# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_'[Pt(BDIQQ)]Cl' _database_code_depnum_ccdc_archive 'CCDC 905827' #TrackingRef '14672_web_deposit_cif_file_0_JustinWilson_1350215088.Good.cif' _audit_creation_date 2012-10-12 _audit_creation_method ; Olex2 1.2 (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_formula_moiety 'C21 H15 N4 Pt, Cl' _chemical_formula_sum 'C21 H15 Cl N4 Pt' _chemical_formula_weight 553.91 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_dispersion_source H 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' C 0.00347 0.00161 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' Cl 0.14873 0.16029 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' Pt -1.63788 8.57892 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' N 0.00653 0.00323 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z-1/2 5 x+1/2,y+1/2,z 6 -x+1/2,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z 8 x+1/2,-y+1/2,z-1/2 _cell_length_a 28.326(4) _cell_length_b 6.7809(9) _cell_length_c 25.610(4) _cell_angle_alpha 90 _cell_angle_beta 116.790(2) _cell_angle_gamma 90 _cell_volume 4391.2(11) _cell_formula_units_Z 8 _cell_measurement_reflns_used 760 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.99 _cell_measurement_theta_min 2.89 _exptl_absorpt_coefficient_mu 6.522 _exptl_absorpt_correction_T_max 0.431122 _exptl_absorpt_correction_T_min 0.267365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'twinabs 2008/4' _exptl_crystal_colour 'dark red' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.6756 _exptl_crystal_density_meas . _exptl_crystal_description needle _exptl_crystal_F_000 2101.3845 _exptl_crystal_preparation ? _exptl_crystal_recrystallization_method 'Vapor diffusion of diethyl ether into a DMF solution' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_unetI/netI 0.0360 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 68863 _diffrn_reflns_theta_full 28.345266 _diffrn_reflns_theta_max 28.35 _diffrn_reflns_theta_min 1.45 _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.997077 _diffrn_measured_fraction_theta_max 0.997077 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _reflns_Friedel_coverage 0.0 _reflns_limit_h_max 33 _reflns_limit_h_min -37 _reflns_limit_k_max 9 _reflns_limit_k_min 0 _reflns_limit_l_max 34 _reflns_limit_l_min 0 _reflns_number_gt 4542 _reflns_number_total 5457 _reflns_threshold_expression I>=2u(I) _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 3.967277 _refine_diff_density_min -5.383622 _refine_diff_density_rms 0.315313 _refine_ls_d_res_high 0.748478 _refine_ls_d_res_low 12.642986 _refine_ls_goodness_of_fit_ref 1.015564 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 30 _refine_ls_number_parameters 243 _refine_ls_number_reflns 5457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.052952 _refine_ls_R_factor_gt 0.043895 _refine_ls_restrained_S_all 1.015564 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+71.1140P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.127743 _refine_special_details ; The crystal is a non-merohedral twin. The data were integrated over two domains, found with the program CELL_NOW. An absorption correction was applied with Twinabs. Only data from the first (major) domain were used for refinement. ; _atom_sites_solution_primary iterative 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_refinement_flags_posn Pt1 Pt 0.725859(9) 0.28755(4) 0.736811(10) 0.01488(10) Uani 1.000000 . N2 N 0.7593(2) 0.2874(8) 0.8238(2) 0.0148(10) Uani 1.000000 . N1 N 0.8038(2) 0.2763(8) 0.7539(3) 0.0164(11) Uani 1.000000 . N3 N 0.6521(2) 0.2800(8) 0.7280(2) 0.0151(10) Uani 1.000000 . N4 N 0.6851(2) 0.3103(7) 0.6480(2) 0.0143(10) Uani 1.000000 . C9 C 0.8375(3) 0.2962(9) 0.8118(3) 0.0160(12) Uani 1.000000 . C13 C 0.6117(3) 0.2895(10) 0.6698(3) 0.0174(12) Uani 1.000000 . C14 C 0.5581(3) 0.2882(10) 0.6515(3) 0.0225(14) Uani 1.000000 . H14 H 0.5450(3) 0.2780(10) 0.6796(3) 0.0270(17) Uiso 1.000000 R C7 C 0.8466(3) 0.3276(10) 0.9106(3) 0.0188(13) Uani 1.000000 . H7 H 0.8313(3) 0.3377(10) 0.9368(3) 0.0226(15) Uiso 1.000000 R C4 C 0.8933(3) 0.2978(9) 0.8347(3) 0.0173(12) Uani 1.000000 . C15 C 0.5226(3) 0.3019(9) 0.5920(3) 0.0200(13) Uani 1.000000 . H15 H 0.4856(3) 0.3022(9) 0.5804(3) 0.0240(16) Uiso 1.000000 R C11 C 0.6777(3) 0.2544(10) 0.8322(3) 0.0199(13) Uani 1.000000 . H11 H 0.6641(3) 0.2395(10) 0.8598(3) 0.0239(16) Uiso 1.000000 R C8 C 0.8143(3) 0.3042(9) 0.8506(3) 0.0159(12) Uani 1.000000 . C17 C 0.5953(2) 0.3202(9) 0.5673(3) 0.0164(12) Uani 1.000000 . C5 C 0.9255(3) 0.3191(8) 0.8960(3) 0.0172(13) Uani 1.000000 . H5 H 0.9630(3) 0.3213(8) 0.9115(3) 0.0206(15) Uiso 1.000000 R C21 C 0.7028(2) 0.3386(10) 0.6080(3) 0.0169(12) Uani 1.000000 . H21 H 0.7398(2) 0.3497(10) 0.6213(3) 0.0203(14) Uiso 1.000000 R C10 C 0.7316(3) 0.2702(10) 0.8546(3) 0.0179(12) Uani 1.000000 . H10 H 0.7513(3) 0.2688(10) 0.8960(3) 0.0215(15) Uiso 1.000000 R C12 C 0.6407(3) 0.2580(9) 0.7733(3) 0.0169(12) Uani 1.000000 . H12 H 0.6046(3) 0.2437(9) 0.7646(3) 0.0203(15) Uiso 1.000000 R C6 C 0.9022(3) 0.3361(11) 0.9321(3) 0.0221(14) Uani 1.000000 . H6 H 0.9239(3) 0.3542(11) 0.9728(3) 0.0265(16) Uiso 1.000000 R C3 C 0.9143(3) 0.2765(10) 0.7935(3) 0.0195(13) Uani 1.000000 . H3 H 0.9513(3) 0.2810(10) 0.8059(3) 0.0234(16) Uiso 1.000000 R C20 C 0.6697(3) 0.3528(11) 0.5474(3) 0.0224(13) Uani 1.000000 . H20 H 0.6844(3) 0.3711(11) 0.5210(3) 0.0269(16) Uiso 1.000000 R C1 C 0.8263(3) 0.2499(9) 0.7178(3) 0.0187(13) Uani 1.000000 . H1 H 0.8037(3) 0.2304(9) 0.6774(3) 0.0225(15) Uiso 1.000000 R C2 C 0.8797(3) 0.2495(11) 0.7360(3) 0.0233(14) Uani 1.000000 . H2 H 0.8929(3) 0.2302(11) 0.7082(3) 0.0280(17) Uiso 1.000000 R C19 C 0.6160(3) 0.3401(10) 0.5271(3) 0.0201(13) Uani 1.000000 . H19 H 0.5931(3) 0.3446(10) 0.4863(3) 0.0241(15) Uiso 1.000000 R C18 C 0.6305(3) 0.3077(8) 0.6275(3) 0.0132(12) Uani 1.000000 . C16 C 0.5398(3) 0.3148(9) 0.5506(3) 0.0207(14) Uani 1.000000 . H16 H 0.5150(3) 0.3203(9) 0.5104(3) 0.0249(16) Uiso 1.000000 R Cl1 Cl 0.72285(15) 0.9319(7) 0.49330(14) 0.0820(10) Uani 1.000000 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.01545(14) 0.01411(15) 0.01659(14) -0.00013(8) 0.00854(10) -0.00111(8) N2 0.015(3) 0.015(3) 0.016(2) -0.0011(19) 0.008(2) -0.0037(19) N1 0.015(3) 0.013(3) 0.023(3) 0.0015(19) 0.010(2) 0.003(2) N3 0.017(3) 0.016(3) 0.018(3) 0.0019(19) 0.013(2) -0.0008(19) N4 0.014(2) 0.013(3) 0.018(3) -0.0002(18) 0.010(2) -0.0010(18) C9 0.020(3) 0.008(3) 0.023(3) 0.001(2) 0.013(3) 0.001(2) C13 0.015(3) 0.022(3) 0.019(3) 0.000(2) 0.011(3) -0.000(2) C14 0.020(3) 0.025(4) 0.025(3) -0.000(3) 0.013(3) 0.001(3) C7 0.024(3) 0.014(3) 0.016(3) -0.001(2) 0.007(3) -0.001(2) C4 0.017(3) 0.017(3) 0.019(3) 0.001(2) 0.009(3) -0.001(2) C15 0.011(3) 0.018(3) 0.028(4) 0.001(2) 0.007(3) -0.004(2) C11 0.025(3) 0.021(3) 0.024(3) -0.002(2) 0.019(3) 0.002(2) C8 0.018(3) 0.014(3) 0.017(3) 0.004(2) 0.009(2) 0.003(2) C17 0.013(3) 0.017(3) 0.019(3) 0.004(2) 0.007(2) -0.000(2) C5 0.021(3) 0.003(3) 0.025(3) -0.000(2) 0.009(3) 0.002(2) C21 0.015(3) 0.023(3) 0.017(3) -0.002(2) 0.010(2) -0.001(2) C10 0.021(3) 0.019(3) 0.019(3) -0.000(2) 0.013(3) -0.001(2) C12 0.022(3) 0.012(3) 0.021(3) 0.001(2) 0.014(3) 0.003(2) C6 0.019(3) 0.020(3) 0.021(3) -0.002(2) 0.004(3) 0.001(3) C3 0.019(3) 0.023(3) 0.023(3) 0.004(2) 0.016(3) 0.005(2) C20 0.024(3) 0.026(3) 0.021(3) 0.001(3) 0.013(3) 0.002(3) C1 0.022(3) 0.014(3) 0.021(3) 0.003(2) 0.009(3) 0.001(2) C2 0.027(4) 0.025(4) 0.022(3) 0.002(3) 0.015(3) 0.003(3) C19 0.022(3) 0.020(3) 0.013(3) 0.003(2) 0.004(2) 0.002(2) C18 0.019(3) 0.003(3) 0.023(3) 0.000(2) 0.014(3) -0.002(2) C16 0.011(3) 0.016(3) 0.028(3) 0.003(2) 0.003(3) 0.001(2) Cl1 0.083(2) 0.104(3) 0.0597(18) -0.014(2) 0.0328(17) 0.0043(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 N2 1.990(5) . Pt1 N1 2.049(6) . Pt1 N3 2.000(5) . Pt1 N4 2.039(5) . N2 C8 1.394(8) . N2 C10 1.344(8) . N1 C9 1.362(9) . N1 C1 1.350(9) . N3 C13 1.413(9) . N3 C12 1.345(8) . N4 C21 1.342(8) . N4 C18 1.392(8) . C9 C4 1.416(9) . C9 C8 1.420(9) . C13 C14 1.374(9) . C13 C18 1.411(9) . C14 H14 0.9500 . C14 C15 1.401(10) . C7 H7 0.9500 . C7 C8 1.398(9) . C7 C6 1.418(9) . C4 C5 1.422(9) . C4 C3 1.433(9) . C15 H15 0.9500 . C15 C16 1.357(10) . C11 H11 0.9500 . C11 C10 1.372(9) . C11 C12 1.396(10) . C17 C19 1.405(9) . C17 C18 1.411(9) . C17 C16 1.430(9) . C5 H5 0.9500 . C5 C6 1.361(10) . C21 H21 0.9500 . C21 C20 1.407(9) . C10 H10 0.9500 . C12 H12 0.9500 . C6 H6 0.9500 . C3 H3 0.9500 . C3 C2 1.364(10) . C20 H20 0.9500 . C20 C19 1.370(9) . C1 H1 0.9500 . C1 C2 1.367(10) . C2 H2 0.9500 . C19 H19 0.9500 . C16 H16 0.9500 . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N1 Pt1 N2 80.6(2) . . N3 Pt1 N2 94.1(2) . . N3 Pt1 N1 173.7(2) . . N4 Pt1 N2 173.2(2) . . N4 Pt1 N1 104.7(2) . . N4 Pt1 N3 80.7(2) . . C8 N2 Pt1 114.4(4) . . C10 N2 Pt1 123.2(5) . . C10 N2 C8 122.4(6) . . C9 N1 Pt1 112.9(4) . . C1 N1 Pt1 130.9(5) . . C1 N1 C9 116.2(6) . . C13 N3 Pt1 115.1(4) . . C12 N3 Pt1 123.3(5) . . C12 N3 C13 121.5(6) . . C21 N4 Pt1 130.2(4) . . C18 N4 Pt1 113.2(4) . . C18 N4 C21 116.5(5) . . C4 C9 N1 123.9(6) . . C8 C9 N1 116.5(6) . . C8 C9 C4 119.6(6) . . C14 C13 N3 127.0(6) . . C18 C13 N3 114.2(6) . . C18 C13 C14 118.8(6) . . H14 C14 C13 119.6(4) . . C15 C14 C13 120.8(7) . . C15 C14 H14 119.6(4) . . C8 C7 H7 120.2(4) . . C6 C7 H7 120.2(4) . . C6 C7 C8 119.6(6) . . C5 C4 C9 119.9(6) . . C3 C4 C9 116.7(6) . . C3 C4 C5 123.3(6) . . H15 C15 C14 119.3(4) . . C16 C15 C14 121.3(6) . . C16 C15 H15 119.3(4) . . C10 C11 H11 116.5(4) . . C12 C11 H11 116.5(4) . . C12 C11 C10 127.0(6) . . C9 C8 N2 114.9(6) . . C7 C8 N2 125.7(6) . . C7 C8 C9 119.5(6) . . C18 C17 C19 118.8(6) . . C16 C17 C19 123.3(6) . . C16 C17 C18 117.9(6) . . H5 C5 C4 120.3(4) . . C6 C5 C4 119.4(6) . . C6 C5 H5 120.3(4) . . H21 C21 N4 118.0(4) . . C20 C21 N4 124.0(6) . . C20 C21 H21 118.0(4) . . C11 C10 N2 126.6(6) . . H10 C10 N2 116.7(4) . . H10 C10 C11 116.7(4) . . C11 C12 N3 125.5(6) . . H12 C12 N3 117.3(4) . . H12 C12 C11 117.3(4) . . C5 C6 C7 121.8(6) . . H6 C6 C7 119.1(4) . . H6 C6 C5 119.1(4) . . H3 C3 C4 120.9(4) . . C2 C3 C4 118.2(6) . . C2 C3 H3 120.9(4) . . H20 C20 C21 120.4(4) . . C19 C20 C21 119.2(6) . . C19 C20 H20 120.4(4) . . H1 C1 N1 118.0(4) . . C2 C1 N1 123.9(7) . . C2 C1 H1 118.0(4) . . C1 C2 C3 120.9(7) . . H2 C2 C3 119.5(4) . . H2 C2 C1 119.5(4) . . C20 C19 C17 119.2(6) . . H19 C19 C17 120.4(4) . . H19 C19 C20 120.4(4) . . C13 C18 N4 116.7(6) . . C17 C18 N4 122.1(6) . . C17 C18 C13 121.1(6) . . C17 C16 C15 120.1(6) . . H16 C16 C15 120.0(4) . . H16 C16 C17 120.0(4) . . _smtbx_masks_special_details ; Each void is postulated to contain 3.2 molecules of diethyl ether, totaling to 134 e per void. The non-H atomic volume, based on this assignment, is reasonable at 19 e per atom. ; loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.905 0.250 309.0 133.2 ? 2 0.000 -0.457 0.750 309.0 133.5 ? 3 0.500 -0.026 0.250 309.0 133.2 ? 4 0.500 -0.726 0.750 309.0 133.5 ?