# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Neil Robertson' 'J Durrant' 'James R. Jennings' 'Lucy P. Moorcraft' 'Ana Morandeira' 'Simon Parsons' 'L M Peter' 'Andrew R Turner' 'Lesley Yellowlees' _publ_contact_author_name 'Neil Robertson' _publ_contact_author_email NEIL.ROBERTSON@ED.AC.UK _publ_section_title ; Synthesis and Properties of [Pt(4-CO2CH3-py)2(mnt)]; comparison of pyridyl and bipyridyl-based dyes for Solar Cells ; # Attachment 'Robertson_-_Ptpy2Cl2.cif.cif' data_nr0508 _database_code_depnum_ccdc_archive 'CCDC 694836' _audit_creation_method SHELXL-97 _audit_creation_date 05-08-02 _chemical_compound_source 'Lucy Moorcraft reaction XD1' _exptl_crystal_recrystallization_method ; >From a mixtire of CH2Cl2 and heptane. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[PtCl2(C7H7NO2)2]' _chemical_formula_sum 'C14 H14 Cl2 N2 O4 Pt' _chemical_formula_weight 540.26 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.0562(3) _cell_length_b 8.2030(2) _cell_length_c 15.3120(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.4710(10) _cell_angle_gamma 90.00 _cell_volume 1625.99(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6769 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30 _exptl_crystal_description tablet _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 8.978 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.137 _exptl_absorpt_correction_T_max 0.280 _exptl_absorpt_process_details 'Sadabs v 2.10' _exptl_special_details ; Data collection strategy optimised with COSMO. Oxford Cryosystems LT device. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'Omega and Phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9237 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 29.68 _reflns_number_total 2175 _reflns_number_gt 2084 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Dirdif _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'XCIF, PLATON' _refine_special_details ; The molecule resides on a .2. axis. The H-atoms attached to C10 were located in a difference synthesis; the CH distances and HCH angles were fixed at ideal values, but the methyl-torion was refined. Checkcif output: 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? These have ideal values; see above. 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 133 The data collection strategy used aimed to achieve a complete data set to 2\q = 54 deg. Some higher angle data were collected in the process and these have been included in the refinement. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 851 851 0 23.01 0.550 1.000 1131 1131 0 25.24 0.600 1.000 1476 1476 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.999 1861 1860 1 29.68 0.697 0.942 2308 2175 133 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.38 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.14 There is a relatively large difference peak (1.33 e/Ang^3) next to Pt1, but this is to be expected in a caompound like this, where absorption effects are significant. ; _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^)+(0.0213P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson in Cc' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom/difmap _refine_ls_hydrogen_treatment 'riding/rotating group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2175 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0431 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 -0.115143(13) 0.2500 0.01871(5) Uani 1 2 d S . . Cl1 Cl 0.07770(5) -0.30915(8) 0.17260(4) 0.02814(13) Uani 1 1 d . . . N1 N 0.06498(14) 0.0604(3) 0.18304(13) 0.0190(4) Uani 1 1 d . . . C2 C 0.15240(19) 0.1383(3) 0.21812(18) 0.0237(5) Uani 1 1 d . . . H2 H 0.1838 0.1092 0.2755 0.028 Uiso 1 1 calc R . . C3 C 0.19672(17) 0.2584(3) 0.17268(16) 0.0243(5) Uani 1 1 d . . . H3 H 0.2586 0.3100 0.1981 0.029 Uiso 1 1 calc R . . C4 C 0.15038(17) 0.3035(3) 0.08950(16) 0.0203(4) Uani 1 1 d . . . C5 C 0.05988(17) 0.2259(3) 0.05396(16) 0.0246(5) Uani 1 1 d . . . H5 H 0.0264 0.2551 -0.0027 0.030 Uiso 1 1 calc R . . C6 C 0.01961(19) 0.1058(3) 0.10239(18) 0.0235(5) Uani 1 1 d . . . H6 H -0.0424 0.0530 0.0782 0.028 Uiso 1 1 calc R . . C7 C 0.19879(18) 0.4347(3) 0.04031(16) 0.0223(5) Uani 1 1 d . . . O8 O 0.27758(13) 0.5038(2) 0.06910(13) 0.0302(4) Uani 1 1 d . . . O9 O 0.14562(14) 0.4608(2) -0.03768(12) 0.0305(4) Uani 1 1 d . . . C10 C 0.1844(3) 0.5850(3) -0.0911(2) 0.0355(6) Uani 1 1 d . . . H10A H 0.1739 0.6924 -0.0658 0.053 Uiso 1 1 calc R . . H10B H 0.1475 0.5796 -0.1510 0.053 Uiso 1 1 calc R . . H10C H 0.2584 0.5674 -0.0930 0.053 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 0.01888(7) 0.01910(8) 0.01829(7) 0.000 0.00296(5) 0.000 Cl1 0.0294(3) 0.0269(3) 0.0276(3) -0.0070(2) 0.0019(2) 0.0050(2) N1 0.0172(8) 0.0202(10) 0.0201(10) -0.0027(8) 0.0036(7) -0.0012(8) C2 0.0217(11) 0.0253(12) 0.0229(12) -0.0005(9) -0.0015(9) -0.0030(9) C3 0.0210(10) 0.0258(13) 0.0252(12) -0.0022(10) -0.0004(9) -0.0036(9) C4 0.0218(10) 0.0191(12) 0.0208(11) -0.0020(9) 0.0056(8) -0.0011(8) C5 0.0235(10) 0.0295(13) 0.0201(12) -0.0001(10) 0.0005(9) -0.0036(9) C6 0.0198(10) 0.0303(14) 0.0201(12) 0.0001(9) 0.0018(9) -0.0039(8) C7 0.0237(10) 0.0201(11) 0.0245(13) -0.0023(10) 0.0084(9) -0.0001(9) O8 0.0260(8) 0.0283(10) 0.0364(11) 0.0016(8) 0.0049(7) -0.0066(7) O9 0.0353(9) 0.0300(10) 0.0261(10) 0.0059(8) 0.0035(8) -0.0084(8) C10 0.0452(16) 0.0295(14) 0.0340(16) 0.0092(12) 0.0135(13) -0.0049(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 N1 2.018(2) 2 ? Pt1 N1 2.018(2) . ? Pt1 Cl1 2.2976(6) . ? Pt1 Cl1 2.2976(6) 2 ? N1 C6 1.351(3) . ? N1 C2 1.356(3) . ? C2 C3 1.376(4) . ? C3 C4 1.387(3) . ? C4 C5 1.389(3) . ? C4 C7 1.500(3) . ? C5 C6 1.378(3) . ? C7 O8 1.206(3) . ? C7 O9 1.318(3) . ? O9 C10 1.440(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 88.91(11) 2 . ? N1 Pt1 Cl1 178.20(6) 2 . ? N1 Pt1 Cl1 89.39(6) . . ? N1 Pt1 Cl1 89.39(6) 2 2 ? N1 Pt1 Cl1 178.20(5) . 2 ? Cl1 Pt1 Cl1 92.32(3) . 2 ? C6 N1 C2 118.6(2) . . ? C6 N1 Pt1 119.87(16) . . ? C2 N1 Pt1 121.50(17) . . ? N1 C2 C3 121.6(2) . . ? C2 C3 C4 119.6(2) . . ? C3 C4 C5 119.0(2) . . ? C3 C4 C7 119.4(2) . . ? C5 C4 C7 121.6(2) . . ? C6 C5 C4 118.8(2) . . ? N1 C6 C5 122.5(2) . . ? O8 C7 O9 125.3(2) . . ? O8 C7 C4 123.3(2) . . ? O9 C7 C4 111.4(2) . . ? C7 O9 C10 116.6(2) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.326 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.125