# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'A. Orpen' 'Chris Adams' 'Hulya Kara' 'Thomas J Podesta' _publ_contact_author_name 'A. Orpen' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close BRISTOL BS8 1TS UNITED KINGDOM ; _publ_contact_author_email GUY.ORPEN@BRIS.AC.UK _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Pyridinium Boronic acid salts in Crystal Synthesis ; data_2 _database_code_depnum_ccdc_archive 'CCDC 614733' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 B2 N2 Ni O10 S4' _chemical_formula_weight 582.87 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2518(8) _cell_length_b 7.4685(9) _cell_length_c 20.571(2) _cell_angle_alpha 94.368(2) _cell_angle_beta 94.193(2) _cell_angle_gamma 92.638(2) _cell_volume 1106.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11825 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5025 _reflns_number_gt 4104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0282P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5025 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Ni1 Ni 0.00146(2) 0.01185(2) 0.244968(9) 0.01510(7) Uani 1 1 d . . . S1 S -0.05187(5) -0.02583(5) 0.346266(19) 0.01932(10) Uani 1 1 d . . . C1 C -0.1157(2) 0.1789(2) 0.37846(8) 0.0189(3) Uani 1 1 d . . . O1 O -0.15674(17) 0.21059(16) 0.43486(5) 0.0268(3) Uani 1 1 d . . . S2 S -0.07903(6) 0.28921(5) 0.252883(19) 0.02154(10) Uani 1 1 d . . . C2 C -0.1237(2) 0.3340(2) 0.33282(7) 0.0179(3) Uani 1 1 d . . . O2 O -0.16482(16) 0.48125(15) 0.35714(5) 0.0249(3) Uani 1 1 d . . . S3 S 0.08782(6) -0.26346(5) 0.237739(19) 0.02128(10) Uani 1 1 d . . . C3 C 0.1342(2) -0.3085(2) 0.15817(8) 0.0185(3) Uani 1 1 d . . . O3 O 0.18147(17) -0.45356(16) 0.13433(6) 0.0269(3) Uani 1 1 d . . . S4 S 0.04844(5) 0.04740(5) 0.142957(19) 0.01923(10) Uani 1 1 d . . . C4 C 0.1179(2) -0.1561(2) 0.11165(8) 0.0186(3) Uani 1 1 d . . . O4 O 0.15629(17) -0.18949(16) 0.05487(5) 0.0281(3) Uani 1 1 d . . . N1 N 0.76202(18) 0.55004(19) 0.49115(7) 0.0218(3) Uani 1 1 d . . . H1A H 0.7961 0.4698 0.4614 0.026 Uiso 1 1 calc R . . C5 C 0.7164(2) 0.4952(2) 0.54890(8) 0.0235(4) Uani 1 1 d . . . H5A H 0.7232 0.3726 0.5577 0.028 Uiso 1 1 calc R . . C6 C 0.6594(2) 0.6201(2) 0.59529(8) 0.0225(3) Uani 1 1 d . . . H6B H 0.6261 0.5826 0.6361 0.027 Uiso 1 1 calc R . . C7 C 0.6503(2) 0.8003(2) 0.58294(7) 0.0179(3) Uani 1 1 d . . . C8 C 0.7016(2) 0.8499(2) 0.52263(7) 0.0212(3) Uani 1 1 d . . . H8A H 0.6981 0.9719 0.5128 0.025 Uiso 1 1 calc R . . C9 C 0.7576(2) 0.7223(2) 0.47707(8) 0.0237(4) Uani 1 1 d . . . H9A H 0.7928 0.7563 0.4360 0.028 Uiso 1 1 calc R . . B1 B 0.5846(2) 0.9433(2) 0.63696(8) 0.0180(4) Uani 1 1 d . . . O5 O 0.54556(18) 0.87608(16) 0.69378(6) 0.0253(3) Uani 1 1 d . . . H5C H 0.519(3) 0.931(3) 0.7191(10) 0.030 Uiso 1 1 d . . . O6 O 0.56740(16) 1.11503(16) 0.62174(6) 0.0238(3) Uani 1 1 d . . . H6C H 0.534(3) 1.182(3) 0.6528(9) 0.029 Uiso 1 1 d . . . N2 N 0.24477(18) 0.47329(18) 0.99875(6) 0.0211(3) Uani 1 1 d . . . H2A H 0.2134 0.5570 1.0277 0.025 Uiso 1 1 calc R . . C10 C 0.2610(2) 0.3055(2) 1.01648(8) 0.0238(4) Uani 1 1 d . . . H10A H 0.2361 0.2779 1.0594 0.029 Uiso 1 1 calc R . . C11 C 0.3139(2) 0.1734(2) 0.97245(7) 0.0210(3) Uani 1 1 d . . . H11A H 0.3267 0.0547 0.9852 0.025 Uiso 1 1 calc R . . C12 C 0.3488(2) 0.2127(2) 0.90917(7) 0.0168(3) Uani 1 1 d . . . C13 C 0.3275(2) 0.3883(2) 0.89271(8) 0.0211(3) Uani 1 1 d . . . H13A H 0.3494 0.4191 0.8499 0.025 Uiso 1 1 calc R . . C14 C 0.2746(2) 0.5183(2) 0.93830(8) 0.0230(3) Uani 1 1 d . . . H14A H 0.2596 0.6379 0.9269 0.028 Uiso 1 1 calc R . . B2 B 0.4120(2) 0.0574(2) 0.85899(9) 0.0171(4) Uani 1 1 d . . . O7 O 0.44113(18) 0.08420(16) 0.79603(6) 0.0223(3) Uani 1 1 d . . . H7C H 0.422(3) 0.157(3) 0.7824(10) 0.027 Uiso 1 1 d . . . O8 O 0.44452(16) -0.10379(16) 0.88197(6) 0.0224(3) Uani 1 1 d . . . H2C H 0.483(2) -0.174(3) 0.8499(9) 0.027 Uiso 1 1 d . . . O9 O 0.41997(18) 0.34841(16) 0.71860(6) 0.0232(3) Uani 1 1 d . . . H4C H 0.334(3) 0.383(3) 0.7000(10) 0.028 Uiso 1 1 d . . . H4D H 0.463(3) 0.423(3) 0.7364(9) 0.028 Uiso 1 1 d . . . O10 O 0.41203(17) 0.35648(17) 0.20866(6) 0.0236(3) Uani 1 1 d . . . H10C H 0.330(3) 0.396(3) 0.1917(10) 0.028 Uiso 1 1 d . . . H10D H 0.377(3) 0.303(3) 0.2328(9) 0.028 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02001(12) 0.01169(12) 0.01377(11) -0.00219(8) 0.00521(7) 0.00157(8) S1 0.0292(2) 0.0135(2) 0.01599(19) -0.00066(15) 0.00668(15) 0.00391(15) C1 0.0205(8) 0.0179(8) 0.0180(8) -0.0018(6) 0.0026(6) 0.0023(6) O1 0.0421(7) 0.0233(6) 0.0167(6) -0.0008(5) 0.0104(5) 0.0089(5) S2 0.0353(2) 0.0142(2) 0.0162(2) -0.00039(15) 0.00824(16) 0.00526(16) C2 0.0194(8) 0.0180(8) 0.0159(7) -0.0031(6) 0.0029(6) 0.0025(6) O2 0.0386(7) 0.0166(6) 0.0202(6) -0.0028(5) 0.0060(5) 0.0101(5) S3 0.0343(2) 0.0144(2) 0.01601(19) -0.00106(15) 0.00750(16) 0.00589(16) C3 0.0183(8) 0.0181(8) 0.0185(8) -0.0024(6) 0.0014(6) 0.0025(6) O3 0.0415(7) 0.0193(6) 0.0207(6) -0.0026(5) 0.0056(5) 0.0136(5) S4 0.0283(2) 0.0136(2) 0.01634(19) -0.00084(15) 0.00686(15) 0.00305(16) C4 0.0181(8) 0.0184(8) 0.0185(8) -0.0047(6) 0.0035(6) 0.0011(6) O4 0.0455(7) 0.0229(6) 0.0174(6) 0.0001(5) 0.0110(5) 0.0081(5) N1 0.0251(7) 0.0212(7) 0.0186(7) -0.0079(6) 0.0053(5) 0.0050(6) C5 0.0303(9) 0.0165(8) 0.0237(9) -0.0015(7) 0.0051(7) 0.0016(7) C6 0.0303(9) 0.0201(9) 0.0179(8) -0.0006(7) 0.0079(6) 0.0028(7) C7 0.0182(8) 0.0202(8) 0.0148(7) -0.0028(6) 0.0015(6) 0.0025(6) C8 0.0287(9) 0.0181(8) 0.0172(8) 0.0010(6) 0.0038(6) 0.0028(7) C9 0.0285(9) 0.0262(9) 0.0166(8) -0.0005(7) 0.0052(6) 0.0016(7) B1 0.0195(9) 0.0188(9) 0.0155(8) -0.0034(7) 0.0032(6) 0.0033(7) O5 0.0406(7) 0.0199(7) 0.0173(6) -0.0006(5) 0.0121(5) 0.0097(5) O6 0.0343(7) 0.0198(6) 0.0181(6) -0.0006(5) 0.0063(5) 0.0077(5) N2 0.0257(7) 0.0195(7) 0.0177(7) -0.0068(6) 0.0070(5) 0.0027(6) C10 0.0300(9) 0.0259(9) 0.0160(8) -0.0010(7) 0.0059(6) 0.0022(7) C11 0.0293(9) 0.0179(8) 0.0166(8) 0.0021(6) 0.0038(6) 0.0032(7) C12 0.0164(7) 0.0177(8) 0.0159(7) -0.0020(6) 0.0018(6) 0.0005(6) C13 0.0280(9) 0.0190(8) 0.0169(8) -0.0007(6) 0.0080(6) 0.0028(7) C14 0.0302(9) 0.0161(8) 0.0232(8) -0.0005(7) 0.0065(7) 0.0033(7) B2 0.0170(8) 0.0161(9) 0.0177(8) -0.0026(7) 0.0028(6) 0.0012(7) O7 0.0351(7) 0.0156(6) 0.0179(6) 0.0019(5) 0.0081(5) 0.0073(5) O8 0.0317(6) 0.0179(6) 0.0188(6) 0.0003(5) 0.0073(5) 0.0073(5) O9 0.0306(7) 0.0174(6) 0.0215(6) -0.0002(5) 0.0002(5) 0.0049(5) O10 0.0303(7) 0.0178(6) 0.0237(7) 0.0043(5) 0.0034(5) 0.0047(5) _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 Ni1 S3 2.1743(5) . ? Ni1 S2 2.1753(5) . ? Ni1 S1 2.1836(5) . ? Ni1 S4 2.1844(5) . ? S1 C1 1.7164(17) . ? C1 O1 1.2271(19) . ? C1 C2 1.546(2) . ? S2 C2 1.7103(16) . ? C2 O2 1.2317(19) . ? S3 C3 1.7067(16) . ? C3 O3 1.2287(19) . ? C3 C4 1.545(2) . ? S4 C4 1.7171(16) . ? C4 O4 1.2300(19) . ? N1 C9 1.341(2) . ? N1 C5 1.344(2) . ? C5 C6 1.382(2) . ? C6 C7 1.392(2) . ? C7 C8 1.393(2) . ? C7 B1 1.596(2) . ? C8 C9 1.381(2) . ? B1 O5 1.350(2) . ? B1 O6 1.352(2) . ? N2 C10 1.339(2) . ? N2 C14 1.343(2) . ? C10 C11 1.375(2) . ? C11 C12 1.394(2) . ? C12 C13 1.391(2) . ? C12 B2 1.599(2) . ? C13 C14 1.385(2) . ? B2 O8 1.351(2) . ? B2 O7 1.355(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ni1 S2 178.802(18) . . ? S3 Ni1 S1 87.327(16) . . ? S2 Ni1 S1 92.657(16) . . ? S3 Ni1 S4 92.675(16) . . ? S2 Ni1 S4 87.367(16) . . ? S1 Ni1 S4 178.718(17) . . ? C1 S1 Ni1 105.65(6) . . ? O1 C1 C2 117.71(14) . . ? O1 C1 S1 124.75(13) . . ? C2 C1 S1 117.54(11) . . ? C2 S2 Ni1 105.59(6) . . ? O2 C2 C1 116.74(13) . . ? O2 C2 S2 124.89(13) . . ? C1 C2 S2 118.36(11) . . ? C3 S3 Ni1 105.72(6) . . ? O3 C3 C4 116.42(14) . . ? O3 C3 S3 125.24(13) . . ? C4 C3 S3 118.34(11) . . ? C4 S4 Ni1 105.48(6) . . ? O4 C4 C3 117.52(14) . . ? O4 C4 S4 124.79(13) . . ? C3 C4 S4 117.69(11) . . ? C9 N1 C5 122.58(14) . . ? N1 C5 C6 118.96(15) . . ? C5 C6 C7 120.82(15) . . ? C6 C7 C8 117.74(15) . . ? C6 C7 B1 120.36(14) . . ? C8 C7 B1 121.90(15) . . ? C9 C8 C7 120.27(15) . . ? N1 C9 C8 119.62(15) . . ? O5 B1 O6 126.39(15) . . ? O5 B1 C7 115.01(14) . . ? O6 B1 C7 118.56(14) . . ? C10 N2 C14 122.31(14) . . ? N2 C10 C11 119.88(15) . . ? C10 C11 C12 120.32(15) . . ? C13 C12 C11 117.74(15) . . ? C13 C12 B2 122.78(14) . . ? C11 C12 B2 119.48(14) . . ? C14 C13 C12 120.46(15) . . ? N2 C14 C13 119.27(15) . . ? O8 B2 O7 119.60(15) . . ? O8 B2 C12 117.68(14) . . ? O7 B2 C12 122.66(15) . . ? 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 S3 Ni1 S1 C1 176.01(6) . . . . ? S2 Ni1 S1 C1 -2.79(6) . . . . ? S4 Ni1 S1 C1 -93.9(8) . . . . ? Ni1 S1 C1 O1 180.00(13) . . . . ? Ni1 S1 C1 C2 0.63(12) . . . . ? S3 Ni1 S2 C2 -85.1(8) . . . . ? S1 Ni1 S2 C2 4.07(6) . . . . ? S4 Ni1 S2 C2 -177.21(6) . . . . ? O1 C1 C2 O2 2.5(2) . . . . ? S1 C1 C2 O2 -178.08(12) . . . . ? O1 C1 C2 S2 -176.55(12) . . . . ? S1 C1 C2 S2 2.87(17) . . . . ? Ni1 S2 C2 O2 176.28(13) . . . . ? Ni1 S2 C2 C1 -4.76(12) . . . . ? S2 Ni1 S3 C3 -94.8(8) . . . . ? S1 Ni1 S3 C3 175.95(6) . . . . ? S4 Ni1 S3 C3 -2.76(6) . . . . ? Ni1 S3 C3 O3 -177.51(13) . . . . ? Ni1 S3 C3 C4 3.02(12) . . . . ? S3 Ni1 S4 C4 2.06(5) . . . . ? S2 Ni1 S4 C4 -179.14(5) . . . . ? S1 Ni1 S4 C4 -88.0(8) . . . . ? O3 C3 C4 O4 -1.3(2) . . . . ? S3 C3 C4 O4 178.24(12) . . . . ? O3 C3 C4 S4 178.93(12) . . . . ? S3 C3 C4 S4 -1.56(16) . . . . ? Ni1 S4 C4 O4 179.45(13) . . . . ? Ni1 S4 C4 C3 -0.77(12) . . . . ? C9 N1 C5 C6 1.2(2) . . . . ? N1 C5 C6 C7 -0.4(2) . . . . ? C5 C6 C7 C8 -0.4(2) . . . . ? C5 C6 C7 B1 -179.91(14) . . . . ? C6 C7 C8 C9 0.6(2) . . . . ? B1 C7 C8 C9 -179.95(14) . . . . ? C5 N1 C9 C8 -1.1(2) . . . . ? C7 C8 C9 N1 0.1(2) . . . . ? C6 C7 B1 O5 1.7(2) . . . . ? C8 C7 B1 O5 -177.78(14) . . . . ? C6 C7 B1 O6 -176.27(14) . . . . ? C8 C7 B1 O6 4.3(2) . . . . ? C14 N2 C10 C11 1.4(2) . . . . ? N2 C10 C11 C12 -0.7(2) . . . . ? C10 C11 C12 C13 -0.2(2) . . . . ? C10 C11 C12 B2 179.38(14) . . . . ? C11 C12 C13 C14 0.4(2) . . . . ? B2 C12 C13 C14 -179.17(14) . . . . ? C10 N2 C14 C13 -1.2(2) . . . . ? C12 C13 C14 N2 0.3(2) . . . . ? C13 C12 B2 O8 174.08(14) . . . . ? C11 C12 B2 O8 -5.5(2) . . . . ? C13 C12 B2 O7 -3.1(2) . . . . ? C11 C12 B2 O7 177.31(15) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.396 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.076 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 614734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 B2 N2 O10 Pd S4' _chemical_formula_weight 630.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4820(15) _cell_length_b 7.4948(15) _cell_length_c 20.573(4) _cell_angle_alpha 94.45(3) _cell_angle_beta 95.44(3) _cell_angle_gamma 92.08(3) _cell_volume 1143.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4158 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13142 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5232 _reflns_number_gt 4065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0754P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5232 _refine_ls_number_parameters 322 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.003 _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 Pd1 Pd -0.00049(4) 0.01179(3) 0.244181(12) 0.02821(10) Uani 1 1 d . . . S1 S -0.05623(14) -0.02584(12) 0.35050(4) 0.0383(2) Uani 1 1 d . . . C1 C -0.1198(5) 0.1803(5) 0.38043(17) 0.0345(8) Uani 1 1 d . . . O1 O -0.1576(4) 0.2117(4) 0.43667(12) 0.0521(8) Uani 1 1 d . . . S2 S -0.09579(16) 0.29820(12) 0.25480(4) 0.0426(3) Uani 1 1 d . . . C2 C -0.1323(5) 0.3342(5) 0.33541(17) 0.0350(8) Uani 1 1 d . . . O2 O -0.1729(4) 0.4800(3) 0.36019(12) 0.0509(8) Uani 1 1 d . . . S3 S 0.09779(15) -0.27375(12) 0.23432(4) 0.0415(2) Uani 1 1 d . . . C3 C 0.1380(5) -0.3090(5) 0.15439(17) 0.0346(8) Uani 1 1 d . . . O3 O 0.1832(4) -0.4533(4) 0.12982(13) 0.0542(8) Uani 1 1 d . . . S4 S 0.05098(14) 0.04760(12) 0.13735(4) 0.0379(2) Uani 1 1 d . . . C4 C 0.1206(5) -0.1567(5) 0.10844(17) 0.0359(8) Uani 1 1 d . . . O4 O 0.1585(5) -0.1896(4) 0.05220(13) 0.0567(8) Uani 1 1 d . . . N1 N 0.7596(4) 0.5509(4) 0.49336(15) 0.0423(8) Uani 1 1 d . . . H1A H 0.7922 0.4730 0.4644 0.051 Uiso 1 1 calc R . . C5 C 0.7169(6) 0.4963(5) 0.55039(19) 0.0471(10) Uani 1 1 d . . . H5A H 0.7245 0.3766 0.5588 0.056 Uiso 1 1 calc R . . C6 C 0.6616(6) 0.6193(5) 0.59630(18) 0.0433(10) Uani 1 1 d . . . H6B H 0.6311 0.5822 0.6361 0.052 Uiso 1 1 calc R . . C7 C 0.6506(5) 0.7988(5) 0.58425(16) 0.0329(8) Uani 1 1 d . . . C8 C 0.6995(5) 0.8467(5) 0.52436(17) 0.0399(9) Uani 1 1 d . . . H8A H 0.6952 0.9657 0.5146 0.048 Uiso 1 1 calc R . . C9 C 0.7536(6) 0.7214(6) 0.47968(17) 0.0452(10) Uani 1 1 d . . . H9A H 0.7863 0.7549 0.4397 0.054 Uiso 1 1 calc R . . B1 B 0.5849(6) 0.9416(5) 0.63724(19) 0.0337(9) Uani 1 1 d . . . O5 O 0.5450(5) 0.8744(4) 0.69318(14) 0.0465(8) Uani 1 1 d . . . H5C H 0.512(7) 0.923(7) 0.709(2) 0.056 Uiso 1 1 d . . . O6 O 0.5721(4) 1.1116(4) 0.62235(13) 0.0452(7) Uani 1 1 d . . . H6C H 0.545(7) 1.169(6) 0.646(2) 0.054 Uiso 1 1 d . . . N2 N 0.2464(4) 0.4723(4) 0.99546(14) 0.0407(8) Uani 1 1 d . . . H2A H 0.2155 0.5535 1.0236 0.049 Uiso 1 1 calc R . . C10 C 0.2637(6) 0.3064(5) 1.01293(17) 0.0436(10) Uani 1 1 d . . . H10A H 0.2400 0.2791 1.0547 0.052 Uiso 1 1 calc R . . C11 C 0.3160(5) 0.1763(5) 0.96973(16) 0.0398(9) Uani 1 1 d . . . H11A H 0.3286 0.0606 0.9824 0.048 Uiso 1 1 calc R . . C12 C 0.3509(5) 0.2139(5) 0.90705(16) 0.0315(8) Uani 1 1 d . . . C13 C 0.3279(5) 0.3893(5) 0.89035(17) 0.0399(9) Uani 1 1 d . . . H13A H 0.3482 0.4199 0.8486 0.048 Uiso 1 1 calc R . . C14 C 0.2753(6) 0.5171(5) 0.93569(18) 0.0445(10) Uani 1 1 d . . . H14A H 0.2600 0.6340 0.9247 0.053 Uiso 1 1 calc R . . B2 B 0.4160(6) 0.0595(5) 0.85780(19) 0.0321(9) Uani 1 1 d . . . O7 O 0.4499(4) 0.0874(3) 0.79637(12) 0.0383(6) Uani 1 1 d . . . H7C H 0.416(5) 0.166(5) 0.7722(19) 0.046 Uiso 1 1 d . . . O8 O 0.4441(4) -0.1007(3) 0.88134(12) 0.0432(7) Uani 1 1 d . . . H2C H 0.477(6) -0.157(6) 0.853(2) 0.052 Uiso 1 1 d . . . O9 O 0.4260(4) 0.3501(4) 0.71756(14) 0.0443(7) Uani 1 1 d D . . H4C H 0.348(6) 0.373(6) 0.691(2) 0.053 Uiso 1 1 d . . . H4D H 0.488(5) 0.439(4) 0.7345(18) 0.053 Uiso 1 1 d D . . O10 O 0.4078(5) 0.3546(4) 0.20715(15) 0.0470(8) Uani 1 1 d . . . H10C H 0.339(7) 0.382(7) 0.191(2) 0.056 Uiso 1 1 d . . . H10D H 0.375(6) 0.289(6) 0.238(2) 0.056 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03274(16) 0.02025(14) 0.03209(16) -0.00485(10) 0.01093(10) 0.00193(10) S1 0.0545(7) 0.0257(4) 0.0367(5) -0.0003(4) 0.0152(4) 0.0088(4) C1 0.038(2) 0.0303(18) 0.0345(18) -0.0046(15) 0.0060(15) 0.0065(16) O1 0.082(2) 0.0450(16) 0.0332(14) -0.0013(12) 0.0220(14) 0.0190(15) S2 0.0676(7) 0.0256(4) 0.0374(5) 0.0004(4) 0.0181(5) 0.0119(5) C2 0.040(2) 0.0292(18) 0.0356(18) -0.0063(15) 0.0084(15) 0.0068(16) O2 0.080(2) 0.0320(14) 0.0417(15) -0.0068(12) 0.0131(14) 0.0233(14) S3 0.0639(7) 0.0262(4) 0.0364(5) -0.0017(4) 0.0161(4) 0.0109(4) C3 0.036(2) 0.0306(18) 0.0364(18) -0.0069(15) 0.0059(15) 0.0084(16) O3 0.086(2) 0.0379(15) 0.0403(15) -0.0058(12) 0.0121(14) 0.0286(15) S4 0.0527(6) 0.0259(4) 0.0372(5) -0.0008(4) 0.0159(4) 0.0054(4) C4 0.037(2) 0.0335(19) 0.0373(19) -0.0050(16) 0.0095(16) 0.0038(16) O4 0.090(2) 0.0459(17) 0.0381(15) -0.0020(13) 0.0269(15) 0.0185(16) N1 0.047(2) 0.0396(18) 0.0396(17) -0.0141(14) 0.0121(14) 0.0063(15) C5 0.063(3) 0.0302(19) 0.049(2) -0.0073(17) 0.018(2) 0.0054(19) C6 0.061(3) 0.033(2) 0.039(2) -0.0011(16) 0.0187(19) 0.0046(19) C7 0.033(2) 0.0325(18) 0.0330(17) -0.0055(15) 0.0086(15) 0.0066(15) C8 0.053(3) 0.0348(19) 0.0335(18) 0.0011(16) 0.0100(17) 0.0077(18) C9 0.056(3) 0.050(2) 0.0315(19) -0.0025(17) 0.0148(18) 0.004(2) B1 0.040(3) 0.031(2) 0.0301(19) -0.0059(17) 0.0089(17) 0.0077(18) O5 0.071(2) 0.0338(15) 0.0385(16) -0.0005(12) 0.0235(14) 0.0159(14) O6 0.066(2) 0.0321(15) 0.0402(15) 0.0000(12) 0.0148(14) 0.0165(14) N2 0.049(2) 0.0362(17) 0.0373(17) -0.0111(14) 0.0142(14) 0.0052(15) C10 0.059(3) 0.043(2) 0.0299(18) -0.0018(17) 0.0145(18) 0.005(2) C11 0.057(3) 0.0313(19) 0.0321(18) 0.0005(15) 0.0109(17) 0.0058(18) C12 0.033(2) 0.0297(17) 0.0314(17) -0.0046(14) 0.0077(14) 0.0009(15) C13 0.055(3) 0.0312(19) 0.0356(19) -0.0007(16) 0.0167(17) 0.0044(18) C14 0.058(3) 0.0297(19) 0.047(2) -0.0006(17) 0.0157(19) 0.0081(19) B2 0.031(2) 0.031(2) 0.034(2) -0.0045(17) 0.0056(16) 0.0019(17) O7 0.0553(18) 0.0290(13) 0.0330(13) -0.0007(10) 0.0155(12) 0.0113(12) O8 0.062(2) 0.0323(14) 0.0378(14) -0.0001(11) 0.0157(13) 0.0135(13) O9 0.056(2) 0.0301(14) 0.0464(16) 0.0014(12) 0.0005(13) 0.0098(13) O10 0.062(2) 0.0326(15) 0.0482(18) 0.0034(13) 0.0090(15) 0.0118(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S2 2.2873(11) . ? Pd1 S3 2.2883(11) . ? Pd1 S4 2.3012(10) . ? Pd1 S1 2.3018(10) . ? S1 C1 1.718(4) . ? C1 O1 1.224(4) . ? C1 C2 1.535(5) . ? S2 C2 1.709(3) . ? C2 O2 1.230(4) . ? S3 C3 1.702(3) . ? C3 O3 1.231(4) . ? C3 C4 1.539(5) . ? S4 C4 1.716(4) . ? C4 O4 1.226(4) . ? N1 C9 1.331(5) . ? N1 C5 1.335(5) . ? C5 C6 1.371(5) . ? C6 C7 1.391(5) . ? C7 C8 1.388(5) . ? C7 B1 1.592(5) . ? C8 C9 1.362(5) . ? B1 O6 1.338(5) . ? B1 O5 1.346(5) . ? N2 C10 1.328(5) . ? N2 C14 1.335(5) . ? C10 C11 1.361(5) . ? C11 C12 1.388(5) . ? C12 C13 1.397(5) . ? C12 B2 1.599(5) . ? C13 C14 1.379(5) . ? B2 O7 1.343(5) . ? B2 O8 1.345(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 S2 Pd1 S3 179.34(4) . . ? S2 Pd1 S4 89.96(4) . . ? S3 Pd1 S4 90.25(4) . . ? S2 Pd1 S1 90.09(4) . . ? S3 Pd1 S1 89.71(4) . . ? S4 Pd1 S1 179.14(4) . . ? C1 S1 Pd1 104.67(13) . . ? O1 C1 C2 117.3(3) . . ? O1 C1 S1 123.1(3) . . ? C2 C1 S1 119.6(2) . . ? C2 S2 Pd1 104.84(13) . . ? O2 C2 C1 116.6(3) . . ? O2 C2 S2 123.1(3) . . ? C1 C2 S2 120.4(2) . . ? C3 S3 Pd1 104.78(13) . . ? O3 C3 C4 116.0(3) . . ? O3 C3 S3 123.4(3) . . ? C4 C3 S3 120.6(2) . . ? C4 S4 Pd1 104.59(13) . . ? O4 C4 C3 117.1(3) . . ? O4 C4 S4 123.4(3) . . ? C3 C4 S4 119.5(2) . . ? C9 N1 C5 122.5(3) . . ? N1 C5 C6 119.0(4) . . ? C5 C6 C7 120.9(4) . . ? C8 C7 C6 117.0(3) . . ? C8 C7 B1 122.0(3) . . ? C6 C7 B1 121.0(3) . . ? C9 C8 C7 120.7(4) . . ? N1 C9 C8 119.8(3) . . ? O6 B1 O5 126.8(3) . . ? O6 B1 C7 118.5(3) . . ? O5 B1 C7 114.7(3) . . ? C10 N2 C14 122.2(3) . . ? N2 C10 C11 120.0(3) . . ? C10 C11 C12 120.9(3) . . ? C11 C12 C13 117.2(3) . . ? C11 C12 B2 119.9(3) . . ? C13 C12 B2 123.0(3) . . ? C14 C13 C12 120.0(3) . . ? N2 C14 C13 119.7(3) . . ? O7 B2 O8 120.3(3) . . ? O7 B2 C12 122.5(3) . . ? O8 B2 C12 117.1(3) . . ? 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 S2 Pd1 S1 C1 -4.41(14) . . . . ? S3 Pd1 S1 C1 174.96(14) . . . . ? S4 Pd1 S1 C1 -98(2) . . . . ? Pd1 S1 C1 O1 -178.8(3) . . . . ? Pd1 S1 C1 C2 1.6(3) . . . . ? S3 Pd1 S2 C2 -66(3) . . . . ? S4 Pd1 S2 C2 -174.86(14) . . . . ? S1 Pd1 S2 C2 6.00(14) . . . . ? O1 C1 C2 O2 2.7(5) . . . . ? S1 C1 C2 O2 -177.7(3) . . . . ? O1 C1 C2 S2 -175.9(3) . . . . ? S1 C1 C2 S2 3.7(4) . . . . ? Pd1 S2 C2 O2 174.7(3) . . . . ? Pd1 S2 C2 C1 -6.9(3) . . . . ? S2 Pd1 S3 C3 -113(3) . . . . ? S4 Pd1 S3 C3 -4.29(14) . . . . ? S1 Pd1 S3 C3 174.85(14) . . . . ? Pd1 S3 C3 O3 -175.6(3) . . . . ? Pd1 S3 C3 C4 5.0(3) . . . . ? S2 Pd1 S4 C4 -177.48(14) . . . . ? S3 Pd1 S4 C4 3.14(14) . . . . ? S1 Pd1 S4 C4 -84(2) . . . . ? O3 C3 C4 O4 -2.3(5) . . . . ? S3 C3 C4 O4 177.2(3) . . . . ? O3 C3 C4 S4 177.8(3) . . . . ? S3 C3 C4 S4 -2.7(4) . . . . ? Pd1 S4 C4 O4 179.0(3) . . . . ? Pd1 S4 C4 C3 -1.1(3) . . . . ? C9 N1 C5 C6 1.2(6) . . . . ? N1 C5 C6 C7 -0.3(6) . . . . ? C5 C6 C7 C8 -0.6(6) . . . . ? C5 C6 C7 B1 179.5(4) . . . . ? C6 C7 C8 C9 0.7(6) . . . . ? B1 C7 C8 C9 -179.4(4) . . . . ? C5 N1 C9 C8 -1.1(6) . . . . ? C7 C8 C9 N1 0.1(6) . . . . ? C8 C7 B1 O6 1.9(6) . . . . ? C6 C7 B1 O6 -178.2(4) . . . . ? C8 C7 B1 O5 -179.0(4) . . . . ? C6 C7 B1 O5 0.9(6) . . . . ? C14 N2 C10 C11 1.4(6) . . . . ? N2 C10 C11 C12 -0.4(6) . . . . ? C10 C11 C12 C13 -0.7(6) . . . . ? C10 C11 C12 B2 178.8(4) . . . . ? C11 C12 C13 C14 0.9(6) . . . . ? B2 C12 C13 C14 -178.5(3) . . . . ? C10 N2 C14 C13 -1.2(6) . . . . ? C12 C13 C14 N2 0.0(6) . . . . ? C11 C12 B2 O7 179.3(4) . . . . ? C13 C12 B2 O7 -1.3(6) . . . . ? C11 C12 B2 O8 -3.7(5) . . . . ? C13 C12 B2 O8 175.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.866 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.129 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 614735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 B2 N2 O10 Pt S4' _chemical_formula_weight 719.25 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4202(8) _cell_length_b 7.4598(8) _cell_length_c 20.396(2) _cell_angle_alpha 94.419(2) _cell_angle_beta 96.480(2) _cell_angle_gamma 92.585(2) _cell_volume 1116.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4480 _cell_measurement_theta_min 2.7425 _cell_measurement_theta_max 27.349 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 6.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.146 _exptl_absorpt_correction_T_max 0.715 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11507 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5057 _reflns_number_gt 4240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5057 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Pt1 Pt -0.00102(3) 0.01126(3) 0.243290(10) 0.01660(8) Uani 1 1 d . . . S1 S -0.0588(2) -0.02598(18) 0.34990(7) 0.0214(3) Uani 1 1 d . . . C1 C -0.1193(8) 0.1808(8) 0.3800(3) 0.0214(12) Uani 1 1 d . . . O1 O -0.1557(6) 0.2128(6) 0.43666(19) 0.0282(10) Uani 1 1 d . . . S2 S -0.0970(2) 0.29787(18) 0.25301(7) 0.0223(3) Uani 1 1 d . . . C2 C -0.1299(8) 0.3365(7) 0.3347(3) 0.0195(12) Uani 1 1 d . . . O2 O -0.1702(6) 0.4831(5) 0.35902(19) 0.0277(10) Uani 1 1 d . . . S3 S 0.0956(2) -0.27513(19) 0.23443(7) 0.0224(3) Uani 1 1 d . . . C3 C 0.1342(8) -0.3126(8) 0.1539(3) 0.0212(12) Uani 1 1 d . . . O3 O 0.1786(6) -0.4582(6) 0.1295(2) 0.0285(10) Uani 1 1 d . . . S4 S 0.0536(2) 0.04645(18) 0.13628(7) 0.0216(3) Uani 1 1 d . . . C4 C 0.1207(8) -0.1592(8) 0.1072(3) 0.0214(12) Uani 1 1 d . . . O4 O 0.1593(7) -0.1921(6) 0.0509(2) 0.0328(11) Uani 1 1 d . . . N1 N 0.7610(7) 0.5487(7) 0.4930(2) 0.0238(11) Uani 1 1 d . . . H1A H 0.7953 0.4685 0.4636 0.029 Uiso 1 1 calc R . . C5 C 0.7166(9) 0.4950(8) 0.5503(3) 0.0284(14) Uani 1 1 d . . . H5A H 0.7248 0.3725 0.5595 0.034 Uiso 1 1 calc R . . C6 C 0.6589(8) 0.6185(8) 0.5960(3) 0.0230(13) Uani 1 1 d . . . H6B H 0.6259 0.5801 0.6366 0.028 Uiso 1 1 calc R . . C7 C 0.6481(8) 0.7983(8) 0.5836(3) 0.0206(12) Uani 1 1 d . . . C8 C 0.7007(8) 0.8474(8) 0.5233(3) 0.0244(13) Uani 1 1 d . . . H8A H 0.6984 0.9696 0.5134 0.029 Uiso 1 1 calc R . . C9 C 0.7550(8) 0.7211(8) 0.4789(3) 0.0262(14) Uani 1 1 d . . . H9A H 0.7888 0.7552 0.4379 0.031 Uiso 1 1 calc R . . B1 B 0.5828(9) 0.9400(9) 0.6368(3) 0.0199(14) Uani 1 1 d . . . O5 O 0.5341(6) 0.8711(6) 0.6919(2) 0.0250(10) Uani 1 1 d . . . H5C H 0.506(10) 0.916(10) 0.718(3) 0.030 Uiso 1 1 d . . . O6 O 0.5747(6) 1.1138(6) 0.6226(2) 0.0246(9) Uani 1 1 d . . . H6C H 0.547(9) 1.183(9) 0.651(3) 0.030 Uiso 1 1 d . . . N2 N 0.2477(7) 0.4726(7) 0.9946(2) 0.0236(11) Uani 1 1 d . . . H2A H 0.2166 0.5562 1.0234 0.028 Uiso 1 1 calc R . . C10 C 0.2631(8) 0.3045(8) 1.0125(3) 0.0224(13) Uani 1 1 d . . . H10A H 0.2359 0.2760 1.0550 0.027 Uiso 1 1 calc R . . C11 C 0.3182(8) 0.1739(8) 0.9695(3) 0.0231(13) Uani 1 1 d . . . H11A H 0.3321 0.0554 0.9827 0.028 Uiso 1 1 calc R . . C12 C 0.3542(7) 0.2136(7) 0.9061(3) 0.0182(12) Uani 1 1 d . . . C13 C 0.3323(8) 0.3888(8) 0.8899(3) 0.0228(13) Uani 1 1 d . . . H13A H 0.3553 0.4204 0.8473 0.027 Uiso 1 1 calc R . . C14 C 0.2782(8) 0.5180(8) 0.9341(3) 0.0250(14) Uani 1 1 d . . . H14A H 0.2625 0.6374 0.9222 0.030 Uiso 1 1 calc R . . B2 B 0.4189(9) 0.0586(8) 0.8571(3) 0.0184(13) Uani 1 1 d . . . O7 O 0.4623(6) 0.0890(6) 0.7962(2) 0.0219(10) Uani 1 1 d . . . H7C H 0.453(10) 0.154(9) 0.781(4) 0.026 Uiso 1 1 d . . . O8 O 0.4439(6) -0.1031(6) 0.8806(2) 0.0257(10) Uani 1 1 d . . . H2C H 0.479(10) -0.155(10) 0.857(4) 0.031 Uiso 1 1 d . . . O9 O 0.4308(7) 0.3501(6) 0.7165(2) 0.0273(11) Uani 1 1 d . . . H4C H 0.354(10) 0.390(10) 0.693(4) 0.033 Uiso 1 1 d . . . H4D H 0.473(10) 0.424(11) 0.735(3) 0.033 Uiso 1 1 d . . . O10 O 0.4045(7) 0.3521(6) 0.2075(2) 0.0277(10) Uani 1 1 d . . . H10C H 0.332(10) 0.412(10) 0.191(4) 0.033 Uiso 1 1 d . . . H10D H 0.374(9) 0.309(10) 0.234(3) 0.033 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02155(13) 0.01024(11) 0.01914(13) -0.00111(8) 0.00894(8) 0.00057(8) S1 0.0317(8) 0.0132(6) 0.0212(7) 0.0007(6) 0.0109(6) 0.0040(6) C1 0.019(3) 0.020(3) 0.026(3) 0.003(3) 0.003(2) 0.004(2) O1 0.041(3) 0.025(2) 0.020(2) -0.0009(18) 0.0122(19) 0.007(2) S2 0.0357(9) 0.0133(7) 0.0199(7) 0.0008(6) 0.0104(6) 0.0053(6) C2 0.021(3) 0.015(3) 0.023(3) -0.003(2) 0.005(2) 0.003(2) O2 0.043(3) 0.019(2) 0.021(2) -0.0025(18) 0.0075(19) 0.0107(19) S3 0.0339(9) 0.0137(7) 0.0213(7) 0.0010(6) 0.0094(6) 0.0064(6) C3 0.018(3) 0.022(3) 0.024(3) -0.002(3) 0.003(2) 0.003(2) O3 0.040(3) 0.022(2) 0.025(2) 0.0007(19) 0.0074(19) 0.0156(19) S4 0.0319(8) 0.0143(7) 0.0204(7) 0.0015(6) 0.0103(6) 0.0036(6) C4 0.022(3) 0.019(3) 0.025(3) -0.002(2) 0.008(2) 0.003(2) O4 0.054(3) 0.025(2) 0.023(2) 0.0018(19) 0.017(2) 0.012(2) N1 0.027(3) 0.023(3) 0.021(2) -0.005(2) 0.009(2) 0.004(2) C5 0.037(4) 0.018(3) 0.033(3) 0.003(3) 0.012(3) -0.001(3) C6 0.029(3) 0.019(3) 0.022(3) 0.003(2) 0.010(2) 0.000(2) C7 0.022(3) 0.020(3) 0.020(3) -0.004(2) 0.005(2) 0.003(2) C8 0.025(3) 0.021(3) 0.029(3) 0.005(3) 0.007(3) 0.004(2) C9 0.033(4) 0.026(3) 0.021(3) 0.002(3) 0.010(3) -0.002(3) B1 0.024(4) 0.016(3) 0.020(3) 0.000(3) 0.005(3) 0.003(3) O5 0.036(3) 0.020(2) 0.022(2) 0.0017(18) 0.0132(19) 0.0081(19) O6 0.034(3) 0.019(2) 0.022(2) -0.0020(18) 0.0091(18) 0.0043(18) N2 0.027(3) 0.021(3) 0.024(3) -0.005(2) 0.009(2) 0.002(2) C10 0.025(3) 0.022(3) 0.022(3) 0.002(2) 0.010(2) 0.003(2) C11 0.029(3) 0.018(3) 0.023(3) 0.002(2) 0.006(2) 0.001(2) C12 0.016(3) 0.019(3) 0.021(3) 0.002(2) 0.004(2) 0.002(2) C13 0.033(3) 0.019(3) 0.017(3) 0.002(2) 0.011(2) 0.001(3) C14 0.032(4) 0.016(3) 0.029(3) 0.003(3) 0.011(3) 0.001(3) B2 0.023(4) 0.014(3) 0.020(3) -0.003(3) 0.008(3) 0.004(3) O7 0.033(2) 0.016(2) 0.019(2) 0.0026(17) 0.0103(18) 0.0076(19) O8 0.037(3) 0.019(2) 0.024(2) 0.0027(18) 0.0115(19) 0.0082(19) O9 0.041(3) 0.017(2) 0.024(2) 0.0023(18) 0.003(2) 0.007(2) O10 0.040(3) 0.017(2) 0.028(2) 0.0064(19) 0.009(2) 0.0086(19) _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 S3 2.2847(14) . ? Pt1 S2 2.2851(14) . ? Pt1 S4 2.2968(13) . ? Pt1 S1 2.2981(13) . ? S1 C1 1.714(6) . ? C1 O1 1.224(7) . ? C1 C2 1.538(7) . ? S2 C2 1.715(5) . ? C2 O2 1.230(7) . ? S3 C3 1.703(6) . ? C3 O3 1.234(7) . ? C3 C4 1.543(8) . ? S4 C4 1.717(6) . ? C4 O4 1.225(6) . ? N1 C5 1.335(7) . ? N1 C9 1.341(8) . ? C5 C6 1.376(8) . ? C6 C7 1.389(8) . ? C7 C8 1.401(7) . ? C7 B1 1.587(8) . ? C8 C9 1.363(8) . ? B1 O5 1.350(7) . ? B1 O6 1.353(7) . ? N2 C10 1.339(7) . ? N2 C14 1.345(7) . ? C10 C11 1.368(8) . ? C11 C12 1.401(7) . ? C12 C13 1.384(8) . ? C12 B2 1.596(8) . ? C13 C14 1.374(8) . ? B2 O8 1.345(8) . ? B2 O7 1.350(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Pt1 S2 179.56(5) . . ? S3 Pt1 S4 90.17(5) . . ? S2 Pt1 S4 90.22(5) . . ? S3 Pt1 S1 89.67(5) . . ? S2 Pt1 S1 89.94(5) . . ? S4 Pt1 S1 179.33(6) . . ? C1 S1 Pt1 104.98(19) . . ? O1 C1 C2 117.1(5) . . ? O1 C1 S1 123.3(4) . . ? C2 C1 S1 119.6(4) . . ? C2 S2 Pt1 105.0(2) . . ? O2 C2 C1 117.1(5) . . ? O2 C2 S2 123.0(4) . . ? C1 C2 S2 119.8(4) . . ? C3 S3 Pt1 104.9(2) . . ? O3 C3 C4 115.8(5) . . ? O3 C3 S3 123.7(4) . . ? C4 C3 S3 120.5(4) . . ? C4 S4 Pt1 104.95(19) . . ? O4 C4 C3 117.4(5) . . ? O4 C4 S4 123.5(4) . . ? C3 C4 S4 119.1(4) . . ? C5 N1 C9 121.9(5) . . ? N1 C5 C6 119.5(5) . . ? C5 C6 C7 120.9(5) . . ? C6 C7 C8 117.0(5) . . ? C6 C7 B1 120.5(5) . . ? C8 C7 B1 122.5(5) . . ? C9 C8 C7 120.5(5) . . ? N1 C9 C8 120.1(5) . . ? O5 B1 O6 126.2(5) . . ? O5 B1 C7 115.3(5) . . ? O6 B1 C7 118.4(5) . . ? C10 N2 C14 122.2(5) . . ? N2 C10 C11 119.9(5) . . ? C10 C11 C12 120.4(5) . . ? C13 C12 C11 117.0(5) . . ? C13 C12 B2 123.7(5) . . ? C11 C12 B2 119.3(5) . . ? C14 C13 C12 121.5(5) . . ? N2 C14 C13 118.9(5) . . ? O8 B2 O7 120.1(5) . . ? O8 B2 C12 117.3(5) . . ? O7 B2 C12 122.4(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.902 _refine_diff_density_min -2.341 _refine_diff_density_rms 0.216 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 614736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 B2 N2 O12 Pt' _chemical_formula_weight 618.98 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' O O 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.6754(6) _cell_length_b 10.5135(17) _cell_length_c 12.215(2) _cell_angle_alpha 102.091(2) _cell_angle_beta 96.403(3) _cell_angle_gamma 98.557(2) _cell_volume 451.38(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4142 _cell_measurement_theta_min 5.873 _cell_measurement_theta_max 54.961 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 7.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.096 _exptl_absorpt_correction_T_max 0.676 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4794 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2041 _reflns_number_gt 2040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0000P)^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_number_reflns 2041 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.5000 0.5000 0.5000 0.01420(7) Uani 1 2 d S . . O5 O 0.3691(7) 0.3669(3) 0.34976(19) 0.0193(5) Uani 1 1 d . . . C1 C 0.1542(9) 0.2602(4) 0.3556(3) 0.0177(7) Uani 1 1 d . . . O1 O 0.0308(7) 0.1676(3) 0.2761(2) 0.0248(6) Uani 1 1 d . . . O6 O 0.2200(7) 0.3518(2) 0.55583(19) 0.0174(5) Uani 1 1 d . . . C2 C 0.0513(9) 0.2550(4) 0.4744(3) 0.0167(7) Uani 1 1 d . . . O2 O -0.1699(7) 0.1620(3) 0.4867(2) 0.0225(6) Uani 1 1 d . . . N1 N 0.3184(8) 0.7974(3) 0.2952(2) 0.0199(6) Uani 1 1 d . . . H1 H 0.2767 0.8094 0.3658 0.024 Uiso 1 1 calc R . . C3 C 0.4481(9) 0.7597(4) 0.0751(3) 0.0164(7) Uani 1 1 d . . . B1 B 0.5324(11) 0.7430(4) -0.0523(3) 0.0175(8) Uani 1 1 d . . . C4 C 0.5352(10) 0.8842(4) 0.1482(3) 0.0185(7) Uani 1 1 d . . . H6 H 0.6427 0.9578 0.1216 0.022 Uiso 1 1 calc R . . C5 C 0.4674(10) 0.9022(4) 0.2589(3) 0.0202(7) Uani 1 1 d . . . H7 H 0.5255 0.9875 0.3084 0.024 Uiso 1 1 calc R . . C6 C 0.2300(10) 0.6752(4) 0.2290(3) 0.0204(7) Uani 1 1 d . . . H3 H 0.1248 0.6036 0.2583 0.024 Uiso 1 1 calc R . . C7 C 0.2927(9) 0.6540(4) 0.1174(3) 0.0192(7) Uani 1 1 d . . . H4 H 0.2300 0.5677 0.0698 0.023 Uiso 1 1 calc R . . O3 O 0.7510(7) 0.8468(3) -0.0724(2) 0.0243(6) Uani 1 1 d . . . H3B H 0.7795 0.8313 -0.1409 0.036 Uiso 1 1 calc R . . O4 O 0.3881(8) 0.6267(3) -0.1271(2) 0.0254(6) Uani 1 1 d . . . H4B H 0.4599 0.6281 -0.1899 0.038 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 0.01724(10) 0.01359(11) 0.01177(10) 0.00252(7) 0.00409(7) 0.00185(7) O5 0.0280(13) 0.0166(13) 0.0118(11) 0.0015(10) 0.0069(10) -0.0010(11) C1 0.0181(16) 0.0198(19) 0.0157(17) 0.0043(15) 0.0057(13) 0.0028(14) O1 0.0336(14) 0.0215(15) 0.0149(12) 0.0001(11) 0.0090(11) -0.0076(12) O6 0.0233(12) 0.0151(13) 0.0144(12) 0.0043(10) 0.0057(10) 0.0015(10) C2 0.0185(16) 0.0182(19) 0.0147(16) 0.0048(14) 0.0046(13) 0.0048(14) O2 0.0304(14) 0.0185(14) 0.0175(12) 0.0034(11) 0.0091(11) -0.0026(11) N1 0.0223(15) 0.0266(18) 0.0128(14) 0.0066(13) 0.0070(12) 0.0043(13) C3 0.0135(15) 0.0191(19) 0.0167(16) 0.0041(14) 0.0017(13) 0.0033(14) B1 0.0198(19) 0.019(2) 0.0158(18) 0.0060(16) 0.0021(15) 0.0058(16) C4 0.0199(17) 0.0168(19) 0.0187(17) 0.0043(14) 0.0047(14) 0.0012(14) C5 0.0221(17) 0.0168(19) 0.0203(18) 0.0017(15) 0.0044(14) 0.0021(15) C6 0.0177(17) 0.021(2) 0.0228(18) 0.0077(15) 0.0039(14) -0.0001(15) C7 0.0190(17) 0.0196(19) 0.0191(17) 0.0048(15) 0.0039(14) 0.0019(15) O3 0.0330(14) 0.0225(15) 0.0156(12) 0.0034(11) 0.0087(11) -0.0035(12) O4 0.0386(15) 0.0196(15) 0.0175(13) 0.0032(11) 0.0110(11) 0.0003(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 Pt1 O6 2.019(2) 2_666 ? Pt1 O6 2.019(2) . ? Pt1 O5 2.021(2) 2_666 ? Pt1 O5 2.021(2) . ? O5 C1 1.293(4) . ? C1 O1 1.212(4) . ? C1 C2 1.550(5) . ? O6 C2 1.288(4) . ? C2 O2 1.221(4) . ? N1 C5 1.337(5) . ? N1 C6 1.338(5) . ? C3 C4 1.391(5) . ? C3 C7 1.395(5) . ? C3 B1 1.599(5) . ? B1 O3 1.338(5) . ? B1 O4 1.357(5) . ? C4 C5 1.382(5) . ? C6 C7 1.384(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 O6 Pt1 O6 180.000(1) 2_666 . ? O6 Pt1 O5 82.61(10) 2_666 2_666 ? O6 Pt1 O5 97.39(9) . 2_666 ? O6 Pt1 O5 97.39(9) 2_666 . ? O6 Pt1 O5 82.61(10) . . ? O5 Pt1 O5 180.000(1) 2_666 . ? C1 O5 Pt1 112.7(2) . . ? O1 C1 O5 124.8(3) . . ? O1 C1 C2 119.5(3) . . ? O5 C1 C2 115.6(3) . . ? C2 O6 Pt1 112.6(2) . . ? O2 C2 O6 124.2(3) . . ? O2 C2 C1 120.3(3) . . ? O6 C2 C1 115.5(3) . . ? C5 N1 C6 123.0(3) . . ? C4 C3 C7 117.9(3) . . ? C4 C3 B1 119.3(3) . . ? C7 C3 B1 122.9(3) . . ? O3 B1 O4 126.9(3) . . ? O3 B1 C3 115.0(3) . . ? O4 B1 C3 118.1(3) . . ? C5 C4 C3 120.8(3) . . ? N1 C5 C4 118.9(3) . . ? N1 C6 C7 119.5(3) . . ? C6 C7 C3 119.9(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.022 _refine_diff_density_min -1.488 _refine_diff_density_rms 0.142 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 614737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 B2 Cu N2 O8 S4' _chemical_formula_weight 551.67 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.8956(8) _cell_length_b 10.119(2) _cell_length_c 13.447(3) _cell_angle_alpha 100.74(3) _cell_angle_beta 94.97(3) _cell_angle_gamma 97.65(3) _cell_volume 512.75(18) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 913 _cell_measurement_theta_min 2.327 _cell_measurement_theta_max 25.8755 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 279 _exptl_absorpt_coefficient_mu 1.519 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.5 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4449 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.1261 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2241 _reflns_number_gt 1419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0764P)^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_number_reflns 2241 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Cu1 Cu 0.5000 0.5000 0.5000 0.0296(4) Uani 1 2 d S . . S1 S 0.4093(4) 0.39743(14) 0.33057(11) 0.0303(4) Uani 1 1 d . . . S2 S 0.1265(4) 0.32960(15) 0.53791(10) 0.0329(4) Uani 1 1 d . . . O1 O 0.0623(13) 0.1576(4) 0.2500(3) 0.0433(13) Uani 1 1 d . . . O2 O -0.2100(13) 0.1120(4) 0.4160(3) 0.0425(13) Uani 1 1 d . . . O4 O 0.3374(16) 0.6250(5) -0.0962(3) 0.0546(15) Uani 1 1 d . . . H4 H 0.3655 0.6249 -0.1559 0.082 Uiso 1 1 calc R . . O3 O 0.7045(14) 0.8427(4) -0.0663(3) 0.0479(14) Uani 1 1 d . . . H3 H 0.7589 0.8139 -0.1230 0.072 Uiso 1 1 calc R . . B1 B 0.500(2) 0.7445(6) -0.0369(5) 0.0312(17) Uani 1 1 d . . . N1 N 0.5617(14) 0.9149(5) 0.2421(4) 0.0329(13) Uani 1 1 d . . . H1 H 0.6597 0.9915 0.2792 0.039 Uiso 1 1 calc R . . C1 C 0.1489(16) 0.2461(5) 0.3281(4) 0.0260(13) Uani 1 1 d . . . C2 C 0.0006(16) 0.2158(5) 0.4251(4) 0.0269(14) Uani 1 1 d . . . C3 C 0.4437(16) 0.7694(5) 0.0799(4) 0.0269(14) Uani 1 1 d . . . C4 C 0.2609(17) 0.6743(6) 0.1253(5) 0.0331(16) Uani 1 1 d . . . H4A H 0.1564 0.5911 0.0855 0.040 Uiso 1 1 calc R . . C5 C 0.2301(18) 0.7003(6) 0.2287(5) 0.0356(16) Uani 1 1 d . . . H5 H 0.1070 0.6359 0.2586 0.043 Uiso 1 1 calc R . . C6 C 0.3869(18) 0.8240(6) 0.2855(5) 0.0359(16) Uani 1 1 d . . . H6 H 0.3703 0.8441 0.3551 0.043 Uiso 1 1 calc R . . C7 C 0.5903(17) 0.8908(6) 0.1416(5) 0.0315(15) Uani 1 1 d . . . H7 H 0.7117 0.9577 0.1135 0.038 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 Cu1 0.0393(7) 0.0198(5) 0.0228(5) -0.0041(4) 0.0075(5) -0.0107(4) S1 0.0427(10) 0.0201(7) 0.0226(7) -0.0017(6) 0.0086(7) -0.0095(6) S2 0.0448(11) 0.0256(7) 0.0211(7) -0.0028(6) 0.0076(7) -0.0123(7) O1 0.068(3) 0.023(2) 0.029(2) -0.0080(19) 0.015(2) -0.017(2) O2 0.062(3) 0.024(2) 0.031(2) -0.0040(19) 0.009(2) -0.019(2) O4 0.092(4) 0.032(2) 0.030(2) -0.007(2) 0.016(3) -0.016(3) O3 0.076(4) 0.028(2) 0.033(2) -0.004(2) 0.020(3) -0.012(2) B1 0.043(5) 0.018(3) 0.029(3) -0.001(3) 0.004(3) 0.001(3) N1 0.046(3) 0.014(2) 0.032(3) -0.007(2) 0.004(2) 0.000(2) C1 0.032(3) 0.018(3) 0.026(3) 0.005(2) 0.003(3) -0.004(2) C2 0.034(4) 0.019(3) 0.025(3) 0.003(2) 0.006(3) -0.006(2) C3 0.034(4) 0.017(3) 0.028(3) 0.001(2) 0.005(3) 0.002(2) C4 0.045(4) 0.019(3) 0.031(3) 0.001(2) 0.007(3) -0.004(3) C5 0.052(4) 0.022(3) 0.033(3) 0.007(3) 0.017(3) -0.004(3) C6 0.048(4) 0.031(3) 0.027(3) 0.000(3) 0.008(3) 0.006(3) C7 0.042(4) 0.019(3) 0.034(3) 0.007(2) 0.007(3) -0.001(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 Cu1 S2 2.2666(17) . ? Cu1 S2 2.2666(17) 2_666 ? Cu1 S1 2.2966(15) 2_666 ? Cu1 S1 2.2966(15) . ? S1 C1 1.714(6) . ? S2 C2 1.714(5) . ? O1 C1 1.235(6) . ? O2 C2 1.223(7) . ? O4 B1 1.360(7) . ? O3 B1 1.331(9) . ? B1 C3 1.582(9) . ? N1 C6 1.324(8) . ? N1 C7 1.346(8) . ? C1 C2 1.537(9) . ? C3 C7 1.369(7) . ? C3 C4 1.384(9) . ? C4 C5 1.384(9) . ? C5 C6 1.372(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Cu1 S2 180.0 . 2_666 ? S2 Cu1 S1 89.50(6) . 2_666 ? S2 Cu1 S1 90.50(6) 2_666 2_666 ? S2 Cu1 S1 90.50(6) . . ? S2 Cu1 S1 89.50(6) 2_666 . ? S1 Cu1 S1 180.0 2_666 . ? C1 S1 Cu1 104.0(2) . . ? C2 S2 Cu1 105.6(2) . . ? O3 B1 O4 126.9(6) . . ? O3 B1 C3 116.3(5) . . ? O4 B1 C3 116.8(6) . . ? C6 N1 C7 121.8(5) . . ? O1 C1 C2 116.2(5) . . ? O1 C1 S1 123.3(5) . . ? C2 C1 S1 120.5(4) . . ? O2 C2 C1 117.1(5) . . ? O2 C2 S2 123.8(5) . . ? C1 C2 S2 119.0(4) . . ? C7 C3 C4 117.1(5) . . ? C7 C3 B1 118.8(6) . . ? C4 C3 B1 124.2(5) . . ? C5 C4 C3 121.5(5) . . ? C6 C5 C4 117.9(6) . . ? N1 C6 C5 120.6(6) . . ? N1 C7 C3 121.1(6) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.656 _refine_diff_density_min -1.420 _refine_diff_density_rms 0.164 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 614738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 B2 N2 Ni O8 S4' _chemical_formula_weight 546.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.9050(8) _cell_length_b 10.220(2) _cell_length_c 13.302(3) _cell_angle_alpha 101.79(3) _cell_angle_beta 95.13(3) _cell_angle_gamma 98.09(3) _cell_volume 510.69(18) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2345 _cell_measurement_theta_min 2.304 _cell_measurement_theta_max 27.3525 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 278 _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.592 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5906 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2334 _reflns_number_gt 1938 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0510P)^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_number_reflns 2334 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Ni1 Ni 0.5000 0.5000 0.5000 0.02607(16) Uani 1 2 d S . . S1 S 0.41513(19) 0.39748(7) 0.33715(5) 0.03038(19) Uani 1 1 d . . . S2 S 0.16296(19) 0.33565(7) 0.54133(5) 0.03238(19) Uani 1 1 d . . . O1 O 0.0641(6) 0.15835(19) 0.24974(15) 0.0433(6) Uani 1 1 d . . . O2 O -0.1947(6) 0.11503(19) 0.42244(15) 0.0435(6) Uani 1 1 d . . . O4 O 0.3326(7) 0.6249(2) -0.09839(17) 0.0564(7) Uani 1 1 d . . . H4 H 0.3917 0.6189 -0.1566 0.085 Uiso 1 1 calc R . . O3 O 0.6979(7) 0.8433(2) -0.06537(16) 0.0488(6) Uani 1 1 d . . . H3 H 0.7634 0.8132 -0.1211 0.073 Uiso 1 1 calc R . . B1 B 0.4906(9) 0.7444(3) -0.0370(3) 0.0346(7) Uani 1 1 d . . . N1 N 0.5489(6) 0.9154(2) 0.24730(18) 0.0350(6) Uani 1 1 d . . . H1 H 0.6437 0.9925 0.2858 0.042 Uiso 1 1 calc R . . C1 C 0.1522(7) 0.2465(3) 0.3301(2) 0.0283(6) Uani 1 1 d . . . C2 C 0.0159(7) 0.2189(3) 0.4290(2) 0.0287(6) Uani 1 1 d . . . C3 C 0.4381(7) 0.7694(3) 0.0810(2) 0.0287(6) Uani 1 1 d . . . C4 C 0.2561(8) 0.6740(3) 0.1262(2) 0.0343(7) Uani 1 1 d . . . H4A H 0.1538 0.5902 0.0852 0.041 Uiso 1 1 calc R . . C5 C 0.2247(8) 0.7011(3) 0.2301(2) 0.0372(7) Uani 1 1 d . . . H5 H 0.1020 0.6364 0.2592 0.045 Uiso 1 1 calc R . . C6 C 0.3755(8) 0.8241(3) 0.2904(2) 0.0368(7) Uani 1 1 d . . . H6 H 0.3572 0.8438 0.3610 0.044 Uiso 1 1 calc R . . C7 C 0.5814(8) 0.8917(3) 0.1460(2) 0.0326(6) Uani 1 1 d . . . H7 H 0.7028 0.9590 0.1190 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0291(3) 0.0272(3) 0.0172(3) 0.00022(18) 0.0046(2) -0.00566(19) S1 0.0368(4) 0.0298(3) 0.0195(3) 0.0010(3) 0.0074(3) -0.0076(3) S2 0.0391(4) 0.0339(4) 0.0188(3) 0.0022(3) 0.0067(3) -0.0091(3) O1 0.0612(14) 0.0350(11) 0.0228(10) -0.0040(8) 0.0101(10) -0.0167(10) O2 0.0569(14) 0.0346(11) 0.0300(11) 0.0021(9) 0.0087(10) -0.0176(10) O4 0.0849(19) 0.0442(12) 0.0281(12) -0.0035(10) 0.0178(12) -0.0197(12) O3 0.0687(16) 0.0415(12) 0.0295(11) 0.0022(9) 0.0184(11) -0.0130(11) B1 0.0417(19) 0.0339(16) 0.0268(16) 0.0046(13) 0.0076(15) 0.0027(14) N1 0.0436(15) 0.0274(11) 0.0277(12) -0.0026(10) 0.0012(11) -0.0010(10) C1 0.0302(14) 0.0263(12) 0.0255(14) 0.0030(11) 0.0043(11) -0.0018(11) C2 0.0326(15) 0.0283(13) 0.0224(13) 0.0027(10) 0.0044(11) -0.0010(11) C3 0.0324(15) 0.0280(13) 0.0242(13) 0.0049(11) 0.0044(12) 0.0010(11) C4 0.0395(17) 0.0284(13) 0.0304(15) 0.0024(11) 0.0050(13) -0.0051(12) C5 0.0458(18) 0.0349(14) 0.0306(15) 0.0104(12) 0.0109(14) -0.0029(13) C6 0.0466(18) 0.0409(16) 0.0235(14) 0.0069(12) 0.0074(13) 0.0074(14) C7 0.0390(16) 0.0296(13) 0.0274(14) 0.0060(11) 0.0054(13) -0.0011(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 Ni1 S2 2.1774(9) 2_666 ? Ni1 S2 2.1774(9) . ? Ni1 S1 2.1786(9) . ? Ni1 S1 2.1786(10) 2_666 ? S1 C1 1.710(3) . ? S2 C2 1.706(3) . ? O1 C1 1.235(3) . ? O2 C2 1.230(3) . ? O4 B1 1.352(4) . ? O3 B1 1.341(4) . ? B1 C3 1.575(4) . ? N1 C6 1.331(4) . ? N1 C7 1.341(4) . ? C1 C2 1.526(4) . ? C3 C7 1.377(4) . ? C3 C4 1.393(4) . ? C4 C5 1.374(4) . ? C5 C6 1.366(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni1 S2 180.0 2_666 . ? S2 Ni1 S1 88.41(4) 2_666 . ? S2 Ni1 S1 91.59(4) . . ? S2 Ni1 S1 91.59(4) 2_666 2_666 ? S2 Ni1 S1 88.41(4) . 2_666 ? S1 Ni1 S1 180.0 . 2_666 ? C1 S1 Ni1 106.08(10) . . ? C2 S2 Ni1 106.51(10) . . ? O3 B1 O4 126.8(3) . . ? O3 B1 C3 116.0(3) . . ? O4 B1 C3 117.2(3) . . ? C6 N1 C7 122.4(2) . . ? O1 C1 C2 117.8(2) . . ? O1 C1 S1 124.1(2) . . ? C2 C1 S1 118.10(19) . . ? O2 C2 C1 118.1(2) . . ? O2 C2 S2 124.4(2) . . ? C1 C2 S2 117.55(18) . . ? C7 C3 C4 116.4(2) . . ? C7 C3 B1 119.5(2) . . ? C4 C3 B1 124.1(3) . . ? C5 C4 C3 121.3(3) . . ? C6 C5 C4 119.4(3) . . ? N1 C6 C5 119.4(3) . . ? N1 C7 C3 121.1(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.490 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.131 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 614739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 B2 N2 O8 Pd S4' _chemical_formula_weight 594.53 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.9415(8) _cell_length_b 10.164(2) _cell_length_c 13.431(3) _cell_angle_alpha 100.46(3) _cell_angle_beta 94.77(3) _cell_angle_gamma 98.41(3) _cell_volume 520.07(18) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3140 _cell_measurement_theta_min 2.327 _cell_measurement_theta_max 27.439 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.773 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5941 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2365 _reflns_number_gt 2145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0448P)^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_number_reflns 2365 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 Pd1 Pd 0.5000 0.5000 0.5000 0.02712(13) Uani 1 2 d S . . S1 S 0.4089(2) 0.39620(8) 0.33117(6) 0.0343(2) Uani 1 1 d . . . S2 S 0.1642(2) 0.31473(8) 0.53815(6) 0.0351(2) Uani 1 1 d . . . O1 O 0.0591(7) 0.1591(2) 0.24783(17) 0.0470(7) Uani 1 1 d . . . O2 O -0.2004(7) 0.1056(2) 0.41464(18) 0.0481(7) Uani 1 1 d . . . O4 O 0.3341(9) 0.6245(3) -0.09522(19) 0.0590(8) Uani 1 1 d . . . H4 H 0.3967 0.6173 -0.1524 0.088 Uiso 1 1 calc R . . O3 O 0.7027(8) 0.8422(3) -0.06550(19) 0.0503(7) Uani 1 1 d . . . H3 H 0.7228 0.8197 -0.1262 0.075 Uiso 1 1 calc R . . B1 B 0.4950(11) 0.7448(4) -0.0363(3) 0.0374(9) Uani 1 1 d . . . N1 N 0.5458(8) 0.9149(3) 0.2420(2) 0.0358(6) Uani 1 1 d . . . H1 H 0.6423 0.9915 0.2790 0.043 Uiso 1 1 calc R . . C1 C 0.1480(8) 0.2439(3) 0.3262(2) 0.0310(7) Uani 1 1 d . . . C2 C 0.0132(9) 0.2090(3) 0.4240(2) 0.0325(7) Uani 1 1 d . . . C3 C 0.4349(9) 0.7686(3) 0.0801(2) 0.0301(7) Uani 1 1 d . . . C4 C 0.2498(9) 0.6746(3) 0.1260(2) 0.0368(8) Uani 1 1 d . . . H4A H 0.1468 0.5910 0.0867 0.044 Uiso 1 1 calc R . . C5 C 0.2142(10) 0.7017(3) 0.2287(3) 0.0394(8) Uani 1 1 d . . . H5 H 0.0890 0.6374 0.2586 0.047 Uiso 1 1 calc R . . C6 C 0.3661(9) 0.8245(3) 0.2854(2) 0.0377(8) Uani 1 1 d . . . H6 H 0.3438 0.8449 0.3547 0.045 Uiso 1 1 calc R . . C7 C 0.5819(9) 0.8908(3) 0.1422(2) 0.0340(7) Uani 1 1 d . . . H7 H 0.7076 0.9572 0.1144 0.041 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 Pd1 0.0296(2) 0.02794(19) 0.01992(17) -0.00039(12) 0.00428(13) -0.00234(13) S1 0.0431(5) 0.0322(4) 0.0223(4) 0.0003(3) 0.0076(3) -0.0076(4) S2 0.0421(5) 0.0365(4) 0.0219(4) 0.0023(3) 0.0066(3) -0.0068(4) O1 0.0650(17) 0.0406(13) 0.0241(11) -0.0051(10) 0.0100(11) -0.0168(12) O2 0.0639(17) 0.0390(13) 0.0315(12) 0.0003(10) 0.0114(12) -0.0195(12) O4 0.087(2) 0.0460(15) 0.0310(13) -0.0065(11) 0.0175(14) -0.0209(14) O3 0.0709(18) 0.0424(13) 0.0305(12) 0.0011(11) 0.0168(13) -0.0128(13) B1 0.046(2) 0.0351(19) 0.0293(18) 0.0038(15) 0.0083(17) 0.0031(17) N1 0.0435(17) 0.0297(14) 0.0293(14) -0.0022(11) 0.0023(12) 0.0010(12) C1 0.0330(17) 0.0310(15) 0.0262(15) 0.0026(12) 0.0056(13) -0.0012(13) C2 0.0377(18) 0.0324(16) 0.0263(15) 0.0043(13) 0.0067(13) 0.0019(14) C3 0.0328(17) 0.0305(15) 0.0254(14) 0.0036(12) 0.0041(13) 0.0018(13) C4 0.043(2) 0.0303(16) 0.0321(17) 0.0006(13) 0.0043(15) -0.0039(14) C5 0.048(2) 0.0370(17) 0.0335(17) 0.0101(14) 0.0110(15) -0.0007(15) C6 0.045(2) 0.0457(19) 0.0224(15) 0.0060(14) 0.0067(14) 0.0081(16) C7 0.0402(19) 0.0296(16) 0.0310(16) 0.0073(13) 0.0063(14) -0.0010(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.2953(10) . ? Pd1 S1 2.2953(10) 2_666 ? Pd1 S2 2.3009(11) 2_666 ? Pd1 S2 2.3009(11) . ? S1 C1 1.716(3) . ? S2 C2 1.709(3) . ? O1 C1 1.222(4) . ? O2 C2 1.227(4) . ? O4 B1 1.364(4) . ? O3 B1 1.327(5) . ? B1 C3 1.582(5) . ? N1 C6 1.326(4) . ? N1 C7 1.342(4) . ? C1 C2 1.538(4) . ? C3 C7 1.381(4) . ? C3 C4 1.382(5) . ? C4 C5 1.380(4) . ? C5 C6 1.363(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 S1 Pd1 S1 180.000(1) . 2_666 ? S1 Pd1 S2 90.92(4) . 2_666 ? S1 Pd1 S2 89.08(4) 2_666 2_666 ? S1 Pd1 S2 89.08(4) . . ? S1 Pd1 S2 90.92(4) 2_666 . ? S2 Pd1 S2 180.0 2_666 . ? C1 S1 Pd1 105.74(11) . . ? C2 S2 Pd1 106.02(12) . . ? O3 B1 O4 127.1(3) . . ? O3 B1 C3 116.6(3) . . ? O4 B1 C3 116.2(3) . . ? C6 N1 C7 122.1(3) . . ? O1 C1 C2 116.8(3) . . ? O1 C1 S1 123.5(3) . . ? C2 C1 S1 119.7(2) . . ? O2 C2 C1 117.1(3) . . ? O2 C2 S2 123.9(2) . . ? C1 C2 S2 119.1(2) . . ? C7 C3 C4 116.7(3) . . ? C7 C3 B1 118.5(3) . . ? C4 C3 B1 124.9(3) . . ? C5 C4 C3 121.6(3) . . ? C6 C5 C4 118.7(3) . . ? N1 C6 C5 120.1(3) . . ? N1 C7 C3 120.9(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.634 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.166 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 614740' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 B2 N2 O12 Pt' _chemical_formula_weight 618.98 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' O O 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.6590(7) _cell_length_b 10.172(2) _cell_length_c 12.576(3) _cell_angle_alpha 103.24(3) _cell_angle_beta 96.89(3) _cell_angle_gamma 98.10(3) _cell_volume 445.41(15) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5105 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 7.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.204 _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5105 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2042 _reflns_number_gt 2042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0189P)^2^+0.1445P] 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 2042 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0151 _refine_ls_R_factor_gt 0.0151 _refine_ls_wR_factor_ref 0.0375 _refine_ls_wR_factor_gt 0.0375 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.5000 0.5000 0.5000 0.01066(5) Uani 1 2 d S . . O5 O 0.4074(5) 0.37314(18) 0.34664(15) 0.0146(3) Uani 1 1 d . . . O6 O 0.2033(5) 0.33847(17) 0.53689(15) 0.0132(3) Uani 1 1 d . . . O1 O 0.0801(6) 0.16636(19) 0.25774(15) 0.0183(4) Uani 1 1 d . . . O2 O -0.1666(5) 0.13943(18) 0.44882(15) 0.0165(4) Uani 1 1 d . . . O4 O 0.3387(6) 0.61967(19) -0.11346(16) 0.0183(4) Uani 1 1 d . . . H4 H 0.3909 0.6207 -0.1749 0.027 Uiso 1 1 calc R . . O3 O 0.7067(6) 0.84808(19) -0.06331(15) 0.0177(4) Uani 1 1 d . . . H3 H 0.7257 0.8292 -0.1292 0.026 Uiso 1 1 calc R . . B1 B 0.4947(8) 0.7419(3) -0.0403(2) 0.0134(5) Uani 1 1 d . . . N1 N 0.5582(6) 0.9172(2) 0.26367(18) 0.0144(4) Uani 1 1 d . . . H1 H 0.6498 0.9978 0.3049 0.017 Uiso 1 1 calc R . . C1 C 0.1867(7) 0.2602(3) 0.3415(2) 0.0130(5) Uani 1 1 d . . . C2 C 0.0591(7) 0.2421(3) 0.4508(2) 0.0128(5) Uani 1 1 d . . . C3 C 0.4379(7) 0.7633(3) 0.0850(2) 0.0124(5) Uani 1 1 d . . . C4 C 0.2725(7) 0.6628(3) 0.1325(2) 0.0146(5) Uani 1 1 d . . . H4A H 0.1758 0.5752 0.0882 0.018 Uiso 1 1 calc R . . C5 C 0.2507(7) 0.6918(3) 0.2445(2) 0.0154(5) Uani 1 1 d . . . H5 H 0.1374 0.6247 0.2751 0.018 Uiso 1 1 calc R . . C6 C 0.3993(7) 0.8219(3) 0.3106(2) 0.0155(5) Uani 1 1 d . . . H6 H 0.3894 0.8429 0.3860 0.019 Uiso 1 1 calc R . . C7 C 0.5797(7) 0.8919(3) 0.1554(2) 0.0138(5) Uani 1 1 d . . . H7 H 0.6913 0.9614 0.1269 0.017 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 0.01303(7) 0.01083(7) 0.00766(7) 0.00164(5) 0.00158(5) 0.00171(4) O5 0.0184(9) 0.0125(8) 0.0113(8) 0.0015(6) 0.0032(7) -0.0007(7) O6 0.0164(8) 0.0126(8) 0.0100(8) 0.0021(6) 0.0025(7) 0.0008(6) O1 0.0250(10) 0.0154(9) 0.0109(9) 0.0002(7) 0.0054(8) -0.0051(7) O2 0.0220(9) 0.0145(9) 0.0121(9) 0.0029(7) 0.0056(7) -0.0012(7) O4 0.0250(10) 0.0166(9) 0.0111(9) 0.0009(7) 0.0048(8) -0.0015(7) O3 0.0248(10) 0.0169(9) 0.0091(8) 0.0015(7) 0.0055(8) -0.0029(7) B1 0.0141(13) 0.0158(13) 0.0107(12) 0.0039(10) 0.0013(10) 0.0030(10) N1 0.0168(10) 0.0146(10) 0.0103(10) 0.0003(8) 0.0016(8) 0.0026(8) C1 0.0150(11) 0.0155(11) 0.0090(11) 0.0039(9) 0.0034(9) 0.0020(9) C2 0.0153(11) 0.0137(11) 0.0106(11) 0.0035(9) 0.0032(9) 0.0046(9) C3 0.0106(11) 0.0153(11) 0.0119(11) 0.0046(9) 0.0017(9) 0.0027(9) C4 0.0138(11) 0.0154(12) 0.0141(12) 0.0047(9) 0.0002(9) 0.0008(9) C5 0.0149(12) 0.0179(12) 0.0145(12) 0.0069(10) 0.0031(10) 0.0011(9) C6 0.0170(12) 0.0211(13) 0.0093(11) 0.0044(9) 0.0038(9) 0.0040(10) C7 0.0155(12) 0.0150(11) 0.0123(12) 0.0053(9) 0.0037(9) 0.0028(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 Pt1 O6 2.0151(18) . ? Pt1 O6 2.0151(18) 2_666 ? Pt1 O5 2.0199(19) . ? Pt1 O5 2.0199(19) 2_666 ? O5 C1 1.292(3) . ? O6 C2 1.282(3) . ? O1 C1 1.228(3) . ? O2 C2 1.230(3) . ? O4 B1 1.366(3) . ? O3 B1 1.347(3) . ? B1 C3 1.584(4) . ? N1 C7 1.341(3) . ? N1 C6 1.346(3) . ? C1 C2 1.545(3) . ? C3 C7 1.390(4) . ? C3 C4 1.400(3) . ? C4 C5 1.387(4) . ? C5 C6 1.386(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Pt1 O6 180.00(6) . 2_666 ? O6 Pt1 O5 83.00(8) . . ? O6 Pt1 O5 97.00(8) 2_666 . ? O6 Pt1 O5 97.00(8) . 2_666 ? O6 Pt1 O5 83.00(8) 2_666 2_666 ? O5 Pt1 O5 180.000(1) . 2_666 ? C1 O5 Pt1 111.66(16) . . ? C2 O6 Pt1 112.62(16) . . ? O3 B1 O4 126.2(2) . . ? O3 B1 C3 115.0(2) . . ? O4 B1 C3 118.7(2) . . ? C7 N1 C6 122.8(2) . . ? O1 C1 O5 125.1(2) . . ? O1 C1 C2 118.4(2) . . ? O5 C1 C2 116.5(2) . . ? O2 C2 O6 125.7(2) . . ? O2 C2 C1 118.8(2) . . ? O6 C2 C1 115.5(2) . . ? C7 C3 C4 116.9(2) . . ? C7 C3 B1 117.1(2) . . ? C4 C3 B1 126.0(2) . . ? C5 C4 C3 121.0(2) . . ? C6 C5 C4 119.4(2) . . ? N1 C6 C5 118.9(2) . . ? N1 C7 C3 121.1(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.433 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.113