# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Mikhail V. Barybin' 'Malcolm H. Chisholm' 'Nathan J. Patmore' 'Randall E. Robinson' _publ_contact_author_address ; Department of Chemistry The Ohio State University 100 West 18th Avenue Columbus Ohio 43210 UNITED STATES OF AMERICA ; _publ_contact_author_email chisholm@chemistry.ohio-state.edu _publ_contact_author_name 'Malcolm Chisholm' _publ_section_title ; Concerning the Molecular and Electronic Structure of a Tungsten-Tungsten Quadruply Bonded Complex Supported by Two 6-Carboethoxy-2-carboxylatoazulene Ligands ; data_trans-W2(TiPB)2(Azu-2)2 _database_code_depnum_ccdc_archive 'CCDC 622539' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H68 O12 W2, 2(C4 H8 O)' _chemical_formula_sum 'C68 H84 O14 W2' _chemical_formula_weight 1493.05 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 10.358(3) _cell_length_b 10.563(3) _cell_length_c 17.222(7) _cell_angle_alpha 106.775(10) _cell_angle_beta 93.233(10) _cell_angle_gamma 114.97(2) _cell_volume 1600.6(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Rectangular Plate' _exptl_crystal_colour Green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 3.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '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 14874 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 23.04 _reflns_number_total 4440 _reflns_number_gt 3244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4440 _refine_ls_number_parameters 380 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 W1 W 0.40312(4) 0.51539(4) 0.51213(3) 0.03864(19) Uani 1 1 d . . . O1 O 0.2695(5) 0.3098(6) 0.4290(4) 0.0402(16) Uani 1 1 d . . . O2 O 0.5327(6) 0.7224(6) 0.5960(4) 0.0376(15) Uani 1 1 d . . . O3 O 0.4130(5) 0.6071(6) 0.4204(4) 0.0390(16) Uani 1 1 d . . . O4 O 0.3899(5) 0.4246(5) 0.6049(4) 0.0354(15) Uani 1 1 d . . . O5 O -0.1078(7) -0.6916(7) 0.0380(4) 0.0573(19) Uani 1 1 d . . . O6 O -0.3048(8) -0.6571(8) 0.0369(5) 0.092(3) Uani 1 1 d . . . O7 O 0.1858(6) 0.5331(6) 0.5719(4) 0.0469(18) Uani 1 1 d . . . C1 C 0.2860(9) -0.0265(9) 0.2976(6) 0.043(2) Uani 1 1 d . . . H1 H 0.3852 -0.0063 0.3024 0.051 Uiso 1 1 calc R . . C2 C 0.2360(8) 0.0756(9) 0.3358(6) 0.039(2) Uani 1 1 d . . . C3 C 0.0821(9) 0.0053(10) 0.3127(6) 0.044(3) Uani 1 1 d . . . H3 H 0.0213 0.0501 0.3303 0.053 Uiso 1 1 calc R . . C4 C -0.1089(10) -0.2486(10) 0.2246(7) 0.051(3) Uani 1 1 d . . . H4 H -0.1817 -0.2216 0.2425 0.061 Uiso 1 1 calc R . . C5 C -0.1582(10) -0.3878(10) 0.1679(7) 0.058(3) Uani 1 1 d . . . H5 H -0.2611 -0.4426 0.1508 0.069 Uiso 1 1 calc R . . C6 C -0.0823(10) -0.4631(10) 0.1309(6) 0.051(3) Uani 1 1 d . . . C7 C 0.0638(10) -0.4203(10) 0.1481(6) 0.051(3) Uani 1 1 d . . . H7 H 0.0938 -0.4909 0.1187 0.061 Uiso 1 1 calc R . . C8 C 0.1745(10) -0.2861(10) 0.2032(6) 0.049(3) Uani 1 1 d . . . H8 H 0.2688 -0.2804 0.2079 0.059 Uiso 1 1 calc R . . C9 C 0.1681(9) -0.1614(9) 0.2516(6) 0.040(2) Uani 1 1 d . . . C10 C 0.0347(9) -0.1406(9) 0.2598(6) 0.044(3) Uani 1 1 d . . . C11 C 0.3268(8) 0.2265(9) 0.3904(6) 0.036(2) Uani 1 1 d . . . C12 C -0.1765(11) -0.6141(11) 0.0647(7) 0.058(3) Uani 1 1 d . . . C13 C -0.1886(11) -0.8305(10) -0.0286(7) 0.063(3) Uani 1 1 d . . . H13A H -0.2343 -0.8156 -0.0751 0.075 Uiso 1 1 calc R . . H13B H -0.2663 -0.9017 -0.0097 0.075 Uiso 1 1 calc R . . C14 C -0.0840(13) -0.8893(11) -0.0562(8) 0.079(4) Uani 1 1 d . . . H14A H -0.1358 -0.9842 -0.1022 0.118 Uiso 1 1 calc R . . H14B H -0.0404 -0.9047 -0.0099 0.118 Uiso 1 1 calc R . . H14C H -0.0072 -0.8177 -0.0744 0.118 Uiso 1 1 calc R . . C15 C 0.5178(9) 0.6217(8) 0.3802(5) 0.031(2) Uani 1 1 d . . . C16 C 0.5324(8) 0.6894(9) 0.3159(6) 0.037(2) Uani 1 1 d . . . C17 C 0.4794(9) 0.5978(10) 0.2315(7) 0.046(3) Uani 1 1 d . . . C18 C 0.5022(9) 0.6708(10) 0.1737(6) 0.044(3) Uani 1 1 d . . . H18 H 0.4660 0.6117 0.1167 0.053 Uiso 1 1 calc R . . C19 C 0.5745(10) 0.8239(11) 0.1946(6) 0.044(2) Uani 1 1 d . B . C20 C 0.6222(9) 0.9097(10) 0.2782(6) 0.037(2) Uani 1 1 d . . . H20 H 0.6704 1.0150 0.2940 0.044 Uiso 1 1 calc R . . C21 C 0.6007(8) 0.8440(9) 0.3403(6) 0.036(2) Uani 1 1 d . . . C22 C 0.6624(8) 0.9394(9) 0.4311(6) 0.038(2) Uani 1 1 d . . . H22 H 0.5999 0.8819 0.4633 0.046 Uiso 1 1 calc R . . C23 C 0.6568(9) 1.0877(9) 0.4549(6) 0.048(3) Uani 1 1 d . . . H23A H 0.5571 1.0698 0.4372 0.072 Uiso 1 1 calc R . . H23B H 0.7222 1.1509 0.4276 0.072 Uiso 1 1 calc R . . H23C H 0.6875 1.1376 0.5151 0.072 Uiso 1 1 calc R . . C24 C 0.8148(9) 0.9640(10) 0.4587(6) 0.051(3) Uani 1 1 d . . . H24A H 0.8502 1.0250 0.5176 0.077 Uiso 1 1 calc R . . H24B H 0.8792 1.0151 0.4262 0.077 Uiso 1 1 calc R . . H24C H 0.8140 0.8678 0.4501 0.077 Uiso 1 1 calc R . . C25 C 0.4010(10) 0.4297(9) 0.2064(7) 0.055(3) Uani 1 1 d . . . H25 H 0.4538 0.4020 0.2436 0.066 Uiso 1 1 calc R . . C26 C 0.3990(15) 0.3456(13) 0.1179(9) 0.123(6) Uani 1 1 d . . . H26A H 0.4988 0.3794 0.1088 0.185 Uiso 1 1 calc R . . H26B H 0.3422 0.3646 0.0792 0.185 Uiso 1 1 calc R . . H26C H 0.3546 0.2388 0.1086 0.185 Uiso 1 1 calc R . . C27 C 0.2473(11) 0.3743(11) 0.2196(8) 0.080(4) Uani 1 1 d . . . H27A H 0.2006 0.2656 0.2027 0.120 Uiso 1 1 calc R . . H27B H 0.1931 0.4041 0.1863 0.120 Uiso 1 1 calc R . . H27C H 0.2481 0.4172 0.2783 0.120 Uiso 1 1 calc R . . C28 C 0.6006(10) 0.8947(12) 0.1281(7) 0.055(3) Uani 1 1 d D . . H28 H 0.5447 0.8203 0.0720 0.067 Uiso 1 1 calc R A 1 C29 C 0.773(2) 0.975(5) 0.131(2) 0.081(11) Uiso 0.48(5) 1 d PD B 1 H29A H 0.8091 0.9005 0.1200 0.122 Uiso 0.48(5) 1 calc PR B 1 H29B H 0.8236 1.0511 0.1852 0.122 Uiso 0.48(5) 1 calc PR B 1 H29C H 0.7909 1.0211 0.0879 0.122 Uiso 0.48(5) 1 calc PR B 1 C29A C 0.743(2) 0.894(4) 0.1007(17) 0.051(9) Uiso 0.52(5) 1 d PD B 2 H29D H 0.7383 0.7959 0.0925 0.076 Uiso 0.52(5) 1 calc PR B 2 H29E H 0.8283 0.9703 0.1438 0.076 Uiso 0.52(5) 1 calc PR B 2 H29F H 0.7515 0.9142 0.0487 0.076 Uiso 0.52(5) 1 calc PR B 2 C30 C 0.5795(12) 1.0302(12) 0.1459(7) 0.069(3) Uani 1 1 d . B . H30A H 0.5966 1.0671 0.0994 0.103 Uiso 1 1 calc R . . H30B H 0.6482 1.1071 0.1965 0.103 Uiso 1 1 calc R . . H30C H 0.4797 1.0057 0.1534 0.103 Uiso 1 1 calc R . . C31 C 0.0516(9) 0.4005(10) 0.5604(7) 0.061(3) Uani 1 1 d . . . H31A H 0.0728 0.3226 0.5701 0.073 Uiso 1 1 calc R . . H31B H -0.0051 0.3609 0.5032 0.073 Uiso 1 1 calc R . . C32 C -0.0330(10) 0.4446(12) 0.6222(7) 0.074(4) Uani 1 1 d . . . H32A H -0.0650 0.3764 0.6542 0.088 Uiso 1 1 calc R . . H32B H -0.1197 0.4434 0.5939 0.088 Uiso 1 1 calc R . . C33 C 0.0730(11) 0.6006(13) 0.6783(8) 0.081(4) Uani 1 1 d . . . H33A H 0.0499 0.6753 0.6656 0.097 Uiso 1 1 calc R . . H33B H 0.0719 0.6118 0.7373 0.097 Uiso 1 1 calc R . . C34 C 0.2161(10) 0.6163(10) 0.6590(7) 0.055(3) Uani 1 1 d . . . H34A H 0.2852 0.7222 0.6711 0.066 Uiso 1 1 calc R . . H34B H 0.2584 0.5752 0.6921 0.066 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 W1 0.0333(2) 0.0358(2) 0.0503(3) 0.01803(19) 0.01516(17) 0.01609(17) O1 0.034(3) 0.037(3) 0.058(5) 0.020(3) 0.017(3) 0.021(3) O2 0.035(3) 0.044(3) 0.044(4) 0.024(3) 0.018(3) 0.021(3) O3 0.032(3) 0.034(3) 0.056(5) 0.017(3) 0.015(3) 0.018(3) O4 0.029(3) 0.029(3) 0.056(5) 0.016(3) 0.017(3) 0.018(3) O5 0.064(4) 0.045(4) 0.057(5) 0.008(4) 0.016(4) 0.026(4) O6 0.056(5) 0.077(5) 0.101(8) -0.022(5) -0.001(5) 0.031(4) O7 0.033(3) 0.036(3) 0.067(6) 0.009(4) 0.006(3) 0.018(3) C1 0.035(5) 0.047(6) 0.047(7) 0.015(5) 0.010(5) 0.020(5) C2 0.032(5) 0.047(6) 0.045(7) 0.020(5) 0.019(5) 0.021(5) C3 0.035(5) 0.051(6) 0.055(7) 0.020(5) 0.019(5) 0.025(5) C4 0.044(6) 0.051(6) 0.056(8) 0.011(6) 0.011(5) 0.024(5) C5 0.043(6) 0.052(6) 0.065(8) 0.004(6) 0.007(5) 0.020(5) C6 0.045(6) 0.047(6) 0.052(8) 0.005(5) 0.012(5) 0.023(5) C7 0.051(6) 0.045(6) 0.049(7) 0.006(5) 0.012(5) 0.022(5) C8 0.051(6) 0.055(6) 0.048(7) 0.021(6) 0.011(5) 0.027(5) C9 0.035(5) 0.041(5) 0.045(7) 0.012(5) 0.011(5) 0.019(5) C10 0.035(5) 0.037(5) 0.053(7) 0.007(5) 0.008(5) 0.015(5) C11 0.031(5) 0.037(5) 0.037(6) 0.016(5) 0.009(4) 0.010(4) C12 0.049(7) 0.060(7) 0.052(8) 0.012(6) 0.013(6) 0.017(6) C13 0.079(8) 0.040(6) 0.050(8) 0.010(6) 0.028(6) 0.012(6) C14 0.106(9) 0.052(7) 0.074(10) 0.014(6) 0.047(8) 0.034(7) C15 0.039(5) 0.030(5) 0.033(6) 0.015(4) 0.020(4) 0.019(4) C16 0.031(5) 0.038(5) 0.044(7) 0.014(5) 0.008(5) 0.018(4) C17 0.033(5) 0.048(6) 0.059(8) 0.019(6) 0.017(5) 0.019(4) C18 0.042(5) 0.053(6) 0.035(7) 0.005(5) 0.008(5) 0.025(5) C19 0.055(6) 0.068(7) 0.030(7) 0.021(6) 0.016(5) 0.041(5) C20 0.045(5) 0.040(5) 0.040(7) 0.024(5) 0.023(5) 0.025(4) C21 0.034(5) 0.036(5) 0.041(7) 0.011(5) 0.013(4) 0.021(4) C22 0.033(5) 0.033(5) 0.045(7) 0.014(5) 0.015(5) 0.010(4) C23 0.051(6) 0.051(6) 0.051(7) 0.017(5) 0.020(5) 0.031(5) C24 0.055(6) 0.061(6) 0.044(7) 0.023(5) 0.008(5) 0.029(5) C25 0.052(6) 0.041(6) 0.057(8) 0.000(5) 0.007(5) 0.019(5) C26 0.126(12) 0.060(8) 0.125(14) -0.016(9) 0.062(11) 0.018(8) C27 0.063(7) 0.053(6) 0.123(12) 0.029(7) 0.030(7) 0.025(6) C28 0.065(6) 0.078(7) 0.041(7) 0.025(6) 0.019(5) 0.045(6) C30 0.092(8) 0.078(8) 0.050(8) 0.040(6) 0.023(7) 0.039(7) C31 0.034(5) 0.054(6) 0.091(10) 0.021(6) 0.011(6) 0.018(5) C32 0.041(6) 0.083(8) 0.072(9) 0.018(7) 0.020(6) 0.011(6) C33 0.071(8) 0.094(9) 0.083(10) 0.034(8) 0.043(7) 0.037(7) C34 0.055(6) 0.050(6) 0.054(8) 0.019(6) 0.023(6) 0.017(5) _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 W1 O1 2.031(6) . ? W1 O2 2.037(6) . ? W1 O3 2.065(6) . ? W1 O4 2.071(6) . ? W1 W1 2.2081(7) 2_666 ? O1 C11 1.311(9) . ? O2 C11 1.300(9) 2_666 ? O3 C15 1.298(9) . ? O4 C15 1.288(9) 2_666 ? O5 C12 1.304(11) . ? O5 C13 1.432(11) . ? O6 C12 1.223(11) . ? O7 C34 1.440(11) . ? O7 C31 1.449(10) . ? C1 C9 1.385(11) . ? C1 C2 1.402(11) . ? C2 C3 1.417(11) . ? C2 C11 1.442(11) . ? C3 C10 1.395(12) . ? C4 C5 1.363(12) . ? C4 C10 1.396(12) . ? C5 C6 1.396(12) . ? C6 C7 1.371(12) . ? C6 C12 1.519(13) . ? C7 C8 1.398(12) . ? C8 C9 1.371(12) . ? C9 C10 1.496(11) . ? C11 O2 1.300(9) 2_666 ? C13 C14 1.498(13) . ? C15 O4 1.288(9) 2_666 ? C15 C16 1.465(12) . ? C16 C21 1.393(11) . ? C16 C17 1.414(13) . ? C17 C18 1.399(13) . ? C17 C25 1.517(12) . ? C18 C19 1.384(12) . ? C19 C20 1.388(12) . ? C19 C28 1.516(13) . ? C20 C21 1.415(12) . ? C21 C22 1.516(12) . ? C22 C24 1.511(11) . ? C22 C23 1.528(11) . ? C25 C27 1.503(12) . ? C25 C26 1.520(16) . ? C28 C30 1.486(13) . ? C28 C29A 1.579(15) . ? C28 C29 1.612(18) . ? C31 C32 1.512(13) . ? C32 C33 1.512(14) . ? C33 C34 1.488(12) . ? 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 W1 O2 178.6(2) . . ? O1 W1 O3 90.4(2) . . ? O2 W1 O3 89.5(2) . . ? O1 W1 O4 89.8(2) . . ? O2 W1 O4 90.3(2) . . ? O3 W1 O4 178.8(2) . . ? O1 W1 W1 91.14(15) . 2_666 ? O2 W1 W1 90.30(15) . 2_666 ? O3 W1 W1 91.35(14) . 2_666 ? O4 W1 W1 89.84(14) . 2_666 ? C11 O1 W1 119.0(5) . . ? C11 O2 W1 119.7(5) 2_666 . ? C15 O3 W1 118.2(5) . . ? C15 O4 W1 119.6(5) 2_666 . ? C12 O5 C13 116.9(8) . . ? C34 O7 C31 103.4(7) . . ? C9 C1 C2 109.3(7) . . ? C1 C2 C3 108.7(8) . . ? C1 C2 C11 125.3(7) . . ? C3 C2 C11 126.0(8) . . ? C10 C3 C2 108.7(8) . . ? C5 C4 C10 128.4(9) . . ? C4 C5 C6 130.6(9) . . ? C7 C6 C5 128.6(9) . . ? C7 C6 C12 116.6(9) . . ? C5 C6 C12 114.8(8) . . ? C6 C7 C8 128.3(9) . . ? C9 C8 C7 130.0(9) . . ? C8 C9 C1 126.1(8) . . ? C8 C9 C10 126.9(8) . . ? C1 C9 C10 106.8(7) . . ? C3 C10 C4 127.1(8) . . ? C3 C10 C9 106.4(7) . . ? C4 C10 C9 126.5(8) . . ? O2 C11 O1 119.9(7) 2_666 . ? O2 C11 C2 119.1(8) 2_666 . ? O1 C11 C2 120.9(7) . . ? O6 C12 O5 122.8(9) . . ? O6 C12 C6 122.7(10) . . ? O5 C12 C6 114.4(9) . . ? O5 C13 C14 107.4(9) . . ? O4 C15 O3 120.9(8) 2_666 . ? O4 C15 C16 118.4(7) 2_666 . ? O3 C15 C16 120.6(7) . . ? C21 C16 C17 121.8(9) . . ? C21 C16 C15 118.3(8) . . ? C17 C16 C15 119.9(8) . . ? C18 C17 C16 116.4(8) . . ? C18 C17 C25 122.6(10) . . ? C16 C17 C25 121.0(9) . . ? C19 C18 C17 124.1(9) . . ? C18 C19 C20 117.6(9) . . ? C18 C19 C28 121.0(9) . . ? C20 C19 C28 121.5(9) . . ? C19 C20 C21 121.6(8) . . ? C16 C21 C20 118.4(9) . . ? C16 C21 C22 120.7(8) . . ? C20 C21 C22 120.7(7) . . ? C24 C22 C21 112.0(7) . . ? C24 C22 C23 110.5(7) . . ? C21 C22 C23 114.2(8) . . ? C27 C25 C17 112.0(8) . . ? C27 C25 C26 108.7(9) . . ? C17 C25 C26 114.9(10) . . ? C30 C28 C19 115.0(8) . . ? C30 C28 C29A 121.1(13) . . ? C19 C28 C29A 106.2(10) . . ? C30 C28 C29 97.0(18) . . ? C19 C28 C29 108.9(13) . . ? C29A C28 C29 28.0(12) . . ? O7 C31 C32 107.0(8) . . ? C31 C32 C33 104.5(8) . . ? C34 C33 C32 103.5(9) . . ? O7 C34 C33 105.3(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.04 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.828 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.138