# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Gerard Parkin ' _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_author_name 'Gerard Parkin' data_wp5brs10 _database_code_depnum_ccdc_archive 'CCDC 842914' #TrackingRef '- WP5+Br-[wp5brs10].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H44 Br P5 W' _chemical_formula_weight 643.11 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Tetragonal _symmetry_space_group_name_H-M P4(2)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' _cell_length_a 13.476(3) _cell_length_b 13.476(3) _cell_length_c 14.118(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2563.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 32.41 _exptl_crystal_description NEEDLE _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 6.373 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.3219 _exptl_absorpt_correction_T_max 0.8318 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44100 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 31.76 _reflns_number_total 4516 _reflns_number_gt 3915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.8663P] 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 4516 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0433 _refine_ls_wR_factor_gt 0.0410 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 W W 0.320056(7) 0.219066(7) 0.0000 0.01106(3) Uani 1 2 d S . . H1 H 0.387(3) 0.110(3) 0.0000 0.032(10) Uiso 1 2 d S . . Br Br 0.16089(2) 0.69741(2) 0.0000 0.02389(6) Uani 1 2 d S . . P1 P 0.19563(5) 0.35151(5) 0.0000 0.01554(13) Uani 1 2 d S . . P2 P 0.50144(5) 0.23655(5) 0.0000 0.01531(12) Uani 1 2 d S . . P3 P 0.18573(5) 0.08726(5) 0.0000 0.01691(13) Uani 1 2 d S . . P4 P 0.32074(4) 0.20343(4) 0.17680(3) 0.01582(9) Uani 1 1 d . . . C11 C 0.3240(2) 0.3658(2) 0.0000 0.0199(5) Uani 1 2 d S . . H2 H 0.367(3) 0.428(3) 0.0000 0.034(10) Uiso 1 2 d S . . C12 C 0.13310(19) 0.41400(17) 0.09806(16) 0.0319(5) Uani 1 1 d . . . H12A H 0.1323 0.4857 0.0865 0.048 Uiso 1 1 calc R . . H12B H 0.1686 0.4003 0.1572 0.048 Uiso 1 1 calc R . . H12C H 0.0648 0.3896 0.1031 0.048 Uiso 1 1 calc R . . C21 C 0.5537(2) 0.3625(2) 0.0000 0.0290(7) Uani 1 2 d S . . H21A H 0.6263 0.3586 0.0000 0.044 Uiso 1 2 calc SR . . H21B H 0.5313 0.3980 0.0567 0.044 Uiso 0.50 1 calc PR . . H21C H 0.5313 0.3980 -0.0567 0.044 Uiso 0.50 1 calc PR . . C22 C 0.57516(15) 0.18076(17) 0.09542(15) 0.0252(4) Uani 1 1 d . . . H22A H 0.6456 0.1956 0.0853 0.038 Uiso 1 1 calc R . . H22B H 0.5654 0.1087 0.0955 0.038 Uiso 1 1 calc R . . H22C H 0.5540 0.2081 0.1565 0.038 Uiso 1 1 calc R . . C31 C 0.0609(2) 0.1341(3) 0.0000 0.0741(19) Uani 1 2 d S . . H31A H 0.0141 0.0784 0.0000 0.111 Uiso 1 2 calc SR . . H31B H 0.0502 0.1747 -0.0567 0.111 Uiso 0.50 1 calc PR . . H31C H 0.0502 0.1747 0.0567 0.111 Uiso 0.50 1 calc PR . . C32 C 0.1848(2) -0.00533(19) -0.09512(18) 0.0456(7) Uani 1 1 d . . . H32A H 0.1313 -0.0532 -0.0838 0.068 Uiso 1 1 calc R . . H32B H 0.2486 -0.0402 -0.0964 0.068 Uiso 1 1 calc R . . H32C H 0.1740 0.0278 -0.1560 0.068 Uiso 1 1 calc R . . C41 C 0.37776(16) 0.09487(15) 0.23310(14) 0.0235(4) Uani 1 1 d . . . H41A H 0.3691 0.0991 0.3019 0.035 Uiso 1 1 calc R . . H41B H 0.4487 0.0931 0.2180 0.035 Uiso 1 1 calc R . . H41C H 0.3459 0.0343 0.2095 0.035 Uiso 1 1 calc R . . C42 C 0.20244(15) 0.20596(17) 0.24236(15) 0.0255(4) Uani 1 1 d . . . H42A H 0.2148 0.1914 0.3093 0.038 Uiso 1 1 calc R . . H42B H 0.1574 0.1560 0.2161 0.038 Uiso 1 1 calc R . . H42C H 0.1722 0.2718 0.2365 0.038 Uiso 1 1 calc R . . C43 C 0.38214(16) 0.30611(16) 0.23883(14) 0.0257(4) Uani 1 1 d . . . H43A H 0.3806 0.2938 0.3072 0.039 Uiso 1 1 calc R . . H43B H 0.3474 0.3683 0.2248 0.039 Uiso 1 1 calc R . . H43C H 0.4512 0.3111 0.2176 0.039 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 W 0.01052(5) 0.01178(5) 0.01088(5) 0.000 0.000 0.00046(3) Br 0.02331(14) 0.02892(15) 0.01943(13) 0.000 0.000 0.00070(11) P1 0.0151(3) 0.0138(3) 0.0177(3) 0.000 0.000 0.0025(2) P2 0.0120(3) 0.0162(3) 0.0178(3) 0.000 0.000 0.0003(2) P3 0.0144(3) 0.0137(3) 0.0226(3) 0.000 0.000 -0.0014(2) P4 0.0170(2) 0.0184(2) 0.0121(2) -0.00074(16) 0.00015(17) 0.00118(16) C11 0.0181(13) 0.0158(12) 0.0258(14) 0.000 0.000 -0.0003(10) C12 0.0385(13) 0.0295(12) 0.0279(11) 0.0007(9) 0.0104(10) 0.0152(9) C21 0.0169(13) 0.0216(15) 0.049(2) 0.000 0.000 -0.0047(11) C22 0.0163(9) 0.0356(12) 0.0239(10) 0.0035(8) -0.0045(7) 0.0027(8) C31 0.0090(14) 0.0193(16) 0.194(6) 0.000 0.000 -0.0020(12) C32 0.071(2) 0.0299(13) 0.0361(13) -0.0097(10) 0.0098(13) -0.0265(13) C41 0.0281(10) 0.0249(10) 0.0176(9) 0.0032(7) -0.0020(8) 0.0028(8) C42 0.0237(10) 0.0351(11) 0.0176(9) -0.0020(8) 0.0070(8) 0.0005(8) C43 0.0286(11) 0.0270(10) 0.0215(9) -0.0078(8) -0.0009(8) -0.0017(8) _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 W H1 1.72(3) . ? W C11 1.978(3) . ? W P1 2.4489(9) . ? W P2 2.4556(9) . ? W P4 2.5049(8) 6 ? W P4 2.5049(8) . ? W P3 2.5361(9) . ? P1 C11 1.741(3) . ? P1 C12 1.826(2) 6 ? P1 C12 1.826(2) . ? P2 C22 1.835(2) 6 ? P2 C22 1.835(2) . ? P2 C21 1.837(3) . ? P3 C31 1.797(3) . ? P3 C32 1.833(2) 6 ? P3 C32 1.833(2) . ? P4 C41 1.834(2) . ? P4 C43 1.835(2) . ? P4 C42 1.844(2) . ? 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 H1 W C11 146.9(11) . . ? H1 W P1 168.4(11) . . ? C11 W P1 44.76(8) . . ? H1 W P2 63.9(11) . . ? C11 W P2 82.95(8) . . ? P1 W P2 127.71(2) . . ? H1 W P4 85.78(5) . 6 ? C11 W P4 94.817(12) . 6 ? P1 W P4 93.660(11) . 6 ? P2 W P4 90.252(11) . 6 ? H1 W P4 85.78(5) . . ? C11 W P4 94.818(12) . . ? P1 W P4 93.661(11) . . ? P2 W P4 90.251(11) . . ? P4 W P4 170.34(2) 6 . ? H1 W P3 77.1(11) . . ? C11 W P3 136.00(8) . . ? P1 W P3 91.24(2) . . ? P2 W P3 141.05(2) . . ? P4 W P3 86.774(12) 6 . ? P4 W P3 86.774(12) . . ? C11 P1 C12 114.05(10) . 6 ? C11 P1 C12 114.05(10) . . ? C12 P1 C12 98.58(15) 6 . ? C11 P1 W 53.13(9) . . ? C12 P1 W 130.69(8) 6 . ? C12 P1 W 130.69(8) . . ? C22 P2 C22 94.47(14) 6 . ? C22 P2 C21 99.85(10) 6 . ? C22 P2 C21 99.84(10) . . ? C22 P2 W 119.97(7) 6 . ? C22 P2 W 119.97(7) . . ? C21 P2 W 118.04(10) . . ? C31 P3 C32 103.47(13) . 6 ? C31 P3 C32 103.47(13) . . ? C32 P3 C32 94.20(18) 6 . ? C31 P3 W 114.98(12) . . ? C32 P3 W 118.78(9) 6 . ? C32 P3 W 118.78(9) . . ? C41 P4 C43 101.87(10) . . ? C41 P4 C42 99.17(10) . . ? C43 P4 C42 97.83(10) . . ? C41 P4 W 120.04(7) . . ? C43 P4 W 114.45(7) . . ? C42 P4 W 119.70(7) . . ? P1 C11 W 82.11(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.76 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.748 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.102 # Attachment '- WP5+I-[WP5IS10].cif' data_wp5is10 _database_code_depnum_ccdc_archive 'CCDC 842915' #TrackingRef '- WP5+I-[WP5IS10].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H44 I P5 W' _chemical_formula_weight 690.10 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 Tetragonal _symmetry_space_group_name_H-M P4(2)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' _cell_length_a 13.598(3) _cell_length_b 13.598(3) _cell_length_c 14.392(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2661.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 32.32 _exptl_crystal_description NEEDLE _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 5.799 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.1524 _exptl_absorpt_correction_T_max 0.7603 _exptl_absorpt_process_details SADABS _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45502 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 31.50 _reflns_number_total 4582 _reflns_number_gt 3938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+1.6751P] 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 0.00014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4582 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0469 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 W W 0.281698(9) 0.179592(9) 0.0000 0.01461(4) Uani 1 2 d S . . H1 H 0.398(4) 0.105(4) 0.0000 0.072(18) Uiso 1 2 d S . . I I 0.196312(17) -0.343855(17) 0.0000 0.02484(6) Uani 1 2 d S . . P1 P 0.15300(6) 0.30524(6) 0.0000 0.01942(16) Uani 1 2 d S . . P2 P 0.26167(7) 0.00042(6) 0.0000 0.02024(16) Uani 1 2 d S . . P3 P 0.41517(6) 0.30941(6) 0.0000 0.02153(17) Uani 1 2 d S . . P4 P 0.29638(5) 0.17879(4) 0.17339(4) 0.02026(12) Uani 1 1 d . . . C11 C 0.1360(3) 0.1785(3) 0.0000 0.0242(7) Uani 1 2 d S . . H2 H 0.084(3) 0.142(3) 0.0000 0.039(13) Uiso 1 2 d S . . C12 C 0.0934(2) 0.3683(2) 0.0970(2) 0.0336(6) Uani 1 1 d . . . H12A H 0.0228 0.3747 0.0843 0.050 Uiso 1 1 calc R . . H12B H 0.1223 0.4337 0.1047 0.050 Uiso 1 1 calc R . . H12C H 0.1029 0.3301 0.1541 0.050 Uiso 1 1 calc R . . C21 C 0.1370(3) -0.0490(3) 0.0000 0.0389(10) Uani 1 2 d S . . H21A H 0.1397 -0.1210 0.0000 0.058 Uiso 1 2 calc SR . . H21B H 0.1022 -0.0263 -0.0556 0.058 Uiso 0.50 1 calc PR . . H21C H 0.1022 -0.0263 0.0556 0.058 Uiso 0.50 1 calc PR . . C22 C 0.3157(2) -0.07292(19) -0.09397(19) 0.0326(6) Uani 1 1 d . . . H22A H 0.2998 -0.1425 -0.0844 0.049 Uiso 1 1 calc R . . H22B H 0.3872 -0.0643 -0.0940 0.049 Uiso 1 1 calc R . . H22C H 0.2888 -0.0511 -0.1537 0.049 Uiso 1 1 calc R . . C31 C 0.3703(3) 0.4345(3) 0.0000 0.0660(19) Uani 1 2 d S . . H31A H 0.4262 0.4801 0.0000 0.099 Uiso 1 2 calc SR . . H31B H 0.3302 0.4457 0.0556 0.099 Uiso 0.50 1 calc PR . . H31C H 0.3302 0.4457 -0.0556 0.099 Uiso 0.50 1 calc PR . . C32 C 0.5059(2) 0.3101(3) 0.0936(2) 0.0444(8) Uani 1 1 d . . . H32A H 0.5545 0.3619 0.0819 0.067 Uiso 1 1 calc R . . H32B H 0.5390 0.2462 0.0961 0.067 Uiso 1 1 calc R . . H32C H 0.4729 0.3227 0.1529 0.067 Uiso 1 1 calc R . . C41 C 0.4027(2) 0.1198(2) 0.22815(18) 0.0293(5) Uani 1 1 d . . . H41A H 0.3984 0.1275 0.2957 0.044 Uiso 1 1 calc R . . H41B H 0.4633 0.1507 0.2056 0.044 Uiso 1 1 calc R . . H41C H 0.4033 0.0497 0.2124 0.044 Uiso 1 1 calc R . . C42 C 0.2957(2) 0.2963(2) 0.23694(18) 0.0302(6) Uani 1 1 d . . . H42A H 0.3104 0.2843 0.3026 0.045 Uiso 1 1 calc R . . H42B H 0.2307 0.3270 0.2314 0.045 Uiso 1 1 calc R . . H42C H 0.3456 0.3402 0.2106 0.045 Uiso 1 1 calc R . . C43 C 0.1935(2) 0.1198(2) 0.23393(19) 0.0328(6) Uani 1 1 d . . . H43A H 0.2060 0.1203 0.3010 0.049 Uiso 1 1 calc R . . H43B H 0.1868 0.0518 0.2124 0.049 Uiso 1 1 calc R . . H43C H 0.1327 0.1559 0.2207 0.049 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 W 0.01621(6) 0.01377(6) 0.01385(6) 0.000 0.000 0.00024(4) I 0.02933(12) 0.02359(11) 0.02159(11) 0.000 0.000 -0.00124(8) P1 0.0177(4) 0.0185(4) 0.0220(4) 0.000 0.000 0.0016(3) P2 0.0226(4) 0.0153(4) 0.0229(4) 0.000 0.000 0.0002(3) P3 0.0175(4) 0.0180(4) 0.0291(5) 0.000 0.000 -0.0015(3) P4 0.0249(3) 0.0214(3) 0.0145(3) 0.0000(2) 0.0007(2) 0.0016(2) C11 0.0245(17) 0.0210(16) 0.0269(17) 0.000 0.000 -0.0032(13) C12 0.0300(14) 0.0375(15) 0.0333(14) -0.0076(12) 0.0010(11) 0.0112(11) C21 0.031(2) 0.0205(18) 0.065(3) 0.000 0.000 -0.0059(15) C22 0.0473(17) 0.0198(12) 0.0308(14) -0.0033(10) 0.0036(12) 0.0040(11) C31 0.026(2) 0.0144(18) 0.157(6) 0.000 0.000 -0.0023(15) C32 0.0307(15) 0.064(2) 0.0388(17) 0.0047(15) -0.0078(13) -0.0184(15) C41 0.0323(14) 0.0331(14) 0.0225(12) 0.0021(10) -0.0060(10) 0.0069(11) C42 0.0391(15) 0.0310(13) 0.0203(12) -0.0068(10) 0.0001(11) 0.0039(11) C43 0.0375(15) 0.0364(15) 0.0244(12) 0.0017(11) 0.0097(11) -0.0020(11) _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 W H1 1.88(6) . ? W C11 1.981(4) . ? W P1 2.4458(10) . ? W P2 2.4517(10) . ? W P4 2.5034(8) . ? W P4 2.5035(8) 6 ? W P3 2.5319(10) . ? P1 C11 1.739(4) . ? P1 C12 1.828(3) . ? P1 C12 1.828(3) 6 ? P2 C21 1.823(4) . ? P2 C22 1.834(3) 6 ? P2 C22 1.834(3) . ? P3 C31 1.807(4) . ? P3 C32 1.827(3) . ? P3 C32 1.827(3) 6 ? P4 C41 1.831(3) . ? P4 C43 1.833(3) . ? P4 C42 1.841(3) . ? C11 H2 0.87(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1 W C11 146.7(17) . . ? H1 W P1 168.6(17) . . ? C11 W P1 44.75(11) . . ? H1 W P2 63.5(17) . . ? C11 W P2 83.19(10) . . ? P1 W P2 127.94(3) . . ? H1 W P4 86.02(7) . . ? C11 W P4 94.574(15) . . ? P1 W P4 93.446(14) . . ? P2 W P4 90.261(14) . . ? H1 W P4 86.03(7) . 6 ? C11 W P4 94.573(15) . 6 ? P1 W P4 93.445(14) . 6 ? P2 W P4 90.261(14) . 6 ? P4 W P4 170.84(3) . 6 ? H1 W P3 77.1(17) . . ? C11 W P3 136.23(10) . . ? P1 W P3 91.48(3) . . ? P2 W P3 140.58(3) . . ? P4 W P3 86.895(15) . . ? P4 W P3 86.895(15) 6 . ? C11 P1 C12 113.93(12) . . ? C11 P1 C12 113.93(12) . 6 ? C12 P1 C12 99.61(19) . 6 ? C11 P1 W 53.32(12) . . ? C12 P1 W 130.16(9) . . ? C12 P1 W 130.16(9) 6 . ? C21 P2 C22 99.89(13) . 6 ? C21 P2 C22 99.89(13) . . ? C22 P2 C22 95.05(19) 6 . ? C21 P2 W 118.00(14) . . ? C22 P2 W 119.74(9) 6 . ? C22 P2 W 119.74(9) . . ? C31 P3 C32 102.88(15) . . ? C31 P3 C32 102.88(15) . 6 ? C32 P3 C32 95.0(2) . 6 ? C31 P3 W 114.48(15) . . ? C32 P3 W 119.21(11) . . ? C32 P3 W 119.21(11) 6 . ? C41 P4 C43 101.91(13) . . ? C41 P4 C42 99.81(13) . . ? C43 P4 C42 98.03(13) . . ? C41 P4 W 119.59(9) . . ? C43 P4 W 114.51(10) . . ? C42 P4 W 119.40(9) . . ? H2 C11 P1 133(3) . . ? H2 C11 W 145(3) . . ? P1 C11 W 81.93(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.020 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.118 # Attachment '- WP5[WP5S10].cif' data_wp5s10 _database_code_depnum_ccdc_archive 'CCDC 842916' #TrackingRef '- WP5[WP5S10].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H45 P5 W' _chemical_formula_weight 564.21 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' P P 0.1023 0.0942 '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 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 14.8321(4) _cell_length_b 9.4806(3) _cell_length_c 18.0198(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.6870(10) _cell_angle_gamma 90.00 _cell_volume 2427.19(12) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9974 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 32.49 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 5.084 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.3876 _exptl_absorpt_correction_T_max 0.5806 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14235 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.51 _reflns_number_total 7349 _reflns_number_gt 6542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7349 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0478 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 W W 0.489653(5) 0.701445(8) 0.235805(5) 0.01151(3) Uani 1 1 d . . . H1 H 0.597(2) 0.787(2) 0.2612(17) 0.028(8) Uiso 1 1 d . . . P1 P 0.36496(4) 0.55282(6) 0.16703(3) 0.01616(11) Uani 1 1 d . . . P2 P 0.48718(4) 0.86973(5) 0.33813(3) 0.01445(10) Uani 1 1 d . . . P3 P 0.60959(4) 0.61981(6) 0.17865(4) 0.02015(12) Uani 1 1 d . . . P4 P 0.54274(4) 0.52406(6) 0.33500(3) 0.01725(11) Uani 1 1 d . . . P5 P 0.43583(4) 0.88215(6) 0.13815(3) 0.01607(11) Uani 1 1 d . . . C11 C 0.33629(15) 0.6609(2) 0.23679(13) 0.0174(4) Uani 1 1 d . . . H11A H 0.3276 0.6129 0.2830 0.021 Uiso 1 1 calc R . . H11B H 0.2905 0.7377 0.2169 0.021 Uiso 1 1 calc R . . C12 C 0.34410(17) 0.3637(2) 0.17827(16) 0.0253(5) Uani 1 1 d . . . H12A H 0.3738 0.3355 0.2321 0.038 Uiso 1 1 calc R . . H12B H 0.3712 0.3090 0.1438 0.038 Uiso 1 1 calc R . . H12C H 0.2762 0.3460 0.1649 0.038 Uiso 1 1 calc R . . C13 C 0.28052(17) 0.5753(3) 0.07084(14) 0.0256(5) Uani 1 1 d . . . H13A H 0.2201 0.5329 0.0705 0.038 Uiso 1 1 calc R . . H13B H 0.3047 0.5289 0.0319 0.038 Uiso 1 1 calc R . . H13C H 0.2716 0.6760 0.0589 0.038 Uiso 1 1 calc R . . C21 C 0.59949(16) 0.9554(2) 0.38642(14) 0.0229(5) Uani 1 1 d . . . H21A H 0.5921 1.0140 0.4291 0.034 Uiso 1 1 calc R . . H21B H 0.6188 1.0147 0.3491 0.034 Uiso 1 1 calc R . . H21C H 0.6476 0.8833 0.4069 0.034 Uiso 1 1 calc R . . C22 C 0.41227(16) 1.0282(2) 0.31894(14) 0.0210(5) Uani 1 1 d . . . H22A H 0.4231 1.0834 0.3667 0.031 Uiso 1 1 calc R . . H22B H 0.3460 1.0000 0.3008 0.031 Uiso 1 1 calc R . . H22C H 0.4279 1.0856 0.2791 0.031 Uiso 1 1 calc R . . C23 C 0.45180(18) 0.8129(2) 0.42329(14) 0.0240(5) Uani 1 1 d . . . H23A H 0.4970 0.7434 0.4527 0.036 Uiso 1 1 calc R . . H23B H 0.3890 0.7704 0.4063 0.036 Uiso 1 1 calc R . . H23C H 0.4506 0.8947 0.4563 0.036 Uiso 1 1 calc R . . C31 C 0.72813(16) 0.5885(3) 0.24435(16) 0.0301(6) Uani 1 1 d . . . H31A H 0.7239 0.5253 0.2863 0.045 Uiso 1 1 calc R . . H31B H 0.7560 0.6784 0.2663 0.045 Uiso 1 1 calc R . . H31C H 0.7677 0.5450 0.2155 0.045 Uiso 1 1 calc R . . C32 C 0.5891(2) 0.4542(3) 0.12248(18) 0.0350(6) Uani 1 1 d . . . H32A H 0.6451 0.4307 0.1066 0.053 Uiso 1 1 calc R . . H32B H 0.5351 0.4660 0.0764 0.053 Uiso 1 1 calc R . . H32C H 0.5760 0.3779 0.1546 0.053 Uiso 1 1 calc R . . C33 C 0.6503(2) 0.7259(3) 0.10853(18) 0.0362(7) Uani 1 1 d . . . H33A H 0.6669 0.8209 0.1294 0.054 Uiso 1 1 calc R . . H33B H 0.6000 0.7319 0.0596 0.054 Uiso 1 1 calc R . . H33C H 0.7058 0.6811 0.0994 0.054 Uiso 1 1 calc R . . C41 C 0.46183(18) 0.4537(3) 0.38804(15) 0.0264(5) Uani 1 1 d . . . H41A H 0.4961 0.3878 0.4282 0.040 Uiso 1 1 calc R . . H41B H 0.4094 0.4044 0.3517 0.040 Uiso 1 1 calc R . . H41C H 0.4374 0.5318 0.4122 0.040 Uiso 1 1 calc R . . C42 C 0.64441(18) 0.5600(3) 0.42032(15) 0.0285(5) Uani 1 1 d . . . H42A H 0.6603 0.4745 0.4519 0.043 Uiso 1 1 calc R . . H42B H 0.6282 0.6358 0.4513 0.043 Uiso 1 1 calc R . . H42C H 0.6985 0.5889 0.4030 0.043 Uiso 1 1 calc R . . C43 C 0.58213(18) 0.3484(2) 0.31165(16) 0.0275(5) Uani 1 1 d . . . H43A H 0.6389 0.3590 0.2947 0.041 Uiso 1 1 calc R . . H43B H 0.5322 0.3049 0.2701 0.041 Uiso 1 1 calc R . . H43C H 0.5961 0.2883 0.3578 0.041 Uiso 1 1 calc R . . C51 C 0.31882(17) 0.9656(2) 0.12343(14) 0.0235(5) Uani 1 1 d . . . H51A H 0.3162 1.0106 0.1717 0.035 Uiso 1 1 calc R . . H51B H 0.2696 0.8934 0.1084 0.035 Uiso 1 1 calc R . . H51C H 0.3089 1.0368 0.0824 0.035 Uiso 1 1 calc R . . C52 C 0.4224(2) 0.8458(3) 0.03413(14) 0.0288(5) Uani 1 1 d . . . H52A H 0.3716 0.9043 0.0019 0.043 Uiso 1 1 calc R . . H52B H 0.4070 0.7459 0.0232 0.043 Uiso 1 1 calc R . . H52C H 0.4813 0.8679 0.0224 0.043 Uiso 1 1 calc R . . C53 C 0.50760(18) 1.0439(2) 0.14662(15) 0.0238(5) Uani 1 1 d . . . H53A H 0.4761 1.1104 0.1057 0.036 Uiso 1 1 calc R . . H53B H 0.5697 1.0198 0.1412 0.036 Uiso 1 1 calc R . . H53C H 0.5151 1.0873 0.1974 0.036 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 W 0.01160(4) 0.01209(4) 0.01099(4) -0.00082(3) 0.00345(3) -0.00047(3) P1 0.0152(2) 0.0161(2) 0.0165(3) -0.0019(2) 0.0034(2) -0.00282(19) P2 0.0160(2) 0.0148(2) 0.0126(3) -0.00135(19) 0.0043(2) 0.00046(19) P3 0.0170(3) 0.0239(3) 0.0219(3) -0.0041(2) 0.0094(2) -0.0002(2) P4 0.0182(3) 0.0149(2) 0.0169(3) 0.0021(2) 0.0023(2) 0.0022(2) P5 0.0195(3) 0.0158(2) 0.0130(3) 0.0012(2) 0.0048(2) -0.0009(2) C11 0.0147(9) 0.0206(10) 0.0179(11) 0.0009(8) 0.0062(8) -0.0016(8) C12 0.0240(12) 0.0164(10) 0.0337(15) -0.0014(9) 0.0053(10) -0.0053(9) C13 0.0233(11) 0.0307(12) 0.0185(12) -0.0024(10) -0.0009(9) -0.0065(10) C21 0.0202(11) 0.0269(11) 0.0203(12) -0.0088(9) 0.0037(9) -0.0044(9) C22 0.0235(11) 0.0181(10) 0.0222(12) -0.0018(9) 0.0079(9) 0.0053(8) C23 0.0318(13) 0.0270(12) 0.0170(12) -0.0006(9) 0.0129(10) 0.0025(10) C31 0.0155(11) 0.0412(14) 0.0351(15) -0.0036(12) 0.0095(10) 0.0049(10) C32 0.0369(15) 0.0352(14) 0.0359(16) -0.0180(12) 0.0150(13) 0.0000(12) C33 0.0278(14) 0.0501(17) 0.0376(17) 0.0035(13) 0.0203(13) -0.0013(12) C41 0.0334(13) 0.0250(12) 0.0210(13) 0.0061(9) 0.0082(11) -0.0017(10) C42 0.0274(13) 0.0292(12) 0.0230(13) 0.0020(10) -0.0022(10) 0.0045(10) C43 0.0299(13) 0.0157(10) 0.0356(15) 0.0039(10) 0.0074(11) 0.0061(9) C51 0.0252(12) 0.0227(11) 0.0205(12) 0.0028(9) 0.0030(10) 0.0038(9) C52 0.0373(14) 0.0348(13) 0.0145(12) 0.0012(10) 0.0080(10) -0.0007(11) C53 0.0325(13) 0.0189(10) 0.0216(13) 0.0019(9) 0.0105(10) -0.0054(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 W H1 1.73(3) . ? W C11 2.312(2) . ? W P1 2.3718(6) . ? W P4 2.4156(6) . ? W P5 2.4212(6) . ? W P3 2.4242(6) . ? W P2 2.4465(5) . ? P1 C11 1.766(2) . ? P1 C13 1.836(2) . ? P1 C12 1.840(2) . ? P2 C21 1.833(2) . ? P2 C23 1.839(2) . ? P2 C22 1.841(2) . ? P3 C31 1.840(3) . ? P3 C32 1.846(3) . ? P3 C33 1.847(3) . ? P4 C42 1.850(3) . ? P4 C43 1.853(2) . ? P4 C41 1.859(2) . ? P5 C53 1.848(2) . ? P5 C51 1.856(2) . ? P5 C52 1.859(3) . ? 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 H1 W C11 155.7(9) . . ? H1 W P1 159.6(9) . . ? C11 W P1 44.27(6) . . ? H1 W P4 92.8(9) . . ? C11 W P4 89.48(6) . . ? P1 W P4 90.73(2) . . ? H1 W P5 87.1(9) . . ? C11 W P5 90.20(6) . . ? P1 W P5 89.753(19) . . ? P4 W P5 178.936(19) . . ? H1 W P3 61.7(9) . . ? C11 W P3 142.54(6) . . ? P1 W P3 98.37(2) . . ? P4 W P3 88.23(2) . . ? P5 W P3 92.64(2) . . ? H1 W P2 73.1(9) . . ? C11 W P2 82.82(6) . . ? P1 W P2 127.092(19) . . ? P4 W P2 88.197(19) . . ? P5 W P2 90.756(19) . . ? P3 W P2 134.429(19) . . ? C11 P1 C13 111.49(11) . . ? C11 P1 C12 113.85(11) . . ? C13 P1 C12 97.25(11) . . ? C11 P1 W 66.07(7) . . ? C13 P1 W 129.98(8) . . ? C12 P1 W 130.67(9) . . ? C21 P2 C23 99.89(12) . . ? C21 P2 C22 98.32(11) . . ? C23 P2 C22 95.41(11) . . ? C21 P2 W 116.02(8) . . ? C23 P2 W 120.49(8) . . ? C22 P2 W 121.97(8) . . ? C31 P3 C32 101.08(13) . . ? C31 P3 C33 95.06(13) . . ? C32 P3 C33 97.06(14) . . ? C31 P3 W 117.41(9) . . ? C32 P3 W 118.62(9) . . ? C33 P3 W 122.75(9) . . ? C42 P4 C43 96.87(12) . . ? C42 P4 C41 97.55(12) . . ? C43 P4 C41 94.95(11) . . ? C42 P4 W 120.09(8) . . ? C43 P4 W 120.98(9) . . ? C41 P4 W 120.58(8) . . ? C53 P5 C51 98.67(11) . . ? C53 P5 C52 97.47(12) . . ? C51 P5 C52 96.29(12) . . ? C53 P5 W 117.73(8) . . ? C51 P5 W 120.34(8) . . ? C52 P5 W 121.26(9) . . ? P1 C11 W 69.66(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.116 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.114