Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_phone '[351]234 370 729' _publ_contact_author_email vfelix@dq.ua.pt _publ_contact_author_name V.Felix _publ_contact_author_address ; Prof. V. Felix Departamento de Quimica Universidade de Aveiro 3810-193 Aveiro Portugal ; loop_ _publ_author_name 'Rita Delgado' 'Silvia Carvalho' 'Carla Cruz' 'M. Drew' 'Vitor Felix' 'Brian J. Goodfellow' #------------------------- data section of block-------------------------- data_[Ni2([28]py2N6(H2O)4]Cl4.3H2O _database_code_CSD 208896 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H58 Cl4 N8 Ni2 O7' _chemical_formula_weight 854.02 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 32.098(34) _cell_length_b 16.040(17) _cell_length_c 7.471(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.88(1) _cell_angle_gamma 90.00 _cell_volume 3777(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.331 _exptl_absorpt_correction_type 'not absorption correction' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'MAR research image plate system' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3563 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.1261 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.02 _reflns_number_total 2315 _reflns_number_gt 1276 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'W. Kabsch, J. Appl. Crystallogr. 21,916,1983' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1654P)^2^+11.2081P] 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 2315 _refine_ls_number_parameters 229 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1973 _refine_ls_R_factor_gt 0.1043 _refine_ls_wR_factor_ref 0.3160 _refine_ls_wR_factor_gt 0.2775 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.216 _refine_ls_shift/su_max 0.000 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.14739(5) 0.24823(10) 0.0942(3) 0.0383(8) Uani 1 d . . . O100 O 0.1360(3) 0.2915(7) -0.1759(16) 0.048(3) Uani 1 d D . . H101 H 0.117(3) 0.269(8) -0.248(11) 0.057 Uiso 1 d D . . H102 H 0.148(3) 0.321(5) -0.239(10) 0.00(3) Uiso 1 d D . . O200 O 0.1598(3) 0.2059(6) 0.3778(18) 0.050(3) Uani 1 d D . . H201 H 0.1358(17) 0.210(9) 0.40(2) 0.061 Uiso 1 d D . . H202 H 0.174(3) 0.236(9) 0.453(17) 0.061 Uiso 1 d D . . N3 N 0.1853(3) 0.3504(6) 0.171(2) 0.044(4) Uani 1 d . . . H3 H 0.1912 0.3500 0.2950 0.052 Uiso 1 calc R . . N7 N 0.0902(4) 0.3051(7) 0.118(2) 0.049(4) Uani 1 d . . . H7 H 0.0877 0.2992 0.2363 0.059 Uiso 1 calc R . . N10 N 0.1076(3) 0.1527(7) 0.036(2) 0.046(4) Uani 1 d . . . N16 N 0.1905(4) 0.1463(6) 0.041(2) 0.042(4) Uani 1 d . . . H16 H 0.2163 0.1526 0.1151 0.050 Uiso 1 calc R . . C1 C 0.2606(4) 0.3985(9) 0.177(2) 0.043(5) Uani 1 d . . . H1A H 0.2614 0.4109 0.3047 0.052 Uiso 1 calc R . . H1B H 0.2553 0.4499 0.1083 0.052 Uiso 1 calc R . . C2 C 0.2267(4) 0.3375(9) 0.111(2) 0.036(4) Uani 1 d . . . H2A H 0.2371 0.2825 0.1510 0.043 Uiso 1 calc R . . H2B H 0.2215 0.3377 -0.0208 0.043 Uiso 1 calc R . . C4 C 0.1665(4) 0.4326(8) 0.118(3) 0.049(5) Uani 1 d . . . H4A H 0.1627 0.4383 -0.0136 0.059 Uiso 1 calc R . . H4B H 0.1860 0.4757 0.1723 0.059 Uiso 1 calc R . . C5 C 0.1231(4) 0.4463(9) 0.176(3) 0.058(6) Uani 1 d . . . H5A H 0.1265 0.4348 0.3053 0.069 Uiso 1 calc R . . H5B H 0.1156 0.5047 0.1581 0.069 Uiso 1 calc R . . C6 C 0.0870(4) 0.3955(9) 0.079(3) 0.060(6) Uani 1 d . . . H6A H 0.0611 0.4162 0.1119 0.072 Uiso 1 calc R . . H6B H 0.0848 0.4037 -0.0510 0.072 Uiso 1 calc R . . C8 C 0.0555(4) 0.2564(10) 0.012(3) 0.054(5) Uani 1 d . . . H8A H 0.0485 0.2791 -0.1105 0.064 Uiso 1 calc R . . H8B H 0.0307 0.2616 0.0673 0.064 Uiso 1 calc R . . C9 C 0.0662(4) 0.1681(10) 0.001(3) 0.044(5) Uani 1 d . . . C11 C 0.1225(4) 0.0753(8) 0.035(2) 0.034(4) Uani 1 d . . . C12 C 0.0953(5) 0.0085(9) -0.013(3) 0.050(5) Uani 1 d . . . H12 H 0.1061 -0.0451 -0.0176 0.060 Uiso 1 calc R . . C13 C 0.0538(5) 0.0216(11) -0.052(3) 0.071(6) Uani 1 d . . . H13 H 0.0354 -0.0226 -0.0884 0.085 Uiso 1 calc R . . C14 C 0.0378(5) 0.1016(12) -0.039(3) 0.070(6) Uani 1 d . . . H14 H 0.0087 0.1107 -0.0568 0.085 Uiso 1 calc R . . C15 C 0.1700(4) 0.0691(9) 0.091(2) 0.041(4) Uani 1 d . . . H15A H 0.1775 0.0606 0.2220 0.049 Uiso 1 calc R . . H15B H 0.1802 0.0215 0.0318 0.049 Uiso 1 calc R . . C17 C 0.1964(4) 0.1399(8) -0.152(2) 0.033(4) Uani 1 d . . . H17A H 0.1939 0.1952 -0.2048 0.040 Uiso 1 calc R . . H17B H 0.1736 0.1062 -0.2187 0.040 Uiso 1 calc R . . O300 O 0.0436(4) 0.4062(8) 0.518(2) 0.104(6) Uani 1 d D . . H301 H 0.0622 0.3702 0.5400 0.124 Uiso 1 d RD . . H302 H 0.0206 0.3736 0.5610 0.124 Uiso 1 d RD . . O400 O 0.0000 0.4875(11) 0.7500 0.094(7) Uani 1 d SD . . H401 H -0.006(8) 0.5186(14) 0.662(4) 0.112 Uiso 1 d D . . Cl1 Cl 0.07135(13) 0.2138(3) 0.5057(7) 0.0613(15) Uani 1 d . . . Cl2 Cl 0.21210(13) 0.3486(2) -0.3759(7) 0.0569(15) Uani 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 Ni 0.0381(10) 0.0296(11) 0.050(2) 0.0015(10) 0.0159(10) 0.0006(8) O100 0.039(6) 0.052(7) 0.057(10) 0.021(7) 0.020(6) 0.002(5) O200 0.060(6) 0.032(6) 0.065(11) 0.001(6) 0.026(7) -0.001(5) N3 0.033(6) 0.025(7) 0.077(13) -0.003(7) 0.024(7) 0.000(5) N7 0.048(7) 0.046(9) 0.062(13) -0.001(7) 0.029(8) 0.000(6) N10 0.040(7) 0.026(7) 0.070(13) 0.002(7) 0.004(7) -0.003(5) N16 0.044(7) 0.028(7) 0.054(13) -0.007(7) 0.008(7) 0.000(5) C1 0.040(8) 0.042(9) 0.054(15) -0.007(8) 0.025(8) -0.006(6) C2 0.039(7) 0.047(9) 0.023(13) -0.012(7) 0.010(8) -0.005(6) C4 0.040(8) 0.029(8) 0.080(16) 0.013(9) 0.017(9) -0.009(6) C5 0.047(9) 0.043(9) 0.092(18) -0.006(10) 0.035(10) 0.004(7) C6 0.033(8) 0.043(10) 0.101(19) -0.018(10) 0.006(9) 0.005(7) C8 0.033(7) 0.056(11) 0.076(17) -0.004(10) 0.023(9) 0.001(7) C9 0.035(8) 0.056(11) 0.043(14) -0.006(9) 0.013(8) -0.008(7) C11 0.047(8) 0.032(8) 0.031(13) -0.009(8) 0.027(8) -0.003(6) C12 0.056(9) 0.030(8) 0.069(15) 0.013(8) 0.025(9) -0.007(7) C13 0.060(11) 0.046(11) 0.11(2) -0.012(12) 0.035(12) -0.016(8) C14 0.030(8) 0.106(16) 0.080(18) 0.030(13) 0.021(10) -0.006(9) C15 0.058(10) 0.043(9) 0.023(13) 0.005(8) 0.013(9) 0.003(7) C17 0.037(7) 0.030(8) 0.035(15) -0.009(8) 0.014(8) -0.009(6) O300 0.095(10) 0.073(9) 0.151(17) 0.011(10) 0.042(11) 0.024(7) O400 0.118(17) 0.061(12) 0.10(2) 0.000 0.018(17) 0.000 Cl1 0.055(2) 0.052(2) 0.082(5) -0.005(3) 0.025(2) -0.0031(19) Cl2 0.070(3) 0.056(3) 0.046(4) -0.002(2) 0.014(2) -0.008(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 Ni N10 1.990(11) . ? Ni N3 2.057(10) . ? Ni N7 2.087(11) . ? Ni O100 2.100(11) . ? Ni O200 2.188(13) . ? Ni N16 2.227(11) . ? O100 H101 0.822(11) . ? O100 H102 0.818(11) . ? O200 H201 0.820(11) . ? O200 H202 0.820(11) . ? N3 C4 1.474(17) . ? N3 C2 1.492(17) . ? N3 H3 0.9100 . ? N7 C8 1.462(18) . ? N7 C6 1.48(2) . ? N7 H7 0.9100 . ? N10 C9 1.327(17) . ? N10 C11 1.332(17) . ? N16 C15 1.485(17) . ? N16 C17 1.49(2) . ? N16 H16 0.9100 . ? C1 C2 1.478(18) . ? C1 C17 1.554(18) 7 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C5 1.551(19) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.49(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C9 1.46(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.40(2) . ? C11 C12 1.386(19) . ? C11 C15 1.506(19) . ? C12 C13 1.33(2) . ? C12 H12 0.9300 . ? C13 C14 1.39(2) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C1 1.554(18) 7 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? O300 H301 0.8245 . ? O300 H302 1.0066 . ? O400 H401 0.820(8) . ? 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 N10 Ni N3 174.8(5) . . ? N10 Ni N7 79.3(4) . . ? N3 Ni N7 96.5(4) . . ? N10 Ni O100 93.3(5) . . ? N3 Ni O100 89.5(5) . . ? N7 Ni O100 86.5(5) . . ? N10 Ni O200 87.9(5) . . ? N3 Ni O200 89.2(5) . . ? N7 Ni O200 93.3(5) . . ? O100 Ni O200 178.7(4) . . ? N10 Ni N16 78.0(4) . . ? N3 Ni N16 106.2(4) . . ? N7 Ni N16 157.3(5) . . ? O100 Ni N16 94.1(5) . . ? O200 Ni N16 86.6(5) . . ? Ni O100 H101 117(7) . . ? Ni O100 H102 137(6) . . ? H101 O100 H102 105(2) . . ? Ni O200 H201 100(10) . . ? Ni O200 H202 117(10) . . ? H201 O200 H202 105(2) . . ? C4 N3 C2 112.7(11) . . ? C4 N3 Ni 116.5(9) . . ? C2 N3 Ni 108.7(8) . . ? C4 N3 H3 106.1 . . ? C2 N3 H3 106.1 . . ? Ni N3 H3 106.1 . . ? C8 N7 C6 113.7(13) . . ? C8 N7 Ni 108.3(9) . . ? C6 N7 Ni 116.2(9) . . ? C8 N7 H7 106.0 . . ? C6 N7 H7 106.0 . . ? Ni N7 H7 106.0 . . ? C9 N10 C11 121.4(11) . . ? C9 N10 Ni 118.5(9) . . ? C11 N10 Ni 120.1(9) . . ? C15 N16 C17 109.3(12) . . ? C15 N16 Ni 104.3(8) . . ? C17 N16 Ni 114.9(9) . . ? C15 N16 H16 109.4 . . ? C17 N16 H16 109.4 . . ? Ni N16 H16 109.4 . . ? C2 C1 C17 108.3(11) . 7 ? C2 C1 H1A 110.0 . . ? C17 C1 H1A 110.0 7 . ? C2 C1 H1B 110.0 . . ? C17 C1 H1B 110.0 7 . ? H1A C1 H1B 108.4 . . ? C1 C2 N3 116.8(11) . . ? C1 C2 H2A 108.1 . . ? N3 C2 H2A 108.1 . . ? C1 C2 H2B 108.1 . . ? N3 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? N3 C4 C5 113.4(12) . . ? N3 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 116.3(15) . . ? C6 C5 H5A 108.2 . . ? C4 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? C4 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? N7 C6 C5 115.2(14) . . ? N7 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? N7 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? N7 C8 C9 112.6(12) . . ? N7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N10 C9 C14 119.2(14) . . ? N10 C9 C8 113.9(12) . . ? C14 C9 C8 126.9(13) . . ? N10 C11 C12 120.8(13) . . ? N10 C11 C15 114.1(11) . . ? C12 C11 C15 125.1(13) . . ? C13 C12 C11 119.4(14) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.0(15) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 118.9(14) . . ? C13 C14 H14 120.6 . . ? C9 C14 H14 120.6 . . ? N16 C15 C11 110.3(11) . . ? N16 C15 H15A 109.6 . . ? C11 C15 H15A 109.6 . . ? N16 C15 H15B 109.6 . . ? C11 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N16 C17 C1 115.0(13) . 7 ? N16 C17 H17A 108.5 . . ? C1 C17 H17A 108.5 7 . ? N16 C17 H17B 108.5 . . ? C1 C17 H17B 108.5 7 . ? H17A C17 H17B 107.5 . . ? H301 O300 H302 96.9 . . ? _diffrn_measured_fraction_theta_max 0.311 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.311 _refine_diff_density_max 0.742 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.136 #==END