# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1850 data_[CoL3(H2O)(NO3)]NO3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H26 Co N8 O7' _chemical_formula_weight 525.40 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.363(2) _cell_length_b 12.633(3) _cell_length_c 17.013(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.80(3) _cell_angle_gamma 90.00 _cell_volume 2436.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 19.2 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method ? _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kuma KM4 automatic diffractometer' _diffrn_measurement_method 'profile data from omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2.5 _diffrn_reflns_number 4391 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.06 _reflns_number_total 4391 _reflns_number_observed 2510 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Kuma KM4 software 1987' _computing_cell_refinement 'Kuma KM4 software 1987' _computing_data_reduction 'Kuma KM4 software 1987' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0530P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4391 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_obs 0.0353 _refine_ls_wR_factor_all 0.0993 _refine_ls_wR_factor_obs 0.0840 _refine_ls_goodness_of_fit_all 0.959 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 0.959 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max 0.040 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.45989(3) 0.11096(3) 0.19753(2) 0.03743(12) Uani 1 d . . O1 O 0.4819(2) 0.2149(2) 0.30050(12) 0.0556(5) Uani 1 d . . O2 O 0.6333(2) 0.1837(2) 0.2363(2) 0.0646(6) Uani 1 d . . O3 O 0.6487(3) 0.2866(2) 0.3379(2) 0.0990(10) Uani 1 d . . O4 O 0.4780(3) -0.1844(2) 0.0918(2) 0.0989(9) Uani 1 d . . O5 O 0.3601(3) -0.1557(3) -0.0087(2) 0.1224(13) Uani 1 d . . O6 O 0.3677(3) -0.3070(3) 0.0469(2) 0.1294(13) Uani 1 d . . O7 O 0.5231(2) 0.0278(2) 0.10535(12) 0.0578(6) Uani 1 d . . N1 N 0.5904(3) 0.2295(2) 0.2931(2) 0.0565(7) Uani 1 d . . N2 N 0.4019(3) -0.2175(3) 0.0425(2) 0.0816(11) Uani 1 d . . N11 N 0.4230(2) 0.2441(2) 0.12367(12) 0.0403(5) Uani 1 d . . N12 N 0.3585(2) 0.3483(2) 0.02644(13) 0.0418(5) Uani 1 d . . N21 N 0.5111(2) -0.0193(2) 0.27335(14) 0.0460(6) Uani 1 d . . N22 N 0.5328(2) -0.1310(2) 0.3726(2) 0.0577(7) Uani 1 d . . N31 N 0.2834(2) 0.0652(2) 0.19478(13) 0.0400(5) Uani 1 d . . N32 N 0.0935(2) 0.0567(2) 0.20768(15) 0.0485(6) Uani 1 d . . C11 C 0.3596(2) 0.2475(2) 0.0566(2) 0.0402(6) Uani 1 d . . C12 C 0.4248(3) 0.4095(2) 0.0784(2) 0.0471(7) Uani 1 d . . H12 H 0.4399(3) 0.4815(2) 0.0737(2) 0.057 Uiso 1 calc R . C13 C 0.4640(3) 0.3459(2) 0.1375(2) 0.0453(7) Uani 1 d . . H13 H 0.5116(3) 0.3671(2) 0.1812(2) 0.054 Uiso 1 calc R . C14 C 0.2946(3) 0.1587(2) 0.0161(2) 0.0530(8) Uani 1 d . . H14A H 0.3070(15) 0.1606(10) -0.0392(3) 0.080 Uiso 1 calc R . H14B H 0.2119(3) 0.1655(9) 0.0234(10) 0.080 Uiso 1 calc R . H14C H 0.3229(13) 0.0926(3) 0.0378(8) 0.080 Uiso 1 calc R . C15 C 0.3048(3) 0.3795(3) -0.0471(2) 0.0576(8) Uani 1 d . . H15 H 0.2825(3) 0.3265(3) -0.0830(2) 0.069 Uiso 1 calc R . C16 C 0.2843(3) 0.4763(3) -0.0680(2) 0.0686(10) Uani 1 d . . H16A H 0.3054(3) 0.5313(3) -0.0336(2) 0.082 Uiso 1 calc R . H16B H 0.2485(3) 0.4911(3) -0.1176(2) 0.082 Uiso 1 calc R . C21 C 0.4713(3) -0.0466(2) 0.3406(2) 0.0514(8) Uani 1 d . . C22 C 0.6162(3) -0.1568(3) 0.3208(2) 0.0629(9) Uani 1 d . . H22 H 0.6713(3) -0.2112(3) 0.3266(2) 0.075 Uiso 1 calc R . C23 C 0.6034(3) -0.0893(2) 0.2606(2) 0.0520(8) Uani 1 d . . H23 H 0.6486(3) -0.0888(2) 0.2170(2) 0.062 Uiso 1 calc R . C24 C 0.3733(3) 0.0038(3) 0.3782(2) 0.0754(11) Uani 1 d . . H24A H 0.3891(12) 0.0033(20) 0.4344(2) 0.113 Uiso 1 calc R . H24B H 0.3018(5) -0.0344(13) 0.3648(13) 0.113 Uiso 1 calc R . H24C H 0.3649(15) 0.0756(7) 0.3602(12) 0.113 Uiso 1 calc R . C25 C 0.5105(4) -0.1818(3) 0.4447(2) 0.0919(13) Uani 1 d . . H25 H 0.4443(4) -0.1595(3) 0.4695(2) 0.110 Uiso 1 calc R . C26 C 0.5712(5) -0.2539(4) 0.4784(3) 0.123(2) Uani 1 d . . H26A H 0.6383(5) -0.2789(4) 0.4559(3) 0.148 Uiso 1 calc R . H26B H 0.5491(5) -0.2821(4) 0.5257(3) 0.148 Uiso 1 calc R . C31 C 0.1915(2) 0.1161(2) 0.2193(2) 0.0410(6) Uani 1 d . . C32 C 0.1248(3) -0.0367(2) 0.1734(2) 0.0558(8) Uani 1 d . . H32 H 0.0753(3) -0.0926(2) 0.1580(2) 0.067 Uiso 1 calc R . C33 C 0.2412(3) -0.0307(2) 0.1669(2) 0.0497(7) Uani 1 d . . H33 H 0.2871(3) -0.0837(2) 0.1464(2) 0.060 Uiso 1 calc R . C34 C 0.1941(3) 0.2234(2) 0.2538(2) 0.0620(9) Uani 1 d . . H34A H 0.1741(19) 0.2196(3) 0.3077(4) 0.093 Uiso 1 calc R . H34B H 0.1381(14) 0.2677(5) 0.2246(8) 0.093 Uiso 1 calc R . H34C H 0.2717(6) 0.2528(7) 0.2516(12) 0.093 Uiso 1 calc R . C35 C -0.0220(3) 0.0862(3) 0.2274(3) 0.0756(12) Uani 1 d . . H35 H -0.0283(3) 0.1395(3) 0.2646(3) 0.091 Uiso 1 calc R . C36 C -0.1162(3) 0.0451(3) 0.1982(3) 0.114(2) Uani 1 d . . H36A H -0.1132(3) -0.0085(3) 0.1609(3) 0.137 Uiso 1 calc R . H36B H -0.1886(3) 0.0684(3) 0.2139(3) 0.137 Uiso 1 calc R . H1 H 0.5030 -0.0383 0.0935 0.060 Uiso 1 d . . H2 H 0.5595 0.0615 0.0641 0.060 Uiso 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 Co 0.0365(2) 0.0323(2) 0.0436(2) -0.0019(2) 0.00417(14) 0.0006(2) O1 0.063(2) 0.0503(13) 0.0530(12) -0.0059(10) -0.0006(10) 0.0057(12) O2 0.0459(13) 0.0512(13) 0.096(2) -0.0035(13) 0.0004(12) 0.0013(11) O3 0.116(2) 0.062(2) 0.109(2) -0.008(2) -0.066(2) -0.013(2) O4 0.100(2) 0.079(2) 0.120(2) -0.027(2) 0.026(2) -0.016(2) O5 0.112(3) 0.148(3) 0.113(3) 0.032(3) 0.048(2) -0.010(2) O6 0.153(3) 0.073(2) 0.165(3) -0.034(2) 0.032(2) -0.045(2) O7 0.078(2) 0.0392(11) 0.0589(13) -0.0048(10) 0.0254(11) 0.0012(11) N1 0.064(2) 0.0344(14) 0.067(2) 0.0035(13) -0.027(2) 0.0019(14) N2 0.090(3) 0.066(2) 0.095(3) -0.031(2) 0.051(2) -0.026(2) N11 0.0434(13) 0.0350(12) 0.0419(13) 0.0024(10) -0.0010(10) -0.0052(10) N12 0.0449(13) 0.0366(12) 0.0436(13) 0.0047(11) 0.0010(10) -0.0006(11) N21 0.0441(14) 0.0408(13) 0.0528(15) 0.0025(12) 0.0015(11) 0.0024(11) N22 0.060(2) 0.048(2) 0.064(2) 0.0104(13) -0.0061(14) -0.0070(13) N31 0.0368(12) 0.0316(11) 0.0524(14) 0.0019(11) 0.0090(10) 0.0024(10) N32 0.0383(14) 0.0346(13) 0.074(2) 0.0081(12) 0.0136(12) 0.0013(11) C11 0.041(2) 0.0368(15) 0.043(2) -0.0004(12) 0.0083(13) -0.0006(12) C12 0.055(2) 0.032(2) 0.054(2) -0.0008(13) 0.0046(14) -0.0052(13) C13 0.051(2) 0.0387(15) 0.046(2) -0.0010(13) -0.0020(13) -0.0046(14) C14 0.057(2) 0.046(2) 0.054(2) -0.0026(15) -0.0046(15) -0.0075(15) C15 0.064(2) 0.051(2) 0.057(2) 0.005(2) -0.008(2) -0.001(2) C16 0.076(2) 0.061(2) 0.068(2) 0.013(2) -0.007(2) 0.005(2) C21 0.052(2) 0.047(2) 0.054(2) 0.003(2) -0.0016(15) -0.0047(15) C22 0.056(2) 0.038(2) 0.092(3) -0.001(2) -0.020(2) 0.003(2) C23 0.045(2) 0.040(2) 0.070(2) -0.010(2) -0.0027(15) -0.0010(14) C24 0.076(3) 0.089(3) 0.062(2) 0.012(2) 0.015(2) 0.005(2) C25 0.105(3) 0.087(3) 0.082(3) 0.034(3) -0.009(2) -0.003(3) C26 0.145(5) 0.124(4) 0.098(3) 0.046(3) -0.007(3) 0.019(4) C31 0.041(2) 0.0316(13) 0.052(2) 0.0029(13) 0.0087(12) 0.0036(13) C32 0.048(2) 0.035(2) 0.086(2) -0.002(2) 0.014(2) -0.0080(14) C33 0.049(2) 0.0296(14) 0.072(2) -0.0031(14) 0.0161(15) -0.0009(13) C34 0.050(2) 0.048(2) 0.088(2) -0.015(2) 0.010(2) 0.006(2) C35 0.044(2) 0.046(2) 0.141(4) 0.013(2) 0.032(2) 0.006(2) C36 0.044(2) 0.061(3) 0.239(6) 0.007(3) 0.023(3) -0.003(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 Co O7 2.056(2) . ? Co N31 2.085(2) . ? Co N11 2.125(2) . ? Co N21 2.147(2) . ? Co O1 2.190(2) . ? Co O2 2.234(2) . ? O1 N1 1.261(3) . ? O2 N1 1.253(3) . ? O3 N1 1.213(3) . ? O4 N2 1.237(4) . ? O5 N2 1.240(5) . ? O6 N2 1.200(4) . ? O7 H1 0.886(2) . ? O7 H2 0.940(2) . ? N11 C11 1.310(3) . ? N11 C13 1.382(3) . ? N12 C12 1.363(4) . ? N12 C11 1.373(3) . ? N12 C15 1.411(4) . ? N21 C21 1.304(4) . ? N21 C23 1.400(4) . ? N22 C21 1.368(4) . ? N22 C22 1.376(4) . ? N22 C25 1.422(5) . ? N31 C31 1.318(3) . ? N31 C33 1.376(3) . ? N32 C31 1.346(3) . ? N32 C32 1.373(4) . ? N32 C35 1.425(4) . ? C11 C14 1.487(4) . ? C12 C13 1.339(4) . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 C16 1.292(4) . ? C15 H15 0.93 . ? C16 H16A 0.93 . ? C16 H16B 0.93 . ? C21 C24 1.467(5) . ? C22 C23 1.333(4) . ? C22 H22 0.93 . ? C23 H23 0.93 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C26 1.257(6) . ? C25 H25 0.93 . ? C26 H26A 0.93 . ? C26 H26B 0.93 . ? C31 C34 1.478(4) . ? C32 C33 1.337(4) . ? C32 H32 0.93 . ? C33 H33 0.93 . ? C34 H34A 0.96 . ? C34 H34B 0.96 . ? C34 H34C 0.96 . ? C35 C36 1.262(5) . ? C35 H35 0.93 . ? C36 H36A 0.93 . ? C36 H36B 0.93 . ? 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 O7 Co N31 103.03(9) . . ? O7 Co N11 91.06(9) . . ? N31 Co N11 93.13(9) . . ? O7 Co N21 88.43(9) . . ? N31 Co N21 91.30(9) . . ? N11 Co N21 175.53(9) . . ? O7 Co O1 152.76(9) . . ? N31 Co O1 104.05(9) . . ? N11 Co O1 90.34(8) . . ? N21 Co O1 88.09(9) . . ? O7 Co O2 95.12(10) . . ? N31 Co O2 161.66(9) . . ? N11 Co O2 89.09(9) . . ? N21 Co O2 86.54(9) . . ? O1 Co O2 57.70(9) . . ? N1 O1 Co 93.9(2) . . ? N1 O2 Co 92.1(2) . . ? Co O7 H1 123.9(2) . . ? Co O7 H2 122.1(2) . . ? H1 O7 H2 112.1(2) . . ? O3 N1 O2 122.3(3) . . ? O3 N1 O1 121.4(3) . . ? O2 N1 O1 116.2(2) . . ? O6 N2 O4 119.4(5) . . ? O6 N2 O5 121.8(5) . . ? O4 N2 O5 118.8(4) . . ? C11 N11 C13 106.1(2) . . ? C11 N11 Co 128.0(2) . . ? C13 N11 Co 125.8(2) . . ? C12 N12 C11 107.0(2) . . ? C12 N12 C15 127.2(2) . . ? C11 N12 C15 125.6(2) . . ? C21 N21 C23 105.9(3) . . ? C21 N21 Co 129.4(2) . . ? C23 N21 Co 124.5(2) . . ? C21 N22 C22 106.5(3) . . ? C21 N22 C25 125.4(3) . . ? C22 N22 C25 128.1(3) . . ? C31 N31 C33 105.9(2) . . ? C31 N31 Co 129.7(2) . . ? C33 N31 Co 124.4(2) . . ? C31 N32 C32 107.8(2) . . ? C31 N32 C35 125.8(3) . . ? C32 N32 C35 126.4(3) . . ? N11 C11 N12 110.2(2) . . ? N11 C11 C14 127.4(3) . . ? N12 C11 C14 122.3(2) . . ? C13 C12 N12 106.8(2) . . ? C13 C12 H12 126.6(2) . . ? N12 C12 H12 126.61(15) . . ? C12 C13 N11 109.8(2) . . ? C12 C13 H13 125.1(2) . . ? N11 C13 H13 125.10(15) . . ? C11 C14 H14A 109.5(2) . . ? C11 C14 H14B 109.5(2) . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5(2) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N12 124.6(3) . . ? C16 C15 H15 117.7(2) . . ? N12 C15 H15 117.7(2) . . ? C15 C16 H16A 120.0(2) . . ? C15 C16 H16B 120.0(2) . . ? H16A C16 H16B 120.0 . . ? N21 C21 N22 111.0(3) . . ? N21 C21 C24 125.8(3) . . ? N22 C21 C24 123.2(3) . . ? C23 C22 N22 107.2(3) . . ? C23 C22 H22 126.4(2) . . ? N22 C22 H22 126.4(2) . . ? C22 C23 N21 109.3(3) . . ? C22 C23 H23 125.4(2) . . ? N21 C23 H23 125.4(2) . . ? C21 C24 H24A 109.5(2) . . ? C21 C24 H24B 109.5(2) . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5(2) . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N22 126.5(5) . . ? C26 C25 H25 116.7(3) . . ? N22 C25 H25 116.7(2) . . ? C25 C26 H26A 120.0(3) . . ? C25 C26 H26B 120.0(3) . . ? H26A C26 H26B 120.0 . . ? N31 C31 N32 110.3(2) . . ? N31 C31 C34 125.3(3) . . ? N32 C31 C34 124.4(3) . . ? C33 C32 N32 105.8(3) . . ? C33 C32 H32 127.1(2) . . ? N32 C32 H32 127.1(2) . . ? C32 C33 N31 110.2(3) . . ? C32 C33 H33 124.9(2) . . ? N31 C33 H33 124.9(2) . . ? C31 C34 H34A 109.5(2) . . ? C31 C34 H34B 109.5(2) . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5(2) . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N32 124.7(4) . . ? C36 C35 H35 117.6(3) . . ? N32 C35 H35 117.6(2) . . ? C35 C36 H36A 120.0(3) . . ? C35 C36 H36B 120.0(3) . . ? H36A C36 H36B 120.0 . . ? 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 O7 Co O1 N1 4.1(3) . . . . ? N31 Co O1 N1 177.8(2) . . . . ? N11 Co O1 N1 -88.9(2) . . . . ? N21 Co O1 N1 86.9(2) . . . . ? O2 Co O1 N1 -0.20(15) . . . . ? O7 Co O2 N1 -177.8(2) . . . . ? N31 Co O2 N1 -6.0(4) . . . . ? N11 Co O2 N1 91.2(2) . . . . ? N21 Co O2 N1 -89.7(2) . . . . ? O1 Co O2 N1 0.20(15) . . . . ? Co O2 N1 O3 -178.7(2) . . . . ? Co O2 N1 O1 -0.3(2) . . . . ? Co O1 N1 O3 178.7(2) . . . . ? Co O1 N1 O2 0.3(2) . . . . ? O7 Co N11 C11 54.2(2) . . . . ? N31 Co N11 C11 -48.9(2) . . . . ? N21 Co N11 C11 137.7(11) . . . . ? O1 Co N11 C11 -153.0(2) . . . . ? O2 Co N11 C11 149.3(2) . . . . ? O7 Co N11 C13 -124.8(2) . . . . ? N31 Co N11 C13 132.0(2) . . . . ? N21 Co N11 C13 -41.4(12) . . . . ? O1 Co N11 C13 28.0(2) . . . . ? O2 Co N11 C13 -29.7(2) . . . . ? O7 Co N21 C21 -156.8(3) . . . . ? N31 Co N21 C21 -53.8(3) . . . . ? N11 Co N21 C21 119.7(11) . . . . ? O1 Co N21 C21 50.2(3) . . . . ? O2 Co N21 C21 108.0(3) . . . . ? O7 Co N21 C23 27.8(2) . . . . ? N31 Co N21 C23 130.8(2) . . . . ? N11 Co N21 C23 -55.8(12) . . . . ? O1 Co N21 C23 -125.2(2) . . . . ? O2 Co N21 C23 -67.5(2) . . . . ? O7 Co N31 C31 -153.6(2) . . . . ? N11 Co N31 C31 -61.7(2) . . . . ? N21 Co N31 C31 117.7(2) . . . . ? O1 Co N31 C31 29.4(2) . . . . ? O2 Co N31 C31 34.8(4) . . . . ? O7 Co N31 C33 28.2(2) . . . . ? N11 Co N31 C33 120.0(2) . . . . ? N21 Co N31 C33 -60.5(2) . . . . ? O1 Co N31 C33 -148.9(2) . . . . ? O2 Co N31 C33 -143.4(3) . . . . ? C13 N11 C11 N12 0.1(3) . . . . ? Co N11 C11 N12 -179.1(2) . . . . ? C13 N11 C11 C14 -179.0(3) . . . . ? Co N11 C11 C14 1.8(4) . . . . ? C12 N12 C11 N11 -0.1(3) . . . . ? C15 N12 C11 N11 176.1(3) . . . . ? C12 N12 C11 C14 179.1(3) . . . . ? C15 N12 C11 C14 -4.7(4) . . . . ? C11 N12 C12 C13 0.1(3) . . . . ? C15 N12 C12 C13 -176.0(3) . . . . ? N12 C12 C13 N11 0.0(3) . . . . ? C11 N11 C13 C12 0.0(3) . . . . ? Co N11 C13 C12 179.2(2) . . . . ? C12 N12 C15 C16 -18.7(5) . . . . ? C11 N12 C15 C16 165.8(3) . . . . ? C23 N21 C21 N22 0.0(3) . . . . ? Co N21 C21 N22 -176.1(2) . . . . ? C23 N21 C21 C24 -179.4(3) . . . . ? Co N21 C21 C24 4.5(5) . . . . ? C22 N22 C21 N21 0.0(3) . . . . ? C25 N22 C21 N21 -178.6(3) . . . . ? C22 N22 C21 C24 179.4(3) . . . . ? C25 N22 C21 C24 0.8(5) . . . . ? C21 N22 C22 C23 0.0(3) . . . . ? C25 N22 C22 C23 178.6(3) . . . . ? N22 C22 C23 N21 0.0(3) . . . . ? C21 N21 C23 C22 0.0(3) . . . . ? Co N21 C23 C22 176.4(2) . . . . ? C21 N22 C25 C26 -174.0(4) . . . . ? C22 N22 C25 C26 7.7(7) . . . . ? C33 N31 C31 N32 -0.3(3) . . . . ? Co N31 C31 N32 -178.8(2) . . . . ? C33 N31 C31 C34 -179.6(3) . . . . ? Co N31 C31 C34 1.9(4) . . . . ? C32 N32 C31 N31 -0.4(3) . . . . ? C35 N32 C31 N31 179.7(3) . . . . ? C32 N32 C31 C34 178.9(3) . . . . ? C35 N32 C31 C34 -1.0(5) . . . . ? C31 N32 C32 C33 1.0(3) . . . . ? C35 N32 C32 C33 -179.1(3) . . . . ? N32 C32 C33 N31 -1.2(4) . . . . ? C31 N31 C33 C32 1.0(3) . . . . ? Co N31 C33 C32 179.6(2) . . . . ? C31 N32 C35 C36 159.8(4) . . . . ? C32 N32 C35 C36 -20.1(6) . . . . ? _refine_diff_density_max 0.539 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.060 #======== END data_[CuL2(NO3)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Cu N6 O6' _chemical_formula_weight 403.85 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2610(10) _cell_length_b 7.931(2) _cell_length_c 14.743(3) _cell_angle_alpha 103.78(3) _cell_angle_beta 95.39(3) _cell_angle_gamma 94.78(3) _cell_volume 816.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _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 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 414 _exptl_absorpt_coefficient_mu 1.382 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kuma KM4CCD' _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 5089 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 28.86 _reflns_number_total 3437 _reflns_number_gt 3323 _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^)+(0.0380P)^2^+0.9046P] 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 3437 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu Cu 0.13527(3) 0.49137(3) 0.261122(14) 0.01439(8) Uani 1 d . . . O1 O -0.09615(18) 0.59648(17) 0.22211(9) 0.0173(3) Uani 1 d . . . O2 O -0.0841(2) 0.5961(2) 0.37018(10) 0.0245(3) Uani 1 d . . . O3 O -0.3017(2) 0.71891(19) 0.30554(11) 0.0250(3) Uani 1 d . . . O4 O 0.26648(19) 0.73465(18) 0.28881(10) 0.0206(3) Uani 1 d . . . O5 O 0.2953(2) 0.60036(18) 0.14668(10) 0.0221(3) Uani 1 d . . . O6 O 0.3920(2) 0.87659(19) 0.19526(12) 0.0269(3) Uani 1 d . . . N1 N -0.1640(2) 0.6398(2) 0.30162(11) 0.0175(3) Uani 1 d . . . N2 N 0.3216(2) 0.7400(2) 0.20877(12) 0.0182(3) Uani 1 d . . . N11 N 0.3045(2) 0.4063(2) 0.34824(11) 0.0162(3) Uani 1 d . . . N12 N 0.4994(2) 0.2447(2) 0.40220(11) 0.0164(3) Uani 1 d . . . N21 N 0.0227(2) 0.2550(2) 0.19593(11) 0.0173(3) Uani 1 d . . . N22 N -0.1488(2) 0.0352(2) 0.09884(11) 0.0156(3) Uani 1 d . . . C11 C 0.4470(2) 0.3152(2) 0.32908(13) 0.0151(3) Uani 1 d . . . C12 C 0.3846(3) 0.2943(3) 0.47134(13) 0.0185(4) Uani 1 d . . . C13 C 0.2647(3) 0.3927(3) 0.43698(13) 0.0184(4) Uani 1 d . . . C14 C 0.5358(3) 0.2915(2) 0.24065(13) 0.0179(4) Uani 1 d . . . C15 C 0.6451(3) 0.1362(3) 0.40432(15) 0.0224(4) Uani 1 d . . . C16 C 0.7348(3) 0.1150(3) 0.48217(16) 0.0273(4) Uani 1 d . . . C21 C -0.0781(2) 0.2049(2) 0.11296(13) 0.0174(4) Uani 1 d . . . C22 C -0.0877(3) -0.0248(3) 0.17698(14) 0.0219(4) Uani 1 d . . . C23 C 0.0175(3) 0.1096(3) 0.23613(14) 0.0210(4) Uani 1 d . . . C24 C -0.1109(3) 0.3145(3) 0.04503(15) 0.0226(4) Uani 1 d . . . C25 C -0.2646(3) -0.0645(3) 0.01824(14) 0.0232(4) Uani 1 d . . . C26 C -0.3438(3) -0.2219(3) 0.01338(17) 0.0280(4) Uani 1 d . . . H1 H 0.172(4) 0.450(3) 0.4659(18) 0.024(6) Uiso 1 d . . . H2 H 0.396(3) 0.257(3) 0.5294(18) 0.022(6) Uiso 1 d . . . H3 H 0.494(4) 0.180(4) 0.206(2) 0.032(7) Uiso 1 d . . . H4 H 0.497(4) 0.377(4) 0.2082(19) 0.030(7) Uiso 1 d . . . H5 H 0.667(4) 0.305(4) 0.254(2) 0.033(7) Uiso 1 d . . . H6 H 0.672(4) 0.076(3) 0.3432(19) 0.026(6) Uiso 1 d . . . H7 H 0.826(4) 0.039(4) 0.479(2) 0.033(7) Uiso 1 d . . . H8 H 0.710(4) 0.172(4) 0.542(2) 0.041(8) Uiso 1 d . . . H9 H 0.072(4) 0.106(3) 0.2966(19) 0.026(6) Uiso 1 d . . . H10 H -0.120(4) -0.145(4) 0.183(2) 0.033(7) Uiso 1 d . . . H11 H -0.025(4) 0.413(4) 0.063(2) 0.042(8) Uiso 1 d . . . H12 H -0.236(4) 0.350(4) 0.048(2) 0.041(8) Uiso 1 d . . . H13 H -0.102(5) 0.251(5) -0.015(3) 0.051(9) Uiso 1 d . . . H14 H -0.275(4) 0.000(4) -0.033(2) 0.038(8) Uiso 1 d . . . H15 H -0.335(4) -0.272(4) 0.065(2) 0.033(7) Uiso 1 d . . . H16 H -0.411(4) -0.285(4) -0.040(2) 0.041(8) Uiso 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 Cu 0.01413(12) 0.01441(12) 0.01500(12) 0.00448(9) 0.00143(8) 0.00146(8) O1 0.0204(6) 0.0183(6) 0.0146(6) 0.0048(5) 0.0039(5) 0.0053(5) O2 0.0236(7) 0.0356(8) 0.0180(6) 0.0114(6) 0.0042(6) 0.0090(6) O3 0.0207(7) 0.0255(7) 0.0307(8) 0.0062(6) 0.0063(6) 0.0118(5) O4 0.0230(7) 0.0188(6) 0.0185(6) 0.0031(5) 0.0028(5) -0.0019(5) O5 0.0257(7) 0.0214(7) 0.0179(6) 0.0034(6) 0.0030(6) 0.0002(5) O6 0.0265(7) 0.0205(7) 0.0377(8) 0.0154(6) 0.0060(7) -0.0015(5) N1 0.0178(7) 0.0157(7) 0.0195(7) 0.0044(6) 0.0045(6) 0.0024(5) N2 0.0160(7) 0.0189(7) 0.0214(8) 0.0087(6) 0.0023(6) 0.0012(5) N11 0.0151(7) 0.0179(7) 0.0160(7) 0.0048(6) 0.0018(6) 0.0021(5) N12 0.0183(7) 0.0168(7) 0.0142(7) 0.0038(6) 0.0014(6) 0.0031(6) N21 0.0144(7) 0.0175(7) 0.0198(7) 0.0035(6) 0.0036(6) 0.0026(5) N22 0.0161(7) 0.0161(7) 0.0153(7) 0.0048(6) 0.0022(6) 0.0022(5) C11 0.0146(8) 0.0149(8) 0.0150(8) 0.0034(7) 0.0001(6) -0.0007(6) C12 0.0199(9) 0.0216(9) 0.0142(8) 0.0045(7) 0.0036(7) 0.0014(7) C13 0.0173(8) 0.0222(9) 0.0151(8) 0.0026(7) 0.0038(7) 0.0021(7) C14 0.0191(9) 0.0179(8) 0.0179(8) 0.0054(7) 0.0041(7) 0.0027(7) C15 0.0232(9) 0.0233(9) 0.0224(9) 0.0061(8) 0.0044(8) 0.0090(7) C16 0.0274(10) 0.0276(10) 0.0266(10) 0.0073(9) -0.0036(8) 0.0068(8) C21 0.0142(8) 0.0195(8) 0.0191(8) 0.0048(7) 0.0043(7) 0.0033(6) C22 0.0253(10) 0.0191(9) 0.0228(9) 0.0081(8) 0.0024(8) 0.0026(7) C23 0.0225(9) 0.0211(9) 0.0199(9) 0.0065(8) 0.0003(7) 0.0039(7) C24 0.0246(10) 0.0216(9) 0.0220(9) 0.0064(8) 0.0025(8) 0.0021(7) C25 0.0216(9) 0.0261(9) 0.0198(9) 0.0027(8) 0.0001(8) 0.0022(7) C26 0.0278(10) 0.0263(10) 0.0253(10) 0.0014(9) -0.0019(9) -0.0036(8) _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 Cu N21 1.9605(17) . ? Cu N11 1.9673(16) . ? Cu O4 2.0106(15) . ? Cu O1 2.0322(14) . ? Cu O5 2.4167(16) . ? Cu O2 2.4246(16) . ? O1 N1 1.296(2) . ? O2 N1 1.253(2) . ? O3 N1 1.223(2) . ? O4 N2 1.290(2) . ? O5 N2 1.245(2) . ? O6 N2 1.226(2) . ? N11 C11 1.324(2) . ? N11 C13 1.393(2) . ? N12 C11 1.366(2) . ? N12 C12 1.383(2) . ? N12 C15 1.421(2) . ? N21 C21 1.320(2) . ? N21 C23 1.416(3) . ? N22 C21 1.360(2) . ? N22 C22 1.397(3) . ? N22 C25 1.413(2) . ? C11 C14 1.487(3) . ? C12 C13 1.358(3) . ? C12 H2 0.97(3) . ? C13 H1 0.92(3) . ? C14 H3 0.92(3) . ? C14 H4 0.96(3) . ? C14 H5 0.95(3) . ? C15 C16 1.319(3) . ? C15 H6 0.96(3) . ? C16 H7 0.93(3) . ? C16 H8 0.93(3) . ? C21 C24 1.490(3) . ? C22 C23 1.333(3) . ? C22 H10 0.99(3) . ? C23 H9 0.95(3) . ? C24 H11 0.93(3) . ? C24 H12 0.98(3) . ? C24 H13 0.92(4) . ? C25 C26 1.313(3) . ? C25 H14 1.01(3) . ? C26 H15 0.94(3) . ? C26 H16 0.90(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 N21 Cu N11 92.96(7) . . ? N21 Cu O4 162.82(7) . . ? N11 Cu O4 96.36(7) . . ? N21 Cu O1 91.49(6) . . ? N11 Cu O1 155.05(6) . . ? O4 Cu O1 86.13(6) . . ? N21 Cu O5 105.77(6) . . ? N11 Cu O5 112.59(6) . . ? O4 Cu O5 57.25(6) . . ? O1 Cu O5 89.67(6) . . ? N21 Cu O2 103.44(7) . . ? N11 Cu O2 97.43(6) . . ? O4 Cu O2 89.66(6) . . ? O1 Cu O2 57.69(5) . . ? O5 Cu O2 136.32(5) . . ? N1 O1 Cu 100.84(10) . . ? N1 O2 Cu 83.89(10) . . ? N2 O4 Cu 102.07(11) . . ? N2 O5 Cu 84.28(11) . . ? O3 N1 O2 123.84(17) . . ? O3 N1 O1 118.80(16) . . ? O2 N1 O1 117.36(15) . . ? O6 N2 O5 122.77(17) . . ? O6 N2 O4 121.15(17) . . ? O5 N2 O4 116.06(15) . . ? C11 N11 C13 106.26(15) . . ? C11 N11 Cu 128.21(13) . . ? C13 N11 Cu 123.66(12) . . ? C11 N12 C12 108.30(15) . . ? C11 N12 C15 124.93(16) . . ? C12 N12 C15 126.76(16) . . ? C21 N21 C23 107.23(16) . . ? C21 N21 Cu 127.66(14) . . ? C23 N21 Cu 124.72(13) . . ? C21 N22 C22 108.79(16) . . ? C21 N22 C25 125.70(17) . . ? C22 N22 C25 125.52(17) . . ? N11 C11 N12 109.96(16) . . ? N11 C11 C14 125.11(17) . . ? N12 C11 C14 124.92(16) . . ? C13 C12 N12 105.48(17) . . ? C13 C12 H2 132.2(15) . . ? N12 C12 H2 122.3(15) . . ? C12 C13 N11 109.99(17) . . ? C12 C13 H1 128.4(16) . . ? N11 C13 H1 121.6(16) . . ? C11 C14 H3 106.2(18) . . ? C11 C14 H4 108.6(17) . . ? H3 C14 H4 111(2) . . ? C11 C14 H5 110.3(17) . . ? H3 C14 H5 110(2) . . ? H4 C14 H5 110(2) . . ? C16 C15 N12 124.1(2) . . ? C16 C15 H6 122.0(15) . . ? N12 C15 H6 113.9(15) . . ? C15 C16 H7 120.2(18) . . ? C15 C16 H8 122.9(19) . . ? H7 C16 H8 117(3) . . ? N21 C21 N22 108.92(17) . . ? N21 C21 C24 126.19(17) . . ? N22 C21 C24 124.89(17) . . ? C23 C22 N22 106.04(17) . . ? C23 C22 H10 130.0(16) . . ? N22 C22 H10 124.0(16) . . ? C22 C23 N21 109.02(17) . . ? C22 C23 H9 123.6(16) . . ? N21 C23 H9 127.3(16) . . ? C21 C24 H11 108.1(19) . . ? C21 C24 H12 108.7(18) . . ? H11 C24 H12 109(3) . . ? C21 C24 H13 110(2) . . ? H11 C24 H13 112(3) . . ? H12 C24 H13 109(3) . . ? C26 C25 N22 122.4(2) . . ? C26 C25 H14 126.0(17) . . ? N22 C25 H14 111.6(17) . . ? C25 C26 H15 122.0(17) . . ? C25 C26 H16 121(2) . . ? H15 C26 H16 117(3) . . ? _diffrn_measured_fraction_theta_max 0.805 _diffrn_reflns_theta_full 28.86 _diffrn_measured_fraction_theta_full 0.805 _refine_diff_density_max 0.586 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.067