Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Zuowei Xie' _publ_contact_author_address ; Department of Chemistry The Chinese University of Hong Kong Shatin N.T. Hong Kong 00000 CHINA ; _publ_contact_author_email ZXIE@CUHK.EDU.H _publ_section_title ; Synthesis, structure, and reactivity of group 4 metallacycles incorporating a Me2C-linked cyclopentadienyl-carboranyl ligand ; loop_ _publ_author_name 'Zuowei Xie.' 'Hoi-Shan Chan.' 'Mei-Mei Sit.' # Attachment 'cif_rev.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 665266' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H30 B10 N2 Ti' _chemical_formula_weight 382.40 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 25.806(4) _cell_length_b 25.806(4) _cell_length_c 9.888(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5702.7(16) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.339 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.97481 _exptl_absorpt_correction_T_max 1.0000 _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 'AFC7R Rigaku DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3637 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1271 _reflns_number_gt 836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0877P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(8) _refine_ls_number_reflns 1271 _refine_ls_number_parameters 133 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.82341(3) 0.17659(3) 0.78441(13) 0.0569(4) Uani 1 2 d S . . N1 N 0.9019(3) 0.2058(3) 0.8438(6) 0.0828(18) Uani 1 1 d . . . C2 C 0.82982(19) 0.17018(19) 0.5666(8) 0.054(2) Uani 1 2 d S . . C1 C 0.80031(18) 0.19969(18) 0.4649(8) 0.052(2) Uani 1 2 d S . . C11 C 0.76967(19) 0.23033(19) 0.5394(10) 0.065(2) Uani 1 2 d S . . C12 C 0.7987(3) 0.2986(3) 0.5004(8) 0.082(2) Uani 1 1 d . . . H12A H 0.7958 0.3022 0.4044 0.123 Uiso 1 1 calc R . . H12B H 0.8400 0.3195 0.5270 0.123 Uiso 1 1 calc R . . H12C H 0.7778 0.3156 0.5461 0.123 Uiso 1 1 calc R . . C13 C 0.77482(18) 0.22518(18) 0.6924(8) 0.057(2) Uani 1 2 d S . . C14 C 0.7335(3) 0.1789(3) 0.7765(8) 0.0714(16) Uani 1 1 d . . . H14A H 0.6944 0.1459 0.7488 0.086 Uiso 1 1 calc R . . C15 C 0.7555(3) 0.1911(3) 0.9073(7) 0.080(2) Uani 1 1 d . . . H15 H 0.7373 0.1673 0.9826 0.096 Uiso 1 1 calc R . . C16 C 0.9557(4) 0.2614(5) 0.8639(12) 0.136(4) Uani 1 1 d . . . H16A H 0.9872 0.2540 0.8910 0.204 Uiso 1 1 calc R . . H16B H 0.9495 0.2838 0.9332 0.204 Uiso 1 1 calc R . . H16C H 0.9667 0.2838 0.7811 0.204 Uiso 1 1 calc R . . C17 C 0.8449(5) 0.0939(4) 0.8930(12) 0.139(4) Uani 1 1 d . . . H17A H 0.8493 0.0654 0.8373 0.166 Uiso 1 1 calc R . . H17B H 0.8364 0.0783 0.9845 0.166 Uiso 1 1 calc R . . B3 B 0.7667(3) 0.1253(3) 0.4774(8) 0.0586(17) Uani 1 1 d . . . H3 H 0.7231 0.0982 0.5273 0.070 Uiso 1 1 calc R . . B5 B 0.8240(3) 0.1058(3) 0.4882(7) 0.0618(18) Uani 1 1 d . . . H5 H 0.8186 0.0663 0.5430 0.074 Uiso 1 1 calc R . . B4 B 0.7734(3) 0.1599(3) 0.3206(7) 0.069(2) Uani 1 1 d . . . H4 H 0.7343 0.1551 0.2653 0.083 Uiso 1 1 calc R . . B6 B 0.7877(4) 0.0997(4) 0.3311(8) 0.071(2) Uani 1 1 d . . . H6 H 0.7584 0.0558 0.2845 0.085 Uiso 1 1 calc R . . B8 B 0.8670(3) 0.1330(3) 0.3346(13) 0.084(4) Uani 1 2 d S . . H8 H 0.8894 0.1106 0.2881 0.101 Uiso 1 2 calc SR . . B7 B 0.8350(3) 0.1650(3) 0.2390(12) 0.077(4) Uani 1 2 d S . . H7 H 0.8366 0.1634 0.1280 0.093 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0599(7) 0.0599(7) 0.0468(7) 0.0011(4) -0.0011(4) 0.0269(9) N1 0.074(4) 0.111(5) 0.063(3) -0.015(3) -0.022(3) 0.047(4) C2 0.048(3) 0.048(3) 0.057(5) -0.003(2) 0.003(2) 0.017(4) C1 0.049(3) 0.049(3) 0.048(4) 0.0062(19) -0.0062(19) 0.017(4) C11 0.061(4) 0.061(4) 0.077(6) 0.006(2) -0.006(2) 0.032(4) C12 0.094(5) 0.055(4) 0.096(5) 0.011(4) -0.001(4) 0.036(4) C13 0.058(4) 0.058(4) 0.061(5) -0.003(2) 0.003(2) 0.034(4) C14 0.064(4) 0.071(4) 0.081(4) 0.005(3) 0.015(4) 0.035(4) C15 0.087(5) 0.105(5) 0.060(4) 0.006(3) 0.019(3) 0.057(4) C16 0.085(6) 0.153(9) 0.164(11) -0.030(8) -0.051(6) 0.054(7) C17 0.188(11) 0.149(9) 0.132(7) 0.020(7) -0.006(7) 0.124(8) B3 0.044(4) 0.051(4) 0.067(4) 0.002(3) -0.003(3) 0.014(3) B5 0.067(5) 0.054(4) 0.065(4) -0.003(3) 0.004(4) 0.032(4) B4 0.066(5) 0.077(5) 0.057(5) -0.012(4) -0.017(3) 0.030(4) B6 0.061(5) 0.075(5) 0.065(5) -0.022(4) 0.002(4) 0.025(4) B8 0.091(6) 0.091(6) 0.075(8) -0.017(3) 0.017(3) 0.049(7) B7 0.091(7) 0.091(7) 0.045(5) -0.003(3) 0.003(3) 0.041(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 1.869(6) 4_665 ? Ti1 N1 1.869(6) . ? Ti1 C2 2.173(8) . ? Ti1 C15 2.311(6) . ? Ti1 C15 2.311(6) 4_665 ? Ti1 C14 2.352(6) . ? Ti1 C14 2.352(6) 4_665 ? Ti1 C13 2.355(8) . ? Ti1 C17 2.683(9) 4_665 ? N1 C16 1.425(11) . ? N1 C17 1.449(11) 4_665 ? C2 C1 1.659(11) . ? C2 B3 1.699(8) . ? C2 B3 1.699(8) 4_665 ? C2 B5 1.770(9) 4_665 ? C2 B5 1.770(9) . ? C1 C11 1.555(12) . ? C1 B3 1.669(8) 4_665 ? C1 B3 1.669(8) . ? C1 B4 1.691(9) . ? C1 B4 1.691(10) 4_665 ? C11 C13 1.530(12) . ? C11 C12 1.580(7) . ? C11 C12 1.580(7) 4_665 ? C13 C14 1.408(9) 4_665 ? C13 C14 1.408(9) . ? C14 C15 1.384(10) . ? C15 C15 1.377(15) 4_665 ? C17 N1 1.449(11) 4_665 ? C17 C17 1.58(2) 4_665 ? B3 B4 1.754(10) . ? B3 B6 1.784(10) . ? B3 B5 1.788(10) . ? B5 B6 1.781(11) . ? B5 B8 1.804(13) . ? B5 B5 1.811(14) 4_665 ? B4 B4 1.721(14) 4_665 ? B4 B7 1.726(13) . ? B4 B6 1.770(11) . ? B6 B7 1.761(10) . ? B6 B8 1.780(11) . ? B8 B7 1.716(19) . ? B8 B6 1.780(11) 4_665 ? B8 B5 1.804(13) 4_665 ? B7 B4 1.726(13) 4_665 ? B7 B6 1.761(10) 4_665 ? 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 N1 Ti1 N1 96.2(4) 4_665 . ? N1 Ti1 C2 103.5(2) 4_665 . ? N1 Ti1 C2 103.5(2) . . ? N1 Ti1 C15 94.8(3) 4_665 . ? N1 Ti1 C15 121.8(3) . . ? C2 Ti1 C15 128.8(3) . . ? N1 Ti1 C15 121.8(3) 4_665 4_665 ? N1 Ti1 C15 94.8(3) . 4_665 ? C2 Ti1 C15 128.8(3) . 4_665 ? C15 Ti1 C15 34.7(4) . 4_665 ? N1 Ti1 C14 99.8(3) 4_665 . ? N1 Ti1 C14 152.2(3) . . ? C2 Ti1 C14 94.7(3) . . ? C15 Ti1 C14 34.5(2) . . ? C15 Ti1 C14 57.5(3) 4_665 . ? N1 Ti1 C14 152.2(3) 4_665 4_665 ? N1 Ti1 C14 99.8(3) . 4_665 ? C2 Ti1 C14 94.7(3) . 4_665 ? C15 Ti1 C14 57.5(3) . 4_665 ? C15 Ti1 C14 34.5(2) 4_665 4_665 ? C14 Ti1 C14 57.4(4) . 4_665 ? N1 Ti1 C13 131.7(2) 4_665 . ? N1 Ti1 C13 131.7(2) . . ? C2 Ti1 C13 74.8(3) . . ? C15 Ti1 C13 57.9(2) . . ? C15 Ti1 C13 57.9(2) 4_665 . ? C14 Ti1 C13 34.8(2) . . ? C14 Ti1 C13 34.8(2) 4_665 . ? N1 Ti1 C17 65.3(3) 4_665 4_665 ? N1 Ti1 C17 31.1(3) . 4_665 ? C2 Ti1 C17 106.4(3) . 4_665 ? C15 Ti1 C17 124.7(3) . 4_665 ? C15 Ti1 C17 113.2(3) 4_665 4_665 ? C14 Ti1 C17 156.3(3) . 4_665 ? C14 Ti1 C17 129.2(3) 4_665 4_665 ? C13 Ti1 C17 162.7(2) . 4_665 ? C16 N1 C17 112.7(7) . 4_665 ? C16 N1 Ti1 139.8(6) . . ? C17 N1 Ti1 107.3(5) 4_665 . ? C1 C2 B3 59.6(3) . . ? C1 C2 B3 59.6(3) . 4_665 ? B3 C2 B3 110.2(6) . 4_665 ? C1 C2 B5 108.8(5) . 4_665 ? B3 C2 B5 111.7(5) . 4_665 ? B3 C2 B5 62.0(4) 4_665 4_665 ? C1 C2 B5 108.8(5) . . ? B3 C2 B5 62.0(4) . . ? B3 C2 B5 111.7(5) 4_665 . ? B5 C2 B5 61.5(6) 4_665 . ? C1 C2 Ti1 119.8(5) . . ? B3 C2 Ti1 118.9(3) . . ? B3 C2 Ti1 118.9(3) 4_665 . ? B5 C2 Ti1 122.1(5) 4_665 . ? B5 C2 Ti1 122.1(5) . . ? C11 C1 C2 114.4(6) . . ? C11 C1 B3 116.4(4) . 4_665 ? C2 C1 B3 61.4(3) . 4_665 ? C11 C1 B3 116.5(4) . . ? C2 C1 B3 61.4(3) . . ? B3 C1 B3 113.2(7) 4_665 . ? C11 C1 B4 123.4(6) . . ? C2 C1 B4 112.1(6) . . ? B3 C1 B4 113.2(6) 4_665 . ? B3 C1 B4 62.9(4) . . ? C11 C1 B4 123.4(6) . 4_665 ? C2 C1 B4 112.1(6) . 4_665 ? B3 C1 B4 62.9(4) 4_665 4_665 ? B3 C1 B4 113.2(6) . 4_665 ? B4 C1 B4 61.2(6) . 4_665 ? C13 C11 C1 109.6(7) . . ? C13 C11 C12 109.0(5) . . ? C1 C11 C12 112.0(5) . . ? C13 C11 C12 109.0(5) . 4_665 ? C1 C11 C12 112.0(5) . 4_665 ? C12 C11 C12 105.2(7) . 4_665 ? C14 C13 C14 106.8(9) 4_665 . ? C14 C13 C11 126.6(4) 4_665 . ? C14 C13 C11 126.6(4) . . ? C14 C13 Ti1 72.5(4) 4_665 . ? C14 C13 Ti1 72.5(4) . . ? C11 C13 Ti1 121.4(5) . . ? C15 C14 C13 108.0(7) . . ? C15 C14 Ti1 71.1(4) . . ? C13 C14 Ti1 72.7(4) . . ? C15 C15 C14 108.6(4) 4_665 . ? C15 C15 Ti1 72.67(19) 4_665 . ? C14 C15 Ti1 74.3(3) . . ? N1 C17 C17 114.4(4) 4_665 4_665 ? C1 B3 C2 59.0(4) . . ? C1 B3 B4 59.1(4) . . ? C2 B3 B4 107.2(5) . . ? C1 B3 B6 106.6(6) . . ? C2 B3 B6 107.9(5) . . ? B4 B3 B6 60.0(5) . . ? C1 B3 B5 107.5(5) . . ? C2 B3 B5 60.9(4) . . ? B4 B3 B5 108.1(5) . . ? B6 B3 B5 59.8(4) . . ? C2 B5 B6 105.0(5) . . ? C2 B5 B3 57.0(4) . . ? B6 B5 B3 60.0(4) . . ? C2 B5 B8 104.9(5) . . ? B6 B5 B8 59.5(5) . . ? B3 B5 B8 105.9(6) . . ? C2 B5 B5 59.2(3) . 4_665 ? B6 B5 B5 107.9(4) . 4_665 ? B3 B5 B5 105.8(3) . 4_665 ? B8 B5 B5 59.9(3) . 4_665 ? C1 B4 B4 59.4(3) . 4_665 ? C1 B4 B7 105.4(5) . . ? B4 B4 B7 60.1(3) 4_665 . ? C1 B4 B3 57.9(4) . . ? B4 B4 B3 107.7(3) 4_665 . ? B7 B4 B3 107.8(6) . . ? C1 B4 B6 106.3(5) . . ? B4 B4 B6 109.5(3) 4_665 . ? B7 B4 B6 60.5(5) . . ? B3 B4 B6 60.8(4) . . ? B7 B6 B4 58.5(5) . . ? B7 B6 B8 58.0(6) . . ? B4 B6 B8 105.8(6) . . ? B7 B6 B5 106.6(6) . . ? B4 B6 B5 107.8(5) . . ? B8 B6 B5 60.9(6) . . ? B7 B6 B3 104.9(6) . . ? B4 B6 B3 59.1(4) . . ? B8 B6 B3 107.1(6) . . ? B5 B6 B3 60.2(4) . . ? B7 B8 B6 60.5(5) . . ? B7 B8 B6 60.5(5) . 4_665 ? B6 B8 B6 109.4(9) . 4_665 ? B7 B8 B5 107.5(7) . 4_665 ? B6 B8 B5 108.2(7) . 4_665 ? B6 B8 B5 59.6(4) 4_665 4_665 ? B7 B8 B5 107.5(7) . . ? B6 B8 B5 59.6(4) . . ? B6 B8 B5 108.2(7) 4_665 . ? B5 B8 B5 60.3(6) 4_665 . ? B8 B7 B4 110.6(7) . . ? B8 B7 B4 110.6(7) . 4_665 ? B4 B7 B4 59.8(6) . 4_665 ? B8 B7 B6 61.6(5) . 4_665 ? B4 B7 B6 109.7(7) . 4_665 ? B4 B7 B6 61.0(4) 4_665 4_665 ? B8 B7 B6 61.6(5) . . ? B4 B7 B6 61.0(4) . . ? B4 B7 B6 109.7(7) 4_665 . ? B6 B7 B6 111.1(8) 4_665 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.204 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.054 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.127 421.0 6.1 2 0.333 0.667 0.045 427.6 5.5 3 0.667 0.333 0.017 424.1 5.9 _platon_squeeze_details ; ; #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 665267' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H32 B10 N2 Ti' _chemical_formula_weight 396.43 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 26.0448(12) _cell_length_b 26.0448(12) _cell_length_c 9.8439(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5782.8(7) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 879 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 22.12 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.819524 _exptl_absorpt_correction_T_max 1.0000 _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 SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13291 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.02 _reflns_number_total 2834 _reflns_number_gt 2321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0726P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 2834 _refine_ls_number_parameters 139 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.506785(12) 0.493215(12) 0.05770(5) 0.04142(16) Uani 1 2 d S . . N1 N 0.42795(10) 0.45694(10) -0.0042(2) 0.0562(6) Uani 1 1 d . . . B3 B 0.56314(12) 0.54597(10) 0.3677(3) 0.0443(6) Uani 1 1 d . . . H3 H 0.6061 0.5736 0.3173 0.053 Uiso 1 1 calc R . . B4 B 0.55707(13) 0.51101(13) 0.5285(3) 0.0524(7) Uani 1 1 d . . . H4 H 0.5960 0.5161 0.5838 0.063 Uiso 1 1 calc R . . B5 B 0.50568(12) 0.56207(11) 0.3587(3) 0.0477(6) Uani 1 1 d . . . H5 H 0.5110 0.6011 0.3030 0.057 Uiso 1 1 calc R . . B6 B 0.54130(15) 0.56921(14) 0.5152(3) 0.0578(7) Uani 1 1 d . . . H6 H 0.5704 0.6127 0.5617 0.069 Uiso 1 1 calc R . . B7 B 0.49426(11) 0.50574(11) 0.6131(5) 0.0584(11) Uani 1 2 d S . . H7 H 0.4922 0.5078 0.7244 0.070 Uiso 1 2 calc SR . . B8 B 0.46289(11) 0.53711(11) 0.5123(5) 0.0604(11) Uani 1 2 d S . . H8 H 0.4406 0.5594 0.5574 0.072 Uiso 1 2 calc SR . . C1 C 0.52966(7) 0.47034(7) 0.3805(3) 0.0409(7) Uani 1 2 d S . . C2 C 0.49946(7) 0.50054(7) 0.2786(3) 0.0367(6) Uani 1 2 d S . . C11 C 0.56065(7) 0.43935(7) 0.3062(4) 0.0456(7) Uani 1 2 d S . . C12 C 0.53169(13) 0.37403(11) 0.3471(3) 0.0640(7) Uani 1 1 d . . . H12A H 0.5512 0.3560 0.3012 0.096 Uiso 1 1 calc R . . H12B H 0.4905 0.3540 0.3223 0.096 Uiso 1 1 calc R . . H12C H 0.5352 0.3712 0.4435 0.096 Uiso 1 1 calc R . . C13 C 0.55528(7) 0.44472(7) 0.1542(4) 0.0461(7) Uani 1 2 d S . . C14 C 0.59618(11) 0.49032(13) 0.0703(3) 0.0548(6) Uani 1 1 d . . . H14 H 0.6311 0.5235 0.0985 0.066 Uiso 1 1 calc R . . C15 C 0.57513(13) 0.47710(16) -0.0650(3) 0.0687(8) Uani 1 1 d . . . H15 H 0.5938 0.5002 -0.1410 0.082 Uiso 1 1 calc R . . C16 C 0.38398(14) 0.39653(16) -0.0387(4) 0.0883(11) Uani 1 1 d . . . H16A H 0.3480 0.3952 -0.0667 0.133 Uiso 1 1 calc R . . H16B H 0.3762 0.3716 0.0393 0.133 Uiso 1 1 calc R . . H16C H 0.3986 0.3828 -0.1114 0.133 Uiso 1 1 calc R . . C17 C 0.40530(14) 0.49730(16) -0.0430(4) 0.0790(9) Uani 1 1 d . . . H17A H 0.4028 0.4977 -0.1412 0.095 Uiso 1 1 calc R . . H17B H 0.3654 0.4810 -0.0076 0.095 Uiso 1 1 calc R . . C18 C 0.44086(10) 0.55914(10) 0.0047(5) 0.0788(13) Uani 1 2 d S . . H18A H 0.4416 0.5584 0.1032 0.095 Uiso 1 2 calc SR . . H18B H 0.4201 0.5799 -0.0210 0.095 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0416(2) 0.0416(2) 0.0358(3) 0.00097(13) -0.00097(13) 0.0168(3) N1 0.0469(11) 0.0632(13) 0.0471(13) -0.0017(10) -0.0104(9) 0.0191(10) B3 0.0420(13) 0.0351(12) 0.0435(14) -0.0012(10) -0.0068(11) 0.0100(10) B4 0.0512(15) 0.0517(15) 0.0400(14) -0.0006(11) -0.0115(12) 0.0148(13) B5 0.0510(15) 0.0378(12) 0.0477(15) -0.0010(11) -0.0020(12) 0.0173(11) B6 0.0624(18) 0.0528(17) 0.0535(19) -0.0126(14) -0.0127(14) 0.0253(14) B7 0.0669(19) 0.0669(19) 0.036(2) 0.0006(9) -0.0006(9) 0.029(2) B8 0.0627(18) 0.0627(18) 0.050(3) -0.0025(11) 0.0025(11) 0.027(2) C1 0.0353(10) 0.0353(10) 0.0429(18) 0.0029(7) -0.0029(7) 0.0108(12) C2 0.0348(10) 0.0348(10) 0.0364(16) 0.0022(6) -0.0022(6) 0.0145(11) C11 0.0457(12) 0.0457(12) 0.0441(18) 0.0030(7) -0.0030(7) 0.0220(14) C12 0.0764(18) 0.0497(14) 0.0703(19) 0.0060(13) -0.0008(15) 0.0348(14) C13 0.0419(12) 0.0419(12) 0.054(2) -0.0002(7) 0.0002(7) 0.0207(14) C14 0.0466(13) 0.0649(14) 0.0530(15) 0.0034(12) 0.0065(12) 0.0279(13) C15 0.0712(17) 0.088(2) 0.0561(17) 0.0092(14) 0.0231(14) 0.0472(15) C16 0.0597(18) 0.076(2) 0.096(3) -0.0103(19) -0.0211(17) 0.0087(16) C17 0.0617(17) 0.100(3) 0.079(2) 0.0048(19) -0.0183(16) 0.0430(18) C18 0.088(3) 0.088(3) 0.078(3) 0.0061(11) -0.0061(11) 0.057(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 Ti1 N1 1.882(2) . ? Ti1 N1 1.882(2) 4_665 ? Ti1 C2 2.199(3) . ? Ti1 C15 2.356(3) 4_665 ? Ti1 C15 2.356(3) . ? Ti1 C14 2.370(2) . ? Ti1 C14 2.370(2) 4_665 ? Ti1 C13 2.385(3) . ? N1 C16 1.449(4) . ? N1 C17 1.489(4) . ? B3 C1 1.714(3) . ? B3 C2 1.720(3) . ? B3 B5 1.747(4) . ? B3 B6 1.773(4) . ? B3 B4 1.793(4) . ? B4 C1 1.731(4) . ? B4 B6 1.762(5) . ? B4 B4 1.773(6) 4_665 ? B4 B7 1.779(5) . ? B5 C2 1.720(4) . ? B5 B6 1.760(4) . ? B5 B5 1.765(5) 4_665 ? B5 B8 1.796(5) . ? B6 B7 1.771(4) . ? B6 B8 1.779(4) . ? B7 B8 1.728(7) . ? B7 B6 1.771(4) 4_665 ? B7 B4 1.779(5) 4_665 ? B8 B6 1.779(4) 4_665 ? B8 B5 1.796(5) 4_665 ? C1 C11 1.578(5) . ? C1 C2 1.692(4) . ? C1 B3 1.714(3) 4_665 ? C1 B4 1.731(4) 4_665 ? C2 B5 1.720(4) 4_665 ? C2 B3 1.720(3) 4_665 ? C11 C13 1.516(5) . ? C11 C12 1.530(3) 4_665 ? C11 C12 1.530(3) . ? C13 C14 1.401(4) . ? C13 C14 1.401(4) 4_665 ? C14 C15 1.416(4) . ? C15 C15 1.360(7) 4_665 ? C17 C18 1.477(4) . ? C18 C17 1.477(4) 4_665 ? 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 N1 Ti1 N1 105.63(14) . 4_665 ? N1 Ti1 C2 104.10(8) . . ? N1 Ti1 C2 104.10(8) 4_665 . ? N1 Ti1 C15 90.95(11) . 4_665 ? N1 Ti1 C15 118.46(11) 4_665 4_665 ? C2 Ti1 C15 128.93(11) . 4_665 ? N1 Ti1 C15 118.46(11) . . ? N1 Ti1 C15 90.95(11) 4_665 . ? C2 Ti1 C15 128.93(11) . . ? C15 Ti1 C15 33.56(17) 4_665 . ? N1 Ti1 C14 147.54(11) . . ? N1 Ti1 C14 94.96(10) 4_665 . ? C2 Ti1 C14 94.61(10) . . ? C15 Ti1 C14 56.89(11) 4_665 . ? C15 Ti1 C14 34.85(10) . . ? N1 Ti1 C14 94.96(10) . 4_665 ? N1 Ti1 C14 147.54(11) 4_665 4_665 ? C2 Ti1 C14 94.61(10) . 4_665 ? C15 Ti1 C14 34.85(10) 4_665 4_665 ? C15 Ti1 C14 56.89(11) . 4_665 ? C14 Ti1 C14 56.76(14) . 4_665 ? N1 Ti1 C13 126.66(7) . . ? N1 Ti1 C13 126.66(7) 4_665 . ? C2 Ti1 C13 75.17(12) . . ? C15 Ti1 C13 57.48(11) 4_665 . ? C15 Ti1 C13 57.48(11) . . ? C14 Ti1 C13 34.27(8) . . ? C14 Ti1 C13 34.27(8) 4_665 . ? C16 N1 C17 109.2(3) . . ? C16 N1 Ti1 133.8(2) . . ? C17 N1 Ti1 116.52(19) . . ? C1 B3 C2 59.04(15) . . ? C1 B3 B5 105.97(19) . . ? C2 B3 B5 59.47(16) . . ? C1 B3 B6 105.4(2) . . ? C2 B3 B6 106.8(2) . . ? B5 B3 B6 60.00(17) . . ? C1 B3 B4 59.09(16) . . ? C2 B3 B4 106.91(18) . . ? B5 B3 B4 107.4(2) . . ? B6 B3 B4 59.24(18) . . ? C1 B4 B6 105.2(2) . . ? C1 B4 B4 59.19(11) . 4_665 ? B6 B4 B4 108.27(14) . 4_665 ? C1 B4 B7 105.4(2) . . ? B6 B4 B7 60.01(19) . . ? B4 B4 B7 60.11(12) 4_665 . ? C1 B4 B3 58.19(14) . . ? B6 B4 B3 59.81(17) . . ? B4 B4 B3 107.34(12) 4_665 . ? B7 B4 B3 107.3(2) . . ? C2 B5 B3 59.48(14) . . ? C2 B5 B6 107.4(2) . . ? B3 B5 B6 60.74(17) . . ? C2 B5 B5 59.13(11) . 4_665 ? B3 B5 B5 107.96(11) . 4_665 ? B6 B5 B5 108.45(14) . 4_665 ? C2 B5 B8 107.2(2) . . ? B3 B5 B8 108.7(2) . . ? B6 B5 B8 60.01(19) . . ? B5 B5 B8 60.58(12) 4_665 . ? B5 B6 B4 108.1(2) . . ? B5 B6 B7 107.2(2) . . ? B4 B6 B7 60.5(2) . . ? B5 B6 B3 59.26(17) . . ? B4 B6 B3 60.95(17) . . ? B7 B6 B3 108.5(2) . . ? B5 B6 B8 61.0(2) . . ? B4 B6 B8 107.7(2) . . ? B7 B6 B8 58.3(2) . . ? B3 B6 B8 108.4(2) . . ? B8 B7 B6 61.08(18) . 4_665 ? B8 B7 B6 61.08(18) . . ? B6 B7 B6 108.7(3) 4_665 . ? B8 B7 B4 109.2(3) . 4_665 ? B6 B7 B4 59.53(18) 4_665 4_665 ? B6 B7 B4 107.6(3) . 4_665 ? B8 B7 B4 109.2(3) . . ? B6 B7 B4 107.6(3) 4_665 . ? B6 B7 B4 59.53(18) . . ? B4 B7 B4 59.8(2) 4_665 . ? B7 B8 B6 60.65(18) . . ? B7 B8 B6 60.65(18) . 4_665 ? B6 B8 B6 108.0(3) . 4_665 ? B7 B8 B5 107.5(3) . 4_665 ? B6 B8 B5 106.2(3) . 4_665 ? B6 B8 B5 58.98(18) 4_665 4_665 ? B7 B8 B5 107.5(3) . . ? B6 B8 B5 58.98(18) . . ? B6 B8 B5 106.2(3) 4_665 . ? B5 B8 B5 58.8(2) 4_665 . ? C11 C1 C2 116.0(3) . . ? C11 C1 B3 117.20(16) . . ? C2 C1 B3 60.64(13) . . ? C11 C1 B3 117.20(16) . 4_665 ? C2 C1 B3 60.64(13) . 4_665 ? B3 C1 B3 112.0(3) . 4_665 ? C11 C1 B4 122.9(2) . . ? C2 C1 B4 111.1(2) . . ? B3 C1 B4 62.72(15) . . ? B3 C1 B4 113.0(2) 4_665 . ? C11 C1 B4 122.9(2) . 4_665 ? C2 C1 B4 111.1(2) . 4_665 ? B3 C1 B4 113.0(2) . 4_665 ? B3 C1 B4 62.72(15) 4_665 4_665 ? B4 C1 B4 61.6(2) . 4_665 ? C1 C2 B5 108.2(2) . . ? C1 C2 B5 108.2(2) . 4_665 ? B5 C2 B5 61.7(2) . 4_665 ? C1 C2 B3 60.32(13) . . ? B5 C2 B3 61.05(15) . . ? B5 C2 B3 111.3(2) 4_665 . ? C1 C2 B3 60.32(13) . 4_665 ? B5 C2 B3 111.3(2) . 4_665 ? B5 C2 B3 61.05(15) 4_665 4_665 ? B3 C2 B3 111.4(2) . 4_665 ? C1 C2 Ti1 117.74(19) . . ? B5 C2 Ti1 124.21(17) . . ? B5 C2 Ti1 124.21(17) 4_665 . ? B3 C2 Ti1 117.92(14) . . ? B3 C2 Ti1 117.92(14) 4_665 . ? C13 C11 C12 110.2(2) . 4_665 ? C13 C11 C12 110.2(2) . . ? C12 C11 C12 106.7(3) 4_665 . ? C13 C11 C1 108.4(3) . . ? C12 C11 C1 110.7(2) 4_665 . ? C12 C11 C1 110.7(2) . . ? C14 C13 C14 107.0(3) . 4_665 ? C14 C13 C11 126.45(17) . . ? C14 C13 C11 126.45(17) 4_665 . ? C14 C13 Ti1 72.29(16) . . ? C14 C13 Ti1 72.29(16) 4_665 . ? C11 C13 Ti1 122.7(2) . . ? C13 C14 C15 108.1(3) . . ? C13 C14 Ti1 73.45(15) . . ? C15 C14 Ti1 72.03(15) . . ? C15 C15 C14 108.38(17) 4_665 . ? C15 C15 Ti1 73.22(9) 4_665 . ? C14 C15 Ti1 73.11(15) . . ? C18 C17 N1 115.8(3) . . ? C17 C18 C17 118.4(5) . 4_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.216 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.049 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.041 410.0 201.5 2 0.333 0.667 0.094 415.4 202.0 3 0.667 0.333 -0.088 415.1 202.0 _platon_squeeze_details ; ; #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 665268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H51 B10 N4 Ti' _chemical_formula_weight 683.80 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.500(2) _cell_length_b 17.092(3) _cell_length_c 21.352(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.56(3) _cell_angle_gamma 90.00 _cell_volume 3789.5(13) _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 Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.94334 _exptl_absorpt_correction_T_max 1.0000 _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 'AFC7R RIGAKU DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7069 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.1842 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6681 _reflns_number_gt 2919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0892P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6681 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2147 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.2227 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.45742(8) 0.31881(5) 0.24971(4) 0.0416(3) Uani 1 1 d . . . N1 N 0.3877(4) 0.2050(3) 0.2241(2) 0.0488(12) Uani 1 1 d . . . N2 N 0.2322(5) 0.2142(3) 0.2961(3) 0.0807(17) Uani 1 1 d . . . N3 N 0.4116(5) 0.3157(3) 0.3993(2) 0.0695(14) Uani 1 1 d . . . N4 N 0.5817(4) 0.3319(2) 0.33583(19) 0.0507(12) Uani 1 1 d . . . C1 C 0.6434(5) 0.3606(3) 0.1345(2) 0.0496(14) Uani 1 1 d . . . C2 C 0.6267(5) 0.2978(3) 0.1958(2) 0.0429(13) Uani 1 1 d . . . C11 C 0.5389(5) 0.4260(3) 0.1220(3) 0.0539(15) Uani 1 1 d . . . C12 C 0.6002(7) 0.5079(3) 0.1270(3) 0.085(2) Uani 1 1 d . . . H12A H 0.5340 0.5468 0.1183 0.128 Uiso 1 1 calc R . . H12B H 0.6591 0.5125 0.0968 0.128 Uiso 1 1 calc R . . H12C H 0.6458 0.5155 0.1690 0.128 Uiso 1 1 calc R . . C13 C 0.4627(7) 0.4180(4) 0.0554(3) 0.087(2) Uani 1 1 d . . . H13A H 0.3999 0.4592 0.0483 0.131 Uiso 1 1 calc R . . H13B H 0.4199 0.3683 0.0515 0.131 Uiso 1 1 calc R . . H13C H 0.5205 0.4217 0.0247 0.131 Uiso 1 1 calc R . . C14 C 0.4465(5) 0.4189(3) 0.1706(2) 0.0470(13) Uani 1 1 d . . . C15 C 0.3292(5) 0.3792(4) 0.1614(3) 0.0613(16) Uani 1 1 d . . . H15A H 0.2906 0.3530 0.1224 0.074 Uiso 1 1 calc R . . C16 C 0.2699(6) 0.3912(4) 0.2155(4) 0.076(2) Uani 1 1 d . . . H16A H 0.1820 0.3757 0.2202 0.091 Uiso 1 1 calc R . . C17 C 0.3509(6) 0.4372(4) 0.2575(3) 0.0680(18) Uani 1 1 d . . . H17A H 0.3293 0.4601 0.2967 0.082 Uiso 1 1 calc R . . C18 C 0.4590(6) 0.4557(3) 0.2296(3) 0.0565(15) Uani 1 1 d . . . H18A H 0.5274 0.4923 0.2465 0.068 Uiso 1 1 calc R . . C21 C 0.3737(5) 0.1307(3) 0.1926(3) 0.0563(15) Uani 1 1 d . . . C22 C 0.2922(6) 0.1243(4) 0.1356(3) 0.0657(17) Uani 1 1 d . . . C23 C 0.2907(8) 0.0553(5) 0.1024(3) 0.093(2) Uani 1 1 d . . . H23A H 0.2360 0.0498 0.0641 0.111 Uiso 1 1 calc R . . C24 C 0.3699(9) -0.0057(5) 0.1256(5) 0.100(3) Uani 1 1 d . . . H24A H 0.3736 -0.0506 0.1012 0.120 Uiso 1 1 calc R . . C25 C 0.4423(7) -0.0009(4) 0.1834(4) 0.083(2) Uani 1 1 d . . . H25A H 0.4909 -0.0439 0.1993 0.099 Uiso 1 1 calc R . . C26 C 0.4456(6) 0.0672(4) 0.2196(3) 0.0637(16) Uani 1 1 d . . . C27 C 0.2065(7) 0.1911(5) 0.1089(3) 0.100(3) Uani 1 1 d . . . H27A H 0.2189 0.2349 0.1373 0.150 Uiso 1 1 calc R . . H27B H 0.1181 0.1748 0.1039 0.150 Uiso 1 1 calc R . . H27C H 0.2282 0.2061 0.0684 0.150 Uiso 1 1 calc R . . C28 C 0.5241(7) 0.0710(4) 0.2833(3) 0.089(2) Uani 1 1 d . . . H28A H 0.5151 0.1218 0.3014 0.134 Uiso 1 1 calc R . . H28B H 0.6129 0.0619 0.2798 0.134 Uiso 1 1 calc R . . H28C H 0.4949 0.0318 0.3101 0.134 Uiso 1 1 calc R . . C31 C 0.6982(6) 0.3420(4) 0.3796(3) 0.0565(15) Uani 1 1 d . . . C32 C 0.7638(6) 0.2760(4) 0.4066(3) 0.0680(17) Uani 1 1 d . . . C33 C 0.8784(7) 0.2864(5) 0.4471(3) 0.088(2) Uani 1 1 d . . . H33A H 0.9244 0.2430 0.4643 0.106 Uiso 1 1 calc R . . C34 C 0.9251(8) 0.3609(7) 0.4623(4) 0.102(3) Uani 1 1 d . . . H34A H 1.0021 0.3675 0.4895 0.122 Uiso 1 1 calc R . . C35 C 0.8585(8) 0.4237(5) 0.4374(3) 0.091(2) Uani 1 1 d . . . H35A H 0.8901 0.4735 0.4483 0.109 Uiso 1 1 calc R . . C36 C 0.7439(7) 0.4161(4) 0.3960(3) 0.0694(18) Uani 1 1 d . . . C37 C 0.7123(8) 0.1958(4) 0.3928(3) 0.099(3) Uani 1 1 d . . . H37A H 0.6326 0.1988 0.3643 0.148 Uiso 1 1 calc R . . H37B H 0.6978 0.1712 0.4315 0.148 Uiso 1 1 calc R . . H37C H 0.7734 0.1657 0.3737 0.148 Uiso 1 1 calc R . . C38 C 0.6731(8) 0.4891(4) 0.3716(4) 0.107(3) Uani 1 1 d . . . H38A H 0.5962 0.4749 0.3437 0.160 Uiso 1 1 calc R . . H38B H 0.7273 0.5202 0.3489 0.160 Uiso 1 1 calc R . . H38C H 0.6506 0.5186 0.4066 0.160 Uiso 1 1 calc R . . C41 C 0.3260(5) 0.2368(3) 0.2641(3) 0.0600(16) Uani 1 1 d . . . C42 C 0.1713(7) 0.1380(4) 0.2917(3) 0.093(2) Uani 1 1 d . . . H42A H 0.2053 0.1070 0.2606 0.139 Uiso 1 1 calc R . . H42B H 0.0800 0.1441 0.2796 0.139 Uiso 1 1 calc R . . H42C H 0.1880 0.1123 0.3321 0.139 Uiso 1 1 calc R . . C43 C 0.1970(7) 0.2705(6) 0.3421(4) 0.119(3) Uani 1 1 d . . . H43A H 0.1827 0.3206 0.3209 0.143 Uiso 1 1 calc R . . H43B H 0.1152 0.2541 0.3537 0.143 Uiso 1 1 calc R . . C44 C 0.2816(7) 0.2824(6) 0.3974(3) 0.111(3) Uani 1 1 d . . . H44A H 0.2928 0.2320 0.4184 0.134 Uiso 1 1 calc R . . H44B H 0.2372 0.3155 0.4241 0.134 Uiso 1 1 calc R . . C45 C 0.4668(6) 0.3211(3) 0.3460(2) 0.0561(14) Uani 1 1 d . . . C46 C 0.4817(7) 0.3256(5) 0.4627(3) 0.107(3) Uani 1 1 d . . . H46A H 0.5635 0.3496 0.4602 0.160 Uiso 1 1 calc R . . H46B H 0.4950 0.2755 0.4829 0.160 Uiso 1 1 calc R . . H46C H 0.4330 0.3584 0.4869 0.160 Uiso 1 1 calc R . . C51 C 0.077(2) 0.4472(13) 0.0109(15) 0.187(6) Uani 1 1 d . . . H51A H 0.1334 0.4058 0.0215 0.224 Uiso 1 1 calc R . . C52 C 0.100(2) 0.512(3) 0.0403(11) 0.257(10) Uani 1 1 d . . . H52A H 0.1767 0.5201 0.0675 0.309 Uiso 1 1 calc R . . C53 C 0.020(4) 0.5639(11) 0.0319(10) 0.197(7) Uani 1 1 d . . . H53 H 0.0285 0.6096 0.0558 0.237 Uiso 1 1 calc R . . B3 B 0.5952(6) 0.2675(4) 0.1178(3) 0.0504(17) Uani 1 1 d . . . H3 H 0.4972 0.2519 0.0957 0.060 Uiso 1 1 calc R . . B4 B 0.7054(7) 0.3154(4) 0.0747(3) 0.0628(19) Uani 1 1 d . . . H4 H 0.6803 0.3304 0.0243 0.075 Uiso 1 1 calc R . . B5 B 0.8019(7) 0.3775(5) 0.1292(4) 0.069(2) Uani 1 1 d . . . H5 H 0.8404 0.4334 0.1146 0.083 Uiso 1 1 calc R . . B6 B 0.7470(6) 0.3658(4) 0.2032(3) 0.0569(18) Uani 1 1 d . . . H6 H 0.7479 0.4147 0.2368 0.068 Uiso 1 1 calc R . . B7 B 0.6840(6) 0.2076(4) 0.1752(3) 0.0539(17) Uani 1 1 d . . . H7 H 0.6454 0.1519 0.1900 0.065 Uiso 1 1 calc R . . B8 B 0.7343(7) 0.2192(4) 0.1003(3) 0.0629(19) Uani 1 1 d . . . H8 H 0.7284 0.1710 0.0659 0.076 Uiso 1 1 calc R . . B9 B 0.8622(7) 0.2864(5) 0.1078(4) 0.071(2) Uani 1 1 d . . . H9 H 0.9405 0.2823 0.0790 0.085 Uiso 1 1 calc R . . B10 B 0.8892(6) 0.3186(5) 0.1877(4) 0.074(2) Uani 1 1 d . . . H10 H 0.9854 0.3362 0.2113 0.088 Uiso 1 1 calc R . . B11 B 0.7790(6) 0.2693(4) 0.2284(3) 0.0585(18) Uani 1 1 d . . . H11 H 0.8038 0.2543 0.2789 0.070 Uiso 1 1 calc R . . B12 B 0.8496(6) 0.2184(4) 0.1702(3) 0.064(2) Uani 1 1 d . . . H12 H 0.9188 0.1704 0.1819 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0410(5) 0.0417(5) 0.0428(5) 0.0069(5) 0.0085(4) 0.0027(5) N1 0.039(3) 0.055(3) 0.053(3) 0.011(2) 0.007(2) -0.001(2) N2 0.078(4) 0.077(4) 0.101(4) -0.025(3) 0.056(3) -0.033(3) N3 0.069(3) 0.095(4) 0.048(3) -0.009(3) 0.021(3) -0.009(3) N4 0.051(3) 0.053(3) 0.048(3) 0.008(2) 0.010(2) -0.001(2) C1 0.054(3) 0.051(3) 0.047(3) 0.002(3) 0.017(3) -0.002(3) C2 0.040(3) 0.047(3) 0.042(3) 0.007(2) 0.006(2) 0.001(2) C11 0.068(4) 0.041(3) 0.056(4) 0.009(3) 0.022(3) 0.001(3) C12 0.105(5) 0.051(4) 0.114(6) 0.010(4) 0.064(5) 0.000(4) C13 0.118(6) 0.091(5) 0.054(4) 0.032(4) 0.018(4) 0.031(5) C14 0.048(3) 0.042(3) 0.052(3) 0.011(3) 0.009(3) 0.007(3) C15 0.052(4) 0.071(4) 0.057(4) 0.024(3) -0.005(3) 0.000(3) C16 0.040(3) 0.080(5) 0.108(6) 0.047(4) 0.015(4) 0.017(4) C17 0.069(4) 0.059(4) 0.084(5) 0.026(4) 0.036(4) 0.028(4) C18 0.063(4) 0.035(3) 0.074(4) 0.011(3) 0.020(3) 0.009(3) C21 0.051(3) 0.052(4) 0.070(4) 0.001(3) 0.022(3) -0.010(3) C22 0.065(4) 0.071(5) 0.060(4) -0.005(4) 0.008(3) -0.020(4) C23 0.097(6) 0.115(7) 0.071(5) -0.020(5) 0.026(4) -0.028(5) C24 0.111(7) 0.092(7) 0.112(7) -0.033(6) 0.068(6) -0.023(6) C25 0.085(5) 0.058(5) 0.115(6) 0.002(5) 0.046(5) 0.001(4) C26 0.056(4) 0.055(4) 0.084(5) 0.005(4) 0.023(3) -0.009(3) C27 0.089(5) 0.120(7) 0.082(5) -0.003(5) -0.019(4) -0.021(5) C28 0.099(5) 0.070(5) 0.093(5) 0.021(4) -0.006(5) -0.006(4) C31 0.064(4) 0.067(4) 0.040(3) -0.002(3) 0.011(3) -0.008(3) C32 0.071(4) 0.076(5) 0.054(4) 0.007(3) -0.001(3) -0.003(4) C33 0.081(5) 0.115(7) 0.067(5) 0.021(5) 0.003(4) 0.010(5) C34 0.079(6) 0.156(9) 0.068(5) -0.001(6) 0.006(4) -0.022(6) C35 0.100(6) 0.099(6) 0.074(5) -0.002(5) 0.011(5) -0.036(5) C36 0.079(5) 0.080(5) 0.050(4) -0.001(3) 0.013(3) -0.013(4) C37 0.133(7) 0.070(5) 0.086(5) 0.021(4) -0.007(5) 0.006(5) C38 0.146(7) 0.058(5) 0.107(6) -0.018(4) -0.010(6) -0.014(5) C41 0.053(4) 0.056(4) 0.075(4) 0.003(3) 0.020(3) 0.001(3) C42 0.097(5) 0.099(6) 0.090(5) -0.006(4) 0.039(4) -0.050(5) C43 0.082(6) 0.154(8) 0.133(8) -0.056(7) 0.054(6) -0.038(6) C44 0.067(5) 0.203(10) 0.070(5) -0.038(6) 0.027(4) -0.010(6) C45 0.061(4) 0.057(4) 0.050(3) -0.001(3) 0.011(3) 0.006(3) C46 0.113(6) 0.158(8) 0.053(4) -0.013(5) 0.025(4) -0.031(6) C51 0.195(19) 0.158(17) 0.198(17) -0.021(13) -0.001(17) 0.009(13) C52 0.23(2) 0.26(3) 0.28(2) -0.04(3) 0.018(18) 0.07(3) C53 0.208(19) 0.201(19) 0.171(16) 0.001(13) -0.013(17) 0.038(19) B3 0.062(4) 0.041(4) 0.049(4) -0.005(3) 0.009(3) -0.005(3) B4 0.089(5) 0.054(4) 0.050(4) 0.000(4) 0.028(4) -0.006(4) B5 0.064(5) 0.076(5) 0.077(5) -0.018(4) 0.039(4) -0.021(4) B6 0.042(4) 0.071(5) 0.059(4) -0.012(4) 0.013(3) -0.014(4) B7 0.043(4) 0.049(4) 0.073(5) 0.002(3) 0.018(3) 0.009(3) B8 0.068(5) 0.060(5) 0.065(5) -0.009(4) 0.023(4) -0.004(4) B9 0.056(4) 0.071(5) 0.093(6) -0.012(4) 0.038(4) -0.006(4) B10 0.041(4) 0.098(6) 0.084(5) -0.029(5) 0.016(4) -0.003(4) B11 0.033(3) 0.077(5) 0.064(4) 0.001(4) 0.003(3) 0.005(4) B12 0.051(4) 0.062(5) 0.081(5) -0.003(4) 0.013(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 C41 2.023(6) . ? Ti1 C45 2.043(5) . ? Ti1 N4 2.102(4) . ? Ti1 N1 2.121(5) . ? Ti1 C2 2.285(5) . ? Ti1 C17 2.331(6) . ? Ti1 C16 2.348(6) . ? Ti1 C18 2.379(5) . ? Ti1 C15 2.383(5) . ? Ti1 C14 2.395(5) . ? N1 C41 1.270(7) . ? N1 C21 1.433(7) . ? N2 C41 1.336(7) . ? N2 C42 1.449(7) . ? N2 C43 1.461(8) . ? N3 C45 1.357(7) . ? N3 C46 1.450(7) . ? N3 C44 1.474(8) . ? N4 C45 1.270(6) . ? N4 C31 1.435(7) . ? C1 C11 1.561(7) . ? C1 B3 1.692(8) . ? C1 B6 1.693(8) . ? C1 B4 1.704(8) . ? C1 B5 1.710(8) . ? C1 C2 1.722(7) . ? C2 B6 1.707(8) . ? C2 B11 1.718(8) . ? C2 B3 1.728(8) . ? C2 B7 1.735(8) . ? C11 C14 1.527(7) . ? C11 C13 1.530(8) . ? C11 C12 1.537(8) . ? C14 C15 1.394(7) . ? C14 C18 1.396(7) . ? C15 C16 1.405(8) . ? C16 C17 1.385(9) . ? C17 C18 1.395(7) . ? C21 C22 1.385(8) . ? C21 C26 1.396(8) . ? C22 C23 1.376(9) . ? C22 C27 1.512(9) . ? C23 C24 1.380(10) . ? C24 C25 1.352(10) . ? C25 C26 1.395(9) . ? C26 C28 1.485(8) . ? C31 C36 1.382(8) . ? C31 C32 1.399(8) . ? C32 C33 1.386(9) . ? C32 C37 1.487(8) . ? C33 C34 1.386(11) . ? C34 C35 1.346(10) . ? C35 C36 1.390(9) . ? C36 C38 1.504(9) . ? C43 C44 1.384(9) . ? C51 C53 1.27(2) 3_565 ? C51 C52 1.29(2) . ? C52 C53 1.21(2) . ? C53 C51 1.27(2) 3_565 ? B3 B7 1.755(9) . ? B3 B8 1.765(9) . ? B3 B4 1.781(9) . ? B4 B8 1.744(10) . ? B4 B9 1.763(10) . ? B4 B5 1.776(10) . ? B5 B10 1.753(11) . ? B5 B9 1.765(10) . ? B5 B6 1.772(9) . ? B6 B11 1.751(10) . ? B6 B10 1.771(9) . ? B7 B11 1.750(9) . ? B7 B12 1.767(9) . ? B7 B8 1.768(9) . ? B8 B9 1.756(10) . ? B8 B12 1.775(10) . ? B9 B10 1.775(10) . ? B9 B12 1.788(11) . ? B10 B11 1.762(10) . ? B10 B12 1.790(10) . ? B11 B12 1.769(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Ti1 C45 78.0(2) . . ? C41 Ti1 N4 106.8(2) . . ? C45 Ti1 N4 35.63(18) . . ? C41 Ti1 N1 35.59(19) . . ? C45 Ti1 N1 103.9(2) . . ? N4 Ti1 N1 117.96(16) . . ? C41 Ti1 C2 124.5(2) . . ? C45 Ti1 C2 125.8(2) . . ? N4 Ti1 C2 91.69(18) . . ? N1 Ti1 C2 89.42(17) . . ? C41 Ti1 C17 104.2(2) . . ? C45 Ti1 C17 82.1(2) . . ? N4 Ti1 C17 95.0(2) . . ? N1 Ti1 C17 131.6(2) . . ? C2 Ti1 C17 126.17(19) . . ? C41 Ti1 C16 81.6(2) . . ? C45 Ti1 C16 102.5(3) . . ? N4 Ti1 C16 126.8(2) . . ? N1 Ti1 C16 99.3(2) . . ? C2 Ti1 C16 127.2(2) . . ? C17 Ti1 C16 34.4(2) . . ? C41 Ti1 C18 137.1(2) . . ? C45 Ti1 C18 99.3(2) . . ? N4 Ti1 C18 91.91(19) . . ? N1 Ti1 C18 150.04(19) . . ? C2 Ti1 C18 92.11(18) . . ? C17 Ti1 C18 34.43(18) . . ? C16 Ti1 C18 56.9(2) . . ? C41 Ti1 C15 95.9(2) . . ? C45 Ti1 C15 136.4(2) . . ? N4 Ti1 C15 148.2(2) . . ? N1 Ti1 C15 93.47(19) . . ? C2 Ti1 C15 93.43(19) . . ? C17 Ti1 C15 57.3(2) . . ? C16 Ti1 C15 34.6(2) . . ? C18 Ti1 C15 56.6(2) . . ? C41 Ti1 C14 129.8(2) . . ? C45 Ti1 C14 133.3(2) . . ? N4 Ti1 C14 119.95(18) . . ? N1 Ti1 C14 119.63(18) . . ? C2 Ti1 C14 73.51(17) . . ? C17 Ti1 C14 57.11(19) . . ? C16 Ti1 C14 56.91(19) . . ? C18 Ti1 C14 34.01(17) . . ? C15 Ti1 C14 33.93(17) . . ? C41 N1 C21 131.8(5) . . ? C41 N1 Ti1 68.0(3) . . ? C21 N1 Ti1 160.2(4) . . ? C41 N2 C42 125.4(5) . . ? C41 N2 C43 115.7(6) . . ? C42 N2 C43 118.8(5) . . ? C45 N3 C46 123.7(5) . . ? C45 N3 C44 120.9(5) . . ? C46 N3 C44 114.2(5) . . ? C45 N4 C31 130.2(5) . . ? C45 N4 Ti1 69.6(3) . . ? C31 N4 Ti1 160.1(4) . . ? C11 C1 B3 117.2(4) . . ? C11 C1 B6 117.2(5) . . ? B3 C1 B6 111.4(4) . . ? C11 C1 B4 122.3(5) . . ? B3 C1 B4 63.2(4) . . ? B6 C1 B4 113.9(5) . . ? C11 C1 B5 122.3(5) . . ? B3 C1 B5 114.0(5) . . ? B6 C1 B5 62.8(4) . . ? B4 C1 B5 62.7(4) . . ? C11 C1 C2 115.4(4) . . ? B3 C1 C2 60.8(3) . . ? B6 C1 C2 60.0(3) . . ? B4 C1 C2 112.3(4) . . ? B5 C1 C2 111.5(4) . . ? B6 C2 B11 61.5(4) . . ? B6 C2 C1 59.2(3) . . ? B11 C2 C1 106.9(4) . . ? B6 C2 B3 109.0(4) . . ? B11 C2 B3 109.8(4) . . ? C1 C2 B3 58.7(3) . . ? B6 C2 B7 110.4(4) . . ? B11 C2 B7 60.9(3) . . ? C1 C2 B7 106.4(4) . . ? B3 C2 B7 60.9(3) . . ? B6 C2 Ti1 117.9(3) . . ? B11 C2 Ti1 126.0(3) . . ? C1 C2 Ti1 117.3(3) . . ? B3 C2 Ti1 118.8(3) . . ? B7 C2 Ti1 126.4(3) . . ? C14 C11 C13 109.1(5) . . ? C14 C11 C12 109.1(5) . . ? C13 C11 C12 107.5(5) . . ? C14 C11 C1 109.1(4) . . ? C13 C11 C1 110.6(5) . . ? C12 C11 C1 111.3(5) . . ? C15 C14 C18 107.9(5) . . ? C15 C14 C11 125.5(5) . . ? C18 C14 C11 126.4(5) . . ? C15 C14 Ti1 72.6(3) . . ? C18 C14 Ti1 72.4(3) . . ? C11 C14 Ti1 124.6(3) . . ? C14 C15 C16 107.7(6) . . ? C14 C15 Ti1 73.5(3) . . ? C16 C15 Ti1 71.4(3) . . ? C17 C16 C15 108.1(5) . . ? C17 C16 Ti1 72.1(3) . . ? C15 C16 Ti1 74.1(3) . . ? C16 C17 C18 108.1(6) . . ? C16 C17 Ti1 73.5(4) . . ? C18 C17 Ti1 74.7(3) . . ? C17 C18 C14 108.1(6) . . ? C17 C18 Ti1 70.9(3) . . ? C14 C18 Ti1 73.6(3) . . ? C22 C21 C26 121.7(6) . . ? C22 C21 N1 119.3(5) . . ? C26 C21 N1 119.0(5) . . ? C23 C22 C21 118.7(7) . . ? C23 C22 C27 119.5(7) . . ? C21 C22 C27 121.8(6) . . ? C22 C23 C24 120.2(8) . . ? C25 C24 C23 120.6(8) . . ? C24 C25 C26 121.4(7) . . ? C25 C26 C21 117.0(7) . . ? C25 C26 C28 120.6(7) . . ? C21 C26 C28 122.4(6) . . ? C36 C31 C32 120.2(6) . . ? C36 C31 N4 120.3(6) . . ? C32 C31 N4 119.4(5) . . ? C33 C32 C31 118.9(7) . . ? C33 C32 C37 119.8(7) . . ? C31 C32 C37 121.3(6) . . ? C32 C33 C34 120.5(7) . . ? C35 C34 C33 119.7(7) . . ? C34 C35 C36 121.8(8) . . ? C31 C36 C35 118.8(7) . . ? C31 C36 C38 122.5(6) . . ? C35 C36 C38 118.7(7) . . ? N1 C41 N2 135.2(6) . . ? N1 C41 Ti1 76.4(3) . . ? N2 C41 Ti1 148.2(5) . . ? C44 C43 N2 118.4(8) . . ? C43 C44 N3 123.7(6) . . ? N4 C45 N3 133.5(5) . . ? N4 C45 Ti1 74.7(3) . . ? N3 C45 Ti1 151.7(5) . . ? C53 C51 C52 123(2) 3_565 . ? C53 C52 C51 119(3) . . ? C52 C53 C51 117(2) . 3_565 ? C1 B3 C2 60.4(3) . . ? C1 B3 B7 106.9(4) . . ? C2 B3 B7 59.7(3) . . ? C1 B3 B8 104.7(5) . . ? C2 B3 B8 107.4(4) . . ? B7 B3 B8 60.3(4) . . ? C1 B3 B4 58.7(3) . . ? C2 B3 B4 108.4(4) . . ? B7 B3 B4 108.1(5) . . ? B8 B3 B4 58.9(4) . . ? C1 B4 B8 105.1(5) . . ? C1 B4 B9 105.4(5) . . ? B8 B4 B9 60.1(4) . . ? C1 B4 B5 58.8(3) . . ? B8 B4 B5 107.6(5) . . ? B9 B4 B5 59.8(4) . . ? C1 B4 B3 58.0(3) . . ? B8 B4 B3 60.1(4) . . ? B9 B4 B3 107.7(5) . . ? B5 B4 B3 106.7(4) . . ? C1 B5 B10 105.5(5) . . ? C1 B5 B9 105.0(5) . . ? B10 B5 B9 60.6(4) . . ? C1 B5 B6 58.1(3) . . ? B10 B5 B6 60.3(4) . . ? B9 B5 B6 107.9(6) . . ? C1 B5 B4 58.5(4) . . ? B10 B5 B4 108.1(5) . . ? B9 B5 B4 59.7(4) . . ? B6 B5 B4 106.7(5) . . ? C1 B6 C2 60.9(3) . . ? C1 B6 B11 106.7(5) . . ? C2 B6 B11 59.5(3) . . ? C1 B6 B10 105.4(5) . . ? C2 B6 B10 107.8(5) . . ? B11 B6 B10 60.0(4) . . ? C1 B6 B5 59.1(4) . . ? C2 B6 B5 109.2(5) . . ? B11 B6 B5 107.9(5) . . ? B10 B6 B5 59.3(4) . . ? C2 B7 B11 59.1(3) . . ? C2 B7 B3 59.4(3) . . ? B11 B7 B3 107.1(5) . . ? C2 B7 B12 107.7(5) . . ? B11 B7 B12 60.4(4) . . ? B3 B7 B12 108.8(5) . . ? C2 B7 B8 106.9(5) . . ? B11 B7 B8 107.5(5) . . ? B3 B7 B8 60.1(4) . . ? B12 B7 B8 60.3(4) . . ? B4 B8 B9 60.5(4) . . ? B4 B8 B3 61.0(4) . . ? B9 B8 B3 108.7(5) . . ? B4 B8 B7 109.2(5) . . ? B9 B8 B7 108.6(5) . . ? B3 B8 B7 59.6(4) . . ? B4 B8 B12 109.7(5) . . ? B9 B8 B12 60.8(4) . . ? B3 B8 B12 108.0(5) . . ? B7 B8 B12 59.8(4) . . ? B8 B9 B4 59.4(4) . . ? B8 B9 B5 107.5(5) . . ? B4 B9 B5 60.5(4) . . ? B8 B9 B10 107.5(5) . . ? B4 B9 B10 107.7(5) . . ? B5 B9 B10 59.4(4) . . ? B8 B9 B12 60.1(4) . . ? B4 B9 B12 108.2(5) . . ? B5 B9 B12 108.2(5) . . ? B10 B9 B12 60.3(4) . . ? B5 B10 B11 108.3(5) . . ? B5 B10 B6 60.4(4) . . ? B11 B10 B6 59.4(4) . . ? B5 B10 B9 60.0(4) . . ? B11 B10 B9 107.6(5) . . ? B6 B10 B9 107.6(5) . . ? B5 B10 B12 108.6(5) . . ? B11 B10 B12 59.7(4) . . ? B6 B10 B12 107.3(5) . . ? B9 B10 B12 60.2(4) . . ? C2 B11 B7 60.0(3) . . ? C2 B11 B6 58.9(3) . . ? B7 B11 B6 107.6(5) . . ? C2 B11 B10 107.8(5) . . ? B7 B11 B10 108.7(5) . . ? B6 B11 B10 60.5(4) . . ? C2 B11 B12 108.5(5) . . ? B7 B11 B12 60.3(4) . . ? B6 B11 B12 109.2(5) . . ? B10 B11 B12 60.9(4) . . ? B7 B12 B11 59.3(4) . . ? B7 B12 B8 59.9(4) . . ? B11 B12 B8 106.4(5) . . ? B7 B12 B9 107.2(5) . . ? B11 B12 B9 106.8(5) . . ? B8 B12 B9 59.0(4) . . ? B7 B12 B10 106.7(5) . . ? B11 B12 B10 59.4(4) . . ? B8 B12 B10 106.0(5) . . ? B9 B12 B10 59.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.287 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.058 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 665269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H51 B10 N4 Zr' _chemical_formula_weight 727.12 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' B B 0.0013 0.0007 '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' 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 10.4718(14) _cell_length_b 17.389(2) _cell_length_c 21.659(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.678(3) _cell_angle_gamma 90.00 _cell_volume 3898.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 936 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 22.31 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.313 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.878306 _exptl_absorpt_correction_T_max 1.00000 _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 SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26972 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9663 _reflns_number_gt 6202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0702P)^2^+1.9009P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9663 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.46058(3) 0.319837(16) 0.250199(13) 0.03501(10) Uani 1 1 d . . . N1 N 0.3796(3) 0.20267(15) 0.22490(12) 0.0433(6) Uani 1 1 d . . . N2 N 0.2267(3) 0.21529(19) 0.29774(16) 0.0669(9) Uani 1 1 d . . . N3 N 0.4133(3) 0.3146(2) 0.40218(14) 0.0679(9) Uani 1 1 d . . . N4 N 0.5857(3) 0.33536(15) 0.34209(12) 0.0465(6) Uani 1 1 d . . . C1 C 0.6548(3) 0.35945(19) 0.13462(15) 0.0457(8) Uani 1 1 d . . . C2 C 0.6369(3) 0.29637(18) 0.19403(14) 0.0412(7) Uani 1 1 d . . . C11 C 0.5516(4) 0.42466(19) 0.12074(16) 0.0548(9) Uani 1 1 d . . . C12 C 0.6168(5) 0.5044(2) 0.1255(3) 0.0935(17) Uani 1 1 d . . . H12A H 0.5521 0.5436 0.1169 0.140 Uiso 1 1 calc R . . H12B H 0.6757 0.5078 0.0957 0.140 Uiso 1 1 calc R . . H12C H 0.6633 0.5114 0.1668 0.140 Uiso 1 1 calc R . . C13 C 0.4767(5) 0.4164(3) 0.05408(18) 0.0910(16) Uani 1 1 d . . . H13A H 0.4139 0.4569 0.0464 0.136 Uiso 1 1 calc R . . H13B H 0.4336 0.3676 0.0500 0.136 Uiso 1 1 calc R . . H13C H 0.5358 0.4197 0.0244 0.136 Uiso 1 1 calc R . . C14 C 0.4553(3) 0.42189(18) 0.16696(15) 0.0459(8) Uani 1 1 d . . . C15 C 0.3338(4) 0.3859(2) 0.15784(18) 0.0620(10) Uani 1 1 d . . . H15A H 0.2937 0.3606 0.1193 0.074 Uiso 1 1 calc R . . C16 C 0.2722(4) 0.4019(3) 0.2099(2) 0.0720(13) Uani 1 1 d . . . H16A H 0.1819 0.3901 0.2131 0.086 Uiso 1 1 calc R . . C17 C 0.3533(4) 0.4472(2) 0.2510(2) 0.0662(11) Uani 1 1 d . . . H17A H 0.3300 0.4732 0.2878 0.079 Uiso 1 1 calc R . . C18 C 0.4661(3) 0.46043(18) 0.22443(17) 0.0515(8) Uani 1 1 d . . . H18A H 0.5355 0.4962 0.2407 0.062 Uiso 1 1 calc R . . C21 C 0.3706(3) 0.12822(19) 0.19685(15) 0.0461(7) Uani 1 1 d . . . C22 C 0.2943(4) 0.1194(2) 0.13891(17) 0.0629(10) Uani 1 1 d . . . C23 C 0.2974(6) 0.0489(3) 0.1089(2) 0.0915(16) Uani 1 1 d . . . H23A H 0.2463 0.0418 0.0703 0.110 Uiso 1 1 calc R . . C24 C 0.3716(7) -0.0091(3) 0.1338(3) 0.102(2) Uani 1 1 d . . . H24A H 0.3736 -0.0549 0.1118 0.122 Uiso 1 1 calc R . . C25 C 0.4446(5) -0.0019(2) 0.1913(3) 0.0838(15) Uani 1 1 d . . . H25A H 0.4945 -0.0432 0.2082 0.101 Uiso 1 1 calc R . . C26 C 0.4454(4) 0.0673(2) 0.2254(2) 0.0622(10) Uani 1 1 d . . . C27 C 0.2111(5) 0.1828(3) 0.1096(2) 0.0956(17) Uani 1 1 d . . . H27A H 0.2208 0.2270 0.1365 0.143 Uiso 1 1 calc R . . H27B H 0.1225 0.1666 0.1034 0.143 Uiso 1 1 calc R . . H27C H 0.2363 0.1959 0.0701 0.143 Uiso 1 1 calc R . . C28 C 0.5214(5) 0.0765(3) 0.2882(2) 0.0978(17) Uani 1 1 d . . . H28A H 0.5089 0.1273 0.3035 0.147 Uiso 1 1 calc R . . H28B H 0.6113 0.0687 0.2860 0.147 Uiso 1 1 calc R . . H28C H 0.4932 0.0393 0.3161 0.147 Uiso 1 1 calc R . . C31 C 0.7035(4) 0.3455(2) 0.38594(15) 0.0538(9) Uani 1 1 d . . . C32 C 0.7722(4) 0.2813(3) 0.41084(17) 0.0644(10) Uani 1 1 d . . . C33 C 0.8871(5) 0.2935(3) 0.4511(2) 0.0879(15) Uani 1 1 d . . . H33A H 0.9346 0.2513 0.4680 0.105 Uiso 1 1 calc R . . C34 C 0.9321(5) 0.3659(4) 0.4664(2) 0.0987(17) Uani 1 1 d . . . H34A H 1.0094 0.3727 0.4932 0.118 Uiso 1 1 calc R . . C35 C 0.8626(5) 0.4281(3) 0.4421(2) 0.0919(16) Uani 1 1 d . . . H35A H 0.8929 0.4772 0.4533 0.110 Uiso 1 1 calc R . . C36 C 0.7474(4) 0.4198(3) 0.40095(19) 0.0710(11) Uani 1 1 d . . . C37 C 0.7216(5) 0.2019(3) 0.3967(2) 0.0946(17) Uani 1 1 d . . . H37A H 0.6420 0.2046 0.3683 0.142 Uiso 1 1 calc R . . H37B H 0.7067 0.1775 0.4347 0.142 Uiso 1 1 calc R . . H37C H 0.7836 0.1727 0.3781 0.142 Uiso 1 1 calc R . . C38 C 0.6728(6) 0.4891(3) 0.3756(3) 0.120(2) Uani 1 1 d . . . H38A H 0.5969 0.4732 0.3480 0.180 Uiso 1 1 calc R . . H38B H 0.7257 0.5203 0.3530 0.180 Uiso 1 1 calc R . . H38C H 0.6479 0.5183 0.4095 0.180 Uiso 1 1 calc R . . C41 C 0.3159(3) 0.23653(19) 0.26375(16) 0.0470(8) Uani 1 1 d . . . C42 C 0.1683(5) 0.1385(3) 0.2973(2) 0.0815(14) Uani 1 1 d . . . H42A H 0.2006 0.1070 0.2667 0.122 Uiso 1 1 calc R . . H42B H 0.0761 0.1429 0.2871 0.122 Uiso 1 1 calc R . . H42C H 0.1899 0.1154 0.3378 0.122 Uiso 1 1 calc R . . C43 C 0.1938(4) 0.2746(3) 0.3411(2) 0.0850(14) Uani 1 1 d . . . H43A H 0.1921 0.3241 0.3204 0.102 Uiso 1 1 calc R . . H43B H 0.1075 0.2645 0.3502 0.102 Uiso 1 1 calc R . . C44 C 0.2806(4) 0.2795(4) 0.3993(2) 0.0960(17) Uani 1 1 d . . . H44A H 0.2926 0.2276 0.4156 0.115 Uiso 1 1 calc R . . H44B H 0.2362 0.3080 0.4282 0.115 Uiso 1 1 calc R . . C45 C 0.4673(3) 0.32312(19) 0.35105(15) 0.0490(8) Uani 1 1 d . . . C46 C 0.4822(5) 0.3227(3) 0.46566(18) 0.103(2) Uani 1 1 d . . . H46A H 0.5644 0.3466 0.4644 0.154 Uiso 1 1 calc R . . H46B H 0.4951 0.2729 0.4846 0.154 Uiso 1 1 calc R . . H46C H 0.4324 0.3541 0.4897 0.154 Uiso 1 1 calc R . . C51 C 0.0807(16) 0.4478(10) 0.0088(9) 0.206(5) Uani 1 1 d . . . H51A H 0.1417 0.4088 0.0173 0.247 Uiso 1 1 calc R . . C52 C 0.0995(14) 0.5123(13) 0.0369(7) 0.216(5) Uani 1 1 d . . . H52A H 0.1769 0.5203 0.0633 0.260 Uiso 1 1 calc R . . C53 C 0.019(2) 0.5639(8) 0.0303(7) 0.191(4) Uani 1 1 d . . . H53 H 0.0315 0.6094 0.0530 0.229 Uiso 1 1 calc R . . B3 B 0.6052(4) 0.2675(2) 0.11775(18) 0.0474(9) Uani 1 1 d . . . H3 H 0.5068 0.2532 0.0954 0.057 Uiso 1 1 calc R . . B4 B 0.7195(5) 0.3138(3) 0.0767(2) 0.0598(11) Uani 1 1 d . . . H4 H 0.6966 0.3291 0.0269 0.072 Uiso 1 1 calc R . . B5 B 0.8157(5) 0.3739(3) 0.1303(2) 0.0672(13) Uani 1 1 d . . . H5 H 0.8556 0.4285 0.1160 0.081 Uiso 1 1 calc R . . B6 B 0.7589(4) 0.3629(3) 0.2033(2) 0.0546(10) Uani 1 1 d . . . H6 H 0.7605 0.4107 0.2367 0.066 Uiso 1 1 calc R . . B7 B 0.6919(4) 0.2081(2) 0.1746(2) 0.0514(9) Uani 1 1 d . . . H7 H 0.6514 0.1539 0.1891 0.062 Uiso 1 1 calc R . . B8 B 0.7445(4) 0.2176(3) 0.1007(2) 0.0586(11) Uani 1 1 d . . . H8 H 0.7377 0.1701 0.0668 0.070 Uiso 1 1 calc R . . B9 B 0.8758(5) 0.2840(3) 0.1102(2) 0.0695(13) Uani 1 1 d . . . H9 H 0.9558 0.2794 0.0828 0.083 Uiso 1 1 calc R . . B10 B 0.9007(4) 0.3155(3) 0.1884(3) 0.0715(14) Uani 1 1 d . . . H10 H 0.9969 0.3321 0.2123 0.086 Uiso 1 1 calc R . . B11 B 0.7877(4) 0.2674(3) 0.2278(2) 0.0596(11) Uani 1 1 d . . . H11 H 0.8108 0.2522 0.2775 0.072 Uiso 1 1 calc R . . B12 B 0.8592(4) 0.2178(3) 0.1699(2) 0.0644(12) Uani 1 1 d . . . H12 H 0.9281 0.1703 0.1813 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.03351(16) 0.03442(16) 0.03781(16) 0.00727(12) 0.00765(11) 0.00039(12) N1 0.0400(14) 0.0444(15) 0.0449(14) 0.0046(12) 0.0039(12) -0.0041(11) N2 0.065(2) 0.062(2) 0.082(2) -0.0191(17) 0.0387(18) -0.0266(16) N3 0.067(2) 0.098(3) 0.0413(16) -0.0022(16) 0.0167(15) -0.0088(19) N4 0.0525(17) 0.0471(16) 0.0389(14) 0.0028(11) 0.0038(12) -0.0064(12) C1 0.0510(19) 0.0422(17) 0.0483(18) 0.0038(14) 0.0213(15) -0.0063(15) C2 0.0362(16) 0.0423(16) 0.0449(17) 0.0069(13) 0.0060(13) 0.0002(13) C11 0.070(2) 0.0439(19) 0.055(2) 0.0148(16) 0.0265(18) 0.0053(17) C12 0.116(4) 0.043(2) 0.141(4) 0.016(3) 0.084(3) -0.001(2) C13 0.123(4) 0.099(4) 0.052(2) 0.030(2) 0.018(2) 0.046(3) C14 0.0460(18) 0.0380(17) 0.0544(19) 0.0177(14) 0.0105(15) 0.0064(14) C15 0.051(2) 0.065(2) 0.064(2) 0.0294(19) -0.0100(18) -0.0031(18) C16 0.039(2) 0.079(3) 0.101(3) 0.051(3) 0.022(2) 0.018(2) C17 0.068(3) 0.056(2) 0.083(3) 0.022(2) 0.039(2) 0.025(2) C18 0.059(2) 0.0346(16) 0.065(2) 0.0097(16) 0.0230(17) 0.0079(15) C21 0.0424(18) 0.0452(18) 0.0534(19) -0.0021(15) 0.0158(15) -0.0072(14) C22 0.063(2) 0.073(3) 0.054(2) -0.0099(19) 0.0142(18) -0.018(2) C23 0.118(4) 0.094(4) 0.067(3) -0.026(3) 0.030(3) -0.033(3) C24 0.134(5) 0.075(4) 0.115(4) -0.036(3) 0.077(4) -0.032(4) C25 0.075(3) 0.046(2) 0.142(5) 0.011(3) 0.053(3) 0.003(2) C26 0.052(2) 0.045(2) 0.092(3) 0.012(2) 0.019(2) -0.0044(16) C27 0.090(4) 0.118(4) 0.067(3) 0.001(3) -0.026(3) -0.009(3) C28 0.092(4) 0.075(3) 0.115(4) 0.038(3) -0.017(3) 0.000(3) C31 0.054(2) 0.067(2) 0.0397(17) 0.0005(16) 0.0061(15) -0.0143(18) C32 0.070(3) 0.075(3) 0.045(2) 0.0118(19) -0.0016(18) -0.005(2) C33 0.076(3) 0.124(4) 0.059(3) 0.021(3) -0.005(2) 0.001(3) C34 0.071(3) 0.152(5) 0.068(3) -0.002(4) -0.003(2) -0.033(4) C35 0.096(4) 0.109(4) 0.068(3) -0.016(3) 0.005(3) -0.049(3) C36 0.080(3) 0.071(3) 0.060(2) -0.008(2) 0.005(2) -0.020(2) C37 0.117(4) 0.068(3) 0.088(3) 0.025(3) -0.018(3) 0.005(3) C38 0.161(6) 0.059(3) 0.126(5) -0.025(3) -0.021(4) -0.020(3) C41 0.0429(18) 0.0417(17) 0.059(2) -0.0004(15) 0.0146(15) -0.0086(14) C42 0.085(3) 0.080(3) 0.085(3) -0.007(2) 0.033(2) -0.046(3) C43 0.069(3) 0.098(4) 0.097(3) -0.020(3) 0.041(3) -0.015(3) C44 0.068(3) 0.158(5) 0.068(3) -0.004(3) 0.031(2) 0.001(3) C45 0.054(2) 0.053(2) 0.0417(17) -0.0003(15) 0.0119(15) 0.0010(16) C46 0.097(4) 0.174(6) 0.040(2) -0.009(3) 0.017(2) -0.034(4) C51 0.206(14) 0.175(14) 0.223(14) -0.026(10) -0.008(11) 0.041(10) C52 0.201(13) 0.189(12) 0.250(14) -0.009(13) 0.008(10) 0.055(13) C53 0.200(13) 0.186(12) 0.182(11) 0.006(9) 0.015(10) 0.049(12) B3 0.047(2) 0.045(2) 0.050(2) -0.0032(17) 0.0064(17) -0.0019(17) B4 0.073(3) 0.061(3) 0.052(2) -0.005(2) 0.031(2) -0.001(2) B5 0.065(3) 0.060(3) 0.088(3) -0.014(2) 0.046(3) -0.018(2) B6 0.041(2) 0.064(3) 0.062(2) -0.017(2) 0.0163(18) -0.0134(19) B7 0.046(2) 0.047(2) 0.063(2) 0.0067(19) 0.0136(19) 0.0074(17) B8 0.056(2) 0.057(3) 0.066(3) -0.012(2) 0.020(2) 0.002(2) B9 0.056(3) 0.074(3) 0.086(3) -0.014(3) 0.035(2) -0.002(2) B10 0.031(2) 0.094(4) 0.091(3) -0.026(3) 0.013(2) -0.008(2) B11 0.038(2) 0.079(3) 0.061(3) -0.002(2) 0.0007(18) 0.013(2) B12 0.045(2) 0.073(3) 0.077(3) -0.008(2) 0.016(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C41 2.148(3) . ? Zr1 C45 2.176(3) . ? Zr1 N4 2.228(3) . ? Zr1 N1 2.243(3) . ? Zr1 C2 2.394(3) . ? Zr1 C16 2.484(3) . ? Zr1 C17 2.485(4) . ? Zr1 C15 2.506(3) . ? Zr1 C18 2.510(3) . ? Zr1 C14 2.524(3) . ? N1 C41 1.292(4) . ? N1 C21 1.427(4) . ? N2 C41 1.326(4) . ? N2 C42 1.469(5) . ? N2 C43 1.470(5) . ? N3 C45 1.325(4) . ? N3 C46 1.460(5) . ? N3 C44 1.511(6) . ? N4 C45 1.301(4) . ? N4 C31 1.450(4) . ? C1 C11 1.564(5) . ? C1 B3 1.703(5) . ? C1 B6 1.708(5) . ? C1 B4 1.709(5) . ? C1 B5 1.720(5) . ? C1 C2 1.722(4) . ? C2 B3 1.711(5) . ? C2 B11 1.713(5) . ? C2 B6 1.713(5) . ? C2 B7 1.713(5) . ? C11 C14 1.526(5) . ? C11 C12 1.542(5) . ? C11 C13 1.542(5) . ? C14 C18 1.403(5) . ? C14 C15 1.405(5) . ? C15 C16 1.408(6) . ? C16 C17 1.381(6) . ? C17 C18 1.409(5) . ? C21 C22 1.391(5) . ? C21 C26 1.404(5) . ? C22 C23 1.391(6) . ? C22 C27 1.487(6) . ? C23 C24 1.336(8) . ? C24 C25 1.364(7) . ? C25 C26 1.412(6) . ? C26 C28 1.478(6) . ? C31 C32 1.393(5) . ? C31 C36 1.394(5) . ? C32 C33 1.391(6) . ? C32 C37 1.492(6) . ? C33 C34 1.368(8) . ? C34 C35 1.363(8) . ? C35 C36 1.396(6) . ? C36 C38 1.494(7) . ? C43 C44 1.441(6) . ? C51 C53 1.259(13) 3_565 ? C51 C52 1.278(15) . ? C52 C53 1.222(14) . ? C53 C51 1.259(13) 3_565 ? B3 B7 1.752(6) . ? B3 B8 1.783(6) . ? B3 B4 1.788(6) . ? B4 B8 1.760(6) . ? B4 B5 1.761(7) . ? B4 B9 1.765(7) . ? B5 B10 1.752(8) . ? B5 B9 1.765(7) . ? B5 B6 1.782(6) . ? B6 B11 1.756(7) . ? B6 B10 1.770(6) . ? B7 B11 1.746(6) . ? B7 B12 1.778(6) . ? B7 B8 1.778(6) . ? B8 B12 1.775(7) . ? B8 B9 1.783(7) . ? B9 B12 1.760(7) . ? B9 B10 1.762(7) . ? B10 B11 1.770(7) . ? B10 B12 1.783(7) . ? B11 B12 1.777(6) . ? 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 C41 Zr1 C45 78.29(13) . . ? C41 Zr1 N4 106.94(11) . . ? C45 Zr1 N4 34.34(11) . . ? C41 Zr1 N1 34.15(11) . . ? C45 Zr1 N1 102.88(11) . . ? N4 Zr1 N1 118.55(9) . . ? C41 Zr1 C2 124.64(12) . . ? C45 Zr1 C2 127.16(12) . . ? N4 Zr1 C2 94.59(10) . . ? N1 Zr1 C2 90.75(10) . . ? C41 Zr1 C16 84.05(13) . . ? C45 Zr1 C16 103.98(14) . . ? N4 Zr1 C16 124.98(14) . . ? N1 Zr1 C16 100.66(13) . . ? C2 Zr1 C16 123.47(12) . . ? C41 Zr1 C17 105.73(13) . . ? C45 Zr1 C17 85.19(13) . . ? N4 Zr1 C17 95.26(13) . . ? N1 Zr1 C17 131.05(13) . . ? C2 Zr1 C17 122.64(11) . . ? C16 Zr1 C17 32.26(14) . . ? C41 Zr1 C15 96.79(13) . . ? C45 Zr1 C15 136.24(14) . . ? N4 Zr1 C15 145.78(12) . . ? N1 Zr1 C15 94.93(11) . . ? C2 Zr1 C15 91.65(12) . . ? C16 Zr1 C15 32.77(13) . . ? C17 Zr1 C15 53.93(15) . . ? C41 Zr1 C18 136.68(12) . . ? C45 Zr1 C18 101.50(12) . . ? N4 Zr1 C18 92.89(11) . . ? N1 Zr1 C18 148.32(11) . . ? C2 Zr1 C18 90.43(11) . . ? C16 Zr1 C18 53.58(13) . . ? C17 Zr1 C18 32.76(11) . . ? C15 Zr1 C18 53.39(13) . . ? C41 Zr1 C14 129.17(12) . . ? C45 Zr1 C14 133.83(12) . . ? N4 Zr1 C14 119.97(10) . . ? N1 Zr1 C14 119.82(10) . . ? C2 Zr1 C14 72.09(10) . . ? C16 Zr1 C14 54.14(11) . . ? C17 Zr1 C14 54.32(12) . . ? C15 Zr1 C14 32.43(11) . . ? C18 Zr1 C14 32.36(11) . . ? C41 N1 C21 133.1(3) . . ? C41 N1 Zr1 68.92(18) . . ? C21 N1 Zr1 157.9(2) . . ? C41 N2 C42 125.3(3) . . ? C41 N2 C43 114.3(3) . . ? C42 N2 C43 120.3(3) . . ? C45 N3 C46 124.3(4) . . ? C45 N3 C44 121.1(3) . . ? C46 N3 C44 113.5(3) . . ? C45 N4 C31 131.2(3) . . ? C45 N4 Zr1 70.63(19) . . ? C31 N4 Zr1 158.1(2) . . ? C11 C1 B3 117.4(3) . . ? C11 C1 B6 118.3(3) . . ? B3 C1 B6 110.7(3) . . ? C11 C1 B4 122.3(3) . . ? B3 C1 B4 63.2(2) . . ? B6 C1 B4 112.6(3) . . ? C11 C1 B5 122.5(3) . . ? B3 C1 B5 113.2(3) . . ? B6 C1 B5 62.6(2) . . ? B4 C1 B5 61.8(2) . . ? C11 C1 C2 117.1(2) . . ? B3 C1 C2 59.9(2) . . ? B6 C1 C2 59.9(2) . . ? B4 C1 C2 110.7(3) . . ? B5 C1 C2 110.6(3) . . ? B3 C2 B11 111.0(3) . . ? B3 C2 B6 110.1(3) . . ? B11 C2 B6 61.7(3) . . ? B3 C2 B7 61.5(2) . . ? B11 C2 B7 61.3(2) . . ? B6 C2 B7 111.2(3) . . ? B3 C2 C1 59.5(2) . . ? B11 C2 C1 108.0(3) . . ? B6 C2 C1 59.6(2) . . ? B7 C2 C1 108.0(2) . . ? B3 C2 Zr1 119.3(2) . . ? B11 C2 Zr1 124.4(2) . . ? B6 C2 Zr1 116.4(2) . . ? B7 C2 Zr1 126.2(2) . . ? C1 C2 Zr1 116.75(19) . . ? C14 C11 C12 108.3(3) . . ? C14 C11 C13 108.5(3) . . ? C12 C11 C13 107.7(3) . . ? C14 C11 C1 110.9(2) . . ? C12 C11 C1 110.7(3) . . ? C13 C11 C1 110.6(3) . . ? C18 C14 C15 106.7(3) . . ? C18 C14 C11 126.4(3) . . ? C15 C14 C11 126.6(3) . . ? C18 C14 Zr1 73.26(18) . . ? C15 C14 Zr1 73.07(18) . . ? C11 C14 Zr1 123.0(2) . . ? C14 C15 C16 108.3(4) . . ? C14 C15 Zr1 74.50(18) . . ? C16 C15 Zr1 72.7(2) . . ? C17 C16 C15 108.5(3) . . ? C17 C16 Zr1 73.9(2) . . ? C15 C16 Zr1 74.5(2) . . ? C16 C17 C18 107.6(4) . . ? C16 C17 Zr1 73.8(2) . . ? C18 C17 Zr1 74.62(19) . . ? C14 C18 C17 108.8(3) . . ? C14 C18 Zr1 74.37(18) . . ? C17 C18 Zr1 72.6(2) . . ? C22 C21 C26 121.4(3) . . ? C22 C21 N1 118.4(3) . . ? C26 C21 N1 120.0(3) . . ? C21 C22 C23 117.9(4) . . ? C21 C22 C27 121.5(4) . . ? C23 C22 C27 120.6(4) . . ? C24 C23 C22 122.0(5) . . ? C23 C24 C25 120.7(5) . . ? C24 C25 C26 120.9(5) . . ? C21 C26 C25 117.0(4) . . ? C21 C26 C28 120.8(4) . . ? C25 C26 C28 122.2(4) . . ? C32 C31 C36 121.4(4) . . ? C32 C31 N4 119.7(3) . . ? C36 C31 N4 118.9(3) . . ? C33 C32 C31 117.9(4) . . ? C33 C32 C37 121.1(4) . . ? C31 C32 C37 121.0(4) . . ? C34 C33 C32 121.7(5) . . ? C35 C34 C33 119.5(5) . . ? C34 C35 C36 121.7(5) . . ? C31 C36 C35 117.8(4) . . ? C31 C36 C38 121.8(4) . . ? C35 C36 C38 120.4(4) . . ? N1 C41 N2 135.3(3) . . ? N1 C41 Zr1 76.94(19) . . ? N2 C41 Zr1 146.5(3) . . ? C44 C43 N2 115.0(4) . . ? C43 C44 N3 120.9(4) . . ? N4 C45 N3 132.8(3) . . ? N4 C45 Zr1 75.02(19) . . ? N3 C45 Zr1 152.0(3) . . ? C53 C51 C52 120.9(15) 3_565 . ? C53 C52 C51 122.4(15) . . ? C52 C53 C51 116.6(15) . 3_565 ? C1 B3 C2 60.61(19) . . ? C1 B3 B7 107.1(3) . . ? C2 B3 B7 59.3(2) . . ? C1 B3 B8 105.6(3) . . ? C2 B3 B8 107.3(3) . . ? B7 B3 B8 60.4(2) . . ? C1 B3 B4 58.6(2) . . ? C2 B3 B4 107.6(3) . . ? B7 B3 B4 107.5(3) . . ? B8 B3 B4 59.1(2) . . ? C1 B4 B8 106.4(3) . . ? C1 B4 B5 59.4(2) . . ? B8 B4 B5 108.9(4) . . ? C1 B4 B9 106.3(3) . . ? B8 B4 B9 60.8(3) . . ? B5 B4 B9 60.1(3) . . ? C1 B4 B3 58.2(2) . . ? B8 B4 B3 60.4(2) . . ? B5 B4 B3 107.3(3) . . ? B9 B4 B3 108.1(3) . . ? C1 B5 B10 105.8(3) . . ? C1 B5 B4 58.8(2) . . ? B10 B5 B4 107.9(3) . . ? C1 B5 B9 105.8(3) . . ? B10 B5 B9 60.1(3) . . ? B4 B5 B9 60.1(3) . . ? C1 B5 B6 58.3(2) . . ? B10 B5 B6 60.1(3) . . ? B4 B5 B6 106.7(3) . . ? B9 B5 B6 107.7(3) . . ? C1 B6 C2 60.5(2) . . ? C1 B6 B11 106.7(3) . . ? C2 B6 B11 59.2(2) . . ? C1 B6 B10 105.5(3) . . ? C2 B6 B10 107.1(3) . . ? B11 B6 B10 60.3(3) . . ? C1 B6 B5 59.0(2) . . ? C2 B6 B5 108.1(3) . . ? B11 B6 B5 107.8(3) . . ? B10 B6 B5 59.1(3) . . ? C2 B7 B11 59.3(2) . . ? C2 B7 B3 59.2(2) . . ? B11 B7 B3 107.5(3) . . ? C2 B7 B12 107.4(3) . . ? B11 B7 B12 60.6(2) . . ? B3 B7 B12 108.3(3) . . ? C2 B7 B8 107.4(3) . . ? B11 B7 B8 108.3(3) . . ? B3 B7 B8 60.7(2) . . ? B12 B7 B8 59.9(3) . . ? B4 B8 B12 107.4(3) . . ? B4 B8 B7 107.5(3) . . ? B12 B8 B7 60.1(2) . . ? B4 B8 B9 59.8(3) . . ? B12 B8 B9 59.3(3) . . ? B7 B8 B9 107.1(3) . . ? B4 B8 B3 60.6(2) . . ? B12 B8 B3 107.1(3) . . ? B7 B8 B3 58.9(2) . . ? B9 B8 B3 107.5(3) . . ? B12 B9 B10 60.8(3) . . ? B12 B9 B4 107.9(3) . . ? B10 B9 B4 107.3(3) . . ? B12 B9 B5 108.6(3) . . ? B10 B9 B5 59.6(3) . . ? B4 B9 B5 59.9(3) . . ? B12 B9 B8 60.1(3) . . ? B10 B9 B8 108.2(3) . . ? B4 B9 B8 59.5(3) . . ? B5 B9 B8 107.7(3) . . ? B5 B10 B9 60.3(3) . . ? B5 B10 B11 108.4(3) . . ? B9 B10 B11 107.7(3) . . ? B5 B10 B6 60.8(3) . . ? B9 B10 B6 108.3(3) . . ? B11 B10 B6 59.5(2) . . ? B5 B10 B12 108.1(3) . . ? B9 B10 B12 59.5(3) . . ? B11 B10 B12 60.0(3) . . ? B6 B10 B12 107.6(3) . . ? C2 B11 B7 59.4(2) . . ? C2 B11 B6 59.2(2) . . ? B7 B11 B6 107.6(3) . . ? C2 B11 B10 107.2(3) . . ? B7 B11 B10 108.6(3) . . ? B6 B11 B10 60.3(3) . . ? C2 B11 B12 107.5(3) . . ? B7 B11 B12 60.6(2) . . ? B6 B11 B12 108.5(3) . . ? B10 B11 B12 60.3(3) . . ? B9 B12 B8 60.6(3) . . ? B9 B12 B11 107.5(3) . . ? B8 B12 B11 107.1(3) . . ? B9 B12 B7 108.1(3) . . ? B8 B12 B7 60.1(2) . . ? B11 B12 B7 58.8(2) . . ? B9 B12 B10 59.7(3) . . ? B8 B12 B10 107.6(3) . . ? B11 B12 B10 59.6(3) . . ? B7 B12 B10 106.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.794 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.069 #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 665270' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H80 B20 N8 O4 Zr2' _chemical_formula_weight 1327.92 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8957(15) _cell_length_b 17.104(2) _cell_length_c 20.437(3) _cell_angle_alpha 73.668(3) _cell_angle_beta 80.768(4) _cell_angle_gamma 74.872(3) _cell_volume 3512.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 718 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 18.74 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.345 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.431915 _exptl_absorpt_correction_T_max 1.0000 _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 SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19247 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.1613 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12298 _reflns_number_gt 5647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0590P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12298 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1446 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.841 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.78338(6) 0.31691(3) 0.76061(3) 0.04091(19) Uani 1 1 d . . . Zr2 Zr 0.39552(5) 0.78967(3) 0.73445(3) 0.03777(18) Uani 1 1 d . . . C1 C 0.9272(6) 0.1955(3) 0.9105(3) 0.0461(16) Uani 1 1 d . . . C2 C 0.8733(6) 0.2943(3) 0.8638(3) 0.0419(15) Uani 1 1 d . . . C11 C 0.9158(6) 0.1222(4) 0.8801(3) 0.0549(18) Uani 1 1 d . . . C12 C 0.8348(7) 0.0668(4) 0.9311(3) 0.079(2) Uani 1 1 d . . . H12A H 0.8278 0.0230 0.9121 0.119 Uiso 1 1 calc R . . H12B H 0.7512 0.1000 0.9401 0.119 Uiso 1 1 calc R . . H12C H 0.8746 0.0426 0.9731 0.119 Uiso 1 1 calc R . . C13 C 1.0464(7) 0.0670(4) 0.8650(4) 0.081(2) Uani 1 1 d . . . H13A H 1.0357 0.0234 0.8469 0.122 Uiso 1 1 calc R . . H13B H 1.0878 0.0426 0.9064 0.122 Uiso 1 1 calc R . . H13C H 1.0979 0.1003 0.8320 0.122 Uiso 1 1 calc R . . C14 C 0.8508(7) 0.1609(3) 0.8138(3) 0.0450(16) Uani 1 1 d . . . C15 C 0.7219(7) 0.1786(3) 0.8062(4) 0.0590(19) Uani 1 1 d . . . H15A H 0.6550 0.1664 0.8432 0.071 Uiso 1 1 calc R . . C16 C 0.7056(8) 0.2032(4) 0.7360(4) 0.069(2) Uani 1 1 d . . . H16A H 0.6261 0.2106 0.7160 0.083 Uiso 1 1 calc R . . C17 C 0.8243(9) 0.2034(4) 0.7003(4) 0.069(2) Uani 1 1 d . . . H17A H 0.8425 0.2108 0.6507 0.083 Uiso 1 1 calc R . . C18 C 0.9175(6) 0.1772(3) 0.7475(3) 0.0505(17) Uani 1 1 d . . . H18A H 1.0103 0.1632 0.7366 0.061 Uiso 1 1 calc R . . C21 C 0.2206(5) 0.9031(3) 0.5914(3) 0.0374(15) Uani 1 1 d . . . C22 C 0.3398(5) 0.8196(3) 0.6205(3) 0.0344(14) Uani 1 1 d . . . C31 C 0.1567(5) 0.9583(3) 0.6420(3) 0.0444(16) Uani 1 1 d . . . C32 C 0.1732(6) 1.0483(3) 0.6127(3) 0.069(2) Uani 1 1 d . . . H32A H 0.1328 1.0810 0.6448 0.103 Uiso 1 1 calc R . . H32B H 0.1347 1.0720 0.5703 0.103 Uiso 1 1 calc R . . H32C H 0.2625 1.0481 0.6047 0.103 Uiso 1 1 calc R . . C33 C 0.0136(6) 0.9625(4) 0.6568(4) 0.074(2) Uani 1 1 d . . . H33A H -0.0229 0.9973 0.6878 0.111 Uiso 1 1 calc R . . H33B H -0.0001 0.9072 0.6770 0.111 Uiso 1 1 calc R . . H33C H -0.0263 0.9856 0.6147 0.111 Uiso 1 1 calc R . . C34 C 0.2169(5) 0.9220(3) 0.7098(3) 0.0423(15) Uani 1 1 d . . . C35 C 0.3219(6) 0.9435(4) 0.7278(3) 0.0524(18) Uani 1 1 d . . . H35A H 0.3653 0.9866 0.6992 0.063 Uiso 1 1 calc R . . C36 C 0.3406(8) 0.9028(5) 0.7962(4) 0.072(2) Uani 1 1 d . . . H36A H 0.3966 0.9138 0.8240 0.086 Uiso 1 1 calc R . . C37 C 0.2474(7) 0.8548(4) 0.8208(4) 0.070(2) Uani 1 1 d . . . H37A H 0.2298 0.8260 0.8689 0.084 Uiso 1 1 calc R . . C38 C 0.1716(6) 0.8659(4) 0.7686(3) 0.0554(18) Uani 1 1 d . . . H38A H 0.0936 0.8456 0.7736 0.066 Uiso 1 1 calc R . . C41 C 0.6220(5) 0.4427(3) 0.6308(3) 0.0385(15) Uani 1 1 d . . . C42 C 0.6579(6) 0.4047(4) 0.5771(3) 0.0508(17) Uani 1 1 d . . . H42A H 0.6714 0.3468 0.5862 0.061 Uiso 1 1 calc R . . C43 C 0.6739(6) 0.4498(4) 0.5114(3) 0.0562(18) Uani 1 1 d . . . H43A H 0.6971 0.4233 0.4758 0.067 Uiso 1 1 calc R . . C44 C 0.6552(5) 0.5360(4) 0.4981(3) 0.0519(17) Uani 1 1 d . . . H44A H 0.6664 0.5677 0.4533 0.062 Uiso 1 1 calc R . . C45 C 0.6209(5) 0.5737(4) 0.5500(3) 0.0480(16) Uani 1 1 d . . . H45A H 0.6097 0.6314 0.5406 0.058 Uiso 1 1 calc R . . C46 C 0.6019(5) 0.5285(3) 0.6174(3) 0.0398(15) Uani 1 1 d . . . H46A H 0.5761 0.5555 0.6526 0.048 Uiso 1 1 calc R . . C47 C 0.5425(6) 0.4019(4) 0.7552(3) 0.0435(15) Uani 1 1 d . . . C48 C 0.3459(6) 0.4759(4) 0.6976(3) 0.069(2) Uani 1 1 d . . . H48A H 0.4037 0.4775 0.6568 0.103 Uiso 1 1 calc R . . H48B H 0.2955 0.5312 0.6969 0.103 Uiso 1 1 calc R . . H48C H 0.2907 0.4395 0.6998 0.103 Uiso 1 1 calc R . . C49 C 0.3438(6) 0.4400(3) 0.8239(3) 0.0535(17) Uani 1 1 d . . . H49A H 0.3995 0.4093 0.8598 0.064 Uiso 1 1 calc R . . H49B H 0.2795 0.4089 0.8268 0.064 Uiso 1 1 calc R . . C50 C 0.2775(6) 0.5258(4) 0.8369(3) 0.0552(18) Uani 1 1 d . . . H50A H 0.2393 0.5617 0.7959 0.066 Uiso 1 1 calc R . . H50B H 0.2094 0.5191 0.8734 0.066 Uiso 1 1 calc R . . C51 C 0.4143(6) 0.5259(4) 0.9224(3) 0.0651(19) Uani 1 1 d . . . H51A H 0.4720 0.5559 0.9297 0.098 Uiso 1 1 calc R . . H51B H 0.4587 0.4692 0.9236 0.098 Uiso 1 1 calc R . . H51C H 0.3447 0.5264 0.9577 0.098 Uiso 1 1 calc R . . C52 C 0.3761(6) 0.6438(4) 0.8198(3) 0.0417(15) Uani 1 1 d . . . C53 C 0.5504(6) 0.6658(4) 0.8708(3) 0.0506(17) Uani 1 1 d . . . C54 C 0.6579(7) 0.6079(4) 0.8553(3) 0.0554(18) Uani 1 1 d . . . H54A H 0.6586 0.5818 0.8209 0.067 Uiso 1 1 calc R . . C55 C 0.7647(7) 0.5886(4) 0.8906(4) 0.073(2) Uani 1 1 d . . . H55A H 0.8363 0.5487 0.8807 0.088 Uiso 1 1 calc R . . C56 C 0.7644(9) 0.6283(5) 0.9403(4) 0.091(3) Uani 1 1 d . . . H56A H 0.8366 0.6165 0.9634 0.110 Uiso 1 1 calc R . . C57 C 0.6553(9) 0.6866(5) 0.9561(4) 0.090(3) Uani 1 1 d . . . H57A H 0.6547 0.7133 0.9900 0.108 Uiso 1 1 calc R . . C58 C 0.5501(7) 0.7045(4) 0.9222(3) 0.065(2) Uani 1 1 d . . . H58A H 0.4774 0.7428 0.9334 0.078 Uiso 1 1 calc R . . C61 C 1.0426(7) 0.3283(3) 0.6467(4) 0.0574(19) Uani 1 1 d . . . C62 C 1.1603(8) 0.3101(4) 0.6714(4) 0.080(2) Uani 1 1 d . . . H62A H 1.1690 0.3241 0.7109 0.096 Uiso 1 1 calc R . . C63 C 1.2675(10) 0.2692(5) 0.6345(6) 0.128(5) Uani 1 1 d . . . H63A H 1.3469 0.2558 0.6513 0.154 Uiso 1 1 calc R . . C64 C 1.2608(14) 0.2492(7) 0.5782(8) 0.160(8) Uani 1 1 d . . . H64A H 1.3336 0.2226 0.5553 0.191 Uiso 1 1 calc R . . C65 C 1.1417(13) 0.2688(6) 0.5532(5) 0.133(5) Uani 1 1 d . . . H65A H 1.1360 0.2554 0.5129 0.160 Uiso 1 1 calc R . . C66 C 1.0331(8) 0.3072(4) 0.5861(4) 0.089(3) Uani 1 1 d . . . H66A H 0.9545 0.3190 0.5689 0.107 Uiso 1 1 calc R . . C67 C 0.8995(6) 0.4394(3) 0.6981(3) 0.0371(14) Uani 1 1 d . . . C68 C 1.0311(7) 0.5115(4) 0.6023(3) 0.080(2) Uani 1 1 d . . . H68A H 1.0535 0.4586 0.5905 0.120 Uiso 1 1 calc R . . H68B H 1.1075 0.5280 0.6049 0.120 Uiso 1 1 calc R . . H68C H 0.9825 0.5529 0.5678 0.120 Uiso 1 1 calc R . . C69 C 0.9134(5) 0.5800(3) 0.6916(3) 0.0486(16) Uani 1 1 d . . . H69A H 0.9838 0.6074 0.6842 0.058 Uiso 1 1 calc R . . H69B H 0.8874 0.5661 0.7404 0.058 Uiso 1 1 calc R . . C70 C 0.8037(5) 0.6388(3) 0.6544(3) 0.0501(17) Uani 1 1 d . . . H70A H 0.8282 0.6495 0.6055 0.060 Uiso 1 1 calc R . . H70B H 0.7318 0.6124 0.6641 0.060 Uiso 1 1 calc R . . C71 C 0.8527(6) 0.7752(4) 0.6518(4) 0.072(2) Uani 1 1 d . . . H71A H 0.8177 0.8250 0.6676 0.107 Uiso 1 1 calc R . . H71B H 0.8662 0.7898 0.6027 0.107 Uiso 1 1 calc R . . H71C H 0.9325 0.7470 0.6706 0.107 Uiso 1 1 calc R . . C72 C 0.6387(6) 0.7459(3) 0.6953(3) 0.0374(14) Uani 1 1 d . . . C73 C 0.6517(6) 0.8662(3) 0.7351(3) 0.0432(15) Uani 1 1 d . . . C74 C 0.7184(6) 0.8337(4) 0.7923(3) 0.065(2) Uani 1 1 d . . . H74A H 0.7279 0.7775 0.8152 0.077 Uiso 1 1 calc R . . C75 C 0.7716(7) 0.8854(6) 0.8155(4) 0.083(2) Uani 1 1 d . . . H75A H 0.8184 0.8637 0.8534 0.100 Uiso 1 1 calc R . . C76 C 0.7550(7) 0.9675(5) 0.7826(4) 0.079(2) Uani 1 1 d . . . H76A H 0.7881 1.0020 0.7995 0.095 Uiso 1 1 calc R . . C77 C 0.6915(7) 1.0007(4) 0.7258(4) 0.068(2) Uani 1 1 d . . . H77A H 0.6835 1.0568 0.7028 0.081 Uiso 1 1 calc R . . C78 C 0.6381(6) 0.9484(4) 0.7025(3) 0.0535(17) Uani 1 1 d . . . H78A H 0.5928 0.9704 0.6640 0.064 Uiso 1 1 calc R . . N1 N 0.6191(5) 0.3914(3) 0.6987(3) 0.0441(13) Uani 1 1 d . . . N2 N 0.4188(5) 0.4445(3) 0.7577(3) 0.0489(13) Uani 1 1 d . . . N3 N 0.3648(5) 0.5661(3) 0.8554(2) 0.0473(13) Uani 1 1 d . . . N4 N 0.4445(4) 0.6908(3) 0.8321(2) 0.0430(12) Uani 1 1 d . . . N5 N 0.9294(4) 0.3635(3) 0.6839(2) 0.0450(13) Uani 1 1 d . . . N6 N 0.9555(5) 0.5036(3) 0.6679(3) 0.0487(13) Uani 1 1 d . . . N7 N 0.7633(4) 0.7197(3) 0.6740(2) 0.0427(12) Uani 1 1 d . . . N8 N 0.5846(4) 0.8158(3) 0.7156(2) 0.0401(12) Uani 1 1 d . . . O1 O 0.5954(4) 0.3608(2) 0.81118(19) 0.0461(10) Uani 1 1 d . . . O2 O 0.3098(3) 0.6815(2) 0.76683(19) 0.0460(10) Uani 1 1 d . . . O3 O 0.8072(4) 0.4459(2) 0.74542(19) 0.0419(10) Uani 1 1 d . . . O4 O 0.5583(3) 0.7021(2) 0.69562(18) 0.0365(9) Uani 1 1 d . . . B3 B 0.7917(8) 0.2556(4) 0.9388(4) 0.050(2) Uani 1 1 d . . . H3 H 0.6972 0.2426 0.9410 0.060 Uiso 1 1 calc R . . B4 B 0.9026(8) 0.1905(5) 0.9956(4) 0.058(2) Uani 1 1 d . . . H4 H 0.8814 0.1358 1.0352 0.069 Uiso 1 1 calc R . . B5 B 1.0532(8) 0.1885(5) 0.9529(4) 0.058(2) Uani 1 1 d . . . H5 H 1.1312 0.1324 0.9648 0.070 Uiso 1 1 calc R . . B6 B 1.0348(7) 0.2520(5) 0.8680(4) 0.052(2) Uani 1 1 d . . . H6 H 1.0995 0.2374 0.8237 0.062 Uiso 1 1 calc R . . B7 B 0.8142(7) 0.3580(4) 0.9176(4) 0.055(2) Uani 1 1 d . . . H7 H 0.7352 0.4134 0.9060 0.066 Uiso 1 1 calc R . . B8 B 0.8305(8) 0.2955(5) 1.0011(4) 0.064(2) Uani 1 1 d . . . H8 H 0.7620 0.3103 1.0441 0.077 Uiso 1 1 calc R . . B9 B 0.9958(9) 0.2526(5) 1.0093(4) 0.074(3) Uani 1 1 d . . . H9 H 1.0360 0.2393 1.0584 0.088 Uiso 1 1 calc R . . B10 B 1.0812(9) 0.2898(5) 0.9298(4) 0.074(3) Uani 1 1 d . . . H10 H 1.1777 0.3005 0.9261 0.089 Uiso 1 1 calc R . . B11 B 0.9685(7) 0.3555(4) 0.8738(4) 0.057(2) Uani 1 1 d . . . H11 H 0.9912 0.4094 0.8337 0.068 Uiso 1 1 calc R . . B12 B 0.9428(8) 0.3557(5) 0.9615(4) 0.070(3) Uani 1 1 d . . . H12 H 0.9488 0.4096 0.9792 0.084 Uiso 1 1 calc R . . B23 B 0.1946(7) 0.8049(4) 0.6115(4) 0.0480(19) Uani 1 1 d . . . H23 H 0.1293 0.7818 0.6554 0.058 Uiso 1 1 calc R . . B24 B 0.1363(7) 0.8804(5) 0.5384(4) 0.060(2) Uani 1 1 d . . . H24 H 0.0335 0.9057 0.5338 0.072 Uiso 1 1 calc R . . B25 B 0.2474(7) 0.9440(5) 0.5055(4) 0.052(2) Uani 1 1 d . . . H25 H 0.2177 1.0106 0.4792 0.062 Uiso 1 1 calc R . . B26 B 0.3736(6) 0.9051(4) 0.5608(3) 0.0399(17) Uani 1 1 d . . . H26 H 0.4253 0.9466 0.5717 0.048 Uiso 1 1 calc R . . B27 B 0.3389(6) 0.7399(4) 0.5861(4) 0.0451(19) Uani 1 1 d . . . H27 H 0.3685 0.6735 0.6130 0.054 Uiso 1 1 calc R . . B28 B 0.2130(7) 0.7763(5) 0.5332(4) 0.059(2) Uani 1 1 d . . . H28 H 0.1602 0.7336 0.5252 0.070 Uiso 1 1 calc R . . B29 B 0.2464(8) 0.8631(5) 0.4679(4) 0.063(2) Uani 1 1 d . . . H29 H 0.2156 0.8774 0.4163 0.076 Uiso 1 1 calc R . . B30 B 0.3921(7) 0.8793(4) 0.4815(4) 0.055(2) Uani 1 1 d . . . H30 H 0.4577 0.9048 0.4388 0.066 Uiso 1 1 calc R . . B31 B 0.4494(6) 0.8028(4) 0.5536(3) 0.0405(17) Uani 1 1 d . . . H31 H 0.5522 0.7778 0.5585 0.049 Uiso 1 1 calc R . . B32 B 0.3714(7) 0.7753(4) 0.4959(4) 0.053(2) Uani 1 1 d . . . H32 H 0.4214 0.7331 0.4634 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0586(4) 0.0278(3) 0.0355(4) -0.0046(3) -0.0107(3) -0.0082(3) Zr2 0.0454(4) 0.0315(3) 0.0336(4) -0.0058(3) -0.0085(3) -0.0036(3) C1 0.064(4) 0.039(4) 0.030(4) -0.003(3) -0.005(3) -0.009(3) C2 0.062(4) 0.034(3) 0.029(3) -0.002(3) -0.006(3) -0.016(3) C11 0.086(5) 0.031(4) 0.045(4) -0.004(3) -0.013(4) -0.009(3) C12 0.145(7) 0.039(4) 0.056(5) 0.007(4) -0.025(5) -0.036(4) C13 0.103(6) 0.049(4) 0.080(6) -0.018(4) -0.034(5) 0.021(4) C14 0.078(5) 0.023(3) 0.033(4) -0.002(3) -0.013(4) -0.010(3) C15 0.079(6) 0.027(4) 0.072(5) -0.002(3) -0.022(4) -0.017(3) C16 0.110(7) 0.029(4) 0.084(6) -0.009(4) -0.050(5) -0.023(4) C17 0.127(7) 0.040(4) 0.042(5) -0.013(4) -0.023(5) -0.010(5) C18 0.075(5) 0.032(3) 0.044(4) -0.018(3) -0.009(4) 0.000(3) C21 0.032(3) 0.033(3) 0.046(4) -0.012(3) -0.017(3) 0.005(3) C22 0.038(3) 0.031(3) 0.034(3) -0.012(3) -0.008(3) 0.001(3) C31 0.043(4) 0.039(4) 0.049(4) -0.018(3) -0.004(3) 0.003(3) C32 0.097(6) 0.034(4) 0.065(5) -0.011(4) -0.017(4) 0.006(4) C33 0.043(5) 0.086(5) 0.080(6) -0.031(5) -0.012(4) 0.021(4) C34 0.038(4) 0.036(4) 0.049(4) -0.019(3) 0.002(3) 0.003(3) C35 0.063(5) 0.036(4) 0.062(5) -0.028(4) -0.009(4) 0.002(3) C36 0.096(6) 0.067(5) 0.060(5) -0.040(5) -0.031(5) 0.009(5) C37 0.083(6) 0.071(5) 0.035(4) -0.018(4) 0.004(4) 0.015(4) C38 0.042(4) 0.065(5) 0.049(5) -0.021(4) 0.014(4) 0.002(3) C41 0.048(4) 0.037(4) 0.030(4) -0.003(3) -0.020(3) -0.005(3) C42 0.078(5) 0.042(4) 0.035(4) -0.010(3) -0.019(4) -0.011(3) C43 0.072(5) 0.053(4) 0.042(4) -0.020(4) -0.016(4) 0.002(4) C44 0.056(4) 0.051(4) 0.040(4) 0.002(3) -0.009(3) -0.009(3) C45 0.052(4) 0.036(4) 0.053(4) 0.000(3) -0.014(3) -0.011(3) C46 0.049(4) 0.030(3) 0.039(4) -0.009(3) -0.015(3) 0.000(3) C47 0.058(5) 0.037(4) 0.042(4) -0.008(3) -0.007(4) -0.023(3) C48 0.054(5) 0.098(6) 0.058(5) -0.010(4) -0.020(4) -0.024(4) C49 0.055(4) 0.040(4) 0.063(5) -0.002(3) -0.002(4) -0.020(3) C50 0.044(4) 0.052(4) 0.067(5) -0.009(4) 0.000(4) -0.015(3) C51 0.089(5) 0.053(4) 0.045(4) 0.007(3) -0.013(4) -0.019(4) C52 0.054(4) 0.039(4) 0.027(3) -0.001(3) -0.009(3) -0.008(3) C53 0.069(5) 0.043(4) 0.036(4) 0.006(3) -0.014(4) -0.017(4) C54 0.075(5) 0.041(4) 0.050(4) 0.001(3) -0.026(4) -0.013(4) C55 0.081(6) 0.052(5) 0.079(6) 0.008(4) -0.035(5) -0.010(4) C56 0.112(8) 0.081(6) 0.087(7) 0.020(5) -0.070(6) -0.041(5) C57 0.137(8) 0.088(7) 0.067(6) -0.018(5) -0.046(6) -0.040(6) C58 0.097(6) 0.055(4) 0.046(4) -0.008(4) -0.029(4) -0.015(4) C61 0.077(5) 0.026(3) 0.056(5) -0.007(3) 0.014(4) -0.004(3) C62 0.078(6) 0.054(5) 0.085(6) 0.008(4) 0.001(5) -0.008(4) C63 0.094(8) 0.062(6) 0.153(11) 0.020(6) 0.063(8) 0.016(5) C64 0.181(13) 0.055(7) 0.178(16) -0.017(8) 0.134(14) -0.021(8) C65 0.228(13) 0.072(7) 0.077(8) -0.039(6) 0.085(10) -0.032(9) C66 0.142(8) 0.067(5) 0.050(5) -0.026(4) 0.026(5) -0.021(5) C67 0.052(4) 0.033(3) 0.026(3) -0.005(3) -0.010(3) -0.009(3) C68 0.093(6) 0.043(4) 0.078(6) 0.001(4) 0.038(5) -0.015(4) C69 0.055(4) 0.033(3) 0.055(4) -0.004(3) -0.006(3) -0.012(3) C70 0.047(4) 0.037(4) 0.071(5) -0.023(3) -0.015(4) -0.001(3) C71 0.049(4) 0.063(5) 0.113(6) -0.032(5) 0.011(4) -0.031(4) C72 0.047(4) 0.032(3) 0.034(4) -0.008(3) -0.016(3) -0.003(3) C73 0.062(4) 0.029(3) 0.040(4) -0.008(3) -0.012(3) -0.009(3) C74 0.090(6) 0.049(4) 0.061(5) 0.007(4) -0.031(4) -0.034(4) C75 0.105(7) 0.111(7) 0.056(5) -0.017(5) -0.023(5) -0.056(6) C76 0.099(7) 0.077(6) 0.089(7) -0.047(6) -0.003(5) -0.044(5) C77 0.078(6) 0.045(4) 0.085(6) -0.023(4) 0.013(5) -0.028(4) C78 0.069(5) 0.037(4) 0.059(4) -0.007(3) -0.010(4) -0.024(3) N1 0.058(3) 0.039(3) 0.038(3) -0.009(3) -0.014(3) -0.011(2) N2 0.048(3) 0.054(3) 0.042(3) -0.006(3) -0.009(3) -0.010(3) N3 0.057(3) 0.038(3) 0.043(3) -0.001(3) -0.011(3) -0.009(3) N4 0.056(3) 0.037(3) 0.035(3) 0.000(2) -0.020(3) -0.010(3) N5 0.058(3) 0.030(3) 0.046(3) -0.016(2) -0.003(3) -0.001(2) N6 0.057(3) 0.024(3) 0.056(4) -0.004(3) 0.009(3) -0.009(2) N7 0.042(3) 0.033(3) 0.055(3) -0.012(3) -0.007(3) -0.010(2) N8 0.058(3) 0.026(3) 0.038(3) -0.011(2) -0.016(2) 0.000(2) O1 0.055(3) 0.043(2) 0.037(3) 0.000(2) -0.015(2) -0.010(2) O2 0.048(3) 0.045(2) 0.042(3) -0.002(2) -0.011(2) -0.011(2) O3 0.053(3) 0.036(2) 0.036(2) -0.0120(19) 0.000(2) -0.0082(19) O4 0.035(2) 0.029(2) 0.048(3) -0.0076(19) -0.0170(19) -0.0045(18) B3 0.068(5) 0.039(4) 0.039(5) -0.010(4) -0.002(4) -0.006(4) B4 0.086(6) 0.051(5) 0.022(4) 0.002(4) -0.002(4) -0.006(4) B5 0.071(6) 0.058(5) 0.038(5) 0.003(4) -0.023(4) -0.008(4) B6 0.047(5) 0.058(5) 0.048(5) -0.009(4) -0.007(4) -0.010(4) B7 0.070(6) 0.034(4) 0.059(5) -0.013(4) -0.023(4) 0.001(4) B8 0.084(7) 0.059(5) 0.048(5) -0.022(4) -0.010(5) -0.002(5) B9 0.111(8) 0.067(6) 0.048(5) 0.003(5) -0.043(5) -0.024(5) B10 0.077(7) 0.071(6) 0.073(7) 0.000(5) -0.032(5) -0.019(5) B11 0.067(6) 0.044(5) 0.058(5) 0.009(4) -0.029(4) -0.020(4) B12 0.093(7) 0.059(5) 0.065(6) -0.009(5) -0.037(5) -0.021(5) B23 0.046(5) 0.043(4) 0.058(5) -0.012(4) -0.016(4) -0.010(4) B24 0.054(5) 0.064(5) 0.070(6) -0.026(5) -0.036(5) 0.002(4) B25 0.059(5) 0.046(5) 0.039(5) -0.006(4) -0.011(4) 0.006(4) B26 0.044(4) 0.035(4) 0.036(4) -0.003(3) 0.001(3) -0.009(3) B27 0.056(5) 0.033(4) 0.046(5) -0.012(4) -0.015(4) -0.001(3) B28 0.058(5) 0.055(5) 0.075(6) -0.026(5) -0.029(5) -0.009(4) B29 0.080(6) 0.067(6) 0.048(5) -0.022(5) -0.039(5) 0.002(5) B30 0.061(5) 0.048(5) 0.046(5) 0.000(4) -0.011(4) -0.004(4) B31 0.034(4) 0.034(4) 0.045(4) -0.006(3) -0.006(3) 0.004(3) B32 0.055(5) 0.051(5) 0.055(5) -0.021(4) -0.027(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 2.186(4) . ? Zr1 N5 2.187(5) . ? Zr1 O3 2.218(3) . ? Zr1 N1 2.249(5) . ? Zr1 C2 2.358(5) . ? Zr1 C17 2.491(6) . ? Zr1 C16 2.510(6) . ? Zr1 C15 2.511(6) . ? Zr1 C18 2.515(5) . ? Zr1 C14 2.538(5) . ? Zr1 C67 2.643(6) . ? Zr1 C47 2.650(7) . ? Zr2 N8 2.173(5) . ? Zr2 O2 2.179(4) . ? Zr2 O4 2.202(3) . ? Zr2 N4 2.259(4) . ? Zr2 C22 2.383(5) . ? Zr2 C37 2.493(6) . ? Zr2 C36 2.495(6) . ? Zr2 C35 2.513(5) . ? Zr2 C38 2.538(6) . ? Zr2 C34 2.557(5) . ? Zr2 C72 2.616(6) . ? Zr2 C52 2.650(6) . ? C1 C11 1.586(7) . ? C1 B3 1.685(9) . ? C1 B6 1.690(9) . ? C1 C2 1.693(7) . ? C1 B4 1.698(8) . ? C1 B5 1.698(9) . ? C2 B3 1.697(9) . ? C2 B7 1.701(8) . ? C2 B11 1.724(8) . ? C2 B6 1.726(9) . ? C11 C13 1.528(8) . ? C11 C14 1.529(8) . ? C11 C12 1.533(8) . ? C14 C15 1.383(8) . ? C14 C18 1.420(8) . ? C15 C16 1.403(8) . ? C16 C17 1.380(9) . ? C17 C18 1.412(8) . ? C21 C31 1.557(7) . ? C21 B26 1.689(8) . ? C21 C22 1.698(7) . ? C21 B23 1.700(8) . ? C21 B25 1.704(9) . ? C21 B24 1.705(8) . ? C22 B31 1.701(8) . ? C22 B26 1.701(8) . ? C22 B27 1.702(7) . ? C22 B23 1.710(8) . ? C31 C33 1.526(8) . ? C31 C34 1.526(8) . ? C31 C32 1.533(8) . ? C34 C35 1.418(8) . ? C34 C38 1.420(8) . ? C35 C36 1.396(9) . ? C36 C37 1.414(9) . ? C37 C38 1.395(8) . ? C41 C46 1.378(7) . ? C41 C42 1.383(7) . ? C41 N1 1.419(7) . ? C42 C43 1.356(8) . ? C43 C44 1.387(7) . ? C44 C45 1.347(7) . ? C45 C46 1.388(7) . ? C47 O1 1.297(6) . ? C47 N1 1.339(7) . ? C47 N2 1.355(7) . ? C48 N2 1.466(7) . ? C49 N2 1.457(7) . ? C49 C50 1.533(7) . ? C50 N3 1.459(7) . ? C51 N3 1.467(7) . ? C52 O2 1.313(6) . ? C52 N4 1.323(7) . ? C52 N3 1.350(7) . ? C53 C54 1.380(8) . ? C53 C58 1.388(8) . ? C53 N4 1.409(7) . ? C54 C55 1.386(8) . ? C55 C56 1.371(9) . ? C56 C57 1.396(10) . ? C57 C58 1.356(9) . ? C61 C62 1.382(9) . ? C61 C66 1.410(9) . ? C61 N5 1.425(7) . ? C62 C63 1.418(10) . ? C63 C64 1.308(16) . ? C64 C65 1.395(17) . ? C65 C66 1.368(11) . ? C67 O3 1.284(6) . ? C67 N6 1.344(7) . ? C67 N5 1.356(6) . ? C68 N6 1.449(7) . ? C69 N6 1.458(6) . ? C69 C70 1.501(7) . ? C70 N7 1.485(6) . ? C71 N7 1.467(7) . ? C72 O4 1.290(6) . ? C72 N8 1.335(6) . ? C72 N7 1.356(6) . ? C73 C78 1.356(7) . ? C73 C74 1.378(8) . ? C73 N8 1.434(6) . ? C74 C75 1.391(8) . ? C75 C76 1.352(10) . ? C76 C77 1.353(9) . ? C77 C78 1.402(8) . ? B3 B4 1.751(10) . ? B3 B8 1.754(10) . ? B3 B7 1.754(9) . ? B4 B5 1.727(11) . ? B4 B9 1.749(11) . ? B4 B8 1.790(10) . ? B5 B9 1.745(11) . ? B5 B10 1.758(11) . ? B5 B6 1.780(10) . ? B6 B11 1.759(10) . ? B6 B10 1.761(10) . ? B7 B8 1.748(10) . ? B7 B12 1.767(10) . ? B7 B11 1.770(10) . ? B8 B12 1.756(12) . ? B8 B9 1.774(11) . ? B9 B12 1.755(11) . ? B9 B10 1.777(12) . ? B10 B11 1.758(10) . ? B10 B12 1.782(11) . ? B11 B12 1.770(11) . ? B23 B24 1.760(10) . ? B23 B27 1.768(9) . ? B23 B28 1.768(10) . ? B24 B29 1.761(11) . ? B24 B25 1.765(11) . ? B24 B28 1.783(10) . ? B25 B30 1.759(10) . ? B25 B29 1.765(9) . ? B25 B26 1.791(9) . ? B26 B30 1.765(9) . ? B26 B31 1.765(8) . ? B27 B31 1.751(9) . ? B27 B28 1.757(9) . ? B27 B32 1.778(10) . ? B28 B32 1.769(11) . ? B28 B29 1.769(11) . ? B29 B30 1.757(10) . ? B29 B32 1.772(10) . ? B30 B31 1.750(9) . ? B30 B32 1.788(10) . ? B31 B32 1.782(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 N5 141.01(15) . . ? O1 Zr1 O3 85.32(13) . . ? N5 Zr1 O3 59.79(14) . . ? O1 Zr1 N1 59.38(16) . . ? N5 Zr1 N1 94.80(18) . . ? O3 Zr1 N1 79.19(15) . . ? O1 Zr1 C2 89.08(17) . . ? N5 Zr1 C2 102.05(19) . . ? O3 Zr1 C2 82.72(16) . . ? N1 Zr1 C2 144.53(18) . . ? O1 Zr1 C17 121.7(2) . . ? N5 Zr1 C17 84.4(2) . . ? O3 Zr1 C17 141.6(2) . . ? N1 Zr1 C17 91.5(2) . . ? C2 Zr1 C17 120.8(2) . . ? O1 Zr1 C16 90.2(2) . . ? N5 Zr1 C16 114.4(2) . . ? O3 Zr1 C16 156.23(19) . . ? N1 Zr1 C16 78.45(19) . . ? C2 Zr1 C16 120.6(2) . . ? C17 Zr1 C16 32.0(2) . . ? O1 Zr1 C15 81.78(19) . . ? N5 Zr1 C15 134.89(19) . . ? O3 Zr1 C15 164.78(19) . . ? N1 Zr1 C15 100.9(2) . . ? C2 Zr1 C15 89.0(2) . . ? C17 Zr1 C15 53.5(2) . . ? C16 Zr1 C15 32.44(19) . . ? O1 Zr1 C18 135.45(18) . . ? N5 Zr1 C18 82.58(19) . . ? O3 Zr1 C18 138.39(18) . . ? N1 Zr1 C18 124.26(18) . . ? C2 Zr1 C18 89.04(19) . . ? C17 Zr1 C18 32.77(19) . . ? C16 Zr1 C18 53.8(2) . . ? C15 Zr1 C18 53.7(2) . . ? O1 Zr1 C14 106.70(18) . . ? N5 Zr1 C14 112.25(19) . . ? O3 Zr1 C14 150.00(17) . . ? N1 Zr1 C14 130.70(19) . . ? C2 Zr1 C14 70.40(18) . . ? C17 Zr1 C14 53.6(2) . . ? C16 Zr1 C14 53.2(2) . . ? C15 Zr1 C14 31.78(18) . . ? C18 Zr1 C14 32.64(18) . . ? O1 Zr1 C67 112.85(16) . . ? N5 Zr1 C67 30.80(15) . . ? O3 Zr1 C67 28.99(13) . . ? N1 Zr1 C67 86.44(17) . . ? C2 Zr1 C67 92.28(17) . . ? C17 Zr1 C67 114.2(2) . . ? C16 Zr1 C67 140.8(2) . . ? C15 Zr1 C67 165.3(2) . . ? C18 Zr1 C67 111.7(2) . . ? C14 Zr1 C67 136.4(2) . . ? O1 Zr1 C47 29.15(15) . . ? N5 Zr1 C47 119.13(18) . . ? O3 Zr1 C47 79.41(15) . . ? N1 Zr1 C47 30.33(16) . . ? C2 Zr1 C47 116.21(19) . . ? C17 Zr1 C47 110.3(2) . . ? C16 Zr1 C47 85.3(2) . . ? C15 Zr1 C47 93.0(2) . . ? C18 Zr1 C47 139.08(19) . . ? C14 Zr1 C47 124.0(2) . . ? C67 Zr1 C47 99.54(17) . . ? N8 Zr2 O2 138.58(14) . . ? N8 Zr2 O4 60.12(13) . . ? O2 Zr2 O4 83.57(13) . . ? N8 Zr2 N4 92.50(17) . . ? O2 Zr2 N4 59.34(15) . . ? O4 Zr2 N4 79.11(15) . . ? N8 Zr2 C22 101.12(18) . . ? O2 Zr2 C22 91.78(16) . . ? O4 Zr2 C22 81.66(14) . . ? N4 Zr2 C22 146.72(17) . . ? N8 Zr2 C37 115.3(2) . . ? O2 Zr2 C37 90.2(2) . . ? O4 Zr2 C37 157.43(19) . . ? N4 Zr2 C37 79.1(2) . . ? C22 Zr2 C37 120.3(2) . . ? N8 Zr2 C36 84.5(2) . . ? O2 Zr2 C36 122.5(2) . . ? O4 Zr2 C36 142.5(2) . . ? N4 Zr2 C36 91.4(2) . . ? C22 Zr2 C36 119.8(2) . . ? C37 Zr2 C36 32.9(2) . . ? N8 Zr2 C35 83.71(18) . . ? O2 Zr2 C35 136.39(18) . . ? O4 Zr2 C35 139.21(19) . . ? N4 Zr2 C35 123.77(19) . . ? C22 Zr2 C35 88.11(19) . . ? C37 Zr2 C35 53.6(2) . . ? C36 Zr2 C35 32.4(2) . . ? N8 Zr2 C38 136.01(18) . . ? O2 Zr2 C38 82.66(18) . . ? O4 Zr2 C38 163.23(18) . . ? N4 Zr2 C38 101.8(2) . . ? C22 Zr2 C38 89.2(2) . . ? C37 Zr2 C38 32.18(19) . . ? C36 Zr2 C38 54.2(2) . . ? C35 Zr2 C38 53.7(2) . . ? N8 Zr2 C34 112.98(18) . . ? O2 Zr2 C34 108.42(17) . . ? O4 Zr2 C34 148.90(16) . . ? N4 Zr2 C34 131.86(18) . . ? C22 Zr2 C34 69.66(17) . . ? C37 Zr2 C34 53.4(2) . . ? C36 Zr2 C34 53.9(2) . . ? C35 Zr2 C34 32.46(17) . . ? C38 Zr2 C34 32.37(18) . . ? N8 Zr2 C72 30.62(14) . . ? O2 Zr2 C72 110.96(15) . . ? O4 Zr2 C72 29.50(13) . . ? N4 Zr2 C72 84.68(17) . . ? C22 Zr2 C72 91.75(17) . . ? C37 Zr2 C72 141.5(2) . . ? C36 Zr2 C72 114.2(2) . . ? C35 Zr2 C72 112.6(2) . . ? C38 Zr2 C72 166.29(19) . . ? C34 Zr2 C72 136.72(19) . . ? N8 Zr2 C52 115.85(17) . . ? O2 Zr2 C52 29.57(15) . . ? O4 Zr2 C52 77.61(15) . . ? N4 Zr2 C52 29.96(15) . . ? C22 Zr2 C52 118.88(18) . . ? C37 Zr2 C52 86.3(2) . . ? C36 Zr2 C52 111.0(2) . . ? C35 Zr2 C52 139.8(2) . . ? C38 Zr2 C52 94.8(2) . . ? C34 Zr2 C52 126.57(19) . . ? C72 Zr2 C52 96.70(17) . . ? C11 C1 B3 118.2(5) . . ? C11 C1 B6 116.5(5) . . ? B3 C1 B6 112.2(5) . . ? C11 C1 C2 116.4(4) . . ? B3 C1 C2 60.3(4) . . ? B6 C1 C2 61.4(4) . . ? C11 C1 B4 122.7(5) . . ? B3 C1 B4 62.3(4) . . ? B6 C1 B4 113.5(5) . . ? C2 C1 B4 110.9(4) . . ? C11 C1 B5 122.3(5) . . ? B3 C1 B5 112.2(5) . . ? B6 C1 B5 63.4(4) . . ? C2 C1 B5 111.7(5) . . ? B4 C1 B5 61.1(4) . . ? C1 C2 B3 59.6(3) . . ? C1 C2 B7 109.1(4) . . ? B3 C2 B7 62.2(4) . . ? C1 C2 B11 108.0(4) . . ? B3 C2 B11 111.8(5) . . ? B7 C2 B11 62.2(4) . . ? C1 C2 B6 59.2(4) . . ? B3 C2 B6 109.9(5) . . ? B7 C2 B6 112.0(5) . . ? B11 C2 B6 61.3(4) . . ? C1 C2 Zr1 120.0(3) . . ? B3 C2 Zr1 118.7(4) . . ? B7 C2 Zr1 121.5(4) . . ? B11 C2 Zr1 122.5(4) . . ? B6 C2 Zr1 119.4(4) . . ? C13 C11 C14 109.1(5) . . ? C13 C11 C12 108.2(5) . . ? C14 C11 C12 109.0(5) . . ? C13 C11 C1 111.9(5) . . ? C14 C11 C1 108.5(5) . . ? C12 C11 C1 110.1(5) . . ? C15 C14 C18 108.1(6) . . ? C15 C14 C11 127.5(6) . . ? C18 C14 C11 124.1(6) . . ? C15 C14 Zr1 73.0(3) . . ? C18 C14 Zr1 72.8(3) . . ? C11 C14 Zr1 124.6(3) . . ? C14 C15 C16 108.6(7) . . ? C14 C15 Zr1 75.2(3) . . ? C16 C15 Zr1 73.7(4) . . ? C17 C16 C15 107.9(7) . . ? C17 C16 Zr1 73.2(4) . . ? C15 C16 Zr1 73.8(3) . . ? C16 C17 C18 109.0(6) . . ? C16 C17 Zr1 74.7(4) . . ? C18 C17 Zr1 74.6(3) . . ? C17 C18 C14 106.4(6) . . ? C17 C18 Zr1 72.7(3) . . ? C14 C18 Zr1 74.6(3) . . ? C31 C21 B26 116.6(4) . . ? C31 C21 C22 116.2(4) . . ? B26 C21 C22 60.3(3) . . ? C31 C21 B23 116.9(5) . . ? B26 C21 B23 112.1(4) . . ? C22 C21 B23 60.4(3) . . ? C31 C21 B25 122.6(5) . . ? B26 C21 B25 63.7(4) . . ? C22 C21 B25 111.3(4) . . ? B23 C21 B25 113.4(4) . . ? C31 C21 B24 122.8(5) . . ? B26 C21 B24 114.3(5) . . ? C22 C21 B24 110.5(4) . . ? B23 C21 B24 62.2(4) . . ? B25 C21 B24 62.4(4) . . ? C21 C22 B31 108.9(4) . . ? C21 C22 B26 59.6(3) . . ? B31 C22 B26 62.5(4) . . ? C21 C22 B27 109.5(4) . . ? B31 C22 B27 61.9(3) . . ? B26 C22 B27 113.1(4) . . ? C21 C22 B23 59.9(3) . . ? B31 C22 B23 112.3(4) . . ? B26 C22 B23 111.1(5) . . ? B27 C22 B23 62.4(3) . . ? C21 C22 Zr2 120.1(3) . . ? B31 C22 Zr2 122.8(3) . . ? B26 C22 Zr2 120.0(3) . . ? B27 C22 Zr2 119.9(4) . . ? B23 C22 Zr2 116.7(4) . . ? C33 C31 C34 108.1(5) . . ? C33 C31 C32 107.4(5) . . ? C34 C31 C32 108.7(5) . . ? C33 C31 C21 111.6(5) . . ? C34 C31 C21 109.8(4) . . ? C32 C31 C21 111.1(5) . . ? C35 C34 C38 107.1(6) . . ? C35 C34 C31 126.3(6) . . ? C38 C34 C31 126.4(6) . . ? C35 C34 Zr2 72.1(3) . . ? C38 C34 Zr2 73.1(3) . . ? C31 C34 Zr2 124.2(3) . . ? C36 C35 C34 109.1(7) . . ? C36 C35 Zr2 73.1(4) . . ? C34 C35 Zr2 75.5(3) . . ? C35 C36 C37 107.0(6) . . ? C35 C36 Zr2 74.5(3) . . ? C37 C36 Zr2 73.5(4) . . ? C38 C37 C36 109.3(7) . . ? C38 C37 Zr2 75.7(3) . . ? C36 C37 Zr2 73.6(4) . . ? C37 C38 C34 107.6(6) . . ? C37 C38 Zr2 72.1(4) . . ? C34 C38 Zr2 74.5(3) . . ? C46 C41 C42 119.3(5) . . ? C46 C41 N1 121.8(5) . . ? C42 C41 N1 118.6(5) . . ? C43 C42 C41 121.5(6) . . ? C42 C43 C44 119.1(6) . . ? C45 C44 C43 119.9(6) . . ? C44 C45 C46 121.7(6) . . ? C41 C46 C45 118.5(5) . . ? O1 C47 N1 112.9(6) . . ? O1 C47 N2 120.5(6) . . ? N1 C47 N2 126.4(6) . . ? O1 C47 Zr1 55.2(3) . . ? N1 C47 Zr1 58.0(3) . . ? N2 C47 Zr1 175.6(5) . . ? N2 C49 C50 113.7(5) . . ? N3 C50 C49 112.8(5) . . ? O2 C52 N4 112.9(5) . . ? O2 C52 N3 118.7(5) . . ? N4 C52 N3 128.3(5) . . ? O2 C52 Zr2 54.9(3) . . ? N4 C52 Zr2 58.4(3) . . ? N3 C52 Zr2 172.0(4) . . ? C54 C53 C58 119.5(6) . . ? C54 C53 N4 121.0(6) . . ? C58 C53 N4 119.3(6) . . ? C53 C54 C55 120.2(6) . . ? C56 C55 C54 119.8(7) . . ? C55 C56 C57 119.7(7) . . ? C58 C57 C56 120.4(7) . . ? C57 C58 C53 120.3(7) . . ? C62 C61 C66 119.6(7) . . ? C62 C61 N5 120.8(7) . . ? C66 C61 N5 119.4(7) . . ? C61 C62 C63 117.8(9) . . ? C64 C63 C62 123.5(13) . . ? C63 C64 C65 118.2(13) . . ? C66 C65 C64 122.0(12) . . ? C65 C66 C61 118.7(9) . . ? O3 C67 N6 120.9(5) . . ? O3 C67 N5 112.5(5) . . ? N6 C67 N5 126.6(5) . . ? O3 C67 Zr1 56.8(3) . . ? N6 C67 Zr1 177.7(4) . . ? N5 C67 Zr1 55.7(3) . . ? N6 C69 C70 111.1(5) . . ? N7 C70 C69 112.6(4) . . ? O4 C72 N8 113.2(5) . . ? O4 C72 N7 119.7(4) . . ? N8 C72 N7 127.1(5) . . ? O4 C72 Zr2 57.2(3) . . ? N8 C72 Zr2 56.0(3) . . ? N7 C72 Zr2 176.8(4) . . ? C78 C73 C74 119.5(6) . . ? C78 C73 N8 120.3(5) . . ? C74 C73 N8 119.8(5) . . ? C73 C74 C75 119.6(6) . . ? C76 C75 C74 119.7(7) . . ? C75 C76 C77 121.9(7) . . ? C76 C77 C78 118.3(7) . . ? C73 C78 C77 121.0(6) . . ? C47 N1 C41 131.3(5) . . ? C47 N1 Zr1 91.7(4) . . ? C41 N1 Zr1 128.8(4) . . ? C47 N2 C49 119.2(5) . . ? C47 N2 C48 122.7(5) . . ? C49 N2 C48 115.9(5) . . ? C52 N3 C50 120.7(5) . . ? C52 N3 C51 122.4(5) . . ? C50 N3 C51 115.4(5) . . ? C52 N4 C53 128.6(5) . . ? C52 N4 Zr2 91.6(3) . . ? C53 N4 Zr2 133.0(4) . . ? C67 N5 C61 127.1(5) . . ? C67 N5 Zr1 93.5(4) . . ? C61 N5 Zr1 136.8(3) . . ? C67 N6 C68 123.9(5) . . ? C67 N6 C69 119.0(5) . . ? C68 N6 C69 115.2(5) . . ? C72 N7 C71 123.2(5) . . ? C72 N7 C70 118.2(5) . . ? C71 N7 C70 116.5(5) . . ? C72 N8 C73 125.4(5) . . ? C72 N8 Zr2 93.3(4) . . ? C73 N8 Zr2 138.4(3) . . ? C47 O1 Zr1 95.7(4) . . ? C52 O2 Zr2 95.5(3) . . ? C67 O3 Zr1 94.2(3) . . ? C72 O4 Zr2 93.3(3) . . ? C1 B3 C2 60.1(4) . . ? C1 B3 B4 59.2(4) . . ? C2 B3 B4 108.2(5) . . ? C1 B3 B8 107.3(5) . . ? C2 B3 B8 107.1(5) . . ? B4 B3 B8 61.4(4) . . ? C1 B3 B7 107.0(5) . . ? C2 B3 B7 59.0(4) . . ? B4 B3 B7 109.1(5) . . ? B8 B3 B7 59.8(4) . . ? C1 B4 B5 59.4(4) . . ? C1 B4 B9 105.8(6) . . ? B5 B4 B9 60.3(5) . . ? C1 B4 B3 58.5(4) . . ? B5 B4 B3 107.7(5) . . ? B9 B4 B3 107.3(5) . . ? C1 B4 B8 105.2(5) . . ? B5 B4 B8 108.4(6) . . ? B9 B4 B8 60.2(4) . . ? B3 B4 B8 59.4(4) . . ? C1 B5 B4 59.4(4) . . ? C1 B5 B9 106.0(6) . . ? B4 B5 B9 60.5(4) . . ? C1 B5 B10 105.3(5) . . ? B4 B5 B10 109.3(6) . . ? B9 B5 B10 61.0(5) . . ? C1 B5 B6 58.1(4) . . ? B4 B5 B6 107.8(5) . . ? B9 B5 B6 108.1(5) . . ? B10 B5 B6 59.7(4) . . ? C1 B6 C2 59.4(4) . . ? C1 B6 B11 106.5(5) . . ? C2 B6 B11 59.3(4) . . ? C1 B6 B10 105.6(5) . . ? C2 B6 B10 106.4(5) . . ? B11 B6 B10 59.9(4) . . ? C1 B6 B5 58.5(4) . . ? C2 B6 B5 106.3(5) . . ? B11 B6 B5 107.4(5) . . ? B10 B6 B5 59.5(4) . . ? C2 B7 B8 107.1(5) . . ? C2 B7 B3 58.8(3) . . ? B8 B7 B3 60.1(4) . . ? C2 B7 B12 106.7(5) . . ? B8 B7 B12 59.9(4) . . ? B3 B7 B12 107.1(5) . . ? C2 B7 B11 59.5(4) . . ? B8 B7 B11 108.3(5) . . ? B3 B7 B11 107.0(5) . . ? B12 B7 B11 60.1(4) . . ? B7 B8 B3 60.1(4) . . ? B7 B8 B12 60.6(5) . . ? B3 B8 B12 107.6(6) . . ? B7 B8 B9 107.9(6) . . ? B3 B8 B9 106.1(5) . . ? B12 B8 B9 59.6(5) . . ? B7 B8 B4 107.7(5) . . ? B3 B8 B4 59.2(4) . . ? B12 B8 B4 106.8(6) . . ? B9 B8 B4 58.8(4) . . ? B5 B9 B4 59.2(4) . . ? B5 B9 B12 108.6(6) . . ? B4 B9 B12 108.7(6) . . ? B5 B9 B8 108.3(5) . . ? B4 B9 B8 61.1(4) . . ? B12 B9 B8 59.7(5) . . ? B5 B9 B10 59.9(4) . . ? B4 B9 B10 107.5(5) . . ? B12 B9 B10 60.6(5) . . ? B8 B9 B10 108.0(6) . . ? B11 B10 B5 108.5(6) . . ? B11 B10 B6 60.0(4) . . ? B5 B10 B6 60.8(4) . . ? B11 B10 B9 107.4(6) . . ? B5 B10 B9 59.2(5) . . ? B6 B10 B9 107.5(6) . . ? B11 B10 B12 60.0(4) . . ? B5 B10 B12 106.8(6) . . ? B6 B10 B12 107.5(6) . . ? B9 B10 B12 59.1(5) . . ? C2 B11 B10 106.6(5) . . ? C2 B11 B6 59.4(4) . . ? B10 B11 B6 60.1(4) . . ? C2 B11 B7 58.3(4) . . ? B10 B11 B7 108.4(6) . . ? B6 B11 B7 107.2(5) . . ? C2 B11 B12 105.6(5) . . ? B10 B11 B12 60.7(4) . . ? B6 B11 B12 108.1(5) . . ? B7 B11 B12 59.9(4) . . ? B9 B12 B8 60.7(5) . . ? B9 B12 B7 107.8(6) . . ? B8 B12 B7 59.5(4) . . ? B9 B12 B11 107.8(6) . . ? B8 B12 B11 107.9(5) . . ? B7 B12 B11 60.0(4) . . ? B9 B12 B10 60.3(5) . . ? B8 B12 B10 108.6(6) . . ? B7 B12 B10 107.4(5) . . ? B11 B12 B10 59.3(4) . . ? C21 B23 C22 59.7(3) . . ? C21 B23 B24 59.0(4) . . ? C22 B23 B24 107.4(5) . . ? C21 B23 B27 106.3(5) . . ? C22 B23 B27 58.6(3) . . ? B24 B23 B27 108.5(5) . . ? C21 B23 B28 106.2(5) . . ? C22 B23 B28 105.8(5) . . ? B24 B23 B28 60.7(4) . . ? B27 B23 B28 59.6(4) . . ? C21 B24 B23 58.8(4) . . ? C21 B24 B29 105.0(5) . . ? B23 B24 B29 107.4(5) . . ? C21 B24 B25 58.8(4) . . ? B23 B24 B25 107.7(5) . . ? B29 B24 B25 60.1(4) . . ? C21 B24 B28 105.3(5) . . ? B23 B24 B28 59.9(4) . . ? B29 B24 B28 59.9(4) . . ? B25 B24 B28 108.3(6) . . ? C21 B25 B30 104.2(5) . . ? C21 B25 B29 104.8(5) . . ? B30 B25 B29 59.8(4) . . ? C21 B25 B24 58.8(4) . . ? B30 B25 B24 107.3(5) . . ? B29 B25 B24 59.8(4) . . ? C21 B25 B26 57.7(3) . . ? B30 B25 B26 59.6(4) . . ? B29 B25 B26 107.0(5) . . ? B24 B25 B26 106.6(5) . . ? C21 B26 C22 60.1(3) . . ? C21 B26 B30 104.6(5) . . ? C22 B26 B30 105.3(5) . . ? C21 B26 B31 106.3(5) . . ? C22 B26 B31 58.7(3) . . ? B30 B26 B31 59.4(4) . . ? C21 B26 B25 58.6(4) . . ? C22 B26 B25 107.1(5) . . ? B30 B26 B25 59.3(4) . . ? B31 B26 B25 107.5(5) . . ? C22 B27 B31 59.0(3) . . ? C22 B27 B28 106.7(4) . . ? B31 B27 B28 108.2(5) . . ? C22 B27 B23 59.0(3) . . ? B31 B27 B23 107.2(4) . . ? B28 B27 B23 60.2(4) . . ? C22 B27 B32 107.1(5) . . ? B31 B27 B32 60.7(4) . . ? B28 B27 B32 60.0(4) . . ? B23 B27 B32 108.2(5) . . ? B27 B28 B23 60.2(4) . . ? B27 B28 B32 60.6(4) . . ? B23 B28 B32 108.6(5) . . ? B27 B28 B29 107.6(5) . . ? B23 B28 B29 106.6(5) . . ? B32 B28 B29 60.1(4) . . ? B27 B28 B24 108.0(5) . . ? B23 B28 B24 59.4(4) . . ? B32 B28 B24 108.5(6) . . ? B29 B28 B24 59.4(4) . . ? B30 B29 B24 107.6(5) . . ? B30 B29 B25 59.9(4) . . ? B24 B29 B25 60.1(4) . . ? B30 B29 B28 107.7(5) . . ? B24 B29 B28 60.7(4) . . ? B25 B29 B28 108.9(5) . . ? B30 B29 B32 60.9(4) . . ? B24 B29 B32 109.3(6) . . ? B25 B29 B32 109.9(5) . . ? B28 B29 B32 59.9(4) . . ? B31 B30 B29 108.1(6) . . ? B31 B30 B25 109.6(5) . . ? B29 B30 B25 60.3(4) . . ? B31 B30 B26 60.3(4) . . ? B29 B30 B26 108.5(5) . . ? B25 B30 B26 61.1(4) . . ? B31 B30 B32 60.5(4) . . ? B29 B30 B32 60.0(4) . . ? B25 B30 B32 109.5(5) . . ? B26 B30 B32 109.1(5) . . ? C22 B31 B30 105.9(4) . . ? C22 B31 B27 59.1(3) . . ? B30 B31 B27 108.3(5) . . ? C22 B31 B26 58.7(3) . . ? B30 B31 B26 60.3(4) . . ? B27 B31 B26 107.7(5) . . ? C22 B31 B32 107.0(5) . . ? B30 B31 B32 60.8(4) . . ? B27 B31 B32 60.4(4) . . ? B26 B31 B32 109.4(5) . . ? B28 B32 B29 60.0(4) . . ? B28 B32 B27 59.4(4) . . ? B29 B32 B27 106.6(5) . . ? B28 B32 B31 106.3(5) . . ? B29 B32 B31 106.1(5) . . ? B27 B32 B31 58.9(4) . . ? B28 B32 B30 106.4(5) . . ? B29 B32 B30 59.2(4) . . ? B27 B32 B30 105.4(5) . . ? B31 B32 B30 58.7(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.541 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.084 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.019 0.326 0.174 38.6 -0.4 2 0.019 0.674 0.826 38.6 -0.4 3 0.500 0.000 1.000 328.4 48.2 4 0.330 0.114 0.483 11.6 0.0 5 0.670 0.886 0.517 11.7 -0.1 _platon_squeeze_details ; ; #===END data_5b _database_code_depnum_ccdc_archive 'CCDC 665271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H80 B20 N8 Si2 Zr2' _chemical_formula_weight 1079.90 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' B B 0.0013 0.0007 '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' Si Si 0.0817 0.0704 '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 15.7412(16) _cell_length_b 10.7205(12) _cell_length_c 16.2567(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.213(2) _cell_angle_gamma 90.00 _cell_volume 2691.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 809 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 27.68 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.469 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 1.0000 _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 '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 17992 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.02 _reflns_number_total 6500 _reflns_number_gt 4257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0701P)^2^+1.9010P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6500 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.32299(2) 0.49079(3) 0.03741(2) 0.02673(12) Uani 1 1 d . . . Si1 Si 0.47529(7) 0.24114(10) 0.15826(7) 0.0358(3) Uani 1 1 d . . . N1 N 0.3962(2) 0.6200(3) 0.1500(2) 0.0391(8) Uani 1 1 d . . . H1 H 0.3621 0.6888 0.1483 0.047 Uiso 1 1 calc R . . N2 N 0.2665(2) 0.4496(3) 0.1404(2) 0.0406(8) Uani 1 1 d . . . C26 C 0.5170(2) 0.3924(3) 0.0536(2) 0.0275(7) Uani 1 1 d . . . C1 C 0.1657(2) 0.6973(4) -0.0857(2) 0.0355(8) Uani 1 1 d . . . C2 C 0.2443(2) 0.6859(3) 0.0033(2) 0.0296(8) Uani 1 1 d . . . C11 C 0.1515(2) 0.5781(4) -0.1408(2) 0.0394(9) Uani 1 1 d . . . C12 C 0.1733(3) 0.6004(5) -0.2279(3) 0.0572(12) Uani 1 1 d . . . H12A H 0.2326 0.6261 -0.2216 0.086 Uiso 1 1 calc R . . H12B H 0.1363 0.6645 -0.2564 0.086 Uiso 1 1 calc R . . H12C H 0.1646 0.5247 -0.2599 0.086 Uiso 1 1 calc R . . C13 C 0.0561(3) 0.5360(5) -0.1543(3) 0.0609(14) Uani 1 1 d . . . H13A H 0.0405 0.5212 -0.1010 0.091 Uiso 1 1 calc R . . H13B H 0.0489 0.4606 -0.1868 0.091 Uiso 1 1 calc R . . H13C H 0.0196 0.6000 -0.1837 0.091 Uiso 1 1 calc R . . C14 C 0.2079(2) 0.4714(3) -0.0983(2) 0.0349(9) Uani 1 1 d . . . C15 C 0.2867(3) 0.4279(4) -0.1174(3) 0.0429(10) Uani 1 1 d . . . H15A H 0.3147 0.4610 -0.1616 0.051 Uiso 1 1 calc R . . C16 C 0.3111(3) 0.3198(4) -0.0712(3) 0.0475(11) Uani 1 1 d . . . H16A H 0.3581 0.2636 -0.0788 0.057 Uiso 1 1 calc R . . C17 C 0.2490(3) 0.2946(4) -0.0223(3) 0.0486(11) Uani 1 1 d . . . H17A H 0.2447 0.2173 0.0088 0.058 Uiso 1 1 calc R . . C18 C 0.1850(3) 0.3872(4) -0.0397(3) 0.0449(10) Uani 1 1 d . . . H18A H 0.1295 0.3863 -0.0209 0.054 Uiso 1 1 calc R . . C19 C 0.4844(3) 0.6698(5) 0.1551(3) 0.0546(12) Uani 1 1 d . . . H19A H 0.5002 0.7190 0.2050 0.082 Uiso 1 1 calc R . . H19B H 0.4859 0.7209 0.1069 0.082 Uiso 1 1 calc R . . H19C H 0.5244 0.6019 0.1566 0.082 Uiso 1 1 calc R . . C20 C 0.3894(3) 0.5578(4) 0.2284(3) 0.0495(11) Uani 1 1 d . . . H20A H 0.4033 0.6160 0.2748 0.059 Uiso 1 1 calc R . . H20B H 0.4300 0.4888 0.2387 0.059 Uiso 1 1 calc R . . C21 C 0.2983(3) 0.5103(4) 0.2219(3) 0.0528(12) Uani 1 1 d . . . H21A H 0.2968 0.4510 0.2666 0.063 Uiso 1 1 calc R . . H21B H 0.2605 0.5793 0.2287 0.063 Uiso 1 1 calc R . . C22 C 0.1887(3) 0.3796(5) 0.1500(3) 0.0665(15) Uani 1 1 d . . . H22A H 0.1829 0.3812 0.2077 0.100 Uiso 1 1 calc R . . H22B H 0.1938 0.2947 0.1327 0.100 Uiso 1 1 calc R . . H22C H 0.1385 0.4170 0.1159 0.100 Uiso 1 1 calc R . . C23 C 0.5693(3) 0.2876(4) 0.2405(3) 0.0524(11) Uani 1 1 d . . . H23A H 0.5538 0.3581 0.2709 0.079 Uiso 1 1 calc R . . H23B H 0.6172 0.3094 0.2147 0.079 Uiso 1 1 calc R . . H23C H 0.5856 0.2192 0.2785 0.079 Uiso 1 1 calc R . . C24 C 0.3820(3) 0.1994(4) 0.2065(3) 0.0560(13) Uani 1 1 d . . . H24A H 0.3338 0.1765 0.1634 0.084 Uiso 1 1 calc R . . H24B H 0.3665 0.2696 0.2371 0.084 Uiso 1 1 calc R . . H24C H 0.3974 0.1304 0.2441 0.084 Uiso 1 1 calc R . . C25 C 0.5012(3) 0.1051(4) 0.0976(3) 0.0551(12) Uani 1 1 d . . . H25A H 0.4514 0.0835 0.0558 0.083 Uiso 1 1 calc R . . H25B H 0.5169 0.0356 0.1347 0.083 Uiso 1 1 calc R . . H25C H 0.5486 0.1255 0.0708 0.083 Uiso 1 1 calc R . . N3 N 0.45124(18) 0.3691(3) 0.08731(19) 0.0312(7) Uani 1 1 d . . . N4 N 0.57702(18) 0.4130(3) 0.02350(19) 0.0320(7) Uani 1 1 d . . . B3 B 0.2602(3) 0.7753(4) -0.0811(3) 0.0351(9) Uani 1 1 d . . . H3 H 0.3084 0.7491 -0.1188 0.042 Uiso 1 1 calc R . . B4 B 0.1600(3) 0.8446(5) -0.1270(3) 0.0444(11) Uani 1 1 d . . . H4 H 0.1427 0.8645 -0.1946 0.053 Uiso 1 1 calc R . . B5 B 0.0819(3) 0.7930(5) -0.0692(3) 0.0511(13) Uani 1 1 d . . . H5 H 0.0136 0.7794 -0.0988 0.061 Uiso 1 1 calc R . . B6 B 0.1370(3) 0.6903(4) 0.0113(3) 0.0370(10) Uani 1 1 d . . . H6 H 0.1049 0.6095 0.0336 0.044 Uiso 1 1 calc R . . B7 B 0.2905(3) 0.8325(4) 0.0214(3) 0.0390(10) Uani 1 1 d . . . H7 H 0.3588 0.8456 0.0512 0.047 Uiso 1 1 calc R . . B8 B 0.2385(3) 0.9338(5) -0.0594(3) 0.0478(12) Uani 1 1 d . . . H8 H 0.2724 1.0121 -0.0826 0.057 Uiso 1 1 calc R . . B9 B 0.1272(4) 0.9432(5) -0.0511(4) 0.0559(14) Uani 1 1 d . . . H9 H 0.0886 1.0280 -0.0685 0.067 Uiso 1 1 calc R . . B10 B 0.1125(3) 0.8470(5) 0.0340(3) 0.0516(13) Uani 1 1 d . . . H10 H 0.0638 0.8689 0.0722 0.062 Uiso 1 1 calc R . . B11 B 0.2138(3) 0.7803(4) 0.0779(3) 0.0390(10) Uani 1 1 d . . . H11 H 0.2317 0.7596 0.1453 0.047 Uiso 1 1 calc R . . B12 B 0.2090(4) 0.9370(5) 0.0407(3) 0.0515(13) Uani 1 1 d . . . H12 H 0.2235 1.0178 0.0829 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02216(17) 0.02949(19) 0.03015(19) 0.00281(15) 0.00905(12) 0.00239(14) Si1 0.0348(6) 0.0349(6) 0.0400(6) 0.0123(5) 0.0125(4) 0.0040(4) N1 0.0337(17) 0.046(2) 0.0364(19) -0.0045(15) 0.0029(14) 0.0038(14) N2 0.0348(18) 0.050(2) 0.041(2) 0.0133(16) 0.0171(15) 0.0091(15) C26 0.0298(18) 0.0260(17) 0.0254(18) 0.0046(14) 0.0016(14) 0.0062(14) C1 0.0288(19) 0.041(2) 0.035(2) 0.0028(17) 0.0011(15) 0.0063(16) C2 0.0248(17) 0.0348(19) 0.0287(19) -0.0015(15) 0.0038(14) 0.0018(14) C11 0.034(2) 0.044(2) 0.037(2) -0.0034(18) -0.0025(16) 0.0012(17) C12 0.066(3) 0.065(3) 0.036(2) -0.005(2) -0.004(2) 0.011(2) C13 0.034(2) 0.064(3) 0.075(4) -0.010(3) -0.013(2) -0.005(2) C14 0.0277(18) 0.034(2) 0.040(2) -0.0079(16) 0.0000(16) -0.0038(15) C15 0.040(2) 0.053(3) 0.034(2) -0.0101(19) 0.0051(17) -0.0008(19) C16 0.049(3) 0.038(2) 0.052(3) -0.014(2) 0.001(2) 0.0088(19) C17 0.050(3) 0.031(2) 0.061(3) -0.0035(19) 0.000(2) -0.0029(19) C18 0.036(2) 0.040(2) 0.056(3) -0.004(2) 0.0013(19) -0.0088(18) C19 0.037(2) 0.072(3) 0.051(3) -0.015(2) -0.0017(19) -0.004(2) C20 0.057(3) 0.060(3) 0.029(2) -0.004(2) 0.0039(19) 0.014(2) C21 0.066(3) 0.062(3) 0.037(2) 0.009(2) 0.025(2) 0.017(2) C22 0.044(3) 0.084(4) 0.080(4) 0.038(3) 0.031(2) 0.004(2) C23 0.052(3) 0.055(3) 0.047(3) 0.014(2) 0.002(2) 0.001(2) C24 0.050(3) 0.055(3) 0.070(3) 0.029(2) 0.027(2) 0.005(2) C25 0.063(3) 0.036(2) 0.068(3) 0.006(2) 0.017(2) 0.005(2) N3 0.0260(15) 0.0347(16) 0.0355(17) 0.0103(13) 0.0129(12) 0.0045(12) N4 0.0263(16) 0.0341(17) 0.0381(18) 0.0107(14) 0.0128(13) 0.0052(12) B3 0.036(2) 0.037(2) 0.032(2) 0.0031(18) 0.0063(18) 0.0021(18) B4 0.043(3) 0.046(3) 0.042(3) 0.010(2) 0.002(2) 0.014(2) B5 0.034(3) 0.063(3) 0.055(3) 0.004(3) 0.006(2) 0.019(2) B6 0.025(2) 0.043(2) 0.046(3) 0.005(2) 0.0129(18) 0.0085(18) B7 0.046(3) 0.034(2) 0.036(2) -0.0018(19) 0.0063(19) 0.002(2) B8 0.062(3) 0.036(3) 0.046(3) 0.005(2) 0.010(2) 0.007(2) B9 0.059(3) 0.049(3) 0.060(4) 0.010(3) 0.010(3) 0.021(3) B10 0.047(3) 0.053(3) 0.061(3) 0.004(3) 0.026(2) 0.022(2) B11 0.045(3) 0.035(2) 0.039(3) -0.0024(19) 0.014(2) 0.011(2) B12 0.074(4) 0.036(3) 0.046(3) -0.004(2) 0.015(3) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N2 2.090(3) . ? Zr1 N4 2.265(3) 3_665 ? Zr1 N1 2.403(3) . ? Zr1 N3 2.408(3) . ? Zr1 C2 2.439(3) . ? Zr1 C17 2.507(4) . ? Zr1 C16 2.526(4) . ? Zr1 C18 2.542(4) . ? Zr1 C15 2.560(4) . ? Zr1 C14 2.577(4) . ? Si1 N3 1.785(3) . ? Si1 C24 1.849(4) . ? Si1 C25 1.850(4) . ? Si1 C23 1.859(4) . ? N1 C20 1.462(5) . ? N1 C19 1.474(5) . ? N2 C21 1.473(6) . ? N2 C22 1.471(5) . ? C26 N4 1.167(4) . ? C26 N3 1.286(4) . ? C1 C11 1.553(5) . ? C1 B3 1.695(6) . ? C1 B4 1.711(6) . ? C1 C2 1.715(5) . ? C1 B6 1.724(6) . ? C1 B5 1.732(6) . ? C2 B11 1.718(6) . ? C2 B6 1.720(5) . ? C2 B7 1.732(6) . ? C2 B3 1.731(6) . ? C11 C14 1.529(5) . ? C11 C12 1.538(6) . ? C11 C13 1.542(6) . ? C14 C18 1.408(6) . ? C14 C15 1.415(5) . ? C15 C16 1.393(6) . ? C16 C17 1.401(6) . ? C17 C18 1.404(6) . ? C20 C21 1.505(6) . ? N4 Zr1 2.265(3) 3_665 ? B3 B7 1.753(6) . ? B3 B4 1.772(6) . ? B3 B8 1.782(7) . ? B4 B8 1.767(7) . ? B4 B5 1.774(7) . ? B4 B9 1.776(8) . ? B5 B10 1.752(8) . ? B5 B9 1.763(8) . ? B5 B6 1.798(7) . ? B6 B11 1.748(7) . ? B6 B10 1.779(7) . ? B7 B11 1.744(7) . ? B7 B8 1.777(7) . ? B7 B12 1.776(7) . ? B8 B12 1.779(7) . ? B8 B9 1.786(8) . ? B9 B12 1.773(8) . ? B9 B10 1.776(8) . ? B10 B11 1.767(7) . ? B10 B12 1.785(8) . ? B11 B12 1.781(7) . ? 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 N2 Zr1 N4 152.47(13) . 3_665 ? N2 Zr1 N1 74.21(13) . . ? N4 Zr1 N1 78.40(11) 3_665 . ? N2 Zr1 N3 94.30(11) . . ? N4 Zr1 N3 77.62(10) 3_665 . ? N1 Zr1 N3 78.99(11) . . ? N2 Zr1 C2 95.00(12) . . ? N4 Zr1 C2 82.83(11) 3_665 . ? N1 Zr1 C2 79.99(11) . . ? N3 Zr1 C2 153.70(11) . . ? N2 Zr1 C17 83.96(15) . . ? N4 Zr1 C17 121.54(14) 3_665 . ? N1 Zr1 C17 153.69(14) . . ? N3 Zr1 C17 88.38(12) . . ? C2 Zr1 C17 117.03(13) . . ? N2 Zr1 C16 114.92(15) . . ? N4 Zr1 C16 89.32(14) 3_665 . ? N1 Zr1 C16 155.42(12) . . ? N3 Zr1 C16 77.61(12) . . ? C2 Zr1 C16 119.87(13) . . ? C17 Zr1 C16 32.33(14) . . ? N2 Zr1 C18 81.21(14) . . ? N4 Zr1 C18 125.66(13) 3_665 . ? N1 Zr1 C18 149.85(13) . . ? N3 Zr1 C18 120.63(12) . . ? C2 Zr1 C18 85.13(12) . . ? C17 Zr1 C18 32.28(13) . . ? C16 Zr1 C18 53.03(14) . . ? N2 Zr1 C15 133.12(14) . . ? N4 Zr1 C15 74.40(12) 3_665 . ? N1 Zr1 C15 151.93(13) . . ? N3 Zr1 C15 101.56(12) . . ? C2 Zr1 C15 89.78(13) . . ? C17 Zr1 C15 53.16(15) . . ? C16 Zr1 C15 31.79(13) . . ? C18 Zr1 C15 52.72(14) . . ? N2 Zr1 C14 109.33(13) . . ? N4 Zr1 C14 95.46(12) 3_665 . ? N1 Zr1 C14 148.42(11) . . ? N3 Zr1 C14 130.43(11) . . ? C2 Zr1 C14 68.48(11) . . ? C17 Zr1 C14 53.44(13) . . ? C16 Zr1 C14 53.05(12) . . ? C18 Zr1 C14 31.93(12) . . ? C15 Zr1 C14 31.99(12) . . ? N3 Si1 C24 111.97(17) . . ? N3 Si1 C25 107.62(18) . . ? C24 Si1 C25 108.1(2) . . ? N3 Si1 C23 107.35(17) . . ? C24 Si1 C23 110.3(2) . . ? C25 Si1 C23 111.6(2) . . ? C20 N1 C19 110.2(3) . . ? C20 N1 Zr1 107.2(2) . . ? C19 N1 Zr1 124.0(2) . . ? C21 N2 C22 105.9(4) . . ? C21 N2 Zr1 120.2(3) . . ? C22 N2 Zr1 133.3(3) . . ? N4 C26 N3 179.5(4) . . ? C11 C1 B3 117.3(3) . . ? C11 C1 B4 122.8(3) . . ? B3 C1 B4 62.7(3) . . ? C11 C1 C2 115.3(3) . . ? B3 C1 C2 61.0(2) . . ? B4 C1 C2 111.8(3) . . ? C11 C1 B6 117.3(3) . . ? B3 C1 B6 111.5(3) . . ? B4 C1 B6 113.3(3) . . ? C2 C1 B6 60.0(2) . . ? C11 C1 B5 123.2(3) . . ? B3 C1 B5 112.9(3) . . ? B4 C1 B5 62.0(3) . . ? C2 C1 B5 111.0(3) . . ? B6 C1 B5 62.7(3) . . ? C1 C2 B11 107.4(3) . . ? C1 C2 B6 60.2(2) . . ? B11 C2 B6 61.1(2) . . ? C1 C2 B7 106.7(3) . . ? B11 C2 B7 60.7(2) . . ? B6 C2 B7 110.3(3) . . ? C1 C2 B3 58.9(2) . . ? B11 C2 B3 109.7(3) . . ? B6 C2 B3 109.9(3) . . ? B7 C2 B3 60.8(2) . . ? C1 C2 Zr1 120.3(2) . . ? B11 C2 Zr1 123.0(2) . . ? B6 C2 Zr1 118.0(2) . . ? B7 C2 Zr1 124.2(2) . . ? B3 C2 Zr1 120.6(2) . . ? C14 C11 C12 108.6(3) . . ? C14 C11 C13 108.0(3) . . ? C12 C11 C13 107.4(4) . . ? C14 C11 C1 110.4(3) . . ? C12 C11 C1 111.7(4) . . ? C13 C11 C1 110.5(3) . . ? C18 C14 C15 106.7(4) . . ? C18 C14 C11 125.6(4) . . ? C15 C14 C11 127.2(4) . . ? C18 C14 Zr1 72.7(2) . . ? C15 C14 Zr1 73.4(2) . . ? C11 C14 Zr1 125.2(2) . . ? C16 C15 C14 108.5(4) . . ? C16 C15 Zr1 72.8(2) . . ? C14 C15 Zr1 74.7(2) . . ? C15 C16 C17 108.5(4) . . ? C15 C16 Zr1 75.4(2) . . ? C17 C16 Zr1 73.1(2) . . ? C16 C17 C18 107.5(4) . . ? C16 C17 Zr1 74.6(2) . . ? C18 C17 Zr1 75.2(2) . . ? C17 C18 C14 108.8(4) . . ? C17 C18 Zr1 72.5(2) . . ? C14 C18 Zr1 75.4(2) . . ? N1 C20 C21 108.9(3) . . ? N2 C21 C20 111.4(3) . . ? C26 N3 Si1 109.7(2) . . ? C26 N3 Zr1 116.3(2) . . ? Si1 N3 Zr1 133.84(15) . . ? C26 N4 Zr1 163.4(3) . 3_665 ? C1 B3 C2 60.1(2) . . ? C1 B3 B7 106.7(3) . . ? C2 B3 B7 59.6(2) . . ? C1 B3 B4 59.1(2) . . ? C2 B3 B4 108.2(3) . . ? B7 B3 B4 108.0(3) . . ? C1 B3 B8 106.2(3) . . ? C2 B3 B8 108.0(3) . . ? B7 B3 B8 60.3(3) . . ? B4 B3 B8 59.6(3) . . ? C1 B4 B8 106.1(3) . . ? C1 B4 B3 58.2(2) . . ? B8 B4 B3 60.5(3) . . ? C1 B4 B5 59.6(3) . . ? B8 B4 B5 108.2(4) . . ? B3 B4 B5 107.3(3) . . ? C1 B4 B9 106.0(3) . . ? B8 B4 B9 60.6(3) . . ? B3 B4 B9 108.2(3) . . ? B5 B4 B9 59.5(3) . . ? C1 B5 B10 105.6(3) . . ? C1 B5 B9 105.7(3) . . ? B10 B5 B9 60.7(3) . . ? C1 B5 B4 58.4(2) . . ? B10 B5 B4 108.4(4) . . ? B9 B5 B4 60.3(3) . . ? C1 B5 B6 58.4(2) . . ? B10 B5 B6 60.1(3) . . ? B9 B5 B6 108.4(4) . . ? B4 B5 B6 106.9(3) . . ? C2 B6 C1 59.7(2) . . ? C2 B6 B11 59.4(2) . . ? C1 B6 B11 105.6(3) . . ? C2 B6 B10 107.3(3) . . ? C1 B6 B10 104.8(3) . . ? B11 B6 B10 60.1(3) . . ? C2 B6 B5 107.7(3) . . ? C1 B6 B5 58.9(2) . . ? B11 B6 B5 106.9(3) . . ? B10 B6 B5 58.7(3) . . ? C2 B7 B11 59.2(2) . . ? C2 B7 B3 59.6(2) . . ? B11 B7 B3 107.5(3) . . ? C2 B7 B8 108.2(3) . . ? B11 B7 B8 108.6(3) . . ? B3 B7 B8 60.6(3) . . ? C2 B7 B12 108.0(3) . . ? B11 B7 B12 60.8(3) . . ? B3 B7 B12 108.5(3) . . ? B8 B7 B12 60.1(3) . . ? B4 B8 B12 107.7(4) . . ? B4 B8 B7 107.2(3) . . ? B12 B8 B7 60.0(3) . . ? B4 B8 B3 59.9(3) . . ? B12 B8 B3 107.1(3) . . ? B7 B8 B3 59.0(3) . . ? B4 B8 B9 60.0(3) . . ? B12 B8 B9 59.6(3) . . ? B7 B8 B9 107.2(4) . . ? B3 B8 B9 107.3(4) . . ? B5 B9 B12 108.1(4) . . ? B5 B9 B4 60.2(3) . . ? B12 B9 B4 107.5(3) . . ? B5 B9 B8 107.8(4) . . ? B12 B9 B8 60.0(3) . . ? B4 B9 B8 59.5(3) . . ? B5 B9 B10 59.3(3) . . ? B12 B9 B10 60.4(3) . . ? B4 B9 B10 107.2(4) . . ? B8 B9 B10 107.8(4) . . ? B5 B10 B11 108.1(3) . . ? B5 B10 B6 61.2(3) . . ? B11 B10 B6 59.1(2) . . ? B5 B10 B9 59.9(3) . . ? B11 B10 B9 107.7(4) . . ? B6 B10 B9 108.6(4) . . ? B5 B10 B12 108.0(4) . . ? B11 B10 B12 60.2(3) . . ? B6 B10 B12 107.8(3) . . ? B9 B10 B12 59.7(3) . . ? C2 B11 B6 59.5(2) . . ? C2 B11 B7 60.0(2) . . ? B6 B11 B7 108.5(3) . . ? C2 B11 B10 107.9(3) . . ? B6 B11 B10 60.8(3) . . ? B7 B11 B10 108.7(3) . . ? C2 B11 B12 108.4(3) . . ? B6 B11 B12 109.4(3) . . ? B7 B11 B12 60.5(3) . . ? B10 B11 B12 60.4(3) . . ? B8 B12 B9 60.4(3) . . ? B8 B12 B7 60.0(3) . . ? B9 B12 B7 107.8(4) . . ? B8 B12 B11 106.9(3) . . ? B9 B12 B11 107.3(4) . . ? B7 B12 B11 58.7(3) . . ? B8 B12 B10 107.7(4) . . ? B9 B12 B10 59.9(3) . . ? B7 B12 B10 106.5(3) . . ? B11 B12 B10 59.4(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.772 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.094 #===END data_6b _database_code_depnum_ccdc_archive 'CCDC 665272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 B20 N8 Zr2' _chemical_formula_weight 1015.66 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' B B 0.0013 0.0007 '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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9331(15) _cell_length_b 9.9265(10) _cell_length_c 17.1701(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.545(2) _cell_angle_gamma 90.00 _cell_volume 2540.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.8412 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13447 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4479 _reflns_number_gt 3108 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0798P)^2^+4.2278P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4479 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.70842(3) 0.61411(5) 0.09545(3) 0.03743(19) Uani 1 1 d . . . C1 C 0.8654(3) 0.3893(5) 0.1979(3) 0.0352(10) Uani 1 1 d . . . C2 C 0.7668(3) 0.4754(5) 0.2061(3) 0.0370(11) Uani 1 1 d . . . C11 C 0.9080(3) 0.3974(5) 0.1173(3) 0.0438(12) Uani 1 1 d . . . C12 C 0.9107(5) 0.2601(6) 0.0780(3) 0.0667(18) Uani 1 1 d . . . H12A H 0.9442 0.1983 0.1115 0.100 Uiso 1 1 calc R . . H12B H 0.9389 0.2683 0.0295 0.100 Uiso 1 1 calc R . . H12C H 0.8506 0.2270 0.0682 0.100 Uiso 1 1 calc R . . C13 C 1.0058(4) 0.4457(8) 0.1283(4) 0.0726(19) Uani 1 1 d . . . H13A H 1.0395 0.3840 0.1617 0.109 Uiso 1 1 calc R . . H13B H 1.0074 0.5337 0.1515 0.109 Uiso 1 1 calc R . . H13C H 1.0316 0.4495 0.0785 0.109 Uiso 1 1 calc R . . C14 C 0.8554(3) 0.4958(6) 0.0643(3) 0.0453(13) Uani 1 1 d . . . C15 C 0.7907(4) 0.4639(7) 0.0034(3) 0.0558(15) Uani 1 1 d . . . H15 H 0.7675 0.3787 -0.0079 0.067 Uiso 1 1 calc R . . C16 C 0.7674(5) 0.5831(8) -0.0371(4) 0.070(2) Uani 1 1 d . . . H16 H 0.7267 0.5901 -0.0801 0.084 Uiso 1 1 calc R . . C17 C 0.8153(4) 0.6881(8) -0.0020(4) 0.072(2) Uani 1 1 d . . . H17 H 0.8120 0.7780 -0.0171 0.086 Uiso 1 1 calc R . . C18 C 0.8699(4) 0.6357(6) 0.0602(4) 0.0585(16) Uani 1 1 d . . . H18 H 0.9091 0.6852 0.0933 0.070 Uiso 1 1 calc R . . C21 C 0.8055(5) 0.8983(6) 0.1417(6) 0.107(3) Uani 1 1 d . . . H21A H 0.8481 0.8661 0.1064 0.161 Uiso 1 1 calc R . . H21B H 0.8346 0.9091 0.1927 0.161 Uiso 1 1 calc R . . H21C H 0.7819 0.9834 0.1236 0.161 Uiso 1 1 calc R . . C22 C 0.6707(5) 0.8576(7) 0.2009(5) 0.081(2) Uani 1 1 d . . . H22A H 0.6659 0.9543 0.1937 0.098 Uiso 1 1 calc R . . H22B H 0.6949 0.8410 0.2538 0.098 Uiso 1 1 calc R . . C23 C 0.5797(5) 0.7962(7) 0.1902(5) 0.084(2) Uani 1 1 d . . . H23A H 0.5448 0.8186 0.2342 0.101 Uiso 1 1 calc R . . H23B H 0.5487 0.8315 0.1432 0.101 Uiso 1 1 calc R . . C24 C 0.4977(4) 0.5906(8) 0.1747(5) 0.094(3) Uani 1 1 d . . . H24A H 0.5023 0.4943 0.1717 0.140 Uiso 1 1 calc R . . H24B H 0.4674 0.6243 0.1278 0.140 Uiso 1 1 calc R . . H24C H 0.4644 0.6148 0.2187 0.140 Uiso 1 1 calc R . . C25 C 0.5601(3) 0.7817(5) -0.0280(3) 0.0458(13) Uani 1 1 d . . . C26 C 0.6160(4) 0.9057(5) -0.0263(4) 0.0616(16) Uani 1 1 d . . . H26A H 0.6690 0.8917 0.0073 0.092 Uiso 1 1 calc R . . H26B H 0.5823 0.9796 -0.0070 0.092 Uiso 1 1 calc R . . H26C H 0.6328 0.9258 -0.0781 0.092 Uiso 1 1 calc R . . C27 C 0.5202(4) 0.2161(5) 0.0741(4) 0.0582(16) Uani 1 1 d . . . H27 H 0.5363 0.1396 0.1030 0.070 Uiso 1 1 calc R . . C28 C 0.5758(4) 0.3282(6) 0.0770(3) 0.0541(15) Uani 1 1 d . . . B3 B 0.7678(4) 0.3013(6) 0.2011(4) 0.0444(14) Uani 1 1 d . . . H3 H 0.7366 0.2461 0.1509 0.053 Uiso 1 1 calc R . . B4 B 0.8686(4) 0.2450(6) 0.2518(3) 0.0445(14) Uani 1 1 d . . . H4 H 0.9029 0.1522 0.2352 0.053 Uiso 1 1 calc R . . B5 B 0.9289(4) 0.3882(7) 0.2849(4) 0.0504(16) Uani 1 1 d . . . H5 H 1.0027 0.3894 0.2901 0.060 Uiso 1 1 calc R . . B6 B 0.8654(4) 0.5332(7) 0.2530(4) 0.0488(15) Uani 1 1 d . . . H6 H 0.8973 0.6279 0.2364 0.059 Uiso 1 1 calc R . . B7 B 0.7043(5) 0.3867(7) 0.2692(4) 0.0546(17) Uani 1 1 d . . . H7 H 0.6305 0.3868 0.2645 0.066 Uiso 1 1 calc R . . B8 B 0.7661(5) 0.2414(7) 0.2978(4) 0.0552(17) Uani 1 1 d . . . H8 H 0.7327 0.1462 0.3112 0.066 Uiso 1 1 calc R . . B9 B 0.8666(5) 0.2964(7) 0.3495(4) 0.0587(18) Uani 1 1 d . . . H9 H 0.8994 0.2371 0.3972 0.070 Uiso 1 1 calc R . . B10 B 0.8647(5) 0.4750(8) 0.3512(4) 0.064(2) Uani 1 1 d . . . H10 H 0.8963 0.5338 0.3999 0.076 Uiso 1 1 calc R . . B11 B 0.7636(5) 0.5276(7) 0.3014(4) 0.0550(17) Uani 1 1 d . . . H11 H 0.7288 0.6200 0.3180 0.066 Uiso 1 1 calc R . . B12 B 0.7658(6) 0.3817(8) 0.3608(4) 0.069(2) Uani 1 1 d . . . H12 H 0.7330 0.3775 0.4164 0.082 Uiso 1 1 calc R . . N1 N 0.7330(3) 0.8020(4) 0.1452(3) 0.0596(13) Uani 1 1 d . . . N2 N 0.5888(4) 0.6499(5) 0.1840(4) 0.0622(14) Uani 1 1 d . . . N3 N 0.5898(3) 0.6781(5) 0.0139(3) 0.0527(13) Uani 1 1 d . . . N4 N 0.6205(3) 0.4225(5) 0.0780(3) 0.0580(13) Uani 1 1 d . . . H3A H 0.563(4) 0.619(6) 0.007(4) 0.06(2) Uiso 1 1 d . . . H2 H 0.612(4) 0.626(5) 0.228(3) 0.051(18) Uiso 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 Zr1 0.0291(3) 0.0361(3) 0.0467(3) 0.0029(2) -0.0004(2) -0.0020(2) C1 0.030(2) 0.041(3) 0.035(2) -0.004(2) -0.0027(19) 0.005(2) C2 0.027(2) 0.044(3) 0.039(3) -0.003(2) 0.000(2) 0.007(2) C11 0.035(3) 0.055(3) 0.041(3) 0.001(2) 0.004(2) 0.010(2) C12 0.088(5) 0.068(4) 0.044(3) -0.009(3) 0.012(3) 0.033(4) C13 0.037(3) 0.109(5) 0.074(4) 0.014(4) 0.015(3) 0.010(3) C14 0.038(3) 0.060(3) 0.039(3) 0.000(3) 0.013(2) 0.005(3) C15 0.058(4) 0.068(4) 0.041(3) -0.005(3) 0.006(3) 0.015(3) C16 0.065(4) 0.103(6) 0.044(3) 0.017(4) 0.009(3) 0.030(4) C17 0.056(4) 0.079(5) 0.084(5) 0.044(4) 0.033(4) 0.019(4) C18 0.034(3) 0.066(4) 0.077(4) 0.011(3) 0.017(3) -0.001(3) C21 0.062(5) 0.048(4) 0.207(10) -0.019(5) -0.022(6) -0.016(3) C22 0.093(6) 0.054(4) 0.098(5) -0.026(4) 0.006(4) 0.020(4) C23 0.088(5) 0.077(5) 0.091(5) -0.010(4) 0.028(4) 0.035(4) C24 0.046(4) 0.103(6) 0.134(7) 0.032(5) 0.033(4) 0.010(4) C25 0.042(3) 0.040(3) 0.055(3) 0.005(3) 0.001(2) -0.004(2) C26 0.055(4) 0.050(3) 0.080(4) 0.014(3) -0.001(3) -0.013(3) C27 0.051(3) 0.038(3) 0.082(4) 0.018(3) -0.020(3) -0.006(3) C28 0.044(3) 0.047(3) 0.068(4) 0.013(3) -0.018(3) 0.002(3) B3 0.032(3) 0.040(3) 0.061(4) 0.006(3) 0.005(3) 0.005(3) B4 0.041(3) 0.052(4) 0.040(3) 0.002(3) -0.003(3) 0.013(3) B5 0.044(3) 0.064(4) 0.042(3) -0.006(3) -0.015(3) 0.006(3) B6 0.046(4) 0.050(4) 0.048(4) -0.005(3) -0.007(3) 0.000(3) B7 0.048(4) 0.061(4) 0.058(4) 0.022(3) 0.024(3) 0.018(3) B8 0.051(4) 0.053(4) 0.063(4) 0.023(3) 0.011(3) 0.011(3) B9 0.068(5) 0.068(5) 0.040(4) 0.004(3) 0.001(3) 0.019(4) B10 0.086(5) 0.067(5) 0.036(4) -0.011(3) -0.009(3) 0.013(4) B11 0.067(4) 0.059(4) 0.041(3) 0.001(3) 0.017(3) 0.017(4) B12 0.087(6) 0.077(5) 0.045(4) 0.009(4) 0.025(4) 0.037(4) N1 0.057(3) 0.038(3) 0.081(3) -0.006(2) -0.015(3) -0.002(2) N2 0.050(3) 0.062(3) 0.077(4) 0.013(3) 0.016(3) 0.017(3) N3 0.040(3) 0.042(3) 0.074(3) 0.012(3) -0.017(2) -0.009(2) N4 0.043(3) 0.043(3) 0.085(4) 0.011(2) -0.022(3) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.075(4) . ? Zr1 N3 2.279(4) . ? Zr1 N4 2.320(5) . ? Zr1 N2 2.443(5) . ? Zr1 C2 2.461(5) . ? Zr1 C17 2.494(6) . ? Zr1 C16 2.509(6) . ? Zr1 C18 2.531(5) . ? Zr1 C15 2.543(6) . ? Zr1 C14 2.575(5) . ? C1 C11 1.561(7) . ? C1 B3 1.703(7) . ? C1 B4 1.705(8) . ? C1 B6 1.712(8) . ? C1 C2 1.716(6) . ? C1 B5 1.719(7) . ? C2 B7 1.716(8) . ? C2 B11 1.721(8) . ? C2 B3 1.731(7) . ? C2 B6 1.731(8) . ? C11 C14 1.520(7) . ? C11 C12 1.523(7) . ? C11 C13 1.538(8) . ? C14 C18 1.408(8) . ? C14 C15 1.416(8) . ? C15 C16 1.404(8) . ? C16 C17 1.381(10) . ? C17 C18 1.403(9) . ? C21 N1 1.448(8) . ? C22 N1 1.481(9) . ? C22 C23 1.490(10) . ? C23 N2 1.463(8) . ? C24 N2 1.482(9) . ? C25 N3 1.317(7) . ? C25 C27 1.395(7) 3_665 ? C25 C26 1.486(7) . ? C27 C28 1.387(8) . ? C27 C25 1.395(7) 3_665 ? C28 N4 1.150(7) . ? B3 B8 1.766(9) . ? B3 B7 1.767(9) . ? B3 B4 1.781(8) . ? B4 B9 1.755(9) . ? B4 B5 1.759(9) . ? B4 B8 1.764(9) . ? B5 B9 1.747(10) . ? B5 B10 1.759(10) . ? B5 B6 1.792(9) . ? B6 B11 1.778(9) . ? B6 B10 1.784(9) . ? B7 B11 1.728(10) . ? B7 B8 1.766(8) . ? B7 B12 1.772(11) . ? B8 B12 1.763(11) . ? B8 B9 1.781(10) . ? B9 B12 1.749(10) . ? B9 B10 1.773(10) . ? B10 B12 1.761(12) . ? B10 B11 1.769(10) . ? B11 B12 1.771(10) . ? 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 N1 Zr1 N3 96.48(19) . . ? N1 Zr1 N4 151.0(2) . . ? N3 Zr1 N4 74.76(17) . . ? N1 Zr1 N2 74.4(2) . . ? N3 Zr1 N2 76.8(2) . . ? N4 Zr1 N2 76.7(2) . . ? N1 Zr1 C2 98.08(17) . . ? N3 Zr1 C2 148.71(17) . . ? N4 Zr1 C2 79.13(16) . . ? N2 Zr1 C2 80.72(17) . . ? N1 Zr1 C17 84.7(3) . . ? N3 Zr1 C17 90.6(2) . . ? N4 Zr1 C17 122.4(2) . . ? N2 Zr1 C17 153.9(2) . . ? C2 Zr1 C17 118.15(18) . . ? N1 Zr1 C16 114.9(2) . . ? N3 Zr1 C16 77.3(2) . . ? N4 Zr1 C16 90.6(2) . . ? N2 Zr1 C16 153.3(2) . . ? C2 Zr1 C16 120.24(18) . . ? C17 Zr1 C16 32.0(2) . . ? N1 Zr1 C18 82.8(2) . . ? N3 Zr1 C18 123.1(2) . . ? N4 Zr1 C18 125.3(2) . . ? N2 Zr1 C18 151.7(2) . . ? C2 Zr1 C18 86.25(18) . . ? C17 Zr1 C18 32.4(2) . . ? C16 Zr1 C18 53.2(2) . . ? N1 Zr1 C15 134.7(2) . . ? N3 Zr1 C15 99.70(19) . . ? N4 Zr1 C15 74.4(2) . . ? N2 Zr1 C15 150.7(2) . . ? C2 Zr1 C15 89.43(17) . . ? C17 Zr1 C15 53.3(2) . . ? C16 Zr1 C15 32.27(19) . . ? C18 Zr1 C15 52.9(2) . . ? N1 Zr1 C14 111.37(19) . . ? N3 Zr1 C14 129.78(18) . . ? N4 Zr1 C14 94.72(17) . . ? N2 Zr1 C14 149.49(18) . . ? C2 Zr1 C14 68.86(16) . . ? C17 Zr1 C14 53.52(19) . . ? C16 Zr1 C14 53.42(18) . . ? C18 Zr1 C14 31.99(17) . . ? C15 Zr1 C14 32.11(17) . . ? C11 C1 B3 116.8(4) . . ? C11 C1 B4 121.7(4) . . ? B3 C1 B4 63.0(3) . . ? C11 C1 B6 117.4(4) . . ? B3 C1 B6 112.4(4) . . ? B4 C1 B6 113.7(4) . . ? C11 C1 C2 116.4(4) . . ? B3 C1 C2 60.8(3) . . ? B4 C1 C2 111.7(4) . . ? B6 C1 C2 60.7(3) . . ? C11 C1 B5 122.5(4) . . ? B3 C1 B5 113.4(4) . . ? B4 C1 B5 61.8(3) . . ? B6 C1 B5 62.9(3) . . ? C2 C1 B5 111.3(4) . . ? C1 C2 B7 107.4(4) . . ? C1 C2 B11 107.6(4) . . ? B7 C2 B11 60.4(4) . . ? C1 C2 B3 59.2(3) . . ? B7 C2 B3 61.7(3) . . ? B11 C2 B3 110.4(4) . . ? C1 C2 B6 59.6(3) . . ? B7 C2 B6 110.8(4) . . ? B11 C2 B6 62.0(4) . . ? B3 C2 B6 110.1(4) . . ? C1 C2 Zr1 118.7(3) . . ? B7 C2 Zr1 126.4(3) . . ? B11 C2 Zr1 122.4(3) . . ? B3 C2 Zr1 121.6(3) . . ? B6 C2 Zr1 115.1(3) . . ? C14 C11 C12 109.7(4) . . ? C14 C11 C13 108.9(5) . . ? C12 C11 C13 106.4(5) . . ? C14 C11 C1 109.9(4) . . ? C12 C11 C1 111.7(4) . . ? C13 C11 C1 110.1(4) . . ? C18 C14 C15 106.5(5) . . ? C18 C14 C11 126.0(5) . . ? C15 C14 C11 127.0(5) . . ? C18 C14 Zr1 72.3(3) . . ? C15 C14 Zr1 72.7(3) . . ? C11 C14 Zr1 125.7(3) . . ? C16 C15 C14 108.3(6) . . ? C16 C15 Zr1 72.5(3) . . ? C14 C15 Zr1 75.2(3) . . ? C17 C16 C15 108.3(6) . . ? C17 C16 Zr1 73.4(4) . . ? C15 C16 Zr1 75.2(3) . . ? C16 C17 C18 108.3(6) . . ? C16 C17 Zr1 74.6(4) . . ? C18 C17 Zr1 75.2(3) . . ? C17 C18 C14 108.6(6) . . ? C17 C18 Zr1 72.3(3) . . ? C14 C18 Zr1 75.7(3) . . ? N1 C22 C23 111.8(5) . . ? N2 C23 C22 109.1(6) . . ? N3 C25 C27 124.8(5) . 3_665 ? N3 C25 C26 117.8(5) . . ? C27 C25 C26 117.4(5) 3_665 . ? C28 C27 C25 119.9(5) . 3_665 ? N4 C28 C27 178.3(6) . . ? C1 B3 C2 59.9(3) . . ? C1 B3 B8 105.3(4) . . ? C2 B3 B8 106.8(5) . . ? C1 B3 B7 105.6(4) . . ? C2 B3 B7 58.7(3) . . ? B8 B3 B7 60.0(4) . . ? C1 B3 B4 58.5(3) . . ? C2 B3 B4 107.4(4) . . ? B8 B3 B4 59.7(4) . . ? B7 B3 B4 107.3(5) . . ? C1 B4 B9 105.8(4) . . ? C1 B4 B5 59.5(3) . . ? B9 B4 B5 59.6(4) . . ? C1 B4 B8 105.3(4) . . ? B9 B4 B8 60.8(4) . . ? B5 B4 B8 108.2(5) . . ? C1 B4 B3 58.4(3) . . ? B9 B4 B3 108.2(4) . . ? B5 B4 B3 107.8(4) . . ? B8 B4 B3 59.7(3) . . ? C1 B5 B9 105.5(4) . . ? C1 B5 B10 105.4(4) . . ? B9 B5 B10 60.8(4) . . ? C1 B5 B4 58.7(3) . . ? B9 B5 B4 60.1(4) . . ? B10 B5 B4 108.4(5) . . ? C1 B5 B6 58.3(3) . . ? B9 B5 B6 108.7(5) . . ? B10 B5 B6 60.3(4) . . ? B4 B5 B6 107.4(4) . . ? C1 B6 C2 59.8(3) . . ? C1 B6 B11 105.2(5) . . ? C2 B6 B11 58.7(3) . . ? C1 B6 B10 104.6(4) . . ? C2 B6 B10 106.2(5) . . ? B11 B6 B10 59.5(4) . . ? C1 B6 B5 58.7(3) . . ? C2 B6 B5 107.2(4) . . ? B11 B6 B5 106.5(5) . . ? B10 B6 B5 58.9(4) . . ? C2 B7 B11 60.0(3) . . ? C2 B7 B8 107.5(4) . . ? B11 B7 B8 108.9(5) . . ? C2 B7 B3 59.6(3) . . ? B11 B7 B3 108.4(5) . . ? B8 B7 B3 60.0(4) . . ? C2 B7 B12 107.7(5) . . ? B11 B7 B12 60.8(4) . . ? B8 B7 B12 59.8(4) . . ? B3 B7 B12 107.7(4) . . ? B12 B8 B4 107.1(5) . . ? B12 B8 B3 108.2(5) . . ? B4 B8 B3 60.6(3) . . ? B12 B8 B7 60.3(4) . . ? B4 B8 B7 108.2(4) . . ? B3 B8 B7 60.1(3) . . ? B12 B8 B9 59.1(4) . . ? B4 B8 B9 59.3(4) . . ? B3 B8 B9 107.7(5) . . ? B7 B8 B9 107.3(5) . . ? B5 B9 B12 108.3(5) . . ? B5 B9 B4 60.3(4) . . ? B12 B9 B4 108.2(5) . . ? B5 B9 B10 59.9(4) . . ? B12 B9 B10 60.0(4) . . ? B4 B9 B10 108.0(5) . . ? B5 B9 B8 108.0(4) . . ? B12 B9 B8 59.9(4) . . ? B4 B9 B8 59.9(4) . . ? B10 B9 B8 107.5(5) . . ? B5 B10 B12 107.2(5) . . ? B5 B10 B11 108.4(4) . . ? B12 B10 B11 60.2(4) . . ? B5 B10 B9 59.3(4) . . ? B12 B10 B9 59.3(4) . . ? B11 B10 B9 107.5(5) . . ? B5 B10 B6 60.8(4) . . ? B12 B10 B6 108.2(5) . . ? B11 B10 B6 60.1(4) . . ? B9 B10 B6 107.8(5) . . ? C2 B11 B7 59.7(4) . . ? C2 B11 B10 107.3(4) . . ? B7 B11 B10 108.7(5) . . ? C2 B11 B12 107.5(5) . . ? B7 B11 B12 60.8(4) . . ? B10 B11 B12 59.7(4) . . ? C2 B11 B6 59.3(3) . . ? B7 B11 B6 108.1(5) . . ? B10 B11 B6 60.4(4) . . ? B12 B11 B6 108.0(5) . . ? B9 B12 B10 60.7(5) . . ? B9 B12 B8 61.0(4) . . ? B10 B12 B8 108.9(5) . . ? B9 B12 B11 108.5(5) . . ? B10 B12 B11 60.1(4) . . ? B8 B12 B11 107.1(5) . . ? B9 B12 B7 108.5(5) . . ? B10 B12 B7 107.1(5) . . ? B8 B12 B7 59.9(4) . . ? B11 B12 B7 58.4(4) . . ? C21 N1 C22 106.4(5) . . ? C21 N1 Zr1 133.6(5) . . ? C22 N1 Zr1 119.9(4) . . ? C23 N2 C24 108.3(6) . . ? C23 N2 Zr1 105.3(4) . . ? C24 N2 Zr1 125.3(5) . . ? C25 N3 Zr1 140.9(4) . . ? C28 N4 Zr1 173.3(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.154 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.096 #===END data_7b _database_code_depnum_ccdc_archive 'CCDC 665273' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H50 B10 N4 Zr' _chemical_formula_weight 702.09 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' B B 0.0013 0.0007 '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' 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 10.6958(16) _cell_length_b 17.369(3) _cell_length_c 21.358(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.446(3) _cell_angle_gamma 90.00 _cell_volume 3942.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 910 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.55 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.804850 _exptl_absorpt_correction_T_max 1.0000 _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 SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20935 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6939 _reflns_number_gt 5373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0536P)^2^+0.6523P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6939 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.97138(2) 0.836268(13) 0.768734(10) 0.02858(9) Uani 1 1 d . . . N1 N 0.89340(18) 0.72185(12) 0.74387(9) 0.0351(5) Uani 1 1 d . . . N2 N 0.7249(2) 0.72454(14) 0.80911(11) 0.0529(6) Uani 1 1 d . . . N3 N 0.9465(2) 0.85886(15) 0.92614(10) 0.0501(6) Uani 1 1 d . . . N4 N 1.10585(19) 0.84455(12) 0.85593(9) 0.0349(5) Uani 1 1 d . . . B3 B 1.1059(3) 0.77957(18) 0.63095(14) 0.0401(7) Uani 1 1 d . . . H3 H 1.0087 0.7646 0.6127 0.048 Uiso 1 1 calc R . . B4 B 1.2120(3) 0.8235(2) 0.58252(17) 0.0513(9) Uani 1 1 d . . . H4 H 1.1848 0.8364 0.5324 0.062 Uiso 1 1 calc R . . B5 B 1.3102(3) 0.8854(2) 0.63227(19) 0.0626(11) Uani 1 1 d . . . H5 H 1.3474 0.9393 0.6146 0.075 Uiso 1 1 calc R . . B6 B 1.2628(3) 0.8784(2) 0.70890(17) 0.0524(9) Uani 1 1 d . . . H6 H 1.2676 0.9278 0.7413 0.063 Uiso 1 1 calc R . . B7 B 1.1958(3) 0.7224(2) 0.68705(15) 0.0461(8) Uani 1 1 d . . . H7 H 1.1586 0.6688 0.7051 0.055 Uiso 1 1 calc R . . B8 B 1.2393(3) 0.7283(2) 0.60960(16) 0.0494(8) Uani 1 1 d . . . H8 H 1.2297 0.6792 0.5769 0.059 Uiso 1 1 calc R . . B9 B 1.3675(3) 0.7944(2) 0.61156(19) 0.0586(10) Uani 1 1 d . . . H9 H 1.4425 0.7884 0.5806 0.070 Uiso 1 1 calc R . . B10 B 1.3980(3) 0.8293(3) 0.6896(2) 0.0673(11) Uani 1 1 d . . . H10 H 1.4933 0.8463 0.7095 0.081 Uiso 1 1 calc R . . B11 B 1.2932(3) 0.7842(2) 0.73603(17) 0.0547(9) Uani 1 1 d . . . H11 H 1.3202 0.7715 0.7862 0.066 Uiso 1 1 calc R . . B12 B 1.3561(3) 0.7312(2) 0.67541(18) 0.0570(9) Uani 1 1 d . . . H12 H 1.4235 0.6838 0.6857 0.068 Uiso 1 1 calc R . . C1 C 1.1560(3) 0.87230(16) 0.64364(12) 0.0422(6) Uani 1 1 d . . . C2 C 1.1432(2) 0.81183(15) 0.70634(12) 0.0363(6) Uani 1 1 d . . . C11 C 1.0546(3) 0.93699(17) 0.63122(14) 0.0542(8) Uani 1 1 d . . . C12 C 1.1163(4) 1.0164(2) 0.6306(2) 0.1041(16) Uani 1 1 d . . . H12A H 1.1661 1.0251 0.6702 0.156 Uiso 1 1 calc R . . H12B H 1.0522 1.0552 0.6241 0.156 Uiso 1 1 calc R . . H12C H 1.1691 1.0186 0.5972 0.156 Uiso 1 1 calc R . . C13 C 0.9742(4) 0.9256(2) 0.56692(15) 0.0874(13) Uani 1 1 d . . . H13A H 0.9128 0.9660 0.5607 0.131 Uiso 1 1 calc R . . H13B H 0.9324 0.8767 0.5665 0.131 Uiso 1 1 calc R . . H13C H 1.0278 0.9272 0.5337 0.131 Uiso 1 1 calc R . . C14 C 0.9661(2) 0.93764(15) 0.68276(12) 0.0396(6) Uani 1 1 d . . . C15 C 0.8450(3) 0.90468(17) 0.67873(13) 0.0510(7) Uani 1 1 d . . . H15A H 0.8017 0.8796 0.6413 0.061 Uiso 1 1 calc R . . C16 C 0.7904(3) 0.92257(19) 0.73336(16) 0.0587(9) Uani 1 1 d . . . H16A H 0.7025 0.9132 0.7400 0.070 Uiso 1 1 calc R . . C17 C 0.8756(3) 0.96732(17) 0.77195(14) 0.0529(8) Uani 1 1 d . . . H17A H 0.8576 0.9947 0.8100 0.064 Uiso 1 1 calc R . . C18 C 0.9838(3) 0.97676(15) 0.74079(13) 0.0436(6) Uani 1 1 d . . . H18A H 1.0545 1.0110 0.7544 0.052 Uiso 1 1 calc R . . C19 C 0.8867(2) 0.64985(15) 0.71057(12) 0.0391(6) Uani 1 1 d . . . C20 C 0.8154(3) 0.64537(18) 0.65209(14) 0.0500(7) Uani 1 1 d . . . C21 C 0.8234(3) 0.5777(2) 0.61731(16) 0.0681(10) Uani 1 1 d . . . H21A H 0.7765 0.5734 0.5781 0.082 Uiso 1 1 calc R . . C22 C 0.8978(4) 0.5181(2) 0.6393(2) 0.0761(12) Uani 1 1 d . . . H22A H 0.9045 0.4747 0.6144 0.091 Uiso 1 1 calc R . . C23 C 0.9626(3) 0.52181(19) 0.6978(2) 0.0717(10) Uani 1 1 d . . . H23A H 1.0110 0.4800 0.7131 0.086 Uiso 1 1 calc R . . C24 C 0.9576(3) 0.58763(17) 0.73542(15) 0.0519(7) Uani 1 1 d . . . C25 C 0.7315(3) 0.7099(2) 0.62686(16) 0.0726(10) Uani 1 1 d . . . H25A H 0.7376 0.7516 0.6565 0.109 Uiso 1 1 calc R . . H25B H 0.6460 0.6921 0.6203 0.109 Uiso 1 1 calc R . . H25C H 0.7569 0.7274 0.5876 0.109 Uiso 1 1 calc R . . C26 C 1.0246(4) 0.5907(2) 0.80101(18) 0.0828(12) Uani 1 1 d . . . H26A H 1.0110 0.6400 0.8193 0.124 Uiso 1 1 calc R . . H26B H 1.1131 0.5830 0.7995 0.124 Uiso 1 1 calc R . . H26C H 0.9926 0.5510 0.8261 0.124 Uiso 1 1 calc R . . C27 C 0.8234(2) 0.75289(16) 0.78335(12) 0.0389(6) Uani 1 1 d . . . C28 C 0.6738(3) 0.6475(2) 0.79865(18) 0.0744(11) Uani 1 1 d . . . H28A H 0.7213 0.6203 0.7701 0.112 Uiso 1 1 calc R . . H28B H 0.5874 0.6508 0.7809 0.112 Uiso 1 1 calc R . . H28C H 0.6789 0.6204 0.8380 0.112 Uiso 1 1 calc R . . C29 C 0.6637(3) 0.7737(2) 0.85291(15) 0.0627(9) Uani 1 1 d . . . H29A H 0.5840 0.7505 0.8600 0.075 Uiso 1 1 calc R . . H29B H 0.6458 0.8233 0.8331 0.075 Uiso 1 1 calc R . . C30 C 0.7415(3) 0.7866(2) 0.91705(15) 0.0659(9) Uani 1 1 d . . . H30A H 0.6857 0.7819 0.9497 0.079 Uiso 1 1 calc R . . H30B H 0.8033 0.7457 0.9236 0.079 Uiso 1 1 calc R . . C31 C 0.8094(3) 0.8630(2) 0.92551(15) 0.0572(8) Uani 1 1 d . . . H31A H 0.7764 0.8972 0.8917 0.069 Uiso 1 1 calc R . . H31B H 0.7906 0.8858 0.9648 0.069 Uiso 1 1 calc R . . C32 C 1.0205(3) 0.8566(3) 0.98812(14) 0.0778(12) Uani 1 1 d . . . H32A H 1.1082 0.8526 0.9829 0.117 Uiso 1 1 calc R . . H32B H 0.9956 0.8129 1.0113 0.117 Uiso 1 1 calc R . . H32C H 1.0061 0.9029 1.0108 0.117 Uiso 1 1 calc R . . C33 C 0.9915(2) 0.85082(15) 0.87101(11) 0.0372(6) Uani 1 1 d . . . C34 C 1.2224(2) 0.85124(16) 0.89641(11) 0.0384(6) Uani 1 1 d . . . C35 C 1.2726(3) 0.92443(18) 0.91038(13) 0.0491(7) Uani 1 1 d . . . C36 C 1.3836(3) 0.9295(2) 0.95028(15) 0.0644(9) Uani 1 1 d . . . H36A H 1.4180 0.9778 0.9600 0.077 Uiso 1 1 calc R . . C37 C 1.4440(3) 0.8661(3) 0.97563(15) 0.0703(10) Uani 1 1 d . . . H37A H 1.5181 0.8712 1.0026 0.084 Uiso 1 1 calc R . . C38 C 1.3952(3) 0.7949(2) 0.96133(14) 0.0631(9) Uani 1 1 d . . . H38A H 1.4374 0.7516 0.9785 0.076 Uiso 1 1 calc R . . C39 C 1.2831(3) 0.78546(18) 0.92142(13) 0.0494(7) Uani 1 1 d . . . C40 C 1.2076(3) 0.9967(2) 0.88419(17) 0.0756(10) Uani 1 1 d . . . H40A H 1.2556 1.0409 0.8993 0.113 Uiso 1 1 calc R . . H40B H 1.1250 0.9996 0.8976 0.113 Uiso 1 1 calc R . . H40C H 1.2008 0.9955 0.8390 0.113 Uiso 1 1 calc R . . C41 C 1.2276(4) 0.7074(2) 0.90781(18) 0.0819(12) Uani 1 1 d . . . H41A H 1.1512 0.7122 0.8799 0.123 Uiso 1 1 calc R . . H41B H 1.2096 0.6838 0.9465 0.123 Uiso 1 1 calc R . . H41C H 1.2863 0.6760 0.8884 0.123 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02897(14) 0.03010(15) 0.02655(14) 0.00158(9) 0.00254(9) 0.00069(10) N1 0.0350(11) 0.0369(12) 0.0332(11) -0.0019(9) 0.0027(9) -0.0055(9) N2 0.0476(14) 0.0567(16) 0.0574(15) -0.0116(12) 0.0196(11) -0.0166(12) N3 0.0451(14) 0.0762(18) 0.0288(12) -0.0034(11) 0.0032(10) 0.0015(12) N4 0.0352(12) 0.0379(12) 0.0305(11) 0.0007(9) -0.0010(8) -0.0046(9) B3 0.0431(17) 0.0407(18) 0.0367(16) -0.0021(13) 0.0060(13) -0.0015(14) B4 0.064(2) 0.050(2) 0.0439(19) -0.0053(15) 0.0233(16) 0.0012(17) B5 0.063(2) 0.051(2) 0.082(3) -0.0174(19) 0.042(2) -0.0172(18) B6 0.0397(18) 0.058(2) 0.062(2) -0.0230(18) 0.0156(15) -0.0150(16) B7 0.0475(19) 0.0410(18) 0.0508(19) 0.0032(15) 0.0101(14) 0.0063(15) B8 0.051(2) 0.048(2) 0.051(2) -0.0110(16) 0.0139(15) 0.0016(16) B9 0.053(2) 0.056(2) 0.073(3) -0.0119(19) 0.0328(18) -0.0022(18) B10 0.0359(19) 0.086(3) 0.082(3) -0.027(2) 0.0160(17) -0.0083(19) B11 0.0343(18) 0.078(3) 0.051(2) -0.0096(18) 0.0005(14) 0.0075(17) B12 0.0422(19) 0.066(2) 0.064(2) -0.0079(19) 0.0114(16) 0.0095(17) C1 0.0485(16) 0.0391(15) 0.0421(15) 0.0003(12) 0.0187(12) -0.0003(13) C2 0.0333(13) 0.0399(14) 0.0361(14) 0.0005(11) 0.0051(10) -0.0026(11) C11 0.075(2) 0.0410(17) 0.0521(18) 0.0130(13) 0.0293(15) 0.0098(15) C12 0.125(3) 0.042(2) 0.164(4) 0.028(2) 0.102(3) 0.010(2) C13 0.115(3) 0.109(3) 0.0395(19) 0.0250(19) 0.0180(19) 0.052(3) C14 0.0457(15) 0.0345(15) 0.0400(15) 0.0108(11) 0.0113(11) 0.0085(12) C15 0.0522(17) 0.0537(18) 0.0437(17) 0.0161(14) -0.0087(13) 0.0039(14) C16 0.0440(17) 0.067(2) 0.067(2) 0.0314(17) 0.0143(15) 0.0202(16) C17 0.069(2) 0.0427(17) 0.0511(18) 0.0101(14) 0.0247(15) 0.0259(15) C18 0.0546(16) 0.0281(14) 0.0482(16) 0.0046(12) 0.0069(12) 0.0054(12) C19 0.0368(14) 0.0397(16) 0.0426(15) -0.0061(12) 0.0123(11) -0.0106(12) C20 0.0493(17) 0.0569(19) 0.0452(16) -0.0124(14) 0.0113(13) -0.0185(14) C21 0.068(2) 0.085(3) 0.055(2) -0.0300(19) 0.0221(16) -0.035(2) C22 0.069(2) 0.068(3) 0.100(3) -0.043(2) 0.043(2) -0.030(2) C23 0.058(2) 0.0411(19) 0.122(3) -0.010(2) 0.036(2) -0.0094(16) C24 0.0493(17) 0.0402(17) 0.068(2) 0.0023(14) 0.0126(14) -0.0103(14) C25 0.063(2) 0.095(3) 0.054(2) -0.0013(19) -0.0181(16) -0.010(2) C26 0.093(3) 0.062(2) 0.086(3) 0.027(2) -0.019(2) 0.002(2) C27 0.0343(14) 0.0447(16) 0.0368(14) -0.0019(12) -0.0003(11) -0.0026(12) C28 0.072(2) 0.068(2) 0.088(3) -0.0123(19) 0.0311(19) -0.0354(19) C29 0.0418(17) 0.082(2) 0.067(2) -0.0147(18) 0.0189(15) -0.0040(16) C30 0.063(2) 0.080(3) 0.059(2) 0.0015(17) 0.0293(16) -0.0050(18) C31 0.0488(18) 0.075(2) 0.0495(18) -0.0089(16) 0.0125(14) 0.0058(16) C32 0.060(2) 0.143(4) 0.0301(17) 0.0028(19) 0.0030(14) -0.007(2) C33 0.0378(14) 0.0422(16) 0.0309(14) 0.0004(11) 0.0010(11) -0.0008(11) C34 0.0328(13) 0.0523(17) 0.0299(13) -0.0038(11) 0.0019(10) -0.0056(12) C35 0.0493(17) 0.0584(19) 0.0396(16) -0.0097(13) 0.0049(12) -0.0131(14) C36 0.0558(19) 0.086(3) 0.0511(19) -0.0203(18) 0.0034(15) -0.0257(19) C37 0.0423(18) 0.114(3) 0.052(2) -0.017(2) -0.0055(14) -0.007(2) C38 0.0468(18) 0.091(3) 0.0491(19) 0.0038(18) -0.0030(14) 0.0144(18) C39 0.0454(16) 0.058(2) 0.0432(16) 0.0008(14) -0.0003(12) 0.0018(14) C40 0.093(3) 0.051(2) 0.079(2) -0.0130(18) -0.0066(19) -0.012(2) C41 0.096(3) 0.053(2) 0.089(3) 0.0159(19) -0.023(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C33 2.186(2) . ? Zr1 C27 2.194(3) . ? Zr1 N1 2.197(2) . ? Zr1 N4 2.226(2) . ? Zr1 C2 2.425(3) . ? Zr1 C16 2.497(3) . ? Zr1 C17 2.500(3) . ? Zr1 C18 2.519(3) . ? Zr1 C15 2.520(3) . ? Zr1 C14 2.540(2) . ? N1 C27 1.306(3) . ? N1 C19 1.436(3) . ? N2 C27 1.336(3) . ? N2 C28 1.454(4) . ? N2 C29 1.472(4) . ? N3 C33 1.329(3) . ? N3 C32 1.464(4) . ? N3 C31 1.466(4) . ? N4 C33 1.304(3) . ? N4 C34 1.439(3) . ? B3 C2 1.709(4) . ? B3 C1 1.710(4) . ? B3 B7 1.757(4) . ? B3 B8 1.784(4) . ? B3 B4 1.790(4) . ? B4 C1 1.719(4) . ? B4 B8 1.764(5) . ? B4 B5 1.772(5) . ? B4 B9 1.782(5) . ? B5 C1 1.709(4) . ? B5 B10 1.753(6) . ? B5 B9 1.769(5) . ? B5 B6 1.771(5) . ? B6 C1 1.703(4) . ? B6 C2 1.720(4) . ? B6 B11 1.754(6) . ? B6 B10 1.767(5) . ? B7 C2 1.718(4) . ? B7 B11 1.756(5) . ? B7 B12 1.766(5) . ? B7 B8 1.771(5) . ? B8 B12 1.774(5) . ? B8 B9 1.785(5) . ? B9 B12 1.765(6) . ? B9 B10 1.768(6) . ? B10 B11 1.762(6) . ? B10 B12 1.778(6) . ? B11 C2 1.726(4) . ? B11 B12 1.780(5) . ? C1 C11 1.564(4) . ? C1 C2 1.720(4) . ? C11 C12 1.529(5) . ? C11 C14 1.531(4) . ? C11 C13 1.549(5) . ? C14 C18 1.407(4) . ? C14 C15 1.410(4) . ? C15 C16 1.397(4) . ? C16 C17 1.395(5) . ? C17 C18 1.408(4) . ? C19 C24 1.390(4) . ? C19 C20 1.391(4) . ? C20 C21 1.399(4) . ? C20 C25 1.499(5) . ? C21 C22 1.357(5) . ? C22 C23 1.360(5) . ? C23 C24 1.402(4) . ? C24 C26 1.501(5) . ? C29 C30 1.537(4) . ? C30 C31 1.515(5) . ? C34 C39 1.391(4) . ? C34 C35 1.399(4) . ? C35 C36 1.385(4) . ? C35 C40 1.511(4) . ? C36 C37 1.359(5) . ? C37 C38 1.363(5) . ? C38 C39 1.401(4) . ? C39 C41 1.496(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 C33 Zr1 C27 85.74(9) . . ? C33 Zr1 N1 109.77(9) . . ? C27 Zr1 N1 34.60(8) . . ? C33 Zr1 N4 34.36(8) . . ? C27 Zr1 N4 109.42(8) . . ? N1 Zr1 N4 116.92(7) . . ? C33 Zr1 C2 125.01(9) . . ? C27 Zr1 C2 124.48(9) . . ? N1 Zr1 C2 89.96(8) . . ? N4 Zr1 C2 90.73(8) . . ? C33 Zr1 C16 102.65(11) . . ? C27 Zr1 C16 83.80(11) . . ? N1 Zr1 C16 102.09(10) . . ? N4 Zr1 C16 128.34(10) . . ? C2 Zr1 C16 123.24(9) . . ? C33 Zr1 C17 82.07(10) . . ? C27 Zr1 C17 107.02(10) . . ? N1 Zr1 C17 133.20(10) . . ? N4 Zr1 C17 98.42(9) . . ? C2 Zr1 C17 120.82(9) . . ? C16 Zr1 C17 32.42(10) . . ? C33 Zr1 C18 97.06(9) . . ? C27 Zr1 C18 137.01(9) . . ? N1 Zr1 C18 147.95(8) . . ? N4 Zr1 C18 95.12(8) . . ? C2 Zr1 C18 88.61(9) . . ? C16 Zr1 C18 53.61(10) . . ? C17 Zr1 C18 32.58(9) . . ? C33 Zr1 C15 133.79(10) . . ? C27 Zr1 C15 94.92(10) . . ? N1 Zr1 C15 94.91(9) . . ? N4 Zr1 C15 148.04(9) . . ? C2 Zr1 C15 92.18(9) . . ? C16 Zr1 C15 32.32(10) . . ? C17 Zr1 C15 53.51(10) . . ? C18 Zr1 C15 53.18(9) . . ? C33 Zr1 C14 129.35(9) . . ? C27 Zr1 C14 127.06(9) . . ? N1 Zr1 C14 118.37(8) . . ? N4 Zr1 C14 121.32(8) . . ? C2 Zr1 C14 71.39(8) . . ? C16 Zr1 C14 53.95(9) . . ? C17 Zr1 C14 54.04(9) . . ? C18 Zr1 C14 32.30(8) . . ? C15 Zr1 C14 32.36(9) . . ? C27 N1 C19 132.8(2) . . ? C27 N1 Zr1 72.55(15) . . ? C19 N1 Zr1 154.62(16) . . ? C27 N2 C28 125.2(2) . . ? C27 N2 C29 118.4(2) . . ? C28 N2 C29 116.4(2) . . ? C33 N3 C32 125.8(2) . . ? C33 N3 C31 117.3(2) . . ? C32 N3 C31 116.6(2) . . ? C33 N4 C34 128.1(2) . . ? C33 N4 Zr1 71.11(13) . . ? C34 N4 Zr1 160.41(17) . . ? C2 B3 C1 60.39(16) . . ? C2 B3 B7 59.40(17) . . ? C1 B3 B7 106.6(2) . . ? C2 B3 B8 107.2(2) . . ? C1 B3 B8 105.4(2) . . ? B7 B3 B8 60.00(18) . . ? C2 B3 B4 108.0(2) . . ? C1 B3 B4 58.80(17) . . ? B7 B3 B4 107.5(2) . . ? B8 B3 B4 59.17(19) . . ? C1 B4 B8 105.8(2) . . ? C1 B4 B5 58.58(18) . . ? B8 B4 B5 107.9(3) . . ? C1 B4 B9 105.5(2) . . ? B8 B4 B9 60.5(2) . . ? B5 B4 B9 59.7(2) . . ? C1 B4 B3 58.27(17) . . ? B8 B4 B3 60.24(19) . . ? B5 B4 B3 106.5(2) . . ? B9 B4 B3 107.8(3) . . ? C1 B5 B10 106.1(3) . . ? C1 B5 B9 106.4(2) . . ? B10 B5 B9 60.3(2) . . ? C1 B5 B6 58.57(17) . . ? B10 B5 B6 60.2(2) . . ? B9 B5 B6 108.2(3) . . ? C1 B5 B4 59.18(18) . . ? B10 B5 B4 108.4(3) . . ? B9 B5 B4 60.4(2) . . ? B6 B5 B4 107.5(2) . . ? C1 B6 C2 60.30(16) . . ? C1 B6 B11 107.2(2) . . ? C2 B6 B11 59.59(18) . . ? C1 B6 B10 105.7(2) . . ? C2 B6 B10 107.1(3) . . ? B11 B6 B10 60.0(2) . . ? C1 B6 B5 58.88(19) . . ? C2 B6 B5 107.8(2) . . ? B11 B6 B5 108.0(2) . . ? B10 B6 B5 59.4(2) . . ? C2 B7 B11 59.58(18) . . ? C2 B7 B3 58.91(17) . . ? B11 B7 B3 107.7(2) . . ? C2 B7 B12 107.8(2) . . ? B11 B7 B12 60.72(19) . . ? B3 B7 B12 108.7(2) . . ? C2 B7 B8 107.4(2) . . ? B11 B7 B8 108.7(2) . . ? B3 B7 B8 60.73(18) . . ? B12 B7 B8 60.19(19) . . ? B4 B8 B7 108.0(2) . . ? B4 B8 B12 108.0(3) . . ? B7 B8 B12 59.79(19) . . ? B4 B8 B3 60.59(18) . . ? B7 B8 B3 59.26(17) . . ? B12 B8 B3 107.2(2) . . ? B4 B8 B9 60.2(2) . . ? B7 B8 B9 107.3(2) . . ? B12 B8 B9 59.5(2) . . ? B3 B8 B9 107.9(2) . . ? B12 B9 B10 60.4(2) . . ? B12 B9 B5 107.9(3) . . ? B10 B9 B5 59.4(2) . . ? B12 B9 B4 107.6(2) . . ? B10 B9 B4 107.3(2) . . ? B5 B9 B4 59.9(2) . . ? B12 B9 B8 59.9(2) . . ? B10 B9 B8 107.6(3) . . ? B5 B9 B8 107.1(2) . . ? B4 B9 B8 59.3(2) . . ? B5 B10 B11 108.4(2) . . ? B5 B10 B6 60.4(2) . . ? B11 B10 B6 59.6(2) . . ? B5 B10 B9 60.3(2) . . ? B11 B10 B9 108.5(3) . . ? B6 B10 B9 108.4(3) . . ? B5 B10 B12 108.0(3) . . ? B11 B10 B12 60.4(2) . . ? B6 B10 B12 107.7(2) . . ? B9 B10 B12 59.7(2) . . ? C2 B11 B6 59.23(18) . . ? C2 B11 B7 59.10(17) . . ? B6 B11 B7 107.3(2) . . ? C2 B11 B10 107.0(3) . . ? B6 B11 B10 60.4(2) . . ? B7 B11 B10 108.0(3) . . ? C2 B11 B12 106.8(2) . . ? B6 B11 B12 108.2(3) . . ? B7 B11 B12 59.92(19) . . ? B10 B11 B12 60.3(2) . . ? B9 B12 B7 108.3(2) . . ? B9 B12 B8 60.6(2) . . ? B7 B12 B8 60.02(18) . . ? B9 B12 B10 59.9(2) . . ? B7 B12 B10 106.8(2) . . ? B8 B12 B10 107.7(3) . . ? B9 B12 B11 107.8(3) . . ? B7 B12 B11 59.36(19) . . ? B8 B12 B11 107.5(2) . . ? B10 B12 B11 59.4(2) . . ? C11 C1 B6 118.9(2) . . ? C11 C1 B5 122.8(2) . . ? B6 C1 B5 62.6(2) . . ? C11 C1 B3 116.8(2) . . ? B6 C1 B3 110.9(2) . . ? B5 C1 B3 113.2(2) . . ? C11 C1 B4 121.3(2) . . ? B6 C1 B4 113.2(2) . . ? B5 C1 B4 62.2(2) . . ? B3 C1 B4 62.93(18) . . ? C11 C1 C2 117.2(2) . . ? B6 C1 C2 60.34(17) . . ? B5 C1 C2 110.8(2) . . ? B3 C1 C2 59.79(16) . . ? B4 C1 C2 110.8(2) . . ? B3 C2 B7 61.70(17) . . ? B3 C2 C1 59.81(16) . . ? B7 C2 C1 108.0(2) . . ? B3 C2 B6 110.1(2) . . ? B7 C2 B6 110.6(2) . . ? C1 C2 B6 59.36(18) . . ? B3 C2 B11 111.3(2) . . ? B7 C2 B11 61.32(19) . . ? C1 C2 B11 107.7(2) . . ? B6 C2 B11 61.2(2) . . ? B3 C2 Zr1 117.64(16) . . ? B7 C2 Zr1 125.38(17) . . ? C1 C2 Zr1 116.92(15) . . ? B6 C2 Zr1 118.14(17) . . ? B11 C2 Zr1 125.26(17) . . ? C12 C11 C14 107.5(3) . . ? C12 C11 C13 107.7(3) . . ? C14 C11 C13 108.2(3) . . ? C12 C11 C1 111.0(3) . . ? C14 C11 C1 110.9(2) . . ? C13 C11 C1 111.4(2) . . ? C18 C14 C15 106.4(2) . . ? C18 C14 C11 127.1(3) . . ? C15 C14 C11 126.3(3) . . ? C18 C14 Zr1 73.04(15) . . ? C15 C14 Zr1 73.05(14) . . ? C11 C14 Zr1 123.33(17) . . ? C16 C15 C14 109.0(3) . . ? C16 C15 Zr1 72.93(16) . . ? C14 C15 Zr1 74.59(14) . . ? C17 C16 C15 108.1(3) . . ? C17 C16 Zr1 73.91(16) . . ? C15 C16 Zr1 74.74(16) . . ? C16 C17 C18 107.6(3) . . ? C16 C17 Zr1 73.68(16) . . ? C18 C17 Zr1 74.45(15) . . ? C14 C18 C17 108.8(3) . . ? C14 C18 Zr1 74.66(15) . . ? C17 C18 Zr1 72.96(15) . . ? C24 C19 C20 121.3(3) . . ? C24 C19 N1 119.5(2) . . ? C20 C19 N1 119.0(2) . . ? C19 C20 C21 117.7(3) . . ? C19 C20 C25 121.8(3) . . ? C21 C20 C25 120.5(3) . . ? C22 C21 C20 121.7(3) . . ? C21 C22 C23 120.0(3) . . ? C22 C23 C24 121.1(3) . . ? C19 C24 C23 118.0(3) . . ? C19 C24 C26 120.8(3) . . ? C23 C24 C26 121.3(3) . . ? N1 C27 N2 130.5(3) . . ? N1 C27 Zr1 72.85(14) . . ? N2 C27 Zr1 156.5(2) . . ? N2 C29 C30 114.6(3) . . ? C31 C30 C29 116.0(3) . . ? N3 C31 C30 115.1(3) . . ? N4 C33 N3 132.2(2) . . ? N4 C33 Zr1 74.53(14) . . ? N3 C33 Zr1 153.3(2) . . ? C39 C34 C35 120.9(2) . . ? C39 C34 N4 120.0(2) . . ? C35 C34 N4 119.1(2) . . ? C36 C35 C34 118.1(3) . . ? C36 C35 C40 120.1(3) . . ? C34 C35 C40 121.8(2) . . ? C37 C36 C35 122.0(3) . . ? C36 C37 C38 119.6(3) . . ? C37 C38 C39 121.5(3) . . ? C34 C39 C38 117.9(3) . . ? C34 C39 C41 120.8(3) . . ? C38 C39 C41 121.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.450 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.053 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 180.8 40.7 2 0.500 1.000 0.500 180.8 37.8 _platon_squeeze_details ; ; #===END data_8b _database_code_depnum_ccdc_archive 'CCDC 665274' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H90 B20 N8 O0.75 Zr2' _chemical_formula_weight 1346.05 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' B B 0.0013 0.0007 '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' Zr Zr -2.9673 0.5597 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.677(2) _cell_length_b 24.137(3) _cell_length_c 34.482(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.689(3) _cell_angle_gamma 90.00 _cell_volume 16189(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 972 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 16.18 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5584 _exptl_absorpt_coefficient_mu 0.297 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.524091 _exptl_absorpt_correction_T_max 1.0000 _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 SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86960 _diffrn_reflns_av_R_equivalents 0.1674 _diffrn_reflns_av_sigmaI/netI 0.3307 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 28466 _reflns_number_gt 7655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0985P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00142(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 28466 _refine_ls_number_parameters 1721 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.2405 _refine_ls_R_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.2507 _refine_ls_wR_factor_gt 0.2113 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.818 _refine_ls_shift/su_max 0.093 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.51091(5) 0.06914(4) 0.18479(3) 0.0538(3) Uani 1 1 d . . . Zr1' Zr -0.04342(5) 0.58981(4) 0.18167(3) 0.0553(3) Uani 1 1 d . . . Zr2 Zr 0.44633(5) 0.25732(4) 0.39295(3) 0.0478(3) Uani 1 1 d . . . Zr2' Zr 0.12962(5) 0.75689(4) 0.40144(3) 0.0509(3) Uani 1 1 d . . . N1' N -0.0146(4) 0.5285(3) 0.2189(2) 0.054(2) Uani 1 1 d . . . N1 N 0.5078(4) 0.1418(3) 0.2098(2) 0.063(2) Uani 1 1 d . . . N2' N 0.0426(4) 0.4729(3) 0.2682(2) 0.059(2) Uani 1 1 d . . . N2 N 0.4840(5) 0.2244(4) 0.2402(2) 0.070(3) Uani 1 1 d . . . N3' N 0.1419(4) 0.6183(4) 0.3264(3) 0.077(3) Uani 1 1 d . . . N3 N 0.5739(4) 0.3457(3) 0.3255(2) 0.052(2) Uani 1 1 d . . . N4' N 0.1293(4) 0.6880(3) 0.3718(2) 0.059(2) Uani 1 1 d . . . N4 N 0.5126(4) 0.3012(3) 0.3703(2) 0.057(2) Uani 1 1 d . . . N5' N -0.0207(4) 0.6575(3) 0.2121(2) 0.066(2) Uani 1 1 d . . . N5 N 0.5084(4) 0.0135(3) 0.2265(2) 0.056(2) Uani 1 1 d . . . N6' N 0.0171(5) 0.7361(4) 0.2474(3) 0.072(3) Uani 1 1 d . . . N6 N 0.4799(4) -0.0396(3) 0.2795(2) 0.0444(19) Uani 1 1 d . . . N7' N -0.0332(4) 0.8513(3) 0.3372(2) 0.058(2) Uani 1 1 d . . . N7 N 0.4030(4) 0.1127(3) 0.3220(2) 0.056(2) Uani 1 1 d . . . N8' N 0.0490(4) 0.7982(3) 0.3776(2) 0.061(2) Uani 1 1 d . . . N8 N 0.4347(4) 0.1888(3) 0.3624(2) 0.055(2) Uani 1 1 d . . . C1 C 0.4115(5) 0.0372(4) 0.0949(2) 0.052(3) Uani 1 1 d . . . C1' C -0.0092(6) 0.5665(4) 0.0865(3) 0.065(3) Uani 1 1 d . . . C2 C 0.4079(5) 0.0624(4) 0.1412(2) 0.052(3) Uani 1 1 d . . . C2' C 0.0265(5) 0.5849(4) 0.1325(3) 0.056(3) Uani 1 1 d . . . C11' C -0.0897(6) 0.5625(5) 0.0786(3) 0.080(4) Uani 1 1 d . . . C11 C 0.4845(6) 0.0275(4) 0.0840(3) 0.067(3) Uani 1 1 d . . . C12' C -0.1205(6) 0.6032(5) 0.0454(3) 0.112(5) Uani 1 1 d . . . H12A H -0.1085 0.6405 0.0532 0.168 Uiso 1 1 calc R . . H12B H -0.1696 0.5994 0.0407 0.168 Uiso 1 1 calc R . . H12C H -0.1023 0.5946 0.0218 0.168 Uiso 1 1 calc R . . C12 C 0.4936(6) 0.0585(5) 0.0471(3) 0.101(4) Uani 1 1 d . . . H12D H 0.4878 0.0975 0.0511 0.152 Uiso 1 1 calc R . . H12E H 0.4599 0.0461 0.0258 0.152 Uiso 1 1 calc R . . H12F H 0.5388 0.0518 0.0410 0.152 Uiso 1 1 calc R . . C13' C -0.1134(6) 0.5038(5) 0.0645(3) 0.109(5) Uani 1 1 d . . . H13A H -0.0962 0.4772 0.0843 0.163 Uiso 1 1 calc R . . H13B H -0.0960 0.4954 0.0407 0.163 Uiso 1 1 calc R . . H13C H -0.1627 0.5025 0.0599 0.163 Uiso 1 1 calc R . . C13 C 0.4960(6) -0.0363(5) 0.0754(3) 0.115(5) Uani 1 1 d . . . H13D H 0.4907 -0.0577 0.0982 0.172 Uiso 1 1 calc R . . H13E H 0.5415 -0.0415 0.0692 0.172 Uiso 1 1 calc R . . H13F H 0.4628 -0.0481 0.0537 0.172 Uiso 1 1 calc R . . C14 C 0.5396(6) 0.0435(6) 0.1176(3) 0.074(3) Uani 1 1 d . . . C14' C -0.1181(5) 0.5761(6) 0.1164(3) 0.070(3) Uani 1 1 d . . . C15' C -0.1345(6) 0.6302(5) 0.1289(4) 0.086(4) Uani 1 1 d . . . H15A H -0.1315 0.6650 0.1146 0.103 Uiso 1 1 calc R . . C15 C 0.5642(7) 0.1000(6) 0.1259(4) 0.091(4) Uani 1 1 d . . . H15B H 0.5514 0.1328 0.1097 0.109 Uiso 1 1 calc R . . C16' C -0.1617(5) 0.6230(5) 0.1632(4) 0.077(4) Uani 1 1 d . . . H16A H -0.1825 0.6528 0.1768 0.092 Uiso 1 1 calc R . . C16 C 0.6149(7) 0.0971(7) 0.1584(4) 0.100(5) Uani 1 1 d . . . H16B H 0.6454 0.1276 0.1684 0.120 Uiso 1 1 calc R . . C17' C -0.1661(5) 0.5672(5) 0.1720(3) 0.073(3) Uani 1 1 d . . . H17A H -0.1916 0.5511 0.1916 0.087 Uiso 1 1 calc R . . C17 C 0.6245(7) 0.0415(7) 0.1695(4) 0.087(4) Uani 1 1 d . . . H17B H 0.6626 0.0269 0.1884 0.104 Uiso 1 1 calc R . . C18' C -0.1396(5) 0.5384(5) 0.1429(3) 0.060(3) Uani 1 1 d . . . H18A H -0.1415 0.4981 0.1394 0.072 Uiso 1 1 calc R . . C18 C 0.5783(6) 0.0098(5) 0.1438(4) 0.073(3) Uani 1 1 d . . . H18B H 0.5773 -0.0308 0.1430 0.088 Uiso 1 1 calc R . . C21 C 0.2898(5) 0.3062(4) 0.4170(3) 0.057(3) Uani 1 1 d . . . C21' C 0.2790(5) 0.8358(4) 0.4268(3) 0.056(3) Uani 1 1 d . . . C22 C 0.3376(5) 0.2989(4) 0.3802(3) 0.052(3) Uani 1 1 d . . . C22' C 0.2258(5) 0.8061(4) 0.3878(3) 0.053(3) Uani 1 1 d . . . C31 C 0.3262(6) 0.2837(4) 0.4590(3) 0.071(3) Uani 1 1 d . . . C31' C 0.2591(6) 0.8238(5) 0.4683(3) 0.073(3) Uani 1 1 d . . . C32' C 0.2413(7) 0.8793(5) 0.4891(3) 0.115(5) Uani 1 1 d . . . H32A H 0.2017 0.8963 0.4741 0.173 Uiso 1 1 calc R . . H32B H 0.2796 0.9043 0.4909 0.173 Uiso 1 1 calc R . . H32C H 0.2318 0.8711 0.5150 0.173 Uiso 1 1 calc R . . C32 C 0.3290(7) 0.3309(5) 0.4896(3) 0.129(6) Uani 1 1 d . . . H32D H 0.3511 0.3177 0.5147 0.194 Uiso 1 1 calc R . . H32E H 0.2831 0.3427 0.4918 0.194 Uiso 1 1 calc R . . H32F H 0.3544 0.3616 0.4815 0.194 Uiso 1 1 calc R . . C33' C 0.3230(6) 0.7994(6) 0.4951(3) 0.121(5) Uani 1 1 d . . . H33A H 0.3369 0.7657 0.4838 0.181 Uiso 1 1 calc R . . H33B H 0.3114 0.7918 0.5206 0.181 Uiso 1 1 calc R . . H33C H 0.3600 0.8256 0.4974 0.181 Uiso 1 1 calc R . . C33 C 0.2813(6) 0.2358(5) 0.4732(3) 0.101(4) Uani 1 1 d . . . H33D H 0.3028 0.2225 0.4983 0.152 Uiso 1 1 calc R . . H33E H 0.2773 0.2060 0.4545 0.152 Uiso 1 1 calc R . . H33F H 0.2363 0.2498 0.4754 0.152 Uiso 1 1 calc R . . C34 C 0.3978(6) 0.2633(4) 0.4566(2) 0.056(3) Uani 1 1 d . . . C34' C 0.1985(6) 0.7845(5) 0.4656(3) 0.069(3) Uani 1 1 d . . . C35 C 0.4168(6) 0.2075(4) 0.4533(3) 0.066(3) Uani 1 1 d . . . H35A H 0.3861 0.1755 0.4531 0.079 Uiso 1 1 calc R . . C35' C 0.2011(6) 0.7264(5) 0.4629(3) 0.072(3) Uani 1 1 d . . . H35B H 0.2430 0.7039 0.4648 0.086 Uiso 1 1 calc R . . C36' C 0.1352(7) 0.7067(5) 0.4642(3) 0.079(4) Uani 1 1 d . . . H36A H 0.1232 0.6676 0.4668 0.095 Uiso 1 1 calc R . . C36 C 0.4884(7) 0.2052(5) 0.4538(3) 0.085(4) Uani 1 1 d . . . H36B H 0.5159 0.1712 0.4552 0.102 Uiso 1 1 calc R . . C37' C 0.0913(7) 0.7504(6) 0.4661(3) 0.083(4) Uani 1 1 d . . . H37A H 0.0435 0.7478 0.4708 0.100 Uiso 1 1 calc R . . C37 C 0.5153(6) 0.2596(6) 0.4596(3) 0.089(4) Uani 1 1 d . . . H37B H 0.5641 0.2694 0.4658 0.107 Uiso 1 1 calc R . . C38 C 0.4589(6) 0.2959(5) 0.4614(3) 0.069(3) Uani 1 1 d . . . H38A H 0.4622 0.3353 0.4685 0.082 Uiso 1 1 calc R . . C38' C 0.1301(6) 0.7977(5) 0.4682(3) 0.073(3) Uani 1 1 d . . . H38B H 0.1134 0.8348 0.4734 0.087 Uiso 1 1 calc R . . C41 C 0.5268(6) 0.1835(4) 0.2326(3) 0.057(3) Uani 1 1 d . . . C41' C -0.0150(5) 0.4946(4) 0.2477(3) 0.051(3) Uani 1 1 d . . . C42 C 0.6012(5) 0.1888(4) 0.2513(3) 0.055(3) Uani 1 1 d . . . C42' C -0.0807(5) 0.4806(4) 0.2614(3) 0.054(3) Uani 1 1 d . . . C43' C -0.1321(6) 0.4534(4) 0.2363(3) 0.066(3) Uani 1 1 d . . . H43A H -0.1245 0.4435 0.2113 0.080 Uiso 1 1 calc R . . C43 C 0.6419(6) 0.2327(5) 0.2425(3) 0.084(4) Uani 1 1 d . . . H43B H 0.6222 0.2610 0.2262 0.100 Uiso 1 1 calc R . . C44 C 0.7105(7) 0.2349(5) 0.2573(4) 0.084(4) Uani 1 1 d . . . H44A H 0.7374 0.2641 0.2506 0.101 Uiso 1 1 calc R . . C44' C -0.1942(6) 0.4411(5) 0.2481(4) 0.083(4) Uani 1 1 d . . . H44B H -0.2275 0.4216 0.2315 0.099 Uiso 1 1 calc R . . C45' C -0.2072(6) 0.4578(6) 0.2848(4) 0.101(4) Uani 1 1 d . . . H45A H -0.2489 0.4493 0.2930 0.121 Uiso 1 1 calc R . . C45 C 0.7401(7) 0.1925(7) 0.2828(4) 0.104(5) Uani 1 1 d . . . H45B H 0.7863 0.1944 0.2937 0.124 Uiso 1 1 calc R . . C46' C -0.1573(7) 0.4872(5) 0.3092(3) 0.097(4) Uani 1 1 d . . . H46A H -0.1669 0.5004 0.3331 0.116 Uiso 1 1 calc R . . C46 C 0.7011(7) 0.1491(6) 0.2915(4) 0.102(4) Uani 1 1 d . . . H46B H 0.7210 0.1213 0.3081 0.122 Uiso 1 1 calc R . . C47 C 0.6322(6) 0.1457(4) 0.2758(3) 0.072(3) Uani 1 1 d . . . H47A H 0.6063 0.1152 0.2813 0.086 Uiso 1 1 calc R . . C47' C -0.0948(6) 0.4971(4) 0.2986(3) 0.074(3) Uani 1 1 d . . . H47B H -0.0610 0.5149 0.3159 0.089 Uiso 1 1 calc R . . C48 C 0.4113(6) 0.2226(5) 0.2197(4) 0.127(5) Uani 1 1 d . . . H48A H 0.4082 0.1980 0.1976 0.190 Uiso 1 1 calc R . . H48B H 0.3971 0.2591 0.2109 0.190 Uiso 1 1 calc R . . H48C H 0.3819 0.2094 0.2375 0.190 Uiso 1 1 calc R . . C48' C 0.0447(5) 0.4328(4) 0.3000(3) 0.071(3) Uani 1 1 d . . . H48D H -0.0013 0.4238 0.3039 0.106 Uiso 1 1 calc R . . H48E H 0.0691 0.4484 0.3237 0.106 Uiso 1 1 calc R . . H48F H 0.0677 0.3998 0.2935 0.106 Uiso 1 1 calc R . . C49' C 0.1098(5) 0.4897(4) 0.2602(3) 0.067(3) Uani 1 1 d . . . H49A H 0.1045 0.5084 0.2350 0.081 Uiso 1 1 calc R . . H49B H 0.1375 0.4569 0.2583 0.081 Uiso 1 1 calc R . . C49 C 0.4960(5) 0.2608(4) 0.2741(3) 0.070(3) Uani 1 1 d . . . H49C H 0.5394 0.2511 0.2899 0.084 Uiso 1 1 calc R . . H49D H 0.4599 0.2553 0.2900 0.084 Uiso 1 1 calc R . . C50 C 0.4977(5) 0.3207(4) 0.2626(3) 0.073(3) Uani 1 1 d . . . H50A H 0.4542 0.3306 0.2469 0.087 Uiso 1 1 calc R . . H50B H 0.5338 0.3264 0.2468 0.087 Uiso 1 1 calc R . . C50' C 0.1477(5) 0.5279(4) 0.2911(3) 0.085(4) Uani 1 1 d . . . H50C H 0.1562 0.5085 0.3161 0.103 Uiso 1 1 calc R . . H50D H 0.1918 0.5377 0.2838 0.103 Uiso 1 1 calc R . . C51 C 0.5105(5) 0.3583(4) 0.2990(3) 0.063(3) Uani 1 1 d . . . H51A H 0.5123 0.3965 0.2905 0.075 Uiso 1 1 calc R . . H51B H 0.4720 0.3549 0.3134 0.075 Uiso 1 1 calc R . . C51' C 0.1071(5) 0.5801(4) 0.2958(3) 0.067(3) Uani 1 1 d . . . H51C H 0.0993 0.5995 0.2709 0.081 Uiso 1 1 calc R . . H51D H 0.0626 0.5699 0.3025 0.081 Uiso 1 1 calc R . . C52 C 0.6389(5) 0.3669(4) 0.3122(3) 0.069(3) Uani 1 1 d . . . H52A H 0.6779 0.3564 0.3309 0.104 Uiso 1 1 calc R . . H52B H 0.6369 0.4066 0.3102 0.104 Uiso 1 1 calc R . . H52C H 0.6430 0.3513 0.2871 0.104 Uiso 1 1 calc R . . C52' C 0.1979(6) 0.6500(4) 0.3151(3) 0.100(4) Uani 1 1 d . . . H52D H 0.2178 0.6728 0.3367 0.150 Uiso 1 1 calc R . . H52E H 0.1809 0.6731 0.2931 0.150 Uiso 1 1 calc R . . H52F H 0.2322 0.6253 0.3080 0.150 Uiso 1 1 calc R . . C53' C 0.1128(5) 0.6407(4) 0.3554(3) 0.058(3) Uani 1 1 d . . . C53 C 0.5705(6) 0.3170(4) 0.3594(3) 0.055(3) Uani 1 1 d . . . C54 C 0.6403(5) 0.3029(4) 0.3830(3) 0.055(3) Uani 1 1 d . . . C54' C 0.0578(6) 0.6067(5) 0.3691(3) 0.066(3) Uani 1 1 d . . . C55 C 0.6630(6) 0.3291(4) 0.4169(3) 0.072(3) Uani 1 1 d . . . H55A H 0.6365 0.3572 0.4255 0.086 Uiso 1 1 calc R . . C55' C 0.0675(7) 0.5525(5) 0.3801(3) 0.085(4) Uani 1 1 d . . . H55B H 0.1089 0.5359 0.3768 0.103 Uiso 1 1 calc R . . C56' C 0.0210(10) 0.5212(7) 0.3957(5) 0.119(6) Uani 1 1 d . . . H56A H 0.0303 0.4846 0.4030 0.143 Uiso 1 1 calc R . . C56 C 0.7252(7) 0.3151(6) 0.4394(3) 0.090(4) Uani 1 1 d . . . H56B H 0.7410 0.3347 0.4622 0.108 Uiso 1 1 calc R . . C57' C -0.0391(12) 0.5452(8) 0.4001(4) 0.130(7) Uani 1 1 d . . . H57A H -0.0712 0.5243 0.4110 0.156 Uiso 1 1 calc R . . C57 C 0.7635(7) 0.2718(6) 0.4277(4) 0.098(4) Uani 1 1 d . . . H57B H 0.8042 0.2608 0.4431 0.117 Uiso 1 1 calc R . . C58 C 0.7404(6) 0.2457(5) 0.3932(3) 0.087(4) Uani 1 1 d . . . H58A H 0.7658 0.2165 0.3851 0.104 Uiso 1 1 calc R . . C58' C -0.0562(7) 0.6010(7) 0.3890(4) 0.118(5) Uani 1 1 d . . . H58B H -0.0986 0.6164 0.3914 0.142 Uiso 1 1 calc R . . C59' C -0.0043(7) 0.6313(5) 0.3740(3) 0.084(4) Uani 1 1 d . . . H59A H -0.0119 0.6684 0.3673 0.101 Uiso 1 1 calc R . . C59 C 0.6802(6) 0.2615(5) 0.3701(3) 0.072(3) Uani 1 1 d . . . H59C H 0.6665 0.2445 0.3459 0.087 Uiso 1 1 calc R . . C60 C 0.5271(5) -0.0163(4) 0.2582(3) 0.043(2) Uani 1 1 d . . . C60' C -0.0288(5) 0.6961(5) 0.2381(3) 0.065(3) Uani 1 1 d . . . C61 C 0.6021(5) -0.0243(4) 0.2725(3) 0.053(3) Uani 1 1 d . . . C61' C -0.0930(6) 0.6961(5) 0.2566(3) 0.060(3) Uani 1 1 d . . . C62' C -0.1098(6) 0.6476(5) 0.2757(3) 0.079(3) Uani 1 1 d . . . H62A H -0.0798 0.6175 0.2780 0.095 Uiso 1 1 calc R . . C62 C 0.6328(6) -0.0002(4) 0.3076(3) 0.062(3) Uani 1 1 d . . . H62B H 0.6067 0.0203 0.3228 0.074 Uiso 1 1 calc R . . C63' C -0.1705(8) 0.6443(7) 0.2910(4) 0.105(5) Uani 1 1 d . . . H63A H -0.1821 0.6120 0.3032 0.126 Uiso 1 1 calc R . . C63 C 0.7012(7) -0.0069(5) 0.3190(4) 0.091(4) Uani 1 1 d . . . H63B H 0.7217 0.0090 0.3425 0.109 Uiso 1 1 calc R . . C64' C -0.2138(7) 0.6896(9) 0.2881(4) 0.107(5) Uani 1 1 d . . . H64A H -0.2543 0.6883 0.2989 0.129 Uiso 1 1 calc R . . C64 C 0.7414(6) -0.0366(5) 0.2969(5) 0.097(4) Uani 1 1 d . . . H64B H 0.7882 -0.0411 0.3053 0.116 Uiso 1 1 calc R . . C65' C -0.1965(8) 0.7375(6) 0.2687(4) 0.105(5) Uani 1 1 d . . . H65A H -0.2266 0.7675 0.2657 0.126 Uiso 1 1 calc R . . C65 C 0.7100(7) -0.0598(5) 0.2619(4) 0.096(4) Uani 1 1 d . . . H65B H 0.7362 -0.0798 0.2464 0.115 Uiso 1 1 calc R . . C66' C -0.1364(6) 0.7404(5) 0.2545(3) 0.075(3) Uani 1 1 d . . . H66A H -0.1244 0.7731 0.2430 0.089 Uiso 1 1 calc R . . C66 C 0.6408(5) -0.0535(5) 0.2499(3) 0.072(3) Uani 1 1 d . . . H66B H 0.6202 -0.0691 0.2263 0.087 Uiso 1 1 calc R . . C67 C 0.4991(5) -0.0739(4) 0.3132(3) 0.070(3) Uani 1 1 d . . . H67A H 0.5479 -0.0800 0.3169 0.105 Uiso 1 1 calc R . . H67B H 0.4757 -0.1088 0.3093 0.105 Uiso 1 1 calc R . . H67C H 0.4866 -0.0560 0.3360 0.105 Uiso 1 1 calc R . . C67' C 0.0766(7) 0.7390(5) 0.2274(4) 0.126(5) Uani 1 1 d . . . H67D H 0.0689 0.7166 0.2042 0.189 Uiso 1 1 calc R . . H67E H 0.1164 0.7257 0.2444 0.189 Uiso 1 1 calc R . . H67F H 0.0840 0.7768 0.2203 0.189 Uiso 1 1 calc R . . C68 C 0.4082(5) -0.0273(4) 0.2701(3) 0.059(3) Uani 1 1 d . . . H68A H 0.3820 -0.0610 0.2719 0.071 Uiso 1 1 calc R . . H68B H 0.3987 -0.0142 0.2432 0.071 Uiso 1 1 calc R . . C68' C 0.0213(5) 0.7698(4) 0.2833(3) 0.064(3) Uani 1 1 d . . . H68C H 0.0662 0.7645 0.2988 0.077 Uiso 1 1 calc R . . H68D H -0.0127 0.7565 0.2987 0.077 Uiso 1 1 calc R . . C69' C 0.0099(5) 0.8318(4) 0.2759(3) 0.069(3) Uani 1 1 d . . . H69A H 0.0429 0.8447 0.2597 0.083 Uiso 1 1 calc R . . H69B H -0.0356 0.8371 0.2612 0.083 Uiso 1 1 calc R . . C69 C 0.3850(5) 0.0157(4) 0.2968(3) 0.063(3) Uani 1 1 d . . . H69C H 0.3915 0.0014 0.3234 0.076 Uiso 1 1 calc R . . H69D H 0.3363 0.0224 0.2890 0.076 Uiso 1 1 calc R . . C70 C 0.4234(5) 0.0706(4) 0.2964(3) 0.060(3) Uani 1 1 d . . . H70A H 0.4722 0.0636 0.3038 0.073 Uiso 1 1 calc R . . H70B H 0.4166 0.0848 0.2698 0.073 Uiso 1 1 calc R . . C70' C 0.0165(5) 0.8668(4) 0.3122(3) 0.064(3) Uani 1 1 d . . . H70C H 0.0625 0.8628 0.3266 0.077 Uiso 1 1 calc R . . H70D H 0.0099 0.9054 0.3047 0.077 Uiso 1 1 calc R . . C71' C -0.1041(5) 0.8751(4) 0.3271(3) 0.080(3) Uani 1 1 d . . . H71A H -0.1324 0.8621 0.3455 0.121 Uiso 1 1 calc R . . H71B H -0.1235 0.8637 0.3011 0.121 Uiso 1 1 calc R . . H71C H -0.1016 0.9148 0.3282 0.121 Uiso 1 1 calc R . . C71 C 0.3372(5) 0.1406(4) 0.3074(3) 0.078(3) Uani 1 1 d . . . H71D H 0.3274 0.1675 0.3263 0.117 Uiso 1 1 calc R . . H71E H 0.3010 0.1136 0.3035 0.117 Uiso 1 1 calc R . . H71F H 0.3406 0.1586 0.2830 0.117 Uiso 1 1 calc R . . C72 C 0.4467(5) 0.1389(4) 0.3502(3) 0.051(3) Uani 1 1 d . . . C72' C -0.0133(6) 0.8170(4) 0.3689(3) 0.063(3) Uani 1 1 d . . . C73 C 0.5099(6) 0.1100(4) 0.3673(3) 0.058(3) Uani 1 1 d . . . C73' C -0.0696(6) 0.8013(4) 0.3917(3) 0.064(3) Uani 1 1 d . . . C74 C 0.5072(6) 0.0588(5) 0.3833(3) 0.075(3) Uani 1 1 d . . . H74A H 0.4653 0.0403 0.3801 0.089 Uiso 1 1 calc R . . C74' C -0.1143(6) 0.7585(5) 0.3799(3) 0.085(4) Uani 1 1 d . . . H74B H -0.1116 0.7418 0.3559 0.101 Uiso 1 1 calc R . . C75' C -0.1630(7) 0.7389(6) 0.4015(5) 0.117(5) Uani 1 1 d . . . H75A H -0.1936 0.7110 0.3920 0.140 Uiso 1 1 calc R . . C75 C 0.5675(8) 0.0312(5) 0.4053(4) 0.102(4) Uani 1 1 d . . . H75B H 0.5657 -0.0038 0.4163 0.122 Uiso 1 1 calc R . . C76' C -0.1639(10) 0.7614(11) 0.4357(6) 0.163(9) Uani 1 1 d . . . H76A H -0.1943 0.7469 0.4513 0.196 Uiso 1 1 calc R . . C76 C 0.6261(7) 0.0614(7) 0.4082(4) 0.097(4) Uani 1 1 d . . . H76B H 0.6663 0.0456 0.4213 0.116 Uiso 1 1 calc R . . C77' C -0.1231(12) 0.8051(11) 0.4504(6) 0.185(10) Uani 1 1 d . . . H77A H -0.1278 0.8210 0.4744 0.222 Uiso 1 1 calc R . . C77 C 0.6302(6) 0.1131(6) 0.3931(4) 0.084(4) Uani 1 1 d . . . H77B H 0.6719 0.1319 0.3969 0.101 Uiso 1 1 calc R . . C78' C -0.0725(7) 0.8255(7) 0.4273(5) 0.134(6) Uani 1 1 d . . . H78A H -0.0429 0.8543 0.4364 0.161 Uiso 1 1 calc R . . C78 C 0.5741(6) 0.1373(4) 0.3727(3) 0.077(3) Uani 1 1 d . . . H78C H 0.5778 0.1723 0.3619 0.092 Uiso 1 1 calc R . . B3' B 0.0328(7) 0.5184(6) 0.1154(4) 0.075(4) Uani 1 1 d . . . H3' H 0.0065 0.4831 0.1270 0.090 Uiso 1 1 calc R . . B3 B 0.3871(7) 0.1044(5) 0.1002(3) 0.063(4) Uani 1 1 d . . . H3 H 0.4189 0.1398 0.0940 0.076 Uiso 1 1 calc R . . B4 B 0.3442(7) 0.0614(5) 0.0639(3) 0.074(4) Uani 1 1 d . . . H4 H 0.3477 0.0690 0.0328 0.089 Uiso 1 1 calc R . . B4' B 0.0433(8) 0.5234(6) 0.0663(4) 0.090(5) Uani 1 1 d . . . H4' H 0.0250 0.4907 0.0451 0.108 Uiso 1 1 calc R . . B5 B 0.3405(6) -0.0070(5) 0.0817(3) 0.065(4) Uani 1 1 d . . . H5 H 0.3415 -0.0439 0.0631 0.078 Uiso 1 1 calc R . . B5' B 0.0376(8) 0.5929(6) 0.0536(4) 0.086(5) Uani 1 1 d . . . H5' H 0.0146 0.6057 0.0239 0.103 Uiso 1 1 calc R . . B6 B 0.3841(6) -0.0058(5) 0.1306(3) 0.065(4) Uani 1 1 d . . . H6 H 0.4143 -0.0412 0.1439 0.079 Uiso 1 1 calc R . . B6' B 0.0248(7) 0.6319(5) 0.0945(4) 0.075(4) Uani 1 1 d . . . H6' H -0.0065 0.6699 0.0925 0.090 Uiso 1 1 calc R . . B7 B 0.3375(6) 0.1061(5) 0.1391(3) 0.059(3) Uani 1 1 d . . . H7 H 0.3362 0.1429 0.1579 0.070 Uiso 1 1 calc R . . B7' B 0.1042(6) 0.5521(5) 0.1413(4) 0.072(4) Uani 1 1 d . . . H7' H 0.1265 0.5374 0.1707 0.087 Uiso 1 1 calc R . . B8 B 0.2969(7) 0.1053(5) 0.0895(4) 0.080(4) Uani 1 1 d . . . H8 H 0.2693 0.1416 0.0757 0.096 Uiso 1 1 calc R . . B8' B 0.1174(8) 0.5137(7) 0.1014(4) 0.092(5) Uani 1 1 d . . . H8' H 0.1476 0.4752 0.1041 0.111 Uiso 1 1 calc R . . B9' B 0.1184(8) 0.5617(6) 0.0632(4) 0.091(5) Uani 1 1 d . . . H9' H 0.1500 0.5536 0.0401 0.109 Uiso 1 1 calc R . . B9 B 0.2669(7) 0.0362(6) 0.0780(4) 0.082(4) Uani 1 1 d . . . H9 H 0.2197 0.0284 0.0572 0.098 Uiso 1 1 calc R . . B10 B 0.2925(7) -0.0078(6) 0.1196(3) 0.076(4) Uani 1 1 d . . . H10 H 0.2629 -0.0446 0.1256 0.091 Uiso 1 1 calc R . . B10' B 0.1078(7) 0.6299(6) 0.0794(4) 0.086(5) Uani 1 1 d . . . H10' H 0.1310 0.6664 0.0673 0.103 Uiso 1 1 calc R . . B11 B 0.3350(6) 0.0384(5) 0.1576(3) 0.065(4) Uani 1 1 d . . . H11 H 0.3321 0.0314 0.1888 0.078 Uiso 1 1 calc R . . B11' B 0.0998(7) 0.6229(6) 0.1288(4) 0.080(4) Uani 1 1 d . . . H11' H 0.1189 0.6556 0.1499 0.096 Uiso 1 1 calc R . . B12 B 0.2636(6) 0.0630(5) 0.1259(4) 0.071(4) Uani 1 1 d . . . H12 H 0.2144 0.0716 0.1362 0.085 Uiso 1 1 calc R . . B12' B 0.1546(7) 0.5812(6) 0.1087(4) 0.086(5) Uani 1 1 d . . . H12' H 0.2106 0.5867 0.1163 0.103 Uiso 1 1 calc R . . B23 B 0.2693(5) 0.2584(5) 0.3822(3) 0.050(3) Uani 1 1 d . . . H23 H 0.2758 0.2137 0.3876 0.060 Uiso 1 1 calc R . . B23' B 0.2218(6) 0.8759(5) 0.3944(3) 0.058(3) Uani 1 1 d . . . H23' H 0.1759 0.8958 0.4027 0.069 Uiso 1 1 calc R . . B24' B 0.3072(8) 0.8990(6) 0.4115(4) 0.089(5) Uani 1 1 d . . . H24' H 0.3168 0.9353 0.4308 0.107 Uiso 1 1 calc R . . B24 B 0.2031(7) 0.2966(5) 0.4010(3) 0.071(4) Uani 1 1 d . . . H24 H 0.1665 0.2774 0.4181 0.085 Uiso 1 1 calc R . . B25' B 0.3622(7) 0.8401(6) 0.4177(4) 0.085(4) Uani 1 1 d . . . H25' H 0.4072 0.8369 0.4407 0.102 Uiso 1 1 calc R . . B25 B 0.2407(8) 0.3654(5) 0.4113(4) 0.086(5) Uani 1 1 d . . . H25 H 0.2275 0.3910 0.4355 0.104 Uiso 1 1 calc R . . B26' B 0.3091(6) 0.7824(5) 0.4015(4) 0.069(4) Uani 1 1 d . . . H26' H 0.3196 0.7409 0.4143 0.083 Uiso 1 1 calc R . . B26 B 0.3256(7) 0.3641(5) 0.3986(4) 0.076(4) Uani 1 1 d . . . H26 H 0.3681 0.3880 0.4150 0.091 Uiso 1 1 calc R . . B27 B 0.2836(6) 0.2889(4) 0.3380(3) 0.060(3) Uani 1 1 d . . . H27 H 0.2984 0.2642 0.3138 0.071 Uiso 1 1 calc R . . B27' B 0.2235(6) 0.8488(5) 0.3479(3) 0.067(4) Uani 1 1 d . . . H27' H 0.1780 0.8516 0.3252 0.080 Uiso 1 1 calc R . . B28 B 0.1963(7) 0.2873(5) 0.3498(4) 0.075(4) Uani 1 1 d . . . H28 H 0.1546 0.2621 0.3339 0.091 Uiso 1 1 calc R . . B28' B 0.2732(6) 0.9070(5) 0.3623(4) 0.066(4) Uani 1 1 d . . . H28' H 0.2607 0.9481 0.3494 0.080 Uiso 1 1 calc R . . B29' B 0.3582(7) 0.8844(6) 0.3767(4) 0.074(4) Uani 1 1 d . . . H29' H 0.4024 0.9110 0.3735 0.089 Uiso 1 1 calc R . . B29 B 0.1816(9) 0.3536(7) 0.3678(4) 0.108(6) Uani 1 1 d . . . H29 H 0.1298 0.3719 0.3636 0.129 Uiso 1 1 calc R . . B30' B 0.3609(7) 0.8127(6) 0.3693(4) 0.079(4) Uani 1 1 d . . . H30' H 0.4061 0.7915 0.3610 0.094 Uiso 1 1 calc R . . B30 B 0.2584(8) 0.3945(6) 0.3671(5) 0.099(5) Uani 1 1 d . . . H30 H 0.2564 0.4396 0.3625 0.119 Uiso 1 1 calc R . . B31 B 0.3186(7) 0.3555(5) 0.3485(4) 0.073(4) Uani 1 1 d . . . H31 H 0.3555 0.3747 0.3317 0.088 Uiso 1 1 calc R . . B31' B 0.2757(6) 0.7905(5) 0.3509(3) 0.065(4) Uani 1 1 d . . . H31' H 0.2649 0.7552 0.3307 0.078 Uiso 1 1 calc R . . B32' B 0.3081(6) 0.8543(5) 0.3353(4) 0.072(4) Uani 1 1 d . . . H32' H 0.3190 0.8607 0.3052 0.086 Uiso 1 1 calc R . . B32 B 0.2289(7) 0.3477(6) 0.3283(4) 0.084(4) Uani 1 1 d . . . H32 H 0.2076 0.3611 0.2984 0.100 Uiso 1 1 calc R . . O1 O 0.2807(12) 0.5960(7) 0.4715(5) 0.169(8) Uani 0.50 1 d PDU . . C81 C 0.3008(14) 0.6064(9) 0.4346(7) 0.136(11) Uani 0.50 1 d PDU . . H81A H 0.3502 0.6071 0.4352 0.164 Uiso 0.50 1 calc PR . . H81B H 0.2794 0.6390 0.4216 0.164 Uiso 0.50 1 calc PR . . C82 C 0.2673(13) 0.5522(9) 0.4192(5) 0.117(9) Uani 0.50 1 d PDU . . H82A H 0.2231 0.5596 0.4034 0.141 Uiso 0.50 1 calc PR . . H82B H 0.2962 0.5335 0.4028 0.141 Uiso 0.50 1 calc PR . . C83 C 0.2577(13) 0.5156(6) 0.4537(6) 0.121(9) Uani 0.50 1 d PDU . . H83A H 0.3007 0.5043 0.4692 0.146 Uiso 0.50 1 calc PR . . H83B H 0.2286 0.4837 0.4463 0.146 Uiso 0.50 1 calc PR . . C84 C 0.2211(11) 0.5619(10) 0.4729(8) 0.152(12) Uani 0.50 1 d PDU . . H84A H 0.1797 0.5754 0.4569 0.183 Uiso 0.50 1 calc PR . . H84B H 0.2128 0.5533 0.4993 0.183 Uiso 0.50 1 calc PR . . O2 O 0.3113(8) 0.0874(6) 0.4513(5) 0.107(5) Uani 0.50 1 d PDU . . C91 C 0.3213(10) 0.0689(7) 0.4139(5) 0.070(6) Uani 0.50 1 d PDU . . H91A H 0.3325 0.0982 0.3966 0.084 Uiso 0.50 1 calc PR . . H91B H 0.2846 0.0456 0.4009 0.084 Uiso 0.50 1 calc PR . . C92 C 0.385(2) 0.036(3) 0.4343(8) 0.61(7) Uani 0.50 1 d PDU . . H92A H 0.3761 -0.0030 0.4308 0.737 Uiso 0.50 1 calc PR . . H92B H 0.4243 0.0457 0.4220 0.737 Uiso 0.50 1 calc PR . . C93 C 0.4005(13) 0.0493(14) 0.4783(8) 0.212(17) Uani 0.50 1 d PDU . . H93A H 0.4244 0.0189 0.4929 0.254 Uiso 0.50 1 calc PR . . H93B H 0.4270 0.0831 0.4833 0.254 Uiso 0.50 1 calc PR . . C94 C 0.3277(16) 0.0559(13) 0.4872(7) 0.211(17) Uani 0.50 1 d PDU . . H94A H 0.3026 0.0213 0.4872 0.253 Uiso 0.50 1 calc PR . . H94B H 0.3247 0.0772 0.5108 0.253 Uiso 0.50 1 calc PR . . O3 O 0.0245(16) 0.4211(10) 0.4873(9) 0.286(15) Uani 0.50 1 d PDU . . C101 C -0.0209(13) 0.3773(16) 0.4921(11) 0.215(17) Uani 0.50 1 d PDU . . H10C H -0.0607 0.3757 0.4718 0.258 Uiso 0.50 1 calc PR . . H10D H -0.0343 0.3756 0.5180 0.258 Uiso 0.50 1 calc PR . . C102 C 0.0362(16) 0.3360(9) 0.4861(11) 0.239(19) Uani 0.50 1 d PDU . . H10E H 0.0305 0.3014 0.4994 0.287 Uiso 0.50 1 calc PR . . H10F H 0.0358 0.3286 0.4584 0.287 Uiso 0.50 1 calc PR . . C103 C 0.1029(12) 0.3647(11) 0.5038(8) 0.152(12) Uani 0.50 1 d PDU . . H103E H 0.1041 0.3737 0.5313 0.182 Uiso 0.50 1 calc PR . . H103F H 0.1434 0.3437 0.5001 0.182 Uiso 0.50 1 calc PR . . C104 C 0.0923(17) 0.4155(12) 0.4774(9) 0.223(18) Uani 0.50 1 d PDU . . H10A H 0.1226 0.4461 0.4863 0.267 Uiso 0.50 1 calc PR . . H10B H 0.0930 0.4075 0.4499 0.267 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0493(6) 0.0616(7) 0.0532(7) -0.0019(5) 0.0167(5) -0.0022(5) Zr1' 0.0447(6) 0.0688(7) 0.0521(6) 0.0049(5) 0.0063(5) 0.0034(5) Zr2 0.0465(6) 0.0447(6) 0.0523(6) 0.0015(5) 0.0074(5) 0.0012(5) Zr2' 0.0421(6) 0.0571(7) 0.0532(6) 0.0054(5) 0.0058(5) -0.0029(5) N1' 0.052(5) 0.069(6) 0.042(5) 0.017(4) 0.009(4) 0.015(4) N1 0.066(6) 0.054(6) 0.073(6) -0.005(5) 0.023(5) -0.005(5) N2' 0.048(6) 0.061(6) 0.066(6) 0.001(5) 0.004(5) 0.008(5) N2 0.073(7) 0.070(7) 0.063(6) -0.011(5) -0.005(5) 0.005(5) N3' 0.052(6) 0.074(7) 0.111(8) -0.018(6) 0.028(6) -0.010(5) N3 0.057(6) 0.036(5) 0.062(6) 0.000(4) 0.008(5) 0.003(4) N4' 0.060(6) 0.062(6) 0.056(6) -0.017(5) 0.009(4) -0.003(5) N4 0.054(6) 0.054(5) 0.064(6) 0.002(4) 0.011(5) -0.004(4) N5' 0.069(6) 0.068(6) 0.065(6) -0.008(5) 0.022(5) -0.005(5) N5 0.042(5) 0.066(6) 0.064(6) -0.002(5) 0.018(4) -0.007(4) N6' 0.066(7) 0.087(7) 0.073(7) -0.009(5) 0.045(5) -0.014(6) N6 0.050(6) 0.039(5) 0.048(5) 0.002(4) 0.017(4) 0.001(4) N7' 0.049(6) 0.057(6) 0.068(6) 0.010(5) 0.007(5) 0.001(5) N7 0.045(5) 0.049(5) 0.074(6) -0.015(5) 0.010(5) 0.011(4) N8' 0.039(5) 0.064(6) 0.078(6) 0.016(5) -0.001(5) 0.004(4) N8 0.047(5) 0.051(5) 0.069(6) -0.015(4) 0.015(4) 0.000(4) C1 0.068(7) 0.056(7) 0.033(6) 0.003(5) 0.008(5) 0.022(6) C1' 0.076(8) 0.083(8) 0.033(6) 0.002(6) 0.003(6) -0.033(7) C2 0.054(7) 0.069(7) 0.035(6) -0.004(5) 0.013(5) -0.001(5) C2' 0.048(6) 0.074(7) 0.045(6) -0.001(5) 0.004(5) 0.000(5) C11' 0.068(8) 0.094(9) 0.068(8) 0.024(7) -0.020(7) -0.033(7) C11 0.081(9) 0.087(9) 0.041(7) 0.006(6) 0.034(6) 0.020(7) C12' 0.100(11) 0.143(12) 0.083(9) 0.042(8) -0.017(8) -0.015(9) C12 0.092(10) 0.147(12) 0.070(9) 0.011(8) 0.025(7) 0.024(9) C13' 0.103(10) 0.117(11) 0.100(10) -0.042(8) -0.003(8) -0.067(9) C13 0.133(12) 0.098(10) 0.119(11) -0.028(8) 0.040(9) 0.052(9) C14 0.070(9) 0.089(10) 0.069(9) 0.002(8) 0.032(7) 0.007(8) C14' 0.055(7) 0.096(10) 0.053(8) 0.026(7) -0.008(6) -0.010(7) C15' 0.079(10) 0.084(10) 0.087(10) 0.033(8) -0.008(8) 0.010(8) C15 0.093(11) 0.114(13) 0.081(10) 0.015(9) 0.061(9) 0.003(9) C16' 0.043(7) 0.070(9) 0.115(11) 0.025(8) 0.004(7) 0.004(6) C16 0.058(9) 0.152(16) 0.097(11) -0.014(10) 0.031(8) -0.042(9) C17' 0.037(7) 0.104(10) 0.077(9) 0.028(8) 0.012(6) 0.002(7) C17 0.067(10) 0.100(11) 0.099(11) 0.022(9) 0.033(8) 0.019(8) C18' 0.035(6) 0.082(8) 0.062(8) 0.016(7) 0.002(6) -0.014(6) C18 0.063(8) 0.086(9) 0.076(9) 0.009(8) 0.029(7) 0.020(8) C21 0.056(7) 0.060(7) 0.060(7) 0.000(5) 0.021(6) 0.014(5) C21' 0.054(7) 0.066(7) 0.048(7) -0.007(5) 0.010(5) -0.020(5) C22 0.059(7) 0.053(6) 0.047(6) -0.006(5) 0.019(5) 0.009(5) C22' 0.051(7) 0.067(7) 0.041(6) 0.006(5) 0.005(5) -0.001(5) C31 0.092(9) 0.071(8) 0.048(7) -0.019(6) 0.004(7) 0.024(7) C31' 0.071(8) 0.086(9) 0.062(8) 0.002(7) 0.017(7) -0.017(7) C32' 0.149(13) 0.112(11) 0.098(10) -0.054(8) 0.063(9) -0.069(9) C32 0.167(14) 0.139(12) 0.075(9) -0.060(8) -0.006(9) 0.064(10) C33' 0.090(10) 0.190(15) 0.071(9) 0.039(9) -0.028(8) -0.028(10) C33 0.082(9) 0.149(12) 0.085(9) 0.045(8) 0.051(7) -0.003(8) C34 0.082(9) 0.051(7) 0.035(6) -0.010(5) 0.006(6) -0.007(7) C34' 0.060(9) 0.099(10) 0.048(7) 0.005(6) 0.012(6) -0.015(7) C35 0.079(9) 0.052(8) 0.065(8) 0.015(6) 0.007(6) 0.011(6) C35' 0.067(9) 0.069(9) 0.079(8) 0.014(6) 0.011(7) -0.002(7) C36' 0.086(10) 0.068(9) 0.082(9) 0.020(7) 0.005(7) -0.016(8) C36 0.089(11) 0.071(9) 0.087(9) 0.002(7) -0.010(8) 0.026(8) C37' 0.074(9) 0.100(11) 0.080(9) 0.011(8) 0.028(7) -0.026(9) C37 0.067(9) 0.133(13) 0.061(8) -0.007(8) -0.013(6) -0.001(9) C38 0.072(9) 0.069(8) 0.065(8) -0.010(6) 0.012(6) -0.009(7) C38' 0.053(8) 0.098(10) 0.072(8) -0.005(7) 0.023(6) 0.010(7) C41 0.069(8) 0.049(7) 0.054(7) 0.001(6) 0.008(6) 0.005(6) C41' 0.040(7) 0.059(7) 0.052(7) -0.009(5) 0.001(6) 0.006(6) C42 0.063(8) 0.051(7) 0.055(7) -0.003(5) 0.017(6) -0.005(6) C42' 0.064(8) 0.047(6) 0.048(7) 0.001(5) -0.003(6) -0.002(5) C43' 0.049(7) 0.084(8) 0.064(8) -0.011(6) 0.003(6) 0.011(6) C43 0.068(9) 0.088(10) 0.099(10) 0.007(7) 0.027(8) 0.003(7) C44 0.073(10) 0.099(10) 0.085(10) -0.005(8) 0.028(8) -0.017(8) C44' 0.054(8) 0.099(10) 0.093(10) -0.025(8) 0.004(7) -0.008(7) C45' 0.063(9) 0.142(13) 0.101(11) -0.009(9) 0.026(9) -0.018(8) C45 0.077(11) 0.147(15) 0.086(11) -0.038(10) 0.009(9) -0.013(11) C46' 0.075(10) 0.151(13) 0.075(9) -0.029(8) 0.042(8) -0.024(9) C46 0.065(10) 0.113(12) 0.121(12) -0.001(9) -0.006(9) 0.019(9) C47 0.089(10) 0.064(8) 0.062(8) 0.004(6) 0.012(7) -0.002(7) C47' 0.075(9) 0.094(9) 0.056(8) -0.023(6) 0.022(7) -0.015(7) C48 0.083(10) 0.124(11) 0.157(13) -0.050(10) -0.034(9) 0.030(9) C48' 0.090(9) 0.049(7) 0.068(7) 0.002(6) -0.002(6) 0.012(6) C49' 0.053(8) 0.080(8) 0.066(8) -0.003(6) -0.002(6) 0.027(6) C49 0.070(8) 0.051(7) 0.086(8) -0.015(6) 0.001(6) -0.001(6) C50 0.080(8) 0.055(7) 0.079(9) 0.017(6) -0.002(7) 0.007(6) C50' 0.039(7) 0.089(9) 0.125(11) -0.034(8) 0.005(7) -0.004(6) C51 0.069(8) 0.040(6) 0.078(8) 0.013(6) 0.009(6) 0.008(5) C51' 0.065(8) 0.066(8) 0.069(7) -0.023(6) 0.004(6) -0.002(6) C52 0.082(8) 0.055(7) 0.077(8) 0.004(6) 0.032(6) -0.028(6) C52' 0.076(9) 0.096(10) 0.143(12) -0.037(8) 0.064(8) -0.023(8) C53' 0.039(7) 0.062(8) 0.078(8) -0.001(6) 0.023(6) 0.019(6) C53 0.074(9) 0.036(6) 0.052(7) -0.001(5) 0.001(7) 0.008(6) C54 0.051(7) 0.063(7) 0.051(7) 0.007(6) 0.009(6) -0.010(6) C54' 0.051(8) 0.075(9) 0.071(8) 0.006(6) 0.010(6) 0.003(7) C55 0.088(10) 0.058(7) 0.065(8) -0.012(6) 0.000(7) -0.016(7) C55' 0.103(11) 0.069(9) 0.081(9) 0.017(7) 0.002(8) -0.039(8) C56' 0.133(16) 0.106(14) 0.111(13) 0.002(10) -0.001(12) 0.001(13) C56 0.099(11) 0.097(11) 0.062(9) 0.016(8) -0.024(8) -0.051(9) C57' 0.23(2) 0.108(14) 0.060(9) -0.001(9) 0.029(12) -0.093(15) C57 0.077(10) 0.122(12) 0.088(11) 0.016(9) -0.006(8) 0.015(9) C58 0.046(8) 0.146(12) 0.066(8) -0.009(8) -0.002(6) 0.009(8) C58' 0.091(11) 0.151(15) 0.124(12) -0.035(11) 0.048(9) -0.052(11) C59' 0.072(9) 0.104(10) 0.078(9) -0.005(7) 0.012(7) -0.035(8) C59 0.058(8) 0.085(9) 0.074(8) 0.002(7) 0.012(7) -0.003(7) C60 0.053(7) 0.036(6) 0.046(7) -0.012(5) 0.021(6) 0.001(5) C60' 0.043(7) 0.072(9) 0.076(9) 0.018(7) -0.002(6) -0.006(6) C61 0.048(7) 0.048(7) 0.064(8) 0.008(5) 0.013(6) 0.001(5) C61' 0.061(8) 0.072(8) 0.046(7) -0.003(6) 0.005(6) -0.020(7) C62' 0.079(10) 0.077(9) 0.085(9) 0.021(7) 0.024(7) 0.008(7) C62 0.051(8) 0.064(7) 0.069(8) -0.004(6) 0.001(6) 0.002(6) C63' 0.071(11) 0.143(14) 0.107(12) -0.001(10) 0.029(9) -0.023(10) C63 0.079(10) 0.086(10) 0.103(11) -0.022(8) -0.004(9) -0.011(8) C64' 0.051(10) 0.197(19) 0.075(10) -0.033(11) 0.015(8) -0.036(11) C64 0.045(8) 0.107(11) 0.138(13) -0.006(9) 0.011(9) 0.004(8) C65' 0.086(12) 0.110(13) 0.114(12) -0.026(10) 0.000(9) 0.002(10) C65 0.084(11) 0.106(11) 0.103(11) -0.027(8) 0.027(9) 0.009(8) C66' 0.055(8) 0.085(9) 0.084(9) -0.007(7) 0.010(7) 0.010(7) C66 0.039(7) 0.107(10) 0.072(8) -0.015(7) 0.013(6) 0.003(6) C67 0.075(8) 0.066(7) 0.072(8) 0.002(6) 0.021(6) 0.011(6) C67' 0.117(12) 0.141(13) 0.140(12) -0.029(10) 0.083(10) -0.044(9) C68 0.044(7) 0.062(7) 0.073(8) -0.009(6) 0.013(6) -0.017(5) C68' 0.064(8) 0.055(7) 0.076(8) 0.010(6) 0.016(6) -0.002(6) C69' 0.066(8) 0.076(8) 0.067(8) 0.019(6) 0.013(6) -0.009(6) C69 0.044(7) 0.062(7) 0.086(8) -0.009(6) 0.022(6) -0.006(6) C70 0.056(7) 0.059(7) 0.075(7) -0.004(6) 0.038(6) 0.000(6) C70' 0.068(8) 0.059(7) 0.067(8) 0.011(6) 0.012(6) -0.006(6) C71' 0.067(8) 0.078(8) 0.092(9) 0.023(7) -0.004(7) 0.027(6) C71 0.063(8) 0.071(8) 0.101(9) -0.020(7) 0.014(7) 0.018(6) C72 0.044(7) 0.067(8) 0.042(6) -0.009(6) 0.008(5) 0.003(6) C72' 0.061(8) 0.059(7) 0.070(8) -0.005(6) 0.018(7) -0.025(6) C73 0.061(8) 0.056(7) 0.062(7) -0.005(6) 0.023(6) 0.008(6) C73' 0.066(8) 0.061(8) 0.065(8) -0.010(6) 0.009(7) 0.002(6) C74 0.063(8) 0.096(10) 0.070(8) 0.007(7) 0.026(6) 0.004(7) C74' 0.092(10) 0.081(9) 0.086(9) -0.005(7) 0.034(8) -0.012(8) C75' 0.094(11) 0.151(14) 0.116(13) 0.004(11) 0.052(11) -0.039(9) C75 0.120(13) 0.073(10) 0.109(11) 0.013(8) 0.009(10) 0.022(10) C76' 0.115(16) 0.28(3) 0.096(16) 0.035(17) 0.029(13) -0.010(16) C76 0.083(11) 0.104(12) 0.093(10) -0.010(9) -0.021(8) 0.038(9) C77' 0.14(2) 0.31(3) 0.115(17) -0.041(17) 0.049(15) 0.030(18) C77 0.066(9) 0.086(10) 0.099(10) -0.009(8) 0.005(8) -0.007(8) C78' 0.086(12) 0.198(17) 0.121(14) -0.072(12) 0.026(10) -0.017(11) C78 0.055(8) 0.067(8) 0.105(10) 0.010(7) 0.000(7) 0.012(7) B3' 0.076(10) 0.087(11) 0.065(9) 0.000(8) 0.017(8) -0.002(8) B3 0.079(10) 0.045(8) 0.068(9) 0.001(6) 0.019(7) 0.011(7) B4 0.093(11) 0.096(11) 0.034(7) -0.001(7) 0.011(7) 0.021(9) B4' 0.113(14) 0.099(12) 0.064(10) -0.002(8) 0.034(10) -0.027(10) B5 0.071(9) 0.063(9) 0.057(9) -0.008(7) -0.002(7) -0.002(7) B5' 0.102(13) 0.113(13) 0.044(8) -0.002(8) 0.013(8) -0.037(10) B6 0.065(9) 0.074(9) 0.056(8) 0.017(7) 0.002(7) 0.006(7) B6' 0.073(10) 0.073(10) 0.081(10) 0.001(8) 0.020(8) -0.022(8) B7 0.067(9) 0.047(8) 0.071(9) -0.010(6) 0.041(7) 0.006(6) B7' 0.065(9) 0.099(11) 0.054(9) 0.015(8) 0.012(7) 0.018(8) B8 0.106(12) 0.048(9) 0.086(11) -0.004(7) 0.013(9) 0.021(8) B8' 0.112(13) 0.114(13) 0.063(10) -0.001(9) 0.050(10) -0.017(10) B9' 0.099(13) 0.126(14) 0.057(9) 0.000(9) 0.040(9) -0.014(10) B9 0.067(10) 0.098(11) 0.078(10) 0.000(8) -0.001(8) 0.016(8) B10 0.071(10) 0.103(11) 0.047(8) 0.012(7) -0.010(7) -0.015(8) B10' 0.080(11) 0.107(12) 0.070(10) 0.007(9) 0.007(8) -0.037(9) B11 0.057(9) 0.097(10) 0.044(8) 0.010(7) 0.016(6) -0.004(7) B11' 0.058(9) 0.091(11) 0.087(11) 0.003(8) -0.002(8) -0.022(8) B12 0.052(8) 0.093(11) 0.068(9) 0.009(8) 0.008(7) -0.004(8) B12' 0.070(10) 0.133(14) 0.065(10) 0.007(9) 0.041(8) 0.003(10) B23 0.047(7) 0.048(7) 0.057(8) -0.001(6) 0.009(6) -0.001(6) B23' 0.051(8) 0.062(8) 0.059(8) 0.008(6) 0.007(6) 0.015(6) B24' 0.111(13) 0.080(11) 0.085(11) -0.016(8) 0.039(10) -0.048(10) B24 0.079(10) 0.087(10) 0.053(9) 0.020(7) 0.036(7) 0.026(8) B25' 0.047(9) 0.105(12) 0.104(12) 0.012(9) 0.016(8) 0.011(8) B25 0.122(14) 0.056(9) 0.093(11) -0.015(8) 0.052(10) 0.028(9) B26' 0.052(9) 0.070(9) 0.081(10) 0.015(7) 0.000(7) 0.010(7) B26 0.071(10) 0.040(8) 0.117(13) 0.003(8) 0.018(9) 0.009(7) B27 0.080(10) 0.039(7) 0.061(8) 0.005(6) 0.014(7) 0.016(7) B27' 0.031(7) 0.126(12) 0.043(8) 0.025(7) 0.007(6) 0.004(7) B28 0.058(9) 0.081(10) 0.085(10) 0.020(8) 0.002(8) -0.002(8) B28' 0.063(9) 0.040(7) 0.099(11) 0.013(7) 0.023(8) -0.007(7) B29' 0.060(9) 0.103(11) 0.064(9) 0.009(8) 0.024(7) -0.015(8) B29 0.113(14) 0.120(14) 0.096(13) 0.020(10) 0.032(11) 0.046(11) B30' 0.058(9) 0.097(11) 0.090(11) -0.004(9) 0.041(8) 0.011(8) B30 0.084(12) 0.052(9) 0.167(16) 0.039(10) 0.037(11) 0.015(8) B31 0.070(10) 0.067(9) 0.085(11) 0.037(8) 0.020(8) 0.020(7) B31' 0.055(9) 0.084(10) 0.062(9) -0.005(7) 0.023(7) 0.002(7) B32' 0.053(9) 0.085(10) 0.081(10) 0.017(8) 0.022(7) -0.003(7) B32 0.058(9) 0.121(13) 0.069(10) 0.012(9) 0.001(8) 0.018(9) O1 0.191(12) 0.154(11) 0.162(11) -0.020(9) 0.025(9) -0.001(9) C81 0.140(13) 0.131(13) 0.147(13) 0.012(9) 0.052(9) 0.022(9) C82 0.116(12) 0.137(12) 0.102(12) -0.006(9) 0.024(9) -0.017(9) C83 0.145(13) 0.092(12) 0.127(12) -0.002(9) 0.019(9) 0.000(9) C84 0.145(14) 0.157(14) 0.159(14) 0.001(9) 0.039(10) -0.009(10) O2 0.110(9) 0.110(9) 0.103(9) -0.003(7) 0.025(7) -0.021(7) C91 0.075(10) 0.055(9) 0.083(10) 0.005(8) 0.022(8) -0.011(8) C92 0.62(7) 0.61(7) 0.62(7) -0.001(10) 0.095(14) -0.011(10) C93 0.218(19) 0.199(18) 0.223(19) -0.004(10) 0.048(10) -0.001(10) C94 0.209(19) 0.187(18) 0.232(19) 0.004(10) 0.020(10) -0.002(10) O3 0.292(18) 0.278(17) 0.289(17) -0.002(10) 0.046(10) 0.004(10) C101 0.215(19) 0.220(19) 0.218(19) 0.001(10) 0.058(10) -0.021(10) C102 0.23(2) 0.24(2) 0.24(2) 0.015(10) 0.031(10) -0.007(10) C103 0.151(14) 0.153(14) 0.148(14) 0.007(9) 0.012(9) 0.015(9) C104 0.22(2) 0.23(2) 0.22(2) 0.003(10) 0.047(10) -0.003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 1.959(8) . ? Zr1 N5 1.974(8) . ? Zr1 C2 2.339(9) . ? Zr1 C16 2.457(11) . ? Zr1 C17 2.465(11) . ? Zr1 C18 2.526(10) . ? Zr1 C15 2.535(10) . ? Zr1 C14 2.544(11) . ? Zr1' N5' 1.958(9) . ? Zr1' N1' 1.985(7) . ? Zr1' C2' 2.342(9) . ? Zr1' C17' 2.449(10) . ? Zr1' C16' 2.454(10) . ? Zr1' C18' 2.479(9) . ? Zr1' C14' 2.518(10) . ? Zr1' C15' 2.547(10) . ? Zr2 N4 1.933(8) . ? Zr2 N8 1.956(8) . ? Zr2 C22 2.343(9) . ? Zr2 C36 2.479(11) . ? Zr2 C37 2.487(10) . ? Zr2 C38 2.515(10) . ? Zr2 C34 2.524(9) . ? Zr2 C35 2.545(10) . ? Zr2' N8' 1.947(8) . ? Zr2' N4' 1.952(8) . ? Zr2' C22' 2.340(9) . ? Zr2' C37' 2.466(11) . ? Zr2' C36' 2.468(10) . ? Zr2' C35' 2.472(10) . ? Zr2' C34' 2.503(10) . ? Zr2' C38' 2.504(10) . ? N1' C41' 1.286(10) . ? N1 C41 1.299(11) . ? N2' C41' 1.348(11) . ? N2' C49' 1.448(11) . ? N2' C48' 1.459(10) . ? N2 C41 1.348(11) . ? N2 C49 1.454(11) . ? N2 C48 1.498(12) . ? N3' C53' 1.339(11) . ? N3' C52' 1.444(11) . ? N3' C51' 1.488(11) . ? N3 C53 1.369(11) . ? N3 C51 1.463(11) . ? N3 C52 1.513(11) . ? N4' C53' 1.293(11) . ? N4 C53 1.309(11) . ? N5' C60' 1.317(12) . ? N5 C60 1.313(10) . ? N6' C60' 1.329(12) . ? N6' C67' 1.449(12) . ? N6' C68' 1.473(11) . ? N6 C60 1.388(10) . ? N6 C67 1.430(10) . ? N6 C68 1.431(10) . ? N7' C72' 1.382(12) . ? N7' C70' 1.447(11) . ? N7' C71' 1.500(11) . ? N7 C72 1.354(10) . ? N7 C70 1.443(10) . ? N7 C71 1.478(10) . ? N8' C72' 1.299(12) . ? N8 C72 1.309(10) . ? C1 C11 1.557(13) . ? C1 B4 1.677(14) . ? C1 B3 1.709(13) . ? C1 C2 1.719(11) . ? C1 B6 1.754(14) . ? C1 B5 1.761(15) . ? C1' C11' 1.569(14) . ? C1' B3' 1.666(16) . ? C1' B4' 1.689(17) . ? C1' B5' 1.691(16) . ? C1' C2' 1.693(12) . ? C1' B6' 1.721(15) . ? C2 B11 1.720(14) . ? C2 B3 1.735(14) . ? C2 B7 1.736(14) . ? C2 B6 1.736(14) . ? C2' B7' 1.708(15) . ? C2' B3' 1.722(15) . ? C2' B6' 1.731(15) . ? C2' B11' 1.731(15) . ? C11' C14' 1.529(15) . ? C11' C13' 1.546(13) . ? C11' C12' 1.561(13) . ? C11 C12 1.510(12) . ? C11 C14 1.512(14) . ? C11 C13 1.589(13) . ? C14 C18 1.360(14) . ? C14 C15 1.462(15) . ? C14' C18' 1.400(12) . ? C14' C15' 1.428(14) . ? C15' C16' 1.380(14) . ? C15 C16 1.387(15) . ? C16' C17' 1.388(13) . ? C16 C17 1.400(16) . ? C17' C18' 1.385(13) . ? C17 C18 1.399(14) . ? C21 C31 1.610(13) . ? C21 B23 1.669(13) . ? C21 C22 1.699(12) . ? C21 B25 1.719(15) . ? C21 B24 1.728(15) . ? C21 B26 1.728(15) . ? C21' C31' 1.565(13) . ? C21' B26' 1.713(15) . ? C21' B25' 1.717(15) . ? C21' C22' 1.731(12) . ? C21' B24' 1.732(15) . ? C21' B23' 1.753(14) . ? C22 B23 1.672(13) . ? C22 B27 1.685(14) . ? C22 B26 1.727(14) . ? C22 B31 1.754(14) . ? C22' B23' 1.704(14) . ? C22' B27' 1.716(13) . ? C22' B26' 1.732(14) . ? C22' B31' 1.764(14) . ? C31 C34 1.507(13) . ? C31 C32 1.549(12) . ? C31 C33 1.578(14) . ? C31' C34' 1.516(13) . ? C31' C33' 1.560(14) . ? C31' C32' 1.583(14) . ? C34 C35 1.408(12) . ? C34 C38 1.425(13) . ? C34' C38' 1.399(13) . ? C34' C35' 1.407(13) . ? C35 C36 1.408(14) . ? C35' C36' 1.389(14) . ? C36' C37' 1.372(14) . ? C36 C37 1.418(14) . ? C37' C38' 1.370(13) . ? C37 C38 1.422(14) . ? C41 C42 1.512(13) . ? C41' C42' 1.481(12) . ? C42 C43 1.388(13) . ? C42 C47 1.420(12) . ? C42' C43' 1.392(12) . ? C42' C47' 1.408(12) . ? C43' C44' 1.377(13) . ? C43 C44 1.371(14) . ? C44 C45 1.418(15) . ? C44' C45' 1.387(14) . ? C45' C46' 1.387(14) . ? C45 C46 1.358(16) . ? C46' C47' 1.357(13) . ? C46 C47 1.384(14) . ? C49' C50' 1.517(12) . ? C49 C50 1.501(11) . ? C50 C51 1.540(12) . ? C50' C51' 1.514(12) . ? C53' C54' 1.492(13) . ? C53 C54 1.526(13) . ? C54 C55 1.345(12) . ? C54 C59 1.386(13) . ? C54' C55' 1.367(14) . ? C54' C59' 1.393(14) . ? C55 C56 1.388(14) . ? C55' C56' 1.359(18) . ? C56' C57' 1.35(2) . ? C56 C57 1.383(15) . ? C57' C58' 1.425(19) . ? C57 C58 1.364(14) . ? C58 C59 1.378(13) . ? C58' C59' 1.415(15) . ? C60 C61 1.497(12) . ? C60' C61' 1.498(14) . ? C61 C66 1.367(12) . ? C61 C62 1.393(12) . ? C61' C66' 1.362(13) . ? C61' C62' 1.409(13) . ? C62' C63' 1.380(15) . ? C62 C63 1.354(14) . ? C63' C64' 1.380(17) . ? C63 C64 1.379(15) . ? C64' C65' 1.405(16) . ? C64 C65 1.390(14) . ? C65' C66' 1.349(16) . ? C65 C66 1.371(14) . ? C68 C69 1.503(11) . ? C68' C69' 1.527(11) . ? C69' C70' 1.497(12) . ? C69 C70 1.526(11) . ? C72 C73 1.468(13) . ? C72' C73' 1.500(13) . ? C73 C74 1.358(13) . ? C73 C78 1.412(13) . ? C73' C78' 1.368(15) . ? C73' C74' 1.379(13) . ? C74 C75 1.467(15) . ? C74' C75' 1.382(15) . ? C75' C76' 1.30(2) . ? C75 C76 1.354(16) . ? C76' C77' 1.38(2) . ? C76 C77 1.359(15) . ? C77' C78' 1.45(2) . ? C77 C78 1.350(13) . ? B3' B4' 1.741(17) . ? B3' B7' 1.747(17) . ? B3' B8' 1.805(19) . ? B3 B4 1.743(17) . ? B3 B8 1.758(18) . ? B3 B7 1.775(16) . ? B4 B8 1.735(17) . ? B4 B5 1.769(17) . ? B4 B9 1.774(18) . ? B4' B5' 1.732(19) . ? B4' B9' 1.759(19) . ? B4' B8' 1.76(2) . ? B5 B10 1.722(17) . ? B5 B6 1.770(16) . ? B5 B9 1.775(17) . ? B5' B9' 1.74(2) . ? B5' B6' 1.746(18) . ? B5' B10' 1.769(18) . ? B6 B10 1.786(17) . ? B6 B11 1.792(17) . ? B6' B11' 1.758(18) . ? B6' B10' 1.789(18) . ? B7 B11 1.758(16) . ? B7 B8 1.777(17) . ? B7 B12 1.791(16) . ? B7' B8' 1.711(17) . ? B7' B12' 1.755(17) . ? B7' B11' 1.764(17) . ? B8 B9 1.793(18) . ? B8 B12 1.816(17) . ? B8' B9' 1.759(19) . ? B8' B12' 1.789(19) . ? B9' B12' 1.691(18) . ? B9' B10' 1.761(19) . ? B9 B12 1.783(17) . ? B9 B10 1.792(17) . ? B10 B12 1.824(18) . ? B10 B11 1.825(17) . ? B10' B12' 1.725(19) . ? B10' B11' 1.742(18) . ? B11 B12 1.750(16) . ? B11' B12' 1.698(18) . ? B23 B27 1.754(15) . ? B23 B24 1.794(15) . ? B23 B28 1.821(16) . ? B23' B27' 1.734(16) . ? B23' B28' 1.773(16) . ? B23' B24' 1.784(17) . ? B24' B29' 1.713(18) . ? B24' B28' 1.736(18) . ? B24' B25' 1.780(19) . ? B24 B28 1.765(17) . ? B24 B29 1.799(18) . ? B24 B25 1.830(18) . ? B25' B29' 1.764(18) . ? B25' B26' 1.781(18) . ? B25' B30' 1.791(18) . ? B25 B30 1.760(19) . ? B25 B29 1.78(2) . ? B25 B26 1.790(18) . ? B26' B30' 1.774(17) . ? B26' B31' 1.780(16) . ? B26 B31 1.725(17) . ? B26 B30 1.740(19) . ? B27 B31 1.764(16) . ? B27 B32 1.781(16) . ? B27 B28 1.823(17) . ? B27' B31' 1.737(16) . ? B27' B28' 1.740(16) . ? B27' B32' 1.789(16) . ? B28 B29 1.756(19) . ? B28 B32 1.795(18) . ? B28' B29' 1.758(17) . ? B28' B32' 1.777(17) . ? B29' B30' 1.753(17) . ? B29' B32' 1.767(17) . ? B29 B32 1.768(19) . ? B29 B30 1.81(2) . ? B30' B32' 1.760(17) . ? B30' B31' 1.783(17) . ? B30 B31 1.711(18) . ? B30 B32 1.78(2) . ? B31 B32 1.805(17) . ? B31' B32' 1.781(16) . ? O1 C81 1.409(9) . ? O1 C84 1.441(9) . ? C81 C82 1.525(9) . ? C82 C83 1.514(9) . ? C83 C84 1.532(9) . ? O2 C91 1.407(8) . ? O2 C94 1.448(9) . ? C91 C92 1.549(9) . ? C92 C93 1.533(9) . ? C93 C94 1.518(9) . ? O3 C101 1.410(9) . ? O3 C104 1.431(9) . ? C101 C102 1.538(9) . ? C102 C103 1.527(9) . ? C103 C104 1.520(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 N5 106.4(3) . . ? N1 Zr1 C2 105.3(3) . . ? N5 Zr1 C2 107.8(3) . . ? N1 Zr1 C16 90.1(4) . . ? N5 Zr1 C16 124.8(5) . . ? C2 Zr1 C16 118.0(4) . . ? N1 Zr1 C17 115.2(5) . . ? N5 Zr1 C17 95.4(4) . . ? C2 Zr1 C17 124.7(4) . . ? C16 Zr1 C17 33.1(4) . . ? N1 Zr1 C18 144.0(4) . . ? N5 Zr1 C18 95.5(3) . . ? C2 Zr1 C18 94.5(4) . . ? C16 Zr1 C18 53.9(4) . . ? C17 Zr1 C18 32.5(3) . . ? N1 Zr1 C15 97.7(4) . . ? N5 Zr1 C15 147.5(4) . . ? C2 Zr1 C15 85.9(4) . . ? C16 Zr1 C15 32.2(4) . . ? C17 Zr1 C15 53.9(4) . . ? C18 Zr1 C15 53.3(4) . . ? N1 Zr1 C14 130.2(4) . . ? N5 Zr1 C14 122.1(4) . . ? C2 Zr1 C14 71.8(4) . . ? C16 Zr1 C14 54.4(4) . . ? C17 Zr1 C14 53.6(4) . . ? C18 Zr1 C14 31.1(3) . . ? C15 Zr1 C14 33.5(3) . . ? N5' Zr1' N1' 104.8(3) . . ? N5' Zr1' C2' 108.6(3) . . ? N1' Zr1' C2' 106.8(3) . . ? N5' Zr1' C17' 113.6(4) . . ? N1' Zr1' C17' 95.8(3) . . ? C2' Zr1' C17' 124.4(4) . . ? N5' Zr1' C16' 89.9(4) . . ? N1' Zr1' C16' 125.4(4) . . ? C2' Zr1' C16' 117.8(4) . . ? C17' Zr1' C16' 32.9(3) . . ? N5' Zr1' C18' 143.2(4) . . ? N1' Zr1' C18' 95.5(3) . . ? C2' Zr1' C18' 93.9(4) . . ? C17' Zr1' C18' 32.6(3) . . ? C16' Zr1' C18' 53.6(4) . . ? N5' Zr1' C14' 130.2(4) . . ? N1' Zr1' C14' 123.5(4) . . ? C2' Zr1' C14' 70.9(3) . . ? C17' Zr1' C14' 54.5(4) . . ? C16' Zr1' C14' 53.7(4) . . ? C18' Zr1' C14' 32.5(3) . . ? N5' Zr1' C15' 98.2(4) . . ? N1' Zr1' C15' 148.1(4) . . ? C2' Zr1' C15' 85.9(4) . . ? C17' Zr1' C15' 54.2(4) . . ? C16' Zr1' C15' 32.0(3) . . ? C18' Zr1' C15' 53.7(4) . . ? C14' Zr1' C15' 32.8(3) . . ? N4 Zr2 N8 106.0(3) . . ? N4 Zr2 C22 110.0(3) . . ? N8 Zr2 C22 103.4(3) . . ? N4 Zr2 C36 117.4(4) . . ? N8 Zr2 C36 91.4(4) . . ? C22 Zr2 C36 123.7(4) . . ? N4 Zr2 C37 93.1(4) . . ? N8 Zr2 C37 121.3(4) . . ? C22 Zr2 C37 121.3(4) . . ? C36 Zr2 C37 33.2(3) . . ? N4 Zr2 C38 101.5(3) . . ? N8 Zr2 C38 143.8(3) . . ? C22 Zr2 C38 88.6(4) . . ? C36 Zr2 C38 54.6(4) . . ? C37 Zr2 C38 33.0(3) . . ? N4 Zr2 C34 133.3(3) . . ? N8 Zr2 C34 119.2(3) . . ? C22 Zr2 C34 71.6(3) . . ? C36 Zr2 C34 54.2(4) . . ? C37 Zr2 C34 54.6(4) . . ? C38 Zr2 C34 32.9(3) . . ? N4 Zr2 C35 147.2(3) . . ? N8 Zr2 C35 91.1(3) . . ? C22 Zr2 C35 92.3(3) . . ? C36 Zr2 C35 32.5(3) . . ? C37 Zr2 C35 54.2(4) . . ? C38 Zr2 C35 53.9(3) . . ? C34 Zr2 C35 32.2(3) . . ? N8' Zr2' N4' 106.1(3) . . ? N8' Zr2' C22' 106.7(3) . . ? N4' Zr2' C22' 105.4(3) . . ? N8' Zr2' C37' 94.3(4) . . ? N4' Zr2' C37' 116.3(4) . . ? C22' Zr2' C37' 125.5(4) . . ? N8' Zr2' C36' 123.2(4) . . ? N4' Zr2' C36' 92.2(4) . . ? C22' Zr2' C36' 119.6(4) . . ? C37' Zr2' C36' 32.3(3) . . ? N8' Zr2' C35' 146.8(4) . . ? N4' Zr2' C35' 98.7(4) . . ? C22' Zr2' C35' 87.1(4) . . ? C37' Zr2' C35' 54.4(4) . . ? C36' Zr2' C35' 32.6(3) . . ? N8' Zr2' C34' 122.3(4) . . ? N4' Zr2' C34' 130.4(4) . . ? C22' Zr2' C34' 72.3(3) . . ? C37' Zr2' C34' 54.3(4) . . ? C36' Zr2' C34' 53.8(4) . . ? C35' Zr2' C34' 32.8(3) . . ? N8' Zr2' C38' 94.4(3) . . ? N4' Zr2' C38' 144.7(4) . . ? C22' Zr2' C38' 95.4(4) . . ? C37' Zr2' C38' 32.0(3) . . ? C36' Zr2' C38' 52.6(4) . . ? C35' Zr2' C38' 53.5(4) . . ? C34' Zr2' C38' 32.4(3) . . ? C41' N1' Zr1' 159.8(7) . . ? C41 N1 Zr1 159.4(8) . . ? C41' N2' C49' 120.7(9) . . ? C41' N2' C48' 125.4(9) . . ? C49' N2' C48' 113.9(8) . . ? C41 N2 C49 124.6(9) . . ? C41 N2 C48 117.9(9) . . ? C49 N2 C48 115.1(9) . . ? C53' N3' C52' 114.6(9) . . ? C53' N3' C51' 125.3(9) . . ? C52' N3' C51' 115.1(9) . . ? C53 N3 C51 119.5(8) . . ? C53 N3 C52 125.8(9) . . ? C51 N3 C52 114.8(8) . . ? C53' N4' Zr2' 164.1(7) . . ? C53 N4 Zr2 160.8(7) . . ? C60' N5' Zr1' 155.9(8) . . ? C60 N5 Zr1 160.7(7) . . ? C60' N6' C67' 119.3(10) . . ? C60' N6' C68' 123.8(9) . . ? C67' N6' C68' 115.3(9) . . ? C60 N6 C67 123.4(8) . . ? C60 N6 C68 120.8(8) . . ? C67 N6 C68 115.8(8) . . ? C72' N7' C70' 119.4(8) . . ? C72' N7' C71' 123.8(9) . . ? C70' N7' C71' 116.8(8) . . ? C72 N7 C70 124.3(8) . . ? C72 N7 C71 117.5(8) . . ? C70 N7 C71 115.0(8) . . ? C72' N8' Zr2' 162.9(8) . . ? C72 N8 Zr2 159.8(7) . . ? C11 C1 B4 124.5(8) . . ? C11 C1 B3 116.9(8) . . ? B4 C1 B3 62.0(6) . . ? C11 C1 C2 116.5(8) . . ? B4 C1 C2 109.2(7) . . ? B3 C1 C2 60.8(6) . . ? C11 C1 B6 118.2(8) . . ? B4 C1 B6 110.9(8) . . ? B3 C1 B6 111.4(8) . . ? C2 C1 B6 60.0(6) . . ? C11 C1 B5 124.8(8) . . ? B4 C1 B5 61.9(7) . . ? B3 C1 B5 112.2(8) . . ? C2 C1 B5 108.2(7) . . ? B6 C1 B5 60.5(6) . . ? C11' C1' B3' 117.2(8) . . ? C11' C1' B4' 123.7(9) . . ? B3' C1' B4' 62.5(7) . . ? C11' C1' B5' 122.9(9) . . ? B3' C1' B5' 113.2(10) . . ? B4' C1' B5' 61.7(8) . . ? C11' C1' C2' 116.4(8) . . ? B3' C1' C2' 61.7(6) . . ? B4' C1' C2' 110.8(9) . . ? B5' C1' C2' 109.9(8) . . ? C11' C1' B6' 116.3(9) . . ? B3' C1' B6' 113.5(9) . . ? B4' C1' B6' 112.5(9) . . ? B5' C1' B6' 61.5(7) . . ? C2' C1' B6' 60.9(6) . . ? C1 C2 B11 109.8(7) . . ? C1 C2 B3 59.3(5) . . ? B11 C2 B3 111.0(8) . . ? C1 C2 B7 108.8(7) . . ? B11 C2 B7 61.2(6) . . ? B3 C2 B7 61.5(6) . . ? C1 C2 B6 61.0(6) . . ? B11 C2 B6 62.5(6) . . ? B3 C2 B6 111.0(7) . . ? B7 C2 B6 112.3(8) . . ? C1 C2 Zr1 117.9(6) . . ? B11 C2 Zr1 119.8(6) . . ? B3 C2 Zr1 123.9(6) . . ? B7 C2 Zr1 126.4(6) . . ? B6 C2 Zr1 112.4(6) . . ? C1' C2' B7' 106.1(8) . . ? C1' C2' B3' 58.4(6) . . ? B7' C2' B3' 61.2(7) . . ? C1' C2' B6' 60.4(6) . . ? B7' C2' B6' 110.7(8) . . ? B3' C2' B6' 110.3(8) . . ? C1' C2' B11' 107.5(8) . . ? B7' C2' B11' 61.7(7) . . ? B3' C2' B11' 111.4(8) . . ? B6' C2' B11' 61.0(7) . . ? C1' C2' Zr1' 119.0(6) . . ? B7' C2' Zr1' 120.1(6) . . ? B3' C2' Zr1' 112.1(6) . . ? B6' C2' Zr1' 124.7(7) . . ? B11' C2' Zr1' 127.9(7) . . ? C14' C11' C13' 109.4(9) . . ? C14' C11' C12' 109.8(10) . . ? C13' C11' C12' 106.3(9) . . ? C14' C11' C1' 109.1(8) . . ? C13' C11' C1' 111.1(10) . . ? C12' C11' C1' 111.1(9) . . ? C12 C11 C14 110.8(10) . . ? C12 C11 C1 111.1(9) . . ? C14 C11 C1 110.9(8) . . ? C12 C11 C13 106.6(9) . . ? C14 C11 C13 106.5(10) . . ? C1 C11 C13 110.7(9) . . ? C18 C14 C15 107.0(12) . . ? C18 C14 C11 128.4(14) . . ? C15 C14 C11 124.5(13) . . ? C18 C14 Zr1 73.7(7) . . ? C15 C14 Zr1 72.9(6) . . ? C11 C14 Zr1 121.9(7) . . ? C18' C14' C15' 106.9(11) . . ? C18' C14' C11' 127.1(12) . . ? C15' C14' C11' 125.7(11) . . ? C18' C14' Zr1' 72.2(6) . . ? C15' C14' Zr1' 74.7(6) . . ? C11' C14' Zr1' 123.4(7) . . ? C16' C15' C14' 106.2(11) . . ? C16' C15' Zr1' 70.3(6) . . ? C14' C15' Zr1' 72.5(6) . . ? C16 C15 C14 106.7(12) . . ? C16 C15 Zr1 70.8(7) . . ? C14 C15 Zr1 73.6(6) . . ? C15' C16' C17' 110.8(12) . . ? C15' C16' Zr1' 77.7(7) . . ? C17' C16' Zr1' 73.3(6) . . ? C15 C16 C17 108.7(13) . . ? C15 C16 Zr1 77.0(7) . . ? C17 C16 Zr1 73.8(7) . . ? C18' C17' C16' 106.6(10) . . ? C18' C17' Zr1' 74.9(6) . . ? C16' C17' Zr1' 73.8(6) . . ? C18 C17 C16 107.6(12) . . ? C18 C17 Zr1 76.1(7) . . ? C16 C17 Zr1 73.2(7) . . ? C17' C18' C14' 109.4(11) . . ? C17' C18' Zr1' 72.5(6) . . ? C14' C18' Zr1' 75.3(6) . . ? C14 C18 C17 109.8(12) . . ? C14 C18 Zr1 75.1(7) . . ? C17 C18 Zr1 71.3(7) . . ? C31 C21 B23 116.1(7) . . ? C31 C21 C22 114.5(8) . . ? B23 C21 C22 59.5(6) . . ? C31 C21 B25 123.3(8) . . ? B23 C21 B25 114.9(8) . . ? C22 C21 B25 111.5(8) . . ? C31 C21 B24 121.8(8) . . ? B23 C21 B24 63.7(6) . . ? C22 C21 B24 112.3(7) . . ? B25 C21 B24 64.1(7) . . ? C31 C21 B26 116.9(9) . . ? B23 C21 B26 111.3(8) . . ? C22 C21 B26 60.5(6) . . ? B25 C21 B26 62.6(7) . . ? B24 C21 B26 115.4(8) . . ? C31' C21' B26' 118.7(8) . . ? C31' C21' B25' 123.8(9) . . ? B26' C21' B25' 62.5(7) . . ? C31' C21' C22' 115.3(7) . . ? B26' C21' C22' 60.4(6) . . ? B25' C21' C22' 111.3(8) . . ? C31' C21' B24' 125.3(8) . . ? B26' C21' B24' 110.8(8) . . ? B25' C21' B24' 62.2(7) . . ? C22' C21' B24' 108.2(7) . . ? C31' C21' B23' 117.4(8) . . ? B26' C21' B23' 109.1(7) . . ? B25' C21' B23' 112.8(8) . . ? C22' C21' B23' 58.5(5) . . ? B24' C21' B23' 61.6(7) . . ? B23 C22 B27 63.0(6) . . ? B23 C22 C21 59.3(6) . . ? B27 C22 C21 108.1(8) . . ? B23 C22 B26 111.2(8) . . ? B27 C22 B26 110.1(8) . . ? C21 C22 B26 60.6(6) . . ? B23 C22 B31 112.5(8) . . ? B27 C22 B31 61.7(6) . . ? C21 C22 B31 107.1(7) . . ? B26 C22 B31 59.4(6) . . ? B23 C22 Zr2 117.3(6) . . ? B27 C22 Zr2 122.7(6) . . ? C21 C22 Zr2 119.8(6) . . ? B26 C22 Zr2 119.6(7) . . ? B31 C22 Zr2 123.6(6) . . ? B23' C22' B27' 60.9(6) . . ? B23' C22' C21' 61.4(6) . . ? B27' C22' C21' 108.2(7) . . ? B23' C22' B26' 110.5(8) . . ? B27' C22' B26' 109.0(7) . . ? C21' C22' B26' 59.3(6) . . ? B23' C22' B31' 110.3(7) . . ? B27' C22' B31' 59.9(6) . . ? C21' C22' B31' 108.2(7) . . ? B26' C22' B31' 61.2(6) . . ? B23' C22' Zr2' 114.9(6) . . ? B27' C22' Zr2' 122.9(6) . . ? C21' C22' Zr2' 117.9(5) . . ? B26' C22' Zr2' 122.6(6) . . ? B31' C22' Zr2' 126.3(6) . . ? C34 C31 C32 110.0(9) . . ? C34 C31 C33 110.5(9) . . ? C32 C31 C33 106.9(10) . . ? C34 C31 C21 110.7(8) . . ? C32 C31 C21 109.3(8) . . ? C33 C31 C21 109.4(9) . . ? C34' C31' C33' 110.8(9) . . ? C34' C31' C21' 111.3(8) . . ? C33' C31' C21' 108.7(9) . . ? C34' C31' C32' 109.4(10) . . ? C33' C31' C32' 105.4(10) . . ? C21' C31' C32' 111.1(9) . . ? C35 C34 C38 108.0(10) . . ? C35 C34 C31 125.3(10) . . ? C38 C34 C31 126.3(10) . . ? C35 C34 Zr2 74.7(6) . . ? C38 C34 Zr2 73.2(6) . . ? C31 C34 Zr2 123.1(6) . . ? C38' C34' C35' 106.0(10) . . ? C38' C34' C31' 127.5(12) . . ? C35' C34' C31' 126.3(12) . . ? C38' C34' Zr2' 73.8(6) . . ? C35' C34' Zr2' 72.4(6) . . ? C31' C34' Zr2' 122.5(7) . . ? C34 C35 C36 108.2(10) . . ? C34 C35 Zr2 73.1(5) . . ? C36 C35 Zr2 71.1(6) . . ? C36' C35' C34' 107.2(11) . . ? C36' C35' Zr2' 73.5(6) . . ? C34' C35' Zr2' 74.8(6) . . ? C37' C36' C35' 109.7(11) . . ? C37' C36' Zr2' 73.8(6) . . ? C35' C36' Zr2' 73.8(6) . . ? C35 C36 C37 108.5(11) . . ? C35 C36 Zr2 76.3(6) . . ? C37 C36 Zr2 73.7(6) . . ? C38' C37' C36' 107.0(12) . . ? C38' C37' Zr2' 75.5(6) . . ? C36' C37' Zr2' 74.0(7) . . ? C36 C37 C38 107.5(11) . . ? C36 C37 Zr2 73.1(6) . . ? C38 C37 Zr2 74.5(6) . . ? C37 C38 C34 107.7(10) . . ? C37 C38 Zr2 72.4(6) . . ? C34 C38 Zr2 73.9(5) . . ? C37' C38' C34' 110.0(11) . . ? C37' C38' Zr2' 72.5(6) . . ? C34' C38' Zr2' 73.8(6) . . ? N1 C41 N2 123.6(10) . . ? N1 C41 C42 119.7(10) . . ? N2 C41 C42 116.7(9) . . ? N1' C41' N2' 123.3(9) . . ? N1' C41' C42' 120.0(9) . . ? N2' C41' C42' 116.6(9) . . ? C43 C42 C47 118.6(10) . . ? C43 C42 C41 121.6(10) . . ? C47 C42 C41 119.6(10) . . ? C43' C42' C47' 118.3(10) . . ? C43' C42' C41' 119.8(9) . . ? C47' C42' C41' 121.8(9) . . ? C44' C43' C42' 120.8(11) . . ? C44 C43 C42 121.1(12) . . ? C43 C44 C45 119.5(12) . . ? C43' C44' C45' 120.0(11) . . ? C46' C45' C44' 119.4(12) . . ? C46 C45 C44 120.1(13) . . ? C47' C46' C45' 120.9(11) . . ? C45 C46 C47 120.8(13) . . ? C46 C47 C42 119.8(11) . . ? C46' C47' C42' 120.5(11) . . ? N2' C49' C50' 113.7(8) . . ? N2 C49 C50 112.1(9) . . ? C49 C50 C51 111.1(8) . . ? C51' C50' C49' 111.6(8) . . ? N3 C51 C50 113.9(8) . . ? N3' C51' C50' 113.4(8) . . ? N4' C53' N3' 125.2(10) . . ? N4' C53' C54' 119.7(10) . . ? N3' C53' C54' 115.2(10) . . ? N4 C53 N3 123.3(9) . . ? N4 C53 C54 122.3(9) . . ? N3 C53 C54 114.3(9) . . ? C55 C54 C59 119.3(10) . . ? C55 C54 C53 120.8(10) . . ? C59 C54 C53 119.8(10) . . ? C55' C54' C59' 117.6(11) . . ? C55' C54' C53' 122.5(11) . . ? C59' C54' C53' 119.7(10) . . ? C54 C55 C56 121.3(11) . . ? C56' C55' C54' 124.6(14) . . ? C57' C56' C55' 117.5(18) . . ? C57 C56 C55 119.6(12) . . ? C56' C57' C58' 123.4(17) . . ? C58 C57 C56 118.7(12) . . ? C57 C58 C59 121.4(12) . . ? C59' C58' C57' 115.8(14) . . ? C54' C59' C58' 121.2(13) . . ? C58 C59 C54 119.5(11) . . ? N5 C60 N6 122.4(9) . . ? N5 C60 C61 119.0(9) . . ? N6 C60 C61 118.6(8) . . ? N5' C60' N6' 122.0(11) . . ? N5' C60' C61' 119.1(10) . . ? N6' C60' C61' 118.8(11) . . ? C66 C61 C62 120.4(10) . . ? C66 C61 C60 118.9(10) . . ? C62 C61 C60 120.7(9) . . ? C66' C61' C62' 119.2(11) . . ? C66' C61' C60' 122.7(11) . . ? C62' C61' C60' 118.1(11) . . ? C63' C62' C61' 120.3(12) . . ? C63 C62 C61 119.0(11) . . ? C64' C63' C62' 119.2(14) . . ? C62 C63 C64 121.9(12) . . ? C63' C64' C65' 119.8(14) . . ? C63 C64 C65 118.4(12) . . ? C66' C65' C64' 120.3(14) . . ? C66 C65 C64 120.5(12) . . ? C65' C66' C61' 121.2(13) . . ? C61 C66 C65 119.9(11) . . ? N6 C68 C69 112.5(8) . . ? N6' C68' C69' 114.5(8) . . ? C70' C69' C68' 114.9(8) . . ? C68 C69 C70 113.4(8) . . ? N7 C70 C69 115.0(8) . . ? N7' C70' C69' 111.8(8) . . ? N8 C72 N7 122.3(9) . . ? N8 C72 C73 119.4(9) . . ? N7 C72 C73 118.3(9) . . ? N8' C72' N7' 122.4(10) . . ? N8' C72' C73' 122.6(10) . . ? N7' C72' C73' 115.0(10) . . ? C74 C73 C78 117.4(10) . . ? C74 C73 C72 120.9(10) . . ? C78 C73 C72 121.2(10) . . ? C78' C73' C74' 118.3(12) . . ? C78' C73' C72' 119.7(12) . . ? C74' C73' C72' 121.5(10) . . ? C73 C74 C75 123.0(11) . . ? C73' C74' C75' 124.1(12) . . ? C76' C75' C74' 116.9(16) . . ? C76 C75 C74 114.1(12) . . ? C75' C76' C77' 125(2) . . ? C75 C76 C77 124.3(12) . . ? C76' C77' C78' 118.0(19) . . ? C78 C77 C76 120.4(12) . . ? C73' C78' C77' 118.1(15) . . ? C77 C78 C73 120.8(11) . . ? C1' B3' C2' 59.9(6) . . ? C1' B3' B4' 59.4(7) . . ? C2' B3' B4' 107.0(9) . . ? C1' B3' B7' 105.6(9) . . ? C2' B3' B7' 59.0(7) . . ? B4' B3' B7' 105.0(10) . . ? C1' B3' B8' 106.1(9) . . ? C2' B3' B8' 105.5(9) . . ? B4' B3' B8' 59.6(8) . . ? B7' B3' B8' 57.6(7) . . ? C1 B3 C2 59.9(5) . . ? C1 B3 B4 58.1(6) . . ? C2 B3 B4 105.5(8) . . ? C1 B3 B8 106.2(8) . . ? C2 B3 B8 106.6(8) . . ? B4 B3 B8 59.4(7) . . ? C1 B3 B7 107.4(8) . . ? C2 B3 B7 59.3(6) . . ? B4 B3 B7 107.2(9) . . ? B8 B3 B7 60.4(7) . . ? C1 B4 B8 108.7(8) . . ? C1 B4 B3 59.9(6) . . ? B8 B4 B3 60.7(7) . . ? C1 B4 B5 61.4(6) . . ? B8 B4 B5 109.9(9) . . ? B3 B4 B5 110.3(8) . . ? C1 B4 B9 109.4(9) . . ? B8 B4 B9 61.4(8) . . ? B3 B4 B9 110.4(9) . . ? B5 B4 B9 60.1(7) . . ? C1' B4' B5' 59.2(8) . . ? C1' B4' B3' 58.1(7) . . ? B5' B4' B3' 107.6(10) . . ? C1' B4' B9' 105.9(10) . . ? B5' B4' B9' 60.0(8) . . ? B3' B4' B9' 108.7(10) . . ? C1' B4' B8' 107.0(10) . . ? B5' B4' B8' 108.6(10) . . ? B3' B4' B8' 62.0(7) . . ? B9' B4' B8' 59.9(8) . . ? B10 B5 C1 108.4(8) . . ? B10 B5 B4 109.2(9) . . ? C1 B5 B4 56.7(6) . . ? B10 B5 B6 61.5(7) . . ? C1 B5 B6 59.6(6) . . ? B4 B5 B6 106.0(8) . . ? B10 B5 B9 61.6(7) . . ? C1 B5 B9 105.6(8) . . ? B4 B5 B9 60.1(7) . . ? B6 B5 B9 109.4(9) . . ? C1' B5' B4' 59.1(7) . . ? C1' B5' B9' 106.4(10) . . ? B4' B5' B9' 60.8(9) . . ? C1' B5' B6' 60.1(7) . . ? B4' B5' B6' 109.2(9) . . ? B9' B5' B6' 108.5(10) . . ? C1' B5' B10' 108.4(9) . . ? B4' B5' B10' 110.2(11) . . ? B9' B5' B10' 60.1(8) . . ? B6' B5' B10' 61.2(7) . . ? C2 B6 C1 59.0(6) . . ? C2 B6 B5 107.0(8) . . ? C1 B6 B5 60.0(6) . . ? C2 B6 B10 107.6(9) . . ? C1 B6 B10 105.9(8) . . ? B5 B6 B10 57.9(7) . . ? C2 B6 B11 58.3(6) . . ? C1 B6 B11 105.0(8) . . ? B5 B6 B11 106.4(8) . . ? B10 B6 B11 61.3(7) . . ? C1' B6' C2' 58.7(6) . . ? C1' B6' B5' 58.4(7) . . ? C2' B6' B5' 105.6(9) . . ? C1' B6' B11' 105.1(9) . . ? C2' B6' B11' 59.5(7) . . ? B5' B6' B11' 105.5(10) . . ? C1' B6' B10' 106.2(10) . . ? C2' B6' B10' 106.8(9) . . ? B5' B6' B10' 60.0(8) . . ? B11' B6' B10' 58.8(7) . . ? C2 B7 B11 59.0(6) . . ? C2 B7 B3 59.2(6) . . ? B11 B7 B3 107.4(8) . . ? C2 B7 B8 105.8(8) . . ? B11 B7 B8 107.8(8) . . ? B3 B7 B8 59.3(7) . . ? C2 B7 B12 105.6(8) . . ? B11 B7 B12 59.1(6) . . ? B3 B7 B12 108.2(8) . . ? B8 B7 B12 61.2(7) . . ? C2' B7' B8' 110.4(10) . . ? C2' B7' B3' 59.8(7) . . ? B8' B7' B3' 62.9(8) . . ? C2' B7' B12' 106.1(9) . . ? B8' B7' B12' 62.1(7) . . ? B3' B7' B12' 110.4(9) . . ? C2' B7' B11' 59.8(6) . . ? B8' B7' B11' 109.6(10) . . ? B3' B7' B11' 108.7(9) . . ? B12' B7' B11' 57.7(7) . . ? B4 B8 B3 59.9(7) . . ? B4 B8 B7 107.5(9) . . ? B3 B8 B7 60.3(7) . . ? B4 B8 B9 60.4(7) . . ? B3 B8 B9 108.9(9) . . ? B7 B8 B9 107.9(9) . . ? B4 B8 B12 106.6(9) . . ? B3 B8 B12 107.8(9) . . ? B7 B8 B12 59.8(7) . . ? B9 B8 B12 59.2(7) . . ? B7' B8' B9' 105.4(11) . . ? B7' B8' B4' 105.6(11) . . ? B9' B8' B4' 59.9(8) . . ? B7' B8' B12' 60.2(8) . . ? B9' B8' B12' 56.9(8) . . ? B4' B8' B12' 104.7(11) . . ? B7' B8' B3' 59.5(7) . . ? B9' B8' B3' 105.9(11) . . ? B4' B8' B3' 58.4(8) . . ? B12' B8' B3' 106.3(10) . . ? B12' B9' B5' 107.5(10) . . ? B12' B9' B8' 62.4(8) . . ? B5' B9' B8' 108.3(10) . . ? B12' B9' B4' 109.2(10) . . ? B5' B9' B4' 59.3(8) . . ? B8' B9' B4' 60.2(8) . . ? B12' B9' B10' 59.9(8) . . ? B5' B9' B10' 60.6(8) . . ? B8' B9' B10' 111.3(10) . . ? B4' B9' B10' 109.4(11) . . ? B4 B9 B5 59.8(7) . . ? B4 B9 B12 106.4(9) . . ? B5 B9 B12 106.9(9) . . ? B4 B9 B10 105.9(9) . . ? B5 B9 B10 57.7(7) . . ? B12 B9 B10 61.3(7) . . ? B4 B9 B8 58.2(7) . . ? B5 B9 B8 107.0(9) . . ? B12 B9 B8 61.0(7) . . ? B10 B9 B8 109.3(9) . . ? B5 B10 B6 60.6(7) . . ? B5 B10 B9 60.6(7) . . ? B6 B10 B9 107.9(9) . . ? B5 B10 B12 107.3(9) . . ? B6 B10 B12 105.9(9) . . ? B9 B10 B12 59.1(7) . . ? B5 B10 B11 107.0(9) . . ? B6 B10 B11 59.5(6) . . ? B9 B10 B11 104.8(9) . . ? B12 B10 B11 57.3(7) . . ? B12' B10' B11' 58.6(7) . . ? B12' B10' B9' 58.0(8) . . ? B11' B10' B9' 104.6(10) . . ? B12' B10' B5' 104.9(10) . . ? B11' B10' B5' 105.2(9) . . ? B9' B10' B5' 59.2(8) . . ? B12' B10' B6' 106.1(10) . . ? B11' B10' B6' 59.7(7) . . ? B9' B10' B6' 105.9(9) . . ? B5' B10' B6' 58.8(7) . . ? C2 B11 B12 108.2(8) . . ? C2 B11 B7 59.9(6) . . ? B12 B11 B7 61.4(7) . . ? C2 B11 B6 59.2(6) . . ? B12 B11 B6 108.8(8) . . ? B7 B11 B6 108.6(8) . . ? C2 B11 B10 106.5(8) . . ? B12 B11 B10 61.3(7) . . ? B7 B11 B10 110.0(8) . . ? B6 B11 B10 59.2(7) . . ? B12' B11' C2' 107.7(10) . . ? B12' B11' B10' 60.2(8) . . ? C2' B11' B10' 108.9(9) . . ? B12' B11' B6' 108.7(10) . . ? C2' B11' B6' 59.5(6) . . ? B10' B11' B6' 61.5(7) . . ? B12' B11' B7' 60.9(8) . . ? C2' B11' B7' 58.5(6) . . ? B10' B11' B7' 109.0(10) . . ? B6' B11' B7' 106.8(9) . . ? B11 B12 B9 108.5(9) . . ? B11 B12 B7 59.5(7) . . ? B9 B12 B7 107.8(9) . . ? B11 B12 B8 106.4(9) . . ? B9 B12 B8 59.7(7) . . ? B7 B12 B8 59.0(7) . . ? B11 B12 B10 61.4(7) . . ? B9 B12 B10 59.6(7) . . ? B7 B12 B10 108.6(9) . . ? B8 B12 B10 106.9(9) . . ? B9' B12' B11' 109.7(11) . . ? B9' B12' B10' 62.1(8) . . ? B11' B12' B10' 61.2(8) . . ? B9' B12' B7' 106.5(10) . . ? B11' B12' B7' 61.4(7) . . ? B10' B12' B7' 110.2(10) . . ? B9' B12' B8' 60.6(8) . . ? B11' B12' B8' 109.0(10) . . ? B10' B12' B8' 111.6(11) . . ? B7' B12' B8' 57.7(7) . . ? C21 B23 C22 61.1(6) . . ? C21 B23 B27 106.3(8) . . ? C22 B23 B27 58.9(6) . . ? C21 B23 B24 59.8(6) . . ? C22 B23 B24 110.3(8) . . ? B27 B23 B24 108.6(8) . . ? C21 B23 B28 105.0(8) . . ? C22 B23 B28 108.3(8) . . ? B27 B23 B28 61.3(6) . . ? B24 B23 B28 58.4(6) . . ? C22' B23' B27' 59.9(6) . . ? C22' B23' C21' 60.1(5) . . ? B27' B23' C21' 106.4(8) . . ? C22' B23' B28' 107.2(8) . . ? B27' B23' B28' 59.5(6) . . ? C21' B23' B28' 105.1(8) . . ? C22' B23' B24' 107.1(8) . . ? B27' B23' B24' 105.9(9) . . ? C21' B23' B24' 58.6(6) . . ? B28' B23' B24' 58.4(7) . . ? B29' B24' C21' 106.4(10) . . ? B29' B24' B28' 61.3(7) . . ? C21' B24' B28' 107.6(9) . . ? B29' B24' B25' 60.6(8) . . ? C21' B24' B25' 58.5(7) . . ? B28' B24' B25' 110.1(10) . . ? B29' B24' B23' 109.1(9) . . ? C21' B24' B23' 59.8(6) . . ? B28' B24' B23' 60.5(7) . . ? B25' B24' B23' 108.4(9) . . ? C21 B24 B28 105.0(8) . . ? C21 B24 B23 56.5(6) . . ? B28 B24 B23 61.5(6) . . ? C21 B24 B29 103.1(9) . . ? B28 B24 B29 59.0(7) . . ? B23 B24 B29 106.1(9) . . ? C21 B24 B25 57.7(7) . . ? B28 B24 B25 106.1(9) . . ? B23 B24 B25 104.0(9) . . ? B29 B24 B25 58.6(8) . . ? C21' B25' B29' 104.8(9) . . ? C21' B25' B24' 59.3(7) . . ? B29' B25' B24' 57.8(7) . . ? C21' B25' B26' 58.6(7) . . ? B29' B25' B26' 105.7(10) . . ? B24' B25' B26' 105.6(9) . . ? C21' B25' B30' 105.6(9) . . ? B29' B25' B30' 59.1(7) . . ? B24' B25' B30' 105.1(10) . . ? B26' B25' B30' 59.6(7) . . ? C21 B25 B30 104.4(9) . . ? C21 B25 B29 104.4(9) . . ? B30 B25 B29 61.5(8) . . ? C21 B25 B26 59.0(6) . . ? B30 B25 B26 58.7(8) . . ? B29 B25 B26 107.8(10) . . ? C21 B25 B24 58.2(6) . . ? B30 B25 B24 108.7(10) . . ? B29 B25 B24 59.8(8) . . ? B26 B25 B24 107.6(8) . . ? C21' B26' C22' 60.3(6) . . ? C21' B26' B30' 106.5(9) . . ? C22' B26' B30' 107.7(8) . . ? C21' B26' B31' 108.2(8) . . ? C22' B26' B31' 60.3(6) . . ? B30' B26' B31' 60.2(7) . . ? C21' B26' B25' 58.8(7) . . ? C22' B26' B25' 108.3(9) . . ? B30' B26' B25' 60.5(7) . . ? B31' B26' B25' 109.5(9) . . ? B31 B26 C22 61.1(7) . . ? B31 B26 C21 107.1(9) . . ? C22 B26 C21 58.9(6) . . ? B31 B26 B30 59.2(8) . . ? C22 B26 B30 106.8(10) . . ? C21 B26 B30 104.9(9) . . ? B31 B26 B25 108.1(10) . . ? C22 B26 B25 106.9(9) . . ? C21 B26 B25 58.5(7) . . ? B30 B26 B25 59.8(8) . . ? C22 B27 B23 58.2(6) . . ? C22 B27 B31 61.1(6) . . ? B23 B27 B31 108.2(8) . . ? C22 B27 B32 109.4(8) . . ? B23 B27 B32 109.0(9) . . ? B31 B27 B32 61.2(7) . . ? C22 B27 B28 107.7(8) . . ? B23 B27 B28 61.2(6) . . ? B31 B27 B28 108.9(8) . . ? B32 B27 B28 59.7(7) . . ? C22' B27' B23' 59.2(6) . . ? C22' B27' B31' 61.5(6) . . ? B23' B27' B31' 110.2(8) . . ? C22' B27' B28' 108.2(8) . . ? B23' B27' B28' 61.4(7) . . ? B31' B27' B28' 109.6(9) . . ? C22' B27' B32' 109.2(8) . . ? B23' B27' B32' 110.3(9) . . ? B31' B27' B32' 60.7(7) . . ? B28' B27' B32' 60.5(7) . . ? B29 B28 B24 61.4(8) . . ? B29 B28 B32 59.7(8) . . ? B24 B28 B32 109.4(10) . . ? B29 B28 B23 106.8(10) . . ? B24 B28 B23 60.0(6) . . ? B32 B28 B23 105.5(9) . . ? B29 B28 B27 105.7(10) . . ? B24 B28 B27 106.8(9) . . ? B32 B28 B27 59.0(7) . . ? B23 B28 B27 57.5(6) . . ? B24' B28' B27' 107.8(8) . . ? B24' B28' B29' 58.7(7) . . ? B27' B28' B29' 107.5(9) . . ? B24' B28' B23' 61.1(7) . . ? B27' B28' B23' 59.1(6) . . ? B29' B28' B23' 107.5(8) . . ? B24' B28' B32' 108.1(9) . . ? B27' B28' B32' 61.1(7) . . ? B29' B28' B32' 60.0(7) . . ? B23' B28' B32' 109.0(8) . . ? B24' B29' B30' 109.8(9) . . ? B24' B29' B28' 60.0(8) . . ? B30' B29' B28' 108.3(9) . . ? B24' B29' B25' 61.6(7) . . ? B30' B29' B25' 61.3(7) . . ? B28' B29' B25' 109.8(9) . . ? B24' B29' B32' 109.7(10) . . ? B30' B29' B32' 60.0(7) . . ? B28' B29' B32' 60.5(7) . . ? B25' B29' B32' 110.5(10) . . ? B28 B29 B32 61.3(8) . . ? B28 B29 B25 108.8(10) . . ? B32 B29 B25 108.1(11) . . ? B28 B29 B24 59.5(7) . . ? B32 B29 B24 109.1(10) . . ? B25 B29 B24 61.6(8) . . ? B28 B29 B30 108.0(10) . . ? B32 B29 B30 59.7(8) . . ? B25 B29 B30 58.8(9) . . ? B24 B29 B30 108.0(11) . . ? B29' B30' B32' 60.4(7) . . ? B29' B30' B26' 106.4(9) . . ? B32' B30' B26' 108.4(9) . . ? B29' B30' B31' 107.5(9) . . ? B32' B30' B31' 60.3(7) . . ? B26' B30' B31' 60.1(7) . . ? B29' B30' B25' 59.7(7) . . ? B32' B30' B25' 109.5(9) . . ? B26' B30' B25' 59.9(7) . . ? B31' B30' B25' 108.9(9) . . ? B31 B30 B26 60.0(7) . . ? B31 B30 B25 110.1(9) . . ? B26 B30 B25 61.5(8) . . ? B31 B30 B32 62.2(8) . . ? B26 B30 B32 109.4(9) . . ? B25 B30 B32 108.3(10) . . ? B31 B30 B29 109.3(10) . . ? B26 B30 B29 108.7(10) . . ? B25 B30 B29 59.7(8) . . ? B32 B30 B29 59.0(8) . . ? B30 B31 B26 60.8(8) . . ? B30 B31 C22 106.8(9) . . ? B26 B31 C22 59.5(6) . . ? B30 B31 B27 107.9(10) . . ? B26 B31 B27 106.6(9) . . ? C22 B31 B27 57.2(6) . . ? B30 B31 B32 60.8(8) . . ? B26 B31 B32 109.0(9) . . ? C22 B31 B32 105.3(9) . . ? B27 B31 B32 59.9(7) . . ? B27' B31' C22' 58.7(6) . . ? B27' B31' B26' 105.8(9) . . ? C22' B31' B26' 58.5(6) . . ? B27' B31' B32' 61.1(7) . . ? C22' B31' B32' 107.4(8) . . ? B26' B31' B32' 107.2(9) . . ? B27' B31' B30' 107.0(9) . . ? C22' B31' B30' 105.9(8) . . ? B26' B31' B30' 59.7(7) . . ? B32' B31' B30' 59.2(7) . . ? B30' B32' B29' 59.6(7) . . ? B30' B32' B28' 107.1(9) . . ? B29' B32' B28' 59.5(7) . . ? B30' B32' B31' 60.5(7) . . ? B29' B32' B31' 107.0(9) . . ? B28' B32' B31' 106.0(9) . . ? B30' B32' B27' 105.8(9) . . ? B29' B32' B27' 105.0(9) . . ? B28' B32' B27' 58.4(7) . . ? B31' B32' B27' 58.2(7) . . ? B29 B32 B30 61.2(8) . . ? B29 B32 B27 107.0(10) . . ? B30 B32 B27 104.2(9) . . ? B29 B32 B28 59.0(8) . . ? B30 B32 B28 107.5(10) . . ? B27 B32 B28 61.3(7) . . ? B29 B32 B31 106.9(10) . . ? B30 B32 B31 57.0(7) . . ? B27 B32 B31 58.9(7) . . ? B28 B32 B31 108.3(9) . . ? C81 O1 C84 118.2(17) . . ? O1 C81 C82 89.8(10) . . ? C83 C82 C81 109.0(8) . . ? C82 C83 C84 92.2(13) . . ? O1 C84 C83 87.9(10) . . ? C91 O2 C94 125.1(17) . . ? O2 C91 C92 87.6(10) . . ? C93 C92 C91 112.1(7) . . ? C94 C93 C92 99.6(18) . . ? O2 C94 C93 88.6(10) . . ? C101 O3 C104 125.8(18) . . ? O3 C101 C102 89.0(10) . . ? C103 C102 C101 104.6(14) . . ? C104 C103 C102 95.4(16) . . ? O3 C104 C103 89.1(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.966 _refine_diff_density_min -2.046 _refine_diff_density_rms 0.149 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.078 0.829 0.116 203.2 38.9 2 -0.078 0.329 0.384 203.2 38.7 3 0.078 0.671 0.616 203.3 39.1 4 -0.078 0.171 0.884 203.2 38.5 5 0.383 0.323 0.089 318.4 63.9 6 0.383 0.177 0.589 318.3 62.1 7 0.339 0.321 0.264 9.5 -0.2 8 0.339 0.178 0.764 9.6 -0.2 9 0.617 0.677 -0.089 318.9 64.2 10 0.617 0.823 0.411 319.4 62.9 11 0.427 0.587 0.010 10.9 1.8 12 0.427 0.913 0.510 10.8 1.6 13 0.573 0.413 -0.011 11.0 1.1 14 0.573 0.087 0.489 11.1 1.2 15 0.661 0.821 0.236 8.7 -0.3 16 0.661 0.678 0.736 8.8 -0.4 _platon_squeeze_details ; ; #===END