# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Stephan, Douglas' _publ_contact_author_email dstephan@chem.utoronto.ca loop_ _publ_author_name 'Michael Sgro' 'Johannes Doemer' 'Douglas Stephan' data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 881300' #TrackingRef '- allcifs-May7.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C22 H39 B2 Cl4 O P' _chemical_formula_weight 513.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 8.9031(5) _cell_length_b 11.5796(7) _cell_length_c 13.1403(8) _cell_angle_alpha 93.817(4) _cell_angle_beta 99.079(4) _cell_angle_gamma 92.330(4) _cell_volume 1332.95(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5288 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6950 _exptl_absorpt_correction_T_max 0.7456 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16039 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4689 _reflns_number_gt 3311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.1889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4689 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Cl1 Cl 0.78188(9) 0.12265(7) -0.04653(6) 0.0254(2) Uani 1 1 d . . . Cl2 Cl 0.69013(9) 0.37051(6) -0.06714(6) 0.0268(2) Uani 1 1 d . . . Cl3 Cl 0.24564(10) 0.21083(9) -0.29107(7) 0.0477(3) Uani 1 1 d . . . Cl4 Cl 0.37991(9) -0.02290(7) -0.25381(7) 0.0385(2) Uani 1 1 d . . . P1 P 0.13102(8) 0.30489(6) 0.25494(6) 0.01400(18) Uani 1 1 d . . . O1 O 0.4950(2) 0.18098(16) -0.14140(14) 0.0173(5) Uani 1 1 d . . . C1 C 0.6911(3) 0.2067(2) -0.2467(2) 0.0147(6) Uani 1 1 d . . . C2 C 0.8257(3) 0.2237(2) -0.2866(2) 0.0199(7) Uani 1 1 d . . . H2 H 0.9168 0.2490 -0.2413 0.024 Uiso 1 1 calc R . . C3 C 0.8282(3) 0.2044(2) -0.3908(2) 0.0227(7) Uani 1 1 d . . . H3 H 0.9204 0.2170 -0.4171 0.027 Uiso 1 1 calc R . . C4 C 0.6954(4) 0.1663(3) -0.4576(2) 0.0250(8) Uani 1 1 d . . . H4 H 0.6965 0.1542 -0.5297 0.030 Uiso 1 1 calc R . . C5 C 0.5619(3) 0.1461(3) -0.4187(2) 0.0224(7) Uani 1 1 d . . . H5 H 0.4718 0.1187 -0.4640 0.027 Uiso 1 1 calc R . . C6 C 0.5589(3) 0.1657(2) -0.3134(2) 0.0169(7) Uani 1 1 d . . . C7 C 0.4254(3) 0.1558(3) -0.0516(2) 0.0235(7) Uani 1 1 d . . . H7A H 0.5070 0.1446 0.0068 0.028 Uiso 1 1 calc R . . H7B H 0.3632 0.0821 -0.0675 0.028 Uiso 1 1 calc R . . C8 C 0.3253(3) 0.2495(3) -0.0181(2) 0.0237(7) Uani 1 1 d . . . H8A H 0.2332 0.2532 -0.0707 0.028 Uiso 1 1 calc R . . H8B H 0.3816 0.3259 -0.0098 0.028 Uiso 1 1 calc R . . C9 C 0.2808(3) 0.2189(3) 0.0841(2) 0.0230(7) Uani 1 1 d . . . H9A H 0.3737 0.2190 0.1365 0.028 Uiso 1 1 calc R . . H9B H 0.2320 0.1397 0.0757 0.028 Uiso 1 1 calc R . . C10 C 0.1704(3) 0.3043(2) 0.1228(2) 0.0173(7) Uani 1 1 d . . . H10A H 0.0716 0.2910 0.0761 0.021 Uiso 1 1 calc R . . H10B H 0.2097 0.3834 0.1131 0.021 Uiso 1 1 calc R . . C11 C 0.2985(3) 0.3815(2) 0.3435(2) 0.0208(7) Uani 1 1 d . . . C12 C 0.2936(4) 0.3640(3) 0.4571(2) 0.0282(8) Uani 1 1 d . . . H12A H 0.3752 0.4124 0.5005 0.042 Uiso 1 1 calc R . . H12B H 0.3077 0.2824 0.4697 0.042 Uiso 1 1 calc R . . H12C H 0.1949 0.3861 0.4741 0.042 Uiso 1 1 calc R . . C13 C 0.3012(4) 0.5123(3) 0.3288(3) 0.0311(8) Uani 1 1 d . . . H13A H 0.2110 0.5453 0.3510 0.047 Uiso 1 1 calc R . . H13B H 0.3011 0.5246 0.2557 0.047 Uiso 1 1 calc R . . H13C H 0.3933 0.5503 0.3703 0.047 Uiso 1 1 calc R . . C14 C 0.4505(3) 0.3399(3) 0.3155(3) 0.0301(8) Uani 1 1 d . . . H14A H 0.5353 0.3764 0.3654 0.045 Uiso 1 1 calc R . . H14B H 0.4607 0.3613 0.2460 0.045 Uiso 1 1 calc R . . H14C H 0.4518 0.2555 0.3175 0.045 Uiso 1 1 calc R . . C15 C -0.0462(3) 0.3908(2) 0.2521(2) 0.0190(7) Uani 1 1 d . . . C16 C -0.0373(3) 0.4931(3) 0.1830(2) 0.0259(8) Uani 1 1 d . . . H16A H -0.1236 0.5419 0.1878 0.039 Uiso 1 1 calc R . . H16B H -0.0408 0.4630 0.1112 0.039 Uiso 1 1 calc R . . H16C H 0.0582 0.5391 0.2063 0.039 Uiso 1 1 calc R . . C17 C -0.0699(4) 0.4379(3) 0.3600(2) 0.0311(8) Uani 1 1 d . . . H17A H -0.1653 0.4780 0.3546 0.047 Uiso 1 1 calc R . . H17B H 0.0153 0.4921 0.3901 0.047 Uiso 1 1 calc R . . H17C H -0.0748 0.3734 0.4043 0.047 Uiso 1 1 calc R . . C18 C -0.1885(3) 0.3146(3) 0.2027(3) 0.0251(8) Uani 1 1 d . . . H18A H -0.2076 0.2545 0.2489 0.038 Uiso 1 1 calc R . . H18B H -0.1716 0.2781 0.1363 0.038 Uiso 1 1 calc R . . H18C H -0.2767 0.3629 0.1916 0.038 Uiso 1 1 calc R . . C19 C 0.0974(3) 0.1521(2) 0.2889(2) 0.0169(7) Uani 1 1 d . . . C20 C 0.0190(4) 0.1465(3) 0.3849(2) 0.0274(8) Uani 1 1 d . . . H20A H -0.0790 0.1830 0.3723 0.041 Uiso 1 1 calc R . . H20B H 0.0840 0.1876 0.4445 0.041 Uiso 1 1 calc R . . H20C H 0.0021 0.0654 0.3990 0.041 Uiso 1 1 calc R . . C21 C -0.0011(3) 0.0799(2) 0.1973(2) 0.0211(7) Uani 1 1 d . . . H21A H -0.0078 -0.0014 0.2132 0.032 Uiso 1 1 calc R . . H21B H 0.0456 0.0860 0.1350 0.032 Uiso 1 1 calc R . . H21C H -0.1035 0.1095 0.1855 0.032 Uiso 1 1 calc R . . C22 C 0.2498(3) 0.0933(2) 0.3113(2) 0.0215(7) Uani 1 1 d . . . H22A H 0.3133 0.1338 0.3719 0.032 Uiso 1 1 calc R . . H22B H 0.3026 0.0964 0.2514 0.032 Uiso 1 1 calc R . . H22C H 0.2306 0.0123 0.3249 0.032 Uiso 1 1 calc R . . B1 B 0.6639(4) 0.2193(3) -0.1319(3) 0.0178(8) Uani 1 1 d . . . B2 B 0.4254(4) 0.1380(3) -0.2522(3) 0.0225(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0293(4) 0.0276(4) 0.0190(4) 0.0007(3) 0.0017(3) 0.0080(3) Cl2 0.0394(5) 0.0186(4) 0.0229(5) -0.0061(3) 0.0109(4) -0.0033(3) Cl3 0.0240(5) 0.0895(8) 0.0323(6) 0.0063(5) 0.0064(4) 0.0268(5) Cl4 0.0313(5) 0.0378(5) 0.0467(6) -0.0144(4) 0.0194(4) -0.0190(4) P1 0.0134(4) 0.0150(4) 0.0141(4) -0.0009(3) 0.0044(3) 0.0009(3) O1 0.0170(11) 0.0225(11) 0.0147(11) 0.0003(9) 0.0103(9) -0.0014(9) C1 0.0179(16) 0.0110(15) 0.0165(16) -0.0007(12) 0.0072(13) 0.0027(12) C2 0.0210(17) 0.0139(16) 0.0258(19) -0.0028(14) 0.0087(14) -0.0015(12) C3 0.0263(18) 0.0167(16) 0.030(2) 0.0042(14) 0.0175(15) 0.0017(13) C4 0.038(2) 0.0271(18) 0.0145(17) 0.0055(14) 0.0124(15) 0.0118(15) C5 0.0223(17) 0.0273(18) 0.0166(18) -0.0006(14) -0.0004(14) 0.0075(14) C6 0.0193(16) 0.0184(16) 0.0143(17) 0.0029(13) 0.0048(13) 0.0077(12) C7 0.0286(18) 0.0245(18) 0.0225(18) 0.0035(14) 0.0186(15) 0.0036(14) C8 0.0284(18) 0.0279(18) 0.0187(18) 0.0025(14) 0.0142(14) 0.0047(14) C9 0.0267(17) 0.0250(17) 0.0215(18) 0.0029(14) 0.0152(14) 0.0059(14) C10 0.0196(16) 0.0190(16) 0.0144(16) 0.0011(13) 0.0063(13) -0.0003(12) C11 0.0188(16) 0.0190(17) 0.0224(18) 0.0009(14) -0.0023(14) -0.0017(13) C12 0.0326(19) 0.0275(19) 0.0201(19) -0.0057(15) -0.0068(15) 0.0026(15) C13 0.0278(19) 0.0236(19) 0.038(2) -0.0019(16) -0.0043(16) -0.0053(14) C14 0.0163(17) 0.0322(19) 0.040(2) 0.0033(16) 0.0003(15) -0.0024(14) C15 0.0151(15) 0.0224(17) 0.0193(17) -0.0041(13) 0.0041(13) 0.0040(12) C16 0.0248(17) 0.0229(17) 0.029(2) -0.0026(15) 0.0028(15) 0.0064(14) C17 0.0291(19) 0.034(2) 0.030(2) -0.0071(16) 0.0079(16) 0.0110(15) C18 0.0135(16) 0.0318(19) 0.030(2) -0.0023(15) 0.0037(14) 0.0028(13) C19 0.0192(16) 0.0156(16) 0.0175(17) 0.0018(13) 0.0075(13) 0.0001(12) C20 0.0340(19) 0.0279(19) 0.0224(19) 0.0028(15) 0.0121(15) -0.0040(15) C21 0.0225(17) 0.0168(16) 0.0247(18) -0.0012(14) 0.0081(14) -0.0037(13) C22 0.0249(17) 0.0174(16) 0.0226(18) 0.0039(14) 0.0044(14) 0.0004(13) B1 0.0177(18) 0.0157(18) 0.020(2) -0.0001(15) 0.0039(15) 0.0003(14) B2 0.0155(18) 0.030(2) 0.021(2) -0.0024(17) 0.0024(16) 0.0020(15) _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 Cl1 B1 1.872(3) . ? Cl2 B1 1.884(3) . ? Cl3 B2 1.855(3) . ? Cl4 B2 1.888(4) . ? P1 C10 1.825(3) . ? P1 C19 1.877(3) . ? P1 C11 1.890(3) . ? P1 C15 1.896(3) . ? O1 C7 1.458(3) . ? O1 B2 1.532(4) . ? O1 B1 1.533(4) . ? C1 C2 1.393(4) . ? C1 C6 1.398(4) . ? C1 B1 1.563(4) . ? C2 C3 1.377(4) . ? C2 H2 0.9500 . ? C3 C4 1.394(4) . ? C3 H3 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.392(4) . ? C5 H5 0.9500 . ? C6 B2 1.570(4) . ? C7 C8 1.517(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.540(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.528(4) . ? C11 C13 1.539(4) . ? C11 C14 1.544(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.534(4) . ? C15 C18 1.541(4) . ? C15 C16 1.546(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.538(4) . ? C19 C22 1.539(4) . ? C19 C21 1.546(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C10 P1 C19 109.70(13) . . ? C10 P1 C11 108.03(14) . . ? C19 P1 C11 111.82(13) . . ? C10 P1 C15 103.80(13) . . ? C19 P1 C15 111.94(13) . . ? C11 P1 C15 111.17(13) . . ? C7 O1 B2 123.3(2) . . ? C7 O1 B1 122.0(2) . . ? B2 O1 B1 112.2(2) . . ? C2 C1 C6 119.1(3) . . ? C2 C1 B1 129.2(3) . . ? C6 C1 B1 111.5(2) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 119.9(3) . . ? C5 C6 B2 128.5(3) . . ? C1 C6 B2 111.4(2) . . ? O1 C7 C8 114.2(2) . . ? O1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? O1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C9 107.5(2) . . ? C7 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? C7 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C8 C9 C10 112.3(2) . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C9 C10 P1 120.6(2) . . ? C9 C10 H10A 107.2 . . ? P1 C10 H10A 107.2 . . ? C9 C10 H10B 107.2 . . ? P1 C10 H10B 107.2 . . ? H10A C10 H10B 106.8 . . ? C12 C11 C13 108.7(3) . . ? C12 C11 C14 109.2(2) . . ? C13 C11 C14 105.5(2) . . ? C12 C11 P1 112.2(2) . . ? C13 C11 P1 110.1(2) . . ? C14 C11 P1 110.9(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C18 108.4(2) . . ? C17 C15 C16 109.1(2) . . ? C18 C15 C16 106.3(2) . . ? C17 C15 P1 112.7(2) . . ? C18 C15 P1 110.3(2) . . ? C16 C15 P1 109.9(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 107.9(2) . . ? C20 C19 C21 108.9(2) . . ? C22 C19 C21 107.0(2) . . ? C20 C19 P1 112.3(2) . . ? C22 C19 P1 110.09(19) . . ? C21 C19 P1 110.52(19) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 B1 C1 102.4(2) . . ? O1 B1 Cl1 109.6(2) . . ? C1 B1 Cl1 113.2(2) . . ? O1 B1 Cl2 107.7(2) . . ? C1 B1 Cl2 116.0(2) . . ? Cl1 B1 Cl2 107.73(17) . . ? O1 B2 C6 102.1(2) . . ? O1 B2 Cl3 109.6(2) . . ? C6 B2 Cl3 116.3(2) . . ? O1 B2 Cl4 107.6(2) . . ? C6 B2 Cl4 112.0(2) . . ? Cl3 B2 Cl4 108.66(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.662 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.067 #===end data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 881301' #TrackingRef '- allcifs-May7.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C19 H31 B2 Cl4 O2 P' _chemical_formula_weight 485.83 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.3108(5) _cell_length_b 14.2805(5) _cell_length_c 14.9742(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2418.69(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3486 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.65 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6903 _exptl_absorpt_correction_T_max 0.7456 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12517 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5551 _reflns_number_gt 3936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(9) _refine_ls_number_reflns 5551 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Cl1 Cl 0.69743(9) 0.29886(7) 0.14572(8) 0.0317(3) Uani 1 1 d . . . Cl2 Cl 0.71018(10) 0.25262(7) 0.34757(7) 0.0289(2) Uani 1 1 d . . . Cl3 Cl 0.48247(10) 0.18357(9) 0.44080(8) 0.0411(3) Uani 1 1 d . . . Cl4 Cl 0.71166(10) 0.07932(8) 0.46969(8) 0.0371(3) Uani 1 1 d . . . P1 P 1.09710(9) 0.17734(7) 0.21205(7) 0.0189(2) Uani 1 1 d . . . O1 O 0.8632(2) 0.18011(19) 0.2186(2) 0.0238(6) Uani 1 1 d . . . O2 O 0.9435(3) 0.3212(2) 0.2406(3) 0.0484(10) Uani 1 1 d . . . C1 C 1.2121(4) 0.2708(3) 0.1928(3) 0.0277(10) Uani 1 1 d . . . C2 C 1.2049(4) 0.3503(3) 0.2624(4) 0.0394(13) Uani 1 1 d . . . H2A H 1.2544 0.4029 0.2430 0.059 Uiso 1 1 calc R . . H2B H 1.2329 0.3273 0.3203 0.059 Uiso 1 1 calc R . . H2C H 1.1227 0.3713 0.2681 0.059 Uiso 1 1 calc R . . C3 C 1.1923(4) 0.3160(3) 0.1015(4) 0.0432(13) Uani 1 1 d . . . H3A H 1.1111 0.3397 0.0978 0.065 Uiso 1 1 calc R . . H3B H 1.2053 0.2694 0.0545 0.065 Uiso 1 1 calc R . . H3C H 1.2479 0.3681 0.0937 0.065 Uiso 1 1 calc R . . C4 C 1.3387(4) 0.2283(3) 0.1968(4) 0.0347(12) Uani 1 1 d . . . H4A H 1.3459 0.1785 0.1522 0.052 Uiso 1 1 calc R . . H4B H 1.3528 0.2024 0.2564 0.052 Uiso 1 1 calc R . . H4C H 1.3970 0.2774 0.1844 0.052 Uiso 1 1 calc R . . C5 C 1.0749(4) 0.0990(3) 0.1114(3) 0.0266(10) Uani 1 1 d . . . C6 C 1.0009(4) 0.1526(3) 0.0388(3) 0.0369(12) Uani 1 1 d . . . H6A H 0.9911 0.1127 -0.0139 0.055 Uiso 1 1 calc R . . H6B H 1.0425 0.2102 0.0218 0.055 Uiso 1 1 calc R . . H6C H 0.9231 0.1685 0.0632 0.055 Uiso 1 1 calc R . . C7 C 1.1936(4) 0.0670(3) 0.0726(3) 0.0381(12) Uani 1 1 d . . . H7A H 1.2368 0.0308 0.1175 0.057 Uiso 1 1 calc R . . H7B H 1.2403 0.1220 0.0555 0.057 Uiso 1 1 calc R . . H7C H 1.1796 0.0279 0.0198 0.057 Uiso 1 1 calc R . . C8 C 1.0028(4) 0.0127(3) 0.1362(3) 0.0327(11) Uani 1 1 d . . . H8A H 0.9936 -0.0274 0.0836 0.049 Uiso 1 1 calc R . . H8B H 0.9247 0.0322 0.1576 0.049 Uiso 1 1 calc R . . H8C H 1.0437 -0.0221 0.1834 0.049 Uiso 1 1 calc R . . C9 C 1.1175(4) 0.1114(3) 0.3204(3) 0.0270(10) Uani 1 1 d . . . C10 C 1.1562(4) 0.1795(4) 0.3942(3) 0.0425(12) Uani 1 1 d . . . H10A H 1.1019 0.2329 0.3960 0.064 Uiso 1 1 calc R . . H10B H 1.2365 0.2018 0.3817 0.064 Uiso 1 1 calc R . . H10C H 1.1551 0.1472 0.4519 0.064 Uiso 1 1 calc R . . C11 C 1.0026(4) 0.0647(3) 0.3505(3) 0.0360(11) Uani 1 1 d . . . H11A H 1.0177 0.0267 0.4038 0.054 Uiso 1 1 calc R . . H11B H 0.9726 0.0245 0.3025 0.054 Uiso 1 1 calc R . . H11C H 0.9438 0.1129 0.3645 0.054 Uiso 1 1 calc R . . C12 C 1.2142(4) 0.0362(3) 0.3071(3) 0.0384(12) Uani 1 1 d . . . H12A H 1.2281 0.0035 0.3637 0.058 Uiso 1 1 calc R . . H12B H 1.2876 0.0662 0.2873 0.058 Uiso 1 1 calc R . . H12C H 1.1882 -0.0089 0.2619 0.058 Uiso 1 1 calc R . . C13 C 0.6545(3) 0.1160(3) 0.2190(3) 0.0211(9) Uani 1 1 d . . . C14 C 0.6343(3) 0.0668(3) 0.1389(3) 0.0274(10) Uani 1 1 d . . . H14 H 0.6721 0.0871 0.0856 0.033 Uiso 1 1 calc R . . C15 C 0.5610(4) -0.0101(3) 0.1362(4) 0.0329(11) Uani 1 1 d . . . H15 H 0.5491 -0.0420 0.0813 0.039 Uiso 1 1 calc R . . C16 C 0.5048(4) -0.0411(3) 0.2121(3) 0.0318(10) Uani 1 1 d . . . H16 H 0.4535 -0.0936 0.2098 0.038 Uiso 1 1 calc R . . C17 C 0.5242(4) 0.0056(3) 0.2925(3) 0.0276(10) Uani 1 1 d . . . H17 H 0.4868 -0.0165 0.3452 0.033 Uiso 1 1 calc R . . C18 C 0.5980(3) 0.0848(3) 0.2972(3) 0.0213(9) Uani 1 1 d . . . C19 C 0.9510(3) 0.2405(3) 0.2260(3) 0.0229(9) Uani 1 1 d . . . B1 B 0.7365(4) 0.2045(3) 0.2238(3) 0.0232(10) Uani 1 1 d . . . B2 B 0.6169(4) 0.1378(4) 0.3873(4) 0.0280(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0356(6) 0.0290(5) 0.0305(6) 0.0100(5) -0.0079(5) 0.0005(5) Cl2 0.0343(6) 0.0268(5) 0.0257(5) -0.0033(5) -0.0020(5) 0.0015(5) Cl3 0.0234(5) 0.0691(8) 0.0307(6) -0.0125(6) 0.0025(5) 0.0097(6) Cl4 0.0291(6) 0.0539(7) 0.0282(6) 0.0144(5) -0.0046(5) 0.0055(6) P1 0.0171(5) 0.0200(5) 0.0197(5) -0.0018(5) 0.0004(5) -0.0006(4) O1 0.0187(13) 0.0196(13) 0.0330(17) 0.0003(15) 0.0007(13) -0.0008(12) O2 0.0247(17) 0.0240(16) 0.096(3) -0.0155(18) -0.0039(18) -0.0010(14) C1 0.018(2) 0.025(2) 0.040(3) -0.0008(19) 0.004(2) -0.0056(19) C2 0.027(2) 0.026(2) 0.065(4) -0.018(2) 0.002(3) -0.009(2) C3 0.041(3) 0.033(2) 0.055(3) 0.016(3) 0.005(3) -0.003(2) C4 0.021(2) 0.034(2) 0.049(3) 0.000(2) 0.007(2) -0.0073(19) C5 0.027(2) 0.028(2) 0.025(2) -0.011(2) 0.0011(19) -0.0058(19) C6 0.043(3) 0.047(3) 0.020(2) -0.002(2) 0.000(2) -0.003(2) C7 0.042(3) 0.040(3) 0.032(3) -0.018(2) 0.006(2) 0.001(2) C8 0.038(3) 0.026(2) 0.034(3) -0.006(2) -0.006(2) -0.004(2) C9 0.026(2) 0.036(2) 0.019(2) 0.0049(19) -0.0010(18) 0.004(2) C10 0.038(3) 0.064(3) 0.026(3) -0.015(3) -0.001(2) -0.003(3) C11 0.037(3) 0.044(3) 0.027(2) 0.011(2) 0.002(2) 0.000(2) C12 0.038(3) 0.040(3) 0.038(3) 0.010(2) -0.004(2) 0.014(2) C13 0.018(2) 0.0188(18) 0.027(2) -0.001(2) 0.0015(19) 0.0073(16) C14 0.025(2) 0.032(2) 0.025(2) 0.001(2) 0.001(2) 0.0037(19) C15 0.031(2) 0.025(2) 0.043(3) -0.009(2) -0.004(2) -0.0001(19) C16 0.022(2) 0.026(2) 0.048(3) -0.002(2) 0.002(2) -0.0041(19) C17 0.018(2) 0.029(2) 0.035(3) 0.009(2) 0.004(2) 0.0024(18) C18 0.0154(19) 0.0221(19) 0.026(2) 0.0022(19) -0.0022(18) 0.0079(17) C19 0.019(2) 0.023(2) 0.027(2) 0.002(2) -0.0006(18) -0.0015(17) B1 0.029(3) 0.025(2) 0.016(2) -0.002(2) 0.004(2) 0.000(2) B2 0.020(3) 0.037(3) 0.027(3) 0.002(2) 0.006(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 B1 1.838(5) . ? Cl2 B1 1.999(5) . ? Cl2 B2 2.038(5) . ? Cl3 B2 1.839(5) . ? Cl4 B2 1.836(5) . ? P1 C1 1.885(4) . ? P1 C9 1.889(4) . ? P1 C19 1.894(4) . ? P1 C5 1.895(4) . ? O1 C19 1.320(4) . ? O1 B1 1.477(5) . ? O2 C19 1.177(5) . ? C1 C3 1.528(6) . ? C1 C2 1.544(6) . ? C1 C4 1.556(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.523(6) . ? C5 C7 1.532(6) . ? C5 C6 1.570(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.530(6) . ? C9 C10 1.535(6) . ? C9 C12 1.546(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.406(6) . ? C13 C14 1.409(6) . ? C13 B1 1.569(6) . ? C14 C15 1.376(6) . ? C14 H14 0.9500 . ? C15 C16 1.377(6) . ? C15 H15 0.9500 . ? C16 C17 1.393(6) . ? C16 H16 0.9500 . ? C17 C18 1.408(6) . ? C17 H17 0.9500 . ? C18 B2 1.561(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Cl2 B2 94.1(2) . . ? C1 P1 C9 113.6(2) . . ? C1 P1 C19 106.36(18) . . ? C9 P1 C19 104.43(19) . . ? C1 P1 C5 112.81(19) . . ? C9 P1 C5 113.89(19) . . ? C19 P1 C5 104.69(19) . . ? C19 O1 B1 124.9(3) . . ? C3 C1 C2 106.5(4) . . ? C3 C1 C4 109.5(4) . . ? C2 C1 C4 108.0(4) . . ? C3 C1 P1 109.6(3) . . ? C2 C1 P1 112.4(3) . . ? C4 C1 P1 110.7(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 108.7(3) . . ? C8 C5 C6 106.1(3) . . ? C7 C5 C6 110.5(4) . . ? C8 C5 P1 110.8(3) . . ? C7 C5 P1 111.2(3) . . ? C6 C5 P1 109.4(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C10 107.8(4) . . ? C11 C9 C12 109.6(4) . . ? C10 C9 C12 109.3(4) . . ? C11 C9 P1 111.5(3) . . ? C10 C9 P1 109.7(3) . . ? C12 C9 P1 108.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.6(4) . . ? C18 C13 B1 119.0(4) . . ? C14 C13 B1 122.4(4) . . ? C15 C14 C13 121.3(4) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.7(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 121.4(4) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C13 C18 C17 118.8(4) . . ? C13 C18 B2 120.3(4) . . ? C17 C18 B2 120.9(4) . . ? O2 C19 O1 127.0(4) . . ? O2 C19 P1 123.4(3) . . ? O1 C19 P1 109.6(3) . . ? O1 B1 C13 112.4(3) . . ? O1 B1 Cl1 111.9(3) . . ? C13 B1 Cl1 114.8(3) . . ? O1 B1 Cl2 105.9(3) . . ? C13 B1 Cl2 103.4(3) . . ? Cl1 B1 Cl2 107.6(2) . . ? C18 B2 Cl4 116.1(3) . . ? C18 B2 Cl3 115.8(3) . . ? Cl4 B2 Cl3 110.6(3) . . ? C18 B2 Cl2 102.0(3) . . ? Cl4 B2 Cl2 105.0(2) . . ? Cl3 B2 Cl2 105.6(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.513 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.079 #===end