# Electronic Supplementary Material (ESI) for Metallomics # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_methyl2 _database_code_depnum_ccdc_archive 'CCDC 922832' #TrackingRef '17391_web_deposit_cif_file_0_SeijiKomeda_1359685244.methyl5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H16 N10 O7 Pt2' _chemical_formula_weight 682.43 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 6.760(10) _cell_length_b 12.76(3) _cell_length_c 18.06(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.31(4) _cell_angle_gamma 90.00 _cell_volume 1557(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 18.003 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11505 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3483 _reflns_number_gt 3019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0660P)^2^+16.1587P] 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 3483 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 1.462 _refine_ls_shift/su_mean 0.073 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 0.02690(5) 0.75516(2) 0.178893(18) 0.01874(14) Uani 1 1 d . . . Pt2 Pt 0.08335(6) 0.51817(3) 0.26914(2) 0.03290(15) Uani 1 1 d . . . O1 O -0.0038(9) 0.5966(5) 0.1758(4) 0.0244(13) Uani 1 1 d . . . H1A H 0.0713 0.5701 0.1352 0.029 Uiso 1 1 calc R . . N2 N 0.0579(12) 0.7440(6) 0.2878(4) 0.0225(16) Uani 1 1 d . . . N7 N -0.0063(14) 0.7670(7) 0.0665(5) 0.0302(18) Uani 1 1 d . . . H7A H -0.1096 0.8079 0.0548 0.045 Uiso 1 1 calc R . . H7B H -0.0264 0.7036 0.0471 0.045 Uiso 1 1 calc R . . H7C H 0.1027 0.7947 0.0485 0.045 Uiso 1 1 calc R . . N3 N 0.0799(11) 0.6529(7) 0.3232(4) 0.0284(17) Uani 1 1 d . . . N6 N 0.0592(12) 0.9127(6) 0.1853(5) 0.0258(16) Uani 1 1 d . . . H6A H 0.0209 0.9349 0.2292 0.039 Uiso 1 1 calc R . . H6B H -0.0148 0.9430 0.1495 0.039 Uiso 1 1 calc R . . H6C H 0.1857 0.9294 0.1801 0.039 Uiso 1 1 calc R . . N1 N 0.0676(12) 0.8229(7) 0.3355(5) 0.0327(19) Uani 1 1 d . . . N4 N 0.1037(13) 0.6708(9) 0.3964(5) 0.039(2) Uani 1 1 d . . . N8 N 0.089(2) 0.3802(8) 0.2123(7) 0.068(4) Uani 1 1 d . . . H8A H -0.0337 0.3611 0.1991 0.101 Uiso 1 1 calc R . . H8B H 0.1453 0.3309 0.2411 0.101 Uiso 1 1 calc R . . H8C H 0.1592 0.3883 0.1720 0.101 Uiso 1 1 calc R . . C5 C 0.0959(16) 0.7753(12) 0.4018(6) 0.044(3) Uani 1 1 d . . . N9 N 0.169(2) 0.4413(9) 0.3634(6) 0.066(4) Uani 1 1 d . . . H9A H 0.2833 0.4678 0.3812 0.100 Uiso 1 1 calc R . . H9B H 0.1849 0.3735 0.3535 0.100 Uiso 1 1 calc R . . H9C H 0.0771 0.4488 0.3968 0.100 Uiso 1 1 calc R . . C51 C 0.118(2) 0.8323(15) 0.4744(7) 0.069(5) Uani 1 1 d . . . H51A H -0.0067 0.8627 0.4863 0.103 Uiso 1 1 calc R . . H51B H 0.2153 0.8866 0.4707 0.103 Uiso 1 1 calc R . . H51C H 0.1596 0.7839 0.5127 0.103 Uiso 1 1 calc R . . O22 O 0.2342(13) 0.5475(8) 0.0680(5) 0.056(2) Uani 1 1 d . . . N21 N 0.2368(18) 0.4701(11) 0.0260(8) 0.070(4) Uani 1 1 d . . . O24 O 0.275(3) 0.4699(15) -0.0392(8) 0.129(7) Uani 1 1 d . . . O12 O 0.2812(17) 0.2142(8) 0.3214(9) 0.088(4) Uani 1 1 d . . . N11 N 0.161(2) 0.1464(9) 0.3225(10) 0.070(4) Uani 1 1 d . . . O14 O 0.068(2) 0.1281(12) 0.2599(11) 0.114(5) Uani 1 1 d . . . O13 O 0.115(3) 0.0912(12) 0.3711(9) 0.124(6) Uani 1 1 d . . . O23 O 0.219(7) 0.3810(15) 0.0586(15) 0.35(3) Uani 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 0.0165(2) 0.01709(19) 0.0225(2) -0.00035(11) -0.00078(14) 0.00020(10) Pt2 0.0369(2) 0.0253(2) 0.0369(3) 0.00981(15) 0.00533(17) 0.00682(15) O1 0.024(3) 0.016(3) 0.032(4) 0.001(2) -0.003(3) -0.002(2) N2 0.021(4) 0.028(4) 0.019(4) -0.002(3) -0.002(3) 0.002(3) N7 0.035(5) 0.028(4) 0.028(4) 0.003(3) -0.001(4) -0.001(3) N3 0.022(4) 0.042(5) 0.022(4) 0.009(4) 0.001(3) 0.006(3) N6 0.027(4) 0.018(3) 0.033(4) -0.003(3) 0.002(3) 0.000(3) N1 0.024(4) 0.045(5) 0.029(4) -0.013(4) 0.001(3) 0.001(4) N4 0.026(4) 0.064(7) 0.028(5) 0.005(4) -0.001(4) 0.000(4) N8 0.106(10) 0.026(5) 0.073(9) 0.007(5) 0.023(8) 0.007(6) C5 0.024(5) 0.079(9) 0.030(6) -0.015(6) 0.001(4) -0.005(6) N9 0.106(10) 0.045(6) 0.048(6) 0.018(5) -0.004(6) 0.035(7) C51 0.052(8) 0.122(15) 0.032(6) -0.034(8) -0.008(6) 0.004(8) O22 0.043(5) 0.078(6) 0.047(5) -0.031(5) 0.010(4) -0.016(4) N21 0.050(7) 0.079(9) 0.083(10) -0.048(8) 0.013(6) -0.001(6) O24 0.141(13) 0.181(16) 0.066(8) -0.084(10) -0.008(8) 0.069(12) O12 0.062(6) 0.034(5) 0.168(14) -0.007(7) 0.023(7) -0.011(5) N11 0.082(9) 0.034(6) 0.096(11) -0.007(7) 0.019(8) -0.011(6) O14 0.110(12) 0.073(9) 0.161(16) -0.039(10) 0.031(11) 0.024(8) O13 0.160(15) 0.078(9) 0.139(14) 0.038(9) 0.086(12) 0.000(9) O23 0.73(7) 0.088(13) 0.26(3) -0.068(16) 0.33(4) -0.16(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 Pt1 N2 1.975(9) . ? Pt1 N6 2.025(9) . ? Pt1 O1 2.034(8) . ? Pt1 N7 2.039(9) . ? Pt2 N3 1.978(10) . ? Pt2 O1 2.028(7) . ? Pt2 N9 2.029(10) . ? Pt2 N8 2.039(12) . ? N2 N1 1.326(11) . ? N2 N3 1.331(11) . ? N3 N4 1.343(12) . ? N1 C5 1.349(16) . ? N4 C5 1.337(17) . ? C5 C51 1.502(16) . ? O22 N21 1.245(14) . ? N21 O23 1.29(3) . ? N21 O24 1.214(19) . ? O12 N11 1.189(16) . ? N11 O13 1.178(18) . ? N11 O14 1.29(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 N2 Pt1 N6 90.4(3) . . ? N2 Pt1 O1 87.8(3) . . ? N6 Pt1 O1 178.3(3) . . ? N2 Pt1 N7 179.8(3) . . ? N6 Pt1 N7 89.5(3) . . ? O1 Pt1 N7 92.3(3) . . ? N3 Pt2 O1 88.4(3) . . ? N3 Pt2 N9 90.8(4) . . ? O1 Pt2 N9 179.2(4) . . ? N3 Pt2 N8 179.2(4) . . ? O1 Pt2 N8 91.1(4) . . ? N9 Pt2 N8 89.6(5) . . ? Pt2 O1 Pt1 116.2(3) . . ? N1 N2 N3 110.4(8) . . ? N1 N2 Pt1 126.4(6) . . ? N3 N2 Pt1 123.2(6) . . ? N2 N3 N4 109.3(8) . . ? N2 N3 Pt2 121.6(6) . . ? N4 N3 Pt2 129.0(7) . . ? N2 N1 C5 103.6(9) . . ? C5 N4 N3 103.8(9) . . ? N4 C5 N1 112.9(10) . . ? N4 C5 C51 123.0(13) . . ? N1 C5 C51 124.2(14) . . ? O23 N21 O24 117.9(15) . . ? O23 N21 O22 114.7(17) . . ? O24 N21 O22 126.9(17) . . ? O13 N11 O12 131(2) . . ? O13 N11 O14 114.3(17) . . ? O12 N11 O14 115.1(17) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 3.224 _refine_diff_density_min -1.864 _refine_diff_density_rms 0.302