# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a12717_2aHOiPr _database_code_depnum_ccdc_archive 'CCDC 897192' #TrackingRef '[ONO]ZrX2 r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H78 N2 O5 Zr' _chemical_formula_sum 'C45 H78 N2 O5 Zr' _chemical_formula_weight 818.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4727(11) _cell_length_b 21.469(2) _cell_length_c 21.279(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.473(3) _cell_angle_gamma 90.00 _cell_volume 4780.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8901 _exptl_absorpt_correction_T_max 0.9839 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30282 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0635 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8373 _reflns_number_gt 5935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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. Distance restraints were introduced for C41, C43; C41, C43'; C41, C42; and C41, C42' with a value of 1.459(2). ; _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^)+(0.0543P)^2^+4.6080P] 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 8373 _refine_ls_number_parameters 475 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 0.8341(3) 0.91161(16) 0.15265(16) 0.0296(8) Uani 1 1 d . . . C2 C 0.8937(3) 0.96116(16) 0.18661(16) 0.0299(8) Uani 1 1 d . . . C3 C 1.0393(3) 0.96257(17) 0.19862(18) 0.0366(9) Uani 1 1 d . . . C4 C 1.1063(4) 0.9649(2) 0.13605(19) 0.0491(11) Uani 1 1 d . . . H4A H 1.0789 1.0022 0.1126 0.074 Uiso 1 1 calc R . . H4B H 1.0838 0.9277 0.1112 0.074 Uiso 1 1 calc R . . H4C H 1.1990 0.9662 0.1443 0.074 Uiso 1 1 calc R . . C5 C 1.0825(4) 0.9050(2) 0.23555(19) 0.0479(11) Uani 1 1 d . . . H5A H 1.0392 0.9037 0.2755 0.072 Uiso 1 1 calc R . . H5B H 1.1751 0.9068 0.2440 0.072 Uiso 1 1 calc R . . H5C H 1.0608 0.8676 0.2110 0.072 Uiso 1 1 calc R . . C6 C 1.0822(4) 1.0205(2) 0.2366(2) 0.0588(13) Uani 1 1 d . . . H6A H 1.0420 1.0203 0.2773 0.088 Uiso 1 1 calc R . . H6B H 1.0566 1.0582 0.2132 0.088 Uiso 1 1 calc R . . H6C H 1.1754 1.0200 0.2433 0.088 Uiso 1 1 calc R . . C7 C 0.8147(3) 1.00731(16) 0.20945(16) 0.0315(8) Uani 1 1 d . . . H7 H 0.8536 1.0409 0.2322 0.038 Uiso 1 1 calc R . . C8 C 0.6814(3) 1.00720(16) 0.20095(16) 0.0296(8) Uani 1 1 d . . . C9 C 0.6029(3) 1.05945(16) 0.22973(17) 0.0348(9) Uani 1 1 d . . . C10 C 0.6345(4) 1.0627(2) 0.30076(18) 0.0537(12) Uani 1 1 d . . . H10A H 0.7263 1.0699 0.3081 0.081 Uiso 1 1 calc R . . H10B H 0.6107 1.0233 0.3204 0.081 Uiso 1 1 calc R . . H10C H 0.5866 1.0969 0.3191 0.081 Uiso 1 1 calc R . . C11 C 0.6351(4) 1.12194(19) 0.2002(2) 0.0572(12) Uani 1 1 d . . . H11A H 0.7273 1.1293 0.2050 0.086 Uiso 1 1 calc R . . H11B H 0.5894 1.1553 0.2212 0.086 Uiso 1 1 calc R . . H11C H 0.6092 1.1214 0.1554 0.086 Uiso 1 1 calc R . . C12 C 0.4594(4) 1.04854(19) 0.2203(2) 0.0483(11) Uani 1 1 d . . . H12A H 0.4130 1.0833 0.2386 0.072 Uiso 1 1 calc R . . H12B H 0.4362 1.0096 0.2410 0.072 Uiso 1 1 calc R . . H12C H 0.4368 1.0457 0.1752 0.072 Uiso 1 1 calc R . . C13 C 0.6276(3) 0.95819(16) 0.16646(16) 0.0306(8) Uani 1 1 d . . . H13 H 0.5375 0.9569 0.1592 0.037 Uiso 1 1 calc R . . C14 C 0.7017(3) 0.91102(16) 0.14236(16) 0.0288(8) Uani 1 1 d . . . C15 C 0.6358(3) 0.85598(17) 0.11123(16) 0.0336(9) Uani 1 1 d . . . H15A H 0.5438 0.8663 0.1063 0.040 Uiso 1 1 calc R . . H15B H 0.6434 0.8207 0.1411 0.040 Uiso 1 1 calc R . . C16 C 0.6520(3) 0.87996(17) -0.00486(18) 0.0360(9) Uani 1 1 d . . . C17 C 0.7367(4) 0.93735(17) 0.00628(19) 0.0435(10) Uani 1 1 d . . . H17A H 0.7170 0.9567 0.0464 0.065 Uiso 1 1 calc R . . H17B H 0.7206 0.9673 -0.0279 0.065 Uiso 1 1 calc R . . H17C H 0.8268 0.9248 0.0074 0.065 Uiso 1 1 calc R . . C18 C 0.5127(4) 0.9023(2) -0.0098(2) 0.0558(12) Uani 1 1 d . . . H18A H 0.4896 0.9205 0.0304 0.084 Uiso 1 1 calc R . . H18B H 0.4564 0.8670 -0.0200 0.084 Uiso 1 1 calc R . . H18C H 0.5031 0.9338 -0.0430 0.084 Uiso 1 1 calc R . . C19 C 0.6866(4) 0.85126(18) -0.06778(17) 0.0418(10) Uani 1 1 d . . . H19A H 0.7755 0.8369 -0.0650 0.063 Uiso 1 1 calc R . . H19B H 0.6765 0.8826 -0.1011 0.063 Uiso 1 1 calc R . . H19C H 0.6300 0.8159 -0.0775 0.063 Uiso 1 1 calc R . . C20 C 0.5948(3) 0.77455(16) 0.03937(17) 0.0339(9) Uani 1 1 d . . . H20A H 0.6019 0.7508 0.0792 0.041 Uiso 1 1 calc R . . H20B H 0.5050 0.7887 0.0342 0.041 Uiso 1 1 calc R . . C21 C 0.6178(3) 0.72948(16) -0.01316(17) 0.0322(8) Uani 1 1 d . . . C22 C 0.5178(3) 0.71299(17) -0.05531(17) 0.0361(9) Uani 1 1 d . . . H22 H 0.4384 0.7342 -0.0532 0.043 Uiso 1 1 calc R . . C23 C 0.5301(3) 0.66683(17) -0.10016(16) 0.0337(9) Uani 1 1 d . . . C24 C 0.4214(4) 0.64760(18) -0.14657(18) 0.0393(9) Uani 1 1 d . . . C25 C 0.3120(4) 0.6945(2) -0.1475(2) 0.0632(13) Uani 1 1 d . . . H25A H 0.3428 0.7351 -0.1616 0.095 Uiso 1 1 calc R . . H25B H 0.2800 0.6986 -0.1051 0.095 Uiso 1 1 calc R . . H25C H 0.2428 0.6801 -0.1764 0.095 Uiso 1 1 calc R . . C26 C 0.4686(4) 0.6430(3) -0.2132(2) 0.0661(14) Uani 1 1 d . . . H26A H 0.4989 0.6839 -0.2266 0.099 Uiso 1 1 calc R . . H26B H 0.3985 0.6292 -0.2418 0.099 Uiso 1 1 calc R . . H26C H 0.5389 0.6129 -0.2140 0.099 Uiso 1 1 calc R . . C27 C 0.3697(4) 0.5844(2) -0.1268(2) 0.0627(13) Uani 1 1 d . . . H27A H 0.4385 0.5534 -0.1268 0.094 Uiso 1 1 calc R . . H27B H 0.3005 0.5715 -0.1565 0.094 Uiso 1 1 calc R . . H27C H 0.3369 0.5875 -0.0845 0.094 Uiso 1 1 calc R . . C28 C 0.6476(3) 0.63543(16) -0.09940(17) 0.0354(9) Uani 1 1 d . . . H28 H 0.6574 0.6027 -0.1288 0.042 Uiso 1 1 calc R . . C29 C 0.7509(3) 0.64923(16) -0.05814(17) 0.0320(8) Uani 1 1 d . . . C30 C 0.8754(4) 0.61187(18) -0.05951(19) 0.0415(10) Uani 1 1 d . . . C31 C 0.8667(4) 0.5570(2) -0.1060(2) 0.0627(14) Uani 1 1 d . . . H31A H 0.9488 0.5350 -0.1055 0.094 Uiso 1 1 calc R . . H31B H 0.8463 0.5727 -0.1485 0.094 Uiso 1 1 calc R . . H31C H 0.7996 0.5282 -0.0936 0.094 Uiso 1 1 calc R . . C32 C 0.9105(4) 0.5849(2) 0.0059(2) 0.0580(12) Uani 1 1 d . . . H32A H 0.9900 0.5610 0.0042 0.087 Uiso 1 1 calc R . . H32B H 0.8417 0.5575 0.0190 0.087 Uiso 1 1 calc R . . H32C H 0.9223 0.6190 0.0363 0.087 Uiso 1 1 calc R . . C33 C 0.9834(4) 0.6546(2) -0.0799(2) 0.0582(12) Uani 1 1 d . . . H33A H 1.0628 0.6306 -0.0815 0.087 Uiso 1 1 calc R . . H33B H 0.9951 0.6886 -0.0495 0.087 Uiso 1 1 calc R . . H33C H 0.9612 0.6718 -0.1216 0.087 Uiso 1 1 calc R . . C34 C 0.7356(3) 0.69866(15) -0.01561(16) 0.0296(8) Uani 1 1 d . . . C35 C 1.0400(4) 0.8650(2) -0.0511(2) 0.0609(13) Uani 1 1 d . . . H35 H 0.9716 0.8804 -0.0815 0.073 Uiso 1 1 d R A . C36 C 1.1189(6) 0.9167(3) -0.0326(3) 0.0530(16) Uiso 0.70 1 d P A 1 H36A H 1.0679 0.9473 -0.0104 0.080 Uiso 0.70 1 calc PR A 1 H36B H 1.1531 0.9361 -0.0700 0.080 Uiso 0.70 1 calc PR A 1 H36C H 1.1896 0.9023 -0.0047 0.080 Uiso 0.70 1 calc PR A 1 C37 C 1.1136(8) 0.8153(4) -0.0870(4) 0.084(2) Uiso 0.70 1 d P A 1 H37A H 1.0565 0.7804 -0.0980 0.126 Uiso 0.70 1 calc PR A 1 H37B H 1.1859 0.8002 -0.0605 0.126 Uiso 0.70 1 calc PR A 1 H37C H 1.1453 0.8336 -0.1256 0.126 Uiso 0.70 1 calc PR A 1 C36' C 1.1758(17) 0.8840(9) -0.0221(8) 0.076(5) Uiso 0.30 1 d P A 2 H36D H 1.1656 0.9067 0.0174 0.113 Uiso 0.30 1 calc PR A 2 H36E H 1.2192 0.9107 -0.0518 0.113 Uiso 0.30 1 calc PR A 2 H36F H 1.2270 0.8465 -0.0137 0.113 Uiso 0.30 1 calc PR A 2 C37' C 1.0348(15) 0.8386(7) -0.1068(7) 0.057(4) Uiso 0.30 1 d P A 2 H37D H 0.9470 0.8250 -0.1171 0.086 Uiso 0.30 1 calc PR A 2 H37E H 1.0920 0.8024 -0.1064 0.086 Uiso 0.30 1 calc PR A 2 H37F H 1.0614 0.8686 -0.1384 0.086 Uiso 0.30 1 calc PR A 2 C38 C 1.2023(5) 0.7433(4) 0.0999(4) 0.124(3) Uani 1 1 d . . . H38 H 1.2256 0.7741 0.0671 0.149 Uiso 1 1 calc R . . C39 C 1.2364(5) 0.6877(3) 0.0677(3) 0.094(2) Uani 1 1 d . . . H39A H 1.1777 0.6814 0.0311 0.141 Uiso 1 1 calc R . . H39B H 1.2308 0.6520 0.0962 0.141 Uiso 1 1 calc R . . H39C H 1.3240 0.6914 0.0537 0.141 Uiso 1 1 calc R . . C40 C 1.2768(5) 0.7674(4) 0.1502(3) 0.116(3) Uani 1 1 d . . . H40A H 1.2409 0.8073 0.1633 0.174 Uiso 1 1 calc R . . H40B H 1.3644 0.7738 0.1371 0.174 Uiso 1 1 calc R . . H40C H 1.2773 0.7381 0.1855 0.174 Uiso 1 1 calc R . . C41 C 0.8605(5) 0.7449(2) 0.2210(2) 0.0731(16) Uani 1 1 d D . . H41 H 0.8968 0.7875 0.2154 0.088 Uiso 1 1 calc R B 3 C42' C 0.9817(8) 0.7212(7) 0.2471(6) 0.092(4) Uiso 0.45 1 d PD C 3 H42A H 1.0384 0.7118 0.2129 0.137 Uiso 0.45 1 calc PR C 3 H42B H 0.9666 0.6831 0.2711 0.137 Uiso 0.45 1 calc PR C 3 H42C H 1.0218 0.7526 0.2750 0.137 Uiso 0.45 1 calc PR C 3 C43' C 0.7679(13) 0.7677(8) 0.2646(6) 0.113(5) Uiso 0.45 1 d PD C 3 H43A H 0.6931 0.7843 0.2410 0.170 Uiso 0.45 1 calc PR C 3 H43B H 0.8069 0.8008 0.2908 0.170 Uiso 0.45 1 calc PR C 3 H43C H 0.7415 0.7335 0.2916 0.170 Uiso 0.45 1 calc PR C 3 C42 C 0.9322(11) 0.6869(4) 0.2306(6) 0.103(4) Uiso 0.55 1 d PD C 4 H42D H 1.0148 0.6903 0.2109 0.154 Uiso 0.55 1 calc PR C 4 H42E H 0.8835 0.6523 0.2116 0.154 Uiso 0.55 1 calc PR C 4 H42F H 0.9463 0.6793 0.2758 0.154 Uiso 0.55 1 calc PR C 4 C43 C 0.7477(7) 0.7286(5) 0.2558(5) 0.084(3) Uiso 0.55 1 d PD C 4 H43D H 0.6871 0.7633 0.2540 0.125 Uiso 0.55 1 calc PR C 4 H43E H 0.7736 0.7199 0.2998 0.125 Uiso 0.55 1 calc PR C 4 H43F H 0.7071 0.6915 0.2370 0.125 Uiso 0.55 1 calc PR C 4 C44 C 0.6175(6) 0.6039(2) 0.0931(2) 0.0691(15) Uani 1 1 d . . . C45 C 0.5392(5) 0.5719(2) 0.0466(2) 0.0676(14) Uani 1 1 d . . . H45A H 0.5849 0.5351 0.0320 0.101 Uiso 1 1 calc R . . H45B H 0.5200 0.5997 0.0110 0.101 Uiso 1 1 calc R . . H45C H 0.4593 0.5588 0.0650 0.101 Uiso 1 1 calc R . . N1 N 0.6771(3) 0.83235(13) 0.04811(13) 0.0284(7) Uani 1 1 d . A . N2 N 0.6786(5) 0.6292(2) 0.1301(2) 0.0998(18) Uani 1 1 d . . . O1 O 0.9028(2) 0.86436(11) 0.12942(11) 0.0334(6) Uani 1 1 d . A . O2 O 0.8307(2) 0.71757(10) 0.02415(11) 0.0327(6) Uani 1 1 d . A . O3 O 0.9774(2) 0.83505(12) -0.00137(12) 0.0413(7) Uani 1 1 d . A . O4 O 1.0716(2) 0.75549(12) 0.09987(12) 0.0449(7) Uani 1 1 d . A . O5 O 0.8224(2) 0.74032(12) 0.15379(11) 0.0421(7) Uani 1 1 d . A . H5 H 0.7533 0.7130 0.1434 0.051 Uiso 1 1 calc R . . Zr1 Zr 0.91117(3) 0.792157(15) 0.069425(16) 0.02856(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0285(19) 0.031(2) 0.030(2) -0.0003(16) 0.0064(15) 0.0069(16) C2 0.0270(19) 0.033(2) 0.030(2) -0.0002(16) 0.0018(15) 0.0009(15) C3 0.027(2) 0.040(2) 0.042(2) -0.0080(18) -0.0003(17) -0.0008(17) C4 0.033(2) 0.058(3) 0.057(3) 0.001(2) 0.012(2) -0.003(2) C5 0.034(2) 0.062(3) 0.047(3) 0.003(2) -0.0093(19) 0.004(2) C6 0.035(2) 0.062(3) 0.078(3) -0.026(3) -0.002(2) -0.005(2) C7 0.032(2) 0.031(2) 0.032(2) -0.0053(16) 0.0039(16) -0.0020(16) C8 0.030(2) 0.030(2) 0.0285(19) -0.0012(16) 0.0050(15) 0.0026(15) C9 0.037(2) 0.031(2) 0.037(2) -0.0048(17) 0.0053(17) 0.0055(17) C10 0.052(3) 0.065(3) 0.044(3) -0.015(2) 0.008(2) 0.013(2) C11 0.062(3) 0.039(3) 0.071(3) -0.003(2) 0.019(2) 0.007(2) C12 0.039(2) 0.046(3) 0.061(3) -0.012(2) 0.011(2) 0.0088(19) C13 0.0248(19) 0.035(2) 0.032(2) -0.0037(17) 0.0026(15) 0.0029(16) C14 0.0263(19) 0.031(2) 0.029(2) -0.0046(16) 0.0036(15) -0.0012(15) C15 0.0237(19) 0.038(2) 0.039(2) -0.0075(17) 0.0066(16) 0.0002(16) C16 0.0262(19) 0.040(2) 0.042(2) 0.0014(18) -0.0046(17) 0.0057(17) C17 0.051(3) 0.035(2) 0.045(2) 0.0050(19) 0.008(2) 0.0004(19) C18 0.041(3) 0.061(3) 0.065(3) 0.012(2) -0.007(2) 0.015(2) C19 0.044(2) 0.043(2) 0.038(2) 0.0022(19) -0.0014(18) -0.0027(19) C20 0.0246(19) 0.036(2) 0.042(2) -0.0096(17) 0.0071(16) -0.0019(15) C21 0.030(2) 0.031(2) 0.037(2) -0.0053(17) 0.0066(16) -0.0012(16) C22 0.027(2) 0.039(2) 0.042(2) -0.0048(18) 0.0034(16) -0.0001(17) C23 0.034(2) 0.035(2) 0.033(2) -0.0043(17) 0.0042(16) -0.0016(17) C24 0.033(2) 0.043(2) 0.042(2) -0.0069(19) -0.0004(18) -0.0017(18) C25 0.051(3) 0.059(3) 0.077(3) -0.018(3) -0.024(2) 0.006(2) C26 0.048(3) 0.103(4) 0.046(3) -0.016(3) -0.003(2) -0.006(3) C27 0.061(3) 0.056(3) 0.069(3) 0.001(2) -0.020(3) -0.016(2) C28 0.040(2) 0.031(2) 0.036(2) -0.0083(17) 0.0074(18) -0.0018(17) C29 0.029(2) 0.032(2) 0.035(2) -0.0018(17) 0.0052(16) 0.0008(16) C30 0.035(2) 0.042(2) 0.048(3) -0.015(2) 0.0033(18) 0.0079(18) C31 0.048(3) 0.060(3) 0.080(3) -0.034(3) -0.001(2) 0.017(2) C32 0.061(3) 0.048(3) 0.065(3) -0.004(2) -0.005(2) 0.017(2) C33 0.035(2) 0.072(3) 0.069(3) -0.013(3) 0.013(2) 0.004(2) C34 0.0282(19) 0.028(2) 0.033(2) -0.0023(16) 0.0038(15) -0.0026(15) C35 0.049(3) 0.071(3) 0.064(3) 0.014(3) 0.021(2) -0.010(2) C38 0.045(3) 0.158(6) 0.166(7) -0.095(6) -0.043(4) 0.057(4) C39 0.056(3) 0.110(5) 0.116(5) -0.033(4) -0.004(3) 0.038(3) C40 0.041(3) 0.183(7) 0.123(6) -0.068(5) -0.023(3) 0.019(4) C41 0.115(5) 0.045(3) 0.058(3) 0.011(2) -0.006(3) -0.026(3) C44 0.093(4) 0.059(3) 0.057(3) -0.001(3) 0.026(3) -0.033(3) C45 0.090(4) 0.058(3) 0.055(3) -0.001(3) 0.009(3) -0.018(3) N1 0.0242(16) 0.0289(16) 0.0323(17) -0.0059(13) 0.0034(12) -0.0018(12) N2 0.139(5) 0.096(4) 0.066(3) -0.007(3) 0.022(3) -0.067(3) O1 0.0268(13) 0.0350(14) 0.0382(14) -0.0061(12) -0.0002(11) 0.0026(11) O2 0.0286(13) 0.0315(14) 0.0377(14) -0.0046(11) -0.0010(11) 0.0022(11) O3 0.0329(15) 0.0471(16) 0.0446(16) 0.0000(13) 0.0105(12) -0.0026(12) O4 0.0316(15) 0.0482(17) 0.0542(18) -0.0057(14) -0.0063(13) 0.0109(12) O5 0.0487(17) 0.0425(16) 0.0349(15) -0.0001(12) -0.0003(12) -0.0063(13) Zr1 0.02252(19) 0.0296(2) 0.0337(2) -0.00288(16) 0.00252(14) 0.00310(15) _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 C1 O1 1.350(4) . ? C1 C14 1.394(5) . ? C1 C2 1.416(5) . ? C2 C7 1.392(5) . ? C2 C3 1.535(5) . ? C3 C5 1.522(5) . ? C3 C4 1.532(5) . ? C3 C6 1.540(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.399(5) . ? C7 H7 0.9500 . ? C8 C13 1.388(5) . ? C8 C9 1.534(5) . ? C9 C12 1.525(5) . ? C9 C11 1.526(5) . ? C9 C10 1.535(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 C14 1.388(5) . ? C13 H13 0.9500 . ? C14 C15 1.507(5) . ? C15 N1 1.516(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.531(5) . ? C16 C19 1.532(5) . ? C16 C18 1.535(5) . ? C16 N1 1.536(4) . ? 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 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.506(5) . ? C20 N1 1.518(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.395(5) . ? C21 C34 1.403(5) . ? C22 C23 1.386(5) . ? C22 H22 0.9500 . ? C23 C28 1.402(5) . ? C23 C24 1.531(5) . ? C24 C26 1.525(5) . ? C24 C27 1.528(6) . ? C24 C25 1.525(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 C29 1.396(5) . ? C28 H28 0.9500 . ? C29 C34 1.408(5) . ? C29 C30 1.532(5) . ? C30 C33 1.532(6) . ? C30 C31 1.539(5) . ? C30 C32 1.538(6) . ? 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 O2 1.342(4) . ? C35 C37' 1.313(15) . ? C35 O3 1.421(5) . ? C35 C36 1.430(7) . ? C35 C37 1.539(9) . ? C35 C36' 1.581(17) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C36' H36D 0.9800 . ? C36' H36E 0.9800 . ? C36' H36F 0.9800 . ? C37' H35 1.2506 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? C38 O4 1.393(5) . ? C38 C40 1.396(7) . ? C38 C39 1.430(7) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43' 1.456(2) . ? C41 C42' 1.457(2) . ? C41 O5 1.470(5) . ? C41 C42 1.464(2) . ? C41 C43 1.464(2) . ? C41 H41 1.0000 . ? C42' H42A 0.9800 . ? C42' H42B 0.9800 . ? C42' H42C 0.9800 . ? C43' H43A 0.9800 . ? C43' H43B 0.9800 . ? C43' H43C 0.9800 . ? C42 H42D 0.9800 . ? C42 H42E 0.9800 . ? C42 H42F 0.9800 . ? C43 H43D 0.9800 . ? C43 H43E 0.9800 . ? C43 H43F 0.9800 . ? C44 N2 1.132(6) . ? C44 C45 1.434(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? N1 Zr1 2.620(3) . ? O1 Zr1 2.012(2) . ? O2 Zr1 2.033(2) . ? O3 Zr1 1.921(2) . ? O4 Zr1 1.942(2) . ? O5 Zr1 2.339(2) . ? O5 H5 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 C1 C14 118.6(3) . . ? O1 C1 C2 121.4(3) . . ? C14 C1 C2 120.1(3) . . ? C7 C2 C1 117.2(3) . . ? C7 C2 C3 121.9(3) . . ? C1 C2 C3 120.9(3) . . ? C5 C3 C4 109.7(3) . . ? C5 C3 C2 109.9(3) . . ? C4 C3 C2 110.2(3) . . ? C5 C3 C6 108.2(3) . . ? C4 C3 C6 107.2(3) . . ? C2 C3 C6 111.6(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 C8 123.9(3) . . ? C2 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C13 C8 C7 116.7(3) . . ? C13 C8 C9 123.6(3) . . ? C7 C8 C9 119.7(3) . . ? C12 C9 C11 108.3(3) . . ? C12 C9 C8 112.2(3) . . ? C11 C9 C8 110.3(3) . . ? C12 C9 C10 107.8(3) . . ? C11 C9 C10 108.9(3) . . ? C8 C9 C10 109.3(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C8 121.9(3) . . ? C14 C13 H13 119.1 . . ? C8 C13 H13 119.1 . . ? C13 C14 C1 120.2(3) . . ? C13 C14 C15 118.8(3) . . ? C1 C14 C15 120.6(3) . . ? C14 C15 N1 120.6(3) . . ? C14 C15 H15A 107.2 . . ? N1 C15 H15A 107.2 . . ? C14 C15 H15B 107.2 . . ? N1 C15 H15B 107.2 . . ? H15A C15 H15B 106.8 . . ? C17 C16 C19 107.6(3) . . ? C17 C16 C18 107.6(3) . . ? C19 C16 C18 109.0(3) . . ? C17 C16 N1 110.0(3) . . ? C19 C16 N1 109.5(3) . . ? C18 C16 N1 113.0(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N1 120.6(3) . . ? C21 C20 H20A 107.2 . . ? N1 C20 H20A 107.2 . . ? C21 C20 H20B 107.2 . . ? N1 C20 H20B 107.2 . . ? H20A C20 H20B 106.8 . . ? C22 C21 C34 119.6(3) . . ? C22 C21 C20 120.1(3) . . ? C34 C21 C20 120.0(3) . . ? C23 C22 C21 122.3(3) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C22 C23 C28 116.3(3) . . ? C22 C23 C24 123.3(3) . . ? C28 C23 C24 120.4(3) . . ? C26 C24 C27 109.3(4) . . ? C26 C24 C25 107.8(4) . . ? C27 C24 C25 108.4(4) . . ? C26 C24 C23 110.8(3) . . ? C27 C24 C23 108.9(3) . . ? C25 C24 C23 111.6(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C23 124.1(3) . . ? C29 C28 H28 117.9 . . ? C23 C28 H28 117.9 . . ? C28 C29 C34 117.2(3) . . ? C28 C29 C30 121.0(3) . . ? C34 C29 C30 121.8(3) . . ? C33 C30 C29 109.3(3) . . ? C33 C30 C31 107.5(3) . . ? C29 C30 C31 112.7(3) . . ? C33 C30 C32 109.3(4) . . ? C29 C30 C32 110.5(3) . . ? C31 C30 C32 107.4(3) . . ? 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 . . ? O2 C34 C21 117.7(3) . . ? O2 C34 C29 122.1(3) . . ? C21 C34 C29 120.3(3) . . ? C37' C35 O3 118.3(8) . . ? C37' C35 C36 125.8(8) . . ? O3 C35 C36 115.2(4) . . ? C37' C35 C37 41.8(7) . . ? O3 C35 C37 108.3(4) . . ? C36 C35 C37 112.3(5) . . ? C37' C35 C36' 117.8(10) . . ? O3 C35 C36' 105.2(7) . . ? C36 C35 C36' 36.0(7) . . ? C37 C35 C36' 84.9(8) . . ? C37' C35 H35 63.8 . . ? O3 C35 H35 106.9 . . ? C36 C35 H35 108.1 . . ? C37 C35 H35 105.5 . . ? C36' C35 H35 140.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C36' H36D 109.5 . . ? C35 C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C35 C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C35 C37' H35 45.8 . . ? C35 C37' H37D 109.5 . . ? H35 C37' H37D 78.6 . . ? C35 C37' H37E 109.5 . . ? H35 C37' H37E 154.1 . . ? H37D C37' H37E 109.5 . . ? C35 C37' H37F 109.5 . . ? H35 C37' H37F 89.7 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? O4 C38 C40 116.6(5) . . ? O4 C38 C39 115.0(5) . . ? C40 C38 C39 122.3(5) . . ? O4 C38 H38 98.3 . . ? C40 C38 H38 98.3 . . ? C39 C38 H38 98.3 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43' C41 C42' 117.8(9) . . ? C43' C41 O5 118.9(8) . . ? C42' C41 O5 122.9(7) . . ? C43' C41 C42 123.2(9) . . ? C42' C41 C42 38.3(6) . . ? O5 C41 C42 101.3(6) . . ? C43' C41 C43 35.3(7) . . ? C42' C41 C43 115.5(8) . . ? O5 C41 C43 106.6(6) . . ? C42 C41 C43 98.3(7) . . ? C43' C41 H41 92.0 . . ? C42' C41 H41 92.0 . . ? O5 C41 H41 92.0 . . ? C42 C41 H41 126.8 . . ? C43 C41 H41 126.8 . . ? C41 C42' H42A 109.5 . . ? C41 C42' H42B 109.5 . . ? H42A C42' H42B 109.5 . . ? C41 C42' H42C 109.5 . . ? H42A C42' H42C 109.5 . . ? H42B C42' H42C 109.5 . . ? C41 C43' H43A 109.5 . . ? C41 C43' H43B 109.5 . . ? H43A C43' H43B 109.5 . . ? C41 C43' H43C 109.5 . . ? H43A C43' H43C 109.5 . . ? H43B C43' H43C 109.5 . . ? C41 C42 H42D 109.5 . . ? C41 C42 H42E 109.5 . . ? H42D C42 H42E 109.5 . . ? C41 C42 H42F 109.5 . . ? H42D C42 H42F 109.5 . . ? H42E C42 H42F 109.5 . . ? C41 C43 H43D 109.5 . . ? C41 C43 H43E 109.5 . . ? H43D C43 H43E 109.5 . . ? C41 C43 H43F 109.5 . . ? H43D C43 H43F 109.5 . . ? H43E C43 H43F 109.5 . . ? N2 C44 C45 179.5(6) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C15 N1 C20 101.5(2) . . ? C15 N1 C16 112.4(3) . . ? C20 N1 C16 112.1(3) . . ? C15 N1 Zr1 104.90(19) . . ? C20 N1 Zr1 105.90(19) . . ? C16 N1 Zr1 118.38(19) . . ? C1 O1 Zr1 148.1(2) . . ? C34 O2 Zr1 144.9(2) . . ? C35 O3 Zr1 173.7(3) . . ? C38 O4 Zr1 155.8(4) . . ? C41 O5 Zr1 127.9(2) . . ? C41 O5 H5 116.1 . . ? Zr1 O5 H5 116.1 . . ? O3 Zr1 O4 96.86(11) . . ? O3 Zr1 O1 98.93(10) . . ? O4 Zr1 O1 99.28(10) . . ? O3 Zr1 O2 99.35(10) . . ? O4 Zr1 O2 100.02(10) . . ? O1 Zr1 O2 151.52(9) . . ? O3 Zr1 O5 177.73(10) . . ? O4 Zr1 O5 85.30(10) . . ? O1 Zr1 O5 81.38(9) . . ? O2 Zr1 O5 79.54(9) . . ? O3 Zr1 N1 94.20(10) . . ? O4 Zr1 N1 168.89(10) . . ? O1 Zr1 N1 77.89(9) . . ? O2 Zr1 N1 79.15(9) . . ? O5 Zr1 N1 83.66(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.702 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.066 data_a12795_2aMeCN _database_code_depnum_ccdc_archive 'CCDC 897193' #TrackingRef '[ONO]ZrX2 r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H73 N3 O4 Zr' _chemical_formula_sum 'C44 H73 N3 O4 Zr' _chemical_formula_weight 799.27 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 44.5839(13) _cell_length_b 11.9319(4) _cell_length_c 20.2471(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.2300(10) _cell_angle_gamma 90.00 _cell_volume 10169.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8927 _exptl_absorpt_correction_T_max 0.9465 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18127 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_unetI/netI 0.0384 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 7.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8393 _reflns_number_gt 6890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.1072P)^2^+11.4721P] 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 8393 _refine_ls_number_parameters 489 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1785 _refine_ls_wR_factor_gt 0.1461 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 C1 C 0.13967(7) 0.5272(3) -0.00429(16) 0.0324(7) Uani 1 1 d . . . C2 C 0.15357(8) 0.6066(3) -0.03705(17) 0.0344(7) Uani 1 1 d . . . C3 C 0.18977(8) 0.6225(3) -0.0140(2) 0.0468(9) Uani 1 1 d . . . C4 C 0.20200(12) 0.6595(5) 0.0626(2) 0.0694(13) Uani 1 1 d . . . H4A H 0.2251 0.6702 0.0773 0.104 Uiso 1 1 calc R . . H4B H 0.1970 0.6019 0.0918 0.104 Uiso 1 1 calc R . . H4C H 0.1918 0.7302 0.0677 0.104 Uiso 1 1 calc R . . C5 C 0.19952(10) 0.7118(4) -0.0575(3) 0.0670(13) Uani 1 1 d . . . H5A H 0.1915 0.6908 -0.1071 0.100 Uiso 1 1 calc R . . H5B H 0.2227 0.7173 -0.0422 0.100 Uiso 1 1 calc R . . H5C H 0.1905 0.7844 -0.0512 0.100 Uiso 1 1 calc R . . C6 C 0.20599(10) 0.5126(4) -0.0228(3) 0.0686(13) Uani 1 1 d . . . H6A H 0.1979 0.4888 -0.0718 0.103 Uiso 1 1 calc R . . H6B H 0.2015 0.4546 0.0069 0.103 Uiso 1 1 calc R . . H6C H 0.2290 0.5244 -0.0090 0.103 Uiso 1 1 calc R . . C7 C 0.13294(8) 0.6710(3) -0.09014(19) 0.0371(7) Uani 1 1 d . . . H7 H 0.1420 0.7241 -0.1131 0.045 Uiso 1 1 calc R . . C8 C 0.09970(8) 0.6625(3) -0.11188(17) 0.0347(7) Uani 1 1 d . . . C9 C 0.07893(9) 0.7370(3) -0.1712(2) 0.0465(9) Uani 1 1 d . . . C10 C 0.08580(13) 0.8611(4) -0.1532(3) 0.0708(13) Uani 1 1 d . . . H10A H 0.0725 0.9073 -0.1917 0.106 Uiso 1 1 calc R . . H10B H 0.1082 0.8767 -0.1460 0.106 Uiso 1 1 calc R . . H10C H 0.0811 0.8786 -0.1104 0.106 Uiso 1 1 calc R . . C11 C 0.08674(13) 0.7120(5) -0.2387(2) 0.0684(12) Uani 1 1 d . . . H11A H 0.0736 0.7594 -0.2768 0.103 Uiso 1 1 calc R . . H11B H 0.0823 0.6329 -0.2513 0.103 Uiso 1 1 calc R . . H11C H 0.1092 0.7277 -0.2307 0.103 Uiso 1 1 calc R . . C12 C 0.04352(11) 0.7155(5) -0.1871(3) 0.0757(15) Uani 1 1 d . . . H12A H 0.0313 0.7646 -0.2253 0.114 Uiso 1 1 calc R . . H12B H 0.0378 0.7311 -0.1453 0.114 Uiso 1 1 calc R . . H12C H 0.0387 0.6371 -0.2010 0.114 Uiso 1 1 calc R . . C13 C 0.08714(8) 0.5844(3) -0.07720(18) 0.0354(7) Uani 1 1 d . . . H13 H 0.0647 0.5765 -0.0902 0.042 Uiso 1 1 calc R . . C14 C 0.10660(7) 0.5173(2) -0.02384(16) 0.0309(6) Uani 1 1 d . . . C15 C 0.09213(7) 0.4420(3) 0.01645(18) 0.0341(7) Uani 1 1 d . . . H15A H 0.0688 0.4463 -0.0059 0.041 Uiso 1 1 calc R . . H15B H 0.0971 0.4742 0.0639 0.041 Uiso 1 1 calc R . . C16 C 0.09007(8) 0.2578(3) -0.04690(17) 0.0364(7) Uani 1 1 d . . . C17 C 0.11092(9) 0.2940(3) -0.09036(19) 0.0441(8) Uani 1 1 d . . . H17A H 0.1333 0.2797 -0.0637 0.066 Uiso 1 1 calc R . . H17B H 0.1079 0.3742 -0.1010 0.066 Uiso 1 1 calc R . . H17C H 0.1049 0.2512 -0.1341 0.066 Uiso 1 1 calc R . . C18 C 0.05560(10) 0.2820(4) -0.0902(2) 0.0579(10) Uani 1 1 d . . . H18A H 0.0417 0.2597 -0.0637 0.087 Uiso 1 1 calc R . . H18B H 0.0499 0.2395 -0.1340 0.087 Uiso 1 1 calc R . . H18C H 0.0530 0.3623 -0.1006 0.087 Uiso 1 1 calc R . . C19 C 0.09495(13) 0.1309(3) -0.0336(2) 0.0591(11) Uani 1 1 d . . . H19A H 0.1171 0.1163 -0.0057 0.089 Uiso 1 1 calc R . . H19B H 0.0898 0.0915 -0.0785 0.089 Uiso 1 1 calc R . . H19C H 0.0810 0.1042 -0.0083 0.089 Uiso 1 1 calc R . . C20 C 0.08222(7) 0.2792(3) 0.07069(17) 0.0323(7) Uani 1 1 d . . . H20A H 0.0595 0.2828 0.0418 0.039 Uiso 1 1 calc R . . H20B H 0.0855 0.3355 0.1084 0.039 Uiso 1 1 calc R . . C21 C 0.08774(8) 0.1649(3) 0.10551(18) 0.0342(7) Uani 1 1 d . . . C22 C 0.06159(8) 0.1016(3) 0.10458(16) 0.0347(7) Uani 1 1 d . . . H22 H 0.0411 0.1233 0.0746 0.042 Uiso 1 1 calc R . . C23 C 0.06453(8) 0.0065(3) 0.14660(17) 0.0371(7) Uani 1 1 d . . . C24 C 0.03467(9) -0.0615(3) 0.1433(2) 0.0482(9) Uani 1 1 d . . . C25 C 0.00879(10) 0.0146(4) 0.1505(3) 0.0632(12) Uani 1 1 d . . . H25A H -0.0099 -0.0303 0.1486 0.095 Uiso 1 1 calc R . . H25B H 0.0030 0.0693 0.1122 0.095 Uiso 1 1 calc R . . H25C H 0.0165 0.0542 0.1954 0.095 Uiso 1 1 calc R . . C26 C 0.02332(11) -0.1212(4) 0.0724(3) 0.0655(12) Uani 1 1 d . . . H26A H 0.0402 -0.1705 0.0683 0.098 Uiso 1 1 calc R . . H26B H 0.0181 -0.0655 0.0348 0.098 Uiso 1 1 calc R . . H26C H 0.0044 -0.1659 0.0689 0.098 Uiso 1 1 calc R . . C27 C 0.04146(12) -0.1499(5) 0.2011(3) 0.0739(14) Uani 1 1 d . . . H27A H 0.0582 -0.2005 0.1977 0.111 Uiso 1 1 calc R . . H27B H 0.0221 -0.1930 0.1958 0.111 Uiso 1 1 calc R . . H27C H 0.0484 -0.1128 0.2469 0.111 Uiso 1 1 calc R . . C28 C 0.09505(9) -0.0241(3) 0.18801(17) 0.0388(7) Uani 1 1 d . . . H28 H 0.0975 -0.0890 0.2164 0.047 Uiso 1 1 calc R . . C29 C 0.12235(8) 0.0359(3) 0.18999(16) 0.0342(7) Uani 1 1 d . . . C30 C 0.15542(9) 0.0004(3) 0.23787(19) 0.0437(8) Uani 1 1 d . . . C31 C 0.15444(12) -0.1077(4) 0.2790(3) 0.0677(12) Uani 1 1 d . . . H31A H 0.1380 -0.1007 0.3011 0.102 Uiso 1 1 calc R . . H31B H 0.1751 -0.1193 0.3151 0.102 Uiso 1 1 calc R . . H31C H 0.1496 -0.1717 0.2469 0.102 Uiso 1 1 calc R . . C32 C 0.17037(9) 0.0920(4) 0.2921(2) 0.0535(9) Uani 1 1 d . . . H32A H 0.1566 0.1067 0.3201 0.080 Uiso 1 1 calc R . . H32B H 0.1728 0.1608 0.2680 0.080 Uiso 1 1 calc R . . H32C H 0.1912 0.0669 0.3227 0.080 Uiso 1 1 calc R . . C33 C 0.17777(11) -0.0212(4) 0.1949(3) 0.0616(11) Uani 1 1 d . . . H33A H 0.1987 -0.0442 0.2264 0.092 Uiso 1 1 calc R . . H33B H 0.1799 0.0476 0.1704 0.092 Uiso 1 1 calc R . . H33C H 0.1689 -0.0807 0.1607 0.092 Uiso 1 1 calc R . . C34 C 0.11832(8) 0.1329(3) 0.14797(17) 0.0334(7) Uani 1 1 d . . . C35 C 0.23162(16) 0.3551(8) 0.2188(4) 0.120(3) Uani 1 1 d . . . H35 H 0.2452 0.3868 0.1926 0.144 Uiso 1 1 calc R . . C36 C 0.2275(3) 0.448(2) 0.2696(8) 0.266(11) Uani 1 1 d . . . H36A H 0.2168 0.5132 0.2424 0.399 Uiso 1 1 calc R . . H36B H 0.2485 0.4706 0.3013 0.399 Uiso 1 1 calc R . . H36C H 0.2147 0.4188 0.2969 0.399 Uiso 1 1 calc R . . C37 C 0.2465(2) 0.2666(11) 0.2538(9) 0.226(9) Uani 1 1 d . . . H37A H 0.2479 0.2083 0.2207 0.338 Uiso 1 1 calc R . . H37B H 0.2348 0.2377 0.2834 0.338 Uiso 1 1 calc R . . H37C H 0.2680 0.2881 0.2831 0.338 Uiso 1 1 calc R . . C38 C 0.1928(10) 0.151(3) 0.015(2) 0.171(7) Uani 0.50 1 d PU A 1 H38A H 0.1903 0.1815 -0.0323 0.205 Uiso 0.50 1 calc PR A 1 C38' C 0.1909(7) 0.155(2) 0.0042(12) 0.128(9) Uani 0.50 1 d P A 2 H38B H 0.2095 0.1499 0.0483 0.153 Uiso 0.50 1 calc PR A 2 C39 C 0.2295(3) 0.1813(14) 0.0633(12) 0.137(7) Uani 0.50 1 d P A 1 H39A H 0.2443 0.1394 0.0459 0.206 Uiso 0.50 1 calc PR A 1 H39B H 0.2329 0.1605 0.1120 0.206 Uiso 0.50 1 calc PR A 1 H39C H 0.2332 0.2618 0.0605 0.206 Uiso 0.50 1 calc PR A 1 C39' C 0.2079(4) 0.1898(12) -0.0274(9) 0.105(5) Uani 0.50 1 d P A 2 H39D H 0.2098 0.2714 -0.0223 0.157 Uiso 0.50 1 calc PR A 2 H39E H 0.1986 0.1706 -0.0770 0.157 Uiso 0.50 1 calc PR A 2 H39F H 0.2290 0.1557 -0.0083 0.157 Uiso 0.50 1 calc PR A 2 C40 C 0.1861(3) 0.0372(8) 0.0054(8) 0.179(5) Uani 1 1 d U . . H40A H 0.2025 0.0007 -0.0098 0.269 Uiso 1 1 calc R A 1 H40B H 0.1653 0.0270 -0.0305 0.269 Uiso 1 1 calc R A 1 H40C H 0.1860 0.0036 0.0494 0.269 Uiso 1 1 calc R A 1 C41 C 0.14121(12) 0.4861(4) 0.2259(2) 0.0613(11) Uani 1 1 d . . . C42 C 0.13764(18) 0.5537(5) 0.2818(3) 0.0864(17) Uani 1 1 d . . . H42A H 0.1564 0.6016 0.3008 0.130 Uiso 1 1 calc R . . H42B H 0.1355 0.5049 0.3189 0.130 Uiso 1 1 calc R . . H42C H 0.1187 0.6007 0.2638 0.130 Uiso 1 1 calc R . . C43 C 0.10450(16) 0.7416(5) 0.0954(3) 0.0892(18) Uani 1 1 d . . . C44 C 0.1089(2) 0.8224(6) 0.0464(4) 0.103(2) Uani 1 1 d . . . H44A H 0.1001 0.7924 -0.0012 0.154 Uiso 1 1 calc R . . H44B H 0.1316 0.8375 0.0572 0.154 Uiso 1 1 calc R . . H44C H 0.0978 0.8921 0.0498 0.154 Uiso 1 1 calc R . . N1 N 0.10096(6) 0.31837(19) 0.02516(15) 0.0305(6) Uani 1 1 d . . . N2 N 0.14329(8) 0.4359(3) 0.17961(17) 0.0517(8) Uani 1 1 d . . . N3 N 0.09957(18) 0.6800(5) 0.1347(3) 0.109(2) Uani 1 1 d . . . O1 O 0.15760(5) 0.46002(19) 0.04675(13) 0.0403(5) Uani 1 1 d . . . O2 O 0.14291(5) 0.19715(19) 0.14890(13) 0.0390(5) Uani 1 1 d . . . O4 O 0.20107(6) 0.3374(2) 0.17023(15) 0.0564(7) Uani 1 1 d . . . O3 O 0.17339(7) 0.2149(2) 0.03942(16) 0.0557(7) Uani 1 1 d . . . Zr1 Zr 0.160557(7) 0.31473(2) 0.100388(16) 0.03243(16) Uani 1 1 d . A . 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 C1 0.0337(16) 0.0295(15) 0.0321(16) 0.0006(13) 0.0083(13) -0.0011(12) C2 0.0337(16) 0.0332(16) 0.0369(17) -0.0006(14) 0.0124(14) -0.0030(13) C3 0.0363(18) 0.050(2) 0.052(2) 0.0116(18) 0.0122(16) -0.0101(16) C4 0.056(3) 0.083(3) 0.054(3) 0.001(2) -0.003(2) -0.028(2) C5 0.042(2) 0.074(3) 0.084(3) 0.025(3) 0.020(2) -0.015(2) C6 0.040(2) 0.076(3) 0.096(4) 0.019(3) 0.031(2) 0.009(2) C7 0.0431(19) 0.0301(16) 0.0424(19) 0.0044(14) 0.0198(16) -0.0039(13) C8 0.0387(17) 0.0329(16) 0.0320(16) 0.0040(13) 0.0109(14) 0.0004(13) C9 0.045(2) 0.044(2) 0.051(2) 0.0167(17) 0.0170(17) 0.0055(16) C10 0.079(3) 0.050(2) 0.080(3) 0.025(2) 0.022(3) 0.015(2) C11 0.075(3) 0.082(3) 0.049(2) 0.020(2) 0.022(2) 0.011(2) C12 0.049(2) 0.091(3) 0.083(3) 0.045(3) 0.016(2) 0.013(2) C13 0.0303(16) 0.0330(16) 0.0431(18) 0.0029(14) 0.0127(14) 0.0015(13) C14 0.0326(16) 0.0251(15) 0.0365(16) 0.0003(13) 0.0133(14) -0.0009(12) C15 0.0312(15) 0.0292(15) 0.0441(18) 0.0048(14) 0.0154(14) 0.0026(12) C16 0.0422(18) 0.0363(17) 0.0313(16) -0.0036(14) 0.0129(14) -0.0051(14) C17 0.051(2) 0.048(2) 0.0373(19) -0.0045(16) 0.0189(17) -0.0040(16) C18 0.048(2) 0.082(3) 0.040(2) -0.011(2) 0.0094(18) -0.016(2) C19 0.097(3) 0.035(2) 0.059(2) -0.0094(18) 0.043(2) -0.014(2) C20 0.0299(15) 0.0343(16) 0.0338(16) 0.0054(13) 0.0121(13) 0.0006(13) C21 0.0393(18) 0.0310(16) 0.0362(17) 0.0006(13) 0.0176(15) -0.0007(13) C22 0.0357(16) 0.0370(17) 0.0304(16) -0.0006(13) 0.0096(13) -0.0057(13) C23 0.0429(18) 0.0341(16) 0.0359(17) -0.0023(14) 0.0152(15) -0.0089(14) C24 0.051(2) 0.045(2) 0.047(2) 0.0031(17) 0.0139(17) -0.0156(17) C25 0.053(2) 0.062(3) 0.085(3) -0.001(2) 0.038(2) -0.017(2) C26 0.059(3) 0.059(3) 0.072(3) -0.015(2) 0.014(2) -0.022(2) C27 0.071(3) 0.071(3) 0.080(3) 0.029(3) 0.025(3) -0.024(2) C28 0.054(2) 0.0298(16) 0.0340(17) 0.0023(13) 0.0164(16) -0.0032(14) C29 0.0429(18) 0.0299(16) 0.0301(16) -0.0008(13) 0.0123(14) -0.0003(13) C30 0.0451(19) 0.0392(18) 0.044(2) 0.0101(16) 0.0116(16) 0.0059(15) C31 0.064(3) 0.056(3) 0.072(3) 0.031(2) 0.007(2) 0.004(2) C32 0.044(2) 0.057(2) 0.049(2) 0.0039(19) 0.0019(17) 0.0001(17) C33 0.056(2) 0.064(3) 0.068(3) 0.010(2) 0.026(2) 0.022(2) C34 0.0378(17) 0.0312(16) 0.0347(16) 0.0006(13) 0.0165(14) -0.0018(13) C35 0.067(4) 0.157(7) 0.101(5) 0.039(5) -0.020(3) -0.023(4) C36 0.147(10) 0.48(3) 0.165(10) -0.167(17) 0.046(9) -0.122(15) C37 0.094(6) 0.192(11) 0.276(15) 0.118(12) -0.095(8) -0.040(7) C38 0.215(14) 0.107(10) 0.260(15) -0.046(10) 0.173(13) 0.042(10) C38' 0.169(16) 0.152(18) 0.119(12) 0.083(12) 0.123(13) 0.115(13) C39 0.039(6) 0.148(13) 0.23(2) -0.050(12) 0.054(9) 0.029(6) C39' 0.109(10) 0.105(10) 0.126(12) -0.018(8) 0.075(10) -0.001(7) C40 0.227(11) 0.102(6) 0.265(13) -0.050(7) 0.157(11) 0.031(6) C41 0.090(3) 0.046(2) 0.047(2) 0.003(2) 0.020(2) -0.005(2) C42 0.142(5) 0.066(3) 0.061(3) -0.004(2) 0.047(3) 0.005(3) C43 0.117(5) 0.066(3) 0.069(3) -0.017(3) 0.009(3) 0.026(3) C44 0.137(6) 0.104(5) 0.084(4) -0.033(4) 0.058(4) -0.016(4) N1 0.0325(14) 0.0251(13) 0.0381(15) 0.0024(10) 0.0176(12) -0.0003(10) N2 0.0556(19) 0.0487(18) 0.0464(18) -0.0087(16) 0.0111(15) 0.0029(15) N3 0.151(6) 0.072(3) 0.083(4) -0.002(3) 0.010(4) 0.030(3) O1 0.0288(11) 0.0368(12) 0.0528(14) 0.0098(11) 0.0098(10) -0.0028(9) O2 0.0312(12) 0.0392(12) 0.0442(14) 0.0095(10) 0.0093(10) -0.0009(9) O4 0.0371(14) 0.0631(17) 0.0518(16) 0.0155(13) -0.0085(12) -0.0083(12) O3 0.0524(16) 0.0569(16) 0.0694(18) 0.0065(14) 0.0359(15) 0.0177(13) Zr1 0.0264(2) 0.0333(2) 0.0368(2) 0.00551(12) 0.00931(15) 0.00004(11) _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 C1 O1 1.343(4) . ? C1 C14 1.400(4) . ? C1 C2 1.411(4) . ? C2 C7 1.393(5) . ? C2 C3 1.537(5) . ? C3 C4 1.530(6) . ? C3 C5 1.533(5) . ? C3 C6 1.536(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.404(5) . ? C7 H7 0.9500 . ? C8 C13 1.391(5) . ? C8 C9 1.536(5) . ? C9 C12 1.526(6) . ? C9 C10 1.531(6) . ? C9 C11 1.545(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 C14 1.394(5) . ? C13 H13 0.9500 . ? C14 C15 1.495(4) . ? C15 N1 1.522(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.525(5) . ? C16 C17 1.537(5) . ? C16 C19 1.541(5) . ? C16 N1 1.556(4) . ? 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 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N1 1.508(4) . ? C20 C21 1.518(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.384(4) . ? C21 C34 1.404(5) . ? C22 C23 1.398(5) . ? C22 H22 0.9500 . ? C23 C28 1.391(5) . ? C23 C24 1.541(5) . ? C24 C25 1.513(6) . ? C24 C27 1.530(6) . ? C24 C26 1.531(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 C29 1.401(5) . ? C28 H28 0.9500 . ? C29 C34 1.412(4) . ? C29 C30 1.533(5) . ? C30 C32 1.536(6) . ? C30 C31 1.544(5) . ? C30 C33 1.545(6) . ? 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 O2 1.333(4) . ? C35 C37 1.323(12) . ? C35 O4 1.409(7) . ? C35 C36 1.56(2) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 O3 1.36(3) . ? C38 C40 1.39(4) . ? C38 C39 1.64(5) . ? C38 H38A 1.0000 . ? C38' C39' 1.22(3) . ? C38' O3 1.41(2) . ? C38' C40 1.42(3) . ? C38' H38B 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C39' H39D 0.9800 . ? C39' H39E 0.9800 . ? C39' H39F 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N2 1.142(5) . ? C41 C42 1.441(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 N3 1.156(9) . ? C43 C44 1.442(11) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? N1 Zr1 2.592(3) . ? N2 Zr1 2.464(3) . ? O1 Zr1 2.027(2) . ? O2 Zr1 2.015(2) . ? O4 Zr1 1.911(3) . ? O3 Zr1 1.932(3) . ? 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 C1 C14 118.1(3) . . ? O1 C1 C2 121.3(3) . . ? C14 C1 C2 120.5(3) . . ? C7 C2 C1 116.9(3) . . ? C7 C2 C3 121.7(3) . . ? C1 C2 C3 121.4(3) . . ? C4 C3 C5 108.0(4) . . ? C4 C3 C6 109.8(4) . . ? C5 C3 C6 107.1(4) . . ? C4 C3 C2 109.3(3) . . ? C5 C3 C2 112.3(3) . . ? C6 C3 C2 110.3(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 C8 124.2(3) . . ? C2 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? C13 C8 C7 116.7(3) . . ? C13 C8 C9 122.9(3) . . ? C7 C8 C9 120.3(3) . . ? C12 C9 C10 108.9(4) . . ? C12 C9 C8 112.5(3) . . ? C10 C9 C8 110.6(3) . . ? C12 C9 C11 107.4(4) . . ? C10 C9 C11 108.2(4) . . ? C8 C9 C11 109.0(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 C14 121.6(3) . . ? C8 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C1 120.0(3) . . ? C13 C14 C15 119.8(3) . . ? C1 C14 C15 120.0(3) . . ? C14 C15 N1 120.3(2) . . ? C14 C15 H15A 107.3 . . ? N1 C15 H15A 107.3 . . ? C14 C15 H15B 107.3 . . ? N1 C15 H15B 107.3 . . ? H15A C15 H15B 106.9 . . ? C18 C16 C17 107.6(3) . . ? C18 C16 C19 110.1(3) . . ? C17 C16 C19 107.4(3) . . ? C18 C16 N1 113.3(3) . . ? C17 C16 N1 110.2(3) . . ? C19 C16 N1 108.1(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 C21 121.6(3) . . ? N1 C20 H20A 106.9 . . ? C21 C20 H20A 106.9 . . ? N1 C20 H20B 106.9 . . ? C21 C20 H20B 106.9 . . ? H20A C20 H20B 106.7 . . ? C22 C21 C34 120.2(3) . . ? C22 C21 C20 118.5(3) . . ? C34 C21 C20 120.4(3) . . ? C21 C22 C23 121.7(3) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C28 C23 C22 117.1(3) . . ? C28 C23 C24 123.2(3) . . ? C22 C23 C24 119.6(3) . . ? C25 C24 C27 107.7(4) . . ? C25 C24 C26 110.0(4) . . ? C27 C24 C26 108.5(4) . . ? C25 C24 C23 110.8(3) . . ? C27 C24 C23 112.3(3) . . ? C26 C24 C23 107.5(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 C29 123.5(3) . . ? C23 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C28 C29 C34 117.7(3) . . ? C28 C29 C30 121.5(3) . . ? C34 C29 C30 120.8(3) . . ? C29 C30 C32 110.8(3) . . ? C29 C30 C31 112.3(3) . . ? C32 C30 C31 107.0(3) . . ? C29 C30 C33 110.8(3) . . ? C32 C30 C33 108.2(3) . . ? C31 C30 C33 107.6(3) . . ? 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 . . ? O2 C34 C21 118.7(3) . . ? O2 C34 C29 121.5(3) . . ? C21 C34 C29 119.8(3) . . ? C37 C35 O4 117.0(8) . . ? C37 C35 C36 111.2(14) . . ? O4 C35 C36 105.6(8) . . ? C37 C35 H35 107.5 . . ? O4 C35 H35 107.5 . . ? C36 C35 H35 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O3 C38 C40 118(3) . . ? O3 C38 C39 107(2) . . ? C40 C38 C39 115(2) . . ? O3 C38 H38A 105.3 . . ? C40 C38 H38A 105.3 . . ? C39 C38 H38A 105.3 . . ? C39' C38' O3 129(2) . . ? C39' C38' C40 118.0(19) . . ? O3 C38' C40 112.6(17) . . ? C39' C38' H38B 90.7 . . ? O3 C38' H38B 90.7 . . ? C40 C38' H38B 90.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38' C39' H39D 109.5 . . ? C38' C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C38' C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C38 C40 C38' 9(2) . . ? C38 C40 H40A 109.5 . . ? C38' C40 H40A 107.7 . . ? C38 C40 H40B 109.5 . . ? C38' C40 H40B 102.7 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? C38' C40 H40C 117.7 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N2 C41 C42 177.0(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N3 C43 C44 176.4(7) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C20 N1 C15 101.3(2) . . ? C20 N1 C16 111.4(2) . . ? C15 N1 C16 110.6(2) . . ? C20 N1 Zr1 107.62(18) . . ? C15 N1 Zr1 105.09(18) . . ? C16 N1 Zr1 119.10(18) . . ? C41 N2 Zr1 165.9(4) . . ? C1 O1 Zr1 147.1(2) . . ? C34 O2 Zr1 147.7(2) . . ? C35 O4 Zr1 176.9(4) . . ? C38 O3 C38' 9(2) . . ? C38 O3 Zr1 158.9(19) . . ? C38' O3 Zr1 164.6(16) . . ? O4 Zr1 O3 98.82(14) . . ? O4 Zr1 O2 99.41(11) . . ? O3 Zr1 O2 97.34(12) . . ? O4 Zr1 O1 98.86(10) . . ? O3 Zr1 O1 99.52(11) . . ? O2 Zr1 O1 152.84(9) . . ? O4 Zr1 N2 81.78(13) . . ? O3 Zr1 N2 177.85(12) . . ? O2 Zr1 N2 80.52(11) . . ? O1 Zr1 N2 82.40(11) . . ? O4 Zr1 N1 165.61(12) . . ? O3 Zr1 N1 95.56(11) . . ? O2 Zr1 N1 78.98(9) . . ? O1 Zr1 N1 78.32(8) . . ? N2 Zr1 N1 83.86(10) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.608 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.074 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.001 0.376 541 41 ' ' 2 0.237 0.117 0.583 7 0 ' ' 3 0.763 0.117 0.917 7 0 ' ' 4 0.320 0.193 0.297 17 1 ' ' 5 0.680 0.193 0.203 16 0 ' ' 6 0.293 0.200 0.165 7 0 ' ' 7 0.707 0.200 0.335 7 0 ' ' 8 0.000 0.499 0.054 541 41 ' ' 9 0.180 0.306 0.703 16 0 ' ' 10 0.820 0.306 0.797 17 1 ' ' 11 0.207 0.300 0.835 7 0 ' ' 12 0.793 0.300 0.665 7 0 ' ' 13 0.263 0.383 0.417 7 0 ' ' 14 0.737 0.383 0.083 7 0 ' ' 15 0.263 0.617 0.917 7 0 ' ' 16 0.737 0.617 0.583 7 0 ' ' 17 0.180 0.693 0.203 16 0 ' ' 18 0.820 0.693 0.297 17 1 ' ' 19 0.207 0.700 0.335 7 0 ' ' 20 0.793 0.700 0.165 7 0 ' ' 21 0.320 0.806 0.797 17 1 ' ' 22 0.680 0.806 0.703 16 0 ' ' 23 0.293 0.800 0.665 7 0 ' ' 24 0.707 0.800 0.835 7 0 ' ' 25 0.237 0.883 0.083 7 0 ' ' 26 0.763 0.883 0.417 7 0 ' ' _platon_squeeze_details ; ; data_a12645_2cHOiPr _database_code_depnum_ccdc_archive 'CCDC 897194' #TrackingRef '[ONO]ZrX2 r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H73 N O5 Zr' _chemical_formula_sum 'C42 H73 N O5 Zr' _chemical_formula_weight 763.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6470(16) _cell_length_b 20.835(3) _cell_length_c 22.341(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.473(2) _cell_angle_gamma 90.00 _cell_volume 4461.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8969 _exptl_absorpt_correction_T_max 0.9639 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27658 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0500 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7839 _reflns_number_gt 5737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.1059P)^2^+6.3654P] 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 7839 _refine_ls_number_parameters 438 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1890 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.998 _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 C1 C 0.5125(4) 0.87160(19) 0.65176(19) 0.0385(10) Uani 1 1 d . . . C2 C 0.5642(5) 0.8542(2) 0.5980(2) 0.0439(10) Uani 1 1 d . . . C3 C 0.7088(5) 0.8227(2) 0.5971(2) 0.0498(11) Uani 1 1 d . . . C4 C 0.7166(5) 0.7613(2) 0.6353(3) 0.0612(14) Uani 1 1 d . . . H4A H 0.6425 0.7317 0.6193 0.092 Uiso 1 1 calc R . . H4B H 0.7049 0.7721 0.6771 0.092 Uiso 1 1 calc R . . H4C H 0.8076 0.7407 0.6338 0.092 Uiso 1 1 calc R . . C5 C 0.8230(5) 0.8699(3) 0.6225(3) 0.0629(14) Uani 1 1 d . . . H5A H 0.9147 0.8496 0.6223 0.094 Uiso 1 1 calc R . . H5B H 0.8086 0.8813 0.6639 0.094 Uiso 1 1 calc R . . H5C H 0.8186 0.9087 0.5976 0.094 Uiso 1 1 calc R . . C6 C 0.7380(7) 0.8043(3) 0.5329(3) 0.0800(18) Uani 1 1 d . . . H6A H 0.6659 0.7746 0.5153 0.120 Uiso 1 1 calc R . . H6B H 0.8296 0.7837 0.5345 0.120 Uiso 1 1 calc R . . H6C H 0.7371 0.8431 0.5080 0.120 Uiso 1 1 calc R . . C7 C 0.4787(5) 0.8658(2) 0.5447(2) 0.0495(12) Uani 1 1 d . . . H7 H 0.5133 0.8549 0.5079 0.059 Uiso 1 1 calc R . . C8 C 0.3450(5) 0.8926(2) 0.5419(2) 0.0468(11) Uani 1 1 d . . . C9 C 0.2615(6) 0.9087(2) 0.4809(2) 0.0592(14) Uani 1 1 d . . . C10 C 0.2757(6) 0.8568(3) 0.4351(2) 0.0690(16) Uani 1 1 d . . . H10A H 0.2216 0.8684 0.3969 0.103 Uiso 1 1 calc R . . H10B H 0.2406 0.8162 0.4497 0.103 Uiso 1 1 calc R . . H10C H 0.3742 0.8519 0.4290 0.103 Uiso 1 1 calc R . . C11 C 0.3192(12) 0.9704(3) 0.4579(3) 0.158(5) Uani 1 1 d . . . H11A H 0.3109 1.0048 0.4872 0.236 Uiso 1 1 calc R . . H11B H 0.2665 0.9820 0.4193 0.236 Uiso 1 1 calc R . . H11C H 0.4177 0.9643 0.4523 0.236 Uiso 1 1 calc R . . C12 C 0.1086(8) 0.9166(5) 0.4868(3) 0.140(4) Uani 1 1 d . . . H12A H 0.0963 0.9503 0.5164 0.209 Uiso 1 1 calc R . . H12B H 0.0708 0.8761 0.5002 0.209 Uiso 1 1 calc R . . H12C H 0.0591 0.9288 0.4478 0.209 Uiso 1 1 calc R . . C13 C 0.2964(5) 0.9064(2) 0.5961(2) 0.0448(11) Uani 1 1 d . . . H13 H 0.2049 0.9232 0.5961 0.054 Uiso 1 1 calc R . . C14 C 0.3778(5) 0.8964(2) 0.6508(2) 0.0411(10) Uani 1 1 d . . . C15 C 0.3212(4) 0.91049(19) 0.70908(19) 0.0384(10) Uani 1 1 d . . . H15A H 0.3200 0.8703 0.7326 0.046 Uiso 1 1 calc R . . H15B H 0.2236 0.9255 0.7004 0.046 Uiso 1 1 calc R . . C16 C 0.4228(4) 1.01931(19) 0.71125(19) 0.0383(9) Uani 1 1 d . . . H16A H 0.4790 1.0078 0.6784 0.046 Uiso 1 1 calc R . . H16B H 0.4786 1.0499 0.7379 0.046 Uiso 1 1 calc R . . C17 C 0.2921(5) 1.0542(2) 0.6832(2) 0.0490(11) Uani 1 1 d . . . H17A H 0.2308 1.0239 0.6585 0.059 Uiso 1 1 calc R . . H17B H 0.2397 1.0713 0.7154 0.059 Uiso 1 1 calc R . . C18 C 0.3339(8) 1.1087(4) 0.6443(4) 0.112(3) Uani 1 1 d . . . H18A H 0.2501 1.1310 0.6261 0.168 Uiso 1 1 calc R . . H18B H 0.3854 1.0916 0.6125 0.168 Uiso 1 1 calc R . . H18C H 0.3933 1.1389 0.6692 0.168 Uiso 1 1 calc R . . C19 C 0.3243(4) 0.97399(19) 0.79879(18) 0.0362(9) Uani 1 1 d . . . H19A H 0.3157 0.9339 0.8218 0.043 Uiso 1 1 calc R . . H19B H 0.2289 0.9881 0.7833 0.043 Uiso 1 1 calc R . . C20 C 0.3901(4) 1.0245(2) 0.84083(17) 0.0362(9) Uani 1 1 d . A . C21 C 0.3183(5) 1.0803(2) 0.84983(19) 0.0414(10) Uani 1 1 d . . . H21 H 0.2291 1.0869 0.8280 0.050 Uiso 1 1 calc R . . C22 C 0.3730(5) 1.1272(2) 0.8900(2) 0.0472(11) Uani 1 1 d . A . C23 C 0.2928(5) 1.1894(2) 0.8982(2) 0.0593(14) Uani 1 1 d . . . C24' C 0.3788(19) 1.2478(9) 0.9096(8) 0.091(5) Uiso 0.40 1 d P A 1 H24D H 0.3180 1.2847 0.9146 0.136 Uiso 0.40 1 calc PR A 1 H24E H 0.4320 1.2555 0.8755 0.136 Uiso 0.40 1 calc PR A 1 H24F H 0.4434 1.2420 0.9464 0.136 Uiso 0.40 1 calc PR A 1 C25' C 0.1687(18) 1.2021(8) 0.8497(8) 0.085(5) Uiso 0.40 1 d P A 1 H25A H 0.1227 1.2423 0.8589 0.127 Uiso 0.40 1 calc PR A 1 H25B H 0.1019 1.1666 0.8493 0.127 Uiso 0.40 1 calc PR A 1 H25C H 0.2028 1.2055 0.8101 0.127 Uiso 0.40 1 calc PR A 1 C26' C 0.211(2) 1.1830(9) 0.9562(8) 0.099(5) Uiso 0.40 1 d P A 1 H26A H 0.1588 1.2226 0.9614 0.148 Uiso 0.40 1 calc PR A 1 H26B H 0.2778 1.1757 0.9920 0.148 Uiso 0.40 1 calc PR A 1 H26C H 0.1459 1.1467 0.9509 0.148 Uiso 0.40 1 calc PR A 1 C24 C 0.3276(15) 1.2346(7) 0.8452(6) 0.110(4) Uiso 0.60 1 d P A 2 H24A H 0.2790 1.2757 0.8478 0.166 Uiso 0.60 1 calc PR A 2 H24B H 0.2968 1.2141 0.8065 0.166 Uiso 0.60 1 calc PR A 2 H24C H 0.4284 1.2421 0.8484 0.166 Uiso 0.60 1 calc PR A 2 C25 C 0.1465(15) 1.1792(7) 0.8953(7) 0.114(4) Uiso 0.60 1 d P A 2 H25D H 0.0998 1.2201 0.9014 0.170 Uiso 0.60 1 calc PR A 2 H25E H 0.1269 1.1488 0.9268 0.170 Uiso 0.60 1 calc PR A 2 H25F H 0.1118 1.1617 0.8557 0.170 Uiso 0.60 1 calc PR A 2 C26 C 0.3516(14) 1.2261(6) 0.9532(6) 0.101(4) Uiso 0.60 1 d P A 2 H26D H 0.4507 1.2349 0.9510 0.151 Uiso 0.60 1 calc PR A 2 H26E H 0.3413 1.2006 0.9893 0.151 Uiso 0.60 1 calc PR A 2 H26F H 0.3012 1.2667 0.9552 0.151 Uiso 0.60 1 calc PR A 2 C27 C 0.5019(5) 1.1143(2) 0.9217(2) 0.0489(11) Uani 1 1 d . . . H27 H 0.5408 1.1456 0.9496 0.059 Uiso 1 1 calc R A . C28 C 0.5784(5) 1.0582(2) 0.91531(19) 0.0436(10) Uani 1 1 d . A . C29 C 0.7170(5) 1.0456(2) 0.9553(2) 0.0530(12) Uani 1 1 d . . . C30 C 0.7468(8) 1.0965(3) 1.0042(3) 0.104(3) Uani 1 1 d . A . H30A H 0.8359 1.0870 1.0281 0.157 Uiso 1 1 calc R . . H30B H 0.6719 1.0963 1.0304 0.157 Uiso 1 1 calc R . . H30C H 0.7517 1.1388 0.9854 0.157 Uiso 1 1 calc R . . C31 C 0.7113(6) 0.9810(3) 0.9872(2) 0.0664(15) Uani 1 1 d . A . H31A H 0.6942 0.9468 0.9571 0.100 Uiso 1 1 calc R . . H31B H 0.6356 0.9815 1.0130 0.100 Uiso 1 1 calc R . . H31C H 0.8002 0.9732 1.0119 0.100 Uiso 1 1 calc R . . C32 C 0.8394(5) 1.0448(3) 0.9160(3) 0.0769(18) Uani 1 1 d . A . H32A H 0.8215 1.0124 0.8843 0.115 Uiso 1 1 calc R . . H32B H 0.9262 1.0344 0.9413 0.115 Uiso 1 1 calc R . . H32C H 0.8480 1.0871 0.8977 0.115 Uiso 1 1 calc R . . C33 C 0.5213(4) 1.0136(2) 0.87198(18) 0.0375(10) Uani 1 1 d . . . C34 C 0.5131(6) 0.7779(2) 0.8510(2) 0.0584(13) Uani 1 1 d . . . H34 H 0.6124 0.7698 0.8674 0.070 Uiso 1 1 calc R . . C35 C 0.4213(8) 0.7623(3) 0.8984(3) 0.099(2) Uani 1 1 d . . . H35A H 0.4479 0.7888 0.9341 0.148 Uiso 1 1 calc R . . H35B H 0.4317 0.7169 0.9092 0.148 Uiso 1 1 calc R . . H35C H 0.3240 0.7711 0.8830 0.148 Uiso 1 1 calc R . . C36 C 0.4793(11) 0.7391(4) 0.7974(4) 0.126(3) Uani 1 1 d . . . H36A H 0.5418 0.7504 0.7673 0.189 Uiso 1 1 calc R . . H36B H 0.3825 0.7472 0.7808 0.189 Uiso 1 1 calc R . . H36C H 0.4909 0.6936 0.8078 0.189 Uiso 1 1 calc R . . C37 C 0.9303(10) 0.8407(6) 0.8373(4) 0.158(5) Uani 1 1 d . . . H37 H 0.9679 0.8843 0.8485 0.190 Uiso 1 1 calc R B 3 C38 C 0.9430(11) 0.8190(7) 0.8940(5) 0.191(6) Uani 1 1 d . C . H38A H 0.8848 0.8450 0.9179 0.286 Uiso 1 1 calc R . . H38B H 1.0407 0.8220 0.9113 0.286 Uiso 1 1 calc R . . H38C H 0.9126 0.7741 0.8943 0.286 Uiso 1 1 calc R . . C39 C 1.0172(17) 0.8313(8) 0.7924(7) 0.130(5) Uiso 0.60 1 d P C 3 H39A H 0.9776 0.8530 0.7555 0.194 Uiso 0.60 1 calc PR C 3 H39B H 1.0255 0.7853 0.7846 0.194 Uiso 0.60 1 calc PR C 3 H39C H 1.1097 0.8491 0.8056 0.194 Uiso 0.60 1 calc PR C 3 C39' C 0.941(3) 0.7773(12) 0.8078(11) 0.131(8) Uiso 0.40 1 d P C 4 H39D H 0.9347 0.7831 0.7640 0.196 Uiso 0.40 1 calc PR C 4 H39E H 0.8656 0.7494 0.8178 0.196 Uiso 0.40 1 calc PR C 4 H39F H 1.0314 0.7576 0.8221 0.196 Uiso 0.40 1 calc PR C 4 C40 C 0.7987(9) 1.0394(3) 0.7332(5) 0.127(3) Uani 1 1 d U . . H40 H 0.7427 1.0440 0.6929 0.152 Uiso 1 1 calc R . . C41 C 0.7636(7) 1.1021(3) 0.7578(3) 0.0844(19) Uani 1 1 d U . . H41A H 0.6663 1.1017 0.7665 0.127 Uiso 1 1 calc R . . H41B H 0.7762 1.1358 0.7283 0.127 Uiso 1 1 calc R . . H41C H 0.8249 1.1105 0.7950 0.127 Uiso 1 1 calc R . . C42 C 0.9280(7) 1.0289(4) 0.7124(4) 0.102(2) Uani 1 1 d . . . H42A H 0.9286 0.9864 0.6936 0.153 Uiso 1 1 calc R . . H42B H 1.0018 1.0309 0.7463 0.153 Uiso 1 1 calc R . . H42C H 0.9445 1.0618 0.6827 0.153 Uiso 1 1 calc R . . N1 N 0.4031(3) 0.96004(15) 0.74671(14) 0.0343(8) Uani 1 1 d . A . O2 O 0.5897(3) 0.86513(14) 0.70593(13) 0.0428(7) Uani 1 1 d . A . O1 O 0.5877(3) 0.95889(14) 0.86044(13) 0.0415(7) Uani 1 1 d . A . O5 O 0.4985(4) 0.84343(16) 0.83369(18) 0.0665(10) Uani 1 1 d . A . H3 H 0.4155 0.8626 0.8445 0.080 Uiso 1 1 calc R . . O4 O 0.7935(3) 0.86312(16) 0.81721(15) 0.0567(9) Uani 1 1 d . A . O3 O 0.7294(3) 0.98821(15) 0.75279(15) 0.0527(8) Uani 1 1 d . A . Zr1 Zr 0.63833(4) 0.915045(19) 0.783490(18) 0.03666(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(2) 0.031(2) 0.045(2) -0.0029(18) 0.0015(19) 0.0028(18) C2 0.045(3) 0.033(2) 0.053(3) -0.0035(19) 0.005(2) 0.0039(19) C3 0.048(3) 0.049(3) 0.054(3) -0.007(2) 0.013(2) 0.010(2) C4 0.051(3) 0.047(3) 0.086(4) -0.006(3) 0.011(3) 0.014(2) C5 0.049(3) 0.064(3) 0.079(4) -0.001(3) 0.021(3) 0.004(3) C6 0.072(4) 0.098(5) 0.073(4) -0.013(3) 0.016(3) 0.032(4) C7 0.060(3) 0.044(3) 0.045(2) -0.006(2) 0.007(2) 0.004(2) C8 0.055(3) 0.034(2) 0.049(3) -0.006(2) -0.003(2) 0.003(2) C9 0.075(4) 0.045(3) 0.054(3) -0.002(2) -0.010(3) 0.007(3) C10 0.083(4) 0.069(4) 0.051(3) -0.008(3) -0.010(3) -0.003(3) C11 0.284(13) 0.056(4) 0.107(6) 0.032(4) -0.092(7) -0.048(6) C12 0.097(6) 0.251(12) 0.063(4) -0.022(5) -0.028(4) 0.091(7) C13 0.041(3) 0.037(2) 0.054(3) -0.009(2) -0.004(2) 0.0018(19) C14 0.042(2) 0.034(2) 0.047(2) -0.0041(18) 0.004(2) -0.0001(19) C15 0.027(2) 0.036(2) 0.052(2) -0.0024(19) 0.0012(18) -0.0031(17) C16 0.035(2) 0.036(2) 0.045(2) -0.0002(18) 0.0069(18) 0.0010(18) C17 0.044(3) 0.048(3) 0.055(3) 0.005(2) 0.005(2) 0.012(2) C18 0.092(5) 0.102(5) 0.147(7) 0.079(5) 0.032(5) 0.037(4) C19 0.026(2) 0.037(2) 0.046(2) -0.0009(18) 0.0061(18) -0.0001(17) C20 0.033(2) 0.040(2) 0.036(2) -0.0028(18) 0.0075(18) -0.0021(18) C21 0.034(2) 0.046(3) 0.044(2) -0.002(2) 0.0045(19) 0.0051(19) C22 0.046(3) 0.045(3) 0.051(3) -0.006(2) 0.009(2) 0.001(2) C23 0.051(3) 0.047(3) 0.078(3) -0.019(3) 0.000(3) 0.007(2) C27 0.050(3) 0.045(3) 0.051(3) -0.011(2) 0.000(2) -0.002(2) C28 0.040(2) 0.047(3) 0.044(2) 0.001(2) 0.002(2) -0.002(2) C29 0.046(3) 0.056(3) 0.054(3) -0.006(2) -0.009(2) -0.001(2) C30 0.104(6) 0.094(5) 0.100(5) -0.040(4) -0.055(4) 0.018(4) C31 0.057(3) 0.086(4) 0.054(3) 0.015(3) -0.008(3) 0.008(3) C32 0.041(3) 0.104(5) 0.083(4) 0.013(4) -0.008(3) -0.012(3) C33 0.038(2) 0.038(2) 0.037(2) 0.0036(18) 0.0079(18) -0.0004(19) C34 0.056(3) 0.046(3) 0.074(3) 0.017(3) 0.007(3) -0.001(2) C35 0.135(7) 0.089(5) 0.074(4) 0.017(4) 0.022(4) -0.025(5) C36 0.194(10) 0.073(5) 0.120(6) -0.033(5) 0.056(6) 0.003(6) C37 0.152(8) 0.231(11) 0.089(5) 0.028(6) 0.000(5) 0.158(9) C38 0.111(8) 0.281(16) 0.173(11) 0.072(11) -0.020(7) 0.032(9) C40 0.123(6) 0.069(4) 0.211(9) -0.011(5) 0.117(6) -0.032(4) C41 0.079(4) 0.052(3) 0.127(5) 0.005(3) 0.031(4) -0.018(3) C42 0.055(4) 0.088(5) 0.169(7) 0.015(5) 0.037(4) -0.013(4) N1 0.0315(18) 0.0317(18) 0.0400(18) -0.0015(14) 0.0054(15) -0.0029(14) O2 0.0391(17) 0.0430(17) 0.0463(16) -0.0015(13) 0.0043(13) 0.0094(13) O1 0.0366(16) 0.0402(16) 0.0468(16) -0.0019(13) 0.0002(13) 0.0048(13) O5 0.050(2) 0.049(2) 0.101(3) 0.0271(19) 0.0121(19) 0.0045(16) O4 0.0431(19) 0.061(2) 0.064(2) 0.0003(17) -0.0044(16) 0.0170(16) O3 0.0431(18) 0.0488(19) 0.068(2) 0.0073(16) 0.0163(16) -0.0066(15) Zr1 0.0297(2) 0.0364(3) 0.0436(3) 0.00128(18) 0.00250(17) 0.00435(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 C1 O2 1.354(5) . ? C1 C14 1.396(6) . ? C1 C2 1.399(6) . ? C2 C7 1.392(6) . ? C2 C3 1.543(6) . ? C3 C4 1.536(7) . ? C3 C5 1.537(7) . ? C3 C6 1.541(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.400(7) . ? C7 H7 0.9500 . ? C8 C13 1.376(6) . ? C8 C9 1.540(6) . ? C9 C10 1.504(7) . ? C9 C12 1.505(9) . ? C9 C11 1.514(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 C14 1.392(6) . ? C13 H13 0.9500 . ? C14 C15 1.497(6) . ? C15 N1 1.499(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N1 1.491(5) . ? C16 C17 1.527(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.513(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N1 1.489(5) . ? C19 C20 1.503(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.380(6) . ? C20 C33 1.393(6) . ? C21 C22 1.389(6) . ? C21 H21 0.9500 . ? C22 C27 1.386(6) . ? C22 C23 1.530(6) . ? C23 C25 1.422(14) . ? C23 C24' 1.480(18) . ? C23 C26 1.503(13) . ? C23 C25' 1.545(17) . ? C23 C24 1.579(14) . ? C23 C26' 1.597(18) . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C25' H25A 0.9800 . ? C25' H25B 0.9800 . ? C25' H25C 0.9800 . ? C26' H26A 0.9800 . ? C26' H26B 0.9800 . ? C26' H26C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25D 0.9800 . ? C25 H25E 0.9800 . ? C25 H25F 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 C28 1.398(7) . ? C27 H27 0.9500 . ? C28 C33 1.409(6) . ? C28 C29 1.544(6) . ? C29 C30 1.525(7) . ? C29 C31 1.527(7) . ? C29 C32 1.548(8) . ? 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 O1 1.346(5) . ? C34 O5 1.421(6) . ? C34 C36 1.451(9) . ? C34 C35 1.491(8) . ? C34 H34 1.0000 . ? 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 C38 1.338(12) . ? C37 C39 1.391(16) . ? C37 O4 1.424(7) . ? C37 C39' 1.48(2) . ? 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 . ? C39' H39D 0.9800 . ? C39' H39E 0.9800 . ? C39' H39F 0.9800 . ? C40 O3 1.358(7) . ? C40 C42 1.397(9) . ? C40 C41 1.471(9) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N1 Zr1 2.507(3) . ? O2 Zr1 2.030(3) . ? O1 Zr1 2.054(3) . ? O5 Zr1 2.376(3) . ? O5 H3 0.9500 . ? O4 Zr1 1.930(3) . ? O3 Zr1 1.924(3) . ? 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 O2 C1 C14 117.9(4) . . ? O2 C1 C2 121.8(4) . . ? C14 C1 C2 120.3(4) . . ? C7 C2 C1 117.0(4) . . ? C7 C2 C3 120.8(4) . . ? C1 C2 C3 122.2(4) . . ? C4 C3 C5 109.8(4) . . ? C4 C3 C6 107.9(4) . . ? C5 C3 C6 107.7(5) . . ? C4 C3 C2 109.6(4) . . ? C5 C3 C2 109.5(4) . . ? C6 C3 C2 112.3(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 C8 124.2(4) . . ? C2 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? C13 C8 C7 116.5(4) . . ? C13 C8 C9 122.5(4) . . ? C7 C8 C9 120.9(4) . . ? C10 C9 C12 107.8(5) . . ? C10 C9 C11 108.3(6) . . ? C12 C9 C11 109.7(7) . . ? C10 C9 C8 111.5(4) . . ? C12 C9 C8 111.5(5) . . ? C11 C9 C8 108.0(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 C14 121.8(4) . . ? C8 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C1 120.0(4) . . ? C13 C14 C15 120.7(4) . . ? C1 C14 C15 119.3(4) . . ? C14 C15 N1 113.7(3) . . ? C14 C15 H15A 108.8 . . ? N1 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? N1 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N1 C16 C17 117.6(4) . . ? N1 C16 H16A 107.9 . . ? C17 C16 H16A 107.9 . . ? N1 C16 H16B 107.9 . . ? C17 C16 H16B 107.9 . . ? H16A C16 H16B 107.2 . . ? C18 C17 C16 109.4(4) . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 114.1(3) . . ? N1 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? N1 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C33 120.5(4) . . ? C21 C20 C19 119.9(4) . . ? C33 C20 C19 119.6(4) . . ? C20 C21 C22 121.7(4) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C27 C22 C21 116.6(4) . . ? C27 C22 C23 122.6(4) . . ? C21 C22 C23 120.8(4) . . ? C25 C23 C24' 131.7(10) . . ? C25 C23 C26 113.3(9) . . ? C24' C23 C26 44.6(7) . . ? C25 C23 C22 112.4(7) . . ? C24' C23 C22 115.9(8) . . ? C26 C23 C22 112.4(6) . . ? C25 C23 C25' 46.1(8) . . ? C24' C23 C25' 110.7(10) . . ? C26 C23 C25' 132.6(9) . . ? C22 C23 C25' 115.0(7) . . ? C25 C23 C24 110.4(9) . . ? C24' C23 C24 58.3(8) . . ? C26 C23 C24 102.5(8) . . ? C22 C23 C24 105.2(6) . . ? C25' C23 C24 65.4(8) . . ? C25 C23 C26' 56.3(9) . . ? C24' C23 C26' 104.4(10) . . ? C26 C23 C26' 63.6(8) . . ? C22 C23 C26' 109.3(8) . . ? C25' C23 C26' 99.7(10) . . ? C24 C23 C26' 145.5(9) . . ? C23 C24' H24D 109.5 . . ? C23 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C23 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? 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 . . ? C23 C26' H26A 109.5 . . ? C23 C26' H26B 109.5 . . ? H26A C26' H26B 109.5 . . ? C23 C26' H26C 109.5 . . ? H26A C26' H26C 109.5 . . ? H26B C26' H26C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25D 109.5 . . ? C23 C25 H25E 109.5 . . ? H25D C25 H25E 109.5 . . ? C23 C25 H25F 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C23 C26 H26D 109.5 . . ? C23 C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? C23 C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C22 C27 C28 124.3(4) . . ? C22 C27 H27 117.8 . . ? C28 C27 H27 117.8 . . ? C27 C28 C33 116.8(4) . . ? C27 C28 C29 121.1(4) . . ? C33 C28 C29 122.1(4) . . ? C30 C29 C31 107.0(5) . . ? C30 C29 C28 112.1(4) . . ? C31 C29 C28 110.2(4) . . ? C30 C29 C32 108.6(5) . . ? C31 C29 C32 109.0(5) . . ? C28 C29 C32 109.9(4) . . ? 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 . . ? O1 C33 C20 117.9(4) . . ? O1 C33 C28 122.2(4) . . ? C20 C33 C28 119.9(4) . . ? O5 C34 C36 107.7(5) . . ? O5 C34 C35 110.7(5) . . ? C36 C34 C35 111.6(6) . . ? O5 C34 H34 108.9 . . ? C36 C34 H34 108.9 . . ? C35 C34 H34 108.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 129.6(10) . . ? C38 C37 O4 113.0(8) . . ? C39 C37 O4 115.6(8) . . ? C38 C37 C39' 96.7(13) . . ? C39 C37 C39' 58.4(11) . . ? O4 C37 C39' 105.3(13) . . ? C38 C37 H37 94.4 . . ? C39 C37 H37 94.4 . . ? O4 C37 H37 94.4 . . ? C39' C37 H37 151.3 . . ? 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 C39' H39D 109.5 . . ? C37 C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C37 C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? O3 C40 C42 118.3(6) . . ? O3 C40 C41 115.7(6) . . ? C42 C40 C41 121.1(6) . . ? O3 C40 H40 97.4 . . ? C42 C40 H40 97.4 . . ? C41 C40 H40 97.4 . . ? 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 . . ? C19 N1 C16 111.1(3) . . ? C19 N1 C15 106.8(3) . . ? C16 N1 C15 111.3(3) . . ? C19 N1 Zr1 109.9(2) . . ? C16 N1 Zr1 108.6(2) . . ? C15 N1 Zr1 109.1(2) . . ? C1 O2 Zr1 139.7(3) . . ? C33 O1 Zr1 134.4(2) . . ? C34 O5 Zr1 133.4(3) . . ? C34 O5 H3 113.3 . . ? Zr1 O5 H3 113.3 . . ? C37 O4 Zr1 163.3(6) . . ? C40 O3 Zr1 177.3(6) . . ? O3 Zr1 O4 102.59(15) . . ? O3 Zr1 O2 99.93(14) . . ? O4 Zr1 O2 98.07(13) . . ? O3 Zr1 O1 96.15(13) . . ? O4 Zr1 O1 99.78(13) . . ? O2 Zr1 O1 152.69(12) . . ? O3 Zr1 O5 166.46(14) . . ? O4 Zr1 O5 85.43(14) . . ? O2 Zr1 O5 89.57(13) . . ? O1 Zr1 O5 71.52(13) . . ? O3 Zr1 N1 91.12(12) . . ? O4 Zr1 N1 166.25(13) . . ? O2 Zr1 N1 78.36(11) . . ? O1 Zr1 N1 79.41(11) . . ? O5 Zr1 N1 81.29(11) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.809 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.136 data_a12523_2cMeCN _database_code_depnum_ccdc_archive 'CCDC 897195' #TrackingRef '[ONO]ZrX2 r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H68 N2 O4 Zr' _chemical_formula_sum 'C41 H68 N2 O4 Zr' _chemical_formula_weight 744.19 _chemical_absolute_configuration unk 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.2006(14) _cell_length_b 15.6501(16) _cell_length_c 19.191(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4264.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8021 _exptl_absorpt_correction_T_max 0.9061 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25025 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_unetI/netI 0.0548 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7390 _reflns_number_gt 6737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0844P)^2^+1.6065P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 7390 _refine_ls_number_parameters 428 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 C1 C 0.2864(3) 0.1305(3) 0.1415(2) 0.0344(10) Uani 1 1 d . . . C2 C 0.3166(3) 0.1980(3) 0.0987(2) 0.0383(11) Uani 1 1 d . . . C3 C 0.2680(3) 0.2210(3) 0.0300(2) 0.0411(11) Uani 1 1 d . . . C4 C 0.1620(4) 0.2437(4) 0.0422(3) 0.0525(13) Uani 1 1 d . . . H4A H 0.1327 0.2588 -0.0024 0.079 Uiso 1 1 calc R . . H4B H 0.1575 0.2922 0.0743 0.079 Uiso 1 1 calc R . . H4C H 0.1295 0.1943 0.0623 0.079 Uiso 1 1 calc R . . C5 C 0.2734(4) 0.1428(3) -0.0191(2) 0.0469(12) Uani 1 1 d . . . H5A H 0.2426 0.1564 -0.0634 0.070 Uiso 1 1 calc R . . H5B H 0.2416 0.0940 0.0026 0.070 Uiso 1 1 calc R . . H5C H 0.3396 0.1283 -0.0277 0.070 Uiso 1 1 calc R . . C6 C 0.3121(4) 0.2963(4) -0.0076(3) 0.0549(14) Uani 1 1 d . . . H6A H 0.2773 0.3077 -0.0506 0.082 Uiso 1 1 calc R . . H6B H 0.3778 0.2829 -0.0189 0.082 Uiso 1 1 calc R . . H6C H 0.3099 0.3468 0.0225 0.082 Uiso 1 1 calc R . . C7 C 0.3948(3) 0.2447(3) 0.1204(2) 0.0434(11) Uani 1 1 d . . . H7 H 0.4158 0.2904 0.0919 0.052 Uiso 1 1 calc R . . C8 C 0.4432(3) 0.2280(4) 0.1812(3) 0.0485(13) Uani 1 1 d . A . C9 C 0.5305(3) 0.2835(3) 0.2031(2) 0.0530(14) Uani 1 1 d D . . C10 C 0.5481(6) 0.3571(4) 0.1512(4) 0.0311(18) Uiso 0.50 1 d PD A 1 H10A H 0.5127 0.3464 0.1082 0.047 Uiso 0.50 1 calc PR A 1 H10B H 0.6154 0.3604 0.1405 0.047 Uiso 0.50 1 calc PR A 1 H10C H 0.5272 0.4111 0.1719 0.047 Uiso 0.50 1 calc PR A 1 C11 C 0.5134(7) 0.3246(7) 0.2748(4) 0.047(2) Uiso 0.50 1 d PD A 1 H11A H 0.4747 0.3760 0.2691 0.070 Uiso 0.50 1 calc PR A 1 H11B H 0.5739 0.3402 0.2958 0.070 Uiso 0.50 1 calc PR A 1 H11C H 0.4806 0.2839 0.3051 0.070 Uiso 0.50 1 calc PR A 1 C10' C 0.6208(10) 0.2560(15) 0.1650(11) 0.143(8) Uiso 0.50 1 d PD A 2 H10D H 0.6141 0.2674 0.1150 0.214 Uiso 0.50 1 calc PR A 2 H10E H 0.6314 0.1948 0.1723 0.214 Uiso 0.50 1 calc PR A 2 H10F H 0.6744 0.2883 0.1834 0.214 Uiso 0.50 1 calc PR A 2 C11' C 0.4975(18) 0.3686(9) 0.2351(13) 0.158(9) Uiso 0.50 1 d PD A 2 H11D H 0.4413 0.3586 0.2636 0.238 Uiso 0.50 1 calc PR A 2 H11E H 0.4824 0.4090 0.1978 0.238 Uiso 0.50 1 calc PR A 2 H11F H 0.5478 0.3922 0.2643 0.238 Uiso 0.50 1 calc PR A 2 C12' C 0.5644(17) 0.2580(17) 0.2765(6) 0.156(9) Uiso 0.50 1 d PD A 1 H12A H 0.5357 0.2034 0.2898 0.235 Uiso 0.50 1 calc PR A 1 H12B H 0.5459 0.3022 0.3100 0.235 Uiso 0.50 1 calc PR A 1 H12C H 0.6331 0.2522 0.2764 0.235 Uiso 0.50 1 calc PR A 1 C12 C 0.6172(5) 0.2246(6) 0.1996(5) 0.042(2) Uiso 0.50 1 d PD A 2 H12D H 0.6343 0.2149 0.1507 0.064 Uiso 0.50 1 calc PR A 2 H12E H 0.6024 0.1698 0.2218 0.064 Uiso 0.50 1 calc PR A 2 H12F H 0.6700 0.2516 0.2239 0.064 Uiso 0.50 1 calc PR A 2 C13 C 0.4108(3) 0.1620(3) 0.2220(3) 0.0447(12) Uani 1 1 d . . . H13A H 0.4425 0.1492 0.2644 0.054 Uiso 1 1 calc R A . C14 C 0.3330(3) 0.1136(3) 0.2031(2) 0.0362(10) Uani 1 1 d . A . C15 C 0.2974(3) 0.0430(3) 0.2495(2) 0.0398(11) Uani 1 1 d . . . H15A H 0.3364 0.0407 0.2922 0.048 Uiso 1 1 calc R A . H15B H 0.3042 -0.0123 0.2250 0.048 Uiso 1 1 calc R . . C16 C 0.1789(3) 0.1420(3) 0.2984(2) 0.0323(9) Uani 1 1 d . . . H16A H 0.1114 0.1467 0.3108 0.039 Uiso 1 1 calc R A . H16B H 0.1912 0.1839 0.2609 0.039 Uiso 1 1 calc R . . C17 C 0.2368(3) 0.1687(3) 0.3624(3) 0.0440(12) Uani 1 1 d . A . H17A H 0.2392 0.1205 0.3958 0.053 Uiso 1 1 calc R . . H17B H 0.3021 0.1816 0.3477 0.053 Uiso 1 1 calc R . . C18 C 0.1956(5) 0.2460(4) 0.3981(3) 0.0652(17) Uani 1 1 d . . . H18A H 0.2346 0.2611 0.4384 0.098 Uiso 1 1 calc R A . H18B H 0.1315 0.2330 0.4137 0.098 Uiso 1 1 calc R . . H18C H 0.1940 0.2940 0.3654 0.098 Uiso 1 1 calc R . . C19 C 0.1710(3) -0.0105(3) 0.3226(2) 0.0354(9) Uani 1 1 d . . . H19A H 0.2172 -0.0079 0.3611 0.042 Uiso 1 1 calc R A . H19B H 0.1756 -0.0677 0.3010 0.042 Uiso 1 1 calc R . . C20 C 0.0721(3) 0.0015(3) 0.3522(2) 0.0340(9) Uani 1 1 d . A . C21 C 0.0592(3) 0.0152(3) 0.4226(2) 0.0384(10) Uani 1 1 d . . . H21 H 0.1128 0.0210 0.4519 0.046 Uiso 1 1 calc R A . C22 C -0.0302(3) 0.0207(3) 0.4517(2) 0.0416(11) Uani 1 1 d . A . C23 C -0.0435(3) 0.0363(3) 0.5288(3) 0.0543(14) Uani 1 1 d D . . C24 C 0.0294(9) -0.0054(11) 0.5773(7) 0.093(5) Uiso 0.50 1 d PD A 1 H24A H 0.0146 0.0088 0.6258 0.139 Uiso 0.50 1 calc PR A 1 H24B H 0.0924 0.0158 0.5657 0.139 Uiso 0.50 1 calc PR A 1 H24C H 0.0277 -0.0676 0.5712 0.139 Uiso 0.50 1 calc PR A 1 C25 C -0.0359(12) 0.1337(4) 0.5394(9) 0.099(5) Uiso 0.50 1 d PD A 1 H25A H -0.0811 0.1627 0.5089 0.148 Uiso 0.50 1 calc PR A 1 H25B H 0.0280 0.1526 0.5279 0.148 Uiso 0.50 1 calc PR A 1 H25C H -0.0498 0.1478 0.5880 0.148 Uiso 0.50 1 calc PR A 1 C26 C -0.1472(5) 0.0323(13) 0.5519(10) 0.115(6) Uiso 0.50 1 d PD A 1 H26A H -0.1864 0.0632 0.5182 0.173 Uiso 0.50 1 calc PR A 1 H26B H -0.1538 0.0585 0.5980 0.173 Uiso 0.50 1 calc PR A 1 H26C H -0.1675 -0.0275 0.5541 0.173 Uiso 0.50 1 calc PR A 1 C24' C 0.0502(5) 0.0433(8) 0.5689(5) 0.049(3) Uiso 0.50 1 d PD A 2 H24D H 0.0886 -0.0075 0.5596 0.073 Uiso 0.50 1 calc PR A 2 H24E H 0.0374 0.0474 0.6189 0.073 Uiso 0.50 1 calc PR A 2 H24F H 0.0842 0.0944 0.5535 0.073 Uiso 0.50 1 calc PR A 2 C25' C -0.1066(7) 0.1142(5) 0.5433(6) 0.052(2) Uiso 0.50 1 d PD A 2 H25D H -0.1134 0.1219 0.5938 0.079 Uiso 0.50 1 calc PR A 2 H25E H -0.1688 0.1049 0.5225 0.079 Uiso 0.50 1 calc PR A 2 H25F H -0.0779 0.1654 0.5230 0.079 Uiso 0.50 1 calc PR A 2 C26' C -0.0914(8) -0.0435(5) 0.5596(6) 0.061(3) Uiso 0.50 1 d PD A 2 H26D H -0.0524 -0.0939 0.5504 0.092 Uiso 0.50 1 calc PR A 2 H26E H -0.1534 -0.0511 0.5380 0.092 Uiso 0.50 1 calc PR A 2 H26F H -0.0991 -0.0362 0.6100 0.092 Uiso 0.50 1 calc PR A 2 C27 C -0.1059(3) 0.0129(3) 0.4064(2) 0.0391(10) Uani 1 1 d . . . H27 H -0.1673 0.0160 0.4258 0.047 Uiso 1 1 calc R A . C28 C -0.0987(3) 0.0011(3) 0.3352(2) 0.0367(9) Uani 1 1 d . A . C29 C -0.1858(3) -0.0084(4) 0.2888(2) 0.0456(12) Uani 1 1 d . . . C30 C -0.2789(3) 0.0015(5) 0.3296(3) 0.0637(16) Uani 1 1 d . A . H30A H -0.3322 -0.0044 0.2975 0.096 Uiso 1 1 calc R . . H30B H -0.2808 0.0580 0.3516 0.096 Uiso 1 1 calc R . . H30C H -0.2827 -0.0428 0.3655 0.096 Uiso 1 1 calc R . . C31 C -0.1861(4) -0.0977(4) 0.2555(3) 0.0640(16) Uani 1 1 d . A . H31A H -0.2415 -0.1037 0.2255 0.096 Uiso 1 1 calc R . . H31B H -0.1879 -0.1412 0.2922 0.096 Uiso 1 1 calc R . . H31C H -0.1289 -0.1051 0.2276 0.096 Uiso 1 1 calc R . . C32 C -0.1858(4) 0.0609(4) 0.2307(3) 0.0604(16) Uani 1 1 d . A . H32A H -0.2421 0.0542 0.2016 0.091 Uiso 1 1 calc R . . H32B H -0.1294 0.0544 0.2018 0.091 Uiso 1 1 calc R . . H32C H -0.1860 0.1178 0.2521 0.091 Uiso 1 1 calc R . . C33 C -0.0057(3) -0.0044(3) 0.3079(2) 0.0335(9) Uani 1 1 d . . . C34 C -0.0138(4) -0.0010(4) 0.0187(3) 0.0563(14) Uani 1 1 d . . . H34 H -0.0224 0.0597 0.0037 0.068 Uiso 1 1 calc R . . C35 C -0.1090(5) -0.0406(7) 0.0249(4) 0.115(3) Uani 1 1 d . . . H35A H -0.1463 -0.0089 0.0592 0.173 Uiso 1 1 calc R . . H35B H -0.1024 -0.1001 0.0401 0.173 Uiso 1 1 calc R . . H35C H -0.1407 -0.0388 -0.0204 0.173 Uiso 1 1 calc R . . C36 C 0.0474(7) -0.0448(6) -0.0348(3) 0.105(3) Uani 1 1 d . . . H36A H 0.1089 -0.0165 -0.0368 0.158 Uiso 1 1 calc R . . H36B H 0.0170 -0.0415 -0.0806 0.158 Uiso 1 1 calc R . . H36C H 0.0559 -0.1049 -0.0218 0.158 Uiso 1 1 calc R . . C37 C 0.1749(4) -0.1899(4) 0.1523(3) 0.0549(14) Uani 1 1 d . . . H37 H 0.1999 -0.2185 0.1951 0.066 Uiso 1 1 calc R . . C38 C 0.0789(5) -0.2278(4) 0.1371(4) 0.0704(18) Uani 1 1 d . . . H38A H 0.0369 -0.2172 0.1767 0.106 Uiso 1 1 calc R . . H38B H 0.0851 -0.2895 0.1297 0.106 Uiso 1 1 calc R . . H38C H 0.0527 -0.2011 0.0952 0.106 Uiso 1 1 calc R . . C39 C 0.2399(6) -0.2081(6) 0.0951(5) 0.111(3) Uani 1 1 d . . . H39A H 0.3017 -0.1835 0.1057 0.166 Uiso 1 1 calc R . . H39B H 0.2156 -0.1831 0.0520 0.166 Uiso 1 1 calc R . . H39C H 0.2461 -0.2701 0.0895 0.166 Uiso 1 1 calc R . . C40 C -0.0051(3) 0.2115(3) 0.1736(2) 0.0413(11) Uani 1 1 d . . . C41 C -0.0526(5) 0.2925(3) 0.1673(3) 0.0644(16) Uani 1 1 d . . . H41A H -0.0321 0.3211 0.1245 0.097 Uiso 1 1 calc R . . H41B H -0.0371 0.3283 0.2076 0.097 Uiso 1 1 calc R . . H41C H -0.1208 0.2831 0.1657 0.097 Uiso 1 1 calc R . . N1 N 0.1950(2) 0.0558(2) 0.26971(19) 0.0318(8) Uani 1 1 d . A . N2 N 0.0332(3) 0.1473(2) 0.1777(2) 0.0362(9) Uani 1 1 d . A . O1 O 0.2119(2) 0.08234(19) 0.12380(15) 0.0346(7) Uani 1 1 d . A . O2 O 0.01046(19) -0.0188(2) 0.23991(14) 0.0355(7) Uani 1 1 d . A . O4 O 0.0313(2) -0.0006(2) 0.08290(14) 0.0415(7) Uani 1 1 d . A . O3 O 0.1687(2) -0.10208(18) 0.16641(18) 0.0421(7) Uani 1 1 d . A . Zr1 Zr 0.10778(3) 0.00907(2) 0.16494(2) 0.02971(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(2) 0.036(2) 0.039(2) -0.0088(19) 0.0044(19) -0.0043(19) C2 0.037(2) 0.042(3) 0.037(2) -0.011(2) 0.007(2) -0.003(2) C3 0.043(3) 0.042(3) 0.038(3) -0.004(2) 0.009(2) -0.004(2) C4 0.056(3) 0.054(3) 0.047(3) 0.001(3) 0.007(2) 0.012(3) C5 0.054(3) 0.052(3) 0.035(3) -0.010(2) 0.007(2) -0.005(3) C6 0.069(4) 0.047(3) 0.049(3) 0.004(2) 0.004(3) -0.013(3) C7 0.038(2) 0.047(3) 0.045(3) -0.009(2) 0.008(2) -0.017(3) C8 0.034(2) 0.055(3) 0.056(3) -0.021(3) 0.009(2) -0.015(2) C9 0.037(3) 0.062(4) 0.060(3) -0.024(3) -0.001(2) -0.013(3) C13 0.031(2) 0.066(3) 0.037(3) -0.014(2) -0.003(2) -0.002(2) C14 0.029(2) 0.039(3) 0.041(3) -0.011(2) 0.0009(19) -0.001(2) C15 0.032(2) 0.047(3) 0.040(2) -0.006(2) -0.0092(19) 0.006(2) C16 0.030(2) 0.031(2) 0.036(2) -0.0028(19) -0.0042(18) -0.0023(19) C17 0.041(3) 0.048(3) 0.043(3) -0.008(2) -0.008(2) 0.000(2) C18 0.104(5) 0.044(3) 0.047(3) -0.012(3) -0.023(3) -0.001(3) C19 0.032(2) 0.035(2) 0.039(2) 0.008(2) -0.0064(17) -0.0051(19) C20 0.036(2) 0.030(2) 0.036(2) 0.0024(19) -0.0012(17) -0.0015(19) C21 0.041(2) 0.033(2) 0.041(2) 0.004(2) -0.0024(19) -0.001(2) C22 0.053(3) 0.035(3) 0.037(2) 0.002(2) -0.002(2) -0.005(2) C23 0.054(3) 0.069(4) 0.039(3) -0.006(3) 0.006(2) -0.003(3) C27 0.042(2) 0.032(2) 0.043(2) -0.0004(19) 0.009(2) 0.001(2) C28 0.037(2) 0.032(2) 0.040(2) 0.002(2) -0.0017(18) -0.004(2) C29 0.033(2) 0.057(3) 0.047(3) -0.015(3) 0.0009(19) 0.000(2) C30 0.033(2) 0.102(5) 0.056(3) -0.023(4) 0.007(2) -0.011(3) C31 0.053(3) 0.071(4) 0.068(4) -0.030(3) -0.005(3) -0.018(3) C32 0.038(3) 0.090(5) 0.054(3) 0.009(3) -0.007(3) 0.003(3) C33 0.037(2) 0.027(2) 0.037(2) -0.004(2) 0.0001(17) 0.000(2) C34 0.070(3) 0.054(3) 0.044(3) 0.006(3) -0.019(2) 0.000(3) C35 0.080(5) 0.183(10) 0.082(5) 0.022(5) -0.044(4) -0.054(6) C36 0.147(8) 0.127(7) 0.043(4) -0.020(4) 0.002(4) 0.026(6) C37 0.062(3) 0.050(3) 0.052(3) -0.007(3) -0.010(3) 0.013(3) C38 0.086(5) 0.046(3) 0.079(4) -0.004(3) -0.017(3) -0.017(3) C39 0.104(7) 0.115(7) 0.113(7) -0.047(5) 0.021(6) 0.032(5) C40 0.044(3) 0.045(3) 0.035(3) -0.005(2) -0.005(2) 0.000(2) C41 0.090(4) 0.037(3) 0.066(4) -0.012(3) -0.015(4) 0.028(3) N1 0.0284(18) 0.0295(19) 0.037(2) -0.0004(16) -0.0045(16) 0.0050(15) N2 0.038(2) 0.0260(19) 0.045(2) -0.0046(16) -0.0019(17) 0.0088(16) O1 0.0353(15) 0.0305(16) 0.0379(17) -0.0053(13) 0.0003(13) -0.0050(14) O2 0.0320(14) 0.0423(19) 0.0321(15) -0.0035(14) 0.0015(12) -0.0043(14) O4 0.0419(16) 0.050(2) 0.0330(15) -0.0067(16) -0.0089(13) 0.0023(18) O3 0.0486(17) 0.0251(14) 0.0526(19) -0.0114(16) 0.0001(17) 0.0047(13) Zr1 0.0302(2) 0.0271(2) 0.0319(2) -0.00534(16) -0.00185(16) -0.00142(16) _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 C1 O1 1.342(5) . ? C1 C14 1.381(6) . ? C1 C2 1.405(7) . ? C2 C7 1.393(6) . ? C2 C3 1.531(7) . ? C3 C6 1.517(7) . ? C3 C5 1.547(7) . ? C3 C4 1.564(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.380(7) . ? C7 H7 0.9500 . ? C8 C13 1.375(7) . ? C8 C9 1.570(6) . ? C9 C10' 1.538(2) . ? C9 C11 1.538(2) . ? C9 C11' 1.539(2) . ? C9 C12 1.540(2) . ? C9 C10 1.543(2) . ? C9 C12' 1.541(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C12' H12A 0.9800 . ? C12' H12B 0.9800 . ? C12' H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C13 C14 1.388(6) . ? C13 H13A 0.9500 . ? C14 C15 1.506(7) . ? C15 N1 1.519(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N1 1.476(5) . ? C16 C17 1.535(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.508(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N1 1.491(5) . ? C19 C20 1.526(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.381(6) . ? C20 C33 1.397(6) . ? C21 C22 1.390(7) . ? C21 H21 0.9500 . ? C22 C27 1.387(7) . ? C22 C23 1.511(7) . ? C23 C24 1.537(2) . ? C23 C25' 1.538(2) . ? C23 C26 1.539(2) . ? C23 C26' 1.541(2) . ? C23 C24' 1.541(2) . ? C23 C25 1.541(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? C26' H26D 0.9800 . ? C26' H26E 0.9800 . ? C26' H26F 0.9800 . ? C27 C28 1.383(6) . ? C27 H27 0.9500 . ? C28 C33 1.423(6) . ? C28 C29 1.532(6) . ? C29 C31 1.537(8) . ? C29 C30 1.543(6) . ? C29 C32 1.555(8) . ? 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 O2 1.344(5) . ? C34 O4 1.388(5) . ? C34 C35 1.492(9) . ? C34 C36 1.510(9) . ? C34 H34 1.0000 . ? 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 O3 1.403(6) . ? C37 C39 1.463(9) . ? C37 C38 1.514(8) . ? 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 . ? C40 N2 1.145(6) . ? C40 C41 1.440(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N1 Zr1 2.472(3) . ? N2 Zr1 2.422(4) . ? O1 Zr1 2.031(3) . ? O2 Zr1 2.042(3) . ? O4 Zr1 1.919(3) . ? O3 Zr1 1.943(3) . ? 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 C1 C14 119.1(4) . . ? O1 C1 C2 121.0(4) . . ? C14 C1 C2 119.9(4) . . ? C7 C2 C1 117.5(4) . . ? C7 C2 C3 119.6(4) . . ? C1 C2 C3 122.8(4) . . ? C6 C3 C2 113.9(4) . . ? C6 C3 C5 107.8(4) . . ? C2 C3 C5 108.4(4) . . ? C6 C3 C4 107.0(4) . . ? C2 C3 C4 111.0(4) . . ? C5 C3 C4 108.6(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C2 123.5(5) . . ? C8 C7 H7 118.3 . . ? C2 C7 H7 118.3 . . ? C7 C8 C13 117.2(4) . . ? C7 C8 C9 121.0(5) . . ? C13 C8 C9 121.9(5) . . ? C10' C9 C11 132.4(10) . . ? C10' C9 C11' 133.3(14) . . ? C11 C9 C11' 39.9(10) . . ? C10' C9 C12 31.2(9) . . ? C11 C9 C12 114.6(6) . . ? C11' C9 C12 141.1(11) . . ? C10' C9 C8 112.1(9) . . ? C11 C9 C8 110.2(5) . . ? C11' C9 C8 110.2(11) . . ? C12 C9 C8 106.8(5) . . ? C10' C9 C10 76.5(10) . . ? C11 C9 C10 106.9(6) . . ? C11' C9 C10 70.2(11) . . ? C12 C9 C10 106.8(6) . . ? C8 C9 C10 111.6(5) . . ? C10' C9 C12' 95.8(13) . . ? C11 C9 C12' 48.7(10) . . ? C11' C9 C12' 87.3(14) . . ? C12 C9 C12' 68.6(11) . . ? C8 C9 C12' 110.3(10) . . ? C10 C9 C12' 137.1(11) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C10' H10D 109.5 . . ? C9 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C9 C11' H11D 109.5 . . ? C9 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C9 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C9 C12' H12A 109.5 . . ? C9 C12' H12B 109.5 . . ? H12A C12' H12B 109.5 . . ? C9 C12' H12C 109.5 . . ? H12A C12' H12C 109.5 . . ? H12B C12' H12C 109.5 . . ? C9 C12 H12D 109.5 . . ? C9 C12 H12E 109.5 . . ? H12D C12 H12E 109.5 . . ? C9 C12 H12F 109.5 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C8 C13 C14 121.8(5) . . ? C8 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? C1 C14 C13 120.1(5) . . ? C1 C14 C15 119.1(4) . . ? C13 C14 C15 120.8(4) . . ? C14 C15 N1 112.1(4) . . ? C14 C15 H15A 109.2 . . ? N1 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? N1 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N1 C16 C17 117.7(4) . . ? N1 C16 H16A 107.9 . . ? C17 C16 H16A 107.9 . . ? N1 C16 H16B 107.9 . . ? C17 C16 H16B 107.9 . . ? H16A C16 H16B 107.2 . . ? C18 C17 C16 112.0(4) . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 112.2(3) . . ? N1 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N1 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C33 120.1(4) . . ? C21 C20 C19 120.3(4) . . ? C33 C20 C19 119.6(4) . . ? C20 C21 C22 121.6(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C27 C22 C21 116.7(4) . . ? C27 C22 C23 122.1(4) . . ? C21 C22 C23 121.2(4) . . ? C24 C23 C25' 128.3(9) . . ? C24 C23 C26 116.9(10) . . ? C25' C23 C26 54.8(8) . . ? C24 C23 C22 116.1(7) . . ? C25' C23 C22 112.2(5) . . ? C26 C23 C22 113.2(8) . . ? C24 C23 C26' 73.8(8) . . ? C25' C23 C26' 108.4(7) . . ? C26 C23 C26' 55.5(9) . . ? C22 C23 C26' 107.4(6) . . ? C24 C23 C24' 31.4(7) . . ? C25' C23 C24' 110.9(7) . . ? C26 C23 C24' 133.3(9) . . ? C22 C23 C24' 113.1(5) . . ? C26' C23 C24' 104.4(7) . . ? C24 C23 C25 107.1(10) . . ? C25' C23 C25 40.0(7) . . ? C26 C23 C25 94.0(10) . . ? C22 C23 C25 106.3(8) . . ? C26' C23 C25 141.5(9) . . ? C24' C23 C25 78.7(8) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C24' H24D 109.5 . . ? C23 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C23 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C23 C25' H25D 109.5 . . ? C23 C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C23 C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C23 C26' H26D 109.5 . . ? C23 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C23 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C28 C27 C22 125.0(4) . . ? C28 C27 H27 117.5 . . ? C22 C27 H27 117.5 . . ? C27 C28 C33 116.2(4) . . ? C27 C28 C29 121.9(4) . . ? C33 C28 C29 121.9(4) . . ? C28 C29 C31 109.4(4) . . ? C28 C29 C30 112.8(4) . . ? C31 C29 C30 107.4(5) . . ? C28 C29 C32 110.5(4) . . ? C31 C29 C32 109.6(5) . . ? C30 C29 C32 107.1(5) . . ? 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 . . ? O2 C33 C20 117.8(4) . . ? O2 C33 C28 121.8(4) . . ? C20 C33 C28 120.3(4) . . ? O4 C34 C35 110.4(5) . . ? O4 C34 C36 109.9(5) . . ? C35 C34 C36 112.8(7) . . ? O4 C34 H34 107.9 . . ? C35 C34 H34 107.9 . . ? C36 C34 H34 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O3 C37 C39 112.1(6) . . ? O3 C37 C38 111.4(5) . . ? C39 C37 C38 110.3(5) . . ? O3 C37 H37 107.6 . . ? C39 C37 H37 107.6 . . ? C38 C37 H37 107.6 . . ? 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 . . ? N2 C40 C41 179.0(6) . . ? 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 . . ? C16 N1 C19 110.3(3) . . ? C16 N1 C15 111.3(3) . . ? C19 N1 C15 107.6(3) . . ? C16 N1 Zr1 119.8(2) . . ? C19 N1 Zr1 103.5(2) . . ? C15 N1 Zr1 103.5(2) . . ? C40 N2 Zr1 169.9(4) . . ? C1 O1 Zr1 142.4(3) . . ? C33 O2 Zr1 139.8(3) . . ? C34 O4 Zr1 171.7(3) . . ? C37 O3 Zr1 154.4(3) . . ? O4 Zr1 O3 101.15(14) . . ? O4 Zr1 O1 97.92(13) . . ? O3 Zr1 O1 100.80(13) . . ? O4 Zr1 O2 100.25(12) . . ? O3 Zr1 O2 95.71(14) . . ? O1 Zr1 O2 152.53(12) . . ? O4 Zr1 N2 84.58(13) . . ? O3 Zr1 N2 173.36(14) . . ? O1 Zr1 N2 81.54(12) . . ? O2 Zr1 N2 79.86(13) . . ? O4 Zr1 N1 166.98(13) . . ? O3 Zr1 N1 91.72(12) . . ? O1 Zr1 N1 77.56(12) . . ? O2 Zr1 N1 80.16(11) . . ? N2 Zr1 N1 82.68(12) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.577 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.112 data_a12511_3cMeCN _database_code_depnum_ccdc_archive 'CCDC 897196' #TrackingRef '[ONO]ZrX2 r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H68 Hf N2 O4' _chemical_formula_sum 'C41 H68 Hf N2 O4' _chemical_formula_weight 831.46 _chemical_absolute_configuration unk 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' Hf Hf -0.5830 6.1852 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.3071(6) _cell_length_b 15.6544(5) _cell_length_c 19.1151(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4281.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 2.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3328 _exptl_absorpt_correction_T_max 0.6374 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23245 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7475 _reflns_number_gt 7034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(8) _refine_ls_number_reflns 7475 _refine_ls_number_parameters 428 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 C1 C 1.0084(3) 0.4967(3) 0.3090(2) 0.0305(9) Uani 1 1 d . . . C2 C 1.1009(3) 0.5029(2) 0.3360(2) 0.0344(9) Uani 1 1 d . . . C3 C 1.1859(3) 0.4945(3) 0.2877(2) 0.0417(10) Uani 1 1 d . . . C4 C 1.1838(4) 0.5645(3) 0.2301(3) 0.0562(14) Uani 1 1 d . . . H4A H 1.2388 0.5584 0.1999 0.084 Uiso 1 1 calc R . . H4B H 1.1845 0.6211 0.2520 0.084 Uiso 1 1 calc R . . H4C H 1.1269 0.5582 0.2020 0.084 Uiso 1 1 calc R . . C5 C 1.1867(4) 0.4058(3) 0.2533(3) 0.0569(14) Uani 1 1 d . . . H5A H 1.1887 0.3617 0.2896 0.085 Uiso 1 1 calc R . . H5B H 1.2419 0.4006 0.2232 0.085 Uiso 1 1 calc R . . H5C H 1.1301 0.3987 0.2250 0.085 Uiso 1 1 calc R . . C6 C 1.2793(3) 0.5051(4) 0.3274(3) 0.0610(14) Uani 1 1 d . . . H6A H 1.2834 0.4620 0.3645 0.092 Uiso 1 1 calc R . . H6B H 1.2822 0.5623 0.3481 0.092 Uiso 1 1 calc R . . H6C H 1.3315 0.4976 0.2948 0.092 Uiso 1 1 calc R . . C7 C 1.1096(3) 0.5143(2) 0.4075(2) 0.0398(10) Uani 1 1 d . . . H7 H 1.1711 0.5177 0.4260 0.048 Uiso 1 1 calc R . . C8 C 1.0354(3) 0.5212(3) 0.4546(2) 0.0393(10) Uani 1 1 d . A . C9 C 1.0500(3) 0.5358(3) 0.5323(3) 0.0523(13) Uani 1 1 d D . . C10 C 1.0970(8) 0.4558(5) 0.5635(6) 0.064(3) Uiso 0.50 1 d PD A 1 H10A H 1.0582 0.4056 0.5541 0.097 Uiso 0.50 1 calc PR A 1 H10B H 1.1041 0.4631 0.6142 0.097 Uiso 0.50 1 calc PR A 1 H10C H 1.1587 0.4480 0.5422 0.097 Uiso 0.50 1 calc PR A 1 C11 C 1.1133(7) 0.6132(5) 0.5467(5) 0.052(2) Uiso 0.50 1 d PD A 1 H11A H 1.1207 0.6207 0.5973 0.078 Uiso 0.50 1 calc PR A 1 H11B H 1.0849 0.6647 0.5266 0.078 Uiso 0.50 1 calc PR A 1 H11C H 1.1747 0.6037 0.5253 0.078 Uiso 0.50 1 calc PR A 1 C12 C 0.9581(5) 0.5424(7) 0.5738(5) 0.056(3) Uiso 0.50 1 d PD A 1 H12A H 0.9196 0.4919 0.5646 0.083 Uiso 0.50 1 calc PR A 1 H12B H 0.9242 0.5939 0.5594 0.083 Uiso 0.50 1 calc PR A 1 H12C H 0.9721 0.5458 0.6239 0.083 Uiso 0.50 1 calc PR A 1 C10' C 1.1527(5) 0.5257(11) 0.5548(9) 0.120(6) Uiso 0.50 1 d PD A 2 H10D H 1.1932 0.5553 0.5213 0.181 Uiso 0.50 1 calc PR A 2 H10E H 1.1690 0.4650 0.5560 0.181 Uiso 0.50 1 calc PR A 2 H10F H 1.1612 0.5506 0.6014 0.181 Uiso 0.50 1 calc PR A 2 C11' C 1.0378(11) 0.6323(4) 0.5450(8) 0.088(4) Uiso 0.50 1 d PD A 2 H11D H 1.0829 0.6640 0.5165 0.132 Uiso 0.50 1 calc PR A 2 H11E H 1.0485 0.6450 0.5946 0.132 Uiso 0.50 1 calc PR A 2 H11F H 0.9742 0.6495 0.5321 0.132 Uiso 0.50 1 calc PR A 2 C12' C 0.9786(8) 0.4916(9) 0.5803(6) 0.088(4) Uiso 0.50 1 d PD A 2 H12D H 0.9156 0.4996 0.5613 0.132 Uiso 0.50 1 calc PR A 2 H12E H 0.9821 0.5166 0.6272 0.132 Uiso 0.50 1 calc PR A 2 H12F H 0.9927 0.4304 0.5829 0.132 Uiso 0.50 1 calc PR A 2 C13 C 0.9459(3) 0.5153(2) 0.4258(2) 0.0355(10) Uani 1 1 d . . . H13 H 0.8930 0.5208 0.4555 0.043 Uiso 1 1 calc R A . C14 C 0.9323(3) 0.5016(3) 0.3546(2) 0.0326(10) Uani 1 1 d . A . C15 C 0.8341(3) 0.4901(2) 0.3264(2) 0.0323(9) Uani 1 1 d . . . H15A H 0.8287 0.4325 0.3054 0.039 Uiso 1 1 calc R A . H15B H 0.7893 0.4934 0.3657 0.039 Uiso 1 1 calc R . . C16 C 0.8245(3) 0.6431(2) 0.3010(2) 0.0296(9) Uani 1 1 d . . . H16A H 0.8099 0.6848 0.2636 0.035 Uiso 1 1 calc R A . H16B H 0.8918 0.6489 0.3121 0.035 Uiso 1 1 calc R . . C17 C 0.7687(4) 0.6675(3) 0.3659(2) 0.0416(12) Uani 1 1 d . A . H17A H 0.7027 0.6774 0.3528 0.050 Uiso 1 1 calc R . . H17B H 0.7706 0.6200 0.4000 0.050 Uiso 1 1 calc R . . C18 C 0.8080(5) 0.7474(3) 0.3993(3) 0.0679(18) Uani 1 1 d . . . H18A H 0.7707 0.7621 0.4406 0.102 Uiso 1 1 calc R A . H18B H 0.8056 0.7945 0.3656 0.102 Uiso 1 1 calc R . . H18C H 0.8729 0.7372 0.4133 0.102 Uiso 1 1 calc R . . C19 C 0.7073(3) 0.5414(3) 0.2544(2) 0.0380(11) Uani 1 1 d . . . H19A H 0.6700 0.5390 0.2980 0.046 Uiso 1 1 calc R A . H19B H 0.7007 0.4858 0.2303 0.046 Uiso 1 1 calc R . . C20 C 0.6689(3) 0.6117(3) 0.2077(2) 0.0346(10) Uani 1 1 d . A . C21 C 0.5901(3) 0.6578(3) 0.2281(3) 0.0412(11) Uani 1 1 d . . . H21 H 0.5591 0.6432 0.2704 0.049 Uiso 1 1 calc R A . C22 C 0.5567(3) 0.7238(3) 0.1884(3) 0.0464(13) Uani 1 1 d . A . C23 C 0.4715(3) 0.7768(3) 0.2115(3) 0.0578(15) Uani 1 1 d D . . C24 C 0.4338(8) 0.7470(7) 0.2831(4) 0.059(3) Uiso 0.50 1 d PD A 1 H24A H 0.4844 0.7482 0.3176 0.089 Uiso 0.50 1 calc PR A 1 H24B H 0.4096 0.6887 0.2789 0.089 Uiso 0.50 1 calc PR A 1 H24C H 0.3835 0.7853 0.2982 0.089 Uiso 0.50 1 calc PR A 1 C25 C 0.5041(7) 0.8681(4) 0.2288(6) 0.048(2) Uiso 0.50 1 d PD A 1 H25A H 0.5555 0.8658 0.2626 0.072 Uiso 0.50 1 calc PR A 1 H25B H 0.4519 0.9006 0.2487 0.072 Uiso 0.50 1 calc PR A 1 H25C H 0.5257 0.8962 0.1859 0.072 Uiso 0.50 1 calc PR A 1 C26 C 0.3904(7) 0.7732(7) 0.1588(5) 0.071(3) Uiso 0.50 1 d PD A 1 H26A H 0.3382 0.8078 0.1762 0.106 Uiso 0.50 1 calc PR A 1 H26B H 0.3699 0.7139 0.1532 0.106 Uiso 0.50 1 calc PR A 1 H26C H 0.4114 0.7956 0.1136 0.106 Uiso 0.50 1 calc PR A 1 C24' C 0.4905(12) 0.8232(10) 0.2809(5) 0.111(6) Uiso 0.50 1 d PD A 2 H24D H 0.4353 0.8563 0.2943 0.167 Uiso 0.50 1 calc PR A 2 H24E H 0.5440 0.8616 0.2753 0.167 Uiso 0.50 1 calc PR A 2 H24F H 0.5044 0.7811 0.3175 0.167 Uiso 0.50 1 calc PR A 2 C25' C 0.4514(11) 0.8497(7) 0.1594(7) 0.102(5) Uiso 0.50 1 d PD A 2 H25D H 0.4386 0.8256 0.1131 0.153 Uiso 0.50 1 calc PR A 2 H25E H 0.5059 0.8875 0.1567 0.153 Uiso 0.50 1 calc PR A 2 H25F H 0.3970 0.8824 0.1754 0.153 Uiso 0.50 1 calc PR A 2 C26' C 0.3822(6) 0.7251(7) 0.1964(7) 0.076(3) Uiso 0.50 1 d PD A 2 H26D H 0.3854 0.7014 0.1490 0.114 Uiso 0.50 1 calc PR A 2 H26E H 0.3276 0.7626 0.2002 0.114 Uiso 0.50 1 calc PR A 2 H26F H 0.3767 0.6785 0.2303 0.114 Uiso 0.50 1 calc PR A 2 C27 C 0.6027(4) 0.7413(3) 0.1265(3) 0.0464(12) Uani 1 1 d . . . H27 H 0.5797 0.7867 0.0984 0.056 Uiso 1 1 calc R A . C28 C 0.6809(3) 0.6966(3) 0.1026(2) 0.0380(11) Uani 1 1 d . A . C29 C 0.7285(3) 0.7199(3) 0.0330(3) 0.0411(12) Uani 1 1 d . . . C30 C 0.6814(4) 0.7951(3) -0.0040(3) 0.0618(15) Uani 1 1 d . A . H30A H 0.7143 0.8072 -0.0479 0.093 Uiso 1 1 calc R . . H30B H 0.6835 0.8456 0.0262 0.093 Uiso 1 1 calc R . . H30C H 0.6161 0.7806 -0.0142 0.093 Uiso 1 1 calc R . . C31 C 0.7241(4) 0.6427(3) -0.0172(2) 0.0474(13) Uani 1 1 d . A . H31A H 0.7537 0.6579 -0.0618 0.071 Uiso 1 1 calc R . . H31B H 0.6586 0.6272 -0.0255 0.071 Uiso 1 1 calc R . . H31C H 0.7570 0.5942 0.0037 0.071 Uiso 1 1 calc R . . C32 C 0.8312(4) 0.7450(3) 0.0455(3) 0.0501(13) Uani 1 1 d . A . H32A H 0.8603 0.7604 0.0008 0.075 Uiso 1 1 calc R . . H32B H 0.8648 0.6967 0.0662 0.075 Uiso 1 1 calc R . . H32C H 0.8339 0.7940 0.0773 0.075 Uiso 1 1 calc R . . C33 C 0.7144(3) 0.6294(3) 0.1454(2) 0.0365(11) Uani 1 1 d . . . C34 C 1.0124(4) 0.5047(4) 0.0198(3) 0.0568(14) Uani 1 1 d . . . H34 H 1.0231 0.5661 0.0078 0.068 Uiso 1 1 calc R . . C35 C 1.1052(5) 0.4627(6) 0.0266(4) 0.106(3) Uani 1 1 d . . . H35A H 1.1396 0.4886 0.0655 0.159 Uiso 1 1 calc R . . H35B H 1.1406 0.4703 -0.0168 0.159 Uiso 1 1 calc R . . H35C H 1.0965 0.4016 0.0357 0.159 Uiso 1 1 calc R . . C36 C 0.9526(6) 0.4661(6) -0.0369(3) 0.122(3) Uani 1 1 d . . . H36A H 0.8924 0.4960 -0.0387 0.183 Uiso 1 1 calc R . . H36B H 0.9421 0.4055 -0.0268 0.183 Uiso 1 1 calc R . . H36C H 0.9844 0.4718 -0.0821 0.183 Uiso 1 1 calc R . . C37 C 0.8235(4) 0.3141(3) 0.1506(3) 0.0524(14) Uani 1 1 d . . . H37 H 0.7964 0.2827 0.1914 0.063 Uiso 1 1 calc R . . C38 C 0.7579(6) 0.3048(6) 0.0911(4) 0.121(3) Uani 1 1 d . . . H38A H 0.6978 0.3308 0.1032 0.182 Uiso 1 1 calc R . . H38B H 0.7487 0.2440 0.0809 0.182 Uiso 1 1 calc R . . H38C H 0.7838 0.3333 0.0498 0.182 Uiso 1 1 calc R . . C39 C 0.9183(5) 0.2752(4) 0.1347(4) 0.087(2) Uani 1 1 d . . . H39A H 0.9590 0.2810 0.1757 0.131 Uiso 1 1 calc R . . H39B H 0.9466 0.3050 0.0949 0.131 Uiso 1 1 calc R . . H39C H 0.9107 0.2146 0.1233 0.131 Uiso 1 1 calc R . . C40 C 1.0022(3) 0.7118(3) 0.1746(3) 0.0366(10) Uani 1 1 d . . . C41 C 1.0499(4) 0.7933(3) 0.1683(3) 0.0670(16) Uani 1 1 d . . . H41A H 1.1146 0.7837 0.1534 0.100 Uiso 1 1 calc R . . H41B H 1.0496 0.8224 0.2137 0.100 Uiso 1 1 calc R . . H41C H 1.0177 0.8288 0.1336 0.100 Uiso 1 1 calc R . . O1 O 0.9913(2) 0.48395(18) 0.24075(15) 0.0348(7) Uani 1 1 d . A . O2 O 0.7883(2) 0.58143(16) 0.12598(15) 0.0335(7) Uani 1 1 d . A . O4 O 0.9662(2) 0.50139(18) 0.08425(14) 0.0396(7) Uani 1 1 d . A . O3 O 0.8334(2) 0.39873(15) 0.16971(18) 0.0429(7) Uani 1 1 d . A . Hf1 Hf 0.892846(12) 0.510776(9) 0.167339(9) 0.02922(6) Uani 1 1 d . . . N1 N 0.8082(2) 0.55526(19) 0.27287(17) 0.0291(8) Uani 1 1 d . A . N2 N 0.9650(3) 0.6486(2) 0.17853(19) 0.0352(9) Uani 1 1 d . A . 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 C1 0.034(2) 0.0277(19) 0.030(2) -0.0045(16) 0.0019(18) -0.0016(19) C2 0.035(2) 0.0310(16) 0.037(2) -0.0027(17) 0.007(2) 0.0038(17) C3 0.031(3) 0.053(3) 0.041(3) -0.001(2) 0.003(2) 0.003(2) C4 0.042(3) 0.077(4) 0.050(3) 0.002(3) 0.008(3) -0.004(3) C5 0.043(3) 0.070(3) 0.057(4) -0.021(3) 0.004(3) 0.015(3) C6 0.030(3) 0.092(4) 0.061(3) -0.011(4) 0.000(3) 0.012(2) C7 0.038(3) 0.038(2) 0.043(3) -0.0038(17) -0.009(2) 0.000(2) C8 0.046(3) 0.038(2) 0.034(2) -0.0010(19) -0.001(2) 0.000(2) C9 0.049(3) 0.063(3) 0.045(3) -0.006(2) -0.007(3) 0.001(3) C13 0.041(3) 0.0335(19) 0.032(2) 0.0006(18) 0.004(2) 0.0001(19) C14 0.035(2) 0.0273(19) 0.035(2) 0.0037(16) 0.0013(19) 0.0023(17) C15 0.034(2) 0.0293(17) 0.034(2) 0.002(2) 0.008(2) -0.0008(16) C16 0.031(2) 0.0259(18) 0.031(2) -0.0004(15) 0.001(2) 0.0023(17) C17 0.046(3) 0.039(2) 0.039(3) -0.0057(19) 0.011(2) 0.003(2) C18 0.110(5) 0.048(3) 0.045(3) -0.013(2) 0.025(4) 0.000(3) C19 0.026(3) 0.044(2) 0.044(3) -0.001(2) 0.005(2) -0.0056(19) C20 0.028(3) 0.043(2) 0.033(3) -0.0081(18) -0.002(2) 0.0004(19) C21 0.021(3) 0.058(3) 0.045(3) -0.012(2) 0.003(2) -0.002(2) C22 0.024(3) 0.059(3) 0.056(4) -0.020(2) -0.006(2) 0.010(2) C23 0.043(3) 0.061(3) 0.069(4) -0.023(3) -0.004(3) 0.011(3) C27 0.040(3) 0.043(2) 0.057(3) -0.013(2) -0.018(3) 0.018(2) C28 0.035(3) 0.038(2) 0.041(3) -0.0118(19) -0.007(2) 0.004(2) C29 0.045(3) 0.037(2) 0.042(3) -0.0049(19) -0.006(2) 0.002(2) C30 0.082(4) 0.051(3) 0.053(3) 0.005(3) -0.018(4) 0.011(3) C31 0.060(4) 0.048(3) 0.034(3) -0.005(2) -0.007(3) 0.002(2) C32 0.052(3) 0.051(3) 0.048(3) 0.004(2) -0.010(3) -0.005(2) C33 0.032(3) 0.036(2) 0.041(3) -0.0098(17) -0.008(2) 0.0026(18) C34 0.068(4) 0.056(3) 0.046(3) 0.010(2) 0.025(3) 0.005(3) C35 0.074(5) 0.171(7) 0.073(5) 0.018(5) 0.036(4) 0.046(5) C36 0.139(7) 0.192(9) 0.035(4) -0.023(5) -0.004(5) 0.000(7) C37 0.067(4) 0.041(2) 0.049(3) -0.009(2) 0.007(3) -0.014(2) C38 0.126(8) 0.146(8) 0.092(6) -0.040(6) -0.016(6) -0.048(6) C39 0.117(6) 0.053(3) 0.093(5) -0.007(3) 0.039(4) 0.018(3) C40 0.038(3) 0.036(2) 0.036(3) -0.008(2) 0.003(2) -0.0011(18) C41 0.079(4) 0.046(2) 0.076(4) -0.010(3) 0.016(4) -0.023(2) O1 0.0341(17) 0.0379(15) 0.0323(16) -0.0041(13) 0.0021(14) 0.0036(13) O2 0.0326(18) 0.0339(14) 0.0342(17) -0.0042(12) -0.0001(14) 0.0039(12) O4 0.0396(18) 0.0487(19) 0.0305(16) -0.0065(15) 0.0043(14) 0.0015(16) O3 0.0478(19) 0.0291(12) 0.0518(19) -0.0092(15) 0.008(2) -0.0055(12) Hf1 0.03032(10) 0.02716(7) 0.03019(9) -0.00467(6) 0.00272(9) 0.00088(6) N1 0.029(2) 0.0295(16) 0.029(2) 0.0003(14) 0.0060(17) -0.0011(14) N2 0.037(2) 0.0351(18) 0.033(2) 0.0018(15) 0.0031(19) -0.0003(15) _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 C1 O1 1.343(5) . ? C1 C14 1.396(6) . ? C1 C2 1.423(6) . ? C2 C7 1.384(6) . ? C2 C3 1.533(6) . ? C3 C5 1.536(7) . ? C3 C6 1.544(6) . ? C3 C4 1.555(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.398(6) . ? C7 H7 0.9500 . ? C8 C13 1.397(6) . ? C8 C9 1.516(6) . ? C9 C12' 1.537(2) . ? C9 C11 1.539(2) . ? C9 C10' 1.539(2) . ? C9 C12 1.540(2) . ? C9 C11' 1.541(2) . ? C9 C10 1.542(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C12' H12D 0.9800 . ? C12' H12E 0.9800 . ? C12' H12F 0.9800 . ? C13 C14 1.391(6) . ? C13 H13 0.9500 . ? C14 C15 1.515(6) . ? C15 N1 1.491(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N1 1.495(4) . ? C16 C17 1.523(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.511(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N1 1.502(5) . ? C19 C20 1.519(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C33 1.386(6) . ? C20 C21 1.394(6) . ? C21 C22 1.368(7) . ? C21 H21 0.9500 . ? C22 C27 1.381(7) . ? C22 C23 1.539(6) . ? C23 C24' 1.537(2) . ? C23 C26 1.538(2) . ? C23 C26' 1.540(2) . ? C23 C25 1.540(2) . ? C23 C24 1.542(2) . ? C23 C25' 1.542(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? C26' H26D 0.9800 . ? C26' H26E 0.9800 . ? C26' H26F 0.9800 . ? C27 C28 1.396(6) . ? C27 H27 0.9500 . ? C28 C33 1.416(6) . ? C28 C29 1.538(7) . ? C29 C30 1.531(6) . ? C29 C32 1.540(7) . ? C29 C31 1.545(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 O2 1.349(5) . ? C34 O4 1.400(5) . ? C34 C35 1.486(8) . ? C34 C36 1.506(8) . ? C34 H34 1.0000 . ? 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 O3 1.381(5) . ? C37 C38 1.482(8) . ? C37 C39 1.518(8) . ? 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 . ? C40 N2 1.126(5) . ? C40 C41 1.451(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? O1 Hf1 2.032(3) . ? O2 Hf1 2.021(3) . ? O4 Hf1 1.910(3) . ? O3 Hf1 1.950(2) . ? Hf1 N2 2.401(3) . ? Hf1 N1 2.453(3) . ? 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 C1 C14 118.2(4) . . ? O1 C1 C2 122.1(4) . . ? C14 C1 C2 119.7(4) . . ? C7 C2 C1 116.8(4) . . ? C7 C2 C3 122.2(4) . . ? C1 C2 C3 121.0(4) . . ? C2 C3 C5 110.0(4) . . ? C2 C3 C6 112.4(4) . . ? C5 C3 C6 107.5(4) . . ? C2 C3 C4 110.5(4) . . ? C5 C3 C4 109.5(4) . . ? C6 C3 C4 106.8(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 C8 125.3(4) . . ? C2 C7 H7 117.4 . . ? C8 C7 H7 117.4 . . ? C13 C8 C7 115.9(4) . . ? C13 C8 C9 121.5(4) . . ? C7 C8 C9 122.5(4) . . ? C8 C9 C12' 115.1(7) . . ? C8 C9 C11 112.0(5) . . ? C12' C9 C11 129.7(8) . . ? C8 C9 C10' 113.0(8) . . ? C12' C9 C10' 114.9(9) . . ? C11 C9 C10' 57.9(7) . . ? C8 C9 C12 113.4(6) . . ? C12' C9 C12 32.4(6) . . ? C11 C9 C12 110.9(7) . . ? C10' C9 C12 132.6(9) . . ? C8 C9 C11' 106.7(7) . . ? C12' C9 C11' 105.8(9) . . ? C11 C9 C11' 42.7(6) . . ? C10' C9 C11' 99.4(9) . . ? C12 C9 C11' 75.8(7) . . ? C8 C9 C10 108.5(6) . . ? C12' C9 C10 72.1(7) . . ? C11 C9 C10 108.3(6) . . ? C10' C9 C10 52.6(8) . . ? C12 C9 C10 103.1(7) . . ? C11' C9 C10 141.7(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C10' H10D 109.5 . . ? C9 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C9 C11' H11D 109.5 . . ? C9 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C9 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C9 C12' H12D 109.5 . . ? C9 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C9 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C14 C13 C8 121.7(4) . . ? C14 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? C13 C14 C1 120.6(4) . . ? C13 C14 C15 119.8(4) . . ? C1 C14 C15 119.6(4) . . ? N1 C15 C14 113.2(3) . . ? N1 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? N1 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.8 . . ? N1 C16 C17 116.3(3) . . ? N1 C16 H16A 108.2 . . ? C17 C16 H16A 108.2 . . ? N1 C16 H16B 108.2 . . ? C17 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? C18 C17 C16 110.9(4) . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 112.4(3) . . ? N1 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N1 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C33 C20 C21 121.1(4) . . ? C33 C20 C19 118.7(4) . . ? C21 C20 C19 120.2(4) . . ? C22 C21 C20 121.2(5) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C27 117.3(4) . . ? C21 C22 C23 121.6(5) . . ? C27 C22 C23 121.1(5) . . ? C24' C23 C26 135.8(9) . . ? C24' C23 C22 111.3(8) . . ? C26 C23 C22 112.9(6) . . ? C24' C23 C26' 123.9(9) . . ? C26 C23 C26' 39.8(6) . . ? C22 C23 C26' 108.7(6) . . ? C24' C23 C25 47.4(7) . . ? C26 C23 C25 113.7(7) . . ? C22 C23 C25 108.8(5) . . ? C26' C23 C25 141.2(7) . . ? C24' C23 C24 55.9(7) . . ? C26 C23 C24 107.8(7) . . ? C22 C23 C24 111.7(6) . . ? C26' C23 C24 73.6(7) . . ? C25 C23 C24 101.3(6) . . ? C24' C23 C25' 103.9(9) . . ? C26 C23 C25' 57.6(7) . . ? C22 C23 C25' 111.2(7) . . ? C26' C23 C25' 96.5(8) . . ? C25 C23 C25' 60.4(7) . . ? C24 C23 C25' 137.0(8) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C24' H24D 109.5 . . ? C23 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C23 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C23 C25' H25D 109.5 . . ? C23 C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C23 C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C23 C26' H26D 109.5 . . ? C23 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C23 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C22 C27 C28 124.3(5) . . ? C22 C27 H27 117.9 . . ? C28 C27 H27 117.9 . . ? C27 C28 C33 117.0(4) . . ? C27 C28 C29 121.3(4) . . ? C33 C28 C29 121.7(4) . . ? C30 C29 C28 112.8(4) . . ? C30 C29 C32 107.2(4) . . ? C28 C29 C32 110.5(4) . . ? C30 C29 C31 107.2(4) . . ? C28 C29 C31 109.5(4) . . ? C32 C29 C31 109.6(4) . . ? 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 . . ? O2 C33 C20 119.6(4) . . ? O2 C33 C28 121.3(4) . . ? C20 C33 C28 119.1(4) . . ? O4 C34 C35 109.1(5) . . ? O4 C34 C36 110.5(5) . . ? C35 C34 C36 113.2(6) . . ? O4 C34 H34 108.0 . . ? C35 C34 H34 108.0 . . ? C36 C34 H34 108.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O3 C37 C38 111.2(5) . . ? O3 C37 C39 110.2(4) . . ? C38 C37 C39 111.9(5) . . ? O3 C37 H37 107.8 . . ? C38 C37 H37 107.8 . . ? C39 C37 H37 107.8 . . ? 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 . . ? N2 C40 C41 179.0(6) . . ? 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 . . ? C1 O1 Hf1 140.1(3) . . ? C33 O2 Hf1 141.0(3) . . ? C34 O4 Hf1 171.6(3) . . ? C37 O3 Hf1 154.3(3) . . ? O4 Hf1 O3 100.96(13) . . ? O4 Hf1 O2 97.10(12) . . ? O3 Hf1 O2 100.27(12) . . ? O4 Hf1 O1 100.23(12) . . ? O3 Hf1 O1 95.77(13) . . ? O2 Hf1 O1 153.65(11) . . ? O4 Hf1 N2 84.66(12) . . ? O3 Hf1 N2 173.55(15) . . ? O2 Hf1 N2 82.01(11) . . ? O1 Hf1 N2 80.01(12) . . ? O4 Hf1 N1 167.67(11) . . ? O3 Hf1 N1 91.20(12) . . ? O2 Hf1 N1 78.53(11) . . ? O1 Hf1 N1 80.37(11) . . ? N2 Hf1 N1 83.32(11) . . ? C15 N1 C16 110.1(3) . . ? C15 N1 C19 107.5(3) . . ? C16 N1 C19 111.5(3) . . ? C15 N1 Hf1 104.3(2) . . ? C16 N1 Hf1 118.7(2) . . ? C19 N1 Hf1 103.9(2) . . ? C40 N2 Hf1 170.7(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.600 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.149 #===END