Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'John S. Field' 'Raymond J. Haines' 'Lesibana P. Ledwaba' 'Murray R. Low' 'McGuire Junior, Robert' 'David R.. McMillin' 'Orde Q. Munro' _publ_contact_author_name 'John S. Field' _publ_contact_author_address ; School of Chemical and Physical Sciences University of Natal Private Bag X01 Pietermaritzburg 3201 SOUTH AFRICA ; _publ_contact_author_email FIELDJ@UKZN.AC.ZA _publ_section_title ; Synthesis, electrochemistry and luminescence of [Pt{4'-(R)trpy}(CN)]+ (R = Ph, o-CH3-Ph, o-Cl-Ph or o-CF3-Ph; trpy = 2,2' :6',2''-terpyridine): Crystal structure of [Pt{4'-(Ph)trpy}(CN)]BF4*CH3CN ; # Attachment 'phcnBF4Soly.cif' data_phcnbf4soly _database_code_depnum_ccdc_archive 'CCDC 616745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common "[Pt{4'-(Ph)terpy}CN]BF4" _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 B F4 N5 Pt' _chemical_formula_sum 'C24 H18 B F4 N5 Pt' _chemical_formula_weight 658.33 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' N N 0.0061 0.0033 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 7.304(3) _cell_length_b 13.015(3) _cell_length_c 13.057(3) _cell_angle_alpha 72.148(19) _cell_angle_beta 76.32(3) _cell_angle_gamma 81.02(3) _cell_volume 1143.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 280(2) _cell_measurement_reflns_used 1500 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 6.193 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.2581 _exptl_absorpt_correction_T_max 0.4569 _exptl_absorpt_process_details 'Crysalis RED 170' _exptl_special_details ; ? ; _diffrn_ambient_temperature 280(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 'Xcalibur CCD' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11424 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.73 _diffrn_reflns_theta_max 31.81 _reflns_number_total 7010 _reflns_number_gt 5941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis CCD 170' _computing_cell_refinement 'Crysalis CCD 170' _computing_data_reduction 'Crysalis RED 170' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.1000P)^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 7010 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 Pt Pt 0.14186(3) 0.666668(19) 0.91792(2) 0.03421(10) Uani 1 1 d . . . N1 N 0.1437(8) 0.7814(5) 0.7721(5) 0.0375(12) Uani 1 1 d . . . N2 N -0.0156(7) 0.7823(4) 0.9692(4) 0.0287(9) Uani 1 1 d . . . N3 N 0.0930(8) 0.5933(4) 1.0818(5) 0.0338(11) Uani 1 1 d . . . N4 N 0.3950(14) 0.4748(7) 0.8465(8) 0.072(2) Uani 1 1 d . . . F1 F 0.2789(12) 1.1977(5) 0.5983(5) 0.089(2) Uani 1 1 d . . . F2 F 0.2441(18) 1.2143(7) 0.4296(7) 0.135(4) Uani 1 1 d . . . F3 F 0.372(2) 1.3357(10) 0.4538(11) 0.172(6) Uani 1 1 d . . . F4 F 0.0918(17) 1.3346(11) 0.5176(7) 0.167(6) Uani 1 1 d . . . B B 0.2338(16) 1.2647(8) 0.5020(7) 0.051(2) Uani 1 1 d . . . C1 C 0.2417(12) 0.7745(7) 0.6723(6) 0.0472(17) Uani 1 1 d . . . H1 H 0.3069 0.7088 0.6654 0.074(8) Uiso 1 1 calc R . . C2 C 0.2473(15) 0.8624(8) 0.5806(7) 0.057(2) Uani 1 1 d . . . H2 H 0.3141 0.8551 0.5128 0.074(8) Uiso 1 1 calc R . . C3 C 0.1544(14) 0.9612(8) 0.5888(7) 0.055(2) Uani 1 1 d . . . H3 H 0.1627 1.0218 0.5279 0.074(8) Uiso 1 1 calc R . . C4 C 0.0464(12) 0.9680(7) 0.6918(6) 0.0454(16) Uani 1 1 d . . . H4 H -0.0231 1.0325 0.6991 0.074(8) Uiso 1 1 calc R . . C5 C 0.0450(9) 0.8788(6) 0.7809(6) 0.0337(12) Uani 1 1 d . . . C6 C -0.0504(9) 0.8786(5) 0.8935(5) 0.0307(11) Uani 1 1 d . . . C7 C -0.1618(9) 0.9631(5) 0.9287(6) 0.0342(12) Uani 1 1 d . . . H7 H -0.1872 1.0288 0.8781 0.074(8) Uiso 1 1 calc R . . C8 C -0.2352(9) 0.9483(5) 1.0409(6) 0.0327(12) Uani 1 1 d . . . C9 C -0.1940(10) 0.8483(5) 1.1161(6) 0.0355(13) Uani 1 1 d . . . H9 H -0.2410 0.8372 1.1910 0.074(8) Uiso 1 1 calc R . . C10 C -0.0834(9) 0.7675(5) 1.0771(5) 0.0320(12) Uani 1 1 d . . . C11 C -0.0216(9) 0.6575(5) 1.1420(5) 0.0329(12) Uani 1 1 d . . . C12 C -0.0681(11) 0.6207(6) 1.2546(6) 0.0424(15) Uani 1 1 d . . . H12 H -0.1459 0.6647 1.2946 0.074(8) Uiso 1 1 calc R . . C13 C 0.0009(13) 0.5185(6) 1.3080(6) 0.0495(19) Uani 1 1 d . . . H13 H -0.0291 0.4928 1.3841 0.074(8) Uiso 1 1 calc R . . C14 C 0.1154(15) 0.4550(7) 1.2464(8) 0.056(2) Uani 1 1 d . . . H14 H 0.1638 0.3859 1.2810 0.074(8) Uiso 1 1 calc R . . C15 C 0.1578(12) 0.4938(6) 1.1340(6) 0.0419(15) Uani 1 1 d . . . H15 H 0.2333 0.4498 1.0932 0.074(8) Uiso 1 1 calc R . . C16 C -0.3558(9) 1.0376(5) 1.0820(6) 0.0354(13) Uani 1 1 d . . . C17 C -0.3917(10) 1.1380(5) 1.0087(7) 0.0406(15) Uani 1 1 d . . . H17 H -0.3420 1.1498 0.9340 0.074(8) Uiso 1 1 calc R . . C18 C -0.5048(12) 1.2225(6) 1.0485(8) 0.0503(19) Uani 1 1 d . . . H18 H -0.5274 1.2900 0.9998 0.074(8) Uiso 1 1 calc R . . C19 C -0.5803(11) 1.2047(7) 1.1585(8) 0.0504(19) Uani 1 1 d . . . H19 H -0.6543 1.2598 1.1846 0.074(8) Uiso 1 1 calc R . . C20 C -0.5458(12) 1.1047(8) 1.2298(8) 0.0523(19) Uani 1 1 d . . . H20 H -0.6009 1.0920 1.3040 0.074(8) Uiso 1 1 calc R . . C21 C -0.4315(10) 1.0230(6) 1.1937(7) 0.0431(16) Uani 1 1 d . . . H21 H -0.4043 0.9575 1.2442 0.074(8) Uiso 1 1 calc R . . C22 C 0.3111(10) 0.5430(6) 0.8677(6) 0.0367(13) Uani 1 1 d . . . NS N -0.288(2) 1.1983(10) 0.7301(10) 0.102(4) Uani 1 1 d . . . CS1 C -0.3298(18) 1.2799(9) 0.6781(9) 0.069(3) Uani 1 1 d . . . CS2 C -0.3880(18) 1.3850(9) 0.6152(11) 0.074(3) Uani 1 1 d . . . HS1 H -0.4647 1.3787 0.5674 0.074(8) Uiso 1 1 calc R . . HS2 H -0.2786 1.4214 0.5722 0.074(8) Uiso 1 1 calc R . . HS3 H -0.4602 1.4259 0.6636 0.074(8) 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 Pt 0.03304(14) 0.03343(15) 0.03544(15) -0.00799(10) -0.00862(9) -0.00163(9) N1 0.039(3) 0.042(3) 0.031(3) -0.007(2) -0.009(2) -0.005(2) N2 0.028(2) 0.030(2) 0.028(2) -0.0053(18) -0.0055(18) -0.0081(18) N3 0.034(3) 0.030(3) 0.035(3) -0.004(2) -0.010(2) -0.001(2) N4 0.080(6) 0.064(5) 0.060(5) -0.018(4) -0.005(4) 0.013(4) F1 0.149(7) 0.059(4) 0.053(3) -0.002(3) -0.045(4) 0.019(4) F2 0.266(12) 0.073(5) 0.079(5) -0.034(4) -0.073(7) 0.031(6) F3 0.216(14) 0.144(10) 0.139(10) 0.042(8) -0.066(10) -0.091(10) F4 0.176(10) 0.202(12) 0.064(5) -0.024(6) -0.021(6) 0.129(9) B 0.064(6) 0.048(5) 0.033(4) -0.009(3) -0.010(4) 0.012(4) C1 0.051(4) 0.051(4) 0.037(4) -0.012(3) -0.006(3) -0.002(3) C2 0.071(6) 0.061(5) 0.032(4) -0.005(3) -0.006(4) -0.008(4) C3 0.066(6) 0.056(5) 0.039(4) -0.004(3) -0.015(4) -0.007(4) C4 0.048(4) 0.042(4) 0.040(4) -0.003(3) -0.012(3) 0.000(3) C5 0.028(3) 0.040(3) 0.034(3) -0.009(2) -0.009(2) -0.006(2) C6 0.030(3) 0.030(3) 0.032(3) -0.003(2) -0.014(2) -0.004(2) C7 0.033(3) 0.032(3) 0.039(3) -0.005(2) -0.016(2) -0.003(2) C8 0.032(3) 0.027(3) 0.043(3) -0.009(2) -0.016(3) -0.002(2) C9 0.041(3) 0.030(3) 0.032(3) -0.004(2) -0.010(3) -0.001(2) C10 0.032(3) 0.033(3) 0.031(3) -0.005(2) -0.011(2) -0.004(2) C11 0.037(3) 0.029(3) 0.032(3) -0.006(2) -0.011(2) 0.000(2) C12 0.055(4) 0.033(3) 0.035(3) -0.007(3) -0.014(3) 0.009(3) C13 0.070(5) 0.040(4) 0.027(3) 0.001(3) -0.009(3) 0.007(3) C14 0.082(6) 0.032(3) 0.052(5) -0.008(3) -0.029(4) 0.013(4) C15 0.053(4) 0.032(3) 0.040(4) -0.011(3) -0.014(3) 0.007(3) C16 0.030(3) 0.027(3) 0.054(4) -0.010(3) -0.019(3) 0.001(2) C17 0.041(3) 0.029(3) 0.051(4) -0.006(3) -0.017(3) -0.001(3) C18 0.048(4) 0.029(3) 0.077(6) -0.014(3) -0.027(4) 0.007(3) C19 0.040(4) 0.048(4) 0.072(5) -0.035(4) -0.013(4) 0.011(3) C20 0.048(4) 0.061(5) 0.054(5) -0.029(4) -0.010(4) 0.002(4) C21 0.036(3) 0.038(4) 0.060(5) -0.020(3) -0.016(3) 0.007(3) C22 0.043(3) 0.037(3) 0.030(3) -0.006(2) -0.010(3) -0.005(3) NS 0.131(10) 0.072(7) 0.082(7) 0.007(6) -0.024(7) 0.000(7) CS1 0.084(8) 0.057(6) 0.056(6) -0.005(5) -0.009(5) -0.011(5) CS2 0.075(7) 0.058(6) 0.079(7) -0.014(5) -0.013(6) 0.002(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 Pt N2 1.936(5) . ? Pt N1 2.026(6) . ? Pt N3 2.028(6) . ? Pt C22 2.048(8) . ? N1 C1 1.353(10) . ? N1 C5 1.380(9) . ? N2 C10 1.342(8) . ? N2 C6 1.368(8) . ? N3 C15 1.336(9) . ? N3 C11 1.374(9) . ? N4 C22 1.068(11) . ? F1 B 1.372(10) . ? F2 B 1.289(12) . ? F3 B 1.377(15) . ? F4 B 1.290(12) . ? C1 C2 1.376(11) . ? C1 H1 0.9300 . ? C2 C3 1.380(14) . ? C2 H2 0.9300 . ? C3 C4 1.410(12) . ? C3 H3 0.9300 . ? C4 C5 1.369(10) . ? C4 H4 0.9300 . ? C5 C6 1.470(9) . ? C6 C7 1.391(9) . ? C7 C8 1.400(10) . ? C7 H7 0.9300 . ? C8 C9 1.407(9) . ? C8 C16 1.501(9) . ? C9 C10 1.374(10) . ? C9 H9 0.9300 . ? C10 C11 1.486(9) . ? C11 C12 1.375(9) . ? C12 C13 1.377(10) . ? C12 H12 0.9300 . ? C13 C14 1.380(12) . ? C13 H13 0.9300 . ? C14 C15 1.372(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.391(9) . ? C16 C21 1.398(12) . ? C17 C18 1.424(11) . ? C17 H17 0.9300 . ? C18 C19 1.372(13) . ? C18 H18 0.9300 . ? C19 C20 1.375(13) . ? C19 H19 0.9300 . ? C20 C21 1.376(11) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? NS CS1 1.113(15) . ? CS1 CS2 1.421(15) . ? CS2 HS1 0.9600 . ? CS2 HS2 0.9600 . ? CS2 HS3 0.9600 . ? 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 N2 Pt N1 80.6(2) . . ? N2 Pt N3 80.5(2) . . ? N1 Pt N3 161.0(3) . . ? N2 Pt C22 178.4(2) . . ? N1 Pt C22 100.7(3) . . ? N3 Pt C22 98.1(2) . . ? C1 N1 C5 118.7(6) . . ? C1 N1 Pt 127.1(5) . . ? C5 N1 Pt 114.0(5) . . ? C10 N2 C6 121.8(6) . . ? C10 N2 Pt 119.8(4) . . ? C6 N2 Pt 118.4(4) . . ? C15 N3 C11 119.2(6) . . ? C15 N3 Pt 127.8(5) . . ? C11 N3 Pt 113.0(4) . . ? F2 B F4 119.5(11) . . ? F2 B F1 112.9(8) . . ? F4 B F1 112.9(8) . . ? F2 B F3 103.2(11) . . ? F4 B F3 98.2(12) . . ? F1 B F3 107.9(10) . . ? N1 C1 C2 121.5(8) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 120.4(8) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 118.3(8) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.3(8) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 N1 121.6(7) . . ? C4 C5 C6 124.1(7) . . ? N1 C5 C6 114.2(6) . . ? N2 C6 C7 119.4(6) . . ? N2 C6 C5 112.7(6) . . ? C7 C6 C5 127.9(6) . . ? C6 C7 C8 119.4(6) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 119.3(6) . . ? C7 C8 C16 120.9(6) . . ? C9 C8 C16 119.7(6) . . ? C10 C9 C8 118.9(6) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C10 C9 121.2(6) . . ? N2 C10 C11 111.3(6) . . ? C9 C10 C11 127.5(6) . . ? N3 C11 C12 120.8(6) . . ? N3 C11 C10 115.3(6) . . ? C12 C11 C10 123.9(6) . . ? C11 C12 C13 119.7(7) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 118.8(7) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 120.0(7) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? N3 C15 C14 121.5(7) . . ? N3 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C17 C16 C21 118.5(7) . . ? C17 C16 C8 120.2(7) . . ? C21 C16 C8 121.3(6) . . ? C16 C17 C18 119.8(8) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 120.1(7) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.5(7) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C21 121.3(8) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 120.6(8) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? N4 C22 Pt 176.1(8) . . ? NS CS1 CS2 177.9(15) . . ? CS1 CS2 HS1 109.5 . . ? CS1 CS2 HS2 109.5 . . ? HS1 CS2 HS2 109.5 . . ? CS1 CS2 HS3 109.5 . . ? HS1 CS2 HS3 109.5 . . ? HS2 CS2 HS3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.846 _refine_diff_density_min -1.961 _refine_diff_density_rms 0.202