Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Jones, Cameron' 'Junk, Peter' 'Williams, Thomas C.' _publ_contact_author_name 'Dr Cameron Jones' _publ_contact_author_address ; Department of Chemistry University of Wales P.O. Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email 'JONESCA6@CARDIFF.AC.UK' _publ_section_title ; Synthesis and Structural Characterisation of the First Tris(diacylpnictido)phosphines, P[E{C(O)R}2]3, E=P or As,R = Rut or Ph ; data_compound_3 _database_code_CSD 184013 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 As3 O6 P' _chemical_formula_weight 766.46 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' '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' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' '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' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 17.372(4) _cell_length_b 17.372(4) _cell_length_c 21.520(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5624(3) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 2.736 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6107 _exptl_absorpt_correction_T_max 0.7006 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Smart CCD' _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 8007 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1469 _reflns_number_gt 1363 _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^)+(0.1191P)^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 SHELXL _refine_ls_extinction_coef 0.00000(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.55(4) _refine_ls_number_reflns 1469 _refine_ls_number_parameters 129 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.004 _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 As1 As 0.20255(5) 0.65243(5) 0.41653(6) 0.0316(3) Uani 1 1 d . . . P1 P 0.3333 0.6667 0.4541(2) 0.0322(9) Uani 1 3 d S . . O1 O 0.2298(5) 0.5527(5) 0.3230(4) 0.051(2) Uani 1 1 d . . . C1 C 0.1789(6) 0.5773(6) 0.3377(5) 0.037(2) Uani 1 1 d . . . O2 O 0.1167(6) 0.4720(5) 0.4556(4) 0.063(2) Uani 1 1 d . . . C2 C 0.0985(7) 0.5591(7) 0.3003(5) 0.046(2) Uani 1 1 d . . . C3 C 0.0160(7) 0.5256(13) 0.3423(7) 0.096(6) Uani 1 1 d . . . H3A H 0.0207 0.5746 0.3669 0.144 Uiso 1 1 calc R . . H3B H 0.0123 0.4796 0.3698 0.144 Uiso 1 1 calc R . . H3C H -0.0370 0.5016 0.3168 0.144 Uiso 1 1 calc R . . C4 C 0.0812(10) 0.4884(7) 0.2503(6) 0.064(3) Uani 1 1 d . . . H4A H 0.0365 0.4843 0.2214 0.096 Uiso 1 1 calc R . . H4B H 0.0605 0.4312 0.2702 0.096 Uiso 1 1 calc R . . H4C H 0.1360 0.5052 0.2281 0.096 Uiso 1 1 calc R . . C5 C 0.1209(11) 0.6450(9) 0.2690(7) 0.083(5) Uani 1 1 d . . . H5A H 0.1306 0.6893 0.3002 0.125 Uiso 1 1 calc R . . H5B H 0.0722 0.6358 0.2422 0.125 Uiso 1 1 calc R . . H5C H 0.1744 0.6653 0.2444 0.125 Uiso 1 1 calc R . . C6 C 0.1354(6) 0.5448(7) 0.4736(5) 0.042(3) Uani 1 1 d . . . C7 C 0.1033(6) 0.5603(6) 0.5359(5) 0.037(2) Uani 1 1 d . . . C8 C 0.0227(8) 0.5723(9) 0.5227(7) 0.068(4) Uani 1 1 d . . . H8A H 0.0035 0.5869 0.5610 0.102 Uiso 1 1 calc R . . H8B H -0.0256 0.5176 0.5058 0.102 Uiso 1 1 calc R . . H8C H 0.0394 0.6200 0.4929 0.102 Uiso 1 1 calc R . . C9 C 0.0721(10) 0.4797(8) 0.5778(6) 0.065(4) Uani 1 1 d . . . H9A H 0.1230 0.4817 0.5979 0.098 Uiso 1 1 calc R . . H9B H 0.0412 0.4260 0.5532 0.098 Uiso 1 1 calc R . . H9C H 0.0321 0.4801 0.6091 0.098 Uiso 1 1 calc R . . C10 C 0.1738(9) 0.6422(7) 0.5680(6) 0.061(3) Uani 1 1 d . . . H10A H 0.2254 0.6359 0.5758 0.092 Uiso 1 1 calc R . . H10B H 0.1509 0.6500 0.6071 0.092 Uiso 1 1 calc R . . H10C H 0.1908 0.6937 0.5418 0.092 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 As1 0.0267(5) 0.0301(6) 0.0399(6) -0.0012(5) -0.0002(4) 0.0156(4) P1 0.0288(13) 0.0288(13) 0.039(3) 0.000 0.000 0.0144(7) O1 0.050(4) 0.063(5) 0.048(5) -0.010(4) -0.007(4) 0.033(4) C1 0.036(5) 0.030(5) 0.043(6) -0.001(4) 0.001(5) 0.015(4) O2 0.081(6) 0.025(4) 0.066(6) -0.012(4) 0.018(4) 0.013(4) C2 0.050(6) 0.050(6) 0.043(6) -0.003(5) -0.004(5) 0.030(5) C3 0.030(7) 0.159(16) 0.077(11) 0.008(10) -0.003(7) 0.031(8) C4 0.069(8) 0.057(7) 0.062(8) -0.015(6) -0.027(7) 0.029(6) C5 0.106(11) 0.066(8) 0.090(12) 0.003(7) -0.050(10) 0.052(9) C6 0.031(5) 0.048(7) 0.046(6) 0.011(5) 0.007(5) 0.020(5) C7 0.029(5) 0.041(5) 0.036(6) -0.005(4) 0.005(4) 0.014(4) C8 0.055(8) 0.085(9) 0.071(9) -0.001(7) 0.011(7) 0.040(7) C9 0.098(10) 0.044(6) 0.044(7) 0.000(5) 0.006(7) 0.028(7) C10 0.061(8) 0.052(7) 0.056(8) -0.011(6) 0.009(6) 0.017(6) _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 As1 C6 2.046(10) . ? As1 C1 2.053(10) . ? As1 P1 2.3054(19) . ? P1 As1 2.3054(19) 3_565 ? P1 As1 2.3054(19) 2_665 ? O1 C1 1.201(12) . ? C1 C2 1.503(15) . ? O2 C6 1.203(13) . ? C2 C5 1.500(16) . ? C2 C3 1.541(16) . ? C2 C4 1.546(15) . ? C6 C7 1.525(14) . ? C7 C10 1.504(15) . ? C7 C9 1.519(15) . ? C7 C8 1.542(15) . ? 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 C6 As1 C1 94.3(4) . . ? C6 As1 P1 88.2(3) . . ? C1 As1 P1 103.4(3) . . ? As1 P1 As1 108.39(11) . 3_565 ? As1 P1 As1 108.39(11) . 2_665 ? As1 P1 As1 108.39(11) 3_565 2_665 ? O1 C1 C2 123.9(9) . . ? O1 C1 As1 119.7(8) . . ? C2 C1 As1 116.4(7) . . ? C5 C2 C1 106.2(9) . . ? C5 C2 C3 111.7(12) . . ? C1 C2 C3 111.0(10) . . ? C5 C2 C4 109.2(11) . . ? C1 C2 C4 109.2(9) . . ? C3 C2 C4 109.5(11) . . ? O2 C6 C7 122.6(9) . . ? O2 C6 As1 119.8(8) . . ? C7 C6 As1 117.3(7) . . ? C10 C7 C9 110.2(10) . . ? C10 C7 C6 111.9(8) . . ? C9 C7 C6 110.7(9) . . ? C10 C7 C8 108.8(10) . . ? C9 C7 C8 107.7(10) . . ? C6 C7 C8 107.4(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 As1 P1 As1 -172.2(3) . . . 3_565 ? C1 As1 P1 As1 93.8(3) . . . 3_565 ? C6 As1 P1 As1 70.3(3) . . . 2_665 ? C1 As1 P1 As1 -23.6(3) . . . 2_665 ? C6 As1 C1 O1 -88.7(9) . . . . ? P1 As1 C1 O1 0.4(9) . . . . ? C6 As1 C1 C2 93.2(7) . . . . ? P1 As1 C1 C2 -177.6(7) . . . . ? O1 C1 C2 C5 -105.2(12) . . . . ? As1 C1 C2 C5 72.8(11) . . . . ? O1 C1 C2 C3 133.3(13) . . . . ? As1 C1 C2 C3 -48.7(12) . . . . ? O1 C1 C2 C4 12.4(15) . . . . ? As1 C1 C2 C4 -169.6(8) . . . . ? C1 As1 C6 O2 14.9(9) . . . . ? P1 As1 C6 O2 -88.3(9) . . . . ? C1 As1 C6 C7 -159.3(7) . . . . ? P1 As1 C6 C7 97.4(7) . . . . ? O2 C6 C7 C10 140.9(11) . . . . ? As1 C6 C7 C10 -45.0(11) . . . . ? O2 C6 C7 C9 17.6(14) . . . . ? As1 C6 C7 C9 -168.4(8) . . . . ? O2 C6 C7 C8 -99.8(13) . . . . ? As1 C6 C7 C8 74.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.191 (near As1) _refine_diff_density_min -0.397 _refine_diff_density_rms 0.137 data_compound_6 _database_code_CSD 184014 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H40 O7 P4' _chemical_formula_weight 828.66 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' '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 12.930(3) _cell_length_b 14.012(3) _cell_length_c 14.939(3) _cell_angle_alpha 97.21(3) _cell_angle_beta 112.28(3) _cell_angle_gamma 116.39(3) _cell_volume 2097.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.98 _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 'Nonius Kappa CCD' _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 41030 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9595 _reflns_number_gt 7499 _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^)+(0.0324P)^2^+0.9508P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9595 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 P1 P 0.41157(4) 0.69629(4) 0.32211(3) 0.01937(10) Uani 1 1 d . . . P2 P 0.44782(4) 0.83107(4) 0.25742(3) 0.02061(10) Uani 1 1 d . . . P3 P 0.42218(5) 0.56590(4) 0.23654(3) 0.02135(10) Uani 1 1 d . . . P4 P 0.57598(4) 0.77213(4) 0.47970(3) 0.01936(10) Uani 1 1 d . . . O1 O 0.56476(13) 0.75317(11) 0.17440(10) 0.0279(3) Uani 1 1 d . . . O2 O 0.27497(13) 0.71814(12) 0.05097(10) 0.0332(3) Uani 1 1 d . . . O3 O 0.68781(12) 0.69153(11) 0.37660(9) 0.0263(3) Uani 1 1 d . . . O4 O 0.47164(13) 0.45208(12) 0.36405(11) 0.0349(3) Uani 1 1 d . . . O5 O 0.71001(12) 0.92605(11) 0.40794(9) 0.0262(3) Uani 1 1 d . . . O6 O 0.58965(13) 0.95716(11) 0.57791(11) 0.0327(3) Uani 1 1 d . . . O7 O 0.18115(14) 1.16508(12) 0.12074(11) 0.0380(3) Uani 1 1 d . . . C1 C 0.54454(17) 0.82880(15) 0.18952(13) 0.0219(4) Uani 1 1 d . . . C2 C 0.28257(18) 0.74669(15) 0.13499(13) 0.0227(4) Uani 1 1 d . . . C3 C 0.59132(17) 0.92689(15) 0.15378(13) 0.0237(4) Uani 1 1 d . . . C4 C 0.60975(19) 1.02935(16) 0.20085(15) 0.0300(4) Uani 1 1 d . . . H4 H 0.5916 1.0374 0.2549 0.036 Uiso 1 1 calc R . . C5 C 0.6553(2) 1.11979(18) 0.16709(17) 0.0363(5) Uani 1 1 d . . . H5 H 0.6689 1.1888 0.1991 0.044 Uiso 1 1 calc R . . C6 C 0.68050(19) 1.10698(18) 0.08576(16) 0.0368(5) Uani 1 1 d . . . H6 H 0.7106 1.1674 0.0630 0.044 Uiso 1 1 calc R . . C7 C 0.66120(19) 1.00540(18) 0.03845(16) 0.0351(5) Uani 1 1 d . . . H7 H 0.6777 0.9973 -0.0165 0.042 Uiso 1 1 calc R . . C8 C 0.61735(18) 0.91519(17) 0.07212(14) 0.0292(4) Uani 1 1 d . . . H8 H 0.6053 0.8468 0.0403 0.035 Uiso 1 1 calc R . . C9 C 0.16375(18) 0.72105(15) 0.14534(13) 0.0232(4) Uani 1 1 d . . . C10 C 0.03930(19) 0.63516(16) 0.06413(14) 0.0298(4) Uani 1 1 d . . . H10 H 0.0322 0.5954 0.0051 0.036 Uiso 1 1 calc R . . C11 C -0.0735(2) 0.60855(18) 0.07052(17) 0.0375(5) Uani 1 1 d . . . H11 H -0.1562 0.5500 0.0168 0.045 Uiso 1 1 calc R . . C12 C -0.0626(2) 0.66962(19) 0.15737(18) 0.0405(5) Uani 1 1 d . . . H12 H -0.1384 0.6526 0.1616 0.049 Uiso 1 1 calc R . . C13 C 0.0599(2) 0.75551(19) 0.23765(17) 0.0386(5) Uani 1 1 d . . . H13 H 0.0661 0.7966 0.2954 0.046 Uiso 1 1 calc R . . C14 C 0.17377(19) 0.78117(17) 0.23311(15) 0.0301(4) Uani 1 1 d . . . H14 H 0.2563 0.8381 0.2882 0.036 Uiso 1 1 calc R . . C15 C 0.60333(18) 0.61198(15) 0.29647(13) 0.0217(4) Uani 1 1 d . . . C16 C 0.38822(18) 0.47107(15) 0.31529(13) 0.0235(4) Uani 1 1 d . . . C17 C 0.63293(18) 0.54044(15) 0.24036(14) 0.0241(4) Uani 1 1 d . . . C18 C 0.7398(2) 0.5317(2) 0.29687(17) 0.0410(5) Uani 1 1 d . . . H18 H 0.7919 0.5710 0.3679 0.049 Uiso 1 1 calc R . . C19 C 0.7688(3) 0.4644(2) 0.24768(19) 0.0531(7) Uani 1 1 d . . . H19 H 0.8394 0.4575 0.2859 0.064 Uiso 1 1 calc R . . C20 C 0.6934(2) 0.40780(19) 0.14224(18) 0.0442(6) Uani 1 1 d . . . H20 H 0.7135 0.3631 0.1094 0.053 Uiso 1 1 calc R . . C21 C 0.5884(2) 0.41709(17) 0.08519(16) 0.0378(5) Uani 1 1 d . . . H21 H 0.5387 0.3798 0.0138 0.045 Uiso 1 1 calc R . . C22 C 0.5565(2) 0.48224(16) 0.13412(15) 0.0307(4) Uani 1 1 d . . . H22 H 0.4841 0.4869 0.0958 0.037 Uiso 1 1 calc R . . C23 C 0.25787(18) 0.41896(15) 0.31246(14) 0.0246(4) Uani 1 1 d . . . C24 C 0.15034(19) 0.41632(17) 0.23878(15) 0.0330(4) Uani 1 1 d . . . H24 H 0.1593 0.4502 0.1903 0.040 Uiso 1 1 calc R . . C25 C 0.0298(2) 0.3634(2) 0.23730(17) 0.0430(5) Uani 1 1 d . . . H25 H -0.0420 0.3618 0.1879 0.052 Uiso 1 1 calc R . . C26 C 0.0169(2) 0.31318(19) 0.30938(17) 0.0420(5) Uani 1 1 d . . . H26 H -0.0645 0.2765 0.3076 0.050 Uiso 1 1 calc R . . C27 C 0.1236(2) 0.31681(18) 0.38426(17) 0.0381(5) Uani 1 1 d . . . H27 H 0.1145 0.2839 0.4333 0.046 Uiso 1 1 calc R . . C28 C 0.24369(19) 0.36960(16) 0.38581(15) 0.0306(4) Uani 1 1 d . . . H28 H 0.3156 0.3722 0.4362 0.037 Uiso 1 1 calc R . . C29 C 0.72159(17) 0.89986(14) 0.48420(13) 0.0203(3) Uani 1 1 d . . . C30 C 0.51855(17) 0.85451(15) 0.53529(13) 0.0216(4) Uani 1 1 d . . . C31 C 0.84912(17) 0.96154(15) 0.58192(13) 0.0218(4) Uani 1 1 d . . . C32 C 0.86092(19) 0.93649(17) 0.67135(14) 0.0299(4) Uani 1 1 d . . . H32 H 0.7870 0.8791 0.6705 0.036 Uiso 1 1 calc R . . C33 C 0.9818(2) 0.99643(19) 0.76135(16) 0.0382(5) Uani 1 1 d . . . H33 H 0.9888 0.9804 0.8212 0.046 Uiso 1 1 calc R . . C34 C 1.0925(2) 1.08049(18) 0.76211(16) 0.0374(5) Uani 1 1 d . . . H34 H 1.1740 1.1202 0.8224 0.045 Uiso 1 1 calc R . . C35 C 1.08224(19) 1.10559(17) 0.67354(16) 0.0336(5) Uani 1 1 d . . . H35 H 1.1569 1.1619 0.6744 0.040 Uiso 1 1 calc R . . C36 C 0.96134(18) 1.04711(16) 0.58393(15) 0.0269(4) Uani 1 1 d . . . H36 H 0.9545 1.0647 0.5247 0.032 Uiso 1 1 calc R . . C37 C 0.38589(18) 0.78723(15) 0.52778(13) 0.0226(4) Uani 1 1 d . . . C38 C 0.32016(19) 0.84238(17) 0.53230(15) 0.0295(4) Uani 1 1 d . . . H38 H 0.3592 0.9191 0.5401 0.035 Uiso 1 1 calc R . . C39 C 0.1972(2) 0.78356(19) 0.52524(17) 0.0380(5) Uani 1 1 d . . . H39 H 0.1538 0.8208 0.5289 0.046 Uiso 1 1 calc R . . C40 C 0.1386(2) 0.66960(19) 0.51276(17) 0.0394(5) Uani 1 1 d . . . H40 H 0.0552 0.6299 0.5071 0.047 Uiso 1 1 calc R . . C41 C 0.2030(2) 0.61411(18) 0.50863(17) 0.0382(5) Uani 1 1 d . . . H41 H 0.1632 0.5374 0.5008 0.046 Uiso 1 1 calc R . . C42 C 0.32661(19) 0.67251(16) 0.51614(15) 0.0291(4) Uani 1 1 d . . . H42 H 0.3700 0.6351 0.5134 0.035 Uiso 1 1 calc R . . C43 C -0.0347(2) 1.1309(2) 0.0238(2) 0.0541(6) Uani 1 1 d . . . H43A H -0.0723 1.0501 0.0005 0.081 Uiso 1 1 calc R . . H43B H -0.0859 1.1493 -0.0283 0.081 Uiso 1 1 calc R . . H43C H -0.0353 1.1543 0.0866 0.081 Uiso 1 1 calc R . . C44 C 0.1054(2) 1.1917(2) 0.04315(17) 0.0447(5) Uani 1 1 d . . . H44A H 0.1066 1.1683 -0.0202 0.054 Uiso 1 1 calc R . . H44B H 0.1433 1.2733 0.0654 0.054 Uiso 1 1 calc R . . C45 C 0.3102(2) 1.2109(2) 0.13460(18) 0.0475(6) Uani 1 1 d . . . H45A H 0.3533 1.2926 0.1506 0.057 Uiso 1 1 calc R . . H45B H 0.3057 1.1774 0.0713 0.057 Uiso 1 1 calc R . . C46 C 0.3883(3) 1.1865(3) 0.2206(2) 0.0644(8) Uani 1 1 d . . . H46A H 0.3972 1.2238 0.2840 0.097 Uiso 1 1 calc R . . H46B H 0.4744 1.2143 0.2275 0.097 Uiso 1 1 calc R . . H46C H 0.3435 1.1058 0.2058 0.097 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 0.0218(2) 0.0189(2) 0.0178(2) 0.00633(18) 0.00958(19) 0.01126(19) P2 0.0246(2) 0.0211(2) 0.0191(2) 0.00820(18) 0.0113(2) 0.0138(2) P3 0.0241(2) 0.0201(2) 0.0193(2) 0.00519(18) 0.0102(2) 0.0124(2) P4 0.0218(2) 0.0189(2) 0.0178(2) 0.00601(18) 0.00995(19) 0.01112(19) O1 0.0362(7) 0.0304(7) 0.0276(7) 0.0126(6) 0.0191(6) 0.0221(6) O2 0.0346(8) 0.0407(8) 0.0208(7) 0.0091(6) 0.0142(6) 0.0176(7) O3 0.0258(7) 0.0263(7) 0.0244(7) 0.0046(6) 0.0118(6) 0.0138(6) O4 0.0336(8) 0.0397(8) 0.0450(8) 0.0247(7) 0.0219(7) 0.0249(7) O5 0.0275(7) 0.0282(7) 0.0225(6) 0.0109(6) 0.0132(6) 0.0135(6) O6 0.0313(7) 0.0196(7) 0.0425(8) 0.0032(6) 0.0200(7) 0.0106(6) O7 0.0395(8) 0.0375(9) 0.0379(8) 0.0166(7) 0.0214(7) 0.0183(7) C1 0.0206(9) 0.0241(10) 0.0169(8) 0.0055(7) 0.0075(7) 0.0107(8) C2 0.0279(9) 0.0201(9) 0.0204(9) 0.0090(7) 0.0099(8) 0.0143(8) C3 0.0189(9) 0.0250(10) 0.0224(9) 0.0096(8) 0.0082(8) 0.0096(8) C4 0.0298(10) 0.0289(11) 0.0310(10) 0.0125(9) 0.0160(9) 0.0142(9) C5 0.0321(11) 0.0258(11) 0.0422(12) 0.0137(9) 0.0145(10) 0.0116(9) C6 0.0267(10) 0.0368(12) 0.0405(12) 0.0246(10) 0.0144(10) 0.0113(10) C7 0.0293(11) 0.0443(13) 0.0323(11) 0.0194(10) 0.0186(10) 0.0158(10) C8 0.0268(10) 0.0331(11) 0.0282(10) 0.0127(9) 0.0146(9) 0.0150(9) C9 0.0267(9) 0.0224(9) 0.0237(9) 0.0110(8) 0.0114(8) 0.0155(8) C10 0.0316(10) 0.0266(10) 0.0252(10) 0.0065(8) 0.0110(9) 0.0143(9) C11 0.0258(10) 0.0320(12) 0.0401(12) 0.0084(10) 0.0106(10) 0.0105(9) C12 0.0330(11) 0.0442(13) 0.0496(13) 0.0166(11) 0.0227(11) 0.0226(11) C13 0.0389(12) 0.0451(13) 0.0390(12) 0.0076(10) 0.0212(11) 0.0278(11) C14 0.0280(10) 0.0322(11) 0.0268(10) 0.0049(8) 0.0101(9) 0.0179(9) C15 0.0279(9) 0.0215(9) 0.0232(9) 0.0116(8) 0.0155(8) 0.0153(8) C16 0.0270(10) 0.0190(9) 0.0228(9) 0.0058(7) 0.0113(8) 0.0122(8) C17 0.0304(10) 0.0207(9) 0.0273(9) 0.0098(8) 0.0182(9) 0.0145(8) C18 0.0519(14) 0.0546(15) 0.0324(11) 0.0146(10) 0.0220(11) 0.0394(13) C19 0.0737(18) 0.0743(18) 0.0529(15) 0.0283(14) 0.0385(14) 0.0626(16) C20 0.0699(16) 0.0415(13) 0.0550(14) 0.0225(11) 0.0472(14) 0.0395(13) C21 0.0523(13) 0.0275(11) 0.0335(11) 0.0062(9) 0.0284(11) 0.0164(10) C22 0.0360(11) 0.0270(10) 0.0303(10) 0.0084(8) 0.0189(9) 0.0160(9) C23 0.0261(9) 0.0169(9) 0.0275(9) 0.0046(7) 0.0129(8) 0.0101(8) C24 0.0270(10) 0.0306(11) 0.0299(10) 0.0079(9) 0.0103(9) 0.0107(9) C25 0.0242(10) 0.0497(14) 0.0372(12) 0.0087(11) 0.0089(10) 0.0135(10) C26 0.0281(11) 0.0400(13) 0.0429(13) 0.0044(10) 0.0196(10) 0.0079(10) C27 0.0410(12) 0.0318(12) 0.0417(12) 0.0138(10) 0.0258(11) 0.0149(10) C28 0.0317(11) 0.0263(10) 0.0342(11) 0.0116(9) 0.0161(9) 0.0158(9) C29 0.0241(9) 0.0208(9) 0.0217(9) 0.0061(7) 0.0131(8) 0.0150(8) C30 0.0257(9) 0.0216(10) 0.0202(8) 0.0079(7) 0.0120(8) 0.0139(8) C31 0.0217(9) 0.0226(9) 0.0225(9) 0.0057(7) 0.0108(8) 0.0135(8) C32 0.0271(10) 0.0296(11) 0.0272(10) 0.0108(8) 0.0110(9) 0.0125(9) C33 0.0359(12) 0.0426(13) 0.0290(11) 0.0143(10) 0.0100(10) 0.0202(11) C34 0.0225(10) 0.0411(13) 0.0320(11) 0.0026(9) 0.0031(9) 0.0160(10) C35 0.0206(10) 0.0343(12) 0.0389(12) 0.0047(9) 0.0152(9) 0.0112(9) C36 0.0274(10) 0.0276(10) 0.0303(10) 0.0074(8) 0.0179(9) 0.0156(9) C37 0.0280(9) 0.0241(9) 0.0184(8) 0.0068(7) 0.0141(8) 0.0139(8) C38 0.0351(11) 0.0281(10) 0.0335(10) 0.0129(9) 0.0209(9) 0.0190(9) C39 0.0374(12) 0.0452(13) 0.0465(13) 0.0190(11) 0.0270(11) 0.0272(11) C40 0.0291(11) 0.0424(13) 0.0421(12) 0.0127(10) 0.0223(10) 0.0124(10) C41 0.0412(12) 0.0261(11) 0.0462(13) 0.0114(9) 0.0299(11) 0.0106(10) C42 0.0368(11) 0.0239(10) 0.0331(10) 0.0095(8) 0.0232(9) 0.0162(9) C43 0.0498(15) 0.0425(15) 0.0617(16) 0.0229(13) 0.0158(13) 0.0269(13) C44 0.0589(15) 0.0371(13) 0.0379(12) 0.0169(10) 0.0219(12) 0.0263(12) C45 0.0484(14) 0.0504(15) 0.0419(13) 0.0121(11) 0.0303(12) 0.0195(12) C46 0.0501(16) 0.090(2) 0.0548(16) 0.0226(16) 0.0279(14) 0.0378(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 P2 2.1759(8) . ? P1 P4 2.1819(15) . ? P1 P3 2.1819(9) . ? P2 C2 1.886(2) . ? P2 C1 1.8928(17) . ? P3 C16 1.8995(18) . ? P3 C15 1.904(2) . ? P4 C30 1.8874(17) . ? P4 C29 1.906(2) . ? O1 C1 1.214(2) . ? O2 C2 1.221(2) . ? O3 C15 1.208(2) . ? O4 C16 1.214(2) . ? O5 C29 1.216(2) . ? O6 C30 1.213(2) . ? O7 C45 1.412(3) . ? O7 C44 1.419(3) . ? C1 C3 1.493(2) . ? C2 C9 1.489(2) . ? C3 C4 1.388(3) . ? C3 C8 1.392(2) . ? C4 C5 1.389(3) . ? C5 C6 1.382(3) . ? C6 C7 1.373(3) . ? C7 C8 1.382(3) . ? C9 C10 1.393(3) . ? C9 C14 1.394(3) . ? C10 C11 1.381(3) . ? C11 C12 1.383(3) . ? C12 C13 1.378(3) . ? C13 C14 1.383(3) . ? C15 C17 1.492(2) . ? C16 C23 1.490(2) . ? C17 C18 1.389(3) . ? C17 C22 1.389(3) . ? C18 C19 1.386(3) . ? C19 C20 1.377(3) . ? C20 C21 1.376(3) . ? C21 C22 1.390(3) . ? C23 C24 1.389(3) . ? C23 C28 1.394(3) . ? C24 C25 1.386(3) . ? C25 C26 1.380(3) . ? C26 C27 1.382(3) . ? C27 C28 1.381(3) . ? C29 C31 1.479(3) . ? C30 C37 1.494(2) . ? C31 C32 1.394(2) . ? C31 C36 1.398(3) . ? C32 C33 1.383(3) . ? C33 C34 1.386(3) . ? C34 C35 1.385(3) . ? C35 C36 1.381(3) . ? C37 C42 1.391(3) . ? C37 C38 1.392(2) . ? C38 C39 1.380(3) . ? C39 C40 1.379(3) . ? C40 C41 1.379(3) . ? C41 C42 1.384(3) . ? C43 C44 1.503(3) . ? C45 C46 1.490(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 P2 P1 P4 106.47(5) . . ? P2 P1 P3 108.75(3) . . ? P4 P1 P3 106.85(4) . . ? C2 P2 C1 94.25(8) . . ? C2 P2 P1 95.66(7) . . ? C1 P2 P1 108.96(6) . . ? C16 P3 C15 92.62(8) . . ? C16 P3 P1 95.13(6) . . ? C15 P3 P1 107.61(7) . . ? C30 P4 C29 96.73(8) . . ? C30 P4 P1 95.64(6) . . ? C29 P4 P1 106.92(7) . . ? C45 O7 C44 111.64(16) . . ? O1 C1 C3 122.72(15) . . ? O1 C1 P2 123.09(13) . . ? C3 C1 P2 114.17(12) . . ? O2 C2 C9 121.96(17) . . ? O2 C2 P2 120.94(14) . . ? C9 C2 P2 117.05(12) . . ? C4 C3 C8 119.63(17) . . ? C4 C3 C1 121.14(16) . . ? C8 C3 C1 119.23(17) . . ? C3 C4 C5 119.93(18) . . ? C6 C5 C4 119.9(2) . . ? C7 C6 C5 120.32(18) . . ? C6 C7 C8 120.36(18) . . ? C7 C8 C3 119.88(19) . . ? C10 C9 C14 119.48(17) . . ? C10 C9 C2 118.65(16) . . ? C14 C9 C2 121.87(17) . . ? C11 C10 C9 120.56(18) . . ? C10 C11 C12 119.5(2) . . ? C13 C12 C11 120.36(19) . . ? C12 C13 C14 120.61(19) . . ? C13 C14 C9 119.45(19) . . ? O3 C15 C17 122.33(16) . . ? O3 C15 P3 122.03(13) . . ? C17 C15 P3 115.59(14) . . ? O4 C16 C23 121.90(16) . . ? O4 C16 P3 119.16(13) . . ? C23 C16 P3 118.91(13) . . ? C18 C17 C22 119.45(17) . . ? C18 C17 C15 118.54(17) . . ? C22 C17 C15 122.02(17) . . ? C19 C18 C17 120.2(2) . . ? C20 C19 C18 120.1(2) . . ? C19 C20 C21 120.30(19) . . ? C20 C21 C22 120.1(2) . . ? C17 C22 C21 119.92(19) . . ? C24 C23 C28 119.23(17) . . ? C24 C23 C16 122.48(16) . . ? C28 C23 C16 118.29(16) . . ? C25 C24 C23 120.26(19) . . ? C26 C25 C24 119.7(2) . . ? C25 C26 C27 120.66(19) . . ? C28 C27 C26 119.60(19) . . ? C27 C28 C23 120.49(19) . . ? O5 C29 C31 121.98(16) . . ? O5 C29 P4 120.60(14) . . ? C31 C29 P4 117.37(12) . . ? O6 C30 C37 122.50(15) . . ? O6 C30 P4 120.37(13) . . ? C37 C30 P4 117.08(13) . . ? C32 C31 C36 119.19(17) . . ? C32 C31 C29 122.15(16) . . ? C36 C31 C29 118.66(16) . . ? C33 C32 C31 120.42(18) . . ? C32 C33 C34 119.81(19) . . ? C35 C34 C33 120.31(19) . . ? C36 C35 C34 120.07(18) . . ? C35 C36 C31 120.18(18) . . ? C42 C37 C38 119.45(17) . . ? C42 C37 C30 122.40(16) . . ? C38 C37 C30 118.15(16) . . ? C39 C38 C37 120.19(18) . . ? C40 C39 C38 119.98(19) . . ? C39 C40 C41 120.38(18) . . ? C40 C41 C42 120.07(19) . . ? C41 C42 C37 119.92(18) . . ? O7 C44 C43 109.38(18) . . ? O7 C45 C46 109.72(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.285 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.066