Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Professor N.C.Norman' _publ_contact_author_address ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; _publ_contact_author_email n.c.norman@bristol.ac.uk _publ_contact_author_phone '+44 117 928 7577' _publ_contact_author_fax '+44 117 925 1295' loop_ _publ_author_name _publ_author_address N.C.Norman ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; J.P.H.Charmant ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; 'Cheng Fan.' ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; P.G.Pringle ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; _publ_section_title ;Synthesis and Reactivity of Dichloroboryl Complexes of Platinum(II) ; data_[PtCl(PMe3)3][BCl4] _database_code_depnum_ccdc_archive 'CCDC 618539' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C9 H27 Cl P3 Pt, B Cl4' _chemical_formula_sum 'C9 H27 B Cl5 P3 Pt' _chemical_formula_weight 611.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 '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 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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 9.9079(4) _cell_length_b 13.2057(4) _cell_length_c 16.0316(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2097.59(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.19 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 20.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.13 _exptl_absorpt_correction_T_max 0.55 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.602 _diffrn_detector_type 'Bruker-AXS SMART 6000' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation 'Osmic CMF12-38Cu6 (blue) mirror optics' _diffrn_radiation_monochromator 'Osmic CMF12-38Cu6 (blue) mirror optics' _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source rotating-anode _diffrn_source_current 120 _diffrn_source_power 4.8 _diffrn_source_size '3 x 0.3mm' _diffrn_source_target Cu _diffrn_source_type 'MAC Science M18XCE' _diffrn_source_voltage 40 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6875 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 68.89 _reflns_number_total 3481 _reflns_number_gt 3297 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.625 (Bruker-AXS, 1997-2001)' _computing_cell_refinement 'SMART v5.625 (Bruker-AXS, 1997-2001)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0456P)^2^+2.3707P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.500(17) _refine_ls_number_reflns 3481 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.98039(3) 0.15644(2) 0.429542(19) 0.01575(10) Uani 1 1 d . . . Cl1 Cl 1.0051(2) 0.31961(13) 0.37117(13) 0.0286(4) Uani 1 1 d . . . P1 P 0.9942(2) 0.09098(14) 0.29452(12) 0.0213(4) Uani 1 1 d . . . P2 P 0.9707(3) 0.00452(14) 0.49355(13) 0.0226(4) Uani 1 1 d . . . P3 P 0.9536(2) 0.24683(15) 0.55481(12) 0.0210(4) Uani 1 1 d . . . C5 C 0.8003(10) -0.0245(8) 0.5307(7) 0.035(2) Uani 1 1 d . . . H5A H 0.8028 -0.0857 0.5653 0.052 Uiso 1 1 calc R . . H5B H 0.7406 -0.0357 0.4829 0.052 Uiso 1 1 calc R . . H5C H 0.7663 0.0323 0.5640 0.052 Uiso 1 1 calc R . . C8 C 1.1142(10) 0.2936(8) 0.5904(7) 0.037(3) Uani 1 1 d . . . H8A H 1.1006 0.3370 0.6392 0.056 Uiso 1 1 calc R . . H8B H 1.1571 0.3327 0.5457 0.056 Uiso 1 1 calc R . . H8C H 1.1722 0.2364 0.6055 0.056 Uiso 1 1 calc R . . C4 C 1.0164(11) -0.1086(6) 0.4380(6) 0.034(2) Uani 1 1 d . . . H4A H 1.1136 -0.1081 0.4267 0.051 Uiso 1 1 calc R . . H4B H 0.9668 -0.1114 0.3851 0.051 Uiso 1 1 calc R . . H4C H 0.9937 -0.1681 0.4718 0.051 Uiso 1 1 calc R . . C7 C 0.8760(10) 0.1932(8) 0.6465(6) 0.033(2) Uani 1 1 d . . . H7A H 0.9257 0.1324 0.6634 0.049 Uiso 1 1 calc R . . H7B H 0.7822 0.1751 0.6340 0.049 Uiso 1 1 calc R . . H7C H 0.8779 0.2428 0.6918 0.049 Uiso 1 1 calc R . . Cl3 Cl 0.9976(2) 0.53827(13) 0.68841(12) 0.0264(4) Uani 1 1 d . . . Cl5 Cl 1.1565(2) 0.71534(16) 0.62010(15) 0.0303(5) Uani 1 1 d . . . Cl4 Cl 0.8703(3) 0.74608(19) 0.67915(17) 0.0397(6) Uani 1 1 d . . . B1 B 0.9865(10) 0.6574(7) 0.6279(6) 0.0256(18) Uani 1 1 d . . . C2 C 0.8470(9) 0.0166(8) 0.2665(6) 0.025(2) Uani 1 1 d . . . H2A H 0.7677 0.0608 0.2637 0.038 Uiso 1 1 calc R . . H2B H 0.8322 -0.0360 0.3087 0.038 Uiso 1 1 calc R . . H2C H 0.8617 -0.0152 0.2120 0.038 Uiso 1 1 calc R . . C3 C 0.9971(11) 0.1848(8) 0.2138(5) 0.038(2) Uani 1 1 d . . . H3A H 1.0816 0.2231 0.2170 0.056 Uiso 1 1 calc R . . H3B H 0.9206 0.2310 0.2209 0.056 Uiso 1 1 calc R . . H3C H 0.9907 0.1515 0.1593 0.056 Uiso 1 1 calc R . . C1 C 1.1411(10) 0.0174(8) 0.2674(7) 0.034(2) Uani 1 1 d . . . H1A H 1.1302 -0.0101 0.2111 0.050 Uiso 1 1 calc R . . H1B H 1.1515 -0.0383 0.3072 0.050 Uiso 1 1 calc R . . H1C H 1.2213 0.0608 0.2693 0.050 Uiso 1 1 calc R . . C9 C 0.8497(9) 0.3592(7) 0.5429(6) 0.029(2) Uani 1 1 d . . . H9A H 0.8573 0.4013 0.5931 0.044 Uiso 1 1 calc R . . H9B H 0.7554 0.3392 0.5350 0.044 Uiso 1 1 calc R . . H9C H 0.8804 0.3979 0.4943 0.044 Uiso 1 1 calc R . . Cl2 Cl 0.9237(3) 0.62868(17) 0.52104(15) 0.0382(6) Uani 1 1 d . . . C6 C 1.0853(10) -0.0057(6) 0.5799(7) 0.031(2) Uani 1 1 d . . . H6A H 1.0625 -0.0656 0.6131 0.047 Uiso 1 1 calc R . . H6B H 1.0782 0.0550 0.6148 0.047 Uiso 1 1 calc R . . H6C H 1.1779 -0.0121 0.5589 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01689(15) 0.01237(14) 0.01800(15) 0.00011(12) -0.00038(14) 0.00039(12) Cl1 0.0355(12) 0.0168(8) 0.0335(9) 0.0084(7) 0.0004(10) -0.0001(8) P1 0.0183(10) 0.0247(9) 0.0209(9) -0.0038(7) 0.0015(9) 0.0016(9) P2 0.0284(11) 0.0137(8) 0.0257(10) 0.0025(7) -0.0026(11) 0.0002(9) P3 0.0209(10) 0.0203(8) 0.0218(10) -0.0059(7) -0.0005(9) -0.0001(8) C5 0.028(5) 0.031(5) 0.045(6) 0.016(5) 0.008(5) -0.011(4) C8 0.033(5) 0.033(5) 0.046(6) -0.020(5) -0.005(5) 0.008(4) C4 0.048(5) 0.020(3) 0.034(4) -0.006(3) -0.008(6) 0.001(4) C7 0.031(5) 0.038(5) 0.028(5) -0.008(4) 0.000(4) 0.008(4) Cl3 0.0321(12) 0.0196(8) 0.0273(9) 0.0031(7) -0.0042(10) -0.0041(9) Cl5 0.0275(11) 0.0239(10) 0.0394(12) 0.0025(9) 0.0026(10) -0.0033(9) Cl4 0.0345(12) 0.0361(12) 0.0486(14) 0.0000(11) 0.0050(12) 0.0133(10) B1 0.026(5) 0.019(4) 0.032(5) -0.002(4) 0.002(4) 0.003(5) C2 0.019(4) 0.033(5) 0.025(5) -0.012(4) -0.007(4) 0.002(4) C3 0.038(6) 0.051(5) 0.024(4) 0.001(4) 0.004(5) -0.001(5) C1 0.026(5) 0.038(6) 0.037(6) -0.007(5) -0.005(5) -0.005(4) C9 0.025(4) 0.024(4) 0.039(5) -0.009(4) 0.004(4) -0.002(4) Cl2 0.0519(15) 0.0308(11) 0.0319(11) 0.0050(9) -0.0106(12) -0.0094(10) C6 0.038(5) 0.021(4) 0.034(5) 0.004(4) -0.002(5) 0.005(4) _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 P2 2.2555(18) . ? Pt1 P1 2.3350(19) . ? Pt1 P3 2.3512(19) . ? Pt1 Cl1 2.3618(16) . ? P1 C3 1.792(9) . ? P1 C1 1.802(10) . ? P1 C2 1.815(9) . ? P2 C6 1.796(10) . ? P2 C4 1.798(8) . ? P2 C5 1.831(10) . ? P3 C8 1.799(10) . ? P3 C7 1.804(10) . ? P3 C9 1.816(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? Cl3 B1 1.852(9) . ? Cl5 B1 1.854(10) . ? Cl4 B1 1.836(10) . ? B1 Cl2 1.861(10) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 95.45(7) . . ? P2 Pt1 P3 93.34(7) . . ? P1 Pt1 P3 170.55(7) . . ? P2 Pt1 Cl1 174.98(9) . . ? P1 Pt1 Cl1 87.96(7) . . ? P3 Pt1 Cl1 83.51(7) . . ? C3 P1 C1 100.7(5) . . ? C3 P1 C2 102.0(5) . . ? C1 P1 C2 107.3(4) . . ? C3 P1 Pt1 114.5(3) . . ? C1 P1 Pt1 118.0(4) . . ? C2 P1 Pt1 112.5(3) . . ? C6 P2 C4 99.2(4) . . ? C6 P2 C5 108.4(5) . . ? C4 P2 C5 102.7(5) . . ? C6 P2 Pt1 113.0(3) . . ? C4 P2 Pt1 120.2(3) . . ? C5 P2 Pt1 111.9(3) . . ? C8 P3 C7 104.7(5) . . ? C8 P3 C9 104.7(4) . . ? C7 P3 C9 99.5(5) . . ? C8 P3 Pt1 110.2(3) . . ? C7 P3 Pt1 123.0(3) . . ? C9 P3 Pt1 112.9(3) . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Cl4 B1 Cl3 110.1(5) . . ? Cl4 B1 Cl5 109.7(5) . . ? Cl3 B1 Cl5 109.4(5) . . ? Cl4 B1 Cl2 109.4(5) . . ? Cl3 B1 Cl2 109.2(5) . . ? Cl5 B1 Cl2 109.0(5) . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 68.89 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.376 _refine_diff_density_min -1.278 _refine_diff_density_rms 0.158 #===END data_Ph3PBCl3 _database_code_depnum_ccdc_archive 'CCDC 618540' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C18 H15 B Cl3 P' _chemical_formula_sum 'C18 H15 B Cl3 P' _chemical_formula_weight 379.43 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.8318(12) _cell_length_b 9.7063(9) _cell_length_c 15.8277(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.467(2) _cell_angle_gamma 90.00 _cell_volume 1816.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.21 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 173 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.192 _diffrn_detector_type 'Bruker-AXS SMART 1k' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Platform' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation '0.5 mm double pin hole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18842 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4179 _reflns_number_gt 2819 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.054 (Bruker-AXS, 1997-1998)' _computing_cell_refinement 'SMART v5.054 (Bruker-AXS, 1997-1998)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0617P)^2^+0.2366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4179 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.4339(3) 0.6598(3) 0.29933(19) 0.0265(6) Uani 1 1 d . . . P1 P 0.45789(5) 0.59890(6) 0.18030(4) 0.02112(16) Uani 1 1 d . . . Cl1 Cl 0.54984(6) 0.58710(7) 0.36785(4) 0.03532(19) Uani 1 1 d . . . Cl2 Cl 0.43683(7) 0.84871(7) 0.30118(5) 0.0414(2) Uani 1 1 d . . . Cl3 Cl 0.29620(6) 0.59328(8) 0.33001(5) 0.03701(19) Uani 1 1 d . . . C1 C 0.3281(2) 0.6089(2) 0.11607(15) 0.0237(5) Uani 1 1 d . . . C2 C 0.2881(2) 0.4969(3) 0.06852(17) 0.0286(6) Uani 1 1 d . . . H2 H 0.3286 0.4123 0.0699 0.034 Uiso 1 1 calc R . . C3 C 0.1885(2) 0.5096(3) 0.01891(18) 0.0349(7) Uani 1 1 d . . . H3 H 0.1610 0.4331 -0.0133 0.042 Uiso 1 1 calc R . . C4 C 0.1298(2) 0.6316(3) 0.01619(18) 0.0373(7) Uani 1 1 d . . . H4 H 0.0628 0.6397 -0.0187 0.045 Uiso 1 1 calc R . . C5 C 0.1680(2) 0.7432(3) 0.06430(19) 0.0387(7) Uani 1 1 d . . . H5 H 0.1262 0.8268 0.0633 0.046 Uiso 1 1 calc R . . C6 C 0.2678(2) 0.7328(3) 0.11411(18) 0.0321(6) Uani 1 1 d . . . H6 H 0.2945 0.8094 0.1465 0.038 Uiso 1 1 calc R . . C7 C 0.5072(2) 0.4229(2) 0.17922(16) 0.0222(5) Uani 1 1 d . . . C8 C 0.6051(2) 0.3840(3) 0.13922(16) 0.0286(6) Uani 1 1 d . . . H8 H 0.6474 0.4510 0.1103 0.034 Uiso 1 1 calc R . . C9 C 0.6410(2) 0.2478(3) 0.14159(18) 0.0347(7) Uani 1 1 d . . . H9 H 0.7073 0.2216 0.1138 0.042 Uiso 1 1 calc R . . C10 C 0.5804(2) 0.1509(3) 0.18425(19) 0.0373(7) Uani 1 1 d . . . H10 H 0.6051 0.0578 0.1860 0.045 Uiso 1 1 calc R . . C11 C 0.4841(2) 0.1883(3) 0.2243(2) 0.0379(7) Uani 1 1 d . . . H11 H 0.4430 0.1209 0.2539 0.046 Uiso 1 1 calc R . . C12 C 0.4467(2) 0.3235(3) 0.22191(19) 0.0321(6) Uani 1 1 d . . . H12 H 0.3798 0.3485 0.2493 0.039 Uiso 1 1 calc R . . C13 C 0.5622(2) 0.7058(2) 0.13128(16) 0.0238(5) Uani 1 1 d . . . C14 C 0.5390(2) 0.7698(3) 0.05362(16) 0.0287(6) Uani 1 1 d . . . H14 H 0.4669 0.7588 0.0256 0.034 Uiso 1 1 calc R . . C15 C 0.6215(2) 0.8498(3) 0.01717(17) 0.0347(7) Uani 1 1 d . . . H15 H 0.6058 0.8930 -0.0359 0.042 Uiso 1 1 calc R . . C16 C 0.7257(2) 0.8666(3) 0.05779(18) 0.0351(7) Uani 1 1 d . . . H16 H 0.7818 0.9209 0.0323 0.042 Uiso 1 1 calc R . . C17 C 0.7495(2) 0.8052(3) 0.13544(19) 0.0365(7) Uani 1 1 d . . . H17 H 0.8215 0.8178 0.1634 0.044 Uiso 1 1 calc R . . C18 C 0.6676(2) 0.7246(3) 0.17256(18) 0.0336(6) Uani 1 1 d . . . H18 H 0.6836 0.6825 0.2259 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0319(16) 0.0204(14) 0.0270(16) 0.0013(12) 0.0005(13) 0.0004(12) P1 0.0210(3) 0.0175(3) 0.0249(3) 0.0007(3) 0.0014(3) 0.0000(3) Cl1 0.0384(4) 0.0350(4) 0.0316(4) 0.0004(3) -0.0092(3) 0.0059(3) Cl2 0.0674(5) 0.0194(3) 0.0373(4) -0.0027(3) 0.0024(4) 0.0047(3) Cl3 0.0325(4) 0.0435(4) 0.0357(4) 0.0026(3) 0.0103(3) 0.0006(3) C1 0.0239(13) 0.0255(13) 0.0218(12) 0.0034(10) 0.0015(10) -0.0008(10) C2 0.0257(14) 0.0292(14) 0.0311(15) 0.0006(11) 0.0033(11) -0.0021(11) C3 0.0300(15) 0.0413(17) 0.0332(16) -0.0012(13) -0.0015(12) -0.0095(13) C4 0.0253(14) 0.0525(19) 0.0337(16) 0.0064(14) -0.0056(12) -0.0031(13) C5 0.0313(16) 0.0417(17) 0.0425(17) 0.0072(14) -0.0035(13) 0.0096(13) C6 0.0311(15) 0.0311(14) 0.0339(15) -0.0026(12) -0.0005(12) 0.0044(12) C7 0.0218(12) 0.0197(12) 0.0249(13) -0.0023(10) -0.0014(10) 0.0017(10) C8 0.0290(14) 0.0296(14) 0.0271(14) 0.0001(11) 0.0011(11) 0.0048(11) C9 0.0345(16) 0.0385(16) 0.0308(15) -0.0085(13) -0.0019(12) 0.0171(13) C10 0.0430(18) 0.0218(13) 0.0459(17) -0.0061(13) -0.0115(14) 0.0105(13) C11 0.0364(17) 0.0210(13) 0.056(2) 0.0038(13) 0.0021(14) -0.0012(12) C12 0.0258(14) 0.0229(13) 0.0483(18) 0.0014(12) 0.0080(12) 0.0004(11) C13 0.0246(13) 0.0201(12) 0.0269(14) -0.0001(10) 0.0027(11) -0.0018(10) C14 0.0292(14) 0.0300(14) 0.0267(14) -0.0005(11) -0.0006(11) -0.0032(11) C15 0.0439(17) 0.0347(15) 0.0258(14) 0.0050(12) 0.0032(12) -0.0079(13) C16 0.0381(16) 0.0323(15) 0.0353(16) 0.0014(13) 0.0078(13) -0.0153(13) C17 0.0278(15) 0.0405(16) 0.0409(17) 0.0052(13) -0.0008(13) -0.0083(13) C18 0.0293(15) 0.0385(16) 0.0326(15) 0.0060(13) -0.0023(12) -0.0065(12) _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 Cl2 1.835(3) . ? B1 Cl3 1.837(3) . ? B1 Cl1 1.852(3) . ? B1 P1 2.006(3) . ? P1 C7 1.806(2) . ? P1 C1 1.807(3) . ? P1 C13 1.812(3) . ? C1 C2 1.393(4) . ? C1 C6 1.398(3) . ? C2 C3 1.393(4) . ? C2 H2 0.9500 . ? C3 C4 1.373(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.393(4) . ? C7 C8 1.396(4) . ? C8 C9 1.388(4) . ? C8 H8 0.9500 . ? C9 C10 1.377(4) . ? C9 H9 0.9500 . ? C10 C11 1.376(4) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.394(4) . ? C13 C18 1.395(4) . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.376(4) . ? C15 H15 0.9500 . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 C18 1.395(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? 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 Cl2 B1 Cl3 111.31(16) . . ? Cl2 B1 Cl1 111.00(16) . . ? Cl3 B1 Cl1 110.77(15) . . ? Cl2 B1 P1 107.82(14) . . ? Cl3 B1 P1 107.93(15) . . ? Cl1 B1 P1 107.85(15) . . ? C7 P1 C1 108.21(11) . . ? C7 P1 C13 108.15(11) . . ? C1 P1 C13 107.82(11) . . ? C7 P1 B1 110.27(12) . . ? C1 P1 B1 111.17(12) . . ? C13 P1 B1 111.11(12) . . ? C2 C1 C6 119.9(2) . . ? C2 C1 P1 121.48(19) . . ? C6 C1 P1 118.66(19) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 119.1(2) . . ? C12 C7 P1 118.52(19) . . ? C8 C7 P1 122.32(19) . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.9(3) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 119.5(2) . . ? C14 C13 P1 121.4(2) . . ? C18 C13 P1 119.1(2) . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.5(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 119.8(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 120.0(3) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.633 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.068 #===END data_[Pt2(mu-Cl)2(PMePh2)4][BCl4]2 _database_code_depnum_ccdc_archive 'CCDC 618541' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C52 H52 Cl2 P4 Pt2, 2(B Cl4)' _chemical_formula_sum 'C52 H52 B2 Cl10 P4 Pt2' _chemical_formula_weight 1567.12 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.896(2) _cell_length_b 11.707(2) _cell_length_c 12.654(3) _cell_angle_alpha 84.45(3) _cell_angle_beta 79.32(3) _cell_angle_gamma 85.85(3) _cell_volume 1431.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4932 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.11 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method none _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 5.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.55 _exptl_absorpt_process_details 'SADABS V2.1 (Bruker-AXS, 2001)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16377 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6541 _reflns_number_gt 5872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0545P)^2^+38.8769P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6541 _refine_ls_number_parameters 345 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.901 _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 0.3356(9) 0.8043(8) 0.8032(8) 0.033(2) Uani 1 1 d . . . C2 C 0.3167(10) 0.8382(9) 0.9085(10) 0.045(3) Uani 1 1 d . . . H2 H 0.3729 0.8031 0.9572 0.055 Uiso 1 1 calc R . . C3 C 0.2168(14) 0.9228(12) 0.9420(16) 0.079(6) Uani 1 1 d . . . H3 H 0.2046 0.9456 1.0134 0.094 Uiso 1 1 calc R . . C4 C 0.1335(14) 0.9747(11) 0.870(2) 0.091(7) Uani 1 1 d . . . H4 H 0.0656 1.0335 0.8919 0.110 Uiso 1 1 calc R . . C5 C 0.1515(12) 0.9395(11) 0.7684(17) 0.076(5) Uani 1 1 d . . . H5 H 0.0939 0.9737 0.7205 0.091 Uiso 1 1 calc R . . C6 C 0.2504(10) 0.8560(9) 0.7330(12) 0.049(3) Uani 1 1 d . . . H6 H 0.2607 0.8336 0.6616 0.059 Uiso 1 1 calc R . . C7 C 0.5734(9) 0.7484(8) 0.6395(6) 0.0244(17) Uani 1 1 d . . . C8 C 0.5783(9) 0.8646(8) 0.6103(7) 0.0260(18) Uani 1 1 d . . . H8 H 0.5234 0.9181 0.6542 0.031 Uiso 1 1 calc R . . C9 C 0.6649(10) 0.9028(9) 0.5155(8) 0.036(2) Uani 1 1 d . . . H9 H 0.6696 0.9829 0.4952 0.043 Uiso 1 1 calc R . . C10 C 0.7433(12) 0.8259(10) 0.4512(8) 0.042(2) Uani 1 1 d . . . H10 H 0.8024 0.8527 0.3869 0.051 Uiso 1 1 calc R . . C11 C 0.7361(10) 0.7092(10) 0.4802(7) 0.037(2) Uani 1 1 d . . . H11 H 0.7888 0.6562 0.4344 0.044 Uiso 1 1 calc R . . C12 C 0.6536(10) 0.6688(9) 0.5745(7) 0.031(2) Uani 1 1 d . . . H12 H 0.6511 0.5887 0.5951 0.038 Uiso 1 1 calc R . . C13 C 0.3680(10) 0.5873(8) 0.7088(8) 0.034(2) Uani 1 1 d . . . H13A H 0.2910 0.5620 0.7646 0.052 Uiso 1 1 calc R . . H13B H 0.4303 0.5209 0.6885 0.052 Uiso 1 1 calc R . . H13C H 0.3326 0.6228 0.6453 0.052 Uiso 1 1 calc R . . C14 C 0.8307(9) 0.7067(8) 0.9775(7) 0.0277(18) Uani 1 1 d . . . C15 C 0.9694(10) 0.6766(11) 0.9660(9) 0.046(3) Uani 1 1 d . . . H15 H 1.0204 0.6582 0.8979 0.055 Uiso 1 1 calc R . . C16 C 1.0349(13) 0.6734(13) 1.0553(11) 0.064(4) Uani 1 1 d . . . H16 H 1.1306 0.6528 1.0475 0.076 Uiso 1 1 calc R . . C17 C 0.9625(15) 0.6995(10) 1.1531(10) 0.056(4) Uani 1 1 d . . . H17 H 1.0085 0.6982 1.2128 0.067 Uiso 1 1 calc R . . C18 C 0.8244(15) 0.7275(11) 1.1661(10) 0.058(4) Uani 1 1 d . . . H18 H 0.7742 0.7448 1.2348 0.069 Uiso 1 1 calc R . . C19 C 0.7571(13) 0.7306(11) 1.0776(9) 0.051(3) Uani 1 1 d . . . H19 H 0.6609 0.7492 1.0864 0.061 Uiso 1 1 calc R . . C20 C 0.8601(9) 0.6900(9) 0.7484(7) 0.032(2) Uani 1 1 d . . . C21 C 0.9192(11) 0.7762(11) 0.6754(8) 0.043(3) Uani 1 1 d . . . H21 H 0.8930 0.8546 0.6855 0.052 Uiso 1 1 calc R . . C22 C 1.0176(12) 0.7466(15) 0.5868(8) 0.056(4) Uani 1 1 d . . . H22 H 1.0588 0.8057 0.5370 0.067 Uiso 1 1 calc R . . C23 C 1.0555(11) 0.6357(16) 0.5705(9) 0.061(4) Uani 1 1 d . . . H23 H 1.1230 0.6169 0.5100 0.073 Uiso 1 1 calc R . . C24 C 0.9952(14) 0.5501(14) 0.6425(10) 0.066(4) Uani 1 1 d . . . H24 H 1.0219 0.4720 0.6311 0.079 Uiso 1 1 calc R . . C25 C 0.8959(12) 0.5759(10) 0.7317(9) 0.046(3) Uani 1 1 d . . . H25 H 0.8537 0.5162 0.7801 0.055 Uiso 1 1 calc R . . C26 C 0.6892(11) 0.8717(9) 0.8575(8) 0.037(2) Uani 1 1 d . . . H26A H 0.7719 0.9152 0.8501 0.056 Uiso 1 1 calc R . . H26B H 0.6249 0.8906 0.9230 0.056 Uiso 1 1 calc R . . H26C H 0.6450 0.8919 0.7945 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.6410(4) 0.5001(4) 1.0440(3) 0.0944(17) Uani 1 1 d . . . P1 P 0.4609(2) 0.69122(19) 0.76047(18) 0.0230(4) Uani 1 1 d . . . P2 P 0.7364(2) 0.7204(2) 0.86636(18) 0.0247(4) Uani 1 1 d . . . Pt1 Pt 0.55618(3) 0.60899(3) 0.89908(3) 0.02680(12) Uani 1 1 d . . . B1 B 0.3372(13) 0.7868(10) 0.2877(8) 0.035(2) Uani 1 1 d . . . Cl2 Cl 0.1678(3) 0.8672(2) 0.3064(2) 0.0468(6) Uani 1 1 d D A . Cl3 Cl 0.4496(13) 0.8621(10) 0.1890(11) 0.199(11) Uani 0.50 1 d PDU A 1 Cl3' Cl 0.4802(7) 0.8839(6) 0.2280(9) 0.068(3) Uani 0.50 1 d PDU A 2 Cl4 Cl 0.3890(8) 0.7795(8) 0.4157(7) 0.065(2) Uani 0.50 1 d PDU A 1 Cl4' Cl 0.3805(7) 0.7041(8) 0.4122(5) 0.069(3) Uani 0.50 1 d PDU A 2 Cl5 Cl 0.3087(13) 0.6491(7) 0.2536(11) 0.139(7) Uani 0.50 1 d PDU A 1 Cl5' Cl 0.3472(6) 0.6738(7) 0.1862(5) 0.0489(18) Uani 0.50 1 d PDU A 2 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 0.020(4) 0.026(4) 0.050(6) -0.003(4) -0.002(4) 0.000(3) C2 0.025(5) 0.036(6) 0.072(8) -0.021(5) 0.010(5) -0.004(4) C3 0.041(7) 0.046(7) 0.137(15) -0.045(9) 0.038(8) -0.015(6) C4 0.029(7) 0.026(6) 0.20(2) -0.009(9) 0.034(10) 0.007(5) C5 0.027(6) 0.035(7) 0.149(16) 0.032(9) 0.002(8) 0.003(5) C6 0.023(5) 0.035(6) 0.086(9) 0.020(6) -0.013(5) 0.002(4) C7 0.023(4) 0.038(5) 0.013(3) -0.001(3) -0.009(3) 0.001(3) C8 0.030(4) 0.028(4) 0.019(4) 0.004(3) -0.010(3) 0.011(3) C9 0.033(5) 0.039(5) 0.036(5) 0.001(4) -0.010(4) 0.006(4) C10 0.046(6) 0.054(7) 0.024(5) 0.003(4) -0.006(4) 0.003(5) C11 0.032(5) 0.058(7) 0.020(4) -0.013(4) -0.005(4) 0.010(4) C12 0.032(5) 0.038(5) 0.028(4) -0.003(4) -0.018(4) 0.008(4) C13 0.035(5) 0.036(5) 0.038(5) -0.006(4) -0.017(4) -0.010(4) C14 0.029(4) 0.028(4) 0.031(4) -0.002(4) -0.018(4) -0.007(4) C15 0.026(5) 0.073(8) 0.040(6) 0.018(5) -0.015(4) -0.016(5) C16 0.039(6) 0.096(10) 0.061(8) 0.039(7) -0.036(6) -0.030(7) C17 0.084(9) 0.043(6) 0.057(8) 0.017(5) -0.053(7) -0.025(6) C18 0.086(10) 0.056(7) 0.045(7) -0.026(6) -0.043(7) 0.020(7) C19 0.058(7) 0.064(8) 0.038(6) -0.027(5) -0.026(5) 0.025(6) C20 0.023(4) 0.050(6) 0.025(4) -0.006(4) -0.008(3) -0.005(4) C21 0.044(6) 0.065(7) 0.025(5) 0.002(5) -0.015(4) -0.016(5) C22 0.038(6) 0.112(12) 0.020(5) -0.006(6) -0.005(4) -0.021(7) C23 0.024(5) 0.135(14) 0.022(5) -0.008(7) -0.005(4) 0.011(7) C24 0.058(8) 0.092(11) 0.043(7) -0.017(7) -0.011(6) 0.046(8) C25 0.043(6) 0.051(7) 0.037(6) 0.000(5) 0.001(5) 0.014(5) C26 0.046(6) 0.037(5) 0.034(5) -0.008(4) -0.017(4) -0.008(4) Cl1 0.069(2) 0.135(3) 0.087(3) 0.087(3) -0.057(2) -0.073(2) P1 0.0196(10) 0.0240(11) 0.0276(11) -0.0046(8) -0.0106(8) 0.0029(8) P2 0.0216(10) 0.0323(12) 0.0232(10) -0.0044(9) -0.0104(8) -0.0018(9) Pt1 0.02076(17) 0.0365(2) 0.02548(17) 0.00543(13) -0.01199(12) -0.00751(12) B1 0.053(7) 0.031(5) 0.022(5) -0.001(4) -0.011(5) -0.009(5) Cl2 0.0377(14) 0.0471(15) 0.0524(16) 0.0043(12) -0.0030(11) -0.0055(11) Cl3 0.194(15) 0.090(9) 0.198(15) 0.094(9) 0.168(13) 0.094(9) Cl3' 0.027(3) 0.022(3) 0.144(8) -0.038(4) 0.035(4) -0.014(2) Cl4 0.058(4) 0.091(6) 0.059(4) -0.012(4) -0.040(3) 0.010(4) Cl4' 0.038(3) 0.126(7) 0.038(3) 0.035(5) -0.014(3) 0.004(4) Cl5 0.195(14) 0.053(5) 0.226(15) -0.081(8) -0.174(13) 0.068(7) Cl5' 0.031(3) 0.068(4) 0.057(4) -0.037(3) -0.013(3) -0.004(3) _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 C6 1.402(14) . ? C1 C2 1.403(16) . ? C1 P1 1.798(9) . ? C2 C3 1.386(16) . ? C2 H2 0.9500 . ? C3 C4 1.41(3) . ? C3 H3 0.9500 . ? C4 C5 1.36(3) . ? C4 H4 0.9500 . ? C5 C6 1.377(18) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.376(12) . ? C7 C12 1.405(13) . ? C7 P1 1.819(9) . ? C8 C9 1.394(13) . ? C8 H8 0.9500 . ? C9 C10 1.372(15) . ? C9 H9 0.9500 . ? C10 C11 1.383(16) . ? C10 H10 0.9500 . ? C11 C12 1.378(14) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 P1 1.815(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.377(14) . ? C14 C19 1.382(14) . ? C14 P2 1.815(8) . ? C15 C16 1.399(15) . ? C15 H15 0.9500 . ? C16 C17 1.36(2) . ? C16 H16 0.9500 . ? C17 C18 1.366(19) . ? C17 H17 0.9500 . ? C18 C19 1.402(14) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.383(15) . ? C20 C21 1.386(14) . ? C20 P2 1.793(10) . ? C21 C22 1.395(16) . ? C21 H21 0.9500 . ? C22 C23 1.35(2) . ? C22 H22 0.9500 . ? C23 C24 1.38(2) . ? C23 H23 0.9500 . ? C24 C25 1.393(16) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 P2 1.797(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Cl1 Pt1 2.371(3) 2_667 ? Cl1 Pt1 2.378(3) . ? P1 Pt1 2.246(2) . ? P2 Pt1 2.239(2) . ? Pt1 Cl1 2.371(3) 2_667 ? B1 Cl5 1.764(13) . ? B1 Cl4 1.779(12) . ? B1 Cl2 1.849(13) . ? B1 Cl3 1.730(14) . ? B1 Cl4' 1.870(12) . ? B1 Cl3' 1.881(13) . ? B1 Cl5' 1.916(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.9(10) . . ? C6 C1 P1 120.2(9) . . ? C2 C1 P1 120.8(8) . . ? C3 C2 C1 120.5(14) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 119.8(16) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.1(12) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 122.3(15) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.5(14) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C8 C7 C12 120.7(8) . . ? C8 C7 P1 122.0(7) . . ? C12 C7 P1 117.3(7) . . ? C7 C8 C9 119.2(8) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 120.7(10) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.8(10) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.9(9) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C7 118.7(9) . . ? C11 C12 H12 120.6 . . ? C7 C12 H12 120.6 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 119.6(9) . . ? C15 C14 P2 123.6(8) . . ? C19 C14 P2 116.8(7) . . ? C14 C15 C16 119.6(11) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.5(12) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.6(10) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 119.6(12) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C14 C19 C18 120.1(11) . . ? C14 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C25 C20 C21 120.1(10) . . ? C25 C20 P2 117.7(8) . . ? C21 C20 P2 122.2(9) . . ? C20 C21 C22 119.3(12) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 121.3(12) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 119.3(11) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C24 C25 121.3(13) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C20 C25 C24 118.7(12) . . ? C20 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Pt1 Cl1 Pt1 95.57(10) 2_667 . ? C1 P1 C13 105.9(5) . . ? C1 P1 C7 107.3(4) . . ? C13 P1 C7 102.5(4) . . ? C1 P1 Pt1 111.1(4) . . ? C13 P1 Pt1 110.4(3) . . ? C7 P1 Pt1 118.7(3) . . ? C20 P2 C26 108.4(5) . . ? C20 P2 C14 106.1(4) . . ? C26 P2 C14 101.5(4) . . ? C20 P2 Pt1 114.2(3) . . ? C26 P2 Pt1 113.8(4) . . ? C14 P2 Pt1 111.9(3) . . ? P2 Pt1 P1 94.92(9) . . ? P2 Pt1 Cl1 172.64(14) . 2_667 ? P1 Pt1 Cl1 89.03(9) . 2_667 ? P2 Pt1 Cl1 92.01(9) . . ? P1 Pt1 Cl1 172.39(11) . . ? Cl1 Pt1 Cl1 84.43(11) 2_667 . ? Cl5 B1 Cl4 111.3(7) . . ? Cl5 B1 Cl2 106.5(7) . . ? Cl4 B1 Cl2 104.9(6) . . ? Cl5 B1 Cl3 113.3(8) . . ? Cl4 B1 Cl3 111.7(9) . . ? Cl2 B1 Cl3 108.6(7) . . ? Cl2 B1 Cl4' 115.0(6) . . ? Cl2 B1 Cl3' 111.4(6) . . ? Cl4' B1 Cl3' 109.1(7) . . ? Cl2 B1 Cl5' 111.4(6) . . ? Cl4' B1 Cl5' 104.6(7) . . ? Cl3' B1 Cl5' 104.7(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 C6 C1 C2 C3 -1.0(15) . . . . ? P1 C1 C2 C3 -177.8(8) . . . . ? C1 C2 C3 C4 0.1(17) . . . . ? C2 C3 C4 C5 0.9(19) . . . . ? C3 C4 C5 C6 -1(2) . . . . ? C4 C5 C6 C1 0.4(18) . . . . ? C2 C1 C6 C5 0.7(15) . . . . ? P1 C1 C6 C5 177.6(8) . . . . ? C12 C7 C8 C9 -0.4(12) . . . . ? P1 C7 C8 C9 -178.8(7) . . . . ? C7 C8 C9 C10 0.7(14) . . . . ? C8 C9 C10 C11 0.4(15) . . . . ? C9 C10 C11 C12 -1.7(15) . . . . ? C10 C11 C12 C7 1.9(14) . . . . ? C8 C7 C12 C11 -0.9(12) . . . . ? P1 C7 C12 C11 177.6(7) . . . . ? C19 C14 C15 C16 -1.5(17) . . . . ? P2 C14 C15 C16 177.0(9) . . . . ? C14 C15 C16 C17 0.1(19) . . . . ? C15 C16 C17 C18 1(2) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C15 C14 C19 C18 1.8(18) . . . . ? P2 C14 C19 C18 -176.8(10) . . . . ? C17 C18 C19 C14 -1(2) . . . . ? C25 C20 C21 C22 -1.7(14) . . . . ? P2 C20 C21 C22 178.3(8) . . . . ? C20 C21 C22 C23 0.5(16) . . . . ? C21 C22 C23 C24 0.3(17) . . . . ? C22 C23 C24 C25 0.1(19) . . . . ? C21 C20 C25 C24 2.1(16) . . . . ? P2 C20 C25 C24 -177.9(9) . . . . ? C23 C24 C25 C20 -1.3(19) . . . . ? C6 C1 P1 C13 -51.2(9) . . . . ? C2 C1 P1 C13 125.6(8) . . . . ? C6 C1 P1 C7 57.7(9) . . . . ? C2 C1 P1 C7 -125.5(8) . . . . ? C6 C1 P1 Pt1 -171.1(7) . . . . ? C2 C1 P1 Pt1 5.7(9) . . . . ? C8 C7 P1 C1 16.0(8) . . . . ? C12 C7 P1 C1 -162.4(7) . . . . ? C8 C7 P1 C13 127.3(7) . . . . ? C12 C7 P1 C13 -51.2(7) . . . . ? C8 C7 P1 Pt1 -110.8(7) . . . . ? C12 C7 P1 Pt1 70.7(7) . . . . ? C25 C20 P2 C26 -171.2(8) . . . . ? C21 C20 P2 C26 8.8(9) . . . . ? C25 C20 P2 C14 80.4(9) . . . . ? C21 C20 P2 C14 -99.6(8) . . . . ? C25 C20 P2 Pt1 -43.3(9) . . . . ? C21 C20 P2 Pt1 136.7(7) . . . . ? C15 C14 P2 C20 -0.9(10) . . . . ? C19 C14 P2 C20 177.7(9) . . . . ? C15 C14 P2 C26 -114.1(9) . . . . ? C19 C14 P2 C26 64.5(9) . . . . ? C15 C14 P2 Pt1 124.2(8) . . . . ? C19 C14 P2 Pt1 -57.2(9) . . . . ? C20 P2 Pt1 P1 -71.6(4) . . . . ? C26 P2 Pt1 P1 53.5(4) . . . . ? C14 P2 Pt1 P1 167.9(3) . . . . ? C20 P2 Pt1 Cl1 105.3(4) . . . . ? C26 P2 Pt1 Cl1 -129.6(4) . . . . ? C14 P2 Pt1 Cl1 -15.3(4) . . . . ? C1 P1 Pt1 P2 -93.7(3) . . . . ? C13 P1 Pt1 P2 149.2(4) . . . . ? C7 P1 Pt1 P2 31.3(3) . . . . ? C1 P1 Pt1 Cl1 80.1(4) . . . 2_667 ? C13 P1 Pt1 Cl1 -37.0(4) . . . 2_667 ? C7 P1 Pt1 Cl1 -154.9(4) . . . 2_667 ? Pt1 Cl1 Pt1 P2 173.55(17) 2_667 . . . ? Pt1 Cl1 Pt1 Cl1 0.0 2_667 . . 2_667 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 7.111 _refine_diff_density_min -2.684 _refine_diff_density_rms 0.200 #===END data_PhMe2PBCl3 _database_code_depnum_ccdc_archive 'CCDC 618542' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C8 H11 B Cl3 P' _chemical_formula_sum 'C8 H11 B Cl3 P' _chemical_formula_weight 255.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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 6.2473(7) _cell_length_b 10.8165(11) _cell_length_c 17.5194(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1183.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.16 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.856 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12612 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2709 _reflns_number_gt 2359 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0330P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(7) _refine_ls_number_reflns 2709 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 B1 B 0.0713(4) 0.6644(2) 0.81016(14) 0.0269(5) Uani 1 1 d . . . P1 P 0.21867(8) 0.54636(4) 0.87712(3) 0.02109(12) Uani 1 1 d . . . Cl1 Cl 0.27538(9) 0.71906(6) 0.74243(4) 0.04711(18) Uani 1 1 d . . . Cl2 Cl -0.03171(10) 0.79093(5) 0.86982(4) 0.03900(15) Uani 1 1 d . . . Cl3 Cl -0.14648(9) 0.58280(5) 0.76109(3) 0.03697(14) Uani 1 1 d . . . C1 C 0.0418(3) 0.48254(18) 0.94808(11) 0.0213(4) Uani 1 1 d . . . C2 C -0.0981(3) 0.38782(19) 0.92797(12) 0.0262(5) Uani 1 1 d . . . H2 H -0.0974 0.3558 0.8775 0.031 Uiso 1 1 calc R . . C3 C -0.2388(4) 0.34017(18) 0.98190(12) 0.0315(5) Uani 1 1 d . . . H3 H -0.3326 0.2746 0.9684 0.038 Uiso 1 1 calc R . . C4 C -0.2428(4) 0.3876(2) 1.05479(13) 0.0349(5) Uani 1 1 d . . . H4 H -0.3401 0.3551 1.0913 0.042 Uiso 1 1 calc R . . C5 C -0.1065(4) 0.4816(2) 1.07479(13) 0.0374(6) Uani 1 1 d . . . H5 H -0.1105 0.5142 1.1251 0.045 Uiso 1 1 calc R . . C6 C 0.0369(3) 0.52928(19) 1.02211(12) 0.0304(5) Uani 1 1 d . . . H6 H 0.1318 0.5938 1.0365 0.036 Uiso 1 1 calc R . . C7 C 0.4366(3) 0.6224(2) 0.92456(13) 0.0309(5) Uani 1 1 d . . . H7A H 0.3827 0.6950 0.9520 0.046 Uiso 1 1 calc R . . H7B H 0.5430 0.6485 0.8867 0.046 Uiso 1 1 calc R . . H7C H 0.5032 0.5652 0.9609 0.046 Uiso 1 1 calc R . . C8 C 0.3256(4) 0.42043(19) 0.82215(12) 0.0333(5) Uani 1 1 d . . . H8A H 0.3821 0.3571 0.8567 0.050 Uiso 1 1 calc R . . H8B H 0.4409 0.4509 0.7892 0.050 Uiso 1 1 calc R . . H8C H 0.2119 0.3846 0.7905 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0239(12) 0.0295(13) 0.0272(13) 0.0046(10) 0.0021(10) -0.0013(10) P1 0.0199(2) 0.0225(2) 0.0209(2) 0.0011(2) 0.0011(2) 0.00070(19) Cl1 0.0344(3) 0.0599(4) 0.0470(4) 0.0302(3) 0.0122(3) 0.0028(3) Cl2 0.0423(3) 0.0293(3) 0.0455(3) -0.0030(3) 0.0004(3) 0.0086(2) Cl3 0.0326(3) 0.0485(3) 0.0298(3) 0.0003(3) -0.0087(2) -0.0027(2) C1 0.0219(9) 0.0209(10) 0.0211(10) 0.0046(8) 0.0000(8) 0.0021(8) C2 0.0289(12) 0.0249(11) 0.0248(11) 0.0019(9) -0.0026(9) 0.0002(8) C3 0.0289(11) 0.0273(11) 0.0382(13) 0.0056(9) -0.0006(10) -0.0040(10) C4 0.0338(12) 0.0377(13) 0.0332(13) 0.0118(10) 0.0086(10) 0.0015(10) C5 0.0471(14) 0.0431(14) 0.0220(12) -0.0010(10) 0.0071(10) 0.0008(11) C6 0.0355(11) 0.0293(11) 0.0263(12) -0.0025(9) 0.0009(9) -0.0047(10) C7 0.0251(11) 0.0356(12) 0.0319(12) 0.0010(10) -0.0021(9) -0.0029(9) C8 0.0356(13) 0.0297(12) 0.0346(12) -0.0019(10) 0.0087(10) 0.0055(10) _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 Cl3 1.836(2) . ? B1 Cl2 1.838(2) . ? B1 Cl1 1.839(2) . ? B1 P1 1.963(2) . ? P1 C7 1.795(2) . ? P1 C8 1.797(2) . ? P1 C1 1.8008(19) . ? C1 C2 1.392(3) . ? C1 C6 1.392(3) . ? C2 C3 1.389(3) . ? C2 H2 0.9500 . ? C3 C4 1.376(3) . ? C3 H3 0.9500 . ? C4 C5 1.372(3) . ? C4 H4 0.9500 . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 B1 Cl2 111.39(12) . . ? Cl3 B1 Cl1 111.48(13) . . ? Cl2 B1 Cl1 111.73(12) . . ? Cl3 B1 P1 108.34(12) . . ? Cl2 B1 P1 107.98(12) . . ? Cl1 B1 P1 105.64(11) . . ? C7 P1 C8 108.27(11) . . ? C7 P1 C1 108.75(10) . . ? C8 P1 C1 107.91(10) . . ? C7 P1 B1 109.54(10) . . ? C8 P1 B1 110.31(11) . . ? C1 P1 B1 111.97(9) . . ? C2 C1 C6 119.28(18) . . ? C2 C1 P1 119.52(15) . . ? C6 C1 P1 121.16(16) . . ? C3 C2 C1 119.9(2) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.1(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C8 H8A 109.5 . . ? P1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.229 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.048 #===END data_[Pt2Cl2(mu-Cl)2(PCy3)2] _database_code_depnum_ccdc_archive 'CCDC 618543' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C36 H66 Cl4 P2 Pt2, C7 H8' _chemical_formula_sum 'C43 H74 Cl4 P2 Pt2' _chemical_formula_weight 1184.94 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' Cl Cl 0.1484 0.1585 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.229(3) _cell_length_b 16.041(3) _cell_length_c 19.920(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.22(3) _cell_angle_gamma 90.00 _cell_volume 4510.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12173 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method none _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 6.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.404 _exptl_absorpt_correction_T_max 0.520 _exptl_absorpt_process_details 'SADABS v2.05 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25604 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5181 _reflns_number_gt 4901 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+11.4026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5181 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0474 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.004 _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 0.67740(18) 0.01979(16) 0.44081(12) 0.0137(5) Uani 1 1 d . . . H1A H 0.6108 0.0042 0.4466 0.016 Uiso 1 1 calc R . . C2 C 0.6747(2) 0.10638(18) 0.40797(14) 0.0259(6) Uani 1 1 d . . . H2A H 0.6464 0.1467 0.4372 0.031 Uiso 1 1 calc R . . H2B H 0.7402 0.1248 0.4040 0.031 Uiso 1 1 calc R . . C3 C 0.6172(2) 0.10583(19) 0.33781(15) 0.0282(7) Uani 1 1 d . . . H3A H 0.5501 0.0936 0.3423 0.034 Uiso 1 1 calc R . . H3B H 0.6200 0.1617 0.3171 0.034 Uiso 1 1 calc R . . C4 C 0.6540(2) 0.04139(19) 0.29187(14) 0.0260(7) Uani 1 1 d . . . H4A H 0.7184 0.0573 0.2828 0.031 Uiso 1 1 calc R . . H4B H 0.6124 0.0400 0.2481 0.031 Uiso 1 1 calc R . . C5 C 0.6572(2) -0.04469(18) 0.32404(14) 0.0252(6) Uani 1 1 d . . . H5A H 0.6857 -0.0845 0.2945 0.030 Uiso 1 1 calc R . . H5B H 0.5918 -0.0634 0.3277 0.030 Uiso 1 1 calc R . . C6 C 0.7145(2) -0.04545(17) 0.39432(13) 0.0198(6) Uani 1 1 d . . . H6A H 0.7818 -0.0338 0.3901 0.024 Uiso 1 1 calc R . . H6B H 0.7107 -0.1015 0.4147 0.024 Uiso 1 1 calc R . . C7 C 0.73620(18) -0.08506(16) 0.55897(12) 0.0132(5) Uani 1 1 d . . . H7A H 0.7657 -0.1219 0.5269 0.016 Uiso 1 1 calc R . . C8 C 0.7954(2) -0.09933(17) 0.62810(14) 0.0204(6) Uani 1 1 d . . . H8A H 0.7676 -0.0676 0.6634 0.024 Uiso 1 1 calc R . . H8B H 0.8609 -0.0791 0.6267 0.024 Uiso 1 1 calc R . . C9 C 0.7971(2) -0.19286(18) 0.64541(16) 0.0253(6) Uani 1 1 d . . . H9A H 0.8303 -0.2236 0.6123 0.030 Uiso 1 1 calc R . . H9B H 0.8327 -0.2014 0.6909 0.030 Uiso 1 1 calc R . . C10 C 0.6972(2) -0.22757(17) 0.64438(15) 0.0228(6) Uani 1 1 d . . . H10A H 0.7006 -0.2883 0.6532 0.027 Uiso 1 1 calc R . . H10B H 0.6663 -0.2011 0.6808 0.027 Uiso 1 1 calc R . . C11 C 0.6386(2) -0.21166(18) 0.57678(15) 0.0233(6) Uani 1 1 d . . . H11A H 0.5732 -0.2319 0.5784 0.028 Uiso 1 1 calc R . . H11B H 0.6657 -0.2433 0.5411 0.028 Uiso 1 1 calc R . . C12 C 0.63606(19) -0.11871(18) 0.55887(15) 0.0217(6) Uani 1 1 d . . . H12A H 0.5998 -0.1106 0.5136 0.026 Uiso 1 1 calc R . . H12B H 0.6036 -0.0875 0.5922 0.026 Uiso 1 1 calc R . . C13 C 0.68874(18) 0.09995(16) 0.57367(12) 0.0143(5) Uani 1 1 d . . . H13A H 0.6984 0.1540 0.5505 0.017 Uiso 1 1 calc R . . C14 C 0.73555(19) 0.11213(17) 0.64688(13) 0.0171(5) Uani 1 1 d . . . H14A H 0.7210 0.0641 0.6750 0.020 Uiso 1 1 calc R . . H14B H 0.8052 0.1158 0.6479 0.020 Uiso 1 1 calc R . . C15 C 0.6974(2) 0.19268(18) 0.67498(14) 0.0225(6) Uani 1 1 d . . . H15A H 0.7259 0.2003 0.7225 0.027 Uiso 1 1 calc R . . H15B H 0.7159 0.2408 0.6485 0.027 Uiso 1 1 calc R . . C16 C 0.5900(2) 0.19026(18) 0.67183(14) 0.0228(6) Uani 1 1 d . . . H16A H 0.5673 0.2446 0.6870 0.027 Uiso 1 1 calc R . . H16B H 0.5721 0.1468 0.7031 0.027 Uiso 1 1 calc R . . C17 C 0.5422(2) 0.17190(18) 0.60073(14) 0.0216(6) Uani 1 1 d . . . H17A H 0.5523 0.2194 0.5707 0.026 Uiso 1 1 calc R . . H17B H 0.4731 0.1656 0.6017 0.026 Uiso 1 1 calc R . . C18 C 0.58160(19) 0.09202(19) 0.57225(14) 0.0219(6) Uani 1 1 d . . . H18A H 0.5667 0.0435 0.5997 0.026 Uiso 1 1 calc R . . H18B H 0.5518 0.0830 0.5252 0.026 Uiso 1 1 calc R . . Cl1 Cl 0.87663(5) 0.19183(4) 0.53515(4) 0.02623(16) Uani 1 1 d . . . Cl2 Cl 0.94006(5) -0.08413(4) 0.49719(4) 0.02144(14) Uani 1 1 d . . . P1 P 0.74685(4) 0.02141(4) 0.52579(3) 0.01110(12) Uani 1 1 d . . . Pt1 Pt 0.897405(7) 0.052960(6) 0.517509(5) 0.01289(4) Uani 1 1 d . . . C19 C 0.0000 -0.0850(3) 0.7500 0.0372(11) Uani 1 2 d S . . H19A H 0.0000 -0.1443 0.7500 0.045 Uiso 1 2 calc SR . . C20 C 0.0385(3) -0.0419(2) 0.70027(19) 0.0373(8) Uani 1 1 d . . . H20A H 0.0660 -0.0714 0.6662 0.045 Uiso 1 1 calc R . . C21 C 0.0373(3) 0.0448(2) 0.70005(19) 0.0368(8) Uani 1 1 d . . . H21A H 0.0625 0.0740 0.6649 0.044 Uiso 1 1 calc R . . C22 C 0.0000 0.0892(3) 0.7500 0.0350(11) Uani 1 2 d S . . C23 C 0.0000 0.1827(4) 0.7500 0.0630(19) Uani 1 2 d S . . H23A H 0.0016 0.2030 0.7038 0.094 Uiso 0.50 1 calc PR . . H23B H 0.0559 0.2030 0.7792 0.094 Uiso 0.50 1 calc PR . . H23C H -0.0575 0.2030 0.7671 0.094 Uiso 0.50 1 calc PR . . 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 0.0142(12) 0.0158(12) 0.0111(11) -0.0006(9) 0.0018(9) -0.0003(10) C2 0.0425(19) 0.0168(13) 0.0163(13) 0.0031(11) -0.0039(13) 0.0001(12) C3 0.0386(19) 0.0259(15) 0.0184(14) 0.0048(12) -0.0037(13) 0.0071(13) C4 0.0302(17) 0.0357(17) 0.0118(13) 0.0033(11) 0.0013(12) 0.0012(13) C5 0.0338(17) 0.0284(16) 0.0127(13) -0.0060(11) 0.0001(12) 0.0021(12) C6 0.0265(15) 0.0206(14) 0.0117(12) -0.0029(10) 0.0009(11) 0.0039(11) C7 0.0130(12) 0.0133(11) 0.0134(12) 0.0016(9) 0.0029(9) -0.0028(9) C8 0.0222(14) 0.0194(13) 0.0182(13) 0.0044(10) -0.0022(11) -0.0040(11) C9 0.0246(15) 0.0220(14) 0.0281(15) 0.0112(12) -0.0016(12) -0.0032(12) C10 0.0282(16) 0.0166(13) 0.0247(15) 0.0044(11) 0.0074(12) -0.0024(11) C11 0.0192(14) 0.0224(14) 0.0281(15) 0.0036(12) 0.0020(12) -0.0074(11) C12 0.0126(13) 0.0241(14) 0.0279(15) 0.0076(12) 0.0005(11) -0.0028(11) C13 0.0150(13) 0.0158(12) 0.0126(12) -0.0024(9) 0.0043(10) 0.0006(10) C14 0.0174(13) 0.0213(13) 0.0124(12) -0.0024(10) 0.0010(10) -0.0005(10) C15 0.0271(16) 0.0222(14) 0.0187(13) -0.0080(11) 0.0049(12) -0.0010(12) C16 0.0277(16) 0.0230(14) 0.0190(14) -0.0051(11) 0.0078(12) 0.0065(12) C17 0.0194(14) 0.0283(15) 0.0182(13) 0.0005(11) 0.0064(11) 0.0073(11) C18 0.0137(13) 0.0324(16) 0.0197(13) -0.0100(12) 0.0023(11) 0.0019(11) Cl1 0.0226(3) 0.0118(3) 0.0475(4) -0.0016(3) 0.0168(3) -0.0004(2) Cl2 0.0133(3) 0.0126(3) 0.0407(4) -0.0067(3) 0.0125(3) -0.0028(2) P1 0.0103(3) 0.0132(3) 0.0101(3) -0.0003(2) 0.0025(2) -0.0003(2) Pt1 0.01120(6) 0.01160(6) 0.01670(6) -0.00122(3) 0.00493(4) -0.00072(3) C19 0.030(3) 0.034(3) 0.044(3) 0.000 -0.008(2) 0.000 C20 0.0265(18) 0.049(2) 0.0358(19) -0.0093(16) 0.0008(15) -0.0007(15) C21 0.0242(17) 0.053(2) 0.0335(19) -0.0025(15) 0.0046(14) -0.0004(15) C22 0.020(2) 0.037(3) 0.049(3) 0.000 0.004(2) 0.000 C23 0.048(4) 0.032(3) 0.112(6) 0.000 0.020(4) 0.000 _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 1.534(4) . ? C1 C6 1.535(4) . ? C1 P1 1.850(3) . ? C1 H1A 1.0000 . ? C2 C3 1.529(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.517(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.521(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.529(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.523(4) . ? C7 C8 1.538(4) . ? C7 P1 1.844(3) . ? C7 H7A 1.0000 . ? C8 C9 1.539(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.523(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.514(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.532(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.526(4) . ? C13 C14 1.537(3) . ? C13 P1 1.838(3) . ? C13 H13A 1.0000 . ? C14 C15 1.535(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.521(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.521(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.536(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? Cl1 Pt1 2.2802(8) . ? Cl2 Pt1 2.3303(8) . ? Cl2 Pt1 2.4195(8) 5_756 ? P1 Pt1 2.2275(8) . ? Pt1 Cl2 2.4196(8) 5_756 ? C19 C20 1.377(5) 2_556 ? C19 C20 1.377(5) . ? C19 H19A 0.9500 . ? C20 C21 1.391(5) . ? C20 H20A 0.9500 . ? C21 C22 1.383(4) . ? C21 H21A 0.9500 . ? C22 C21 1.383(4) 2_556 ? C22 C23 1.499(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 110.6(2) . . ? C2 C1 P1 111.06(18) . . ? C6 C1 P1 112.15(18) . . ? C2 C1 H1A 107.6 . . ? C6 C1 H1A 107.6 . . ? P1 C1 H1A 107.6 . . ? C3 C2 C1 111.5(2) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 111.7(3) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 111.0(2) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 112.2(2) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C1 111.3(2) . . ? C5 C6 H6A 109.4 . . ? C1 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C12 C7 C8 110.8(2) . . ? C12 C7 P1 116.53(18) . . ? C8 C7 P1 113.47(18) . . ? C12 C7 H7A 104.9 . . ? C8 C7 H7A 104.9 . . ? P1 C7 H7A 104.9 . . ? C7 C8 C9 109.7(2) . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 111.4(2) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.0(2) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 111.4(2) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C7 C12 C11 110.5(2) . . ? C7 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? C7 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C18 C13 C14 109.9(2) . . ? C18 C13 P1 116.53(18) . . ? C14 C13 P1 114.19(18) . . ? C18 C13 H13A 105.0 . . ? C14 C13 H13A 105.0 . . ? P1 C13 H13A 105.0 . . ? C15 C14 C13 108.8(2) . . ? C15 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C14 111.3(2) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 111.9(2) . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 111.3(2) . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C13 C18 C17 109.5(2) . . ? C13 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? C13 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? Pt1 Cl2 Pt1 95.73(2) . 5_756 ? C13 P1 C7 112.71(12) . . ? C13 P1 C1 105.13(12) . . ? C7 P1 C1 104.86(12) . . ? C13 P1 Pt1 112.47(9) . . ? C7 P1 Pt1 111.10(8) . . ? C1 P1 Pt1 110.09(9) . . ? P1 Pt1 Cl1 93.79(3) . . ? P1 Pt1 Cl2 94.15(2) . . ? Cl1 Pt1 Cl2 172.05(2) . . ? P1 Pt1 Cl2 177.08(2) . 5_756 ? Cl1 Pt1 Cl2 87.78(2) . 5_756 ? Cl2 Pt1 Cl2 84.27(2) . 5_756 ? C20 C19 C20 119.8(5) 2_556 . ? C20 C19 H19A 120.1 2_556 . ? C20 C19 H19A 120.1 . . ? C19 C20 C21 119.9(4) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C22 C21 C20 121.3(4) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C21 117.9(5) 2_556 . ? C21 C22 C23 121.1(2) 2_556 . ? C21 C22 C23 121.1(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.876 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.105 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 618544' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C36 H30 B Cl3 P2 Pt' _chemical_formula_sum 'C36 H30 B Cl3 P2 Pt' _chemical_formula_weight 836.79 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' Cl Cl 0.1484 0.1585 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.471(6) _cell_length_b 11.886(2) _cell_length_c 19.635(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.45(3) _cell_angle_gamma 90.00 _cell_volume 6534(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21676 _cell_measurement_theta_min 2.205 _cell_measurement_theta_max 27.482 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method none _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 4.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.315 _exptl_absorpt_correction_T_max 0.393 _exptl_absorpt_process_details 'SADABS V2.1 (BUCKER AXS, 2001)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36654 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7502 _reflns_number_gt 7166 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0195P)^2^+14.9407P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7502 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0446 _refine_ls_wR_factor_gt 0.0439 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _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 Pt1 Pt 0.129701(3) 0.828043(6) 0.327922(4) 0.01055(3) Uani 1 1 d . . . Cl1 Cl 0.18159(2) 0.85401(5) 0.24319(3) 0.01773(10) Uani 1 1 d . . . P1 P 0.129084(18) 1.01871(4) 0.34789(3) 0.01044(10) Uani 1 1 d . . . P2 P 0.14473(2) 0.63964(5) 0.31795(3) 0.01323(11) Uani 1 1 d . . . C7 C 0.10715(8) 1.06443(17) 0.42538(10) 0.0119(4) Uani 1 1 d . . . C19 C 0.20827(8) 0.62347(18) 0.34808(11) 0.0153(4) Uani 1 1 d . . . C11 C 0.04202(8) 1.10602(18) 0.48474(11) 0.0156(4) Uani 1 1 d . . . H11 H 0.0088 1.1156 0.4839 0.019 Uiso 1 1 calc R . . C23 C 0.28870(9) 0.6108(2) 0.32644(12) 0.0236(5) Uani 1 1 d . . . H23 H 0.3101 0.5997 0.2951 0.028 Uiso 1 1 calc R . . C2 C 0.22771(8) 1.0067(2) 0.38895(11) 0.0194(5) Uani 1 1 d . . . H2 H 0.2226 0.9286 0.3948 0.023 Uiso 1 1 calc R . . C8 C 0.13944(8) 1.07914(18) 0.48777(11) 0.0144(4) Uani 1 1 d . . . H8 H 0.1727 1.0703 0.4889 0.017 Uiso 1 1 calc R . . C17 C 0.06599(8) 1.1155(2) 0.15408(11) 0.0169(4) Uani 1 1 d . . . H17 H 0.0619 1.0845 0.1088 0.020 Uiso 1 1 calc R . . C9 C 0.12271(8) 1.10672(18) 0.54798(11) 0.0160(4) Uani 1 1 d . . . H9 H 0.1446 1.1160 0.5903 0.019 Uiso 1 1 calc R . . C25 C 0.13013(8) 0.58055(19) 0.23123(11) 0.0164(4) Uani 1 1 d . . . C13 C 0.09509(7) 1.09879(17) 0.27670(10) 0.0118(4) Uani 1 1 d . . . C24 C 0.23995(8) 0.6077(2) 0.30225(11) 0.0194(5) Uani 1 1 d . . . H24 H 0.2280 0.5949 0.2545 0.023 Uiso 1 1 calc R . . C4 C 0.28130(9) 1.1638(3) 0.39645(14) 0.0308(6) Uani 1 1 d . . . H4 H 0.3127 1.1934 0.4079 0.037 Uiso 1 1 calc R . . C10 C 0.07441(8) 1.12066(18) 0.54632(11) 0.0157(4) Uani 1 1 d . . . H10 H 0.0632 1.1404 0.5874 0.019 Uiso 1 1 calc R . . C28 C 0.09990(10) 0.4833(2) 0.10216(12) 0.0267(5) Uani 1 1 d . . . H28 H 0.0896 0.4501 0.0580 0.032 Uiso 1 1 calc R . . C22 C 0.30665(9) 0.6297(2) 0.39558(12) 0.0223(5) Uani 1 1 d . . . H22 H 0.3402 0.6321 0.4117 0.027 Uiso 1 1 calc R . . C18 C 0.08826(8) 1.05289(18) 0.21012(11) 0.0143(4) Uani 1 1 d . . . H18 H 0.0989 0.9787 0.2033 0.017 Uiso 1 1 calc R . . C1 C 0.18938(7) 1.07674(19) 0.36267(10) 0.0144(4) Uani 1 1 d . . . C14 C 0.07852(8) 1.20744(19) 0.28605(11) 0.0153(4) Uani 1 1 d . . . H14 H 0.0828 1.2393 0.3311 0.018 Uiso 1 1 calc R . . C30 C 0.09873(9) 0.6381(2) 0.18070(12) 0.0199(5) Uani 1 1 d . . . H30 H 0.0877 0.7109 0.1901 0.024 Uiso 1 1 calc R . . C29 C 0.08345(9) 0.5885(2) 0.11621(12) 0.0250(5) Uani 1 1 d . . . H29 H 0.0616 0.6272 0.0818 0.030 Uiso 1 1 calc R . . C20 C 0.22655(9) 0.6429(2) 0.41835(12) 0.0205(5) Uani 1 1 d . . . H20 H 0.2054 0.6544 0.4500 0.025 Uiso 1 1 calc R . . C21 C 0.27549(9) 0.6452(2) 0.44156(12) 0.0234(5) Uani 1 1 d . . . H21 H 0.2878 0.6575 0.4893 0.028 Uiso 1 1 calc R . . C12 C 0.05843(8) 1.07735(18) 0.42450(11) 0.0143(4) Uani 1 1 d . . . H12 H 0.0363 1.0665 0.3826 0.017 Uiso 1 1 calc R . . C15 C 0.05585(8) 1.26865(19) 0.22941(12) 0.0180(4) Uani 1 1 d . . . H15 H 0.0445 1.3423 0.2358 0.022 Uiso 1 1 calc R . . C5 C 0.24357(10) 1.2339(2) 0.36957(14) 0.0300(6) Uani 1 1 d . . . H5 H 0.2492 1.3113 0.3622 0.036 Uiso 1 1 calc R . . C26 C 0.14639(9) 0.47408(19) 0.21712(12) 0.0203(5) Uani 1 1 d . . . H26 H 0.1677 0.4343 0.2517 0.024 Uiso 1 1 calc R . . C3 C 0.27328(9) 1.0516(2) 0.40659(12) 0.0263(5) Uani 1 1 d . . . H3 H 0.2992 1.0043 0.4259 0.032 Uiso 1 1 calc R . . C6 C 0.19749(9) 1.1907(2) 0.35333(12) 0.0211(5) Uani 1 1 d . . . H6 H 0.1715 1.2390 0.3358 0.025 Uiso 1 1 calc R . . C27 C 0.13134(10) 0.4263(2) 0.15216(13) 0.0250(5) Uani 1 1 d . . . H27 H 0.1427 0.3542 0.1422 0.030 Uiso 1 1 calc R . . Cl2 Cl 0.01919(2) 0.81869(5) 0.35035(4) 0.02734(13) Uani 1 1 d . . . Cl3 Cl 0.09180(2) 0.77042(5) 0.47639(3) 0.02787(13) Uani 1 1 d . . . C31 C 0.11446(8) 0.53897(18) 0.36520(11) 0.0163(4) Uani 1 1 d . . . C16 C 0.04967(8) 1.22280(19) 0.16339(11) 0.0173(4) Uani 1 1 d . . . H16 H 0.0343 1.2651 0.1247 0.021 Uiso 1 1 calc R . . C36 C 0.13787(9) 0.46112(19) 0.41265(11) 0.0198(5) Uani 1 1 d . . . H36 H 0.1718 0.4587 0.4226 0.024 Uiso 1 1 calc R . . C32 C 0.06462(9) 0.54010(19) 0.35049(12) 0.0200(5) Uani 1 1 d . . . H32 H 0.0485 0.5920 0.3175 0.024 Uiso 1 1 calc R . . B1 B 0.08131(9) 0.8050(2) 0.38679(13) 0.0156(5) Uani 1 1 d . . . C33 C 0.03839(9) 0.4661(2) 0.38359(13) 0.0235(5) Uani 1 1 d . . . H33 H 0.0045 0.4676 0.3735 0.028 Uiso 1 1 calc R . . C35 C 0.11134(10) 0.3867(2) 0.44550(12) 0.0255(5) Uani 1 1 d . . . H35 H 0.1272 0.3335 0.4777 0.031 Uiso 1 1 calc R . . C34 C 0.06207(10) 0.3903(2) 0.43138(12) 0.0259(5) Uani 1 1 d . . . H34 H 0.0443 0.3402 0.4546 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01415(5) 0.00886(4) 0.00961(4) 0.00111(3) 0.00473(3) 0.00171(3) Cl1 0.0237(3) 0.0154(2) 0.0173(2) 0.00342(19) 0.0123(2) 0.0043(2) P1 0.0124(2) 0.0102(2) 0.0093(2) 0.00060(19) 0.00356(18) 0.00083(19) P2 0.0195(3) 0.0102(2) 0.0109(2) 0.00148(19) 0.0049(2) 0.0024(2) C7 0.0178(10) 0.0083(9) 0.0106(9) 0.0017(7) 0.0056(8) -0.0003(8) C19 0.0196(11) 0.0118(10) 0.0149(10) 0.0023(8) 0.0039(8) 0.0041(8) C11 0.0170(10) 0.0125(10) 0.0190(10) 0.0023(8) 0.0083(8) 0.0004(8) C23 0.0255(12) 0.0242(13) 0.0228(12) -0.0012(9) 0.0087(9) 0.0070(10) C2 0.0179(11) 0.0263(12) 0.0146(10) 0.0013(9) 0.0044(8) 0.0022(9) C8 0.0168(10) 0.0130(10) 0.0142(10) 0.0021(8) 0.0050(8) 0.0017(8) C17 0.0170(10) 0.0202(11) 0.0127(10) -0.0019(8) 0.0006(8) 0.0011(9) C9 0.0249(11) 0.0133(10) 0.0098(9) 0.0019(8) 0.0029(8) -0.0013(9) C25 0.0225(11) 0.0149(11) 0.0132(10) -0.0005(8) 0.0068(8) -0.0029(9) C13 0.0121(9) 0.0115(10) 0.0119(9) 0.0022(7) 0.0028(7) -0.0006(8) C24 0.0245(12) 0.0194(11) 0.0144(10) 0.0002(8) 0.0041(9) 0.0057(9) C4 0.0191(12) 0.0509(18) 0.0227(12) -0.0010(11) 0.0046(10) -0.0135(11) C10 0.0262(12) 0.0102(10) 0.0134(10) 0.0012(8) 0.0108(8) -0.0004(8) C28 0.0383(14) 0.0263(13) 0.0176(11) -0.0067(10) 0.0104(10) -0.0155(11) C22 0.0212(12) 0.0209(12) 0.0238(12) 0.0018(9) 0.0016(9) 0.0045(10) C18 0.0172(10) 0.0111(10) 0.0147(10) -0.0012(8) 0.0029(8) 0.0012(8) C1 0.0131(10) 0.0207(11) 0.0102(9) -0.0001(8) 0.0040(7) -0.0020(8) C14 0.0192(11) 0.0140(10) 0.0134(10) -0.0021(8) 0.0046(8) 0.0002(8) C30 0.0266(12) 0.0158(11) 0.0179(11) 0.0007(9) 0.0053(9) -0.0008(9) C29 0.0322(13) 0.0254(13) 0.0162(11) 0.0008(9) 0.0008(9) -0.0062(11) C20 0.0272(12) 0.0192(11) 0.0161(11) -0.0009(9) 0.0066(9) 0.0023(9) C21 0.0288(13) 0.0238(12) 0.0163(11) 0.0009(9) 0.0001(9) 0.0032(10) C12 0.0169(10) 0.0125(10) 0.0140(10) 0.0014(8) 0.0043(8) 0.0001(8) C15 0.0230(11) 0.0113(10) 0.0202(11) 0.0010(8) 0.0048(9) 0.0026(8) C5 0.0305(14) 0.0306(14) 0.0294(13) 0.0014(11) 0.0071(11) -0.0145(11) C26 0.0298(12) 0.0139(11) 0.0193(11) 0.0006(8) 0.0097(9) -0.0007(9) C3 0.0153(11) 0.0458(16) 0.0182(11) 0.0019(10) 0.0044(9) 0.0027(11) C6 0.0211(12) 0.0231(12) 0.0201(11) 0.0017(9) 0.0058(9) -0.0044(9) C27 0.0372(14) 0.0141(11) 0.0274(12) -0.0057(9) 0.0160(11) -0.0071(10) Cl2 0.0161(3) 0.0283(3) 0.0391(3) -0.0082(3) 0.0089(2) -0.0012(2) Cl3 0.0459(4) 0.0255(3) 0.0149(2) 0.0005(2) 0.0128(2) -0.0072(3) C31 0.0262(12) 0.0097(10) 0.0141(10) -0.0007(8) 0.0061(8) 0.0011(8) C16 0.0175(10) 0.0167(11) 0.0165(10) 0.0034(8) -0.0001(8) 0.0009(9) C36 0.0310(13) 0.0125(11) 0.0158(10) -0.0015(8) 0.0036(9) 0.0005(9) C32 0.0286(12) 0.0118(11) 0.0214(11) 0.0005(8) 0.0088(9) -0.0002(9) B1 0.0193(12) 0.0123(11) 0.0169(11) -0.0008(9) 0.0077(9) -0.0013(9) C33 0.0302(13) 0.0165(11) 0.0263(12) -0.0059(9) 0.0115(10) -0.0072(10) C35 0.0504(16) 0.0122(11) 0.0131(10) 0.0016(8) 0.0039(10) -0.0041(11) C34 0.0469(16) 0.0170(12) 0.0159(11) -0.0034(9) 0.0109(10) -0.0130(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 Pt1 B1 1.972(3) . ? Pt1 P2 2.2950(7) . ? Pt1 P1 2.3005(7) . ? Pt1 Cl1 2.4368(8) . ? P1 C13 1.818(2) . ? P1 C1 1.824(2) . ? P1 C7 1.829(2) . ? P2 C19 1.809(2) . ? P2 C25 1.819(2) . ? P2 C31 1.824(2) . ? C7 C12 1.393(3) . ? C7 C8 1.403(3) . ? C19 C24 1.398(3) . ? C19 C20 1.403(3) . ? C11 C12 1.391(3) . ? C11 C10 1.392(3) . ? C11 H11 0.9500 . ? C23 C22 1.380(3) . ? C23 C24 1.384(3) . ? C23 H23 0.9500 . ? C2 C3 1.387(3) . ? C2 C1 1.395(3) . ? C2 H2 0.9500 . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C17 C16 1.380(3) . ? C17 C18 1.384(3) . ? C17 H17 0.9500 . ? C9 C10 1.380(3) . ? C9 H9 0.9500 . ? C25 C30 1.389(3) . ? C25 C26 1.392(3) . ? C13 C18 1.397(3) . ? C13 C14 1.398(3) . ? C24 H24 0.9500 . ? C4 C3 1.373(4) . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C10 H10 0.9500 . ? C28 C29 1.380(4) . ? C28 C27 1.380(4) . ? C28 H28 0.9500 . ? C22 C21 1.388(4) . ? C22 H22 0.9500 . ? C18 H18 0.9500 . ? C1 C6 1.391(3) . ? C14 C15 1.386(3) . ? C14 H14 0.9500 . ? C30 C29 1.393(3) . ? C30 H30 0.9500 . ? C29 H29 0.9500 . ? C20 C21 1.385(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C12 H12 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C5 C6 1.391(3) . ? C5 H5 0.9500 . ? C26 C27 1.391(3) . ? C26 H26 0.9500 . ? C3 H3 0.9500 . ? C6 H6 0.9500 . ? C27 H27 0.9500 . ? Cl2 B1 1.791(3) . ? Cl3 B1 1.779(3) . ? C31 C36 1.394(3) . ? C31 C32 1.396(3) . ? C16 H16 0.9500 . ? C36 C35 1.394(3) . ? C36 H36 0.9500 . ? C32 C33 1.389(3) . ? C32 H32 0.9500 . ? C33 C34 1.385(4) . ? C33 H33 0.9500 . ? C35 C34 1.380(4) . ? C35 H35 0.9500 . ? C34 H34 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Pt1 P2 94.33(7) . . ? B1 Pt1 P1 90.52(7) . . ? P2 Pt1 P1 169.45(2) . . ? B1 Pt1 Cl1 173.03(8) . . ? P2 Pt1 Cl1 85.40(2) . . ? P1 Pt1 Cl1 90.91(4) . . ? C13 P1 C1 106.19(10) . . ? C13 P1 C7 105.64(10) . . ? C1 P1 C7 102.05(10) . . ? C13 P1 Pt1 113.84(7) . . ? C1 P1 Pt1 111.32(8) . . ? C7 P1 Pt1 116.67(7) . . ? C19 P2 C25 108.09(11) . . ? C19 P2 C31 107.51(10) . . ? C25 P2 C31 100.02(10) . . ? C19 P2 Pt1 105.47(7) . . ? C25 P2 Pt1 116.24(8) . . ? C31 P2 Pt1 118.96(7) . . ? C12 C7 C8 119.37(19) . . ? C12 C7 P1 120.80(16) . . ? C8 C7 P1 119.67(16) . . ? C24 C19 C20 119.2(2) . . ? C24 C19 P2 121.85(17) . . ? C20 C19 P2 118.36(17) . . ? C12 C11 C10 119.8(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C22 C23 C24 120.8(2) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C3 C2 C1 119.7(2) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C9 C8 C7 120.0(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C16 C17 C18 120.6(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C30 C25 C26 120.0(2) . . ? C30 C25 P2 119.12(17) . . ? C26 C25 P2 120.62(17) . . ? C18 C13 C14 119.36(19) . . ? C18 C13 P1 118.64(16) . . ? C14 C13 P1 121.86(16) . . ? C23 C24 C19 120.0(2) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C3 C4 C5 120.1(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C29 C28 C27 120.1(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C17 C18 C13 120.0(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C6 C1 C2 119.5(2) . . ? C6 C1 P1 121.39(17) . . ? C2 C1 P1 118.94(17) . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C25 C30 C29 119.7(2) . . ? C25 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C21 C20 C19 119.9(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.4(2) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C11 C12 C7 120.3(2) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C27 C26 C25 119.7(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C4 C3 C2 120.7(2) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C6 C1 120.1(2) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C28 C27 C26 120.3(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C36 C31 C32 119.3(2) . . ? C36 C31 P2 124.26(18) . . ? C32 C31 P2 116.41(17) . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C31 C36 C35 119.8(2) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C33 C32 C31 120.6(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? Cl3 B1 Cl2 113.12(14) . . ? Cl3 B1 Pt1 127.03(15) . . ? Cl2 B1 Pt1 119.85(14) . . ? C34 C33 C32 119.5(2) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C34 C35 C36 120.3(2) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C34 C33 120.5(2) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.504 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.088 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 618545' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C26 H26 B Cl3 P2 Pt' _chemical_formula_sum 'C26 H26 B Cl3 P2 Pt' _chemical_formula_weight 712.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 14.938(3) _cell_length_b 10.071(2) _cell_length_c 18.279(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.18(3) _cell_angle_gamma 90.00 _cell_volume 2697.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 5.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.225 _exptl_absorpt_correction_T_max 0.259 _exptl_absorpt_process_details 'SADABS v2.1 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30316 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6189 _reflns_number_gt 5803 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0440P)^2^+0.5581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6189 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.004 _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 C12 C 0.4067(2) 1.1473(3) 0.75153(17) 0.0235(6) Uani 1 1 d . . . H12 H 0.3583 1.1105 0.7719 0.028 Uiso 1 1 calc R . . Pt1 Pt 0.524689(7) 0.803057(9) 0.839031(5) 0.01376(5) Uani 1 1 d . . . P2 P 0.58794(5) 0.73658(7) 0.95826(4) 0.01353(13) Uani 1 1 d . . . Cl1 Cl 0.41498(5) 0.62047(7) 0.82888(4) 0.02286(15) Uani 1 1 d . . . P1 P 0.45129(5) 0.88521(7) 0.72607(4) 0.01536(14) Uani 1 1 d . . . C20 C 0.66190(18) 0.8555(3) 1.01589(14) 0.0144(5) Uani 1 1 d . . . C13 C 0.32913(19) 0.8552(3) 0.70650(17) 0.0223(6) Uani 1 1 d . . . H13A H 0.3018 0.8974 0.6591 0.033 Uiso 1 1 calc R . . H13B H 0.3020 0.8928 0.7466 0.033 Uiso 1 1 calc R . . H13C H 0.3176 0.7594 0.7032 0.033 Uiso 1 1 calc R . . C26 C 0.5015(2) 0.6981(3) 1.01204(18) 0.0202(6) Uani 1 1 d . . . H26A H 0.4672 0.6195 0.9910 0.030 Uiso 1 1 calc R . . H26B H 0.4598 0.7736 1.0104 0.030 Uiso 1 1 calc R . . H26C H 0.5307 0.6803 1.0639 0.030 Uiso 1 1 calc R . . C14 C 0.65718(18) 0.5888(3) 0.96143(16) 0.0165(5) Uani 1 1 d . . . C7 C 0.4621(2) 1.0645(3) 0.71784(15) 0.0194(6) Uani 1 1 d . . . C5 C 0.4738(2) 0.8029(3) 0.51125(18) 0.0250(7) Uani 1 1 d . . . H5 H 0.4494 0.8359 0.4628 0.030 Uiso 1 1 calc R . . C2 C 0.5465(2) 0.7069(3) 0.65304(18) 0.0199(6) Uani 1 1 d . . . H2 H 0.5722 0.6751 0.7015 0.024 Uiso 1 1 calc R . . C21 C 0.75556(19) 0.8534(3) 1.01805(16) 0.0190(6) Uani 1 1 d . . . H21 H 0.7811 0.7863 0.9919 0.023 Uiso 1 1 calc R . . C25 C 0.62517(19) 0.9554(3) 1.05402(15) 0.0183(5) Uani 1 1 d . . . H25 H 0.5615 0.9570 1.0535 0.022 Uiso 1 1 calc R . . C1 C 0.4880(2) 0.8151(3) 0.64508(17) 0.0174(6) Uani 1 1 d . . . C4 C 0.5308(2) 0.6934(3) 0.51994(19) 0.0262(7) Uani 1 1 d . . . H4 H 0.5448 0.6510 0.4771 0.031 Uiso 1 1 calc R . . C6 C 0.4524(2) 0.8644(3) 0.57392(16) 0.0206(6) Uani 1 1 d . . . H6 H 0.4137 0.9401 0.5683 0.025 Uiso 1 1 calc R . . C8 C 0.5325(2) 1.1192(3) 0.68832(16) 0.0235(6) Uani 1 1 d . . . H8 H 0.5708 1.0634 0.6659 0.028 Uiso 1 1 calc R . . C22 C 0.81182(19) 0.9485(3) 1.05818(17) 0.0230(6) Uani 1 1 d . . . H22 H 0.8759 0.9448 1.0605 0.028 Uiso 1 1 calc R . . C19 C 0.6823(2) 0.5392(3) 0.89713(18) 0.0289(7) Uani 1 1 d . . . H19 H 0.6644 0.5838 0.8508 0.035 Uiso 1 1 calc R . . C9 C 0.5473(2) 1.2565(3) 0.69138(18) 0.0282(7) Uani 1 1 d . . . H9 H 0.5947 1.2941 0.6701 0.034 Uiso 1 1 calc R . . C23 C 0.7749(2) 1.0489(3) 1.09497(16) 0.0224(6) Uani 1 1 d . . . H23 H 0.8135 1.1150 1.1216 0.027 Uiso 1 1 calc R . . C15 C 0.68557(19) 0.5227(3) 1.02938(16) 0.0204(6) Uani 1 1 d . . . H15 H 0.6698 0.5572 1.0736 0.024 Uiso 1 1 calc R . . C3 C 0.5677(2) 0.6444(3) 0.59052(18) 0.0253(6) Uani 1 1 d . . . H3 H 0.6070 0.5693 0.5960 0.030 Uiso 1 1 calc R . . Cl3 Cl 0.62710(5) 1.09796(7) 0.87959(4) 0.02579(16) Uani 1 1 d . . . Cl2 Cl 0.72067(5) 0.89596(9) 0.80314(5) 0.03502(19) Uani 1 1 d . . . C11 C 0.4225(3) 1.2827(3) 0.75522(19) 0.0291(7) Uani 1 1 d . . . H11 H 0.3848 1.3386 0.7783 0.035 Uiso 1 1 calc R . . C24 C 0.6814(2) 1.0528(3) 1.09291(16) 0.0213(6) Uani 1 1 d . . . H24 H 0.6559 1.1216 1.1179 0.026 Uiso 1 1 calc R . . C10 C 0.4924(2) 1.3374(3) 0.72561(19) 0.0299(7) Uani 1 1 d . . . H10 H 0.5030 1.4304 0.7287 0.036 Uiso 1 1 calc R . . B1 B 0.6231(2) 0.9370(3) 0.84203(17) 0.0184(6) Uani 1 1 d . . . C17 C 0.7602(2) 0.3582(3) 0.9688(2) 0.0320(8) Uani 1 1 d . . . H17 H 0.7950 0.2788 0.9710 0.038 Uiso 1 1 calc R . . C18 C 0.7341(3) 0.4232(4) 0.9016(2) 0.0384(9) Uani 1 1 d . . . H18 H 0.7514 0.3886 0.8581 0.046 Uiso 1 1 calc R . . C16 C 0.7366(2) 0.4072(3) 1.03236(19) 0.0254(6) Uani 1 1 d . . . H16 H 0.7551 0.3620 1.0784 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C12 0.0256(15) 0.0225(15) 0.0217(15) 0.0023(12) 0.0028(12) 0.0057(12) Pt1 0.01500(7) 0.01415(7) 0.01153(7) 0.00027(3) 0.00105(4) 0.00121(3) P2 0.0138(3) 0.0135(3) 0.0125(3) 0.0004(3) 0.0007(3) 0.0015(3) Cl1 0.0293(4) 0.0177(3) 0.0200(3) -0.0006(3) 0.0007(3) -0.0059(3) P1 0.0166(3) 0.0165(3) 0.0122(3) 0.0013(3) 0.0008(3) 0.0005(3) C20 0.0173(13) 0.0140(12) 0.0109(12) 0.0013(10) -0.0001(10) 0.0002(10) C13 0.0162(14) 0.0307(16) 0.0183(14) 0.0023(12) -0.0006(11) 0.0001(12) C26 0.0175(14) 0.0254(16) 0.0183(16) 0.0008(11) 0.0051(12) 0.0006(11) C14 0.0126(12) 0.0149(12) 0.0209(14) -0.0011(11) 0.0005(10) 0.0017(10) C7 0.0245(14) 0.0177(13) 0.0132(13) 0.0028(10) -0.0031(11) 0.0021(11) C5 0.0274(17) 0.0308(18) 0.0165(16) -0.0003(11) 0.0032(13) -0.0070(12) C2 0.0193(15) 0.0207(15) 0.0190(15) 0.0011(11) 0.0023(12) -0.0016(11) C21 0.0193(14) 0.0150(13) 0.0218(15) 0.0012(11) 0.0016(11) 0.0030(11) C25 0.0183(13) 0.0205(13) 0.0152(13) -0.0005(11) 0.0013(11) 0.0030(11) C1 0.0188(14) 0.0180(14) 0.0154(13) -0.0018(10) 0.0037(11) -0.0055(10) C4 0.0298(18) 0.0288(17) 0.0229(17) -0.0088(12) 0.0120(14) -0.0065(13) C6 0.0216(14) 0.0211(14) 0.0183(14) 0.0005(11) 0.0024(11) -0.0019(12) C8 0.0302(16) 0.0226(15) 0.0169(14) -0.0014(11) 0.0022(12) -0.0025(13) C22 0.0152(13) 0.0223(14) 0.0291(16) 0.0019(12) -0.0016(12) -0.0007(11) C19 0.0364(18) 0.0276(16) 0.0225(16) -0.0012(13) 0.0056(13) 0.0115(14) C9 0.0337(18) 0.0264(17) 0.0234(16) 0.0036(13) 0.0023(13) -0.0068(14) C23 0.0248(15) 0.0184(14) 0.0201(15) 0.0008(11) -0.0048(12) -0.0013(12) C15 0.0185(14) 0.0191(14) 0.0212(15) 0.0003(11) -0.0021(11) -0.0018(11) C3 0.0222(15) 0.0242(15) 0.0308(17) -0.0037(13) 0.0083(13) 0.0009(12) Cl3 0.0336(4) 0.0208(3) 0.0218(4) -0.0010(3) 0.0025(3) -0.0054(3) Cl2 0.0230(4) 0.0469(5) 0.0382(5) -0.0065(4) 0.0133(3) -0.0040(3) C11 0.0368(19) 0.0248(16) 0.0234(17) -0.0002(13) 0.0000(14) 0.0093(14) C24 0.0279(15) 0.0198(14) 0.0160(14) -0.0033(11) 0.0036(11) 0.0013(12) C10 0.042(2) 0.0184(14) 0.0247(17) 0.0025(13) -0.0059(14) 0.0004(14) B1 0.0179(15) 0.0243(16) 0.0120(14) 0.0032(12) 0.0003(12) 0.0038(12) C17 0.0214(16) 0.0217(15) 0.051(2) -0.0026(15) 0.0012(14) 0.0099(13) C18 0.047(2) 0.0343(19) 0.036(2) -0.0097(15) 0.0136(17) 0.0146(17) C16 0.0196(14) 0.0169(14) 0.0364(18) 0.0048(13) -0.0031(13) 0.0006(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 C12 C11 1.384(5) . ? C12 C7 1.398(4) . ? C12 H12 0.9500 . ? Pt1 B1 1.988(3) . ? Pt1 P1 2.2961(9) . ? Pt1 P2 2.3005(9) . ? Pt1 Cl1 2.4461(8) . ? P2 C14 1.807(3) . ? P2 C26 1.810(3) . ? P2 C20 1.821(3) . ? P1 C13 1.815(3) . ? P1 C1 1.818(3) . ? P1 C7 1.821(3) . ? C20 C21 1.392(4) . ? C20 C25 1.395(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C14 C19 1.394(4) . ? C14 C15 1.400(4) . ? C7 C8 1.386(4) . ? C5 C4 1.383(4) . ? C5 C6 1.393(4) . ? C5 H5 0.9500 . ? C2 C1 1.386(4) . ? C2 C3 1.394(4) . ? C2 H2 0.9500 . ? C21 C22 1.387(4) . ? C21 H21 0.9500 . ? C25 C24 1.393(4) . ? C25 H25 0.9500 . ? C1 C6 1.397(4) . ? C4 C3 1.392(5) . ? C4 H4 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.399(5) . ? C8 H8 0.9500 . ? C22 C23 1.387(4) . ? C22 H22 0.9500 . ? C19 C18 1.395(4) . ? C19 H19 0.9500 . ? C9 C10 1.388(5) . ? C9 H9 0.9500 . ? C23 C24 1.391(4) . ? C23 H23 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C3 H3 0.9500 . ? Cl3 B1 1.757(3) . ? Cl2 B1 1.789(3) . ? C11 C10 1.381(5) . ? C11 H11 0.9500 . ? C24 H24 0.9500 . ? C10 H10 0.9500 . ? C17 C16 1.371(5) . ? C17 C18 1.378(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C16 H16 0.9500 . ? 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 C11 C12 C7 120.0(3) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? B1 Pt1 P1 90.12(9) . . ? B1 Pt1 P2 90.32(9) . . ? P1 Pt1 P2 173.51(2) . . ? B1 Pt1 Cl1 173.25(9) . . ? P1 Pt1 Cl1 90.37(3) . . ? P2 Pt1 Cl1 89.95(3) . . ? C14 P2 C26 105.69(13) . . ? C14 P2 C20 104.13(13) . . ? C26 P2 C20 104.09(14) . . ? C14 P2 Pt1 113.42(10) . . ? C26 P2 Pt1 111.81(11) . . ? C20 P2 Pt1 116.64(9) . . ? C13 P1 C1 103.01(14) . . ? C13 P1 C7 104.48(14) . . ? C1 P1 C7 105.80(13) . . ? C13 P1 Pt1 113.82(10) . . ? C1 P1 Pt1 115.18(10) . . ? C7 P1 Pt1 113.39(9) . . ? C21 C20 C25 119.2(3) . . ? C21 C20 P2 120.0(2) . . ? C25 C20 P2 120.7(2) . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C19 C14 C15 119.5(3) . . ? C19 C14 P2 120.9(2) . . ? C15 C14 P2 119.5(2) . . ? C8 C7 C12 119.5(3) . . ? C8 C7 P1 120.8(2) . . ? C12 C7 P1 119.0(2) . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C2 C3 120.5(3) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C24 C25 C20 120.4(3) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C2 C1 C6 119.7(3) . . ? C2 C1 P1 120.2(2) . . ? C6 C1 P1 120.0(2) . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C5 C6 C1 120.0(3) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C7 C8 C9 120.2(3) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C14 C19 C18 119.2(3) . . ? C14 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C22 C23 C24 119.9(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? Cl3 B1 Cl2 113.57(18) . . ? Cl3 B1 Pt1 127.27(17) . . ? Cl2 B1 Pt1 119.16(18) . . ? C16 C17 C18 120.6(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C17 C16 C15 119.9(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.156 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.128 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 618546' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C16 H22 B Cl3 P2 Pt' _chemical_formula_sum 'C16 H22 B Cl3 P2 Pt' _chemical_formula_weight 588.53 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' Cl Cl 0.1484 0.1585 '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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.466(4) _cell_length_b 6.0751(12) _cell_length_c 21.219(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.81(3) _cell_angle_gamma 90.00 _cell_volume 2059.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 7.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.147 _exptl_absorpt_correction_T_max 0.23 _exptl_absorpt_process_details 'SADABS V2.1 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23631 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9398 _reflns_number_gt 8866 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0276P)^2^+1.9092P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(5) _refine_ls_number_reflns 9398 _refine_ls_number_parameters 423 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _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 C25 C 0.2647(4) 0.1099(10) 0.6868(3) 0.0264(14) Uani 1 1 d . . . H25A H 0.2083 0.0468 0.6707 0.040 Uiso 1 1 calc R . . H25B H 0.2695 0.2328 0.7181 0.040 Uiso 1 1 calc R . . H25C H 0.3061 -0.0032 0.7111 0.040 Uiso 1 1 calc R . . Pt1 Pt 0.089806(12) 0.93329(2) 0.871356(10) 0.01268(8) Uani 1 1 d . . . Pt2 Pt 0.407519(12) 0.38268(3) 0.632535(10) 0.01250(8) Uani 1 1 d . . . Cl1 Cl 0.12451(9) 0.9397(4) 0.99478(7) 0.0237(4) Uani 1 1 d . . . Cl4 Cl 0.37344(9) 0.3546(3) 0.50925(7) 0.0235(4) Uani 1 1 d . . . P2 P -0.03301(9) 1.1102(2) 0.85566(7) 0.0138(3) Uani 1 1 d . . . P1 P 0.21481(9) 0.7544(2) 0.89474(8) 0.0153(3) Uani 1 1 d . . . P4 P 0.28330(9) 0.2082(2) 0.61354(8) 0.0170(3) Uani 1 1 d . . . P3 P 0.52742(9) 0.5648(2) 0.64244(7) 0.0140(3) Uani 1 1 d . . . B1 B 0.0640(4) 0.9451(12) 0.7724(3) 0.0131(13) Uani 1 1 d . . . B2 B 0.4351(4) 0.4148(12) 0.7318(3) 0.0151(14) Uani 1 1 d . . . C28 C 0.1609(4) 0.4036(12) 0.4960(3) 0.0208(14) Uani 1 1 d . . . H28 H 0.1866 0.3247 0.4710 0.025 Uiso 1 1 calc R . . C3 C 0.3056(3) 0.9300(10) 0.9390(3) 0.0148(12) Uani 1 1 d . . . C27 C 0.1930(3) 0.3832(12) 0.5676(3) 0.0171(12) Uani 1 1 d . . . C18 C 0.5840(4) 0.4226(10) 0.5991(3) 0.0229(13) Uani 1 1 d . . . H18A H 0.5462 0.3943 0.5511 0.034 Uiso 1 1 calc R . . H18B H 0.6056 0.2826 0.6225 0.034 Uiso 1 1 calc R . . H18C H 0.6308 0.5144 0.6004 0.034 Uiso 1 1 calc R . . C10 C -0.0861(4) 0.9896(10) 0.9048(3) 0.0240(13) Uani 1 1 d . . . H10A H -0.0497 0.9968 0.9540 0.036 Uiso 1 1 calc R . . H10B H -0.0995 0.8355 0.8911 0.036 Uiso 1 1 calc R . . H10C H -0.1379 1.0709 0.8959 0.036 Uiso 1 1 calc R . . C26 C 0.2679(4) -0.0384(9) 0.5611(3) 0.0275(13) Uani 1 1 d . . . H26A H 0.3079 -0.1518 0.5875 0.041 Uiso 1 1 calc R . . H26B H 0.2769 -0.0032 0.5195 0.041 Uiso 1 1 calc R . . H26C H 0.2108 -0.0929 0.5480 0.041 Uiso 1 1 calc R . . C9 C -0.0117(4) 1.3921(9) 0.8870(3) 0.0227(13) Uani 1 1 d . . . H9A H -0.0639 1.4626 0.8830 0.034 Uiso 1 1 calc R . . H9B H 0.0123 1.4739 0.8594 0.034 Uiso 1 1 calc R . . H9C H 0.0281 1.3916 0.9353 0.034 Uiso 1 1 calc R . . C32 C 0.1559(3) 0.5059(10) 0.6025(3) 0.0213(12) Uani 1 1 d . . . H32 H 0.1771 0.4967 0.6513 0.026 Uiso 1 1 calc R . . C19 C 0.6066(3) 0.6200(8) 0.7281(3) 0.0139(10) Uani 1 1 d . . . C8 C 0.3409(4) 0.9463(12) 1.0103(3) 0.0189(13) Uani 1 1 d . . . H8 H 0.3180 0.8630 1.0364 0.023 Uiso 1 1 calc R . . C11 C -0.1138(3) 1.1303(9) 0.7682(3) 0.0164(11) Uani 1 1 d . . . C4 C 0.3392(3) 1.0568(9) 0.9017(3) 0.0203(12) Uani 1 1 d . . . H4 H 0.3156 1.0487 0.8529 0.024 Uiso 1 1 calc R . . C31 C 0.0878(4) 0.6428(9) 0.5674(3) 0.0226(12) Uani 1 1 d . . . H31 H 0.0628 0.7252 0.5921 0.027 Uiso 1 1 calc R . . C5 C 0.4065(3) 1.1945(10) 0.9351(3) 0.0231(13) Uani 1 1 d . . . H5 H 0.4287 1.2803 0.9090 0.028 Uiso 1 1 calc R . . C23 C 0.7220(4) 0.5019(12) 0.8314(3) 0.0324(15) Uani 1 1 d . . . H23 H 0.7612 0.3911 0.8557 0.039 Uiso 1 1 calc R . . C29 C 0.0930(4) 0.5355(10) 0.4607(3) 0.0243(13) Uani 1 1 d . . . H29 H 0.0711 0.5419 0.4119 0.029 Uiso 1 1 calc R . . C24 C 0.6651(4) 0.4636(10) 0.7635(3) 0.0272(15) Uani 1 1 d . . . H24 H 0.6669 0.3283 0.7418 0.033 Uiso 1 1 calc R . . C22 C 0.7214(4) 0.6988(10) 0.8629(3) 0.0230(12) Uani 1 1 d . . . H22 H 0.7601 0.7252 0.9089 0.028 Uiso 1 1 calc R . . C13 C -0.2240(4) 0.9679(12) 0.6703(4) 0.0367(16) Uani 1 1 d . . . H13 H -0.2604 0.8475 0.6502 0.044 Uiso 1 1 calc R . . C17 C 0.4996(4) 0.8286(9) 0.5998(3) 0.0207(13) Uani 1 1 d . . . H17A H 0.4794 0.9262 0.6265 0.031 Uiso 1 1 calc R . . H17B H 0.4556 0.8083 0.5535 0.031 Uiso 1 1 calc R . . H17C H 0.5490 0.8942 0.5961 0.031 Uiso 1 1 calc R . . C6 C 0.4416(3) 1.2080(9) 1.0062(3) 0.0229(13) Uani 1 1 d . . . H6 H 0.4878 1.3029 1.0290 0.028 Uiso 1 1 calc R . . C30 C 0.0566(4) 0.6583(9) 0.4958(3) 0.0249(13) Uani 1 1 d . . . H30 H 0.0107 0.7525 0.4715 0.030 Uiso 1 1 calc R . . C14 C -0.2277(4) 1.1500(11) 0.6311(3) 0.0287(14) Uani 1 1 d . . . H14 H -0.2664 1.1563 0.5843 0.034 Uiso 1 1 calc R . . C12 C -0.1673(4) 0.9557(10) 0.7396(4) 0.0307(15) Uani 1 1 d . . . H12 H -0.1658 0.8293 0.7664 0.037 Uiso 1 1 calc R . . C20 C 0.6068(4) 0.8195(10) 0.7601(3) 0.0282(14) Uani 1 1 d . . . H20 H 0.5676 0.9307 0.7363 0.034 Uiso 1 1 calc R . . C21 C 0.6647(4) 0.8564(11) 0.8275(3) 0.0340(15) Uani 1 1 d . . . H21 H 0.6646 0.9934 0.8490 0.041 Uiso 1 1 calc R . . Cl3 Cl 0.08718(10) 1.1742(2) 0.73097(8) 0.0266(3) Uani 1 1 d . . . Cl2 Cl 0.01255(10) 0.7309(2) 0.71189(8) 0.0289(3) Uani 1 1 d . . . Cl6 Cl 0.40741(10) 0.6498(3) 0.76829(8) 0.0302(3) Uani 1 1 d . . . Cl5 Cl 0.48872(11) 0.2149(2) 0.79580(7) 0.0312(4) Uani 1 1 d . . . C2 C 0.2281(4) 0.5165(10) 0.9503(3) 0.0268(13) Uani 1 1 d . . . H2A H 0.1900 0.3991 0.9243 0.040 Uiso 1 1 calc R . . H2B H 0.2155 0.5583 0.9897 0.040 Uiso 1 1 calc R . . H2C H 0.2860 0.4641 0.9668 0.040 Uiso 1 1 calc R . . C1 C 0.2336(4) 0.6396(10) 0.8230(3) 0.0250(13) Uani 1 1 d . . . H1A H 0.2910 0.5833 0.8398 0.037 Uiso 1 1 calc R . . H1B H 0.2258 0.7545 0.7886 0.037 Uiso 1 1 calc R . . H1C H 0.1941 0.5192 0.8021 0.037 Uiso 1 1 calc R . . C16 C -0.1180(4) 1.3142(10) 0.7287(3) 0.0281(14) Uani 1 1 d . . . H16 H -0.0818 1.4354 0.7484 0.034 Uiso 1 1 calc R . . C7 C 0.4092(4) 1.0829(10) 1.0440(3) 0.0243(13) Uani 1 1 d . . . H7 H 0.4335 1.0901 1.0929 0.029 Uiso 1 1 calc R . . C15 C -0.1749(4) 1.3230(12) 0.6603(4) 0.0368(17) Uani 1 1 d . . . H15 H -0.1773 1.4503 0.6336 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C25 0.015(3) 0.034(3) 0.031(4) 0.013(3) 0.010(3) 0.003(2) Pt1 0.00970(13) 0.0142(2) 0.01440(12) 0.00055(8) 0.00516(10) -0.00066(8) Pt2 0.00945(12) 0.0152(2) 0.01306(12) 0.00044(9) 0.00476(10) 0.00087(9) Cl1 0.0163(7) 0.0398(10) 0.0140(6) 0.0023(7) 0.0049(6) 0.0012(7) Cl4 0.0175(7) 0.0388(10) 0.0139(7) -0.0028(7) 0.0061(6) -0.0016(7) P2 0.0115(7) 0.0143(7) 0.0161(7) -0.0004(5) 0.0061(6) -0.0008(5) P1 0.0101(7) 0.0156(7) 0.0188(7) 0.0001(6) 0.0046(6) 0.0001(5) P4 0.0124(7) 0.0170(7) 0.0212(8) 0.0024(6) 0.0065(6) 0.0015(6) P3 0.0114(7) 0.0158(7) 0.0155(7) 0.0002(5) 0.0062(6) -0.0006(5) B1 0.011(3) 0.012(3) 0.016(3) -0.002(2) 0.005(3) -0.001(2) B2 0.014(3) 0.015(4) 0.017(3) 0.002(3) 0.006(3) 0.002(2) C28 0.015(3) 0.022(3) 0.022(3) -0.004(3) 0.004(3) 0.001(3) C3 0.012(3) 0.011(3) 0.022(3) 0.002(2) 0.007(2) 0.003(2) C27 0.007(3) 0.022(3) 0.021(3) 0.000(3) 0.004(2) -0.002(3) C18 0.017(3) 0.033(4) 0.022(3) -0.005(3) 0.012(2) 0.000(3) C10 0.019(3) 0.029(3) 0.028(3) 0.005(3) 0.014(3) 0.000(3) C26 0.020(3) 0.019(3) 0.042(4) -0.007(3) 0.011(3) -0.002(2) C9 0.021(3) 0.020(3) 0.028(3) -0.004(2) 0.010(3) -0.003(2) C32 0.017(3) 0.021(3) 0.024(3) -0.001(2) 0.007(2) -0.007(2) C19 0.011(3) 0.014(2) 0.017(3) 0.002(2) 0.006(2) -0.0008(19) C8 0.016(3) 0.018(3) 0.021(3) 0.000(3) 0.007(3) -0.002(2) C11 0.010(3) 0.019(3) 0.021(3) -0.003(2) 0.008(2) 0.002(2) C4 0.017(3) 0.025(3) 0.019(3) 0.003(2) 0.007(2) 0.002(2) C31 0.019(3) 0.024(3) 0.028(3) 0.000(2) 0.013(3) 0.006(2) C5 0.015(3) 0.025(3) 0.029(3) 0.004(2) 0.009(3) -0.004(2) C23 0.022(3) 0.036(4) 0.026(3) 0.002(3) -0.003(3) 0.009(3) C29 0.020(3) 0.030(3) 0.019(3) 0.003(2) 0.003(3) -0.002(2) C24 0.027(3) 0.017(3) 0.028(3) -0.005(3) 0.001(3) 0.006(3) C22 0.016(3) 0.028(3) 0.021(3) 0.001(2) 0.003(2) -0.004(2) C13 0.022(3) 0.040(4) 0.038(4) -0.013(3) 0.003(3) -0.013(3) C17 0.020(3) 0.021(3) 0.020(3) 0.005(2) 0.007(3) -0.001(2) C6 0.012(3) 0.019(3) 0.032(3) -0.004(2) 0.004(3) -0.002(2) C30 0.019(3) 0.018(3) 0.037(4) 0.002(2) 0.010(3) 0.001(2) C14 0.019(3) 0.044(4) 0.017(3) -0.002(3) 0.001(3) 0.010(3) C12 0.031(4) 0.018(3) 0.037(4) 0.002(3) 0.007(3) -0.003(3) C20 0.029(3) 0.022(3) 0.025(3) -0.002(2) 0.002(3) 0.010(2) C21 0.035(4) 0.032(3) 0.025(3) -0.013(3) 0.001(3) 0.003(3) Cl3 0.0351(8) 0.0213(7) 0.0285(8) 0.0036(6) 0.0183(7) -0.0074(6) Cl2 0.0436(9) 0.0205(7) 0.0206(7) -0.0036(6) 0.0109(7) -0.0102(6) Cl6 0.0405(9) 0.0268(8) 0.0265(8) -0.0011(6) 0.0167(7) 0.0150(6) Cl5 0.0482(10) 0.0242(7) 0.0172(7) 0.0039(6) 0.0091(7) 0.0149(7) C2 0.024(3) 0.018(3) 0.038(4) 0.009(3) 0.012(3) 0.002(2) C1 0.023(3) 0.028(3) 0.024(3) -0.006(2) 0.010(3) 0.001(2) C16 0.030(4) 0.026(3) 0.024(3) 0.005(2) 0.005(3) -0.002(2) C7 0.017(3) 0.027(3) 0.022(3) -0.002(2) 0.000(3) 0.001(2) C15 0.035(4) 0.042(4) 0.025(4) 0.008(3) 0.005(3) -0.003(3) _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 C25 P4 1.813(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? Pt1 B1 1.963(6) . ? Pt1 P2 2.3003(15) . ? Pt1 P1 2.3065(15) . ? Pt1 Cl1 2.4385(15) . ? Pt2 B2 1.971(6) . ? Pt2 P4 2.2994(15) . ? Pt2 P3 2.3017(15) . ? Pt2 Cl4 2.4433(15) . ? P2 C10 1.807(6) . ? P2 C9 1.820(6) . ? P2 C11 1.827(6) . ? P1 C2 1.819(6) . ? P1 C1 1.820(6) . ? P1 C3 1.826(6) . ? P4 C26 1.821(6) . ? P4 C27 1.823(6) . ? P3 C17 1.808(5) . ? P3 C19 1.816(6) . ? P3 C18 1.817(5) . ? B1 Cl3 1.778(7) . ? B1 Cl2 1.794(7) . ? B2 Cl5 1.780(7) . ? B2 Cl6 1.782(7) . ? C28 C29 1.375(8) . ? C28 C27 1.397(8) . ? C28 H28 0.9500 . ? C3 C8 1.387(8) . ? C3 C4 1.393(7) . ? C27 C32 1.384(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C32 C31 1.395(8) . ? C32 H32 0.9500 . ? C19 C24 1.376(8) . ? C19 C20 1.389(8) . ? C8 C7 1.392(8) . ? C8 H8 0.9500 . ? C11 C16 1.380(8) . ? C11 C12 1.382(8) . ? C4 C5 1.382(8) . ? C4 H4 0.9500 . ? C31 C30 1.393(9) . ? C31 H31 0.9500 . ? C5 C6 1.384(8) . ? C5 H5 0.9500 . ? C23 C22 1.373(9) . ? C23 C24 1.400(8) . ? C23 H23 0.9500 . ? C29 C30 1.378(8) . ? C29 H29 0.9500 . ? C24 H24 0.9500 . ? C22 C21 1.364(8) . ? C22 H22 0.9500 . ? C13 C14 1.369(10) . ? C13 C12 1.404(9) . ? C13 H13 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C6 C7 1.381(8) . ? C6 H6 0.9500 . ? C30 H30 0.9500 . ? C14 C15 1.370(9) . ? C14 H14 0.9500 . ? C12 H12 0.9500 . ? C20 C21 1.395(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C16 C15 1.390(9) . ? C16 H16 0.9500 . ? C7 H7 0.9500 . ? C15 H15 0.9500 . ? 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 P4 C25 H25A 109.5 . . ? P4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? B1 Pt1 P2 91.70(19) . . ? B1 Pt1 P1 92.08(19) . . ? P2 Pt1 P1 176.22(5) . . ? B1 Pt1 Cl1 176.8(2) . . ? P2 Pt1 Cl1 87.77(6) . . ? P1 Pt1 Cl1 88.47(6) . . ? B2 Pt2 P4 92.3(2) . . ? B2 Pt2 P3 91.9(2) . . ? P4 Pt2 P3 175.46(5) . . ? B2 Pt2 Cl4 178.3(2) . . ? P4 Pt2 Cl4 88.58(6) . . ? P3 Pt2 Cl4 87.18(6) . . ? C10 P2 C9 104.4(3) . . ? C10 P2 C11 104.3(3) . . ? C9 P2 C11 105.6(3) . . ? C10 P2 Pt1 113.1(2) . . ? C9 P2 Pt1 110.2(2) . . ? C11 P2 Pt1 118.10(17) . . ? C2 P1 C1 102.6(3) . . ? C2 P1 C3 105.9(3) . . ? C1 P1 C3 104.0(3) . . ? C2 P1 Pt1 112.1(2) . . ? C1 P1 Pt1 118.4(2) . . ? C3 P1 Pt1 112.68(19) . . ? C25 P4 C26 102.7(3) . . ? C25 P4 C27 103.6(3) . . ? C26 P4 C27 105.7(3) . . ? C25 P4 Pt2 119.0(2) . . ? C26 P4 Pt2 112.5(2) . . ? C27 P4 Pt2 112.1(2) . . ? C17 P3 C19 106.2(3) . . ? C17 P3 C18 105.0(3) . . ? C19 P3 C18 104.1(3) . . ? C17 P3 Pt2 109.3(2) . . ? C19 P3 Pt2 118.53(17) . . ? C18 P3 Pt2 112.7(2) . . ? Cl3 B1 Cl2 111.2(3) . . ? Cl3 B1 Pt1 123.9(4) . . ? Cl2 B1 Pt1 124.9(4) . . ? Cl5 B2 Cl6 111.4(3) . . ? Cl5 B2 Pt2 125.1(4) . . ? Cl6 B2 Pt2 123.5(4) . . ? C29 C28 C27 121.5(6) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C8 C3 C4 118.5(6) . . ? C8 C3 P1 120.9(4) . . ? C4 C3 P1 120.6(4) . . ? C32 C27 C28 117.7(6) . . ? C32 C27 P4 121.3(4) . . ? C28 C27 P4 120.9(5) . . ? P3 C18 H18A 109.5 . . ? P3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P4 C26 H26A 109.5 . . ? P4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C27 C32 C31 121.2(5) . . ? C27 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C24 C19 C20 118.7(5) . . ? C24 C19 P3 121.1(4) . . ? C20 C19 P3 120.1(4) . . ? C3 C8 C7 120.9(6) . . ? C3 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C16 C11 C12 119.6(6) . . ? C16 C11 P2 120.0(4) . . ? C12 C11 P2 120.2(5) . . ? C5 C4 C3 120.7(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C30 C31 C32 119.8(5) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C4 C5 C6 120.4(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C22 C23 C24 120.2(6) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C28 C29 C30 120.5(6) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C19 C24 C23 120.7(6) . . ? C19 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C21 C22 C23 119.3(6) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C14 C13 C12 121.2(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? P3 C17 H17A 109.5 . . ? P3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C7 C6 C5 119.7(5) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C29 C30 C31 119.3(5) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C13 C14 C15 119.2(6) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C11 C12 C13 119.0(6) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 121.1(6) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C11 C16 C15 120.3(6) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C6 C7 C8 119.8(6) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C14 C15 C16 120.6(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.012 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.129 #===END data_Cl3BP(Ph)2CH2(Ph)2PBCl3 _database_code_depnum_ccdc_archive 'CCDC 618547' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C25 H22 B2 Cl6 P2' _chemical_formula_sum 'C25 H22 B2 Cl6 P2' _chemical_formula_weight 618.68 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' 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 'P c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 11.066(2) _cell_length_b 10.003(2) _cell_length_c 16.371(5) _cell_angle_alpha 90.00 _cell_angle_beta 129.95(2) _cell_angle_gamma 90.00 _cell_volume 1389.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.41 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15704 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6270 _reflns_number_gt 6082 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 6270 _refine_ls_number_parameters 316 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.25256(6) 0.30336(5) 1.04103(4) 0.01973(12) Uani 1 1 d . . . Cl2 Cl -0.03760(6) 0.34058(6) 0.80729(5) 0.02356(13) Uani 1 1 d . . . Cl3 Cl 0.13755(7) 0.07253(5) 0.88989(5) 0.02077(12) Uani 1 1 d . . . Cl4 Cl 0.83298(6) 0.24734(5) 1.20528(4) 0.01780(11) Uani 1 1 d . . . Cl5 Cl 0.76930(6) -0.01255(5) 1.08628(4) 0.01743(11) Uani 1 1 d . . . Cl6 Cl 0.99514(6) 0.19372(5) 1.11191(4) 0.01896(11) Uani 1 1 d . . . P1 P 0.29023(6) 0.32585(5) 0.87217(4) 0.01150(11) Uani 1 1 d . . . P2 P 0.63734(6) 0.24344(5) 0.95882(4) 0.01143(11) Uani 1 1 d . . . C1 C 0.3369(2) 0.4981(2) 0.91498(17) 0.0130(4) Uani 1 1 d . . . C2 C 0.4677(3) 0.5279(2) 1.02034(18) 0.0167(4) Uani 1 1 d . . . H2 H 0.5374 0.4586 1.0669 0.020 Uiso 1 1 calc R . . C3 C 0.4960(3) 0.6589(2) 1.0571(2) 0.0211(5) Uani 1 1 d . . . H3 H 0.5858 0.6792 1.1285 0.025 Uiso 1 1 calc R . . C4 C 0.3933(3) 0.7597(2) 0.9897(2) 0.0224(5) Uani 1 1 d . . . H4 H 0.4128 0.8493 1.0146 0.027 Uiso 1 1 calc R . . C5 C 0.2624(3) 0.7300(2) 0.8861(2) 0.0229(5) Uani 1 1 d . . . H5 H 0.1918 0.7993 0.8401 0.027 Uiso 1 1 calc R . . C6 C 0.2331(3) 0.5996(2) 0.84870(18) 0.0187(5) Uani 1 1 d . . . H6 H 0.1420 0.5798 0.7777 0.022 Uiso 1 1 calc R . . C7 C 0.2067(3) 0.3042(2) 0.73532(17) 0.0138(4) Uani 1 1 d . . . C8 C 0.2209(3) 0.3999(2) 0.67954(19) 0.0200(5) Uani 1 1 d . . . H8 H 0.2677 0.4842 0.7111 0.024 Uiso 1 1 calc R . . C9 C 0.1664(3) 0.3712(2) 0.57783(19) 0.0242(5) Uani 1 1 d . . . H9 H 0.1760 0.4362 0.5400 0.029 Uiso 1 1 calc R . . C10 C 0.0984(3) 0.2490(2) 0.53128(19) 0.0216(5) Uani 1 1 d . . . H10 H 0.0637 0.2295 0.4624 0.026 Uiso 1 1 calc R . . C11 C 0.0805(3) 0.1549(2) 0.58474(19) 0.0195(5) Uani 1 1 d . . . H11 H 0.0323 0.0713 0.5521 0.023 Uiso 1 1 calc R . . C12 C 0.1331(3) 0.1824(2) 0.68608(19) 0.0176(5) Uani 1 1 d . . . H12 H 0.1189 0.1183 0.7221 0.021 Uiso 1 1 calc R . . C13 C 0.4720(2) 0.2301(2) 0.95823(17) 0.0130(4) Uani 1 1 d . . . H13A H 0.4404 0.1348 0.9445 0.016 Uiso 1 1 calc R . . H13B H 0.5157 0.2485 1.0321 0.016 Uiso 1 1 calc R . . C14 C 0.6684(2) 0.4132(2) 0.93813(17) 0.0143(4) Uani 1 1 d . . . C15 C 0.7575(3) 0.5002(2) 1.02449(19) 0.0186(5) Uani 1 1 d . . . H15 H 0.8068 0.4692 1.0944 0.022 Uiso 1 1 calc R . . C16 C 0.7738(3) 0.6324(2) 1.0078(2) 0.0227(5) Uani 1 1 d . . . H16 H 0.8329 0.6925 1.0663 0.027 Uiso 1 1 calc R . . C17 C 0.7050(3) 0.6772(2) 0.9069(2) 0.0265(5) Uani 1 1 d . . . H17 H 0.7160 0.7683 0.8962 0.032 Uiso 1 1 calc R . . C18 C 0.6202(3) 0.5909(2) 0.8213(2) 0.0270(5) Uani 1 1 d . . . H18 H 0.5747 0.6223 0.7521 0.032 Uiso 1 1 calc R . . C19 C 0.6013(3) 0.4584(2) 0.83605(19) 0.0204(5) Uani 1 1 d . . . H19 H 0.5431 0.3988 0.7772 0.025 Uiso 1 1 calc R . . C20 C 0.5989(2) 0.1405(2) 0.85440(16) 0.0138(4) Uani 1 1 d . . . C21 C 0.7049(3) 0.1475(2) 0.83562(19) 0.0204(5) Uani 1 1 d . . . H21 H 0.7884 0.2107 0.8731 0.025 Uiso 1 1 calc R . . C22 C 0.6886(3) 0.0624(2) 0.7623(2) 0.0251(5) Uani 1 1 d . . . H22 H 0.7617 0.0663 0.7501 0.030 Uiso 1 1 calc R . . C23 C 0.5659(3) -0.0281(2) 0.7071(2) 0.0261(5) Uani 1 1 d . . . H23 H 0.5538 -0.0855 0.6561 0.031 Uiso 1 1 calc R . . C24 C 0.4602(3) -0.0360(2) 0.7255(2) 0.0262(5) Uani 1 1 d . . . H24 H 0.3755 -0.0981 0.6868 0.031 Uiso 1 1 calc R . . C25 C 0.4783(3) 0.0474(2) 0.80069(19) 0.0202(5) Uani 1 1 d . . . H25 H 0.4080 0.0404 0.8152 0.024 Uiso 1 1 calc R . . B1 B 0.1531(3) 0.2561(2) 0.9020(2) 0.0150(5) Uani 1 1 d . . . B2 B 0.8184(3) 0.1666(2) 1.0976(2) 0.0139(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0260(3) 0.0192(3) 0.0178(3) 0.0026(2) 0.0158(3) 0.0032(2) Cl2 0.0139(3) 0.0291(3) 0.0264(3) 0.0107(2) 0.0124(3) 0.0058(2) Cl3 0.0265(3) 0.0143(2) 0.0269(3) -0.0003(2) 0.0196(3) -0.0034(2) Cl4 0.0177(3) 0.0224(3) 0.0131(2) -0.00196(19) 0.0098(2) 0.0003(2) Cl5 0.0209(3) 0.0136(2) 0.0188(3) 0.0028(2) 0.0132(2) 0.00233(19) Cl6 0.0131(2) 0.0248(3) 0.0189(3) -0.0016(2) 0.0102(2) -0.0005(2) P1 0.0104(2) 0.0109(2) 0.0119(3) 0.00031(19) 0.0066(2) 0.00013(19) P2 0.0117(3) 0.0116(2) 0.0116(3) -0.00053(19) 0.0078(2) -0.00020(19) C1 0.0136(10) 0.0145(9) 0.0123(10) -0.0009(8) 0.0089(9) -0.0005(8) C2 0.0140(11) 0.0182(10) 0.0153(11) 0.0012(8) 0.0082(10) 0.0026(8) C3 0.0182(12) 0.0229(11) 0.0171(11) -0.0064(9) 0.0089(10) -0.0019(9) C4 0.0258(13) 0.0158(11) 0.0255(13) -0.0043(9) 0.0165(12) -0.0020(9) C5 0.0235(13) 0.0172(11) 0.0221(13) 0.0014(9) 0.0120(11) 0.0050(9) C6 0.0157(11) 0.0178(11) 0.0142(11) -0.0009(8) 0.0059(10) -0.0001(8) C7 0.0117(10) 0.0155(10) 0.0121(10) 0.0011(8) 0.0067(9) 0.0018(8) C8 0.0224(12) 0.0176(10) 0.0212(12) -0.0042(9) 0.0146(11) -0.0078(9) C9 0.0301(13) 0.0264(12) 0.0187(12) 0.0001(10) 0.0169(11) -0.0078(10) C10 0.0210(12) 0.0291(13) 0.0152(11) -0.0031(9) 0.0119(11) -0.0014(9) C11 0.0186(12) 0.0181(11) 0.0178(12) -0.0026(9) 0.0099(10) -0.0023(9) C12 0.0175(12) 0.0164(11) 0.0197(12) 0.0010(8) 0.0124(11) -0.0014(8) C13 0.0129(11) 0.0126(9) 0.0145(11) 0.0013(8) 0.0092(10) 0.0011(8) C14 0.0120(10) 0.0122(9) 0.0190(11) 0.0007(8) 0.0102(10) -0.0005(8) C15 0.0149(11) 0.0193(11) 0.0183(11) 0.0002(9) 0.0093(10) -0.0008(9) C16 0.0206(12) 0.0179(11) 0.0255(13) -0.0037(9) 0.0129(12) -0.0050(9) C17 0.0215(13) 0.0188(11) 0.0317(14) 0.0082(10) 0.0136(12) -0.0008(9) C18 0.0265(13) 0.0256(12) 0.0216(13) 0.0080(10) 0.0122(12) -0.0009(10) C19 0.0219(12) 0.0188(10) 0.0176(11) 0.0000(9) 0.0114(11) -0.0018(9) C20 0.0156(11) 0.0153(10) 0.0107(10) 0.0000(8) 0.0085(9) 0.0020(8) C21 0.0196(12) 0.0236(11) 0.0209(12) -0.0016(9) 0.0143(11) -0.0005(9) C22 0.0307(14) 0.0317(13) 0.0211(13) 0.0020(10) 0.0204(12) 0.0066(10) C23 0.0304(14) 0.0266(13) 0.0158(12) -0.0024(10) 0.0124(11) 0.0088(10) C24 0.0219(13) 0.0246(12) 0.0225(13) -0.0091(10) 0.0099(11) -0.0009(9) C25 0.0177(12) 0.0191(11) 0.0222(12) -0.0044(9) 0.0122(11) 0.0001(9) B1 0.0144(12) 0.0147(11) 0.0175(13) 0.0007(9) 0.0109(11) 0.0008(9) B2 0.0129(11) 0.0150(11) 0.0140(12) -0.0009(9) 0.0088(11) 0.0001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 B1 1.844(3) . ? Cl2 B1 1.835(3) . ? Cl3 B1 1.843(2) . ? Cl4 B2 1.850(3) . ? Cl5 B2 1.847(2) . ? Cl6 B2 1.835(3) . ? P1 C7 1.806(2) . ? P1 C1 1.806(2) . ? P1 C13 1.819(2) . ? P1 B1 1.995(3) . ? P2 C20 1.797(2) . ? P2 C14 1.807(2) . ? P2 C13 1.829(2) . ? P2 B2 1.980(3) . ? C1 C6 1.388(3) . ? C1 C2 1.397(3) . ? C2 C3 1.391(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.398(3) . ? C7 C8 1.400(3) . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C10 1.380(3) . ? C9 H9 0.9500 . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.392(3) . ? C14 C19 1.398(3) . ? C15 C16 1.386(3) . ? C15 H15 0.9500 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.379(4) . ? C17 H17 0.9500 . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.383(3) . ? C20 C21 1.392(3) . ? C21 C22 1.386(3) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.384(4) . ? C23 H23 0.9500 . ? C24 C25 1.391(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? 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 C7 P1 C1 112.76(10) . . ? C7 P1 C13 109.16(10) . . ? C1 P1 C13 107.68(10) . . ? C7 P1 B1 113.45(11) . . ? C1 P1 B1 108.15(10) . . ? C13 P1 B1 105.22(10) . . ? C20 P2 C14 108.51(10) . . ? C20 P2 C13 109.15(10) . . ? C14 P2 C13 112.22(9) . . ? C20 P2 B2 108.43(10) . . ? C14 P2 B2 113.93(10) . . ? C13 P2 B2 104.45(10) . . ? C6 C1 C2 119.37(19) . . ? C6 C1 P1 120.50(17) . . ? C2 C1 P1 119.58(16) . . ? C3 C2 C1 120.1(2) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.0(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.1(2) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C12 C7 C8 119.2(2) . . ? C12 C7 P1 117.66(16) . . ? C8 C7 P1 123.02(17) . . ? C9 C8 C7 119.8(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.5(2) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.2(2) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? P1 C13 P2 124.78(12) . . ? P1 C13 H13A 106.1 . . ? P2 C13 H13A 106.1 . . ? P1 C13 H13B 106.1 . . ? P2 C13 H13B 106.1 . . ? H13A C13 H13B 106.3 . . ? C15 C14 C19 119.83(19) . . ? C15 C14 P2 119.54(17) . . ? C19 C14 P2 120.61(16) . . ? C16 C15 C14 119.6(2) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 120.1(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 119.6(2) . . ? C18 C19 H19 120.2 . . ? C14 C19 H19 120.2 . . ? C25 C20 C21 119.9(2) . . ? C25 C20 P2 122.22(17) . . ? C21 C20 P2 117.55(17) . . ? C22 C21 C20 120.0(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.8(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.6(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 119.8(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C20 C25 C24 119.9(2) . . ? C20 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? Cl2 B1 Cl3 113.01(13) . . ? Cl2 B1 Cl1 112.08(13) . . ? Cl3 B1 Cl1 109.21(13) . . ? Cl2 B1 P1 105.94(12) . . ? Cl3 B1 P1 110.80(12) . . ? Cl1 B1 P1 105.50(12) . . ? Cl6 B2 Cl5 112.15(12) . . ? Cl6 B2 Cl4 112.35(13) . . ? Cl5 B2 Cl4 111.06(13) . . ? Cl6 B2 P2 107.43(12) . . ? Cl5 B2 P2 104.23(12) . . ? Cl4 B2 P2 109.20(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.435 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.061 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 618548' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C12 H36 B2 Cl5 P4 Pt2, B Cl4' _chemical_formula_sum 'C12 H36 B3 Cl9 P4 Pt2' _chemical_formula_weight 1045.95 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' Cl Cl 0.1484 0.1585 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.306(3) _cell_length_b 13.214(3) _cell_length_c 20.313(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.35(3) _cell_angle_gamma 90.00 _cell_volume 3297.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.53 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method none _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 9.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.116 _exptl_absorpt_correction_T_max 0.240 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 173 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.192 _diffrn_detector_type 'Bruker-AXS SMART 1k' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Platform' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation '0.5 mm double pin hole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36989 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7566 _reflns_number_gt 6902 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.054 (Bruker-AXS, 1997-1998)' _computing_cell_refinement 'SMART v5.054 (Bruker-AXS, 1997-1998)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0132P)^2^+9.2045P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7566 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Pt1 Pt 0.788066(10) 0.885936(10) 0.982225(7) 0.00951(4) Uani 1 1 d . . . Pt2 Pt 0.750685(11) 0.897302(10) 0.761340(7) 0.01002(4) Uani 1 1 d . . . Cl3 Cl 0.83525(7) 0.95126(7) 0.87113(4) 0.01445(18) Uani 1 1 d . . . P1 P 0.79019(8) 0.71591(7) 0.95491(5) 0.01257(19) Uani 1 1 d . . . P2 P 0.78800(8) 1.05305(7) 1.01701(5) 0.01316(19) Uani 1 1 d . . . P4 P 0.92217(8) 0.90632(7) 0.72093(5) 0.01313(19) Uani 1 1 d . . . P3 P 0.57336(8) 0.91718(8) 0.78992(5) 0.0138(2) Uani 1 1 d . . . Cl4 Cl 0.69482(9) 0.70135(7) 0.67256(5) 0.0243(2) Uani 1 1 d . . . Cl5 Cl 0.64412(10) 0.89768(8) 0.60590(5) 0.0306(3) Uani 1 1 d . . . Cl1 Cl 0.85322(12) 0.82089(9) 1.13479(6) 0.0411(3) Uani 1 1 d . . . Cl2 Cl 0.61676(11) 0.83572(10) 1.09509(7) 0.0421(3) Uani 1 1 d . . . C12 C 0.9367(4) 0.8778(4) 0.6345(2) 0.0252(9) Uani 1 1 d . . . H12A H 0.8904 0.9234 0.6071 0.038 Uiso 1 1 calc R . . H12B H 0.9148 0.8076 0.6256 0.038 Uiso 1 1 calc R . . H12C H 1.0128 0.8869 0.6240 0.038 Uiso 1 1 calc R . . C5 C 0.9070(3) 1.1239(3) 0.9965(2) 0.0224(9) Uani 1 1 d . . . H5A H 0.9176 1.1169 0.9493 0.034 Uiso 1 1 calc R . . H5B H 0.9711 1.0977 1.0219 0.034 Uiso 1 1 calc R . . H5C H 0.8969 1.1954 1.0072 0.034 Uiso 1 1 calc R . . C6 C 0.6734(3) 1.1237(3) 0.9809(2) 0.0229(9) Uani 1 1 d . . . H6A H 0.6780 1.1941 0.9959 0.034 Uiso 1 1 calc R . . H6B H 0.6055 1.0936 0.9946 0.034 Uiso 1 1 calc R . . H6C H 0.6745 1.1216 0.9327 0.034 Uiso 1 1 calc R . . C10 C 1.0239(3) 0.8269(3) 0.7629(2) 0.0229(9) Uani 1 1 d . . . H10A H 1.0957 0.8427 0.7470 0.034 Uiso 1 1 calc R . . H10B H 1.0066 0.7556 0.7539 0.034 Uiso 1 1 calc R . . H10C H 1.0246 0.8393 0.8104 0.034 Uiso 1 1 calc R . . C1 C 0.8208(4) 0.6884(3) 0.8710(2) 0.0249(10) Uani 1 1 d . . . H1A H 0.8929 0.7152 0.8626 0.037 Uiso 1 1 calc R . . H1B H 0.7659 0.7200 0.8407 0.037 Uiso 1 1 calc R . . H1C H 0.8201 0.6150 0.8641 0.037 Uiso 1 1 calc R . . B2 B 0.6954(4) 0.8357(3) 0.6785(2) 0.0152(9) Uani 1 1 d . . . C4 C 0.7821(4) 1.0772(3) 1.1047(2) 0.0264(10) Uani 1 1 d . . . H4A H 0.7780 1.1503 1.1123 0.040 Uiso 1 1 calc R . . H4B H 0.8475 1.0499 1.1282 0.040 Uiso 1 1 calc R . . H4C H 0.7174 1.0444 1.1210 0.040 Uiso 1 1 calc R . . C11 C 0.9736(3) 1.0335(3) 0.7302(2) 0.0235(9) Uani 1 1 d . . . H11A H 0.9756 1.0528 0.7768 0.035 Uiso 1 1 calc R . . H11B H 0.9258 1.0800 0.7044 0.035 Uiso 1 1 calc R . . H11C H 1.0472 1.0368 0.7143 0.035 Uiso 1 1 calc R . . B1 B 0.7532(4) 0.8457(3) 1.0714(2) 0.0180(9) Uani 1 1 d . . . C2 C 0.6648(3) 0.6476(3) 0.9663(3) 0.0266(10) Uani 1 1 d . . . H2A H 0.6064 0.6757 0.9370 0.040 Uiso 1 1 calc R . . H2B H 0.6455 0.6542 1.0122 0.040 Uiso 1 1 calc R . . H2C H 0.6750 0.5759 0.9559 0.040 Uiso 1 1 calc R . . C9 C 0.4704(3) 0.8383(4) 0.7487(3) 0.0393(13) Uani 1 1 d . . . H9A H 0.3992 0.8542 0.7653 0.059 Uiso 1 1 calc R . . H9B H 0.4876 0.7669 0.7573 0.059 Uiso 1 1 calc R . . H9C H 0.4686 0.8510 0.7011 0.059 Uiso 1 1 calc R . . C3 C 0.8901(3) 0.6438(3) 1.0041(2) 0.0192(8) Uani 1 1 d . . . H3A H 0.8946 0.5751 0.9861 0.029 Uiso 1 1 calc R . . H3B H 0.8685 0.6403 1.0497 0.029 Uiso 1 1 calc R . . H3C H 0.9613 0.6767 1.0030 0.029 Uiso 1 1 calc R . . C7 C 0.5462(4) 0.9017(4) 0.8759(2) 0.0342(12) Uani 1 1 d . . . H7A H 0.6045 0.9338 0.9035 0.051 Uiso 1 1 calc R . . H7B H 0.5430 0.8295 0.8864 0.051 Uiso 1 1 calc R . . H7C H 0.4765 0.9336 0.8843 0.051 Uiso 1 1 calc R . . C8 C 0.5304(4) 1.0442(3) 0.7698(2) 0.0278(10) Uani 1 1 d . . . H8A H 0.4558 1.0544 0.7829 0.042 Uiso 1 1 calc R . . H8B H 0.5330 1.0550 0.7222 0.042 Uiso 1 1 calc R . . H8C H 0.5790 1.0925 0.7934 0.042 Uiso 1 1 calc R . . Cl7 Cl 0.12092(9) 0.61235(9) 0.91058(6) 0.0325(3) Uani 1 1 d . . . Cl8 Cl 0.25846(9) 0.45171(8) 0.84991(6) 0.0279(2) Uani 1 1 d . . . Cl9 Cl 0.25837(11) 0.66458(11) 0.79831(8) 0.0491(4) Uani 1 1 d . . . Cl6 Cl 0.36572(11) 0.61609(12) 0.93210(8) 0.0528(4) Uani 1 1 d . . . B3 B 0.2513(4) 0.5870(4) 0.8726(2) 0.0187(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00935(7) 0.00940(7) 0.00964(7) -0.00003(5) -0.00064(5) -0.00022(5) Pt2 0.00934(7) 0.00910(7) 0.01150(7) -0.00033(5) -0.00032(5) -0.00039(5) Cl3 0.0187(4) 0.0142(4) 0.0104(4) -0.0009(3) 0.0006(3) -0.0046(3) P1 0.0136(4) 0.0109(5) 0.0131(5) -0.0006(4) -0.0005(4) -0.0007(4) P2 0.0141(5) 0.0122(5) 0.0130(5) -0.0021(4) -0.0011(4) -0.0003(4) P4 0.0136(5) 0.0123(5) 0.0138(5) -0.0008(4) 0.0031(4) -0.0005(4) P3 0.0099(4) 0.0151(5) 0.0164(5) -0.0002(4) -0.0003(4) 0.0004(4) Cl4 0.0364(6) 0.0131(5) 0.0237(5) -0.0051(4) 0.0028(4) -0.0041(4) Cl5 0.0439(7) 0.0252(6) 0.0207(6) 0.0040(4) -0.0158(5) -0.0056(5) Cl1 0.0741(9) 0.0312(6) 0.0160(6) 0.0013(5) -0.0149(6) 0.0138(6) Cl2 0.0454(7) 0.0398(7) 0.0445(8) -0.0124(6) 0.0328(6) -0.0165(6) C12 0.023(2) 0.032(2) 0.022(2) -0.0015(19) 0.0098(17) 0.0043(18) C5 0.017(2) 0.016(2) 0.034(3) -0.0060(18) 0.0001(17) -0.0065(16) C6 0.018(2) 0.023(2) 0.028(2) -0.0032(18) -0.0022(17) 0.0083(17) C10 0.0151(19) 0.026(2) 0.027(2) 0.0057(19) 0.0012(17) 0.0002(17) C1 0.046(3) 0.015(2) 0.014(2) -0.0021(16) 0.0006(18) 0.0017(19) B2 0.018(2) 0.013(2) 0.014(2) -0.0008(17) -0.0014(17) -0.0011(17) C4 0.036(3) 0.025(2) 0.018(2) -0.0054(18) -0.0006(19) -0.0025(19) C11 0.023(2) 0.015(2) 0.034(3) -0.0020(18) 0.0169(19) -0.0064(16) B1 0.031(2) 0.012(2) 0.012(2) 0.0023(17) 0.0049(18) -0.0020(18) C2 0.021(2) 0.017(2) 0.043(3) -0.0022(19) 0.0034(19) -0.0069(17) C9 0.013(2) 0.045(3) 0.059(4) -0.022(3) -0.001(2) -0.007(2) C3 0.024(2) 0.016(2) 0.018(2) 0.0023(16) -0.0002(16) 0.0053(16) C7 0.019(2) 0.062(4) 0.022(2) 0.015(2) 0.0064(18) 0.008(2) C8 0.029(2) 0.021(2) 0.035(3) 0.0048(19) 0.011(2) 0.0090(18) Cl7 0.0249(5) 0.0332(6) 0.0415(7) 0.0013(5) 0.0194(5) 0.0075(5) Cl8 0.0281(5) 0.0207(5) 0.0363(6) -0.0073(5) 0.0134(5) -0.0032(4) Cl9 0.0458(7) 0.0462(8) 0.0587(9) 0.0339(7) 0.0319(7) 0.0220(6) Cl6 0.0300(7) 0.0592(9) 0.0668(10) -0.0334(8) -0.0171(6) 0.0009(6) B3 0.015(2) 0.017(2) 0.025(3) -0.0003(19) 0.0059(18) 0.0007(17) _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 B1 1.960(5) . ? Pt1 P1 2.3147(11) . ? Pt1 P2 2.3185(11) . ? Pt1 Cl3 2.5155(10) . ? Pt2 B2 1.955(4) . ? Pt2 P3 2.3057(11) . ? Pt2 P4 2.3118(11) . ? Pt2 Cl3 2.5088(11) . ? P1 C1 1.804(4) . ? P1 C3 1.809(4) . ? P1 C2 1.814(4) . ? P2 C6 1.811(4) . ? P2 C5 1.807(4) . ? P2 C4 1.816(4) . ? P4 C11 1.802(4) . ? P4 C10 1.809(4) . ? P4 C12 1.815(4) . ? P3 C8 1.800(4) . ? P3 C7 1.808(5) . ? P3 C9 1.808(5) . ? Cl4 B2 1.780(5) . ? Cl5 B2 1.771(5) . ? Cl1 B1 1.759(5) . ? Cl2 B1 1.778(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? Cl7 B3 1.852(5) . ? Cl8 B3 1.849(5) . ? Cl9 B3 1.830(5) . ? Cl6 B3 1.842(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Pt1 P1 87.98(14) . . ? B1 Pt1 P2 88.42(13) . . ? P1 Pt1 P2 176.11(4) . . ? B1 Pt1 Cl3 175.54(13) . . ? P1 Pt1 Cl3 96.41(3) . . ? P2 Pt1 Cl3 87.18(3) . . ? B2 Pt2 P3 88.70(14) . . ? B2 Pt2 P4 89.70(14) . . ? P3 Pt2 P4 168.70(4) . . ? B2 Pt2 Cl3 171.40(13) . . ? P3 Pt2 Cl3 95.35(4) . . ? P4 Pt2 Cl3 87.78(4) . . ? Pt2 Cl3 Pt1 126.48(4) . . ? C1 P1 C3 104.0(2) . . ? C1 P1 C2 104.2(2) . . ? C3 P1 C2 102.9(2) . . ? C1 P1 Pt1 115.35(14) . . ? C3 P1 Pt1 113.33(14) . . ? C2 P1 Pt1 115.53(15) . . ? C6 P2 C5 105.2(2) . . ? C6 P2 C4 103.4(2) . . ? C5 P2 C4 102.4(2) . . ? C6 P2 Pt1 112.43(15) . . ? C5 P2 Pt1 114.10(14) . . ? C4 P2 Pt1 117.84(15) . . ? C11 P4 C10 105.2(2) . . ? C11 P4 C12 103.9(2) . . ? C10 P4 C12 103.3(2) . . ? C11 P4 Pt2 109.47(14) . . ? C10 P4 Pt2 115.10(14) . . ? C12 P4 Pt2 118.46(15) . . ? C8 P3 C7 104.8(2) . . ? C8 P3 C9 104.1(2) . . ? C7 P3 C9 102.6(3) . . ? C8 P3 Pt2 108.59(15) . . ? C7 P3 Pt2 117.47(15) . . ? C9 P3 Pt2 117.75(17) . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Cl5 B2 Cl4 113.9(2) . . ? Cl5 B2 Pt2 127.9(2) . . ? Cl4 B2 Pt2 118.3(2) . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Cl1 B1 Cl2 114.8(3) . . ? Cl1 B1 Pt1 123.0(3) . . ? Cl2 B1 Pt1 122.1(3) . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Cl9 B3 Cl6 110.6(2) . . ? Cl9 B3 Cl8 109.4(3) . . ? Cl6 B3 Cl8 108.6(2) . . ? Cl9 B3 Cl7 109.0(2) . . ? Cl6 B3 Cl7 109.6(3) . . ? Cl8 B3 Cl7 109.5(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.703 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.137 #===END data_[Pt(PMe3)2(dppm)]Cl2 _database_code_depnum_ccdc_archive 'CCDC 618549' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C31 H40 P4 Pt, 2(Cl)' _chemical_formula_sum 'C31 H40 Cl2 P4 Pt' _chemical_formula_weight 802.50 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' Cl Cl 0.1484 0.1585 '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' 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 b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 29.9175(16) _cell_length_b 20.6730(11) _cell_length_c 11.5155(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7122.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.49 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method none _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 4.288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.46 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 173 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.192 _diffrn_detector_type 'Bruker-AXS SMART 1k' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Platform' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation '0.5 mm double pin hole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 71496 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.44 _reflns_number_total 8138 _reflns_number_gt 6996 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.054 (Bruker-AXS, 1997-1998)' _computing_cell_refinement 'SMART v5.054 (Bruker-AXS, 1997-1998)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0345P)^2^+16.0037P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8138 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Pt1 Pt 0.102164(4) 0.303374(6) 0.376588(11) 0.02056(5) Uani 1 1 d . . . C1 C 0.19277(11) 0.41117(16) 0.2821(3) 0.0223(6) Uani 1 1 d . . . C2 C 0.21299(13) 0.42179(18) 0.3896(3) 0.0301(8) Uani 1 1 d . . . H2 H 0.2120 0.3894 0.4480 0.036 Uiso 1 1 calc R . . C3 C 0.23467(14) 0.4802(2) 0.4107(4) 0.0377(9) Uani 1 1 d . . . H3 H 0.2490 0.4871 0.4833 0.045 Uiso 1 1 calc R . . C4 C 0.23563(14) 0.52817(18) 0.3273(4) 0.0376(9) Uani 1 1 d . . . H4 H 0.2502 0.5680 0.3431 0.045 Uiso 1 1 calc R . . C5 C 0.21536(13) 0.51817(18) 0.2206(3) 0.0339(8) Uani 1 1 d . . . H5 H 0.2157 0.5515 0.1637 0.041 Uiso 1 1 calc R . . C6 C 0.19458(12) 0.45957(17) 0.1966(3) 0.0278(7) Uani 1 1 d . . . H6 H 0.1816 0.4522 0.1225 0.033 Uiso 1 1 calc R . . C7 C 0.15263(11) 0.33394(17) 0.1041(3) 0.0239(7) Uani 1 1 d . . . C8 C 0.18844(13) 0.31924(19) 0.0307(3) 0.0326(8) Uani 1 1 d . . . H8 H 0.2164 0.3063 0.0624 0.039 Uiso 1 1 calc R . . C9 C 0.18293(14) 0.3237(2) -0.0885(3) 0.0374(9) Uani 1 1 d . . . H9 H 0.2070 0.3128 -0.1386 0.045 Uiso 1 1 calc R . . C10 C 0.14305(15) 0.3437(2) -0.1349(3) 0.0400(10) Uani 1 1 d . . . H10 H 0.1401 0.3485 -0.2166 0.048 Uiso 1 1 calc R . . C11 C 0.10685(13) 0.3570(2) -0.0626(4) 0.0360(9) Uani 1 1 d . . . H11 H 0.0790 0.3700 -0.0949 0.043 Uiso 1 1 calc R . . C12 C 0.11172(12) 0.35132(18) 0.0567(3) 0.0294(8) Uani 1 1 d . . . H12 H 0.0869 0.3593 0.1063 0.035 Uiso 1 1 calc R . . C13 C 0.19610(11) 0.26775(15) 0.3021(3) 0.0241(7) Uani 1 1 d . . . H13A H 0.2161 0.2525 0.2392 0.029 Uiso 1 1 calc R . . H13B H 0.2133 0.2755 0.3741 0.029 Uiso 1 1 calc R . . C14 C 0.16165(12) 0.14750(17) 0.4178(4) 0.0325(8) Uani 1 1 d . . . C15 C 0.18425(13) 0.1575(2) 0.5211(4) 0.0412(10) Uani 1 1 d . . . H15 H 0.1950 0.1994 0.5402 0.049 Uiso 1 1 calc R . . C16 C 0.19115(16) 0.1058(2) 0.5972(5) 0.0520(12) Uani 1 1 d . . . H16 H 0.2070 0.1125 0.6677 0.062 Uiso 1 1 calc R . . C17 C 0.17506(16) 0.0452(2) 0.5703(5) 0.0564(14) Uani 1 1 d . . . H17 H 0.1794 0.0104 0.6229 0.068 Uiso 1 1 calc R . . C18 C 0.15267(16) 0.0349(2) 0.4673(5) 0.0570(14) Uani 1 1 d . . . H18 H 0.1418 -0.0071 0.4491 0.068 Uiso 1 1 calc R . . C19 C 0.14600(14) 0.08524(19) 0.3904(4) 0.0435(10) Uani 1 1 d . . . H19 H 0.1309 0.0778 0.3191 0.052 Uiso 1 1 calc R . . C20 C 0.13649(12) 0.18120(16) 0.1822(4) 0.0292(8) Uani 1 1 d . . . C21 C 0.09428(15) 0.1849(2) 0.1327(4) 0.0435(11) Uani 1 1 d . . . H21 H 0.0699 0.2016 0.1760 0.052 Uiso 1 1 calc R . . C22 C 0.08809(17) 0.1638(2) 0.0195(5) 0.0577(14) Uani 1 1 d . . . H22 H 0.0591 0.1651 -0.0139 0.069 Uiso 1 1 calc R . . C23 C 0.12344(18) 0.1409(2) -0.0452(4) 0.0526(12) Uani 1 1 d . . . H23 H 0.1190 0.1282 -0.1236 0.063 Uiso 1 1 calc R . . C24 C 0.16544(15) 0.1365(2) 0.0042(4) 0.0453(11) Uani 1 1 d . . . H24 H 0.1898 0.1203 -0.0399 0.054 Uiso 1 1 calc R . . C25 C 0.17181(14) 0.15579(19) 0.1177(4) 0.0381(9) Uani 1 1 d . . . H25 H 0.2005 0.1517 0.1522 0.046 Uiso 1 1 calc R . . C26 C 0.08871(16) 0.4666(2) 0.3111(5) 0.0506(13) Uani 1 1 d . . . H26A H 0.0708 0.5057 0.3240 0.076 Uiso 1 1 calc R . . H26B H 0.0833 0.4502 0.2325 0.076 Uiso 1 1 calc R . . H26C H 0.1205 0.4771 0.3199 0.076 Uiso 1 1 calc R . . C27 C 0.09521(14) 0.4365(2) 0.5515(4) 0.0430(10) Uani 1 1 d . . . H27A H 0.1278 0.4314 0.5524 0.064 Uiso 1 1 calc R . . H27B H 0.0822 0.4125 0.6165 0.064 Uiso 1 1 calc R . . H27C H 0.0876 0.4825 0.5588 0.064 Uiso 1 1 calc R . . C28 C 0.01301(12) 0.41612(17) 0.4238(4) 0.0306(8) Uani 1 1 d . . . H28A H 0.0030 0.4099 0.5040 0.046 Uiso 1 1 calc R . . H28B H -0.0016 0.3843 0.3733 0.046 Uiso 1 1 calc R . . H28C H 0.0052 0.4599 0.3981 0.046 Uiso 1 1 calc R . . C29 C 0.00543(13) 0.27835(18) 0.5619(3) 0.0321(8) Uani 1 1 d . . . H29A H -0.0081 0.2468 0.6149 0.048 Uiso 1 1 calc R . . H29B H -0.0144 0.2853 0.4954 0.048 Uiso 1 1 calc R . . H29C H 0.0100 0.3194 0.6029 0.048 Uiso 1 1 calc R . . C30 C 0.08929(16) 0.2370(3) 0.6458(4) 0.0507(12) Uani 1 1 d . . . H30A H 0.0902 0.2780 0.6885 0.076 Uiso 1 1 calc R . . H30B H 0.1198 0.2230 0.6282 0.076 Uiso 1 1 calc R . . H30C H 0.0744 0.2041 0.6932 0.076 Uiso 1 1 calc R . . C31 C 0.04407(13) 0.16695(17) 0.4639(4) 0.0362(9) Uani 1 1 d . . . H31A H 0.0277 0.1447 0.5259 0.054 Uiso 1 1 calc R . . H31B H 0.0714 0.1429 0.4458 0.054 Uiso 1 1 calc R . . H31C H 0.0253 0.1695 0.3943 0.054 Uiso 1 1 calc R . . P1 P 0.16123(3) 0.33732(4) 0.25923(7) 0.02094(17) Uani 1 1 d . . . P2 P 0.14732(3) 0.21532(4) 0.32421(9) 0.02620(19) Uani 1 1 d . . . P3 P 0.07320(3) 0.40553(4) 0.41617(8) 0.02317(17) Uani 1 1 d . . . P4 P 0.05857(3) 0.24812(4) 0.51136(8) 0.02462(18) Uani 1 1 d . . . Cl1 Cl 0.21384(3) 0.30927(5) 0.61622(8) 0.0340(2) Uani 1 1 d . . . Cl2 Cl 0.0000 0.41685(6) 0.7500 0.0330(3) Uani 1 2 d S . . Cl3 Cl 0.0000 0.27435(7) 0.2500 0.0356(3) Uani 1 2 d S . . 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 0.02122(7) 0.01666(7) 0.02381(7) -0.00013(5) 0.00278(5) 0.00128(4) C1 0.0202(15) 0.0223(15) 0.0245(16) -0.0011(13) 0.0018(13) 0.0005(13) C2 0.0328(19) 0.0287(18) 0.0289(19) 0.0014(15) -0.0013(15) -0.0029(15) C3 0.042(2) 0.041(2) 0.0303(19) -0.0071(17) -0.0042(17) -0.0107(18) C4 0.039(2) 0.0279(19) 0.046(2) -0.0082(17) 0.0085(18) -0.0116(16) C5 0.037(2) 0.0269(18) 0.037(2) 0.0037(16) 0.0084(17) -0.0037(16) C6 0.0294(18) 0.0259(17) 0.0282(18) 0.0022(14) 0.0020(15) -0.0014(14) C7 0.0237(16) 0.0247(16) 0.0234(17) -0.0039(13) 0.0023(13) -0.0021(13) C8 0.0269(19) 0.041(2) 0.0302(19) -0.0068(16) 0.0053(15) 0.0006(16) C9 0.038(2) 0.046(2) 0.0282(19) -0.0082(17) 0.0099(17) -0.0046(18) C10 0.052(3) 0.043(2) 0.0252(19) -0.0015(17) -0.0037(18) -0.0145(19) C11 0.034(2) 0.039(2) 0.035(2) 0.0010(17) -0.0079(17) -0.0057(17) C12 0.0247(17) 0.0330(19) 0.0304(19) -0.0015(15) 0.0007(14) -0.0014(14) C13 0.0210(16) 0.0192(15) 0.0321(18) -0.0002(13) -0.0013(14) 0.0021(12) C14 0.0250(18) 0.0210(17) 0.052(2) 0.0041(16) 0.0052(17) 0.0056(14) C15 0.032(2) 0.033(2) 0.058(3) 0.0062(19) -0.0001(19) 0.0025(16) C16 0.044(3) 0.049(3) 0.063(3) 0.014(2) -0.003(2) 0.010(2) C17 0.043(3) 0.039(2) 0.087(4) 0.028(3) 0.005(3) 0.012(2) C18 0.045(3) 0.023(2) 0.102(4) 0.015(2) 0.001(3) 0.0029(18) C19 0.035(2) 0.0226(18) 0.073(3) 0.0032(19) -0.002(2) 0.0023(16) C20 0.0245(17) 0.0177(15) 0.045(2) -0.0055(15) 0.0004(16) 0.0024(13) C21 0.032(2) 0.037(2) 0.061(3) -0.013(2) -0.005(2) 0.0089(17) C22 0.049(3) 0.051(3) 0.073(4) -0.020(3) -0.028(3) 0.020(2) C23 0.070(3) 0.038(2) 0.050(3) -0.016(2) -0.014(2) 0.014(2) C24 0.044(2) 0.034(2) 0.058(3) -0.019(2) 0.006(2) 0.0032(18) C25 0.0289(19) 0.0286(19) 0.057(3) -0.0144(18) -0.0008(18) 0.0005(15) C26 0.056(3) 0.030(2) 0.066(3) 0.018(2) 0.033(2) 0.0161(19) C27 0.037(2) 0.047(2) 0.045(2) -0.024(2) -0.0040(18) -0.0005(18) C28 0.0248(17) 0.0265(17) 0.040(2) -0.0002(16) 0.0016(15) 0.0040(14) C29 0.0304(19) 0.0289(18) 0.037(2) 0.0005(16) 0.0066(16) -0.0009(15) C30 0.043(2) 0.076(4) 0.033(2) 0.015(2) -0.0073(19) -0.009(2) C31 0.034(2) 0.0216(17) 0.053(3) 0.0018(17) 0.0084(18) -0.0049(15) P1 0.0203(4) 0.0189(4) 0.0236(4) -0.0018(3) 0.0023(3) 0.0010(3) P2 0.0223(4) 0.0171(4) 0.0393(5) -0.0017(4) 0.0023(4) 0.0019(3) P3 0.0247(4) 0.0189(4) 0.0259(4) -0.0020(3) 0.0054(3) 0.0018(3) P4 0.0240(4) 0.0234(4) 0.0265(4) 0.0024(3) 0.0004(3) -0.0023(3) Cl1 0.0388(5) 0.0359(5) 0.0273(4) 0.0002(4) 0.0016(4) -0.0006(4) Cl2 0.0406(7) 0.0305(6) 0.0281(6) 0.000 0.0054(5) 0.000 Cl3 0.0426(7) 0.0356(7) 0.0287(6) 0.000 -0.0020(5) 0.000 _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 P4 2.3268(9) . ? Pt1 P3 2.3279(8) . ? Pt1 P1 2.3328(8) . ? Pt1 P2 2.3459(9) . ? C1 C2 1.395(5) . ? C1 C6 1.405(5) . ? C1 P1 1.814(3) . ? C2 C3 1.392(5) . ? C2 H2 0.9500 . ? C3 C4 1.381(6) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 H4 0.9500 . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.387(5) . ? C7 C8 1.398(5) . ? C7 P1 1.807(3) . ? C8 C9 1.386(6) . ? C8 H8 0.9500 . ? C9 C10 1.372(6) . ? C9 H9 0.9500 . ? C10 C11 1.394(6) . ? C10 H10 0.9500 . ? C11 C12 1.387(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 P2 1.836(3) . ? C13 P1 1.844(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.384(6) . ? C14 C19 1.405(5) . ? C14 P2 1.819(4) . ? C15 C16 1.397(6) . ? C15 H15 0.9500 . ? C16 C17 1.378(7) . ? C16 H16 0.9500 . ? C17 C18 1.379(8) . ? C17 H17 0.9500 . ? C18 C19 1.381(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.387(5) . ? C20 C25 1.394(5) . ? C20 P2 1.810(4) . ? C21 C22 1.388(7) . ? C21 H21 0.9500 . ? C22 C23 1.377(7) . ? C22 H22 0.9500 . ? C23 C24 1.382(7) . ? C23 H23 0.9500 . ? C24 C25 1.380(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 P3 1.809(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 P3 1.809(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 P3 1.816(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 P4 1.805(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 P4 1.815(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 P4 1.817(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P4 Pt1 P3 96.09(3) . . ? P4 Pt1 P1 163.47(3) . . ? P3 Pt1 P1 97.04(3) . . ? P4 Pt1 P2 96.51(3) . . ? P3 Pt1 P2 165.64(3) . . ? P1 Pt1 P2 69.40(3) . . ? C2 C1 C6 119.6(3) . . ? C2 C1 P1 119.2(3) . . ? C6 C1 P1 121.1(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 119.9(3) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C12 C7 C8 119.7(3) . . ? C12 C7 P1 120.3(3) . . ? C8 C7 P1 119.8(3) . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.2(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.6(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 120.3(3) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? P2 C13 P1 92.75(15) . . ? P2 C13 H13A 113.2 . . ? P1 C13 H13A 113.2 . . ? P2 C13 H13B 113.2 . . ? P1 C13 H13B 113.2 . . ? H13A C13 H13B 110.5 . . ? C15 C14 C19 119.5(4) . . ? C15 C14 P2 120.6(3) . . ? C19 C14 P2 119.6(3) . . ? C14 C15 C16 119.8(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.2(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.3(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 119.9(5) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C21 C20 C25 119.4(4) . . ? C21 C20 P2 120.8(3) . . ? C25 C20 P2 119.5(3) . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 119.7(4) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C20 120.6(4) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? P3 C26 H26A 109.5 . . ? P3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P3 C27 H27A 109.5 . . ? P3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? P3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? P3 C28 H28A 109.5 . . ? P3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P4 C29 H29A 109.5 . . ? P4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? P4 C30 H30A 109.5 . . ? P4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P4 C31 H31A 109.5 . . ? P4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C7 P1 C1 104.51(16) . . ? C7 P1 C13 108.37(16) . . ? C1 P1 C13 108.85(15) . . ? C7 P1 Pt1 116.97(12) . . ? C1 P1 Pt1 124.26(11) . . ? C13 P1 Pt1 92.23(11) . . ? C20 P2 C14 106.08(18) . . ? C20 P2 C13 104.30(17) . . ? C14 P2 C13 110.49(16) . . ? C20 P2 Pt1 115.56(12) . . ? C14 P2 Pt1 125.55(13) . . ? C13 P2 Pt1 92.02(11) . . ? C26 P3 C27 103.6(2) . . ? C26 P3 C28 101.7(2) . . ? C27 P3 C28 106.07(19) . . ? C26 P3 Pt1 114.01(14) . . ? C27 P3 Pt1 110.77(15) . . ? C28 P3 Pt1 119.20(12) . . ? C29 P4 C30 102.4(2) . . ? C29 P4 C31 101.91(18) . . ? C30 P4 C31 105.1(2) . . ? C29 P4 Pt1 122.61(13) . . ? C30 P4 Pt1 110.31(16) . . ? C31 P4 Pt1 112.73(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.487 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.105 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 618550' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C10 H28 B Cl2 N P2 Pt' _chemical_formula_sum 'C10 H28 B Cl2 N P2 Pt' _chemical_formula_weight 501.07 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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 10.125(2) _cell_length_b 11.154(2) _cell_length_c 16.404(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1852.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17668 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method none _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 8.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.05 _exptl_absorpt_correction_T_max 0.09 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21217 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4242 _reflns_number_gt 4234 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0268P)^2^+3.1693P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(6) _refine_ls_number_reflns 4242 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Pt1 Pt 0.946178(14) 0.397612(11) -0.041877(8) 0.01492(4) Uani 1 1 d . . . P2 P 0.95488(12) 0.52646(9) -0.14961(6) 0.02032(19) Uani 1 1 d . . . P1 P 0.93943(12) 0.26413(8) 0.06359(5) 0.01734(18) Uani 1 1 d . . . Cl2 Cl 0.71786(10) 0.56355(9) 0.04460(7) 0.02746(19) Uani 1 1 d . . . Cl1 Cl 1.00370(11) 0.23142(9) -0.13388(6) 0.0263(2) Uani 1 1 d . . . N1 N 0.9799(3) 0.6072(4) 0.0767(2) 0.0247(7) Uani 1 1 d . . . C7 C 1.1235(4) 0.5978(5) 0.0656(3) 0.0316(10) Uani 1 1 d . . . H7A H 1.1586 0.6784 0.0524 0.038 Uiso 1 1 calc R . . H7B H 1.1412 0.5452 0.0183 0.038 Uiso 1 1 calc R . . C2 C 0.8374(5) 0.1345(3) 0.0420(3) 0.0286(8) Uani 1 1 d . . . H2A H 0.8656 0.0980 -0.0094 0.043 Uiso 1 1 calc R . . H2B H 0.7448 0.1594 0.0376 0.043 Uiso 1 1 calc R . . H2C H 0.8464 0.0760 0.0862 0.043 Uiso 1 1 calc R . . B1 B 0.8957(5) 0.5331(4) 0.0322(3) 0.0213(9) Uani 1 1 d . . . C9 C 0.9365(5) 0.6980(4) 0.1359(3) 0.0301(9) Uani 1 1 d . . . H9A H 0.9918 0.6918 0.1855 0.036 Uiso 1 1 calc R . . H9B H 0.8440 0.6812 0.1518 0.036 Uiso 1 1 calc R . . C3 C 1.0988(4) 0.1991(4) 0.0890(3) 0.0290(9) Uani 1 1 d . . . H3A H 1.1586 0.2625 0.1078 0.044 Uiso 1 1 calc R . . H3B H 1.1363 0.1604 0.0406 0.044 Uiso 1 1 calc R . . H3C H 1.0875 0.1395 0.1324 0.044 Uiso 1 1 calc R . . C1 C 0.8744(5) 0.3141(4) 0.1611(3) 0.0288(9) Uani 1 1 d . . . H1A H 0.8757 0.2473 0.1999 0.043 Uiso 1 1 calc R . . H1B H 0.7835 0.3423 0.1540 0.043 Uiso 1 1 calc R . . H1C H 0.9292 0.3797 0.1821 0.043 Uiso 1 1 calc R . . C10 C 0.9452(7) 0.8235(4) 0.1033(4) 0.0474(14) Uani 1 1 d . . . H10A H 1.0344 0.8380 0.0823 0.071 Uiso 1 1 calc R . . H10B H 0.9259 0.8806 0.1470 0.071 Uiso 1 1 calc R . . H10C H 0.8810 0.8337 0.0591 0.071 Uiso 1 1 calc R . . C4 C 1.1181(5) 0.5413(6) -0.1911(3) 0.0428(14) Uani 1 1 d . . . H4A H 1.1152 0.5926 -0.2395 0.064 Uiso 1 1 calc R . . H4B H 1.1518 0.4619 -0.2062 0.064 Uiso 1 1 calc R . . H4C H 1.1764 0.5773 -0.1502 0.064 Uiso 1 1 calc R . . C5 C 0.8606(7) 0.4731(6) -0.2370(3) 0.0533(17) Uani 1 1 d . . . H5A H 0.7663 0.4880 -0.2278 0.080 Uiso 1 1 calc R . . H5B H 0.8754 0.3869 -0.2441 0.080 Uiso 1 1 calc R . . H5C H 0.8892 0.5158 -0.2861 0.080 Uiso 1 1 calc R . . C6 C 0.8992(9) 0.6785(5) -0.1384(4) 0.066(2) Uani 1 1 d . . . H6A H 0.9543 0.7196 -0.0980 0.099 Uiso 1 1 calc R . . H6B H 0.8071 0.6788 -0.1202 0.099 Uiso 1 1 calc R . . H6C H 0.9060 0.7199 -0.1909 0.099 Uiso 1 1 calc R . . C8 C 1.1966(6) 0.5501(5) 0.1374(4) 0.0436(12) Uani 1 1 d . . . H8A H 1.1857 0.6048 0.1837 0.065 Uiso 1 1 calc R . . H8B H 1.2906 0.5431 0.1240 0.065 Uiso 1 1 calc R . . H8C H 1.1617 0.4710 0.1519 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02025(7) 0.01199(6) 0.01252(6) 0.00071(5) 0.00135(5) 0.00119(5) P2 0.0240(5) 0.0194(4) 0.0176(4) 0.0055(3) 0.0031(4) 0.0043(4) P1 0.0211(4) 0.0154(4) 0.0155(4) 0.0021(3) 0.0006(4) 0.0013(4) Cl2 0.0266(4) 0.0298(5) 0.0260(5) -0.0015(4) 0.0038(4) 0.0056(4) Cl1 0.0387(5) 0.0215(4) 0.0187(4) -0.0065(4) 0.0012(4) 0.0013(4) N1 0.0297(18) 0.0215(17) 0.0231(16) -0.0040(15) 0.0017(13) 0.0032(15) C7 0.029(2) 0.030(2) 0.036(2) -0.014(2) -0.0041(17) -0.003(2) C2 0.034(2) 0.0195(18) 0.033(2) 0.0080(17) 0.002(2) -0.0015(16) B1 0.032(2) 0.019(2) 0.0132(19) 0.0004(16) 0.0039(17) -0.0004(17) C9 0.041(2) 0.0239(19) 0.025(2) -0.0111(16) -0.003(2) 0.005(2) C3 0.025(2) 0.029(2) 0.033(2) 0.0114(19) -0.0002(17) 0.0046(17) C1 0.033(2) 0.035(2) 0.0180(19) 0.0067(18) 0.0052(16) 0.0057(19) C10 0.057(3) 0.021(2) 0.064(3) -0.005(2) 0.028(3) 0.006(3) C4 0.028(2) 0.068(4) 0.033(3) 0.032(3) 0.012(2) 0.009(2) C5 0.067(4) 0.055(4) 0.037(3) 0.021(3) -0.029(3) -0.022(3) C6 0.128(7) 0.033(3) 0.037(3) 0.021(2) 0.033(3) 0.034(3) C8 0.050(3) 0.031(2) 0.050(3) -0.005(2) -0.006(3) 0.003(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 Pt1 B1 2.005(4) . ? Pt1 P2 2.2795(10) . ? Pt1 P1 2.2835(10) . ? Pt1 Cl1 2.4604(10) . ? P2 C4 1.795(5) . ? P2 C6 1.796(5) . ? P2 C5 1.822(5) . ? P1 C3 1.818(4) . ? P1 C1 1.818(4) . ? P1 C2 1.812(4) . ? Cl2 B1 1.843(5) . ? N1 B1 1.394(6) . ? N1 C7 1.468(5) . ? N1 C9 1.472(5) . ? C7 C8 1.490(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C9 C10 1.501(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Pt1 P2 90.27(13) . . ? B1 Pt1 P1 91.40(13) . . ? P2 Pt1 P1 178.33(4) . . ? B1 Pt1 Cl1 178.86(15) . . ? P2 Pt1 Cl1 89.44(4) . . ? P1 Pt1 Cl1 88.89(4) . . ? C4 P2 C6 103.9(3) . . ? C4 P2 C5 102.4(3) . . ? C6 P2 C5 103.0(3) . . ? C4 P2 Pt1 112.80(16) . . ? C6 P2 Pt1 120.25(18) . . ? C5 P2 Pt1 112.57(19) . . ? C3 P1 C1 104.0(2) . . ? C3 P1 C2 103.5(2) . . ? C1 P1 C2 102.1(2) . . ? C3 P1 Pt1 114.04(15) . . ? C1 P1 Pt1 118.54(15) . . ? C2 P1 Pt1 112.91(16) . . ? B1 N1 C7 120.0(4) . . ? B1 N1 C9 124.8(4) . . ? C7 N1 C9 115.2(4) . . ? N1 C7 C8 114.8(5) . . ? N1 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 B1 Cl2 115.5(3) . . ? N1 B1 Pt1 127.4(3) . . ? Cl2 B1 Pt1 117.1(2) . . ? N1 C9 C10 112.9(4) . . ? N1 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.622 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.100 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 618551' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C12 H22 B Cl O2 P2 Pt' _chemical_formula_sum 'C12 H22 B Cl O2 P2 Pt' _chemical_formula_weight 501.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 '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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 5.8930(16) _cell_length_b 22.748(9) _cell_length_c 12.946(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.56(3) _cell_angle_gamma 90.00 _cell_volume 1727.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_theta_min 28.8385 _cell_measurement_theta_max 70.0625 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method none _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 18.328 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.118 _exptl_absorpt_correction_T_max 0.693 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.602 _diffrn_detector_type 'Bruker-AXS SMART 6000' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation 'Osmic CMF12-38Cu6 (blue) mirror optics' _diffrn_radiation_monochromator 'Osmic CMF12-38Cu6 (blue) mirror optics' _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source rotating-anode _diffrn_source_current 120 _diffrn_source_power 4.8 _diffrn_source_size '3 x 0.3mm' _diffrn_source_target Cu _diffrn_source_type 'MAC Science M18XCE' _diffrn_source_voltage 40 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12164 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 69.99 _reflns_number_total 2972 _reflns_number_gt 2858 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.625 (Bruker-AXS, 1997-2001)' _computing_cell_refinement 'SMART v5.625 (Bruker-AXS, 1997-2001)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.1347P)^2^+0.2504P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2972 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Pt1 Pt 0.29960(4) 0.370266(9) 0.717527(16) 0.0079(2) Uani 1 1 d . . . P2 P 0.0611(4) 0.37546(6) 0.56740(17) 0.0119(4) Uani 1 1 d . . . P1 P 0.5301(4) 0.36388(6) 0.86946(16) 0.0098(4) Uani 1 1 d . . . O1 O 0.0479(6) 0.47590(16) 0.7925(3) 0.0120(8) Uani 1 1 d . . . O2 O 0.3756(7) 0.50345(17) 0.7210(3) 0.0133(8) Uani 1 1 d . . . C1 C 0.0675(9) 0.5365(2) 0.7956(4) 0.0099(11) Uani 1 1 d . . . C6 C -0.0778(9) 0.5765(2) 0.8335(4) 0.0138(11) Uani 1 1 d . . . H6 H -0.2128 0.5645 0.8623 0.017 Uiso 1 1 calc R . . C5 C -0.0161(13) 0.6363(2) 0.8276(5) 0.0150(14) Uani 1 1 d . . . H5 H -0.1124 0.6656 0.8522 0.018 Uiso 1 1 calc R . . C4 C 0.1828(10) 0.6530(3) 0.7864(4) 0.0146(14) Uani 1 1 d . . . H4 H 0.2198 0.6935 0.7837 0.018 Uiso 1 1 calc R . . C2 C 0.2671(10) 0.5537(3) 0.7539(4) 0.0125(11) Uani 1 1 d . . . B1 B 0.2399(10) 0.4549(3) 0.7448(4) 0.0091(12) Uani 1 1 d . . . C3 C 0.3315(11) 0.6114(3) 0.7483(5) 0.0145(12) Uani 1 1 d . . . H3 H 0.4684 0.6227 0.7205 0.017 Uiso 1 1 calc R . . Cl Cl 0.3789(2) 0.26689(6) 0.68988(11) 0.0192(4) Uani 1 1 d . . . C7 C 0.4165(10) 0.3134(3) 0.9599(5) 0.0230(14) Uani 1 1 d . . . H7A H 0.5324 0.3057 1.0178 0.034 Uiso 1 1 calc R . . H7B H 0.3743 0.2764 0.9243 0.034 Uiso 1 1 calc R . . H7C H 0.2814 0.3308 0.9863 0.034 Uiso 1 1 calc R . . C8 C 0.5858(12) 0.4298(3) 0.9459(5) 0.0231(14) Uani 1 1 d . . . H8A H 0.4412 0.4494 0.9557 0.035 Uiso 1 1 calc R . . H8B H 0.6823 0.4564 0.9098 0.035 Uiso 1 1 calc R . . H8C H 0.6638 0.4194 1.0137 0.035 Uiso 1 1 calc R . . C10 C -0.1048(12) 0.3097(3) 0.5359(5) 0.0242(15) Uani 1 1 d . . . H10A H -0.2253 0.3063 0.5826 0.036 Uiso 1 1 calc R . . H10B H -0.0052 0.2751 0.5439 0.036 Uiso 1 1 calc R . . H10C H -0.1735 0.3120 0.4640 0.036 Uiso 1 1 calc R . . C12 C 0.2203(13) 0.3868(3) 0.4553(5) 0.0246(15) Uani 1 1 d . . . H12A H 0.3352 0.3558 0.4529 0.037 Uiso 1 1 calc R . . H12B H 0.2959 0.4252 0.4608 0.037 Uiso 1 1 calc R . . H12C H 0.1156 0.3855 0.3917 0.037 Uiso 1 1 calc R . . C9 C 0.8128(10) 0.3346(3) 0.8579(5) 0.0216(13) Uani 1 1 d . . . H9A H 0.8935 0.3298 0.9272 0.032 Uiso 1 1 calc R . . H9B H 0.8977 0.3618 0.8173 0.032 Uiso 1 1 calc R . . H9C H 0.8000 0.2964 0.8230 0.032 Uiso 1 1 calc R . . C11 C -0.1536(11) 0.4334(3) 0.5571(5) 0.0206(14) Uani 1 1 d . . . H11A H -0.2346 0.4330 0.4873 0.031 Uiso 1 1 calc R . . H11B H -0.0793 0.4716 0.5699 0.031 Uiso 1 1 calc R . . H11C H -0.2623 0.4267 0.6086 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0107(3) 0.0037(3) 0.0094(3) -0.00030(6) 0.00173(19) 0.00013(6) P2 0.0130(10) 0.0106(8) 0.0118(9) 0.0005(5) -0.0002(8) -0.0014(5) P1 0.0115(9) 0.0075(7) 0.0106(9) 0.0008(5) 0.0011(7) -0.0005(5) O1 0.017(2) 0.0031(17) 0.0170(18) -0.0014(15) 0.0058(17) 0.0022(15) O2 0.012(2) 0.0076(19) 0.020(2) 0.0038(16) 0.0014(16) 0.0025(16) C1 0.013(3) 0.008(3) 0.008(2) 0.001(2) -0.004(2) 0.000(2) C6 0.013(3) 0.009(3) 0.019(3) 0.001(2) 0.002(2) 0.001(2) C5 0.021(4) 0.007(3) 0.016(3) -0.006(2) 0.000(3) 0.004(2) C4 0.023(4) 0.005(4) 0.015(3) -0.0004(19) 0.000(3) 0.000(2) C2 0.013(3) 0.010(3) 0.014(3) -0.002(2) 0.000(2) 0.002(2) B1 0.008(3) 0.010(3) 0.009(3) 0.003(2) -0.001(3) 0.000(2) C3 0.013(3) 0.009(3) 0.021(3) 0.001(3) 0.000(3) 0.000(2) Cl 0.0212(8) 0.0076(6) 0.0280(8) -0.0075(5) -0.0009(6) 0.0025(5) C7 0.015(3) 0.034(4) 0.020(3) 0.011(3) 0.002(3) -0.006(3) C8 0.038(4) 0.016(3) 0.014(3) -0.007(2) -0.003(3) -0.001(3) C10 0.031(4) 0.015(3) 0.025(3) 0.000(3) -0.008(3) -0.009(3) C12 0.021(4) 0.035(4) 0.019(3) 0.006(3) 0.007(3) 0.003(3) C9 0.013(3) 0.027(3) 0.025(3) -0.005(3) 0.004(3) 0.002(3) C11 0.021(3) 0.025(3) 0.016(3) 0.002(3) 0.001(3) 0.009(3) _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 B1 1.995(6) . ? Pt1 P1 2.284(2) . ? Pt1 P2 2.289(2) . ? Pt1 Cl 2.4308(16) . ? P2 C10 1.812(7) . ? P2 C12 1.821(7) . ? P2 C11 1.823(7) . ? P1 C8 1.809(6) . ? P1 C7 1.813(6) . ? P1 C9 1.814(6) . ? O1 C1 1.384(6) . ? O1 B1 1.423(7) . ? O2 C2 1.397(7) . ? O2 B1 1.415(7) . ? C1 C6 1.372(8) . ? C1 C2 1.397(8) . ? C6 C5 1.412(8) . ? C6 H6 0.9500 . ? C5 C4 1.387(10) . ? C5 H5 0.9500 . ? C4 C3 1.410(9) . ? C4 H4 0.9500 . ? C2 C3 1.370(8) . ? C3 H3 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Pt1 P1 90.54(18) . . ? B1 Pt1 P2 89.77(18) . . ? P1 Pt1 P2 178.48(5) . . ? B1 Pt1 Cl 178.15(18) . . ? P1 Pt1 Cl 87.63(5) . . ? P2 Pt1 Cl 92.05(5) . . ? C10 P2 C12 104.2(3) . . ? C10 P2 C11 103.0(4) . . ? C12 P2 C11 104.3(3) . . ? C10 P2 Pt1 115.0(2) . . ? C12 P2 Pt1 111.3(3) . . ? C11 P2 Pt1 117.7(2) . . ? C8 P1 C7 103.3(3) . . ? C8 P1 C9 103.3(3) . . ? C7 P1 C9 102.7(3) . . ? C8 P1 Pt1 118.7(2) . . ? C7 P1 Pt1 111.7(2) . . ? C9 P1 Pt1 115.3(2) . . ? C1 O1 B1 106.2(4) . . ? C2 O2 B1 106.7(4) . . ? C6 C1 O1 128.1(5) . . ? C6 C1 C2 122.1(5) . . ? O1 C1 C2 109.8(5) . . ? C1 C6 C5 116.4(5) . . ? C1 C6 H6 121.8 . . ? C5 C6 H6 121.8 . . ? C4 C5 C6 121.1(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C4 C3 121.9(6) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C3 C2 O2 129.1(5) . . ? C3 C2 C1 122.5(6) . . ? O2 C2 C1 108.4(5) . . ? O2 B1 O1 108.8(5) . . ? O2 B1 Pt1 127.0(4) . . ? O1 B1 Pt1 124.2(4) . . ? C2 C3 C4 116.0(5) . . ? C2 C3 H3 122.0 . . ? C4 C3 H3 122.0 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C8 H8A 109.5 . . ? P1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P2 C12 H12A 109.5 . . ? P2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C9 H9A 109.5 . . ? P1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 2.514 _refine_diff_density_min -2.923 _refine_diff_density_rms 0.396 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 618552' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C18 H26 B2 O4 P2 Pt' _chemical_formula_sum 'C18 H26 B2 O4 P2 Pt' _chemical_formula_weight 585.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 14.4914(3) _cell_length_b 9.3235(2) _cell_length_c 16.1496(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.4770(10) _cell_angle_gamma 90.00 _cell_volume 2181.91(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method none _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 13.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.117 _exptl_absorpt_correction_T_max 0.260 _exptl_absorpt_process_details 'SADABS v2.05 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.602 _diffrn_detector_type 'Bruker-AXS SMART 6000' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation 'Osmic CMF12-38Cu6 (blue) mirror optics' _diffrn_radiation_monochromator 'Osmic CMF12-38Cu6 (blue) mirror optics' _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source rotating-anode _diffrn_source_current 120 _diffrn_source_power 4.8 _diffrn_source_size '3 x 0.3mm' _diffrn_source_target Cu _diffrn_source_type 'MAC Science M18XCE' _diffrn_source_voltage 40 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16409 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 70.11 _reflns_number_total 3893 _reflns_number_gt 3792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v5.625 (Bruker-AXS, 1997-2001)' _computing_cell_refinement 'SMART v5.625 (Bruker-AXS, 1997-2001)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.8457P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3893 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.9041(3) -0.1427(4) 0.5537(3) 0.0296(8) Uani 1 1 d . . . C2 C 0.9609(3) -0.2497(5) 0.5245(4) 0.0465(12) Uani 1 1 d . . . H2 H 0.9379 -0.3252 0.4906 0.056 Uiso 1 1 calc R . . C3 C 1.0537(3) -0.2415(5) 0.5470(3) 0.0454(12) Uani 1 1 d . . . H3 H 1.0950 -0.3137 0.5287 0.054 Uiso 1 1 calc R . . C4 C 1.0866(3) -0.1317(6) 0.5949(3) 0.0465(12) Uani 1 1 d . . . H4 H 1.1504 -0.1288 0.6087 0.056 Uiso 1 1 calc R . . C5 C 1.0282(3) -0.0231(7) 0.6242(3) 0.0464(11) Uani 1 1 d . . . H5 H 1.0508 0.0538 0.6571 0.056 Uiso 1 1 calc R . . C6 C 0.9373(3) -0.0342(5) 0.6027(2) 0.0293(8) Uani 1 1 d . . . C7 C 0.6996(3) 0.3320(4) 0.4007(2) 0.0316(9) Uani 1 1 d . . . C8 C 0.7029(4) 0.3751(6) 0.3188(3) 0.0524(14) Uani 1 1 d . . . H8 H 0.6840 0.3140 0.2747 0.063 Uiso 1 1 calc R . . C9 C 0.7361(4) 0.5157(7) 0.3046(3) 0.0586(17) Uani 1 1 d . . . H9 H 0.7406 0.5495 0.2493 0.070 Uiso 1 1 calc R . . C10 C 0.7620(3) 0.6045(6) 0.3684(3) 0.0446(11) Uani 1 1 d . . . H10 H 0.7838 0.6981 0.3563 0.054 Uiso 1 1 calc R . . C11 C 0.7569(3) 0.5607(4) 0.4496(3) 0.0355(10) Uani 1 1 d . . . H11 H 0.7737 0.6224 0.4940 0.043 Uiso 1 1 calc R . . C12 C 0.7262(3) 0.4230(4) 0.4632(3) 0.0252(8) Uani 1 1 d . . . C13 C 0.5957(11) -0.0667(11) 0.8137(6) 0.065(4) Uani 0.683(12) 1 d P A 1 H13A H 0.5289 -0.0510 0.8100 0.097 Uiso 0.683(12) 1 calc PR A 1 H13B H 0.6258 0.0201 0.8348 0.097 Uiso 0.683(12) 1 calc PR A 1 H13C H 0.6085 -0.1469 0.8513 0.097 Uiso 0.683(12) 1 calc PR A 1 C14 C 0.5829(8) -0.2662(9) 0.6831(6) 0.074(4) Uani 0.683(12) 1 d P A 1 H14A H 0.6087 -0.3034 0.6315 0.111 Uiso 0.683(12) 1 calc PR A 1 H14B H 0.5170 -0.2460 0.6750 0.111 Uiso 0.683(12) 1 calc PR A 1 H14C H 0.5906 -0.3377 0.7271 0.111 Uiso 0.683(12) 1 calc PR A 1 C15 C 0.7555(6) -0.1794(12) 0.7480(6) 0.067(4) Uani 0.683(12) 1 d P A 1 H15A H 0.7460 -0.2490 0.7925 0.101 Uiso 0.683(12) 1 calc PR A 1 H15B H 0.7933 -0.0998 0.7687 0.101 Uiso 0.683(12) 1 calc PR A 1 H15C H 0.7871 -0.2261 0.7018 0.101 Uiso 0.683(12) 1 calc PR A 1 C16 C 0.4185(5) 0.1062(8) 0.6827(6) 0.060(2) Uani 0.735(7) 1 d P A 1 H16A H 0.3634 0.1667 0.6778 0.090 Uiso 0.735(7) 1 calc PR A 1 H16B H 0.4380 0.1011 0.7409 0.090 Uiso 0.735(7) 1 calc PR A 1 H16C H 0.4042 0.0095 0.6625 0.090 Uiso 0.735(7) 1 calc PR A 1 C17 C 0.4548(5) 0.2103(10) 0.5236(5) 0.065(3) Uani 0.735(7) 1 d P A 1 H17A H 0.3962 0.2605 0.5320 0.098 Uiso 0.735(7) 1 calc PR A 1 H17B H 0.4429 0.1174 0.4972 0.098 Uiso 0.735(7) 1 calc PR A 1 H17C H 0.4947 0.2682 0.4881 0.098 Uiso 0.735(7) 1 calc PR A 1 C18 C 0.5216(5) 0.3609(6) 0.6623(4) 0.0403(16) Uani 0.735(7) 1 d P A 1 H18A H 0.5693 0.4126 0.6317 0.061 Uiso 0.735(7) 1 calc PR A 1 H18B H 0.5389 0.3562 0.7210 0.061 Uiso 0.735(7) 1 calc PR A 1 H18C H 0.4626 0.4113 0.6562 0.061 Uiso 0.735(7) 1 calc PR A 1 C13A C 0.5154(11) -0.1957(16) 0.7217(9) 0.041(4) Uani 0.317(12) 1 d P A 2 H13D H 0.4949 -0.2319 0.6676 0.061 Uiso 0.317(12) 1 calc PR A 2 H13E H 0.4718 -0.1230 0.7412 0.061 Uiso 0.317(12) 1 calc PR A 2 H13F H 0.5180 -0.2750 0.7614 0.061 Uiso 0.317(12) 1 calc PR A 2 C14A C 0.7065(18) -0.264(2) 0.6994(13) 0.074(9) Uani 0.317(12) 1 d P A 2 H14D H 0.6991 -0.3252 0.7480 0.111 Uiso 0.317(12) 1 calc PR A 2 H14E H 0.7716 -0.2373 0.6937 0.111 Uiso 0.317(12) 1 calc PR A 2 H14F H 0.6860 -0.3154 0.6497 0.111 Uiso 0.317(12) 1 calc PR A 2 C15A C 0.6532(19) -0.0502(19) 0.8082(12) 0.047(5) Uani 0.317(12) 1 d P A 2 H15D H 0.5966 -0.0020 0.8258 0.071 Uiso 0.317(12) 1 calc PR A 2 H15E H 0.7049 0.0175 0.8110 0.071 Uiso 0.317(12) 1 calc PR A 2 H15F H 0.6658 -0.1318 0.8448 0.071 Uiso 0.317(12) 1 calc PR A 2 C16A C 0.4060(10) 0.1025(17) 0.5775(9) 0.025(3) Uani 0.265(7) 1 d P A 2 H16D H 0.3568 0.1747 0.5755 0.038 Uiso 0.265(7) 1 calc PR A 2 H16E H 0.3865 0.0217 0.6120 0.038 Uiso 0.265(7) 1 calc PR A 2 H16F H 0.4186 0.0684 0.5213 0.038 Uiso 0.265(7) 1 calc PR A 2 C17A C 0.5021(10) 0.3667(14) 0.5783(10) 0.031(4) Uani 0.265(7) 1 d P A 2 H17D H 0.5166 0.3645 0.5191 0.046 Uiso 0.265(7) 1 calc PR A 2 H17E H 0.5460 0.4296 0.6072 0.046 Uiso 0.265(7) 1 calc PR A 2 H17F H 0.4393 0.4032 0.5857 0.046 Uiso 0.265(7) 1 calc PR A 2 C18A C 0.4720(10) 0.2185(18) 0.7270(9) 0.033(4) Uani 0.265(7) 1 d P A 2 H18D H 0.4211 0.2877 0.7254 0.049 Uiso 0.265(7) 1 calc PR A 2 H18E H 0.5233 0.2582 0.7596 0.049 Uiso 0.265(7) 1 calc PR A 2 H18F H 0.4509 0.1291 0.7525 0.049 Uiso 0.265(7) 1 calc PR A 2 B1 B 0.7841(3) -0.0035(4) 0.5873(2) 0.0231(8) Uani 1 1 d . . . B2 B 0.6844(3) 0.2133(4) 0.5203(2) 0.0204(8) Uani 1 1 d . . . O1 O 0.81040(18) -0.1255(3) 0.5416(2) 0.0345(6) Uani 1 1 d . . . O2 O 0.8645(2) 0.0552(3) 0.62382(18) 0.0305(7) Uani 1 1 d . . . O3 O 0.6733(2) 0.2012(3) 0.43347(16) 0.0315(6) Uani 1 1 d . . . O4 O 0.71741(17) 0.3531(3) 0.53767(15) 0.0249(5) Uani 1 1 d . . . P1 P 0.64017(7) -0.10852(11) 0.71111(6) 0.0292(2) Uani 1 1 d . . . P2 P 0.51059(6) 0.18233(9) 0.62168(6) 0.0226(2) Uani 1 1 d . . . Pt1 Pt 0.652346(10) 0.067199(14) 0.609648(8) 0.01977(9) Uani 1 1 d . A . 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 0.0230(19) 0.0235(18) 0.042(2) 0.0078(15) 0.0033(16) 0.0056(14) C2 0.028(2) 0.031(2) 0.080(4) -0.003(2) 0.010(2) 0.0089(17) C3 0.033(3) 0.044(3) 0.059(3) 0.019(2) 0.013(2) 0.0151(19) C4 0.025(2) 0.079(4) 0.036(2) 0.013(2) 0.0013(17) 0.014(2) C5 0.030(2) 0.079(3) 0.030(3) -0.007(2) -0.0043(17) 0.004(2) C6 0.027(2) 0.044(2) 0.017(2) 0.0043(16) 0.0027(15) 0.0069(17) C7 0.040(2) 0.033(2) 0.022(2) 0.0081(15) 0.0068(16) 0.0184(16) C8 0.079(4) 0.057(3) 0.021(2) 0.006(2) 0.008(2) 0.029(3) C9 0.074(4) 0.062(4) 0.041(3) 0.036(3) 0.022(3) 0.032(3) C10 0.042(3) 0.042(2) 0.051(3) 0.020(2) 0.014(2) 0.016(2) C11 0.027(2) 0.032(2) 0.047(3) 0.0084(16) 0.0081(19) 0.0079(14) C12 0.021(2) 0.029(2) 0.025(2) 0.0071(13) 0.0053(15) 0.0114(13) C13 0.104(10) 0.061(6) 0.030(5) 0.009(3) 0.027(6) 0.027(6) C14 0.116(9) 0.047(5) 0.059(6) 0.003(4) -0.007(5) -0.049(5) C15 0.057(6) 0.090(8) 0.054(7) 0.047(6) 0.015(5) 0.021(5) C16 0.031(4) 0.038(3) 0.111(7) 0.013(4) 0.023(4) 0.004(3) C17 0.049(5) 0.105(7) 0.041(4) -0.033(4) -0.021(3) 0.048(4) C18 0.051(4) 0.032(3) 0.039(4) -0.023(2) 0.011(3) -0.003(2) C13A 0.057(10) 0.044(8) 0.020(7) 0.008(5) -0.006(6) -0.023(7) C14A 0.115(19) 0.059(12) 0.049(12) 0.048(10) 0.049(12) 0.051(13) C15A 0.077(16) 0.048(10) 0.017(9) 0.005(6) -0.008(10) -0.002(9) C16A 0.019(7) 0.038(7) 0.019(7) -0.009(6) -0.009(5) 0.009(6) C17A 0.031(8) 0.016(7) 0.046(10) -0.008(6) 0.013(6) -0.004(5) C18A 0.028(8) 0.049(9) 0.022(8) -0.018(6) -0.002(6) 0.014(6) B1 0.026(2) 0.027(2) 0.0157(19) 0.0045(15) 0.0040(14) 0.0070(15) B2 0.022(2) 0.0222(19) 0.0167(19) -0.0013(14) 0.0005(14) 0.0069(14) O1 0.0232(14) 0.0260(15) 0.0543(18) -0.0075(12) 0.0025(12) 0.0072(10) O2 0.0281(17) 0.0437(17) 0.0197(15) -0.0059(10) 0.0027(12) 0.0068(10) O3 0.0512(18) 0.0273(13) 0.0159(13) -0.0035(10) -0.0001(11) 0.0110(11) O4 0.0255(13) 0.0269(13) 0.0222(13) 0.0006(10) -0.0020(10) 0.0005(10) P1 0.0395(6) 0.0236(5) 0.0246(5) 0.0041(4) 0.0087(4) 0.0009(4) P2 0.0236(5) 0.0216(4) 0.0225(5) -0.0088(3) -0.0012(3) 0.0035(3) Pt1 0.02329(14) 0.01863(12) 0.01740(13) -0.00121(4) 0.00092(8) 0.00413(4) _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 C6 1.370(6) . ? C1 C2 1.379(6) . ? C1 O1 1.379(5) . ? C2 C3 1.392(7) . ? C2 H2 0.9500 . ? C3 C4 1.366(8) . ? C3 H3 0.9500 . ? C4 C5 1.403(7) . ? C4 H4 0.9500 . ? C5 C6 1.363(6) . ? C5 H5 0.9500 . ? C6 O2 1.390(5) . ? C7 C12 1.372(6) . ? C7 C8 1.383(6) . ? C7 O3 1.385(5) . ? C8 C9 1.416(9) . ? C8 H8 0.9500 . ? C9 C10 1.371(9) . ? C9 H9 0.9500 . ? C10 C11 1.375(7) . ? C10 H10 0.9500 . ? C11 C12 1.377(6) . ? C11 H11 0.9500 . ? C12 O4 1.374(5) . ? C13 P1 1.824(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 P1 1.746(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 P1 1.889(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 P2 1.811(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 P2 1.791(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 P2 1.796(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C13A P1 1.991(14) . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14A P1 1.748(16) . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C15A P1 1.669(19) . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C16A P2 1.828(14) . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17A P2 1.860(14) . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A P2 1.826(14) . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? B1 O1 1.410(5) . ? B1 O2 1.411(5) . ? B1 Pt1 2.055(4) . ? B2 O3 1.415(5) . ? B2 O4 1.416(5) . ? B2 Pt1 2.040(4) . ? P1 Pt1 2.3249(9) . ? P2 Pt1 2.3273(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.6(4) . . ? C6 C1 O1 109.7(3) . . ? C2 C1 O1 128.8(4) . . ? C1 C2 C3 116.7(5) . . ? C1 C2 H2 121.7 . . ? C3 C2 H2 121.7 . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 121.5(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 116.3(5) . . ? C6 C5 H5 121.8 . . ? C4 C5 H5 121.8 . . ? C5 C6 C1 122.5(4) . . ? C5 C6 O2 128.8(4) . . ? C1 C6 O2 108.7(4) . . ? C12 C7 C8 120.9(4) . . ? C12 C7 O3 109.8(3) . . ? C8 C7 O3 129.3(4) . . ? C7 C8 C9 115.9(5) . . ? C7 C8 H8 122.0 . . ? C9 C8 H8 122.0 . . ? C10 C9 C8 121.9(4) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 121.4(5) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C12 116.7(5) . . ? C10 C11 H11 121.7 . . ? C12 C11 H11 121.7 . . ? C7 C12 O4 108.9(3) . . ? C7 C12 C11 123.2(4) . . ? O4 C12 C11 127.9(4) . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? P1 C13A H13D 109.5 . . ? P1 C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? P1 C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? P1 C14A H14D 109.5 . . ? P1 C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? P1 C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? P1 C15A H15D 109.5 . . ? P1 C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? P1 C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? P2 C16A H16D 109.5 . . ? P2 C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? P2 C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? P2 C17A H17D 109.5 . . ? P2 C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? P2 C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? P2 C18A H18D 109.5 . . ? P2 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? P2 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? O1 B1 O2 107.8(3) . . ? O1 B1 Pt1 127.3(3) . . ? O2 B1 Pt1 124.6(3) . . ? O3 B2 O4 107.7(3) . . ? O3 B2 Pt1 128.5(3) . . ? O4 B2 Pt1 123.6(3) . . ? C1 O1 B1 106.9(3) . . ? C6 O2 B1 106.9(3) . . ? C7 O3 B2 106.2(3) . . ? C12 O4 B2 107.3(3) . . ? C15A P1 C14A 108.3(11) . . ? C14 P1 C13 104.1(6) . . ? C14 P1 C15 101.8(5) . . ? C13 P1 C15 96.1(5) . . ? C15A P1 C13A 98.5(10) . . ? C14A P1 C13A 99.9(10) . . ? C15A P1 Pt1 115.1(6) . . ? C14 P1 Pt1 116.7(3) . . ? C14A P1 Pt1 117.5(5) . . ? C13 P1 Pt1 121.3(3) . . ? C15 P1 Pt1 113.4(2) . . ? C13A P1 Pt1 115.0(4) . . ? C17 P2 C18 103.1(4) . . ? C17 P2 C16 102.0(5) . . ? C18 P2 C16 103.2(3) . . ? C18A P2 C16A 100.3(7) . . ? C18A P2 C17A 99.2(7) . . ? C16A P2 C17A 100.2(7) . . ? C17 P2 Pt1 112.7(2) . . ? C18 P2 Pt1 112.5(2) . . ? C16 P2 Pt1 121.3(2) . . ? C18A P2 Pt1 116.1(5) . . ? C16A P2 Pt1 120.6(4) . . ? C17A P2 Pt1 116.8(4) . . ? B2 Pt1 B1 82.66(15) . . ? B2 Pt1 P1 171.02(11) . . ? B1 Pt1 P1 88.50(11) . . ? B2 Pt1 P2 87.57(11) . . ? B1 Pt1 P2 169.98(11) . . ? P1 Pt1 P2 101.18(3) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 70.11 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.467 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.131