Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal CrystEngComm loop_ _publ_author_name 'Harry Goodwin' 'Donald C. Craig' 'Marcia Scudder' _publ_contact_author_name 'Harold Goodwin' _publ_contact_author_address ; School of Chemistry University of New South Wales Sydney New South Wales 2052 AUSTRALIA ; _publ_contact_author_email 'H.GOODWIN@UNSW.EDU.AU ' _publ_section_title ; Hydrogen bonding influences on the properties of heavily hydrated chloride salts of iron(II) and ruthenium(II) complexes of 2,6-bis(pyrazol-3-yl)pyridine, 2,6-bis(1,2,4-triazol-3-yl)pyridine and 2,2':6',2"-terpyridine. ; data_DHG76_[Fe(bpp)2]Cl2.6.5H2O _database_code_depnum_ccdc_archive 'CCDC 281664' _audit_creation_method 'RAELSPUB and manual entry' # SUBMISSION DETAILS # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C22 H18 Fe N10 2+,2(Cl 1-),6.5(H2 O)' _chemical_formula_sum 'C22 H31 Cl2 Fe N10 O6.5' _chemical_formula_iupac ? _chemical_formula_weight 666.3 # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b a 2' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 1/2-x,1/2+y,z 4 1/2+x,1/2-y,z _cell_length_a 16.199(3) _cell_length_b 23.421(3) _cell_length_c 8.289(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3145(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380.0 _exptl_absorpt_coefficient_mu 0.704 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 2970 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 21 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 2970 _reflns_number_gt 1842 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.063 _refine_ls_wR_factor_ref 0.073 _refine_ls_abs_structure_Flack 0.17(15) _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1842 _refine_ls_number_parameters 208 _refine_ls_goodness_of_fit_ref 1.91 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.90 _refine_diff_density_min -1.23 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description Cl/O 0.5Cl+0.5O loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe1 0.32997(8) 0.21460(6) 0.50000(0) 0.0333(4) Uani Fe 1.0 N1A 0.4357(5) 0.2393(4) 0.5914(14) 0.041(2) Uani N 1.0 N2A 0.5040(5) 0.2145(5) 0.6547(13) 0.051(2) Uani N 1.0 N3A 0.3165(5) 0.2957(3) 0.4925(20) 0.044(2) Uani N 1.0 N4A 0.1586(6) 0.1852(4) 0.3565(14) 0.051(1) Uani N 1.0 N5A 0.2189(5) 0.2210(4) 0.4081(13) 0.040(1) Uani N 1.0 C1A 0.5578(7) 0.2544(7) 0.7098(19) 0.067(2) Uani C 1.0 C2A 0.5228(8) 0.3070(6) 0.6844(20) 0.071(2) Uani C 1.0 C3A 0.4464(7) 0.2961(5) 0.6096(18) 0.053(2) Uani C 1.0 C4A 0.3786(8) 0.3300(5) 0.5480(18) 0.058(2) Uani C 1.0 C5A 0.3719(9) 0.3889(5) 0.5391(24) 0.087(3) Uani C 1.0 C6A 0.3027(10) 0.4123(6) 0.4674(28) 0.101(4) Uani C 1.0 C7A 0.2388(9) 0.3770(6) 0.4155(22) 0.083(4) Uani C 1.0 C8A 0.2482(8) 0.3179(5) 0.4286(18) 0.055(2) Uani C 1.0 C9A 0.1920(6) 0.2746(5) 0.3822(17) 0.050(2) Uani C 1.0 C10A 0.1128(8) 0.2723(6) 0.3067(19) 0.066(3) Uani C 1.0 C11A 0.0936(7) 0.2166(7) 0.2958(19) 0.065(2) Uani C 1.0 N1B 0.3805(5) 0.2013(4) 0.2891(14) 0.046(2) Uani N 1.0 N2B 0.4029(6) 0.2334(5) 0.1623(15) 0.068(2) Uani N 1.0 N3B 0.3458(5) 0.1330(3) 0.5074(18) 0.045(2) Uani N 1.0 N4B 0.2537(6) 0.2241(5) 0.8422(14) 0.066(2) Uani N 1.0 N5B 0.2873(6) 0.1960(4) 0.7139(14) 0.045(2) Uani N 1.0 C1B 0.4373(9) 0.2002(9) 0.0491(17) 0.096(4) Uani C 1.0 C2B 0.4390(9) 0.1466(8) 0.1022(21) 0.093(4) Uani C 1.0 C3B 0.4021(7) 0.1487(6) 0.2543(19) 0.061(2) Uani C 1.0 C4B 0.3840(8) 0.1085(6) 0.3759(20) 0.061(2) Uani C 1.0 C5B 0.3988(9) 0.0504(7) 0.3848(27) 0.096(3) Uani C 1.0 C6B 0.3758(10) 0.0190(6) 0.5213(31) 0.114(3) Uani C 1.0 C7B 0.3363(10) 0.0450(6) 0.6495(27) 0.099(3) Uani C 1.0 C8B 0.3237(8) 0.1041(6) 0.6360(21) 0.062(2) Uani C 1.0 C9B 0.2868(8) 0.1401(6) 0.7526(19) 0.061(2) Uani C 1.0 C10B 0.2508(10) 0.1344(8) 0.9100(21) 0.095(4) Uani C 1.0 C11B 0.2321(9) 0.1872(9) 0.9598(18) 0.096(4) Uani C 1.0 Cl1 0.5000(0) 0.0000(0) 0.9312(9) 0.089(2) Uani Cl 1.0 Cl2 0.7147(3) 0.1478(2) 0.8796(8) 0.125(2) Uani Cl 1.0 Cl/OW 0.0692(9) 0.0330(5) 0.6954(25) 0.319(9) Uani Cl 1.0 OW1 0.5525(6) 0.1042(4) 0.6997(14) 0.077(3) Uani O 1.0 OW2 0.1402(9) 0.0680(4) 0.3876(24) 0.163(7) Uani O 1.0 OW3 0.3814(9) 0.3440(6) 0.0932(20) 0.152(6) Uani O 1.0 OW4 0.6454(11) 0.0537(8) 1.1146(22) 0.237(9) Uani O 1.0 OW5 0.2137(14) 0.0085(9) 0.1383(32) 0.152(8) Uani O 0.5 OW5' 0.1658(15) -0.0298(8) -0.1042(32) 0.152(8) Uani O 0.5 OW6 0.5158(20) 0.4124(14) 0.0121(47) 0.256(9) Uani O 0.5 OW6' 0.4866(21) 0.4354(15) 0.1018(55) 0.256(9) Uani O 0.5 HN2A 0.5135 0.1724 0.6600 0.055 Uani H 1.0 HN4A 0.1610 0.1426 0.3615 0.058 Uani H 1.0 HC1A 0.6128 0.2468 0.7599 0.083 Uani H 1.0 HC2A 0.5466 0.3451 0.7129 0.092 Uani H 1.0 HC5A 0.4163 0.4140 0.5837 0.107 Uani H 1.0 HC6A 0.2985 0.4546 0.4529 0.133 Uani H 1.0 HC7A 0.1871 0.3937 0.3695 0.100 Uani H 1.0 HC10A 0.0787 0.3053 0.2695 0.084 Uani H 1.0 HC11A 0.0411 0.2006 0.2514 0.081 Uani H 1.0 HN2B 0.3950 0.2757 0.1536 0.076 Uani H 1.0 HN4B 0.2461 0.2664 0.8482 0.073 Uani H 1.0 HC1B 0.4583 0.2136 -0.0579 0.129 Uani H 1.0 HC2B 0.4618 0.1124 0.0456 0.123 Uani H 1.0 HC5B 0.4263 0.0305 0.2924 0.122 Uani H 1.0 HC6B 0.3881 -0.0228 0.5262 0.154 Uani H 1.0 HC7B 0.3178 0.0230 0.7463 0.126 Uani H 1.0 HC10B 0.2415 0.0981 0.9706 0.126 Uani H 1.0 HC11B 0.2065 0.1974 1.0657 0.128 Uani H 1.0 H1OW1 0.5324 0.0713 0.7659 0.077 Uani H 1.0 H2OW1 0.6038 0.1202 0.7494 0.077 Uani H 1.0 H1OW2 0.1192 0.0480 0.4858 0.163 Uani H 1.0 H2OW2 0.1645 0.0395 0.3115 0.163 Uani H 1.0 H1OW3 0.3346 0.3608 0.0303 0.152 Uani H 1.0 H2OW3 0.3759 0.3015 0.0950 0.152 Uani H 1.0 H1OW4 0.5976 0.0352 1.0588 0.237 Uani H 1.0 H2OW4 0.6692 0.0840 1.0433 0.237 Uani H 1.0 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 _atom_site_aniso_type_symbol Fe1 0.0308(7) 0.0424(8) 0.0268(7) 0.0037(8) -0.001(1) 0.001(1) Fe N1A 0.032(2) 0.054(2) 0.036(2) 0.000(2) 0.006(2) 0.000(2) N N2A 0.032(2) 0.079(3) 0.040(2) 0.004(2) 0.003(2) 0.002(2) N N3A 0.044(2) 0.039(3) 0.049(3) 0.005(2) 0.007(2) 0.003(3) N N4A 0.034(2) 0.076(3) 0.043(2) -0.004(2) 0.003(2) -0.002(2) N N5A 0.031(2) 0.055(2) 0.034(3) 0.005(2) 0.006(2) 0.003(2) N C1A 0.038(2) 0.109(4) 0.054(4) -0.010(3) -0.002(2) -0.007(4) C C2A 0.052(3) 0.090(3) 0.070(6) -0.023(3) 0.000(3) -0.016(4) C C3A 0.046(2) 0.058(2) 0.055(3) -0.011(2) 0.005(2) -0.007(3) C C4A 0.059(3) 0.042(3) 0.071(4) -0.005(2) 0.007(3) -0.003(3) C C5A 0.096(5) 0.041(3) 0.123(8) -0.008(2) 0.007(5) -0.004(3) C C6A 0.114(7) 0.040(3) 0.148(9) 0.011(2) 0.007(7) 0.010(3) C C7A 0.087(5) 0.050(2) 0.111(7) 0.025(2) 0.006(5) 0.017(3) C C8A 0.054(3) 0.048(2) 0.063(3) 0.016(2) 0.007(3) 0.010(3) C C9A 0.039(2) 0.064(2) 0.046(3) 0.016(2) 0.005(2) 0.010(2) C C10A 0.041(2) 0.101(4) 0.055(5) 0.022(3) 0.000(3) 0.014(4) C C11A 0.034(2) 0.112(5) 0.049(4) 0.004(2) -0.001(2) 0.003(4) C N1B 0.030(2) 0.078(3) 0.029(2) 0.001(2) -0.002(2) -0.009(2) N N2B 0.042(2) 0.130(4) 0.031(2) -0.009(3) 0.002(2) 0.007(3) N N3B 0.039(3) 0.043(3) 0.054(2) 0.001(2) -0.016(2) -0.004(2) N N4B 0.040(2) 0.129(4) 0.030(2) -0.001(3) 0.002(2) -0.010(3) N N5B 0.032(2) 0.074(3) 0.029(2) -0.005(2) -0.003(2) 0.003(2) N C1B 0.052(3) 0.203(7) 0.034(2) 0.000(5) 0.008(2) -0.017(3) C C2B 0.051(4) 0.175(6) 0.053(3) 0.022(5) -0.001(3) -0.054(4) C C3B 0.039(3) 0.095(3) 0.048(3) 0.014(3) -0.007(2) -0.034(3) C C4B 0.049(3) 0.060(3) 0.076(3) 0.015(3) -0.022(3) -0.031(3) C C5B 0.082(6) 0.062(3) 0.143(7) 0.027(3) -0.048(5) -0.046(3) C C6B 0.110(8) 0.044(3) 0.189(9) 0.012(3) -0.069(7) -0.009(3) C C7B 0.096(7) 0.053(3) 0.147(7) -0.013(3) -0.052(6) 0.032(3) C C8B 0.056(3) 0.052(3) 0.078(3) -0.010(2) -0.025(3) 0.019(3) C C9B 0.049(3) 0.085(3) 0.050(2) -0.018(3) -0.011(2) 0.028(3) C C10B 0.068(5) 0.161(5) 0.056(3) -0.033(5) -0.006(3) 0.051(4) C C11B 0.057(4) 0.197(6) 0.034(2) -0.017(5) 0.006(2) 0.016(3) C Cl1 0.099(4) 0.076(4) 0.092(5) -0.009(3) 0.0000(0) 0.0000(0) Cl Cl2 0.113(4) 0.135(4) 0.125(5) -0.045(3) -0.025(4) 0.049(4) Cl Cl/OW 0.315(9) 0.156(9) 0.486(9) 0.073(9) -0.015(9) 0.013(9) Cl OW1 0.083(7) 0.064(6) 0.083(8) 0.001(5) -0.013(6) 0.004(6) O OW2 0.175(9) 0.069(8) 0.245(9) 0.020(8) -0.053(9) -0.036(9) O OW3 0.150(9) 0.170(9) 0.137(9) 0.028(9) -0.021(9) 0.063(9) O OW4 0.307(9) 0.222(9) 0.180(9) -0.168(9) -0.153(9) 0.126(9) O OW5 0.178(9) 0.102(9) 0.175(9) 0.033(9) 0.020(9) 0.019(9) O OW5' 0.178(9) 0.102(9) 0.175(9) 0.033(9) 0.020(9) 0.019(9) O OW6 0.256(9) 0.256(9) 0.256(9) 0.0000(0) 0.0000(0) 0.0000(0) O OW6' 0.256(9) 0.256(9) 0.256(9) 0.0000(0) 0.0000(0) 0.0000(0) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1A 1.960(9) 1_555 1_555 no Fe1 N3A 1.913(7) 1_555 1_555 no Fe1 N5A 1.959(9) 1_555 1_555 no Fe1 N1B 1.955(11) 1_555 1_555 no Fe1 N3B 1.928(8) 1_555 1_555 no Fe1 N5B 1.953(11) 1_555 1_555 no N1A N2A 1.355(11) 1_555 1_555 no N1A C3A 1.351(14) 1_555 1_555 no N2A C1A 1.355(15) 1_555 1_555 no N3A C4A 1.367(14) 1_555 1_555 no N3A C8A 1.332(14) 1_555 1_555 no N4A N5A 1.356(12) 1_555 1_555 no N4A C11A 1.379(15) 1_555 1_555 no N5A C9A 1.345(13) 1_555 1_555 no C1A C2A 1.374(19) 1_555 1_555 no C2A C3A 1.407(16) 1_555 1_555 no C3A C4A 1.449(16) 1_555 1_555 no C4A C5A 1.386(16) 1_555 1_555 no C5A C6A 1.382(20) 1_555 1_555 no C6A C7A 1.393(20) 1_555 1_555 no C7A C8A 1.396(16) 1_555 1_555 no C8A C9A 1.418(16) 1_555 1_555 no C9A C10A 1.428(16) 1_555 1_555 no C10A C11A 1.343(18) 1_555 1_555 no N1B N2B 1.342(14) 1_555 1_555 no N1B C3B 1.314(14) 1_555 1_555 no N2B C1B 1.341(17) 1_555 1_555 no N3B C4B 1.379(17) 1_555 1_555 no N3B C8B 1.313(16) 1_555 1_555 no N4B N5B 1.364(13) 1_555 1_555 no N4B C11B 1.350(18) 1_555 1_555 no N5B C9B 1.347(15) 1_555 1_555 no C1B C2B 1.331(22) 1_555 1_555 no C2B C3B 1.396(20) 1_555 1_555 no C3B C4B 1.410(19) 1_555 1_555 no C4B C5B 1.384(18) 1_555 1_555 no C5B C6B 1.400(26) 1_555 1_555 no C6B C7B 1.381(27) 1_555 1_555 no C7B C8B 1.404(18) 1_555 1_555 no C8B C9B 1.415(20) 1_555 1_555 no C9B C10B 1.435(19) 1_555 1_555 no C10B C11B 1.337(22) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe1 N3A 79.6(4) 1_555 1_555 1_555 no N1A Fe1 N5A 158.4(4) 1_555 1_555 1_555 no N1A Fe1 N1B 91.5(4) 1_555 1_555 1_555 no N1A Fe1 N3B 99.4(4) 1_555 1_555 1_555 no N1A Fe1 N5B 91.4(5) 1_555 1_555 1_555 no N3A Fe1 N5A 78.8(4) 1_555 1_555 1_555 no N3A Fe1 N1B 100.2(6) 1_555 1_555 1_555 no N3A Fe1 N3B 178.9(4) 1_555 1_555 1_555 no N3A Fe1 N5B 102.2(5) 1_555 1_555 1_555 no N5A Fe1 N1B 92.8(4) 1_555 1_555 1_555 no N5A Fe1 N3B 102.2(4) 1_555 1_555 1_555 no N5A Fe1 N5B 92.6(4) 1_555 1_555 1_555 no N1B Fe1 N3B 79.4(5) 1_555 1_555 1_555 no N1B Fe1 N5B 157.6(4) 1_555 1_555 1_555 no N3B Fe1 N5B 78.3(5) 1_555 1_555 1_555 no Fe1 N1A N2A 137.5(8) 1_555 1_555 1_555 no Fe1 N1A C3A 116.5(8) 1_555 1_555 1_555 no N2A N1A C3A 105.9(10) 1_555 1_555 1_555 no N1A N2A C1A 111.2(11) 1_555 1_555 1_555 no Fe1 N3A C4A 119.2(8) 1_555 1_555 1_555 no Fe1 N3A C8A 119.7(8) 1_555 1_555 1_555 no C4A N3A C8A 121.0(9) 1_555 1_555 1_555 no N5A N4A C11A 109.6(10) 1_555 1_555 1_555 no Fe1 N5A N4A 137.4(8) 1_555 1_555 1_555 no Fe1 N5A C9A 115.6(8) 1_555 1_555 1_555 no N4A N5A C9A 107.0(9) 1_555 1_555 1_555 no N2A C1A C2A 107.5(11) 1_555 1_555 1_555 no C1A C2A C3A 105.5(12) 1_555 1_555 1_555 no N1A C3A C2A 109.9(12) 1_555 1_555 1_555 no N1A C3A C4A 113.8(10) 1_555 1_555 1_555 no C2A C3A C4A 136.3(12) 1_555 1_555 1_555 no N3A C4A C3A 110.8(10) 1_555 1_555 1_555 no N3A C4A C5A 120.6(12) 1_555 1_555 1_555 no C3A C4A C5A 128.6(12) 1_555 1_555 1_555 no C4A C5A C6A 118.8(14) 1_555 1_555 1_555 no C5A C6A C7A 119.9(12) 1_555 1_555 1_555 no C6A C7A C8A 118.9(13) 1_555 1_555 1_555 no N3A C8A C7A 120.6(12) 1_555 1_555 1_555 no N3A C8A C9A 111.2(10) 1_555 1_555 1_555 no C7A C8A C9A 128.2(12) 1_555 1_555 1_555 no N5A C9A C8A 114.6(10) 1_555 1_555 1_555 no N5A C9A C10A 109.1(11) 1_555 1_555 1_555 no C8A C9A C10A 136.3(12) 1_555 1_555 1_555 no C9A C10A C11A 105.9(12) 1_555 1_555 1_555 no N4A C11A C10A 108.4(12) 1_555 1_555 1_555 no Fe1 N1B N2B 136.4(9) 1_555 1_555 1_555 no Fe1 N1B C3B 117.2(9) 1_555 1_555 1_555 no N2B N1B C3B 106.3(11) 1_555 1_555 1_555 no N1B N2B C1B 109.7(13) 1_555 1_555 1_555 no Fe1 N3B C4B 116.6(10) 1_555 1_555 1_555 no Fe1 N3B C8B 120.1(10) 1_555 1_555 1_555 no C4B N3B C8B 123.3(11) 1_555 1_555 1_555 no N5B N4B C11B 110.9(13) 1_555 1_555 1_555 no Fe1 N5B N4B 137.8(9) 1_555 1_555 1_555 no Fe1 N5B C9B 115.8(9) 1_555 1_555 1_555 no N4B N5B C9B 106.4(11) 1_555 1_555 1_555 no N2B C1B C2B 108.9(13) 1_555 1_555 1_555 no C1B C2B C3B 104.9(14) 1_555 1_555 1_555 no N1B C3B C2B 110.2(15) 1_555 1_555 1_555 no N1B C3B C4B 114.4(12) 1_555 1_555 1_555 no C2B C3B C4B 135.3(15) 1_555 1_555 1_555 no N3B C4B C3B 112.3(12) 1_555 1_555 1_555 no N3B C4B C5B 116.5(16) 1_555 1_555 1_555 no C3B C4B C5B 131.2(16) 1_555 1_555 1_555 no C4B C5B C6B 120.9(17) 1_555 1_555 1_555 no C5B C6B C7B 120.8(14) 1_555 1_555 1_555 no C6B C7B C8B 116.2(17) 1_555 1_555 1_555 no N3B C8B C7B 122.3(15) 1_555 1_555 1_555 no N3B C8B C9B 111.3(12) 1_555 1_555 1_555 no C7B C8B C9B 126.5(16) 1_555 1_555 1_555 no N5B C9B C8B 114.4(12) 1_555 1_555 1_555 no N5B C9B C10B 108.0(14) 1_555 1_555 1_555 no C8B C9B C10B 137.5(15) 1_555 1_555 1_555 no C9B C10B C11B 106.7(14) 1_555 1_555 1_555 no N4B C11B C10B 108.0(13) 1_555 1_555 1_555 no data_DHG74_[Fe(btp)2]Cl2.6H2O _database_code_depnum_ccdc_archive 'CCDC 281665' _audit_creation_method 'RAELSPUB and manual entry' # SUBMISSION DETAILS # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C18 H14 Fe N14 2+,2(Cl 1-),6(H2 O)' _chemical_formula_sum 'C18 H26 Cl2 Fe N14 O6' _chemical_formula_iupac ? _chemical_formula_weight 661.2 # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2-y,z 3 3/4-y,1/4+x,1/4+z 4 1/4+y,1/4-x,1/4+z 5 -x,-y,-z 6 x,1/2+y,-z 7 1/4+y,3/4-x,3/4-z 8 3/4-y,3/4+x,3/4-z 9 1/2+x,1/2+y,1/2+z 10 1/2-x,-y,1/2+z 11 1/4-y,3/4+x,3/4+z 12 3/4+y,3/4-x,3/4+z 13 1/2-x,1/2-y,1/2-z 14 1/2+x,y,1/2-z 15 3/4+y,1/4-x,1/4-z 16 1/4-y,1/4+x,1/4-z _cell_length_a 11.733(2) _cell_length_b 11.733(2) _cell_length_c 20.664(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2844.7(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.54 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360.0 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 1382 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 1251 _reflns_number_gt 927 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.071 _refine_ls_wR_factor_ref 0.105 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 927 _refine_ls_number_parameters 97 _refine_ls_goodness_of_fit_ref 1.70 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.62 _refine_diff_density_min -0.39 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe1 0.5000(0) 0.7500(0) 0.6250(0) 0.0630(6) Uani Fe 1.0 N1 0.3984(3) 0.5999(4) 0.5968(2) 0.065(1) Uani N 1.0 N2 0.2970(4) 0.4543(4) 0.5709(2) 0.078(1) Uani N 1.0 N3 0.3260(4) 0.4999(4) 0.5134(2) 0.077(1) Uani N 1.0 N4 0.5000(0) 0.7500(0) 0.5207(2) 0.059(1) Uani N 1.0 C1 0.3380(5) 0.5125(5) 0.6196(2) 0.075(2) Uani C 1.0 C2 0.3882(4) 0.5874(4) 0.5313(2) 0.061(1) Uani C 1.0 C3 0.4435(4) 0.6704(4) 0.4888(2) 0.063(1) Uani C 1.0 C4 0.4393(6) 0.6678(5) 0.4212(2) 0.081(2) Uani C 1.0 C5 0.5000(0) 0.7500(0) 0.3878(3) 0.091(3) Uani C 1.0 Cl1 0.1413(5) 0.2637(4) 0.5220(2) 0.194(2) Uani Cl 0.5 OW1 0.1726(13) 0.2538(11) 0.5787(5) 0.194(2) Uani O 0.5 OW2 0.0363(7) 0.0373(7) 0.5550(4) 0.359(9) Uani O 1.0 HN2 0.2496 0.3840 0.5757 0.078 Uani H 1.0 HC1 0.3260 0.4944 0.6664 0.075 Uani H 1.0 HC4 0.3938 0.6086 0.3978 0.081 Uani H 1.0 HC5 0.5000 0.7500 0.3394 0.091 Uani H 1.0 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 _atom_site_aniso_type_symbol Fe1 0.0749(8) 0.0749(8) 0.0394(8) 0.0000(0) 0.0000(0) 0.0000(0) Fe N1 0.075(3) 0.073(3) 0.048(2) 0.002(2) 0.001(2) -0.005(2) N N2 0.086(3) 0.078(3) 0.071(3) -0.011(2) 0.007(2) -0.005(2) N N3 0.093(3) 0.079(3) 0.060(3) -0.004(3) -0.003(2) -0.011(2) N N4 0.072(4) 0.060(3) 0.045(3) 0.010(3) 0.0000(0) 0.0000(0) N C1 0.088(4) 0.078(4) 0.060(3) -0.001(3) 0.011(3) -0.009(3) C C2 0.066(3) 0.067(3) 0.050(2) 0.009(2) -0.002(2) -0.002(2) C C3 0.074(3) 0.068(3) 0.047(2) 0.013(3) 0.000(2) -0.003(2) C C4 0.114(4) 0.083(4) 0.047(3) 0.007(3) -0.013(3) -0.007(3) C C5 0.147(8) 0.082(5) 0.043(4) 0.007(5) 0.0000(0) 0.0000(0) C Cl1 0.215(6) 0.193(5) 0.174(5) -0.024(5) -0.035(5) -0.018(5) Cl OW1 0.215(6) 0.193(5) 0.174(5) -0.024(5) -0.035(5) -0.018(5) O OW2 0.174(9) 0.325(9) 0.580(9) 0.057(9) -0.043(9) 0.058(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.205(4) 1_555 1_555 no Fe1 N1 2.205(4) 1_555 2_665 no Fe1 N1 2.205(4) 1_555 7_466 no Fe1 N1 2.205(4) 1_555 8_656 no Fe1 N4 2.154(5) 1_555 1_555 no Fe1 N4 2.154(5) 1_555 7_466 no N1 C1 1.332(7) 1_555 1_555 no N1 C2 1.366(6) 1_555 1_555 no N2 N3 1.345(5) 1_555 1_555 no N2 C1 1.308(6) 1_555 1_555 no N3 C2 1.312(6) 1_555 1_555 no N4 C3 1.322(5) 1_555 1_555 no N4 C3 1.322(5) 1_555 2_665 no C2 C3 1.464(7) 1_555 1_555 no C3 C4 1.397(6) 1_555 1_555 no C4 C5 1.384(7) 1_555 1_555 no C5 C4 1.384(7) 1_555 2_665 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 149.3(2) 1_555 1_555 2_665 no N1 Fe1 N1 94.01(5) 1_555 1_555 7_466 no N1 Fe1 N1 94.01(5) 1_555 1_555 8_656 no N1 Fe1 N4 74.7(1) 1_555 1_555 1_555 no N1 Fe1 N4 105.3(1) 1_555 1_555 7_466 no N1 Fe1 N1 94.01(5) 2_665 1_555 7_466 no N1 Fe1 N1 94.01(5) 2_665 1_555 8_656 no N1 Fe1 N4 74.7(1) 2_665 1_555 1_555 no N1 Fe1 N4 105.3(1) 2_665 1_555 7_466 no N1 Fe1 N1 149.3(2) 7_466 1_555 8_656 no N1 Fe1 N4 105.3(1) 7_466 1_555 1_555 no N1 Fe1 N4 74.7(1) 7_466 1_555 7_466 no N1 Fe1 N4 105.3(1) 8_656 1_555 1_555 no N1 Fe1 N4 74.7(1) 8_656 1_555 7_466 no N4 Fe1 N4 180.00(0) 1_555 1_555 7_466 no Fe1 N1 C1 143.9(3) 1_555 1_555 1_555 no Fe1 N1 C2 113.3(3) 1_555 1_555 1_555 no C1 N1 C2 102.8(4) 1_555 1_555 1_555 no N3 N2 C1 112.2(4) 1_555 1_555 1_555 no N2 N3 C2 101.7(4) 1_555 1_555 1_555 no Fe1 N4 C3 120.0(3) 1_555 1_555 1_555 no Fe1 N4 C3 120.0(3) 1_555 1_555 2_665 no C3 N4 C3 120.0(5) 1_555 1_555 2_665 no N1 C1 N2 109.0(4) 1_555 1_555 1_555 no N1 C2 N3 114.3(4) 1_555 1_555 1_555 no N1 C2 C3 119.0(4) 1_555 1_555 1_555 no N3 C2 C3 126.7(4) 1_555 1_555 1_555 no N4 C3 C2 113.1(4) 1_555 1_555 1_555 no N4 C3 C4 122.2(5) 1_555 1_555 1_555 no C2 C3 C4 124.7(5) 1_555 1_555 1_555 no C3 C4 C5 117.7(5) 1_555 1_555 1_555 no C4 C5 C4 120.1(6) 1_555 1_555 2_665 no data_DHG75_[Ru(bpp)2]Cl2.6.5H2O _database_code_depnum_ccdc_archive 'CCDC 281666' _audit_creation_method 'RAELSPUB and manual entry' # SUBMISSION DETAILS # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C22 H18 N10 Ru 2+,2(Cl 1-),6.5(H2 O)' _chemical_formula_sum 'C22 H31 Cl2 N10 O6.5 Ru' _chemical_formula_iupac ? _chemical_formula_weight 711.5 # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b a 2' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 1/2-x,1/2+y,z 4 1/2+x,1/2-y,z _cell_length_a 16.299(4) _cell_length_b 23.473(5) _cell_length_c 8.339(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3190(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.48 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452.0 _exptl_absorpt_coefficient_mu 0.704 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.94 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3010 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 3010 _reflns_number_gt 2280 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.067 _refine_ls_abs_structure_Flack 0.30(25) _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2280 _refine_ls_number_parameters 206 _refine_ls_goodness_of_fit_ref 1.95 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 0.93 _refine_diff_density_min -1.16 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description Cl/O 0.5Cl+0.5O loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Ru1 0.32603(4) 0.21415(3) 0.50000 0.0346(2) Uani Ru 1.0 N1A 0.4344(5) 0.2430(4) 0.5945(12) 0.045(2) Uani N 1.0 N2A 0.5028(6) 0.2194(5) 0.6583(12) 0.056(1) Uani N 1.0 N3A 0.3132(5) 0.2987(3) 0.4851(19) 0.049(2) Uani N 1.0 N4A 0.1482(6) 0.1890(5) 0.3543(13) 0.057(1) Uani N 1.0 N5A 0.2118(6) 0.2243(4) 0.4044(12) 0.044(1) Uani N 1.0 C1A 0.5546(8) 0.2634(8) 0.7078(21) 0.075(2) Uani C 1.0 C2A 0.5177(9) 0.3119(7) 0.6755(20) 0.080(2) Uani C 1.0 C3A 0.4434(8) 0.3001(6) 0.6027(18) 0.059(2) Uani C 1.0 C4A 0.3763(8) 0.3323(5) 0.5411(17) 0.064(2) Uani C 1.0 C5A 0.3699(10) 0.3909(5) 0.5286(27) 0.095(3) Uani C 1.0 C6A 0.3019(11) 0.4148(6) 0.4605(29) 0.110(5) Uani C 1.0 C7A 0.2369(11) 0.3781(6) 0.4077(23) 0.089(4) Uani C 1.0 C8A 0.2471(8) 0.3204(5) 0.4225(18) 0.059(2) Uani C 1.0 C9A 0.1877(7) 0.2778(6) 0.3745(16) 0.054(2) Uani C 1.0 C10A 0.1103(8) 0.2766(7) 0.3063(18) 0.071(3) Uani C 1.0 C11A 0.0874(8) 0.2230(8) 0.2943(19) 0.071(2) Uani C 1.0 N1B 0.3791(6) 0.1967(5) 0.2842(12) 0.050(1) Uani N 1.0 N2B 0.4032(6) 0.2244(6) 0.1536(14) 0.076(1) Uani N 1.0 N3B 0.3423(5) 0.1291(3) 0.5192(16) 0.050(1) Uani N 1.0 N4B 0.2496(7) 0.2220(6) 0.8504(13) 0.076(1) Uani N 1.0 N5B 0.2803(6) 0.1948(5) 0.7253(12) 0.051(1) Uani N 1.0 C1B 0.4354(10) 0.1875(10) 0.0480(16) 0.110(2) Uani C 1.0 C2B 0.4386(9) 0.1353(10) 0.1083(22) 0.109(2) Uani C 1.0 C3B 0.3977(8) 0.1411(7) 0.2638(18) 0.068(2) Uani C 1.0 C4B 0.3795(8) 0.1021(6) 0.3908(21) 0.069(2) Uani C 1.0 C5B 0.3933(11) 0.0453(7) 0.4008(29) 0.109(5) Uani C 1.0 C6B 0.3689(12) 0.0171(6) 0.5442(34) 0.128(6) Uani C 1.0 C7B 0.3312(12) 0.0433(7) 0.6618(30) 0.110(5) Uani C 1.0 C8B 0.3181(8) 0.1018(6) 0.6487(21) 0.069(2) Uani C 1.0 C9B 0.2827(8) 0.1388(7) 0.7611(18) 0.069(2) Uani C 1.0 C10B 0.2445(10) 0.1358(9) 0.9220(21) 0.109(3) Uani C 1.0 C11B 0.2267(10) 0.1885(11) 0.9662(17) 0.111(2) Uani C 1.0 Cl1 0.5000 0.0000 0.9187(9) 0.093(2) Uani Cl 1.0 Cl2 0.7140(4) 0.1485(3) 0.8746(8) 0.139(2) Uani Cl 1.0 Cl/OW 0.0681(9) 0.0329(5) 0.7002(28) 0.312(9) Uani Cl/O 1.0 OW1 0.5492(6) 0.1089(4) 0.7048(13) 0.079(3) Uani O 1.0 OW2 0.1366(9) 0.0708(5) 0.3881(23) 0.148(6) Uani O 1.0 OW3 0.3777(8) 0.3341(6) 0.0927(19) 0.148(6) Uani O 1.0 OW4 0.6462(9) 0.0524(6) 1.1005(18) 0.166(7) Uani O 1.0 OW5 0.1999(16) -0.0003(12) 0.1129(41) 0.385(9) Uani O 1.0 OW6 0.4958(13) 0.4179(10) 0.0422(51) 0.350(9) Uani O 1.0 HN2A 0.5142 0.1777 0.6682 0.060 Uani H 1.0 HN4A 0.1472 0.1465 0.3611 0.065 Uani H 1.0 HC1A 0.6098 0.2589 0.7587 0.093 Uani H 1.0 HC2A 0.5397 0.3508 0.6994 0.104 Uani H 1.0 HC5A 0.4150 0.4158 0.5695 0.118 Uani H 1.0 HC6A 0.2976 0.4570 0.4477 0.144 Uani H 1.0 HC7A 0.1853 0.3943 0.3613 0.105 Uani H 1.0 HC10A 0.0775 0.3105 0.2720 0.089 Uani H 1.0 HC11A 0.0341 0.2093 0.2487 0.090 Uani H 1.0 HN2B 0.3982 0.2664 0.1366 0.085 Uani H 1.0 HN4B 0.2445 0.2645 0.8555 0.084 Uani H 1.0 HC1B 0.4544 0.1980 -0.0621 0.148 Uani H 1.0 HC2B 0.4631 0.1004 0.0593 0.144 Uani H 1.0 HC5B 0.4197 0.0240 0.3106 0.140 Uani H 1.0 HC6B 0.3812 -0.0244 0.5557 0.173 Uani H 1.0 HC7B 0.3122 0.0218 0.7585 0.142 Uani H 1.0 HC10B 0.2340 0.1005 0.9857 0.146 Uani H 1.0 HC11B 0.2006 0.2003 1.0694 0.150 Uani H 1.0 H1OW1 0.5304 0.0747 0.7662 0.079 Uani H 1.0 H2OW1 0.6013 0.1236 0.7525 0.079 Uani H 1.0 H1OW2 0.1152 0.0513 0.4863 0.148 Uani H 1.0 H2OW2 0.1551 0.0416 0.3087 0.148 Uani H 1.0 H1OW3 0.3282 0.3406 0.0241 0.148 Uani H 1.0 H2OW3 0.4189 0.3647 0.0720 0.148 Uani H 1.0 H1OW4 0.5984 0.0344 1.0448 0.166 Uani H 1.0 H2OW4 0.6694 0.0834 1.0315 0.166 Uani H 1.0 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 _atom_site_aniso_type_symbol Ru1 0.0340(4) 0.0431(4) 0.0267(4) 0.0038(4) 0.0011(7) 0.0012(9) Ru N1A 0.039(2) 0.061(2) 0.034(3) 0.001(2) 0.003(2) 0.001(2) N N2A 0.039(2) 0.088(3) 0.040(2) 0.005(2) -0.001(2) 0.001(2) N N3A 0.053(2) 0.045(3) 0.048(3) 0.007(2) 0.004(2) 0.006(3) N N4A 0.040(2) 0.087(3) 0.044(2) -0.001(2) -0.001(2) -0.002(2) N N5A 0.038(2) 0.063(2) 0.031(3) 0.007(2) 0.003(2) 0.004(2) N C1A 0.047(2) 0.117(4) 0.062(4) -0.011(3) -0.007(3) -0.010(4) C C2A 0.062(3) 0.096(3) 0.081(6) -0.023(3) -0.006(3) -0.016(4) C C3A 0.055(2) 0.064(2) 0.059(4) -0.010(2) 0.000(2) -0.005(3) C C4A 0.069(3) 0.049(2) 0.073(4) -0.004(2) 0.002(3) -0.001(3) C C5A 0.109(5) 0.048(2) 0.129(8) -0.007(2) -0.001(5) -0.001(3) C C6A 0.131(7) 0.046(3) 0.152(9) 0.012(2) -0.002(7) 0.013(3) C C7A 0.100(5) 0.057(2) 0.108(7) 0.028(2) 0.000(5) 0.019(3) C C8A 0.063(3) 0.054(2) 0.060(4) 0.018(2) 0.003(3) 0.012(3) C C9A 0.048(2) 0.072(2) 0.043(3) 0.020(2) 0.001(2) 0.011(2) C C10A 0.050(2) 0.109(4) 0.053(5) 0.028(3) -0.004(3) 0.013(4) C C11A 0.041(2) 0.122(5) 0.051(4) 0.010(2) -0.006(2) 0.002(4) C N1B 0.035(2) 0.084(2) 0.031(2) 0.004(2) -0.003(2) -0.009(2) N N2B 0.046(2) 0.150(4) 0.032(2) -0.006(3) 0.002(2) 0.005(3) N N3B 0.046(3) 0.040(3) 0.063(2) 0.001(2) -0.023(2) -0.001(2) N N4B 0.045(2) 0.151(4) 0.032(2) 0.002(3) 0.002(2) -0.008(2) N N5B 0.036(2) 0.085(2) 0.031(2) -0.006(2) -0.004(2) 0.007(2) N C1B 0.058(4) 0.234(8) 0.038(2) 0.012(6) 0.007(3) -0.028(3) C C2B 0.063(4) 0.198(6) 0.065(3) 0.038(5) -0.008(3) -0.069(4) C C3B 0.047(3) 0.099(3) 0.057(2) 0.022(3) -0.014(2) -0.039(3) C C4B 0.060(3) 0.057(3) 0.090(4) 0.020(3) -0.033(3) -0.032(3) C C5B 0.100(6) 0.059(3) 0.167(8) 0.034(3) -0.070(6) -0.048(3) C C6B 0.128(9) 0.041(3) 0.215(9) 0.008(3) -0.097(8) 0.000(3) C C7B 0.109(7) 0.055(3) 0.167(8) -0.021(3) -0.074(6) 0.044(3) C C8B 0.065(4) 0.055(3) 0.088(3) -0.015(2) -0.035(3) 0.029(3) C C9B 0.054(3) 0.096(3) 0.056(2) -0.023(3) -0.016(2) 0.037(3) C C10B 0.073(5) 0.194(6) 0.060(3) -0.041(5) -0.010(3) 0.064(4) C C11B 0.063(4) 0.235(8) 0.037(2) -0.018(6) 0.006(2) 0.022(3) C Cl1 0.098(4) 0.086(4) 0.095(4) -0.015(3) 0.0000 0.0000 Cl Cl2 0.128(4) 0.159(5) 0.130(5) -0.057(4) -0.032(4) 0.058(5) Cl Cl/OW 0.257(9) 0.169(9) 0.512(9) 0.071(9) 0.071(9) 0.051(9) Cl/O OW1 0.090(7) 0.060(6) 0.086(8) 0.001(5) -0.004(7) 0.010(6) O OW2 0.170(9) 0.069(8) 0.205(9) 0.031(8) -0.008(9) -0.025(9) O OW3 0.118(9) 0.179(9) 0.146(9) -0.025(9) -0.042(9) 0.070(9) O OW4 0.194(9) 0.175(9) 0.130(9) -0.094(9) -0.096(9) 0.073(9) O OW5 0.373(9) 0.333(9) 0.449(9) 0.261(9) 0.260(9) 0.266(9) O OW6 0.257(9) 0.290(9) 0.502(9) -0.135(9) -0.022(9) 0.058(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1A 2.048(9) 1_555 1_555 no Ru1 N3A 1.999(7) 1_555 1_555 no Ru1 N5A 2.040(9) 1_555 1_555 no Ru1 N1B 2.039(10) 1_555 1_555 no Ru1 N3B 2.020(8) 1_555 1_555 no Ru1 N5B 2.072(10) 1_555 1_555 no N1A N2A 1.354(12) 1_555 1_555 no N1A C3A 1.349(14) 1_555 1_555 no N2A C1A 1.397(16) 1_555 1_555 no N3A C4A 1.377(15) 1_555 1_555 no N3A C8A 1.301(14) 1_555 1_555 no N4A N5A 1.391(13) 1_555 1_555 no N4A C11A 1.367(16) 1_555 1_555 no N5A C9A 1.340(14) 1_555 1_555 no C1A C2A 1.315(21) 1_555 1_555 no C2A C3A 1.383(18) 1_555 1_555 no C3A C4A 1.426(17) 1_555 1_555 no C4A C5A 1.384(16) 1_555 1_555 no C5A C6A 1.365(22) 1_555 1_555 no C6A C7A 1.434(22) 1_555 1_555 no C7A C8A 1.371(17) 1_555 1_555 no C8A C9A 1.447(18) 1_555 1_555 no C9A C10A 1.384(17) 1_555 1_555 no C10A C11A 1.318(20) 1_555 1_555 no N1B N2B 1.328(15) 1_555 1_555 no N1B C3B 1.350(16) 1_555 1_555 no N2B C1B 1.341(20) 1_555 1_555 no N3B C4B 1.384(18) 1_555 1_555 no N3B C8B 1.317(18) 1_555 1_555 no N4B N5B 1.322(15) 1_555 1_555 no N4B C11B 1.300(21) 1_555 1_555 no N5B C9B 1.348(17) 1_555 1_555 no C1B C2B 1.325(27) 1_555 1_555 no C2B C3B 1.464(22) 1_555 1_555 no C3B C4B 1.431(21) 1_555 1_555 no C4B C5B 1.355(18) 1_555 1_555 no C5B C6B 1.424(30) 1_555 1_555 no C6B C7B 1.310(32) 1_555 1_555 no C7B C8B 1.393(19) 1_555 1_555 no C8B C9B 1.403(21) 1_555 1_555 no C9B C10B 1.481(22) 1_555 1_555 no C10B C11B 1.321(25) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Ru1 N3A 77.6(4) 1_555 1_555 1_555 no N1A Ru1 N5A 154.0(4) 1_555 1_555 1_555 no N1A Ru1 N1B 92.3(4) 1_555 1_555 1_555 no N1A Ru1 N3B 100.5(4) 1_555 1_555 1_555 no N1A Ru1 N5B 91.9(4) 1_555 1_555 1_555 no N3A Ru1 N5A 76.4(4) 1_555 1_555 1_555 no N3A Ru1 N1B 100.9(5) 1_555 1_555 1_555 no N3A Ru1 N3B 178.2(4) 1_555 1_555 1_555 no N3A Ru1 N5B 103.7(5) 1_555 1_555 1_555 no N5A Ru1 N1B 93.8(4) 1_555 1_555 1_555 no N5A Ru1 N3B 105.4(4) 1_555 1_555 1_555 no N5A Ru1 N5B 93.0(4) 1_555 1_555 1_555 no N1B Ru1 N3B 79.4(5) 1_555 1_555 1_555 no N1B Ru1 N5B 155.4(4) 1_555 1_555 1_555 no N3B Ru1 N5B 76.0(5) 1_555 1_555 1_555 no Ru1 N1A N2A 136.5(8) 1_555 1_555 1_555 no Ru1 N1A C3A 116.2(8) 1_555 1_555 1_555 no N2A N1A C3A 107.2(10) 1_555 1_555 1_555 no N1A N2A C1A 108.1(11) 1_555 1_555 1_555 no Ru1 N3A C4A 118.0(8) 1_555 1_555 1_555 no Ru1 N3A C8A 120.0(9) 1_555 1_555 1_555 no C4A N3A C8A 122.1(10) 1_555 1_555 1_555 no N5A N4A C11A 107.6(11) 1_555 1_555 1_555 no Ru1 N5A N4A 136.7(8) 1_555 1_555 1_555 no Ru1 N5A C9A 116.7(8) 1_555 1_555 1_555 no N4A N5A C9A 106.6(10) 1_555 1_555 1_555 no N2A C1A C2A 107.7(12) 1_555 1_555 1_555 no C1A C2A C3A 108.4(14) 1_555 1_555 1_555 no N1A C3A C2A 108.5(12) 1_555 1_555 1_555 no N1A C3A C4A 115.1(11) 1_555 1_555 1_555 no C2A C3A C4A 136.3(13) 1_555 1_555 1_555 no N3A C4A C3A 113.1(10) 1_555 1_555 1_555 no N3A C4A C5A 119.1(13) 1_555 1_555 1_555 no C3A C4A C5A 127.8(13) 1_555 1_555 1_555 no C4A C5A C6A 120.1(14) 1_555 1_555 1_555 no C5A C6A C7A 118.8(12) 1_555 1_555 1_555 no C6A C7A C8A 118.4(14) 1_555 1_555 1_555 no N3A C8A C7A 121.5(14) 1_555 1_555 1_555 no N3A C8A C9A 113.3(11) 1_555 1_555 1_555 no C7A C8A C9A 125.2(13) 1_555 1_555 1_555 no N5A C9A C8A 113.5(11) 1_555 1_555 1_555 no N5A C9A C10A 108.9(13) 1_555 1_555 1_555 no C8A C9A C10A 137.5(13) 1_555 1_555 1_555 no C9A C10A C11A 108.1(13) 1_555 1_555 1_555 no N4A C11A C10A 108.9(12) 1_555 1_555 1_555 no Ru1 N1B N2B 138.7(10) 1_555 1_555 1_555 no Ru1 N1B C3B 113.6(10) 1_555 1_555 1_555 no N2B N1B C3B 107.7(12) 1_555 1_555 1_555 no N1B N2B C1B 109.8(14) 1_555 1_555 1_555 no Ru1 N3B C4B 116.7(10) 1_555 1_555 1_555 no Ru1 N3B C8B 120.5(10) 1_555 1_555 1_555 no C4B N3B C8B 122.8(11) 1_555 1_555 1_555 no N5B N4B C11B 113.6(15) 1_555 1_555 1_555 no Ru1 N5B N4B 138.1(10) 1_555 1_555 1_555 no Ru1 N5B C9B 113.8(10) 1_555 1_555 1_555 no N4B N5B C9B 108.0(12) 1_555 1_555 1_555 no N2B C1B C2B 111.2(14) 1_555 1_555 1_555 no C1B C2B C3B 103.5(14) 1_555 1_555 1_555 no N1B C3B C2B 107.6(16) 1_555 1_555 1_555 no N1B C3B C4B 118.6(12) 1_555 1_555 1_555 no C2B C3B C4B 133.7(16) 1_555 1_555 1_555 no N3B C4B C3B 111.8(11) 1_555 1_555 1_555 no N3B C4B C5B 118.4(17) 1_555 1_555 1_555 no C3B C4B C5B 129.8(17) 1_555 1_555 1_555 no C4B C5B C6B 117.6(19) 1_555 1_555 1_555 no C5B C6B C7B 122.8(15) 1_555 1_555 1_555 no C6B C7B C8B 118.4(21) 1_555 1_555 1_555 no N3B C8B C7B 119.9(18) 1_555 1_555 1_555 no N3B C8B C9B 111.6(12) 1_555 1_555 1_555 no C7B C8B C9B 128.4(18) 1_555 1_555 1_555 no N5B C9B C8B 117.9(13) 1_555 1_555 1_555 no N5B C9B C10B 103.5(16) 1_555 1_555 1_555 no C8B C9B C10B 138.5(17) 1_555 1_555 1_555 no C9B C10B C11B 107.5(15) 1_555 1_555 1_555 no N4B C11B C10B 107.3(14) 1_555 1_555 1_555 no data_DHG78_[Ru(terpy)2]Cl2.6H2O _database_code_depnum_ccdc_archive 'CCDC 281667' _audit_creation_method 'RAELSPUB and manual entry' # SUBMISSION DETAILS # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C30 H22 N6 Ru 2+,2(Cl 1-),6(H2 O)' _chemical_formula_sum 'C30 H34 Cl2 N6 O6 Ru' _chemical_formula_iupac ? _chemical_formula_weight 746.6 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 8.836(3) _cell_length_b 20.969(4) _cell_length_c 17.825(4) _cell_angle_alpha 90 _cell_angle_beta 91.26(2) _cell_angle_gamma 90 _cell_volume 3302(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.50 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528.0 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.95 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5999 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5801 _reflns_number_gt 3952 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_ref 0.069 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3952 _refine_ls_number_parameters 214 _refine_ls_goodness_of_fit_ref 1.87 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.009 _refine_diff_density_max 1.08 _refine_diff_density_min -1.05 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description Cl/O1 0.50Cl+0.50O Cl/O2 0.33Cl+0.67O Cl/O3 0.34Cl+0.66O Cl/O4 0.22Cl+0.78O Cl/O5 0.11Cl+0.89O Cl/O6 0.26Cl+0.74O Cl/O7 0.24Cl+0.76O loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Ru1 0.36053(6) 0.22815(3) 0.42920(3) 0.0366(2) Uani Ru 1.0 N1A 0.1470(6) 0.2116(3) 0.3843(3) 0.0431(8) Uani N 1.0 N2A 0.3683(6) 0.1353(3) 0.4140(3) 0.0417(8) Uani N 1.0 N3A 0.5751(6) 0.2070(3) 0.4714(3) 0.0428(8) Uani N 1.0 C1A 0.0357(7) 0.2545(3) 0.3708(4) 0.0502(8) Uani C 1.0 C2A -0.1029(8) 0.2361(4) 0.3384(4) 0.064(1) Uani C 1.0 C3A -0.1268(8) 0.1746(4) 0.3200(4) 0.071(2) Uani C 1.0 C4A -0.0160(8) 0.1298(4) 0.3329(4) 0.063(1) Uani C 1.0 C5A 0.1210(7) 0.1497(3) 0.3658(4) 0.0491(8) Uani C 1.0 C6A 0.2471(8) 0.1058(3) 0.3814(4) 0.0482(8) Uani C 1.0 C7A 0.2557(9) 0.0405(4) 0.3664(4) 0.060(1) Uani C 1.0 C8A 0.3827(9) 0.0071(4) 0.3846(4) 0.065(1) Uani C 1.0 C9A 0.5047(9) 0.0380(3) 0.4171(4) 0.059(1) Uani C 1.0 C10A 0.4953(8) 0.1023(3) 0.4323(4) 0.0472(8) Uani C 1.0 C11A 0.6105(7) 0.1435(3) 0.4676(4) 0.0477(8) Uani C 1.0 C12A 0.7483(8) 0.1202(4) 0.4948(4) 0.061(1) Uani C 1.0 C13A 0.8493(8) 0.1626(4) 0.5283(4) 0.069(2) Uani C 1.0 C14A 0.8126(8) 0.2265(4) 0.5335(4) 0.064(1) Uani C 1.0 C15A 0.6747(7) 0.2472(4) 0.5031(4) 0.0506(8) Uani C 1.0 N1B 0.2765(5) 0.2366(3) 0.5365(3) 0.0421(9) Uani N 1.0 N2B 0.3548(6) 0.3226(3) 0.4416(3) 0.0509(9) Uani N 1.0 N3B 0.4457(6) 0.2570(3) 0.3275(3) 0.0431(9) Uani N 1.0 C1B 0.2395(7) 0.1892(4) 0.5825(4) 0.0507(8) Uani C 1.0 C2B 0.1777(8) 0.2009(4) 0.6523(4) 0.063(1) Uani C 1.0 C3B 0.1553(9) 0.2637(5) 0.6737(4) 0.068(2) Uani C 1.0 C4B 0.1944(9) 0.3129(4) 0.6275(4) 0.067(2) Uani C 1.0 C5B 0.2538(8) 0.2981(4) 0.5585(4) 0.052(1) Uani C 1.0 C6B 0.3004(9) 0.3469(4) 0.5049(4) 0.062(1) Uani C 1.0 C7B 0.2958(12) 0.4119(4) 0.5122(5) 0.094(2) Uani C 1.0 C8B 0.3435(14) 0.4508(4) 0.4569(6) 0.117(3) Uani C 1.0 C9B 0.3978(13) 0.4244(4) 0.3903(5) 0.100(3) Uani C 1.0 C10B 0.4027(9) 0.3590(4) 0.3841(4) 0.066(1) Uani C 1.0 C11B 0.4579(8) 0.3220(3) 0.3208(4) 0.057(1) Uani C 1.0 C12B 0.5212(10) 0.3501(4) 0.2586(4) 0.077(2) Uani C 1.0 C13B 0.5726(10) 0.3097(5) 0.2010(4) 0.076(2) Uani C 1.0 C14B 0.5572(8) 0.2453(4) 0.2077(4) 0.063(1) Uani C 1.0 C15B 0.4928(7) 0.2211(4) 0.2715(3) 0.0490(8) Uani C 1.0 Cl/OW1 0.1114(4) 0.4648(2) 0.0607(2) 0.109(1) Uani Cl/O1 1.0 Cl/OW2 0.2117(8) 0.0217(3) 0.7127(4) 0.185(3) Uani Cl/O2 1.0 Cl/OW3 0.5539(10) 0.0704(3) 0.2162(4) 0.227(4) Uani Cl/O3 1.0 Cl/OW4 0.7548(12) 0.1164(3) 0.0966(4) 0.212(4) Uani Cl/O4 1.0 Cl/OW5 0.2705(12) 0.0008(5) 0.1846(4) 0.199(4) Uani Cl/O5 1.0 Cl/OW6 0.1768(15) 0.8939(6) 0.0714(7) 0.343(7) Uani Cl/O6 1.0 Cl/OW7 -0.0090(14) 0.0339(7) 0.1594(8) 0.374(7) Uani Cl/O7 1.0 OW 0.0988(15) 0.9008(5) 0.2764(10) 0.344(9) Uani O 1.0 HC1A 0.0528 0.3002 0.3842 0.050 Uani H 1.0 HC2A -0.1841 0.2685 0.3289 0.075 Uani H 1.0 HC3A -0.2261 0.1614 0.2968 0.087 Uani H 1.0 HC4A -0.0328 0.0841 0.3190 0.073 Uani H 1.0 HC7A 0.1675 0.0182 0.3419 0.071 Uani H 1.0 HC8A 0.3875 -0.0398 0.3746 0.078 Uani H 1.0 HC9A 0.5998 0.0140 0.4295 0.067 Uani H 1.0 HC12A 0.7741 0.0739 0.4902 0.069 Uani H 1.0 HC13A 0.9488 0.1469 0.5488 0.084 Uani H 1.0 HC14A 0.8837 0.2573 0.5587 0.076 Uani H 1.0 HC15A 0.6494 0.2937 0.5051 0.052 Uani H 1.0 HC1B 0.2566 0.1441 0.5665 0.058 Uani H 1.0 HC2B 0.1501 0.1650 0.6862 0.077 Uani H 1.0 HC3B 0.1102 0.2732 0.7234 0.083 Uani H 1.0 HC4B 0.1803 0.3582 0.6432 0.086 Uani H 1.0 HC7B 0.2564 0.4310 0.5594 0.111 Uani H 1.0 HC8B 0.3400 0.4981 0.4635 0.155 Uani H 1.0 HC9B 0.4320 0.4524 0.3485 0.123 Uani H 1.0 HC12B 0.5304 0.3975 0.2546 0.101 Uani H 1.0 HC13B 0.6201 0.3283 0.1556 0.094 Uani H 1.0 HC14B 0.5919 0.2161 0.1672 0.072 Uani H 1.0 HC15B 0.4809 0.1738 0.2757 0.052 Uani H 1.0 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 _atom_site_aniso_type_symbol Ru1 0.0359(3) 0.0410(3) 0.0332(3) 0.0044(3) 0.0015(2) 0.0007(3) Ru N1A 0.038(1) 0.056(1) 0.035(1) 0.0003(9) 0.0032(9) 0.0009(9) N N2A 0.046(1) 0.046(1) 0.034(1) 0.0021(9) 0.0074(8) 0.001(1) N N3A 0.038(1) 0.056(1) 0.035(1) 0.0038(8) 0.0037(9) 0.0024(9) N C1A 0.039(1) 0.068(1) 0.044(1) 0.0055(9) 0.0010(9) 0.003(1) C C2A 0.042(1) 0.091(2) 0.060(2) 0.003(1) -0.006(1) 0.003(2) C C3A 0.047(1) 0.097(2) 0.068(2) -0.010(1) -0.010(1) -0.003(2) C C4A 0.053(1) 0.078(2) 0.059(2) -0.014(1) -0.005(1) -0.006(2) C C5A 0.046(1) 0.059(1) 0.043(1) -0.006(1) 0.0017(9) -0.003(1) C C6A 0.053(1) 0.050(1) 0.041(1) -0.0044(9) 0.006(1) -0.003(1) C C7A 0.075(2) 0.050(1) 0.056(2) -0.007(1) 0.008(2) -0.007(1) C C8A 0.087(3) 0.047(1) 0.062(3) 0.003(1) 0.013(2) -0.004(1) C C9A 0.073(2) 0.049(1) 0.054(2) 0.013(1) 0.013(2) 0.002(1) C C10A 0.052(1) 0.049(1) 0.040(1) 0.0089(9) 0.0089(9) 0.003(1) C C11A 0.044(1) 0.058(1) 0.041(1) 0.011(1) 0.0052(9) 0.005(1) C C12A 0.050(1) 0.076(1) 0.056(2) 0.020(1) 0.002(1) 0.009(2) C C13A 0.046(1) 0.096(2) 0.065(2) 0.015(1) -0.006(1) 0.008(2) C C14A 0.043(1) 0.091(2) 0.059(2) 0.002(1) -0.008(1) 0.002(2) C C15A 0.041(1) 0.068(1) 0.044(1) -0.0008(9) -0.0009(9) 0.0004(9) C N1B 0.038(2) 0.054(1) 0.035(1) 0.007(1) -0.002(1) 0.0004(9) N N2B 0.065(2) 0.043(1) 0.045(1) 0.009(1) 0.002(1) 0.0009(9) N N3B 0.041(2) 0.053(1) 0.035(1) 0.004(1) -0.002(1) 0.0035(9) N C1B 0.050(1) 0.065(1) 0.037(1) 0.000(1) 0.001(1) 0.0052(9) C C2B 0.060(2) 0.091(2) 0.038(1) -0.004(2) 0.005(1) 0.003(1) C C3B 0.063(2) 0.102(2) 0.042(1) 0.005(2) 0.009(1) -0.009(1) C C4B 0.073(3) 0.082(2) 0.048(1) 0.015(2) 0.010(1) -0.014(1) C C5B 0.056(2) 0.059(1) 0.042(1) 0.013(1) 0.003(1) -0.007(1) C C6B 0.085(2) 0.048(1) 0.053(1) 0.014(1) 0.007(1) -0.006(1) C C7B 0.157(4) 0.049(1) 0.078(2) 0.018(2) 0.021(3) -0.011(1) C C8B 0.215(6) 0.043(1) 0.095(3) 0.011(1) 0.030(4) -0.003(1) C C9B 0.177(5) 0.044(1) 0.080(3) 0.001(1) 0.021(3) 0.008(1) C C10B 0.098(2) 0.045(1) 0.054(1) 0.003(1) 0.007(1) 0.0064(9) C C11B 0.073(2) 0.055(1) 0.044(1) -0.002(1) 0.003(1) 0.009(1) C C12B 0.106(3) 0.074(1) 0.052(2) -0.016(2) 0.010(2) 0.015(1) C C13B 0.086(3) 0.097(2) 0.045(1) -0.018(2) 0.010(2) 0.012(2) C C14B 0.057(2) 0.093(2) 0.038(1) -0.003(2) 0.006(1) 0.001(1) C C15B 0.044(1) 0.067(1) 0.036(1) 0.005(1) 0.001(1) -0.0008(9) C Cl/OW1 0.090(3) 0.070(2) 0.165(4) -0.017(2) -0.030(3) 0.021(2) Cl/O1 Cl/OW2 0.267(7) 0.148(6) 0.141(5) -0.045(5) 0.049(5) -0.019(4) Cl/O2 Cl/OW3 0.381(9) 0.117(5) 0.186(7) -0.001(6) 0.070(7) -0.048(5) Cl/O3 Cl/OW4 0.401(9) 0.088(5) 0.148(6) -0.018(6) 0.014(7) 0.018(4) Cl/O4 Cl/OW5 0.296(9) 0.219(9) 0.083(5) -0.014(8) 0.009(6) 0.027(5) Cl/O5 Cl/OW6 0.497(9) 0.190(9) 0.343(9) -0.024(9) 0.076(9) -0.027(9) Cl/O6 Cl/OW7 0.315(9) 0.427(9) 0.384(9) -0.090(9) 0.070(9) -0.033(9) Cl/O7 OW 0.310(9) 0.136(9) 0.599(9) -0.033(9) 0.281(9) -0.001(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1A 2.063(5) 1_555 1_555 no Ru1 N2A 1.968(5) 1_555 1_555 no Ru1 N3A 2.072(5) 1_555 1_555 no Ru1 N1B 2.074(5) 1_555 1_555 no Ru1 N2B 1.993(5) 1_555 1_555 no Ru1 N3B 2.068(5) 1_555 1_555 no N1A C1A 1.350(8) 1_555 1_555 no N1A C5A 1.357(8) 1_555 1_555 no N2A C6A 1.356(7) 1_555 1_555 no N2A C10A 1.351(8) 1_555 1_555 no N3A C11A 1.369(8) 1_555 1_555 no N3A C15A 1.337(8) 1_555 1_555 no C1A C2A 1.396(9) 1_555 1_555 no C2A C3A 1.346(11) 1_555 1_555 no C3A C4A 1.372(10) 1_555 1_555 no C4A C5A 1.397(9) 1_555 1_555 no C5A C6A 1.468(9) 1_555 1_555 no C6A C7A 1.398(9) 1_555 1_555 no C7A C8A 1.357(10) 1_555 1_555 no C8A C9A 1.375(10) 1_555 1_555 no C9A C10A 1.378(9) 1_555 1_555 no C10A C11A 1.466(9) 1_555 1_555 no C11A C12A 1.390(9) 1_555 1_555 no C12A C13A 1.385(10) 1_555 1_555 no C13A C14A 1.384(10) 1_555 1_555 no C14A C15A 1.391(9) 1_555 1_555 no N1B C1B 1.336(8) 1_555 1_555 no N1B C5B 1.364(8) 1_555 1_555 no N2B C6B 1.338(8) 1_555 1_555 no N2B C10B 1.354(8) 1_555 1_555 no N3B C11B 1.371(8) 1_555 1_555 no N3B C15B 1.325(8) 1_555 1_555 no C1B C2B 1.391(9) 1_555 1_555 no C2B C3B 1.385(11) 1_555 1_555 no C3B C4B 1.369(11) 1_555 1_555 no C4B C5B 1.383(9) 1_555 1_555 no C5B C6B 1.464(10) 1_555 1_555 no C6B C7B 1.370(10) 1_555 1_555 no C7B C8B 1.353(12) 1_555 1_555 no C8B C9B 1.405(12) 1_555 1_555 no C9B C10B 1.377(11) 1_555 1_555 no C10B C11B 1.462(10) 1_555 1_555 no C11B C12B 1.383(9) 1_555 1_555 no C12B C13B 1.413(11) 1_555 1_555 no C13B C14B 1.363(11) 1_555 1_555 no C14B C15B 1.379(9) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Ru1 N2A 79.3(2) 1_555 1_555 1_555 no N1A Ru1 N3A 157.9(2) 1_555 1_555 1_555 no N1A Ru1 N1B 91.7(2) 1_555 1_555 1_555 no N1A Ru1 N2B 100.7(2) 1_555 1_555 1_555 no N1A Ru1 N3B 93.3(2) 1_555 1_555 1_555 no N2A Ru1 N3A 78.7(2) 1_555 1_555 1_555 no N2A Ru1 N1B 103.1(2) 1_555 1_555 1_555 no N2A Ru1 N2B 178.4(2) 1_555 1_555 1_555 no N2A Ru1 N3B 98.9(2) 1_555 1_555 1_555 no N3A Ru1 N1B 91.6(2) 1_555 1_555 1_555 no N3A Ru1 N2B 101.4(2) 1_555 1_555 1_555 no N3A Ru1 N3B 91.9(2) 1_555 1_555 1_555 no N1B Ru1 N2B 78.6(2) 1_555 1_555 1_555 no N1B Ru1 N3B 158.0(2) 1_555 1_555 1_555 no N2B Ru1 N3B 79.4(2) 1_555 1_555 1_555 no Ru1 N1A C1A 127.9(5) 1_555 1_555 1_555 no Ru1 N1A C5A 113.8(4) 1_555 1_555 1_555 no C1A N1A C5A 118.3(6) 1_555 1_555 1_555 no Ru1 N2A C6A 118.7(4) 1_555 1_555 1_555 no Ru1 N2A C10A 120.3(4) 1_555 1_555 1_555 no C6A N2A C10A 120.9(6) 1_555 1_555 1_555 no Ru1 N3A C11A 113.5(4) 1_555 1_555 1_555 no Ru1 N3A C15A 127.4(5) 1_555 1_555 1_555 no C11A N3A C15A 119.1(6) 1_555 1_555 1_555 no N1A C1A C2A 121.3(7) 1_555 1_555 1_555 no C1A C2A C3A 119.8(7) 1_555 1_555 1_555 no C2A C3A C4A 120.4(7) 1_555 1_555 1_555 no C3A C4A C5A 118.4(7) 1_555 1_555 1_555 no N1A C5A C4A 121.8(7) 1_555 1_555 1_555 no N1A C5A C6A 115.5(6) 1_555 1_555 1_555 no C4A C5A C6A 122.7(7) 1_555 1_555 1_555 no N2A C6A C5A 112.6(6) 1_555 1_555 1_555 no N2A C6A C7A 118.9(6) 1_555 1_555 1_555 no C5A C6A C7A 128.5(7) 1_555 1_555 1_555 no C6A C7A C8A 120.5(7) 1_555 1_555 1_555 no C7A C8A C9A 119.6(7) 1_555 1_555 1_555 no C8A C9A C10A 119.6(7) 1_555 1_555 1_555 no N2A C10A C9A 120.4(7) 1_555 1_555 1_555 no N2A C10A C11A 111.6(6) 1_555 1_555 1_555 no C9A C10A C11A 128.0(7) 1_555 1_555 1_555 no N3A C11A C10A 115.8(6) 1_555 1_555 1_555 no N3A C11A C12A 121.6(7) 1_555 1_555 1_555 no C10A C11A C12A 122.6(7) 1_555 1_555 1_555 no C11A C12A C13A 118.4(7) 1_555 1_555 1_555 no C12A C13A C14A 120.1(7) 1_555 1_555 1_555 no C13A C14A C15A 118.7(7) 1_555 1_555 1_555 no N3A C15A C14A 122.1(7) 1_555 1_555 1_555 no Ru1 N1B C1B 126.9(5) 1_555 1_555 1_555 no Ru1 N1B C5B 113.8(4) 1_555 1_555 1_555 no C1B N1B C5B 119.2(6) 1_555 1_555 1_555 no Ru1 N2B C6B 118.9(5) 1_555 1_555 1_555 no Ru1 N2B C10B 117.8(5) 1_555 1_555 1_555 no C6B N2B C10B 123.2(6) 1_555 1_555 1_555 no Ru1 N3B C11B 113.5(4) 1_555 1_555 1_555 no Ru1 N3B C15B 128.3(5) 1_555 1_555 1_555 no C11B N3B C15B 118.2(6) 1_555 1_555 1_555 no N1B C1B C2B 121.6(7) 1_555 1_555 1_555 no C1B C2B C3B 118.4(7) 1_555 1_555 1_555 no C2B C3B C4B 120.7(7) 1_555 1_555 1_555 no C3B C4B C5B 118.2(7) 1_555 1_555 1_555 no N1B C5B C4B 121.9(7) 1_555 1_555 1_555 no N1B C5B C6B 115.3(6) 1_555 1_555 1_555 no C4B C5B C6B 122.8(7) 1_555 1_555 1_555 no N2B C6B C5B 113.3(6) 1_555 1_555 1_555 no N2B C6B C7B 118.1(8) 1_555 1_555 1_555 no C5B C6B C7B 128.6(7) 1_555 1_555 1_555 no C6B C7B C8B 121.3(8) 1_555 1_555 1_555 no C7B C8B C9B 119.8(8) 1_555 1_555 1_555 no C8B C9B C10B 118.2(8) 1_555 1_555 1_555 no N2B C10B C9B 119.3(7) 1_555 1_555 1_555 no N2B C10B C11B 113.6(6) 1_555 1_555 1_555 no C9B C10B C11B 127.1(7) 1_555 1_555 1_555 no N3B C11B C10B 115.5(6) 1_555 1_555 1_555 no N3B C11B C12B 121.8(7) 1_555 1_555 1_555 no C10B C11B C12B 122.7(7) 1_555 1_555 1_555 no C11B C12B C13B 118.0(8) 1_555 1_555 1_555 no C12B C13B C14B 119.7(7) 1_555 1_555 1_555 no C13B C14B C15B 118.8(7) 1_555 1_555 1_555 no N3B C15B C14B 123.6(7) 1_555 1_555 1_555 no