# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email chem.tanmoy@gmail.com _publ_contact_author_name 'Tanmoy Kumar Saha' loop_ _publ_author_name 'Debashis Chakraborty' 'Tanmoy Kumar Saha' 'Bijja Rajashekhar' data_c2c _database_code_depnum_ccdc_archive 'CCDC 836424' #TrackingRef '6422_web_deposit_cif_file_0_tanmoykumarsaha_1311514612.c2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H60 Hf N4 O8' _chemical_formula_sum 'C54 H60 Hf N4 O8' _chemical_formula_weight 1071.55 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' Hf Hf -0.5830 6.1852 '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 _symmetry_space_group_name_Hall '-C 2yc ' 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 19.017(3) _cell_length_b 19.507(3) _cell_length_c 15.973(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.708(6) _cell_angle_gamma 90.00 _cell_volume 5245.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5477 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.77 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 2.043 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6508 _exptl_absorpt_correction_T_max 0.7492 _exptl_absorpt_process_details ' SADABS (Bruker,2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36623 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 36.50 _reflns_number_total 11509 _reflns_number_gt 8233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEXII (Bruker, 2004)' _computing_cell_refinement 'APEXII/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) ' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0455P)^2^+0.8734P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11509 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.41142(13) 0.16974(12) 0.85684(16) 0.0381(4) Uani 1 1 d . . . C2 C 0.33872(14) 0.16646(13) 0.86108(18) 0.0430(5) Uani 1 1 d . . . C3 C 0.32272(18) 0.21583(17) 0.9131(2) 0.0641(8) Uani 1 1 d . . . H3 H 0.2736 0.2136 0.9151 0.077 Uiso 1 1 calc R . . C4 C 0.3751(2) 0.2678(2) 0.9617(3) 0.0780(11) Uani 1 1 d . . . C5 C 0.44570(19) 0.27041(18) 0.9571(2) 0.0671(9) Uani 1 1 d . . . H5 H 0.4829 0.3054 0.9908 0.081 Uiso 1 1 calc R . . C6 C 0.46425(14) 0.22357(14) 0.90476(18) 0.0468(5) Uani 1 1 d . . . C7 C 0.28018(15) 0.11503(13) 0.8063(2) 0.0445(5) Uani 1 1 d . . . H7 H 0.2935 0.0807 0.7740 0.053 Uiso 1 1 calc R . . C8 C 0.15372(15) 0.06607(15) 0.7438(2) 0.0520(6) Uani 1 1 d . . . C9 C 0.16943(17) -0.00033(16) 0.7309(2) 0.0658(8) Uani 1 1 d . . . H9 H 0.2228 -0.0160 0.7586 0.079 Uiso 1 1 calc R . . C10 C 0.1079(2) -0.04514(18) 0.6774(3) 0.0777(10) Uani 1 1 d . . . H10 H 0.1197 -0.0910 0.6683 0.093 Uiso 1 1 calc R . . C11 C 0.03018(17) -0.02387(16) 0.6378(2) 0.0624(7) Uani 1 1 d . . . C12 C 0.01485(19) 0.0417(2) 0.6507(4) 0.0971(15) Uani 1 1 d . . . H12 H -0.0386 0.0572 0.6233 0.116 Uiso 1 1 calc R . . C13 C 0.0759(2) 0.08672(19) 0.7032(4) 0.0946(16) Uani 1 1 d . . . H13 H 0.0637 0.1327 0.7112 0.113 Uiso 1 1 calc R . . C14 C -0.1069(2) -0.0511(2) 0.5526(3) 0.0968(14) Uani 1 1 d . . . H14A H -0.1143 -0.0263 0.6013 0.145 Uiso 1 1 calc R . . H14B H -0.1416 -0.0914 0.5324 0.145 Uiso 1 1 calc R . . H14C H -0.1203 -0.0209 0.4982 0.145 Uiso 1 1 calc R . . C15 C 0.53820(14) 0.23378(13) 0.89986(18) 0.0459(5) Uani 1 1 d . . . H15 H 0.5705 0.2708 0.9359 0.055 Uiso 1 1 calc R . . C16 C 0.63826(13) 0.22294(13) 0.85790(16) 0.0419(5) Uani 1 1 d . . . C17 C 0.64594(17) 0.28872(16) 0.8324(2) 0.0590(7) Uani 1 1 d . . . H17 H 0.6029 0.3200 0.8131 0.071 Uiso 1 1 calc R . . C18 C 0.7172(2) 0.30945(19) 0.8350(3) 0.0738(9) Uani 1 1 d . . . H18 H 0.7229 0.3550 0.8180 0.089 Uiso 1 1 calc R . . C19 C 0.77878(17) 0.2643(2) 0.8618(2) 0.0691(9) Uani 1 1 d . . . C20 C 0.77144(15) 0.19968(18) 0.8877(2) 0.0628(8) Uani 1 1 d . . . H20 H 0.8148 0.1688 0.9075 0.075 Uiso 1 1 calc R . . C21 C 0.70126(14) 0.17829(15) 0.88564(19) 0.0526(6) Uani 1 1 d . . . H21 H 0.6965 0.1327 0.9034 0.063 Uiso 1 1 calc R . . C22 C 0.8589(4) 0.3257(4) 0.8148(5) 0.171(3) Uani 1 1 d . . . H22A H 0.8178 0.3203 0.7491 0.256 Uiso 1 1 calc R . . H22B H 0.9115 0.3219 0.8180 0.256 Uiso 1 1 calc R . . H22C H 0.8535 0.3707 0.8384 0.256 Uiso 1 1 calc R . . C23 C 0.3934(2) -0.00860(17) 0.5857(2) 0.0697(9) Uani 1 1 d . . . C24 C 0.4515(4) -0.0636(3) 0.6034(4) 0.161(3) Uani 1 1 d . . . H24A H 0.5033 -0.0435 0.6187 0.242 Uiso 1 1 calc R . . H24B H 0.4338 -0.0922 0.5467 0.242 Uiso 1 1 calc R . . H24C H 0.4562 -0.0918 0.6565 0.242 Uiso 1 1 calc R . . C25 C 0.3655(6) 0.0259(4) 0.4932(4) 0.220(5) Uani 1 1 d . . . H25A H 0.3649 0.0757 0.5018 0.329 Uiso 1 1 calc R . . H25B H 0.3118 0.0101 0.4499 0.329 Uiso 1 1 calc R . . H25C H 0.4014 0.0149 0.4667 0.329 Uiso 1 1 calc R . . C26 C 0.3211(4) -0.0344(4) 0.5869(7) 0.220(5) Uani 1 1 d . . . H26A H 0.3338 -0.0483 0.6513 0.330 Uiso 1 1 calc R . . H26B H 0.3007 -0.0740 0.5445 0.330 Uiso 1 1 calc R . . H26C H 0.2808 0.0018 0.5656 0.330 Uiso 1 1 calc R . . C27 C 0.3560(3) 0.3194(3) 1.0191(5) 0.146(3) Uani 1 1 d . . . H27A H 0.2984 0.3208 0.9961 0.219 Uiso 1 1 calc R . . H27B H 0.3747 0.3649 1.0124 0.219 Uiso 1 1 calc R . . H27C H 0.3824 0.3059 1.0858 0.219 Uiso 1 1 calc R . . Hf1 Hf 0.5000 0.102794(6) 0.7500 0.03499(5) Uani 1 2 d S . . N1 N 0.56475(11) 0.19897(10) 0.85302(14) 0.0393(4) Uani 1 1 d . . . N2 N 0.21136(14) 0.11510(12) 0.8009(2) 0.0553(6) Uani 1 1 d . . . O1 O 0.42713(9) 0.12418(9) 0.80735(12) 0.0415(3) Uani 1 1 d . . . O2 O 0.42673(10) 0.04131(9) 0.65571(13) 0.0495(4) Uani 1 1 d . . . O3 O -0.02646(14) -0.07234(14) 0.5901(2) 0.0888(8) Uani 1 1 d . . . O4 O 0.85090(16) 0.2788(2) 0.8656(2) 0.1159(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 0.0378(10) 0.0413(11) 0.0372(11) 0.0002(8) 0.0190(9) -0.0039(8) C2 0.0408(11) 0.0478(13) 0.0456(13) 0.0011(10) 0.0245(10) -0.0038(9) C3 0.0579(16) 0.074(2) 0.080(2) -0.0199(16) 0.0487(16) -0.0144(14) C4 0.081(2) 0.081(2) 0.099(3) -0.041(2) 0.066(2) -0.0243(18) C5 0.0673(18) 0.072(2) 0.077(2) -0.0350(16) 0.0459(17) -0.0252(15) C6 0.0432(12) 0.0552(14) 0.0471(13) -0.0113(11) 0.0253(11) -0.0102(10) C7 0.0417(12) 0.0479(14) 0.0481(14) 0.0036(10) 0.0243(11) -0.0020(9) C8 0.0403(12) 0.0541(16) 0.0652(17) -0.0021(12) 0.0276(12) -0.0054(10) C9 0.0437(14) 0.0552(17) 0.087(2) 0.0051(15) 0.0210(15) 0.0036(12) C10 0.0614(18) 0.0504(18) 0.104(3) -0.0071(17) 0.0233(19) 0.0027(14) C11 0.0501(15) 0.0543(17) 0.0721(19) -0.0016(14) 0.0193(14) -0.0064(12) C12 0.0388(14) 0.069(2) 0.153(4) -0.022(2) 0.020(2) -0.0021(14) C13 0.0446(16) 0.061(2) 0.163(5) -0.032(2) 0.035(2) -0.0024(14) C14 0.0530(18) 0.089(3) 0.116(3) -0.015(2) 0.011(2) -0.0179(18) C15 0.0411(12) 0.0499(14) 0.0447(13) -0.0094(10) 0.0183(11) -0.0139(10) C16 0.0373(10) 0.0503(13) 0.0371(11) -0.0062(9) 0.0163(9) -0.0120(9) C17 0.0522(15) 0.0566(17) 0.0684(18) 0.0043(13) 0.0284(14) -0.0117(12) C18 0.0683(19) 0.070(2) 0.080(2) 0.0099(17) 0.0320(18) -0.0286(16) C19 0.0446(14) 0.103(3) 0.0594(18) -0.0085(17) 0.0240(14) -0.0274(16) C20 0.0354(12) 0.085(2) 0.0602(17) -0.0097(15) 0.0153(12) -0.0072(13) C21 0.0374(11) 0.0623(17) 0.0501(14) -0.0021(12) 0.0136(11) -0.0084(10) C22 0.127(5) 0.231(8) 0.190(7) 0.013(6) 0.103(5) -0.073(5) C23 0.0609(18) 0.0591(18) 0.0651(19) -0.0248(15) 0.0089(15) -0.0032(14) C24 0.145(5) 0.121(5) 0.145(5) -0.074(4) 0.006(4) 0.055(4) C25 0.362(12) 0.160(6) 0.056(3) -0.017(3) 0.029(5) 0.073(7) C26 0.111(5) 0.151(6) 0.378(13) -0.112(8) 0.098(7) -0.078(5) C27 0.137(4) 0.154(5) 0.215(6) -0.122(5) 0.139(5) -0.067(4) Hf1 0.02901(6) 0.03428(7) 0.03865(8) 0.000 0.01317(5) 0.000 N1 0.0339(8) 0.0444(10) 0.0385(10) -0.0016(8) 0.0159(8) -0.0075(7) N2 0.0433(11) 0.0572(14) 0.0718(17) -0.0060(11) 0.0322(12) -0.0072(9) O1 0.0358(7) 0.0416(8) 0.0483(9) -0.0064(7) 0.0205(7) -0.0067(6) O2 0.0440(9) 0.0446(9) 0.0540(10) -0.0133(8) 0.0177(8) -0.0065(7) O3 0.0626(14) 0.0657(15) 0.110(2) -0.0199(14) 0.0167(14) -0.0142(12) O4 0.0633(15) 0.169(3) 0.122(3) 0.011(2) 0.0489(17) -0.0435(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.313(3) . ? C1 C6 1.408(3) . ? C1 C2 1.417(3) . ? C2 C3 1.394(4) . ? C2 C7 1.451(3) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.379(4) . ? C4 C27 1.515(5) . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C15 1.458(3) . ? C7 N2 1.271(3) . ? C7 H7 0.9500 . ? C8 C9 1.366(4) . ? C8 C13 1.371(4) . ? C8 N2 1.420(4) . ? C9 C10 1.391(4) . ? C9 H9 0.9500 . ? C10 C11 1.373(4) . ? C10 H10 0.9500 . ? C11 C12 1.349(5) . ? C11 O3 1.368(4) . ? C12 C13 1.385(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O3 1.421(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N1 1.276(3) . ? C15 H15 0.9500 . ? C16 C17 1.374(4) . ? C16 C21 1.377(4) . ? C16 N1 1.441(3) . ? C17 C18 1.397(4) . ? C17 H17 0.9500 . ? C18 C19 1.365(5) . ? C18 H18 0.9500 . ? C19 C20 1.354(5) . ? C19 O4 1.374(4) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O4 1.277(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O2 1.393(3) . ? C23 C24 1.470(6) . ? C23 C26 1.473(7) . ? C23 C25 1.479(7) . ? 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 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Hf1 O2 1.9227(16) . ? Hf1 O2 1.9227(16) 2_656 ? Hf1 O1 2.0284(17) 2_656 ? Hf1 O1 2.0284(17) . ? Hf1 N1 2.4206(19) . ? Hf1 N1 2.4206(19) 2_656 ? 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 C6 121.8(2) . . ? O1 C1 C2 119.9(2) . . ? C6 C1 C2 118.2(2) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 C7 121.2(2) . . ? C1 C2 C7 119.6(2) . . ? C4 C3 C2 122.8(3) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C5 C4 C3 117.5(3) . . ? C5 C4 C27 121.5(3) . . ? C3 C4 C27 121.0(3) . . ? C4 C5 C6 122.3(3) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 120.1(2) . . ? C5 C6 C15 117.6(2) . . ? C1 C6 C15 122.3(2) . . ? N2 C7 C2 121.2(3) . . ? N2 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? C9 C8 C13 118.1(3) . . ? C9 C8 N2 125.3(3) . . ? C13 C8 N2 116.6(3) . . ? C8 C9 C10 120.5(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.8(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 O3 124.8(3) . . ? C12 C11 C10 118.6(3) . . ? O3 C11 C10 116.6(3) . . ? C11 C12 C13 120.9(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 121.1(3) . . ? C8 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 127.8(2) . . ? N1 C15 H15 116.1 . . ? C6 C15 H15 116.1 . . ? C17 C16 C21 119.3(2) . . ? C17 C16 N1 121.4(2) . . ? C21 C16 N1 119.3(2) . . ? C16 C17 C18 119.8(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.1(3) . . ? C20 C19 O4 114.9(4) . . ? C18 C19 O4 125.0(4) . . ? C19 C20 C21 120.6(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 120.1(3) . . ? C16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 C24 109.6(3) . . ? O2 C23 C26 107.9(4) . . ? C24 C23 C26 111.7(5) . . ? O2 C23 C25 107.5(4) . . ? C24 C23 C25 114.4(5) . . ? C26 C23 C25 105.4(6) . . ? 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 . . ? C4 C27 H27A 109.5 . . ? C4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 Hf1 O2 102.82(11) . 2_656 ? O2 Hf1 O1 99.96(8) . 2_656 ? O2 Hf1 O1 94.79(7) 2_656 2_656 ? O2 Hf1 O1 94.79(7) . . ? O2 Hf1 O1 99.96(8) 2_656 . ? O1 Hf1 O1 156.26(10) 2_656 . ? O2 Hf1 N1 165.99(7) . . ? O2 Hf1 N1 89.80(8) 2_656 . ? O1 Hf1 N1 84.79(7) 2_656 . ? O1 Hf1 N1 76.82(6) . . ? O2 Hf1 N1 89.80(7) . 2_656 ? O2 Hf1 N1 165.99(7) 2_656 2_656 ? O1 Hf1 N1 76.82(6) 2_656 2_656 ? O1 Hf1 N1 84.79(7) . 2_656 ? N1 Hf1 N1 78.38(9) . 2_656 ? C15 N1 C16 115.7(2) . . ? C15 N1 Hf1 126.61(15) . . ? C16 N1 Hf1 117.53(15) . . ? C7 N2 C8 120.4(3) . . ? C1 O1 Hf1 143.68(14) . . ? C23 O2 Hf1 163.3(2) . . ? C11 O3 C14 116.6(3) . . ? C22 O4 C19 122.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.2(3) . . . . ? C6 C1 C2 C3 -0.7(4) . . . . ? O1 C1 C2 C7 -3.5(4) . . . . ? C6 C1 C2 C7 175.0(2) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C7 C2 C3 C4 -176.3(3) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? C2 C3 C4 C27 -178.6(4) . . . . ? C3 C4 C5 C6 0.9(6) . . . . ? C27 C4 C5 C6 -179.9(5) . . . . ? C4 C5 C6 C1 -2.2(5) . . . . ? C4 C5 C6 C15 176.1(4) . . . . ? O1 C1 C6 C5 -179.4(3) . . . . ? C2 C1 C6 C5 2.1(4) . . . . ? O1 C1 C6 C15 2.3(4) . . . . ? C2 C1 C6 C15 -176.2(2) . . . . ? C3 C2 C7 N2 2.9(4) . . . . ? C1 C2 C7 N2 -172.7(3) . . . . ? C13 C8 C9 C10 0.3(6) . . . . ? N2 C8 C9 C10 176.5(3) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C9 C10 C11 C12 0.9(6) . . . . ? C9 C10 C11 O3 -177.1(4) . . . . ? O3 C11 C12 C13 177.4(4) . . . . ? C10 C11 C12 C13 -0.4(7) . . . . ? C9 C8 C13 C12 0.2(7) . . . . ? N2 C8 C13 C12 -176.3(4) . . . . ? C11 C12 C13 C8 -0.2(8) . . . . ? C5 C6 C15 N1 -176.8(3) . . . . ? C1 C6 C15 N1 1.5(5) . . . . ? C21 C16 C17 C18 0.0(4) . . . . ? N1 C16 C17 C18 -177.8(3) . . . . ? C16 C17 C18 C19 0.6(5) . . . . ? C17 C18 C19 C20 -1.2(5) . . . . ? C17 C18 C19 O4 179.0(3) . . . . ? C18 C19 C20 C21 1.2(5) . . . . ? O4 C19 C20 C21 -179.0(3) . . . . ? C17 C16 C21 C20 0.0(4) . . . . ? N1 C16 C21 C20 177.8(2) . . . . ? C19 C20 C21 C16 -0.6(5) . . . . ? C6 C15 N1 C16 177.1(3) . . . . ? C6 C15 N1 Hf1 1.5(4) . . . . ? C17 C16 N1 C15 -56.6(3) . . . . ? C21 C16 N1 C15 125.7(3) . . . . ? C17 C16 N1 Hf1 119.4(2) . . . . ? C21 C16 N1 Hf1 -58.3(3) . . . . ? O2 Hf1 N1 C15 49.0(4) . . . . ? O2 Hf1 N1 C15 -105.5(2) 2_656 . . . ? O1 Hf1 N1 C15 159.6(2) 2_656 . . . ? O1 Hf1 N1 C15 -5.3(2) . . . . ? N1 Hf1 N1 C15 82.0(2) 2_656 . . . ? O2 Hf1 N1 C16 -126.5(3) . . . . ? O2 Hf1 N1 C16 78.95(17) 2_656 . . . ? O1 Hf1 N1 C16 -15.88(16) 2_656 . . . ? O1 Hf1 N1 C16 179.24(17) . . . . ? N1 Hf1 N1 C16 -93.46(17) 2_656 . . . ? C2 C7 N2 C8 177.4(3) . . . . ? C9 C8 N2 C7 35.4(5) . . . . ? C13 C8 N2 C7 -148.4(4) . . . . ? C6 C1 O1 Hf1 -12.8(4) . . . . ? C2 C1 O1 Hf1 165.66(19) . . . . ? O2 Hf1 O1 C1 -156.6(3) . . . . ? O2 Hf1 O1 C1 99.5(3) 2_656 . . . ? O1 Hf1 O1 C1 -28.1(3) 2_656 . . . ? N1 Hf1 O1 C1 12.0(3) . . . . ? N1 Hf1 O1 C1 -67.2(3) 2_656 . . . ? C24 C23 O2 Hf1 34.5(10) . . . . ? C26 C23 O2 Hf1 156.4(7) . . . . ? C25 C23 O2 Hf1 -90.4(8) . . . . ? O2 Hf1 O2 C23 -63.2(7) 2_656 . . . ? O1 Hf1 O2 C23 34.1(7) 2_656 . . . ? O1 Hf1 O2 C23 -164.5(7) . . . . ? N1 Hf1 O2 C23 143.0(7) . . . . ? N1 Hf1 O2 C23 110.7(7) 2_656 . . . ? C12 C11 O3 C14 -0.5(6) . . . . ? C10 C11 O3 C14 177.3(4) . . . . ? C20 C19 O4 C22 155.0(5) . . . . ? C18 C19 O4 C22 -25.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.366 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.091 # Attachment '6423_web_deposit_cif_file_1_tanmoykumarsaha_1311514612.new_1.cif' data_new1 _database_code_depnum_ccdc_archive 'CCDC 836425' #TrackingRef '6423_web_deposit_cif_file_1_tanmoykumarsaha_1311514612.new_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H90 Cl2 N4 O4 Zr' _chemical_formula_weight 1213.58 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' Cl Cl 0.1484 0.1585 '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 12.070(2) _cell_length_b 22.740(5) _cell_length_c 27.720(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.89(3) _cell_angle_gamma 90.00 _cell_volume 7471(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'clear light yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52626 _diffrn_reflns_av_R_equivalents 0.1099 _diffrn_reflns_av_sigmaI/netI 0.1832 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.33 _reflns_number_total 17045 _reflns_number_gt 7427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1827P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17045 _refine_ls_number_parameters 750 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2163 _refine_ls_R_factor_gt 0.0988 _refine_ls_wR_factor_ref 0.3318 _refine_ls_wR_factor_gt 0.2589 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.844 _refine_ls_shift/su_mean 0.023 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 0.3987(5) 0.1848(3) 0.0671(2) 0.0308(14) Uani 1 1 d . . . C2 C 0.5032(5) 0.1574(3) 0.0654(2) 0.0315(15) Uani 1 1 d . . . C3 C 0.5717(5) 0.1796(3) 0.0343(2) 0.0371(16) Uani 1 1 d . . . H3 H 0.6403 0.1615 0.0332 0.045 Uiso 1 1 calc R . . C4 C 0.5394(5) 0.2268(3) 0.0060(3) 0.0424(17) Uani 1 1 d . . . C5 C 0.4383(6) 0.2554(3) 0.0081(2) 0.0448(18) Uani 1 1 d . . . H5 H 0.4180 0.2887 -0.0109 0.054 Uiso 1 1 calc R . . C6 C 0.3685(5) 0.2348(3) 0.0381(2) 0.0355(15) Uani 1 1 d . . . C7 C 0.2647(6) 0.2673(3) 0.0429(2) 0.0432(17) Uani 1 1 d . . . H7 H 0.2186 0.2522 0.0633 0.052 Uiso 1 1 calc R . . C8 C 0.1419(7) 0.3469(4) 0.0309(3) 0.075(3) Uani 1 1 d . . . C9 C 0.0498(8) 0.3554(5) -0.0070(3) 0.094(4) Uani 1 1 d . . . C10 C -0.0432(10) 0.3873(7) 0.0032(5) 0.138(6) Uani 1 1 d . . . H10 H -0.1043 0.3948 -0.0220 0.165 Uiso 1 1 calc R . . C11 C -0.0452(11) 0.4071(6) 0.0486(5) 0.133(6) Uani 1 1 d . . . H11 H -0.1096 0.4257 0.0549 0.159 Uiso 1 1 calc R . . C12 C 0.0462(11) 0.4004(5) 0.0857(4) 0.112(5) Uani 1 1 d . . . H12 H 0.0443 0.4157 0.1166 0.134 Uiso 1 1 calc R . . C13 C 0.1411(8) 0.3713(4) 0.0777(3) 0.076(3) Uani 1 1 d . . . C14 C 0.0531(10) 0.3321(7) -0.0593(4) 0.116(5) Uani 1 1 d . . . H14 H 0.1227 0.3090 -0.0563 0.139 Uiso 1 1 calc R . . C15 C 0.066(3) 0.3835(11) -0.0942(7) 0.32(2) Uani 1 1 d . . . H15A H 0.0828 0.3683 -0.1242 0.487 Uiso 1 1 calc R . . H15B H 0.1257 0.4089 -0.0788 0.487 Uiso 1 1 calc R . . H15C H -0.0036 0.4053 -0.1011 0.487 Uiso 1 1 calc R . . C16 C -0.035(2) 0.2936(13) -0.0778(6) 0.288(17) Uani 1 1 d . . . H16A H -0.0971 0.3155 -0.0959 0.433 Uiso 1 1 calc R . . H16B H -0.0584 0.2734 -0.0511 0.433 Uiso 1 1 calc R . . H16C H -0.0094 0.2656 -0.0992 0.433 Uiso 1 1 calc R . . C17 C 0.2438(9) 0.3674(5) 0.1189(4) 0.088(3) Uani 1 1 d . . . H17 H 0.3033 0.3472 0.1057 0.105 Uiso 1 1 calc R . . C18 C 0.2880(11) 0.4267(6) 0.1356(5) 0.126(5) Uani 1 1 d . . . H18A H 0.2367 0.4454 0.1534 0.189 Uiso 1 1 calc R . . H18B H 0.2951 0.4502 0.1076 0.189 Uiso 1 1 calc R . . H18C H 0.3605 0.4226 0.1566 0.189 Uiso 1 1 calc R . . C19 C 0.2217(12) 0.3322(6) 0.1612(4) 0.136(5) Uani 1 1 d . . . H19A H 0.2909 0.3266 0.1843 0.205 Uiso 1 1 calc R . . H19B H 0.1911 0.2947 0.1498 0.205 Uiso 1 1 calc R . . H19C H 0.1687 0.3526 0.1770 0.205 Uiso 1 1 calc R . . C20 C 0.5479(5) 0.1092(3) 0.0964(2) 0.0285(14) Uani 1 1 d . . . H20 H 0.6182 0.0954 0.0925 0.034 Uiso 1 1 calc R . . C21 C 0.5748(5) 0.0373(3) 0.1559(2) 0.0276(13) Uani 1 1 d . . . C22 C 0.6533(5) 0.0538(3) 0.1976(2) 0.0312(14) Uani 1 1 d . . . C23 C 0.7207(5) 0.0100(3) 0.2225(3) 0.0425(17) Uani 1 1 d . . . H23 H 0.7729 0.0197 0.2505 0.051 Uiso 1 1 calc R . . C24 C 0.7124(6) -0.0476(3) 0.2068(3) 0.0508(19) Uani 1 1 d . . . H24 H 0.7592 -0.0761 0.2239 0.061 Uiso 1 1 calc R . . C25 C 0.6351(6) -0.0627(3) 0.1659(3) 0.0437(17) Uani 1 1 d . . . H25 H 0.6299 -0.1016 0.1556 0.052 Uiso 1 1 calc R . . C26 C 0.5637(5) -0.0207(3) 0.1392(2) 0.0338(15) Uani 1 1 d . . . C27 C 0.6673(5) 0.1176(3) 0.2154(2) 0.0383(16) Uani 1 1 d . . . H27 H 0.6005 0.1393 0.1990 0.046 Uiso 1 1 calc R . . C28 C 0.6720(8) 0.1230(4) 0.2700(3) 0.068(2) Uani 1 1 d . . . H28A H 0.6104 0.1016 0.2789 0.102 Uiso 1 1 calc R . . H28B H 0.6666 0.1637 0.2785 0.102 Uiso 1 1 calc R . . H28C H 0.7421 0.1072 0.2873 0.102 Uiso 1 1 calc R . . C29 C 0.7683(7) 0.1458(4) 0.2002(3) 0.075(3) Uani 1 1 d . . . H29A H 0.8356 0.1260 0.2160 0.113 Uiso 1 1 calc R . . H29B H 0.7722 0.1864 0.2098 0.113 Uiso 1 1 calc R . . H29C H 0.7614 0.1429 0.1652 0.113 Uiso 1 1 calc R . . C30 C 0.4829(5) -0.0385(3) 0.0935(3) 0.0423(17) Uani 1 1 d . . . H30 H 0.4297 -0.0061 0.0839 0.051 Uiso 1 1 calc R . . C31 C 0.5481(7) -0.0491(4) 0.0515(3) 0.064(2) Uani 1 1 d . . . H31A H 0.5861 -0.0136 0.0452 0.096 Uiso 1 1 calc R . . H31B H 0.4963 -0.0605 0.0223 0.096 Uiso 1 1 calc R . . H31C H 0.6026 -0.0798 0.0608 0.096 Uiso 1 1 calc R . . C32 C 0.4153(8) -0.0940(4) 0.1014(4) 0.078(3) Uani 1 1 d . . . H32A H 0.4663 -0.1260 0.1112 0.118 Uiso 1 1 calc R . . H32B H 0.3651 -0.1039 0.0713 0.118 Uiso 1 1 calc R . . H32C H 0.3722 -0.0865 0.1265 0.118 Uiso 1 1 calc R . . C33 C 0.1599(6) 0.0372(4) 0.0519(3) 0.063(2) Uani 1 1 d . . . H33 H 0.0857 0.0525 0.0552 0.076 Uiso 1 1 calc R . . C34 C 0.1947(9) 0.0689(5) 0.0107(3) 0.095(4) Uani 1 1 d . . . H34A H 0.1885 0.1105 0.0154 0.142 Uiso 1 1 calc R . . H34B H 0.1467 0.0576 -0.0196 0.142 Uiso 1 1 calc R . . H34C H 0.2715 0.0591 0.0094 0.142 Uiso 1 1 calc R . . C35 C 0.1475(9) -0.0283(5) 0.0439(4) 0.110(4) Uani 1 1 d . . . H35A H 0.2194 -0.0450 0.0416 0.165 Uiso 1 1 calc R . . H35B H 0.0947 -0.0358 0.0140 0.165 Uiso 1 1 calc R . . H35C H 0.1204 -0.0458 0.0710 0.165 Uiso 1 1 calc R . . C36 C 0.3225(5) 0.1971(3) 0.2293(2) 0.0286(14) Uani 1 1 d . . . C37 C 0.2116(5) 0.1882(3) 0.2382(2) 0.0347(15) Uani 1 1 d . . . C38 C 0.1752(5) 0.2179(3) 0.2760(3) 0.0424(18) Uani 1 1 d . . . H38 H 0.1025 0.2117 0.2817 0.051 Uiso 1 1 calc R . . C39 C 0.2459(5) 0.2565(3) 0.3052(3) 0.0469(19) Uani 1 1 d . . . C40 C 0.3525(5) 0.2671(3) 0.2963(2) 0.0424(17) Uani 1 1 d . . . H40 H 0.3991 0.2937 0.3160 0.051 Uiso 1 1 calc R . . C41 C 0.3916(5) 0.2389(3) 0.2585(2) 0.0345(15) Uani 1 1 d . . . C42 C 0.5068(5) 0.2506(3) 0.2497(2) 0.0356(15) Uani 1 1 d . . . H42 H 0.5342 0.2280 0.2265 0.043 Uiso 1 1 calc R . . C43 C 0.6822(5) 0.2960(3) 0.2637(2) 0.0368(16) Uani 1 1 d . . . C44 C 0.7698(5) 0.2800(3) 0.3029(2) 0.0410(17) Uani 1 1 d . . . C45 C 0.8797(6) 0.2858(3) 0.2956(3) 0.0490(19) Uani 1 1 d . . . H45 H 0.9388 0.2755 0.3208 0.059 Uiso 1 1 calc R . . C46 C 0.9040(6) 0.3064(3) 0.2521(3) 0.054(2) Uani 1 1 d . . . H46 H 0.9784 0.3097 0.2479 0.064 Uiso 1 1 calc R . . C47 C 0.8165(6) 0.3223(3) 0.2148(3) 0.053(2) Uani 1 1 d . . . H47 H 0.8336 0.3363 0.1856 0.063 Uiso 1 1 calc R . . C48 C 0.7036(6) 0.3181(3) 0.2191(3) 0.0424(17) Uani 1 1 d . . . C49 C 0.7420(6) 0.2582(3) 0.3498(3) 0.052(2) Uani 1 1 d . . . H49 H 0.6712 0.2361 0.3415 0.062 Uiso 1 1 calc R . . C50 C 0.8330(8) 0.2150(5) 0.3782(4) 0.100(4) Uani 1 1 d . . . H50A H 0.8466 0.1840 0.3566 0.150 Uiso 1 1 calc R . . H50B H 0.8061 0.1985 0.4057 0.150 Uiso 1 1 calc R . . H50C H 0.9018 0.2360 0.3897 0.150 Uiso 1 1 calc R . . C51 C 0.7216(10) 0.3084(5) 0.3837(4) 0.099(4) Uani 1 1 d . . . H51A H 0.7895 0.3311 0.3927 0.148 Uiso 1 1 calc R . . H51B H 0.7002 0.2926 0.4127 0.148 Uiso 1 1 calc R . . H51C H 0.6623 0.3332 0.3668 0.148 Uiso 1 1 calc R . . C52 C 0.6119(6) 0.3379(4) 0.1780(3) 0.053(2) Uani 1 1 d . . . H52 H 0.5417 0.3378 0.1909 0.064 Uiso 1 1 calc R . . C53 C 0.6268(10) 0.3984(5) 0.1609(4) 0.101(4) Uani 1 1 d . . . H53A H 0.6249 0.4256 0.1872 0.151 Uiso 1 1 calc R . . H53B H 0.5672 0.4075 0.1338 0.151 Uiso 1 1 calc R . . H53C H 0.6982 0.4014 0.1505 0.151 Uiso 1 1 calc R . . C54 C 0.5945(10) 0.2967(5) 0.1352(4) 0.102(4) Uani 1 1 d . . . H54A H 0.6574 0.2994 0.1187 0.154 Uiso 1 1 calc R . . H54B H 0.5265 0.3071 0.1128 0.154 Uiso 1 1 calc R . . H54C H 0.5884 0.2572 0.1466 0.154 Uiso 1 1 calc R . . C55 C 0.1297(5) 0.1524(3) 0.2066(2) 0.0367(16) Uani 1 1 d . . . H55 H 0.0571 0.1530 0.2133 0.044 Uiso 1 1 calc R . . C56 C 0.0397(5) 0.0937(3) 0.1436(3) 0.0382(16) Uani 1 1 d . . . C57 C -0.0276(5) 0.1258(4) 0.1063(3) 0.0477(19) Uani 1 1 d . . . C58 C -0.1257(5) 0.0992(4) 0.0809(3) 0.059(2) Uani 1 1 d . . . H58 H -0.1714 0.1195 0.0555 0.071 Uiso 1 1 calc R . . C59 C -0.1558(6) 0.0437(5) 0.0927(3) 0.068(3) Uani 1 1 d . . . H59 H -0.2219 0.0270 0.0755 0.081 Uiso 1 1 calc R . . C60 C -0.0906(6) 0.0126(4) 0.1293(3) 0.066(3) Uani 1 1 d . . . H60 H -0.1132 -0.0249 0.1367 0.079 Uiso 1 1 calc R . . C61 C 0.0111(5) 0.0361(4) 0.1566(3) 0.050(2) Uani 1 1 d . . . C62 C 0.0030(6) 0.1865(4) 0.0923(3) 0.062(2) Uani 1 1 d . . . H62 H 0.0843 0.1910 0.1043 0.074 Uiso 1 1 calc R . . C63 C -0.0573(8) 0.2351(5) 0.1183(4) 0.092(3) Uani 1 1 d . . . H63A H -0.1375 0.2315 0.1081 0.137 Uiso 1 1 calc R . . H63B H -0.0337 0.2733 0.1095 0.137 Uiso 1 1 calc R . . H63C H -0.0374 0.2303 0.1533 0.137 Uiso 1 1 calc R . . C64 C -0.0182(8) 0.1992(6) 0.0383(4) 0.103(4) Uani 1 1 d . . . H64A H 0.0277 0.1738 0.0226 0.155 Uiso 1 1 calc R . . H64B H 0.0005 0.2394 0.0331 0.155 Uiso 1 1 calc R . . H64C H -0.0963 0.1925 0.0246 0.155 Uiso 1 1 calc R . . C65 C 0.0830(6) 0.0022(4) 0.1971(3) 0.064(2) Uani 1 1 d . . . H65 H 0.1602 0.0172 0.2006 0.076 Uiso 1 1 calc R . . C66 C 0.0873(10) -0.0654(4) 0.1871(5) 0.120(5) Uani 1 1 d . . . H66A H 0.0138 -0.0821 0.1860 0.179 Uiso 1 1 calc R . . H66B H 0.1402 -0.0837 0.2130 0.179 Uiso 1 1 calc R . . H66C H 0.1105 -0.0718 0.1563 0.179 Uiso 1 1 calc R . . C67 C 0.0451(7) 0.0132(5) 0.2451(4) 0.090(3) Uani 1 1 d . . . H67A H 0.0452 0.0548 0.2513 0.136 Uiso 1 1 calc R . . H67B H 0.0956 -0.0060 0.2712 0.136 Uiso 1 1 calc R . . H67C H -0.0298 -0.0020 0.2432 0.136 Uiso 1 1 calc R . . C68 C 0.4178(6) 0.0171(4) 0.2445(3) 0.051(2) Uani 1 1 d . . . H68 H 0.4990 0.0243 0.2481 0.061 Uiso 1 1 calc R . . C69 C 0.3987(9) -0.0488(4) 0.2442(4) 0.082(3) Uani 1 1 d . . . H69A H 0.3196 -0.0566 0.2417 0.123 Uiso 1 1 calc R . . H69B H 0.4397 -0.0655 0.2741 0.123 Uiso 1 1 calc R . . H69C H 0.4245 -0.0659 0.2167 0.123 Uiso 1 1 calc R . . C70 C 0.3759(7) 0.0478(4) 0.2865(3) 0.067(2) Uani 1 1 d . . . H70A H 0.3980 0.0884 0.2875 0.100 Uiso 1 1 calc R . . H70B H 0.4081 0.0292 0.3170 0.100 Uiso 1 1 calc R . . H70C H 0.2951 0.0451 0.2814 0.100 Uiso 1 1 calc R . . N1 N 0.5025(4) 0.0823(2) 0.12906(18) 0.0262(11) Uani 1 1 d . . . N2 N 0.1440(4) 0.1195(2) 0.1701(2) 0.0352(13) Uani 1 1 d . . . N3 N 0.2369(5) 0.3148(3) 0.0204(2) 0.0585(18) Uani 1 1 d . . . N4 N 0.5699(4) 0.2904(3) 0.2727(2) 0.0436(15) Uani 1 1 d . . . O1 O 0.3320(3) 0.1644(2) 0.09536(16) 0.0373(11) Uani 1 1 d . . . O2 O 0.2349(3) 0.0493(2) 0.09648(17) 0.0428(12) Uani 1 1 d . . . O3 O 0.3597(3) 0.1694(2) 0.19458(16) 0.0388(11) Uani 1 1 d . . . O4 O 0.3631(3) 0.0422(2) 0.20006(17) 0.0397(11) Uani 1 1 d . . . Cl1 Cl 0.62756(18) 0.25421(11) -0.03243(9) 0.0732(7) Uani 1 1 d . . . Cl2 Cl 0.20090(17) 0.29035(13) 0.35391(9) 0.0887(9) Uani 1 1 d . . . Zr1 Zr 0.31988(4) 0.09775(3) 0.14705(2) 0.0308(2) 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 0.030(3) 0.034(4) 0.028(4) -0.006(3) 0.001(3) 0.003(3) C2 0.019(3) 0.043(4) 0.033(4) -0.003(3) 0.004(3) 0.006(3) C3 0.033(4) 0.043(4) 0.036(4) 0.002(3) 0.008(3) 0.008(3) C4 0.039(4) 0.053(5) 0.037(4) 0.002(3) 0.012(3) 0.004(3) C5 0.048(4) 0.050(5) 0.033(4) 0.001(3) -0.002(3) 0.009(3) C6 0.033(3) 0.043(4) 0.028(4) -0.004(3) 0.001(3) 0.004(3) C7 0.045(4) 0.050(5) 0.032(4) 0.006(3) 0.000(3) 0.015(3) C8 0.072(6) 0.091(7) 0.058(6) 0.021(5) 0.005(4) 0.041(5) C9 0.084(7) 0.136(10) 0.053(6) 0.003(6) -0.007(5) 0.075(7) C10 0.115(10) 0.188(15) 0.097(10) -0.012(9) -0.012(7) 0.112(10) C11 0.114(10) 0.168(13) 0.112(11) -0.024(10) 0.010(8) 0.100(9) C12 0.132(10) 0.119(10) 0.079(8) -0.009(7) 0.006(7) 0.085(8) C13 0.090(7) 0.081(7) 0.054(6) 0.006(5) 0.005(5) 0.047(5) C14 0.092(8) 0.170(13) 0.070(8) -0.016(8) -0.027(6) 0.071(8) C15 0.64(6) 0.23(3) 0.163(19) 0.087(19) 0.24(3) 0.17(3) C16 0.34(3) 0.44(4) 0.083(13) -0.12(2) 0.043(15) -0.16(3) C17 0.101(8) 0.098(8) 0.059(7) -0.022(6) 0.004(5) 0.036(6) C18 0.133(11) 0.124(11) 0.117(11) -0.042(9) 0.016(8) 0.017(9) C19 0.175(14) 0.145(13) 0.080(9) 0.017(9) 0.000(8) 0.043(10) C20 0.019(3) 0.036(4) 0.032(4) -0.001(3) 0.007(3) 0.009(2) C21 0.026(3) 0.025(3) 0.033(4) 0.001(3) 0.009(3) 0.002(2) C22 0.023(3) 0.034(4) 0.038(4) 0.001(3) 0.009(3) 0.003(3) C23 0.035(4) 0.050(5) 0.041(4) 0.006(4) 0.004(3) 0.000(3) C24 0.052(5) 0.044(5) 0.057(5) 0.010(4) 0.011(4) 0.010(3) C25 0.047(4) 0.028(4) 0.059(5) 0.001(3) 0.019(4) 0.001(3) C26 0.031(3) 0.033(4) 0.041(4) -0.002(3) 0.015(3) -0.008(3) C27 0.033(4) 0.038(4) 0.041(4) -0.005(3) -0.001(3) 0.004(3) C28 0.102(7) 0.063(6) 0.037(5) -0.018(4) 0.010(4) -0.015(5) C29 0.084(6) 0.046(5) 0.107(8) -0.028(5) 0.050(6) -0.034(4) C30 0.032(4) 0.032(4) 0.061(5) -0.013(3) 0.004(3) -0.006(3) C31 0.071(5) 0.070(6) 0.050(5) -0.009(4) 0.005(4) -0.006(4) C32 0.066(6) 0.077(7) 0.092(8) -0.014(6) 0.012(5) -0.033(5) C33 0.040(4) 0.095(7) 0.050(5) -0.028(5) -0.002(4) -0.004(4) C34 0.107(8) 0.126(10) 0.050(6) -0.025(6) 0.011(5) -0.036(7) C35 0.092(8) 0.121(10) 0.105(9) -0.075(8) -0.012(6) -0.024(7) C36 0.023(3) 0.030(3) 0.034(4) -0.005(3) 0.009(3) 0.004(2) C37 0.022(3) 0.042(4) 0.040(4) -0.014(3) 0.007(3) -0.005(3) C38 0.026(3) 0.056(5) 0.048(4) -0.019(4) 0.016(3) -0.005(3) C39 0.029(4) 0.066(5) 0.047(5) -0.026(4) 0.012(3) 0.006(3) C40 0.037(4) 0.045(4) 0.042(4) -0.020(3) -0.001(3) 0.001(3) C41 0.025(3) 0.038(4) 0.038(4) -0.013(3) -0.001(3) 0.006(3) C42 0.040(4) 0.029(4) 0.038(4) -0.009(3) 0.008(3) -0.001(3) C43 0.031(3) 0.035(4) 0.043(4) -0.016(3) 0.002(3) -0.011(3) C44 0.038(4) 0.043(4) 0.041(4) -0.012(3) 0.004(3) -0.012(3) C45 0.038(4) 0.042(4) 0.064(5) -0.011(4) -0.001(3) -0.005(3) C46 0.034(4) 0.054(5) 0.076(6) -0.013(4) 0.020(4) -0.009(3) C47 0.059(5) 0.056(5) 0.049(5) -0.008(4) 0.022(4) -0.013(4) C48 0.049(4) 0.035(4) 0.042(4) -0.012(3) 0.005(3) -0.008(3) C49 0.049(4) 0.052(5) 0.052(5) -0.008(4) 0.006(4) -0.022(4) C50 0.068(6) 0.149(11) 0.071(7) 0.041(7) -0.021(5) -0.026(6) C51 0.147(10) 0.085(8) 0.075(7) -0.028(6) 0.048(7) -0.060(7) C52 0.059(5) 0.057(5) 0.043(5) -0.002(4) 0.006(4) -0.003(4) C53 0.134(10) 0.081(8) 0.073(7) 0.016(6) -0.019(6) -0.005(7) C54 0.123(9) 0.096(9) 0.072(7) -0.027(6) -0.024(6) -0.011(7) C55 0.020(3) 0.042(4) 0.050(4) -0.009(3) 0.011(3) -0.003(3) C56 0.013(3) 0.055(4) 0.049(4) -0.017(4) 0.013(3) -0.007(3) C57 0.021(3) 0.072(5) 0.051(5) -0.025(4) 0.010(3) 0.001(3) C58 0.020(3) 0.100(7) 0.057(5) -0.031(5) 0.005(3) 0.007(4) C59 0.017(4) 0.114(8) 0.073(6) -0.050(6) 0.011(4) -0.014(4) C60 0.038(4) 0.066(6) 0.096(7) -0.046(5) 0.021(5) -0.016(4) C61 0.019(3) 0.070(5) 0.066(5) -0.028(4) 0.018(3) -0.014(3) C62 0.022(4) 0.102(7) 0.058(5) 0.002(5) -0.003(3) 0.012(4) C63 0.083(7) 0.077(7) 0.115(9) -0.012(6) 0.019(6) 0.014(5) C64 0.064(6) 0.174(12) 0.067(7) 0.007(8) 0.001(5) 0.002(7) C65 0.029(4) 0.064(6) 0.099(7) -0.009(5) 0.014(4) -0.015(4) C66 0.118(9) 0.048(7) 0.187(14) -0.004(8) 0.014(9) -0.022(6) C67 0.052(5) 0.119(9) 0.102(9) 0.023(7) 0.019(5) 0.005(5) C68 0.036(4) 0.066(5) 0.053(5) 0.013(4) 0.015(3) -0.004(3) C69 0.109(8) 0.059(6) 0.086(7) 0.013(5) 0.042(6) 0.009(5) C70 0.063(5) 0.083(7) 0.054(5) -0.003(5) 0.009(4) -0.003(5) N1 0.022(2) 0.027(3) 0.029(3) -0.005(2) 0.006(2) -0.0007(19) N2 0.020(3) 0.044(3) 0.041(3) -0.014(3) 0.004(2) -0.007(2) N3 0.056(4) 0.071(5) 0.047(4) 0.007(4) 0.005(3) 0.035(3) N4 0.038(3) 0.047(4) 0.045(4) -0.020(3) 0.004(3) -0.011(3) O1 0.025(2) 0.048(3) 0.041(3) 0.004(2) 0.012(2) 0.0106(19) O2 0.028(2) 0.056(3) 0.044(3) -0.020(2) 0.0054(19) -0.008(2) O3 0.027(2) 0.046(3) 0.044(3) -0.020(2) 0.0098(19) -0.0108(19) O4 0.026(2) 0.049(3) 0.045(3) 0.003(2) 0.0076(19) -0.0009(19) Cl1 0.0667(13) 0.0887(17) 0.0726(16) 0.0358(13) 0.0347(11) 0.0143(12) Cl2 0.0529(12) 0.140(2) 0.0779(17) -0.0707(17) 0.0254(11) -0.0098(13) Zr1 0.0169(3) 0.0407(4) 0.0354(4) -0.0094(3) 0.0060(2) -0.0023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.309(7) . ? C1 C6 1.400(9) . ? C1 C2 1.416(8) . ? C2 C3 1.397(9) . ? C2 C20 1.434(8) . ? C3 C4 1.344(9) . ? C3 H3 0.9300 . ? C4 C5 1.393(9) . ? C4 Cl1 1.756(7) . ? C5 C6 1.373(10) . ? C5 H5 0.9300 . ? C6 C7 1.482(9) . ? C7 N3 1.260(9) . ? C7 H7 0.9300 . ? C8 C9 1.391(11) . ? C8 C13 1.413(12) . ? C8 N3 1.435(10) . ? C9 C10 1.410(13) . ? C9 C14 1.552(14) . ? C10 C11 1.339(15) . ? C10 H10 0.9300 . ? C11 C12 1.368(16) . ? C11 H11 0.9300 . ? C12 C13 1.375(13) . ? C12 H12 0.9300 . ? C13 C17 1.521(13) . ? C14 C16 1.40(2) . ? C14 C15 1.54(2) . ? C14 H14 0.9800 . ? C15 H15A 0.9651 . ? C15 H15B 0.9653 . ? C15 H15C 0.9647 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C19 1.486(15) . ? C17 C18 1.490(15) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N1 1.297(8) . ? C20 H20 0.9300 . ? C21 C26 1.396(8) . ? C21 C22 1.399(8) . ? C21 N1 1.454(7) . ? C22 C23 1.386(9) . ? C22 C27 1.532(9) . ? C23 C24 1.376(10) . ? C23 H23 0.9300 . ? C24 C25 1.369(10) . ? C24 H24 0.9300 . ? C25 C26 1.399(9) . ? C25 H25 0.9300 . ? C26 C30 1.502(9) . ? C27 C29 1.504(10) . ? C27 C28 1.509(9) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C32 1.541(10) . ? C30 C31 1.543(10) . ? C30 H30 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O2 1.414(8) . ? C33 C34 1.477(12) . ? C33 C35 1.510(13) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O3 1.301(7) . ? C36 C41 1.412(8) . ? C36 C37 1.420(8) . ? C37 C38 1.388(9) . ? C37 C55 1.441(8) . ? C38 C39 1.376(9) . ? C38 H38 0.9300 . ? C39 C40 1.377(9) . ? C39 Cl2 1.728(7) . ? C40 C41 1.386(9) . ? C40 H40 0.9300 . ? C41 C42 1.482(9) . ? C42 N4 1.274(8) . ? C42 H42 0.9300 . ? C43 C48 1.402(10) . ? C43 C44 1.413(9) . ? C43 N4 1.429(8) . ? C44 C45 1.385(9) . ? C44 C49 1.489(10) . ? C45 C46 1.375(11) . ? C45 H45 0.9300 . ? C46 C47 1.378(11) . ? C46 H46 0.9300 . ? C47 C48 1.394(10) . ? C47 H47 0.9300 . ? C48 C52 1.501(10) . ? C49 C51 1.527(12) . ? C49 C50 1.570(12) . ? C49 H49 0.9800 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.477(12) . ? C52 C54 1.496(11) . ? C52 H52 0.9800 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N2 1.296(8) . ? C55 H55 0.9300 . ? C56 C57 1.393(10) . ? C56 C61 1.420(10) . ? C56 N2 1.457(7) . ? C57 C58 1.396(10) . ? C57 C62 1.500(12) . ? C58 C59 1.370(12) . ? C58 H58 0.9300 . ? C59 C60 1.359(13) . ? C59 H59 0.9300 . ? C60 C61 1.419(10) . ? C60 H60 0.9300 . ? C61 C65 1.498(11) . ? C62 C64 1.498(12) . ? C62 C63 1.573(12) . ? C62 H62 0.9800 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C67 1.506(12) . ? C65 C66 1.563(12) . ? C65 H65 0.9800 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 O4 1.406(8) . ? C68 C69 1.514(11) . ? C68 C70 1.522(11) . ? C68 H68 0.9800 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? N1 Zr1 2.376(5) . ? N2 Zr1 2.382(5) . ? O1 Zr1 2.110(4) . ? O2 Zr1 1.920(4) . ? O3 Zr1 2.093(4) . ? O4 Zr1 1.933(5) . ? 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 C6 120.6(5) . . ? O1 C1 C2 121.0(6) . . ? C6 C1 C2 118.3(6) . . ? C3 C2 C1 119.8(6) . . ? C3 C2 C20 116.5(5) . . ? C1 C2 C20 123.6(6) . . ? C4 C3 C2 120.6(6) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.5(6) . . ? C3 C4 Cl1 119.7(5) . . ? C5 C4 Cl1 119.8(6) . . ? C6 C5 C4 120.6(7) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 120.1(6) . . ? C5 C6 C7 120.7(6) . . ? C1 C6 C7 119.0(6) . . ? N3 C7 C6 122.2(7) . . ? N3 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C9 C8 C13 119.7(8) . . ? C9 C8 N3 118.2(8) . . ? C13 C8 N3 122.1(7) . . ? C8 C9 C10 118.2(9) . . ? C8 C9 C14 120.0(8) . . ? C10 C9 C14 121.7(8) . . ? C11 C10 C9 121.2(10) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 120.9(10) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 120.8(10) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C8 119.1(9) . . ? C12 C13 C17 119.5(9) . . ? C8 C13 C17 121.3(8) . . ? C16 C14 C15 113.8(17) . . ? C16 C14 C9 113.9(14) . . ? C15 C14 C9 110.5(13) . . ? C16 C14 H14 106.2 . . ? C15 C14 H14 105.6 . . ? C9 C14 H14 106.2 . . ? C14 C15 H15A 110.1 . . ? C14 C15 H15B 110.4 . . ? H15A C15 H15B 109.0 . . ? C14 C15 H15C 109.4 . . ? H15A C15 H15C 109.0 . . ? H15B C15 H15C 108.9 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.4 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 110.4(10) . . ? C19 C17 C13 112.4(10) . . ? C18 C17 C13 111.9(10) . . ? C19 C17 H17 107.3 . . ? C18 C17 H17 107.2 . . ? C13 C17 H17 107.3 . . ? C17 C18 H18A 109.4 . . ? 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 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 C2 128.2(5) . . ? N1 C20 H20 115.9 . . ? C2 C20 H20 115.9 . . ? C26 C21 C22 122.2(6) . . ? C26 C21 N1 119.0(5) . . ? C22 C21 N1 118.8(5) . . ? C23 C22 C21 117.4(6) . . ? C23 C22 C27 120.2(6) . . ? C21 C22 C27 122.4(5) . . ? C24 C23 C22 121.7(7) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.1 . . ? C25 C24 C23 119.8(7) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 121.4(7) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C21 C26 C25 117.3(6) . . ? C21 C26 C30 122.7(6) . . ? C25 C26 C30 119.9(6) . . ? C29 C27 C28 111.5(6) . . ? C29 C27 C22 111.0(6) . . ? C28 C27 C22 112.4(6) . . ? C29 C27 H27 107.2 . . ? C28 C27 H27 107.2 . . ? C22 C27 H27 107.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 C32 112.2(6) . . ? C26 C30 C31 109.7(5) . . ? C32 C30 C31 109.8(6) . . ? C26 C30 H30 108.3 . . ? C32 C30 H30 108.4 . . ? C31 C30 H30 108.3 . . ? 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 . . ? O2 C33 C34 110.6(7) . . ? O2 C33 C35 110.5(8) . . ? C34 C33 C35 113.7(8) . . ? O2 C33 H33 107.2 . . ? C34 C33 H33 107.2 . . ? C35 C33 H33 107.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.4 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.4 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O3 C36 C41 120.1(5) . . ? O3 C36 C37 121.8(5) . . ? C41 C36 C37 118.1(5) . . ? C38 C37 C36 120.3(5) . . ? C38 C37 C55 117.1(5) . . ? C36 C37 C55 122.5(6) . . ? C39 C38 C37 120.4(6) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 120.2(6) . . ? C38 C39 Cl2 119.5(5) . . ? C40 C39 Cl2 120.3(5) . . ? C39 C40 C41 121.2(6) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C36 119.8(6) . . ? C40 C41 C42 120.4(6) . . ? C36 C41 C42 119.8(5) . . ? N4 C42 C41 122.4(6) . . ? N4 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? C48 C43 C44 122.2(6) . . ? C48 C43 N4 121.6(6) . . ? C44 C43 N4 116.1(6) . . ? C45 C44 C43 117.4(7) . . ? C45 C44 C49 122.7(6) . . ? C43 C44 C49 119.9(6) . . ? C46 C45 C44 122.0(7) . . ? C46 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? C45 C46 C47 119.1(7) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C46 C47 C48 122.8(7) . . ? C46 C47 H47 118.6 . . ? C48 C47 H47 118.6 . . ? C47 C48 C43 116.5(6) . . ? C47 C48 C52 120.5(7) . . ? C43 C48 C52 123.0(6) . . ? C44 C49 C51 112.2(7) . . ? C44 C49 C50 113.2(7) . . ? C51 C49 C50 109.8(8) . . ? C44 C49 H49 107.1 . . ? C51 C49 H49 107.1 . . ? C50 C49 H49 107.1 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C54 109.6(8) . . ? C53 C52 C48 114.0(7) . . ? C54 C52 C48 112.8(7) . . ? C53 C52 H52 106.7 . . ? C54 C52 H52 106.6 . . ? C48 C52 H52 106.6 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N2 C55 C37 128.5(5) . . ? N2 C55 H55 115.8 . . ? C37 C55 H55 115.8 . . ? C57 C56 C61 122.4(6) . . ? C57 C56 N2 119.5(6) . . ? C61 C56 N2 118.1(6) . . ? C56 C57 C58 117.9(8) . . ? C56 C57 C62 122.4(6) . . ? C58 C57 C62 119.6(8) . . ? C59 C58 C57 121.0(8) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C60 C59 C58 121.1(7) . . ? C60 C59 H59 119.5 . . ? C58 C59 H59 119.5 . . ? C59 C60 C61 121.5(9) . . ? C59 C60 H60 119.2 . . ? C61 C60 H60 119.3 . . ? C60 C61 C56 116.1(8) . . ? C60 C61 C65 121.7(8) . . ? C56 C61 C65 122.2(6) . . ? C64 C62 C57 115.7(8) . . ? C64 C62 C63 108.4(8) . . ? C57 C62 C63 111.8(7) . . ? C64 C62 H62 106.8 . . ? C57 C62 H62 106.8 . . ? C63 C62 H62 106.8 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C61 C65 C67 110.3(7) . . ? C61 C65 C66 114.0(8) . . ? C67 C65 C66 110.3(9) . . ? C61 C65 H65 107.3 . . ? C67 C65 H65 107.3 . . ? C66 C65 H65 107.3 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.4 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O4 C68 C69 110.6(7) . . ? O4 C68 C70 108.3(6) . . ? C69 C68 C70 112.7(7) . . ? O4 C68 H68 108.4 . . ? C69 C68 H68 108.4 . . ? C70 C68 H68 108.4 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.4 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C20 N1 C21 113.4(5) . . ? C20 N1 Zr1 127.4(4) . . ? C21 N1 Zr1 119.1(4) . . ? C55 N2 C56 113.4(5) . . ? C55 N2 Zr1 125.9(4) . . ? C56 N2 Zr1 120.6(4) . . ? C7 N3 C8 118.9(7) . . ? C42 N4 C43 118.2(5) . . ? C1 O1 Zr1 142.3(4) . . ? C33 O2 Zr1 156.2(5) . . ? C36 O3 Zr1 140.7(4) . . ? C68 O4 Zr1 161.3(4) . . ? O2 Zr1 O4 102.2(2) . . ? O2 Zr1 O3 158.97(18) . . ? O4 Zr1 O3 91.88(19) . . ? O2 Zr1 O1 90.70(19) . . ? O4 Zr1 O1 160.43(16) . . ? O3 Zr1 O1 80.28(18) . . ? O2 Zr1 N1 98.66(17) . . ? O4 Zr1 N1 86.29(17) . . ? O3 Zr1 N1 97.78(16) . . ? O1 Zr1 N1 77.14(16) . . ? O2 Zr1 N2 86.29(17) . . ? O4 Zr1 N2 93.30(18) . . ? O3 Zr1 N2 77.25(16) . . ? O1 Zr1 N2 102.29(17) . . ? N1 Zr1 N2 175.01(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 178.9(6) . . . . ? C6 C1 C2 C3 -1.6(9) . . . . ? O1 C1 C2 C20 -4.9(9) . . . . ? C6 C1 C2 C20 174.6(6) . . . . ? C1 C2 C3 C4 0.0(10) . . . . ? C20 C2 C3 C4 -176.4(6) . . . . ? C2 C3 C4 C5 1.8(10) . . . . ? C2 C3 C4 Cl1 179.4(5) . . . . ? C3 C4 C5 C6 -2.1(11) . . . . ? Cl1 C4 C5 C6 -179.7(5) . . . . ? C4 C5 C6 C1 0.4(10) . . . . ? C4 C5 C6 C7 176.0(6) . . . . ? O1 C1 C6 C5 -179.1(6) . . . . ? C2 C1 C6 C5 1.3(9) . . . . ? O1 C1 C6 C7 5.3(9) . . . . ? C2 C1 C6 C7 -174.3(6) . . . . ? C5 C6 C7 N3 -0.5(11) . . . . ? C1 C6 C7 N3 175.0(7) . . . . ? C13 C8 C9 C10 -1.5(19) . . . . ? N3 C8 C9 C10 -179.5(12) . . . . ? C13 C8 C9 C14 176.2(12) . . . . ? N3 C8 C9 C14 -1.9(18) . . . . ? C8 C9 C10 C11 -2(2) . . . . ? C14 C9 C10 C11 179.9(16) . . . . ? C9 C10 C11 C12 4(3) . . . . ? C10 C11 C12 C13 -2(3) . . . . ? C11 C12 C13 C8 -2(2) . . . . ? C11 C12 C13 C17 176.7(13) . . . . ? C9 C8 C13 C12 3.6(17) . . . . ? N3 C8 C13 C12 -178.5(11) . . . . ? C9 C8 C13 C17 -174.8(11) . . . . ? N3 C8 C13 C17 3.1(16) . . . . ? C8 C9 C14 C16 123.0(18) . . . . ? C10 C9 C14 C16 -59(2) . . . . ? C8 C9 C14 C15 -107.6(17) . . . . ? C10 C9 C14 C15 70(2) . . . . ? C12 C13 C17 C19 65.5(15) . . . . ? C8 C13 C17 C19 -116.2(12) . . . . ? C12 C13 C17 C18 -59.5(15) . . . . ? C8 C13 C17 C18 118.9(11) . . . . ? C3 C2 C20 N1 177.8(6) . . . . ? C1 C2 C20 N1 1.5(10) . . . . ? C26 C21 C22 C23 -0.4(9) . . . . ? N1 C21 C22 C23 179.8(5) . . . . ? C26 C21 C22 C27 178.7(5) . . . . ? N1 C21 C22 C27 -1.1(8) . . . . ? C21 C22 C23 C24 0.9(10) . . . . ? C27 C22 C23 C24 -178.3(6) . . . . ? C22 C23 C24 C25 -0.7(11) . . . . ? C23 C24 C25 C26 0.2(11) . . . . ? C22 C21 C26 C25 -0.1(9) . . . . ? N1 C21 C26 C25 179.7(5) . . . . ? C22 C21 C26 C30 -177.5(6) . . . . ? N1 C21 C26 C30 2.2(9) . . . . ? C24 C25 C26 C21 0.2(10) . . . . ? C24 C25 C26 C30 177.8(6) . . . . ? C23 C22 C27 C29 78.2(8) . . . . ? C21 C22 C27 C29 -100.9(7) . . . . ? C23 C22 C27 C28 -47.5(8) . . . . ? C21 C22 C27 C28 133.4(7) . . . . ? C21 C26 C30 C32 -134.1(7) . . . . ? C25 C26 C30 C32 48.5(9) . . . . ? C21 C26 C30 C31 103.6(7) . . . . ? C25 C26 C30 C31 -73.8(8) . . . . ? O3 C36 C37 C38 179.1(6) . . . . ? C41 C36 C37 C38 -3.0(10) . . . . ? O3 C36 C37 C55 -6.0(10) . . . . ? C41 C36 C37 C55 171.9(6) . . . . ? C36 C37 C38 C39 0.3(11) . . . . ? C55 C37 C38 C39 -174.9(7) . . . . ? C37 C38 C39 C40 1.7(12) . . . . ? C37 C38 C39 Cl2 -177.0(6) . . . . ? C38 C39 C40 C41 -1.0(12) . . . . ? Cl2 C39 C40 C41 177.7(6) . . . . ? C39 C40 C41 C36 -1.8(11) . . . . ? C39 C40 C41 C42 -179.6(7) . . . . ? O3 C36 C41 C40 -178.3(6) . . . . ? C37 C36 C41 C40 3.7(9) . . . . ? O3 C36 C41 C42 -0.5(9) . . . . ? C37 C36 C41 C42 -178.5(6) . . . . ? C40 C41 C42 N4 -6.9(10) . . . . ? C36 C41 C42 N4 175.3(6) . . . . ? C48 C43 C44 C45 -1.0(10) . . . . ? N4 C43 C44 C45 -179.0(6) . . . . ? C48 C43 C44 C49 178.5(6) . . . . ? N4 C43 C44 C49 0.5(9) . . . . ? C43 C44 C45 C46 0.0(10) . . . . ? C49 C44 C45 C46 -179.5(7) . . . . ? C44 C45 C46 C47 0.6(11) . . . . ? C45 C46 C47 C48 -0.3(12) . . . . ? C46 C47 C48 C43 -0.7(10) . . . . ? C46 C47 C48 C52 177.8(7) . . . . ? C44 C43 C48 C47 1.3(10) . . . . ? N4 C43 C48 C47 179.2(6) . . . . ? C44 C43 C48 C52 -177.2(6) . . . . ? N4 C43 C48 C52 0.7(10) . . . . ? C45 C44 C49 C51 96.2(9) . . . . ? C43 C44 C49 C51 -83.3(9) . . . . ? C45 C44 C49 C50 -28.8(10) . . . . ? C43 C44 C49 C50 151.7(7) . . . . ? C47 C48 C52 C53 -52.6(10) . . . . ? C43 C48 C52 C53 125.9(9) . . . . ? C47 C48 C52 C54 73.3(10) . . . . ? C43 C48 C52 C54 -108.3(9) . . . . ? C38 C37 C55 N2 -177.7(7) . . . . ? C36 C37 C55 N2 7.2(11) . . . . ? C61 C56 C57 C58 -0.8(10) . . . . ? N2 C56 C57 C58 178.6(6) . . . . ? C61 C56 C57 C62 -179.5(6) . . . . ? N2 C56 C57 C62 -0.2(10) . . . . ? C56 C57 C58 C59 1.0(10) . . . . ? C62 C57 C58 C59 179.8(7) . . . . ? C57 C58 C59 C60 -0.6(12) . . . . ? C58 C59 C60 C61 -0.2(12) . . . . ? C59 C60 C61 C56 0.5(11) . . . . ? C59 C60 C61 C65 179.7(7) . . . . ? C57 C56 C61 C60 0.0(10) . . . . ? N2 C56 C61 C60 -179.3(6) . . . . ? C57 C56 C61 C65 -179.2(7) . . . . ? N2 C56 C61 C65 1.5(10) . . . . ? C56 C57 C62 C64 139.1(7) . . . . ? C58 C57 C62 C64 -39.6(10) . . . . ? C56 C57 C62 C63 -96.2(8) . . . . ? C58 C57 C62 C63 85.1(9) . . . . ? C60 C61 C65 C67 -88.1(9) . . . . ? C56 C61 C65 C67 91.1(8) . . . . ? C60 C61 C65 C66 36.6(11) . . . . ? C56 C61 C65 C66 -144.3(8) . . . . ? C2 C20 N1 C21 -176.4(6) . . . . ? C2 C20 N1 Zr1 4.9(9) . . . . ? C26 C21 N1 C20 -93.4(6) . . . . ? C22 C21 N1 C20 86.4(7) . . . . ? C26 C21 N1 Zr1 85.5(6) . . . . ? C22 C21 N1 Zr1 -94.8(5) . . . . ? C37 C55 N2 C56 -174.6(7) . . . . ? C37 C55 N2 Zr1 7.3(11) . . . . ? C57 C56 N2 C55 85.5(8) . . . . ? C61 C56 N2 C55 -95.2(7) . . . . ? C57 C56 N2 Zr1 -96.4(6) . . . . ? C61 C56 N2 Zr1 83.0(7) . . . . ? C6 C7 N3 C8 -173.4(7) . . . . ? C9 C8 N3 C7 -118.3(10) . . . . ? C13 C8 N3 C7 63.8(13) . . . . ? C41 C42 N4 C43 176.3(6) . . . . ? C48 C43 N4 C42 71.1(9) . . . . ? C44 C43 N4 C42 -110.9(7) . . . . ? C6 C1 O1 Zr1 -178.3(5) . . . . ? C2 C1 O1 Zr1 1.3(10) . . . . ? C34 C33 O2 Zr1 52.9(14) . . . . ? C35 C33 O2 Zr1 179.7(8) . . . . ? C41 C36 O3 Zr1 167.9(5) . . . . ? C37 C36 O3 Zr1 -14.2(10) . . . . ? C69 C68 O4 Zr1 -164.7(10) . . . . ? C70 C68 O4 Zr1 71.4(14) . . . . ? C33 O2 Zr1 O4 165.0(11) . . . . ? C33 O2 Zr1 O3 34.1(13) . . . . ? C33 O2 Zr1 O1 -29.9(11) . . . . ? C33 O2 Zr1 N1 -107.0(11) . . . . ? C33 O2 Zr1 N2 72.4(11) . . . . ? C68 O4 Zr1 O2 166.8(13) . . . . ? C68 O4 Zr1 O3 -28.9(13) . . . . ? C68 O4 Zr1 O1 36.7(16) . . . . ? C68 O4 Zr1 N1 68.7(13) . . . . ? C68 O4 Zr1 N2 -106.3(13) . . . . ? C36 O3 Zr1 O2 59.8(9) . . . . ? C36 O3 Zr1 O4 -72.5(7) . . . . ? C36 O3 Zr1 O1 125.6(7) . . . . ? C36 O3 Zr1 N1 -159.0(6) . . . . ? C36 O3 Zr1 N2 20.5(6) . . . . ? C1 O1 Zr1 O2 -95.8(6) . . . . ? C1 O1 Zr1 O4 35.8(10) . . . . ? C1 O1 Zr1 O3 103.3(7) . . . . ? C1 O1 Zr1 N1 3.0(6) . . . . ? C1 O1 Zr1 N2 177.9(6) . . . . ? C20 N1 Zr1 O2 83.1(5) . . . . ? C21 N1 Zr1 O2 -95.5(4) . . . . ? C20 N1 Zr1 O4 -175.1(5) . . . . ? C21 N1 Zr1 O4 6.2(4) . . . . ? C20 N1 Zr1 O3 -83.7(5) . . . . ? C21 N1 Zr1 O3 97.6(4) . . . . ? C20 N1 Zr1 O1 -5.6(5) . . . . ? C21 N1 Zr1 O1 175.7(4) . . . . ? C20 N1 Zr1 N2 -90(2) . . . . ? C21 N1 Zr1 N2 92(2) . . . . ? C55 N2 Zr1 O2 178.1(6) . . . . ? C56 N2 Zr1 O2 0.2(5) . . . . ? C55 N2 Zr1 O4 76.1(6) . . . . ? C56 N2 Zr1 O4 -101.8(5) . . . . ? C55 N2 Zr1 O3 -15.1(6) . . . . ? C56 N2 Zr1 O3 167.0(5) . . . . ? C55 N2 Zr1 O1 -92.0(6) . . . . ? C56 N2 Zr1 O1 90.1(5) . . . . ? C55 N2 Zr1 N1 -9(2) . . . . ? C56 N2 Zr1 N1 173.0(19) . . . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.524 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.141 # Attachment '6424_web_deposit_cif_file_2_tanmoykumarsaha_1311514612.new.cif' data_new2 _database_code_depnum_ccdc_archive 'CCDC 836426' #TrackingRef '6424_web_deposit_cif_file_2_tanmoykumarsaha_1311514612.new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C79 H104 N4 O6 Ti' _chemical_formula_sum 'C79 H104 N4 O6 Ti' _chemical_formula_weight 1253.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc ' 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 12.0283(3) _cell_length_b 28.2315(9) _cell_length_c 21.6400(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.2510(10) _cell_angle_gamma 90.00 _cell_volume 7272.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8543 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.23 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9426 _exptl_absorpt_correction_T_max 0.9585 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56295 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.46 _reflns_number_total 17605 _reflns_number_gt 9768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEXII (Bruker, 2004)' _computing_cell_refinement 'APEXII/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) ' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^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_number_reflns 17605 _refine_ls_number_parameters 834 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 0.22718(18) 0.88492(8) 0.84177(12) 0.0192(5) Uani 1 1 d . . . C2 C 0.12357(19) 0.86653(8) 0.85518(12) 0.0205(5) Uani 1 1 d . . . C3 C 0.0539(2) 0.89410(9) 0.88749(13) 0.0261(6) Uani 1 1 d . . . H3 H -0.0146 0.8812 0.8970 0.031 Uiso 1 1 calc R . . C4 C 0.0836(2) 0.93956(9) 0.90554(13) 0.0278(6) Uani 1 1 d . . . C5 C 0.18074(19) 0.95892(9) 0.88838(12) 0.0243(6) Uani 1 1 d . . . H5 H 0.1990 0.9909 0.8990 0.029 Uiso 1 1 calc R . . C6 C 0.25163(18) 0.93304(8) 0.85637(12) 0.0194(5) Uani 1 1 d . . . C7 C 0.34905(19) 0.95549(8) 0.83510(12) 0.0221(5) Uani 1 1 d . . . H7 H 0.3977 0.9365 0.8145 0.027 Uiso 1 1 calc R . . C8 C 0.46648(19) 1.01703(8) 0.81749(13) 0.0229(6) Uani 1 1 d . . . C9 C 0.5582(2) 1.03331(9) 0.85976(14) 0.0273(6) Uani 1 1 d . . . C10 C 0.6524(2) 1.04938(9) 0.83580(16) 0.0360(7) Uani 1 1 d . . . H10 H 0.7164 1.0595 0.8636 0.043 Uiso 1 1 calc R . . C11 C 0.6547(2) 1.05089(9) 0.77267(17) 0.0379(8) Uani 1 1 d . . . H11 H 0.7206 1.0613 0.7572 0.045 Uiso 1 1 calc R . . C12 C 0.5617(2) 1.03739(9) 0.73143(15) 0.0342(7) Uani 1 1 d . . . H12 H 0.5636 1.0397 0.6878 0.041 Uiso 1 1 calc R . . C13 C 0.4652(2) 1.02038(8) 0.75256(14) 0.0267(6) Uani 1 1 d . . . C14 C 0.08308(19) 0.82050(8) 0.83415(12) 0.0213(5) Uani 1 1 d . . . H14 H 0.0131 0.8113 0.8459 0.026 Uiso 1 1 calc R . . C15 C 0.06036(19) 0.74869(8) 0.78281(13) 0.0216(6) Uani 1 1 d . . . C16 C -0.01929(19) 0.75136(8) 0.72910(13) 0.0236(6) Uani 1 1 d . . . C17 C -0.0833(2) 0.71110(9) 0.71210(14) 0.0312(6) Uani 1 1 d . . . H17 H -0.1375 0.7118 0.6756 0.037 Uiso 1 1 calc R . . C18 C -0.0695(2) 0.67027(9) 0.74737(15) 0.0342(7) Uani 1 1 d . . . H18 H -0.1136 0.6431 0.7348 0.041 Uiso 1 1 calc R . . C19 C 0.0070(2) 0.66874(9) 0.80003(15) 0.0326(7) Uani 1 1 d . . . H19 H 0.0142 0.6406 0.8243 0.039 Uiso 1 1 calc R . . C20 C 0.0752(2) 0.70745(8) 0.81948(13) 0.0253(6) Uani 1 1 d . . . C21 C -0.0897(2) 0.95647(11) 0.94199(16) 0.0423(8) Uani 1 1 d . . . H21A H -0.1310 0.9559 0.8995 0.063 Uiso 1 1 calc R . . H21B H -0.1233 0.9800 0.9670 0.063 Uiso 1 1 calc R . . H21C H -0.0933 0.9251 0.9611 0.063 Uiso 1 1 calc R . . C22 C 0.5499(2) 1.03489(11) 0.92853(14) 0.0377(7) Uani 1 1 d . . . H22 H 0.4980 1.0087 0.9367 0.045 Uiso 1 1 calc R . . C23 C 0.4941(4) 1.08043(15) 0.9439(2) 0.0940(16) Uani 1 1 d . . . H23A H 0.5417 1.1073 0.9362 0.141 Uiso 1 1 calc R . . H23B H 0.4834 1.0802 0.9880 0.141 Uiso 1 1 calc R . . H23C H 0.4210 1.0833 0.9176 0.141 Uiso 1 1 calc R . . C24 C 0.6591(3) 1.02605(18) 0.97050(19) 0.0827(14) Uani 1 1 d . . . H24A H 0.6940 0.9971 0.9571 0.124 Uiso 1 1 calc R . . H24B H 0.6446 1.0223 1.0137 0.124 Uiso 1 1 calc R . . H24C H 0.7098 1.0530 0.9680 0.124 Uiso 1 1 calc R . . C25 C 0.3593(2) 1.00950(10) 0.70755(14) 0.0343(7) Uani 1 1 d . . . H25 H 0.3302 0.9782 0.7197 0.041 Uiso 1 1 calc R . . C26 C 0.2702(2) 1.04682(11) 0.71504(16) 0.0432(8) Uani 1 1 d . . . H26A H 0.2584 1.0483 0.7589 0.065 Uiso 1 1 calc R . . H26B H 0.1995 1.0383 0.6890 0.065 Uiso 1 1 calc R . . H26C H 0.2955 1.0778 0.7021 0.065 Uiso 1 1 calc R . . C27 C 0.3764(3) 1.00621(12) 0.63944(15) 0.0532(9) Uani 1 1 d . . . H27A H 0.3997 1.0371 0.6253 0.080 Uiso 1 1 calc R . . H27B H 0.3058 0.9967 0.6141 0.080 Uiso 1 1 calc R . . H27C H 0.4346 0.9827 0.6350 0.080 Uiso 1 1 calc R . . C28 C -0.0382(2) 0.79617(9) 0.69004(13) 0.0258(6) Uani 1 1 d . . . H28 H 0.0301 0.8165 0.7004 0.031 Uiso 1 1 calc R . . C29 C -0.0535(3) 0.78704(11) 0.62049(15) 0.0467(8) Uani 1 1 d . . . H29A H 0.0096 0.7681 0.6101 0.070 Uiso 1 1 calc R . . H29B H -0.0561 0.8173 0.5981 0.070 Uiso 1 1 calc R . . H29C H -0.1239 0.7698 0.6081 0.070 Uiso 1 1 calc R . . C30 C -0.1380(3) 0.82415(11) 0.70693(17) 0.0506(9) Uani 1 1 d . . . H30A H -0.2057 0.8044 0.6998 0.076 Uiso 1 1 calc R . . H30B H -0.1491 0.8526 0.6808 0.076 Uiso 1 1 calc R . . H30C H -0.1234 0.8334 0.7510 0.076 Uiso 1 1 calc R . . C31 C 0.1590(2) 0.70471(9) 0.87864(14) 0.0345(7) Uani 1 1 d . . . H31 H 0.2125 0.7318 0.8779 0.041 Uiso 1 1 calc R . . C32 C 0.2276(4) 0.65937(13) 0.8826(2) 0.0846(15) Uani 1 1 d . . . H32A H 0.1771 0.6320 0.8810 0.127 Uiso 1 1 calc R . . H32B H 0.2793 0.6589 0.9220 0.127 Uiso 1 1 calc R . . H32C H 0.2706 0.6580 0.8475 0.127 Uiso 1 1 calc R . . C33 C 0.1010(3) 0.71068(17) 0.93585(18) 0.0807(14) Uani 1 1 d . . . H33A H 0.0616 0.7411 0.9336 0.121 Uiso 1 1 calc R . . H33B H 0.1571 0.7098 0.9735 0.121 Uiso 1 1 calc R . . H33C H 0.0469 0.6849 0.9375 0.121 Uiso 1 1 calc R . . C34 C 0.28367(18) 0.85687(8) 0.65320(12) 0.0194(5) Uani 1 1 d . . . C35 C 0.39767(19) 0.85043(8) 0.64421(12) 0.0210(5) Uani 1 1 d . . . C36 C 0.4361(2) 0.86922(9) 0.59115(13) 0.0271(6) Uani 1 1 d . . . H36 H 0.5115 0.8635 0.5847 0.033 Uiso 1 1 calc R . . C37 C 0.3673(2) 0.89570(9) 0.54825(13) 0.0277(6) Uani 1 1 d . . . C38 C 0.2572(2) 0.90366(9) 0.55732(13) 0.0260(6) Uani 1 1 d . . . H38 H 0.2094 0.9219 0.5277 0.031 Uiso 1 1 calc R . . C39 C 0.21528(19) 0.88530(8) 0.60918(12) 0.0205(5) Uani 1 1 d . . . C40 C 0.09829(19) 0.89515(8) 0.61754(13) 0.0222(5) Uani 1 1 d . . . H40 H 0.0705 0.8827 0.6532 0.027 Uiso 1 1 calc R . . C41 C -0.08077(19) 0.92654(9) 0.58881(12) 0.0234(6) Uani 1 1 d . . . C42 C -0.1646(2) 0.90524(9) 0.54501(13) 0.0279(6) Uani 1 1 d . . . C43 C -0.2764(2) 0.91184(10) 0.55309(14) 0.0348(7) Uani 1 1 d . . . H43 H -0.3342 0.8977 0.5245 0.042 Uiso 1 1 calc R . . C44 C -0.3044(2) 0.93843(9) 0.60168(15) 0.0335(7) Uani 1 1 d . . . H44 H -0.3810 0.9418 0.6071 0.040 Uiso 1 1 calc R . . C45 C -0.2219(2) 0.96015(9) 0.64241(14) 0.0301(6) Uani 1 1 d . . . H45 H -0.2427 0.9790 0.6753 0.036 Uiso 1 1 calc R . . C46 C -0.1088(2) 0.95531(8) 0.63680(13) 0.0239(6) Uani 1 1 d . . . C47 C 0.48013(19) 0.82779(8) 0.68984(12) 0.0218(6) Uani 1 1 d . . . H47 H 0.5544 0.8266 0.6798 0.026 Uiso 1 1 calc R . . C48 C 0.57094(18) 0.79389(8) 0.77963(12) 0.0210(5) Uani 1 1 d . . . C49 C 0.63436(19) 0.82744(8) 0.81754(12) 0.0208(5) Uani 1 1 d . . . C50 C 0.73524(19) 0.81273(9) 0.85162(13) 0.0260(6) Uani 1 1 d . . . H50 H 0.7793 0.8348 0.8777 0.031 Uiso 1 1 calc R . . C51 C 0.7728(2) 0.76677(9) 0.84846(13) 0.0305(6) Uani 1 1 d . . . H51 H 0.8420 0.7575 0.8722 0.037 Uiso 1 1 calc R . . C52 C 0.7099(2) 0.73456(9) 0.81107(14) 0.0307(7) Uani 1 1 d . . . H52 H 0.7369 0.7030 0.8090 0.037 Uiso 1 1 calc R . . C53 C 0.60749(19) 0.74680(8) 0.77592(14) 0.0265(6) Uani 1 1 d . . . C54 C 0.3585(3) 0.94997(11) 0.46338(15) 0.0446(8) Uani 1 1 d . . . H54A H 0.2886 0.9379 0.4398 0.067 Uiso 1 1 calc R . . H54B H 0.4066 0.9626 0.4344 0.067 Uiso 1 1 calc R . . H54C H 0.3412 0.9752 0.4917 0.067 Uiso 1 1 calc R . . C55 C -0.1323(3) 0.87840(11) 0.49019(15) 0.0432(8) Uani 1 1 d . . . H55 H -0.0604 0.8614 0.5049 0.052 Uiso 1 1 calc R . . C56 C -0.2183(3) 0.84124(16) 0.4638(2) 0.0852(15) Uani 1 1 d . . . H56A H -0.2348 0.8204 0.4975 0.128 Uiso 1 1 calc R . . H56B H -0.1879 0.8225 0.4320 0.128 Uiso 1 1 calc R . . H56C H -0.2875 0.8570 0.4449 0.128 Uiso 1 1 calc R . . C57 C -0.1086(4) 0.91379(16) 0.44043(18) 0.0808(14) Uani 1 1 d . . . H57A H -0.1771 0.9317 0.4257 0.121 Uiso 1 1 calc R . . H57B H -0.0841 0.8967 0.4053 0.121 Uiso 1 1 calc R . . H57C H -0.0494 0.9357 0.4583 0.121 Uiso 1 1 calc R . . C58 C -0.0222(2) 0.98228(9) 0.68099(14) 0.0315(6) Uani 1 1 d . . . H58 H 0.0512 0.9795 0.6647 0.038 Uiso 1 1 calc R . . C59 C -0.0514(3) 1.03476(10) 0.68240(18) 0.0476(9) Uani 1 1 d . . . H59A H -0.0633 1.0472 0.6397 0.071 Uiso 1 1 calc R . . H59B H 0.0105 1.0519 0.7071 0.071 Uiso 1 1 calc R . . H59C H -0.1201 1.0389 0.7013 0.071 Uiso 1 1 calc R . . C60 C -0.0065(4) 0.96195(13) 0.74596(17) 0.0672(11) Uani 1 1 d . . . H60A H -0.0777 0.9635 0.7629 0.101 Uiso 1 1 calc R . . H60B H 0.0507 0.9803 0.7727 0.101 Uiso 1 1 calc R . . H60C H 0.0178 0.9289 0.7446 0.101 Uiso 1 1 calc R . . C61 C 0.5977(2) 0.87880(8) 0.82013(13) 0.0250(6) Uani 1 1 d . . . H61 H 0.5168 0.8807 0.8015 0.030 Uiso 1 1 calc R . . C62 C 0.6084(2) 0.89791(10) 0.88659(14) 0.0380(7) Uani 1 1 d . . . H62A H 0.5611 0.8791 0.9107 0.057 Uiso 1 1 calc R . . H62B H 0.5840 0.9311 0.8856 0.057 Uiso 1 1 calc R . . H62C H 0.6869 0.8958 0.9062 0.057 Uiso 1 1 calc R . . C63 C 0.6649(3) 0.90959(9) 0.78074(16) 0.0443(8) Uani 1 1 d . . . H63A H 0.7448 0.9081 0.7979 0.066 Uiso 1 1 calc R . . H63B H 0.6388 0.9424 0.7814 0.066 Uiso 1 1 calc R . . H63C H 0.6543 0.8980 0.7376 0.066 Uiso 1 1 calc R . . C64 C 0.5406(2) 0.71032(9) 0.73486(16) 0.0426(8) Uani 1 1 d . . . H64 H 0.4628 0.7231 0.7232 0.051 Uiso 1 1 calc R . . C65 C 0.5314(4) 0.66412(13) 0.7708(3) 0.131(3) Uani 1 1 d . . . H65A H 0.6068 0.6516 0.7847 0.197 Uiso 1 1 calc R . . H65B H 0.4880 0.6410 0.7435 0.197 Uiso 1 1 calc R . . H65C H 0.4935 0.6702 0.8072 0.197 Uiso 1 1 calc R . . C66 C 0.5909(3) 0.7031(2) 0.6746(2) 0.120(2) Uani 1 1 d . . . H66A H 0.5974 0.7338 0.6543 0.180 Uiso 1 1 calc R . . H66B H 0.5421 0.6822 0.6466 0.180 Uiso 1 1 calc R . . H66C H 0.6655 0.6888 0.6844 0.180 Uiso 1 1 calc R . . C67 C 0.2198(2) 0.71862(9) 0.67495(13) 0.0283(6) Uani 1 1 d . . . H67 H 0.1375 0.7257 0.6692 0.034 Uiso 1 1 calc R . . C68 C 0.2360(3) 0.66625(10) 0.68766(18) 0.0578(10) Uani 1 1 d . . . H68A H 0.3160 0.6584 0.6908 0.087 Uiso 1 1 calc R . . H68B H 0.1937 0.6481 0.6534 0.087 Uiso 1 1 calc R . . H68C H 0.2089 0.6582 0.7269 0.087 Uiso 1 1 calc R . . C69 C 0.2659(3) 0.73365(12) 0.61686(16) 0.0494(9) Uani 1 1 d . . . H69A H 0.2540 0.7677 0.6103 0.074 Uiso 1 1 calc R . . H69B H 0.2273 0.7163 0.5808 0.074 Uiso 1 1 calc R . . H69C H 0.3466 0.7267 0.6216 0.074 Uiso 1 1 calc R . . C70 C 0.4364(2) 0.78127(11) 0.90415(14) 0.0377(7) Uani 1 1 d . . . H70 H 0.4906 0.8072 0.8984 0.045 Uiso 1 1 calc R . . C71 C 0.3620(3) 0.79821(12) 0.94988(15) 0.0514(9) Uani 1 1 d . . . H71A H 0.3171 0.8252 0.9320 0.077 Uiso 1 1 calc R . . H71B H 0.4085 0.8080 0.9887 0.077 Uiso 1 1 calc R . . H71C H 0.3119 0.7725 0.9587 0.077 Uiso 1 1 calc R . . C72 C 0.5031(3) 0.73850(16) 0.92875(19) 0.0779(13) Uani 1 1 d . . . H72A H 0.4518 0.7124 0.9343 0.117 Uiso 1 1 calc R . . H72B H 0.5479 0.7462 0.9690 0.117 Uiso 1 1 calc R . . H72C H 0.5532 0.7290 0.8990 0.117 Uiso 1 1 calc R . . C73 C 0.8221(4) 0.87955(16) 0.0867(2) 0.0748(12) Uani 1 1 d . . . H73 H 0.7811 0.8998 0.1103 0.090 Uiso 1 1 calc R . . C74 C 0.9342(4) 0.88677(17) 0.0891(2) 0.0769(12) Uani 1 1 d . . . C75 C 0.9941(5) 0.8573(2) 0.0524(2) 0.1041(18) Uani 1 1 d . . . H75 H 1.0721 0.8614 0.0513 0.125 Uiso 1 1 calc R . . C76 C 0.9303(6) 0.82052(19) 0.0168(2) 0.0956(19) Uani 1 1 d . . . H76 H 0.9662 0.7993 -0.0081 0.115 Uiso 1 1 calc R . . C77 C 0.8160(6) 0.8167(2) 0.0193(3) 0.111(2) Uani 1 1 d . . . H77 H 0.7748 0.7924 -0.0043 0.133 Uiso 1 1 calc R . . C78 C 0.7649(6) 0.8438(2) 0.0512(3) 0.1081(18) Uani 1 1 d . . . H78 H 0.6864 0.8399 0.0512 0.130 Uiso 1 1 calc R . . C79 C 0.9942(5) 0.92275(18) 0.1289(3) 0.125(2) Uani 1 1 d . . . H79A H 0.9401 0.9430 0.1462 0.187 Uiso 1 1 calc R . . H79B H 1.0392 0.9421 0.1042 0.187 Uiso 1 1 calc R . . H79C H 1.0437 0.9074 0.1630 0.187 Uiso 1 1 calc R . . O4 O 0.29770(13) 0.85852(5) 0.81648(9) 0.0241(4) Uani 1 1 d . . . N3 N 0.37145(16) 0.99938(7) 0.84295(10) 0.0228(5) Uani 1 1 d . . . N1 N 0.12960(16) 0.79021(6) 0.80141(10) 0.0190(4) Uani 1 1 d . . . O3 O 0.24528(13) 0.83747(6) 0.70057(8) 0.0255(4) Uani 1 1 d . . . N4 N 0.03331(16) 0.91969(7) 0.57874(11) 0.0270(5) Uani 1 1 d . . . N2 N 0.46624(15) 0.80903(6) 0.74234(10) 0.0195(5) Uani 1 1 d . . . O1 O 0.27234(13) 0.74412(6) 0.72806(9) 0.0260(4) Uani 1 1 d . . . O2 O 0.37367(13) 0.77088(6) 0.84455(9) 0.0255(4) Uani 1 1 d . . . O5 O 0.02377(15) 0.96852(7) 0.93968(10) 0.0440(6) Uani 1 1 d . . . O6 O 0.41513(16) 0.91270(8) 0.49852(10) 0.0443(6) Uani 1 1 d . . . Ti1 Ti 0.30021(3) 0.796661(14) 0.77386(2) 0.01841(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 0.0177(11) 0.0212(12) 0.0181(14) 0.0006(10) 0.0009(10) -0.0005(9) C2 0.0196(11) 0.0215(12) 0.0208(15) -0.0016(10) 0.0041(11) -0.0026(9) C3 0.0210(12) 0.0305(14) 0.0279(17) -0.0047(12) 0.0069(12) -0.0059(10) C4 0.0247(12) 0.0321(14) 0.0273(17) -0.0097(12) 0.0060(12) 0.0001(11) C5 0.0210(12) 0.0219(12) 0.0284(16) -0.0063(11) -0.0022(11) -0.0036(10) C6 0.0167(11) 0.0186(12) 0.0220(15) -0.0020(10) -0.0001(10) -0.0014(9) C7 0.0179(11) 0.0200(12) 0.0274(16) -0.0026(10) -0.0001(11) 0.0001(9) C8 0.0194(11) 0.0150(11) 0.0337(17) -0.0041(10) 0.0021(11) -0.0001(9) C9 0.0225(12) 0.0214(13) 0.0380(18) -0.0047(11) 0.0044(12) -0.0006(10) C10 0.0221(13) 0.0291(15) 0.056(2) -0.0069(14) 0.0045(14) -0.0074(11) C11 0.0287(14) 0.0267(15) 0.062(2) -0.0037(14) 0.0196(16) -0.0052(11) C12 0.0397(16) 0.0266(14) 0.040(2) -0.0019(13) 0.0190(15) -0.0028(12) C13 0.0268(13) 0.0163(12) 0.0370(18) -0.0051(11) 0.0052(12) -0.0010(10) C14 0.0192(11) 0.0233(13) 0.0219(15) 0.0032(11) 0.0045(11) -0.0033(10) C15 0.0193(11) 0.0163(12) 0.0304(16) -0.0034(10) 0.0080(11) -0.0036(9) C16 0.0197(11) 0.0209(12) 0.0307(17) -0.0037(11) 0.0055(11) -0.0007(10) C17 0.0230(12) 0.0307(15) 0.0386(19) -0.0057(13) -0.0002(12) -0.0019(11) C18 0.0275(13) 0.0231(14) 0.052(2) -0.0063(13) 0.0050(14) -0.0088(11) C19 0.0280(13) 0.0167(13) 0.053(2) 0.0055(12) 0.0059(14) -0.0032(10) C20 0.0223(12) 0.0201(12) 0.0334(17) 0.0017(11) 0.0036(11) -0.0002(10) C21 0.0244(13) 0.0465(18) 0.059(2) -0.0203(16) 0.0172(15) -0.0013(13) C22 0.0263(14) 0.0471(18) 0.037(2) -0.0082(14) -0.0033(13) -0.0042(12) C23 0.144(4) 0.085(3) 0.057(3) -0.018(2) 0.025(3) 0.045(3) C24 0.047(2) 0.146(4) 0.049(3) -0.010(3) -0.0136(19) -0.001(2) C25 0.0354(15) 0.0314(15) 0.0354(19) -0.0026(13) 0.0027(14) -0.0080(12) C26 0.0323(15) 0.0545(19) 0.041(2) 0.0000(16) -0.0008(14) 0.0002(14) C27 0.066(2) 0.058(2) 0.035(2) -0.0095(17) 0.0042(18) 0.0034(18) C28 0.0239(12) 0.0256(13) 0.0269(16) 0.0019(11) 0.0007(11) -0.0042(10) C29 0.057(2) 0.0486(19) 0.032(2) -0.0006(15) -0.0005(16) 0.0095(15) C30 0.055(2) 0.0366(17) 0.065(3) 0.0185(16) 0.0238(19) 0.0189(15) C31 0.0328(14) 0.0298(14) 0.0396(19) 0.0118(13) 0.0004(13) -0.0088(12) C32 0.086(3) 0.052(2) 0.099(4) 0.002(2) -0.044(3) 0.021(2) C33 0.062(2) 0.138(4) 0.040(3) 0.002(3) 0.001(2) -0.024(3) C34 0.0175(11) 0.0193(12) 0.0211(15) -0.0013(10) 0.0021(10) -0.0023(9) C35 0.0173(11) 0.0218(12) 0.0239(16) -0.0008(10) 0.0024(11) 0.0008(9) C36 0.0185(12) 0.0333(14) 0.0300(17) 0.0008(12) 0.0052(12) 0.0007(10) C37 0.0232(12) 0.0375(15) 0.0232(16) 0.0054(12) 0.0060(12) 0.0008(11) C38 0.0245(12) 0.0301(14) 0.0220(16) 0.0061(11) -0.0020(11) 0.0015(11) C39 0.0188(11) 0.0216(12) 0.0203(15) -0.0014(10) -0.0003(10) 0.0001(9) C40 0.0193(11) 0.0220(12) 0.0252(16) 0.0012(11) 0.0027(11) 0.0007(10) C41 0.0174(11) 0.0295(13) 0.0226(15) 0.0075(11) 0.0006(11) 0.0039(10) C42 0.0268(13) 0.0318(14) 0.0244(16) 0.0017(12) 0.0007(12) 0.0089(11) C43 0.0218(13) 0.0407(16) 0.040(2) -0.0012(14) -0.0027(13) 0.0002(12) C44 0.0203(12) 0.0340(15) 0.047(2) 0.0025(14) 0.0086(13) 0.0044(11) C45 0.0261(13) 0.0289(14) 0.0368(18) 0.0018(12) 0.0097(13) 0.0040(11) C46 0.0235(12) 0.0226(12) 0.0253(16) 0.0040(11) 0.0023(11) 0.0022(10) C47 0.0151(11) 0.0243(13) 0.0264(16) -0.0027(11) 0.0041(11) 0.0019(9) C48 0.0142(10) 0.0241(12) 0.0247(15) 0.0034(11) 0.0027(10) 0.0012(9) C49 0.0184(11) 0.0222(12) 0.0225(15) 0.0033(10) 0.0049(11) 0.0012(9) C50 0.0177(11) 0.0322(14) 0.0265(16) 0.0023(12) -0.0019(11) -0.0023(10) C51 0.0184(12) 0.0399(16) 0.0320(18) 0.0115(13) -0.0008(12) 0.0046(11) C52 0.0220(12) 0.0256(13) 0.0441(19) 0.0083(12) 0.0033(13) 0.0058(11) C53 0.0192(11) 0.0225(13) 0.0378(18) 0.0015(11) 0.0037(12) 0.0022(10) C54 0.0485(18) 0.056(2) 0.031(2) 0.0165(15) 0.0115(15) -0.0001(15) C55 0.0396(16) 0.057(2) 0.0301(19) -0.0086(15) -0.0045(14) 0.0173(15) C56 0.057(2) 0.107(3) 0.084(3) -0.063(3) -0.015(2) 0.007(2) C57 0.107(3) 0.105(3) 0.033(2) 0.012(2) 0.020(2) 0.050(3) C58 0.0266(13) 0.0302(14) 0.0364(19) -0.0050(12) 0.0002(13) 0.0031(11) C59 0.0387(16) 0.0302(16) 0.073(3) -0.0079(16) 0.0058(17) 0.0005(13) C60 0.091(3) 0.061(2) 0.041(2) 0.0001(19) -0.021(2) -0.007(2) C61 0.0207(11) 0.0250(13) 0.0278(16) -0.0013(11) -0.0023(11) 0.0001(10) C62 0.0401(16) 0.0338(16) 0.039(2) -0.0077(14) 0.0034(15) 0.0010(13) C63 0.061(2) 0.0233(15) 0.051(2) 0.0076(14) 0.0170(18) 0.0019(14) C64 0.0256(13) 0.0259(15) 0.072(3) -0.0158(15) -0.0065(15) 0.0056(11) C65 0.104(4) 0.030(2) 0.227(7) 0.030(3) -0.088(4) -0.026(2) C66 0.049(2) 0.184(5) 0.130(5) -0.128(4) 0.023(3) -0.023(3) C67 0.0219(12) 0.0299(14) 0.0318(17) -0.0107(12) 0.0002(12) 0.0009(10) C68 0.075(2) 0.0284(17) 0.067(3) -0.0157(16) 0.000(2) -0.0049(16) C69 0.057(2) 0.052(2) 0.040(2) -0.0182(16) 0.0100(17) -0.0126(16) C70 0.0301(14) 0.0522(18) 0.0273(18) 0.0113(14) -0.0078(13) -0.0160(13) C71 0.065(2) 0.061(2) 0.0246(19) 0.0015(16) -0.0046(16) 0.0054(18) C72 0.057(2) 0.127(4) 0.046(3) 0.026(2) -0.003(2) 0.039(2) C73 0.088(3) 0.077(3) 0.056(3) 0.007(2) -0.003(2) 0.012(3) C74 0.086(3) 0.081(3) 0.060(3) 0.013(2) -0.005(3) 0.017(3) C75 0.119(4) 0.128(5) 0.063(4) 0.023(3) 0.003(3) 0.064(4) C76 0.154(5) 0.097(4) 0.038(3) 0.021(3) 0.020(3) 0.072(4) C77 0.164(7) 0.106(4) 0.060(4) 0.027(3) 0.010(4) 0.054(4) C78 0.143(5) 0.115(5) 0.061(4) 0.028(3) -0.001(4) 0.023(4) C79 0.130(5) 0.077(4) 0.160(6) 0.023(4) -0.005(4) 0.010(3) O4 0.0204(8) 0.0195(8) 0.0336(12) -0.0061(8) 0.0082(8) -0.0024(7) N3 0.0183(9) 0.0198(10) 0.0304(14) -0.0034(9) 0.0037(9) -0.0031(8) N1 0.0207(9) 0.0161(10) 0.0199(12) 0.0008(8) 0.0019(9) -0.0024(8) O3 0.0182(8) 0.0307(10) 0.0280(11) 0.0110(8) 0.0054(8) 0.0049(7) N4 0.0199(10) 0.0335(12) 0.0271(14) 0.0055(10) 0.0020(10) 0.0063(9) N2 0.0168(9) 0.0172(10) 0.0235(13) -0.0009(8) -0.0003(9) 0.0026(8) O1 0.0214(8) 0.0225(9) 0.0337(12) -0.0072(8) 0.0032(8) -0.0020(7) O2 0.0220(8) 0.0262(9) 0.0276(11) 0.0053(8) 0.0007(8) -0.0014(7) O5 0.0309(10) 0.0416(12) 0.0638(16) -0.0315(11) 0.0222(11) -0.0072(9) O6 0.0325(10) 0.0666(14) 0.0362(14) 0.0266(11) 0.0133(10) 0.0080(10) Ti1 0.01580(19) 0.0163(2) 0.0228(3) 0.00079(18) 0.00175(18) 0.00042(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 O4 1.307(3) . ? C1 C6 1.416(3) . ? C1 C2 1.418(3) . ? C2 C3 1.402(3) . ? C2 C14 1.439(3) . ? C3 C4 1.374(3) . ? C3 H3 0.9500 . ? C4 O5 1.373(3) . ? C4 C5 1.388(3) . ? C5 C6 1.382(3) . ? C5 H5 0.9500 . ? C6 C7 1.463(3) . ? C7 N3 1.274(3) . ? C7 H7 0.9500 . ? C8 C9 1.406(4) . ? C8 C13 1.406(4) . ? C8 N3 1.428(3) . ? C9 C10 1.388(4) . ? C9 C22 1.506(4) . ? C10 C11 1.371(4) . ? C10 H10 0.9500 . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? C12 C13 1.393(4) . ? C12 H12 0.9500 . ? C13 C25 1.520(4) . ? C14 N1 1.288(3) . ? C14 H14 0.9500 . ? C15 C16 1.398(4) . ? C15 C20 1.406(3) . ? C15 N1 1.461(3) . ? C16 C17 1.392(3) . ? C16 C28 1.520(3) . ? C17 C18 1.379(4) . ? C17 H17 0.9500 . ? C18 C19 1.359(4) . ? C18 H18 0.9500 . ? C19 C20 1.395(3) . ? C19 H19 0.9500 . ? C20 C31 1.513(4) . ? C21 O5 1.414(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.507(4) . ? C22 C23 1.509(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.520(4) . ? C25 C26 1.529(4) . ? C25 H25 1.0000 . ? 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 1.512(4) . ? C28 C30 1.525(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.515(5) . ? C31 C32 1.518(4) . ? C31 H31 1.0000 . ? 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 O3 1.304(3) . ? C34 C39 1.415(3) . ? C34 C35 1.424(3) . ? C35 C36 1.402(4) . ? C35 C47 1.444(3) . ? C36 C37 1.373(4) . ? C36 H36 0.9500 . ? C37 O6 1.377(3) . ? C37 C38 1.385(3) . ? C38 C39 1.394(4) . ? C38 H38 0.9500 . ? C39 C40 1.471(3) . ? C40 N4 1.268(3) . ? C40 H40 0.9500 . ? C41 C46 1.397(4) . ? C41 C42 1.415(4) . ? C41 N4 1.433(3) . ? C42 C43 1.393(3) . ? C42 C55 1.505(4) . ? C43 C44 1.373(4) . ? C43 H43 0.9500 . ? C44 C45 1.374(4) . ? C44 H44 0.9500 . ? C45 C46 1.390(3) . ? C45 H45 0.9500 . ? C46 C58 1.514(4) . ? C47 N2 1.286(3) . ? C47 H47 0.9500 . ? C48 C49 1.405(3) . ? C48 C53 1.406(3) . ? C48 N2 1.459(3) . ? C49 C50 1.390(3) . ? C49 C61 1.519(3) . ? C50 C51 1.379(4) . ? C50 H50 0.9500 . ? C51 C52 1.370(4) . ? C51 H51 0.9500 . ? C52 C53 1.396(4) . ? C52 H52 0.9500 . ? C53 C64 1.514(4) . ? C54 O6 1.414(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.525(5) . ? C55 C57 1.526(5) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C60 1.505(4) . ? C58 C59 1.524(4) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.524(4) . ? C61 C63 1.528(4) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C66 1.527(5) . ? C64 C65 1.530(5) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 O1 1.425(3) . ? C67 C69 1.506(4) . ? C67 C68 1.511(4) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 O2 1.428(3) . ? C70 C72 1.504(4) . ? C70 C71 1.505(4) . ? C70 H70 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.357(6) . ? C73 C78 1.391(7) . ? C73 H73 0.9500 . ? C74 C75 1.416(6) . ? C74 C79 1.455(7) . ? C75 C76 1.445(7) . ? C75 H75 0.9500 . ? C76 C77 1.388(8) . ? C76 H76 0.9500 . ? C77 C78 1.250(7) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? O4 Ti1 1.9773(16) . ? N1 Ti1 2.2252(19) . ? O3 Ti1 1.9946(17) . ? N2 Ti1 2.2285(19) . ? O1 Ti1 1.7887(17) . ? O2 Ti1 1.8062(18) . ? 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 O4 C1 C6 120.9(2) . . ? O4 C1 C2 121.3(2) . . ? C6 C1 C2 117.8(2) . . ? C3 C2 C1 120.3(2) . . ? C3 C2 C14 117.4(2) . . ? C1 C2 C14 122.2(2) . . ? C4 C3 C2 120.7(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? O5 C4 C3 125.0(2) . . ? O5 C4 C5 115.8(2) . . ? C3 C4 C5 119.1(2) . . ? C6 C5 C4 122.0(2) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 119.7(2) . . ? C5 C6 C7 120.5(2) . . ? C1 C6 C7 119.7(2) . . ? N3 C7 C6 122.9(2) . . ? N3 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C9 C8 C13 121.5(2) . . ? C9 C8 N3 117.4(2) . . ? C13 C8 N3 121.0(2) . . ? C10 C9 C8 118.0(3) . . ? C10 C9 C22 122.2(3) . . ? C8 C9 C22 119.7(2) . . ? C11 C10 C9 121.1(3) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 121.3(3) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C12 C13 C8 117.5(2) . . ? C12 C13 C25 121.4(3) . . ? C8 C13 C25 121.0(2) . . ? N1 C14 C2 128.3(2) . . ? N1 C14 H14 115.9 . . ? C2 C14 H14 115.9 . . ? C16 C15 C20 122.0(2) . . ? C16 C15 N1 118.8(2) . . ? C20 C15 N1 119.2(2) . . ? C17 C16 C15 117.6(2) . . ? C17 C16 C28 120.0(2) . . ? C15 C16 C28 122.5(2) . . ? C18 C17 C16 121.2(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 121.8(3) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 117.2(2) . . ? C19 C20 C31 120.4(2) . . ? C15 C20 C31 122.4(2) . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C9 C22 C24 114.5(3) . . ? C9 C22 C23 109.8(3) . . ? C24 C22 C23 112.6(3) . . ? C9 C22 H22 106.5 . . ? C24 C22 H22 106.5 . . ? C23 C22 H22 106.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C13 C25 C27 114.6(2) . . ? C13 C25 C26 109.2(2) . . ? C27 C25 C26 109.8(3) . . ? C13 C25 H25 107.6 . . ? C27 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C16 113.5(2) . . ? C29 C28 C30 109.8(2) . . ? C16 C28 C30 111.0(2) . . ? C29 C28 H28 107.4 . . ? C16 C28 H28 107.4 . . ? C30 C28 H28 107.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C20 C31 C33 110.9(3) . . ? C20 C31 C32 112.4(3) . . ? C33 C31 C32 111.0(3) . . ? C20 C31 H31 107.4 . . ? C33 C31 H31 107.4 . . ? C32 C31 H31 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O3 C34 C39 122.0(2) . . ? O3 C34 C35 120.7(2) . . ? C39 C34 C35 117.3(2) . . ? C36 C35 C34 120.1(2) . . ? C36 C35 C47 116.9(2) . . ? C34 C35 C47 122.9(2) . . ? C37 C36 C35 121.5(2) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 O6 116.1(2) . . ? C36 C37 C38 119.2(2) . . ? O6 C37 C38 124.7(2) . . ? C37 C38 C39 121.2(2) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C38 C39 C34 120.7(2) . . ? C38 C39 C40 119.4(2) . . ? C34 C39 C40 119.9(2) . . ? N4 C40 C39 122.1(2) . . ? N4 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? C46 C41 C42 121.4(2) . . ? C46 C41 N4 122.0(2) . . ? C42 C41 N4 116.5(2) . . ? C43 C42 C41 117.8(2) . . ? C43 C42 C55 121.9(3) . . ? C41 C42 C55 120.2(2) . . ? C44 C43 C42 121.1(3) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 120.0(2) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 121.8(3) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? C45 C46 C41 117.7(2) . . ? C45 C46 C58 119.2(2) . . ? C41 C46 C58 123.0(2) . . ? N2 C47 C35 128.5(2) . . ? N2 C47 H47 115.7 . . ? C35 C47 H47 115.7 . . ? C49 C48 C53 121.5(2) . . ? C49 C48 N2 118.6(2) . . ? C53 C48 N2 119.8(2) . . ? C50 C49 C48 117.9(2) . . ? C50 C49 C61 120.1(2) . . ? C48 C49 C61 121.9(2) . . ? C51 C50 C49 121.5(2) . . ? C51 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C52 C51 C50 119.8(2) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C53 121.8(2) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C52 C53 C48 117.5(2) . . ? C52 C53 C64 120.3(2) . . ? C48 C53 C64 122.2(2) . . ? O6 C54 H54A 109.5 . . ? O6 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O6 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C42 C55 C56 113.9(3) . . ? C42 C55 C57 108.8(3) . . ? C56 C55 C57 111.8(3) . . ? C42 C55 H55 107.4 . . ? C56 C55 H55 107.4 . . ? C57 C55 H55 107.4 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C60 C58 C46 112.4(2) . . ? C60 C58 C59 110.5(3) . . ? C46 C58 C59 111.2(2) . . ? C60 C58 H58 107.5 . . ? C46 C58 H58 107.5 . . ? C59 C58 H58 107.5 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C49 C61 C62 112.8(2) . . ? C49 C61 C63 110.1(2) . . ? C62 C61 C63 110.2(2) . . ? C49 C61 H61 107.9 . . ? C62 C61 H61 107.9 . . ? C63 C61 H61 107.9 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C53 C64 C66 110.4(3) . . ? C53 C64 C65 110.7(3) . . ? C66 C64 C65 112.7(4) . . ? C53 C64 H64 107.6 . . ? C66 C64 H64 107.6 . . ? C65 C64 H64 107.6 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O1 C67 C69 110.9(2) . . ? O1 C67 C68 108.5(2) . . ? C69 C67 C68 112.0(3) . . ? O1 C67 H67 108.5 . . ? C69 C67 H67 108.5 . . ? C68 C67 H67 108.5 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O2 C70 C72 109.9(3) . . ? O2 C70 C71 111.8(2) . . ? C72 C70 C71 111.1(3) . . ? O2 C70 H70 107.9 . . ? C72 C70 H70 107.9 . . ? C71 C70 H70 107.9 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C78 122.7(5) . . ? C74 C73 H73 118.7 . . ? C78 C73 H73 118.7 . . ? C73 C74 C75 118.2(5) . . ? C73 C74 C79 122.2(5) . . ? C75 C74 C79 119.6(5) . . ? C74 C75 C76 116.6(5) . . ? C74 C75 H75 121.7 . . ? C76 C75 H75 121.7 . . ? C77 C76 C75 119.2(5) . . ? C77 C76 H76 120.4 . . ? C75 C76 H76 120.4 . . ? C78 C77 C76 122.9(7) . . ? C78 C77 H77 118.6 . . ? C76 C77 H77 118.6 . . ? C77 C78 C73 120.4(7) . . ? C77 C78 H78 119.8 . . ? C73 C78 H78 119.8 . . ? C74 C79 H79A 109.5 . . ? C74 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C74 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C1 O4 Ti1 138.88(15) . . ? C7 N3 C8 117.0(2) . . ? C14 N1 C15 114.12(19) . . ? C14 N1 Ti1 125.67(15) . . ? C15 N1 Ti1 120.21(14) . . ? C34 O3 Ti1 138.90(14) . . ? C40 N4 C41 119.1(2) . . ? C47 N2 C48 113.46(19) . . ? C47 N2 Ti1 124.79(16) . . ? C48 N2 Ti1 121.68(15) . . ? C67 O1 Ti1 153.14(16) . . ? C70 O2 Ti1 144.39(17) . . ? C4 O5 C21 117.3(2) . . ? C37 O6 C54 117.2(2) . . ? O1 Ti1 O2 99.51(8) . . ? O1 Ti1 O4 167.61(8) . . ? O2 Ti1 O4 89.95(8) . . ? O1 Ti1 O3 91.38(8) . . ? O2 Ti1 O3 166.43(8) . . ? O4 Ti1 O3 80.51(7) . . ? O1 Ti1 N1 88.50(7) . . ? O2 Ti1 N1 95.62(7) . . ? O4 Ti1 N1 82.58(7) . . ? O3 Ti1 N1 92.71(7) . . ? O1 Ti1 N2 93.74(7) . . ? O2 Ti1 N2 88.36(7) . . ? O4 Ti1 N2 94.52(7) . . ? O3 Ti1 N2 82.84(7) . . ? N1 Ti1 N2 175.05(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 C1 C2 C3 174.1(2) . . . . ? C6 C1 C2 C3 -6.2(4) . . . . ? O4 C1 C2 C14 -8.9(4) . . . . ? C6 C1 C2 C14 170.8(2) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C14 C2 C3 C4 -175.8(3) . . . . ? C2 C3 C4 O5 -176.9(3) . . . . ? C2 C3 C4 C5 3.5(4) . . . . ? O5 C4 C5 C6 177.1(2) . . . . ? C3 C4 C5 C6 -3.4(4) . . . . ? C4 C5 C6 C1 -1.7(4) . . . . ? C4 C5 C6 C7 175.6(2) . . . . ? O4 C1 C6 C5 -173.9(2) . . . . ? C2 C1 C6 C5 6.4(4) . . . . ? O4 C1 C6 C7 8.7(4) . . . . ? C2 C1 C6 C7 -171.0(2) . . . . ? C5 C6 C7 N3 -2.2(4) . . . . ? C1 C6 C7 N3 175.1(2) . . . . ? C13 C8 C9 C10 -5.2(4) . . . . ? N3 C8 C9 C10 178.3(2) . . . . ? C13 C8 C9 C22 172.1(2) . . . . ? N3 C8 C9 C22 -4.4(3) . . . . ? C8 C9 C10 C11 2.2(4) . . . . ? C22 C9 C10 C11 -175.0(3) . . . . ? C9 C10 C11 C12 1.5(4) . . . . ? C10 C11 C12 C13 -2.3(4) . . . . ? C11 C12 C13 C8 -0.6(4) . . . . ? C11 C12 C13 C25 174.6(2) . . . . ? C9 C8 C13 C12 4.4(3) . . . . ? N3 C8 C13 C12 -179.2(2) . . . . ? C9 C8 C13 C25 -170.8(2) . . . . ? N3 C8 C13 C25 5.5(3) . . . . ? C3 C2 C14 N1 176.5(3) . . . . ? C1 C2 C14 N1 -0.6(4) . . . . ? C20 C15 C16 C17 -1.0(3) . . . . ? N1 C15 C16 C17 179.3(2) . . . . ? C20 C15 C16 C28 178.3(2) . . . . ? N1 C15 C16 C28 -1.3(3) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C28 C16 C17 C18 -178.7(2) . . . . ? C16 C17 C18 C19 0.5(4) . . . . ? C17 C18 C19 C20 -1.4(4) . . . . ? C18 C19 C20 C15 1.1(4) . . . . ? C18 C19 C20 C31 179.6(3) . . . . ? C16 C15 C20 C19 0.2(4) . . . . ? N1 C15 C20 C19 179.8(2) . . . . ? C16 C15 C20 C31 -178.3(2) . . . . ? N1 C15 C20 C31 1.3(3) . . . . ? C10 C9 C22 C24 -35.2(4) . . . . ? C8 C9 C22 C24 147.6(3) . . . . ? C10 C9 C22 C23 92.6(4) . . . . ? C8 C9 C22 C23 -84.6(3) . . . . ? C12 C13 C25 C27 15.2(4) . . . . ? C8 C13 C25 C27 -169.7(2) . . . . ? C12 C13 C25 C26 -108.5(3) . . . . ? C8 C13 C25 C26 66.6(3) . . . . ? C17 C16 C28 C29 -42.6(3) . . . . ? C15 C16 C28 C29 138.0(3) . . . . ? C17 C16 C28 C30 81.7(3) . . . . ? C15 C16 C28 C30 -97.7(3) . . . . ? C19 C20 C31 C33 -78.0(3) . . . . ? C15 C20 C31 C33 100.4(3) . . . . ? C19 C20 C31 C32 46.8(4) . . . . ? C15 C20 C31 C32 -134.8(3) . . . . ? O3 C34 C35 C36 176.3(2) . . . . ? C39 C34 C35 C36 -4.2(3) . . . . ? O3 C34 C35 C47 -8.1(4) . . . . ? C39 C34 C35 C47 171.4(2) . . . . ? C34 C35 C36 C37 2.7(4) . . . . ? C47 C35 C36 C37 -173.1(2) . . . . ? C35 C36 C37 O6 179.2(2) . . . . ? C35 C36 C37 C38 -0.6(4) . . . . ? C36 C37 C38 C39 0.1(4) . . . . ? O6 C37 C38 C39 -179.7(2) . . . . ? C37 C38 C39 C34 -1.7(4) . . . . ? C37 C38 C39 C40 179.1(2) . . . . ? O3 C34 C39 C38 -176.8(2) . . . . ? C35 C34 C39 C38 3.7(3) . . . . ? O3 C34 C39 C40 2.3(4) . . . . ? C35 C34 C39 C40 -177.1(2) . . . . ? C38 C39 C40 N4 0.5(4) . . . . ? C34 C39 C40 N4 -178.7(2) . . . . ? C46 C41 C42 C43 -3.3(4) . . . . ? N4 C41 C42 C43 -179.1(2) . . . . ? C46 C41 C42 C55 174.0(3) . . . . ? N4 C41 C42 C55 -1.9(4) . . . . ? C41 C42 C43 C44 0.5(4) . . . . ? C55 C42 C43 C44 -176.7(3) . . . . ? C42 C43 C44 C45 1.7(4) . . . . ? C43 C44 C45 C46 -1.3(4) . . . . ? C44 C45 C46 C41 -1.4(4) . . . . ? C44 C45 C46 C58 176.7(3) . . . . ? C42 C41 C46 C45 3.7(4) . . . . ? N4 C41 C46 C45 179.3(2) . . . . ? C42 C41 C46 C58 -174.3(2) . . . . ? N4 C41 C46 C58 1.3(4) . . . . ? C36 C35 C47 N2 178.3(2) . . . . ? C34 C35 C47 N2 2.6(4) . . . . ? C53 C48 C49 C50 0.0(4) . . . . ? N2 C48 C49 C50 -178.5(2) . . . . ? C53 C48 C49 C61 177.8(2) . . . . ? N2 C48 C49 C61 -0.7(3) . . . . ? C48 C49 C50 C51 0.2(4) . . . . ? C61 C49 C50 C51 -177.6(2) . . . . ? C49 C50 C51 C52 0.0(4) . . . . ? C50 C51 C52 C53 -0.5(4) . . . . ? C51 C52 C53 C48 0.7(4) . . . . ? C51 C52 C53 C64 179.7(3) . . . . ? C49 C48 C53 C52 -0.4(4) . . . . ? N2 C48 C53 C52 178.0(2) . . . . ? C49 C48 C53 C64 -179.5(2) . . . . ? N2 C48 C53 C64 -1.0(4) . . . . ? C43 C42 C55 C56 -27.3(4) . . . . ? C41 C42 C55 C56 155.5(3) . . . . ? C43 C42 C55 C57 98.0(3) . . . . ? C41 C42 C55 C57 -79.1(3) . . . . ? C45 C46 C58 C60 72.9(3) . . . . ? C41 C46 C58 C60 -109.1(3) . . . . ? C45 C46 C58 C59 -51.6(3) . . . . ? C41 C46 C58 C59 126.4(3) . . . . ? C50 C49 C61 C62 -47.6(3) . . . . ? C48 C49 C61 C62 134.7(2) . . . . ? C50 C49 C61 C63 75.9(3) . . . . ? C48 C49 C61 C63 -101.8(3) . . . . ? C52 C53 C64 C66 -77.8(4) . . . . ? C48 C53 C64 C66 101.2(4) . . . . ? C52 C53 C64 C65 47.7(4) . . . . ? C48 C53 C64 C65 -133.3(3) . . . . ? C78 C73 C74 C75 1.7(7) . . . . ? C78 C73 C74 C79 -176.8(5) . . . . ? C73 C74 C75 C76 -1.9(6) . . . . ? C79 C74 C75 C76 176.6(4) . . . . ? C74 C75 C76 C77 1.1(7) . . . . ? C75 C76 C77 C78 0.1(8) . . . . ? C76 C77 C78 C73 -0.5(8) . . . . ? C74 C73 C78 C77 -0.4(8) . . . . ? C6 C1 O4 Ti1 -166.11(18) . . . . ? C2 C1 O4 Ti1 13.5(4) . . . . ? C6 C7 N3 C8 -177.4(2) . . . . ? C9 C8 N3 C7 -114.4(3) . . . . ? C13 C8 N3 C7 69.1(3) . . . . ? C2 C14 N1 C15 -174.1(2) . . . . ? C2 C14 N1 Ti1 6.5(4) . . . . ? C16 C15 N1 C14 84.6(3) . . . . ? C20 C15 N1 C14 -95.0(3) . . . . ? C16 C15 N1 Ti1 -96.0(2) . . . . ? C20 C15 N1 Ti1 84.4(2) . . . . ? C39 C34 O3 Ti1 -179.37(17) . . . . ? C35 C34 O3 Ti1 0.0(4) . . . . ? C39 C40 N4 C41 177.9(2) . . . . ? C46 C41 N4 C40 71.1(3) . . . . ? C42 C41 N4 C40 -113.1(3) . . . . ? C35 C47 N2 C48 -173.8(2) . . . . ? C35 C47 N2 Ti1 9.1(4) . . . . ? C49 C48 N2 C47 84.2(3) . . . . ? C53 C48 N2 C47 -94.3(3) . . . . ? C49 C48 N2 Ti1 -98.5(2) . . . . ? C53 C48 N2 Ti1 82.9(3) . . . . ? C69 C67 O1 Ti1 68.9(4) . . . . ? C68 C67 O1 Ti1 -167.7(3) . . . . ? C72 C70 O2 Ti1 -160.9(2) . . . . ? C71 C70 O2 Ti1 75.2(3) . . . . ? C3 C4 O5 C21 -18.2(4) . . . . ? C5 C4 O5 C21 161.4(3) . . . . ? C36 C37 O6 C54 -163.2(3) . . . . ? C38 C37 O6 C54 16.6(4) . . . . ? C67 O1 Ti1 O2 169.9(3) . . . . ? C67 O1 Ti1 O4 30.6(6) . . . . ? C67 O1 Ti1 O3 -18.2(3) . . . . ? C67 O1 Ti1 N1 74.4(3) . . . . ? C67 O1 Ti1 N2 -101.2(3) . . . . ? C70 O2 Ti1 O1 172.3(3) . . . . ? C70 O2 Ti1 O4 -15.7(3) . . . . ? C70 O2 Ti1 O3 29.4(5) . . . . ? C70 O2 Ti1 N1 -98.3(3) . . . . ? C70 O2 Ti1 N2 78.8(3) . . . . ? C1 O4 Ti1 O1 37.4(5) . . . . ? C1 O4 Ti1 O2 -102.6(3) . . . . ? C1 O4 Ti1 O3 87.1(2) . . . . ? C1 O4 Ti1 N1 -6.9(2) . . . . ? C1 O4 Ti1 N2 169.0(2) . . . . ? C34 O3 Ti1 O1 -86.0(2) . . . . ? C34 O3 Ti1 O2 57.6(4) . . . . ? C34 O3 Ti1 O4 103.4(2) . . . . ? C34 O3 Ti1 N1 -174.5(2) . . . . ? C34 O3 Ti1 N2 7.6(2) . . . . ? C14 N1 Ti1 O1 -174.7(2) . . . . ? C15 N1 Ti1 O1 6.00(18) . . . . ? C14 N1 Ti1 O2 85.9(2) . . . . ? C15 N1 Ti1 O2 -93.40(18) . . . . ? C14 N1 Ti1 O4 -3.3(2) . . . . ? C15 N1 Ti1 O4 177.38(18) . . . . ? C14 N1 Ti1 O3 -83.3(2) . . . . ? C15 N1 Ti1 O3 97.32(18) . . . . ? C14 N1 Ti1 N2 -57.5(10) . . . . ? C15 N1 Ti1 N2 123.1(9) . . . . ? C47 N2 Ti1 O1 79.6(2) . . . . ? C48 N2 Ti1 O1 -97.27(17) . . . . ? C47 N2 Ti1 O2 179.1(2) . . . . ? C48 N2 Ti1 O2 2.15(17) . . . . ? C47 N2 Ti1 O4 -91.1(2) . . . . ? C48 N2 Ti1 O4 91.97(17) . . . . ? C47 N2 Ti1 O3 -11.28(19) . . . . ? C48 N2 Ti1 O3 171.80(17) . . . . ? C47 N2 Ti1 N1 -37.3(10) . . . . ? C48 N2 Ti1 N1 145.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.736 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.060