Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_jbb16 _database_code_depnum_ccdc_archive 'CCDC 246570' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H38 B16 N2' _chemical_formula_weight 407.42 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5010(3) _cell_length_b 10.7708(3) _cell_length_c 23.1683(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.6910(12) _cell_angle_gamma 90.00 _cell_volume 2566.07(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9911 _exptl_absorpt_correction_T_max 0.9990 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12545 _diffrn_reflns_av_R_equivalents 0.0933 _diffrn_reflns_av_sigmaI/netI 0.1317 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4921 _reflns_number_gt 2482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4921 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1527 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1731 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4358(3) 0.2977(2) 0.05944(11) 0.0352(6) Uani 1 1 d . . . C2 C 0.3973(3) 0.2085(3) 0.01776(12) 0.0478(8) Uani 1 1 d . . . H21 H 0.3084 0.1845 0.0082 0.057 Uiso 1 1 calc R . . C3 C 0.4858(4) 0.1522(3) -0.01085(13) 0.0561(9) Uani 1 1 d . . . H31 H 0.4567 0.0930 -0.0410 0.067 Uiso 1 1 calc R . . C4 C 0.6135(4) 0.1815(3) 0.00401(13) 0.0569(9) Uani 1 1 d . . . H41 H 0.6738 0.1392 -0.0145 0.068 Uiso 1 1 calc R . . C5 C 0.6593(3) 0.2744(3) 0.04692(12) 0.0438(8) Uani 1 1 d . . . C6 C 0.7917(3) 0.3066(3) 0.06303(14) 0.0601(9) Uani 1 1 d . . . H61 H 0.8528 0.2649 0.0448 0.072 Uiso 1 1 calc R . . C7 C 0.8343(3) 0.3952(4) 0.10371(15) 0.0621(10) Uani 1 1 d . . . H71 H 0.9247 0.4127 0.1145 0.075 Uiso 1 1 calc R . . C8 C 0.7457(3) 0.4620(3) 0.13025(12) 0.0473(8) Uani 1 1 d . . . H81 H 0.7754 0.5260 0.1579 0.057 Uiso 1 1 calc R . . C9 C 0.6169(2) 0.4332(2) 0.11566(11) 0.0338(6) Uani 1 1 d . . . C10 C 0.5680(2) 0.3376(2) 0.07478(11) 0.0342(6) Uani 1 1 d . . . N1 N 0.3444(2) 0.3508(2) 0.09254(9) 0.0374(6) Uani 1 1 d . . . C11 C 0.3147(3) 0.2599(3) 0.13621(13) 0.0527(8) Uani 1 1 d . . . H11A H 0.2737 0.1863 0.1156 0.079 Uiso 1 1 calc R . . H11B H 0.2554 0.2978 0.1588 0.079 Uiso 1 1 calc R . . H11C H 0.3955 0.2358 0.1631 0.079 Uiso 1 1 calc R . . C12 C 0.2235(3) 0.3980(3) 0.05494(14) 0.0620(9) Uani 1 1 d . . . H12A H 0.2453 0.4528 0.0246 0.093 Uiso 1 1 calc R . . H12B H 0.1736 0.4445 0.0792 0.093 Uiso 1 1 calc R . . H12C H 0.1714 0.3281 0.0361 0.093 Uiso 1 1 calc R . . N2 N 0.5218(2) 0.50557(19) 0.13993(9) 0.0322(5) Uani 1 1 d . . . H29 H 0.432(3) 0.452(3) 0.1263(13) 0.071(9) Uiso 1 1 d . . . C13 C 0.5514(3) 0.5174(3) 0.20492(11) 0.0500(8) Uani 1 1 d . . . H13A H 0.5666 0.4348 0.2227 0.075 Uiso 1 1 calc R . . H13B H 0.4778 0.5566 0.2179 0.075 Uiso 1 1 calc R . . H13C H 0.6294 0.5685 0.2172 0.075 Uiso 1 1 calc R . . C14 C 0.4997(3) 0.6291(2) 0.11096(14) 0.0498(8) Uani 1 1 d . . . H14A H 0.5787 0.6794 0.1217 0.075 Uiso 1 1 calc R . . H14B H 0.4276 0.6711 0.1240 0.075 Uiso 1 1 calc R . . H14C H 0.4781 0.6182 0.0681 0.075 Uiso 1 1 calc R . . B1 B 0.0288(3) 1.0190(3) 0.11202(14) 0.0387(8) Uani 1 1 d . . . H1 H 0.038(2) 1.118(2) 0.0965(9) 0.030(6) Uiso 1 1 d . . . B2 B -0.1189(3) 0.9343(3) 0.10012(14) 0.0390(8) Uani 1 1 d . . . H2 H -0.207(2) 0.974(2) 0.0713(10) 0.034(6) Uiso 1 1 d . . . B3 B 0.0102(3) 0.8783(3) 0.06968(15) 0.0456(9) Uani 1 1 d . . . H3 H -0.005(2) 0.868(3) 0.0202(13) 0.062(8) Uiso 1 1 d . . . B4 B 0.1675(3) 0.9207(3) 0.11003(15) 0.0449(9) Uani 1 1 d . . . H4 H 0.240(2) 0.956(2) 0.0862(10) 0.038(6) Uiso 1 1 d . . . B5 B -0.0429(3) 0.9905(3) 0.17120(14) 0.0357(8) Uani 1 1 d . . . B6 B -0.1290(3) 0.8547(3) 0.16431(14) 0.0368(8) Uani 1 1 d . . . H67 H -0.063(3) 0.751(3) 0.1613(13) 0.066(9) Uiso 1 1 d . . . B7 B -0.0789(3) 0.7729(3) 0.10483(15) 0.0424(8) Uani 1 1 d . . . H7 H -0.136(2) 0.698(2) 0.0819(10) 0.036(7) Uiso 1 1 d . . . B8 B 0.1129(3) 0.7645(3) 0.10900(17) 0.0459(9) Uani 1 1 d . . . H8 H 0.146(2) 0.688(3) 0.0852(11) 0.050(7) Uiso 1 1 d . . . H89 H 0.131(2) 0.738(3) 0.1630(12) 0.056(8) Uiso 1 1 d . . . B9 B 0.2112(3) 0.8322(3) 0.17167(17) 0.0492(9) Uani 1 1 d . . . H9 H 0.313(2) 0.800(2) 0.1947(11) 0.053(8) Uiso 1 1 d . . . H910 H 0.147(3) 0.883(3) 0.2081(12) 0.062(8) Uiso 1 1 d . . . B10 B 0.1399(3) 0.9799(3) 0.17807(15) 0.0407(8) Uani 1 1 d . . . H10 H 0.201(2) 1.058(3) 0.2042(11) 0.051(7) Uiso 1 1 d . . . B1' B -0.0900(3) 0.9285(3) 0.23317(14) 0.0349(7) Uani 1 1 d . . . H1' H -0.017(2) 0.902(2) 0.2715(11) 0.043(7) Uiso 1 1 d . . . B2' B -0.2363(3) 0.9972(3) 0.24457(15) 0.0380(8) Uani 1 1 d . . . H2' H -0.249(2) 1.016(2) 0.2912(10) 0.031(6) Uiso 1 1 d . . . B4' B -0.2396(3) 0.8470(3) 0.20847(14) 0.0435(8) Uani 1 1 d . . . H4' H -0.255(2) 0.760(2) 0.2322(11) 0.047(7) Uiso 1 1 d . . . B5' B -0.3580(3) 0.9500(4) 0.18542(15) 0.0480(9) Uani 1 1 d . . . H56' H -0.343(2) 1.028(2) 0.1463(11) 0.043(7) Uiso 1 1 d . . . H5' H -0.469(2) 0.931(3) 0.1816(11) 0.056(8) Uiso 1 1 d . . . B6' B -0.2996(3) 1.0990(3) 0.18965(15) 0.0428(8) Uani 1 1 d . . . H6' H -0.354(2) 1.185(3) 0.1875(11) 0.055(8) Uiso 1 1 d . . . H67' H -0.197(3) 1.125(3) 0.1697(12) 0.061(8) Uiso 1 1 d . . . B7' B -0.1228(3) 1.0906(3) 0.21406(14) 0.0359(8) Uani 1 1 d . . . H7' H -0.073(2) 1.169(3) 0.2381(11) 0.052(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0497(16) 0.0253(15) 0.0303(15) 0.0047(12) 0.0074(13) 0.0012(13) C2 0.073(2) 0.0340(17) 0.0371(17) -0.0024(14) 0.0121(15) -0.0006(15) C3 0.093(3) 0.0354(18) 0.0420(19) 0.0004(15) 0.0181(18) 0.0048(18) C4 0.101(3) 0.0399(19) 0.0367(19) 0.0089(15) 0.0297(19) 0.0344(19) C5 0.0531(18) 0.0425(18) 0.0395(18) 0.0183(15) 0.0178(14) 0.0217(14) C6 0.062(2) 0.078(3) 0.046(2) 0.0232(19) 0.0242(17) 0.0331(19) C7 0.0337(16) 0.099(3) 0.055(2) 0.020(2) 0.0105(15) 0.0114(18) C8 0.0386(16) 0.062(2) 0.0402(18) 0.0122(15) 0.0057(13) -0.0028(14) C9 0.0339(14) 0.0350(16) 0.0329(15) 0.0088(13) 0.0074(12) 0.0026(12) C10 0.0461(16) 0.0302(15) 0.0268(14) 0.0101(12) 0.0082(12) 0.0114(13) N1 0.0402(12) 0.0346(13) 0.0374(13) -0.0038(11) 0.0074(10) -0.0047(10) C11 0.0575(18) 0.0466(19) 0.059(2) -0.0047(16) 0.0232(16) -0.0147(15) C12 0.0478(17) 0.065(2) 0.064(2) -0.0164(18) -0.0106(16) 0.0126(16) N2 0.0349(12) 0.0287(12) 0.0326(13) 0.0004(10) 0.0054(10) -0.0040(10) C13 0.0475(17) 0.070(2) 0.0318(17) -0.0093(15) 0.0065(13) -0.0144(15) C14 0.0547(18) 0.0308(17) 0.064(2) 0.0034(15) 0.0109(15) 0.0034(13) B1 0.0469(19) 0.0359(19) 0.0333(18) 0.0009(15) 0.0078(14) 0.0007(15) B2 0.0435(18) 0.0347(18) 0.0354(19) 0.0004(15) 0.0001(15) 0.0002(15) B3 0.062(2) 0.047(2) 0.0312(19) -0.0056(16) 0.0161(16) -0.0031(17) B4 0.053(2) 0.040(2) 0.047(2) -0.0050(17) 0.0228(17) -0.0032(16) B5 0.0333(16) 0.0335(18) 0.0387(19) -0.0062(15) 0.0038(14) -0.0052(14) B6 0.0364(17) 0.0337(19) 0.0368(18) -0.0057(15) -0.0010(14) -0.0001(14) B7 0.055(2) 0.038(2) 0.034(2) -0.0050(16) 0.0067(16) -0.0034(16) B8 0.059(2) 0.0335(19) 0.051(2) -0.0054(17) 0.0249(18) 0.0040(16) B9 0.044(2) 0.043(2) 0.060(2) -0.0057(18) 0.0116(18) 0.0047(17) B10 0.0399(17) 0.041(2) 0.043(2) 0.0002(17) 0.0110(15) 0.0002(15) B1' 0.0424(17) 0.0258(17) 0.0331(18) 0.0001(14) -0.0008(14) 0.0002(14) B2' 0.0400(17) 0.043(2) 0.0330(19) 0.0036(15) 0.0116(14) -0.0004(15) B4' 0.057(2) 0.037(2) 0.0367(19) 0.0007(16) 0.0104(16) -0.0162(16) B5' 0.0429(19) 0.061(2) 0.042(2) -0.0065(19) 0.0141(16) -0.0109(17) B6' 0.0436(19) 0.050(2) 0.0360(19) -0.0001(17) 0.0103(15) 0.0105(17) B7' 0.0430(17) 0.0299(18) 0.0346(19) -0.0028(15) 0.0072(15) -0.0019(14) _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 C1 C2 1.364(4) . ? C1 C10 1.428(4) . ? C1 N1 1.460(3) . ? C2 C3 1.386(4) . ? C2 H21 0.9500 . ? C3 C4 1.352(4) . ? C3 H31 0.9500 . ? C4 C5 1.424(4) . ? C4 H41 0.9500 . ? C5 C6 1.408(4) . ? C5 C10 1.431(3) . ? C6 C7 1.352(5) . ? C6 H61 0.9500 . ? C7 C8 1.412(4) . ? C7 H71 0.9500 . ? C8 C9 1.362(3) . ? C8 H81 0.9500 . ? C9 C10 1.422(4) . ? C9 N2 1.466(3) . ? N1 C12 1.477(3) . ? N1 C11 1.485(3) . ? N2 C13 1.480(3) . ? N2 C14 1.487(3) . ? N2 H29 1.10(3) . ? B1 B5 1.720(4) . ? B1 B2 1.772(4) . ? B1 B10 1.777(5) . ? B1 B3 1.794(5) . ? B1 B4 1.809(5) . ? B1 H1 1.14(2) . ? B2 B6 1.738(5) . ? B2 B3 1.757(5) . ? B2 B5 1.784(4) . ? B2 B7 1.786(5) . ? B2 H2 1.11(2) . ? B3 B8 1.760(5) . ? B3 B7 1.771(5) . ? B3 B4 1.785(5) . ? B3 H3 1.13(3) . ? B4 B9 1.701(5) . ? B4 B8 1.776(5) . ? B4 B10 1.778(5) . ? B4 H4 1.10(2) . ? B5 B6 1.710(4) . ? B5 B1' 1.743(4) . ? B5 B7' 1.786(4) . ? B5 B10 1.897(4) . ? B6 B4' 1.699(4) . ? B6 B1' 1.755(4) . ? B6 B7 1.802(5) . ? B6 H67 1.32(3) . ? B7 B8 1.998(5) . ? B7 H67 1.31(3) . ? B7 H7 1.08(2) . ? B8 B9 1.760(5) . ? B8 H8 1.08(3) . ? B8 H89 1.26(3) . ? B9 B10 1.778(5) . ? B9 H89 1.31(3) . ? B9 H9 1.15(3) . ? B9 H910 1.30(3) . ? B10 H910 1.25(3) . ? B10 H10 1.15(3) . ? B1' B2' 1.772(4) . ? B1' B4' 1.790(4) . ? B1' B7' 1.817(4) . ? B1' H1' 1.08(2) . ? B2' B6' 1.709(5) . ? B2' B5' 1.749(5) . ? B2' B7' 1.809(4) . ? B2' B4' 1.819(5) . ? B2' H2' 1.13(2) . ? B4' B5' 1.671(5) . ? B4' H4' 1.11(3) . ? B5' B6' 1.713(5) . ? B5' H56' 1.27(2) . ? B5' H5' 1.17(2) . ? B6' B7' 1.830(4) . ? B6' H56' 1.27(3) . ? B6' H6' 1.09(3) . ? B6' H67' 1.28(3) . ? B7' H67' 1.22(3) . ? B7' H7' 1.08(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 C2 C1 C10 121.4(3) . . ? C2 C1 N1 121.0(2) . . ? C10 C1 N1 117.4(2) . . ? C1 C2 C3 121.0(3) . . ? C1 C2 H21 119.5 . . ? C3 C2 H21 119.5 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H31 119.9 . . ? C2 C3 H31 119.9 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H41 119.4 . . ? C5 C4 H41 119.4 . . ? C6 C5 C4 122.3(3) . . ? C6 C5 C10 118.6(3) . . ? C4 C5 C10 119.2(3) . . ? C7 C6 C5 121.9(3) . . ? C7 C6 H61 119.0 . . ? C5 C6 H61 119.0 . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H71 119.7 . . ? C8 C7 H71 119.7 . . ? C9 C8 C7 119.0(3) . . ? C9 C8 H81 120.5 . . ? C7 C8 H81 120.5 . . ? C8 C9 C10 122.4(3) . . ? C8 C9 N2 120.2(3) . . ? C10 C9 N2 117.3(2) . . ? C9 C10 C1 125.8(2) . . ? C9 C10 C5 117.4(2) . . ? C1 C10 C5 116.8(3) . . ? C1 N1 C12 113.7(2) . . ? C1 N1 C11 110.5(2) . . ? C12 N1 C11 110.8(2) . . ? C9 N2 C13 114.6(2) . . ? C9 N2 C14 111.0(2) . . ? C13 N2 C14 111.3(2) . . ? C9 N2 H29 103.1(15) . . ? C13 N2 H29 109.2(15) . . ? C14 N2 H29 106.9(16) . . ? B5 B1 B2 61.43(17) . . ? B5 B1 B10 65.68(19) . . ? B2 B1 B10 114.4(2) . . ? B5 B1 B3 105.6(2) . . ? B2 B1 B3 59.03(18) . . ? B10 B1 B3 104.5(2) . . ? B5 B1 B4 113.6(2) . . ? B2 B1 B4 112.3(2) . . ? B10 B1 B4 59.45(18) . . ? B3 B1 B4 59.40(19) . . ? B5 B1 H1 119.9(11) . . ? B2 B1 H1 124.3(11) . . ? B10 B1 H1 114.2(11) . . ? B3 B1 H1 128.9(11) . . ? B4 B1 H1 114.8(11) . . ? B6 B2 B3 111.1(2) . . ? B6 B2 B1 108.9(2) . . ? B3 B2 B1 61.10(18) . . ? B6 B2 B5 58.06(17) . . ? B3 B2 B5 104.4(2) . . ? B1 B2 B5 57.85(17) . . ? B6 B2 B7 61.47(19) . . ? B3 B2 B7 59.96(19) . . ? B1 B2 B7 107.7(2) . . ? B5 B2 B7 102.6(2) . . ? B6 B2 H2 121.0(11) . . ? B3 B2 H2 120.6(12) . . ? B1 B2 H2 119.5(12) . . ? B5 B2 H2 125.8(12) . . ? B7 B2 H2 124.6(12) . . ? B2 B3 B8 118.2(2) . . ? B2 B3 B7 60.84(18) . . ? B8 B3 B7 68.9(2) . . ? B2 B3 B4 114.2(2) . . ? B8 B3 B4 60.14(19) . . ? B7 B3 B4 116.3(3) . . ? B2 B3 B1 59.87(18) . . ? B8 B3 B1 108.5(2) . . ? B7 B3 B1 107.4(2) . . ? B4 B3 B1 60.73(18) . . ? B2 B3 H3 118.5(14) . . ? B8 B3 H3 113.7(14) . . ? B7 B3 H3 115.0(14) . . ? B4 B3 H3 118.9(13) . . ? B1 B3 H3 128.0(15) . . ? B9 B4 B8 60.7(2) . . ? B9 B4 B10 61.4(2) . . ? B8 B4 B10 104.0(2) . . ? B9 B4 B3 111.1(2) . . ? B8 B4 B3 59.2(2) . . ? B10 B4 B3 104.8(2) . . ? B9 B4 B1 112.8(2) . . ? B8 B4 B1 107.1(2) . . ? B10 B4 B1 59.37(18) . . ? B3 B4 B1 59.88(19) . . ? B9 B4 H4 121.4(12) . . ? B8 B4 H4 125.2(13) . . ? B10 B4 H4 125.3(13) . . ? B3 B4 H4 119.3(12) . . ? B1 B4 H4 117.2(13) . . ? B6 B5 B1 112.7(2) . . ? B6 B5 B1' 61.09(18) . . ? B1 B5 B1' 165.4(3) . . ? B6 B5 B2 59.62(18) . . ? B1 B5 B2 60.72(18) . . ? B1' B5 B2 118.8(2) . . ? B6 B5 B7' 105.6(2) . . ? B1 B5 B7' 131.8(2) . . ? B1' B5 B7' 61.95(17) . . ? B2 B5 B7' 123.0(2) . . ? B6 B5 B10 117.6(2) . . ? B1 B5 B10 58.59(17) . . ? B1' B5 B10 111.0(2) . . ? B2 B5 B10 108.2(2) . . ? B7' B5 B10 124.8(2) . . ? B4' B6 B5 113.5(2) . . ? B4' B6 B2 135.0(2) . . ? B5 B6 B2 62.32(18) . . ? B4' B6 B1' 62.40(18) . . ? B5 B6 B1' 60.39(18) . . ? B2 B6 B1' 120.7(2) . . ? B4' B6 B7 141.1(2) . . ? B5 B6 B7 105.0(2) . . ? B2 B6 B7 60.58(18) . . ? B1' B6 B7 150.0(2) . . ? B4' B6 H67 114.8(12) . . ? B5 B6 H67 117.1(12) . . ? B2 B6 H67 104.3(13) . . ? B1' B6 H67 113.8(13) . . ? B7 B6 H67 46.3(13) . . ? B3 B7 B2 59.19(19) . . ? B3 B7 B6 107.6(2) . . ? B2 B7 B6 57.95(18) . . ? B3 B7 B8 55.27(18) . . ? B2 B7 B8 105.6(2) . . ? B6 B7 B8 115.6(2) . . ? B3 B7 H67 127.2(12) . . ? B2 B7 H67 102.4(13) . . ? B6 B7 H67 47.0(12) . . ? B8 B7 H67 91.3(12) . . ? B3 B7 H7 123.0(13) . . ? B2 B7 H7 126.8(12) . . ? B6 B7 H7 121.7(12) . . ? B8 B7 H7 116.2(12) . . ? H67 B7 H7 107.7(17) . . ? B9 B8 B3 109.5(2) . . ? B9 B8 B4 57.5(2) . . ? B3 B8 B4 60.64(19) . . ? B9 B8 B7 116.0(2) . . ? B3 B8 B7 55.79(18) . . ? B4 B8 B7 106.1(2) . . ? B9 B8 H8 122.5(13) . . ? B3 B8 H8 119.3(14) . . ? B4 B8 H8 125.9(14) . . ? B7 B8 H8 115.8(13) . . ? B9 B8 H89 47.9(12) . . ? B3 B8 H89 128.9(12) . . ? B4 B8 H89 102.7(13) . . ? B7 B8 H89 90.4(12) . . ? H8 B8 H89 109.4(18) . . ? B4 B9 B8 61.7(2) . . ? B4 B9 B10 61.4(2) . . ? B8 B9 B10 104.6(2) . . ? B4 B9 H89 104.6(13) . . ? B8 B9 H89 45.7(12) . . ? B10 B9 H89 116.1(11) . . ? B4 B9 H9 128.8(13) . . ? B8 B9 H9 126.5(13) . . ? B10 B9 H9 126.8(13) . . ? H89 B9 H9 110.2(18) . . ? B4 B9 H910 102.9(13) . . ? B8 B9 H910 114.4(12) . . ? B10 B9 H910 44.7(13) . . ? H89 B9 H910 91.3(17) . . ? H9 B9 H910 112.4(17) . . ? B1 B10 B4 61.18(19) . . ? B1 B10 B9 110.7(2) . . ? B4 B10 B9 57.17(19) . . ? B1 B10 B5 55.72(17) . . ? B4 B10 B5 106.9(2) . . ? B9 B10 B5 118.9(2) . . ? B1 B10 H910 129.1(12) . . ? B4 B10 H910 101.0(13) . . ? B9 B10 H910 47.1(13) . . ? B5 B10 H910 92.3(12) . . ? B1 B10 H10 118.6(13) . . ? B4 B10 H10 123.5(12) . . ? B9 B10 H10 119.7(12) . . ? B5 B10 H10 116.7(12) . . ? H910 B10 H10 110.8(18) . . ? B5 B1' B6 58.52(18) . . ? B5 B1' B2' 111.2(2) . . ? B6 B1' B2' 106.0(2) . . ? B5 B1' B4' 107.6(2) . . ? B6 B1' B4' 57.25(17) . . ? B2' B1' B4' 61.40(18) . . ? B5 B1' B7' 60.19(17) . . ? B6 B1' B7' 102.5(2) . . ? B2' B1' B7' 60.51(17) . . ? B4' B1' B7' 106.4(2) . . ? B5 B1' H1' 120.2(12) . . ? B6 B1' H1' 128.4(13) . . ? B2' B1' H1' 118.4(12) . . ? B4' B1' H1' 124.2(13) . . ? B7' B1' H1' 121.1(13) . . ? B6' B2' B5' 59.4(2) . . ? B6' B2' B1' 112.0(2) . . ? B5' B2' B1' 106.2(2) . . ? B6' B2' B7' 62.62(18) . . ? B5' B2' B7' 106.9(2) . . ? B1' B2' B7' 60.96(17) . . ? B6' B2' B4' 105.1(2) . . ? B5' B2' B4' 55.80(19) . . ? B1' B2' B4' 59.77(18) . . ? B7' B2' B4' 105.5(2) . . ? B6' B2' H2' 119.3(11) . . ? B5' B2' H2' 126.0(11) . . ? B1' B2' H2' 119.5(11) . . ? B7' B2' H2' 119.3(11) . . ? B4' B2' H2' 127.1(11) . . ? B5' B4' B6 109.3(2) . . ? B5' B4' B1' 108.9(2) . . ? B6 B4' B1' 60.35(17) . . ? B5' B4' B2' 60.00(19) . . ? B6 B4' B2' 106.4(2) . . ? B1' B4' B2' 58.83(17) . . ? B5' B4' H4' 123.1(13) . . ? B6 B4' H4' 121.4(13) . . ? B1' B4' H4' 117.3(13) . . ? B2' B4' H4' 120.9(13) . . ? B4' B5' B6' 111.7(2) . . ? B4' B5' B2' 64.2(2) . . ? B6' B5' B2' 59.12(19) . . ? B4' B5' H56' 118.4(10) . . ? B6' B5' H56' 47.4(12) . . ? B2' B5' H56' 100.8(11) . . ? B4' B5' H5' 125.1(14) . . ? B6' B5' H5' 120.4(14) . . ? B2' B5' H5' 132.0(13) . . ? H56' B5' H5' 109.2(17) . . ? B2' B6' B5' 61.5(2) . . ? B2' B6' B7' 61.38(18) . . ? B5' B6' B7' 107.5(2) . . ? B2' B6' H56' 103.2(12) . . ? B5' B6' H56' 47.8(11) . . ? B7' B6' H56' 113.1(10) . . ? B2' B6' H6' 134.7(14) . . ? B5' B6' H6' 128.1(13) . . ? B7' B6' H6' 123.3(14) . . ? H56' B6' H6' 112.0(17) . . ? B2' B6' H67' 100.3(13) . . ? B5' B6' H67' 119.8(12) . . ? B7' B6' H67' 41.5(13) . . ? H56' B6' H67' 91.9(16) . . ? H6' B6' H67' 105.9(18) . . ? B5 B7' B2' 107.6(2) . . ? B5 B7' B1' 57.86(17) . . ? B2' B7' B1' 58.52(17) . . ? B5 B7' B6' 114.8(2) . . ? B2' B7' B6' 56.00(18) . . ? B1' B7' B6' 104.7(2) . . ? B5 B7' H67' 90.3(13) . . ? B2' B7' H67' 97.8(13) . . ? B1' B7' H67' 123.6(13) . . ? B6' B7' H67' 44.3(13) . . ? B5 B7' H7' 121.6(13) . . ? B2' B7' H7' 121.2(13) . . ? B1' B7' H7' 125.0(14) . . ? B6' B7' H7' 118.2(13) . . ? H67' B7' H7' 111.2(18) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.225 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.040 data_jb188_22 _database_code_depnum_ccdc_archive 'CCDC 246571' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H42 B16 P2 Pt' _chemical_formula_weight 676.50 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' 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 monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 10.6570(2) _cell_length_b 16.8137(4) _cell_length_c 17.3033(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.1590(13) _cell_angle_gamma 90.00 _cell_volume 3030.91(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 4.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1512 _exptl_absorpt_correction_T_max 0.7639 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26037 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5949 _reflns_number_gt 5298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+5.2815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00153(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5949 _refine_ls_number_parameters 331 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt9 Pt 0.499662(13) 0.505268(8) 0.740916(9) 0.02325(9) Uani 1 1 d . . . P1 P 0.35678(11) 0.39773(6) 0.72547(7) 0.0299(2) Uani 1 1 d D . . C111 C 0.3277(4) 0.3499(2) 0.6294(2) 0.0313(9) Uani 1 1 d D . . C112 C 0.2447(5) 0.2852(3) 0.6143(3) 0.0476(12) Uani 1 1 d D . . H112 H 0.2040 0.2664 0.6546 0.057 Uiso 1 1 calc R . . C113 C 0.2206(5) 0.2482(3) 0.5417(3) 0.0575(15) Uani 1 1 d D . . H113 H 0.1645 0.2037 0.5325 0.069 Uiso 1 1 calc R . . C114 C 0.2779(4) 0.2756(3) 0.4822(3) 0.0456(12) Uani 1 1 d D . . H114 H 0.2603 0.2503 0.4319 0.055 Uiso 1 1 calc R . . C115 C 0.3605(4) 0.3398(3) 0.4955(3) 0.0389(10) Uani 1 1 d D . . H115 H 0.3995 0.3587 0.4545 0.047 Uiso 1 1 calc R . . C116 C 0.3868(4) 0.3766(3) 0.5694(2) 0.0320(9) Uani 1 1 d D . . H116 H 0.4451 0.4201 0.5789 0.038 Uiso 1 1 calc R . . C12 C 0.4119(5) 0.3194(3) 0.7968(3) 0.0441(11) Uani 1 1 d . . . H12A H 0.4919 0.2968 0.7871 0.066 Uiso 1 1 calc R . . H12B H 0.3465 0.2776 0.7914 0.066 Uiso 1 1 calc R . . H12C H 0.4270 0.3415 0.8504 0.066 Uiso 1 1 calc R . . C13 C 0.1948(4) 0.4132(3) 0.7422(3) 0.0426(11) Uani 1 1 d . . . H13A H 0.1458 0.3637 0.7316 0.064 Uiso 1 1 calc R . . H13B H 0.1520 0.4550 0.7067 0.064 Uiso 1 1 calc R . . H13C H 0.1997 0.4293 0.7972 0.064 Uiso 1 1 calc R . . P2 P 0.34551(10) 0.60305(6) 0.74374(6) 0.0278(2) Uani 1 1 d D . . C211 C 0.2330(4) 0.5967(2) 0.6495(2) 0.0276(9) Uani 1 1 d D . . C212 C 0.1038(4) 0.6167(3) 0.6399(3) 0.0412(11) Uani 1 1 d D . . H212 H 0.0708 0.6335 0.6842 0.049 Uiso 1 1 calc R . . C213 C 0.0236(4) 0.6120(3) 0.5661(3) 0.0507(13) Uani 1 1 d D . . H213 H -0.0644 0.6256 0.5599 0.061 Uiso 1 1 calc R . . C214 C 0.0700(5) 0.5877(3) 0.5010(3) 0.0487(13) Uani 1 1 d D . . H214 H 0.0139 0.5851 0.4505 0.058 Uiso 1 1 calc R . . C215 C 0.1965(4) 0.5672(3) 0.5092(3) 0.0427(11) Uani 1 1 d D . . H215 H 0.2282 0.5499 0.4647 0.051 Uiso 1 1 calc R . . C216 C 0.2783(4) 0.5719(3) 0.5832(2) 0.0354(10) Uani 1 1 d D . . H216 H 0.3662 0.5580 0.5888 0.042 Uiso 1 1 calc R . . C22 C 0.3991(4) 0.7056(2) 0.7428(3) 0.0382(10) Uani 1 1 d . . . H22A H 0.3253 0.7413 0.7383 0.057 Uiso 1 1 calc R . . H22B H 0.4400 0.7138 0.6978 0.057 Uiso 1 1 calc R . . H22C H 0.4611 0.7170 0.7920 0.057 Uiso 1 1 calc R . . C23 C 0.2502(4) 0.6049(3) 0.8193(3) 0.0403(11) Uani 1 1 d . . . H23A H 0.1845 0.5633 0.8083 0.061 Uiso 1 1 calc R . . H23B H 0.2087 0.6569 0.8191 0.061 Uiso 1 1 calc R . . H23C H 0.3060 0.5955 0.8712 0.061 Uiso 1 1 calc R . . B1 B 0.8060(4) 0.5490(3) 0.7179(3) 0.0329(11) Uani 1 1 d . . . H1 H 0.8615 0.5804 0.6788 0.039 Uiso 1 1 calc R . . B2 B 0.8021(4) 0.5878(3) 0.8111(3) 0.0310(10) Uani 1 1 d . . . H2 H 0.8573 0.6428 0.8334 0.037 Uiso 1 1 calc R . . B3 B 0.6607(5) 0.5915(3) 0.7346(3) 0.0304(10) Uani 1 1 d . . . H3 H 0.6231 0.6494 0.7072 0.037 Uiso 1 1 calc R . . B4 B 0.6609(4) 0.4982(3) 0.6779(3) 0.0273(10) Uani 1 1 d . . . H4 H 0.6214 0.4979 0.6126 0.033 Uiso 1 1 calc R . . B5 B 0.8008(5) 0.4427(3) 0.7194(3) 0.0328(11) Uani 1 1 d . . . H5 H 0.8552 0.4068 0.6830 0.039 Uiso 1 1 calc R . . B6 B 0.8802(5) 0.4949(3) 0.8054(3) 0.0317(11) Uani 1 1 d . . . H6 H 0.9865 0.4898 0.8272 0.038 Uiso 1 1 calc R . . B7 B 0.7814(5) 0.5060(3) 0.8730(3) 0.0272(10) Uani 1 1 d . . . B8 B 0.6495(4) 0.5659(3) 0.8324(3) 0.0244(9) Uani 1 1 d . . . B10 B 0.6495(4) 0.4090(3) 0.7310(3) 0.0276(10) Uani 1 1 d . . . H101 H 0.6634 0.4026 0.7998 0.033 Uiso 1 1 d . . . H10 H 0.6122 0.3554 0.7103 0.033 Uiso 1 1 d . . . B11 B 0.7853(5) 0.4116(3) 0.8154(3) 0.0303(10) Uani 1 1 d . . . H11 H 0.8279 0.3597 0.8451 0.036 Uiso 1 1 d . . . B1' B 0.6587(4) 0.5175(3) 0.9218(3) 0.0289(10) Uani 1 1 d . . . H1' H 0.5913 0.4667 0.9234 0.035 Uiso 1 1 calc R . . B2' B 0.7010(5) 0.5812(3) 1.0080(3) 0.0334(11) Uani 1 1 d . . . H2' H 0.6603 0.5696 1.0616 0.040 Uiso 1 1 calc R . . B4' B 0.6054(5) 0.6187(3) 0.9165(3) 0.0325(11) Uani 1 1 d . . . H4' H 0.5015 0.6426 0.9083 0.039 Uiso 1 1 d . . . H45' H 0.6739 0.6658 0.9011 0.039 Uiso 1 1 d . . . B5' B 0.7259(5) 0.6785(3) 0.9802(3) 0.0380(12) Uani 1 1 d . . . C5' C 0.7010(6) 0.7623(3) 1.0143(3) 0.0549(14) Uani 1 1 d . . . H5'A H 0.7638 0.7716 1.0637 0.082 Uiso 1 1 calc R . . H5'B H 0.6142 0.7638 1.0247 0.082 Uiso 1 1 calc R . . H5'C H 0.7097 0.8037 0.9759 0.082 Uiso 1 1 calc R . . B6' B 0.8558(5) 0.6160(3) 1.0190(3) 0.0355(11) Uani 1 1 d . . . H6' H 0.9191 0.6386 1.0760 0.043 Uiso 1 1 d . . . H56' H 0.8400 0.6740 0.9692 0.043 Uiso 1 1 d . . . B7' B 0.8207(5) 0.5178(3) 0.9794(3) 0.0330(10) Uani 1 1 d . . . H7' H 0.8554 0.4718 1.0184 0.040 Uiso 1 1 d . . . H67' H 0.8861 0.5719 0.9810 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt9 0.02325(11) 0.02415(11) 0.02342(11) -0.00116(5) 0.00732(6) 0.00053(6) P1 0.0327(6) 0.0288(6) 0.0312(6) -0.0029(4) 0.0134(5) -0.0055(5) C111 0.033(2) 0.026(2) 0.034(2) -0.0025(17) 0.0057(18) -0.0031(17) C112 0.046(3) 0.044(3) 0.059(3) -0.016(2) 0.023(2) -0.017(2) C113 0.061(3) 0.045(3) 0.070(4) -0.026(3) 0.022(3) -0.020(3) C114 0.039(3) 0.047(3) 0.047(3) -0.021(2) 0.000(2) -0.003(2) C115 0.043(3) 0.044(3) 0.028(2) -0.0044(19) 0.0039(19) 0.003(2) C116 0.032(2) 0.033(2) 0.030(2) -0.0018(18) 0.0050(17) -0.0043(18) C12 0.053(3) 0.039(3) 0.043(3) 0.009(2) 0.017(2) -0.005(2) C13 0.032(2) 0.050(3) 0.050(3) -0.006(2) 0.020(2) -0.010(2) P2 0.0249(5) 0.0305(6) 0.0275(5) -0.0025(4) 0.0048(4) 0.0041(4) C211 0.020(2) 0.033(2) 0.030(2) -0.0018(17) 0.0049(16) -0.0003(16) C212 0.025(2) 0.064(3) 0.036(2) 0.002(2) 0.0099(19) 0.000(2) C213 0.021(2) 0.083(4) 0.046(3) 0.009(3) 0.002(2) 0.001(2) C214 0.038(3) 0.067(3) 0.036(3) 0.005(2) -0.002(2) -0.010(2) C215 0.045(3) 0.054(3) 0.030(2) -0.001(2) 0.009(2) 0.002(2) C216 0.032(2) 0.041(3) 0.033(2) 0.0009(19) 0.0060(18) 0.0058(19) C22 0.037(3) 0.031(2) 0.043(3) -0.0015(19) -0.001(2) 0.0083(19) C23 0.031(2) 0.059(3) 0.034(2) -0.006(2) 0.0115(19) 0.011(2) B1 0.023(2) 0.048(3) 0.029(2) 0.003(2) 0.0088(19) 0.000(2) B2 0.026(2) 0.036(3) 0.032(3) 0.004(2) 0.0070(19) -0.001(2) B3 0.034(3) 0.026(2) 0.030(3) 0.0036(19) 0.004(2) -0.001(2) B4 0.025(2) 0.031(3) 0.028(2) 0.0019(17) 0.0096(19) -0.0010(18) B5 0.034(3) 0.038(3) 0.029(3) 0.003(2) 0.013(2) 0.010(2) B6 0.027(2) 0.044(3) 0.026(2) 0.0040(19) 0.011(2) 0.002(2) B7 0.028(2) 0.031(2) 0.024(2) -0.0002(17) 0.0068(18) 0.0014(18) B8 0.019(2) 0.026(2) 0.026(2) -0.0022(18) 0.0007(17) -0.0033(17) B10 0.023(2) 0.030(2) 0.030(2) -0.0036(19) 0.0049(18) 0.0035(19) B11 0.033(3) 0.032(3) 0.027(2) 0.002(2) 0.0079(19) 0.003(2) B1' 0.027(2) 0.037(3) 0.023(2) -0.002(2) 0.0047(18) -0.002(2) B2' 0.032(3) 0.043(3) 0.024(2) -0.005(2) 0.0041(19) 0.002(2) B4' 0.027(2) 0.038(3) 0.031(3) -0.004(2) 0.003(2) 0.001(2) B5' 0.041(3) 0.044(3) 0.029(3) -0.005(2) 0.006(2) 0.000(2) C5' 0.069(4) 0.049(3) 0.045(3) -0.013(2) 0.009(3) 0.001(3) B6' 0.030(3) 0.048(3) 0.027(2) -0.008(2) 0.003(2) -0.002(2) B7' 0.030(2) 0.040(3) 0.029(3) 0.005(2) 0.007(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt9 B4 2.224(5) . ? Pt9 B8 2.243(4) . ? Pt9 B3 2.266(5) . ? Pt9 B10 2.305(5) . ? Pt9 P2 2.3320(10) . ? Pt9 P1 2.3426(11) . ? P1 C111 1.814(4) . ? P1 C12 1.816(5) . ? P1 C13 1.828(4) . ? C111 C112 1.391(6) . ? C111 C116 1.398(6) . ? C112 C113 1.376(7) . ? C113 C114 1.383(7) . ? C114 C115 1.381(6) . ? C115 C116 1.394(6) . ? P2 C211 1.812(4) . ? P2 C23 1.817(4) . ? P2 C22 1.818(4) . ? C211 C212 1.393(6) . ? C211 C216 1.399(6) . ? C212 C213 1.382(6) . ? C213 C214 1.384(7) . ? C214 C215 1.370(7) . ? C215 C216 1.391(6) . ? B1 B2 1.749(7) . ? B1 B4 1.774(7) . ? B1 B3 1.783(7) . ? B1 B5 1.787(8) . ? B1 B6 1.799(7) . ? B2 B8 1.779(6) . ? B2 B6 1.781(7) . ? B2 B7 1.785(7) . ? B2 B3 1.787(7) . ? B3 B8 1.774(6) . ? B3 B4 1.849(7) . ? B4 B10 1.778(6) . ? B4 B5 1.778(7) . ? B5 B10 1.761(7) . ? B5 B6 1.780(7) . ? B5 B11 1.782(7) . ? B6 B7 1.741(7) . ? B6 B11 1.757(7) . ? B7 B1' 1.710(7) . ? B7 B8 1.752(6) . ? B7 B7' 1.811(7) . ? B7 B11 1.878(7) . ? B8 B1' 1.733(6) . ? B8 B4' 1.848(7) . ? B10 B11 1.828(7) . ? B1' B4' 1.790(7) . ? B1' B7' 1.803(7) . ? B1' B2' 1.815(7) . ? B2' B6' 1.723(7) . ? B2' B5' 1.742(7) . ? B2' B4' 1.807(7) . ? B2' B7' 1.810(7) . ? B4' B5' 1.811(7) . ? B5' C5' 1.571(7) . ? B5' B6' 1.756(7) . ? B6' B7' 1.798(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B4 Pt9 B8 82.02(17) . . ? B4 Pt9 B3 48.63(17) . . ? B8 Pt9 B3 46.32(16) . . ? B4 Pt9 B10 46.18(16) . . ? B8 Pt9 B10 88.31(16) . . ? B3 Pt9 B10 84.40(19) . . ? B4 Pt9 P2 131.93(12) . . ? B8 Pt9 P2 93.71(12) . . ? B3 Pt9 P2 95.40(13) . . ? B10 Pt9 P2 177.00(12) . . ? B4 Pt9 P1 116.99(12) . . ? B8 Pt9 P1 141.33(12) . . ? B3 Pt9 P1 165.61(13) . . ? B10 Pt9 P1 83.86(12) . . ? P2 Pt9 P1 95.89(4) . . ? C111 P1 C12 105.6(2) . . ? C111 P1 C13 102.9(2) . . ? C12 P1 C13 100.2(2) . . ? C111 P1 Pt9 115.37(13) . . ? C12 P1 Pt9 111.89(16) . . ? C13 P1 Pt9 119.00(16) . . ? C112 C111 C116 118.7(4) . . ? C112 C111 P1 119.9(3) . . ? C116 C111 P1 121.5(3) . . ? C113 C112 C111 121.0(5) . . ? C112 C113 C114 120.1(5) . . ? C115 C114 C113 120.1(4) . . ? C114 C115 C116 119.9(4) . . ? C115 C116 C111 120.2(4) . . ? C211 P2 C23 106.5(2) . . ? C211 P2 C22 101.42(19) . . ? C23 P2 C22 102.4(2) . . ? C211 P2 Pt9 105.97(13) . . ? C23 P2 Pt9 122.02(16) . . ? C22 P2 Pt9 116.39(15) . . ? C212 C211 C216 118.5(4) . . ? C212 C211 P2 122.9(3) . . ? C216 C211 P2 118.5(3) . . ? C213 C212 C211 120.0(4) . . ? C212 C213 C214 120.8(4) . . ? C215 C214 C213 120.2(4) . . ? C214 C215 C216 119.6(4) . . ? C215 C216 C211 120.9(4) . . ? B2 B1 B4 110.6(3) . . ? B2 B1 B3 60.8(3) . . ? B4 B1 B3 62.6(3) . . ? B2 B1 B5 110.7(3) . . ? B4 B1 B5 59.9(3) . . ? B3 B1 B5 111.6(3) . . ? B2 B1 B6 60.3(3) . . ? B4 B1 B6 106.2(3) . . ? B3 B1 B6 108.0(3) . . ? B5 B1 B6 59.5(3) . . ? B1 B2 B8 108.2(3) . . ? B1 B2 B6 61.3(3) . . ? B8 B2 B6 106.7(3) . . ? B1 B2 B7 107.2(4) . . ? B8 B2 B7 58.9(3) . . ? B6 B2 B7 58.4(3) . . ? B1 B2 B3 60.6(3) . . ? B8 B2 B3 59.7(3) . . ? B6 B2 B3 108.7(3) . . ? B7 B2 B3 106.2(3) . . ? B8 B3 B1 107.0(3) . . ? B8 B3 B2 60.0(3) . . ? B1 B3 B2 58.7(3) . . ? B8 B3 B4 108.0(3) . . ? B1 B3 B4 58.4(3) . . ? B2 B3 B4 105.6(3) . . ? B8 B3 Pt9 66.1(2) . . ? B1 B3 Pt9 116.3(3) . . ? B2 B3 Pt9 118.1(3) . . ? B4 B3 Pt9 64.5(2) . . ? B1 B4 B10 110.7(3) . . ? B1 B4 B5 60.4(3) . . ? B10 B4 B5 59.4(3) . . ? B1 B4 B3 58.9(3) . . ? B10 B4 B3 115.7(4) . . ? B5 B4 B3 109.0(3) . . ? B1 B4 Pt9 118.9(3) . . ? B10 B4 Pt9 69.3(2) . . ? B5 B4 Pt9 119.9(3) . . ? B3 B4 Pt9 66.9(2) . . ? B10 B5 B4 60.3(3) . . ? B10 B5 B6 110.5(3) . . ? B4 B5 B6 106.8(3) . . ? B10 B5 B11 62.1(3) . . ? B4 B5 B11 107.2(3) . . ? B6 B5 B11 59.1(3) . . ? B10 B5 B1 110.8(3) . . ? B4 B5 B1 59.7(3) . . ? B6 B5 B1 60.6(3) . . ? B11 B5 B1 108.4(3) . . ? B7 B6 B11 64.9(3) . . ? B7 B6 B5 111.5(3) . . ? B11 B6 B5 60.5(3) . . ? B7 B6 B2 60.9(3) . . ? B11 B6 B2 114.1(4) . . ? B5 B6 B2 109.5(3) . . ? B7 B6 B1 106.9(3) . . ? B11 B6 B1 109.0(3) . . ? B5 B6 B1 59.9(3) . . ? B2 B6 B1 58.5(3) . . ? B1' B7 B6 167.8(4) . . ? B1' B7 B8 60.1(3) . . ? B6 B7 B8 109.8(3) . . ? B1' B7 B2 114.4(3) . . ? B6 B7 B2 60.7(3) . . ? B8 B7 B2 60.4(3) . . ? B1' B7 B7' 61.5(3) . . ? B6 B7 B7' 130.6(4) . . ? B8 B7 B7' 109.9(3) . . ? B2 B7 B7' 119.6(3) . . ? B1' B7 B11 117.5(3) . . ? B6 B7 B11 58.0(3) . . ? B8 B7 B11 112.3(3) . . ? B2 B7 B11 108.3(3) . . ? B7' B7 B11 127.3(3) . . ? B1' B8 B7 58.8(3) . . ? B1' B8 B3 164.4(4) . . ? B7 B8 B3 108.3(3) . . ? B1' B8 B2 113.5(3) . . ? B7 B8 B2 60.7(3) . . ? B3 B8 B2 60.4(3) . . ? B1' B8 B4' 59.9(3) . . ? B7 B8 B4' 106.0(3) . . ? B3 B8 B4' 135.6(3) . . ? B2 B8 B4' 117.3(3) . . ? B1' B8 Pt9 108.3(3) . . ? B7 B8 Pt9 114.4(3) . . ? B3 B8 Pt9 67.5(2) . . ? B2 B8 Pt9 119.6(3) . . ? B4' B8 Pt9 120.8(3) . . ? B5 B10 B4 60.3(3) . . ? B5 B10 B11 59.5(3) . . ? B4 B10 B11 105.3(3) . . ? B5 B10 Pt9 116.6(3) . . ? B4 B10 Pt9 64.5(2) . . ? B11 B10 Pt9 111.6(3) . . ? B6 B11 B5 60.4(3) . . ? B6 B11 B10 108.4(3) . . ? B5 B11 B10 58.4(3) . . ? B6 B11 B7 57.1(3) . . ? B5 B11 B7 105.3(3) . . ? B10 B11 B7 110.0(3) . . ? B7 B1' B8 61.2(3) . . ? B7 B1' B4' 110.5(3) . . ? B8 B1' B4' 63.2(3) . . ? B7 B1' B7' 62.0(3) . . ? B8 B1' B7' 111.1(3) . . ? B4' B1' B7' 106.4(3) . . ? B7 B1' B2' 112.9(3) . . ? B8 B1' B2' 114.4(3) . . ? B4' B1' B2' 60.2(3) . . ? B7' B1' B2' 60.0(3) . . ? B6' B2' B5' 60.9(3) . . ? B6' B2' B4' 109.2(4) . . ? B5' B2' B4' 61.3(3) . . ? B6' B2' B7' 61.1(3) . . ? B5' B2' B7' 108.7(4) . . ? B4' B2' B7' 105.4(3) . . ? B6' B2' B1' 111.0(3) . . ? B5' B2' B1' 110.7(3) . . ? B4' B2' B1' 59.2(3) . . ? B7' B2' B1' 59.7(3) . . ? B1' B4' B2' 60.6(3) . . ? B1' B4' B5' 108.7(3) . . ? B2' B4' B5' 57.6(3) . . ? B1' B4' B8 56.9(2) . . ? B2' B4' B8 109.4(3) . . ? B5' B4' B8 118.7(3) . . ? C5' B5' B2' 133.7(4) . . ? C5' B5' B6' 125.0(4) . . ? B2' B5' B6' 59.0(3) . . ? C5' B5' B4' 125.0(4) . . ? B2' B5' B4' 61.1(3) . . ? B6' B5' B4' 107.5(4) . . ? B2' B6' B5' 60.1(3) . . ? B2' B6' B7' 61.9(3) . . ? B5' B6' B7' 108.7(3) . . ? B6' B7' B1' 108.1(3) . . ? B6' B7' B2' 57.0(3) . . ? B1' B7' B2' 60.3(3) . . ? B6' B7' B7 118.3(3) . . ? B1' B7' B7 56.5(3) . . ? B2' B7' B7 108.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.772 _refine_diff_density_min -1.401 _refine_diff_density_rms 0.174