# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Matthew Jones' _publ_contact_author_email MJ205@BATH.AC.UK _publ_section_title ; Novel Ti(IV) and Zr(IV) complexes and their application in the ring opening polymerisation of cyclic esters ; loop_ _publ_author_name 'Matthew Jones' 'Gabriele Kociok-Kohn' 'Mary Mahon' 'Emma Whitelaw' # Attachment 'cif.CIF' data_Ti(1)(OiPr) _database_code_depnum_ccdc_archive 'CCDC 736070' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H55 N O4 Ti' _chemical_formula_weight 649.74 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' Ti Ti 0.2776 0.4457 '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 10.8850(4) _cell_length_b 11.8990(5) _cell_length_c 14.7140(5) _cell_angle_alpha 82.401(3) _cell_angle_beta 80.713(2) _cell_angle_gamma 76.7430(10) _cell_volume 1821.65(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31087 _cell_measurement_theta_min 3.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17476 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 25.24 _reflns_number_total 17478 _reflns_number_gt 14110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.0955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.020(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17478 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.90776(4) 0.06667(4) 0.69193(3) 0.02643(14) Uani 1 1 d . . . O1 O 1.05952(15) 0.07458(14) 0.71590(11) 0.0334(4) Uani 1 1 d . . . O2 O 0.84464(14) 0.22381(13) 0.66445(11) 0.0296(4) Uani 1 1 d . . . O3 O 0.95775(15) -0.03832(14) 0.60184(11) 0.0321(4) Uani 1 1 d . . . O4 O 0.84993(14) -0.01075(13) 0.79993(10) 0.0287(4) Uani 1 1 d . . . N1 N 0.71346(17) 0.05109(15) 0.65289(12) 0.0248(4) Uani 1 1 d . . . C1 C 1.1822(2) 0.0454(2) 0.74289(17) 0.0353(6) Uani 1 1 d . . . H1 H 1.1780 -0.0024 0.8041 0.042 Uiso 1 1 calc R . . C2 C 1.2244(3) 0.1540(3) 0.7540(2) 0.0508(7) Uani 1 1 d . . . H2A H 1.2410 0.1964 0.6932 0.076 Uiso 1 1 calc R . . H2B H 1.3025 0.1333 0.7832 0.076 Uiso 1 1 calc R . . H2C H 1.1573 0.2030 0.7930 0.076 Uiso 1 1 calc R . . C3 C 1.2711(2) -0.0276(3) 0.6726(2) 0.0447(7) Uani 1 1 d . . . H3A H 1.2325 -0.0906 0.6617 0.067 Uiso 1 1 calc R . . H3B H 1.3523 -0.0606 0.6962 0.067 Uiso 1 1 calc R . . H3C H 1.2859 0.0209 0.6145 0.067 Uiso 1 1 calc R . . C4 C 0.7303(2) 0.29964(19) 0.66036(15) 0.0266(5) Uani 1 1 d . . . C5 C 0.7068(2) 0.40939(19) 0.69384(15) 0.0260(5) Uani 1 1 d . . . C6 C 0.5855(2) 0.4786(2) 0.68965(15) 0.0269(5) Uani 1 1 d . . . H6 H 0.5675 0.5527 0.7122 0.032 Uiso 1 1 calc R . . C7 C 0.4878(2) 0.44562(19) 0.65400(15) 0.0267(5) Uani 1 1 d . . . C8 C 0.5175(2) 0.3372(2) 0.62031(15) 0.0272(5) Uani 1 1 d . . . H8 H 0.4542 0.3118 0.5956 0.033 Uiso 1 1 calc R . . C9 C 0.6374(2) 0.26544(19) 0.62197(15) 0.0263(5) Uani 1 1 d . . . C10 C 0.6702(2) 0.15007(19) 0.58263(15) 0.0277(5) Uani 1 1 d . . . H10A H 0.5944 0.1374 0.5595 0.033 Uiso 1 1 calc R . . H10B H 0.7385 0.1515 0.5295 0.033 Uiso 1 1 calc R . . C11 C 0.8116(2) 0.4515(2) 0.73041(16) 0.0298(5) Uani 1 1 d . . . C12 C 0.7656(3) 0.5747(2) 0.7589(2) 0.0419(6) Uani 1 1 d . . . H12A H 0.7373 0.6276 0.7058 0.063 Uiso 1 1 calc R . . H12B H 0.8355 0.5991 0.7799 0.063 Uiso 1 1 calc R . . H12C H 0.6944 0.5765 0.8092 0.063 Uiso 1 1 calc R . . C13 C 0.9271(2) 0.4501(2) 0.65402(18) 0.0397(6) Uani 1 1 d . . . H13A H 0.8996 0.4979 0.5984 0.059 Uiso 1 1 calc R . . H13B H 0.9633 0.3702 0.6394 0.059 Uiso 1 1 calc R . . H13C H 0.9918 0.4814 0.6758 0.059 Uiso 1 1 calc R . . C14 C 0.8563(3) 0.3717(2) 0.81559(17) 0.0398(6) Uani 1 1 d . . . H14A H 0.9254 0.3981 0.8359 0.060 Uiso 1 1 calc R . . H14B H 0.8869 0.2920 0.7992 0.060 Uiso 1 1 calc R . . H14C H 0.7849 0.3744 0.8658 0.060 Uiso 1 1 calc R . . C15 C 0.3526(2) 0.5208(2) 0.65911(16) 0.0296(5) Uani 1 1 d . . . C16 C 0.3529(3) 0.6507(2) 0.6494(2) 0.0417(6) Uani 1 1 d . . . H16A H 0.3874 0.6686 0.7020 0.062 Uiso 1 1 calc R . . H16B H 0.2656 0.6958 0.6483 0.062 Uiso 1 1 calc R . . H16C H 0.4059 0.6705 0.5918 0.062 Uiso 1 1 calc R . . C17 C 0.2829(2) 0.4994(2) 0.58249(18) 0.0401(6) Uani 1 1 d . . . H17A H 0.3341 0.5110 0.5222 0.060 Uiso 1 1 calc R . . H17B H 0.2002 0.5538 0.5838 0.060 Uiso 1 1 calc R . . H17C H 0.2698 0.4196 0.5925 0.060 Uiso 1 1 calc R . . C18 C 0.2786(3) 0.4883(2) 0.75332(18) 0.0428(6) Uani 1 1 d . . . H18A H 0.2744 0.4063 0.7585 0.064 Uiso 1 1 calc R . . H18B H 0.1921 0.5363 0.7585 0.064 Uiso 1 1 calc R . . H18C H 0.3221 0.5016 0.8030 0.064 Uiso 1 1 calc R . . C19 C 0.8745(2) -0.09671(19) 0.58046(15) 0.0277(5) Uani 1 1 d . . . C20 C 0.9151(2) -0.1947(2) 0.53264(16) 0.0342(6) Uani 1 1 d . . . H20 H 1.0032 -0.2221 0.5125 0.041 Uiso 1 1 calc R . . C21 C 0.8256(2) -0.2521(2) 0.51470(16) 0.0363(6) Uani 1 1 d . . . H21 H 0.8531 -0.3193 0.4822 0.044 Uiso 1 1 calc R . . C22 C 0.6969(2) -0.2133(2) 0.54322(17) 0.0355(6) Uani 1 1 d . . . H22 H 0.6368 -0.2541 0.5311 0.043 Uiso 1 1 calc R . . C23 C 0.6562(2) -0.1141(2) 0.58977(16) 0.0312(5) Uani 1 1 d . . . H23 H 0.5680 -0.0863 0.6089 0.037 Uiso 1 1 calc R . . C24 C 0.7445(2) -0.05615(19) 0.60803(15) 0.0262(5) Uani 1 1 d . . . C25 C 0.7646(2) -0.07805(19) 0.83547(15) 0.0252(5) Uani 1 1 d . . . C26 C 0.7958(2) -0.1738(2) 0.90022(15) 0.0269(5) Uani 1 1 d . . . C27 C 0.6966(2) -0.2271(2) 0.94284(15) 0.0283(5) Uani 1 1 d . . . H27 H 0.7152 -0.2904 0.9887 0.034 Uiso 1 1 calc R . . C28 C 0.5721(2) -0.1931(2) 0.92231(15) 0.0279(5) Uani 1 1 d . . . C29 C 0.5496(2) -0.1051(2) 0.85081(15) 0.0280(5) Uani 1 1 d . . . H29 H 0.4676 -0.0838 0.8313 0.034 Uiso 1 1 calc R . . C30 C 0.6433(2) -0.0479(2) 0.80747(15) 0.0260(5) Uani 1 1 d . . . C31 C 0.6140(2) 0.0527(2) 0.73540(15) 0.0277(5) Uani 1 1 d . . . H31A H 0.5318 0.0526 0.7149 0.033 Uiso 1 1 calc R . . H31B H 0.6038 0.1257 0.7639 0.033 Uiso 1 1 calc R . . C32 C 0.9330(2) -0.2179(2) 0.92322(16) 0.0318(5) Uani 1 1 d . . . C33 C 1.0266(2) -0.2405(2) 0.83413(18) 0.0394(6) Uani 1 1 d . . . H33A H 1.1122 -0.2747 0.8501 0.059 Uiso 1 1 calc R . . H33B H 1.0277 -0.1672 0.7952 0.059 Uiso 1 1 calc R . . H33C H 0.9995 -0.2942 0.8003 0.059 Uiso 1 1 calc R . . C34 C 0.9694(3) -0.1270(2) 0.97285(19) 0.0411(6) Uani 1 1 d . . . H34A H 0.9111 -0.1143 1.0305 0.062 Uiso 1 1 calc R . . H34B H 0.9635 -0.0539 0.9327 0.062 Uiso 1 1 calc R . . H34C H 1.0568 -0.1548 0.9871 0.062 Uiso 1 1 calc R . . C35 C 0.9469(3) -0.3320(2) 0.9858(2) 0.0457(7) Uani 1 1 d . . . H35A H 1.0362 -0.3602 0.9954 0.069 Uiso 1 1 calc R . . H35B H 0.9193 -0.3897 0.9566 0.069 Uiso 1 1 calc R . . H35C H 0.8940 -0.3193 1.0456 0.069 Uiso 1 1 calc R . . C36 C 0.4627(2) -0.2460(2) 0.97651(16) 0.0339(5) Uani 1 1 d . . . C37 C 0.3605(3) -0.1481(3) 1.0194(2) 0.0543(8) Uani 1 1 d . . . H37A H 0.3274 -0.0911 0.9700 0.081 Uiso 1 1 calc R . . H37B H 0.3982 -0.1103 1.0598 0.081 Uiso 1 1 calc R . . H37C H 0.2907 -0.1807 1.0556 0.081 Uiso 1 1 calc R . . C38 C 0.4020(3) -0.3009(3) 0.9112(2) 0.0497(7) Uani 1 1 d . . . H38A H 0.3732 -0.2424 0.8613 0.075 Uiso 1 1 calc R . . H38B H 0.3292 -0.3302 0.9458 0.075 Uiso 1 1 calc R . . H38C H 0.4651 -0.3652 0.8846 0.075 Uiso 1 1 calc R . . C39 C 0.5069(3) -0.3390(3) 1.0532(2) 0.0678(10) Uani 1 1 d . . . H39A H 0.4347 -0.3719 1.0846 0.102 Uiso 1 1 calc R . . H39B H 0.5408 -0.3042 1.0980 0.102 Uiso 1 1 calc R . . H39C H 0.5737 -0.4005 1.0264 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0205(2) 0.0266(2) 0.0321(2) -0.00228(16) -0.00471(16) -0.00451(16) O1 0.0206(8) 0.0337(9) 0.0454(10) -0.0031(7) -0.0071(7) -0.0034(7) O2 0.0217(8) 0.0255(8) 0.0405(9) -0.0014(7) -0.0066(7) -0.0025(7) O3 0.0235(8) 0.0335(9) 0.0381(9) -0.0079(7) 0.0003(7) -0.0043(7) O4 0.0248(8) 0.0302(9) 0.0318(8) -0.0007(7) -0.0071(6) -0.0064(7) N1 0.0243(10) 0.0220(9) 0.0269(9) -0.0021(7) -0.0036(7) -0.0022(8) C1 0.0247(12) 0.0407(15) 0.0410(14) -0.0032(11) -0.0084(10) -0.0057(11) C2 0.0334(15) 0.0580(19) 0.0674(19) -0.0241(15) -0.0052(13) -0.0137(13) C3 0.0288(14) 0.0477(17) 0.0567(17) -0.0161(13) -0.0057(12) -0.0002(12) C4 0.0238(12) 0.0264(12) 0.0280(11) 0.0004(9) -0.0027(9) -0.0043(9) C5 0.0256(12) 0.0276(12) 0.0254(11) -0.0015(9) -0.0054(9) -0.0064(9) C6 0.0282(12) 0.0270(12) 0.0265(11) -0.0051(9) -0.0023(9) -0.0075(10) C7 0.0257(12) 0.0272(12) 0.0264(11) -0.0002(9) -0.0042(9) -0.0051(9) C8 0.0255(12) 0.0291(12) 0.0282(11) -0.0021(9) -0.0071(9) -0.0060(10) C9 0.0289(12) 0.0245(12) 0.0256(11) 0.0008(9) -0.0060(9) -0.0064(9) C10 0.0291(12) 0.0259(12) 0.0279(11) -0.0018(9) -0.0084(9) -0.0031(10) C11 0.0239(12) 0.0316(13) 0.0351(12) -0.0037(10) -0.0054(9) -0.0071(10) C12 0.0330(14) 0.0455(16) 0.0528(16) -0.0189(12) -0.0087(12) -0.0097(12) C13 0.0346(14) 0.0407(15) 0.0461(15) -0.0085(12) 0.0012(11) -0.0154(12) C14 0.0363(14) 0.0494(16) 0.0379(14) -0.0041(12) -0.0135(11) -0.0119(12) C15 0.0253(12) 0.0278(12) 0.0342(12) -0.0041(9) -0.0046(9) -0.0017(10) C16 0.0366(15) 0.0329(14) 0.0561(16) -0.0052(12) -0.0155(12) -0.0016(11) C17 0.0293(13) 0.0421(15) 0.0486(15) -0.0121(12) -0.0125(11) 0.0021(11) C18 0.0335(14) 0.0456(16) 0.0439(15) -0.0035(12) -0.0007(11) -0.0012(12) C19 0.0271(12) 0.0264(12) 0.0283(12) -0.0013(9) -0.0024(9) -0.0047(10) C20 0.0321(13) 0.0338(14) 0.0341(13) -0.0067(10) 0.0004(10) -0.0030(11) C21 0.0427(15) 0.0322(14) 0.0340(13) -0.0089(10) -0.0006(11) -0.0079(11) C22 0.0368(14) 0.0329(14) 0.0389(13) -0.0079(10) -0.0044(11) -0.0100(11) C23 0.0268(12) 0.0329(13) 0.0339(12) -0.0041(10) -0.0039(10) -0.0061(10) C24 0.0269(12) 0.0246(12) 0.0264(11) -0.0012(9) -0.0049(9) -0.0040(9) C25 0.0233(11) 0.0258(12) 0.0272(11) -0.0060(9) -0.0026(9) -0.0053(9) C26 0.0277(12) 0.0286(12) 0.0261(11) -0.0058(9) -0.0074(9) -0.0047(10) C27 0.0329(13) 0.0251(12) 0.0267(11) -0.0020(9) -0.0065(9) -0.0044(10) C28 0.0283(12) 0.0299(12) 0.0264(11) -0.0057(9) -0.0020(9) -0.0075(10) C29 0.0223(11) 0.0324(13) 0.0298(12) -0.0054(10) -0.0050(9) -0.0046(10) C30 0.0236(11) 0.0285(12) 0.0253(11) -0.0055(9) -0.0044(9) -0.0021(9) C31 0.0264(12) 0.0267(12) 0.0294(12) -0.0042(9) -0.0027(9) -0.0040(9) C32 0.0282(13) 0.0321(13) 0.0371(13) -0.0024(10) -0.0132(10) -0.0047(10) C33 0.0264(13) 0.0392(15) 0.0509(15) -0.0076(12) -0.0102(11) 0.0013(11) C34 0.0391(15) 0.0419(15) 0.0479(15) -0.0062(12) -0.0200(12) -0.0090(12) C35 0.0388(15) 0.0408(16) 0.0589(17) 0.0077(13) -0.0237(13) -0.0066(12) C36 0.0312(13) 0.0365(14) 0.0338(13) -0.0020(10) -0.0016(10) -0.0095(11) C37 0.0495(18) 0.059(2) 0.0539(17) -0.0155(14) 0.0168(14) -0.0218(15) C38 0.0441(16) 0.0556(18) 0.0550(17) -0.0101(14) 0.0017(13) -0.0250(14) C39 0.0477(19) 0.083(3) 0.070(2) 0.0353(19) -0.0129(16) -0.0293(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.7692(16) . ? Ti1 O4 1.8237(15) . ? Ti1 O2 1.8527(16) . ? Ti1 O3 1.8728(17) . ? Ti1 N1 2.3319(19) . ? O1 C1 1.408(3) . ? O2 C4 1.365(3) . ? O3 C19 1.357(3) . ? O4 C25 1.361(3) . ? N1 C24 1.460(3) . ? N1 C31 1.490(3) . ? N1 C10 1.503(3) . ? C1 C2 1.504(4) . ? C1 C3 1.513(4) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.393(3) . ? C4 C5 1.411(3) . ? C5 C6 1.393(3) . ? C5 C11 1.541(3) . ? C6 C7 1.410(3) . ? C6 H6 0.9500 . ? C7 C8 1.393(3) . ? C7 C15 1.533(3) . ? C8 C9 1.388(3) . ? C8 H8 0.9500 . ? C9 C10 1.505(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.527(3) . ? C11 C14 1.542(3) . ? C11 C13 1.544(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.534(3) . ? C15 C17 1.534(3) . ? C15 C18 1.537(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.390(3) . ? C19 C24 1.397(3) . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C21 C22 1.385(4) . ? C21 H21 0.9500 . ? C22 C23 1.391(3) . ? C22 H22 0.9500 . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C25 C30 1.400(3) . ? C25 C26 1.400(3) . ? C26 C27 1.397(3) . ? C26 C32 1.542(3) . ? C27 C28 1.393(3) . ? C27 H27 0.9500 . ? C28 C29 1.392(3) . ? C28 C36 1.535(3) . ? C29 C30 1.379(3) . ? C29 H29 0.9500 . ? C30 C31 1.503(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C35 1.528(3) . ? C32 C34 1.536(4) . ? C32 C33 1.538(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C39 1.527(4) . ? C36 C38 1.534(4) . ? C36 C37 1.538(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O4 100.07(7) . . ? O1 Ti1 O2 98.29(7) . . ? O4 Ti1 O2 121.20(7) . . ? O1 Ti1 O3 99.47(8) . . ? O4 Ti1 O3 108.07(7) . . ? O2 Ti1 O3 123.07(7) . . ? O1 Ti1 N1 176.75(8) . . ? O4 Ti1 N1 81.75(7) . . ? O2 Ti1 N1 82.94(7) . . ? O3 Ti1 N1 77.38(7) . . ? C1 O1 Ti1 162.87(16) . . ? C4 O2 Ti1 139.26(15) . . ? C19 O3 Ti1 120.88(14) . . ? C25 O4 Ti1 141.49(14) . . ? C24 N1 C31 114.40(17) . . ? C24 N1 C10 108.19(16) . . ? C31 N1 C10 109.35(17) . . ? C24 N1 Ti1 103.82(13) . . ? C31 N1 Ti1 111.64(13) . . ? C10 N1 Ti1 109.22(13) . . ? O1 C1 C2 109.7(2) . . ? O1 C1 C3 108.6(2) . . ? C2 C1 C3 113.3(2) . . ? O1 C1 H1 108.4 . . ? C2 C1 H1 108.4 . . ? C3 C1 H1 108.4 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C9 118.0(2) . . ? O2 C4 C5 121.1(2) . . ? C9 C4 C5 121.0(2) . . ? C6 C5 C4 116.6(2) . . ? C6 C5 C11 121.9(2) . . ? C4 C5 C11 121.47(19) . . ? C5 C6 C7 124.0(2) . . ? C5 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? C8 C7 C6 116.7(2) . . ? C8 C7 C15 121.4(2) . . ? C6 C7 C15 121.7(2) . . ? C9 C8 C7 121.5(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C4 120.1(2) . . ? C8 C9 C10 121.3(2) . . ? C4 C9 C10 118.6(2) . . ? N1 C10 C9 112.34(17) . . ? N1 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? N1 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C5 111.97(19) . . ? C12 C11 C14 107.7(2) . . ? C5 C11 C14 110.93(19) . . ? C12 C11 C13 108.4(2) . . ? C5 C11 C13 109.33(19) . . ? C14 C11 C13 108.4(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C15 C16 111.9(2) . . ? C7 C15 C17 111.4(2) . . ? C16 C15 C17 107.7(2) . . ? C7 C15 C18 108.07(18) . . ? C16 C15 C18 109.2(2) . . ? C17 C15 C18 108.6(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C19 C20 121.9(2) . . ? O3 C19 C24 118.3(2) . . ? C20 C19 C24 119.8(2) . . ? C21 C20 C19 119.1(2) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 121.2(2) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.6(2) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 119.8(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.5(2) . . ? C23 C24 N1 124.9(2) . . ? C19 C24 N1 114.56(19) . . ? O4 C25 C30 118.50(19) . . ? O4 C25 C26 120.95(19) . . ? C30 C25 C26 120.5(2) . . ? C27 C26 C25 116.7(2) . . ? C27 C26 C32 121.8(2) . . ? C25 C26 C32 121.5(2) . . ? C28 C27 C26 124.0(2) . . ? C28 C27 H27 118.0 . . ? C26 C27 H27 118.0 . . ? C29 C28 C27 116.6(2) . . ? C29 C28 C36 120.7(2) . . ? C27 C28 C36 122.7(2) . . ? C30 C29 C28 121.7(2) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C25 119.8(2) . . ? C29 C30 C31 120.7(2) . . ? C25 C30 C31 119.3(2) . . ? N1 C31 C30 113.84(18) . . ? N1 C31 H31A 108.8 . . ? C30 C31 H31A 108.8 . . ? N1 C31 H31B 108.8 . . ? C30 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C35 C32 C34 108.5(2) . . ? C35 C32 C33 107.1(2) . . ? C34 C32 C33 109.7(2) . . ? C35 C32 C26 111.7(2) . . ? C34 C32 C26 109.5(2) . . ? C33 C32 C26 110.31(18) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C38 108.4(2) . . ? C39 C36 C28 112.3(2) . . ? C38 C36 C28 110.3(2) . . ? C39 C36 C37 109.2(2) . . ? C38 C36 C37 108.3(2) . . ? C28 C36 C37 108.3(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ti1 O1 C1 49.1(6) . . . . ? O2 Ti1 O1 C1 172.9(5) . . . . ? O3 Ti1 O1 C1 -61.4(5) . . . . ? N1 Ti1 O1 C1 -74.9(15) . . . . ? O1 Ti1 O2 C4 -159.4(2) . . . . ? O4 Ti1 O2 C4 -52.3(2) . . . . ? O3 Ti1 O2 C4 93.5(2) . . . . ? N1 Ti1 O2 C4 23.6(2) . . . . ? O1 Ti1 O3 C19 161.31(16) . . . . ? O4 Ti1 O3 C19 57.38(17) . . . . ? O2 Ti1 O3 C19 -92.24(17) . . . . ? N1 Ti1 O3 C19 -19.46(15) . . . . ? O1 Ti1 O4 C25 -157.6(2) . . . . ? O2 Ti1 O4 C25 96.2(2) . . . . ? O3 Ti1 O4 C25 -54.1(2) . . . . ? N1 Ti1 O4 C25 19.7(2) . . . . ? O1 Ti1 N1 C24 32.1(13) . . . . ? O4 Ti1 N1 C24 -92.20(13) . . . . ? O2 Ti1 N1 C24 144.75(13) . . . . ? O3 Ti1 N1 C24 18.51(12) . . . . ? O1 Ti1 N1 C31 155.9(12) . . . . ? O4 Ti1 N1 C31 31.52(14) . . . . ? O2 Ti1 N1 C31 -91.53(14) . . . . ? O3 Ti1 N1 C31 142.24(15) . . . . ? O1 Ti1 N1 C10 -83.1(13) . . . . ? O4 Ti1 N1 C10 152.57(14) . . . . ? O2 Ti1 N1 C10 29.52(14) . . . . ? O3 Ti1 N1 C10 -96.72(14) . . . . ? Ti1 O1 C1 C2 -165.1(5) . . . . ? Ti1 O1 C1 C3 70.6(6) . . . . ? Ti1 O2 C4 C9 -41.5(3) . . . . ? Ti1 O2 C4 C5 138.6(2) . . . . ? O2 C4 C5 C6 -177.69(19) . . . . ? C9 C4 C5 C6 2.4(3) . . . . ? O2 C4 C5 C11 4.1(3) . . . . ? C9 C4 C5 C11 -175.8(2) . . . . ? C4 C5 C6 C7 -0.4(3) . . . . ? C11 C5 C6 C7 177.8(2) . . . . ? C5 C6 C7 C8 -0.8(3) . . . . ? C5 C6 C7 C15 174.4(2) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C15 C7 C8 C9 -175.2(2) . . . . ? C7 C8 C9 C4 1.9(3) . . . . ? C7 C8 C9 C10 -178.0(2) . . . . ? O2 C4 C9 C8 176.9(2) . . . . ? C5 C4 C9 C8 -3.2(3) . . . . ? O2 C4 C9 C10 -3.2(3) . . . . ? C5 C4 C9 C10 176.70(19) . . . . ? C24 N1 C10 C9 -179.24(18) . . . . ? C31 N1 C10 C9 55.6(2) . . . . ? Ti1 N1 C10 C9 -66.9(2) . . . . ? C8 C9 C10 N1 -122.6(2) . . . . ? C4 C9 C10 N1 57.5(3) . . . . ? C6 C5 C11 C12 -0.6(3) . . . . ? C4 C5 C11 C12 177.5(2) . . . . ? C6 C5 C11 C14 119.7(2) . . . . ? C4 C5 C11 C14 -62.2(3) . . . . ? C6 C5 C11 C13 -120.8(2) . . . . ? C4 C5 C11 C13 57.4(3) . . . . ? C8 C7 C15 C16 -150.9(2) . . . . ? C6 C7 C15 C16 34.1(3) . . . . ? C8 C7 C15 C17 -30.3(3) . . . . ? C6 C7 C15 C17 154.7(2) . . . . ? C8 C7 C15 C18 88.9(3) . . . . ? C6 C7 C15 C18 -86.1(3) . . . . ? Ti1 O3 C19 C20 -163.34(17) . . . . ? Ti1 O3 C19 C24 16.5(3) . . . . ? O3 C19 C20 C21 178.5(2) . . . . ? C24 C19 C20 C21 -1.3(3) . . . . ? C19 C20 C21 C22 0.2(4) . . . . ? C20 C21 C22 C23 0.8(4) . . . . ? C21 C22 C23 C24 -0.8(4) . . . . ? C22 C23 C24 C19 -0.3(3) . . . . ? C22 C23 C24 N1 177.4(2) . . . . ? O3 C19 C24 C23 -178.5(2) . . . . ? C20 C19 C24 C23 1.3(3) . . . . ? O3 C19 C24 N1 3.5(3) . . . . ? C20 C19 C24 N1 -176.62(19) . . . . ? C31 N1 C24 C23 44.2(3) . . . . ? C10 N1 C24 C23 -77.9(3) . . . . ? Ti1 N1 C24 C23 166.10(19) . . . . ? C31 N1 C24 C19 -137.98(19) . . . . ? C10 N1 C24 C19 99.9(2) . . . . ? Ti1 N1 C24 C19 -16.1(2) . . . . ? Ti1 O4 C25 C30 -41.2(3) . . . . ? Ti1 O4 C25 C26 140.3(2) . . . . ? O4 C25 C26 C27 170.81(19) . . . . ? C30 C25 C26 C27 -7.7(3) . . . . ? O4 C25 C26 C32 -9.2(3) . . . . ? C30 C25 C26 C32 172.3(2) . . . . ? C25 C26 C27 C28 2.3(3) . . . . ? C32 C26 C27 C28 -177.7(2) . . . . ? C26 C27 C28 C29 4.0(3) . . . . ? C26 C27 C28 C36 -174.2(2) . . . . ? C27 C28 C29 C30 -5.1(3) . . . . ? C36 C28 C29 C30 173.2(2) . . . . ? C28 C29 C30 C25 -0.1(3) . . . . ? C28 C29 C30 C31 -175.4(2) . . . . ? O4 C25 C30 C29 -171.7(2) . . . . ? C26 C25 C30 C29 6.8(3) . . . . ? O4 C25 C30 C31 3.6(3) . . . . ? C26 C25 C30 C31 -177.9(2) . . . . ? C24 N1 C31 C30 54.3(2) . . . . ? C10 N1 C31 C30 175.84(19) . . . . ? Ti1 N1 C31 C30 -63.2(2) . . . . ? C29 C30 C31 N1 -137.3(2) . . . . ? C25 C30 C31 N1 47.5(3) . . . . ? C27 C26 C32 C35 7.5(3) . . . . ? C25 C26 C32 C35 -172.5(2) . . . . ? C27 C26 C32 C34 -112.7(2) . . . . ? C25 C26 C32 C34 67.3(3) . . . . ? C27 C26 C32 C33 126.6(2) . . . . ? C25 C26 C32 C33 -53.4(3) . . . . ? C29 C28 C36 C39 -178.7(3) . . . . ? C27 C28 C36 C39 -0.5(4) . . . . ? C29 C28 C36 C38 60.4(3) . . . . ? C27 C28 C36 C38 -121.5(3) . . . . ? C29 C28 C36 C37 -57.9(3) . . . . ? C27 C28 C36 C37 120.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.814 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.076 #===END data_Ti(2)(OiPr) _database_code_depnum_ccdc_archive 'CCDC 736071' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H57 N O4 Ti' _chemical_formula_weight 663.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9500(5) _cell_length_b 14.0800(6) _cell_length_c 14.2790(8) _cell_angle_alpha 66.472(2) _cell_angle_beta 74.247(2) _cell_angle_gamma 86.724(2) _cell_volume 1939.37(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28883 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.258 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17062 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6752 _reflns_number_gt 4962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+1.8445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6752 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.76119(5) 0.13447(4) 0.72152(4) 0.02823(17) Uani 1 1 d . . . O1 O 0.92461(19) 0.13744(19) 0.71448(18) 0.0427(6) Uani 1 1 d . . . N1 N 0.5478(2) 0.10705(16) 0.73646(17) 0.0236(5) Uani 1 1 d . . . C1 C 1.0507(4) 0.1109(5) 0.7129(4) 0.0922(18) Uani 1 1 d . . . H1 H 1.0473 0.0366 0.7230 0.111 Uiso 1 1 calc R . . O2 O 0.69911(17) 0.13803(14) 0.85465(15) 0.0278(4) Uani 1 1 d . . . C2 C 1.0797(4) 0.1037(6) 0.8088(4) 0.105(2) Uani 1 1 d . . . H2A H 1.1596 0.0695 0.8138 0.158 Uiso 1 1 calc R . . H2B H 1.0109 0.0632 0.8709 0.158 Uiso 1 1 calc R . . H2C H 1.0881 0.1735 0.8067 0.158 Uiso 1 1 calc R . . O3 O 0.7606(2) 0.01639(16) 0.69247(18) 0.0385(5) Uani 1 1 d . . . C3 C 1.1342(5) 0.1577(6) 0.6117(4) 0.132(3) Uani 1 1 d . . . H3A H 1.1065 0.1379 0.5619 0.199 Uiso 1 1 calc R . . H3B H 1.2200 0.1347 0.6137 0.199 Uiso 1 1 calc R . . H3C H 1.1348 0.2333 0.5885 0.199 Uiso 1 1 calc R . . O4 O 0.75011(18) 0.25074(15) 0.60714(15) 0.0302(5) Uani 1 1 d . . . C4 C 0.5905(3) 0.1641(2) 0.9106(2) 0.0255(6) Uani 1 1 d . . . C5 C 0.5936(3) 0.2246(2) 0.9682(2) 0.0262(6) Uani 1 1 d . . . C6 C 0.4764(3) 0.2528(2) 1.0160(2) 0.0289(6) Uani 1 1 d . . . H6 H 0.4761 0.2936 1.0554 0.035 Uiso 1 1 calc R . . C7 C 0.3593(3) 0.2246(2) 1.0096(2) 0.0277(6) Uani 1 1 d . . . C8 C 0.3618(3) 0.1593(2) 0.9568(2) 0.0270(6) Uani 1 1 d . . . H8 H 0.2839 0.1353 0.9543 0.032 Uiso 1 1 calc R . . C9 C 0.4746(3) 0.1288(2) 0.9082(2) 0.0248(6) Uani 1 1 d . . . C10 C 0.7199(3) 0.2568(2) 0.9781(2) 0.0305(7) Uani 1 1 d . . . C11 C 0.8043(3) 0.3269(3) 0.8691(3) 0.0418(8) Uani 1 1 d . . . H11A H 0.8214 0.2899 0.8219 0.063 Uiso 1 1 calc R . . H11B H 0.8847 0.3457 0.8768 0.063 Uiso 1 1 calc R . . H11C H 0.7607 0.3900 0.8387 0.063 Uiso 1 1 calc R . . C12 C 0.7901(3) 0.1595(2) 1.0281(3) 0.0364(7) Uani 1 1 d . . . H12A H 0.7391 0.1179 1.1003 0.055 Uiso 1 1 calc R . . H12B H 0.8726 0.1806 1.0306 0.055 Uiso 1 1 calc R . . H12C H 0.8034 0.1182 0.9852 0.055 Uiso 1 1 calc R . . C13 C 0.6989(3) 0.3160(3) 1.0505(3) 0.0448(8) Uani 1 1 d . . . H13A H 0.6561 0.3797 1.0206 0.067 Uiso 1 1 calc R . . H13B H 0.7812 0.3340 1.0560 0.067 Uiso 1 1 calc R . . H13C H 0.6461 0.2723 1.1213 0.067 Uiso 1 1 calc R . . C14 C 0.2331(3) 0.2672(2) 1.0515(2) 0.0332(7) Uani 1 1 d . . . C15 C 0.2483(3) 0.3295(3) 1.1147(3) 0.0540(10) Uani 1 1 d . . . H15A H 0.1654 0.3528 1.1422 0.081 Uiso 1 1 calc R . . H15B H 0.3072 0.3900 1.0683 0.081 Uiso 1 1 calc R . . H15C H 0.2819 0.2857 1.1740 0.081 Uiso 1 1 calc R . . C16 C 0.1313(3) 0.1793(3) 1.1223(3) 0.0449(8) Uani 1 1 d . . . H16A H 0.1169 0.1413 1.0816 0.067 Uiso 1 1 calc R . . H16B H 0.0519 0.2085 1.1475 0.067 Uiso 1 1 calc R . . H16C H 0.1598 0.1320 1.1833 0.067 Uiso 1 1 calc R . . C17 C 0.1870(3) 0.3397(3) 0.9560(3) 0.0476(9) Uani 1 1 d . . . H17A H 0.1738 0.3007 0.9157 0.071 Uiso 1 1 calc R . . H17B H 0.2510 0.3968 0.9102 0.071 Uiso 1 1 calc R . . H17C H 0.1068 0.3679 0.9811 0.071 Uiso 1 1 calc R . . C18 C 0.4778(3) 0.0580(2) 0.8524(2) 0.0252(6) Uani 1 1 d . . . H18A H 0.3895 0.0377 0.8596 0.030 Uiso 1 1 calc R . . H18B H 0.5192 -0.0059 0.8872 0.030 Uiso 1 1 calc R . . C19 C 0.4865(2) 0.2052(2) 0.6861(2) 0.0239(6) Uani 1 1 d . . . H19A H 0.4852 0.2493 0.7257 0.029 Uiso 1 1 calc R . . H19B H 0.3971 0.1874 0.6937 0.029 Uiso 1 1 calc R . . C20 C 0.5493(2) 0.26774(19) 0.5704(2) 0.0221(6) Uani 1 1 d . . . C21 C 0.6803(3) 0.2904(2) 0.5348(2) 0.0244(6) Uani 1 1 d . . . C22 C 0.7391(3) 0.3546(2) 0.4286(2) 0.0253(6) Uani 1 1 d . . . C23 C 0.6591(3) 0.3990(2) 0.3631(2) 0.0259(6) Uani 1 1 d . . . H23 H 0.6967 0.4436 0.2913 0.031 Uiso 1 1 calc R . . C24 C 0.5266(3) 0.38149(19) 0.3969(2) 0.0233(6) Uani 1 1 d . . . C25 C 0.4740(3) 0.31372(19) 0.5012(2) 0.0228(6) Uani 1 1 d . . . H25 H 0.3848 0.2982 0.5260 0.027 Uiso 1 1 calc R . . C26 C 0.8842(3) 0.3765(2) 0.3871(2) 0.0310(7) Uani 1 1 d . . . C27 C 0.9249(3) 0.4472(3) 0.2689(3) 0.0417(8) Uani 1 1 d . . . H27A H 0.8974 0.4143 0.2285 0.063 Uiso 1 1 calc R . . H27B H 1.0177 0.4587 0.2451 0.063 Uiso 1 1 calc R . . H27C H 0.8858 0.5139 0.2574 0.063 Uiso 1 1 calc R . . C28 C 0.9492(3) 0.2736(3) 0.4010(3) 0.0413(8) Uani 1 1 d . . . H28A H 0.9260 0.2267 0.4764 0.062 Uiso 1 1 calc R . . H28B H 1.0417 0.2873 0.3753 0.062 Uiso 1 1 calc R . . H28C H 0.9213 0.2413 0.3604 0.062 Uiso 1 1 calc R . . C29 C 0.9290(3) 0.4302(3) 0.4473(3) 0.0456(9) Uani 1 1 d . . . H29A H 0.8872 0.4955 0.4372 0.068 Uiso 1 1 calc R . . H29B H 1.0213 0.4444 0.4201 0.068 Uiso 1 1 calc R . . H29C H 0.9074 0.3849 0.5230 0.068 Uiso 1 1 calc R . . C30 C 0.4463(3) 0.4412(2) 0.3211(2) 0.0266(6) Uani 1 1 d . . . C31 C 0.4925(3) 0.4269(2) 0.2164(2) 0.0362(7) Uani 1 1 d . . . H31A H 0.4804 0.3537 0.2301 0.054 Uiso 1 1 calc R . . H31B H 0.5829 0.4489 0.1847 0.054 Uiso 1 1 calc R . . H31C H 0.4437 0.4691 0.1675 0.054 Uiso 1 1 calc R . . C32 C 0.4610(3) 0.5571(2) 0.2985(3) 0.0383(8) Uani 1 1 d . . . H32A H 0.4133 0.5975 0.2479 0.057 Uiso 1 1 calc R . . H32B H 0.5511 0.5806 0.2684 0.057 Uiso 1 1 calc R . . H32C H 0.4280 0.5671 0.3648 0.057 Uiso 1 1 calc R . . C33 C 0.3052(3) 0.4061(2) 0.3685(3) 0.0377(7) Uani 1 1 d . . . H33A H 0.2949 0.3317 0.3864 0.056 Uiso 1 1 calc R . . H33B H 0.2583 0.4446 0.3166 0.056 Uiso 1 1 calc R . . H33C H 0.2720 0.4196 0.4327 0.056 Uiso 1 1 calc R . . C34 C 0.6593(3) -0.0166(2) 0.6737(2) 0.0336(7) Uani 1 1 d . . . C35 C 0.6657(4) -0.0953(2) 0.6369(3) 0.0435(8) Uani 1 1 d . . . H35 H 0.7432 -0.1278 0.6234 0.052 Uiso 1 1 calc R . . C36 C 0.5586(4) -0.1255(2) 0.6204(3) 0.0447(9) Uani 1 1 d . . . H36 H 0.5640 -0.1786 0.5945 0.054 Uiso 1 1 calc R . . C37 C 0.4430(3) -0.0810(2) 0.6402(2) 0.0381(8) Uani 1 1 d . . . C38 C 0.4384(3) -0.0016(2) 0.6756(2) 0.0316(7) Uani 1 1 d . . . H38 H 0.3611 0.0311 0.6888 0.038 Uiso 1 1 calc R . . C39 C 0.5452(3) 0.0302(2) 0.6916(2) 0.0267(6) Uani 1 1 d . . . C40 C 0.3261(4) -0.1175(3) 0.6243(3) 0.0504(9) Uani 1 1 d . . . H40A H 0.2811 -0.1749 0.6897 0.076 Uiso 1 1 calc R . . H40B H 0.3513 -0.1413 0.5663 0.076 Uiso 1 1 calc R . . H40C H 0.2699 -0.0601 0.6065 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0235(3) 0.0359(3) 0.0256(3) -0.0114(2) -0.0091(2) 0.0049(2) O1 0.0215(11) 0.0700(15) 0.0383(13) -0.0228(12) -0.0102(10) 0.0087(10) N1 0.0256(12) 0.0237(11) 0.0202(12) -0.0073(9) -0.0063(10) 0.0001(9) C1 0.029(2) 0.180(6) 0.055(3) -0.036(3) -0.013(2) 0.022(3) O2 0.0230(10) 0.0366(11) 0.0259(11) -0.0144(9) -0.0071(8) 0.0018(8) C2 0.049(3) 0.205(7) 0.091(4) -0.077(4) -0.044(3) 0.039(3) O3 0.0356(12) 0.0432(12) 0.0427(13) -0.0221(11) -0.0147(10) 0.0139(10) C3 0.043(3) 0.225(8) 0.073(4) -0.003(4) -0.013(3) 0.013(4) O4 0.0239(10) 0.0371(11) 0.0270(11) -0.0076(9) -0.0101(9) -0.0031(8) C4 0.0267(15) 0.0253(14) 0.0212(14) -0.0048(11) -0.0079(12) -0.0006(11) C5 0.0285(15) 0.0266(14) 0.0225(15) -0.0067(12) -0.0092(12) -0.0027(11) C6 0.0306(16) 0.0304(15) 0.0274(16) -0.0124(13) -0.0088(13) 0.0002(12) C7 0.0253(15) 0.0312(15) 0.0246(15) -0.0092(12) -0.0063(12) 0.0007(12) C8 0.0265(15) 0.0307(15) 0.0213(15) -0.0060(12) -0.0086(12) -0.0039(12) C9 0.0278(15) 0.0250(13) 0.0183(14) -0.0044(11) -0.0070(12) -0.0019(11) C10 0.0265(15) 0.0345(15) 0.0321(17) -0.0135(13) -0.0093(13) -0.0028(12) C11 0.0350(18) 0.0433(18) 0.043(2) -0.0096(15) -0.0136(15) -0.0112(14) C12 0.0342(17) 0.0406(17) 0.0366(18) -0.0110(14) -0.0189(14) -0.0018(13) C13 0.0385(19) 0.056(2) 0.055(2) -0.0329(18) -0.0181(17) -0.0024(16) C14 0.0266(15) 0.0407(17) 0.0305(17) -0.0134(14) -0.0066(13) 0.0036(13) C15 0.041(2) 0.076(3) 0.063(3) -0.049(2) -0.0109(18) 0.0159(18) C16 0.0299(17) 0.050(2) 0.044(2) -0.0135(16) -0.0024(15) 0.0043(14) C17 0.042(2) 0.048(2) 0.043(2) -0.0107(16) -0.0107(16) 0.0144(16) C18 0.0278(15) 0.0265(14) 0.0194(14) -0.0063(11) -0.0068(12) -0.0035(11) C19 0.0217(14) 0.0240(13) 0.0258(15) -0.0094(12) -0.0068(12) 0.0003(11) C20 0.0246(14) 0.0200(13) 0.0237(15) -0.0110(11) -0.0056(11) -0.0016(10) C21 0.0242(14) 0.0248(13) 0.0256(15) -0.0099(12) -0.0092(12) 0.0014(11) C22 0.0239(14) 0.0243(13) 0.0282(16) -0.0116(12) -0.0057(12) -0.0016(11) C23 0.0275(15) 0.0246(13) 0.0245(15) -0.0091(12) -0.0056(12) -0.0032(11) C24 0.0277(14) 0.0199(13) 0.0238(15) -0.0100(11) -0.0075(12) 0.0015(11) C25 0.0219(13) 0.0218(13) 0.0267(15) -0.0111(11) -0.0071(12) 0.0001(10) C26 0.0229(15) 0.0364(16) 0.0289(16) -0.0101(13) -0.0030(12) -0.0036(12) C27 0.0284(16) 0.0464(19) 0.0355(19) -0.0055(15) -0.0005(14) -0.0062(14) C28 0.0287(17) 0.0483(19) 0.0393(19) -0.0139(16) -0.0031(14) 0.0035(14) C29 0.0293(17) 0.057(2) 0.051(2) -0.0227(18) -0.0060(16) -0.0150(15) C30 0.0279(15) 0.0273(14) 0.0258(16) -0.0099(12) -0.0104(12) 0.0012(11) C31 0.0437(18) 0.0377(17) 0.0315(17) -0.0144(14) -0.0159(15) 0.0021(14) C32 0.0464(19) 0.0292(16) 0.0428(19) -0.0120(14) -0.0219(16) 0.0058(14) C33 0.0325(17) 0.0415(17) 0.0344(18) -0.0066(14) -0.0154(14) 0.0037(13) C34 0.0400(18) 0.0309(15) 0.0304(17) -0.0123(13) -0.0114(14) 0.0073(13) C35 0.059(2) 0.0341(17) 0.042(2) -0.0194(15) -0.0170(17) 0.0134(15) C36 0.073(3) 0.0312(16) 0.0349(19) -0.0172(15) -0.0167(18) 0.0045(16) C37 0.061(2) 0.0271(15) 0.0267(17) -0.0086(13) -0.0142(15) -0.0050(15) C38 0.0427(18) 0.0279(15) 0.0262(16) -0.0102(12) -0.0129(14) 0.0002(13) C39 0.0371(16) 0.0219(13) 0.0213(15) -0.0070(11) -0.0105(13) 0.0010(12) C40 0.076(3) 0.0374(18) 0.046(2) -0.0168(16) -0.027(2) -0.0112(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.767(2) . ? Ti1 O4 1.8200(19) . ? Ti1 O2 1.8571(19) . ? Ti1 O3 1.868(2) . ? Ti1 N1 2.328(2) . ? O1 C1 1.406(4) . ? N1 C39 1.465(3) . ? N1 C19 1.497(3) . ? N1 C18 1.505(3) . ? C1 C3 1.397(7) . ? C1 C2 1.452(6) . ? C1 H1 1.0000 . ? O2 C4 1.361(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C34 1.356(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C21 1.372(3) . ? C4 C9 1.402(4) . ? C4 C5 1.409(4) . ? C5 C6 1.397(4) . ? C5 C10 1.539(4) . ? C6 C7 1.401(4) . ? C6 H6 0.9500 . ? C7 C8 1.397(4) . ? C7 C14 1.540(4) . ? C8 C9 1.379(4) . ? C8 H8 0.9500 . ? C9 C18 1.499(4) . ? C10 C11 1.532(4) . ? C10 C13 1.535(4) . ? C10 C12 1.541(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.529(4) . ? C14 C16 1.531(4) . ? C14 C17 1.537(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.506(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.394(4) . ? C20 C25 1.395(4) . ? C21 C22 1.405(4) . ? C22 C23 1.396(4) . ? C22 C26 1.539(4) . ? C23 C24 1.402(4) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 C30 1.535(4) . ? C25 H25 0.9500 . ? C26 C27 1.529(4) . ? C26 C29 1.530(4) . ? C26 C28 1.541(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C33 1.531(4) . ? C30 C31 1.533(4) . ? C30 C32 1.542(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.388(4) . ? C34 C35 1.395(4) . ? C35 C36 1.379(5) . ? C35 H35 0.9500 . ? C36 C37 1.390(5) . ? C36 H36 0.9500 . ? C37 C38 1.393(4) . ? C37 C40 1.511(5) . ? C38 C39 1.381(4) . ? C38 H38 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O4 102.58(10) . . ? O1 Ti1 O2 97.53(9) . . ? O4 Ti1 O2 117.40(9) . . ? O1 Ti1 O3 96.09(10) . . ? O4 Ti1 O3 110.73(9) . . ? O2 Ti1 O3 125.20(9) . . ? O1 Ti1 N1 172.40(10) . . ? O4 Ti1 N1 83.13(8) . . ? O2 Ti1 N1 84.04(8) . . ? O3 Ti1 N1 77.05(8) . . ? C1 O1 Ti1 164.0(3) . . ? C39 N1 C19 114.1(2) . . ? C39 N1 C18 107.4(2) . . ? C19 N1 C18 108.3(2) . . ? C39 N1 Ti1 105.37(16) . . ? C19 N1 Ti1 112.95(15) . . ? C18 N1 Ti1 108.51(15) . . ? C3 C1 O1 112.3(4) . . ? C3 C1 C2 123.4(5) . . ? O1 C1 C2 111.2(4) . . ? C3 C1 H1 102.2 . . ? O1 C1 H1 102.2 . . ? C2 C1 H1 102.2 . . ? C4 O2 Ti1 137.37(17) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C34 O3 Ti1 122.87(18) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C21 O4 Ti1 141.41(17) . . ? O2 C4 C9 117.5(2) . . ? O2 C4 C5 121.7(2) . . ? C9 C4 C5 120.9(3) . . ? C6 C5 C4 116.5(2) . . ? C6 C5 C10 122.3(3) . . ? C4 C5 C10 121.2(2) . . ? C5 C6 C7 124.1(3) . . ? C5 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? C8 C7 C6 116.7(3) . . ? C8 C7 C14 120.2(2) . . ? C6 C7 C14 122.9(3) . . ? C9 C8 C7 121.7(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C4 119.9(3) . . ? C8 C9 C18 121.9(2) . . ? C4 C9 C18 118.2(2) . . ? C11 C10 C13 107.9(3) . . ? C11 C10 C5 110.7(2) . . ? C13 C10 C5 111.8(2) . . ? C11 C10 C12 109.7(3) . . ? C13 C10 C12 106.8(2) . . ? C5 C10 C12 109.8(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 108.5(3) . . ? C15 C14 C17 108.1(3) . . ? C16 C14 C17 108.5(3) . . ? C15 C14 C7 112.2(2) . . ? C16 C14 C7 111.1(2) . . ? C17 C14 C7 108.3(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C9 C18 N1 112.7(2) . . ? C9 C18 H18A 109.0 . . ? N1 C18 H18A 109.0 . . ? C9 C18 H18B 109.0 . . ? N1 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N1 C19 C20 115.4(2) . . ? N1 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? N1 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C21 C20 C25 119.7(2) . . ? C21 C20 C19 120.5(2) . . ? C25 C20 C19 119.4(2) . . ? O4 C21 C20 118.2(2) . . ? O4 C21 C22 120.6(2) . . ? C20 C21 C22 121.1(2) . . ? C23 C22 C21 116.6(2) . . ? C23 C22 C26 121.7(2) . . ? C21 C22 C26 121.7(2) . . ? C22 C23 C24 123.9(3) . . ? C22 C23 H23 118.0 . . ? C24 C23 H23 118.0 . . ? C25 C24 C23 117.1(2) . . ? C25 C24 C30 123.1(2) . . ? C23 C24 C30 119.7(2) . . ? C24 C25 C20 121.4(2) . . ? C24 C25 H25 119.3 . . ? C20 C25 H25 119.3 . . ? C27 C26 C29 107.9(3) . . ? C27 C26 C22 111.8(2) . . ? C29 C26 C22 109.8(2) . . ? C27 C26 C28 107.4(3) . . ? C29 C26 C28 110.5(3) . . ? C22 C26 C28 109.4(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C33 C30 C31 108.1(2) . . ? C33 C30 C24 112.4(2) . . ? C31 C30 C24 110.7(2) . . ? C33 C30 C32 108.6(2) . . ? C31 C30 C32 109.2(2) . . ? C24 C30 C32 107.8(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O3 C34 C39 118.6(3) . . ? O3 C34 C35 122.4(3) . . ? C39 C34 C35 119.0(3) . . ? C36 C35 C34 119.3(3) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 122.3(3) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C36 C37 C38 117.7(3) . . ? C36 C37 C40 121.3(3) . . ? C38 C37 C40 121.0(3) . . ? C39 C38 C37 120.7(3) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C34 120.9(3) . . ? C38 C39 N1 124.8(3) . . ? C34 C39 N1 114.0(2) . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.902 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.062 #===END data_Ti(4)(OiPr) _database_code_depnum_ccdc_archive 'CCDC 736072' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H54 Cl N O4 Ti' _chemical_formula_weight 684.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0570(4) _cell_length_b 12.0150(5) _cell_length_c 16.4190(5) _cell_angle_alpha 75.615(2) _cell_angle_beta 89.264(2) _cell_angle_gamma 62.851(2) _cell_volume 1867.26(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19796 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27493 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6559 _reflns_number_gt 4726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.2681P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6559 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1366 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.48337(5) 0.39247(5) 0.84794(3) 0.02228(17) Uani 1 1 d . . . Cl1 Cl 0.70094(8) 0.82290(8) 0.62184(5) 0.0369(2) Uani 1 1 d . . . O1 O 0.3304(2) 0.3764(2) 0.85018(12) 0.0283(5) Uani 1 1 d . . . N1 N 0.6582(2) 0.4485(2) 0.84100(14) 0.0218(5) Uani 1 1 d . . . C1 C 0.1856(3) 0.4477(3) 0.83956(19) 0.0280(7) Uani 1 1 d . . . H1 H 0.1579 0.5399 0.8381 0.034 Uiso 1 1 calc R . . O2 O 0.5694(2) 0.3124(2) 0.76822(12) 0.0273(5) Uani 1 1 d . . . C2 C 0.1310(4) 0.4446(4) 0.7564(2) 0.0447(9) Uani 1 1 d . . . H2A H 0.1745 0.4759 0.7102 0.067 Uiso 1 1 calc R . . H2B H 0.0317 0.5008 0.7461 0.067 Uiso 1 1 calc R . . H2C H 0.1513 0.3553 0.7590 0.067 Uiso 1 1 calc R . . O3 O 0.3901(2) 0.5749(2) 0.80418(13) 0.0283(5) Uani 1 1 d . . . C3 C 0.1314(4) 0.3889(4) 0.9144(2) 0.0417(8) Uani 1 1 d . . . H3A H 0.1595 0.2980 0.9167 0.063 Uiso 1 1 calc R . . H3B H 0.0312 0.4377 0.9078 0.063 Uiso 1 1 calc R . . H3C H 0.1683 0.3930 0.9668 0.063 Uiso 1 1 calc R . . O4 O 0.5567(2) 0.3116(2) 0.95908(12) 0.0269(5) Uani 1 1 d . . . C4 C 0.6666(3) 0.3037(3) 0.71403(18) 0.0242(6) Uani 1 1 d . . . C5 C 0.6562(3) 0.2734(3) 0.63803(18) 0.0253(7) Uani 1 1 d . . . C6 C 0.7648(3) 0.2563(3) 0.58940(19) 0.0283(7) Uani 1 1 d . . . H6 H 0.7617 0.2335 0.5384 0.034 Uiso 1 1 calc R . . C7 C 0.8772(3) 0.2706(3) 0.61103(18) 0.0267(7) Uani 1 1 d . A . C8 C 0.8794(3) 0.3056(3) 0.68541(18) 0.0257(7) Uani 1 1 d . . . H8 H 0.9533 0.3187 0.7012 0.031 Uiso 1 1 calc R . . C9 C 0.7750(3) 0.3217(3) 0.73724(18) 0.0231(6) Uani 1 1 d . . . C10 C 0.5307(3) 0.2637(3) 0.60878(19) 0.0317(7) Uani 1 1 d . . . C11 C 0.5465(4) 0.2253(4) 0.5251(2) 0.0472(10) Uani 1 1 d . . . H11A H 0.4661 0.2177 0.5091 0.071 Uiso 1 1 calc R . . H11B H 0.6288 0.1417 0.5322 0.071 Uiso 1 1 calc R . . H11C H 0.5547 0.2921 0.4805 0.071 Uiso 1 1 calc R . . C12 C 0.5089(4) 0.1605(4) 0.6744(2) 0.0391(8) Uani 1 1 d . . . H12A H 0.4948 0.1835 0.7282 0.059 Uiso 1 1 calc R . . H12B H 0.5897 0.0755 0.6827 0.059 Uiso 1 1 calc R . . H12C H 0.4284 0.1566 0.6541 0.059 Uiso 1 1 calc R . . C13 C 0.4047(3) 0.3965(4) 0.5940(2) 0.0429(9) Uani 1 1 d . . . H13A H 0.3908 0.4222 0.6469 0.064 Uiso 1 1 calc R . . H13B H 0.3241 0.3915 0.5750 0.064 Uiso 1 1 calc R . . H13C H 0.4183 0.4609 0.5506 0.064 Uiso 1 1 calc R . . C14 C 0.9939(3) 0.2464(3) 0.55497(19) 0.0306(7) Uani 1 1 d . . . C15 C 0.945(2) 0.240(3) 0.4638(14) 0.052(7) Uani 0.20 1 d P A 1 H15A H 1.0121 0.2422 0.4245 0.078 Uiso 0.20 1 calc PR A 1 H15B H 0.8556 0.3154 0.4411 0.078 Uiso 0.20 1 calc PR A 1 H15C H 0.9386 0.1600 0.4710 0.078 Uiso 0.20 1 calc PR A 1 C16 C 1.1127(19) 0.141(2) 0.5974(12) 0.045(5) Uani 0.20 1 d P A 1 H16A H 1.1899 0.1387 0.5665 0.068 Uiso 0.20 1 calc PR A 1 H16B H 1.1063 0.0612 0.6019 0.068 Uiso 0.20 1 calc PR A 1 H16C H 1.1269 0.1484 0.6543 0.068 Uiso 0.20 1 calc PR A 1 C17 C 1.0055(17) 0.3779(17) 0.5324(10) 0.031(4) Uani 0.20 1 d P A 1 H17A H 1.0270 0.3941 0.5847 0.047 Uiso 0.20 1 calc PR A 1 H17B H 0.9183 0.4504 0.5027 0.047 Uiso 0.20 1 calc PR A 1 H17C H 1.0783 0.3701 0.4960 0.047 Uiso 0.20 1 calc PR A 1 C18 C 0.7875(3) 0.3462(3) 0.82181(18) 0.0240(6) Uani 1 1 d . . . H18A H 0.8163 0.2640 0.8669 0.029 Uiso 1 1 calc R . . H18B H 0.8601 0.3725 0.8229 0.029 Uiso 1 1 calc R . . C19 C 0.4580(3) 0.6377(3) 0.76318(18) 0.0245(6) Uani 1 1 d . . . C20 C 0.3910(3) 0.7609(3) 0.70792(18) 0.0283(7) Uani 1 1 d . . . H20 H 0.2938 0.8056 0.6989 0.034 Uiso 1 1 calc R . . C21 C 0.4658(3) 0.8195(3) 0.66551(18) 0.0285(7) Uani 1 1 d . . . H21 H 0.4203 0.9042 0.6277 0.034 Uiso 1 1 calc R . . C22 C 0.6073(3) 0.7526(3) 0.67922(18) 0.0264(7) Uani 1 1 d . . . C23 C 0.6768(3) 0.6306(3) 0.73552(17) 0.0248(6) Uani 1 1 d . . . H23 H 0.7739 0.5872 0.7451 0.030 Uiso 1 1 calc R . . C24 C 0.6015(3) 0.5731(3) 0.77767(17) 0.0225(6) Uani 1 1 d . . . C25 C 0.6830(3) 0.4691(3) 0.92547(17) 0.0231(6) Uani 1 1 d . . . H25A H 0.7477 0.5057 0.9205 0.028 Uiso 1 1 calc R . . H25B H 0.5956 0.5334 0.9391 0.028 Uiso 1 1 calc R . . C26 C 0.7398(3) 0.3463(3) 0.99674(17) 0.0229(6) Uani 1 1 d . . . C27 C 0.6713(3) 0.2713(3) 1.01273(18) 0.0242(6) Uani 1 1 d . . . C28 C 0.7179(3) 0.1591(3) 1.08106(18) 0.0243(6) Uani 1 1 d . . . C29 C 0.8358(3) 0.1261(3) 1.13079(18) 0.0253(7) Uani 1 1 d . . . H29 H 0.8687 0.0509 1.1776 0.030 Uiso 1 1 calc R . . C30 C 0.9097(3) 0.1963(3) 1.11666(18) 0.0246(6) Uani 1 1 d . . . C31 C 0.8595(3) 0.3070(3) 1.04825(18) 0.0241(6) Uani 1 1 d . . . H31 H 0.9074 0.3566 1.0364 0.029 Uiso 1 1 calc R . . C32 C 0.6484(3) 0.0712(3) 1.09582(19) 0.0279(7) Uani 1 1 d . . . C33 C 0.6655(4) 0.0107(3) 1.0215(2) 0.0367(8) Uani 1 1 d . . . H33A H 0.7631 -0.0420 1.0182 0.055 Uiso 1 1 calc R . . H33B H 0.6239 0.0800 0.9686 0.055 Uiso 1 1 calc R . . H33C H 0.6204 -0.0444 1.0303 0.055 Uiso 1 1 calc R . . C34 C 0.4944(3) 0.1488(3) 1.1040(2) 0.0324(7) Uani 1 1 d . . . H34A H 0.4543 0.0895 1.1170 0.049 Uiso 1 1 calc R . . H34B H 0.4479 0.2153 1.0506 0.049 Uiso 1 1 calc R . . H34C H 0.4837 0.1908 1.1497 0.049 Uiso 1 1 calc R . . C35 C 0.7125(4) -0.0407(3) 1.1767(2) 0.0362(8) Uani 1 1 d . . . H35A H 0.6672 -0.0955 1.1828 0.054 Uiso 1 1 calc R . . H35B H 0.7011 -0.0055 1.2257 0.054 Uiso 1 1 calc R . . H35C H 0.8102 -0.0929 1.1734 0.054 Uiso 1 1 calc R . . C36 C 1.0416(3) 0.1471(3) 1.17483(19) 0.0283(7) Uani 1 1 d . . . C37 C 1.1189(3) 0.2249(3) 1.1451(2) 0.0337(8) Uani 1 1 d . . . H37A H 1.1387 0.2240 1.0868 0.051 Uiso 1 1 calc R . . H37B H 1.2050 0.1859 1.1821 0.051 Uiso 1 1 calc R . . H37C H 1.0627 0.3149 1.1472 0.051 Uiso 1 1 calc R . . C38 C 1.0057(4) 0.1560(4) 1.2644(2) 0.0409(9) Uani 1 1 d . . . H38A H 1.0895 0.1253 1.3017 0.061 Uiso 1 1 calc R . . H38B H 0.9614 0.1018 1.2860 0.061 Uiso 1 1 calc R . . H38C H 0.9432 0.2465 1.2627 0.061 Uiso 1 1 calc R . . C39 C 1.1373(4) 0.0054(4) 1.1777(3) 0.0447(9) Uani 1 1 d . . . H39A H 1.1542 -0.0018 1.1201 0.067 Uiso 1 1 calc R . . H39B H 1.0948 -0.0487 1.2036 0.067 Uiso 1 1 calc R . . H39C H 1.2242 -0.0241 1.2114 0.067 Uiso 1 1 calc R . . C15' C 0.9403(5) 0.3218(7) 0.4642(3) 0.0581(16) Uani 0.80 1 d P A 2 H15D H 1.0165 0.3014 0.4296 0.087 Uiso 0.80 1 calc PR A 2 H15E H 0.8948 0.4151 0.4597 0.087 Uiso 0.80 1 calc PR A 2 H15F H 0.8747 0.2980 0.4440 0.087 Uiso 0.80 1 calc PR A 2 C16' C 1.0734(6) 0.0983(5) 0.5621(4) 0.0616(16) Uani 0.80 1 d P A 2 H16D H 1.1502 0.0813 0.5282 0.092 Uiso 0.80 1 calc PR A 2 H16E H 1.0117 0.0707 0.5412 0.092 Uiso 0.80 1 calc PR A 2 H16F H 1.1081 0.0497 0.6214 0.092 Uiso 0.80 1 calc PR A 2 C17' C 1.1024(6) 0.2786(7) 0.5843(3) 0.0587(15) Uani 0.80 1 d P A 2 H17D H 1.1383 0.2294 0.6435 0.088 Uiso 0.80 1 calc PR A 2 H17E H 1.0610 0.3719 0.5794 0.088 Uiso 0.80 1 calc PR A 2 H17F H 1.1773 0.2551 0.5489 0.088 Uiso 0.80 1 calc PR A 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 Ti1 0.0200(3) 0.0289(3) 0.0215(3) -0.0080(2) 0.0034(2) -0.0139(2) Cl1 0.0400(5) 0.0396(5) 0.0368(4) -0.0049(4) 0.0082(4) -0.0263(4) O1 0.0228(11) 0.0343(13) 0.0304(11) -0.0080(9) 0.0035(9) -0.0160(10) N1 0.0231(12) 0.0247(14) 0.0184(12) -0.0063(10) 0.0013(10) -0.0116(11) C1 0.0198(15) 0.0311(18) 0.0342(17) -0.0074(14) 0.0038(13) -0.0137(14) O2 0.0258(11) 0.0380(13) 0.0271(11) -0.0147(9) 0.0080(9) -0.0195(10) C2 0.0284(18) 0.061(3) 0.042(2) -0.0124(18) -0.0047(15) -0.0192(18) O3 0.0226(10) 0.0312(12) 0.0311(11) -0.0063(9) 0.0063(9) -0.0138(10) C3 0.0363(19) 0.046(2) 0.048(2) -0.0118(17) 0.0138(16) -0.0239(17) O4 0.0266(11) 0.0353(13) 0.0222(10) -0.0045(9) 0.0013(8) -0.0189(10) C4 0.0229(15) 0.0240(16) 0.0250(15) -0.0063(12) 0.0048(12) -0.0106(13) C5 0.0255(15) 0.0284(17) 0.0251(15) -0.0072(13) 0.0029(12) -0.0154(14) C6 0.0290(16) 0.0348(18) 0.0275(16) -0.0131(14) 0.0054(13) -0.0179(15) C7 0.0271(16) 0.0250(17) 0.0269(16) -0.0061(13) 0.0058(13) -0.0118(14) C8 0.0218(15) 0.0278(17) 0.0295(16) -0.0067(13) 0.0012(12) -0.0137(13) C9 0.0222(15) 0.0228(16) 0.0249(15) -0.0085(12) 0.0037(12) -0.0101(13) C10 0.0287(16) 0.046(2) 0.0278(16) -0.0166(15) 0.0040(13) -0.0208(16) C11 0.048(2) 0.080(3) 0.039(2) -0.032(2) 0.0101(17) -0.043(2) C12 0.044(2) 0.052(2) 0.0399(19) -0.0205(17) 0.0065(16) -0.0344(19) C13 0.0325(19) 0.056(2) 0.0419(19) -0.0140(18) -0.0012(15) -0.0220(18) C14 0.0275(17) 0.039(2) 0.0276(16) -0.0102(14) 0.0080(13) -0.0167(15) C15 0.061(14) 0.10(2) 0.051(12) -0.055(14) 0.045(11) -0.070(15) C16 0.033(10) 0.050(13) 0.037(10) -0.009(9) 0.030(9) -0.009(10) C17 0.034(9) 0.047(11) 0.028(8) -0.019(8) 0.027(8) -0.027(9) C18 0.0186(14) 0.0261(16) 0.0275(15) -0.0091(13) 0.0027(12) -0.0098(13) C19 0.0250(15) 0.0308(17) 0.0232(15) -0.0112(13) 0.0053(12) -0.0157(14) C20 0.0237(15) 0.0294(18) 0.0281(16) -0.0074(14) 0.0009(13) -0.0097(14) C21 0.0319(17) 0.0273(17) 0.0240(15) -0.0065(13) 0.0020(13) -0.0122(14) C22 0.0326(17) 0.0336(18) 0.0217(15) -0.0104(13) 0.0062(13) -0.0213(15) C23 0.0235(15) 0.0292(17) 0.0250(15) -0.0094(13) 0.0013(12) -0.0140(14) C24 0.0238(15) 0.0246(16) 0.0201(14) -0.0088(12) 0.0028(12) -0.0109(13) C25 0.0269(15) 0.0284(17) 0.0202(14) -0.0090(12) 0.0027(12) -0.0168(13) C26 0.0222(15) 0.0276(17) 0.0196(14) -0.0091(12) 0.0049(12) -0.0110(13) C27 0.0226(15) 0.0304(17) 0.0223(14) -0.0097(13) 0.0018(12) -0.0133(13) C28 0.0264(16) 0.0290(17) 0.0220(14) -0.0092(12) 0.0053(12) -0.0155(13) C29 0.0266(16) 0.0267(17) 0.0215(15) -0.0042(12) 0.0043(12) -0.0127(14) C30 0.0260(15) 0.0268(17) 0.0219(14) -0.0077(12) 0.0040(12) -0.0127(13) C31 0.0247(15) 0.0260(16) 0.0277(15) -0.0113(13) 0.0061(12) -0.0151(13) C32 0.0302(17) 0.0325(18) 0.0260(16) -0.0081(13) 0.0042(13) -0.0188(15) C33 0.044(2) 0.038(2) 0.0387(18) -0.0173(16) 0.0069(16) -0.0245(17) C34 0.0308(17) 0.039(2) 0.0345(17) -0.0099(15) 0.0088(14) -0.0230(16) C35 0.0379(19) 0.0335(19) 0.0388(18) -0.0029(15) 0.0003(15) -0.0213(16) C36 0.0230(15) 0.0311(18) 0.0277(16) -0.0029(13) -0.0001(13) -0.0125(14) C37 0.0250(16) 0.041(2) 0.0346(17) -0.0039(15) -0.0004(14) -0.0181(15) C38 0.040(2) 0.061(3) 0.0258(17) -0.0038(16) -0.0023(15) -0.0317(19) C39 0.0309(19) 0.034(2) 0.058(2) -0.0030(17) -0.0066(16) -0.0110(16) C15' 0.033(3) 0.092(5) 0.034(3) -0.002(3) 0.010(2) -0.024(3) C16' 0.047(3) 0.041(3) 0.086(5) -0.019(3) 0.039(3) -0.013(3) C17' 0.052(3) 0.103(5) 0.053(3) -0.039(3) 0.031(3) -0.054(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.787(2) . ? Ti1 O2 1.8170(19) . ? Ti1 O4 1.835(2) . ? Ti1 O3 1.886(2) . ? Ti1 N1 2.312(2) . ? Cl1 C22 1.747(3) . ? O1 C1 1.418(4) . ? N1 C24 1.450(4) . ? N1 C18 1.493(4) . ? N1 C25 1.517(3) . ? C1 C2 1.516(4) . ? C1 C3 1.518(4) . ? C1 H1 1.0000 . ? O2 C4 1.369(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C19 1.356(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C27 1.369(3) . ? C4 C9 1.385(4) . ? C4 C5 1.404(4) . ? C5 C6 1.398(4) . ? C5 C10 1.537(4) . ? C6 C7 1.392(4) . ? C6 H6 0.9500 . ? C7 C8 1.391(4) . ? C7 C14 1.535(4) . ? C8 C9 1.396(4) . ? C8 H8 0.9500 . ? C9 C18 1.510(4) . ? C10 C13 1.528(5) . ? C10 C12 1.535(5) . ? C10 C11 1.538(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.371(19) . ? C14 C15' 1.502(6) . ? C14 C17' 1.535(6) . ? C14 C16' 1.557(6) . ? C14 C17 1.595(16) . ? C14 C15 1.63(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.383(4) . ? C19 C24 1.404(4) . ? C20 C21 1.391(4) . ? C20 H20 0.9500 . ? C21 C22 1.385(4) . ? C21 H21 0.9500 . ? C22 C23 1.382(4) . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C25 C26 1.501(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C31 1.396(4) . ? C26 C27 1.398(4) . ? C27 C28 1.404(4) . ? C28 C29 1.385(4) . ? C28 C32 1.540(4) . ? C29 C30 1.400(4) . ? C29 H29 0.9500 . ? C30 C31 1.393(4) . ? C30 C36 1.535(4) . ? C31 H31 0.9500 . ? C32 C35 1.530(4) . ? C32 C33 1.537(4) . ? C32 C34 1.547(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C39 1.529(5) . ? C36 C37 1.529(4) . ? C36 C38 1.535(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 0.9800 . ? C17' H17D 0.9800 . ? C17' H17E 0.9800 . ? C17' H17F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 103.01(9) . . ? O1 Ti1 O4 100.06(9) . . ? O2 Ti1 O4 118.11(10) . . ? O1 Ti1 O3 94.05(9) . . ? O2 Ti1 O3 111.87(9) . . ? O4 Ti1 O3 122.76(9) . . ? O1 Ti1 N1 170.86(10) . . ? O2 Ti1 N1 82.32(8) . . ? O4 Ti1 N1 83.60(8) . . ? O3 Ti1 N1 76.99(9) . . ? C1 O1 Ti1 143.5(2) . . ? C24 N1 C18 114.5(2) . . ? C24 N1 C25 108.3(2) . . ? C18 N1 C25 109.6(2) . . ? C24 N1 Ti1 103.82(16) . . ? C18 N1 Ti1 112.12(17) . . ? C25 N1 Ti1 108.26(16) . . ? O1 C1 C2 109.2(2) . . ? O1 C1 C3 108.7(3) . . ? C2 C1 C3 111.8(3) . . ? O1 C1 H1 109.0 . . ? C2 C1 H1 109.0 . . ? C3 C1 H1 109.0 . . ? C4 O2 Ti1 143.07(19) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C19 O3 Ti1 119.53(18) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C27 O4 Ti1 141.65(18) . . ? O2 C4 C9 118.6(2) . . ? O2 C4 C5 119.6(3) . . ? C9 C4 C5 121.8(2) . . ? C6 C5 C4 116.1(3) . . ? C6 C5 C10 122.0(3) . . ? C4 C5 C10 121.9(2) . . ? C7 C6 C5 124.1(3) . . ? C7 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? C8 C7 C6 117.2(3) . . ? C8 C7 C14 122.1(3) . . ? C6 C7 C14 120.6(3) . . ? C7 C8 C9 121.1(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C4 C9 C8 119.6(3) . . ? C4 C9 C18 120.4(2) . . ? C8 C9 C18 119.8(3) . . ? C13 C10 C5 108.8(3) . . ? C13 C10 C12 110.2(3) . . ? C5 C10 C12 111.3(3) . . ? C13 C10 C11 107.8(3) . . ? C5 C10 C11 111.6(2) . . ? C12 C10 C11 107.1(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15' 136.1(8) . . ? C16 C14 C17' 64.8(11) . . ? C15' C14 C17' 109.0(4) . . ? C16 C14 C7 110.5(7) . . ? C15' C14 C7 111.3(3) . . ? C17' C14 C7 113.3(3) . . ? C16 C14 C16' 42.4(10) . . ? C15' C14 C16' 109.9(4) . . ? C17' C14 C16' 104.4(4) . . ? C7 C14 C16' 108.8(3) . . ? C16 C14 C17 112.3(13) . . ? C15' C14 C17 68.8(7) . . ? C17' C14 C17 48.4(7) . . ? C7 C14 C17 104.6(5) . . ? C16' C14 C17 143.9(6) . . ? C16 C14 C15 115.6(14) . . ? C15' C14 C15 35.3(9) . . ? C17' C14 C15 133.2(7) . . ? C7 C14 C15 109.7(7) . . ? C16' C14 C15 77.9(11) . . ? C17 C14 C15 103.4(11) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? N1 C18 C9 113.8(2) . . ? N1 C18 H18A 108.8 . . ? C9 C18 H18A 108.8 . . ? N1 C18 H18B 108.8 . . ? C9 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O3 C19 C20 122.4(3) . . ? O3 C19 C24 117.8(3) . . ? C20 C19 C24 119.8(3) . . ? C19 C20 C21 120.0(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 119.1(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C23 C22 C21 122.0(3) . . ? C23 C22 Cl1 119.0(2) . . ? C21 C22 Cl1 119.0(2) . . ? C22 C23 C24 118.5(3) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C23 C24 C19 120.5(3) . . ? C23 C24 N1 125.3(3) . . ? C19 C24 N1 114.1(2) . . ? C26 C25 N1 113.1(2) . . ? C26 C25 H25A 109.0 . . ? N1 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? N1 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C31 C26 C27 119.4(3) . . ? C31 C26 C25 120.7(3) . . ? C27 C26 C25 119.9(3) . . ? O4 C27 C26 117.4(3) . . ? O4 C27 C28 121.1(3) . . ? C26 C27 C28 121.5(3) . . ? C29 C28 C27 116.5(3) . . ? C29 C28 C32 121.6(3) . . ? C27 C28 C32 121.8(3) . . ? C28 C29 C30 124.4(3) . . ? C28 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? C31 C30 C29 117.1(3) . . ? C31 C30 C36 123.5(3) . . ? C29 C30 C36 119.3(3) . . ? C30 C31 C26 121.1(3) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? C35 C32 C33 107.3(3) . . ? C35 C32 C28 112.1(3) . . ? C33 C32 C28 109.2(2) . . ? C35 C32 C34 107.2(2) . . ? C33 C32 C34 109.6(3) . . ? C28 C32 C34 111.3(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C37 107.7(3) . . ? C39 C36 C38 109.2(3) . . ? C37 C36 C38 108.4(3) . . ? C39 C36 C30 109.4(3) . . ? C37 C36 C30 112.9(3) . . ? C38 C36 C30 109.1(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C14 C15' H15D 109.5 . . ? C14 C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C14 C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C14 C16' H16D 109.5 . . ? C14 C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C14 C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C14 C17' H17D 109.5 . . ? C14 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C14 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.423 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.105 #===END data_Zr(1)(OiPr) _database_code_depnum_ccdc_archive 'CCDC 736073' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H134 N2 O8 Zr2' _chemical_formula_weight 1662.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 12.7140(2) _cell_length_b 15.7070(3) _cell_length_c 22.6870(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.6470(10) _cell_angle_gamma 90.00 _cell_volume 4528.69(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24501 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The solvent of crystallisation are disordered. Attempts to model further were unsuccessful thus resulting in ellipsoids with higher than desirable ADPs. There is also a short H10e H10h interaction between the toluene moieties, which is chemically insignificant. ; _diffrn_ambient_temperature 150(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_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37439 _diffrn_reflns_av_R_equivalents 0.1143 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 24.98 _reflns_number_total 7897 _reflns_number_gt 5755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+3.6864P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7897 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.40898(2) 0.512669(17) 0.060717(12) 0.01749(9) Uani 1 1 d . . . O1 O 0.31401(15) 0.59626(13) 0.02810(9) 0.0259(5) Uani 1 1 d . . . N1 N 0.52141(17) 0.42010(15) 0.12147(10) 0.0181(5) Uani 1 1 d . . . C1 C 0.4951(2) 0.58412(19) 0.18423(12) 0.0188(6) Uani 1 1 d . . . O2 O 0.43316(14) 0.58034(12) 0.13428(8) 0.0202(4) Uani 1 1 d . . . C2 C 0.5359(2) 0.66205(19) 0.20546(13) 0.0206(6) Uani 1 1 d . . . O3 O 0.56880(14) 0.53001(12) 0.03364(8) 0.0189(4) Uani 1 1 d . . . C3 C 0.6006(2) 0.65815(19) 0.25627(13) 0.0227(7) Uani 1 1 d . . . H3 H 0.6293 0.7099 0.2713 0.027 Uiso 1 1 calc R . . O4 O 0.31533(14) 0.41465(12) 0.07703(8) 0.0213(5) Uani 1 1 d . . . C4 C 0.6254(2) 0.58311(19) 0.28627(13) 0.0224(7) Uani 1 1 d . . . C5 C 0.5832(2) 0.50782(19) 0.26365(12) 0.0213(6) Uani 1 1 d . . . H5 H 0.5976 0.4556 0.2834 0.026 Uiso 1 1 calc R . . C6 C 0.5202(2) 0.50783(18) 0.21252(12) 0.0186(6) Uani 1 1 d . . . C7 C 0.5124(2) 0.74626(19) 0.17389(14) 0.0249(7) Uani 1 1 d . . . C8 C 0.3936(3) 0.7650(2) 0.17375(16) 0.0364(8) Uani 1 1 d . . . H8A H 0.3552 0.7177 0.1551 0.055 Uiso 1 1 calc R . . H8B H 0.3791 0.8176 0.1517 0.055 Uiso 1 1 calc R . . H8C H 0.3710 0.7718 0.2144 0.055 Uiso 1 1 calc R . . C9 C 0.5491(3) 0.7423(2) 0.10984(15) 0.0376(9) Uani 1 1 d . . . H9A H 0.6227 0.7236 0.1096 0.056 Uiso 1 1 calc R . . H9B H 0.5430 0.7988 0.0918 0.056 Uiso 1 1 calc R . . H9C H 0.5051 0.7018 0.0874 0.056 Uiso 1 1 calc R . . C10 C 0.5698(3) 0.8218(2) 0.20344(15) 0.0342(8) Uani 1 1 d . . . H10A H 0.5470 0.8276 0.2441 0.051 Uiso 1 1 calc R . . H10B H 0.5531 0.8741 0.1816 0.051 Uiso 1 1 calc R . . H10C H 0.6459 0.8119 0.2034 0.051 Uiso 1 1 calc R . . C11 C 0.6979(2) 0.5806(2) 0.34172(13) 0.0265(7) Uani 1 1 d . . . C12 C 0.7559(3) 0.6650(2) 0.35197(16) 0.0391(9) Uani 1 1 d . . . H12A H 0.7962 0.6791 0.3171 0.059 Uiso 1 1 calc R . . H12B H 0.8038 0.6598 0.3864 0.059 Uiso 1 1 calc R . . H12C H 0.7046 0.7103 0.3590 0.059 Uiso 1 1 calc R . . C13 C 0.6308(3) 0.5616(2) 0.39515(14) 0.0382(8) Uani 1 1 d . . . H13A H 0.5785 0.6069 0.3995 0.057 Uiso 1 1 calc R . . H13B H 0.6762 0.5589 0.4308 0.057 Uiso 1 1 calc R . . H13C H 0.5949 0.5070 0.3894 0.057 Uiso 1 1 calc R . . C14 C 0.7802(3) 0.5102(2) 0.33577(16) 0.0443(9) Uani 1 1 d . . . H14A H 0.7449 0.4549 0.3326 0.066 Uiso 1 1 calc R . . H14B H 0.8278 0.5105 0.3705 0.066 Uiso 1 1 calc R . . H14C H 0.8208 0.5203 0.3003 0.066 Uiso 1 1 calc R . . C15 C 0.4862(2) 0.42506(18) 0.18468(12) 0.0202(6) Uani 1 1 d . . . H15A H 0.4086 0.4202 0.1855 0.024 Uiso 1 1 calc R . . H15B H 0.5170 0.3770 0.2076 0.024 Uiso 1 1 calc R . . C16 C 0.6486(2) 0.51154(19) 0.07442(12) 0.0185(6) Uani 1 1 d . . . C17 C 0.7455(2) 0.55131(19) 0.07247(13) 0.0225(7) Uani 1 1 d . . . H17 H 0.7573 0.5949 0.0444 0.027 Uiso 1 1 calc R . . C18 C 0.8255(2) 0.5271(2) 0.11194(13) 0.0267(7) Uani 1 1 d . . . H18 H 0.8922 0.5541 0.1108 0.032 Uiso 1 1 calc R . . C19 C 0.8086(2) 0.4639(2) 0.15289(13) 0.0268(7) Uani 1 1 d . . . H19 H 0.8640 0.4470 0.1794 0.032 Uiso 1 1 calc R . . C20 C 0.7109(2) 0.42504(19) 0.15545(13) 0.0231(7) Uani 1 1 d . . . H20 H 0.6994 0.3813 0.1835 0.028 Uiso 1 1 calc R . . C21 C 0.6301(2) 0.45021(18) 0.11701(12) 0.0184(6) Uani 1 1 d . . . C22 C 0.5093(2) 0.33126(18) 0.09733(14) 0.0224(7) Uani 1 1 d . . . H22A H 0.5668 0.2953 0.1140 0.027 Uiso 1 1 calc R . . H22B H 0.5167 0.3330 0.0540 0.027 Uiso 1 1 calc R . . C23 C 0.3108(2) 0.33477(18) 0.09962(13) 0.0207(6) Uani 1 1 d . . . C24 C 0.4050(2) 0.29056(19) 0.11093(13) 0.0223(7) Uani 1 1 d . . . C25 C 0.4030(2) 0.20985(19) 0.13569(14) 0.0274(7) Uani 1 1 d . . . H25 H 0.4676 0.1809 0.1431 0.033 Uiso 1 1 calc R . . C26 C 0.3094(2) 0.1700(2) 0.14997(15) 0.0318(8) Uani 1 1 d . . . C27 C 0.2166(2) 0.2163(2) 0.13875(15) 0.0302(8) Uani 1 1 d . . . H27 H 0.1518 0.1906 0.1484 0.036 Uiso 1 1 calc R . . C28 C 0.2137(2) 0.29751(19) 0.11438(13) 0.0238(7) Uani 1 1 d . . . C29 C 0.3037(3) 0.0825(2) 0.18008(19) 0.0458(10) Uani 1 1 d . . . C30 C 0.2308(4) 0.0236(3) 0.1443(3) 0.0808(16) Uani 1 1 d . . . H30A H 0.2312 -0.0331 0.1624 0.121 Uiso 1 1 calc R . . H30B H 0.2554 0.0194 0.1039 0.121 Uiso 1 1 calc R . . H30C H 0.1592 0.0466 0.1438 0.121 Uiso 1 1 calc R . . C31 C 0.2599(4) 0.0927(3) 0.2418(2) 0.0681(14) Uani 1 1 d . . . H31A H 0.2548 0.0367 0.2605 0.102 Uiso 1 1 calc R . . H31B H 0.1899 0.1187 0.2387 0.102 Uiso 1 1 calc R . . H31C H 0.3069 0.1292 0.2656 0.102 Uiso 1 1 calc R . . C32 C 0.4115(3) 0.0395(3) 0.1854(2) 0.0627(13) Uani 1 1 d . . . H32A H 0.4597 0.0756 0.2088 0.094 Uiso 1 1 calc R . . H32B H 0.4394 0.0313 0.1460 0.094 Uiso 1 1 calc R . . H32C H 0.4044 -0.0158 0.2048 0.094 Uiso 1 1 calc R . . C33 C 0.1099(2) 0.34772(19) 0.10872(13) 0.0234(7) Uani 1 1 d . . . C34 C 0.0905(2) 0.3836(2) 0.04630(14) 0.0311(8) Uani 1 1 d . . . H34A H 0.0219 0.4119 0.0440 0.047 Uiso 1 1 calc R . . H34B H 0.0916 0.3370 0.0176 0.047 Uiso 1 1 calc R . . H34C H 0.1458 0.4248 0.0375 0.047 Uiso 1 1 calc R . . C35 C 0.1149(2) 0.4207(2) 0.15372(14) 0.0301(7) Uani 1 1 d . . . H35A H 0.1747 0.4578 0.1454 0.045 Uiso 1 1 calc R . . H35B H 0.1237 0.3972 0.1936 0.045 Uiso 1 1 calc R . . H35C H 0.0496 0.4537 0.1509 0.045 Uiso 1 1 calc R . . C36 C 0.0146(2) 0.2916(2) 0.12232(16) 0.0350(8) Uani 1 1 d . . . H36A H -0.0499 0.3255 0.1187 0.053 Uiso 1 1 calc R . . H36B H 0.0223 0.2693 0.1626 0.053 Uiso 1 1 calc R . . H36C H 0.0106 0.2440 0.0944 0.053 Uiso 1 1 calc R . . C37 C 0.2248(2) 0.6485(2) 0.01458(15) 0.0328(8) Uani 1 1 d . . . H37 H 0.1929 0.6296 -0.0240 0.039 Uiso 1 1 calc R . . C38 C 0.1444(3) 0.6358(2) 0.06211(17) 0.0427(9) Uani 1 1 d . . . H38A H 0.1225 0.5760 0.0627 0.064 Uiso 1 1 calc R . . H38B H 0.0830 0.6720 0.0537 0.064 Uiso 1 1 calc R . . H38C H 0.1759 0.6512 0.1006 0.064 Uiso 1 1 calc R . . C39 C 0.2588(3) 0.7397(2) 0.00886(18) 0.0486(10) Uani 1 1 d . . . H39A H 0.2863 0.7602 0.0471 0.073 Uiso 1 1 calc R . . H39B H 0.1985 0.7745 -0.0039 0.073 Uiso 1 1 calc R . . H39C H 0.3140 0.7437 -0.0203 0.073 Uiso 1 1 calc R . . C100 C 0.5388(9) 0.3635(4) 0.4681(4) 0.200(5) Uani 1 1 d . . . H10D H 0.4855 0.4084 0.4693 0.300 Uiso 1 1 calc R . . H10E H 0.6086 0.3882 0.4761 0.300 Uiso 1 1 calc R . . H10F H 0.5242 0.3204 0.4980 0.300 Uiso 1 1 calc R . . C101 C 0.5362(8) 0.3222(4) 0.4071(4) 0.114(3) Uani 1 1 d . . . C102 C 0.4525(8) 0.3309(6) 0.3724(6) 0.151(5) Uani 1 1 d . . . H102 H 0.3946 0.3637 0.3851 0.181 Uiso 1 1 calc R . . C103 C 0.4478(6) 0.2928(7) 0.3176(5) 0.148(5) Uani 1 1 d . . . H103 H 0.3870 0.2991 0.2926 0.177 Uiso 1 1 calc R . . C104 C 0.5332(6) 0.2452(4) 0.2991(3) 0.096(2) Uani 1 1 d . . . H104 H 0.5304 0.2169 0.2620 0.116 Uiso 1 1 calc R . . C105 C 0.6194(5) 0.2397(4) 0.3344(3) 0.0873(17) Uani 1 1 d . . . H105 H 0.6793 0.2096 0.3214 0.105 Uiso 1 1 calc R . . C106 C 0.6216(5) 0.2774(3) 0.3893(3) 0.0822(16) Uani 1 1 d . . . H106 H 0.6822 0.2723 0.4145 0.099 Uiso 1 1 calc R . . C107 C 0.3147(7) 0.1063(6) -0.0009(4) 0.065(3) Uani 0.50 1 d P . . H10G H 0.3264 0.1553 0.0252 0.097 Uiso 0.50 1 calc PR A 1 H10H H 0.2538 0.0738 0.0121 0.097 Uiso 0.50 1 calc PR A 1 H10I H 0.3014 0.1263 -0.0413 0.097 Uiso 0.50 1 calc PR A 1 C108 C 0.412(2) 0.0493(19) 0.0011(10) 0.068(11) Uani 0.50 1 d P . 1 C109 C 0.5100(4) 0.0870(3) 0.0037(2) 0.0623(13) Uani 1 1 d . . . H109 H 0.5164 0.1471 0.0061 0.075 Uiso 1 1 calc R . 1 C110 C 0.5983(4) 0.0366(3) 0.00281(19) 0.0649(13) Uani 1 1 d . . . H110 H 0.6663 0.0616 0.0049 0.078 Uiso 1 1 calc R . . C118 C 0.4101(19) 0.0536(19) 0.0009(10) 0.061(10) Uani 0.50 1 d P . 2 H118 H 0.3495 0.0889 0.0015 0.073 Uiso 0.50 1 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 0.01480(14) 0.01951(16) 0.01815(14) 0.00063(13) 0.00048(9) 0.00104(12) O1 0.0243(11) 0.0275(13) 0.0255(12) 0.0005(9) -0.0042(9) 0.0092(9) N1 0.0163(12) 0.0178(14) 0.0204(13) -0.0010(10) 0.0028(9) -0.0017(9) C1 0.0173(15) 0.0237(17) 0.0154(15) -0.0012(12) 0.0019(11) -0.0012(12) O2 0.0195(10) 0.0210(12) 0.0201(11) -0.0002(8) -0.0017(8) 0.0020(8) C2 0.0194(15) 0.0215(17) 0.0212(16) -0.0008(13) 0.0046(12) 0.0012(12) O3 0.0159(10) 0.0246(12) 0.0162(10) -0.0004(8) -0.0001(7) 0.0001(8) C3 0.0220(16) 0.0212(17) 0.0251(17) -0.0057(13) 0.0031(12) -0.0014(12) O4 0.0175(10) 0.0225(12) 0.0241(11) 0.0025(9) -0.0002(8) -0.0023(8) C4 0.0208(15) 0.0268(18) 0.0197(16) -0.0010(13) 0.0034(12) 0.0002(12) C5 0.0242(15) 0.0203(17) 0.0196(14) 0.0017(13) 0.0020(11) 0.0032(12) C6 0.0181(14) 0.0180(16) 0.0201(14) -0.0014(12) 0.0036(11) 0.0005(12) C7 0.0262(16) 0.0182(17) 0.0303(18) 0.0018(13) -0.0010(13) -0.0005(12) C8 0.0355(19) 0.023(2) 0.050(2) 0.0000(16) -0.0075(16) 0.0038(14) C9 0.052(2) 0.028(2) 0.033(2) 0.0091(16) 0.0063(16) -0.0018(16) C10 0.041(2) 0.0217(19) 0.039(2) -0.0009(15) -0.0045(16) -0.0029(14) C11 0.0274(17) 0.0273(19) 0.0246(17) -0.0048(14) -0.0053(13) 0.0027(13) C12 0.042(2) 0.041(2) 0.033(2) -0.0005(16) -0.0126(16) -0.0077(16) C13 0.043(2) 0.046(2) 0.0255(18) 0.0033(16) -0.0053(15) 0.0021(16) C14 0.0363(19) 0.052(3) 0.043(2) -0.0124(19) -0.0180(15) 0.0173(17) C15 0.0221(15) 0.0208(17) 0.0177(16) 0.0028(12) 0.0008(12) 0.0002(12) C16 0.0150(13) 0.0215(16) 0.0192(14) -0.0048(13) 0.0008(10) 0.0045(12) C17 0.0201(16) 0.0237(17) 0.0239(16) -0.0001(13) 0.0025(12) -0.0014(12) C18 0.0172(15) 0.034(2) 0.0290(17) -0.0055(15) 0.0019(12) -0.0036(13) C19 0.0196(16) 0.034(2) 0.0267(17) -0.0018(14) -0.0022(12) 0.0031(13) C20 0.0224(16) 0.0243(18) 0.0224(16) 0.0003(13) -0.0006(12) 0.0027(12) C21 0.0141(14) 0.0195(16) 0.0215(16) -0.0039(12) 0.0016(11) -0.0018(11) C22 0.0187(15) 0.0185(17) 0.0299(17) -0.0016(13) 0.0012(12) 0.0032(12) C23 0.0217(15) 0.0184(17) 0.0223(16) -0.0042(13) 0.0029(12) -0.0022(12) C24 0.0210(15) 0.0212(18) 0.0247(17) -0.0057(13) 0.0003(12) -0.0012(12) C25 0.0237(16) 0.0203(18) 0.038(2) -0.0013(14) 0.0031(14) 0.0032(13) C26 0.0303(18) 0.0207(18) 0.045(2) -0.0014(15) 0.0079(15) -0.0019(13) C27 0.0256(17) 0.0253(19) 0.040(2) -0.0007(15) 0.0093(14) -0.0038(13) C28 0.0234(16) 0.0242(18) 0.0237(17) -0.0067(13) 0.0007(12) -0.0013(12) C29 0.041(2) 0.024(2) 0.073(3) 0.0097(19) 0.0173(19) 0.0007(16) C30 0.075(3) 0.025(3) 0.142(5) 0.010(3) 0.005(3) -0.021(2) C31 0.071(3) 0.055(3) 0.080(3) 0.037(3) 0.037(3) 0.017(2) C32 0.050(2) 0.034(2) 0.106(4) 0.025(2) 0.025(2) 0.0112(18) C33 0.0181(15) 0.0223(18) 0.0299(18) -0.0028(13) 0.0046(12) -0.0017(12) C34 0.0203(16) 0.039(2) 0.0338(19) 0.0006(15) -0.0006(13) -0.0022(14) C35 0.0256(17) 0.032(2) 0.0326(19) -0.0042(15) 0.0057(13) 0.0016(14) C36 0.0228(17) 0.035(2) 0.047(2) -0.0027(17) 0.0068(14) -0.0060(14) C37 0.0300(18) 0.037(2) 0.0310(19) -0.0022(15) -0.0088(14) 0.0160(15) C38 0.0297(19) 0.039(2) 0.060(3) -0.0016(19) 0.0066(17) 0.0108(15) C39 0.050(2) 0.041(3) 0.056(3) 0.0152(19) 0.0159(19) 0.0219(18) C100 0.392(15) 0.069(5) 0.148(7) 0.000(5) 0.181(9) -0.032(7) C101 0.175(8) 0.040(3) 0.132(6) 0.029(4) 0.094(6) -0.007(4) C102 0.121(7) 0.112(7) 0.225(12) 0.135(8) 0.092(8) 0.058(6) C103 0.076(5) 0.178(10) 0.188(9) 0.145(9) -0.007(6) -0.025(5) C104 0.116(6) 0.071(4) 0.102(5) 0.037(4) -0.001(4) -0.029(4) C105 0.087(4) 0.060(4) 0.116(5) 0.021(4) 0.024(4) -0.001(3) C106 0.094(4) 0.055(3) 0.099(5) 0.014(3) 0.035(3) -0.009(3) C107 0.064(6) 0.081(7) 0.049(5) 0.000(5) -0.006(4) -0.001(5) C108 0.11(2) 0.056(17) 0.037(13) -0.011(10) -0.038(11) 0.011(12) C109 0.078(4) 0.059(3) 0.048(3) 0.012(2) -0.025(2) -0.008(3) C110 0.064(3) 0.081(4) 0.048(3) 0.015(3) -0.019(2) -0.013(3) C118 0.040(13) 0.09(2) 0.056(15) 0.039(11) -0.001(9) 0.004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 1.9178(19) . ? Zr1 O4 1.9875(19) . ? Zr1 O2 1.9949(19) . ? Zr1 O3 2.1568(18) . ? Zr1 O3 2.2686(18) 3_665 ? Zr1 N1 2.438(2) . ? Zr1 Zr1 3.6703(5) 3_665 ? O1 C37 1.426(3) . ? N1 C21 1.467(3) . ? N1 C22 1.505(4) . ? N1 C15 1.516(4) . ? C1 O2 1.362(3) . ? C1 C6 1.392(4) . ? C1 C2 1.409(4) . ? C2 C3 1.398(4) . ? C2 C7 1.530(4) . ? O3 C16 1.384(3) . ? O3 Zr1 2.2686(18) 3_665 ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? O4 C23 1.357(3) . ? C4 C5 1.391(4) . ? C4 C11 1.539(4) . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C15 1.503(4) . ? C7 C10 1.537(4) . ? C7 C8 1.539(4) . ? C7 C9 1.540(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.531(4) . ? C11 C14 1.531(4) . ? C11 C13 1.531(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.384(4) . ? C16 C21 1.389(4) . ? C17 C18 1.389(4) . ? C17 H17 0.9500 . ? C18 C19 1.380(4) . ? C18 H18 0.9500 . ? C19 C20 1.387(4) . ? C19 H19 0.9500 . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C22 C24 1.511(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.402(4) . ? C23 C28 1.415(4) . ? C24 C25 1.387(4) . ? C25 C26 1.391(4) . ? C25 H25 0.9500 . ? C26 C27 1.403(4) . ? C26 C29 1.538(5) . ? C27 C28 1.390(4) . ? C27 H27 0.9500 . ? C28 C33 1.539(4) . ? C29 C30 1.526(6) . ? C29 C32 1.529(5) . ? C29 C31 1.530(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.535(4) . ? C33 C36 1.537(4) . ? C33 C34 1.538(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.503(5) . ? C37 C38 1.520(5) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C100 C101 1.528(10) . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C100 H10F 0.9800 . ? C101 C102 1.313(12) . ? C101 C106 1.365(9) . ? C102 C103 1.380(14) . ? C102 H102 0.9500 . ? C103 C104 1.393(11) . ? C103 H103 0.9500 . ? C104 C105 1.341(8) . ? C104 H104 0.9500 . ? C105 C106 1.379(8) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 C108 1.53(3) . ? C107 H10G 0.9800 . ? C107 H10H 0.9800 . ? C107 H10I 0.9800 . ? C108 C110 1.36(3) 3_655 ? C108 C109 1.38(3) . ? C109 C110 1.374(7) . ? C109 C118 1.37(2) . ? C109 H109 0.9500 . ? C110 C108 1.36(3) 3_655 ? C110 C118 1.42(3) 3_655 ? C110 H110 0.9500 . ? C118 C110 1.42(3) 3_655 ? C118 H118 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 O4 103.19(8) . . ? O1 Zr1 O2 92.19(8) . . ? O4 Zr1 O2 109.61(8) . . ? O1 Zr1 O3 113.05(8) . . ? O4 Zr1 O3 136.48(8) . . ? O2 Zr1 O3 92.71(7) . . ? O1 Zr1 O3 86.12(8) . 3_665 ? O4 Zr1 O3 92.19(7) . 3_665 ? O2 Zr1 O3 157.89(7) . 3_665 ? O3 Zr1 O3 67.96(8) . 3_665 ? O1 Zr1 N1 168.19(8) . . ? O4 Zr1 N1 77.14(7) . . ? O2 Zr1 N1 76.76(8) . . ? O3 Zr1 N1 72.21(7) . . ? O3 Zr1 N1 105.69(7) 3_665 . ? O1 Zr1 Zr1 100.85(6) . 3_665 ? O4 Zr1 Zr1 116.73(6) . 3_665 ? O2 Zr1 Zr1 126.90(5) . 3_665 ? O3 Zr1 Zr1 34.95(5) . 3_665 ? O3 Zr1 Zr1 33.00(4) 3_665 3_665 ? N1 Zr1 Zr1 89.29(5) . 3_665 ? C37 O1 Zr1 164.8(2) . . ? C21 N1 C22 111.1(2) . . ? C21 N1 C15 110.7(2) . . ? C22 N1 C15 111.2(2) . . ? C21 N1 Zr1 107.87(16) . . ? C22 N1 Zr1 107.15(16) . . ? C15 N1 Zr1 108.66(16) . . ? O2 C1 C6 117.7(2) . . ? O2 C1 C2 121.4(3) . . ? C6 C1 C2 120.8(2) . . ? C1 O2 Zr1 142.24(18) . . ? C3 C2 C1 116.5(3) . . ? C3 C2 C7 121.8(3) . . ? C1 C2 C7 121.7(3) . . ? C16 O3 Zr1 117.48(15) . . ? C16 O3 Zr1 117.40(15) . 3_665 ? Zr1 O3 Zr1 112.04(8) . 3_665 ? C4 C3 C2 124.0(3) . . ? C4 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? C23 O4 Zr1 144.96(17) . . ? C5 C4 C3 117.4(3) . . ? C5 C4 C11 119.7(3) . . ? C3 C4 C11 122.9(3) . . ? C6 C5 C4 121.0(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 120.3(3) . . ? C5 C6 C15 120.1(3) . . ? C1 C6 C15 119.4(2) . . ? C2 C7 C10 112.3(3) . . ? C2 C7 C8 110.2(2) . . ? C10 C7 C8 107.8(3) . . ? C2 C7 C9 110.3(3) . . ? C10 C7 C9 106.9(3) . . ? C8 C7 C9 109.3(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 108.1(3) . . ? C12 C11 C13 109.0(3) . . ? C14 C11 C13 109.1(3) . . ? C12 C11 C4 112.1(3) . . ? C14 C11 C4 109.9(2) . . ? C13 C11 C4 108.5(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C6 C15 N1 110.7(2) . . ? C6 C15 H15A 109.5 . . ? N1 C15 H15A 109.5 . . ? C6 C15 H15B 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 O3 121.4(3) . . ? C17 C16 C21 120.3(2) . . ? O3 C16 C21 118.4(2) . . ? C16 C17 C18 119.5(3) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 120.4(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 119.9(2) . . ? C20 C21 N1 123.2(3) . . ? C16 C21 N1 116.8(2) . . ? N1 C22 C24 113.5(2) . . ? N1 C22 H22A 108.9 . . ? C24 C22 H22A 108.9 . . ? N1 C22 H22B 108.9 . . ? C24 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? O4 C23 C24 118.8(2) . . ? O4 C23 C28 121.2(2) . . ? C24 C23 C28 119.9(3) . . ? C25 C24 C23 120.1(3) . . ? C25 C24 C22 119.7(3) . . ? C23 C24 C22 120.2(3) . . ? C24 C25 C26 122.1(3) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 116.5(3) . . ? C25 C26 C29 123.8(3) . . ? C27 C26 C29 119.6(3) . . ? C28 C27 C26 124.1(3) . . ? C28 C27 H27 117.9 . . ? C26 C27 H27 117.9 . . ? C27 C28 C23 117.4(3) . . ? C27 C28 C33 121.1(3) . . ? C23 C28 C33 121.3(3) . . ? C30 C29 C32 107.7(4) . . ? C30 C29 C31 108.6(4) . . ? C32 C29 C31 108.9(4) . . ? C30 C29 C26 110.0(3) . . ? C32 C29 C26 112.1(3) . . ? C31 C29 C26 109.6(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C36 108.2(3) . . ? C35 C33 C34 109.9(3) . . ? C36 C33 C34 106.8(2) . . ? C35 C33 C28 107.9(2) . . ? C36 C33 C28 111.6(3) . . ? C34 C33 C28 112.3(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 C39 109.7(3) . . ? O1 C37 C38 108.6(3) . . ? C39 C37 C38 112.8(3) . . ? O1 C37 H37 108.5 . . ? C39 C37 H37 108.5 . . ? C38 C37 H37 108.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C101 C100 H10D 109.5 . . ? C101 C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C101 C100 H10F 109.5 . . ? H10D C100 H10F 109.5 . . ? H10E C100 H10F 109.5 . . ? C102 C101 C106 121.0(8) . . ? C102 C101 C100 119.7(10) . . ? C106 C101 C100 119.4(9) . . ? C101 C102 C103 120.5(8) . . ? C101 C102 H102 119.7 . . ? C103 C102 H102 119.7 . . ? C102 C103 C104 119.4(8) . . ? C102 C103 H103 120.3 . . ? C104 C103 H103 120.3 . . ? C105 C104 C103 119.0(8) . . ? C105 C104 H104 120.5 . . ? C103 C104 H104 120.5 . . ? C104 C105 C106 120.5(6) . . ? C104 C105 H105 119.8 . . ? C106 C105 H105 119.8 . . ? C101 C106 C105 119.6(7) . . ? C101 C106 H106 120.2 . . ? C105 C106 H106 120.2 . . ? C110 C108 C109 121(2) 3_655 . ? C110 C108 C107 120(2) 3_655 . ? C109 C108 C107 119(2) . . ? C110 C109 C118 122.2(13) . . ? C110 C109 C108 119.2(14) . . ? C118 C109 C108 3(3) . . ? C110 C109 H109 120.4 . . ? C118 C109 H109 117.4 . . ? C108 C109 H109 120.4 . . ? C108 C110 C109 119.6(13) 3_655 . ? C108 C110 C118 1(2) 3_655 3_655 ? C109 C110 C118 121.0(11) . 3_655 ? C108 C110 H110 120.2 3_655 . ? C109 C110 H110 120.2 . . ? C118 C110 H110 118.8 3_655 . ? C109 C118 C110 117(2) . 3_655 ? C109 C118 H118 121.6 . . ? C110 C118 H118 121.6 3_655 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.407 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.091 #===END data_Zr(2)(OiPr) _database_code_depnum_ccdc_archive 'CCDC 736074' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H136 N2 O8 Zr2' _chemical_formula_weight 1592.48 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 11.3349(3) _cell_length_b 13.6262(3) _cell_length_c 15.5329(4) _cell_angle_alpha 103.5680(10) _cell_angle_beta 101.1950(10) _cell_angle_gamma 96.8930(10) _cell_volume 2253.01(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9114 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 24.11 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The solvent of crystallisation are disordered. Attempts to model further were unsuccessful thus resulting in ellipsoids with higher than desirable ADPs. ; _diffrn_ambient_temperature 150(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_type 'Nonius Kappa CCD' _diffrn_measurement_method '120 2.0 degree images with \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16004 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 24.03 _reflns_number_total 6964 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.4611P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6964 _refine_ls_number_parameters 505 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr -0.04179(2) 0.61883(2) 0.473819(19) 0.02478(10) Uani 1 1 d . . . O1 O -0.20674(17) 0.60288(16) 0.48711(13) 0.0338(5) Uani 1 1 d . . . N1 N 0.1535(2) 0.65219(16) 0.43189(15) 0.0248(5) Uani 1 1 d . . . C1 C -0.3253(3) 0.6006(3) 0.5054(2) 0.0405(8) Uani 1 1 d . . . H1 H -0.3312 0.5607 0.5513 0.049 Uiso 1 1 calc R . . O2 O 0.03922(17) 0.74817(14) 0.56628(13) 0.0300(5) Uani 1 1 d . . . C2 C -0.4201(3) 0.5469(3) 0.4192(3) 0.0565(10) Uani 1 1 d . . . H2A H -0.4159 0.5854 0.3736 0.085 Uiso 1 1 calc R . . H2B H -0.5015 0.5430 0.4322 0.085 Uiso 1 1 calc R . . H2C H -0.4046 0.4775 0.3958 0.085 Uiso 1 1 calc R . . O3 O 0.00704(16) 0.47333(14) 0.41978(12) 0.0255(4) Uani 1 1 d . . . C3 C -0.3426(4) 0.7089(3) 0.5454(3) 0.0675(12) Uani 1 1 d . . . H3A H -0.2764 0.7416 0.5991 0.101 Uiso 1 1 calc R . . H3B H -0.4211 0.7073 0.5631 0.101 Uiso 1 1 calc R . . H3C H -0.3416 0.7481 0.5000 0.101 Uiso 1 1 calc R . . O4 O -0.08761(17) 0.65096(14) 0.35443(12) 0.0279(4) Uani 1 1 d . . . C4 C 0.1445(3) 0.8191(2) 0.59662(19) 0.0294(7) Uani 1 1 d . . . C5 C 0.1457(3) 0.9210(2) 0.6447(2) 0.0341(7) Uani 1 1 d . . . C6 C 0.2574(3) 0.9868(2) 0.6706(2) 0.0390(8) Uani 1 1 d . . . H6 H 0.2599 1.0556 0.7033 0.047 Uiso 1 1 calc R . . C7 C 0.3660(3) 0.9593(2) 0.6520(2) 0.0344(7) Uani 1 1 d . . . C8 C 0.3605(3) 0.8588(2) 0.60335(19) 0.0307(7) Uani 1 1 d . . . H8 H 0.4326 0.8373 0.5887 0.037 Uiso 1 1 calc R . . C9 C 0.2518(3) 0.7890(2) 0.57560(18) 0.0275(6) Uani 1 1 d . . . C10 C 0.0305(3) 0.9583(2) 0.6701(3) 0.0481(9) Uani 1 1 d . . . C11 C -0.0729(4) 0.9420(4) 0.5833(3) 0.0759(13) Uani 1 1 d . . . H11A H -0.0496 0.9885 0.5477 0.114 Uiso 1 1 calc R . . H11B H -0.1487 0.9563 0.6012 0.114 Uiso 1 1 calc R . . H11C H -0.0854 0.8709 0.5465 0.114 Uiso 1 1 calc R . . C12 C -0.0174(4) 0.8996(3) 0.7318(3) 0.0643(12) Uani 1 1 d . . . H12A H -0.0472 0.8277 0.6980 0.097 Uiso 1 1 calc R . . H12B H -0.0845 0.9297 0.7528 0.097 Uiso 1 1 calc R . . H12C H 0.0485 0.9036 0.7844 0.097 Uiso 1 1 calc R . . C13 C 0.0557(4) 1.0731(3) 0.7182(4) 0.0855(17) Uani 1 1 d . . . H13A H 0.1176 1.0864 0.7752 0.128 Uiso 1 1 calc R . . H13B H -0.0198 1.0944 0.7316 0.128 Uiso 1 1 calc R . . H13C H 0.0854 1.1119 0.6787 0.128 Uiso 1 1 calc R . . C14 C 0.4841(3) 1.0393(2) 0.6833(2) 0.0438(8) Uani 1 1 d . . . C15 C 0.5061(4) 1.0893(3) 0.7863(2) 0.0556(10) Uani 1 1 d . . . H15A H 0.5808 1.1409 0.8062 0.083 Uiso 1 1 calc R . . H15B H 0.5149 1.0366 0.8194 0.083 Uiso 1 1 calc R . . H15C H 0.4366 1.1221 0.7987 0.083 Uiso 1 1 calc R . . C16 C 0.4697(4) 1.1217(3) 0.6316(3) 0.0585(10) Uani 1 1 d . . . H16A H 0.4620 1.0910 0.5666 0.088 Uiso 1 1 calc R . . H16B H 0.5416 1.1762 0.6548 0.088 Uiso 1 1 calc R . . H16C H 0.3964 1.1505 0.6403 0.088 Uiso 1 1 calc R . . C17 C 0.5966(3) 0.9917(3) 0.6664(3) 0.0617(12) Uani 1 1 d . . . H17A H 0.5863 0.9616 0.6010 0.093 Uiso 1 1 calc R . . H17B H 0.6055 0.9382 0.6986 0.093 Uiso 1 1 calc R . . H17C H 0.6697 1.0450 0.6889 0.093 Uiso 1 1 calc R . . C18 C 0.2490(3) 0.6817(2) 0.51938(18) 0.0279(6) Uani 1 1 d . . . H18A H 0.3300 0.6765 0.5055 0.033 Uiso 1 1 calc R . . H18B H 0.2330 0.6326 0.5555 0.033 Uiso 1 1 calc R . . C19 C 0.1679(2) 0.5571(2) 0.36992(18) 0.0242(6) Uani 1 1 d . . . C20 C 0.0854(2) 0.4699(2) 0.36194(18) 0.0252(6) Uani 1 1 d . . . C21 C 0.0861(3) 0.3797(2) 0.29781(19) 0.0300(7) Uani 1 1 d . . . H21 H 0.0280 0.3201 0.2900 0.036 Uiso 1 1 calc R . . C22 C 0.1720(3) 0.3774(2) 0.24541(19) 0.0314(7) Uani 1 1 d . . . H22 H 0.1727 0.3152 0.2024 0.038 Uiso 1 1 calc R . . C23 C 0.2573(3) 0.4632(2) 0.25374(19) 0.0303(7) Uani 1 1 d . . . C24 C 0.2536(3) 0.5539(2) 0.31714(18) 0.0274(6) Uani 1 1 d . . . H24 H 0.3105 0.6139 0.3241 0.033 Uiso 1 1 calc R . . C25 C 0.3479(3) 0.4597(2) 0.1946(2) 0.0404(8) Uani 1 1 d . . . H25A H 0.4120 0.4230 0.2160 0.061 Uiso 1 1 calc R . . H25B H 0.3845 0.5298 0.1978 0.061 Uiso 1 1 calc R . . H25C H 0.3062 0.4241 0.1315 0.061 Uiso 1 1 calc R . . C26 C 0.1547(3) 0.7378(2) 0.38632(19) 0.0274(6) Uani 1 1 d . . . H26A H 0.1270 0.7961 0.4236 0.033 Uiso 1 1 calc R . . H26B H 0.2394 0.7613 0.3831 0.033 Uiso 1 1 calc R . . C27 C 0.0744(3) 0.7065(2) 0.29217(18) 0.0262(6) Uani 1 1 d . . . C28 C -0.0485(3) 0.6650(2) 0.27998(19) 0.0258(6) Uani 1 1 d . . . C29 C -0.1283(3) 0.6398(2) 0.19335(19) 0.0279(6) Uani 1 1 d . . . C30 C -0.0770(3) 0.6559(2) 0.1218(2) 0.0344(7) Uani 1 1 d . . . H30 H -0.1292 0.6388 0.0627 0.041 Uiso 1 1 calc R . . C31 C 0.0451(3) 0.6953(2) 0.1312(2) 0.0354(7) Uani 1 1 d . A . C32 C 0.1193(3) 0.7203(2) 0.21820(19) 0.0301(7) Uani 1 1 d . . . H32 H 0.2032 0.7476 0.2273 0.036 Uiso 1 1 calc R . . C33 C -0.2641(3) 0.5993(2) 0.1793(2) 0.0339(7) Uani 1 1 d . . . C34 C -0.3353(3) 0.5813(3) 0.0804(2) 0.0507(9) Uani 1 1 d . . . H34A H -0.3259 0.6456 0.0625 0.076 Uiso 1 1 calc R . . H34B H -0.4220 0.5573 0.0756 0.076 Uiso 1 1 calc R . . H34C H -0.3035 0.5295 0.0402 0.076 Uiso 1 1 calc R . . C35 C -0.3212(3) 0.6778(2) 0.2390(2) 0.0373(7) Uani 1 1 d . . . H35A H -0.2806 0.6892 0.3031 0.056 Uiso 1 1 calc R . . H35B H -0.4084 0.6518 0.2300 0.056 Uiso 1 1 calc R . . H35C H -0.3112 0.7427 0.2220 0.056 Uiso 1 1 calc R . . C36 C -0.2807(3) 0.4959(2) 0.2035(2) 0.0427(8) Uani 1 1 d . . . H36A H -0.2421 0.4472 0.1658 0.064 Uiso 1 1 calc R . . H36B H -0.3680 0.4689 0.1922 0.064 Uiso 1 1 calc R . . H36C H -0.2424 0.5058 0.2679 0.064 Uiso 1 1 calc R . . C37 C 0.0976(3) 0.7114(3) 0.0510(2) 0.0493(9) Uani 1 1 d D . . C38 C 0.2152(4) 0.6610(4) 0.0517(3) 0.0570(14) Uani 0.847(6) 1 d PD A 1 H38A H 0.2719 0.6882 0.1113 0.085 Uiso 0.847(6) 1 calc PR A 1 H38B H 0.2546 0.6768 0.0045 0.085 Uiso 0.847(6) 1 calc PR A 1 H38C H 0.1924 0.5865 0.0396 0.085 Uiso 0.847(6) 1 calc PR A 1 C39 C 0.0124(5) 0.6658(6) -0.0390(3) 0.081(2) Uani 0.847(6) 1 d PD A 1 H39A H 0.0519 0.6789 -0.0870 0.121 Uiso 0.847(6) 1 calc PR A 1 H39B H -0.0616 0.6966 -0.0413 0.121 Uiso 0.847(6) 1 calc PR A 1 H39C H -0.0094 0.5917 -0.0482 0.121 Uiso 0.847(6) 1 calc PR A 1 C40 C 0.1408(5) 0.8271(4) 0.0668(3) 0.0600(15) Uani 0.847(6) 1 d PD A 1 H40A H 0.1975 0.8544 0.1265 0.090 Uiso 0.847(6) 1 calc PR A 1 H40B H 0.0701 0.8622 0.0648 0.090 Uiso 0.847(6) 1 calc PR A 1 H40C H 0.1823 0.8383 0.0193 0.090 Uiso 0.847(6) 1 calc PR A 1 C38A C 0.048(3) 0.6103(16) -0.0294(16) 0.049(7) Uiso 0.153(6) 1 d PD A 2 H38D H -0.0404 0.5922 -0.0383 0.074 Uiso 0.153(6) 1 calc PR A 2 H38E H 0.0872 0.5542 -0.0141 0.074 Uiso 0.153(6) 1 calc PR A 2 H38F H 0.0674 0.6219 -0.0855 0.074 Uiso 0.153(6) 1 calc PR A 2 C39A C 0.012(2) 0.7796(17) 0.0034(16) 0.051(7) Uiso 0.153(6) 1 d PD A 2 H39D H -0.0727 0.7587 0.0055 0.076 Uiso 0.153(6) 1 calc PR A 2 H39E H 0.0181 0.7693 -0.0602 0.076 Uiso 0.153(6) 1 calc PR A 2 H39F H 0.0397 0.8522 0.0358 0.076 Uiso 0.153(6) 1 calc PR A 2 C40A C 0.2210(17) 0.756(2) 0.061(2) 0.068(9) Uiso 0.153(6) 1 d PD A 2 H40D H 0.2336 0.7647 0.0026 0.102 Uiso 0.153(6) 1 calc PR A 2 H40E H 0.2751 0.7115 0.0824 0.102 Uiso 0.153(6) 1 calc PR A 2 H40F H 0.2394 0.8232 0.1059 0.102 Uiso 0.153(6) 1 calc PR A 2 C51 C 0.6709(17) 0.211(2) 0.1751(17) 0.157(8) Uiso 0.50 1 d PD B 1 H51A H 0.6866 0.1895 0.2318 0.236 Uiso 0.50 1 calc PR B 1 H51B H 0.7009 0.2843 0.1880 0.236 Uiso 0.50 1 calc PR B 1 H51C H 0.7134 0.1727 0.1324 0.236 Uiso 0.50 1 calc PR B 1 C52 C 0.5362(12) 0.1882(12) 0.1338(12) 0.127(6) Uiso 0.50 1 d PGD B 1 C53 C 0.5021(17) 0.1515(13) 0.0396(11) 0.200(11) Uiso 0.50 1 d PG B 1 H53 H 0.5624 0.1505 0.0047 0.240 Uiso 0.50 1 calc PR B 1 C54 C 0.380(2) 0.1165(14) -0.0037(8) 0.198(11) Uiso 0.50 1 d PG B 1 H54 H 0.3564 0.0915 -0.0681 0.238 Uiso 0.50 1 calc PR B 1 C55 C 0.2914(13) 0.1180(14) 0.0473(12) 0.31(2) Uiso 0.50 1 d PG B 1 H55 H 0.2078 0.0941 0.0177 0.371 Uiso 0.50 1 calc PR B 1 C56 C 0.3256(13) 0.1547(11) 0.1415(12) 0.166(7) Uiso 0.50 1 d PG B 1 H56 H 0.2653 0.1557 0.1763 0.199 Uiso 0.50 1 calc PR B 1 C57 C 0.4479(15) 0.1897(10) 0.1848(8) 0.181(7) Uiso 0.50 1 d PG B 1 H57 H 0.4713 0.2147 0.2492 0.217 Uiso 0.50 1 calc PR B 1 C61 C 0.182(2) 0.0741(16) -0.0125(14) 0.084(6) Uiso 0.25 1 d PD C 2 H61A H 0.1028 0.0446 -0.0049 0.126 Uiso 0.25 1 calc PR C 2 H61B H 0.2118 0.0224 -0.0545 0.126 Uiso 0.25 1 calc PR C 2 H61C H 0.1732 0.1333 -0.0373 0.126 Uiso 0.25 1 calc PR C 2 C62 C 0.273(2) 0.1080(18) 0.0790(15) 0.090(7) Uiso 0.25 1 d PD C 2 H62A H 0.2901 0.0503 0.1054 0.108 Uiso 0.25 1 calc PR C 2 H62B H 0.2492 0.1624 0.1236 0.108 Uiso 0.25 1 calc PR C 2 C63 C 0.376(3) 0.148(6) 0.040(3) 0.20(3) Uiso 0.25 1 d PD C 2 H63A H 0.3608 0.2111 0.0212 0.240 Uiso 0.25 1 calc PR C 2 H63B H 0.3852 0.0959 -0.0138 0.240 Uiso 0.25 1 calc PR C 2 C64 C 0.488(2) 0.1703(18) 0.1180(15) 0.075(6) Uiso 0.25 1 d PD C 2 H64A H 0.4725 0.2237 0.1678 0.082 Uiso 0.25 1 calc PR C 2 H64B H 0.4887 0.1074 0.1394 0.090 Uiso 0.25 1 calc PR C 2 C65 C 0.6151(15) 0.2031(15) 0.1110(12) 0.069(5) Uiso 0.25 1 d PD C 2 H65A H 0.6131 0.2654 0.0888 0.082 Uiso 0.25 1 calc PR C 2 H65B H 0.6294 0.1494 0.0608 0.082 Uiso 0.25 1 calc PR C 2 C66 C 0.7329(15) 0.2273(15) 0.1870(12) 0.050(4) Uiso 0.25 1 d PD C 2 H66A H 0.8035 0.2449 0.1623 0.075 Uiso 0.25 1 calc PR C 2 H66B H 0.7420 0.1672 0.2104 0.075 Uiso 0.25 1 calc PR C 2 H66C H 0.7279 0.2853 0.2365 0.075 Uiso 0.25 1 calc PR C 2 C71 C 0.166(2) 0.0880(18) 0.0412(18) 0.095(7) Uiso 0.25 1 d PD D 3 H71A H 0.0965 0.0463 -0.0065 0.142 Uiso 0.25 1 calc PR D 3 H71B H 0.1491 0.1575 0.0619 0.142 Uiso 0.25 1 calc PR D 3 H71C H 0.1787 0.0571 0.0925 0.142 Uiso 0.25 1 calc PR D 3 C72 C 0.278(3) 0.093(4) 0.004(3) 0.24(3) Uiso 0.25 1 d PD D 3 H72A H 0.2631 0.1231 -0.0482 0.283 Uiso 0.25 1 calc PR D 3 H72B H 0.2909 0.0216 -0.0198 0.283 Uiso 0.25 1 calc PR D 3 C73 C 0.396(3) 0.152(3) 0.069(3) 0.107(10) Uiso 0.25 1 d PD D 3 H73A H 0.3820 0.1500 0.1300 0.129 Uiso 0.25 1 calc PR D 3 H73B H 0.3937 0.2240 0.0668 0.129 Uiso 0.25 1 calc PR D 3 C74 C 0.529(3) 0.142(3) 0.077(3) 0.181(17) Uiso 0.25 1 d PD D 3 H74A H 0.5615 0.1635 0.0279 0.217 Uiso 0.25 1 calc PR D 3 H74B H 0.5434 0.0726 0.0779 0.217 Uiso 0.25 1 calc PR D 3 C75 C 0.576(3) 0.220(3) 0.169(2) 0.120(10) Uiso 0.25 1 d PD D 3 H75A H 0.5457 0.2008 0.2193 0.144 Uiso 0.25 1 calc PR D 3 H75B H 0.5690 0.2917 0.1688 0.144 Uiso 0.25 1 calc PR D 3 C76 C 0.701(2) 0.192(2) 0.1604(18) 0.075(7) Uiso 0.25 1 d PD D 3 H76A H 0.7617 0.2277 0.2166 0.113 Uiso 0.25 1 calc PR D 3 H76B H 0.7240 0.2133 0.1090 0.113 Uiso 0.25 1 calc PR D 3 H76C H 0.6961 0.1180 0.1502 0.113 Uiso 0.25 1 calc PR D 3 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 Zr 0.01674(15) 0.02920(16) 0.03006(16) 0.00852(11) 0.00756(11) 0.00548(11) O1 0.0181(11) 0.0493(12) 0.0405(12) 0.0188(10) 0.0113(9) 0.0099(9) N1 0.0200(13) 0.0251(11) 0.0274(12) 0.0031(10) 0.0049(10) 0.0055(9) C1 0.0153(16) 0.066(2) 0.051(2) 0.0297(17) 0.0140(14) 0.0137(15) O2 0.0254(11) 0.0302(10) 0.0370(11) 0.0069(9) 0.0139(9) 0.0074(8) C2 0.0208(18) 0.092(3) 0.064(2) 0.040(2) 0.0074(17) 0.0049(18) O3 0.0189(10) 0.0308(10) 0.0268(10) 0.0060(8) 0.0077(8) 0.0031(8) C3 0.045(2) 0.080(3) 0.093(3) 0.027(2) 0.031(2) 0.034(2) O4 0.0205(10) 0.0341(10) 0.0317(11) 0.0121(9) 0.0073(8) 0.0058(8) C4 0.0263(16) 0.0304(15) 0.0319(16) 0.0072(13) 0.0095(13) 0.0041(13) C5 0.0372(19) 0.0277(15) 0.0424(18) 0.0080(13) 0.0193(15) 0.0110(13) C6 0.044(2) 0.0262(15) 0.0455(19) 0.0001(14) 0.0182(16) 0.0055(14) C7 0.0324(18) 0.0319(16) 0.0348(17) 0.0027(13) 0.0082(14) 0.0019(13) C8 0.0254(16) 0.0337(16) 0.0302(15) 0.0030(13) 0.0063(13) 0.0049(13) C9 0.0269(16) 0.0300(15) 0.0247(14) 0.0037(12) 0.0062(12) 0.0075(12) C10 0.044(2) 0.0271(16) 0.081(3) 0.0074(17) 0.038(2) 0.0109(14) C11 0.051(3) 0.089(3) 0.113(4) 0.040(3) 0.042(3) 0.041(2) C12 0.076(3) 0.048(2) 0.089(3) 0.017(2) 0.060(3) 0.022(2) C13 0.077(3) 0.0300(19) 0.163(5) 0.007(2) 0.079(3) 0.0160(19) C14 0.0346(19) 0.0331(17) 0.053(2) -0.0047(15) 0.0097(16) -0.0020(14) C15 0.050(2) 0.046(2) 0.054(2) -0.0062(18) 0.0017(18) -0.0030(17) C16 0.056(2) 0.047(2) 0.068(3) 0.0072(19) 0.024(2) -0.0089(18) C17 0.030(2) 0.052(2) 0.082(3) -0.015(2) 0.0100(19) -0.0058(16) C18 0.0212(15) 0.0321(15) 0.0272(15) 0.0021(12) 0.0044(12) 0.0058(12) C19 0.0193(14) 0.0258(14) 0.0255(14) 0.0038(12) 0.0034(11) 0.0058(11) C20 0.0192(15) 0.0327(15) 0.0248(14) 0.0085(12) 0.0048(12) 0.0070(12) C21 0.0292(17) 0.0279(15) 0.0301(15) 0.0033(12) 0.0077(13) 0.0018(12) C22 0.0320(17) 0.0322(15) 0.0270(15) 0.0011(13) 0.0076(13) 0.0063(13) C23 0.0224(16) 0.0388(16) 0.0289(15) 0.0050(13) 0.0071(12) 0.0089(13) C24 0.0187(15) 0.0324(15) 0.0296(15) 0.0072(13) 0.0047(12) 0.0028(12) C25 0.0344(19) 0.0462(18) 0.0400(18) 0.0028(15) 0.0177(15) 0.0070(15) C26 0.0208(15) 0.0280(14) 0.0356(16) 0.0097(12) 0.0100(12) 0.0044(12) C27 0.0249(16) 0.0242(14) 0.0305(15) 0.0058(12) 0.0086(12) 0.0076(12) C28 0.0241(16) 0.0267(14) 0.0314(15) 0.0100(12) 0.0117(12) 0.0092(12) C29 0.0241(16) 0.0273(14) 0.0307(15) 0.0043(12) 0.0060(12) 0.0053(12) C30 0.0329(18) 0.0408(17) 0.0263(15) 0.0055(13) 0.0044(13) 0.0052(14) C31 0.0353(19) 0.0378(17) 0.0329(17) 0.0069(14) 0.0107(14) 0.0057(14) C32 0.0257(16) 0.0305(15) 0.0342(16) 0.0077(13) 0.0092(13) 0.0032(12) C33 0.0257(17) 0.0383(16) 0.0339(16) 0.0040(13) 0.0056(13) 0.0040(13) C34 0.0303(19) 0.071(2) 0.0381(18) 0.0029(17) -0.0023(15) -0.0007(17) C35 0.0239(17) 0.0418(17) 0.0449(18) 0.0094(15) 0.0057(14) 0.0082(13) C36 0.0304(18) 0.0383(17) 0.053(2) 0.0006(16) 0.0133(15) -0.0014(14) C37 0.051(2) 0.063(2) 0.0360(18) 0.0122(17) 0.0194(16) 0.0021(18) C38 0.052(3) 0.075(3) 0.042(2) 0.002(2) 0.027(2) 0.006(2) C39 0.054(3) 0.149(7) 0.030(2) 0.021(3) 0.011(2) -0.013(4) C40 0.059(3) 0.079(3) 0.055(3) 0.037(2) 0.024(2) 0.006(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 Zr O1 1.9129(19) . ? Zr O2 1.9808(19) . ? Zr O4 1.9904(19) . ? Zr O3 2.1458(18) . ? Zr O3 2.3030(19) 2_566 ? Zr N1 2.447(2) . ? O1 C1 1.425(3) . ? N1 C19 1.469(3) . ? N1 C18 1.499(3) . ? N1 C26 1.499(4) . ? C1 C2 1.508(5) . ? C1 C3 1.514(5) . ? C1 H1 1.0000 . ? O2 C4 1.368(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C20 1.378(3) . ? O3 Zr 2.3030(19) 2_566 ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C28 1.361(3) . ? C4 C9 1.402(4) . ? C4 C5 1.412(4) . ? C5 C6 1.389(4) . ? C5 C10 1.544(4) . ? C6 C7 1.391(4) . ? C6 H6 0.9500 . ? C7 C8 1.388(4) . ? C7 C14 1.537(4) . ? C8 C9 1.389(4) . ? C8 H8 0.9500 . ? C9 C18 1.510(4) . ? C10 C12 1.520(5) . ? C10 C13 1.532(4) . ? C10 C11 1.556(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.532(5) . ? C14 C17 1.537(5) . ? C14 C15 1.543(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.386(4) . ? C19 C20 1.386(4) . ? C20 C21 1.390(4) . ? C21 C22 1.384(4) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.398(4) . ? C23 C25 1.503(4) . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.498(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.385(4) . ? C27 C28 1.398(4) . ? C28 C29 1.408(4) . ? C29 C30 1.399(4) . ? C29 C33 1.526(4) . ? C30 C31 1.389(4) . ? C30 H30 0.9500 . ? C31 C32 1.387(4) . ? C31 C37 1.530(4) . ? C32 H32 0.9500 . ? C33 C35 1.536(4) . ? C33 C34 1.538(4) . ? C33 C36 1.541(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C40A 1.420(17) . ? C37 C39 1.482(5) . ? C37 C40 1.540(6) . ? C37 C38 1.570(6) . ? C37 C38A 1.583(16) . ? C37 C39A 1.615(16) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C51 C52 1.501(16) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 C57 1.3900 . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C61 C62 1.518(17) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.52(2) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.53(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.488(18) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.544(16) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C72 1.50(2) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.51(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.51(2) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.52(2) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.525(19) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr O2 103.92(8) . . ? O1 Zr O4 92.87(8) . . ? O2 Zr O4 107.91(8) . . ? O1 Zr O3 111.15(8) . . ? O2 Zr O3 136.43(7) . . ? O4 Zr O3 95.55(7) . . ? O1 Zr O3 85.63(8) . 2_566 ? O2 Zr O3 91.10(7) . 2_566 ? O4 Zr O3 160.68(7) . 2_566 ? O3 Zr O3 67.32(8) . 2_566 ? O1 Zr N1 168.86(8) . . ? O2 Zr N1 78.16(7) . . ? O4 Zr N1 76.16(8) . . ? O3 Zr N1 72.44(7) . . ? O3 Zr N1 105.35(7) 2_566 . ? C1 O1 Zr 173.7(2) . . ? C19 N1 C18 112.1(2) . . ? C19 N1 C26 110.6(2) . . ? C18 N1 C26 110.6(2) . . ? C19 N1 Zr 107.37(15) . . ? C18 N1 Zr 105.75(16) . . ? C26 N1 Zr 110.24(15) . . ? O1 C1 C2 109.4(3) . . ? O1 C1 C3 109.2(3) . . ? C2 C1 C3 112.7(3) . . ? O1 C1 H1 108.5 . . ? C2 C1 H1 108.5 . . ? C3 C1 H1 108.5 . . ? C4 O2 Zr 143.55(17) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C20 O3 Zr 117.56(16) . . ? C20 O3 Zr 116.23(15) . 2_566 ? Zr O3 Zr 112.68(8) . 2_566 ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C28 O4 Zr 145.46(17) . . ? O2 C4 C9 118.1(2) . . ? O2 C4 C5 121.6(3) . . ? C9 C4 C5 120.3(3) . . ? C6 C5 C4 116.5(3) . . ? C6 C5 C10 120.9(3) . . ? C4 C5 C10 122.5(3) . . ? C5 C6 C7 124.8(3) . . ? C5 C6 H6 117.6 . . ? C7 C6 H6 117.6 . . ? C8 C7 C6 116.9(3) . . ? C8 C7 C14 123.0(3) . . ? C6 C7 C14 120.1(3) . . ? C7 C8 C9 121.3(3) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 120.2(3) . . ? C8 C9 C18 119.5(3) . . ? C4 C9 C18 120.2(3) . . ? C12 C10 C13 108.7(3) . . ? C12 C10 C5 110.8(3) . . ? C13 C10 C5 111.8(3) . . ? C12 C10 C11 108.0(3) . . ? C13 C10 C11 106.7(4) . . ? C5 C10 C11 110.7(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C17 109.1(3) . . ? C16 C14 C7 108.8(3) . . ? C17 C14 C7 112.4(3) . . ? C16 C14 C15 109.4(3) . . ? C17 C14 C15 107.8(3) . . ? C7 C14 C15 109.3(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C9 112.8(2) . . ? N1 C18 H18A 109.0 . . ? C9 C18 H18A 109.0 . . ? N1 C18 H18B 109.0 . . ? C9 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C24 C19 C20 120.5(2) . . ? C24 C19 N1 122.9(2) . . ? C20 C19 N1 116.5(2) . . ? O3 C20 C19 119.3(2) . . ? O3 C20 C21 121.2(2) . . ? C19 C20 C21 119.4(3) . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 122.0(3) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C24 117.7(3) . . ? C22 C23 C25 121.1(3) . . ? C24 C23 C25 121.1(3) . . ? C19 C24 C23 120.8(3) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 N1 112.6(2) . . ? C27 C26 H26A 109.1 . . ? N1 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? N1 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C32 C27 C28 119.9(3) . . ? C32 C27 C26 121.2(3) . . ? C28 C27 C26 118.8(2) . . ? O4 C28 C27 117.8(2) . . ? O4 C28 C29 121.7(2) . . ? C27 C28 C29 120.5(3) . . ? C30 C29 C28 116.4(3) . . ? C30 C29 C33 122.1(3) . . ? C28 C29 C33 121.4(3) . . ? C31 C30 C29 124.6(3) . . ? C31 C30 H30 117.7 . . ? C29 C30 H30 117.7 . . ? C32 C31 C30 116.6(3) . . ? C32 C31 C37 120.5(3) . . ? C30 C31 C37 122.9(3) . . ? C27 C32 C31 121.9(3) . . ? C27 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C29 C33 C35 109.5(2) . . ? C29 C33 C34 112.8(3) . . ? C35 C33 C34 106.9(3) . . ? C29 C33 C36 109.7(2) . . ? C35 C33 C36 110.5(3) . . ? C34 C33 C36 107.3(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C40A C37 C39 123.0(12) . . ? C40A C37 C31 122.8(12) . . ? C39 C37 C31 113.9(3) . . ? C40A C37 C40 56.4(12) . . ? C39 C37 C40 111.7(4) . . ? C31 C37 C40 108.4(3) . . ? C40A C37 C38 49.6(12) . . ? C39 C37 C38 107.9(4) . . ? C31 C37 C38 108.6(3) . . ? C40 C37 C38 106.1(3) . . ? C40A C37 C38A 115.4(16) . . ? C39 C37 C38A 35.1(10) . . ? C31 C37 C38A 106.9(11) . . ? C40 C37 C38A 140.4(11) . . ? C38 C37 C38A 78.7(11) . . ? C40A C37 C39A 107.4(15) . . ? C39 C37 C39A 59.3(9) . . ? C31 C37 C39A 105.7(9) . . ? C40 C37 C39A 59.2(9) . . ? C38 C37 C39A 145.6(9) . . ? C38A C37 C39A 94.4(14) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C37 C38A H38D 109.5 . . ? C37 C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37 C39A H39D 109.5 . . ? C37 C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37 C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C37 C40A H40D 109.5 . . ? C37 C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C37 C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C53 C52 C57 120.0 . . ? C53 C52 C51 116.0(16) . . ? C57 C52 C51 123.5(15) . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 120.0 . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C57 C56 C55 120.0 . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C52 120.0 . . ? C56 C57 H57 120.0 . . ? C52 C57 H57 120.0 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C61 C62 C63 93(2) . . ? C61 C62 H62A 113.1 . . ? C63 C62 H62A 113.1 . . ? C61 C62 H62B 113.1 . . ? C63 C62 H62B 113.1 . . ? H62A C62 H62B 110.4 . . ? C62 C63 C64 103(2) . . ? C62 C63 H63A 111.1 . . ? C64 C63 H63A 111.1 . . ? C62 C63 H63B 111.1 . . ? C64 C63 H63B 111.1 . . ? H63A C63 H63B 109.0 . . ? C65 C64 C63 124.4(19) . . ? C65 C64 H64A 106.2 . . ? C63 C64 H64A 106.2 . . ? C65 C64 H64B 106.2 . . ? C63 C64 H64B 106.2 . . ? H64A C64 H64B 106.4 . . ? C64 C65 C66 127.4(18) . . ? C64 C65 H65A 105.5 . . ? C66 C65 H65A 105.5 . . ? C64 C65 H65B 105.5 . . ? C66 C65 H65B 105.5 . . ? H65A C65 H65B 106.0 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C71 C72 C73 117(3) . . ? C71 C72 H72A 108.1 . . ? C73 C72 H72A 108.1 . . ? C71 C72 H72B 108.1 . . ? C73 C72 H72B 108.1 . . ? H72A C72 H72B 107.3 . . ? C72 C73 C74 133(3) . . ? C72 C73 H73A 103.9 . . ? C74 C73 H73A 103.9 . . ? C72 C73 H73B 103.9 . . ? C74 C73 H73B 103.9 . . ? H73A C73 H73B 105.4 . . ? C73 C74 C75 96(3) . . ? C73 C74 H74A 112.6 . . ? C75 C74 H74A 112.6 . . ? C73 C74 H74B 112.6 . . ? C75 C74 H74B 112.6 . . ? H74A C74 H74B 110.1 . . ? C74 C75 C76 85(2) . . ? C74 C75 H75A 114.5 . . ? C76 C75 H75A 114.5 . . ? C74 C75 H75B 114.5 . . ? C76 C75 H75B 114.5 . . ? H75A C75 H75B 111.6 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.339 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.056 #===END data_Zr(3)(OiPr) _database_code_depnum_ccdc_archive 'CCDC 736075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H77 N O4 Zr,(C6 H14)' _chemical_formula_sum 'C98 H154 N2 O8 Zr2' _chemical_formula_weight 1670.75 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 11.6130(2) _cell_length_b 14.8593(2) _cell_length_c 16.3050(3) _cell_angle_alpha 67.635(2) _cell_angle_beta 76.3350(10) _cell_angle_gamma 67.9570(10) _cell_volume 2397.40(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40399 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The solvent of crystallisation are disordered. Attempts to model further were unsuccessful thus resulting in ellipsoids with higher than desirable ADPs. ; _diffrn_ambient_temperature 150(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_type 'Nonius Kappa CCD' _diffrn_measurement_method '364 1.5 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37660 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 25.04 _reflns_number_total 8406 _reflns_number_gt 6922 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+2.5406P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8406 _refine_ls_number_parameters 512 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr -0.06271(2) 0.07235(2) 0.391850(19) 0.02358(10) Uani 1 1 d . . . O1 O -0.23727(18) 0.11888(16) 0.43148(14) 0.0321(5) Uani 1 1 d . . . N1 N 0.1462(2) 0.00827(17) 0.31884(16) 0.0254(5) Uani 1 1 d . . . C1 C -0.3660(3) 0.1660(3) 0.4514(4) 0.0711(14) Uani 1 1 d . . . H1 H -0.3712 0.1757 0.5097 0.085 Uiso 1 1 calc R . . O2 O -0.09112(18) 0.01861(15) 0.30590(13) 0.0292(5) Uani 1 1 d . . . C2 C -0.4401(4) 0.1017(4) 0.4708(4) 0.0940(19) Uani 1 1 d . . . H2A H -0.4433 0.0902 0.4162 0.141 Uiso 1 1 calc R . . H2B H -0.5249 0.1347 0.4943 0.141 Uiso 1 1 calc R . . H2C H -0.4033 0.0358 0.5153 0.141 Uiso 1 1 calc R . . O3 O 0.02567(18) -0.07847(14) 0.47885(13) 0.0271(4) Uani 1 1 d . . . C3 C -0.4097(4) 0.2727(3) 0.3890(3) 0.0645(12) Uani 1 1 d . . . H3A H -0.3649 0.3138 0.3948 0.097 Uiso 1 1 calc R . . H3B H -0.4996 0.3030 0.4036 0.097 Uiso 1 1 calc R . . H3C H -0.3935 0.2715 0.3276 0.097 Uiso 1 1 calc R . . O4 O -0.02196(17) 0.20066(14) 0.31944(13) 0.0278(4) Uani 1 1 d . . . C4 C -0.0359(3) -0.0364(2) 0.2495(2) 0.0287(6) Uani 1 1 d . . . C5 C 0.0814(3) -0.0304(2) 0.20322(19) 0.0269(6) Uani 1 1 d . . . C6 C 0.1404(3) -0.0837(2) 0.14338(19) 0.0300(7) Uani 1 1 d . . . H6 H 0.2192 -0.0786 0.1123 0.036 Uiso 1 1 calc R . . C7 C 0.0875(3) -0.1447(2) 0.1274(2) 0.0343(7) Uani 1 1 d . . . C8 C -0.0270(3) -0.1512(2) 0.1755(2) 0.0368(7) Uani 1 1 d . . . H8 H -0.0638 -0.1933 0.1662 0.044 Uiso 1 1 calc R . . C9 C -0.0910(3) -0.0990(2) 0.2369(2) 0.0330(7) Uani 1 1 d . . . C10 C -0.2158(3) -0.1105(3) 0.2899(3) 0.0440(8) Uani 1 1 d . . . C11 C -0.3191(3) -0.0066(3) 0.2661(3) 0.0568(10) Uani 1 1 d . . . H11A H -0.2965 0.0435 0.2790 0.085 Uiso 1 1 calc R . . H11B H -0.3979 -0.0139 0.3015 0.085 Uiso 1 1 calc R . . H11C H -0.3290 0.0170 0.2025 0.085 Uiso 1 1 calc R . . C12 C -0.2029(4) -0.1524(3) 0.3905(3) 0.0567(10) Uani 1 1 d . . . H12A H -0.1323 -0.2161 0.4037 0.085 Uiso 1 1 calc R . . H12B H -0.2799 -0.1662 0.4240 0.085 Uiso 1 1 calc R . . H12C H -0.1884 -0.1016 0.4079 0.085 Uiso 1 1 calc R . . C13 C -0.2548(4) -0.1868(4) 0.2692(4) 0.0738(14) Uani 1 1 d . . . H13A H -0.2655 -0.1621 0.2056 0.111 Uiso 1 1 calc R . . H13B H -0.3338 -0.1931 0.3049 0.111 Uiso 1 1 calc R . . H13C H -0.1899 -0.2540 0.2837 0.111 Uiso 1 1 calc R . . C14 C 0.1533(3) -0.2004(3) 0.0583(2) 0.0419(8) Uani 1 1 d . . . C15 C 0.0948(5) -0.2787(5) 0.0637(4) 0.0886(18) Uani 1 1 d . . . H15A H 0.0126 -0.2431 0.0416 0.133 Uiso 1 1 calc R . . H15B H 0.0854 -0.3224 0.1259 0.133 Uiso 1 1 calc R . . H15C H 0.1488 -0.3213 0.0272 0.133 Uiso 1 1 calc R . . C16 C 0.1571(6) -0.1232(4) -0.0338(3) 0.0866(18) Uani 1 1 d . . . H16A H 0.2002 -0.1592 -0.0773 0.130 Uiso 1 1 calc R . . H16B H 0.2021 -0.0782 -0.0357 0.130 Uiso 1 1 calc R . . H16C H 0.0717 -0.0821 -0.0483 0.130 Uiso 1 1 calc R . . C17 C 0.2904(4) -0.2630(3) 0.0776(3) 0.0595(11) Uani 1 1 d . . . H17A H 0.2917 -0.3092 0.1394 0.089 Uiso 1 1 calc R . . H17B H 0.3365 -0.2161 0.0686 0.089 Uiso 1 1 calc R . . H17C H 0.3297 -0.3034 0.0370 0.089 Uiso 1 1 calc R . . C18 C 0.1404(3) 0.0339(2) 0.22107(19) 0.0277(6) Uani 1 1 d . . . H18A H 0.2261 0.0234 0.1898 0.033 Uiso 1 1 calc R . . H18B H 0.0918 0.1072 0.1964 0.033 Uiso 1 1 calc R . . C19 C 0.1911(3) -0.1030(2) 0.36246(19) 0.0254(6) Uani 1 1 d . . . C20 C 0.1225(3) -0.1445(2) 0.43995(19) 0.0258(6) Uani 1 1 d . . . C21 C 0.1546(3) -0.2500(2) 0.4788(2) 0.0306(7) Uani 1 1 d . . . H21 H 0.1051 -0.2793 0.5300 0.037 Uiso 1 1 calc R . . C22 C 0.2586(3) -0.3126(2) 0.4430(2) 0.0307(7) Uani 1 1 d . . . H22 H 0.2801 -0.3848 0.4709 0.037 Uiso 1 1 calc R . . C23 C 0.3338(3) -0.2730(2) 0.3666(2) 0.0282(6) Uani 1 1 d . . . C24 C 0.2964(3) -0.1668(2) 0.32688(19) 0.0265(6) Uani 1 1 d . . . H24 H 0.3436 -0.1372 0.2743 0.032 Uiso 1 1 calc R . . C25 C 0.4537(3) -0.3444(2) 0.3330(2) 0.0333(7) Uani 1 1 d . . . C26 C 0.4280(3) -0.4355(3) 0.3263(2) 0.0421(8) Uani 1 1 d . . . H26A H 0.4022 -0.4770 0.3859 0.063 Uiso 1 1 calc R . . H26B H 0.5041 -0.4778 0.3006 0.063 Uiso 1 1 calc R . . H26C H 0.3612 -0.4098 0.2880 0.063 Uiso 1 1 calc R . . C27 C 0.5505(3) -0.3841(3) 0.3992(2) 0.0429(8) Uani 1 1 d . . . H27A H 0.5692 -0.3261 0.4015 0.064 Uiso 1 1 calc R . . H27B H 0.6273 -0.4316 0.3796 0.064 Uiso 1 1 calc R . . H27C H 0.5167 -0.4199 0.4586 0.064 Uiso 1 1 calc R . . C28 C 0.5087(3) -0.2897(3) 0.2404(2) 0.0384(8) Uani 1 1 d . . . H28A H 0.4469 -0.2621 0.1980 0.058 Uiso 1 1 calc R . . H28B H 0.5839 -0.3385 0.2209 0.058 Uiso 1 1 calc R . . H28C H 0.5304 -0.2333 0.2433 0.058 Uiso 1 1 calc R . . C29 C 0.2244(3) 0.0598(2) 0.3344(2) 0.0300(7) Uani 1 1 d . . . H29A H 0.3137 0.0237 0.3201 0.036 Uiso 1 1 calc R . . H29B H 0.2112 0.0530 0.3985 0.036 Uiso 1 1 calc R . . C30 C 0.0728(3) 0.2386(2) 0.27264(19) 0.0259(6) Uani 1 1 d . . . C31 C 0.1957(3) 0.1726(2) 0.2796(2) 0.0280(6) Uani 1 1 d . . . C32 C 0.2948(3) 0.2101(2) 0.2348(2) 0.0293(7) Uani 1 1 d . . . H32 H 0.3780 0.1646 0.2401 0.035 Uiso 1 1 calc R . . C33 C 0.2748(3) 0.3123(2) 0.1826(2) 0.0308(7) Uani 1 1 d . . . C34 C 0.1509(3) 0.3746(2) 0.1734(2) 0.0315(7) Uani 1 1 d . . . H34 H 0.1358 0.4441 0.1361 0.038 Uiso 1 1 calc R . . C35 C 0.0481(3) 0.3413(2) 0.21545(19) 0.0274(6) Uani 1 1 d . . . C36 C 0.3825(3) 0.3574(2) 0.1355(2) 0.0377(8) Uani 1 1 d . . . C37 C 0.5103(3) 0.2760(3) 0.1490(3) 0.0469(9) Uani 1 1 d . . . H37A H 0.5201 0.2255 0.1209 0.070 Uiso 1 1 calc R . . H37B H 0.5175 0.2416 0.2130 0.070 Uiso 1 1 calc R . . H37C H 0.5757 0.3086 0.1219 0.070 Uiso 1 1 calc R . . C38 C 0.3709(4) 0.4077(3) 0.0359(3) 0.0531(10) Uani 1 1 d . . . H38A H 0.3734 0.3567 0.0106 0.080 Uiso 1 1 calc R . . H38B H 0.4404 0.4351 0.0065 0.080 Uiso 1 1 calc R . . H38C H 0.2915 0.4637 0.0263 0.080 Uiso 1 1 calc R . . C39 C 0.3753(4) 0.4377(3) 0.1758(3) 0.0520(10) Uani 1 1 d . . . H39A H 0.4447 0.4654 0.1478 0.078 Uiso 1 1 calc R . . H39B H 0.3807 0.4055 0.2401 0.078 Uiso 1 1 calc R . . H39C H 0.2958 0.4935 0.1651 0.078 Uiso 1 1 calc R . . C40 C -0.0864(3) 0.4123(2) 0.1971(2) 0.0330(7) Uani 1 1 d . . . C41 C -0.1448(3) 0.3657(3) 0.1549(3) 0.0478(9) Uani 1 1 d . . . H41A H -0.0939 0.3577 0.0994 0.072 Uiso 1 1 calc R . . H41B H -0.2296 0.4112 0.1421 0.072 Uiso 1 1 calc R . . H41C H -0.1483 0.2985 0.1964 0.072 Uiso 1 1 calc R . . C42 C -0.1658(3) 0.4258(3) 0.2842(2) 0.0413(8) Uani 1 1 d . . . H42A H -0.1698 0.3589 0.3261 0.062 Uiso 1 1 calc R . . H42B H -0.2505 0.4716 0.2714 0.062 Uiso 1 1 calc R . . H42C H -0.1278 0.4556 0.3108 0.062 Uiso 1 1 calc R . . C43 C -0.0897(3) 0.5196(3) 0.1331(3) 0.0483(9) Uani 1 1 d . . . H43A H -0.0545 0.5516 0.1593 0.073 Uiso 1 1 calc R . . H43B H -0.1764 0.5616 0.1225 0.073 Uiso 1 1 calc R . . H43C H -0.0404 0.5144 0.0764 0.073 Uiso 1 1 calc R . . C44 C 0.4352(4) 0.0387(4) -0.0140(3) 0.0687(12) Uani 1 1 d . . . H44A H 0.4419 0.0683 -0.0799 0.082 Uiso 1 1 calc R . . H44B H 0.3740 0.0009 0.0047 0.082 Uiso 1 1 calc R . . C45 C 0.3869(5) 0.1237(4) 0.0241(3) 0.0719(13) Uani 1 1 d . . . H45A H 0.4448 0.1647 0.0017 0.086 Uiso 1 1 calc R . . H45B H 0.3862 0.0941 0.0898 0.086 Uiso 1 1 calc R . . C46 C 0.2576(5) 0.1938(4) 0.0021(4) 0.0811(14) Uani 1 1 d . . . H46A H 0.2592 0.2295 -0.0623 0.122 Uiso 1 1 calc R . . H46B H 0.2289 0.2442 0.0336 0.122 Uiso 1 1 calc R . . H46C H 0.2004 0.1533 0.0208 0.122 Uiso 1 1 calc R . . C51 C -0.1737(13) 0.6248(10) 0.5989(10) 0.116(4) Uiso 0.50 1 d PD . . H51A H -0.1982 0.6387 0.6558 0.174 Uiso 0.50 1 calc PR . . H51B H -0.2486 0.6447 0.5700 0.174 Uiso 0.50 1 calc PR . . H51C H -0.1190 0.6645 0.5601 0.174 Uiso 0.50 1 calc PR . . C52 C -0.1108(14) 0.5212(11) 0.6143(11) 0.098(4) Uiso 0.50 1 d PD . . H52A H -0.1657 0.4847 0.6597 0.118 Uiso 0.50 1 calc PR . . H52B H -0.0366 0.5055 0.6434 0.118 Uiso 0.50 1 calc PR . . C53 C -0.065(4) 0.470(4) 0.544(3) 0.40(3) Uiso 0.50 1 d PD . . H53A H -0.0507 0.3950 0.5688 0.479 Uiso 0.50 1 calc PR . . H53B H -0.1201 0.5017 0.4957 0.479 Uiso 0.50 1 calc PR . . C54 C 0.047(2) 0.4951(19) 0.5177(16) 0.169(8) Uiso 0.50 1 d PD . . H54A H 0.1054 0.4557 0.5642 0.203 Uiso 0.50 1 calc PR . . H54B H 0.0310 0.5694 0.5039 0.203 Uiso 0.50 1 calc PR . . C55 C 0.098(4) 0.463(2) 0.4344(16) 0.32(2) Uiso 0.50 1 d PD . . H55A H 0.0601 0.4115 0.4385 0.390 Uiso 0.50 1 calc PR . . H55B H 0.1889 0.4283 0.4356 0.390 Uiso 0.50 1 calc PR . . C56 C 0.0761(17) 0.5483(15) 0.3416(12) 0.143(6) Uiso 0.50 1 d PD . . H56A H 0.1116 0.5171 0.2943 0.214 Uiso 0.50 1 calc PR . . H56B H 0.1168 0.5983 0.3344 0.214 Uiso 0.50 1 calc PR . . H56C H -0.0138 0.5830 0.3381 0.214 Uiso 0.50 1 calc PR . . 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 Zr 0.02087(15) 0.01985(15) 0.02658(16) -0.00769(11) 0.00038(10) -0.00439(11) O1 0.0226(10) 0.0330(12) 0.0363(12) -0.0134(10) -0.0007(9) -0.0032(9) N1 0.0265(12) 0.0152(12) 0.0303(13) -0.0045(10) -0.0017(10) -0.0059(10) C1 0.0222(18) 0.050(3) 0.115(4) -0.015(3) 0.002(2) -0.0007(17) O2 0.0292(11) 0.0291(11) 0.0290(11) -0.0122(9) 0.0003(9) -0.0084(9) C2 0.030(2) 0.093(4) 0.132(5) -0.017(4) 0.002(3) -0.017(2) O3 0.0276(10) 0.0197(10) 0.0302(11) -0.0087(8) -0.0022(8) -0.0034(8) C3 0.039(2) 0.053(3) 0.091(3) -0.021(2) -0.021(2) 0.0026(19) O4 0.0234(10) 0.0205(10) 0.0325(11) -0.0068(9) 0.0003(8) -0.0033(8) C4 0.0319(16) 0.0251(16) 0.0266(16) -0.0088(13) -0.0036(13) -0.0059(13) C5 0.0293(15) 0.0203(15) 0.0267(15) -0.0037(12) -0.0038(12) -0.0067(12) C6 0.0324(16) 0.0288(16) 0.0250(15) -0.0075(13) 0.0001(13) -0.0089(13) C7 0.0393(18) 0.0306(17) 0.0310(17) -0.0101(14) -0.0044(14) -0.0085(14) C8 0.0427(19) 0.0346(18) 0.0402(19) -0.0164(15) -0.0066(15) -0.0141(15) C9 0.0318(16) 0.0334(17) 0.0347(17) -0.0106(14) -0.0039(13) -0.0118(14) C10 0.0400(19) 0.053(2) 0.051(2) -0.0267(18) 0.0057(16) -0.0243(17) C11 0.0331(19) 0.076(3) 0.065(3) -0.032(2) -0.0009(18) -0.0156(19) C12 0.053(2) 0.066(3) 0.053(2) -0.017(2) 0.0144(19) -0.036(2) C13 0.065(3) 0.097(4) 0.096(4) -0.056(3) 0.022(3) -0.059(3) C14 0.046(2) 0.043(2) 0.0403(19) -0.0238(16) -0.0050(16) -0.0069(16) C15 0.076(3) 0.112(4) 0.123(5) -0.095(4) 0.016(3) -0.036(3) C16 0.125(4) 0.060(3) 0.035(2) -0.019(2) -0.012(3) 0.019(3) C17 0.056(2) 0.059(3) 0.062(3) -0.035(2) -0.007(2) 0.000(2) C18 0.0281(15) 0.0236(15) 0.0263(15) -0.0066(12) 0.0009(12) -0.0066(12) C19 0.0251(15) 0.0212(15) 0.0282(15) -0.0085(12) -0.0029(12) -0.0050(12) C20 0.0249(14) 0.0241(15) 0.0272(15) -0.0102(12) -0.0024(12) -0.0050(12) C21 0.0355(17) 0.0236(16) 0.0292(16) -0.0069(13) 0.0025(13) -0.0110(13) C22 0.0376(17) 0.0181(15) 0.0320(16) -0.0051(12) -0.0059(13) -0.0060(13) C23 0.0277(15) 0.0246(16) 0.0313(16) -0.0089(13) -0.0045(12) -0.0067(12) C24 0.0254(15) 0.0260(16) 0.0258(15) -0.0077(12) -0.0001(12) -0.0077(12) C25 0.0322(16) 0.0249(16) 0.0368(18) -0.0104(14) -0.0033(14) -0.0025(13) C26 0.045(2) 0.0308(18) 0.049(2) -0.0201(16) 0.0028(16) -0.0072(15) C27 0.0337(18) 0.0354(19) 0.047(2) -0.0097(16) -0.0054(15) -0.0006(15) C28 0.0331(17) 0.0319(18) 0.0430(19) -0.0163(15) 0.0021(14) -0.0022(14) C29 0.0249(15) 0.0227(15) 0.0399(18) -0.0087(13) -0.0063(13) -0.0049(12) C30 0.0243(14) 0.0214(15) 0.0298(16) -0.0096(12) 0.0008(12) -0.0057(12) C31 0.0275(15) 0.0197(15) 0.0342(17) -0.0068(12) -0.0054(13) -0.0057(12) C32 0.0254(15) 0.0240(16) 0.0352(17) -0.0080(13) -0.0003(13) -0.0075(12) C33 0.0321(16) 0.0256(16) 0.0355(17) -0.0110(13) 0.0003(13) -0.0112(13) C34 0.0374(17) 0.0176(15) 0.0333(17) -0.0046(13) -0.0013(13) -0.0073(13) C35 0.0307(16) 0.0201(15) 0.0276(15) -0.0079(12) -0.0016(12) -0.0050(12) C36 0.0369(18) 0.0297(17) 0.045(2) -0.0085(15) 0.0034(15) -0.0167(14) C37 0.0356(19) 0.044(2) 0.058(2) -0.0103(18) 0.0017(17) -0.0193(16) C38 0.051(2) 0.054(2) 0.045(2) -0.0020(18) 0.0023(18) -0.0265(19) C39 0.047(2) 0.039(2) 0.074(3) -0.0193(19) 0.0024(19) -0.0219(17) C40 0.0313(16) 0.0231(16) 0.0339(17) -0.0042(13) -0.0014(13) -0.0035(13) C41 0.043(2) 0.045(2) 0.049(2) -0.0097(17) -0.0168(17) -0.0060(17) C42 0.0354(18) 0.0289(18) 0.042(2) -0.0084(15) 0.0014(15) 0.0030(14) C43 0.0396(19) 0.0291(19) 0.051(2) 0.0014(16) -0.0028(16) -0.0001(15) C44 0.071(3) 0.070(3) 0.063(3) -0.010(2) -0.002(2) -0.034(2) C45 0.074(3) 0.071(3) 0.073(3) -0.024(3) 0.011(2) -0.036(3) C46 0.089(4) 0.071(3) 0.073(3) -0.014(3) -0.012(3) -0.022(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 Zr O1 1.9168(19) . ? Zr O4 1.9882(19) . ? Zr O2 1.994(2) . ? Zr O3 2.1518(19) . ? Zr O3 2.289(2) 2_556 ? Zr N1 2.444(2) . ? Zr Zr 3.6726(6) 2_556 ? O1 C1 1.410(4) . ? N1 C19 1.464(4) . ? N1 C29 1.502(4) . ? N1 C18 1.503(4) . ? C1 C2 1.419(6) . ? C1 C3 1.489(6) . ? C1 H1 1.0000 . ? O2 C4 1.351(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C20 1.392(3) . ? O3 Zr 2.289(2) 2_556 ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C30 1.361(3) . ? C4 C9 1.404(4) . ? C4 C5 1.409(4) . ? C5 C6 1.383(4) . ? C5 C18 1.505(4) . ? C6 C7 1.393(4) . ? C6 H6 0.9500 . ? C7 C8 1.393(5) . ? C7 C14 1.538(4) . ? C8 C9 1.400(4) . ? C8 H8 0.9500 . ? C9 C10 1.536(4) . ? C10 C11 1.532(5) . ? C10 C13 1.534(5) . ? C10 C12 1.540(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.506(6) . ? C14 C15 1.521(6) . ? C14 C17 1.550(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.383(4) . ? C19 C24 1.394(4) . ? C20 C21 1.384(4) . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 C23 1.404(4) . ? C22 H22 0.9500 . ? C23 C24 1.392(4) . ? C23 C25 1.529(4) . ? C24 H24 0.9500 . ? C25 C28 1.532(4) . ? C25 C26 1.538(4) . ? C25 C27 1.539(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.517(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.398(4) . ? C30 C35 1.413(4) . ? C31 C32 1.394(4) . ? C32 C33 1.390(4) . ? C32 H32 0.9500 . ? C33 C34 1.395(4) . ? C33 C36 1.544(4) . ? C34 C35 1.393(4) . ? C34 H34 0.9500 . ? C35 C40 1.545(4) . ? C36 C37 1.523(5) . ? C36 C38 1.523(5) . ? C36 C39 1.536(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C43 1.530(4) . ? C40 C41 1.531(5) . ? C40 C42 1.539(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.482(6) . ? C44 C44 1.556(9) 2_655 ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.505(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C51 C52 1.384(14) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.50(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.417(19) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.52(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.561(19) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr O4 104.22(8) . . ? O1 Zr O2 93.17(8) . . ? O4 Zr O2 106.47(8) . . ? O1 Zr O3 110.47(8) . . ? O4 Zr O3 138.76(8) . . ? O2 Zr O3 93.39(8) . . ? O1 Zr O3 87.01(8) . 2_556 ? O4 Zr O3 92.32(8) . 2_556 ? O2 Zr O3 160.51(8) . 2_556 ? O3 Zr O3 68.46(8) . 2_556 ? O1 Zr N1 168.98(8) . . ? O4 Zr N1 77.41(7) . . ? O2 Zr N1 76.01(8) . . ? O3 Zr N1 72.82(7) . . ? O3 Zr N1 103.88(7) 2_556 . ? O1 Zr Zr 99.93(6) . 2_556 ? O4 Zr Zr 117.76(6) . 2_556 ? O2 Zr Zr 128.48(6) . 2_556 ? O3 Zr Zr 35.44(5) . 2_556 ? O3 Zr Zr 33.02(5) 2_556 2_556 ? N1 Zr Zr 88.65(6) . 2_556 ? C1 O1 Zr 172.1(2) . . ? C19 N1 C29 111.2(2) . . ? C19 N1 C18 110.9(2) . . ? C29 N1 C18 111.8(2) . . ? C19 N1 Zr 107.12(16) . . ? C29 N1 Zr 105.76(16) . . ? C18 N1 Zr 109.95(16) . . ? O1 C1 C2 114.2(4) . . ? O1 C1 C3 111.3(3) . . ? C2 C1 C3 118.3(4) . . ? O1 C1 H1 103.7 . . ? C2 C1 H1 103.7 . . ? C3 C1 H1 103.7 . . ? C4 O2 Zr 145.23(19) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C20 O3 Zr 117.08(17) . . ? C20 O3 Zr 115.59(16) . 2_556 ? Zr O3 Zr 111.54(8) . 2_556 ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C30 O4 Zr 143.83(17) . . ? O2 C4 C9 122.1(3) . . ? O2 C4 C5 118.0(3) . . ? C9 C4 C5 120.0(3) . . ? C6 C5 C4 120.0(3) . . ? C6 C5 C18 121.3(3) . . ? C4 C5 C18 118.6(3) . . ? C5 C6 C7 121.8(3) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C8 117.0(3) . . ? C6 C7 C14 120.7(3) . . ? C8 C7 C14 122.3(3) . . ? C7 C8 C9 123.7(3) . . ? C7 C8 H8 118.2 . . ? C9 C8 H8 118.2 . . ? C8 C9 C4 117.5(3) . . ? C8 C9 C10 121.7(3) . . ? C4 C9 C10 120.8(3) . . ? C11 C10 C13 107.9(3) . . ? C11 C10 C9 109.8(3) . . ? C13 C10 C9 111.9(3) . . ? C11 C10 C12 110.7(3) . . ? C13 C10 C12 107.0(3) . . ? C9 C10 C12 109.6(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 112.2(4) . . ? C16 C14 C7 110.0(3) . . ? C15 C14 C7 112.4(3) . . ? C16 C14 C17 107.2(4) . . ? C15 C14 C17 105.1(3) . . ? C7 C14 C17 109.7(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C5 112.7(2) . . ? N1 C18 H18A 109.1 . . ? C5 C18 H18A 109.1 . . ? N1 C18 H18B 109.1 . . ? C5 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C24 120.1(3) . . ? C20 C19 N1 117.5(2) . . ? C24 C19 N1 122.3(3) . . ? C19 C20 C21 119.5(3) . . ? C19 C20 O3 118.8(2) . . ? C21 C20 O3 121.7(3) . . ? C22 C21 C20 119.9(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 122.2(3) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C24 C23 C22 116.7(3) . . ? C24 C23 C25 122.7(3) . . ? C22 C23 C25 120.5(3) . . ? C23 C24 C19 121.5(3) . . ? C23 C24 H24 119.2 . . ? C19 C24 H24 119.2 . . ? C23 C25 C28 112.2(2) . . ? C23 C25 C26 110.5(3) . . ? C28 C25 C26 107.5(3) . . ? C23 C25 C27 108.3(3) . . ? C28 C25 C27 108.6(3) . . ? C26 C25 C27 109.7(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 C31 113.8(2) . . ? N1 C29 H29A 108.8 . . ? C31 C29 H29A 108.8 . . ? N1 C29 H29B 108.8 . . ? C31 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? O4 C30 C31 118.6(2) . . ? O4 C30 C35 121.1(2) . . ? C31 C30 C35 120.3(3) . . ? C32 C31 C30 119.9(3) . . ? C32 C31 C29 118.7(3) . . ? C30 C31 C29 121.4(3) . . ? C33 C32 C31 121.6(3) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C34 116.9(3) . . ? C32 C33 C36 122.9(3) . . ? C34 C33 C36 120.2(3) . . ? C35 C34 C33 124.1(3) . . ? C35 C34 H34 118.0 . . ? C33 C34 H34 118.0 . . ? C34 C35 C30 117.0(3) . . ? C34 C35 C40 121.3(3) . . ? C30 C35 C40 121.6(3) . . ? C37 C36 C38 108.9(3) . . ? C37 C36 C39 107.3(3) . . ? C38 C36 C39 109.7(3) . . ? C37 C36 C33 112.2(3) . . ? C38 C36 C33 110.1(3) . . ? C39 C36 C33 108.6(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C43 C40 C41 108.0(3) . . ? C43 C40 C42 106.9(3) . . ? C41 C40 C42 110.0(3) . . ? C43 C40 C35 112.1(3) . . ? C41 C40 C35 109.2(3) . . ? C42 C40 C35 110.5(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C44 114.3(5) . 2_655 ? C45 C44 H44A 108.7 . . ? C44 C44 H44A 108.7 2_655 . ? C45 C44 H44B 108.7 . . ? C44 C44 H44B 108.7 2_655 . ? H44A C44 H44B 107.6 . . ? C44 C45 C46 114.0(4) . . ? C44 C45 H45A 108.8 . . ? C46 C45 H45A 108.8 . . ? C44 C45 H45B 108.8 . . ? C46 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C51 C52 C53 125(3) . . ? C51 C52 H52A 106.1 . . ? C53 C52 H52A 106.1 . . ? C51 C52 H52B 106.1 . . ? C53 C52 H52B 106.1 . . ? H52A C52 H52B 106.3 . . ? C54 C53 C52 94(2) . . ? C52 C53 C53 108(2) . 2_566 ? C54 C53 H53A 112.9 . . ? C52 C53 H53A 112.9 . . ? C53 C53 H53A 121.8 2_566 . ? C54 C53 H53B 112.9 . . ? C52 C53 H53B 112.9 . . ? C53 C53 H53B 88.6 2_566 . ? H53A C53 H53B 110.3 . . ? C53 C54 C55 101(2) . . ? C53 C54 H54A 111.5 . . ? C55 C54 H54A 111.5 . . ? C53 C54 H54B 111.5 . . ? C55 C54 H54B 111.5 . . ? H54A C54 H54B 109.3 . . ? C54 C55 C56 118(2) . . ? C54 C55 H55A 107.8 . . ? C56 C55 H55A 107.8 . . ? C54 C55 H55B 107.8 . . ? C56 C55 H55B 107.8 . . ? H55A C55 H55B 107.1 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.680 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.068 #===END