Supplementary Material (ESI) for PCCP This journal is (c) The Royal Society of Chemistry 2001 data_global CCDC 156911 and 156912 _journal_coden_Cambridge 1326 _publ_requested_journal 'Physical Chemistry Chemical Physics' loop_ _publ_author_name 'Saija Luukkanen' 'Matti Haukka' 'Esa Eskelinen' 'Tapani A. Pakkanen' 'Viivi Lehtovuori' 'Jani Kallioinen' 'Pasi Myllyperkio' 'Jouko Korppi-Tommola' _publ_contact_author_name 'Matti Haukka' _publ_contact_author_address ; Matti Haukka Department of Chemistry Univeristy of Joensuu POBox 111 FIN-80101 Joensuu FINLAND ; data_structure_1 _database_code_CSD 156911 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ru(dcbpy)(CO)2Br2.(H2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Br2 N2 O7 Ru' _chemical_formula_weight 579.13 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' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.57440(10) _cell_length_b 19.6040(4) _cell_length_c 13.4362(2) _cell_angle_alpha 90.0000(10) _cell_angle_beta 92.7382(12) _cell_angle_gamma 90.00 _cell_volume 1729.74(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 5.567 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.2101 _exptl_absorpt_correction_T_max 0.3068 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23446 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3801 _reflns_number_gt 3558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0268P)^2^+2.6533P] 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 3801 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4666(4) 0.59133(12) 0.50370(18) 0.0189(5) Uani 1 1 d . . . C2 C 0.8493(4) 0.58383(12) 0.59057(19) 0.0179(5) Uani 1 1 d . . . C10 C 1.0302(3) 0.72855(12) 0.66179(18) 0.0154(4) Uani 1 1 d . . . H10 H 1.0766 0.6836 0.6762 0.018 Uiso 1 1 calc R . . C11 C 1.1485(3) 0.78288(12) 0.69480(17) 0.0148(4) Uani 1 1 d . . . H11 H 1.2752 0.7754 0.7302 0.018 Uiso 1 1 calc R . . C12 C 1.0798(4) 0.84836(11) 0.67555(18) 0.0137(5) Uani 1 1 d . . . C13 C 0.8923(3) 0.85807(12) 0.62368(18) 0.0143(4) Uani 1 1 d . . . H13 H 0.8412 0.9027 0.6107 0.017 Uiso 1 1 calc R . . C14 C 0.7823(3) 0.80081(12) 0.59165(17) 0.0127(4) Uani 1 1 d . . . C15 C 0.5828(3) 0.80494(12) 0.53614(17) 0.0128(4) Uani 1 1 d . . . C16 C 0.4893(3) 0.86610(12) 0.50812(17) 0.0142(4) Uani 1 1 d . . . H16 H 0.5529 0.9085 0.5242 0.017 Uiso 1 1 calc R . . C17 C 0.3012(3) 0.86424(12) 0.45619(17) 0.0138(4) Uani 1 1 d . . . C18 C 0.2118(3) 0.80147(12) 0.43312(18) 0.0153(4) Uani 1 1 d . . . H18 H 0.0838 0.7991 0.3974 0.018 Uiso 1 1 calc R . . C19 C 0.3133(3) 0.74271(12) 0.46329(18) 0.0142(4) Uani 1 1 d . . . H19 H 0.2522 0.6998 0.4478 0.017 Uiso 1 1 calc R . . C41 C 1.2046(4) 0.90890(12) 0.70882(18) 0.0168(5) Uani 1 1 d . . . C42 C 0.1969(4) 0.92995(13) 0.4275(2) 0.0191(5) Uani 1 1 d . . . N1 N 0.8519(3) 0.73672(10) 0.61002(15) 0.0133(4) Uani 1 1 d . . . N2 N 0.4952(3) 0.74385(10) 0.51378(15) 0.0128(4) Uani 1 1 d . . . O1 O 0.3495(3) 0.55755(10) 0.47558(16) 0.0273(4) Uani 1 1 d . . . O2 O 0.9635(3) 0.54316(10) 0.60995(16) 0.0267(4) Uani 1 1 d . . . O99 O 1.6310(3) 0.98867(11) 0.7887(2) 0.0457(7) Uani 1 1 d . . . O411 O 1.1469(3) 0.96695(10) 0.70010(17) 0.0340(5) Uani 1 1 d . . . O412 O 1.3832(3) 0.89099(9) 0.74724(15) 0.0265(4) Uani 1 1 d . . . O421 O 0.2576(3) 0.98472(10) 0.45625(19) 0.0380(6) Uani 1 1 d . . . O422 O 0.0317(3) 0.91976(9) 0.36976(17) 0.0307(5) Uani 1 1 d . . . Br1 Br 0.51898(4) 0.651128(12) 0.725247(19) 0.01932(8) Uani 1 1 d . . . Br2 Br 0.82727(4) 0.664891(13) 0.389539(18) 0.01985(8) Uani 1 1 d . . . Ru1 Ru 0.66633(3) 0.655941(9) 0.555070(13) 0.01130(7) Uani 1 1 d . . . H412 H 1.4660 0.9284 0.7666 0.050 Uiso 1 1 d . . . H422 H -0.0277 0.9602 0.3520 0.050 Uiso 1 1 d . . . H991 H 1.6131 1.0297 0.7852 0.050 Uiso 1 1 d . . . H992 H 1.7515 0.9855 0.8093 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0301(14) 0.0132(11) 0.0137(12) 0.0024(9) 0.0035(10) 0.0133(10) C2 0.0188(12) 0.0166(12) 0.0184(13) -0.0032(9) 0.0011(9) -0.0069(9) C10 0.0152(11) 0.0147(11) 0.0159(12) -0.0004(8) -0.0013(8) 0.0028(8) C11 0.0136(10) 0.0180(11) 0.0126(12) -0.0010(8) -0.0022(8) 0.0011(8) C12 0.0155(11) 0.0150(11) 0.0106(12) -0.0016(8) -0.0005(9) -0.0011(8) C13 0.0141(11) 0.0131(10) 0.0155(12) 0.0001(8) -0.0006(8) 0.0007(8) C14 0.0120(10) 0.0144(11) 0.0117(11) 0.0000(8) 0.0008(8) -0.0003(8) C15 0.0121(10) 0.0149(11) 0.0116(11) 0.0003(8) 0.0007(8) -0.0005(8) C16 0.0139(10) 0.0130(11) 0.0157(12) 0.0001(8) 0.0000(8) -0.0006(8) C17 0.0140(10) 0.0152(11) 0.0121(11) 0.0006(8) 0.0008(8) 0.0012(9) C18 0.0126(10) 0.0174(11) 0.0157(12) 0.0016(9) -0.0019(8) -0.0002(9) C19 0.0139(10) 0.0141(11) 0.0144(11) -0.0013(8) -0.0003(8) -0.0011(8) C41 0.0175(11) 0.0175(11) 0.0149(12) -0.0005(9) -0.0044(9) -0.0011(9) C42 0.0171(11) 0.0165(12) 0.0232(13) 0.0030(9) -0.0052(9) 0.0008(9) N1 0.0134(9) 0.0129(9) 0.0135(10) -0.0012(7) -0.0004(7) -0.0001(7) N2 0.0118(9) 0.0124(9) 0.0143(10) 0.0002(7) 0.0001(7) -0.0007(7) O1 0.0208(9) 0.0216(10) 0.0394(12) 0.0028(8) -0.0018(8) -0.0006(8) O2 0.0202(9) 0.0196(9) 0.0398(12) -0.0001(8) -0.0048(8) 0.0047(7) O99 0.0283(11) 0.0209(11) 0.0853(19) -0.0014(11) -0.0238(11) -0.0050(9) O411 0.0332(11) 0.0148(9) 0.0517(14) 0.0007(9) -0.0240(10) 0.0005(8) O412 0.0187(9) 0.0176(9) 0.0419(12) -0.0059(8) -0.0135(8) 0.0000(7) O421 0.0347(11) 0.0138(9) 0.0630(16) -0.0004(9) -0.0252(10) 0.0003(8) O422 0.0269(10) 0.0159(9) 0.0471(13) 0.0015(8) -0.0210(9) 0.0030(8) Br1 0.02165(14) 0.01869(13) 0.01798(15) 0.00228(8) 0.00471(10) 0.00357(9) Br2 0.01855(13) 0.02479(14) 0.01644(14) -0.00292(9) 0.00324(9) -0.00516(9) Ru1 0.01070(10) 0.01021(10) 0.01295(12) -0.00002(6) 0.00018(7) 0.00022(6) _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 C1 O1 1.070(3) . ? C1 Ru1 1.928(3) . ? C2 O2 1.117(3) . ? C2 Ru1 1.902(3) . ? C10 N1 1.344(3) . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C12 1.381(3) . ? C11 H11 0.9500 . ? C12 C13 1.400(3) . ? C12 C41 1.499(3) . ? C13 C14 1.392(3) . ? C13 H13 0.9500 . ? C14 N1 1.356(3) . ? C14 C15 1.480(3) . ? C15 N2 1.356(3) . ? C15 C16 1.391(3) . ? C16 C17 1.391(3) . ? C16 H16 0.9500 . ? C17 C18 1.392(3) . ? C17 C42 1.501(3) . ? C18 C19 1.382(3) . ? C18 H18 0.9500 . ? C19 N2 1.347(3) . ? C19 H19 0.9500 . ? C41 O411 1.203(3) . ? C41 O412 1.308(3) . ? C42 O421 1.203(3) . ? C42 O422 1.319(3) . ? N1 Ru1 2.1107(19) . ? N2 Ru1 2.1174(19) . ? O99 H991 0.8140 . ? O99 H992 0.8288 . ? O412 H412 0.9425 . ? O422 H422 0.9106 . ? Br1 Ru1 2.5273(3) . ? Br2 Ru1 2.5143(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Ru1 176.9(2) . . ? O2 C2 Ru1 177.0(2) . . ? N1 C10 C11 122.6(2) . . ? N1 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 118.9(2) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C11 C12 C13 119.5(2) . . ? C11 C12 C41 120.7(2) . . ? C13 C12 C41 119.8(2) . . ? C14 C13 C12 118.4(2) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? N1 C14 C13 121.7(2) . . ? N1 C14 C15 115.20(19) . . ? C13 C14 C15 123.1(2) . . ? N2 C15 C16 121.6(2) . . ? N2 C15 C14 114.82(19) . . ? C16 C15 C14 123.6(2) . . ? C17 C16 C15 118.9(2) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 119.4(2) . . ? C16 C17 C42 119.4(2) . . ? C18 C17 C42 121.2(2) . . ? C19 C18 C17 118.6(2) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? N2 C19 C18 122.6(2) . . ? N2 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? O411 C41 O412 124.4(2) . . ? O411 C41 C12 123.7(2) . . ? O412 C41 C12 111.9(2) . . ? O421 C42 O422 125.1(2) . . ? O421 C42 C17 122.9(2) . . ? O422 C42 C17 112.0(2) . . ? C10 N1 C14 118.9(2) . . ? C10 N1 Ru1 124.54(16) . . ? C14 N1 Ru1 116.56(15) . . ? C19 N2 C15 118.9(2) . . ? C19 N2 Ru1 124.51(16) . . ? C15 N2 Ru1 116.50(15) . . ? H991 O99 H992 103.1 . . ? C41 O412 H412 113.3 . . ? C42 O422 H422 110.7 . . ? C2 Ru1 C1 90.76(10) . . ? C2 Ru1 N1 97.00(9) . . ? C1 Ru1 N1 172.03(8) . . ? C2 Ru1 N2 172.87(9) . . ? C1 Ru1 N2 95.54(8) . . ? N1 Ru1 N2 76.82(8) . . ? C2 Ru1 Br2 89.19(8) . . ? C1 Ru1 Br2 92.14(7) . . ? N1 Ru1 Br2 89.80(5) . . ? N2 Ru1 Br2 87.26(5) . . ? C2 Ru1 Br1 90.60(8) . . ? C1 Ru1 Br1 90.88(7) . . ? N1 Ru1 Br1 87.23(5) . . ? N2 Ru1 Br1 92.62(5) . . ? Br2 Ru1 Br1 176.972(11) . . ? 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 N1 C10 C11 C12 1.2(4) . . . . ? C10 C11 C12 C13 0.3(4) . . . . ? C10 C11 C12 C41 -179.2(2) . . . . ? C11 C12 C13 C14 -1.1(3) . . . . ? C41 C12 C13 C14 178.5(2) . . . . ? C12 C13 C14 N1 0.4(3) . . . . ? C12 C13 C14 C15 -179.9(2) . . . . ? N1 C14 C15 N2 1.7(3) . . . . ? C13 C14 C15 N2 -178.1(2) . . . . ? N1 C14 C15 C16 -178.3(2) . . . . ? C13 C14 C15 C16 2.0(4) . . . . ? N2 C15 C16 C17 0.2(3) . . . . ? C14 C15 C16 C17 -179.9(2) . . . . ? C15 C16 C17 C18 -0.3(3) . . . . ? C15 C16 C17 C42 178.7(2) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C42 C17 C18 C19 -178.7(2) . . . . ? C17 C18 C19 N2 -0.2(4) . . . . ? C11 C12 C41 O411 -174.9(3) . . . . ? C13 C12 C41 O411 5.6(4) . . . . ? C11 C12 C41 O412 5.8(3) . . . . ? C13 C12 C41 O412 -173.7(2) . . . . ? C16 C17 C42 O421 -8.1(4) . . . . ? C18 C17 C42 O421 170.9(3) . . . . ? C16 C17 C42 O422 173.2(2) . . . . ? C18 C17 C42 O422 -7.8(3) . . . . ? C11 C10 N1 C14 -1.9(3) . . . . ? C11 C10 N1 Ru1 178.79(18) . . . . ? C13 C14 N1 C10 1.0(3) . . . . ? C15 C14 N1 C10 -178.7(2) . . . . ? C13 C14 N1 Ru1 -179.57(17) . . . . ? C15 C14 N1 Ru1 0.7(3) . . . . ? C18 C19 N2 C15 0.1(3) . . . . ? C18 C19 N2 Ru1 -176.39(18) . . . . ? C16 C15 N2 C19 -0.1(3) . . . . ? C14 C15 N2 C19 -180.0(2) . . . . ? C16 C15 N2 Ru1 176.68(17) . . . . ? C14 C15 N2 Ru1 -3.2(3) . . . . ? O2 C2 Ru1 C1 139(4) . . . . ? O2 C2 Ru1 N1 -43(4) . . . . ? O2 C2 Ru1 N2 -14(5) . . . . ? O2 C2 Ru1 Br2 47(4) . . . . ? O2 C2 Ru1 Br1 -130(4) . . . . ? O1 C1 Ru1 C2 160(4) . . . . ? O1 C1 Ru1 N1 -7(5) . . . . ? O1 C1 Ru1 N2 -24(4) . . . . ? O1 C1 Ru1 Br2 -111(4) . . . . ? O1 C1 Ru1 Br1 69(4) . . . . ? C10 N1 Ru1 C2 -6.0(2) . . . . ? C14 N1 Ru1 C2 174.58(17) . . . . ? C10 N1 Ru1 C1 160.7(6) . . . . ? C14 N1 Ru1 C1 -18.7(7) . . . . ? C10 N1 Ru1 N2 177.6(2) . . . . ? C14 N1 Ru1 N2 -1.81(16) . . . . ? C10 N1 Ru1 Br2 -95.21(18) . . . . ? C14 N1 Ru1 Br2 85.42(16) . . . . ? C10 N1 Ru1 Br1 84.22(18) . . . . ? C14 N1 Ru1 Br1 -95.15(16) . . . . ? C19 N2 Ru1 C2 149.1(7) . . . . ? C15 N2 Ru1 C2 -27.5(8) . . . . ? C19 N2 Ru1 C1 -3.0(2) . . . . ? C15 N2 Ru1 C1 -179.56(17) . . . . ? C19 N2 Ru1 N1 179.3(2) . . . . ? C15 N2 Ru1 N1 2.76(16) . . . . ? C19 N2 Ru1 Br2 88.88(18) . . . . ? C15 N2 Ru1 Br2 -87.67(16) . . . . ? C19 N2 Ru1 Br1 -94.15(18) . . . . ? C15 N2 Ru1 Br1 89.30(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O412 H412 O99 0.94 1.62 2.558(3) 171.9 . _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.657 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.095 #===END========================================================================= data_structure_2 _database_code_CSD 156912 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ru(dcbpy)(CO)2I2.(H2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 I2 N2 O7 Ru' _chemical_formula_weight 673.11 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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.8645(3) _cell_length_b 19.7584(12) _cell_length_c 13.7107(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.978(3) _cell_angle_gamma 90.00 _cell_volume 1849.49(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 4.225 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3638 _exptl_absorpt_correction_T_max 0.6774 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10911 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3130 _reflns_number_gt 2533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0199P)^2^+2.4563P] 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 3130 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.32279(6) 0.65898(2) 0.44306(3) 0.01349(13) Uani 1 1 d . . . I1 I 0.45369(5) 0.655645(17) 0.26402(2) 0.01976(12) Uani 1 1 d . . . I2 I 0.17000(5) 0.663644(17) 0.61596(2) 0.01976(12) Uani 1 1 d . . . N1 N 0.1393(5) 0.73988(19) 0.3916(3) 0.0133(9) Uani 1 1 d . . . N2 N 0.4924(5) 0.7456(2) 0.4854(3) 0.0149(9) Uani 1 1 d . . . C1 C 0.5146(8) 0.5955(3) 0.4918(4) 0.0179(12) Uani 1 1 d . . . O1 O 0.6337(5) 0.55989(19) 0.5204(3) 0.0276(9) Uani 1 1 d . . . C2 C 0.1481(7) 0.5882(3) 0.4057(4) 0.0199(12) Uani 1 1 d . . . O2 O 0.0384(5) 0.54629(19) 0.3840(3) 0.0292(9) Uani 1 1 d . . . C10 C -0.0391(7) 0.7329(3) 0.3418(3) 0.0154(11) Uani 1 1 d . . . H10 H -0.0882 0.6886 0.3282 0.019 Uiso 1 1 calc R . . C11 C -0.1535(7) 0.7875(3) 0.3097(3) 0.0169(11) Uani 1 1 d . . . H11 H -0.2784 0.7808 0.2741 0.020 Uiso 1 1 calc R . . C12 C -0.0836(7) 0.8521(2) 0.3301(4) 0.0160(11) Uani 1 1 d . . . C13 C 0.1004(7) 0.8602(3) 0.3805(3) 0.0158(11) Uani 1 1 d . . . H13 H 0.1509 0.9043 0.3947 0.019 Uiso 1 1 calc R . . C14 C 0.2100(7) 0.8039(2) 0.4100(3) 0.0137(11) Uani 1 1 d . . . C15 C 0.4081(7) 0.8067(2) 0.4635(3) 0.0137(11) Uani 1 1 d . . . C16 C 0.5048(7) 0.8667(3) 0.4903(3) 0.0157(11) Uani 1 1 d . . . H16 H 0.4430 0.9089 0.4743 0.019 Uiso 1 1 calc R . . C17 C 0.6910(7) 0.8652(2) 0.5401(3) 0.0130(11) Uani 1 1 d . . . C18 C 0.7756(7) 0.8026(3) 0.5629(3) 0.0159(11) Uani 1 1 d . . . H18 H 0.9026 0.7998 0.5975 0.019 Uiso 1 1 calc R . . C19 C 0.6729(7) 0.7443(3) 0.5347(4) 0.0164(11) Uani 1 1 d . . . H19 H 0.7319 0.7017 0.5508 0.020 Uiso 1 1 calc R . . C41 C -0.2061(7) 0.9129(3) 0.2982(4) 0.0184(12) Uani 1 1 d . . . O411 O -0.1498(5) 0.97023(19) 0.3075(3) 0.0342(10) Uani 1 1 d . . . O412 O -0.3805(6) 0.8952(2) 0.2591(3) 0.0341(11) Uani 1 1 d . . . C42 C 0.7948(7) 0.9300(3) 0.5681(4) 0.0210(12) Uani 1 1 d . . . O421 O 0.7381(6) 0.9840(2) 0.5389(3) 0.0445(12) Uani 1 1 d . . . O422 O 0.9574(6) 0.9188(2) 0.6259(4) 0.0397(13) Uani 1 1 d . . . O99 O -0.6329(6) 0.9903(2) 0.2228(4) 0.0687(17) Uani 1 1 d . . . H412 H -0.453(9) 0.922(3) 0.248(4) 0.03(2) Uiso 1 1 d . . . H422 H 0.999(8) 0.951(3) 0.634(4) 0.026(19) Uiso 1 1 d . . . H991 H -0.6161 1.0433 0.2156 0.050 Uiso 1 1 d . . . H992 H -0.7260 0.9813 0.1849 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0117(2) 0.0131(3) 0.0151(2) -0.00013(16) -0.0011(2) -0.00068(16) I1 0.0211(2) 0.0204(2) 0.0179(2) -0.00150(14) 0.00268(16) -0.00310(14) I2 0.0184(2) 0.0237(2) 0.0171(2) 0.00277(14) 0.00143(16) 0.00460(14) N1 0.012(2) 0.013(2) 0.014(2) -0.0010(17) -0.0021(19) -0.0008(17) N2 0.012(2) 0.015(2) 0.017(2) 0.0020(18) 0.0002(19) 0.0020(17) C1 0.018(3) 0.016(3) 0.019(3) -0.004(2) 0.000(2) -0.007(2) O1 0.0176(19) 0.019(2) 0.045(2) -0.0004(19) -0.0060(19) 0.0040(17) C2 0.020(3) 0.019(3) 0.020(3) 0.001(2) -0.003(2) 0.008(2) O2 0.022(2) 0.025(2) 0.038(2) 0.0001(19) -0.0050(19) -0.0044(18) C10 0.014(3) 0.015(3) 0.017(3) -0.003(2) 0.000(2) -0.005(2) C11 0.014(3) 0.023(3) 0.013(3) 0.001(2) -0.004(2) 0.001(2) C12 0.013(3) 0.015(3) 0.019(3) 0.004(2) -0.002(2) 0.001(2) C13 0.017(3) 0.014(3) 0.015(3) 0.001(2) -0.003(2) -0.004(2) C14 0.011(2) 0.017(3) 0.013(3) -0.001(2) -0.003(2) -0.003(2) C15 0.012(3) 0.017(3) 0.012(3) -0.001(2) 0.002(2) 0.002(2) C16 0.013(3) 0.016(3) 0.018(3) -0.002(2) 0.003(2) 0.004(2) C17 0.012(3) 0.016(3) 0.011(2) 0.001(2) 0.002(2) -0.002(2) C18 0.013(3) 0.020(3) 0.014(3) -0.001(2) -0.002(2) -0.001(2) C19 0.015(3) 0.015(3) 0.018(3) 0.003(2) 0.000(2) 0.007(2) C41 0.014(3) 0.020(3) 0.020(3) 0.004(2) -0.004(2) 0.002(2) O411 0.027(2) 0.018(2) 0.053(3) -0.004(2) -0.018(2) -0.0006(17) O412 0.021(2) 0.021(3) 0.055(3) 0.008(2) -0.021(2) 0.0003(19) C42 0.015(3) 0.019(3) 0.028(3) -0.002(3) -0.003(3) -0.001(2) O421 0.038(2) 0.017(2) 0.071(3) 0.003(2) -0.031(2) -0.0019(19) O422 0.029(2) 0.017(3) 0.066(3) -0.002(2) -0.028(2) -0.005(2) O99 0.040(3) 0.024(3) 0.131(5) -0.001(3) -0.046(3) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.878(6) . ? Ru1 C1 1.889(6) . ? Ru1 N1 2.111(4) . ? Ru1 N2 2.117(4) . ? Ru1 I2 2.6919(5) . ? Ru1 I1 2.7013(5) . ? N1 C10 1.346(6) . ? N1 C14 1.369(6) . ? N2 C19 1.348(6) . ? N2 C15 1.358(6) . ? C1 O1 1.118(6) . ? C2 O2 1.138(6) . ? C10 C11 1.379(7) . ? C10 H10 0.9500 . ? C11 C12 1.382(7) . ? C11 H11 0.9500 . ? C12 C13 1.385(6) . ? C12 C41 1.504(7) . ? C13 C14 1.380(7) . ? C13 H13 0.9500 . ? C14 C15 1.477(6) . ? C15 C16 1.389(7) . ? C16 C17 1.386(6) . ? C16 H16 0.9500 . ? C17 C18 1.387(7) . ? C17 C42 1.497(7) . ? C18 C19 1.384(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C41 O411 1.200(6) . ? C41 O412 1.308(6) . ? O412 H412 0.73(6) . ? C42 O421 1.190(6) . ? C42 O422 1.319(6) . ? O422 H422 0.70(6) . ? O99 H991 1.0586 . ? O99 H992 0.8009 . ? 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 C2 Ru1 C1 90.2(2) . . ? C2 Ru1 N1 97.51(18) . . ? C1 Ru1 N1 172.16(18) . . ? C2 Ru1 N2 173.73(18) . . ? C1 Ru1 N2 95.54(18) . . ? N1 Ru1 N2 76.79(15) . . ? C2 Ru1 I2 88.25(15) . . ? C1 Ru1 I2 91.83(15) . . ? N1 Ru1 I2 89.68(10) . . ? N2 Ru1 I2 89.11(11) . . ? C2 Ru1 I1 89.85(15) . . ? C1 Ru1 I1 91.15(15) . . ? N1 Ru1 I1 87.61(10) . . ? N2 Ru1 I1 92.49(11) . . ? I2 Ru1 I1 176.468(18) . . ? C10 N1 C14 118.3(4) . . ? C10 N1 Ru1 124.9(3) . . ? C14 N1 Ru1 116.8(3) . . ? C19 N2 C15 118.4(4) . . ? C19 N2 Ru1 124.9(3) . . ? C15 N2 Ru1 116.6(3) . . ? O1 C1 Ru1 177.2(5) . . ? O2 C2 Ru1 178.2(5) . . ? N1 C10 C11 122.7(4) . . ? N1 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 118.9(4) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C11 C12 C13 119.2(4) . . ? C11 C12 C41 120.4(4) . . ? C13 C12 C41 120.4(4) . . ? C14 C13 C12 119.6(5) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? N1 C14 C13 121.3(4) . . ? N1 C14 C15 114.6(4) . . ? C13 C14 C15 124.1(4) . . ? N2 C15 C16 121.3(4) . . ? N2 C15 C14 115.2(4) . . ? C16 C15 C14 123.5(4) . . ? C17 C16 C15 120.2(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 118.2(4) . . ? C16 C17 C42 119.9(4) . . ? C18 C17 C42 121.9(4) . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N2 C19 C18 122.6(4) . . ? N2 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? O411 C41 O412 124.5(5) . . ? O411 C41 C12 124.0(5) . . ? O412 C41 C12 111.5(5) . . ? C41 O412 H412 118(5) . . ? O421 C42 O422 125.4(5) . . ? O421 C42 C17 123.4(5) . . ? O422 C42 C17 111.1(5) . . ? C42 O422 H422 105(5) . . ? H991 O99 H992 104.3 . . ? 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 C2 Ru1 N1 C10 -4.4(4) . . . . ? C1 Ru1 N1 C10 166.2(12) . . . . ? N2 Ru1 N1 C10 178.3(4) . . . . ? I2 Ru1 N1 C10 -92.5(4) . . . . ? I1 Ru1 N1 C10 85.2(4) . . . . ? C2 Ru1 N1 C14 176.4(3) . . . . ? C1 Ru1 N1 C14 -13.0(15) . . . . ? N2 Ru1 N1 C14 -1.0(3) . . . . ? I2 Ru1 N1 C14 88.2(3) . . . . ? I1 Ru1 N1 C14 -94.1(3) . . . . ? C2 Ru1 N2 C19 154.3(16) . . . . ? C1 Ru1 N2 C19 -2.5(4) . . . . ? N1 Ru1 N2 C19 179.2(4) . . . . ? I2 Ru1 N2 C19 89.3(4) . . . . ? I1 Ru1 N2 C19 -93.9(4) . . . . ? C2 Ru1 N2 C15 -23.4(18) . . . . ? C1 Ru1 N2 C15 179.9(3) . . . . ? N1 Ru1 N2 C15 1.5(3) . . . . ? I2 Ru1 N2 C15 -88.4(3) . . . . ? I1 Ru1 N2 C15 88.5(3) . . . . ? C2 Ru1 C1 O1 159(9) . . . . ? N1 Ru1 C1 O1 -12(10) . . . . ? N2 Ru1 C1 O1 -24(9) . . . . ? I2 Ru1 C1 O1 -113(9) . . . . ? I1 Ru1 C1 O1 69(9) . . . . ? C1 Ru1 C2 O2 137(16) . . . . ? N1 Ru1 C2 O2 -44(16) . . . . ? N2 Ru1 C2 O2 -20(17) . . . . ? I2 Ru1 C2 O2 45(16) . . . . ? I1 Ru1 C2 O2 -132(16) . . . . ? C14 N1 C10 C11 -0.7(7) . . . . ? Ru1 N1 C10 C11 -180.0(3) . . . . ? N1 C10 C11 C12 -0.6(7) . . . . ? C10 C11 C12 C13 1.2(7) . . . . ? C10 C11 C12 C41 -178.6(4) . . . . ? C11 C12 C13 C14 -0.4(7) . . . . ? C41 C12 C13 C14 179.4(4) . . . . ? C10 N1 C14 C13 1.5(7) . . . . ? Ru1 N1 C14 C13 -179.2(4) . . . . ? C10 N1 C14 C15 -179.0(4) . . . . ? Ru1 N1 C14 C15 0.4(5) . . . . ? C12 C13 C14 N1 -0.9(7) . . . . ? C12 C13 C14 C15 179.6(5) . . . . ? C19 N2 C15 C16 0.5(7) . . . . ? Ru1 N2 C15 C16 178.4(3) . . . . ? C19 N2 C15 C14 -179.6(4) . . . . ? Ru1 N2 C15 C14 -1.8(5) . . . . ? N1 C14 C15 N2 0.9(6) . . . . ? C13 C14 C15 N2 -179.5(4) . . . . ? N1 C14 C15 C16 -179.2(4) . . . . ? C13 C14 C15 C16 0.3(7) . . . . ? N2 C15 C16 C17 0.1(7) . . . . ? C14 C15 C16 C17 -179.8(5) . . . . ? C15 C16 C17 C18 -0.6(7) . . . . ? C15 C16 C17 C42 179.6(4) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C42 C17 C18 C19 -179.7(5) . . . . ? C15 N2 C19 C18 -0.7(7) . . . . ? Ru1 N2 C19 C18 -178.3(4) . . . . ? C17 C18 C19 N2 0.2(7) . . . . ? C11 C12 C41 O411 -174.8(5) . . . . ? C13 C12 C41 O411 5.4(8) . . . . ? C11 C12 C41 O412 5.1(7) . . . . ? C13 C12 C41 O412 -174.7(5) . . . . ? C16 C17 C42 O421 -10.3(8) . . . . ? C18 C17 C42 O421 169.9(5) . . . . ? C16 C17 C42 O422 171.6(5) . . . . ? C18 C17 C42 O422 -8.2(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O412 H412 O99 0.73(6) 1.84(6) 2.570(6) 179(7) . _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.581 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.140 #===END=========================================================================