# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof A Orpen' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close BRISTOL BS8 1TS ; _publ_contact_author_email GUY.ORPEN@BRIS.AC.UK _publ_section_title ; Thermal solid state synthesis of coordination complexes from hydrogen bonded precursors. ; loop_ _publ_author_name 'A. Orpen' 'Christopher J. Adams' 'Paul C. Crawford' 'Thomas J. Podesta' 'Benjamin Salt' data_1[4-picolininium]2[PtCl4]motteret _database_code_depnum_ccdc_archive 'CCDC 263081' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Cl4 N2 Pt' _chemical_formula_weight 525.16 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.430(6) _cell_length_b 8.401(6) _cell_length_c 14.686(11) _cell_angle_alpha 102.459(11) _cell_angle_beta 91.078(11) _cell_angle_gamma 114.901(11) _cell_volume 805.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 9.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.608278 _exptl_absorpt_correction_T_max 0.901068 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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_% ? _diffrn_reflns_number 8403 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3653 _reflns_number_gt 3168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (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^)+(0.0307P)^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 3653 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Pt3 Pt 0.43848(2) 0.29034(2) 0.239793(11) 0.02061(6) Uani 1 1 d . . . Cl4 Cl 0.49646(16) 0.03659(14) 0.22971(7) 0.0280(2) Uani 1 1 d . . . Cl3 Cl 0.63496(17) 0.42258(15) 0.38384(8) 0.0309(2) Uani 1 1 d . . . Cl2 Cl 0.24296(18) 0.15502(15) 0.09594(8) 0.0332(2) Uani 1 1 d . . . Cl1 Cl 0.37940(17) 0.54200(15) 0.25224(8) 0.0313(2) Uani 1 1 d . . . N1 N 0.7271(6) 0.2117(5) -0.0135(3) 0.0339(9) Uani 1 1 d . . . H1 H 0.6925 0.1084 -0.0525 0.041 Uiso 1 1 calc R . . N2 N 0.3458(5) 0.0502(5) 0.4373(3) 0.0274(8) Uani 1 1 d . . . H2 H 0.4162 0.1065 0.3986 0.033 Uiso 1 1 calc R . . C11 C 0.8349(7) 0.5389(7) 0.1104(3) 0.0338(11) Uani 1 1 d . . . C21 C 0.1199(6) -0.1294(6) 0.5598(3) 0.0277(9) Uani 1 1 d . . . C14 C 0.6869(7) 0.3357(7) -0.0399(3) 0.0343(11) Uani 1 1 d . . . H14 H 0.6223 0.3103 -0.0998 0.041 Uiso 1 1 calc R . . C23 C 0.2422(7) -0.1307(7) 0.4107(3) 0.0320(10) Uani 1 1 d . . . H23 H 0.2482 -0.1931 0.3512 0.038 Uiso 1 1 calc R . . C22 C 0.1289(7) -0.2230(6) 0.4700(3) 0.0319(10) Uani 1 1 d . . . H22 H 0.0572 -0.3483 0.4511 0.038 Uiso 1 1 calc R . . C13 C 0.8183(7) 0.2414(7) 0.0705(4) 0.0393(12) Uani 1 1 d . . . H13 H 0.8461 0.1518 0.0861 0.047 Uiso 1 1 calc R . . C25 C 0.2318(7) 0.0570(6) 0.5849(3) 0.0292(10) Uani 1 1 d . . . H25 H 0.2320 0.1229 0.6445 0.035 Uiso 1 1 calc R . . C24 C 0.3423(7) 0.1445(6) 0.5220(3) 0.0309(10) Uani 1 1 d . . . H24 H 0.4147 0.2699 0.5386 0.037 Uiso 1 1 calc R . . C12 C 0.8724(7) 0.4031(8) 0.1349(4) 0.0420(13) Uani 1 1 d . . . H12 H 0.9338 0.4224 0.1947 0.050 Uiso 1 1 calc R . . C26 C -0.0027(8) -0.2284(8) 0.6275(4) 0.0452(13) Uani 1 1 d . . . H26C H -0.0446 -0.1498 0.6698 0.068 Uiso 1 1 calc R . . H26A H 0.0763 -0.2655 0.6627 0.068 Uiso 1 1 calc R . . H26B H -0.1183 -0.3332 0.5932 0.068 Uiso 1 1 calc R . . C15 C 0.7403(7) 0.5003(7) 0.0206(3) 0.0332(10) Uani 1 1 d . . . H15 H 0.7132 0.5875 0.0016 0.040 Uiso 1 1 calc R . . C16 C 0.8942(10) 0.7172(8) 0.1791(5) 0.0670(19) Uani 1 1 d . . . H16C H 0.8593 0.6978 0.2397 0.101 Uiso 1 1 calc R . . H16A H 0.8255 0.7800 0.1584 0.101 Uiso 1 1 calc R . . H16B H 1.0359 0.7885 0.1834 0.101 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 Pt3 0.02083(9) 0.01794(9) 0.02260(9) 0.00515(6) 0.00390(6) 0.00790(6) Cl4 0.0371(6) 0.0246(5) 0.0268(5) 0.0060(4) 0.0033(4) 0.0178(5) Cl3 0.0357(6) 0.0228(5) 0.0295(5) 0.0015(5) -0.0051(5) 0.0109(5) Cl2 0.0426(6) 0.0278(6) 0.0299(6) 0.0013(5) -0.0076(5) 0.0192(5) Cl1 0.0374(6) 0.0224(5) 0.0354(6) 0.0039(5) -0.0009(5) 0.0159(5) N1 0.034(2) 0.025(2) 0.037(2) 0.0012(18) 0.0108(18) 0.0102(18) N2 0.0267(19) 0.029(2) 0.029(2) 0.0091(17) 0.0042(16) 0.0134(17) C11 0.023(2) 0.035(3) 0.034(3) 0.005(2) 0.014(2) 0.005(2) C21 0.022(2) 0.034(3) 0.030(2) 0.009(2) 0.0045(18) 0.014(2) C14 0.036(3) 0.040(3) 0.026(2) 0.009(2) 0.003(2) 0.016(2) C23 0.034(2) 0.033(3) 0.027(2) -0.002(2) -0.0030(19) 0.018(2) C22 0.025(2) 0.023(2) 0.040(3) 0.002(2) -0.002(2) 0.0062(19) C13 0.036(3) 0.042(3) 0.057(3) 0.030(3) 0.020(3) 0.023(2) C25 0.030(2) 0.031(3) 0.024(2) -0.0028(19) -0.0016(18) 0.016(2) C24 0.026(2) 0.020(2) 0.041(3) 0.002(2) -0.002(2) 0.0069(19) C12 0.028(2) 0.067(4) 0.028(2) 0.020(3) 0.003(2) 0.014(3) C26 0.039(3) 0.060(4) 0.051(3) 0.028(3) 0.020(3) 0.027(3) C15 0.035(3) 0.032(3) 0.040(3) 0.015(2) 0.007(2) 0.018(2) C16 0.052(4) 0.049(4) 0.064(4) -0.015(3) 0.022(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 Pt3 Cl1 2.3052(18) . ? Pt3 Cl2 2.3073(18) . ? Pt3 Cl3 2.3118(18) . ? Pt3 Cl4 2.3219(18) . ? N1 C13 1.317(7) . ? N1 C14 1.325(6) . ? N2 C24 1.330(6) . ? N2 C23 1.342(6) . ? C11 C15 1.389(7) . ? C11 C12 1.396(7) . ? C11 C16 1.494(8) . ? C21 C25 1.386(6) . ? C21 C22 1.401(6) . ? C21 C26 1.504(6) . ? C14 C15 1.362(7) . ? C23 C22 1.356(6) . ? C13 C12 1.369(8) . ? C25 C24 1.371(6) . ? 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 Cl1 Pt3 Cl2 90.78(5) . . ? Cl1 Pt3 Cl3 89.96(5) . . ? Cl2 Pt3 Cl3 179.26(4) . . ? Cl1 Pt3 Cl4 179.06(4) . . ? Cl2 Pt3 Cl4 89.81(5) . . ? Cl3 Pt3 Cl4 89.45(5) . . ? C13 N1 C14 122.3(4) . . ? C24 N2 C23 121.7(4) . . ? C15 C11 C12 117.3(5) . . ? C15 C11 C16 122.1(5) . . ? C12 C11 C16 120.6(5) . . ? C25 C21 C22 117.6(4) . . ? C25 C21 C26 121.3(4) . . ? C22 C21 C26 121.1(4) . . ? N1 C14 C15 119.9(4) . . ? N2 C23 C22 120.5(4) . . ? C23 C22 C21 119.9(4) . . ? N1 C13 C12 120.5(4) . . ? C24 C25 C21 120.3(4) . . ? N2 C24 C25 120.0(4) . . ? C13 C12 C11 119.6(5) . . ? C14 C15 C11 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.983 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.169 data_2[4-picolininium]2[PdCl4]beaver _database_code_depnum_ccdc_archive 'CCDC 263082' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C6 H8 N), Cl4 Pd' _chemical_formula_sum 'C12 H16 Cl4 N2 Pd' _chemical_formula_weight 436.47 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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 10.592(3) _cell_length_b 11.311(3) _cell_length_c 7.4277(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.81(2) _cell_angle_gamma 90.00 _cell_volume 820.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 65 _cell_measurement_theta_min 5.512 _cell_measurement_theta_max 53.293 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.776549 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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_% ? _diffrn_reflns_number 3970 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.48 _reflns_number_total 986 _reflns_number_gt 847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (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^)+(0.0208P)^2^+0.6438P] 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 986 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 -0.5000 0.0000 -0.5000 0.02415(13) Uani 1 4 d S . . Cl1 Cl -0.57328(7) -0.14368(5) -0.73954(9) 0.03403(18) Uani 1 1 d . . . N1 N -0.7058(3) 0.0000 -0.1455(4) 0.0295(7) Uani 1 2 d S . . H1A H -0.6579 0.0000 -0.0187 0.035 Uiso 1 2 calc SR . . C1 C -0.8501(3) 0.0000 -0.5397(5) 0.0305(8) Uani 1 2 d S . . C2 C -0.8144(3) -0.1048(2) -0.4361(4) 0.0344(6) Uani 1 1 d . . . H2A H -0.8410 -0.1781 -0.5025 0.041 Uiso 1 1 calc R . . C4 C -0.7410(3) -0.1035(2) -0.2386(4) 0.0326(6) Uani 1 1 d . . . H4A H -0.7152 -0.1756 -0.1682 0.039 Uiso 1 1 calc R . . C6 C -0.9235(4) 0.0000 -0.7586(6) 0.0426(11) Uani 1 2 d S . . H6A H -0.859(5) 0.0000 -0.819(8) 0.081(17) Uiso 1 2 d S . . H6B H -0.983(3) 0.064(3) -0.803(5) 0.077(12) 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 0.0237(2) 0.0273(2) 0.0179(2) 0.000 0.00420(16) 0.000 Cl1 0.0425(4) 0.0304(4) 0.0214(4) -0.0017(2) 0.0039(3) -0.0016(3) N1 0.0231(15) 0.0415(18) 0.0203(15) 0.000 0.0044(13) 0.000 C1 0.0205(17) 0.046(2) 0.0236(18) 0.000 0.0070(15) 0.000 C2 0.0345(15) 0.0371(15) 0.0272(14) -0.0057(12) 0.0072(12) 0.0024(12) C4 0.0330(14) 0.0302(14) 0.0318(15) 0.0006(11) 0.0094(12) 0.0022(11) C6 0.032(2) 0.070(3) 0.021(2) 0.000 0.0065(19) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3106(7) . ? Pd1 Cl1 2.3106(7) 5_454 ? Pd1 Cl1 2.3106(7) 2_454 ? Pd1 Cl1 2.3106(7) 6 ? N1 C4 1.337(3) . ? N1 C4 1.337(3) 6 ? N1 H1A 0.8800 . ? C1 C2 1.384(3) 6 ? C1 C2 1.384(3) . ? C1 C6 1.506(5) . ? C2 C4 1.368(4) . ? C2 H2A 0.9500 . ? C4 H4A 0.9500 . ? C6 H6A 0.96(5) . ? C6 H6B 0.94(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 Cl1 Pd1 Cl1 180.0 . 5_454 ? Cl1 Pd1 Cl1 90.60(4) . 2_454 ? Cl1 Pd1 Cl1 89.40(4) 5_454 2_454 ? Cl1 Pd1 Cl1 89.40(4) . 6 ? Cl1 Pd1 Cl1 90.60(4) 5_454 6 ? Cl1 Pd1 Cl1 180.00(2) 2_454 6 ? C4 N1 C4 122.2(3) . 6 ? C4 N1 H1A 118.9 . . ? C4 N1 H1A 118.9 6 . ? C2 C1 C2 117.9(3) 6 . ? C2 C1 C6 121.05(17) 6 . ? C2 C1 C6 121.05(17) . . ? C4 C2 C1 120.4(3) . . ? C4 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? N1 C4 C2 119.5(3) . . ? N1 C4 H4A 120.2 . . ? C2 C4 H4A 120.2 . . ? C1 C6 H6A 110(3) . . ? C1 C6 H6B 112(2) . . ? H6A C6 H6B 110(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.373 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.078 data_3[4-picolininium][PtCl3(4-picoline)]pc135as _database_code_depnum_ccdc_archive 'CCDC 263083' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H15 Cl3 N2 Pt' _chemical_formula_weight 488.70 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5223(19) _cell_length_b 16.206(3) _cell_length_c 9.6271(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.73(3) _cell_angle_gamma 90.00 _cell_volume 1449.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4854 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 10.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747737 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16641 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3330 _reflns_number_gt 3062 _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^)+(0.0277P)^2^+3.7593P] 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 3330 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.192498(17) 0.050580(10) 0.192176(16) 0.01149(6) Uani 1 1 d . . . Cl1 Cl 0.22982(14) 0.18929(7) 0.23935(12) 0.0247(3) Uani 1 1 d . . . Cl2 Cl 0.08804(12) 0.03921(6) 0.38523(11) 0.0154(2) Uani 1 1 d . . . Cl3 Cl 0.15520(12) -0.08838(7) 0.14879(12) 0.0187(2) Uani 1 1 d . . . N1 N 0.1784(5) 0.2021(2) 0.5677(4) 0.0242(9) Uani 1 1 d . . . H1A H 0.1661 0.1737 0.4879 0.029 Uiso 1 1 calc R . . N2 N 0.2818(4) 0.0596(2) 0.0213(4) 0.0143(7) Uani 1 1 d . . . C1 C 0.2793(6) 0.2602(3) 0.5923(5) 0.0240(10) Uani 1 1 d . . . H1B H 0.3373 0.2699 0.5254 0.029 Uiso 1 1 calc R . . C2 C 0.2992(5) 0.3061(3) 0.7151(5) 0.0208(10) Uani 1 1 d . . . H2A H 0.3716 0.3475 0.7336 0.025 Uiso 1 1 calc R . . C3 C 0.2126(5) 0.2918(3) 0.8128(5) 0.0168(9) Uani 1 1 d . . . C4 C 0.1101(5) 0.2293(3) 0.7813(5) 0.0219(10) Uani 1 1 d . . . H4A H 0.0503 0.2176 0.8459 0.026 Uiso 1 1 calc R . . C5 C 0.0948(5) 0.1848(3) 0.6587(5) 0.0255(11) Uani 1 1 d . . . H5A H 0.0254 0.1418 0.6382 0.031 Uiso 1 1 calc R . . C6 C 0.2251(6) 0.3427(3) 0.9448(5) 0.0295(12) Uani 1 1 d . . . H6A H 0.1562 0.3227 0.9992 0.044 Uiso 1 1 calc R . . H6B H 0.2042 0.4006 0.9184 0.044 Uiso 1 1 calc R . . H6C H 0.3231 0.3382 1.0032 0.044 Uiso 1 1 calc R . . C7 C 0.4083(5) 0.0988(3) 0.0275(5) 0.0180(9) Uani 1 1 d . . . H7A H 0.4550 0.1238 0.1148 0.022 Uiso 1 1 calc R . . C8 C 0.4723(5) 0.1042(3) -0.0873(5) 0.0179(9) Uani 1 1 d . . . H8A H 0.5615 0.1322 -0.0784 0.022 Uiso 1 1 calc R . . C9 C 0.4054(5) 0.0682(3) -0.2168(5) 0.0172(9) Uani 1 1 d . . . C10 C 0.2758(5) 0.0282(3) -0.2224(5) 0.0164(9) Uani 1 1 d . . . H10A H 0.2272 0.0029 -0.3086 0.020 Uiso 1 1 calc R . . C11 C 0.2161(5) 0.0246(3) -0.1038(5) 0.0163(9) Uani 1 1 d . . . H11A H 0.1269 -0.0031 -0.1103 0.020 Uiso 1 1 calc R . . C12 C 0.4730(5) 0.0727(3) -0.3436(5) 0.0219(10) Uani 1 1 d . . . H12A H 0.4112 0.0445 -0.4246 0.033 Uiso 1 1 calc R . . H12B H 0.5676 0.0459 -0.3208 0.033 Uiso 1 1 calc R . . H12C H 0.4844 0.1306 -0.3683 0.033 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 0.01269(9) 0.01179(9) 0.01050(9) -0.00034(6) 0.00364(6) -0.00119(6) Cl1 0.0427(7) 0.0141(5) 0.0220(5) -0.0033(4) 0.0175(5) -0.0069(5) Cl2 0.0188(5) 0.0162(5) 0.0124(5) 0.0000(4) 0.0058(4) -0.0024(4) Cl3 0.0206(5) 0.0139(5) 0.0240(5) -0.0039(4) 0.0105(4) -0.0045(4) N1 0.034(2) 0.017(2) 0.0185(19) -0.0045(16) -0.0006(18) 0.0065(18) N2 0.0151(19) 0.0145(18) 0.0136(17) -0.0016(14) 0.0036(14) 0.0008(14) C1 0.033(3) 0.016(2) 0.026(2) 0.0025(19) 0.013(2) 0.004(2) C2 0.026(3) 0.010(2) 0.026(2) 0.0041(18) 0.006(2) -0.0010(18) C3 0.019(2) 0.016(2) 0.015(2) 0.0006(17) 0.0026(17) 0.0046(17) C4 0.021(2) 0.017(2) 0.030(3) 0.0006(19) 0.010(2) 0.0032(18) C5 0.020(3) 0.021(2) 0.035(3) -0.003(2) 0.003(2) -0.0008(19) C6 0.045(3) 0.027(3) 0.018(2) -0.001(2) 0.011(2) 0.002(2) C7 0.020(2) 0.018(2) 0.015(2) -0.0015(17) 0.0016(18) -0.0056(18) C8 0.014(2) 0.020(2) 0.020(2) 0.0001(18) 0.0059(17) -0.0025(17) C9 0.015(2) 0.019(2) 0.018(2) 0.0023(17) 0.0045(18) 0.0046(17) C10 0.017(2) 0.020(2) 0.011(2) -0.0026(16) 0.0021(17) 0.0011(17) C11 0.013(2) 0.020(2) 0.015(2) -0.0013(17) 0.0017(17) -0.0001(17) C12 0.019(2) 0.033(3) 0.015(2) -0.0004(19) 0.0068(18) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.016(4) . ? Pt1 Cl2 2.3005(12) . ? Pt1 Cl1 2.3052(12) . ? Pt1 Cl3 2.3036(11) . ? N1 C1 1.329(6) . ? N1 C5 1.338(6) . ? N1 H1A 0.8800 . ? N2 C7 1.352(6) . ? N2 C11 1.353(6) . ? C1 C2 1.374(7) . ? C1 H1B 0.9500 . ? C2 C3 1.401(7) . ? C2 H2A 0.9500 . ? C3 C4 1.392(7) . ? C3 C6 1.498(6) . ? C4 C5 1.363(7) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.378(6) . ? C7 H7A 0.9500 . ? C8 C9 1.397(6) . ? C8 H8A 0.9500 . ? C9 C10 1.385(6) . ? C9 C12 1.502(6) . ? C10 C11 1.384(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 Cl2 179.19(11) . . ? N2 Pt1 Cl1 90.90(10) . . ? Cl2 Pt1 Cl1 89.67(4) . . ? N2 Pt1 Cl3 89.93(10) . . ? Cl2 Pt1 Cl3 89.50(4) . . ? Cl1 Pt1 Cl3 179.09(4) . . ? C1 N1 C5 122.9(4) . . ? C1 N1 H1A 118.6 . . ? C5 N1 H1A 118.6 . . ? C7 N2 C11 118.0(4) . . ? C7 N2 Pt1 122.0(3) . . ? C11 N2 Pt1 120.0(3) . . ? N1 C1 C2 119.7(5) . . ? N1 C1 H1B 120.2 . . ? C2 C1 H1B 120.2 . . ? C1 C2 C3 119.8(5) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C2 C3 C4 117.5(4) . . ? C2 C3 C6 122.0(4) . . ? C4 C3 C6 120.5(4) . . ? C5 C4 C3 120.7(5) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? N1 C5 C4 119.4(5) . . ? N1 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 122.8(4) . . ? N2 C7 H7A 118.6 . . ? C8 C7 H7A 118.6 . . ? C7 C8 C9 119.7(4) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 117.2(4) . . ? C10 C9 C12 122.0(4) . . ? C8 C9 C12 120.8(4) . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? N2 C11 C10 121.5(4) . . ? N2 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 Cl2 Pt1 N2 C7 -178(100) . . . . ? Cl1 Pt1 N2 C7 47.5(3) . . . . ? Cl3 Pt1 N2 C7 -132.1(3) . . . . ? Cl2 Pt1 N2 C11 1(8) . . . . ? Cl1 Pt1 N2 C11 -133.6(3) . . . . ? Cl3 Pt1 N2 C11 46.8(3) . . . . ? C5 N1 C1 C2 -1.0(7) . . . . ? N1 C1 C2 C3 -0.4(7) . . . . ? C1 C2 C3 C4 1.2(7) . . . . ? C1 C2 C3 C6 -177.0(4) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C6 C3 C4 C5 177.6(5) . . . . ? C1 N1 C5 C4 1.5(7) . . . . ? C3 C4 C5 N1 -0.6(7) . . . . ? C11 N2 C7 C8 -0.3(7) . . . . ? Pt1 N2 C7 C8 178.6(3) . . . . ? N2 C7 C8 C9 0.2(7) . . . . ? C7 C8 C9 C10 -0.1(7) . . . . ? C7 C8 C9 C12 -179.8(4) . . . . ? C8 C9 C10 C11 0.1(7) . . . . ? C12 C9 C10 C11 179.7(4) . . . . ? C7 N2 C11 C10 0.2(6) . . . . ? Pt1 N2 C11 C10 -178.7(3) . . . . ? C9 C10 C11 N2 -0.2(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.074 _refine_diff_density_min -1.044 _refine_diff_density_rms 0.147 data_pc142bs _database_code_depnum_ccdc_archive 'CCDC 263084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Cl2 N2 Pd' _chemical_formula_sum 'C12 H14 Cl2 N2 Pd' _chemical_formula_weight 363.55 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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.461(2) _cell_length_b 3.9775(8) _cell_length_c 15.911(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.73(3) _cell_angle_gamma 90.00 _cell_volume 654.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2827 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.44 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 1.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details 'SADABS, Bruker AXS 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6909 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1503 _reflns_number_gt 1418 _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^)+(0.0207P)^2^+0.9017P] 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 1503 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _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 0.5000 0.0000 1.0000 0.01170(9) Uani 1 2 d S . . Cl1 Cl 0.70436(5) -0.23160(16) 1.01992(4) 0.01623(13) Uani 1 1 d . . . N1 N 0.50353(19) 0.0365(5) 0.87410(13) 0.0132(4) Uani 1 1 d . . . C1 C 0.4077(2) -0.0994(6) 0.81751(16) 0.0137(5) Uani 1 1 d . . . H1A H 0.3397 -0.2170 0.8381 0.016 Uiso 1 1 calc R . . C2 C 0.4059(2) -0.0726(6) 0.73122(16) 0.0145(5) Uani 1 1 d . . . H2A H 0.3372 -0.1709 0.6933 0.017 Uiso 1 1 calc R . . C3 C 0.5045(2) 0.0983(6) 0.69912(16) 0.0140(5) Uani 1 1 d . . . C4 C 0.6022(2) 0.2343(7) 0.75854(16) 0.0156(5) Uani 1 1 d . . . H4A H 0.6712 0.3536 0.7397 0.019 Uiso 1 1 calc R . . C5 C 0.5997(2) 0.1976(6) 0.84455(16) 0.0150(5) Uani 1 1 d . . . H5A H 0.6683 0.2893 0.8838 0.018 Uiso 1 1 calc R . . C6 C 0.5050(3) 0.1343(8) 0.60539(16) 0.0208(5) Uani 1 1 d . . . H6A H 0.5851 0.2453 0.5956 0.031 Uiso 1 1 calc R . . H6B H 0.4306 0.2697 0.5804 0.031 Uiso 1 1 calc R . . H6C H 0.4997 -0.0887 0.5789 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01072(13) 0.01525(14) 0.00876(13) -0.00098(10) 0.00029(8) 0.00082(10) Cl1 0.0133(3) 0.0209(3) 0.0140(3) -0.0013(2) 0.00046(19) 0.0039(2) N1 0.0124(9) 0.0148(10) 0.0117(10) -0.0009(8) 0.0000(7) 0.0017(8) C1 0.0125(11) 0.0149(12) 0.0136(12) 0.0001(9) 0.0018(9) -0.0004(9) C2 0.0131(11) 0.0167(13) 0.0127(11) -0.0027(9) -0.0011(9) 0.0009(9) C3 0.0159(12) 0.0131(11) 0.0135(12) 0.0010(9) 0.0032(9) 0.0045(9) C4 0.0131(11) 0.0153(12) 0.0189(12) 0.0012(10) 0.0041(9) 0.0007(10) C5 0.0127(11) 0.0149(12) 0.0167(12) -0.0028(10) 0.0000(9) -0.0003(9) C6 0.0236(13) 0.0267(14) 0.0124(12) 0.0003(11) 0.0037(10) -0.0011(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.014(2) 3_657 ? Pd1 N1 2.014(2) . ? Pd1 Cl1 2.3052(7) . ? Pd1 Cl1 2.3052(7) 3_657 ? N1 C5 1.337(3) . ? N1 C1 1.354(3) . ? C1 C2 1.374(3) . ? C1 H1A 0.9500 . ? C2 C3 1.395(3) . ? C2 H2A 0.9500 . ? C3 C4 1.392(3) . ? C3 C6 1.499(3) . ? C4 C5 1.380(3) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.000(1) 3_657 . ? N1 Pd1 Cl1 89.49(6) 3_657 . ? N1 Pd1 Cl1 90.51(6) . . ? N1 Pd1 Cl1 90.51(6) 3_657 3_657 ? N1 Pd1 Cl1 89.49(6) . 3_657 ? Cl1 Pd1 Cl1 180.0 . 3_657 ? C5 N1 C1 118.6(2) . . ? C5 N1 Pd1 120.84(16) . . ? C1 N1 Pd1 120.61(16) . . ? N1 C1 C2 122.0(2) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C1 C2 C3 120.3(2) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C4 C3 C2 116.6(2) . . ? C4 C3 C6 121.7(2) . . ? C2 C3 C6 121.7(2) . . ? C5 C4 C3 120.7(2) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? N1 C5 C4 121.8(2) . . ? N1 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 Cl1 Pd1 N1 C5 -54.67(18) . . . . ? Cl1 Pd1 N1 C5 125.33(18) 3_657 . . . ? Cl1 Pd1 N1 C1 125.89(18) . . . . ? Cl1 Pd1 N1 C1 -54.11(18) 3_657 . . . ? C5 N1 C1 C2 -0.9(4) . . . . ? Pd1 N1 C1 C2 178.58(18) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C1 C2 C3 C6 -179.6(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C6 C3 C4 C5 -179.9(2) . . . . ? C1 N1 C5 C4 1.4(4) . . . . ? Pd1 N1 C5 C4 -178.06(19) . . . . ? C3 C4 C5 N1 -1.1(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.698 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.096