# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_ni _database_code_CSD 156038 _journal_coden_Cambridge 0440 _publ_requested_journal ' New J.Chem.(Nouv.J.Chim.)' loop_ _publ_author_name 'Chen, X.-M.' 'Gao, S.' 'Ji, L.-N.' 'Lu, T.-B.' 'Mao, Zongwan' 'Xiang, Hua' _publ_contact_author_name 'Dr T.-B. Lu' _publ_contact_author_address ; Dr T-B Lu Department of Chemistry Zhongshan University Guangzhou 510275 CHINA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H126 Cr2 N30 Ni3 O24' _chemical_formula_weight 1787.76 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' 'Cr' 'Cr' 0.3209 0.6236 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 15.049(2) _cell_length_b 15.049(2) _cell_length_c 18.794(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3685.9(10) _cell_formula_units_Z 2 _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 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type ? _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 ? _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 16667 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.23 _diffrn_reflns_theta_max 30.11 _reflns_number_total 3583 _reflns_number_gt 2070 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.1872P] 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 3583 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Cr Cr 0.6667 0.3333 0.34291(3) 0.02003(12) Uani 1 d S . . Ni Ni 0.5000 0.0000 0.5000 0.02317(10) Uani 1 d S . . N4 N 0.36605(13) -0.02231(14) 0.45085(9) 0.0303(4) Uani 1 d . . . H4N H 0.3148 -0.0853 0.4684 0.036 Uiso 1 d R . . N3 N 0.34363(14) 0.08997(14) 0.53462(9) 0.0357(4) Uani 1 d . . . N2 N 0.58522(14) 0.14041(14) 0.44796(9) 0.0329(4) Uani 1 d . . . N5 N 0.51847(13) -0.07014(13) 0.41121(8) 0.0281(4) Uani 1 d . . . H5N H 0.5617 -0.0130 0.3806 0.034 Uiso 1 d R . . C2 C 0.61526(14) 0.20847(15) 0.40962(10) 0.0253(4) Uani 1 d . . . C6 C 0.34615(18) 0.06396(18) 0.46077(11) 0.0357(5) Uani 1 d . . . H6A H 0.3995 0.1238 0.4365 0.043 Uiso 1 d R . . H6B H 0.2812 0.0464 0.4386 0.043 Uiso 1 d R . . C8 C 0.41777(17) -0.12058(19) 0.37519(12) 0.0384(6) Uani 1 d . . . H8A H 0.3713 -0.1834 0.4002 0.046 Uiso 1 d R . . H8B H 0.4251 -0.1380 0.3267 0.046 Uiso 1 d R . . C5 C 0.44003(17) 0.13879(16) 0.57190(11) 0.0341(5) Uani 1 d . . . H5A H 0.4317 0.1677 0.6159 0.041 Uiso 1 d R . . H5B H 0.4901 0.1951 0.5431 0.041 Uiso 1 d R . . C7 C 0.37479(19) -0.04791(19) 0.37533(11) 0.0384(5) Uani 1 d . . . H7A H 0.4204 0.0143 0.3495 0.046 Uiso 1 d R . . H7B H 0.3080 -0.0801 0.3525 0.046 Uiso 1 d R . . O1 O 0.19390(15) 0.11231(15) 0.62661(10) 0.0575(5) Uani 1 d . . . H1A H 0.1768 0.1299 0.6690 0.069 Uiso 0.50 d PR . . H1B H 0.1493 0.0769 0.5803 0.069 Uiso 0.50 d PR . . C4 C 0.25669(18) 0.0080(2) 0.57398(13) 0.0443(6) Uani 1 d . . . H4A H 0.2734 -0.0446 0.5859 0.053 Uiso 1 d R . . H4B H 0.1972 -0.0229 0.5430 0.053 Uiso 1 d R . . C1 C 0.53056(19) 0.26283(18) 0.28559(11) 0.0377(5) Uani 1 d . . . C3 C 0.2289(2) 0.0427(2) 0.64087(14) 0.0546(7) Uani 1 d . . . H3A H 0.1753 -0.0167 0.6654 0.065 Uiso 1 d R . . H3B H 0.2884 0.0747 0.6719 0.065 Uiso 1 d R . . N1 N 0.4516(2) 0.2277(2) 0.25968(14) 0.0699(8) Uani 1 d . . . O1W O 0.0000 0.0000 0.57239(18) 0.0563(8) Uani 1 d S . . H1WA H 0.0698 0.0421 0.5957 0.068 Uiso 0.50 d PR . . H1WB H -0.0280 -0.0213 0.5225 0.068 Uiso 0.17 d PR . . O2W O 0.4089(2) 0.4089(2) 0.2500 0.1005(12) Uani 1 d S . . H2WA H 0.3933 0.3396 0.2683 0.121 Uiso 1 d R . . O3W O 0.2342(3) 0.1962(3) 0.7613(3) 0.0799(15) Uani 0.50 d P . . H3WC H 0.1978 0.1588 0.7956 0.096 Uiso 0.50 d PR . . H3WA H 0.2949 0.2005 0.7601 0.096 Uiso 0.50 d PR . . 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 Cr 0.02089(17) 0.02089(17) 0.0183(2) 0.000 0.000 0.01044(9) Ni 0.0266(2) 0.01857(18) 0.02299(17) 0.00068(13) 0.00106(15) 0.01032(17) N4 0.0305(10) 0.0305(10) 0.0313(9) -0.0029(8) -0.0017(8) 0.0164(8) N3 0.0345(10) 0.0378(11) 0.0385(10) -0.0035(8) 0.0011(8) 0.0209(9) N2 0.0360(11) 0.0253(9) 0.0348(9) 0.0045(8) 0.0043(8) 0.0133(8) N5 0.0282(9) 0.0265(9) 0.0278(9) -0.0018(7) 0.0011(7) 0.0124(8) C2 0.0246(11) 0.0240(10) 0.0268(9) -0.0021(8) 0.0007(8) 0.0119(9) C6 0.0363(13) 0.0377(13) 0.0403(12) -0.0015(10) -0.0032(10) 0.0240(11) C8 0.0369(13) 0.0408(13) 0.0368(12) -0.0155(11) -0.0065(10) 0.0189(11) C5 0.0359(12) 0.0291(12) 0.0387(12) -0.0050(10) 0.0037(10) 0.0174(10) C7 0.0390(13) 0.0454(14) 0.0325(12) -0.0078(10) -0.0103(10) 0.0223(12) O1 0.0516(12) 0.0636(13) 0.0613(11) -0.0125(10) 0.0021(9) 0.0318(10) C4 0.0343(13) 0.0462(15) 0.0542(15) 0.0005(12) 0.0057(11) 0.0214(12) C1 0.0414(13) 0.0426(14) 0.0294(10) -0.0076(10) -0.0074(10) 0.0213(12) C3 0.0449(16) 0.0692(19) 0.0506(15) 0.0074(14) 0.0075(12) 0.0293(15) N1 0.0511(15) 0.091(2) 0.0661(15) -0.0264(14) -0.0267(13) 0.0346(15) O1W 0.0513(12) 0.0513(12) 0.067(2) 0.000 0.000 0.0256(6) O2W 0.0868(19) 0.0868(19) 0.132(3) -0.0176(11) 0.0176(11) 0.047(2) O3W 0.054(2) 0.112(4) 0.073(3) -0.012(3) 0.009(2) 0.041(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C2 2.061(2) . ? Cr C2 2.061(2) 2_655 ? Cr C2 2.061(2) 3_665 ? Cr C1 2.076(2) 2_655 ? Cr C1 2.076(2) . ? Cr C1 2.076(2) 3_665 ? Ni N5 2.0662(16) 7_656 ? Ni N5 2.0662(16) . ? Ni N4 2.0862(17) . ? Ni N4 2.0862(17) 7_656 ? Ni N2 2.0872(18) 7_656 ? Ni N2 2.0872(18) . ? N4 C6 1.483(3) . ? N4 C7 1.493(3) . ? N3 C5 1.439(3) . ? N3 C6 1.448(3) . ? N3 C4 1.472(3) . ? N2 C2 1.144(3) . ? N5 C8 1.477(3) . ? N5 C5 1.484(3) 7_656 ? C8 C7 1.524(3) . ? C5 N5 1.484(3) 7_656 ? O1 C3 1.414(3) . ? C4 C3 1.498(3) . ? C1 N1 1.141(3) . ? O3W O3W 1.078(8) 4_556 ? 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 Cr C2 86.84(8) . 2_655 ? C2 Cr C2 86.84(8) . 3_665 ? C2 Cr C2 86.84(8) 2_655 3_665 ? C2 Cr C1 86.00(8) . 2_655 ? C2 Cr C1 91.43(8) 2_655 2_655 ? C2 Cr C1 172.72(8) 3_665 2_655 ? C2 Cr C1 91.43(8) . . ? C2 Cr C1 172.72(8) 2_655 . ? C2 Cr C1 86.00(8) 3_665 . ? C1 Cr C1 95.51(9) 2_655 . ? C2 Cr C1 172.72(9) . 3_665 ? C2 Cr C1 86.00(8) 2_655 3_665 ? C2 Cr C1 91.43(8) 3_665 3_665 ? C1 Cr C1 95.51(8) 2_655 3_665 ? C1 Cr C1 95.51(9) . 3_665 ? N5 Ni N5 180.0 7_656 . ? N5 Ni N4 94.23(6) 7_656 . ? N5 Ni N4 85.77(6) . . ? N5 Ni N4 85.77(6) 7_656 7_656 ? N5 Ni N4 94.23(6) . 7_656 ? N4 Ni N4 180.0 . 7_656 ? N5 Ni N2 88.12(7) 7_656 7_656 ? N5 Ni N2 91.88(7) . 7_656 ? N4 Ni N2 89.39(7) . 7_656 ? N4 Ni N2 90.61(7) 7_656 7_656 ? N5 Ni N2 91.88(7) 7_656 . ? N5 Ni N2 88.12(7) . . ? N4 Ni N2 90.61(7) . . ? N4 Ni N2 89.39(7) 7_656 . ? N2 Ni N2 180.0 7_656 . ? C6 N4 C7 115.32(16) . . ? C6 N4 Ni 113.91(13) . . ? C7 N4 Ni 105.05(13) . . ? C5 N3 C6 116.68(18) . . ? C5 N3 C4 115.47(18) . . ? C6 N3 C4 112.82(19) . . ? C2 N2 Ni 165.68(17) . . ? C8 N5 C5 114.89(17) . 7_656 ? C8 N5 Ni 105.50(12) . . ? C5 N5 Ni 113.19(12) 7_656 . ? N2 C2 Cr 177.82(17) . . ? N3 C6 N4 113.66(17) . . ? N5 C8 C7 108.97(17) . . ? N3 C5 N5 114.61(17) . 7_656 ? N4 C7 C8 108.09(17) . . ? N3 C4 C3 114.6(2) . . ? N1 C1 Cr 172.6(2) . . ? O1 C3 C4 111.8(2) . . ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.892 _refine_diff_density_max 0.553 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.062