# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FI _publ_contact_author_email pino@ifsc.usp.br data_s93 _database_code_depnum_ccdc_archive 'CCDC 841553' _audit_creation_date 2011-08-24T09:00:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'H14 N5 O4 P Ru, Cl4 Zn' _chemical_formula_sum 'Cl4 H14 N5 O4 P Ru Zn' _chemical_formula_weight 487.37 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn 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 7.02700(10) _cell_length_b 22.1460(8) _cell_length_c 9.2010(3) _cell_angle_alpha 90 _cell_angle_beta 91.499(2) _cell_angle_gamma 90 _cell_volume 1431.37(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7396 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.228 _exptl_crystal_size_mid 0.093 _exptl_crystal_size_min 0.062 _exptl_crystal_density_diffrn 2.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.026 0 1 1 0.036 0 -1 1 0.042 0 -1 0 0.053 0 1 0 0.04 13 -2 1 0.109 -12 -1 11 0.117 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.593 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 8 x 8 x 8 = 512 sampling points was used ; _exptl_absorpt_correction_T_min 0.6288 _exptl_absorpt_correction_T_max 0.8193 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.274859E-1 _diffrn_orient_matrix_ub_12 0.48249E-2 _diffrn_orient_matrix_ub_13 0.105452 _diffrn_orient_matrix_ub_21 0.13962 _diffrn_orient_matrix_ub_22 0.22721E-2 _diffrn_orient_matrix_ub_23 0.232897E-1 _diffrn_orient_matrix_ub_31 -0.41173E-2 _diffrn_orient_matrix_ub_32 0.448397E-1 _diffrn_orient_matrix_ub_33 -0.125272E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_unetI/netI 0.0488 _diffrn_reflns_number 10916 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 2752 _reflns_number_gt 2264 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0530P)^2^+0.8924P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2752 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.919 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ru Ru 0.91824(5) 0.132422(13) 0.13845(3) 0.02878(14) Uani 1 1 d . . . P P 0.67817(14) 0.05449(4) 0.12753(12) 0.0303(2) Uani 1 1 d . . . O O 1.1795(5) 0.23425(15) 0.1206(4) 0.0560(9) Uani 1 1 d . . . O1 O 0.7436(4) -0.00322(12) 0.0565(3) 0.0367(7) Uani 1 1 d . . . O2 O 0.6021(5) 0.04279(12) 0.2850(3) 0.0501(8) Uani 1 1 d . . . H2 H 0.6664 0.0164 0.325 0.075 Uiso 1 1 d R . . O3 O 0.4985(4) 0.08128(12) 0.0445(3) 0.0424(7) Uani 1 1 d . . . H3 H 0.4318 0.0536 0.013 0.064 Uiso 1 1 d R . . N1 N 0.9727(5) 0.10539(15) -0.0773(3) 0.0383(8) Uani 1 1 d . . . H1A H 1.0423 0.1335 -0.1202 0.046 Uiso 1 1 d R . . H1B H 0.8628 0.1009 -0.1265 0.046 Uiso 1 1 d R . . H1C H 1.0356 0.0705 -0.076 0.046 Uiso 1 1 d R . . N2 N 0.6996(5) 0.19062(15) 0.0601(4) 0.0456(9) Uani 1 1 d . . . H2A H 0.6388 0.2063 0.1349 0.055 Uiso 1 1 d R . . H2B H 0.6179 0.1698 0.0041 0.055 Uiso 1 1 d R . . H2C H 0.7502 0.2202 0.0083 0.055 Uiso 1 1 d R . . N3 N 0.8441(5) 0.15039(16) 0.3557(4) 0.0398(8) Uani 1 1 d . . . H3A H 0.9394 0.1394 0.4156 0.048 Uiso 1 1 d R . . H3B H 0.74 0.1296 0.3767 0.048 Uiso 1 1 d R . . H3C H 0.8215 0.1897 0.366 0.048 Uiso 1 1 d R . . N4 N 1.1066(5) 0.06453(15) 0.2198(4) 0.0380(8) Uani 1 1 d . . . H4A H 1.2114 0.0818 0.2572 0.046 Uiso 1 1 d R . . H4B H 1.1377 0.0399 0.1478 0.046 Uiso 1 1 d R . . H4C H 1.0494 0.0435 0.2887 0.046 Uiso 1 1 d R . . N5 N 1.0871(5) 0.19300(15) 0.1329(3) 0.0348(8) Uani 1 1 d . . . Zn Zn 0.37059(7) 0.13208(2) 0.61567(5) 0.03770(17) Uani 1 1 d . . . Cl1 Cl 0.13574(17) 0.06312(6) 0.58707(12) 0.0504(3) Uani 1 1 d . . . Cl2 Cl 0.37645(16) 0.18539(5) 0.40273(12) 0.0462(3) Uani 1 1 d . . . Cl3 Cl 0.64622(18) 0.08580(8) 0.66529(15) 0.0717(4) Uani 1 1 d . . . Cl4 Cl 0.30231(19) 0.19834(5) 0.79791(13) 0.0553(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 Ru 0.0287(2) 0.0287(2) 0.0288(2) -0.00059(13) -0.00167(13) -0.00197(12) P 0.0302(5) 0.0265(5) 0.0344(6) 0.0002(4) 0.0011(4) -0.0012(4) O 0.059(2) 0.054(2) 0.054(2) 0.0076(16) -0.0081(16) -0.0242(17) O1 0.0346(14) 0.0322(15) 0.0433(17) -0.0071(12) -0.0009(12) 0.0004(11) O2 0.070(2) 0.0380(17) 0.0436(19) 0.0061(14) 0.0219(16) 0.0001(14) O3 0.0333(15) 0.0314(15) 0.062(2) -0.0007(14) -0.0102(14) -0.0010(12) N1 0.042(2) 0.043(2) 0.0294(19) -0.0017(16) 0.0014(15) -0.0069(16) N2 0.043(2) 0.0309(19) 0.062(3) 0.0088(17) -0.0127(18) -0.0030(15) N3 0.042(2) 0.043(2) 0.035(2) -0.0032(16) -0.0001(15) 0.0004(16) N4 0.0350(18) 0.040(2) 0.039(2) 0.0007(16) -0.0020(15) 0.0040(15) N5 0.0360(19) 0.039(2) 0.0293(19) -0.0005(15) -0.0027(14) -0.0045(15) Zn 0.0391(3) 0.0389(3) 0.0351(3) 0.0015(2) -0.0008(2) 0.00135(19) Cl1 0.0522(7) 0.0550(7) 0.0436(7) 0.0032(5) -0.0039(5) -0.0138(5) Cl2 0.0550(7) 0.0449(6) 0.0387(6) 0.0072(5) -0.0021(5) 0.0047(5) Cl3 0.0483(7) 0.1133(13) 0.0530(8) 0.0120(8) -0.0076(6) 0.0261(7) Cl4 0.0813(9) 0.0379(6) 0.0473(7) -0.0043(5) 0.0162(6) -0.0072(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ru N5 1.793(3) . ? Ru N3 2.116(3) . ? Ru N2 2.117(3) . ? Ru N1 2.118(3) . ? Ru N4 2.126(3) . ? Ru P 2.4136(10) . ? P O1 1.513(3) . ? P O3 1.574(3) . ? P O2 1.579(3) . ? O N5 1.128(4) . ? O2 H2 0.82 . ? O3 H3 0.82 . ? N1 H1A 0.89 . ? N1 H1B 0.8901 . ? N1 H1C 0.8901 . ? N2 H2A 0.89 . ? N2 H2B 0.89 . ? N2 H2C 0.89 . ? N3 H3A 0.8899 . ? N3 H3B 0.89 . ? N3 H3C 0.89 . ? N4 H4A 0.89 . ? N4 H4B 0.89 . ? N4 H4C 0.89 . ? Zn Cl3 2.2280(13) . ? Zn Cl1 2.2588(12) . ? Zn Cl4 2.2885(12) . ? Zn Cl2 2.2887(12) . ? 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 N5 Ru N3 93.78(14) . . ? N5 Ru N2 90.55(14) . . ? N3 Ru N2 90.74(15) . . ? N5 Ru N1 92.79(14) . . ? N3 Ru N1 173.38(13) . . ? N2 Ru N1 89.99(14) . . ? N5 Ru N4 97.64(14) . . ? N3 Ru N4 88.09(13) . . ? N2 Ru N4 171.79(13) . . ? N1 Ru N4 90.25(14) . . ? N5 Ru P 175.11(11) . . ? N3 Ru P 89.12(10) . . ? N2 Ru P 85.47(10) . . ? N1 Ru P 84.38(9) . . ? N4 Ru P 86.39(10) . . ? O1 P O3 110.98(16) . . ? O1 P O2 111.83(16) . . ? O3 P O2 102.73(17) . . ? O1 P Ru 113.71(11) . . ? O3 P Ru 107.54(11) . . ? O2 P Ru 109.41(13) . . ? P O2 H2 109.5 . . ? P O3 H3 109.5 . . ? Ru N1 H1A 109.5 . . ? Ru N1 H1B 109.4 . . ? H1A N1 H1B 109.5 . . ? Ru N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Ru N2 H2A 109.4 . . ? Ru N2 H2B 109.4 . . ? H2A N2 H2B 109.5 . . ? Ru N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Ru N3 H3A 109.5 . . ? Ru N3 H3B 109.4 . . ? H3A N3 H3B 109.5 . . ? Ru N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Ru N4 H4A 109.5 . . ? Ru N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Ru N4 H4C 109.4 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? O N5 Ru 172.8(3) . . ? Cl3 Zn Cl1 109.97(6) . . ? Cl3 Zn Cl4 110.04(6) . . ? Cl1 Zn Cl4 110.63(5) . . ? Cl3 Zn Cl2 112.19(5) . . ? Cl1 Zn Cl2 106.17(4) . . ? Cl4 Zn Cl2 107.78(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 N5 Ru P O1 97.6(13) . . . . ? N3 Ru P O1 -135.97(16) . . . . ? N2 Ru P O1 133.22(17) . . . . ? N1 Ru P O1 42.78(16) . . . . ? N4 Ru P O1 -47.83(16) . . . . ? N5 Ru P O3 -25.7(13) . . . . ? N3 Ru P O3 100.74(16) . . . . ? N2 Ru P O3 9.93(17) . . . . ? N1 Ru P O3 -80.51(16) . . . . ? N4 Ru P O3 -171.12(16) . . . . ? N5 Ru P O2 -136.5(13) . . . . ? N3 Ru P O2 -10.14(16) . . . . ? N2 Ru P O2 -100.95(17) . . . . ? N1 Ru P O2 168.61(16) . . . . ? N4 Ru P O2 78.00(16) . . . . ? N3 Ru N5 O -105(3) . . . . ? N2 Ru N5 O -15(3) . . . . ? N1 Ru N5 O 75(3) . . . . ? N4 Ru N5 O 166(3) . . . . ? P Ru N5 O 21(4) . . . . ? # END of CIF