(9) C(16) 0.0269(10) 0.0290(11) 0.0317(11) -0.0120(9) 0.0002(8) -0.0066(9) C(51) 0.0432(13) 0.0387(12) 0.0230(11) -0.0192(10) -0.0036(9) 0.0007(9) C(52) 0.0636(17) 0.0475(15) 0.0333(13) -0.0273(13) -0.0005(12) -0.0068(11) C(53) 0.0504(15) 0.0648(18) 0.0292(12) -0.0301(14) 0.0055(11) -0.0074(12) C(54) 0.0578(16) 0.0434(14) 0.0302(12) -0.0208(12) -0.0052(11) 0.0056(11) C(60) 0.0360(13) 0.0474(14) 0.0424(14) -0.0189(11) -0.0092(10) 0.0041(11) C(61) 0.0232(11) 0.0495(14) 0.0411(13) -0.0145(10) -0.0025(9) 0.0024(11) C(62) 0.0385(14) 0.0520(16) 0.0669(19) -0.0222(13) -0.0032(13) -0.0014(14) C(63) 0.0447(17) 0.060(2) 0.131(4) -0.0310(16) -0.021(2) 0.017(2) C(64) 0.0431(18) 0.113(4) 0.129(4) -0.049(2) -0.031(2) 0.069(3) C(65) 0.0431(18) 0.169(5) 0.063(2) -0.054(3) -0.0068(16) 0.040(3) C(66) 0.0332(14) 0.099(3) 0.0483(16) -0.0296(15) 0.0019(12) -0.0036(16) C(71) 0.0417(13) 0.0277(11) 0.0350(12) -0.0134(10) -0.0049(10) 0.0002(9) C(72) 0.0490(15) 0.0427(14) 0.0526(16) -0.0241(12) -0.0104(12) -0.0005(12) C(73) 0.0536(16) 0.0387(14) 0.0467(15) -0.0210(12) -0.0103(12) 0.0109(12) C(74) 0.0561(16) 0.0367(14) 0.0473(15) -0.0134(12) -0.0008(12) -0.0112(12) C(80) 0.0298(11) 0.0332(12) 0.0466(14) -0.0091(10) 0.0040(10) -0.0041(10) C(81) 0.0271(11) 0.0326(12) 0.0474(14) -0.0117(9) 0.0021(10) 0.0001(10) C(82) 0.0311(12) 0.0396(13) 0.0506(15) -0.0140(10) 0.0020(10) -0.0015(11) C(83) 0.0433(14) 0.0580(17) 0.0554(17) -0.0295(13) 0.0054(12) -0.0077(13) C(84) 0.0534(17) 0.075(2) 0.0530(17) -0.0388(16) -0.0100(14) 0.0110(16) C(85) 0.0484(16) 0.0533(18) 0.067(2) -0.0210(14) -0.0143(14) 0.0202(15) C(86) 0.0376(13) 0.0349(13) 0.0627(18) -0.0138(11) -0.0026(12) 0.0063(12) C(121) 0.0292(11) 0.0276(11) 0.0430(13) -0.0106(9) 0.0033(9) -0.0023(9) C(122) 0.0362(13) 0.0383(13) 0.0488(15) -0.0088(11) 0.0075(11) -0.0044(11) C(123) 0.0458(16) 0.0463(16) 0.0596(18) -0.0081(13) 0.0218(14) -0.0014(13) C(124) 0.0345(14) 0.0427(15) 0.093(2) -0.0119(12) 0.0252(15) -0.0056(15) C(125) 0.0304(13) 0.0480(16) 0.084(2) -0.0174(12) 0.0075(13) -0.0115(15) C(126) 0.0322(12) 0.0419(14) 0.0565(16) -0.0138(11) 0.0034(11) -0.0056(12) C(141) 0.0342(12) 0.0408(13) 0.0346(12) -0.0167(10) 0.0004(9) 0.0019(10) C(142) 0.094(2) 0.085(2) 0.0385(16) -0.055(2) -0.0063(16) -0.0016(16) C(143) 0.0566(17) 0.0405(15) 0.0620(19) -0.0140(13) 0.0040(14) 0.0120(13) C(144) 0.0470(15) 0.0603(18) 0.0528(17) -0.0276(14) 0.0015(13) 0.0151(14) C(161) 0.0291(11) 0.0324(11) 0.0339(12) -0.0141(9) -0.0019(9) -0.0032(9) C(162) 0.0400(13) 0.0461(14) 0.0363(13) -0.0159(11) -0.0082(10) -0.0061(11) C(163) 0.0297(11) 0.0384(13) 0.0419(13) -0.0109(10) 0.0009(10) -0.0059(10) C(164) 0.0328(12) 0.0456(14) 0.0572(16) -0.0194(11) -0.0071(11) 0.0047(12) # 10. MOLECULAR GEOMETRY _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_publ_flag Zr O(10) 2.0562(15) ? Zr N(5) 2.2447(17) ? Zr C(6) 2.245(2) ? Zr C(8) 2.257(2) ? Zr N(7) 2.2666(18) ? Zr C(4) 2.528(2) ? Zr C(3) 2.536(2) ? Zr C(5) 2.584(2) ? Zr C(2) 2.593(2) ? Zr C(1) 2.609(2) ? O(10) C(11) 1.349(2) ? N(5) C(6) 1.275(3) ? N(5) C(51) 1.502(3) ? N(7) C(8) 1.275(3) ? N(7) C(71) 1.498(3) ? C(1) C(2) 1.383(4) ? C(1) C(5) 1.394(4) ? C(2) C(3) 1.400(4) ? C(3) C(4) 1.396(4) ? C(4) C(5) 1.392(4) ? C(6) C(60) 1.521(3) ? C(8) C(80) 1.527(3) ? C(11) C(12) 1.418(3) ? C(11) C(16) 1.423(3) ? C(12) C(13) 1.392(3) ? C(12) C(121) 1.495(3) ? C(13) C(14) 1.393(3) ? C(14) C(15) 1.388(3) ? C(14) C(141) 1.532(3) ? C(15) C(16) 1.398(3) ? C(16) C(161) 1.542(3) ? C(51) C(53) 1.522(3) ? C(51) C(52) 1.525(4) ? C(51) C(54) 1.529(3) ? C(60) C(61) 1.511(3) ? C(61) C(62) 1.374(4) ? C(61) C(66) 1.379(4) ? C(62) C(63) 1.380(4) ? C(63) C(64) 1.375(6) ? C(64) C(65) 1.367(7) ? C(65) C(66) 1.391(5) ? C(71) C(72) 1.524(3) ? C(71) C(74) 1.524(4) ? C(71) C(73) 1.531(3) ? C(80) C(81) 1.518(4) ? C(81) C(82) 1.383(4) ? C(81) C(86) 1.389(3) ? C(82) C(83) 1.389(4) ? C(83) C(84) 1.381(4) ? C(84) C(85) 1.368(5) ? C(85) C(86) 1.385(4) ? C(121) C(122) 1.385(3) ? C(121) C(126) 1.394(3) ? C(122) C(123) 1.387(4) ? C(123) C(124) 1.385(5) ? C(124) C(125) 1.366(4) ? C(125) C(126) 1.396(3) ? C(141) C(142) 1.520(4) ? C(141) C(144) 1.530(3) ? C(141) C(143) 1.533(4) ? C(161) C(163) 1.531(3) ? C(161) C(162) 1.535(3) ? C(161) C(164) 1.539(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(10) Zr N(5) 86.50(6) ? O(10) Zr C(6) 102.94(7) ? N(5) Zr C(6) 32.99(7) ? O(10) Zr C(8) 108.79(7) ? N(5) Zr C(8) 95.41(7) ? C(6) Zr C(8) 115.77(8) ? O(10) Zr N(7) 138.19(6) ? N(5) Zr N(7) 83.84(6) ? C(6) Zr N(7) 90.40(8) ? C(8) Zr N(7) 32.75(7) ? O(10) Zr C(4) 103.56(7) ? N(5) Zr C(4) 123.36(8) ? C(6) Zr C(4) 91.45(8) ? C(8) Zr C(4) 130.49(8) ? N(7) Zr C(4) 115.68(8) ? O(10) Zr C(3) 132.21(8) ? N(5) Zr C(3) 127.39(9) ? C(6) Zr C(3) 96.34(10) ? C(8) Zr C(3) 101.00(9) ? N(7) Zr C(3) 83.98(8) ? C(4) Zr C(3) 32.00(9) ? O(10) Zr C(5) 80.13(7) ? N(5) Zr C(5) 142.50(7) ? C(6) Zr C(5) 117.38(8) ? C(8) Zr C(5) 122.05(8) ? N(7) Zr C(5) 128.26(7) ? C(4) Zr C(5) 31.58(8) ? C(3) Zr C(5) 52.27(9) ? O(10) Zr C(2) 121.15(9) ? N(5) Zr C(2) 152.24(10) ? C(6) Zr C(2) 126.57(10) ? C(8) Zr C(2) 78.86(8) ? N(7) Zr C(2) 76.76(8) ? C(4) Zr C(2) 52.26(9) ? C(3) Zr C(2) 31.65(10) ? C(5) Zr C(2) 51.52(9) ? O(10) Zr C(1) 90.45(9) ? N(5) Zr C(1) 173.59(8) ? C(6) Zr C(1) 143.32(9) ? C(8) Zr C(1) 90.91(9) ? N(7) Zr C(1) 102.13(9) ? C(4) Zr C(1) 52.01(8) ? C(3) Zr C(1) 51.93(10) ? C(5) Zr C(1) 31.15(8) ? C(2) Zr C(1) 30.83(10) ? C(11) O(10) Zr 147.60(14) ? C(6) N(5) C(51) 131.70(19) ? C(6) N(5) Zr 73.52(13) ? C(51) N(5) Zr 154.64(14) ? C(8) N(7) C(71) 130.82(19) ? C(8) N(7) Zr 73.22(13) ? C(71) N(7) Zr 155.53(15) ? C(2) C(1) C(5) 108.2(3) ? C(2) C(1) Zr 73.94(14) ? C(5) C(1) Zr 73.42(14) ? C(1) C(2) C(3) 108.2(2) ? C(1) C(2) Zr 75.23(14) ? C(3) C(2) Zr 71.93(14) ? C(4) C(3) C(2) 107.6(3) ? C(4) C(3) Zr 73.65(14) ? C(2) C(3) Zr 76.42(15) ? C(5) C(4) C(3) 108.0(2) ? C(5) C(4) Zr 76.44(14) ? C(3) C(4) Zr 74.35(14) ? C(4) C(5) C(1) 108.0(3) ? C(4) C(5) Zr 71.98(14) ? C(1) C(5) Zr 75.43(15) ? N(5) C(6) C(60) 129.3(2) ? N(5) C(6) Zr 73.50(13) ? C(60) C(6) Zr 157.02(17) ? N(7) C(8) C(80) 127.9(2) ? N(7) C(8) Zr 74.03(13) ? C(80) C(8) Zr 157.73(18) ? O(10) C(11) C(12) 119.48(18) ? O(10) C(11) C(16) 122.23(18) ? C(12) C(11) C(16) 118.28(18) ? C(13) C(12) C(11) 120.08(19) ? C(13) C(12) C(121) 117.62(18) ? C(11) C(12) C(121) 122.27(19) ? C(12) C(13) C(14) 122.3(2) ? C(15) C(14) C(13) 116.34(19) ? C(15) C(14) C(141) 123.13(19) ? C(13) C(14) C(141) 120.53(19) ? C(14) C(15) C(16) 124.3(2) ? C(15) C(16) C(11) 117.92(19) ? C(15) C(16) C(161) 119.63(18) ? C(11) C(16) C(161) 122.45(18) ? N(5) C(51) C(53) 106.18(18) ? N(5) C(51) C(52) 109.01(18) ? C(53) C(51) C(52) 110.4(2) ? N(5) C(51) C(54) 111.28(19) ? C(53) C(51) C(54) 109.1(2) ? C(52) C(51) C(54) 110.8(2) ? C(61) C(60) C(6) 112.17(19) ? C(62) C(61) C(66) 118.8(3) ? C(62) C(61) C(60) 120.2(2) ? C(66) C(61) C(60) 121.0(3) ? C(61) C(62) C(63) 121.4(3) ? C(64) C(63) C(62) 119.2(4) ? C(65) C(64) C(63) 120.2(3) ? C(64) C(65) C(66) 120.3(4) ? C(61) C(66) C(65) 120.0(4) ? N(7) C(71) C(72) 106.20(18) ? N(7) C(71) C(74) 111.35(19) ? C(72) C(71) C(74) 108.7(2) ? N(7) C(71) C(73) 109.5(2) ? C(72) C(71) C(73) 110.2(2) ? C(74) C(71) C(73) 110.8(2) ? C(81) C(80) C(8) 112.1(2) ? C(82) C(81) C(86) 118.2(2) ? C(82) C(81) C(80) 121.9(2) ? C(86) C(81) C(80) 119.8(2) ? C(81) C(82) C(83) 121.1(2) ? C(84) C(83) C(82) 119.8(3) ? C(85) C(84) C(83) 119.6(3) ? C(84) C(85) C(86) 120.7(3) ? C(85) C(86) C(81) 120.5(3) ? C(122) C(121) C(126) 117.6(2) ? C(122) C(121) C(12) 120.7(2) ? C(126) C(121) C(12) 121.5(2) ? C(121) C(122) C(123) 121.5(3) ? C(124) C(123) C(122) 119.9(3) ? C(125) C(124) C(123) 119.7(2) ? C(124) C(125) C(126) 120.3(3) ? C(121) C(126) C(125) 120.9(3) ? C(142) C(141) C(144) 108.8(2) ? C(142) C(141) C(143) 109.8(2) ? C(144) C(141) C(143) 106.3(2) ? C(142) C(141) C(14) 109.5(2) ? C(144) C(141) C(14) 112.27(19) ? C(143) C(141) C(14) 110.0(2) ? C(163) C(161) C(162) 110.67(19) ? C(163) C(161) C(164) 106.99(19) ? C(162) C(161) C(164) 106.2(2) ? C(163) C(161) C(16) 110.81(18) ? C(162) C(161) C(16) 109.61(18) ? C(164) C(161) C(16) 112.44(18) ? #============================================================================== #============================================================================== data_JTLEE2 _database_code_CSD 182089 _audit_creation_date 24-06-99 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C53 H64 N2 O Zr' _chemical_formula_structural ? _chemical_formula_weight 836.33 _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 11.9950(7) _cell_length_b 13.3697(9) _cell_length_c 14.9039(5) _cell_angle_alpha 99.974(3) _cell_angle_beta 99.813(3) _cell_angle_gamma 97.689(2) _cell_volume 2286.5(4) _cell_measurement_reflns_used 21157 _cell_measurement_theta_min 4 _cell_measurement_theta_max 24 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.272 _cell_measurement_temperature 193 _exptl_crystal_F_000 888 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6141 _exptl_absorpt_correction_T_max 0.9600 _diffrn_reflns_number 21157 _reflns_number_total 7929 _reflns_number_gt 6018 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.081 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 24.96 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 17 # 7. REFINEMENT DATA _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_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.109 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7929 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.2567P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.48 _refine_diff_density_min -0.44 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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_calc_flag Zr 0.07404(3) 0.28112(3) 0.277558(19) 0.02574(10) Uani ? O(50) -0.03774(17) 0.14547(17) 0.22595(13) 0.0275(7) Uani ? N(10) 0.1368(2) 0.2563(2) 0.14253(16) 0.0277(8) Uani ? N(30) 0.0785(2) 0.4499(2) 0.26323(17) 0.0333(9) Uani ? C(1) 0.2093(3) 0.3400(3) 0.4338(2) 0.0431(13) Uani ? C(2) 0.1113(4) 0.3801(3) 0.4477(2) 0.0517(14) Uani ? C(3) 0.0209(3) 0.2976(4) 0.4396(2) 0.0487(13) Uani ? C(4) 0.0674(3) 0.2069(3) 0.4236(2) 0.0380(10) Uani ? C(5) 0.1808(3) 0.2334(3) 0.4186(2) 0.0389(13) Uani ? C(11) 0.1266(3) 0.2355(3) 0.0387(2) 0.0334(10) Uani ? C(12) 0.1957(3) 0.1559(3) 0.0050(2) 0.0482(14) Uani ? C(13) 0.1644(4) 0.3380(3) 0.0118(2) 0.0523(15) Uani ? C(14) 0.0002(3) 0.1975(3) -0.0027(2) 0.0474(13) Uani ? C(20) 0.2238(3) 0.2751(3) 0.2086(2) 0.0324(10) Uani ? C(21) 0.3487(3) 0.2756(4) 0.2016(2) 0.0539(15) Uani ? C(22) 0.4306(3) 0.3128(3) 0.2938(2) 0.0404(13) Uani ? C(23) 0.4489(4) 0.2473(4) 0.3543(3) 0.0577(16) Uani ? C(24) 0.5270(4) 0.2869(6) 0.4424(3) 0.084(2) Uani ? C(25) 0.5802(4) 0.3910(5) 0.4588(3) 0.076(2) Uani ? C(26) 0.5605(4) 0.4510(5) 0.3987(4) 0.085(2) Uani ? C(27) 0.4875(3) 0.4130(4) 0.3176(3) 0.0623(17) Uani ? C(31) 0.1318(3) 0.5597(3) 0.2680(2) 0.0378(11) Uani ? C(32) 0.1270(3) 0.6261(3) 0.3614(2) 0.0488(11) Uani ? C(33) 0.2571(3) 0.5569(3) 0.2610(3) 0.0487(13) Uani ? C(34) 0.0724(3) 0.6034(3) 0.1879(3) 0.0530(15) Uani ? C(40) -0.0257(3) 0.4093(3) 0.2559(2) 0.0338(10) Uani ? C(41) -0.1294(3) 0.4627(3) 0.2546(2) 0.0397(11) Uani ? C(42) -0.2113(3) 0.4384(3) 0.1612(2) 0.0379(11) Uani ? C(43) -0.3265(3) 0.4448(3) 0.1587(3) 0.0547(15) Uani ? C(44) -0.4028(4) 0.4233(4) 0.0742(4) 0.069(2) Uani ? C(45) -0.3668(4) 0.3958(4) -0.0068(3) 0.0713(18) Uani ? C(46) -0.2531(4) 0.3883(4) -0.0054(3) 0.0634(16) Uani ? C(47) -0.1755(3) 0.4107(3) 0.0791(3) 0.0474(13) Uani ? C(51) -0.0998(3) 0.0581(2) 0.23647(19) 0.0246(9) Uani ? C(52) -0.0439(3) -0.0220(3) 0.26244(19) 0.0254(9) Uani ? C(53) -0.1072(3) -0.1119(3) 0.27691(19) 0.0275(10) Uani ? C(54) -0.2253(3) -0.1266(3) 0.2659(2) 0.0277(10) Uani ? C(55) -0.2792(3) -0.0474(3) 0.23777(19) 0.0279(10) Uani ? C(56) -0.2228(3) 0.0419(3) 0.2204(2) 0.0276(10) Uani ? C(521) 0.0832(3) -0.0183(2) 0.2689(2) 0.0265(10) Uani ? C(522) 0.1313(3) -0.0031(3) 0.1942(2) 0.0334(10) Uani ? C(523) 0.2464(3) -0.0146(3) 0.1913(2) 0.0433(13) Uani ? C(524) 0.3129(3) -0.0399(3) 0.2649(2) 0.0430(13) Uani ? C(525) 0.2703(3) -0.0510(3) 0.3456(2) 0.0339(10) Uani ? C(526) 0.3416(3) -0.0699(3) 0.4254(2) 0.0438(13) Uani ? C(527) 0.3020(3) -0.0772(3) 0.5042(2) 0.0433(13) Uani ? C(528) 0.1879(3) -0.0667(3) 0.5083(2) 0.0387(11) Uani ? C(529) 0.1152(3) -0.0505(3) 0.4326(2) 0.0296(10) Uani ? C(52A) 0.1541(3) -0.0411(3) 0.3491(2) 0.0273(10) Uani ? C(541) -0.2964(3) -0.2216(3) 0.2847(2) 0.0334(10) Uani ? C(542) -0.2220(3) -0.2971(3) 0.3171(3) 0.0454(11) Uani ? C(543) -0.3643(3) -0.1893(3) 0.3606(3) 0.0531(16) Uani ? C(544) -0.3810(3) -0.2770(3) 0.1955(3) 0.0569(15) Uani ? C(561) -0.2924(3) 0.1222(3) 0.1883(2) 0.0331(10) Uani ? C(562) -0.2698(3) 0.2186(3) 0.2659(3) 0.0445(11) Uani ? C(563) -0.4220(3) 0.0822(3) 0.1658(3) 0.0511(15) Uani ? C(564) -0.2602(3) 0.1498(3) 0.0997(2) 0.0461(13) Uani ? H(1) 0.2807 0.3775 0.4345 0.0560 Uiso calc H(2) 0.1060 0.4497 0.4603 0.0670 Uiso calc H(3) -0.0547 0.3025 0.4440 0.0630 Uiso calc H(4) 0.0284 0.1403 0.4174 0.0500 Uiso calc H(5) 0.2305 0.1872 0.4069 0.0510 Uiso calc H(23) 0.4119 0.1791 0.3390 0.0750 Uiso calc H(24) 0.5415 0.2459 0.4860 0.1090 Uiso calc H(25) 0.6315 0.4183 0.5147 0.0990 Uiso calc H(26) 0.5970 0.5193 0.4124 0.1100 Uiso calc H(27) 0.4748 0.4561 0.2755 0.0810 Uiso calc H(43) -0.3523 0.4633 0.2137 0.0710 Uiso calc H(44) -0.4797 0.4279 0.0728 0.0890 Uiso calc H(45) -0.4188 0.3821 -0.0631 0.0930 Uiso calc H(46) -0.2283 0.3683 -0.0606 0.0820 Uiso calc H(47) -0.0985 0.4068 0.0800 0.0610 Uiso calc H(53) -0.0683 -0.1633 0.2945 0.0360 Uiso calc H(55) -0.3587 -0.0557 0.2303 0.0360 Uiso calc H(12A) 0.2761 0.1834 0.0248 0.0630 Uiso calc H(12B) 0.1770 0.1378 -0.0617 0.0630 Uiso calc H(12C) 0.1782 0.0956 0.0302 0.0630 Uiso calc H(13A) 0.1195 0.3875 0.0345 0.0680 Uiso calc H(13B) 0.1533 0.3285 -0.0547 0.0680 Uiso calc H(13C) 0.2441 0.3625 0.0385 0.0680 Uiso calc H(14A) -0.0235 0.1328 0.0139 0.0620 Uiso calc H(14B) -0.0119 0.1886 -0.0691 0.0620 Uiso calc H(14C) -0.0441 0.2471 0.0210 0.0620 Uiso calc H(21A) 0.3584 0.2064 0.1755 0.0700 Uiso calc H(21B) 0.3681 0.3196 0.1592 0.0700 Uiso calc H(32A) 0.0484 0.6255 0.3670 0.0630 Uiso calc H(32B) 0.1633 0.6955 0.3648 0.0630 Uiso calc H(32C) 0.1663 0.5988 0.4110 0.0630 Uiso calc H(33A) 0.2928 0.5258 0.3093 0.0630 Uiso calc H(33B) 0.2969 0.6258 0.2677 0.0630 Uiso calc H(33C) 0.2603 0.5173 0.2015 0.0630 Uiso calc H(34A) 0.0732 0.5595 0.1299 0.0690 Uiso calc H(34B) 0.1121 0.6712 0.1898 0.0690 Uiso calc H(34C) -0.0056 0.6068 0.1937 0.0690 Uiso calc H(41A) -0.1034 0.5365 0.2719 0.0520 Uiso calc H(41B) -0.1706 0.4426 0.3010 0.0520 Uiso calc H(522) 0.0871 0.0154 0.1440 0.0440 Uiso calc H(523) 0.2765 -0.0049 0.1393 0.0560 Uiso calc H(524) 0.3875 -0.0500 0.2617 0.0560 Uiso calc H(526) 0.4171 -0.0775 0.4234 0.0570 Uiso calc H(527) 0.3503 -0.0891 0.5557 0.0560 Uiso calc H(528) 0.1614 -0.0707 0.5629 0.0510 Uiso calc H(529) 0.0393 -0.0457 0.4359 0.0380 Uiso calc H(54A) -0.1790 -0.3187 0.2707 0.0590 Uiso calc H(54B) -0.2700 -0.3560 0.3271 0.0590 Uiso calc H(54C) -0.1700 -0.2642 0.3742 0.0590 Uiso calc H(54D) -0.3121 -0.1519 0.4160 0.0690 Uiso calc H(54E) -0.4063 -0.2496 0.3737 0.0690 Uiso calc H(54F) -0.4169 -0.1462 0.3393 0.0690 Uiso calc H(54G) -0.4278 -0.2300 0.1734 0.0740 Uiso calc H(54H) -0.4290 -0.3342 0.2082 0.0740 Uiso calc H(54I) -0.3393 -0.3016 0.1490 0.0740 Uiso calc H(56A) -0.2880 0.1996 0.3216 0.0580 Uiso calc H(56B) -0.3169 0.2670 0.2473 0.0580 Uiso calc H(56C) -0.1904 0.2495 0.2773 0.0580 Uiso calc H(56D) -0.4468 0.0685 0.2210 0.0660 Uiso calc H(56E) -0.4386 0.0200 0.1193 0.0660 Uiso calc H(56F) -0.4619 0.1332 0.1429 0.0660 Uiso calc H(56G) -0.3084 0.1959 0.0776 0.0590 Uiso calc H(56H) -0.2706 0.0882 0.0531 0.0590 Uiso calc H(56I) -0.1814 0.1827 0.1128 0.0590 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr 0.02556(18) 0.0284(2) 0.02365(17) 0.00573(13) 0.00516(12) 0.00511(12) O(50) 0.0266(11) 0.0266(14) 0.0304(11) 0.0048(10) 0.0065(9) 0.0077(9) N(10) 0.0316(15) 0.0255(16) 0.0257(13) 0.0044(12) 0.0061(12) 0.0042(11) N(30) 0.0421(18) 0.0298(18) 0.0277(14) 0.0094(14) 0.0050(12) 0.0041(12) C(1) 0.044(2) 0.053(3) 0.0250(17) -0.007(2) -0.0008(15) 0.0074(17) C(2) 0.096(3) 0.037(3) 0.0206(17) 0.021(2) 0.0053(19) 0.0005(16) C(3) 0.046(2) 0.079(3) 0.0261(18) 0.021(2) 0.0150(16) 0.0084(19) C(4) 0.050(2) 0.039(2) 0.0244(17) 0.0033(19) 0.0075(15) 0.0080(15) C(5) 0.044(2) 0.046(3) 0.0279(18) 0.0120(19) 0.0025(15) 0.0116(16) C(11) 0.044(2) 0.036(2) 0.0199(15) 0.0057(17) 0.0067(14) 0.0052(14) C(12) 0.065(3) 0.054(3) 0.0299(18) 0.021(2) 0.0158(18) 0.0053(17) C(13) 0.071(3) 0.052(3) 0.035(2) 0.003(2) 0.0117(18) 0.0159(19) C(14) 0.051(2) 0.055(3) 0.0294(18) 0.006(2) 0.0007(16) -0.0009(17) C(20) 0.0308(18) 0.035(2) 0.0320(17) 0.0061(16) 0.0091(14) 0.0047(15) C(21) 0.032(2) 0.087(4) 0.041(2) 0.010(2) 0.0092(16) 0.006(2) C(22) 0.0221(18) 0.059(3) 0.0374(19) 0.0082(18) 0.0073(15) 0.0002(18) C(23) 0.054(3) 0.071(3) 0.060(3) 0.029(2) 0.027(2) 0.016(2) C(24) 0.076(4) 0.142(6) 0.068(3) 0.076(4) 0.034(3) 0.047(4) C(25) 0.056(3) 0.100(5) 0.059(3) 0.018(3) -0.008(2) -0.007(3) C(26) 0.072(4) 0.086(5) 0.079(4) 0.003(3) 0.002(3) -0.012(3) C(27) 0.044(2) 0.070(4) 0.069(3) 0.005(2) 0.015(2) 0.003(2) C(31) 0.043(2) 0.025(2) 0.045(2) 0.0034(17) 0.0082(16) 0.0084(16) C(32) 0.055(2) 0.033(2) 0.052(2) 0.0034(19) 0.0070(18) -0.0021(18) C(33) 0.051(2) 0.045(3) 0.049(2) 0.002(2) 0.0099(18) 0.0110(19) C(34) 0.057(3) 0.044(3) 0.062(2) 0.009(2) 0.008(2) 0.025(2) C(40) 0.0325(19) 0.035(2) 0.0310(18) 0.0033(16) 0.0015(14) 0.0056(15) C(41) 0.038(2) 0.032(2) 0.051(2) 0.0151(17) 0.0070(16) 0.0082(17) C(42) 0.042(2) 0.023(2) 0.050(2) 0.0107(17) 0.0042(17) 0.0113(16) C(43) 0.040(2) 0.052(3) 0.069(3) 0.011(2) 0.001(2) 0.011(2) C(44) 0.044(3) 0.067(4) 0.093(4) 0.010(2) -0.004(2) 0.027(3) C(45) 0.059(3) 0.071(4) 0.071(3) -0.007(3) -0.024(2) 0.029(3) C(46) 0.071(3) 0.060(3) 0.055(3) -0.003(2) -0.002(2) 0.025(2) C(47) 0.045(2) 0.046(3) 0.050(2) 0.0044(19) 0.0035(18) 0.0146(19) C(51) 0.0276(17) 0.0221(19) 0.0226(15) 0.0027(14) 0.0059(12) 0.0009(13) C(52) 0.0250(16) 0.028(2) 0.0229(15) 0.0060(14) 0.0036(12) 0.0044(13) C(53) 0.0292(17) 0.027(2) 0.0264(16) 0.0103(15) 0.0035(13) 0.0032(14) C(54) 0.0279(17) 0.029(2) 0.0258(16) 0.0044(15) 0.0039(13) 0.0064(14) C(55) 0.0210(16) 0.031(2) 0.0300(17) 0.0026(15) 0.0031(13) 0.0048(14) C(56) 0.0243(17) 0.028(2) 0.0299(16) 0.0052(15) 0.0040(13) 0.0052(14) C(521) 0.0262(17) 0.0221(19) 0.0304(16) 0.0058(14) 0.0045(13) 0.0028(14) C(522) 0.0335(19) 0.038(2) 0.0315(17) 0.0114(16) 0.0100(14) 0.0071(15) C(523) 0.040(2) 0.058(3) 0.042(2) 0.0158(19) 0.0207(16) 0.0188(18) C(524) 0.0289(19) 0.056(3) 0.054(2) 0.0167(18) 0.0201(17) 0.0188(19) C(525) 0.0254(17) 0.036(2) 0.0428(19) 0.0109(16) 0.0075(14) 0.0093(16) C(526) 0.0277(19) 0.057(3) 0.052(2) 0.0154(18) 0.0073(16) 0.0198(19) C(527) 0.038(2) 0.050(3) 0.044(2) 0.0157(18) -0.0014(16) 0.0183(18) C(528) 0.042(2) 0.042(2) 0.0353(18) 0.0113(18) 0.0083(16) 0.0128(17) C(529) 0.0243(17) 0.035(2) 0.0303(17) 0.0078(15) 0.0052(13) 0.0067(15) C(52A) 0.0240(16) 0.0255(19) 0.0322(17) 0.0042(14) 0.0058(13) 0.0054(14) C(541) 0.0319(18) 0.030(2) 0.0375(18) 0.0026(16) 0.0050(14) 0.0087(15) C(542) 0.046(2) 0.033(2) 0.060(2) 0.0061(18) 0.0077(18) 0.0203(19) C(543) 0.054(3) 0.047(3) 0.073(3) 0.012(2) 0.034(2) 0.028(2) C(544) 0.050(2) 0.044(3) 0.064(3) -0.012(2) -0.011(2) 0.014(2) C(561) 0.0260(17) 0.034(2) 0.0435(19) 0.0087(15) 0.0059(14) 0.0173(16) C(562) 0.044(2) 0.037(2) 0.063(2) 0.0199(19) 0.0216(18) 0.0176(19) C(563) 0.0255(19) 0.053(3) 0.082(3) 0.0124(18) 0.0072(18) 0.032(2) C(564) 0.042(2) 0.056(3) 0.048(2) 0.018(2) 0.0080(17) 0.0245(19) # 10. MOLECULAR GEOMETRY _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_publ_flag Zr O(50) 2.048(2) ? Zr C(20) 2.221(3) ? Zr N(10) 2.253(2) ? Zr C(40) 2.254(3) ? Zr N(30) 2.297(3) ? Zr C(5) 2.496(3) ? Zr C(1) 2.532(3) ? Zr C(4) 2.552(3) ? Zr C(3) 2.582(3) ? Zr C(2) 2.584(3) ? O(50) C(51) 1.347(4) ? N(10) C(20) 1.271(4) ? N(10) C(11) 1.504(4) ? N(30) C(40) 1.273(4) ? N(30) C(31) 1.506(4) ? C(1) C(2) 1.387(5) ? C(1) C(5) 1.389(5) ? C(2) C(3) 1.413(6) ? C(3) C(4) 1.402(5) ? C(4) C(5) 1.376(5) ? C(11) C(12) 1.506(5) ? C(11) C(14) 1.519(5) ? C(11) C(13) 1.527(5) ? C(20) C(21) 1.518(4) ? C(21) C(22) 1.508(5) ? C(22) C(27) 1.376(6) ? C(22) C(23) 1.374(6) ? C(23) C(24) 1.445(7) ? C(24) C(25) 1.413(8) ? C(25) C(26) 1.315(7) ? C(26) C(27) 1.340(6) ? C(31) C(33) 1.529(5) ? C(31) C(34) 1.528(5) ? C(31) C(32) 1.531(5) ? C(40) C(41) 1.513(5) ? C(41) C(42) 1.517(5) ? C(42) C(47) 1.372(5) ? C(42) C(43) 1.390(5) ? C(43) C(44) 1.385(5) ? C(44) C(45) 1.357(6) ? C(45) C(46) 1.378(6) ? C(46) C(47) 1.392(5) ? C(51) C(52) 1.412(4) ? C(51) C(56) 1.435(4) ? C(52) C(53) 1.402(4) ? C(52) C(521) 1.505(4) ? C(53) C(54) 1.381(4) ? C(54) C(55) 1.400(4) ? C(54) C(541) 1.527(5) ? C(55) C(56) 1.379(4) ? C(56) C(561) 1.536(4) ? C(521) C(522) 1.371(4) ? C(521) C(52A) 1.448(4) ? C(522) C(523) 1.416(4) ? C(523) C(524) 1.362(5) ? C(524) C(525) 1.407(5) ? C(525) C(526) 1.424(4) ? C(525) C(52A) 1.426(4) ? C(526) C(527) 1.353(5) ? C(527) C(528) 1.405(5) ? C(528) C(529) 1.371(4) ? C(529) C(52A) 1.421(4) ? C(541) C(542) 1.520(5) ? C(541) C(544) 1.531(5) ? C(541) C(543) 1.539(5) ? C(561) C(564) 1.528(5) ? C(561) C(562) 1.534(5) ? C(561) C(563) 1.534(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(50) Zr C(20) 107.70(11) ? O(50) Zr N(10) 87.20(9) ? C(20) Zr N(10) 33.01(10) ? O(50) Zr C(40) 106.91(10) ? C(20) Zr C(40) 115.95(12) ? N(10) Zr C(40) 99.43(11) ? O(50) Zr N(30) 136.12(9) ? C(20) Zr N(30) 89.26(12) ? N(10) Zr N(30) 86.48(9) ? C(40) Zr N(30) 32.46(10) ? O(50) Zr C(5) 98.51(11) ? C(20) Zr C(5) 91.50(12) ? N(10) Zr C(5) 120.63(11) ? C(40) Zr C(5) 133.34(12) ? N(30) Zr C(5) 121.77(11) ? O(50) Zr C(1) 129.21(11) ? C(20) Zr C(1) 89.71(12) ? N(10) Zr C(1) 122.54(11) ? C(40) Zr C(1) 107.05(13) ? N(30) Zr C(1) 89.73(11) ? C(5) Zr C(1) 32.08(12) ? O(50) Zr C(4) 78.15(10) ? C(20) Zr C(4) 120.64(12) ? N(10) Zr C(4) 142.16(11) ? C(40) Zr C(4) 118.13(12) ? N(30) Zr C(4) 127.72(10) ? C(5) Zr C(4) 31.62(11) ? C(1) Zr C(4) 52.70(12) ? O(50) Zr C(3) 92.84(12) ? C(20) Zr C(3) 141.46(12) ? N(10) Zr C(3) 173.16(11) ? C(40) Zr C(3) 87.11(12) ? N(30) Zr C(3) 98.17(12) ? C(5) Zr C(3) 52.60(12) ? C(1) Zr C(3) 52.82(12) ? C(4) Zr C(3) 31.69(12) ? O(50) Zr C(2) 124.45(12) ? C(20) Zr C(2) 117.53(13) ? N(10) Zr C(2) 147.03(13) ? C(40) Zr C(2) 81.26(12) ? N(30) Zr C(2) 76.61(11) ? C(5) Zr C(2) 52.18(12) ? C(1) Zr C(2) 31.45(12) ? C(4) Zr C(2) 52.11(12) ? C(3) Zr C(2) 31.74(13) ? C(51) O(50) Zr 152.12(18) ? C(20) N(10) C(11) 131.4(3) ? C(20) N(10) Zr 72.09(17) ? C(11) N(10) Zr 156.5(2) ? C(40) N(30) C(31) 130.7(3) ? C(40) N(30) Zr 71.9(2) ? C(31) N(30) Zr 156.8(2) ? C(2) C(1) C(5) 107.2(3) ? C(2) C(1) Zr 76.35(19) ? C(5) C(1) Zr 72.56(19) ? C(1) C(2) C(3) 108.7(4) ? C(1) C(2) Zr 72.20(19) ? C(3) C(2) Zr 74.1(2) ? C(4) C(3) C(2) 106.5(3) ? C(4) C(3) Zr 72.97(18) ? C(2) C(3) Zr 74.2(2) ? C(5) C(4) C(3) 108.2(4) ? C(5) C(4) Zr 71.96(19) ? C(3) C(4) Zr 75.3(2) ? C(4) C(5) C(1) 109.3(3) ? C(4) C(5) Zr 76.42(19) ? C(1) C(5) Zr 75.37(19) ? C(12) C(11) N(10) 113.0(3) ? C(12) C(11) C(14) 109.6(3) ? N(10) C(11) C(14) 106.2(3) ? C(12) C(11) C(13) 111.1(3) ? N(10) C(11) C(13) 107.3(3) ? C(14) C(11) C(13) 109.4(3) ? N(10) C(20) C(21) 127.8(3) ? N(10) C(20) Zr 74.90(18) ? C(21) C(20) Zr 157.1(2) ? C(22) C(21) C(20) 113.3(3) ? C(27) C(22) C(23) 119.7(4) ? C(27) C(22) C(21) 119.9(4) ? C(23) C(22) C(21) 120.4(4) ? C(22) C(23) C(24) 118.4(5) ? C(25) C(24) C(23) 116.7(5) ? C(26) C(25) C(24) 122.9(5) ? C(25) C(26) C(27) 119.5(6) ? C(26) C(27) C(22) 122.8(5) ? N(30) C(31) C(33) 105.8(3) ? N(30) C(31) C(34) 111.5(3) ? C(33) C(31) C(34) 109.9(3) ? N(30) C(31) C(32) 109.9(3) ? C(33) C(31) C(32) 109.4(3) ? C(34) C(31) C(32) 110.4(3) ? N(30) C(40) C(41) 127.9(3) ? N(30) C(40) Zr 75.6(2) ? C(41) C(40) Zr 154.9(3) ? C(40) C(41) C(42) 113.9(3) ? C(47) C(42) C(43) 119.0(3) ? C(47) C(42) C(41) 122.2(3) ? C(43) C(42) C(41) 118.8(3) ? C(44) C(43) C(42) 119.8(4) ? C(45) C(44) C(43) 120.9(4) ? C(44) C(45) C(46) 119.9(4) ? C(45) C(46) C(47) 119.6(4) ? C(42) C(47) C(46) 120.8(4) ? O(50) C(51) C(52) 120.0(3) ? O(50) C(51) C(56) 122.1(3) ? C(52) C(51) C(56) 117.9(3) ? C(53) C(52) C(51) 120.5(3) ? C(53) C(52) C(521) 117.4(3) ? C(51) C(52) C(521) 121.9(3) ? C(54) C(53) C(52) 122.2(3) ? C(53) C(54) C(55) 116.3(3) ? C(53) C(54) C(541) 123.6(3) ? C(55) C(54) C(541) 120.1(3) ? C(56) C(55) C(54) 124.7(3) ? C(55) C(56) C(51) 118.2(3) ? C(55) C(56) C(561) 119.5(3) ? C(51) C(56) C(561) 122.2(3) ? C(522) C(521) C(52A) 118.9(3) ? C(522) C(521) C(52) 119.7(3) ? C(52A) C(521) C(52) 121.0(3) ? C(521) C(522) C(523) 121.8(3) ? C(524) C(523) C(522) 119.9(3) ? C(523) C(524) C(525) 120.9(3) ? C(524) C(525) C(526) 121.4(3) ? C(524) C(525) C(52A) 120.0(3) ? C(526) C(525) C(52A) 118.7(3) ? C(527) C(526) C(525) 121.5(3) ? C(526) C(527) C(528) 120.0(3) ? C(529) C(528) C(527) 120.6(3) ? C(528) C(529) C(52A) 120.9(3) ? C(529) C(52A) C(525) 118.2(3) ? C(529) C(52A) C(521) 123.4(3) ? C(525) C(52A) C(521) 118.4(3) ? C(542) C(541) C(54) 112.2(3) ? C(542) C(541) C(544) 108.4(3) ? C(54) C(541) C(544) 109.4(3) ? C(542) C(541) C(543) 107.9(3) ? C(54) C(541) C(543) 110.0(3) ? C(544) C(541) C(543) 108.9(3) ? C(564) C(561) C(562) 110.5(3) ? C(564) C(561) C(563) 106.8(3) ? C(562) C(561) C(563) 107.5(3) ? C(564) C(561) C(56) 110.2(3) ? C(562) C(561) C(56) 109.6(3) ? C(563) C(561) C(56) 112.2(3) ? #============================================================================== data_MT46G _database_code_CSD 182090 #============================================================================== _audit_creation_date 30-07-98 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C39 H44 O1 Zr1' _chemical_formula_structural ? _chemical_formula_weight 620.01 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'c 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -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' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 27.9412(6) _cell_length_b 13.9072(3) _cell_length_c 20.6729(4) _cell_angle_alpha 90.00 _cell_angle_beta 124.4934(10) _cell_angle_gamma 90.00 _cell_volume 6620.9(5) _cell_measurement_reflns_used 25919 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _cell_formula_units_z 8 _exptl_crystal_density_diffrn 1.24 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.352 _cell_measurement_temperature 203 _exptl_crystal_F_000 2608 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6569 _exptl_absorpt_correction_T_max 0.9158 _diffrn_reflns_number 25919 _reflns_number_total 8668 _reflns_number_gt 5794 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 30.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_max 22 # 7. REFINEMENT DATA _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_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.122 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 8668 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+3.4709P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.65 _refine_diff_density_min -0.84 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.33E-02 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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_calc_flag Zr 0.158781(9) -0.004591(15) 0.322159(14) 0.03950(11) Uani ? O(10) 0.23672(6) -0.04531(12) 0.40725(10) 0.0410(7) Uani ? C(1) 0.08893(13) -0.0516(2) 0.18016(17) 0.0579(12) Uani ? C(2) 0.13589(13) -0.1128(2) 0.21226(17) 0.0551(13) Uani ? C(3) 0.18439(14) -0.0601(3) 0.23177(19) 0.0662(15) Uani ? C(4) 0.16710(19) 0.0364(3) 0.2128(2) 0.0780(19) Uani ? C(5) 0.10710(16) 0.0407(2) 0.18036(18) 0.0687(15) Uani ? C(11) 0.29180(10) -0.08200(17) 0.44373(14) 0.0384(9) Uani ? C(12) 0.29849(10) -0.17822(17) 0.43117(14) 0.0386(9) Uani ? C(13) 0.35461(10) -0.21572(18) 0.46588(15) 0.0429(10) Uani ? C(14) 0.40396(10) -0.16032(19) 0.51329(15) 0.0436(10) Uani ? C(15) 0.39555(10) -0.06573(19) 0.52575(15) 0.0453(10) Uani ? C(16) 0.34119(11) -0.02311(18) 0.49259(15) 0.0422(9) Uani ? C(20) 0.15249(13) 0.15465(19) 0.34182(19) 0.0579(15) Uani ? C(21) 0.13354(11) 0.23533(19) 0.28554(17) 0.0510(12) Uani ? C(22) 0.17298(13) 0.2836(2) 0.27597(19) 0.0598(14) Uani ? C(23) 0.15702(17) 0.3581(2) 0.2228(2) 0.0770(16) Uani ? C(24) 0.10238(18) 0.3884(3) 0.1784(2) 0.0863(19) Uani ? C(25) 0.06112(17) 0.3467(3) 0.1858(2) 0.096(2) Uani ? C(26) 0.07701(14) 0.2680(3) 0.2394(2) 0.0858(18) Uani ? C(30) 0.09356(11) -0.0849(2) 0.33363(17) 0.0536(12) Uani ? C(31) 0.09957(12) -0.0267(2) 0.39692(17) 0.0491(12) Uani ? C(32) 0.05696(13) 0.0400(2) 0.3832(2) 0.0576(14) Uani ? C(33) 0.06467(15) 0.0995(3) 0.4415(2) 0.0702(19) Uani ? C(34) 0.11503(17) 0.0963(3) 0.5151(2) 0.082(2) Uani ? C(35) 0.15843(16) 0.0321(3) 0.5312(2) 0.0716(15) Uani ? C(36) 0.15105(13) -0.0281(2) 0.47321(18) 0.0571(13) Uani ? C(121) 0.24843(10) -0.24509(17) 0.38295(14) 0.0396(9) Uani ? C(122) 0.20628(10) -0.25999(18) 0.39803(14) 0.0431(10) Uani ? C(123) 0.16255(11) -0.3277(2) 0.35617(16) 0.0517(11) Uani ? C(124) 0.15951(12) -0.38058(19) 0.29768(18) 0.0576(13) Uani ? C(125) 0.20015(13) -0.3654(2) 0.28047(19) 0.0591(14) Uani ? C(126) 0.24416(12) -0.29900(18) 0.32297(17) 0.0507(12) Uani ? C(141) 0.46594(10) -0.20086(19) 0.55411(16) 0.0479(11) Uani ? C(142) 0.49094(13) -0.2161(3) 0.64160(18) 0.0683(14) Uani ? C(143) 0.46668(12) -0.2964(2) 0.5184(2) 0.0640(14) Uani ? C(144) 0.50511(12) -0.1301(2) 0.5477(2) 0.0695(17) Uani ? C(161) 0.33612(11) 0.08335(18) 0.50725(16) 0.0480(10) Uani ? C(162) 0.39564(12) 0.1287(2) 0.5678(2) 0.0667(14) Uani ? C(163) 0.31119(12) 0.1393(2) 0.43077(18) 0.0591(13) Uani ? C(164) 0.29893(12) 0.0965(2) 0.53966(17) 0.0562(12) Uani ? H(1) 0.0511 -0.0696 0.1614 0.0750 Uiso calc H(2) 0.1351 -0.1787 0.2196 0.0720 Uiso calc H(3) 0.2216 -0.0841 0.2535 0.0860 Uiso calc H(4) 0.1909 0.0880 0.2203 0.1010 Uiso calc H(5) 0.0841 0.0956 0.1624 0.0890 Uiso calc H(13) 0.3588 -0.2797 0.4568 0.0560 Uiso calc H(15) 0.4283 -0.0282 0.5584 0.0590 Uiso calc H(22) 0.2117 0.2649 0.3067 0.0780 Uiso calc H(23) 0.1849 0.3872 0.2182 0.1000 Uiso calc H(24) 0.0921 0.4378 0.1424 0.1130 Uiso calc H(25) 0.0231 0.3692 0.1562 0.1250 Uiso calc H(26) 0.0487 0.2387 0.2431 0.1120 Uiso calc H(32) 0.0227 0.0440 0.3333 0.0750 Uiso calc H(33) 0.0354 0.1421 0.4309 0.0920 Uiso calc H(34) 0.1201 0.1372 0.5542 0.1060 Uiso calc H(35) 0.1926 0.0296 0.5812 0.0930 Uiso calc H(36) 0.1806 -0.0706 0.4847 0.0740 Uiso calc H(122) 0.2074 -0.2240 0.4368 0.0560 Uiso calc H(123) 0.1352 -0.3374 0.3677 0.0670 Uiso calc H(124) 0.1304 -0.4262 0.2699 0.0750 Uiso calc H(125) 0.1979 -0.4000 0.2403 0.0770 Uiso calc H(126) 0.2715 -0.2901 0.3113 0.0660 Uiso calc H(14A) 0.4678 -0.2627 0.6466 0.0890 Uiso calc H(14B) 0.4904 -0.1563 0.6644 0.0890 Uiso calc H(14C) 0.5302 -0.2389 0.6684 0.0890 Uiso calc H(14D) 0.4459 -0.3439 0.5270 0.0830 Uiso calc H(14E) 0.5061 -0.3171 0.5426 0.0830 Uiso calc H(14F) 0.4485 -0.2885 0.4630 0.0830 Uiso calc H(14G) 0.5435 -0.1565 0.5737 0.0900 Uiso calc H(14H) 0.5067 -0.0703 0.5721 0.0900 Uiso calc H(14I) 0.4897 -0.1192 0.4934 0.0900 Uiso calc H(16A) 0.3904 0.1945 0.5766 0.0870 Uiso calc H(16B) 0.4197 0.1261 0.5484 0.0870 Uiso calc H(16C) 0.4139 0.0937 0.6163 0.0870 Uiso calc H(16D) 0.2752 0.1105 0.3900 0.0770 Uiso calc H(16E) 0.3383 0.1377 0.4162 0.0770 Uiso calc H(16F) 0.3044 0.2048 0.4382 0.0770 Uiso calc H(16G) 0.2614 0.0683 0.5041 0.0730 Uiso calc H(16H) 0.2946 0.1639 0.5453 0.0730 Uiso calc H(16I) 0.3175 0.0656 0.5899 0.0730 Uiso calc H(20A) 0.1276 0.1578 0.3605 0.0760 Uiso calc H(20B) 0.1910 0.1725 0.3861 0.0760 Uiso calc H(30A) 0.0547 -0.0820 0.2860 0.0700 Uiso calc H(30B) 0.1047 -0.1514 0.3491 0.0700 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr 0.02858(14) 0.03592(15) 0.04786(16) -0.00114(9) 0.01796(11) -0.00270(9) O(10) 0.0298(8) 0.0412(9) 0.0463(9) -0.0002(7) 0.0182(7) -0.0040(7) C(1) 0.0489(15) 0.0607(17) 0.0511(16) -0.0007(14) 0.0206(13) -0.0093(13) C(2) 0.0650(18) 0.0473(14) 0.0547(16) 0.0032(13) 0.0350(14) -0.0041(12) C(3) 0.0559(18) 0.089(2) 0.064(2) 0.0105(17) 0.0401(16) 0.0027(17) C(4) 0.099(3) 0.079(2) 0.072(2) -0.030(2) 0.058(2) -0.0013(19) C(5) 0.080(2) 0.0569(18) 0.0534(18) 0.0137(17) 0.0283(17) 0.0087(14) C(11) 0.0304(11) 0.0427(12) 0.0401(12) -0.0001(9) 0.0188(10) 0.0014(10) C(12) 0.0314(11) 0.0421(12) 0.0414(12) -0.0003(10) 0.0201(10) 0.0003(10) C(13) 0.0354(12) 0.0427(12) 0.0524(15) 0.0050(10) 0.0260(11) 0.0042(11) C(14) 0.0336(11) 0.0496(14) 0.0475(14) 0.0027(10) 0.0229(11) 0.0082(11) C(15) 0.0318(12) 0.0483(14) 0.0483(14) -0.0033(10) 0.0181(11) 0.0012(11) C(16) 0.0328(11) 0.0451(12) 0.0426(13) -0.0021(10) 0.0177(10) -0.0009(10) C(20) 0.0655(18) 0.0392(14) 0.084(2) -0.0038(13) 0.0513(17) -0.0031(13) C(21) 0.0384(13) 0.0413(13) 0.0640(17) 0.0017(11) 0.0234(13) -0.0118(12) C(22) 0.0568(17) 0.0478(15) 0.073(2) 0.0028(13) 0.0357(15) 0.0047(14) C(23) 0.085(2) 0.0561(18) 0.086(2) 0.0071(18) 0.046(2) 0.0081(17) C(24) 0.081(3) 0.068(2) 0.077(2) 0.008(2) 0.025(2) -0.0015(18) C(25) 0.056(2) 0.081(3) 0.089(3) 0.030(2) 0.0039(19) -0.006(2) C(26) 0.0416(16) 0.069(2) 0.117(3) 0.0003(15) 0.0270(19) -0.024(2) C(30) 0.0407(14) 0.0605(16) 0.0615(17) -0.0033(12) 0.0300(13) -0.0029(13) C(31) 0.0423(14) 0.0536(14) 0.0613(17) -0.0028(12) 0.0353(13) 0.0091(12) C(32) 0.0480(15) 0.0643(18) 0.072(2) 0.0027(14) 0.0408(15) 0.0093(15) C(33) 0.068(2) 0.070(2) 0.092(3) 0.0030(17) 0.057(2) -0.0031(18) C(34) 0.088(3) 0.089(3) 0.093(3) -0.014(2) 0.066(2) -0.022(2) C(35) 0.067(2) 0.095(2) 0.0557(19) -0.0076(19) 0.0364(17) -0.0019(17) C(36) 0.0521(16) 0.0641(17) 0.0604(18) 0.0013(14) 0.0350(15) 0.0131(14) C(121) 0.0347(11) 0.0369(11) 0.0440(13) 0.0044(10) 0.0203(10) 0.0028(9) C(122) 0.0377(12) 0.0462(13) 0.0399(13) -0.0007(10) 0.0186(10) 0.0000(10) C(123) 0.0388(13) 0.0527(15) 0.0590(16) -0.0056(12) 0.0250(12) 0.0067(13) C(124) 0.0501(15) 0.0413(14) 0.0649(18) -0.0075(12) 0.0226(14) -0.0107(12) C(125) 0.0602(17) 0.0477(15) 0.0687(19) -0.0023(14) 0.0360(15) -0.0152(14) C(126) 0.0493(14) 0.0448(14) 0.0640(17) -0.0001(12) 0.0356(14) -0.0091(12) C(141) 0.0339(12) 0.0526(15) 0.0562(15) 0.0037(11) 0.0249(12) 0.0098(12) C(142) 0.0466(15) 0.086(2) 0.0619(19) 0.0173(16) 0.0244(14) 0.0209(16) C(143) 0.0437(15) 0.0657(18) 0.079(2) 0.0153(14) 0.0325(15) 0.0073(16) C(144) 0.0407(14) 0.071(2) 0.097(3) 0.0040(14) 0.0391(16) 0.0236(18) C(161) 0.0353(12) 0.0438(13) 0.0522(15) -0.0046(11) 0.0171(11) -0.0054(11) C(162) 0.0435(15) 0.0547(17) 0.074(2) -0.0082(13) 0.0166(14) -0.0137(15) C(163) 0.0486(15) 0.0455(14) 0.0721(19) -0.0040(13) 0.0275(14) 0.0035(13) C(164) 0.0471(15) 0.0534(15) 0.0586(17) -0.0020(13) 0.0242(13) -0.0141(13) # 10. MOLECULAR GEOMETRY _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_publ_flag Zr O(10) 1.9542(15) ? Zr C(30) 2.262(3) ? Zr C(20) 2.276(3) ? Zr C(4) 2.466(3) ? Zr C(3) 2.472(3) ? Zr C(2) 2.488(3) ? Zr C(5) 2.506(3) ? Zr C(1) 2.523(3) ? Zr C(31) 2.849(3) ? O(10) C(11) 1.372(3) ? C(1) C(2) 1.379(4) ? C(1) C(5) 1.379(5) ? C(2) C(3) 1.385(4) ? C(3) C(4) 1.404(5) ? C(4) C(5) 1.411(5) ? C(11) C(12) 1.396(3) ? C(11) C(16) 1.420(3) ? C(12) C(13) 1.404(3) ? C(12) C(121) 1.495(3) ? C(13) C(14) 1.387(3) ? C(14) C(15) 1.386(4) ? C(14) C(141) 1.541(3) ? C(15) C(16) 1.396(3) ? C(16) C(161) 1.534(3) ? C(20) C(21) 1.482(4) ? C(21) C(26) 1.380(4) ? C(21) C(22) 1.397(4) ? C(22) C(23) 1.388(4) ? C(23) C(24) 1.328(5) ? C(24) C(25) 1.374(6) ? C(25) C(26) 1.437(6) ? C(30) C(31) 1.466(4) ? C(31) C(32) 1.405(4) ? C(31) C(36) 1.410(4) ? C(32) C(33) 1.375(5) ? C(33) C(34) 1.368(5) ? C(34) C(35) 1.387(5) ? C(35) C(36) 1.379(5) ? C(121) C(122) 1.394(3) ? C(121) C(126) 1.395(3) ? C(122) C(123) 1.390(3) ? C(123) C(124) 1.376(4) ? C(124) C(125) 1.385(4) ? C(125) C(126) 1.383(4) ? C(141) C(143) 1.527(4) ? C(141) C(144) 1.532(4) ? C(141) C(142) 1.541(4) ? C(161) C(163) 1.531(4) ? C(161) C(164) 1.533(4) ? C(161) C(162) 1.540(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(10) Zr C(30) 108.41(9) ? O(10) Zr C(20) 106.29(9) ? C(30) Zr C(20) 108.28(10) ? O(10) Zr C(4) 104.86(12) ? C(30) Zr C(4) 135.23(12) ? C(20) Zr C(4) 89.76(12) ? O(10) Zr C(3) 86.44(9) ? C(30) Zr C(3) 121.36(11) ? C(20) Zr C(3) 121.54(12) ? C(4) Zr C(3) 33.02(13) ? O(10) Zr C(2) 103.05(8) ? C(30) Zr C(2) 89.49(10) ? C(20) Zr C(2) 138.22(11) ? C(4) Zr C(2) 53.97(11) ? C(3) Zr C(2) 32.43(10) ? O(10) Zr C(5) 137.39(10) ? C(30) Zr C(5) 106.38(12) ? C(20) Zr C(5) 85.00(11) ? C(4) Zr C(5) 32.95(12) ? C(3) Zr C(5) 54.27(11) ? C(2) Zr C(5) 53.42(10) ? O(10) Zr C(1) 134.89(8) ? C(30) Zr C(1) 81.69(11) ? C(20) Zr C(1) 111.90(11) ? C(4) Zr C(1) 53.55(12) ? C(3) Zr C(1) 53.42(10) ? C(2) Zr C(1) 31.93(9) ? C(5) Zr C(1) 31.84(11) ? O(10) Zr C(31) 100.02(8) ? C(30) Zr C(31) 30.67(9) ? C(20) Zr C(31) 83.15(10) ? C(4) Zr C(31) 155.12(12) ? C(3) Zr C(31) 151.88(11) ? C(2) Zr C(31) 120.14(9) ? C(5) Zr C(31) 122.32(11) ? C(1) Zr C(31) 107.40(10) ? C(11) O(10) Zr 159.03(16) ? C(2) C(1) C(5) 108.9(3) ? C(2) C(1) Zr 72.65(16) ? C(5) C(1) Zr 73.41(17) ? C(1) C(2) C(3) 108.7(3) ? C(1) C(2) Zr 75.42(17) ? C(3) C(2) Zr 73.16(17) ? C(2) C(3) C(4) 107.4(3) ? C(2) C(3) Zr 74.41(17) ? C(4) C(3) Zr 73.25(19) ? C(3) C(4) C(5) 107.6(3) ? C(3) C(4) Zr 73.72(18) ? C(5) C(4) Zr 75.07(19) ? C(1) C(5) C(4) 107.3(3) ? C(1) C(5) Zr 74.75(17) ? C(4) C(5) Zr 71.98(18) ? O(10) C(11) C(12) 118.7(2) ? O(10) C(11) C(16) 120.8(2) ? C(12) C(11) C(16) 120.4(2) ? C(11) C(12) C(13) 119.3(2) ? C(11) C(12) C(121) 123.2(2) ? C(13) C(12) C(121) 117.5(2) ? C(14) C(13) C(12) 122.0(2) ? C(15) C(14) C(13) 116.9(2) ? C(15) C(14) C(141) 120.1(2) ? C(13) C(14) C(141) 122.9(2) ? C(14) C(15) C(16) 124.3(2) ? C(15) C(16) C(11) 117.0(2) ? C(15) C(16) C(161) 120.6(2) ? C(11) C(16) C(161) 122.4(2) ? C(21) C(20) Zr 128.8(2) ? C(26) C(21) C(22) 115.5(3) ? C(26) C(21) C(20) 123.5(3) ? C(22) C(21) C(20) 121.0(2) ? C(23) C(22) C(21) 123.1(3) ? C(24) C(23) C(22) 120.8(4) ? C(23) C(24) C(25) 119.9(4) ? C(24) C(25) C(26) 119.7(3) ? C(21) C(26) C(25) 121.1(4) ? C(31) C(30) Zr 97.40(17) ? C(32) C(31) C(36) 116.5(3) ? C(32) C(31) C(30) 121.9(3) ? C(36) C(31) C(30) 121.3(3) ? C(32) C(31) Zr 120.34(19) ? C(36) C(31) Zr 94.03(17) ? C(30) C(31) Zr 51.93(13) ? C(33) C(32) C(31) 121.7(3) ? C(34) C(33) C(32) 120.5(3) ? C(33) C(34) C(35) 119.7(3) ? C(36) C(35) C(34) 120.2(3) ? C(35) C(36) C(31) 121.3(3) ? C(122) C(121) C(126) 117.4(2) ? C(122) C(121) C(12) 122.2(2) ? C(126) C(121) C(12) 120.3(2) ? C(123) C(122) C(121) 121.2(2) ? C(124) C(123) C(122) 120.3(3) ? C(123) C(124) C(125) 119.5(3) ? C(124) C(125) C(126) 120.1(3) ? C(125) C(126) C(121) 121.4(3) ? C(143) C(141) C(144) 108.1(2) ? C(143) C(141) C(14) 111.9(2) ? C(144) C(141) C(14) 110.7(2) ? C(143) C(141) C(142) 109.1(2) ? C(144) C(141) C(142) 108.6(3) ? C(14) C(141) C(142) 108.4(2) ? C(163) C(161) C(164) 111.5(2) ? C(163) C(161) C(16) 109.0(2) ? C(164) C(161) C(16) 111.3(2) ? C(163) C(161) C(162) 106.4(2) ? C(164) C(161) C(162) 106.4(2) ? C(16) C(161) C(162) 112.2(2) ? #============================================================================== #============================================================================== data_MT48G _database_code_CSD 182091 _audit_creation_date 27-08-98 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C45.66 H56.98 N1 O1 Zr1' _chemical_formula_structural ? _chemical_formula_weight 727.09 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21/n 1' 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 16.5371(8) _cell_length_b 17.3716(10) _cell_length_c 31.2041(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.265(3) _cell_angle_gamma 90.00 _cell_volume 8820.7(13) _cell_measurement_reflns_used 38266 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _cell_formula_units_z 8 _exptl_crystal_density_diffrn 1.09 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.272 _cell_measurement_temperature 203 _exptl_crystal_F_000 3104 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.7028 _exptl_absorpt_correction_T_max 0.9666 _diffrn_reflns_number 38266 _reflns_number_total 10901 _reflns_number_gt 6065 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.140 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 30.15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_max 39 # 7. REFINEMENT DATA _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_R_factor_gt 0.084 _refine_ls_wR_factor_ref 0.207 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 10901 _refine_ls_number_parameters 888 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.68 _refine_diff_density_min -0.71 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.12E-02 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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_calc_flag Zr(1) 0.15152(5) 0.06454(5) 0.29358(2) 0.0319(3) Uani ? Zr(2) -0.34775(5) 0.10461(5) 0.29890(2) 0.0299(3) Uani ? O(110) 0.1126(3) 0.0203(3) 0.23399(16) 0.0360(17) Uani ? O(210) -0.3849(3) 0.1479(3) 0.23932(14) 0.0313(17) Uani ? N(17) 0.0913(4) -0.0255(4) 0.32702(19) 0.036(2) Uani ? N(27) -0.4105(4) 0.1932(4) 0.33141(19) 0.035(2) Uani ? C(11) 0.2997(5) 0.0770(6) 0.2892(3) 0.051(3) Uani ? C(12) 0.2616(6) 0.1237(8) 0.2564(3) 0.065(4) Uani ? C(13) 0.2277(6) 0.1869(6) 0.2776(4) 0.065(4) Uani ? C(14) 0.2471(6) 0.1743(7) 0.3224(3) 0.064(4) Uani ? C(15) 0.2936(5) 0.1071(6) 0.3292(3) 0.052(3) Uani ? C(18) 0.1606(5) -0.0119(5) 0.3499(2) 0.035(3) Uani ? C(19) 0.0468(5) 0.1508(5) 0.2990(3) 0.048(3) Uani ? C(21) -0.1984(5) 0.0921(6) 0.2966(3) 0.047(3) Uani ? C(22) -0.2075(5) 0.0603(6) 0.3362(3) 0.044(3) Uani ? C(23) -0.2541(5) -0.0049(6) 0.3281(3) 0.052(3) Uani ? C(24) -0.2709(5) -0.0150(6) 0.2821(3) 0.052(3) Uani ? C(25) -0.2370(6) 0.0443(6) 0.2623(3) 0.053(3) Uani ? C(28) -0.3402(5) 0.1818(5) 0.3563(3) 0.035(3) Uani ? C(29) -0.4537(5) 0.0193(5) 0.3030(2) 0.039(3) Uani ? C(111) 0.1176(5) -0.0033(5) 0.1930(2) 0.037(3) Uani ? C(112) 0.1790(5) -0.0577(5) 0.1880(2) 0.035(3) Uani ? C(113) 0.1841(5) -0.0824(5) 0.1460(3) 0.040(3) Uani ? C(114) 0.1313(6) -0.0542(5) 0.1094(2) 0.046(3) Uani ? C(115) 0.0725(5) -0.0016(5) 0.1161(3) 0.042(3) Uani ? C(116) 0.0629(5) 0.0256(5) 0.1565(3) 0.041(3) Uani ? C(121) 0.2376(5) -0.0871(4) 0.2255(2) 0.030(3) Uani ? C(122) 0.3209(5) -0.0875(5) 0.2252(2) 0.041(3) Uani ? C(123) 0.3762(5) -0.1135(5) 0.2594(3) 0.050(3) Uani ? C(124) 0.3499(6) -0.1436(5) 0.2964(3) 0.053(3) Uani ? C(125) 0.2672(6) -0.1450(6) 0.2968(3) 0.049(3) Uani ? C(126) 0.2123(5) -0.1186(5) 0.2615(2) 0.037(3) Uani ? C(141) 0.1410(8) -0.0806(7) 0.0625(3) 0.070(4) Uani ? C(142) 0.1880(12) -0.1564(12) 0.0625(4) 0.198(9) Uani ? C(143) 0.0525(10) -0.1109(13) 0.0411(4) 0.182(11) Uani ? C(144) 0.1644(17) -0.0121(11) 0.0385(5) 0.286(16) Uani ? C(161) -0.0031(5) 0.0847(5) 0.1605(3) 0.041(3) Uani ? C(162) -0.0588(6) 0.1011(6) 0.1166(3) 0.063(3) Uani ? C(163) 0.0365(5) 0.1610(5) 0.1775(3) 0.050(3) Uani ? C(164) -0.0606(5) 0.0544(6) 0.1913(3) 0.053(3) Uani ? C(171) 0.0227(5) -0.0783(6) 0.3329(3) 0.047(3) Uani ? C(172) -0.0143(6) -0.0537(6) 0.3727(3) 0.065(4) Uani ? C(173) 0.0589(6) -0.1624(5) 0.3407(3) 0.055(3) Uani ? C(174) -0.0417(5) -0.0762(6) 0.2917(3) 0.059(3) Uani ? C(180) 0.2008(5) -0.0445(6) 0.3936(3) 0.053(3) Uani ? C(181) 0.2494(5) 0.0169(6) 0.4211(2) 0.039(3) Uani ? C(182) 0.2108(6) 0.0838(6) 0.4307(3) 0.051(3) Uani ? C(183) 0.2558(8) 0.1428(7) 0.4532(3) 0.067(4) Uani ? C(184) 0.3378(9) 0.1377(7) 0.4663(3) 0.075(5) Uani ? C(185) 0.3778(7) 0.0685(8) 0.4581(3) 0.082(5) Uani ? C(186) 0.3335(6) 0.0093(6) 0.4360(3) 0.061(4) Uani ? C(191) 0.0474(5) 0.1984(6) 0.3372(2) 0.039(3) Uani ? C(192) 0.0798(6) 0.2743(6) 0.3387(3) 0.056(4) Uani ? C(193) 0.0808(6) 0.3261(7) 0.3730(4) 0.065(4) Uani ? C(194) 0.0528(8) 0.3007(9) 0.4108(4) 0.090(5) Uani ? C(195) 0.0212(7) 0.2274(10) 0.4102(3) 0.083(5) Uani ? C(196) 0.0188(5) 0.1756(6) 0.3746(3) 0.055(3) Uani ? C(211) -0.3801(5) 0.1720(5) 0.1989(2) 0.036(3) Uani ? C(212) -0.3193(5) 0.2293(5) 0.1945(2) 0.034(3) Uani ? C(213) -0.3120(5) 0.2561(5) 0.1522(2) 0.044(3) Uani ? C(214) -0.3634(5) 0.2298(5) 0.1155(2) 0.042(3) Uani ? C(215) -0.4222(5) 0.1740(5) 0.1213(2) 0.041(3) Uani ? C(216) -0.4320(5) 0.1453(5) 0.1621(2) 0.037(3) Uani ? C(221) -0.2597(5) 0.2604(5) 0.2323(2) 0.037(3) Uani ? C(222) -0.2874(5) 0.2904(5) 0.2688(3) 0.043(3) Uani ? C(223) -0.2326(6) 0.3184(5) 0.3035(3) 0.048(3) Uani ? C(224) -0.1486(6) 0.3174(5) 0.3039(3) 0.049(3) Uani ? C(225) -0.1205(6) 0.2875(5) 0.2672(3) 0.050(3) Uani ? C(226) -0.1779(5) 0.2591(5) 0.2324(2) 0.040(3) Uani ? C(241) -0.3548(6) 0.2564(7) 0.0693(3) 0.056(4) Uani ? C(242) -0.3148(11) 0.1921(8) 0.0480(4) 0.137(7) Uani ? C(243) -0.4400(7) 0.2757(8) 0.0433(3) 0.096(5) Uani ? C(244) -0.3069(8) 0.3298(7) 0.0703(3) 0.082(5) Uani ? C(261) -0.4974(5) 0.0854(5) 0.1648(3) 0.046(3) Uani ? C(262) -0.5542(5) 0.1130(5) 0.1962(3) 0.050(3) Uani ? C(263) -0.4550(6) 0.0083(6) 0.1808(3) 0.055(3) Uani ? C(264) -0.5546(6) 0.0678(6) 0.1202(3) 0.059(3) Uani ? C(271) -0.4793(5) 0.2472(5) 0.3364(2) 0.038(3) Uani ? C(272) -0.5413(5) 0.2438(6) 0.2938(2) 0.053(3) Uani ? C(273) -0.4491(6) 0.3292(6) 0.3457(3) 0.057(3) Uani ? C(274) -0.5221(5) 0.2169(6) 0.3731(3) 0.054(3) Uani ? C(280) -0.3032(5) 0.2152(5) 0.3996(2) 0.048(3) Uani ? C(281) -0.2562(6) 0.1575(6) 0.4288(2) 0.046(3) Uani ? C(282) -0.1772(7) 0.1711(7) 0.4478(3) 0.085(4) Uani ? C(283) -0.1321(8) 0.1147(10) 0.4748(5) 0.127(7) Uani ? C(284) -0.1663(8) 0.0466(8) 0.4819(3) 0.089(5) Uani ? C(285) -0.2435(7) 0.0321(7) 0.4638(3) 0.069(4) Uani ? C(286) -0.2882(6) 0.0883(6) 0.4378(3) 0.059(4) Uani ? C(291) -0.4513(4) -0.0364(5) 0.3387(2) 0.028(2) Uani ? C(292) -0.4715(5) -0.0161(6) 0.3794(3) 0.049(3) Uani ? C(293) -0.4643(6) -0.0672(7) 0.4137(3) 0.059(4) Uani ? C(294) -0.4381(6) -0.1379(8) 0.4104(3) 0.063(4) Uani ? C(295) -0.4175(5) -0.1615(6) 0.3700(3) 0.055(3) Uani ? C(296) -0.4244(5) -0.1104(6) 0.3357(3) 0.044(3) Uani ? C(901) 0.2310(11) 0.1622(11) 0.1233(5) 0.088(6) Uiso ? C(902) 0.238(2) 0.204(2) 0.0856(9) 0.185(13) Uiso ? C(903) 0.162(2) 0.237(2) 0.0666(11) 0.198(14) Uiso ? C(904) 0.1432(17) 0.2740(19) 0.0270(9) 0.161(11) Uiso ? C(905) 0.0762(10) 0.3078(11) 0.0051(5) 0.084(6) Uiso ? H(11) 0.3263 0.0312 0.2850 0.0660 Uiso calc H(12) 0.2581 0.1162 0.2267 0.0850 Uiso calc H(13) 0.1984 0.2284 0.2638 0.0850 Uiso calc H(14) 0.2317 0.2053 0.3439 0.0830 Uiso calc H(15) 0.3164 0.0863 0.3561 0.0670 Uiso calc H(21) -0.1710 0.1378 0.2932 0.0610 Uiso calc H(22) -0.1858 0.0799 0.3635 0.0570 Uiso calc H(23) -0.2715 -0.0366 0.3487 0.0670 Uiso calc H(24) -0.3004 -0.0558 0.2676 0.0680 Uiso calc H(25) -0.2390 0.0516 0.2326 0.0690 Uiso calc H(113) 0.2237 -0.1186 0.1423 0.0530 Uiso calc H(115) 0.0369 0.0169 0.0919 0.0550 Uiso calc H(122) 0.3397 -0.0695 0.2006 0.0530 Uiso calc H(123) 0.4321 -0.1113 0.2585 0.0650 Uiso calc H(124) 0.3875 -0.1621 0.3199 0.0690 Uiso calc H(125) 0.2481 -0.1639 0.3210 0.0640 Uiso calc H(126) 0.1563 -0.1221 0.2620 0.0480 Uiso calc H(14A) 0.2460 -0.1466 0.0698 0.2550 Uiso calc H(14B) 0.1756 -0.1795 0.0342 0.2550 Uiso calc H(14C) 0.1720 -0.1907 0.0836 0.2550 Uiso calc H(14D) 0.0374 -0.1530 0.0579 0.2360 Uiso calc H(14E) 0.0534 -0.1281 0.0119 0.2360 Uiso calc H(14F) 0.0133 -0.0701 0.0404 0.2360 Uiso calc H(14G) 0.1156 0.0135 0.0241 0.3720 Uiso calc H(14H) 0.1963 -0.0285 0.0173 0.3720 Uiso calc H(14I) 0.1962 0.0226 0.0587 0.3720 Uiso calc H(16A) -0.0279 0.1273 0.0977 0.0820 Uiso calc H(16B) -0.1040 0.1328 0.1212 0.0820 Uiso calc H(16C) -0.0794 0.0534 0.1034 0.0820 Uiso calc H(16D) 0.0836 0.1509 0.1996 0.0650 Uiso calc H(16E) -0.0025 0.1911 0.1897 0.0650 Uiso calc H(16F) 0.0533 0.1888 0.1540 0.0650 Uiso calc H(16G) -0.0859 0.0071 0.1800 0.0690 Uiso calc H(16H) -0.1025 0.0919 0.1932 0.0690 Uiso calc H(16I) -0.0290 0.0455 0.2198 0.0690 Uiso calc H(17A) 0.0264 -0.0587 0.3986 0.0850 Uiso calc H(17B) -0.0605 -0.0859 0.3750 0.0850 Uiso calc H(17C) -0.0320 -0.0010 0.3693 0.0850 Uiso calc H(17D) 0.0835 -0.1775 0.3163 0.0720 Uiso calc H(17E) 0.0155 -0.1976 0.3437 0.0720 Uiso calc H(17F) 0.0998 -0.1632 0.3667 0.0720 Uiso calc H(17G) -0.0641 -0.0252 0.2875 0.0770 Uiso calc H(17H) -0.0849 -0.1119 0.2943 0.0770 Uiso calc H(17I) -0.0170 -0.0902 0.2672 0.0770 Uiso calc H(182) 0.1543 0.0891 0.4219 0.0670 Uiso calc H(183) 0.2287 0.1872 0.4595 0.0870 Uiso calc H(184) 0.3675 0.1786 0.4805 0.0980 Uiso calc H(185) 0.4341 0.0631 0.4677 0.1070 Uiso calc H(186) 0.3599 -0.0362 0.4309 0.0790 Uiso calc H(18A) 0.1589 -0.0648 0.4087 0.0700 Uiso calc H(18B) 0.2370 -0.0865 0.3891 0.0700 Uiso calc H(192) 0.1022 0.2908 0.3150 0.0730 Uiso calc H(193) 0.0994 0.3763 0.3711 0.0850 Uiso calc H(194) 0.0556 0.3322 0.4351 0.1170 Uiso calc H(195) 0.0004 0.2107 0.4344 0.1080 Uiso calc H(196) -0.0021 0.1262 0.3763 0.0720 Uiso calc H(19A) 0.0429 0.1854 0.2743 0.0620 Uiso calc H(19B) -0.0039 0.1214 0.2948 0.0620 Uiso calc H(213) -0.2716 0.2920 0.1493 0.0580 Uiso calc H(215) -0.4565 0.1551 0.0967 0.0530 Uiso calc H(222) -0.3434 0.2914 0.2695 0.0560 Uiso calc H(223) -0.2522 0.3385 0.3273 0.0630 Uiso calc H(224) -0.1119 0.3360 0.3277 0.0640 Uiso calc H(225) -0.0646 0.2867 0.2662 0.0650 Uiso calc H(226) -0.1591 0.2385 0.2085 0.0520 Uiso calc H(24A) -0.3112 0.2064 0.0187 0.1790 Uiso calc H(24B) -0.3471 0.1461 0.0476 0.1790 Uiso calc H(24C) -0.2606 0.1829 0.0641 0.1790 Uiso calc H(24D) -0.4686 0.3084 0.0603 0.1250 Uiso calc H(24E) -0.4706 0.2290 0.0363 0.1250 Uiso calc H(24F) -0.4341 0.3017 0.0168 0.1250 Uiso calc H(24G) -0.2524 0.3220 0.0863 0.1070 Uiso calc H(24H) -0.3337 0.3693 0.0841 0.1070 Uiso calc H(24I) -0.3040 0.3453 0.0410 0.1070 Uiso calc H(26A) -0.5216 0.1251 0.2240 0.0650 Uiso calc H(26B) -0.5926 0.0730 0.1996 0.0650 Uiso calc H(26C) -0.5836 0.1581 0.1844 0.0650 Uiso calc H(26D) -0.4269 -0.0119 0.1588 0.0710 Uiso calc H(26E) -0.4957 -0.0280 0.1863 0.0710 Uiso calc H(26F) -0.4162 0.0170 0.2071 0.0710 Uiso calc H(26G) -0.5859 0.1129 0.1102 0.0770 Uiso calc H(26H) -0.5913 0.0265 0.1239 0.0770 Uiso calc H(26I) -0.5216 0.0531 0.0991 0.0770 Uiso calc H(27A) -0.5149 0.2588 0.2701 0.0690 Uiso calc H(27B) -0.5860 0.2782 0.2955 0.0690 Uiso calc H(27C) -0.5619 0.1922 0.2891 0.0690 Uiso calc H(27D) -0.4108 0.3305 0.3727 0.0740 Uiso calc H(27E) -0.4950 0.3620 0.3478 0.0740 Uiso calc H(27F) -0.4226 0.3468 0.3225 0.0740 Uiso calc H(27G) -0.5434 0.1663 0.3658 0.0700 Uiso calc H(27H) -0.5663 0.2508 0.3766 0.0700 Uiso calc H(27I) -0.4831 0.2148 0.3999 0.0700 Uiso calc H(282) -0.1525 0.2177 0.4431 0.1110 Uiso calc H(283) -0.0781 0.1247 0.4878 0.1650 Uiso calc H(284) -0.1359 0.0098 0.4994 0.1160 Uiso calc H(285) -0.2675 -0.0149 0.4683 0.0890 Uiso calc H(286) -0.3428 0.0780 0.4260 0.0760 Uiso calc H(28A) -0.2671 0.2574 0.3953 0.0620 Uiso calc H(28B) -0.3467 0.2359 0.4134 0.0620 Uiso calc H(292) -0.4904 0.0335 0.3832 0.0640 Uiso calc H(293) -0.4783 -0.0512 0.4399 0.0770 Uiso calc H(294) -0.4331 -0.1717 0.4338 0.0820 Uiso calc H(295) -0.3992 -0.2114 0.3668 0.0710 Uiso calc H(296) -0.4103 -0.1269 0.3096 0.0570 Uiso calc H(29A) -0.5028 0.0501 0.3025 0.0510 Uiso calc H(29B) -0.4622 -0.0102 0.2762 0.0510 Uiso calc H(90A) 0.1739 0.1545 0.1244 0.1140 Uiso calc H(90B) 0.2565 0.1907 0.1485 0.1140 Uiso calc H(90C) 0.2576 0.1132 0.1228 0.1140 Uiso calc H(90E) 0.2566 0.1692 0.0647 0.2410 Uiso calc H(90F) 0.2792 0.2436 0.0928 0.2410 Uiso calc H(90G) 0.1219 0.1961 0.0656 0.2570 Uiso calc H(90H) 0.1497 0.2738 0.0880 0.2570 Uiso calc H(90I) 0.1849 0.3137 0.0288 0.2100 Uiso calc H(90J) 0.1573 0.2364 0.0066 0.2100 Uiso calc H(90K) 0.0368 0.2692 -0.0065 0.1090 Uiso calc H(90L) 0.0906 0.3376 -0.0184 0.1090 Uiso calc H(90M) 0.0530 0.3410 0.0243 0.1090 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr(1) 0.0307(5) 0.0258(6) 0.0400(5) -0.0016(4) 0.0085(4) -0.0023(4) Zr(2) 0.0298(5) 0.0263(6) 0.0344(5) 0.0015(4) 0.0081(3) 0.0042(3) O(110) 0.032(3) 0.028(4) 0.048(3) 0.007(3) 0.007(2) -0.001(3) O(210) 0.030(3) 0.033(4) 0.030(3) -0.005(3) 0.003(2) 0.003(2) N(17) 0.039(4) 0.030(5) 0.043(4) -0.011(4) 0.016(3) -0.005(3) N(27) 0.032(4) 0.029(5) 0.048(4) 0.003(3) 0.017(3) 0.006(3) C(11) 0.042(6) 0.031(6) 0.085(8) -0.002(5) 0.022(5) -0.014(6) C(12) 0.044(6) 0.110(11) 0.048(6) -0.039(7) 0.024(5) -0.022(7) C(13) 0.055(7) 0.047(8) 0.095(8) -0.013(6) 0.016(6) 0.037(6) C(14) 0.059(7) 0.059(8) 0.078(7) -0.044(7) 0.025(5) -0.030(6) C(15) 0.040(6) 0.057(8) 0.053(6) -0.018(6) -0.005(4) 0.011(5) C(18) 0.031(5) 0.026(5) 0.049(5) -0.005(4) 0.009(4) -0.006(4) C(19) 0.047(6) 0.035(6) 0.061(6) 0.010(5) 0.009(4) -0.002(5) C(21) 0.040(6) 0.038(6) 0.062(6) -0.003(5) 0.007(5) 0.004(5) C(22) 0.021(5) 0.048(7) 0.059(6) 0.010(5) -0.002(4) -0.004(5) C(23) 0.043(6) 0.034(6) 0.081(7) 0.014(5) 0.019(5) 0.024(5) C(24) 0.031(5) 0.035(7) 0.085(7) 0.011(5) -0.005(5) -0.021(5) C(25) 0.049(6) 0.069(8) 0.047(6) 0.032(6) 0.024(5) 0.010(5) C(28) 0.031(5) 0.024(5) 0.052(5) 0.002(4) 0.014(4) 0.007(4) C(29) 0.037(5) 0.033(6) 0.048(5) 0.000(4) 0.013(4) 0.005(4) C(111) 0.040(5) 0.031(6) 0.040(5) -0.003(5) 0.011(4) -0.011(4) C(112) 0.041(5) 0.024(5) 0.042(5) -0.010(4) 0.016(4) -0.002(4) C(113) 0.048(6) 0.019(5) 0.057(6) -0.001(4) 0.017(4) -0.008(4) C(114) 0.071(7) 0.039(6) 0.026(4) -0.011(5) 0.002(4) -0.003(4) C(115) 0.051(6) 0.027(6) 0.048(5) -0.004(5) 0.007(4) 0.002(4) C(116) 0.046(6) 0.031(6) 0.045(5) -0.002(5) 0.002(4) 0.003(4) C(121) 0.029(5) 0.017(5) 0.045(5) -0.003(4) 0.010(4) -0.001(4) C(122) 0.052(6) 0.033(6) 0.039(5) -0.004(5) 0.012(4) -0.011(4) C(123) 0.035(5) 0.037(6) 0.080(7) 0.000(5) 0.015(5) -0.015(5) C(124) 0.066(7) 0.038(6) 0.050(6) 0.005(5) -0.006(5) -0.010(4) C(125) 0.045(6) 0.040(7) 0.064(6) 0.006(5) 0.013(5) 0.000(5) C(126) 0.032(5) 0.025(5) 0.050(5) 0.008(4) -0.002(4) -0.004(4) C(141) 0.112(9) 0.049(8) 0.048(6) 0.010(7) 0.015(6) -0.003(5) C(142) 0.28(2) 0.26(2) 0.057(8) 0.17(2) 0.040(10) -0.048(11) C(143) 0.188(18) 0.27(3) 0.072(10) 0.036(18) -0.021(10) -0.078(12) C(144) 0.67(5) 0.122(17) 0.150(14) -0.04(2) 0.30(2) -0.015(12) C(161) 0.045(6) 0.029(6) 0.045(5) 0.003(5) 0.000(4) 0.001(4) C(162) 0.075(7) 0.048(7) 0.062(6) 0.027(6) 0.003(5) 0.001(5) C(163) 0.057(6) 0.028(6) 0.060(6) 0.010(5) -0.002(5) -0.008(4) C(164) 0.044(6) 0.047(7) 0.064(6) 0.014(5) -0.001(5) 0.003(5) C(171) 0.037(5) 0.046(7) 0.059(6) -0.008(5) 0.012(4) 0.004(5) C(172) 0.049(6) 0.060(8) 0.094(7) -0.016(6) 0.036(5) -0.001(6) C(173) 0.055(6) 0.026(6) 0.089(7) 0.006(5) 0.023(5) 0.010(5) C(174) 0.043(6) 0.057(8) 0.077(6) -0.013(5) 0.009(5) 0.008(5) C(180) 0.045(6) 0.050(7) 0.060(6) 0.002(5) -0.004(5) 0.013(5) C(181) 0.031(5) 0.050(7) 0.033(4) 0.003(5) 0.000(4) 0.011(4) C(182) 0.050(6) 0.063(8) 0.042(5) 0.007(6) 0.011(4) 0.003(5) C(183) 0.089(9) 0.062(8) 0.050(6) -0.005(7) 0.015(6) -0.021(5) C(184) 0.121(12) 0.057(9) 0.045(6) -0.022(8) 0.007(7) -0.004(5) C(185) 0.070(8) 0.083(11) 0.081(8) -0.032(8) -0.022(6) 0.009(7) C(186) 0.072(8) 0.045(7) 0.065(6) 0.009(6) 0.009(5) 0.012(5) C(191) 0.031(5) 0.045(7) 0.042(5) 0.010(5) 0.013(4) -0.001(4) C(192) 0.060(7) 0.048(8) 0.064(6) 0.012(6) 0.020(5) -0.002(5) C(193) 0.055(7) 0.055(8) 0.081(7) 0.007(6) -0.001(6) -0.016(6) C(194) 0.098(10) 0.086(11) 0.076(9) 0.032(9) -0.015(7) -0.030(8) C(195) 0.079(9) 0.130(14) 0.048(6) 0.043(9) 0.031(6) 0.013(7) C(196) 0.048(6) 0.052(7) 0.067(6) 0.001(5) 0.012(5) 0.015(5) C(211) 0.038(5) 0.043(6) 0.026(5) 0.008(5) 0.007(4) 0.004(4) C(212) 0.032(5) 0.037(6) 0.033(5) 0.001(4) 0.009(4) -0.001(4) C(213) 0.048(5) 0.052(7) 0.034(5) 0.002(5) 0.010(4) 0.007(4) C(214) 0.049(6) 0.044(6) 0.034(5) 0.005(5) 0.009(4) 0.008(4) C(215) 0.050(6) 0.041(6) 0.030(5) 0.007(5) 0.004(4) -0.003(4) C(216) 0.046(5) 0.030(6) 0.033(5) 0.001(5) 0.002(4) -0.003(4) C(221) 0.055(6) 0.029(5) 0.027(4) 0.000(5) 0.007(4) 0.012(4) C(222) 0.039(5) 0.043(6) 0.048(5) 0.004(5) 0.010(4) 0.010(4) C(223) 0.070(7) 0.028(6) 0.048(5) -0.008(5) 0.014(5) -0.009(4) C(224) 0.051(6) 0.044(7) 0.049(6) -0.010(5) 0.000(5) 0.005(5) C(225) 0.045(6) 0.032(6) 0.067(6) -0.023(5) -0.010(5) 0.021(5) C(226) 0.028(5) 0.048(7) 0.046(5) 0.002(4) 0.010(4) 0.011(4) C(241) 0.060(6) 0.071(9) 0.041(5) -0.010(6) 0.018(5) 0.002(5) C(242) 0.249(19) 0.100(12) 0.096(9) 0.071(13) 0.120(11) 0.042(8) C(243) 0.092(9) 0.123(13) 0.067(7) -0.006(9) -0.003(6) 0.025(7) C(244) 0.135(11) 0.064(9) 0.055(6) -0.017(8) 0.037(6) 0.019(6) C(261) 0.047(6) 0.037(6) 0.055(5) -0.011(5) 0.014(4) -0.008(4) C(262) 0.049(6) 0.039(6) 0.060(6) -0.012(5) 0.007(5) -0.009(5) C(263) 0.069(7) 0.043(7) 0.052(5) 0.005(6) 0.012(5) 0.002(5) C(264) 0.055(6) 0.070(8) 0.047(5) -0.013(6) -0.006(5) 0.002(5) C(271) 0.039(5) 0.031(6) 0.049(5) 0.000(4) 0.020(4) 0.002(4) C(272) 0.050(6) 0.053(7) 0.056(6) 0.015(5) 0.007(4) 0.005(5) C(273) 0.051(6) 0.039(7) 0.082(7) 0.011(5) 0.014(5) 0.000(5) C(274) 0.040(5) 0.052(7) 0.072(6) 0.004(5) 0.015(5) 0.000(5) C(280) 0.046(5) 0.046(7) 0.050(5) 0.003(5) 0.004(4) -0.010(4) C(281) 0.050(6) 0.051(7) 0.036(5) -0.010(5) 0.005(4) -0.007(4) C(282) 0.072(8) 0.080(10) 0.088(8) -0.036(7) -0.028(6) 0.030(7) C(283) 0.061(9) 0.146(17) 0.153(13) -0.042(10) -0.038(8) 0.063(12) C(284) 0.097(10) 0.092(12) 0.070(8) -0.006(9) -0.010(7) 0.023(7) C(285) 0.073(8) 0.075(9) 0.058(6) -0.012(7) 0.011(6) 0.010(6) C(286) 0.058(7) 0.052(8) 0.067(6) -0.002(6) 0.014(5) 0.003(5) C(291) 0.024(4) 0.017(5) 0.043(5) -0.013(4) 0.005(4) 0.000(4) C(292) 0.038(5) 0.051(7) 0.060(6) -0.006(5) 0.014(4) -0.001(5) C(293) 0.063(7) 0.062(9) 0.056(6) 0.010(6) 0.020(5) 0.013(6) C(294) 0.051(7) 0.079(10) 0.061(7) -0.014(7) 0.012(5) 0.016(6) C(295) 0.055(6) 0.031(6) 0.071(7) -0.007(5) -0.008(5) 0.015(5) C(296) 0.040(5) 0.044(7) 0.045(5) 0.001(5) -0.001(4) -0.008(5) # 10. MOLECULAR GEOMETRY _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_publ_flag Zr(1) O(110) 2.009(5) ? Zr(1) C(18) 2.186(8) ? Zr(1) N(17) 2.213(7) ? Zr(1) C(19) 2.319(8) ? Zr(1) C(11) 2.489(9) ? Zr(1) C(15) 2.524(8) ? Zr(1) C(14) 2.538(9) ? Zr(1) C(12) 2.542(9) ? Zr(1) C(13) 2.565(9) ? Zr(2) O(210) 1.998(4) ? Zr(2) N(27) 2.202(7) ? Zr(2) C(28) 2.223(8) ? Zr(2) C(29) 2.317(8) ? Zr(2) C(21) 2.494(8) ? Zr(2) C(23) 2.519(8) ? Zr(2) C(22) 2.522(8) ? Zr(2) C(24) 2.540(9) ? Zr(2) C(25) 2.550(8) ? O(110) C(111) 1.359(8) ? O(210) C(211) 1.346(8) ? N(17) C(18) 1.259(9) ? N(17) C(171) 1.496(11) ? N(27) C(28) 1.293(9) ? N(27) C(271) 1.504(10) ? C(11) C(12) 1.367(13) ? C(11) C(15) 1.374(12) ? C(12) C(13) 1.444(15) ? C(13) C(14) 1.397(13) ? C(14) C(15) 1.393(14) ? C(18) C(180) 1.518(11) ? C(19) C(191) 1.451(11) ? C(21) C(22) 1.385(11) ? C(21) C(25) 1.415(12) ? C(22) C(23) 1.367(12) ? C(23) C(24) 1.425(12) ? C(24) C(25) 1.372(13) ? C(28) C(280) 1.498(10) ? C(29) C(291) 1.471(10) ? C(111) C(116) 1.415(11) ? C(111) C(112) 1.416(11) ? C(112) C(113) 1.397(10) ? C(112) C(121) 1.471(10) ? C(113) C(114) 1.398(11) ? C(114) C(115) 1.378(12) ? C(114) C(141) 1.569(12) ? C(115) C(116) 1.380(11) ? C(116) C(161) 1.519(12) ? C(121) C(122) 1.379(11) ? C(121) C(126) 1.381(10) ? C(122) C(123) 1.355(11) ? C(123) C(124) 1.405(12) ? C(124) C(125) 1.371(12) ? C(125) C(126) 1.374(10) ? C(141) C(144) 1.492(19) ? C(141) C(142) 1.529(18) ? C(141) C(143) 1.585(19) ? C(161) C(163) 1.531(11) ? C(161) C(162) 1.535(11) ? C(161) C(164) 1.562(12) ? C(171) C(174) 1.516(11) ? C(171) C(172) 1.541(12) ? C(171) C(173) 1.581(12) ? C(180) C(181) 1.509(12) ? C(181) C(182) 1.384(12) ? C(181) C(186) 1.391(12) ? C(182) C(183) 1.382(13) ? C(183) C(184) 1.348(15) ? C(184) C(185) 1.417(16) ? C(185) C(186) 1.375(14) ? C(191) C(196) 1.393(11) ? C(191) C(192) 1.421(13) ? C(192) C(193) 1.396(13) ? C(193) C(194) 1.412(16) ? C(194) C(195) 1.374(17) ? C(195) C(196) 1.426(15) ? C(211) C(216) 1.383(10) ? C(211) C(212) 1.439(11) ? C(212) C(213) 1.425(10) ? C(212) C(221) 1.496(10) ? C(213) C(214) 1.377(11) ? C(214) C(215) 1.406(12) ? C(214) C(241) 1.547(11) ? C(215) C(216) 1.404(10) ? C(216) C(261) 1.513(12) ? C(221) C(226) 1.352(11) ? C(221) C(222) 1.402(11) ? C(222) C(223) 1.371(11) ? C(223) C(224) 1.386(12) ? C(224) C(225) 1.409(12) ? C(225) C(226) 1.399(11) ? C(241) C(244) 1.499(14) ? C(241) C(242) 1.511(15) ? C(241) C(243) 1.533(13) ? C(261) C(262) 1.550(12) ? C(261) C(263) 1.554(12) ? C(261) C(264) 1.567(11) ? C(271) C(273) 1.519(12) ? C(271) C(272) 1.528(10) ? C(271) C(274) 1.543(11) ? C(280) C(281) 1.478(12) ? C(281) C(282) 1.356(12) ? C(281) C(286) 1.364(13) ? C(282) C(283) 1.414(16) ? C(283) C(284) 1.347(18) ? C(284) C(285) 1.324(15) ? C(285) C(286) 1.392(14) ? C(291) C(296) 1.369(11) ? C(291) C(292) 1.414(11) ? C(292) C(293) 1.380(12) ? C(293) C(294) 1.312(14) ? C(294) C(295) 1.421(13) ? C(295) C(296) 1.379(12) ? C(901) C(902) 1.40(3) ? C(905) C(904) 1.33(3) ? C(904) C(903) 1.38(3) ? C(902) C(903) 1.42(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(110) Zr(1) C(18) 118.4(3) ? O(110) Zr(1) N(17) 93.9(2) ? C(18) Zr(1) N(17) 33.3(2) ? O(110) Zr(1) C(19) 101.2(2) ? C(18) Zr(1) C(19) 106.2(3) ? N(17) Zr(1) C(19) 91.0(3) ? O(110) Zr(1) C(11) 98.0(3) ? C(18) Zr(1) C(11) 99.8(3) ? N(17) Zr(1) C(11) 128.2(3) ? C(19) Zr(1) C(11) 134.7(3) ? O(110) Zr(1) C(15) 129.8(3) ? C(18) Zr(1) C(15) 84.2(3) ? N(17) Zr(1) C(15) 117.5(3) ? C(19) Zr(1) C(15) 115.3(4) ? C(11) Zr(1) C(15) 31.8(3) ? O(110) Zr(1) C(14) 133.9(3) ? C(18) Zr(1) C(14) 102.8(3) ? N(17) Zr(1) C(14) 131.9(3) ? C(19) Zr(1) C(14) 85.1(4) ? C(11) Zr(1) C(14) 52.9(3) ? C(15) Zr(1) C(14) 31.9(3) ? O(110) Zr(1) C(12) 82.6(3) ? C(18) Zr(1) C(12) 131.3(4) ? N(17) Zr(1) C(12) 156.8(4) ? C(19) Zr(1) C(12) 112.1(4) ? C(11) Zr(1) C(12) 31.5(3) ? C(15) Zr(1) C(12) 52.9(3) ? C(14) Zr(1) C(12) 53.6(3) ? O(110) Zr(1) C(13) 103.0(3) ? C(18) Zr(1) C(13) 134.0(3) ? N(17) Zr(1) C(13) 162.9(3) ? C(19) Zr(1) C(13) 83.0(4) ? C(11) Zr(1) C(13) 52.7(3) ? C(15) Zr(1) C(13) 52.5(3) ? C(14) Zr(1) C(13) 31.8(3) ? C(12) Zr(1) C(13) 32.8(3) ? O(210) Zr(2) N(27) 94.2(2) ? O(210) Zr(2) C(28) 119.1(3) ? N(27) Zr(2) C(28) 34.0(2) ? O(210) Zr(2) C(29) 100.5(2) ? N(27) Zr(2) C(29) 89.9(3) ? C(28) Zr(2) C(29) 106.0(3) ? O(210) Zr(2) C(21) 98.5(2) ? N(27) Zr(2) C(21) 128.6(3) ? C(28) Zr(2) C(21) 99.3(3) ? C(29) Zr(2) C(21) 135.2(3) ? O(210) Zr(2) C(23) 133.5(3) ? N(27) Zr(2) C(23) 132.1(3) ? C(28) Zr(2) C(23) 102.8(3) ? C(29) Zr(2) C(23) 85.4(3) ? C(21) Zr(2) C(23) 52.9(3) ? O(210) Zr(2) C(22) 130.5(3) ? N(27) Zr(2) C(22) 118.1(3) ? C(28) Zr(2) C(22) 84.1(3) ? C(29) Zr(2) C(22) 114.9(3) ? C(21) Zr(2) C(22) 32.1(3) ? C(23) Zr(2) C(22) 31.5(3) ? O(210) Zr(2) C(24) 101.4(3) ? N(27) Zr(2) C(24) 164.1(3) ? C(28) Zr(2) C(24) 134.6(3) ? C(29) Zr(2) C(24) 84.2(3) ? C(21) Zr(2) C(24) 52.3(3) ? C(23) Zr(2) C(24) 32.7(3) ? C(22) Zr(2) C(24) 52.6(3) ? O(210) Zr(2) C(25) 82.2(2) ? N(27) Zr(2) C(25) 158.2(3) ? C(28) Zr(2) C(25) 131.8(3) ? C(29) Zr(2) C(25) 111.9(4) ? C(21) Zr(2) C(25) 32.6(3) ? C(23) Zr(2) C(25) 53.7(3) ? C(22) Zr(2) C(25) 53.6(3) ? C(24) Zr(2) C(25) 31.3(3) ? C(111) O(110) Zr(1) 157.3(5) ? C(211) O(210) Zr(2) 158.5(5) ? C(18) N(17) C(171) 132.8(7) ? C(18) N(17) Zr(1) 72.2(5) ? C(171) N(17) Zr(1) 155.0(5) ? C(28) N(27) C(271) 130.5(7) ? C(28) N(27) Zr(2) 73.9(5) ? C(271) N(27) Zr(2) 155.6(5) ? C(12) C(11) C(15) 110.7(9) ? C(12) C(11) Zr(1) 76.4(5) ? C(15) C(11) Zr(1) 75.5(5) ? C(11) C(12) C(13) 106.0(8) ? C(11) C(12) Zr(1) 72.1(5) ? C(13) C(12) Zr(1) 74.5(5) ? C(14) C(13) C(12) 107.5(9) ? C(14) C(13) Zr(1) 73.0(5) ? C(12) C(13) Zr(1) 72.7(6) ? C(15) C(14) C(13) 107.7(9) ? C(15) C(14) Zr(1) 73.5(5) ? C(13) C(14) Zr(1) 75.2(5) ? C(11) C(15) C(14) 108.1(8) ? C(11) C(15) Zr(1) 72.7(5) ? C(14) C(15) Zr(1) 74.6(5) ? N(17) C(18) C(180) 130.4(8) ? N(17) C(18) Zr(1) 74.6(5) ? C(180) C(18) Zr(1) 155.0(6) ? C(191) C(19) Zr(1) 122.2(5) ? C(22) C(21) C(25) 109.5(9) ? C(22) C(21) Zr(2) 75.1(5) ? C(25) C(21) Zr(2) 75.9(5) ? C(23) C(22) C(21) 108.3(8) ? C(23) C(22) Zr(2) 74.1(5) ? C(21) C(22) Zr(2) 72.8(5) ? C(22) C(23) C(24) 106.9(8) ? C(22) C(23) Zr(2) 74.4(5) ? C(24) C(23) Zr(2) 74.4(5) ? C(25) C(24) C(23) 109.8(8) ? C(25) C(24) Zr(2) 74.8(5) ? C(23) C(24) Zr(2) 72.8(5) ? C(24) C(25) C(21) 105.4(7) ? C(24) C(25) Zr(2) 73.9(5) ? C(21) C(25) Zr(2) 71.5(5) ? N(27) C(28) C(280) 131.4(7) ? N(27) C(28) Zr(2) 72.1(5) ? C(280) C(28) Zr(2) 156.4(6) ? C(291) C(29) Zr(2) 123.0(5) ? O(110) C(111) C(116) 120.9(7) ? O(110) C(111) C(112) 118.1(7) ? C(116) C(111) C(112) 121.1(7) ? C(113) C(112) C(111) 118.2(7) ? C(113) C(112) C(121) 119.9(8) ? C(111) C(112) C(121) 121.9(7) ? C(112) C(113) C(114) 121.7(8) ? C(115) C(114) C(113) 117.5(7) ? C(115) C(114) C(141) 122.0(8) ? C(113) C(114) C(141) 120.5(9) ? C(114) C(115) C(116) 124.5(8) ? C(115) C(116) C(111) 116.9(8) ? C(115) C(116) C(161) 120.5(7) ? C(111) C(116) C(161) 122.7(7) ? C(122) C(121) C(126) 116.9(7) ? C(122) C(121) C(112) 120.9(7) ? C(126) C(121) C(112) 122.1(7) ? C(123) C(122) C(121) 122.0(8) ? C(122) C(123) C(124) 120.5(9) ? C(125) C(124) C(123) 118.0(8) ? C(124) C(125) C(126) 120.4(9) ? C(125) C(126) C(121) 122.0(8) ? C(144) C(141) C(142) 120.7(14) ? C(144) C(141) C(114) 108.2(9) ? C(142) C(141) C(114) 112.8(8) ? C(144) C(141) C(143) 110.9(14) ? C(142) C(141) C(143) 98.4(13) ? C(114) C(141) C(143) 104.5(9) ? C(116) C(161) C(163) 110.1(7) ? C(116) C(161) C(162) 112.2(7) ? C(163) C(161) C(162) 107.6(7) ? C(116) C(161) C(164) 110.4(7) ? C(163) C(161) C(164) 110.3(7) ? C(162) C(161) C(164) 106.1(7) ? N(17) C(171) C(174) 108.4(7) ? N(17) C(171) C(172) 110.3(7) ? C(174) C(171) C(172) 110.9(8) ? N(17) C(171) C(173) 108.1(7) ? C(174) C(171) C(173) 110.0(8) ? C(172) C(171) C(173) 109.1(7) ? C(181) C(180) C(18) 110.5(7) ? C(182) C(181) C(186) 118.7(9) ? C(182) C(181) C(180) 119.8(8) ? C(186) C(181) C(180) 121.4(9) ? C(183) C(182) C(181) 120.3(9) ? C(184) C(183) C(182) 121.8(11) ? C(183) C(184) C(185) 118.5(11) ? C(186) C(185) C(184) 120.0(11) ? C(185) C(186) C(181) 120.5(11) ? C(196) C(191) C(192) 114.8(8) ? C(196) C(191) C(19) 125.0(9) ? C(192) C(191) C(19) 120.3(8) ? C(193) C(192) C(191) 125.2(9) ? C(192) C(193) C(194) 118.6(11) ? C(195) C(194) C(193) 117.4(10) ? C(194) C(195) C(196) 123.5(11) ? C(191) C(196) C(195) 120.5(10) ? O(210) C(211) C(216) 122.8(8) ? O(210) C(211) C(212) 117.5(6) ? C(216) C(211) C(212) 119.6(7) ? C(213) C(212) C(211) 119.3(7) ? C(213) C(212) C(221) 117.3(7) ? C(211) C(212) C(221) 123.4(6) ? C(214) C(213) C(212) 121.3(8) ? C(213) C(214) C(215) 117.4(7) ? C(213) C(214) C(241) 122.0(8) ? C(215) C(214) C(241) 120.4(7) ? C(216) C(215) C(214) 123.7(7) ? C(211) C(216) C(215) 118.5(8) ? C(211) C(216) C(261) 121.9(7) ? C(215) C(216) C(261) 119.5(7) ? C(226) C(221) C(222) 118.4(8) ? C(226) C(221) C(212) 121.0(7) ? C(222) C(221) C(212) 120.6(8) ? C(223) C(222) C(221) 120.5(8) ? C(222) C(223) C(224) 121.6(8) ? C(223) C(224) C(225) 118.2(8) ? C(226) C(225) C(224) 119.0(9) ? C(221) C(226) C(225) 122.4(8) ? C(244) C(241) C(242) 111.6(10) ? C(244) C(241) C(243) 104.9(10) ? C(242) C(241) C(243) 111.2(10) ? C(244) C(241) C(214) 111.8(8) ? C(242) C(241) C(214) 108.1(9) ? C(243) C(241) C(214) 109.3(8) ? C(216) C(261) C(262) 110.0(7) ? C(216) C(261) C(263) 109.0(7) ? C(262) C(261) C(263) 110.7(7) ? C(216) C(261) C(264) 114.2(7) ? C(262) C(261) C(264) 106.5(7) ? C(263) C(261) C(264) 106.4(7) ? N(27) C(271) C(273) 112.1(7) ? N(27) C(271) C(272) 106.8(6) ? C(273) C(271) C(272) 110.4(7) ? N(27) C(271) C(274) 108.7(7) ? C(273) C(271) C(274) 110.8(7) ? C(272) C(271) C(274) 107.9(7) ? C(281) C(280) C(28) 112.2(7) ? C(282) C(281) C(286) 116.2(9) ? C(282) C(281) C(280) 120.8(9) ? C(286) C(281) C(280) 123.0(8) ? C(281) C(282) C(283) 120.3(11) ? C(284) C(283) C(282) 121.0(11) ? C(285) C(284) C(283) 119.8(12) ? C(284) C(285) C(286) 119.1(11) ? C(281) C(286) C(285) 123.6(10) ? C(296) C(291) C(292) 115.4(7) ? C(296) C(291) C(29) 122.1(7) ? C(292) C(291) C(29) 122.4(8) ? C(293) C(292) C(291) 122.3(10) ? C(294) C(293) C(292) 121.6(10) ? C(293) C(294) C(295) 118.4(9) ? C(296) C(295) C(294) 120.2(10) ? C(291) C(296) C(295) 122.2(8) ? C(905) C(904) C(903) 135(3) ? C(901) C(902) C(903) 111(3) ? C(904) C(903) C(902) 127(3) ?