Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof D W Stephan' _publ_contact_author_address ; Dept of Chemistry & Biochemistry University of Windsor Windsor Ontario N9P 3P4 CANADA ; _publ_contact_author_email STEPHAN@UWINDSOR.CA _publ_section_title ; Syntheses and Reactions of The bis-Boryloxide O(Bpin)2 (pin = O2C2Me4) ; loop_ _publ_author_name 'D. W. Stephan' 'Sarah Hawkeswood' data_O(Bpin)2 _database_code_depnum_ccdc_archive 'CCDC 266791' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C12 H24 B2 O5' _chemical_formula_weight 269.93 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' 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)/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 6.544(4) _cell_length_b 21.289(13) _cell_length_c 11.767(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.599(12) _cell_angle_gamma 90.00 _cell_volume 1631.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.146529 _exptl_absorpt_correction_T_max 0.256573 _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_reflns_number 6727 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.1057 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2344 _reflns_number_gt 869 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1873P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2340 _refine_ls_number_parameters 253 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.2040 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.3185 _refine_ls_wR_factor_gt 0.2677 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.884 _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 B1 B 0.0290(14) 0.0905(4) 0.7679(9) 0.087(3) Uani 1 1 d . . . B2 B 0.2605(13) 0.1767(4) 0.8569(8) 0.081(2) Uani 1 1 d . . . O1 O -0.033(2) 0.0656(6) 0.8535(8) 0.074(4) Uani 0.50 1 d P . . O1A O -0.069(4) 0.0480(13) 0.8526(18) 0.201(13) Uani 0.50 1 d P . . O2 O -0.028(5) 0.0538(11) 0.6726(18) 0.199(13) Uani 0.50 1 d P . . O2A O -0.0471(15) 0.0746(7) 0.6607(12) 0.063(3) Uani 0.50 1 d P . . O3 O 0.343(3) 0.2303(8) 0.8363(18) 0.134(8) Uani 0.50 1 d P . . O3A O 0.438(2) 0.2059(10) 0.8492(15) 0.131(7) Uani 0.50 1 d P . . O4 O 0.280(3) 0.1605(8) 0.9661(15) 0.143(8) Uani 0.50 1 d P . . O4A O 0.182(2) 0.1915(9) 0.9477(17) 0.160(9) Uani 0.50 1 d P . . O5 O 0.1640(15) 0.1441(6) 0.7669(13) 0.052(3) Uani 0.50 1 d P . . O5A O 0.162(4) 0.1355(13) 0.776(2) 0.186(13) Uani 0.50 1 d P . . C1 C -0.1433(14) 0.0034(5) 0.8085(7) 0.062(4) Uani 0.50 1 d PD . . C1A C -0.269(3) 0.0276(14) 0.7759(18) 0.66(8) Uani 0.50 1 d PD . . C2 C -0.2122(14) 0.0262(5) 0.6862(6) 0.049(3) Uani 0.50 1 d PD . . C2A C -0.113(5) -0.0122(9) 0.7159(15) 0.63(7) Uani 0.50 1 d PD . . C3 C 0.0179(15) -0.0509(4) 0.8088(10) 0.184(5) Uani 1 1 d D . . C4 C -0.4160(11) 0.0641(4) 0.6864(9) 0.154(3) Uani 1 1 d D . . C5 C -0.3130(13) -0.0073(4) 0.8870(7) 0.150(4) Uani 1 1 d D . . C6 C -0.2243(12) -0.0266(4) 0.5958(6) 0.133(3) Uani 1 1 d D . . C7 C 0.4199(15) 0.2604(5) 0.9404(12) 0.079(4) Uani 0.50 1 d PD . . C7A C 0.306(2) 0.2475(7) 1.0042(12) 0.138(8) Uani 0.50 1 d PD . . C8 C 0.3938(18) 0.2097(5) 1.0302(8) 0.072(4) Uani 0.50 1 d PD . . C8A C 0.516(2) 0.2279(5) 0.9683(12) 0.118(7) Uani 0.50 1 d PD . . C9 C 0.6362(15) 0.2895(5) 0.9468(8) 0.186(4) Uani 1 1 d D . . C10 C 0.2904(19) 0.2341(7) 1.1320(9) 0.244(7) Uani 1 1 d D . . C11 C 0.604(2) 0.1756(4) 1.0528(14) 0.311(11) Uani 1 1 d D . . C12 C 0.2610(19) 0.3137(5) 0.9490(12) 0.248(7) Uani 1 1 d 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 B1 0.091(6) 0.072(6) 0.091(7) -0.021(6) -0.022(5) -0.004(4) B2 0.083(6) 0.066(5) 0.094(6) -0.014(5) 0.005(5) -0.010(4) O1 0.125(8) 0.075(6) 0.021(5) -0.017(5) 0.004(5) -0.089(6) O1A 0.22(2) 0.25(3) 0.148(18) 0.095(16) 0.086(15) 0.100(18) O2 0.37(3) 0.16(2) 0.079(12) -0.057(13) 0.048(13) -0.070(16) O2A 0.063(5) 0.069(7) 0.055(6) 0.005(5) -0.001(4) -0.035(4) O3 0.20(2) 0.079(8) 0.114(10) 0.005(7) -0.038(13) -0.039(10) O3A 0.098(11) 0.21(2) 0.099(11) -0.063(12) 0.050(9) -0.082(11) O4 0.20(2) 0.145(13) 0.070(7) 0.032(9) -0.033(11) -0.084(11) O4A 0.114(12) 0.24(2) 0.135(15) -0.122(16) 0.053(10) -0.091(12) O5 0.053(5) 0.041(5) 0.060(8) -0.009(5) -0.008(5) -0.024(4) O5A 0.29(3) 0.18(2) 0.089(17) -0.013(16) 0.017(16) -0.033(19) C1 0.084(8) 0.066(8) 0.037(6) -0.030(6) 0.001(6) -0.058(8) C1A 0.77(12) 0.28(5) 0.79(13) 0.18(7) -0.61(12) -0.36(7) C2 0.057(7) 0.046(7) 0.045(6) -0.002(5) 0.014(5) -0.034(5) C2A 0.99(18) 0.26(6) 0.65(13) 0.20(7) 0.14(12) -0.37(9) C3 0.186(9) 0.094(6) 0.256(12) 0.035(7) -0.068(8) 0.012(6) C4 0.097(6) 0.154(8) 0.205(9) -0.006(7) -0.016(5) 0.007(5) C5 0.186(8) 0.163(8) 0.106(6) 0.005(6) 0.042(6) -0.065(7) C6 0.150(6) 0.154(7) 0.093(5) -0.054(5) 0.001(4) -0.029(5) C7 0.042(8) 0.094(11) 0.103(11) -0.018(9) 0.015(8) -0.021(8) C7A 0.093(13) 0.106(16) 0.21(3) -0.060(16) 0.004(13) -0.019(12) C8 0.087(11) 0.067(9) 0.062(7) -0.015(7) 0.000(7) -0.038(8) C8A 0.074(11) 0.153(18) 0.121(14) -0.059(14) -0.015(10) -0.012(11) C9 0.226(10) 0.175(8) 0.156(8) 0.006(7) 0.009(7) -0.118(8) C10 0.277(13) 0.346(16) 0.124(8) -0.118(10) 0.098(8) -0.165(12) C11 0.323(17) 0.120(7) 0.43(2) 0.028(11) -0.264(18) -0.011(9) C12 0.236(12) 0.154(9) 0.338(18) -0.102(11) -0.050(11) 0.057(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O1 1.240(15) . ? B1 O5A 1.29(3) . ? B1 O2A 1.353(16) . ? B1 O2 1.39(2) . ? B1 O5 1.443(18) . ? B1 O1A 1.53(2) . ? B2 O4A 1.270(18) . ? B2 O3 1.30(2) . ? B2 O4 1.324(18) . ? B2 O3A 1.328(18) . ? B2 O5 1.369(17) . ? B2 O5A 1.40(3) . ? O1 C1 1.576(14) . ? O1 C1A 1.90(3) . ? O1A C1 1.17(3) . ? O1A C1A 1.58(3) . ? O2 C2 1.37(3) . ? O2 C2A 1.61(4) . ? O2A C2 1.543(19) . ? O3 O3A 0.81(2) . ? O3 C7 1.43(2) . ? O3 C8A 1.83(2) . ? O3A C8A 1.52(2) . ? O3A C7 1.59(2) . ? O4 O4A 0.93(2) . ? O4 C8 1.45(2) . ? O4 C7A 1.91(2) . ? O4A C7A 1.56(2) . ? O4A C8 1.66(2) . ? C1 C1A 1.016(19) . ? C1 C2A 1.17(2) . ? C1 C5 1.529(9) . ? C1 C2 1.544(9) . ? C1 C3 1.564(9) . ? C1A C2 1.15(2) . ? C1A C2A 1.548(10) . ? C1A C5 1.554(10) . ? C1A C4 1.560(10) . ? C2 C2A 1.079(19) . ? C2 C6 1.544(8) . ? C2 C4 1.558(8) . ? C2A C6 1.555(10) . ? C2A C3 1.558(10) . ? C7 C8A 0.969(14) . ? C7 C7A 1.141(17) . ? C7 C8 1.532(9) . ? C7 C9 1.540(9) . ? C7 C12 1.548(9) . ? C7A C8 1.016(16) . ? C7A C8A 1.531(10) . ? C7A C10 1.544(10) . ? C7A C12 1.568(9) . ? C8 C8A 1.196(16) . ? C8 C10 1.523(9) . ? C8 C11 1.554(9) . ? C8A C9 1.563(9) . ? C8A C11 1.565(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 B1 O5A 121.6(15) . . ? O1 B1 O2A 122.0(10) . . ? O5A B1 O2A 116.2(17) . . ? O1 B1 O2 109.5(14) . . ? O5A B1 O2 127(2) . . ? O2A B1 O2 20.0(14) . . ? O1 B1 O5 126.3(9) . . ? O5A B1 O5 6.4(16) . . ? O2A B1 O5 111.1(12) . . ? O2 B1 O5 123.6(16) . . ? O1 B1 O1A 13.9(13) . . ? O5A B1 O1A 135.2(19) . . ? O2A B1 O1A 108.6(14) . . ? O2 B1 O1A 95.6(17) . . ? O5 B1 O1A 140.1(15) . . ? O4A B2 O3 98.6(15) . . ? O4A B2 O4 42.0(10) . . ? O3 B2 O4 114.1(14) . . ? O4A B2 O3A 111.7(12) . . ? O3 B2 O3A 36.0(10) . . ? O4 B2 O3A 100.8(12) . . ? O4A B2 O5 125.7(11) . . ? O3 B2 O5 118.2(13) . . ? O4 B2 O5 127.7(12) . . ? O3A B2 O5 121.7(12) . . ? O4A B2 O5A 121.8(16) . . ? O3 B2 O5A 126.7(16) . . ? O4 B2 O5A 119.2(15) . . ? O3A B2 O5A 126.4(16) . . ? O5 B2 O5A 8.8(16) . . ? B1 O1 C1 105.2(8) . . ? B1 O1 C1A 96.1(8) . . ? C1 O1 C1A 32.3(9) . . ? C1 O1A B1 112.0(17) . . ? C1 O1A C1A 40.0(14) . . ? B1 O1A C1A 99.6(13) . . ? C2 O2 B1 108.5(18) . . ? C2 O2 C2A 41.4(12) . . ? B1 O2 C2A 108.0(16) . . ? B1 O2A C2 100.8(11) . . ? O3A O3 B2 74(2) . . ? O3A O3 C7 86(3) . . ? B2 O3 C7 110.6(15) . . ? O3A O3 C8A 55(2) . . ? B2 O3 C8A 92.9(10) . . ? C7 O3 C8A 31.7(7) . . ? O3 O3A B2 70(2) . . ? O3 O3A C8A 99(3) . . ? B2 O3A C8A 107.3(12) . . ? O3 O3A C7 63(2) . . ? B2 O3A C7 99.9(10) . . ? C8A O3A C7 36.2(7) . . ? O4A O4 B2 65.9(17) . . ? O4A O4 C8 85(2) . . ? B2 O4 C8 108.1(12) . . ? O4A O4 C7A 53.9(19) . . ? B2 O4 C7A 88.5(10) . . ? C8 O4 C7A 31.6(7) . . ? O4 O4A B2 72(2) . . ? O4 O4A C7A 97(2) . . ? B2 O4A C7A 108.2(14) . . ? O4 O4A C8 60.9(19) . . ? B2 O4A C8 99.6(11) . . ? C7A O4A C8 36.7(7) . . ? B2 O5 B1 129.2(13) . . ? B1 O5A B2 141(2) . . ? C1A C1 O1A 93(2) . . ? C1A C1 C2A 89.8(11) . . ? O1A C1 C2A 123(2) . . ? C1A C1 C5 72.1(9) . . ? O1A C1 C5 98.6(12) . . ? C2A C1 C5 135.7(18) . . ? C1A C1 C2 48.4(12) . . ? O1A C1 C2 103.3(13) . . ? C2A C1 C2 44.2(9) . . ? C5 C1 C2 116.5(8) . . ? C1A C1 C3 154(2) . . ? O1A C1 C3 110.3(13) . . ? C2A C1 C3 67.6(8) . . ? C5 C1 C3 114.7(9) . . ? C2 C1 C3 111.7(7) . . ? C1A C1 O1 92(2) . . ? O1A C1 O1 7.0(13) . . ? C2A C1 O1 115.9(16) . . ? C5 C1 O1 105.0(8) . . ? C2 C1 O1 97.5(8) . . ? C3 C1 O1 109.4(9) . . ? C1 C1A C2 90.5(19) . . ? C1 C1A C2A 49.3(13) . . ? C2 C1A C2A 44.1(10) . . ? C1 C1A C5 69.5(7) . . ? C2 C1A C5 149(3) . . ? C2A C1A C5 107.8(18) . . ? C1 C1A C4 158.5(19) . . ? C2 C1A C4 68.2(7) . . ? C2A C1A C4 110.7(13) . . ? C5 C1A C4 130.8(15) . . ? C1 C1A O1A 47.5(15) . . ? C2 C1A O1A 101.8(17) . . ? C2A C1A O1A 82.1(14) . . ? C5 C1A O1A 82.1(13) . . ? C4 C1A O1A 132(2) . . ? C1 C1A O1 56.0(15) . . ? C2 C1A O1 97.4(15) . . ? C2A C1A O1 84.8(13) . . ? C5 C1A O1 90.5(12) . . ? C4 C1A O1 122.1(17) . . ? O1A C1A O1 10.1(11) . . ? C2A C2 C1A 87.7(10) . . ? C2A C2 O2 82(2) . . ? C1A C2 O2 117.7(19) . . ? C2A C2 O2A 99.2(18) . . ? C1A C2 O2A 117.2(19) . . ? O2 C2 O2A 17.6(13) . . ? C2A C2 C1 49.3(12) . . ? C1A C2 C1 41.1(10) . . ? O2 C2 C1 93.6(11) . . ? O2A C2 C1 104.2(8) . . ? C2A C2 C6 70.1(8) . . ? C1A C2 C6 130(2) . . ? O2 C2 C6 102.6(11) . . ? O2A C2 C6 110.0(8) . . ? C1 C2 C6 113.8(8) . . ? C2A C2 C4 151.3(18) . . ? C1A C2 C4 68.4(8) . . ? O2 C2 C4 123.0(13) . . ? O2A C2 C4 105.7(8) . . ? C1 C2 C4 109.5(7) . . ? C6 C2 C4 113.1(7) . . ? C2 C2A C1 86.4(18) . . ? C2 C2A C1A 48.1(12) . . ? C1 C2A C1A 41.0(10) . . ? C2 C2A C6 69.1(6) . . ? C1 C2A C6 143(3) . . ? C1A C2A C6 104.6(19) . . ? C2 C2A C3 154.1(19) . . ? C1 C2A C3 68.2(7) . . ? C1A C2A C3 108.2(13) . . ? C6 C2A C3 135.2(15) . . ? C2 C2A O2 56.9(15) . . ? C1 C2A O2 98.2(16) . . ? C1A C2A O2 86.2(16) . . ? C6 C2A O2 91.7(14) . . ? C3 C2A O2 119.8(18) . . ? C2A C3 C1 44.1(9) . . ? C2 C4 C1A 43.4(9) . . ? C1 C5 C1A 38.4(8) . . ? C2 C6 C2A 40.8(8) . . ? C8A C7 C7A 92.6(12) . . ? C8A C7 O3 97.6(15) . . ? C7A C7 O3 105.1(14) . . ? C8A C7 C8 51.3(10) . . ? C7A C7 C8 41.6(8) . . ? O3 C7 C8 102.9(10) . . ? C8A C7 C9 73.1(8) . . ? C7A C7 C9 136.0(14) . . ? O3 C7 C9 117.8(13) . . ? C8 C7 C9 114.4(9) . . ? C8A C7 C12 156.4(17) . . ? C7A C7 C12 69.5(7) . . ? O3 C7 C12 101.7(10) . . ? C8 C7 C12 110.5(9) . . ? C9 C7 C12 108.8(10) . . ? C8A C7 O3A 67.7(13) . . ? C7A C7 O3A 111.4(12) . . ? O3 C7 O3A 30.6(9) . . ? C8 C7 O3A 88.4(9) . . ? C9 C7 O3A 101.4(9) . . ? C12 C7 O3A 132.2(11) . . ? C8 C7A C7 90.3(12) . . ? C8 C7A C8A 51.3(10) . . ? C7 C7A C8A 39.2(7) . . ? C8 C7A C10 69.5(8) . . ? C7 C7A C10 142.8(14) . . ? C8A C7A C10 111.5(11) . . ? C8 C7A O4A 77.2(14) . . ? C7 C7A O4A 104.5(14) . . ? C8A C7A O4A 96.8(11) . . ? C10 C7A O4A 101.1(12) . . ? C8 C7A C12 156.0(15) . . ? C7 C7A C12 67.6(7) . . ? C8A C7A C12 105.6(9) . . ? C10 C7A C12 122.8(13) . . ? O4A C7A C12 116.2(12) . . ? C8 C7A O4 48.7(11) . . ? C7 C7A O4 97.4(13) . . ? C8A C7A O4 74.6(9) . . ? C10 C7A O4 92.1(9) . . ? O4A C7A O4 28.9(8) . . ? C12 C7A O4 139.9(11) . . ? C7A C8 C8A 87.2(10) . . ? C7A C8 O4 99.7(15) . . ? C8A C8 O4 104.8(12) . . ? C7A C8 C10 71.8(8) . . ? C8A C8 C10 138.0(11) . . ? O4 C8 C10 114.1(11) . . ? C7A C8 C7 48.1(9) . . ? C8A C8 C7 39.3(6) . . ? O4 C8 C7 103.6(9) . . ? C10 C8 C7 113.0(10) . . ? C7A C8 C11 152.2(14) . . ? C8A C8 C11 68.0(7) . . ? O4 C8 C11 98.7(10) . . ? C10 C8 C11 118.6(12) . . ? C7 C8 C11 107.0(8) . . ? C7A C8 O4A 66.1(13) . . ? C8A C8 O4A 106.7(12) . . ? O4 C8 O4A 34.0(9) . . ? C10 C8 O4A 97.5(9) . . ? C7 C8 O4A 84.5(10) . . ? C11 C8 O4A 131.6(10) . . ? C7 C8A C8 89.4(12) . . ? C7 C8A O3A 76.1(14) . . ? C8 C8A O3A 106.2(12) . . ? C7 C8A C7A 48.1(10) . . ? C8 C8A C7A 41.5(8) . . ? O3A C8A C7A 96.4(10) . . ? C7 C8A C9 70.5(8) . . ? C8 C8A C9 138.3(13) . . ? O3A C8A C9 103.8(11) . . ? C7A C8A C9 107.2(10) . . ? C7 C8A C11 155.4(16) . . ? C8 C8A C11 66.9(7) . . ? O3A C8A C11 115.9(12) . . ? C7A C8A C11 107.6(10) . . ? C9 C8A C11 122.7(10) . . ? C7 C8A O3 50.7(12) . . ? C8 C8A O3 97.7(11) . . ? O3A C8A O3 26.0(9) . . ? C7A C8A O3 74.5(10) . . ? C9 C8A O3 96.8(9) . . ? C11 C8A O3 135.8(10) . . ? C7 C9 C8A 36.4(5) . . ? C8 C10 C7A 38.7(6) . . ? C8 C11 C8A 45.1(7) . . ? C7 C12 C7A 42.9(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.228 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.057 #===end data_[tBu3PNH2][(BpinO)2Bpin] _database_code_depnum_ccdc_archive 'CCDC 266792' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C30 H65 B3 N O8 P' _chemical_formula_weight 631.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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 10.752(3) _cell_length_b 13.737(4) _cell_length_c 14.181(4) _cell_angle_alpha 94.422(6) _cell_angle_beta 104.550(6) _cell_angle_gamma 106.244(6) _cell_volume 1921.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 8994 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.3611 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 23.32 _reflns_number_total 5469 _reflns_number_gt 1562 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5469 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2470 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.843 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.2990(2) 0.31408(16) 0.22742(15) 0.0558(6) Uani 1 1 d . . . N1 N 0.1706(6) 0.3559(5) 0.1808(4) 0.0588(19) Uani 1 1 d . . . H1A H 0.133(6) 0.387(5) 0.228(5) 0.071 Uiso 1 1 d . . . H1B H 0.075(6) 0.298(5) 0.158(4) 0.071 Uiso 1 1 d . . . C1 C 0.2933(8) 0.2787(7) 0.3516(7) 0.073(3) Uani 1 1 d . . . C2 C 0.1511(8) 0.2213(6) 0.3516(6) 0.094(3) Uani 1 1 d . . . H2A H 0.1518 0.2033 0.4157 0.140 Uiso 1 1 calc R . . H2B H 0.1168 0.1600 0.3034 0.140 Uiso 1 1 calc R . . H2C H 0.0944 0.2641 0.3355 0.140 Uiso 1 1 calc R . . C3 C 0.3889(8) 0.2142(6) 0.3904(5) 0.092(3) Uani 1 1 d . . . H3A H 0.3810 0.1977 0.4536 0.138 Uiso 1 1 calc R . . H3B H 0.4807 0.2534 0.3966 0.138 Uiso 1 1 calc R . . H3C H 0.3639 0.1520 0.3447 0.138 Uiso 1 1 calc R . . C4 C 0.3362(8) 0.3782(6) 0.4291(5) 0.092(3) Uani 1 1 d . . . H4A H 0.3335 0.3596 0.4926 0.138 Uiso 1 1 calc R . . H4B H 0.2751 0.4171 0.4094 0.138 Uiso 1 1 calc R . . H4C H 0.4263 0.4189 0.4328 0.138 Uiso 1 1 calc R . . C5 C 0.2799(8) 0.2036(7) 0.1366(7) 0.077(3) Uani 1 1 d . . . C6 C 0.4065(8) 0.1714(6) 0.1504(6) 0.103(3) Uani 1 1 d . . . H6A H 0.3899 0.1136 0.1013 0.154 Uiso 1 1 calc R . . H6B H 0.4308 0.1529 0.2149 0.154 Uiso 1 1 calc R . . H6C H 0.4791 0.2275 0.1439 0.154 Uiso 1 1 calc R . . C7 C 0.2384(8) 0.2275(7) 0.0313(6) 0.115(4) Uani 1 1 d . . . H7A H 0.2287 0.1694 -0.0152 0.173 Uiso 1 1 calc R . . H7B H 0.3065 0.2862 0.0236 0.173 Uiso 1 1 calc R . . H7C H 0.1539 0.2418 0.0198 0.173 Uiso 1 1 calc R . . C8 C 0.1625(9) 0.1104(6) 0.1432(6) 0.109(3) Uani 1 1 d . . . H8A H 0.1526 0.0527 0.0961 0.164 Uiso 1 1 calc R . . H8B H 0.0800 0.1279 0.1292 0.164 Uiso 1 1 calc R . . H8C H 0.1822 0.0931 0.2085 0.164 Uiso 1 1 calc R . . C9 C 0.4493(7) 0.4253(6) 0.2355(6) 0.062(2) Uani 1 1 d . . . C10 C 0.4287(7) 0.5257(5) 0.2735(6) 0.088(3) Uani 1 1 d . . . H10A H 0.5068 0.5824 0.2769 0.131 Uiso 1 1 calc R . . H10B H 0.4161 0.5228 0.3380 0.131 Uiso 1 1 calc R . . H10C H 0.3504 0.5346 0.2293 0.131 Uiso 1 1 calc R . . C11 C 0.5809(7) 0.4125(6) 0.3043(6) 0.083(3) Uani 1 1 d . . . H11A H 0.6568 0.4706 0.3067 0.124 Uiso 1 1 calc R . . H11B H 0.5949 0.3509 0.2787 0.124 Uiso 1 1 calc R . . H11C H 0.5715 0.4082 0.3695 0.124 Uiso 1 1 calc R . . C12 C 0.4710(8) 0.4373(6) 0.1337(6) 0.088(3) Uani 1 1 d . . . H12A H 0.5492 0.4951 0.1402 0.132 Uiso 1 1 calc R . . H12B H 0.3931 0.4482 0.0909 0.132 Uiso 1 1 calc R . . H12C H 0.4844 0.3762 0.1063 0.132 Uiso 1 1 calc R . . B1 B -0.1731(8) 0.2937(7) 0.1910(6) 0.046(2) Uani 1 1 d . . . B2 B -0.0197(9) 0.4724(7) 0.2894(6) 0.044(2) Uani 1 1 d . . . B3 B -0.2508(9) 0.1462(8) 0.2804(7) 0.052(2) Uani 1 1 d . . . O1 O -0.1211(4) 0.2347(3) 0.1256(3) 0.0465(13) Uani 1 1 d . . . O2 O -0.2691(4) 0.3314(3) 0.1242(4) 0.0494(13) Uani 1 1 d . . . O3 O -0.0545(4) 0.3745(4) 0.2548(3) 0.0617(15) Uani 1 1 d . . . O4 O 0.1117(5) 0.5331(4) 0.3103(4) 0.0640(15) Uani 1 1 d . . . O5 O -0.0994(5) 0.5275(4) 0.3126(4) 0.0738(17) Uani 1 1 d . . . O6 O -0.2415(5) 0.2353(4) 0.2546(3) 0.0621(15) Uani 1 1 d . . . O7 O -0.1771(6) 0.0830(4) 0.2738(4) 0.098(2) Uani 1 1 d . . . O8 O -0.3486(7) 0.0987(5) 0.3257(5) 0.121(3) Uani 1 1 d . . . C13 C -0.2087(7) 0.2161(6) 0.0294(5) 0.054(2) Uani 1 1 d . . . C14 C -0.3243(7) 0.1173(5) 0.0174(5) 0.069(2) Uani 1 1 d . . . H14A H -0.3727 0.1248 0.0645 0.103 Uiso 1 1 calc R . . H14B H -0.2883 0.0612 0.0283 0.103 Uiso 1 1 calc R . . H14C H -0.3845 0.1036 -0.0482 0.103 Uiso 1 1 calc R . . C15 C -0.1336(7) 0.2035(6) -0.0473(5) 0.077(3) Uani 1 1 d . . . H15A H -0.0613 0.2656 -0.0408 0.116 Uiso 1 1 calc R . . H15B H -0.1952 0.1894 -0.1124 0.116 Uiso 1 1 calc R . . H15C H -0.0972 0.1476 -0.0366 0.116 Uiso 1 1 calc R . . C16 C -0.2564(7) 0.3140(5) 0.0278(5) 0.051(2) Uani 1 1 d . . . C17 C -0.3917(6) 0.2999(5) -0.0470(5) 0.067(2) Uani 1 1 d . . . H17A H -0.4587 0.2418 -0.0372 0.101 Uiso 1 1 calc R . . H17B H -0.3835 0.2886 -0.1125 0.101 Uiso 1 1 calc R . . H17C H -0.4181 0.3605 -0.0385 0.101 Uiso 1 1 calc R . . C18 C -0.1525(7) 0.4077(5) 0.0117(5) 0.076(2) Uani 1 1 d . . . H18A H -0.0663 0.4176 0.0581 0.114 Uiso 1 1 calc R . . H18B H -0.1806 0.4674 0.0210 0.114 Uiso 1 1 calc R . . H18C H -0.1454 0.3973 -0.0542 0.114 Uiso 1 1 calc R . . C19 C 0.1280(10) 0.6319(7) 0.3641(8) 0.086(3) Uani 1 1 d . . . C20 C 0.2265(9) 0.7156(6) 0.3341(7) 0.125(4) Uani 1 1 d . . . H20A H 0.1932 0.7170 0.2649 0.187 Uiso 1 1 calc R . . H20B H 0.3122 0.7030 0.3472 0.187 Uiso 1 1 calc R . . H20C H 0.2372 0.7805 0.3710 0.187 Uiso 1 1 calc R . . C21 C 0.1775(10) 0.6243(7) 0.4730(7) 0.131(4) Uani 1 1 d . . . H21A H 0.2689 0.6224 0.4882 0.196 Uiso 1 1 calc R . . H21B H 0.1209 0.5628 0.4868 0.196 Uiso 1 1 calc R . . H21C H 0.1740 0.6829 0.5124 0.196 Uiso 1 1 calc R . . C22 C -0.0207(10) 0.6333(6) 0.3360(7) 0.077(3) Uani 1 1 d . . . C23 C -0.0597(9) 0.6781(7) 0.2413(7) 0.129(4) Uani 1 1 d . . . H23A H -0.0321 0.6468 0.1905 0.194 Uiso 1 1 calc R . . H23B H -0.0154 0.7509 0.2536 0.194 Uiso 1 1 calc R . . H23C H -0.1558 0.6647 0.2203 0.194 Uiso 1 1 calc R . . C24 C -0.0629(9) 0.6844(7) 0.4133(7) 0.133(4) Uani 1 1 d . . . H24A H -0.1553 0.6822 0.3875 0.200 Uiso 1 1 calc R . . H24B H -0.0064 0.7546 0.4327 0.200 Uiso 1 1 calc R . . H24C H -0.0541 0.6495 0.4695 0.200 Uiso 1 1 calc R . . C25 C -0.2319(10) -0.0140(7) 0.3029(7) 0.080(3) Uani 1 1 d . . . C26 C -0.2934(11) -0.0919(7) 0.2131(7) 0.154(5) Uani 1 1 d . . . H26A H -0.3698 -0.0775 0.1722 0.231 Uiso 1 1 calc R . . H26B H -0.3222 -0.1587 0.2313 0.231 Uiso 1 1 calc R . . H26C H -0.2280 -0.0903 0.1775 0.231 Uiso 1 1 calc R . . C27 C -0.1159(11) -0.0410(8) 0.3657(8) 0.177(6) Uani 1 1 d . . . H27A H -0.1493 -0.1050 0.3879 0.266 Uiso 1 1 calc R . . H27B H -0.0688 0.0120 0.4218 0.266 Uiso 1 1 calc R . . H27C H -0.0553 -0.0475 0.3279 0.266 Uiso 1 1 calc R . . C28 C -0.3329(11) 0.0053(7) 0.3542(7) 0.083(3) Uani 1 1 d . . . C29 C -0.4681(12) -0.0754(9) 0.3239(10) 0.193(6) Uani 1 1 d . . . H29A H -0.4986 -0.0928 0.2533 0.289 Uiso 1 1 calc R . . H29B H -0.5317 -0.0497 0.3465 0.289 Uiso 1 1 calc R . . H29C H -0.4608 -0.1354 0.3524 0.289 Uiso 1 1 calc R . . C30 C -0.2780(13) 0.0293(8) 0.4641(8) 0.192(6) Uani 1 1 d . . . H30A H -0.1892 0.0784 0.4818 0.288 Uiso 1 1 calc R . . H30B H -0.2731 -0.0324 0.4901 0.288 Uiso 1 1 calc R . . H30C H -0.3364 0.0574 0.4910 0.288 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 P1 0.0412(13) 0.0639(15) 0.0661(16) 0.0104(12) 0.0134(10) 0.0240(12) N1 0.040(4) 0.087(6) 0.057(5) 0.013(4) 0.014(3) 0.030(4) C1 0.032(5) 0.100(8) 0.094(7) 0.021(6) 0.017(5) 0.031(6) C2 0.064(7) 0.105(8) 0.102(8) 0.011(6) 0.031(5) 0.005(6) C3 0.101(8) 0.106(7) 0.072(7) 0.041(6) 0.013(5) 0.038(6) C4 0.099(7) 0.112(8) 0.053(6) -0.012(6) 0.015(5) 0.027(6) C5 0.048(6) 0.080(7) 0.100(8) -0.013(6) 0.016(5) 0.028(5) C6 0.072(7) 0.091(7) 0.145(9) -0.018(6) 0.026(6) 0.038(6) C7 0.089(8) 0.178(11) 0.078(8) -0.028(7) 0.012(6) 0.064(8) C8 0.095(8) 0.088(7) 0.129(9) -0.026(6) 0.027(6) 0.018(7) C9 0.045(5) 0.065(6) 0.076(7) 0.006(5) 0.019(4) 0.020(5) C10 0.070(6) 0.061(6) 0.136(8) 0.019(6) 0.044(6) 0.013(5) C11 0.051(6) 0.083(7) 0.116(8) 0.015(6) 0.040(5) 0.012(5) C12 0.090(7) 0.095(7) 0.114(8) 0.041(6) 0.057(6) 0.054(6) B1 0.038(6) 0.052(6) 0.054(7) 0.007(5) 0.014(5) 0.021(5) B2 0.037(6) 0.052(6) 0.046(6) 0.000(5) 0.016(4) 0.017(5) B3 0.036(6) 0.053(7) 0.064(7) -0.006(5) 0.014(5) 0.013(6) O1 0.042(3) 0.058(3) 0.046(3) 0.010(2) 0.013(2) 0.024(3) O2 0.047(3) 0.053(3) 0.053(4) 0.010(3) 0.010(3) 0.027(3) O3 0.049(3) 0.058(4) 0.070(4) -0.010(3) 0.001(3) 0.022(3) O4 0.044(4) 0.053(3) 0.085(4) -0.009(3) 0.011(3) 0.010(3) O5 0.062(4) 0.056(4) 0.110(5) -0.006(3) 0.039(3) 0.019(3) O6 0.077(4) 0.059(4) 0.076(4) 0.028(3) 0.044(3) 0.037(3) O7 0.118(6) 0.068(4) 0.146(6) 0.047(4) 0.063(4) 0.057(4) O8 0.144(6) 0.113(5) 0.187(7) 0.100(5) 0.120(5) 0.082(5) C13 0.046(5) 0.068(6) 0.046(6) 0.002(4) 0.005(4) 0.022(5) C14 0.059(6) 0.062(6) 0.066(6) -0.003(4) -0.005(4) 0.014(5) C15 0.083(7) 0.105(7) 0.051(6) 0.006(5) 0.021(5) 0.041(6) C16 0.042(5) 0.057(5) 0.047(6) 0.009(4) 0.002(4) 0.014(4) C17 0.063(6) 0.078(6) 0.066(6) 0.024(4) 0.011(4) 0.035(5) C18 0.066(6) 0.069(6) 0.083(7) 0.021(5) 0.016(5) 0.007(5) C19 0.072(8) 0.072(8) 0.106(9) -0.020(6) 0.024(6) 0.018(6) C20 0.091(8) 0.071(7) 0.208(12) 0.004(7) 0.087(8) -0.016(6) C21 0.172(11) 0.110(9) 0.086(9) -0.004(6) -0.006(7) 0.048(8) C22 0.095(8) 0.041(6) 0.108(8) 0.010(6) 0.046(6) 0.024(6) C23 0.129(10) 0.088(8) 0.169(12) 0.053(8) 0.020(8) 0.043(7) C24 0.129(10) 0.088(8) 0.200(12) -0.023(8) 0.095(9) 0.029(7) C25 0.094(8) 0.061(7) 0.081(8) 0.029(6) 0.004(6) 0.031(6) C26 0.199(13) 0.092(8) 0.125(10) -0.040(8) 0.037(9) -0.004(8) C27 0.159(12) 0.180(13) 0.216(14) 0.083(11) 0.027(10) 0.099(11) C28 0.110(9) 0.069(7) 0.072(8) 0.023(6) 0.037(6) 0.019(7) C29 0.132(12) 0.142(12) 0.272(17) 0.021(11) 0.087(11) -0.030(10) C30 0.36(2) 0.142(11) 0.088(11) 0.036(8) 0.073(11) 0.079(12) _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 P1 N1 1.648(6) . ? P1 C5 1.844(8) . ? P1 C9 1.859(8) . ? P1 C1 1.874(9) . ? C1 C2 1.512(10) . ? C1 C3 1.563(9) . ? C1 C4 1.565(10) . ? C5 C6 1.517(9) . ? C5 C7 1.536(10) . ? C5 C8 1.554(10) . ? C9 C12 1.532(9) . ? C9 C10 1.535(9) . ? C9 C11 1.568(9) . ? B1 O6 1.454(9) . ? B1 O2 1.455(8) . ? B1 O3 1.466(9) . ? B1 O1 1.492(8) . ? B2 O3 1.308(8) . ? B2 O4 1.368(8) . ? B2 O5 1.372(8) . ? B3 O6 1.289(10) . ? B3 O7 1.342(9) . ? B3 O8 1.401(10) . ? O1 C13 1.407(7) . ? O2 C16 1.417(7) . ? O4 C19 1.447(9) . ? O5 C22 1.427(8) . ? O7 C25 1.436(9) . ? O8 C28 1.416(9) . ? C13 C14 1.527(9) . ? C13 C15 1.534(9) . ? C13 C16 1.567(8) . ? C16 C17 1.522(8) . ? C16 C18 1.526(8) . ? C19 C20 1.499(11) . ? C19 C21 1.524(11) . ? C19 C22 1.553(11) . ? C22 C24 1.486(10) . ? C22 C23 1.533(10) . ? C25 C26 1.475(11) . ? C25 C27 1.496(11) . ? C25 C28 1.519(11) . ? C28 C29 1.496(12) . ? C28 C30 1.496(11) . ? 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 P1 C5 105.1(4) . . ? N1 P1 C9 103.5(3) . . ? C5 P1 C9 112.8(4) . . ? N1 P1 C1 109.7(3) . . ? C5 P1 C1 112.9(4) . . ? C9 P1 C1 112.1(4) . . ? C2 C1 C3 109.3(8) . . ? C2 C1 C4 104.9(7) . . ? C3 C1 C4 107.6(7) . . ? C2 C1 P1 111.5(6) . . ? C3 C1 P1 113.2(6) . . ? C4 C1 P1 109.8(6) . . ? C6 C5 C7 108.8(7) . . ? C6 C5 C8 108.6(7) . . ? C7 C5 C8 105.9(7) . . ? C6 C5 P1 113.6(6) . . ? C7 C5 P1 110.3(6) . . ? C8 C5 P1 109.4(6) . . ? C12 C9 C10 106.0(7) . . ? C12 C9 C11 107.8(6) . . ? C10 C9 C11 109.9(6) . . ? C12 C9 P1 111.4(6) . . ? C10 C9 P1 110.4(5) . . ? C11 C9 P1 111.2(5) . . ? O6 B1 O2 108.5(6) . . ? O6 B1 O3 107.6(7) . . ? O2 B1 O3 114.3(6) . . ? O6 B1 O1 115.6(6) . . ? O2 B1 O1 105.0(6) . . ? O3 B1 O1 106.0(6) . . ? O3 B2 O4 120.7(7) . . ? O3 B2 O5 128.3(8) . . ? O4 B2 O5 111.0(7) . . ? O6 B3 O7 131.1(9) . . ? O6 B3 O8 121.8(8) . . ? O7 B3 O8 107.1(8) . . ? C13 O1 B1 107.8(5) . . ? C16 O2 B1 108.5(5) . . ? B2 O3 B1 138.7(6) . . ? B2 O4 C19 109.6(6) . . ? B2 O5 C22 107.8(7) . . ? B3 O6 B1 134.3(6) . . ? B3 O7 C25 112.1(8) . . ? B3 O8 C28 111.8(7) . . ? O1 C13 C14 108.7(6) . . ? O1 C13 C15 110.6(6) . . ? C14 C13 C15 108.9(6) . . ? O1 C13 C16 101.7(5) . . ? C14 C13 C16 112.8(6) . . ? C15 C13 C16 113.9(7) . . ? O2 C16 C17 109.1(6) . . ? O2 C16 C18 109.0(6) . . ? C17 C16 C18 108.3(6) . . ? O2 C16 C13 102.6(5) . . ? C17 C16 C13 114.6(6) . . ? C18 C16 C13 113.0(6) . . ? O4 C19 C20 110.4(8) . . ? O4 C19 C21 106.0(8) . . ? C20 C19 C21 111.8(8) . . ? O4 C19 C22 100.6(7) . . ? C20 C19 C22 116.0(9) . . ? C21 C19 C22 111.1(8) . . ? O5 C22 C24 108.8(8) . . ? O5 C22 C23 105.2(8) . . ? C24 C22 C23 108.0(8) . . ? O5 C22 C19 104.3(7) . . ? C24 C22 C19 116.6(9) . . ? C23 C22 C19 113.1(8) . . ? O7 C25 C26 107.9(8) . . ? O7 C25 C27 107.3(8) . . ? C26 C25 C27 107.7(8) . . ? O7 C25 C28 103.6(7) . . ? C26 C25 C28 113.9(9) . . ? C27 C25 C28 115.9(9) . . ? O8 C28 C29 109.1(9) . . ? O8 C28 C30 104.2(9) . . ? C29 C28 C30 110.9(9) . . ? O8 C28 C25 103.1(7) . . ? C29 C28 C25 115.1(10) . . ? C30 C28 C25 113.4(10) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.178 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.056 #===end data_Cp2Zr(OBpin)2 _database_code_depnum_ccdc_archive 'CCDC 266793' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C22 H34 B2 O6 Zr' _chemical_formula_weight 507.33 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.276(11) _cell_length_b 13.162(8) _cell_length_c 19.540(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.694(13) _cell_angle_gamma 90.00 _cell_volume 5124(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.063515 _exptl_absorpt_correction_T_max 0.145098 _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_reflns_number 10474 _diffrn_reflns_av_R_equivalents 0.1357 _diffrn_reflns_av_sigmaI/netI 0.1290 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 23.29 _reflns_number_total 3687 _reflns_number_gt 1802 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1155P)^2^+4.1864P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3687 _refine_ls_number_parameters 260 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1848 _refine_ls_R_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.2934 _refine_ls_wR_factor_gt 0.2410 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.031 _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 0.24290(5) 0.03948(8) 0.24370(6) 0.0539(5) Uani 1 1 d . . . O1 O 0.1799(4) 0.1364(6) 0.2801(5) 0.076(3) Uani 1 1 d . . . O2 O 0.1167(6) 0.2601(8) 0.3221(6) 0.111(4) Uani 1 1 d . . . O3 O 0.1268(6) 0.1148(7) 0.3789(6) 0.110(4) Uani 1 1 d . . . O4 O 0.2865(5) 0.1413(7) 0.1896(6) 0.095(3) Uani 1 1 d . . . O5 O 0.3745(5) 0.1104(7) 0.1286(7) 0.113(4) Uani 1 1 d . . . O6 O 0.3308(7) 0.2639(8) 0.1249(7) 0.131(5) Uani 1 1 d . . . B1 B 0.1440(7) 0.1697(11) 0.3234(9) 0.060(4) Uani 1 1 d . . . B2 B 0.3304(7) 0.1706(11) 0.1544(9) 0.061(4) Uani 1 1 d . . . C1 C 0.1317(8) -0.0379(17) 0.1898(10) 0.105(6) Uani 1 1 d . . . H1A H 0.0892 -0.0287 0.2061 0.126 Uiso 1 1 calc R . . C2 C 0.1519(10) 0.0146(14) 0.1375(10) 0.107(6) Uani 1 1 d . . . H2A H 0.1266 0.0686 0.1097 0.128 Uiso 1 1 calc R . . C3 C 0.2089(10) -0.0330(16) 0.1235(9) 0.112(6) Uani 1 1 d . . . H3A H 0.2307 -0.0188 0.0837 0.135 Uiso 1 1 calc R . . C4 C 0.2220(9) -0.1143(12) 0.1675(11) 0.094(5) Uani 1 1 d . . . H4A H 0.2555 -0.1669 0.1643 0.112 Uiso 1 1 calc R . . C5 C 0.1764(12) -0.1206(13) 0.2062(11) 0.110(7) Uani 1 1 d . . . H5A H 0.1704 -0.1778 0.2365 0.132 Uiso 1 1 calc R . . C6 C 0.2816(11) -0.045(4) 0.3603(14) 0.181(17) Uani 1 1 d . . . H6A H 0.2540 -0.0792 0.3894 0.217 Uiso 1 1 calc R . . C7 C 0.315(2) -0.0862(16) 0.3154(19) 0.18(2) Uani 1 1 d . . . H7A H 0.3162 -0.1590 0.3051 0.220 Uiso 1 1 calc R . . C8 C 0.3586(18) -0.018(5) 0.2978(16) 0.24(3) Uani 1 1 d . . . H8A H 0.3950 -0.0327 0.2727 0.284 Uiso 1 1 calc R . . C9 C 0.3513(16) 0.064(3) 0.330(3) 0.23(2) Uani 1 1 d . . . H9A H 0.3807 0.1234 0.3326 0.273 Uiso 1 1 calc R . . C10 C 0.3037(19) 0.049(2) 0.3661(14) 0.156(13) Uani 1 1 d . . . H10A H 0.2927 0.0977 0.4003 0.187 Uiso 1 1 calc R . . C11 C 0.4105(8) 0.1687(12) 0.0868(8) 0.100(5) Uiso 1 1 d D . . C12 C 0.3890(10) 0.2797(12) 0.0938(10) 0.126(7) Uiso 1 1 d D . . C13 C 0.3765(17) 0.135(3) 0.0127(11) 0.108(11) Uiso 0.50 1 d PD . . C13A C 0.440(2) 0.119(3) 0.0279(17) 0.141(14) Uiso 0.50 1 d PD . . C14 C 0.4847(9) 0.143(2) 0.0898(18) 0.094(9) Uiso 0.50 1 d PD . . C14A C 0.4756(17) 0.186(4) 0.141(2) 0.165(18) Uiso 0.50 1 d PD . . C15A C 0.443(2) 0.318(4) 0.154(2) 0.151(19) Uiso 0.50 1 d PD . . C15 C 0.4389(18) 0.362(3) 0.127(2) 0.120(14) Uiso 0.50 1 d PD . . C16 C 0.3731(17) 0.363(2) 0.0377(15) 0.101(10) Uiso 0.50 1 d PD . . C16A C 0.347(3) 0.287(5) 0.0193(16) 0.20(2) Uiso 0.50 1 d PD . . C17 C 0.0639(15) 0.254(2) 0.3671(14) 0.079(9) Uiso 0.50 1 d PD . . C17A C 0.0898(10) 0.2836(13) 0.3853(11) 0.048(6) Uiso 0.50 1 d PD . . C18 C 0.1031(15) 0.188(2) 0.4265(14) 0.072(8) Uiso 0.50 1 d PD . . C18A C 0.0728(14) 0.1738(15) 0.4043(14) 0.058(7) Uiso 0.50 1 d PD . . C19A C -0.0074(18) 0.199(3) 0.341(2) 0.112(12) Uiso 0.50 1 d PD . . C19 C 0.1376(14) 0.350(2) 0.4371(15) 0.086(9) Uiso 0.50 1 d PD . . C20 C 0.0259(12) 0.346(2) 0.3568(16) 0.085(9) Uiso 0.50 1 d PD . . C20A C 0.0548(16) 0.369(2) 0.3847(17) 0.087(9) Uiso 0.50 1 d PD . . C21A C 0.0048(17) 0.133(3) 0.368(2) 0.114(12) Uiso 0.50 1 d PD . . C21 C 0.161(3) 0.274(4) 0.474(3) 0.173(19) Uiso 0.50 1 d PD . . C22 C 0.0546(16) 0.127(3) 0.4634(17) 0.091(10) Uiso 0.50 1 d PD . . C22A C 0.0889(18) 0.152(3) 0.4870(17) 0.099(11) Uiso 0.50 1 d PD . . 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 0.0661(8) 0.0305(6) 0.0721(9) 0.0012(7) 0.0310(6) 0.0013(6) O1 0.083(6) 0.067(6) 0.093(7) 0.008(5) 0.053(5) 0.020(5) O2 0.161(10) 0.066(7) 0.134(10) 0.031(7) 0.100(8) 0.044(7) O3 0.163(10) 0.044(6) 0.150(10) 0.017(6) 0.099(9) 0.035(6) O4 0.120(8) 0.055(6) 0.134(9) 0.011(6) 0.088(7) -0.007(5) O5 0.143(9) 0.042(6) 0.189(12) 0.019(7) 0.117(9) 0.006(6) O6 0.175(12) 0.059(7) 0.200(14) 0.028(8) 0.145(11) 0.017(7) B1 0.052(9) 0.050(9) 0.085(11) 0.013(9) 0.029(8) 0.008(7) B2 0.070(10) 0.034(8) 0.093(12) 0.008(8) 0.056(9) -0.005(7) C1 0.087(11) 0.125(17) 0.104(13) -0.013(13) 0.024(10) -0.050(12) C2 0.107(14) 0.106(14) 0.088(12) 0.007(12) -0.030(11) 0.004(12) C3 0.124(15) 0.114(17) 0.097(12) 0.013(13) 0.016(11) -0.003(13) C4 0.118(14) 0.041(10) 0.120(15) -0.026(10) 0.018(12) 0.007(9) C5 0.140(17) 0.045(10) 0.130(17) 0.013(10) -0.011(14) -0.035(11) C6 0.115(16) 0.35(5) 0.073(16) 0.09(2) 0.004(13) -0.07(3) C7 0.31(5) 0.051(11) 0.13(3) -0.003(14) -0.12(3) 0.041(18) C8 0.15(3) 0.45(7) 0.12(2) 0.04(4) 0.04(2) 0.21(4) C9 0.080(18) 0.24(4) 0.32(5) 0.10(3) -0.07(2) -0.11(2) C10 0.16(3) 0.15(2) 0.121(19) -0.093(19) -0.066(18) 0.050(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O4 2.011(9) . ? Zr1 O1 2.025(8) . ? Zr1 C7 2.470(19) . ? Zr1 C10 2.482(19) . ? Zr1 C4 2.501(14) . ? Zr1 C8 2.50(2) . ? Zr1 C3 2.509(18) . ? Zr1 C1 2.520(14) . ? Zr1 C6 2.52(2) . ? Zr1 C9 2.53(2) . ? Zr1 C2 2.530(14) . ? Zr1 C5 2.536(15) . ? O1 B1 1.291(16) . ? O2 B1 1.311(17) . ? O2 C17A 1.47(2) . ? O2 C17 1.51(3) . ? O3 B1 1.400(17) . ? O3 C18 1.48(3) . ? O3 C18A 1.50(3) . ? O4 B2 1.280(15) . ? O5 B2 1.360(16) . ? O5 C11 1.418(18) . ? O6 B2 1.357(16) . ? O6 C12 1.44(2) . ? C1 C2 1.36(2) . ? C1 C5 1.41(2) . ? C2 C3 1.39(2) . ? C3 C4 1.37(2) . ? C4 C5 1.30(2) . ? C6 C10 1.31(4) . ? C6 C7 1.33(4) . ? C7 C8 1.34(5) . ? C8 C9 1.26(5) . ? C9 C10 1.32(4) . ? C11 C14 1.533(10) . ? C11 C12 1.538(10) . ? C11 C13A 1.539(10) . ? C11 C14A 1.548(10) . ? C11 C13 1.549(10) . ? C12 C16 1.538(10) . ? C12 C15 1.540(10) . ? C12 C15A 1.546(10) . ? C12 C16A 1.549(10) . ? C13 C13A 1.29(4) . ? C13A C14 1.40(5) . ? C14 C14A 1.20(5) . ? C14A C15A 1.89(7) . ? C15A C15 0.77(6) . ? C15 C16 2.00(5) . ? C16 C16A 1.16(6) . ? C17 C17A 0.69(3) . ? C17 C18A 1.28(3) . ? C17 C20 1.43(4) . ? C17 C18 1.546(10) . ? C17 C20A 1.56(4) . ? C17 C19A 1.61(4) . ? C17 C21A 2.00(5) . ? C17A C20A 1.33(4) . ? C17A C18 1.49(3) . ? C17A C19 1.537(10) . ? C17A C18A 1.546(10) . ? C17A C20 1.549(10) . ? C18 C18A 0.71(3) . ? C18 C22A 1.35(4) . ? C18 C22 1.55(4) . ? C18 C21 1.77(5) . ? C18A C22 1.42(4) . ? C18A C21A 1.53(4) . ? C18A C22A 1.61(4) . ? C18A C19A 1.88(4) . ? C19A C21A 1.03(4) . ? C19 C21 1.26(5) . ? C19 C20A 1.81(4) . ? C20 C20A 0.78(3) . ? C21A C22 1.95(5) . ? C22 C22A 0.83(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zr1 O1 97.6(3) . . ? O4 Zr1 C7 118.1(13) . . ? O1 Zr1 C7 124.8(12) . . ? O4 Zr1 C10 106.5(12) . . ? O1 Zr1 C10 82.1(7) . . ? C7 Zr1 C10 49.5(8) . . ? O4 Zr1 C4 105.6(6) . . ? O1 Zr1 C4 132.1(5) . . ? C7 Zr1 C4 79.2(7) . . ? C10 Zr1 C4 127.9(7) . . ? O4 Zr1 C8 87.4(14) . . ? O1 Zr1 C8 130.1(10) . . ? C7 Zr1 C8 31.3(10) . . ? C10 Zr1 C8 49.4(9) . . ? C4 Zr1 C8 92.8(14) . . ? O4 Zr1 C3 80.4(5) . . ? O1 Zr1 C3 119.1(6) . . ? C7 Zr1 C3 107.9(9) . . ? C10 Zr1 C3 157.2(7) . . ? C4 Zr1 C3 31.7(5) . . ? C8 Zr1 C3 110.7(11) . . ? O4 Zr1 C1 119.8(6) . . ? O1 Zr1 C1 80.1(5) . . ? C7 Zr1 C1 111.0(10) . . ? C10 Zr1 C1 132.0(13) . . ? C4 Zr1 C1 52.0(6) . . ? C8 Zr1 C1 138.6(17) . . ? C3 Zr1 C1 52.2(6) . . ? O4 Zr1 C6 132.3(8) . . ? O1 Zr1 C6 94.0(12) . . ? C7 Zr1 C6 30.8(9) . . ? C10 Zr1 C6 30.3(8) . . ? C4 Zr1 C6 99.9(14) . . ? C8 Zr1 C6 51.4(10) . . ? C3 Zr1 C6 131.6(14) . . ? C1 Zr1 C6 107.7(9) . . ? O4 Zr1 C9 81.5(8) . . ? O1 Zr1 C9 102.3(14) . . ? C7 Zr1 C9 49.8(10) . . ? C10 Zr1 C9 30.4(10) . . ? C4 Zr1 C9 121.9(13) . . ? C8 Zr1 C9 29.1(11) . . ? C3 Zr1 C9 136.4(15) . . ? C1 Zr1 C9 158.4(8) . . ? C6 Zr1 C9 50.9(9) . . ? O4 Zr1 C2 88.9(6) . . ? O1 Zr1 C2 87.6(6) . . ? C7 Zr1 C2 130.2(6) . . ? C10 Zr1 C2 162.4(13) . . ? C4 Zr1 C2 52.4(6) . . ? C8 Zr1 C2 142.3(11) . . ? C3 Zr1 C2 31.9(6) . . ? C1 Zr1 C2 31.2(5) . . ? C6 Zr1 C2 137.8(11) . . ? C9 Zr1 C2 166.9(13) . . ? O4 Zr1 C5 131.6(6) . . ? O1 Zr1 C5 106.8(7) . . ? C7 Zr1 C5 80.6(8) . . ? C10 Zr1 C5 117.6(11) . . ? C4 Zr1 C5 29.9(5) . . ? C8 Zr1 C5 106.1(16) . . ? C3 Zr1 C5 51.3(6) . . ? C1 Zr1 C5 32.5(5) . . ? C6 Zr1 C5 87.5(12) . . ? C9 Zr1 C5 130.4(9) . . ? C2 Zr1 C5 52.2(6) . . ? B1 O1 Zr1 156.0(9) . . ? B1 O2 C17A 113.2(12) . . ? B1 O2 C17 106.6(14) . . ? C17A O2 C17 26.8(12) . . ? B1 O3 C18 107.7(13) . . ? B1 O3 C18A 106.9(12) . . ? C18 O3 C18A 27.4(11) . . ? B2 O4 Zr1 154.2(9) . . ? B2 O5 C11 110.0(11) . . ? B2 O6 C12 112.4(11) . . ? O1 B1 O2 125.7(14) . . ? O1 B1 O3 125.7(13) . . ? O2 B1 O3 108.6(13) . . ? O4 B2 O6 124.1(13) . . ? O4 B2 O5 126.4(12) . . ? O6 B2 O5 108.3(11) . . ? C2 C1 C5 107.0(17) . . ? C2 C1 Zr1 74.8(9) . . ? C5 C1 Zr1 74.4(9) . . ? C1 C2 C3 107.3(17) . . ? C1 C2 Zr1 74.0(9) . . ? C3 C2 Zr1 73.2(10) . . ? C4 C3 C2 107.5(18) . . ? C4 C3 Zr1 73.8(10) . . ? C2 C3 Zr1 74.8(11) . . ? C5 C4 C3 109.9(18) . . ? C5 C4 Zr1 76.5(10) . . ? C3 C4 Zr1 74.5(10) . . ? C4 C5 C1 108.3(17) . . ? C4 C5 Zr1 73.6(10) . . ? C1 C5 Zr1 73.1(8) . . ? C10 C6 C7 104(2) . . ? C10 C6 Zr1 73.1(14) . . ? C7 C6 Zr1 72.3(12) . . ? C6 C7 C8 109(3) . . ? C6 C7 Zr1 76.8(14) . . ? C8 C7 Zr1 75.8(14) . . ? C9 C8 C7 108(3) . . ? C9 C8 Zr1 76.5(16) . . ? C7 C8 Zr1 73.0(15) . . ? C8 C9 C10 108(3) . . ? C8 C9 Zr1 74.4(19) . . ? C10 C9 Zr1 72.9(12) . . ? C6 C10 C9 111(3) . . ? C6 C10 Zr1 76.6(12) . . ? C9 C10 Zr1 76.7(17) . . ? O5 C11 C14 117.6(17) . . ? O5 C11 C12 106.1(13) . . ? C14 C11 C12 120.0(18) . . ? O5 C11 C13A 121(2) . . ? C14 C11 C13A 54.4(19) . . ? C12 C11 C13A 129(2) . . ? O5 C11 C14A 99(2) . . ? C14 C11 C14A 46(2) . . ? C12 C11 C14A 91(2) . . ? C13A C11 C14A 100(3) . . ? O5 C11 C13 101.3(18) . . ? C14 C11 C13 104(2) . . ? C12 C11 C13 105.8(18) . . ? C13A C11 C13 49.2(18) . . ? C14A C11 C13 149(3) . . ? O6 C12 C11 99.7(13) . . ? O6 C12 C16 109.0(18) . . ? C11 C12 C16 129(2) . . ? O6 C12 C15 117(2) . . ? C11 C12 C15 122(2) . . ? C16 C12 C15 81(2) . . ? O6 C12 C15A 104(3) . . ? C11 C12 C15A 102(2) . . ? C16 C12 C15A 110(3) . . ? C15 C12 C15A 29(2) . . ? O6 C12 C16A 93(3) . . ? C11 C12 C16A 95(3) . . ? C16 C12 C16A 44(2) . . ? C15 C12 C16A 124(3) . . ? C15A C12 C16A 153(4) . . ? C13A C13 C11 65.0(10) . . ? C13 C13A C14 128.4(14) . . ? C13 C13A C11 65.8(11) . . ? C14 C13A C11 62.6(11) . . ? C14A C14 C13A 130.7(16) . . ? C14A C14 C11 67.8(12) . . ? C13A C14 C11 63.0(11) . . ? C14 C14A C11 66.5(12) . . ? C14 C14A C15A 132(4) . . ? C11 C14A C15A 88(2) . . ? C15 C15A C12 75.0(16) . . ? C15 C15A C14A 126(7) . . ? C12 C15A C14A 79(2) . . ? C15A C15 C12 76.0(16) . . ? C15A C15 C16 125.4(19) . . ? C12 C15 C16 49.5(12) . . ? C16A C16 C12 68.5(14) . . ? C16A C16 C15 117.6(18) . . ? C12 C16 C15 49.6(12) . . ? C16 C16A C12 67.5(13) . . ? C17A C17 C18A 99(3) . . ? C17A C17 C20 87(3) . . ? C18A C17 C20 143(3) . . ? C17A C17 O2 74(4) . . ? C18A C17 O2 109(2) . . ? C20 C17 O2 107(2) . . ? C17A C17 C18 72(3) . . ? C18A C17 C18 27.0(13) . . ? C20 C17 C18 140(3) . . ? O2 C17 C18 98(2) . . ? C17A C17 C20A 58(3) . . ? C18A C17 C20A 133(3) . . ? C20 C17 C20A 29.9(14) . . ? O2 C17 C20A 102(2) . . ? C18 C17 C20A 116(3) . . ? C17A C17 C19A 164(5) . . ? C18A C17 C19A 80(3) . . ? C20 C17 C19A 85(2) . . ? O2 C17 C19A 122(3) . . ? C18 C17 C19A 107(3) . . ? C20A C17 C19A 112(3) . . ? C17A C17 C21A 147(3) . . ? C18A C17 C21A 49.7(19) . . ? C20 C17 C21A 112(2) . . ? O2 C17 C21A 122(2) . . ? C18 C17 C21A 77(2) . . ? C20A C17 C21A 132(3) . . ? C19A C17 C21A 30.8(16) . . ? C17 C17A C20A 96(3) . . ? C17 C17A O2 79(4) . . ? C20A C17A O2 117(2) . . ? C17 C17A C18 82(2) . . ? C20A C17A C18 139(3) . . ? O2 C17A C18 102.7(17) . . ? C17 C17A C19 168(5) . . ? C20A C17A C19 78(2) . . ? O2 C17A C19 112.7(19) . . ? C18 C17A C19 95(2) . . ? C17 C17A C18A 55(2) . . ? C20A C17A C18A 130(2) . . ? O2 C17A C18A 98.1(15) . . ? C18 C17A C18A 26.9(12) . . ? C19 C17A C18A 121(2) . . ? C17 C17A C20 67(3) . . ? C20A C17A C20 30.3(15) . . ? O2 C17A C20 103.0(17) . . ? C18 C17A C20 134(2) . . ? C19 C17A C20 109(2) . . ? C18A C17A C20 112(2) . . ? C18A C18 C22A 98(4) . . ? C18A C18 O3 78(4) . . ? C22A C18 O3 118(2) . . ? C18A C18 C17A 81(2) . . ? C22A C18 C17A 136(3) . . ? O3 C18 C17A 104.9(19) . . ? C18A C18 C17 55(2) . . ? C22A C18 C17 134(3) . . ? O3 C18 C17 94(2) . . ? C17A C18 C17 26.3(12) . . ? C18A C18 C22 66(3) . . ? C22A C18 C22 32.4(17) . . ? O3 C18 C22 105(2) . . ? C17A C18 C22 129(2) . . ? C17 C18 C22 111(3) . . ? C18A C18 C21 156(4) . . ? C22A C18 C21 90(3) . . ? O3 C18 C21 119(3) . . ? C17A C18 C21 77(2) . . ? C17 C18 C21 103(3) . . ? C22 C18 C21 121(3) . . ? C18 C18A C17 98(3) . . ? C18 C18A C22 87(4) . . ? C17 C18A C22 143(3) . . ? C18 C18A O3 75(4) . . ? C17 C18A O3 106(2) . . ? C22 C18A O3 111(2) . . ? C18 C18A C21A 170(4) . . ? C17 C18A C21A 91(3) . . ? C22 C18A C21A 83(2) . . ? O3 C18A C21A 108(2) . . ? C18 C18A C17A 72(3) . . ? C17 C18A C17A 26.2(14) . . ? C22 C18A C17A 135(2) . . ? O3 C18A C17A 101.2(16) . . ? C21A C18A C17A 116(2) . . ? C18 C18A C22A 56(3) . . ? C17 C18A C22A 134(3) . . ? C22 C18A C22A 31.0(16) . . ? O3 C18A C22A 103(2) . . ? C21A C18A C22A 114(2) . . ? C17A C18A C22A 113(2) . . ? C18 C18A C19A 154(3) . . ? C17 C18A C19A 58(2) . . ? C22 C18A C19A 107(2) . . ? O3 C18A C19A 118(2) . . ? C21A C18A C19A 33.2(17) . . ? C17A C18A C19A 83.0(17) . . ? C22A C18A C19A 133(2) . . ? C21A C19A C17 96(4) . . ? C21A C19A C18A 54(3) . . ? C17 C19A C18A 42.1(14) . . ? C21 C19 C17A 93(3) . . ? C21 C19 C20A 130(3) . . ? C17A C19 C20A 45.7(14) . . ? C20A C20 C17 85(3) . . ? C20A C20 C17A 59(3) . . ? C17 C20 C17A 26.5(13) . . ? C20 C20A C17A 91(3) . . ? C20 C20A C17 65(3) . . ? C17A C20A C17 26.1(13) . . ? C20 C20A C19 147(4) . . ? C17A C20A C19 56.0(15) . . ? C17 C20A C19 81.8(19) . . ? C19A C21A C18A 93(4) . . ? C19A C21A C22 124(4) . . ? C18A C21A C22 46.2(15) . . ? C19A C21A C17 53(3) . . ? C18A C21A C17 39.7(14) . . ? C22 C21A C17 80.5(17) . . ? C19 C21 C18 93(3) . . ? C22A C22 C18A 88(4) . . ? C22A C22 C18 61(3) . . ? C18A C22 C18 27.1(13) . . ? C22A C22 C21A 138(4) . . ? C18A C22 C21A 51.1(19) . . ? C18 C22 C21A 78(2) . . ? C22 C22A C18 87(4) . . ? C22 C22A C18A 61(3) . . ? C18 C22A C18A 25.8(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.999 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.127 #===end