#Copyright The Royal Society of Chemistry, 1998 # PLATINUM CATALYSED 1,4-DIBORATION OF 1,3-DIENES # # N.C. NORMAN (Corresponding Author) # # # data_1 _publ_section_exptl_refinement ; Unit cell dimensions were determined from 13827 reflections (at 0.3\% steps in \w) each at 30 seconds exposure (Clegg, in-house programme). A full hemisphere of reiciprocal space was scanned by 0.3\% \w steps at \f 0, 90 and 180\% with the area detector held at 2\q = -29\%. The crystal-to-detector distance was 5.0 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times the U~iso~ value of their attached carbon (1.5 U~iso~ for methyl hydrogens). ; _audit_creation_method SHELXL _chemical_name_systematic ; bis(dimethyl-L-tartrate)diboron ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 B2 O12' _chemical_formula_weight 373.87 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 2~1~ 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 9.0355(8) _cell_length_b 16.9385(15) _cell_length_c 22.382(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3425.5(5) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 13827 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method ? _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 21864 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.56 _reflns_number_total 8032 _reflns_number_observed 6283 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'local programs' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'see text' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(6) _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 -0.26(74) _refine_ls_number_reflns 8031 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_obs 0.0512 _refine_ls_wR_factor_all 0.1206 _refine_ls_wR_factor_obs 0.1119 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.023 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max -0.062 _refine_ls_shift/esd_mean 0.008 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group B1 B 0.8323(3) 0.93443(15) 0.22169(13) 0.0256(6) Uani 1 d . . O1 O 0.6832(2) 0.94740(9) 0.21506(7) 0.0275(4) Uani 1 d . . O2 O 0.9130(2) 0.96264(10) 0.17454(7) 0.0276(4) Uani 1 d . . C1 C 0.6630(3) 0.99776(13) 0.16434(10) 0.0247(5) Uani 1 d . . H1 H 0.5765(3) 0.98074(13) 0.13960(10) 0.030 Uiso 1 calc R . C2 C 0.8108(3) 0.98861(13) 0.12967(11) 0.0253(5) Uani 1 d . . H2 H 0.8428(3) 1.04043(13) 0.11258(11) 0.030 Uiso 1 calc R . C3 C 0.7989(3) 0.92722(14) 0.08128(11) 0.0276(5) Uani 1 d . . O3 O 0.8412(2) 0.85940(11) 0.08672(8) 0.0411(5) Uani 1 d . . O4 O 0.7340(2) 0.95641(10) 0.03345(7) 0.0335(4) Uani 1 d . . C4 C 0.7051(4) 0.9001(2) -0.01490(11) 0.0431(7) Uani 1 d . . H4A H 0.7992(4) 0.8804(9) -0.0307(6) 0.065 Uiso 1 calc R . H4B H 0.6499(20) 0.9265(4) -0.0469(4) 0.065 Uiso 1 calc R . H4C H 0.6467(19) 0.8558(6) 0.0006(2) 0.065 Uiso 1 calc R . C5 C 0.6469(3) 1.08321(14) 0.18499(11) 0.0241(5) Uani 1 d . . O5 O 0.6984(2) 1.10879(10) 0.23028(7) 0.0304(4) Uani 1 d . . O6 O 0.5755(2) 1.12432(9) 0.14343(8) 0.0327(4) Uani 1 d . . C6 C 0.5636(3) 1.20920(14) 0.15484(13) 0.0401(7) Uani 1 d . . H6A H 0.4789(14) 1.2193(2) 0.1811(7) 0.060 Uiso 1 calc R . H6B H 0.5495(22) 1.2372(2) 0.1169(2) 0.060 Uiso 1 calc R . H6C H 0.6545(10) 1.2279(3) 0.1741(8) 0.060 Uiso 1 calc R . B2 B 0.9045(3) 0.88664(15) 0.28185(12) 0.0250(6) Uani 1 d . . O7 O 1.0415(2) 0.90037(9) 0.30525(7) 0.0255(4) Uani 1 d . . O8 O 0.8244(2) 0.83152(9) 0.31249(7) 0.0252(4) Uani 1 d . . C7 C 1.0612(3) 0.84867(13) 0.35509(10) 0.0236(5) Uani 1 d . . H7 H 1.1447(3) 0.81151(13) 0.34677(10) 0.028 Uiso 1 calc R . C8 C 0.9151(3) 0.80198(13) 0.35943(10) 0.0237(5) Uani 1 d . . H8 H 0.8668(3) 0.81476(13) 0.39845(10) 0.028 Uiso 1 calc R . C9 C 0.9344(3) 0.71235(13) 0.35529(10) 0.0238(5) Uani 1 d . . O9 O 1.0453(2) 0.67875(10) 0.37015(8) 0.0343(4) Uani 1 d . . O10 O 0.8100(2) 0.67879(10) 0.33709(9) 0.0342(4) Uani 1 d . . C10 C 0.8110(3) 0.59272(14) 0.33264(14) 0.0391(6) Uani 1 d . . H10A H 0.8943(13) 0.5759(2) 0.3076(7) 0.059 Uiso 1 calc R . H10B H 0.7180(10) 0.5747(2) 0.3147(8) 0.059 Uiso 1 calc R . H10C H 0.8215(21) 0.56982(14) 0.3726(2) 0.059 Uiso 1 calc R . C11 C 1.0951(3) 0.89605(15) 0.41068(11) 0.0280(5) Uani 1 d . . O11 O 1.1100(2) 0.96661(11) 0.41323(8) 0.0360(4) Uani 1 d . . O12 O 1.1070(3) 0.84815(12) 0.45770(8) 0.0519(6) Uani 1 d . . C12 C 1.1430(5) 0.8872(2) 0.51382(13) 0.0680(11) Uani 1 d . . H12A H 1.2415(14) 0.9111(14) 0.5109(5) 0.102 Uiso 1 calc R . H12B H 1.1421(31) 0.8485(4) 0.5463(2) 0.102 Uiso 1 calc R . H12C H 1.0696(18) 0.9284(11) 0.5220(6) 0.102 Uiso 1 calc R . B3 B 0.6207(3) 0.4429(2) 0.21502(13) 0.0262(6) Uani 1 d . . O13 O 0.6037(2) 0.41725(10) 0.15749(7) 0.0310(4) Uani 1 d . . O14 O 0.5738(2) 0.51872(9) 0.22312(7) 0.0273(4) Uani 1 d . . C13 C 0.5431(3) 0.48177(14) 0.12259(11) 0.0266(5) Uani 1 d . . H13 H 0.6189(3) 0.50280(14) 0.09417(11) 0.032 Uiso 1 calc R . C14 C 0.5023(3) 0.54460(14) 0.16971(11) 0.0251(5) Uani 1 d . . H14 H 0.3927(3) 0.54423(14) 0.17599(11) 0.030 Uiso 1 calc R . C15 C 0.5507(3) 0.62712(14) 0.15177(11) 0.0258(5) Uani 1 d . . O15 O 0.5229(2) 0.65337(11) 0.10347(9) 0.0426(5) Uani 1 d . . O16 O 0.6179(2) 0.66474(10) 0.19558(8) 0.0348(4) Uani 1 d . . C16 C 0.6650(3) 0.7457(2) 0.18351(14) 0.0400(7) Uani 1 d . . H16A H 0.7051(19) 0.7692(4) 0.2201(2) 0.060 Uiso 1 calc R . H16B H 0.5799(5) 0.7768(3) 0.1699(8) 0.060 Uiso 1 calc R . H16C H 0.7414(15) 0.7456(2) 0.1525(6) 0.060 Uiso 1 calc R . C17 C 0.4116(3) 0.44779(14) 0.08873(11) 0.0274(5) Uani 1 d . . O17 O 0.2852(2) 0.45384(11) 0.10279(8) 0.0351(4) Uani 1 d . . O18 O 0.4614(2) 0.40668(12) 0.04183(8) 0.0414(5) Uani 1 d . . C18 C 0.3502(4) 0.3628(2) 0.00880(13) 0.0493(8) Uani 1 d . . H18A H 0.3137(18) 0.3191(8) 0.0334(4) 0.074 Uiso 1 calc R . H18B H 0.3941(8) 0.3417(11) -0.0279(5) 0.074 Uiso 1 calc R . H18C H 0.2677(12) 0.3979(4) -0.0014(9) 0.074 Uiso 1 calc R . B4 B 0.6907(3) 0.3871(2) 0.27074(12) 0.0248(6) Uani 1 d . . O19 O 0.6793(2) 0.30602(9) 0.27107(8) 0.0319(4) Uani 1 d . . O20 O 0.7542(2) 0.41587(9) 0.32090(8) 0.0305(4) Uani 1 d . . C19 C 0.7462(3) 0.27653(14) 0.32402(11) 0.0275(5) Uani 1 d . . H19 H 0.6731(3) 0.24472(14) 0.34738(11) 0.033 Uiso 1 calc R . C20 C 0.7910(3) 0.35191(14) 0.35978(11) 0.0271(5) Uani 1 d . . H20 H 0.8993(3) 0.35169(14) 0.36901(11) 0.033 Uiso 1 calc R . C21 C 0.7011(3) 0.3582(2) 0.41602(11) 0.0320(6) Uani 1 d . . O23 O 0.5863(3) 0.3940(2) 0.42077(9) 0.0604(7) Uani 1 d . . O24 O 0.7624(2) 0.31605(12) 0.45911(8) 0.0422(5) Uani 1 d . . C22 C 0.6809(4) 0.3125(2) 0.51490(13) 0.0572(9) Uani 1 d . . H22A H 0.7429(11) 0.2880(14) 0.5457(3) 0.086 Uiso 1 calc R . H22B H 0.5910(15) 0.2810(12) 0.5093(3) 0.086 Uiso 1 calc R . H22C H 0.6539(24) 0.3660(2) 0.5274(6) 0.086 Uiso 1 calc R . C23 C 0.8774(3) 0.22570(14) 0.30675(11) 0.0248(5) Uani 1 d . . O21 O 0.9634(2) 0.24117(11) 0.26820(9) 0.0400(5) Uani 1 d . . O22 O 0.8826(2) 0.16143(10) 0.34108(8) 0.0349(4) Uani 1 d . . C24 C 0.9961(3) 0.1040(2) 0.32522(15) 0.0479(8) Uani 1 d . . H24A H 1.0932(5) 0.1298(3) 0.3251(10) 0.072 Uiso 1 calc R . H24B H 0.9753(14) 0.0826(10) 0.2854(4) 0.072 Uiso 1 calc R . H24C H 0.9962(17) 0.0610(7) 0.3545(6) 0.072 Uiso 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 B1 0.0336(14) 0.0100(12) 0.033(2) -0.0036(11) -0.0045(12) 0.0004(10) O1 0.0349(9) 0.0167(8) 0.0307(9) 0.0073(7) -0.0002(8) 0.0007(7) O2 0.0321(8) 0.0215(9) 0.0292(9) -0.0003(7) -0.0043(7) -0.0002(7) C1 0.0336(12) 0.0158(11) 0.0246(12) 0.0018(9) -0.0051(10) -0.0010(10) C2 0.0324(12) 0.0155(11) 0.0279(12) 0.0034(9) -0.0040(10) -0.0022(10) C3 0.0325(12) 0.0217(13) 0.0285(13) 0.0005(10) 0.0013(10) -0.0048(10) O3 0.0625(12) 0.0204(10) 0.0404(11) -0.0027(8) -0.0073(10) 0.0039(9) O4 0.0497(11) 0.0258(10) 0.0249(9) -0.0014(7) -0.0061(8) -0.0052(8) C4 0.062(2) 0.041(2) 0.0259(14) -0.0067(12) -0.0013(13) -0.012(2) C5 0.0277(11) 0.0171(12) 0.0275(13) 0.0026(10) -0.0031(10) -0.0030(9) O5 0.0429(10) 0.0193(9) 0.0290(9) -0.0010(7) -0.0024(8) -0.0061(8) O6 0.0473(10) 0.0106(8) 0.0403(10) -0.0010(7) -0.0147(9) 0.0042(7) C6 0.054(2) 0.0093(11) 0.057(2) -0.0009(11) -0.0118(14) 0.0046(12) B2 0.0357(14) 0.0118(12) 0.0276(14) -0.0045(10) 0.0016(12) 0.0051(11) O7 0.0366(9) 0.0155(8) 0.0242(8) 0.0044(6) -0.0025(7) -0.0004(7) O8 0.0316(8) 0.0125(8) 0.0314(9) 0.0007(7) -0.0007(7) 0.0028(7) C7 0.0335(12) 0.0131(10) 0.0241(12) 0.0025(9) 0.0011(10) 0.0011(10) C8 0.0317(11) 0.0113(11) 0.0282(12) -0.0003(9) 0.0009(10) 0.0024(9) C9 0.0354(13) 0.0136(11) 0.0223(12) 0.0021(9) 0.0001(10) -0.0004(10) O9 0.0434(10) 0.0145(8) 0.0451(11) 0.0029(7) -0.0106(9) 0.0042(8) O10 0.0362(9) 0.0085(8) 0.0578(12) -0.0026(8) 0.0001(9) -0.0011(7) C10 0.051(2) 0.0073(11) 0.059(2) -0.0011(11) -0.0015(14) -0.0019(11) C11 0.0359(13) 0.0220(12) 0.0262(12) 0.0018(10) -0.0023(10) -0.0026(11) O11 0.0510(11) 0.0183(9) 0.0386(10) -0.0056(8) -0.0074(9) -0.0030(8) O12 0.097(2) 0.0300(11) 0.0283(10) 0.0050(8) -0.0155(11) -0.0187(12) C12 0.113(3) 0.061(2) 0.030(2) 0.0015(15) -0.013(2) -0.033(2) B3 0.0273(13) 0.0174(13) 0.034(2) 0.0006(11) 0.0021(12) -0.0007(10) O13 0.0432(10) 0.0182(9) 0.0317(10) -0.0010(7) -0.0031(8) 0.0096(7) O14 0.0387(9) 0.0151(8) 0.0280(9) 0.0001(7) -0.0011(7) 0.0027(7) C13 0.0360(12) 0.0135(11) 0.0303(13) 0.0023(9) 0.0026(11) 0.0040(10) C14 0.0298(12) 0.0137(11) 0.0319(13) -0.0015(9) 0.0002(10) 0.0002(9) C15 0.0292(12) 0.0153(11) 0.0329(14) 0.0004(10) -0.0042(11) 0.0039(9) O15 0.0614(12) 0.0207(10) 0.0457(12) 0.0074(8) -0.0153(10) -0.0042(9) O16 0.0454(10) 0.0170(9) 0.0419(11) 0.0018(7) -0.0060(8) -0.0093(8) C16 0.045(2) 0.0166(13) 0.059(2) 0.0022(12) -0.0045(14) -0.0116(12) C17 0.0425(14) 0.0150(11) 0.0248(12) 0.0041(9) 0.0027(11) 0.0015(11) O17 0.0430(11) 0.0257(10) 0.0365(11) 0.0001(8) -0.0017(8) -0.0028(8) O18 0.0563(12) 0.0336(11) 0.0342(11) -0.0108(8) 0.0081(9) -0.0047(10) C18 0.076(2) 0.039(2) 0.034(2) -0.0129(13) 0.005(2) -0.015(2) B4 0.0292(13) 0.0120(12) 0.0331(15) 0.0008(10) 0.0036(12) 0.0021(10) O19 0.0387(9) 0.0114(8) 0.0457(11) -0.0007(7) -0.0138(8) 0.0008(7) O20 0.0489(10) 0.0117(8) 0.0310(9) 0.0043(7) -0.0019(8) -0.0030(7) C19 0.0320(12) 0.0126(11) 0.0379(14) 0.0014(10) -0.0015(11) -0.0004(10) C20 0.0329(12) 0.0152(11) 0.0332(13) 0.0028(10) -0.0028(10) 0.0013(10) C21 0.0415(14) 0.0239(14) 0.0304(13) 0.0042(11) -0.0038(11) 0.0058(12) O23 0.0673(15) 0.074(2) 0.0396(12) 0.0197(11) 0.0132(11) 0.0429(14) O24 0.0516(11) 0.0407(12) 0.0343(10) 0.0123(9) -0.0015(9) 0.0124(10) C22 0.073(2) 0.066(2) 0.032(2) 0.0160(15) 0.005(2) 0.019(2) C23 0.0329(12) 0.0141(11) 0.0274(12) 0.0035(9) -0.0026(11) -0.0030(9) O21 0.0448(10) 0.0235(10) 0.0517(12) 0.0085(8) 0.0119(10) 0.0026(9) O22 0.0531(11) 0.0149(9) 0.0367(10) 0.0074(7) 0.0025(8) 0.0102(8) C24 0.059(2) 0.0213(14) 0.064(2) 0.0040(13) -0.002(2) 0.0181(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O2 1.369(3) . ? B1 O1 1.373(3) . ? B1 B2 1.701(4) . ? O1 C1 1.432(3) . ? O2 C2 1.433(3) . ? C1 C5 1.526(3) . ? C1 C2 1.553(3) . ? C2 C3 1.505(3) . ? C3 O3 1.217(3) . ? C3 O4 1.317(3) . ? O4 C4 1.466(3) . ? C5 O5 1.197(3) . ? C5 O6 1.329(3) . ? O6 C6 1.464(3) . ? B2 O7 1.363(3) . ? B2 O8 1.366(3) . ? O7 C7 1.429(3) . ? O8 C8 1.423(3) . ? C7 C11 1.512(3) . ? C7 C8 1.542(3) . ? C8 C9 1.531(3) . ? C9 O9 1.199(3) . ? C9 O10 1.324(3) . ? O10 C10 1.461(3) . ? C11 O11 1.204(3) . ? C11 O12 1.333(3) . ? O12 C12 1.457(3) . ? B3 O14 1.365(3) . ? B3 O13 1.368(3) . ? B3 B4 1.688(4) . ? O13 C13 1.451(3) . ? O14 C14 1.428(3) . ? C13 C17 1.523(4) . ? C13 C14 1.543(3) . ? C14 C15 1.519(3) . ? C15 O15 1.196(3) . ? C15 O16 1.317(3) . ? O16 C16 1.462(3) . ? C17 O17 1.189(3) . ? C17 O18 1.338(3) . ? O18 C18 1.452(3) . ? B4 O20 1.352(3) . ? B4 O19 1.377(3) . ? O19 C19 1.421(3) . ? O20 C20 1.429(3) . ? C19 C23 1.515(3) . ? C19 C20 1.560(3) . ? C20 C21 1.502(4) . ? C21 O23 1.206(3) . ? C21 O24 1.322(3) . ? O24 C22 1.451(4) . ? C23 O21 1.190(3) . ? C23 O22 1.333(3) . ? O22 C24 1.457(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 O2 B1 O1 112.5(2) . . ? O2 B1 B2 124.9(2) . . ? O1 B1 B2 122.6(2) . . ? B1 O1 C1 107.8(2) . . ? B1 O2 C2 107.7(2) . . ? O1 C1 C5 109.7(2) . . ? O1 C1 C2 103.1(2) . . ? C5 C1 C2 109.1(2) . . ? O2 C2 C3 109.8(2) . . ? O2 C2 C1 103.6(2) . . ? C3 C2 C1 111.5(2) . . ? O3 C3 O4 125.1(2) . . ? O3 C3 C2 123.9(2) . . ? O4 C3 C2 110.9(2) . . ? C3 O4 C4 115.8(2) . . ? O5 C5 O6 126.3(2) . . ? O5 C5 C1 124.3(2) . . ? O6 C5 C1 109.3(2) . . ? C5 O6 C6 115.3(2) . . ? O7 B2 O8 113.9(2) . . ? O7 B2 B1 124.8(2) . . ? O8 B2 B1 121.3(2) . . ? B2 O7 C7 108.0(2) . . ? B2 O8 C8 107.8(2) . . ? O7 C7 C11 110.0(2) . . ? O7 C7 C8 104.8(2) . . ? C11 C7 C8 113.2(2) . . ? O8 C8 C9 111.7(2) . . ? O8 C8 C7 105.4(2) . . ? C9 C8 C7 114.0(2) . . ? O9 C9 O10 126.2(2) . . ? O9 C9 C8 123.3(2) . . ? O10 C9 C8 110.3(2) . . ? C9 O10 C10 116.3(2) . . ? O11 C11 O12 123.9(2) . . ? O11 C11 C7 126.1(2) . . ? O12 C11 C7 110.1(2) . . ? C11 O12 C12 115.0(2) . . ? O14 B3 O13 112.9(2) . . ? O14 B3 B4 123.0(2) . . ? O13 B3 B4 124.1(2) . . ? B3 O13 C13 108.1(2) . . ? B3 O14 C14 108.6(2) . . ? O13 C13 C17 106.1(2) . . ? O13 C13 C14 104.0(2) . . ? C17 C13 C14 114.5(2) . . ? O14 C14 C15 111.9(2) . . ? O14 C14 C13 104.6(2) . . ? C15 C14 C13 112.7(2) . . ? O15 C15 O16 126.2(2) . . ? O15 C15 C14 121.4(2) . . ? O16 C15 C14 112.4(2) . . ? C15 O16 C16 116.8(2) . . ? O17 C17 O18 125.1(2) . . ? O17 C17 C13 125.8(2) . . ? O18 C17 C13 109.0(2) . . ? C17 O18 C18 115.7(2) . . ? O20 B4 O19 112.8(2) . . ? O20 B4 B3 124.8(2) . . ? O19 B4 B3 122.3(2) . . ? B4 O19 C19 108.8(2) . . ? B4 O20 C20 109.3(2) . . ? O19 C19 C23 108.7(2) . . ? O19 C19 C20 104.5(2) . . ? C23 C19 C20 113.2(2) . . ? O20 C20 C21 109.3(2) . . ? O20 C20 C19 104.3(2) . . ? C21 C20 C19 110.4(2) . . ? O23 C21 O24 124.6(3) . . ? O23 C21 C20 125.1(2) . . ? O24 C21 C20 110.2(2) . . ? C21 O24 C22 116.0(2) . . ? O21 C23 O22 125.1(2) . . ? O21 C23 C19 124.8(2) . . ? O22 C23 C19 110.1(2) . . ? C23 O22 C24 115.4(2) . . ? 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 O1 C1 C2 O2 -22.6(2) . . . . ? O7 C7 C8 O8 -0.7(2) . . . . ? O19 C19 C20 O20 -4.2(2) . . . . ? O14 C14 C14 O13 0.00(12) . . . . ? O1 B1 B2 O8 28.0(3) . . . . ? O2 B1 B2 O7 31.6(4) . . . . ? O19 B4 B3 O13 -27.9(4) . . . . ? O20 B4 B3 O14 -23.9(4) . . . . ? O2 B1 B2 O8 -150.6(2) . . . . ? O1 B1 B2 O7 -149.7(2) . . . . ? O20 B4 B3 O13 156.7(2) . . . . ? O19 B4 B3 O14 151.6(2) . . . . ? _refine_diff_density_max 0.400 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.073 #=end data_2 _publ_section_exptl_refinement ; Unit cell dimensions were determined from 174 reflections taken from three sets of 30 frames (at 0.3\% steps in \w) each at 10 seconds exposure. A full hemisphere of reiciprocal space was scanned by 0.3\% \w steps at \f 0, 90 and 180\% with the area detector held at 2\q = -29\%. Each exposure at 40 s. The crystal-to-detector distance was 4.974 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times the U~iso~ value of their attached carbons. ; _audit_creation_method SHELXL _chemical_name_systematic ; bis(phenylethane 1,2-diol)diboron ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H16 B2 O4' _chemical_formula_weight 293.91 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 2~1~ 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 9.6718(12) _cell_length_b 11.8885(12) _cell_length_c 26.482(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3045.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 174 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method ? _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19284 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6936 _reflns_number_observed 4935 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] where P=(Max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'see text' _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 -0.79(71) _refine_ls_number_reflns 6936 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_obs 0.0382 _refine_ls_wR_factor_all 0.0824 _refine_ls_wR_factor_obs 0.0736 _refine_ls_goodness_of_fit_all 0.915 _refine_ls_goodness_of_fit_obs 0.981 _refine_ls_restrained_S_all 0.915 _refine_ls_restrained_S_obs 0.981 _refine_ls_shift/esd_max -0.107 _refine_ls_shift/esd_mean 0.011 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group B1 B 0.6223(2) 0.7306(2) 0.06606(7) 0.0259(4) Uani 1 d . . B2 B 0.5275(2) 0.8198(2) 0.10202(7) 0.0272(5) Uani 1 d . . B3 B 0.4697(2) 0.8039(2) 0.39946(7) 0.0289(5) Uani 1 d . . B4 B 0.3833(2) 0.7160(2) 0.43869(7) 0.0280(4) Uani 1 d . . O11 O 0.75225(11) 0.75356(9) 0.04828(5) 0.0330(3) Uani 1 d . . O12 O 0.57395(12) 0.62857(10) 0.05122(4) 0.0321(3) Uani 1 d . . O21 O 0.57168(12) 0.92132(9) 0.11956(4) 0.0319(3) Uani 1 d . . O22 O 0.39559(12) 0.79392(11) 0.11663(4) 0.0353(3) Uani 1 d . . O31 O 0.41974(13) 0.90508(10) 0.38389(5) 0.0388(3) Uani 1 d . . O32 O 0.59835(12) 0.78031(11) 0.38031(4) 0.0350(3) Uani 1 d . . O41 O 0.44215(11) 0.62351(10) 0.46045(4) 0.0324(3) Uani 1 d . . O42 O 0.24811(11) 0.73161(10) 0.45263(4) 0.0324(3) Uani 1 d . . C11 C 0.7935(2) 0.66187(14) 0.01594(7) 0.0289(4) Uani 1 d . . H11A H 0.8852(2) 0.63259(14) 0.02604(7) 0.035 Uiso 1 calc R . H11B H 0.7981(2) 0.68673(14) -0.01970(7) 0.035 Uiso 1 calc R . C12 C 0.6814(2) 0.57111(14) 0.02276(6) 0.0256(4) Uani 1 d . . H12A H 0.7196(2) 0.50822(14) 0.04361(6) 0.031 Uiso 1 calc R . C13 C 0.6242(2) 0.52424(13) -0.02554(6) 0.0227(4) Uani 1 d . . C14 C 0.6786(2) 0.42589(14) -0.04590(7) 0.0293(4) Uani 1 d . . H14A H 0.7532(2) 0.38907(14) -0.02941(7) 0.035 Uiso 1 calc R . C15 C 0.6247(2) 0.3811(2) -0.09014(7) 0.0349(4) Uani 1 d . . H15A H 0.6617(2) 0.3134(2) -0.10358(7) 0.042 Uiso 1 calc R . C16 C 0.5174(2) 0.4348(2) -0.11465(7) 0.0366(4) Uani 1 d . . H16A H 0.4807(2) 0.4043(2) -0.14497(7) 0.044 Uiso 1 calc R . C17 C 0.4632(2) 0.5334(2) -0.09491(7) 0.0364(4) Uani 1 d . . H17A H 0.3893(2) 0.5705(2) -0.11171(7) 0.044 Uiso 1 calc R . C18 C 0.5165(2) 0.57770(15) -0.05091(6) 0.0303(4) Uani 1 d . . H18A H 0.4792(2) 0.64555(15) -0.03771(6) 0.036 Uiso 1 calc R . C21 C 0.4612(2) 0.97159(15) 0.14860(7) 0.0341(4) Uani 1 d . . H21A H 0.4317(2) 1.04361(15) 0.13324(7) 0.041 Uiso 1 calc R . H21B H 0.4915(2) 0.98601(15) 0.18372(7) 0.041 Uiso 1 calc R . C22 C 0.3416(2) 0.88486(15) 0.14757(6) 0.0306(4) Uani 1 d . . H22A H 0.2594(2) 0.91892(15) 0.13049(6) 0.037 Uiso 1 calc R . C23 C 0.2994(2) 0.84054(15) 0.19833(6) 0.0281(4) Uani 1 d . . C24 C 0.1703(2) 0.8649(2) 0.21840(7) 0.0428(5) Uani 1 d . . H24A H 0.1073(2) 0.9091(2) 0.19937(7) 0.051 Uiso 1 calc R . C25 C 0.1317(2) 0.8261(2) 0.26548(8) 0.0534(6) Uani 1 d . . H25A H 0.0432(2) 0.8443(2) 0.27869(8) 0.064 Uiso 1 calc R . C26 C 0.2218(2) 0.7609(2) 0.29336(7) 0.0443(5) Uani 1 d . . H26A H 0.1957(2) 0.7340(2) 0.32576(7) 0.053 Uiso 1 calc R . C27 C 0.3502(2) 0.7352(2) 0.27375(7) 0.0404(5) Uani 1 d . . H27A H 0.4125(2) 0.6900(2) 0.29268(7) 0.048 Uiso 1 calc R . C28 C 0.3885(2) 0.7746(2) 0.22688(7) 0.0360(4) Uani 1 d . . H28A H 0.4773(2) 0.7565(2) 0.21389(7) 0.043 Uiso 1 calc R . C31 C 0.5191(2) 0.9551(2) 0.34983(7) 0.0399(5) Uani 1 d . . H31A H 0.5440(2) 1.0319(2) 0.36106(7) 0.048 Uiso 1 calc R . H31B H 0.4812(2) 0.9593(2) 0.31514(7) 0.048 Uiso 1 calc R . C32 C 0.6463(2) 0.8765(2) 0.35169(7) 0.0327(4) Uani 1 d . . H32A H 0.7219(2) 0.9146(2) 0.37098(7) 0.039 Uiso 1 calc R . C33 C 0.7009(2) 0.8424(2) 0.30065(6) 0.0290(4) Uani 1 d . . C34 C 0.7221(2) 0.7311(2) 0.28746(7) 0.0343(4) Uani 1 d . . H34A H 0.7038(2) 0.6732(2) 0.31126(7) 0.041 Uiso 1 calc R . C35 C 0.7704(2) 0.7035(2) 0.23948(7) 0.0410(5) Uani 1 d . . H35A H 0.7850(2) 0.6269(2) 0.23082(7) 0.049 Uiso 1 calc R . C36 C 0.7971(2) 0.7862(2) 0.20457(7) 0.0435(5) Uani 1 d . . H36A H 0.8286(2) 0.7669(2) 0.17171(7) 0.052 Uiso 1 calc R . C37 C 0.7776(2) 0.8979(2) 0.21769(7) 0.0417(5) Uani 1 d . . H37A H 0.7961(2) 0.9555(2) 0.19378(7) 0.050 Uiso 1 calc R . C38 C 0.7312(2) 0.9257(2) 0.26560(7) 0.0341(4) Uani 1 d . . H38A H 0.7201(2) 1.0026(2) 0.27455(7) 0.041 Uiso 1 calc R . C41 C 0.3349(2) 0.56241(14) 0.48778(6) 0.0274(4) Uani 1 d . . H41A H 0.3035(2) 0.49691(14) 0.46705(6) 0.033 Uiso 1 calc R . C42 C 0.2170(2) 0.64966(14) 0.49126(7) 0.0287(4) Uani 1 d . . H42A H 0.1263(2) 0.61376(14) 0.48489(7) 0.034 Uiso 1 calc R . H42B H 0.2152(2) 0.68533(14) 0.52503(7) 0.034 Uiso 1 calc R . C43 C 0.3861(2) 0.52107(14) 0.53802(6) 0.0247(4) Uani 1 d . . C45 C 0.5364(2) 0.5372(2) 0.61004(7) 0.0388(5) Uani 1 d . . H45A H 0.6094(2) 0.5749(2) 0.62714(7) 0.047 Uiso 1 calc R . C46 C 0.4753(2) 0.4433(2) 0.63169(7) 0.0419(5) Uani 1 d . . H46A H 0.5059(2) 0.4168(2) 0.66364(7) 0.050 Uiso 1 calc R . C46 C 0.4918(2) 0.57612(15) 0.56384(7) 0.0305(4) Uani 1 d . . H46B H 0.5333(2) 0.64105(15) 0.54947(7) 0.037 Uiso 1 calc R . C47 C 0.3698(2) 0.3884(2) 0.60658(8) 0.0410(5) Uani 1 d . . H47A H 0.3276(2) 0.3242(2) 0.62131(8) 0.049 Uiso 1 calc R . C48 C 0.3255(2) 0.42703(15) 0.55987(7) 0.0334(4) Uani 1 d . . H48A H 0.2531(2) 0.38886(15) 0.54271(7) 0.040 Uiso 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 B1 0.0229(10) 0.0318(11) 0.0230(10) 0.0040(9) -0.0005(8) -0.0015(8) B2 0.0249(11) 0.0336(12) 0.0230(10) 0.0048(8) -0.0023(8) -0.0010(9) B3 0.0298(11) 0.0376(12) 0.0192(10) -0.0062(9) -0.0009(9) 0.0000(9) B4 0.0266(11) 0.0345(12) 0.0230(10) -0.0048(9) 0.0001(9) -0.0001(9) O11 0.0230(6) 0.0325(7) 0.0435(7) -0.0076(6) 0.0075(5) -0.0064(5) O12 0.0258(6) 0.0346(7) 0.0358(7) -0.0067(6) 0.0114(5) -0.0059(5) O21 0.0301(7) 0.0303(6) 0.0354(7) -0.0033(6) 0.0093(6) -0.0034(5) O22 0.0259(7) 0.0470(8) 0.0330(7) -0.0137(6) 0.0077(6) -0.0077(6) O31 0.0411(8) 0.0358(7) 0.0396(8) 0.0002(6) 0.0160(6) 0.0069(6) O32 0.0285(7) 0.0464(8) 0.0300(7) 0.0094(6) 0.0060(6) 0.0042(6) O41 0.0239(6) 0.0381(7) 0.0352(7) 0.0038(6) 0.0110(5) 0.0055(5) O42 0.0244(7) 0.0381(7) 0.0346(7) 0.0049(6) 0.0043(5) 0.0040(5) C11 0.0228(9) 0.0291(9) 0.0347(10) -0.0024(8) 0.0054(8) -0.0004(7) C12 0.0204(8) 0.0273(9) 0.0291(9) 0.0020(8) 0.0029(7) 0.0009(7) C13 0.0183(8) 0.0233(9) 0.0263(9) 0.0049(7) 0.0040(7) -0.0014(7) C14 0.0253(9) 0.0280(9) 0.0346(10) 0.0031(8) 0.0011(8) 0.0051(8) C15 0.0379(11) 0.0291(10) 0.0376(11) -0.0049(9) 0.0075(9) -0.0019(8) C16 0.0352(11) 0.0455(11) 0.0290(10) -0.0020(9) -0.0007(8) -0.0104(9) C17 0.0267(10) 0.0480(12) 0.0346(10) 0.0061(9) -0.0053(8) 0.0039(9) C18 0.0246(9) 0.0318(10) 0.0343(10) 0.0017(8) 0.0032(8) 0.0068(8) C21 0.0368(10) 0.0324(10) 0.0332(10) -0.0026(8) 0.0086(9) 0.0004(8) C22 0.0244(9) 0.0400(11) 0.0273(9) -0.0037(8) 0.0011(7) 0.0055(8) C23 0.0245(9) 0.0325(10) 0.0273(10) -0.0039(8) 0.0010(8) -0.0022(8) C24 0.0249(10) 0.0678(14) 0.0356(11) 0.0039(11) 0.0022(8) 0.0088(10) C25 0.0272(11) 0.094(2) 0.0388(12) 0.0078(12) 0.0075(10) 0.0004(11) C26 0.0430(12) 0.0617(14) 0.0283(10) 0.0079(10) 0.0011(9) -0.0178(10) C27 0.0431(12) 0.0393(12) 0.0388(11) 0.0085(10) -0.0054(9) -0.0006(9) C28 0.0305(10) 0.0420(11) 0.0354(10) 0.0013(9) 0.0010(8) 0.0056(9) C31 0.0476(12) 0.0357(11) 0.0362(10) 0.0019(9) 0.0165(10) 0.0019(9) C32 0.0310(10) 0.0392(11) 0.0279(10) 0.0024(8) 0.0017(8) -0.0053(8) C33 0.0196(9) 0.0423(11) 0.0253(9) 0.0041(8) 0.0006(7) -0.0016(8) C34 0.0295(10) 0.0417(11) 0.0316(10) 0.0060(9) 0.0025(8) 0.0005(8) C35 0.0371(12) 0.0448(12) 0.0412(12) -0.0006(10) 0.0043(10) 0.0083(9) C36 0.0357(11) 0.0637(14) 0.0311(11) 0.0018(11) 0.0085(9) 0.0105(10) C37 0.0349(11) 0.0572(14) 0.0329(11) 0.0134(10) 0.0067(9) 0.0041(10) C38 0.0281(10) 0.0386(10) 0.0357(10) 0.0067(9) 0.0033(8) 0.0017(8) C41 0.0226(9) 0.0279(10) 0.0318(9) -0.0050(8) 0.0047(7) -0.0018(7) C42 0.0215(9) 0.0319(10) 0.0325(10) 0.0003(8) 0.0036(8) -0.0004(7) C43 0.0195(8) 0.0241(9) 0.0304(9) -0.0061(8) 0.0036(7) 0.0024(7) C45 0.0266(10) 0.0483(12) 0.0414(12) -0.0063(10) -0.0051(9) -0.0024(9) C46 0.0376(11) 0.0497(13) 0.0383(11) 0.0073(10) -0.0047(9) 0.0108(10) C46 0.0236(9) 0.0296(10) 0.0382(10) -0.0039(8) 0.0032(8) -0.0032(8) C47 0.0395(12) 0.0321(11) 0.0513(13) 0.0105(9) 0.0043(10) -0.0018(9) C48 0.0256(9) 0.0281(10) 0.0466(12) -0.0019(9) 0.0004(8) -0.0033(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 B1 O12 1.358(2) . ? B1 O11 1.370(2) . ? B1 B2 1.695(3) . ? B2 O21 1.362(2) . ? B2 O22 1.368(2) . ? B3 O31 1.360(2) . ? B3 O32 1.373(2) . ? B3 B4 1.694(3) . ? B4 O41 1.366(2) . ? B4 O42 1.371(2) . ? O11 C11 1.443(2) . ? O12 C12 1.454(2) . ? O21 C21 1.446(2) . ? O22 C22 1.454(2) . ? O31 C31 1.446(2) . ? O32 C32 1.448(2) . ? O41 C41 1.458(2) . ? O42 C42 1.444(2) . ? C11 C12 1.540(2) . ? C12 C13 1.501(2) . ? C13 C14 1.391(2) . ? C13 C18 1.393(2) . ? C14 C15 1.389(2) . ? C15 C16 1.381(2) . ? C16 C17 1.386(2) . ? C17 C18 1.379(2) . ? C21 C22 1.550(2) . ? C22 C23 1.500(2) . ? C23 C24 1.388(2) . ? C23 C28 1.388(2) . ? C24 C25 1.381(3) . ? C25 C26 1.380(3) . ? C26 C27 1.380(3) . ? C27 C28 1.378(2) . ? C31 C32 1.546(2) . ? C32 C33 1.507(2) . ? C33 C34 1.384(2) . ? C33 C38 1.389(2) . ? C34 C35 1.393(2) . ? C35 C36 1.374(3) . ? C36 C37 1.385(3) . ? C37 C38 1.386(3) . ? C41 C43 1.503(2) . ? C41 C42 1.544(2) . ? C43 C48 1.389(2) . ? C43 C46 1.393(2) . ? C45 C46 1.377(2) . ? C45 C46 1.388(3) . ? C46 C47 1.382(3) . ? C47 C48 1.387(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 O12 B1 O11 113.3(2) . . ? O12 B1 B2 122.4(2) . . ? O11 B1 B2 124.4(2) . . ? O21 B2 O22 113.3(2) . . ? O21 B2 B1 125.2(2) . . ? O22 B2 B1 121.5(2) . . ? O31 B3 O32 113.0(2) . . ? O31 B3 B4 123.8(2) . . ? O32 B3 B4 123.2(2) . . ? O41 B4 O42 113.1(2) . . ? O41 B4 B3 123.4(2) . . ? O42 B4 B3 123.5(2) . . ? B1 O11 C11 107.87(13) . . ? B1 O12 C12 108.86(13) . . ? B2 O21 C21 108.42(14) . . ? B2 O22 C22 109.09(14) . . ? B3 O31 C31 108.50(14) . . ? B3 O32 C32 108.80(14) . . ? B4 O41 C41 108.29(13) . . ? B4 O42 C42 107.32(13) . . ? O11 C11 C12 105.37(12) . . ? O12 C12 C13 110.66(12) . . ? O12 C12 C11 103.58(12) . . ? C13 C12 C11 114.80(14) . . ? C14 C13 C18 118.7(2) . . ? C14 C13 C12 120.20(15) . . ? C18 C13 C12 121.1(2) . . ? C15 C14 C13 120.5(2) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C17 119.9(2) . . ? C18 C17 C16 120.0(2) . . ? C17 C18 C13 120.9(2) . . ? O21 C21 C22 105.51(13) . . ? O22 C22 C23 109.97(14) . . ? O22 C22 C21 103.66(13) . . ? C23 C22 C21 114.88(15) . . ? C24 C23 C28 117.9(2) . . ? C24 C23 C22 120.9(2) . . ? C28 C23 C22 121.2(2) . . ? C25 C24 C23 121.3(2) . . ? C26 C25 C24 120.0(2) . . ? C25 C26 C27 119.4(2) . . ? C28 C27 C26 120.4(2) . . ? C27 C28 C23 121.0(2) . . ? O31 C31 C32 105.08(14) . . ? O32 C32 C33 111.66(15) . . ? O32 C32 C31 103.83(13) . . ? C33 C32 C31 114.4(2) . . ? C34 C33 C38 118.8(2) . . ? C34 C33 C32 122.4(2) . . ? C38 C33 C32 118.8(2) . . ? C33 C34 C35 120.3(2) . . ? C36 C35 C34 120.5(2) . . ? C35 C36 C37 119.5(2) . . ? C36 C37 C38 120.2(2) . . ? C37 C38 C33 120.7(2) . . ? O41 C41 C43 111.59(13) . . ? O41 C41 C42 102.72(12) . . ? C43 C41 C42 114.22(13) . . ? O42 C42 C41 104.89(12) . . ? C48 C43 C46 118.9(2) . . ? C48 C43 C41 119.53(15) . . ? C46 C43 C41 121.5(2) . . ? C46 C45 C46 120.2(2) . . ? C47 C46 C45 119.7(2) . . ? C45 C46 C43 120.6(2) . . ? C46 C47 C48 120.1(2) . . ? C47 C48 C43 120.5(2) . . ? 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 O22 B2 B1 O12 -1.8(3) . . . . ? O22 B2 B1 O11 176.9(2) . . . . ? O21 B2 B1 O11 -3.7(3) . . . . ? O21 B2 B1 O12 177.6(2) . . . . ? O41 B4 B3 O31 -169.3(2) . . . . ? O41 B4 B3 O32 10.3(3) . . . . ? O42 B4 B3 O32 -171.1(2) . . . . ? O42 B4 B3 O31 9.3(3) . . . . ? O41 C41 C42 O42 18.9(2) . . . . ? O31 C31 C32 O32 8.8(2) . . . . ? O21 C21 C22 O22 -1.3(2) . . . . ? O12 C12 C11 O11 10.2(2) . . . . ? _refine_diff_density_max 0.177 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.044 #=END data_3 _publ_section_exptl_refinement ; Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times the U~iso~ value of their attached carbon. ; _audit_creation_method SHELXL _chemical_name_systematic ; bis(1,2-diphenylethane-1,2-diol)diboron ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '(B O2 C2 H2 Ph2) 2' _chemical_formula_analytical ? _chemical_formula_sum 'C28 H24 B2 O4' _chemical_formula_weight 446.09 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4~1~ 2~1~ 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.731(2) _cell_length_b 12.731(2) _cell_length_c 14.653(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2374.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 174 _cell_measurement_theta_min 9 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method ? _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3020 _diffrn_reflns_av_R_equivalents 0.1253 _diffrn_reflns_av_sigmaI/netI 0.1033 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2083 _reflns_number_observed 1769 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1995c)' _computing_cell_refinement 'XSCANS (Siemens, 1995c)' _computing_data_reduction 'XSCANS (Siemens, 1995c)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.2845P] where P=(Max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'see text' _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 0.39(163) _refine_ls_number_reflns 2082 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_obs 0.0384 _refine_ls_wR_factor_all 0.0974 _refine_ls_wR_factor_obs 0.0888 _refine_ls_goodness_of_fit_all 1.092 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.095 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max -0.049 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group B1 B 0.0297(2) 0.0297(2) 0.0000 0.0550(8) Uani 1 d S . B2 B 0.1241(2) 0.1241(2) 0.0000 0.0575(8) Uani 1 d S . O1 O 0.05116(10) -0.07484(11) 0.00192(10) 0.0618(4) Uani 1 d . . O2 O 0.11099(11) 0.22000(11) 0.03940(9) 0.0599(4) Uani 1 d . . C11 C -0.04604(15) -0.13290(15) -0.00198(13) 0.0516(4) Uani 1 d . . H11A H -0.05173(15) -0.17795(15) 0.05202(13) 0.062 Uiso 1 calc R . C12 C -0.05156(14) -0.19954(14) -0.08645(12) 0.0483(4) Uani 1 d . . C13 C 0.0040(2) -0.1755(2) -0.16444(14) 0.0626(5) Uani 1 d . . H13A H 0.0497(2) -0.1185(2) -0.16434(14) 0.075 Uiso 1 calc R . C14 C -0.0072(2) -0.2344(2) -0.24214(15) 0.0693(6) Uani 1 d . . H14A H 0.0312(2) -0.2171(2) -0.29401(15) 0.083 Uiso 1 calc R . C15 C -0.0741(2) -0.3181(2) -0.24420(15) 0.0648(6) Uani 1 d . . H15A H -0.0817(2) -0.3576(2) -0.29719(15) 0.078 Uiso 1 calc R . C16 C -0.1297(2) -0.3432(2) -0.1677(2) 0.0701(6) Uani 1 d . . H16A H -0.1757(2) -0.4000(2) -0.1686(2) 0.084 Uiso 1 calc R . C17 C -0.1182(2) -0.2848(2) -0.08876(14) 0.0640(6) Uani 1 d . . H17A H -0.1558(2) -0.3033(2) -0.03675(14) 0.077 Uiso 1 calc R . C21 C 0.21121(15) 0.27397(15) 0.03609(13) 0.0516(4) Uani 1 d . . H21A H 0.24607(15) 0.26704(15) 0.09541(13) 0.062 Uiso 1 calc R . C22 C 0.19906(15) 0.3884(2) 0.01391(13) 0.0521(4) Uani 1 d . . C23 C 0.1208(2) 0.4240(2) -0.0424(2) 0.0724(6) Uani 1 d . . H23A H 0.0710(2) 0.3772(2) -0.0649(2) 0.087 Uiso 1 calc R . C24 C 0.1151(2) 0.5294(2) -0.0661(2) 0.0912(8) Uani 1 d . . H24A H 0.0617(2) 0.5526(2) -0.1044(2) 0.109 Uiso 1 calc R . C25 C 0.1869(3) 0.5988(2) -0.0340(2) 0.0884(8) Uani 1 d . . H25A H 0.1824(3) 0.6695(2) -0.0496(2) 0.106 Uiso 1 calc R . C26 C 0.2659(2) 0.5640(2) 0.0213(2) 0.0874(8) Uani 1 d . . H26A H 0.3161(2) 0.6111(2) 0.0423(2) 0.105 Uiso 1 calc R . C27 C 0.2720(2) 0.4597(2) 0.0464(2) 0.0686(6) Uani 1 d . . H27A H 0.3253(2) 0.4373(2) 0.0852(2) 0.082 Uiso 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 B1 0.0568(12) 0.0568(12) 0.051(2) -0.0015(11) 0.0015(11) -0.0041(15) B2 0.0585(11) 0.0585(11) 0.055(2) -0.0064(11) 0.0064(11) -0.006(2) O1 0.0489(8) 0.0578(9) 0.0786(9) -0.0076(7) -0.0074(7) -0.0040(6) O2 0.0546(8) 0.0575(8) 0.0676(8) -0.0086(7) 0.0158(6) -0.0080(7) C11 0.0524(11) 0.0490(11) 0.0534(10) 0.0003(9) 0.0020(9) -0.0064(8) C12 0.0479(10) 0.0448(10) 0.0521(10) 0.0024(8) 0.0046(8) 0.0002(8) C13 0.0698(14) 0.0538(12) 0.0642(12) -0.0013(10) 0.0173(10) -0.0088(10) C14 0.087(2) 0.0614(13) 0.0592(12) 0.0003(11) 0.0226(12) 0.0051(12) C15 0.088(2) 0.0509(12) 0.0557(11) -0.0055(9) -0.0019(11) 0.0123(11) C16 0.087(2) 0.0514(12) 0.0718(13) -0.0035(10) 0.0013(13) -0.0147(11) C17 0.0773(14) 0.0572(12) 0.0576(11) 0.0007(10) 0.0132(11) -0.0163(11) C21 0.0470(10) 0.0531(11) 0.0548(10) -0.0070(9) 0.0053(8) -0.0029(9) C22 0.0475(10) 0.0519(10) 0.0568(10) -0.0110(9) 0.0098(9) -0.0023(8) C23 0.0587(13) 0.0619(13) 0.097(2) -0.0086(12) -0.0094(12) 0.0038(11) C24 0.094(2) 0.074(2) 0.105(2) 0.0078(15) -0.006(2) 0.024(2) C25 0.107(2) 0.0562(14) 0.102(2) 0.0005(14) 0.031(2) 0.0024(15) C26 0.092(2) 0.064(2) 0.106(2) -0.0247(14) 0.023(2) -0.0242(14) C27 0.0651(14) 0.0634(14) 0.0773(13) -0.0168(11) 0.0002(11) -0.0063(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 B1 O1 1.359(2) 7 ? B1 O1 1.359(2) . ? B1 B2 1.700(5) . ? B2 O2 1.361(2) . ? B2 O2 1.361(2) 7 ? O1 C11 1.443(2) . ? O2 C21 1.450(2) . ? C11 C12 1.502(3) . ? C11 C11 1.565(4) 7 ? C12 C13 1.378(3) . ? C12 C17 1.379(3) . ? C13 C14 1.371(3) . ? C14 C15 1.364(3) . ? C15 C16 1.364(3) . ? C16 C17 1.382(3) . ? C21 C22 1.501(3) . ? C21 C21 1.547(4) 7 ? C22 C23 1.371(3) . ? C22 C27 1.382(3) . ? C23 C24 1.388(3) . ? C24 C25 1.355(4) . ? C25 C26 1.366(4) . ? C26 C27 1.380(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 O1 B1 O1 113.3(3) 7 . ? O1 B1 B2 123.37(13) 7 . ? O1 B1 B2 123.37(13) . . ? O2 B2 O2 113.6(3) . 7 ? O2 B2 B1 123.21(13) . . ? O2 B2 B1 123.21(13) 7 . ? B1 O1 C11 109.2(2) . . ? B2 O2 C21 107.6(2) . . ? O1 C11 C12 111.23(15) . . ? O1 C11 C11 104.04(9) . 7 ? C12 C11 C11 113.4(2) . 7 ? C13 C12 C17 118.1(2) . . ? C13 C12 C11 122.3(2) . . ? C17 C12 C11 119.6(2) . . ? C14 C13 C12 120.9(2) . . ? C15 C14 C13 120.7(2) . . ? C14 C15 C16 119.3(2) . . ? C15 C16 C17 120.4(2) . . ? C12 C17 C16 120.6(2) . . ? O2 C21 C22 112.1(2) . . ? O2 C21 C21 103.45(9) . 7 ? C22 C21 C21 114.0(2) . 7 ? C23 C22 C27 118.6(2) . . ? C23 C22 C21 121.7(2) . . ? C27 C22 C21 119.5(2) . . ? C22 C23 C24 120.5(2) . . ? C25 C24 C23 120.6(3) . . ? C24 C25 C26 119.4(3) . . ? C25 C26 C27 120.8(2) . . ? C26 C27 C22 120.1(2) . . ? 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 O2 C21 C21 O2 -20.3(3) . . 7 7 ? O1 C11 C11 O1 5.7(3) . . 7 7 ? O1 B1 B2 O2 31.89(10) . . . 7 ? O1 B1 B2 O2 31.89(10) 7 . . . ? O1 B1 B2 O2 -148.11(10) . . . . ? O1 B1 B2 O2 -148.11(10) 7 . . 7 ? _refine_diff_density_max 0.107 _refine_diff_density_min -0.114 _refine_diff_density_rms 0.026 #=END data_4 _publ_section_exptl_refinement ; Unit cell dimensions were determined from 216 reflections taken from three sets of 30 frames (at 0.3\% steps in \w) each at 20 seconds exposure. A full hemisphere of reiciprocal space was scanned by 0.3\% \w steps at \f 0, 90 and 180\% with the area detector held at 2\q = -29\%. The crystal-to-detector distance was 4.974 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times the U~iso~ value of their attached carbon and 1.5 U~iso~ for methyl carbons. Bond lengths in the toluene solvent molecule were restranied to an idealized geometry. ; _audit_creation_method SHELXL _chemical_name_systematic ; bis(1,1'-bi-2-napthol)diboron ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '(B O C10 H6) 2' _chemical_formula_analytical ? _chemical_formula_sum 'C47 H32 B2 O4' _chemical_formula_weight 682.35 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2~1~ /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 14.063(2) _cell_length_b 10.8214(11) _cell_length_c 24.853(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.194(10) _cell_angle_gamma 90.00 _cell_volume 3649.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 216 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method ? _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18479 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6411 _reflns_number_observed 4221 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+1.4894P] where P=(Max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'see text' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6404 _refine_ls_number_parameters 481 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_obs 0.0546 _refine_ls_wR_factor_all 0.1543 _refine_ls_wR_factor_obs 0.1344 _refine_ls_goodness_of_fit_all 1.038 _refine_ls_goodness_of_fit_obs 1.136 _refine_ls_restrained_S_all 1.163 _refine_ls_restrained_S_obs 1.312 _refine_ls_shift/esd_max 0.047 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.49605(13) 0.4760(2) 0.18397(8) 0.0316(5) Uani 1 d . . O2 O 0.53129(13) 0.2299(2) 0.09839(8) 0.0316(5) Uani 1 d . . O3 O 0.61217(13) 0.3938(2) 0.07117(8) 0.0320(5) Uani 1 d . . O4 O 0.66188(13) 0.4350(2) 0.21392(7) 0.0294(5) Uani 1 d . . B1 B 0.5728(2) 0.3449(3) 0.11146(14) 0.0289(7) Uani 1 d . . B2 B 0.5766(2) 0.4206(3) 0.17264(14) 0.0283(7) Uani 1 d . . C10 C 0.3671(2) 0.3511(2) 0.12615(11) 0.0263(6) Uani 1 d . . C11 C 0.4072(2) 0.4653(3) 0.14312(12) 0.0293(6) Uani 1 d . . C12 C 0.3609(2) 0.5762(3) 0.12074(13) 0.0350(7) Uani 1 d . . H12 H 0.3897(2) 0.6535(3) 0.13415(13) 0.042 Uiso 1 calc R . C13 C 0.2753(2) 0.5725(3) 0.08008(12) 0.0353(7) Uani 1 d . . H13 H 0.2439(2) 0.6476(3) 0.06552(12) 0.042 Uiso 1 calc R . C14 C 0.2320(2) 0.4584(3) 0.05894(11) 0.0287(6) Uani 1 d . . C15 C 0.2781(2) 0.3464(2) 0.08219(11) 0.0263(6) Uani 1 d . . C16 C 0.2347(2) 0.2332(3) 0.05955(12) 0.0306(7) Uani 1 d . . H16 H 0.2633(2) 0.1573(3) 0.07504(12) 0.037 Uiso 1 calc R . C17 C 0.1520(2) 0.2315(3) 0.01569(12) 0.0346(7) Uani 1 d . . H17 H 0.1247(2) 0.1546(3) 0.00068(12) 0.042 Uiso 1 calc R . C18 C 0.1070(2) 0.3425(3) -0.00736(12) 0.0368(7) Uani 1 d . . H18 H 0.0499(2) 0.3406(3) -0.03794(12) 0.044 Uiso 1 calc R . C19 C 0.1457(2) 0.4529(3) 0.01436(12) 0.0362(7) Uani 1 d . . H19 H 0.1141(2) 0.5275(3) -0.00074(12) 0.043 Uiso 1 calc R . C20 C 0.4131(2) 0.2335(2) 0.15308(11) 0.0257(6) Uani 1 d . . C21 C 0.4890(2) 0.1764(2) 0.13758(11) 0.0269(6) Uani 1 d . . C22 C 0.5288(2) 0.0626(3) 0.16029(12) 0.0311(7) Uani 1 d . . H22 H 0.5808(2) 0.0253(3) 0.14821(12) 0.037 Uiso 1 calc R . C23 C 0.4923(2) 0.0063(3) 0.19969(12) 0.0325(7) Uani 1 d . . H23 H 0.5182(2) -0.0714(3) 0.21437(12) 0.039 Uiso 1 calc R . C24 C 0.4163(2) 0.0618(3) 0.21907(11) 0.0284(6) Uani 1 d . . C25 C 0.3762(2) 0.1767(2) 0.19574(11) 0.0259(6) Uani 1 d . . C26 C 0.3026(2) 0.2330(3) 0.21718(12) 0.0328(7) Uani 1 d . . H26 H 0.2743(2) 0.3092(3) 0.20196(12) 0.039 Uiso 1 calc R . C27 C 0.2718(2) 0.1789(3) 0.25953(13) 0.0394(8) Uani 1 d . . H27 H 0.2229(2) 0.2184(3) 0.27352(13) 0.047 Uiso 1 calc R . C28 C 0.3116(2) 0.0659(3) 0.28247(13) 0.0413(8) Uani 1 d . . H28 H 0.2900(2) 0.0296(3) 0.31203(13) 0.050 Uiso 1 calc R . C29 C 0.3811(2) 0.0080(3) 0.26245(12) 0.0364(7) Uani 1 d . . H29 H 0.4066(2) -0.0695(3) 0.27765(12) 0.044 Uiso 1 calc R . C30 C 0.7423(2) 0.5233(2) 0.12517(11) 0.0253(6) Uani 1 d . . C31 C 0.6593(2) 0.5083(3) 0.08213(11) 0.0287(6) Uani 1 d . . C32 C 0.6161(2) 0.6060(3) 0.04637(12) 0.0350(7) Uani 1 d . . H32 H 0.5587(2) 0.5917(3) 0.01688(12) 0.042 Uiso 1 calc R . C33 C 0.6570(2) 0.7205(3) 0.05431(12) 0.0363(7) Uani 1 d . . H33 H 0.6273(2) 0.7863(3) 0.03048(12) 0.044 Uiso 1 calc R . C34 C 0.7428(2) 0.7429(3) 0.09741(12) 0.0299(7) Uani 1 d . . C35 C 0.7875(2) 0.6435(2) 0.13291(11) 0.0265(6) Uani 1 d . . C36 C 0.8760(2) 0.6678(3) 0.17439(11) 0.0292(6) Uani 1 d . . H36 H 0.9071(2) 0.6028(3) 0.19830(11) 0.035 Uiso 1 calc R . C37 C 0.9174(2) 0.7827(3) 0.18066(13) 0.0376(7) Uani 1 d . . H37 H 0.9774(2) 0.7963(3) 0.20838(13) 0.045 Uiso 1 calc R . C38 C 0.8723(2) 0.8812(3) 0.14648(14) 0.0435(8) Uani 1 d . . H38 H 0.9010(2) 0.9613(3) 0.15157(14) 0.052 Uiso 1 calc R . C39 C 0.7873(2) 0.8615(3) 0.10609(13) 0.0395(8) Uani 1 d . . H39 H 0.7572(2) 0.9285(3) 0.08321(13) 0.047 Uiso 1 calc R . C40 C 0.7867(2) 0.4183(2) 0.16359(11) 0.0261(6) Uani 1 d . . C41 C 0.7464(2) 0.3798(2) 0.20565(11) 0.0272(6) Uani 1 d . . C42 C 0.7869(2) 0.2831(3) 0.24234(12) 0.0340(7) Uani 1 d . . H42 H 0.7579(2) 0.2609(3) 0.27148(12) 0.041 Uiso 1 calc R . C43 C 0.8675(2) 0.2214(3) 0.23600(13) 0.0343(7) Uani 1 d . . H43 H 0.8937(2) 0.1547(3) 0.26020(13) 0.041 Uiso 1 calc R . C44 C 0.9129(2) 0.2558(2) 0.19372(12) 0.0297(7) Uani 1 d . . C45 C 0.8734(2) 0.3558(2) 0.15769(11) 0.0265(6) Uani 1 d . . C46 C 0.9224(2) 0.3911(3) 0.11702(12) 0.0330(7) Uani 1 d . . H46 H 0.8981(2) 0.4590(3) 0.09310(12) 0.040 Uiso 1 calc R . C47 C 1.0042(2) 0.3291(3) 0.11171(13) 0.0391(8) Uani 1 d . . H47 H 1.0358(2) 0.3544(3) 0.08411(13) 0.047 Uiso 1 calc R . C48 C 1.0421(2) 0.2287(3) 0.14634(13) 0.0395(8) Uani 1 d . . H48 H 1.0984(2) 0.1855(3) 0.14180(13) 0.047 Uiso 1 calc R . C49 C 0.9978(2) 0.1932(3) 0.18669(13) 0.0354(7) Uani 1 d . . H49 H 1.0241(2) 0.1257(3) 0.21039(13) 0.043 Uiso 1 calc R . C91 C 0.8038(4) 0.1397(4) 0.0134(3) 0.087(2) Uani 1 d D . H91 H 0.8067(4) 0.1553(4) 0.0514(3) 0.104 Uiso 1 calc R . C92 C 0.8808(5) 0.1334(4) -0.0084(2) 0.085(2) Uani 1 d D . H92 H 0.9418(5) 0.1474(4) 0.0184(2) 0.103 Uiso 1 calc R . C93 C 0.8943(4) 0.1063(5) -0.0724(4) 0.154(4) Uani 1 d D . H93 H 0.9498(4) 0.1005(5) -0.0874(4) 0.185 Uiso 1 calc R . C94 C 0.8114(4) 0.0976(5) -0.0912(4) 0.164(4) Uani 1 d D . H94 H 0.8053(4) 0.0842(5) -0.1298(4) 0.197 Uiso 1 calc R . C95 C 0.7185(3) 0.0963(3) -0.0875(2) 0.0485(9) Uani 1 d D . H95 H 0.6660(3) 0.0821(3) -0.1197(2) 0.058 Uiso 1 calc R . C96 C 0.6996(6) 0.1151(4) -0.0384(3) 0.129(3) Uani 1 d D . C97 C 0.6427(8) 0.1267(6) -0.0115(4) 0.212(5) Uani 1 d . . H97A H 0.6767(15) 0.1586(79) 0.0255(13) 0.319 Uiso 1 calc R . H97B H 0.6131(50) 0.0463(17) -0.0075(32) 0.319 Uiso 1 calc R . H97C H 0.5909(37) 0.1847(66) -0.0300(19) 0.319 Uiso 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 O1 0.0301(11) 0.0300(11) 0.0342(11) -0.0075(9) 0.0076(9) -0.0022(8) O2 0.0359(11) 0.0285(11) 0.0328(11) -0.0051(9) 0.0135(9) -0.0053(9) O3 0.0347(11) 0.0329(11) 0.0278(11) -0.0024(9) 0.0073(9) -0.0086(9) O4 0.0282(10) 0.0341(11) 0.0276(10) -0.0016(9) 0.0101(9) -0.0015(8) B1 0.024(2) 0.028(2) 0.034(2) 0.0002(15) 0.0057(14) -0.0004(13) B2 0.031(2) 0.023(2) 0.033(2) 0.0010(14) 0.0114(15) -0.0043(13) C10 0.0272(15) 0.0249(15) 0.0280(15) 0.0027(12) 0.0095(12) 0.0009(11) C11 0.0286(15) 0.029(2) 0.032(2) -0.0003(13) 0.0100(13) -0.0001(12) C12 0.042(2) 0.022(2) 0.042(2) -0.0005(13) 0.0129(15) -0.0035(13) C13 0.042(2) 0.026(2) 0.038(2) 0.0064(13) 0.0102(15) 0.0045(13) C14 0.035(2) 0.027(2) 0.0270(15) 0.0060(12) 0.0130(13) 0.0018(12) C15 0.0282(15) 0.0271(15) 0.0262(15) 0.0028(12) 0.0118(12) -0.0002(12) C16 0.033(2) 0.027(2) 0.033(2) 0.0033(13) 0.0108(13) -0.0009(12) C17 0.034(2) 0.037(2) 0.033(2) -0.0032(14) 0.0077(14) -0.0047(13) C18 0.036(2) 0.048(2) 0.025(2) 0.0036(14) 0.0039(13) 0.0009(14) C19 0.040(2) 0.038(2) 0.030(2) 0.0096(14) 0.0083(14) 0.0044(14) C20 0.0252(14) 0.0225(14) 0.0281(15) -0.0015(12) 0.0048(12) -0.0013(11) C21 0.0276(14) 0.0257(15) 0.0268(15) -0.0052(12) 0.0060(12) -0.0041(12) C22 0.0283(15) 0.029(2) 0.035(2) -0.0052(13) 0.0063(13) 0.0024(12) C23 0.035(2) 0.0255(15) 0.033(2) 0.0014(13) 0.0016(13) 0.0034(12) C24 0.0258(14) 0.027(2) 0.0279(15) -0.0012(12) -0.0014(12) -0.0031(12) C25 0.0238(14) 0.0248(15) 0.0266(14) 0.0002(12) 0.0020(12) -0.0034(11) C26 0.0263(15) 0.035(2) 0.037(2) 0.0043(14) 0.0074(13) 0.0030(12) C27 0.034(2) 0.047(2) 0.041(2) 0.003(2) 0.0162(15) 0.0001(14) C28 0.044(2) 0.044(2) 0.037(2) 0.008(2) 0.014(2) -0.004(2) C29 0.040(2) 0.032(2) 0.034(2) 0.0084(13) 0.0032(14) -0.0026(13) C30 0.0261(14) 0.029(2) 0.0214(14) 0.0026(12) 0.0082(12) -0.0007(12) C31 0.033(2) 0.030(2) 0.0248(15) 0.0001(12) 0.0100(13) -0.0048(12) C32 0.030(2) 0.043(2) 0.028(2) 0.0050(14) 0.0001(13) -0.0009(13) C33 0.036(2) 0.037(2) 0.034(2) 0.0100(14) 0.0044(14) 0.0029(14) C34 0.032(2) 0.031(2) 0.028(2) 0.0029(13) 0.0106(13) 0.0006(12) C35 0.0289(15) 0.029(2) 0.0245(15) 0.0013(12) 0.0124(12) 0.0009(12) C36 0.0284(15) 0.033(2) 0.0250(15) 0.0006(12) 0.0053(12) -0.0002(12) C37 0.035(2) 0.042(2) 0.035(2) -0.0037(14) 0.0065(14) -0.0074(14) C38 0.050(2) 0.030(2) 0.050(2) -0.002(2) 0.012(2) -0.0119(15) C39 0.048(2) 0.027(2) 0.042(2) 0.0065(14) 0.011(2) 0.0005(14) C40 0.0278(14) 0.0260(15) 0.0224(14) 0.0001(12) 0.0027(12) -0.0038(12) C41 0.0261(14) 0.028(2) 0.027(2) -0.0023(12) 0.0074(12) -0.0032(12) C42 0.036(2) 0.037(2) 0.029(2) 0.0088(13) 0.0088(13) -0.0061(14) C43 0.034(2) 0.029(2) 0.038(2) 0.0103(13) 0.0046(14) -0.0032(13) C44 0.0292(15) 0.0245(15) 0.032(2) -0.0004(12) 0.0025(13) -0.0053(12) C45 0.0277(14) 0.0255(15) 0.0255(14) -0.0030(12) 0.0056(12) -0.0047(12) C46 0.037(2) 0.036(2) 0.027(2) 0.0003(13) 0.0101(13) -0.0016(13) C47 0.035(2) 0.047(2) 0.038(2) -0.006(2) 0.0157(14) -0.0030(15) C48 0.029(2) 0.039(2) 0.049(2) -0.015(2) 0.0071(15) 0.0012(14) C49 0.031(2) 0.028(2) 0.044(2) -0.0043(14) 0.0033(14) 0.0002(13) C91 0.076(3) 0.053(3) 0.104(4) 0.030(3) -0.024(3) -0.022(2) C92 0.133(5) 0.055(3) 0.049(3) 0.006(2) -0.010(3) -0.023(3) C93 0.069(4) 0.064(4) 0.307(12) 0.042(5) 0.011(5) -0.007(3) C94 0.081(4) 0.042(3) 0.368(13) 0.065(5) 0.057(6) 0.010(3) C95 0.050(2) 0.031(2) 0.053(2) -0.005(2) -0.008(2) -0.003(2) C96 0.266(9) 0.026(2) 0.147(6) 0.007(3) 0.146(6) 0.002(3) C97 0.412(15) 0.072(4) 0.242(10) 0.062(5) 0.244(11) 0.092(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 O1 B2 1.375(4) . ? O1 C11 1.393(3) . ? O2 B1 1.377(4) . ? O2 C21 1.393(3) . ? O3 B1 1.372(4) . ? O3 C31 1.397(3) . ? O4 B2 1.367(4) . ? O4 C41 1.393(3) . ? B1 B2 1.715(5) . ? C10 C11 1.378(4) . ? C10 C15 1.431(4) . ? C10 C20 1.503(4) . ? C11 C12 1.409(4) . ? C12 C13 1.354(4) . ? C13 C14 1.415(4) . ? C14 C19 1.414(4) . ? C14 C15 1.424(4) . ? C15 C16 1.418(4) . ? C16 C17 1.370(4) . ? C17 C18 1.408(4) . ? C18 C19 1.364(4) . ? C20 C21 1.372(4) . ? C20 C25 1.435(4) . ? C21 C22 1.409(4) . ? C22 C23 1.363(4) . ? C23 C24 1.416(4) . ? C24 C29 1.423(4) . ? C24 C25 1.424(4) . ? C25 C26 1.420(4) . ? C26 C27 1.370(4) . ? C27 C28 1.403(4) . ? C28 C29 1.361(4) . ? C30 C31 1.371(4) . ? C30 C35 1.438(4) . ? C30 C40 1.510(4) . ? C31 C32 1.412(4) . ? C32 C33 1.359(4) . ? C33 C34 1.408(4) . ? C34 C39 1.419(4) . ? C34 C35 1.429(4) . ? C35 C36 1.417(4) . ? C36 C37 1.364(4) . ? C37 C38 1.407(4) . ? C38 C39 1.361(4) . ? C40 C41 1.378(4) . ? C40 C45 1.435(4) . ? C41 C42 1.406(4) . ? C42 C43 1.360(4) . ? C43 C44 1.414(4) . ? C44 C45 1.421(4) . ? C44 C49 1.423(4) . ? C45 C46 1.417(4) . ? C46 C47 1.368(4) . ? C47 C48 1.402(4) . ? C48 C49 1.368(4) . ? C91 C92 1.334(7) . ? C91 C96 1.699(8) . ? C92 C93 1.677(9) . ? C93 C94 1.141(7) . ? C94 C95 1.334(6) . ? C95 C96 1.329(6) . ? C96 C97 1.177(8) . ? 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 B2 O1 C11 116.4(2) . . ? B1 O2 C21 116.3(2) . . ? B1 O3 C31 117.5(2) . . ? B2 O4 C41 117.0(2) . . ? O3 B1 O2 113.8(3) . . ? O3 B1 B2 122.5(2) . . ? O2 B1 B2 123.6(3) . . ? O4 B2 O1 113.8(3) . . ? O4 B2 B1 122.5(2) . . ? O1 B2 B1 123.6(3) . . ? C11 C10 C15 118.1(2) . . ? C11 C10 C20 122.0(2) . . ? C15 C10 C20 119.9(2) . . ? C10 C11 O1 121.0(2) . . ? C10 C11 C12 122.3(3) . . ? O1 C11 C12 116.8(2) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C14 121.0(3) . . ? C19 C14 C13 121.7(3) . . ? C19 C14 C15 119.2(3) . . ? C13 C14 C15 119.1(3) . . ? C16 C15 C14 118.2(2) . . ? C16 C15 C10 122.2(2) . . ? C14 C15 C10 119.6(2) . . ? C17 C16 C15 121.0(3) . . ? C16 C17 C18 120.6(3) . . ? C19 C18 C17 119.8(3) . . ? C18 C19 C14 121.2(3) . . ? C21 C20 C25 118.2(2) . . ? C21 C20 C10 122.1(2) . . ? C25 C20 C10 119.6(2) . . ? C20 C21 O2 121.0(2) . . ? C20 C21 C22 122.5(3) . . ? O2 C21 C22 116.5(2) . . ? C23 C22 C21 119.6(3) . . ? C22 C23 C24 121.0(3) . . ? C23 C24 C29 121.8(3) . . ? C23 C24 C25 119.1(3) . . ? C29 C24 C25 119.1(3) . . ? C26 C25 C24 118.2(3) . . ? C26 C25 C20 122.3(2) . . ? C24 C25 C20 119.5(2) . . ? C27 C26 C25 120.9(3) . . ? C26 C27 C28 120.8(3) . . ? C29 C28 C27 120.1(3) . . ? C28 C29 C24 121.0(3) . . ? C31 C30 C35 117.9(2) . . ? C31 C30 C40 122.0(2) . . ? C35 C30 C40 120.1(2) . . ? C30 C31 O3 121.4(2) . . ? C30 C31 C32 122.7(3) . . ? O3 C31 C32 115.9(2) . . ? C33 C32 C31 119.7(3) . . ? C32 C33 C34 120.9(3) . . ? C33 C34 C39 121.8(3) . . ? C33 C34 C35 119.4(3) . . ? C39 C34 C35 118.8(3) . . ? C36 C35 C34 118.1(2) . . ? C36 C35 C30 122.6(2) . . ? C34 C35 C30 119.4(2) . . ? C37 C36 C35 121.3(3) . . ? C36 C37 C38 120.6(3) . . ? C39 C38 C37 119.8(3) . . ? C38 C39 C34 121.4(3) . . ? C41 C40 C45 117.7(2) . . ? C41 C40 C30 121.6(2) . . ? C45 C40 C30 120.8(2) . . ? C40 C41 O4 121.2(2) . . ? C40 C41 C42 122.7(3) . . ? O4 C41 C42 116.1(2) . . ? C43 C42 C41 119.9(3) . . ? C42 C43 C44 120.6(3) . . ? C43 C44 C45 119.4(3) . . ? C43 C44 C49 121.5(3) . . ? C45 C44 C49 119.1(3) . . ? C46 C45 C44 118.2(3) . . ? C46 C45 C40 122.0(3) . . ? C44 C45 C40 119.8(2) . . ? C47 C46 C45 121.0(3) . . ? C46 C47 C48 121.0(3) . . ? C49 C48 C47 119.6(3) . . ? C48 C49 C44 121.0(3) . . ? C92 C91 C96 108.3(5) . . ? C91 C92 C93 134.5(5) . . ? C94 C93 C92 92.6(8) . . ? C93 C94 C95 152.5(11) . . ? C96 C95 C94 119.8(6) . . ? C97 C96 C95 150.1(10) . . ? C97 C96 C91 97.6(7) . . ? C95 C96 C91 112.3(6) . . ? 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 O1 B2 B1 O2 -74.5(4) . . . . ? O3 B1 B2 O4 -71.3(4) . . . . ? O1 B2 B1 O3 106.2(3) . . . . ? O2 B1 B2 O4 108.0(3) . . . . ? C21 C20 C10 C11 -83.8(3) . . . . ? C21 C20 C10 C15 97.3(3) . . . . ? C25 C20 C10 C11 97.4(3) . . . . ? C25 C20 C10 C15 -81.5(3) . . . . ? C45 C40 C30 C35 -76.5(3) . . . . ? C45 C40 C30 C31 103.1(3) . . . . ? C41 C40 C30 C35 103.0(3) . . . . ? C41 C40 C30 C31 -77.5(4) . . . . ? _refine_diff_density_max 0.691 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.047 #=END data_5 _publ_section_exptl_refinement ; Unit cell dimensions were determined from 287 reflections taken from three sets of 30 frames (at 0.3\% steps in \w) each at 30 seconds exposure. A full hemisphere of reiciprocal space was scanned by 0.3\% \w steps at \f 0, 90 and 180\% with the area detector held at 2\q = -29\%. The crystal-to-detector distance was 4.974 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times the U~iso~ value of their attached carbon for aromatic hydrogens and 1.5 U~iso~ for all others. Two toluene solvent molecules were present and the first C81-C84 was refined without any restraints, and was disordered about a two fold axis of symmetry. The phenyl ring of the second toluene molecule C91-97 was constranied to a regular hexagonal geometry (C-C 1.39 \A) ; _audit_creation_method SHELXL _chemical_name_systematic ; bistriphenylphospine-bis{(dimethyl-L-tartrate)boryl} platinum toluene solvate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural 'Pt (P Ph3)2 (B O2 C2 H2 C O2 Me)2 (Me C6 H5) 1.5' _chemical_formula_analytical ? _chemical_formula_sum 'C58.50 H58 B2 O12 P2 Pt' _chemical_formula_weight 1231.70 _chemical_melting_point ? _chemical_compound_source ? 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 15.668(2) _cell_length_b 28.485(3) _cell_length_c 12.696(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5666.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 287 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method ? _exptl_crystal_F_000 2492 _exptl_absorpt_coefficient_mu 2.593 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.68 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 35886 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12895 _reflns_number_observed 9168 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.0000P] where P=(Max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'see text' _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 -0.010(7) _refine_ls_number_reflns 12895 _refine_ls_number_parameters 654 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_obs 0.0442 _refine_ls_wR_factor_all 0.0867 _refine_ls_wR_factor_obs 0.0753 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.049 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max -3.573 _refine_ls_shift/esd_mean 0.193 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt -0.380377(12) 0.702573(7) 0.99837(3) 0.02097(6) Uani 1 d . . B1 B -0.3834(4) 0.6301(2) 0.9984(9) 0.0263(13) Uani 1 d . . B2 B -0.3839(6) 0.6820(3) 1.1533(6) 0.027(2) Uani 1 d . . O1 O -0.3076(3) 0.6750(2) 1.2081(4) 0.0260(12) Uani 1 d . . O2 O -0.4528(3) 0.6737(2) 1.2194(4) 0.0287(11) Uani 1 d . . O3 O -0.3225(3) 0.5999(2) 1.0393(3) 0.0328(12) Uani 1 d . . O4 O -0.4498(3) 0.60363(15) 0.9513(3) 0.0272(11) Uani 1 d . . O11 O -0.1895(4) 0.6494(3) 1.3734(5) 0.068(2) Uani 1 d . . O12 O -0.2790(4) 0.7008(2) 1.4503(4) 0.063(2) Uani 1 d . . O13 O -0.4231(3) 0.6074(2) 1.4545(4) 0.0469(14) Uani 1 d . . O14 O -0.5424(3) 0.6144(2) 1.3577(4) 0.0408(13) Uani 1 d . . O21 O -0.3671(5) 0.5467(2) 1.2118(4) 0.077(2) Uani 1 d . . O22 O -0.3830(6) 0.4827(2) 1.1100(4) 0.072(2) Uani 1 d . . O23 O -0.4249(4) 0.5588(2) 0.7638(4) 0.059(2) Uani 1 d . . O24 O -0.3904(4) 0.4922(2) 0.8448(4) 0.049(2) Uani 1 d . . P1 P -0.36122(10) 0.70447(7) 0.81339(12) 0.0245(4) Uani 1 d . . P2 P -0.39056(11) 0.78211(5) 1.04312(13) 0.0229(4) Uani 1 d . . C1 C -0.4780(4) 0.8110(2) 0.9739(5) 0.029(2) Uani 1 d . . C2 C -0.5498(4) 0.7842(2) 0.9517(6) 0.035(2) Uani 1 d . . H2A H -0.5500(4) 0.7517(2) 0.9685(6) 0.042 Uiso 1 calc R . C3 C -0.6213(5) 0.8042(3) 0.9052(5) 0.042(2) Uani 1 d . . H3A H -0.6703(5) 0.7856(3) 0.8911(5) 0.050 Uiso 1 calc R . C4 C -0.6209(5) 0.8508(2) 0.8799(6) 0.042(2) Uani 1 d . . H4A H -0.6702(5) 0.8647(2) 0.8495(6) 0.051 Uiso 1 calc R . C5 C -0.5498(5) 0.8778(3) 0.8982(8) 0.062(3) Uani 1 d . . H5A H -0.5489(5) 0.9099(3) 0.8774(8) 0.075 Uiso 1 calc R . C6 C -0.4793(5) 0.8579(3) 0.9472(6) 0.048(2) Uani 1 d . . H6A H -0.4312(5) 0.8770(3) 0.9626(6) 0.058 Uiso 1 calc R . C11 C -0.2964(4) 0.8197(2) 1.0273(5) 0.029(2) Uani 1 d . . C12 C -0.2955(5) 0.8653(2) 1.0699(6) 0.041(2) Uani 1 d . . H12A H -0.3432(5) 0.8763(2) 1.1091(6) 0.049 Uiso 1 calc R . C13 C -0.2252(6) 0.8947(3) 1.0550(7) 0.063(3) Uani 1 d . . H13A H -0.2254(6) 0.9260(3) 1.0808(7) 0.075 Uiso 1 calc R . C14 C -0.1546(5) 0.8769(3) 1.0013(10) 0.067(3) Uani 1 d . . H14A H -0.1062(5) 0.8965(3) 0.9916(10) 0.080 Uiso 1 calc R . C15 C -0.1529(5) 0.8328(3) 0.9628(6) 0.055(3) Uani 1 d . . H15A H -0.1033(5) 0.8215(3) 0.9281(6) 0.066 Uiso 1 calc R . C16 C -0.2252(4) 0.8033(3) 0.9741(5) 0.038(2) Uani 1 d . . H16A H -0.2248(4) 0.7725(3) 0.9454(5) 0.046 Uiso 1 calc R . C21 C -0.4160(4) 0.7933(2) 1.1823(5) 0.0259(14) Uani 1 d . . C22 C -0.4951(5) 0.8069(3) 1.2175(6) 0.051(2) Uani 1 d . . H22A H -0.5393(5) 0.8119(3) 1.1676(6) 0.061 Uiso 1 calc R . C23 C -0.5125(6) 0.8137(4) 1.3232(7) 0.069(3) Uani 1 d . . H23A H -0.5678(6) 0.8232(4) 1.3452(7) 0.082 Uiso 1 calc R . C24 C -0.4495(5) 0.8067(3) 1.3952(6) 0.051(2) Uani 1 d . . H24A H -0.4614(5) 0.8109(3) 1.4680(6) 0.061 Uiso 1 calc R . C25 C -0.3690(5) 0.7937(3) 1.3646(5) 0.040(2) Uani 1 d . . H25A H -0.3255(5) 0.7898(3) 1.4159(5) 0.048 Uiso 1 calc R . C26 C -0.3506(6) 0.7862(3) 1.2574(6) 0.035(2) Uani 1 d . . H26A H -0.2952(6) 0.7766(3) 1.2359(6) 0.042 Uiso 1 calc R . C31 C -0.2885(5) 0.6566(2) 0.7713(6) 0.027(2) Uani 1 d . . C32 C -0.2268(4) 0.6416(2) 0.8405(6) 0.033(2) Uani 1 d . . H32A H -0.2220(4) 0.6561(2) 0.9076(6) 0.040 Uiso 1 calc R . C33 C -0.1716(5) 0.6056(3) 0.8135(7) 0.051(2) Uani 1 d . . H33A H -0.1286(5) 0.5957(3) 0.8614(7) 0.061 Uiso 1 calc R . C34 C -0.1795(6) 0.5840(3) 0.7153(7) 0.056(2) Uani 1 d . . H34A H -0.1427(6) 0.5589(3) 0.6965(7) 0.067 Uiso 1 calc R . C35 C -0.2409(5) 0.5993(3) 0.6457(7) 0.049(2) Uani 1 d . . H35A H -0.2460(5) 0.5848(3) 0.5786(7) 0.059 Uiso 1 calc R . C36 C -0.2953(5) 0.6357(3) 0.6728(6) 0.038(2) Uani 1 d . . H36A H -0.3371(5) 0.6463(3) 0.6242(6) 0.046 Uiso 1 calc R . C41 C -0.4590(4) 0.6974(2) 0.7350(5) 0.0267(15) Uani 1 d . . C42 C -0.5315(4) 0.6792(2) 0.7832(5) 0.030(2) Uani 1 d . . H42A H -0.5292(4) 0.6700(2) 0.8551(5) 0.036 Uiso 1 calc R . C43 C -0.6066(5) 0.6743(3) 0.7277(6) 0.044(2) Uani 1 d . . H43A H -0.6556(5) 0.6615(3) 0.7612(6) 0.052 Uiso 1 calc R . C44 C -0.6108(5) 0.6881(3) 0.6227(6) 0.049(2) Uani 1 d . . H44A H -0.6626(5) 0.6851(3) 0.5844(6) 0.059 Uiso 1 calc R . C45 C -0.5387(5) 0.7063(3) 0.5743(5) 0.044(2) Uani 1 d . . H45A H -0.5411(5) 0.7158(3) 0.5027(5) 0.053 Uiso 1 calc R . C46 C -0.4633(4) 0.7108(3) 0.6301(5) 0.031(2) Uani 1 d . . H46A H -0.4141(4) 0.7232(3) 0.5963(5) 0.037 Uiso 1 calc R . C51 C -0.3124(5) 0.7562(2) 0.7520(6) 0.029(2) Uani 1 d . . C52 C -0.2253(5) 0.7571(3) 0.7260(7) 0.044(2) Uani 1 d . . H52A H -0.1916(5) 0.7297(3) 0.7341(7) 0.053 Uiso 1 calc R . C53 C -0.1890(5) 0.7979(3) 0.6886(7) 0.058(2) Uani 1 d . . H53A H -0.1303(5) 0.7982(3) 0.6696(7) 0.070 Uiso 1 calc R . C54 C -0.2382(7) 0.8392(3) 0.6783(7) 0.068(3) Uani 1 d . . H54A H -0.2123(7) 0.8675(3) 0.6551(7) 0.082 Uiso 1 calc R . C55 C -0.3236(6) 0.8381(3) 0.7020(7) 0.054(3) Uani 1 d . . H55A H -0.3575(6) 0.8654(3) 0.6924(7) 0.065 Uiso 1 calc R . C56 C -0.3605(6) 0.7973(3) 0.7397(6) 0.040(2) Uani 1 d . . H56A H -0.4194(6) 0.7972(3) 0.7575(6) 0.048 Uiso 1 calc R . C61 C -0.3274(4) 0.6523(3) 1.3059(5) 0.026(2) Uani 1 d . . H61A H -0.3206(4) 0.6176(3) 1.2987(5) 0.031 Uiso 1 calc R . C62 C -0.4203(4) 0.6645(2) 1.3231(5) 0.029(2) Uani 1 d . . H62A H -0.4240(4) 0.6939(2) 1.3660(5) 0.035 Uiso 1 calc R . C63 C -0.4711(5) 0.6257(2) 1.3779(6) 0.033(2) Uani 1 d . . C64 C -0.4667(6) 0.5737(3) 1.5213(7) 0.072(3) Uani 1 d . . H64A H -0.4271(6) 0.5621(3) 1.5751(7) 0.107 Uiso 1 calc R . H64B H -0.4869(6) 0.5474(3) 1.4783(7) 0.107 Uiso 1 calc R . H64C H -0.5154(6) 0.5890(3) 1.5555(7) 0.107 Uiso 1 calc R . C65 C -0.2649(6) 0.6711(3) 1.3871(6) 0.045(2) Uani 1 d . . C66 C -0.1179(6) 0.6673(4) 1.4343(8) 0.114(5) Uani 1 d . . H66A H -0.0666(6) 0.6490(4) 1.4183(8) 0.171 Uiso 1 calc R . H66B H -0.1308(6) 0.6648(4) 1.5096(8) 0.171 Uiso 1 calc R . H66C H -0.1080(6) 0.7003(4) 1.4161(8) 0.171 Uiso 1 calc R . C71 C -0.3471(4) 0.5526(2) 1.0226(5) 0.031(2) Uani 1 d . . H71A H -0.3009(4) 0.5353(2) 0.9844(5) 0.037 Uiso 1 calc R . C72 C -0.4281(4) 0.5551(2) 0.9538(5) 0.029(2) Uani 1 d . . H72A H -0.4750(4) 0.5370(2) 0.9884(5) 0.035 Uiso 1 calc R . C73 C -0.4153(5) 0.5371(3) 0.8429(6) 0.034(2) Uani 1 d . . C74 C -0.3724(7) 0.4721(3) 0.7420(6) 0.061(3) Uani 1 d . . H74A H -0.3547(7) 0.4393(3) 0.7504(6) 0.091 Uiso 1 calc R . H74B H -0.3264(7) 0.4899(3) 0.7081(6) 0.091 Uiso 1 calc R . H74C H -0.4238(7) 0.4735(3) 0.6983(6) 0.091 Uiso 1 calc R . C75 C -0.3663(7) 0.5283(3) 1.1282(6) 0.050(2) Uani 1 d . . C76 C -0.4018(7) 0.4539(3) 1.2025(6) 0.071(3) Uani 1 d . . H76A H -0.4129(7) 0.4215(3) 1.1804(6) 0.107 Uiso 1 calc R . H76B H -0.4522(7) 0.4664(3) 1.2386(6) 0.107 Uiso 1 calc R . H76C H -0.3528(7) 0.4545(3) 1.2506(6) 0.107 Uiso 1 calc R . C82 C -0.4492(10) 0.9925(6) 1.0133(18) 0.171(6) Uiso 1 d . . C81 C -0.3984(13) 0.9858(7) 0.9258(16) 0.188(8) Uiso 1 d . . H81A H -0.3394(13) 0.9783(7) 0.9306(16) 0.225 Uiso 1 calc R . C83 C -0.4416(18) 0.9912(13) 0.8279(24) 0.351(19) Uiso 1 d . . H83A H -0.4122(18) 0.9861(13) 0.7634(24) 0.421 Uiso 1 calc R . C84 C -0.4710(24) 0.9948(19) 1.1167(23) 0.163(15) Uiso 0.50 d P . H84A H -0.5318(24) 1.0023(19) 1.1230(23) 0.244 Uiso 0.50 calc PR . H84B H -0.4372(24) 1.0192(19) 1.1515(23) 0.244 Uiso 0.50 calc PR . H84C H -0.4597(24) 0.9644(19) 1.1503(23) 0.244 Uiso 0.50 calc PR . C91 C -0.1185(10) 0.4909(8) 0.4993(21) 0.274(17) Uani 1 d GD . C92 C -0.1395(12) 0.4507(8) 0.5558(14) 0.302(24) Uani 1 d G . C93 C -0.2210(15) 0.4317(5) 0.5476(13) 0.207(10) Uani 1 d G . C94 C -0.2814(7) 0.4529(9) 0.4831(17) 0.273(17) Uani 1 d G . C95 C -0.2604(16) 0.4930(9) 0.4266(11) 0.351(24) Uani 1 d GD . C96 C -0.1790(20) 0.5121(5) 0.4348(15) 0.327(33) Uani 1 d G . H91 H -0.0694(12) 0.5035(12) 0.5140(31) 0.393 Uiso 1 calc G . H93 H -0.2352(27) 0.4013(6) 0.5895(21) 0.393 Uiso 1 d G . H94 H -0.3357(8) 0.4389(13) 0.4707(28) 0.393 Uiso 1 d G . H95 H -0.3052(22) 0.5087(13) 0.4012(16) 0.393 Uiso 1 d G . H96 H -0.1575(33) 0.5425(6) 0.3782(25) 0.393 Uiso 1 d G . C97 C -0.0988(26) 0.4350(12) 0.6391(33) 0.505(32) Uani 1 d . . H97A H -0.0418(26) 0.4491(12) 0.6420(33) 0.758 Uiso 1 calc R . H97B H -0.0935(26) 0.4008(12) 0.6347(33) 0.758 Uiso 1 calc R . H97C H -0.1306(26) 0.4434(12) 0.7028(33) 0.758 Uiso 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 Pt1 0.02366(10) 0.01997(9) 0.01926(9) 0.0017(2) 0.0013(2) -0.00216(11) B1 0.028(3) 0.023(3) 0.027(3) 0.008(5) 0.013(7) -0.001(3) B2 0.032(4) 0.022(4) 0.026(4) 0.001(3) 0.003(4) 0.003(4) O1 0.022(3) 0.037(3) 0.020(3) 0.001(2) 0.000(2) -0.002(2) O2 0.029(3) 0.035(3) 0.022(3) 0.007(2) 0.003(2) 0.001(2) O3 0.034(3) 0.026(2) 0.039(3) -0.001(2) -0.012(2) 0.000(2) O4 0.026(2) 0.016(2) 0.039(3) -0.003(2) 0.000(2) -0.002(2) O11 0.038(3) 0.123(6) 0.043(4) -0.008(4) -0.019(3) -0.013(4) O12 0.095(5) 0.060(4) 0.036(3) -0.009(3) -0.026(3) -0.018(4) O13 0.057(3) 0.056(3) 0.028(3) 0.017(3) -0.008(2) -0.017(3) O14 0.038(3) 0.047(3) 0.038(3) 0.004(3) 0.001(3) -0.011(3) O21 0.156(7) 0.047(4) 0.029(3) 0.001(3) -0.002(5) -0.019(5) O22 0.155(7) 0.023(3) 0.039(3) 0.010(3) -0.008(5) -0.001(4) O23 0.100(5) 0.047(4) 0.030(3) 0.002(3) -0.003(3) -0.003(3) O24 0.082(4) 0.032(3) 0.033(3) -0.008(2) 0.001(3) 0.014(3) P1 0.0279(9) 0.0250(8) 0.0207(8) 0.0037(8) 0.0019(7) 0.0007(9) P2 0.0218(8) 0.0216(7) 0.0254(8) 0.0001(6) 0.0029(7) -0.0044(7) C1 0.033(4) 0.029(3) 0.025(5) -0.001(3) 0.004(3) -0.001(3) C2 0.029(4) 0.028(4) 0.047(4) 0.003(3) -0.008(3) -0.001(3) C3 0.036(4) 0.043(4) 0.047(4) -0.003(4) -0.001(4) -0.002(4) C4 0.033(4) 0.043(4) 0.051(5) 0.008(4) -0.009(4) 0.011(4) C5 0.049(5) 0.030(4) 0.108(8) 0.014(5) -0.029(6) 0.003(4) C6 0.047(5) 0.037(4) 0.061(5) 0.007(4) -0.027(4) -0.007(4) C11 0.025(3) 0.030(3) 0.031(5) 0.010(3) -0.010(3) -0.010(3) C12 0.050(5) 0.028(4) 0.044(5) 0.002(4) -0.016(4) -0.010(4) C13 0.062(6) 0.035(4) 0.091(7) 0.027(5) -0.041(6) -0.031(5) C14 0.042(4) 0.074(6) 0.085(6) 0.045(8) -0.024(8) -0.033(4) C15 0.023(4) 0.088(7) 0.053(6) 0.036(5) -0.007(4) -0.012(4) C16 0.026(3) 0.052(4) 0.037(5) 0.022(4) -0.004(3) -0.002(3) C21 0.032(3) 0.017(3) 0.029(4) -0.007(3) 0.001(3) 0.000(3) C22 0.035(4) 0.079(7) 0.038(5) -0.009(5) -0.001(4) 0.014(4) C23 0.044(5) 0.121(10) 0.042(5) -0.018(6) 0.006(4) 0.012(6) C24 0.055(5) 0.072(7) 0.025(4) -0.009(4) 0.015(4) 0.002(5) C25 0.045(5) 0.046(4) 0.029(4) -0.005(4) -0.005(3) -0.002(4) C26 0.043(5) 0.031(5) 0.031(4) -0.004(4) 0.005(4) -0.003(4) C31 0.021(4) 0.025(4) 0.036(5) 0.001(3) 0.008(3) 0.002(3) C32 0.030(4) 0.036(4) 0.034(4) 0.001(3) 0.003(3) 0.000(3) C33 0.031(4) 0.061(6) 0.060(6) 0.009(5) 0.000(4) 0.015(4) C34 0.060(6) 0.044(5) 0.063(6) -0.007(5) 0.013(5) 0.019(4) C35 0.052(5) 0.044(5) 0.053(5) -0.020(4) 0.008(5) 0.012(4) C36 0.038(5) 0.043(5) 0.034(5) 0.002(4) 0.003(4) 0.006(4) C41 0.026(3) 0.028(4) 0.027(4) 0.000(3) 0.001(3) 0.004(3) C42 0.030(4) 0.033(4) 0.026(4) 0.014(3) 0.006(3) 0.006(3) C43 0.023(4) 0.061(5) 0.047(5) 0.011(4) -0.002(4) 0.002(4) C44 0.040(5) 0.063(5) 0.044(5) 0.006(4) -0.013(4) -0.006(4) C45 0.049(5) 0.058(5) 0.025(4) 0.006(4) -0.006(3) 0.010(5) C46 0.028(4) 0.042(5) 0.024(4) 0.002(3) 0.002(3) 0.000(3) C51 0.036(4) 0.028(4) 0.022(4) 0.004(3) 0.005(3) -0.008(3) C52 0.047(5) 0.043(5) 0.042(5) 0.009(4) 0.018(4) -0.006(4) C53 0.056(5) 0.056(5) 0.064(6) -0.006(6) 0.032(5) -0.020(5) C54 0.099(8) 0.058(7) 0.047(6) 0.019(5) 0.013(6) -0.028(6) C55 0.083(7) 0.035(5) 0.046(5) 0.013(4) 0.006(5) -0.006(5) C56 0.051(5) 0.031(4) 0.037(4) 0.009(4) 0.008(4) 0.004(5) C61 0.024(4) 0.037(4) 0.016(4) 0.002(3) 0.001(3) -0.005(3) C62 0.037(4) 0.032(4) 0.017(4) 0.001(3) 0.002(3) -0.004(3) C63 0.042(5) 0.028(4) 0.030(4) 0.000(3) 0.003(4) -0.004(3) C64 0.082(6) 0.081(6) 0.051(7) 0.043(6) -0.006(5) -0.029(5) C65 0.052(6) 0.051(5) 0.031(5) 0.013(4) -0.009(4) -0.023(4) C66 0.063(7) 0.202(14) 0.077(7) 0.016(8) -0.053(6) -0.047(8) C71 0.046(4) 0.020(3) 0.026(5) 0.002(3) -0.005(3) 0.008(3) C72 0.037(4) 0.023(3) 0.027(4) -0.001(3) 0.003(3) -0.003(3) C73 0.045(5) 0.030(4) 0.028(4) 0.002(4) -0.009(4) -0.006(4) C74 0.107(8) 0.047(5) 0.028(4) -0.017(4) 0.013(6) -0.002(6) C75 0.086(7) 0.028(4) 0.034(5) 0.009(4) -0.014(5) -0.005(5) C76 0.143(11) 0.041(5) 0.030(5) 0.014(4) 0.014(6) -0.004(6) C91 0.241(29) 0.204(22) 0.377(40) -0.144(30) -0.017(40) -0.028(22) C92 0.130(18) 0.385(56) 0.391(51) -0.201(39) -0.116(25) 0.057(24) C93 0.142(17) 0.296(23) 0.182(21) -0.165(19) 0.003(16) 0.040(19) C94 0.097(11) 0.539(42) 0.183(25) -0.262(30) -0.045(15) 0.079(17) C95 0.322(51) 0.591(55) 0.139(21) -0.207(29) -0.056(23) 0.246(38) C96 0.345(55) 0.413(65) 0.224(39) -0.213(43) -0.102(37) 0.241(50) C97 0.717(86) 0.204(32) 0.594(89) -0.073(45) 0.119(58) 0.144(50) _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 Pt1 B2 2.054(7) . ? Pt1 B1 2.065(5) . ? Pt1 P2 2.341(2) . ? Pt1 P1 2.368(2) . ? B1 O3 1.385(8) . ? B1 O4 1.417(9) . ? B1 B2 2.460(13) . ? B2 O2 1.387(9) . ? B2 O1 1.398(9) . ? O1 C61 1.434(8) . ? O2 C62 1.435(8) . ? O3 C71 1.417(7) . ? O4 C72 1.424(7) . ? O11 C65 1.345(10) . ? O11 C66 1.456(10) . ? O12 C65 1.186(9) . ? O13 C63 1.335(8) . ? O13 C64 1.450(8) . ? O14 C63 1.191(8) . ? O21 C75 1.183(9) . ? O22 C75 1.345(9) . ? O22 C76 1.463(8) . ? O23 C73 1.188(9) . ? O24 C73 1.339(9) . ? O24 C74 1.453(8) . ? P1 C51 1.835(7) . ? P1 C41 1.838(7) . ? P1 C31 1.855(7) . ? P2 C1 1.824(7) . ? P2 C11 1.834(6) . ? P2 C21 1.839(6) . ? C1 C6 1.380(9) . ? C1 C2 1.387(9) . ? C2 C3 1.389(9) . ? C3 C4 1.365(9) . ? C4 C5 1.373(11) . ? C5 C6 1.388(10) . ? C11 C16 1.386(9) . ? C11 C12 1.408(9) . ? C12 C13 1.395(10) . ? C13 C14 1.394(13) . ? C14 C15 1.349(12) . ? C15 C16 1.417(9) . ? C21 C22 1.373(9) . ? C21 C26 1.414(10) . ? C22 C23 1.383(11) . ? C23 C24 1.361(11) . ? C24 C25 1.370(10) . ? C25 C26 1.407(9) . ? C31 C32 1.375(10) . ? C31 C36 1.389(10) . ? C32 C33 1.385(10) . ? C33 C34 1.396(11) . ? C34 C35 1.377(11) . ? C35 C36 1.384(10) . ? C41 C46 1.387(9) . ? C41 C42 1.391(8) . ? C42 C43 1.379(9) . ? C43 C44 1.392(10) . ? C44 C45 1.386(10) . ? C45 C46 1.383(9) . ? C51 C52 1.404(10) . ? C51 C56 1.400(10) . ? C52 C53 1.378(10) . ? C53 C54 1.412(12) . ? C54 C55 1.372(12) . ? C55 C56 1.382(11) . ? C61 C62 1.512(9) . ? C61 C65 1.519(10) . ? C62 C63 1.530(9) . ? C71 C75 1.538(9) . ? C71 C72 1.541(9) . ? C72 C73 1.511(10) . ? C82 C84 1.36(3) . ? C82 C81 1.38(2) . ? C82 C82 1.65(3) 2_475 ? C81 C83 1.42(3) . ? C83 C83 1.90(6) 2_475 ? C91 C92 1.39 . ? C91 C96 1.39 . ? C92 C97 1.31(4) . ? C92 C93 1.39 . ? C93 C94 1.39 . ? C94 C95 1.39 . ? C95 C96 1.39 . ? 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 B2 Pt1 B1 73.3(4) . . ? B2 Pt1 P2 92.4(2) . . ? B1 Pt1 P2 165.0(3) . . ? B2 Pt1 P1 163.7(2) . . ? B1 Pt1 P1 91.5(3) . . ? P2 Pt1 P1 103.14(6) . . ? O3 B1 O4 109.5(4) . . ? O3 B1 Pt1 127.3(5) . . ? O4 B1 Pt1 123.3(5) . . ? O3 B1 B2 94.4(6) . . ? O4 B1 B2 130.8(5) . . ? Pt1 B1 B2 53.1(3) . . ? O2 B2 O1 109.9(5) . . ? O2 B2 Pt1 130.5(6) . . ? O1 B2 Pt1 119.6(5) . . ? O2 B2 B1 112.7(5) . . ? O1 B2 B1 108.0(5) . . ? Pt1 B2 B1 53.6(3) . . ? B2 O1 C61 108.1(5) . . ? B2 O2 C62 108.1(5) . . ? B1 O3 C71 110.3(5) . . ? B1 O4 C72 109.3(5) . . ? C65 O11 C66 116.5(8) . . ? C63 O13 C64 114.8(6) . . ? C75 O22 C76 116.3(6) . . ? C73 O24 C74 114.7(6) . . ? C51 P1 C41 101.9(3) . . ? C51 P1 C31 102.3(3) . . ? C41 P1 C31 105.9(3) . . ? C51 P1 Pt1 119.5(2) . . ? C41 P1 Pt1 115.4(2) . . ? C31 P1 Pt1 110.3(3) . . ? C1 P2 C11 106.7(3) . . ? C1 P2 C21 102.8(3) . . ? C11 P2 C21 100.3(3) . . ? C1 P2 Pt1 111.8(2) . . ? C11 P2 Pt1 118.9(2) . . ? C21 P2 Pt1 114.5(2) . . ? C6 C1 C2 118.1(6) . . ? C6 C1 P2 124.5(5) . . ? C2 C1 P2 117.3(5) . . ? C1 C2 C3 121.0(6) . . ? C4 C3 C2 119.7(7) . . ? C3 C4 C5 120.6(7) . . ? C4 C5 C6 119.5(7) . . ? C1 C6 C5 121.2(7) . . ? C16 C11 C12 119.4(6) . . ? C16 C11 P2 120.3(5) . . ? C12 C11 P2 120.3(6) . . ? C13 C12 C11 120.5(8) . . ? C14 C13 C12 118.4(8) . . ? C15 C14 C13 122.0(7) . . ? C14 C15 C16 120.0(8) . . ? C11 C16 C15 119.5(7) . . ? C22 C21 C26 118.4(6) . . ? C22 C21 P2 123.9(5) . . ? C26 C21 P2 117.8(5) . . ? C21 C22 C23 122.2(8) . . ? C24 C23 C22 119.3(8) . . ? C23 C24 C25 121.1(7) . . ? C24 C25 C26 120.3(7) . . ? C25 C26 C21 118.8(7) . . ? C32 C31 C36 119.7(7) . . ? C32 C31 P1 118.4(6) . . ? C36 C31 P1 121.9(6) . . ? C31 C32 C33 120.7(7) . . ? C32 C33 C34 119.5(8) . . ? C35 C34 C33 119.7(8) . . ? C34 C35 C36 120.5(8) . . ? C35 C36 C31 119.9(8) . . ? C46 C41 C42 119.0(6) . . ? C46 C41 P1 122.1(5) . . ? C42 C41 P1 118.9(5) . . ? C43 C42 C41 120.6(6) . . ? C42 C43 C44 120.1(7) . . ? C45 C44 C43 119.5(7) . . ? C46 C45 C44 120.2(7) . . ? C45 C46 C41 120.5(6) . . ? C52 C51 C56 118.8(7) . . ? C52 C51 P1 121.3(6) . . ? C56 C51 P1 119.7(6) . . ? C53 C52 C51 119.9(8) . . ? C52 C53 C54 120.5(8) . . ? C55 C54 C53 119.6(8) . . ? C54 C55 C56 120.2(9) . . ? C55 C56 C51 121.1(9) . . ? O1 C61 C62 103.3(6) . . ? O1 C61 C65 106.8(5) . . ? C62 C61 C65 116.2(7) . . ? O2 C62 C61 104.6(6) . . ? O2 C62 C63 111.4(6) . . ? C61 C62 C63 113.5(6) . . ? O14 C63 O13 125.5(7) . . ? O14 C63 C62 125.8(7) . . ? O13 C63 C62 108.8(6) . . ? O12 C65 O11 125.4(8) . . ? O12 C65 C61 126.2(8) . . ? O11 C65 C61 108.5(7) . . ? O3 C71 C75 110.4(5) . . ? O3 C71 C72 105.3(5) . . ? C75 C71 C72 110.8(6) . . ? O4 C72 C73 109.9(6) . . ? O4 C72 C71 104.8(5) . . ? C73 C72 C71 113.8(6) . . ? O23 C73 O24 123.3(7) . . ? O23 C73 C72 126.5(7) . . ? O24 C73 C72 110.2(6) . . ? O21 C75 O22 125.3(7) . . ? O21 C75 C71 125.9(7) . . ? O22 C75 C71 108.7(6) . . ? C84 C82 C81 158.4(25) . . ? C84 C82 C82 75.2(18) . 2_475 ? C81 C82 C82 126.4(12) . 2_475 ? C82 C81 C83 114.4(21) . . ? C81 C83 C83 119.1(16) . 2_475 ? C92 C91 C96 120.0 . . ? C97 C92 C93 111.9(27) . . ? C97 C92 C91 125.5(26) . . ? C93 C92 C91 120.0 . . ? C92 C93 C94 120.0 . . ? C93 C94 C95 120.0 . . ? C96 C95 C94 120.0 . . ? C95 C96 C91 120.0 . . ? 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 O3 C71 C72 O4 -8.8(6) . . . . ? O1 C62 C61 O2 -24.5(7) . . . . ? _refine_diff_density_max 0.814 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.113 #=END data_6 _publ_section_exptl_refinement ; Unit cell dimensions were determined from 454 reflections taken from three sets of 10 frames (at 0.3\% steps in \w) each at 10 seconds exposure. A full hemisphere of reiciprocal space was scanned by 0.3\% \w steps at \f 0, 90 and 180\% with the area detector held at 2\q = -29\%. The crystal-to-detector distance was 4.974 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analysing the duplicate reflections. No decay was observed. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times the U~iso~ value of their attached carbon. Three dichloromethane solvent molecules were present in the crystal structure. The C(96) solvate was disordered over two positions in the ratio 27:73, the other two molecules which lay on 2-fold axes were refined in the occupancy 50 : 50. ; _audit_creation_method SHELXL _chemical_name_systematic ; bistriphenylphosphine-{bis(phenylethane-1,2-diol)boryl} platinum dichloromethane solvate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural 'Pt (P Ph3) 2 (B O2 C2 H3 Ph)2 (C H2 Cl2)2.0' _chemical_formula_analytical ? _chemical_formula_sum 'C54 H50 B2 Cl4 O4 P2 Pt' _chemical_formula_weight 1183.39 _chemical_melting_point ? _chemical_compound_source ? 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' 'Pt' 'Pt' -1.7033 8.3905 '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 monoclinic _symmetry_space_group_name_H-M 'C 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 38.311(3) _cell_length_b 12.1983(13) _cell_length_c 11.1210(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.530(7) _cell_angle_gamma 90.00 _cell_volume 5180.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 454 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description 'block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method ? _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 3.021 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.457 _exptl_absorpt_correction_T_max 0.547 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16962 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11487 _reflns_number_observed 10455 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+0.0000P] where P=(Max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'see text' _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 -0.021(3) _refine_ls_number_reflns 11487 _refine_ls_number_parameters 642 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_obs 0.0219 _refine_ls_wR_factor_all 0.0487 _refine_ls_wR_factor_obs 0.0481 _refine_ls_goodness_of_fit_all 0.966 _refine_ls_goodness_of_fit_obs 1.004 _refine_ls_restrained_S_all 0.972 _refine_ls_restrained_S_obs 1.010 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.635260(3) -0.002020(11) 0.677155(9) 0.02596(3) Uani 1 d . . P1 P 0.68187(2) 0.05051(7) 0.81454(8) 0.0280(2) Uani 1 d . . P2 P 0.63504(2) -0.19390(7) 0.69644(8) 0.0246(2) Uani 1 d . . B1 B 0.59637(9) -0.0075(5) 0.5371(3) 0.0305(7) Uani 1 d . . B2 B 0.63024(12) 0.1575(3) 0.6192(4) 0.0371(10) Uani 1 d . . O1 O 0.56119(5) 0.0147(3) 0.5476(2) 0.0369(7) Uani 1 d . . O2 O 0.60192(6) -0.0352(2) 0.4196(2) 0.0353(6) Uani 1 d . . O3 O 0.60574(8) 0.2331(2) 0.6497(3) 0.0505(8) Uani 1 d . . O4 O 0.65328(8) 0.2048(2) 0.5459(3) 0.0490(8) Uani 1 d . . C1 C 0.69435(9) 0.1958(3) 0.8139(3) 0.0294(7) Uani 1 d . . C2 C 0.67200(13) 0.2710(3) 0.8596(4) 0.0396(11) Uani 1 d . . H2 H 0.65061(13) 0.2474(3) 0.8889(4) 0.048 Uiso 1 calc R . C3 C 0.68113(11) 0.3838(3) 0.8625(4) 0.0452(10) Uani 1 d . . H3 H 0.66603(11) 0.4356(3) 0.8955(4) 0.054 Uiso 1 calc R . C4 C 0.71140(11) 0.4180(3) 0.8182(4) 0.0456(10) Uani 1 d . . H4 H 0.71742(11) 0.4936(3) 0.8206(4) 0.055 Uiso 1 calc R . C5 C 0.73315(11) 0.3437(3) 0.7704(4) 0.0457(10) Uani 1 d . . H5 H 0.75418(11) 0.3679(3) 0.7390(4) 0.055 Uiso 1 calc R . C6 C 0.72458(10) 0.2327(3) 0.7677(3) 0.0376(9) Uani 1 d . . H6 H 0.73975(10) 0.1818(3) 0.7335(3) 0.045 Uiso 1 calc R . C7 C 0.67924(9) 0.0307(2) 0.9767(3) 0.0282(8) Uani 1 d . . C8 C 0.70254(10) 0.0798(3) 1.0627(3) 0.0366(9) Uani 1 d . . H8 H 0.72080(10) 0.1247(3) 1.0372(3) 0.044 Uiso 1 calc R . C9 C 0.69960(11) 0.0644(3) 1.1844(3) 0.0409(9) Uani 1 d . . H9 H 0.71595(11) 0.0980(3) 1.2416(3) 0.049 Uiso 1 calc R . C10 C 0.67352(9) 0.0014(5) 1.2228(3) 0.0433(8) Uani 1 d . . H10 H 0.67141(9) -0.0078(5) 1.3067(3) 0.052 Uiso 1 calc R . C11 C 0.64989(11) -0.0496(3) 1.1400(4) 0.0447(10) Uani 1 d . . H11 H 0.63206(11) -0.0955(3) 1.1670(4) 0.054 Uiso 1 calc R . C12 C 0.65243(10) -0.0334(2) 1.0175(3) 0.0360(9) Uani 1 d . . H12 H 0.63572(10) -0.0662(2) 0.9609(3) 0.043 Uiso 1 calc R . C13 C 0.72161(8) -0.0206(3) 0.7765(3) 0.0278(9) Uani 1 d . . C14 C 0.74923(9) -0.0506(3) 0.8583(3) 0.0357(8) Uani 1 d . . H14 H 0.74920(9) -0.0286(3) 0.9402(3) 0.043 Uiso 1 calc R . C15 C 0.77662(10) -0.1120(3) 0.8219(4) 0.0440(10) Uani 1 d . . H15 H 0.79547(10) -0.1310(3) 0.8787(4) 0.053 Uiso 1 calc R . C16 C 0.77705(10) -0.1465(3) 0.7033(4) 0.0435(10) Uani 1 d . . H16 H 0.79574(10) -0.1906(3) 0.6793(4) 0.052 Uiso 1 calc R . C17 C 0.75003(10) -0.1161(3) 0.6202(4) 0.0399(9) Uani 1 d . . H17 H 0.75027(10) -0.1384(3) 0.5384(4) 0.048 Uiso 1 calc R . C18 C 0.72283(9) -0.0538(3) 0.6559(3) 0.0328(8) Uani 1 d . . H18 H 0.70450(9) -0.0327(3) 0.5980(3) 0.039 Uiso 1 calc R . C19 C 0.65142(10) -0.2584(3) 0.8387(3) 0.0274(7) Uani 1 d . . C20 C 0.68724(11) -0.2588(3) 0.8723(4) 0.0320(9) Uani 1 d . . H20 H 0.70301(11) -0.2312(3) 0.8179(4) 0.038 Uiso 1 calc R . C21 C 0.70024(11) -0.2983(3) 0.9830(3) 0.0433(10) Uani 1 d . . H21 H 0.72473(11) -0.2974(3) 1.0045(3) 0.052 Uiso 1 calc R . C22 C 0.67766(14) -0.3392(4) 1.0623(4) 0.0570(13) Uani 1 d . . H22 H 0.68654(14) -0.3679(4) 1.1380(4) 0.068 Uiso 1 calc R . C23 C 0.64271(13) -0.3383(4) 1.0319(4) 0.0580(12) Uani 1 d . . H23 H 0.62718(13) -0.3648(4) 1.0877(4) 0.070 Uiso 1 calc R . C24 C 0.62920(11) -0.2990(3) 0.9202(4) 0.0462(10) Uani 1 d . . H24 H 0.60465(11) -0.3002(3) 0.8999(4) 0.055 Uiso 1 calc R . C25 C 0.66031(9) -0.2638(3) 0.5864(3) 0.0255(7) Uani 1 d . . C26 C 0.67697(9) -0.3646(3) 0.6110(3) 0.0298(7) Uani 1 d . . H26 H 0.67521(9) -0.3987(3) 0.6871(3) 0.036 Uiso 1 calc R . C27 C 0.69579(10) -0.4146(3) 0.5264(3) 0.0368(9) Uani 1 d . . H27 H 0.70742(10) -0.4820(3) 0.5448(3) 0.044 Uiso 1 calc R . C28 C 0.69786(10) -0.3671(3) 0.4143(3) 0.0395(9) Uani 1 d . . H28 H 0.71069(10) -0.4021(3) 0.3555(3) 0.047 Uiso 1 calc R . C29 C 0.68137(11) -0.2691(3) 0.3881(3) 0.0410(9) Uani 1 d . . H29 H 0.68268(11) -0.2366(3) 0.3110(3) 0.049 Uiso 1 calc R . C30 C 0.66273(10) -0.2174(3) 0.4744(3) 0.0319(8) Uani 1 d . . H30 H 0.65154(10) -0.1493(3) 0.4559(3) 0.038 Uiso 1 calc R . C31 C 0.59130(10) -0.2552(3) 0.6716(4) 0.0310(9) Uani 1 d . . C32 C 0.58598(11) -0.3585(3) 0.6204(4) 0.0488(11) Uani 1 d . . H32 H 0.60515(11) -0.3987(3) 0.5937(4) 0.059 Uiso 1 calc R . C33 C 0.55269(12) -0.4018(4) 0.6085(5) 0.068(2) Uani 1 d . . H33 H 0.54891(12) -0.4710(4) 0.5705(5) 0.082 Uiso 1 calc R . C34 C 0.52492(11) -0.3469(4) 0.6506(5) 0.0588(13) Uani 1 d . . H34 H 0.50234(11) -0.3796(4) 0.6449(5) 0.071 Uiso 1 calc R . C35 C 0.52964(10) -0.2459(3) 0.7004(4) 0.0458(10) Uani 1 d . . H35 H 0.51030(10) -0.2069(3) 0.7277(4) 0.055 Uiso 1 calc R . C36 C 0.56316(9) -0.1995(3) 0.7114(3) 0.0366(8) Uani 1 d . . H36 H 0.56651(9) -0.1290(3) 0.7465(3) 0.044 Uiso 1 calc R . C37 C 0.54183(9) -0.0164(6) 0.4373(3) 0.0482(12) Uani 1 d . . H37A H 0.52409(9) 0.0399(6) 0.4124(3) 0.058 Uiso 1 calc R . H37B H 0.52986(9) -0.0874(6) 0.4467(3) 0.058 Uiso 1 calc R . C38 C 0.56925(8) -0.0256(3) 0.3447(3) 0.0391(11) Uani 1 d . . H38 H 0.56944(8) 0.0435(3) 0.2964(3) 0.047 Uiso 1 calc R . C39 C 0.56374(9) -0.1215(4) 0.2617(3) 0.0420(10) Uani 1 d . . C40 C 0.56722(11) -0.2269(4) 0.3048(5) 0.0566(12) Uani 1 d . . H40 H 0.57466(11) -0.2379(4) 0.3875(5) 0.068 Uiso 1 calc R . C41 C 0.56037(13) -0.3162(5) 0.2330(6) 0.081(2) Uani 1 d . . H41 H 0.56291(13) -0.3882(5) 0.2651(6) 0.097 Uiso 1 calc R . C42 C 0.54949(14) -0.2997(7) 0.1110(7) 0.097(2) Uani 1 d . . H42 H 0.54414(14) -0.3609(7) 0.0600(7) 0.117 Uiso 1 calc R . C43 C 0.54659(13) -0.1965(7) 0.0657(5) 0.088(2) Uani 1 d . . H43 H 0.53984(13) -0.1856(7) -0.0174(5) 0.106 Uiso 1 calc R . C44 C 0.55346(10) -0.1064(5) 0.1407(4) 0.0577(12) Uani 1 d . . H44 H 0.55110(10) -0.0343(5) 0.1087(4) 0.069 Uiso 1 calc R . C45 C 0.61339(14) 0.3379(3) 0.5995(5) 0.0607(13) Uani 1 d . . H45A H 0.62165(14) 0.3901(3) 0.6637(5) 0.073 Uiso 1 calc R . H45B H 0.59238(14) 0.3689(3) 0.5541(5) 0.073 Uiso 1 calc R . C46 C 0.64195(12) 0.3152(3) 0.5159(5) 0.0572(12) Uani 1 d . . H46 H 0.66187(12) 0.3668(3) 0.5356(5) 0.069 Uiso 1 calc R . C47 C 0.63099(12) 0.3229(3) 0.3843(5) 0.0589(13) Uani 1 d . . C48 C 0.62860(15) 0.2325(4) 0.3130(5) 0.073(2) Uani 1 d . . H48 H 0.63401(15) 0.1626(4) 0.3471(5) 0.088 Uiso 1 calc R . C49 C 0.6183(2) 0.2410(6) 0.1899(5) 0.115(3) Uani 1 d . . H49 H 0.6166(2) 0.1774(6) 0.1406(5) 0.138 Uiso 1 calc R . C50 C 0.6107(2) 0.3428(7) 0.1413(6) 0.135(4) Uani 1 d . . H50 H 0.6042(2) 0.3499(7) 0.0574(6) 0.162 Uiso 1 calc R . C51 C 0.6124(2) 0.4303(6) 0.2110(8) 0.144(4) Uani 1 d . . H51 H 0.6052(2) 0.4993(6) 0.1779(8) 0.172 Uiso 1 calc R . C52 C 0.6243(2) 0.4235(4) 0.3319(7) 0.104(2) Uani 1 d . . H52 H 0.6280(2) 0.4884(4) 0.3784(7) 0.125 Uiso 1 calc R . C96 C 0.55122(13) 0.1347(5) -0.1974(4) 0.086(2) Uani 0.273(11) d PD 1 H96A H 0.54100(13) 0.1967(5) -0.2456(4) 0.103 Uiso 0.273(11) calc PR 1 H96B H 0.56891(13) 0.0982(5) -0.2439(4) 0.103 Uiso 0.273(11) calc PR 1 Cl1 Cl 0.5709(3) 0.1826(9) -0.0560(8) 0.112(4) Uani 0.273(11) d PD 1 Cl2 Cl 0.5189(2) 0.0430(5) -0.1656(8) 0.055(2) Uani 0.273(11) d PD 1 C96' C 0.55122(13) 0.1347(5) -0.1974(4) 0.086(2) Uani 0.727(11) d PD 2 H96C H 0.55916(9) 0.0903(7) -0.2646(5) 0.103 Uiso 0.727(11) calc PR 2 H96D H 0.55014(9) 0.2121(7) -0.2242(5) 0.103 Uiso 0.727(11) calc PR 2 Cl1' Cl 0.58033(9) 0.1242(7) -0.0815(5) 0.147(3) Uani 0.727(11) d PD 2 Cl2' Cl 0.5097(2) 0.0929(9) -0.1691(4) 0.157(3) Uani 0.727(11) d PD 2 C91 C 0.5000 -0.6465(14) 0.0000 0.260(11) Uani 1 d S . Cl8 Cl 0.4806(7) -0.5673(13) 0.1099(15) 0.476(13) Uani 0.50 d P . Cl9 Cl 0.5226(2) -0.5597(5) -0.0979(4) 0.130(2) Uani 0.50 d P . C98 C 0.5000 -0.7443(14) -0.5000 0.324(20) Uani 1 d S . Cl6 Cl 0.4701(3) -0.6860(12) -0.3808(13) 0.260(7) Uani 0.50 d P . Cl7 Cl 0.5088(3) -0.6687(7) -0.5915(10) 0.200(4) Uani 0.50 d P . 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 Pt1 0.02307(5) 0.02365(5) 0.03069(6) -0.00218(10) -0.00080(4) 0.00074(10) P1 0.0253(5) 0.0265(4) 0.0321(5) -0.0030(4) 0.0008(4) -0.0023(4) P2 0.0206(4) 0.0255(4) 0.0277(5) -0.0015(3) 0.0021(4) 0.0012(3) B1 0.031(2) 0.024(2) 0.037(2) 0.003(3) 0.0011(13) 0.002(3) B2 0.033(2) 0.029(2) 0.047(3) -0.007(2) -0.007(2) -0.001(2) O1 0.0261(11) 0.052(2) 0.0325(11) -0.0048(13) -0.0005(9) 0.0061(13) O2 0.0233(12) 0.052(2) 0.0301(12) 0.0021(10) -0.0024(10) 0.0025(10) O3 0.051(2) 0.0301(15) 0.071(2) 0.0031(13) 0.013(2) 0.0066(14) O4 0.043(2) 0.032(2) 0.072(2) 0.012(2) 0.005(2) 0.0035(14) C1 0.031(2) 0.027(2) 0.029(2) -0.0016(14) -0.0057(15) -0.0018(15) C2 0.039(3) 0.037(2) 0.044(3) -0.007(2) 0.006(2) -0.005(2) C3 0.057(3) 0.033(2) 0.046(2) -0.011(2) -0.001(2) 0.006(2) C4 0.056(3) 0.026(2) 0.051(2) 0.000(2) -0.019(2) -0.005(2) C5 0.039(2) 0.039(2) 0.059(3) 0.010(2) -0.002(2) -0.011(2) C6 0.036(2) 0.030(2) 0.046(2) 0.001(2) 0.000(2) 0.000(2) C7 0.027(2) 0.025(2) 0.032(2) -0.0030(12) 0.0016(14) 0.0021(12) C8 0.036(2) 0.037(2) 0.037(2) -0.002(2) 0.003(2) -0.006(2) C9 0.048(2) 0.038(2) 0.036(2) -0.001(2) -0.005(2) 0.003(2) C10 0.060(2) 0.039(2) 0.033(2) 0.002(3) 0.0112(15) 0.013(3) C11 0.043(2) 0.040(2) 0.054(3) 0.006(2) 0.020(2) 0.001(2) C12 0.033(2) 0.029(2) 0.046(2) -0.0060(14) 0.006(2) 0.0020(13) C13 0.0249(15) 0.020(3) 0.038(2) -0.0055(14) 0.0021(13) -0.0046(13) C14 0.031(2) 0.037(2) 0.039(2) 0.0003(15) -0.001(2) -0.002(2) C15 0.029(2) 0.040(2) 0.062(3) 0.010(2) -0.002(2) 0.003(2) C16 0.032(2) 0.036(2) 0.065(3) 0.003(2) 0.017(2) 0.003(2) C17 0.042(2) 0.036(2) 0.045(2) -0.002(2) 0.019(2) -0.006(2) C18 0.029(2) 0.031(2) 0.039(2) 0.0021(14) 0.005(2) -0.0073(15) C19 0.030(2) 0.024(2) 0.029(2) -0.0015(13) 0.006(2) 0.0019(15) C20 0.030(2) 0.034(2) 0.032(2) -0.005(2) -0.001(2) 0.008(2) C21 0.048(2) 0.043(2) 0.038(2) -0.007(2) -0.007(2) 0.016(2) C22 0.083(4) 0.057(3) 0.030(2) 0.010(2) 0.006(2) 0.035(3) C23 0.068(3) 0.062(3) 0.047(3) 0.023(2) 0.025(2) 0.017(2) C24 0.040(2) 0.049(2) 0.051(3) 0.011(2) 0.014(2) 0.006(2) C25 0.023(2) 0.025(2) 0.029(2) -0.0053(14) 0.0057(14) -0.0025(14) C26 0.038(2) 0.026(2) 0.026(2) -0.0002(13) 0.0061(15) 0.0037(15) C27 0.045(2) 0.029(2) 0.037(2) -0.0002(15) 0.009(2) 0.009(2) C28 0.047(2) 0.037(2) 0.036(2) -0.005(2) 0.015(2) 0.006(2) C29 0.054(3) 0.039(2) 0.032(2) 0.004(2) 0.012(2) 0.007(2) C30 0.035(2) 0.027(2) 0.034(2) 0.004(2) 0.002(2) 0.004(2) C31 0.020(2) 0.035(2) 0.038(2) -0.001(2) 0.001(2) 0.000(2) C32 0.032(2) 0.037(2) 0.077(3) -0.015(2) 0.007(2) -0.004(2) C33 0.038(3) 0.047(3) 0.119(5) -0.028(3) 0.005(3) -0.017(2) C34 0.027(2) 0.058(3) 0.091(4) -0.010(3) 0.003(2) -0.011(2) C35 0.025(2) 0.052(2) 0.061(3) 0.002(2) 0.004(2) 0.003(2) C36 0.033(2) 0.042(2) 0.035(2) 0.000(2) 0.005(2) -0.002(2) C37 0.026(2) 0.082(4) 0.036(2) -0.006(3) -0.0031(13) 0.013(3) C38 0.027(2) 0.055(3) 0.034(2) 0.006(2) -0.0060(14) 0.005(2) C39 0.020(2) 0.068(3) 0.039(2) -0.007(2) 0.005(2) 0.000(2) C40 0.031(2) 0.071(3) 0.069(3) -0.013(3) 0.010(2) -0.002(2) C41 0.043(3) 0.076(4) 0.126(5) -0.032(4) 0.021(3) -0.002(3) C42 0.040(3) 0.127(6) 0.127(6) -0.081(5) 0.020(3) -0.014(4) C43 0.044(3) 0.162(7) 0.059(3) -0.053(4) 0.002(3) 0.000(4) C44 0.033(2) 0.102(4) 0.038(2) -0.009(2) 0.002(2) 0.004(2) C45 0.077(4) 0.031(2) 0.073(3) -0.001(2) -0.001(3) 0.009(2) C46 0.054(3) 0.026(2) 0.091(4) 0.011(2) 0.004(3) -0.008(2) C47 0.057(3) 0.038(2) 0.086(4) 0.026(2) 0.030(3) 0.007(2) C48 0.088(4) 0.068(3) 0.065(3) 0.026(3) 0.023(3) 0.031(3) C49 0.173(7) 0.117(5) 0.058(4) 0.024(3) 0.023(4) 0.077(5) C50 0.170(7) 0.164(8) 0.081(5) 0.076(5) 0.067(5) 0.112(7) C51 0.188(9) 0.114(6) 0.140(7) 0.099(5) 0.083(6) 0.088(6) C52 0.124(6) 0.056(3) 0.135(6) 0.050(4) 0.030(5) 0.014(3) C96 0.076(4) 0.109(5) 0.076(4) -0.038(3) 0.023(3) -0.025(3) Cl1 0.078(6) 0.137(7) 0.124(6) -0.085(6) 0.028(4) -0.033(5) Cl2 0.046(3) 0.072(4) 0.049(3) -0.012(2) 0.020(2) -0.002(2) C96' 0.076(4) 0.109(5) 0.076(4) -0.038(3) 0.023(3) -0.025(3) Cl1' 0.066(2) 0.242(6) 0.130(3) 0.091(3) -0.010(2) 0.011(3) Cl2' 0.107(3) 0.277(7) 0.088(2) -0.031(4) 0.019(2) -0.110(4) C91 0.453(33) 0.130(13) 0.221(20) 0.000 0.184(22) 0.000 Cl8 0.825(39) 0.274(17) 0.335(18) -0.069(12) 0.081(21) -0.135(20) Cl9 0.230(6) 0.084(3) 0.079(3) -0.019(2) 0.028(3) -0.041(4) C98 0.763(63) 0.099(11) 0.108(12) 0.000 0.036(23) 0.000 Cl6 0.163(8) 0.331(14) 0.276(12) 0.092(10) -0.052(8) -0.055(8) Cl7 0.255(12) 0.145(5) 0.188(7) -0.019(5) -0.047(8) 0.061(7) _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 Pt1 B2 2.054(4) . ? Pt1 B1 2.070(3) . ? Pt1 P1 2.3456(9) . ? Pt1 P2 2.3505(9) . ? P1 C7 1.830(3) . ? P1 C13 1.831(3) . ? P1 C1 1.835(3) . ? P2 C25 1.830(3) . ? P2 C19 1.833(4) . ? P2 C31 1.836(4) . ? B1 O2 1.383(4) . ? B1 O1 1.389(4) . ? B2 O4 1.375(6) . ? B2 O3 1.378(5) . ? O1 C37 1.433(4) . ? O2 C38 1.452(4) . ? O3 C45 1.434(5) . ? O4 C46 1.445(5) . ? C1 C2 1.379(5) . ? C1 C6 1.380(5) . ? C2 C3 1.420(6) . ? C3 C4 1.361(6) . ? C4 C5 1.367(6) . ? C5 C6 1.394(5) . ? C7 C8 1.391(5) . ? C7 C12 1.395(4) . ? C8 C9 1.380(5) . ? C9 C10 1.356(6) . ? C10 C11 1.387(6) . ? C11 C12 1.387(5) . ? C13 C14 1.389(4) . ? C13 C18 1.405(5) . ? C14 C15 1.376(5) . ? C15 C16 1.385(6) . ? C16 C17 1.383(5) . ? C17 C18 1.374(5) . ? C19 C24 1.383(5) . ? C19 C20 1.394(5) . ? C20 C21 1.378(5) . ? C21 C22 1.377(6) . ? C22 C23 1.355(6) . ? C23 C24 1.393(5) . ? C25 C30 1.378(5) . ? C25 C26 1.402(5) . ? C26 C27 1.373(5) . ? C27 C28 1.383(5) . ? C28 C29 1.372(5) . ? C29 C30 1.392(5) . ? C31 C36 1.376(5) . ? C31 C32 1.391(5) . ? C32 C33 1.377(6) . ? C33 C34 1.371(6) . ? C34 C35 1.357(6) . ? C35 C36 1.400(5) . ? C37 C38 1.532(5) . ? C38 C39 1.495(5) . ? C39 C40 1.375(6) . ? C39 C44 1.385(5) . ? C40 C41 1.364(7) . ? C41 C42 1.402(9) . ? C42 C43 1.358(9) . ? C43 C44 1.391(7) . ? C45 C46 1.516(7) . ? C46 C47 1.494(7) . ? C47 C48 1.357(7) . ? C47 C52 1.374(6) . ? C48 C49 1.398(7) . ? C49 C50 1.377(9) . ? C50 C51 1.318(11) . ? C51 C52 1.389(10) . ? C96 Cl2 1.725(8) . ? C96 Cl1 1.788(7) . ? C96' Cl1' 1.642(6) . ? C96' Cl2' 1.722(6) . ? C91 Cl8 1.77(2) . ? C91 Cl8 1.77(2) 2_655 ? C91 Cl9 1.790(12) . ? C91 Cl9 1.790(12) 2_655 ? Cl8 Cl9 0.20(2) 2_655 ? Cl9 Cl8 0.20(2) 2_655 ? C98 Cl7 1.432(13) . ? C98 Cl7 1.432(13) 2_654 ? C98 Cl6 1.95(2) . ? C98 Cl6 1.95(2) 2_654 ? Cl6 Cl7 0.912(13) 2_654 ? Cl7 Cl6 0.912(13) 2_654 ? Cl7 Cl7 2.19(2) 2_654 ? 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 B2 Pt1 B1 75.5(2) . . ? B2 Pt1 P1 89.63(12) . . ? B1 Pt1 P1 164.7(2) . . ? B2 Pt1 P2 166.16(13) . . ? B1 Pt1 P2 91.7(2) . . ? P1 Pt1 P2 102.75(3) . . ? C7 P1 C13 106.04(15) . . ? C7 P1 C1 99.56(15) . . ? C13 P1 C1 103.6(2) . . ? C7 P1 Pt1 120.49(11) . . ? C13 P1 Pt1 108.93(11) . . ? C1 P1 Pt1 116.51(11) . . ? C25 P2 C19 102.3(2) . . ? C25 P2 C31 103.6(2) . . ? C19 P2 C31 101.6(2) . . ? C25 P2 Pt1 113.41(12) . . ? C19 P2 Pt1 120.18(11) . . ? C31 P2 Pt1 113.70(12) . . ? O2 B1 O1 110.5(3) . . ? O2 B1 Pt1 124.3(2) . . ? O1 B1 Pt1 125.2(2) . . ? O4 B2 O3 110.2(3) . . ? O4 B2 Pt1 122.4(3) . . ? O3 B2 Pt1 127.3(3) . . ? B1 O1 C37 108.5(3) . . ? B1 O2 C38 109.4(2) . . ? B2 O3 C45 109.7(4) . . ? B2 O4 C46 109.4(3) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 P1 118.1(3) . . ? C6 C1 P1 122.9(3) . . ? C1 C2 C3 119.6(4) . . ? C4 C3 C2 120.3(4) . . ? C3 C4 C5 120.0(3) . . ? C4 C5 C6 120.2(4) . . ? C1 C6 C5 120.8(4) . . ? C8 C7 C12 117.8(3) . . ? C8 C7 P1 122.6(3) . . ? C12 C7 P1 119.6(3) . . ? C9 C8 C7 121.2(4) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 120.3(3) . . ? C10 C11 C12 119.7(4) . . ? C11 C12 C7 120.7(3) . . ? C14 C13 C18 117.9(3) . . ? C14 C13 P1 125.3(3) . . ? C18 C13 P1 116.6(2) . . ? C15 C14 C13 120.6(3) . . ? C14 C15 C16 120.8(4) . . ? C17 C16 C15 119.4(4) . . ? C18 C17 C16 120.0(4) . . ? C17 C18 C13 121.2(3) . . ? C24 C19 C20 117.8(4) . . ? C24 C19 P2 122.2(3) . . ? C20 C19 P2 119.7(3) . . ? C21 C20 C19 121.3(4) . . ? C22 C21 C20 119.9(4) . . ? C23 C22 C21 119.7(4) . . ? C22 C23 C24 121.1(4) . . ? C19 C24 C23 120.2(4) . . ? C30 C25 C26 118.3(3) . . ? C30 C25 P2 119.3(3) . . ? C26 C25 P2 122.4(3) . . ? C27 C26 C25 120.8(3) . . ? C26 C27 C28 120.1(3) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 120.0(3) . . ? C25 C30 C29 120.8(3) . . ? C36 C31 C32 119.0(4) . . ? C36 C31 P2 118.7(3) . . ? C32 C31 P2 122.2(3) . . ? C33 C32 C31 119.4(4) . . ? C34 C33 C32 121.2(4) . . ? C35 C34 C33 120.1(4) . . ? C34 C35 C36 119.6(4) . . ? C31 C36 C35 120.6(4) . . ? O1 C37 C38 105.0(3) . . ? O2 C38 C39 111.3(3) . . ? O2 C38 C37 103.1(3) . . ? C39 C38 C37 113.7(4) . . ? C40 C39 C44 118.4(4) . . ? C40 C39 C38 120.8(4) . . ? C44 C39 C38 120.8(4) . . ? C41 C40 C39 122.3(5) . . ? C40 C41 C42 118.7(6) . . ? C43 C42 C41 120.1(6) . . ? C42 C43 C44 120.3(6) . . ? C39 C44 C43 120.2(5) . . ? O3 C45 C46 104.8(3) . . ? O4 C46 C47 109.9(4) . . ? O4 C46 C45 104.3(3) . . ? C47 C46 C45 115.4(4) . . ? C48 C47 C52 118.4(5) . . ? C48 C47 C46 121.5(4) . . ? C52 C47 C46 120.0(5) . . ? C47 C48 C49 120.9(5) . . ? C50 C49 C48 119.1(7) . . ? C51 C50 C49 120.0(7) . . ? C50 C51 C52 121.2(6) . . ? C47 C52 C51 120.0(6) . . ? Cl2 C96 Cl1 106.9(5) . . ? Cl1' C96' Cl2' 114.4(4) . . ? Cl8 C91 Cl8 113.7(15) . 2_655 ? Cl8 C91 Cl9 110.3(10) . . ? Cl8 C91 Cl9 6.3(8) 2_655 . ? Cl8 C91 Cl9 6.3(8) . 2_655 ? Cl8 C91 Cl9 110.3(10) 2_655 2_655 ? Cl9 C91 Cl9 107.5(10) . 2_655 ? Cl9 Cl8 C91 93.5(63) 2_655 . ? Cl8 Cl9 C91 80.2(66) 2_655 . ? Cl7 C98 Cl7 99.9(14) . 2_654 ? Cl7 C98 Cl6 115.6(12) . . ? Cl7 C98 Cl6 25.9(4) 2_654 . ? Cl7 C98 Cl6 25.9(4) . 2_654 ? Cl7 C98 Cl6 115.6(12) 2_654 2_654 ? Cl6 C98 Cl6 137.3(13) . 2_654 ? Cl7 Cl6 C98 43.3(12) 2_654 . ? Cl6 Cl7 C98 110.8(15) 2_654 . ? Cl6 Cl7 Cl7 131.2(17) 2_654 2_654 ? C98 Cl7 Cl7 40.0(7) . 2_654 ? _refine_diff_density_max 0.820 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.060 #=END _publ_section_references ; Sheldrick, G.M. (1996). SADABS (Siemens Area Detector Absorption Program). University of G\"ottingen, Germany. Siemens (1995a). SHELXTL. Version 5.03 Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Siemens (1995b). SMART and SAINT Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Siemens (1995c). XSCANS. Version 2.1 Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ;