# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1610 data_global #============================================================================== _publ_contact_author_name 'Professor Tian-Huey Lu' _publ_contact_author_address ; Department of Physics National Tsing Hua University Hsinchu, Taiwan 300, R.O.C. ; _publ_contact_author_email thlu@phys.nthu.edu.tw _publ_contact_author_fax +886-3-572-3052 _publ_contact_author_phone +886-3-574-2543 _publ_contact_letter ? _publ_requested_journal 'J. Chem. Soc., Dalton Trans' _publ_requested_category 'Full paper' _publ_section_title ; Cu(II) complexes of C-meso-1,5,8,12-tetramethyl-1,4,8,11- tetraazacyclotetradecane: Syntheses, structures and properties ; loop_ _publ_author_name _publ_author_address 'Lu, Tian-Huey' ; Department of Physics National Tsing Hua University Hsinchu, Taiwan 300, R.O.C. ; 'Lin, Shih-Chi' ; Department of Chemistry National Tsing Hua University Hsinchu, Taiwan 300, R.O.C. ; 'Aneetha, Halikhedkar' ; Department of Chemistry National Tsing Hua University Hsinchu, Taiwan 300, R.O.C. ; 'Panneerselvam, Kaliyamoorthy' ; Department of Physics National Tsing Hua University Hsinchu, Taiwan 300, R.O.C. ; 'Chung, Chung-Sun' ; Department of Chemistry National Tsing Hua University Hsinchu, Taiwan 300, R.O.C. ; #============================================================================== data_[CuL1(ClO4)](ClO4),1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 Cl2 Cu N4 O8' _chemical_formula_weight 518.88 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' 'Cl' 'Cl' 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P21/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 9.6358(1) _cell_length_b 14.5935(2) _cell_length_c 15.1412(1) _cell_angle_alpha 90.00 _cell_angle_beta 94.718(1) _cell_angle_gamma 90.00 _cell_volume 2121.94(4) _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 purple _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 1.330 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'SMART CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12359 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.06 _reflns_number_total 4636 _reflns_number_gt 3996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART CCD (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'NRCVAX (Gabe, et al., 1989)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1246P)^2^+13.7073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom method' _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 4636 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1215 _refine_ls_R_factor_gt 0.1103 _refine_ls_wR_factor_ref 0.2966 _refine_ls_wR_factor_gt 0.2865 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_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_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 Cu1 Cu 0.24243(8) 0.10685(6) 0.23960(5) 0.0333(3) Uani 1 1 d . . . Cl1 Cl 0.2382(2) -0.14237(11) 0.15531(12) 0.0441(5) Uani 1 1 d . . . Cl2 Cl 0.6633(3) 0.36165(14) 0.21554(18) 0.0587(6) Uani 1 1 d . . . O1 O 0.2085(7) -0.2179(4) 0.2105(4) 0.0563(15) Uani 1 1 d . . . O2 O 0.1874(8) -0.0585(4) 0.1910(4) 0.0617(17) Uani 1 1 d . . . O3 O 0.3861(9) -0.1348(5) 0.1556(6) 0.074(2) Uani 1 1 d . . . O4 O 0.1788(10) -0.1556(5) 0.0677(5) 0.081(2) Uani 1 1 d . . . O5 O 0.5382(11) 0.3720(10) 0.1581(8) 0.125(4) Uani 1 1 d . . . O6 O 0.6542(11) 0.2779(6) 0.2603(9) 0.118(4) Uani 1 1 d . . . O7 O 0.6656(12) 0.4363(7) 0.2746(9) 0.129(4) Uani 1 1 d . . . O8 O 0.7798(12) 0.3630(8) 0.1654(9) 0.120(4) Uani 1 1 d . . . N1 N 0.1488(7) 0.1530(4) 0.1209(4) 0.0376(13) Uani 1 1 d . . . N2 N 0.0494(6) 0.0992(4) 0.2813(4) 0.0392(13) Uani 1 1 d . . . H1N2 H 0.0272 0.0386 0.2814 0.080 Uiso 1 1 calc R . . N3 N 0.3403(7) 0.0633(4) 0.3584(4) 0.0378(13) Uani 1 1 d . . . N4 N 0.4362(7) 0.1236(4) 0.2006(4) 0.0365(13) Uani 1 1 d . . . H1N4 H 0.4575 0.1842 0.2059 0.080 Uiso 1 1 calc R . . C1 C 0.0292(11) 0.2010(7) 0.1490(7) 0.068(3) Uani 1 1 d . . . H1A H -0.0325 0.2171 0.0974 0.080 Uiso 1 1 calc R . . H1B H 0.0593 0.2572 0.1788 0.080 Uiso 1 1 calc R . . C2 C -0.0488(9) 0.1427(6) 0.2108(7) 0.057(2) Uani 1 1 d . . . H2A H -0.1157 0.1804 0.2386 0.080 Uiso 1 1 calc R . . H2B H -0.0997 0.0952 0.1771 0.080 Uiso 1 1 calc R . . C3 C 0.0297(10) 0.1334(5) 0.3717(6) 0.049(2) Uani 1 1 d . . . H3 H 0.0523 0.1989 0.3727 0.080 Uiso 1 1 calc R . . C4 C 0.1276(11) 0.0874(9) 0.4413(7) 0.066(3) Uani 1 1 d . . . H4A H 0.1135 0.0217 0.4373 0.080 Uiso 1 1 calc R . . H4B H 0.1034 0.1067 0.4993 0.080 Uiso 1 1 calc R . . C5 C 0.2807(12) 0.1075(7) 0.4338(7) 0.062(2) Uani 1 1 d . . . H5A H 0.2926 0.1733 0.4289 0.080 Uiso 1 1 calc R . . H5B H 0.3329 0.0878 0.4880 0.080 Uiso 1 1 calc R . . C6 C 0.4846(11) 0.0865(8) 0.3552(7) 0.064(3) Uani 1 1 d . . . H6A H 0.5403 0.0488 0.3973 0.080 Uiso 1 1 calc R . . H6B H 0.4985 0.1501 0.3727 0.080 Uiso 1 1 calc R . . C7 C 0.5327(8) 0.0730(6) 0.2649(5) 0.0454(17) Uani 1 1 d . . . H7A H 0.6268 0.0961 0.2629 0.080 Uiso 1 1 calc R . . H7B H 0.5325 0.0083 0.2502 0.080 Uiso 1 1 calc R . . C8 C 0.4490(9) 0.0972(6) 0.1066(5) 0.0452(18) Uani 1 1 d . . . H8 H 0.4046 0.0374 0.0955 0.080 Uiso 1 1 calc R . . C9 C 0.3728(12) 0.1689(8) 0.0464(7) 0.069(3) Uani 1 1 d . . . H9A H 0.3442 0.1396 -0.0096 0.080 Uiso 1 1 calc R . . H9B H 0.4394 0.2163 0.0344 0.080 Uiso 1 1 calc R . . C10 C 0.2420(12) 0.2169(7) 0.0803(7) 0.066(3) Uani 1 1 d . . . H10A H 0.2726 0.2634 0.1234 0.080 Uiso 1 1 calc R . . H10B H 0.1908 0.2475 0.0309 0.080 Uiso 1 1 calc R . . C11 C 0.1065(15) 0.0818(7) 0.0519(8) 0.084(4) Uani 1 1 d . . . H11A H 0.0346 0.0438 0.0726 0.080 Uiso 1 1 calc R . . H11B H 0.1856 0.0446 0.0412 0.080 Uiso 1 1 calc R . . H11C H 0.0724 0.1115 -0.0021 0.080 Uiso 1 1 calc R . . C12 C -0.1181(11) 0.1241(7) 0.3953(7) 0.062(2) Uani 1 1 d . . . H12A H -0.1211 0.1312 0.4582 0.080 Uiso 1 1 calc R . . H12B H -0.1531 0.0648 0.3777 0.080 Uiso 1 1 calc R . . H12C H -0.1744 0.1706 0.3652 0.080 Uiso 1 1 calc R . . C13 C 0.3268(15) -0.0395(7) 0.3708(8) 0.083(4) Uani 1 1 d . . . H13A H 0.3694 -0.0565 0.4280 0.080 Uiso 1 1 calc R . . H13B H 0.3725 -0.0708 0.3256 0.080 Uiso 1 1 calc R . . H13C H 0.2301 -0.0561 0.3667 0.080 Uiso 1 1 calc R . . C14 C 0.6009(10) 0.0914(8) 0.0841(7) 0.065(3) Uani 1 1 d . . . H14A H 0.6474 0.0433 0.1181 0.080 Uiso 1 1 calc R . . H14B H 0.6466 0.1487 0.0980 0.080 Uiso 1 1 calc R . . H14C H 0.6037 0.0787 0.0220 0.080 Uiso 1 1 calc R . . 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 Cu1 0.0366(5) 0.0256(5) 0.0370(5) 0.0043(3) -0.0019(3) 0.0040(3) Cl1 0.0684(13) 0.0185(8) 0.0445(10) 0.0034(6) 0.0004(8) 0.0007(7) Cl2 0.0598(13) 0.0278(9) 0.0884(17) -0.0010(9) 0.0062(11) 0.0027(8) O1 0.079(4) 0.030(3) 0.060(3) 0.013(3) 0.007(3) -0.003(3) O2 0.095(5) 0.020(3) 0.070(4) -0.012(3) 0.003(3) 0.017(3) O3 0.076(5) 0.043(4) 0.105(6) -0.003(4) 0.016(4) -0.010(3) O4 0.134(7) 0.041(4) 0.063(4) -0.005(3) -0.016(4) 0.009(4) O5 0.077(6) 0.192(14) 0.105(8) 0.013(8) -0.006(5) 0.011(7) O6 0.117(8) 0.041(4) 0.199(12) 0.035(6) 0.026(7) -0.003(5) O7 0.132(9) 0.060(6) 0.195(12) -0.066(7) 0.020(8) -0.012(6) O8 0.095(7) 0.114(9) 0.157(11) 0.016(7) 0.048(7) 0.016(6) N1 0.047(3) 0.024(3) 0.041(3) 0.005(2) -0.007(3) 0.002(2) N2 0.041(3) 0.029(3) 0.048(3) 0.000(3) 0.006(3) -0.004(3) N3 0.047(3) 0.023(3) 0.042(3) 0.007(2) -0.005(3) 0.002(2) N4 0.046(3) 0.021(3) 0.042(3) 0.000(2) 0.001(3) 0.002(2) C1 0.067(6) 0.048(5) 0.086(7) 0.003(5) -0.016(5) 0.015(5) C2 0.037(4) 0.049(5) 0.084(6) 0.014(5) -0.003(4) 0.009(4) C3 0.060(5) 0.030(4) 0.060(5) -0.013(3) 0.014(4) -0.017(3) C4 0.065(6) 0.081(8) 0.054(5) -0.001(5) 0.009(4) -0.013(5) C5 0.079(7) 0.049(5) 0.057(5) 0.003(4) 0.003(5) -0.002(5) C6 0.064(6) 0.063(6) 0.064(6) 0.008(5) -0.008(5) 0.001(5) C7 0.046(4) 0.040(4) 0.049(4) 0.001(3) -0.005(3) 0.004(3) C8 0.050(4) 0.043(4) 0.043(4) -0.001(3) 0.005(3) -0.003(3) C9 0.078(7) 0.073(7) 0.057(5) 0.021(5) 0.011(5) 0.026(6) C10 0.091(7) 0.037(5) 0.068(6) 0.011(4) -0.003(5) 0.001(5) C11 0.130(11) 0.038(5) 0.078(7) -0.014(5) -0.033(7) 0.025(6) C12 0.068(6) 0.051(5) 0.071(6) -0.008(5) 0.024(5) 0.000(4) C13 0.137(11) 0.032(5) 0.077(7) 0.020(5) -0.013(7) -0.003(6) C14 0.059(5) 0.075(7) 0.062(6) -0.011(5) 0.016(4) 0.003(5) _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 Cu1 N2 2.016(6) . ? Cu1 N4 2.019(7) . ? Cu1 N1 2.057(6) . ? Cu1 N3 2.061(6) . ? Cl1 O4 1.415(8) . ? Cl1 O1 1.426(6) . ? Cl1 O3 1.429(8) . ? Cl1 O2 1.440(5) . ? Cl2 O6 1.404(9) . ? Cl2 O8 1.406(11) . ? Cl2 O7 1.408(9) . ? Cl2 O5 1.435(11) . ? N1 C1 1.442(12) . ? N1 C10 1.464(12) . ? N1 C11 1.506(12) . ? N2 C3 1.485(10) . ? N2 C2 1.507(11) . ? N2 H1N2 0.9100 . ? N3 C6 1.436(12) . ? N3 C5 1.469(12) . ? N3 C13 1.519(11) . ? N4 C7 1.487(10) . ? N4 C8 1.489(10) . ? N4 H1N4 0.9100 . ? C1 C2 1.510(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C12 1.503(13) . ? C3 C4 1.512(14) . ? C3 H3 0.9800 . ? C4 C5 1.517(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.493(13) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C14 1.532(12) . ? C8 C9 1.535(12) . ? C8 H8 0.9800 . ? C9 C10 1.565(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 N2 Cu1 N4 176.1(2) . . ? N2 Cu1 N1 86.7(3) . . ? N4 Cu1 N1 93.1(3) . . ? N2 Cu1 N3 94.5(3) . . ? N4 Cu1 N3 85.7(2) . . ? N1 Cu1 N3 178.4(2) . . ? O4 Cl1 O1 111.0(4) . . ? O4 Cl1 O3 109.9(6) . . ? O1 Cl1 O3 107.8(4) . . ? O4 Cl1 O2 110.1(4) . . ? O1 Cl1 O2 110.2(4) . . ? O3 Cl1 O2 107.7(4) . . ? O6 Cl2 O8 110.9(7) . . ? O6 Cl2 O7 111.4(8) . . ? O8 Cl2 O7 111.1(7) . . ? O6 Cl2 O5 107.5(7) . . ? O8 Cl2 O5 109.8(8) . . ? O7 Cl2 O5 105.8(8) . . ? C1 N1 C10 110.3(7) . . ? C1 N1 C11 111.2(8) . . ? C10 N1 C11 106.8(8) . . ? C1 N1 Cu1 101.8(5) . . ? C10 N1 Cu1 109.6(5) . . ? C11 N1 Cu1 117.0(5) . . ? C3 N2 C2 113.0(7) . . ? C3 N2 Cu1 117.5(5) . . ? C2 N2 Cu1 107.3(5) . . ? C3 N2 H1N2 106.1 . . ? C2 N2 H1N2 106.1 . . ? Cu1 N2 H1N2 106.1 . . ? C6 N3 C5 111.3(7) . . ? C6 N3 C13 109.3(8) . . ? C5 N3 C13 107.1(8) . . ? C6 N3 Cu1 105.8(5) . . ? C5 N3 Cu1 111.3(5) . . ? C13 N3 Cu1 112.0(6) . . ? C7 N4 C8 113.6(6) . . ? C7 N4 Cu1 107.0(5) . . ? C8 N4 Cu1 113.6(5) . . ? C7 N4 H1N4 107.5 . . ? C8 N4 H1N4 107.5 . . ? Cu1 N4 H1N4 107.5 . . ? N1 C1 C2 111.1(8) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 111.2(7) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C12 112.6(7) . . ? N2 C3 C4 111.9(8) . . ? C12 C3 C4 110.1(8) . . ? N2 C3 H3 107.3 . . ? C12 C3 H3 107.3 . . ? C4 C3 H3 107.3 . . ? C3 C4 C5 114.6(8) . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N3 C5 C4 114.7(8) . . ? N3 C5 H5A 108.6 . . ? C4 C5 H5A 108.6 . . ? N3 C5 H5B 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N3 C6 C7 111.9(8) . . ? N3 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N3 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N4 C7 C6 108.0(7) . . ? N4 C7 H7A 110.1 . . ? C6 C7 H7A 110.1 . . ? N4 C7 H7B 110.1 . . ? C6 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? N4 C8 C14 112.5(7) . . ? N4 C8 C9 108.5(7) . . ? C14 C8 C9 108.9(8) . . ? N4 C8 H8 109.0 . . ? C14 C8 H8 109.0 . . ? C9 C8 H8 109.0 . . ? C8 C9 C10 118.0(8) . . ? C8 C9 H9A 107.8 . . ? C10 C9 H9A 107.8 . . ? C8 C9 H9B 107.8 . . ? C10 C9 H9B 107.8 . . ? H9A C9 H9B 107.1 . . ? N1 C10 C9 113.0(8) . . ? N1 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 C12 H12A 109.5 . . ? C3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.658 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.215 #--------------------------------------END----------------------------------- data_[CuL1(N3)],2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 Cu N10' _chemical_formula_weight 404.04 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 7.3939(1) _cell_length_b 16.1227(3) _cell_length_c 8.5698(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.381(1) _cell_angle_gamma 90.00 _cell_volume 930.50(3) _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 blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 430 _exptl_absorpt_coefficient_mu 1.194 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'SMART CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5049 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.64 _reflns_number_total 1971 _reflns_number_gt 1490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART CCD (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'NRCVAX (Gabe, et al., 1989)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1971 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.0000 0.03389(18) Uani 1 2 d S . . N1 N 0.0105(3) -0.09796(12) 0.1632(3) 0.0350(5) Uani 1 1 d . . . N2 N 0.1879(3) 0.06166(13) 0.2142(3) 0.0350(5) Uani 1 1 d . . . H1N2 H 0.3099 0.0602 0.2121 0.060 Uiso 1 1 calc R . . N3 N -0.3045(4) 0.06357(16) 0.0089(3) 0.0503(6) Uani 1 1 d . . . N4 N -0.3429(3) 0.07649(13) 0.1281(3) 0.0401(5) Uani 1 1 d . . . N5 N -0.3805(4) 0.08950(16) 0.2460(3) 0.0541(6) Uani 1 1 d . . . C1 C 0.1946(4) -0.07983(17) 0.3170(3) 0.0433(7) Uani 1 1 d . . . H1A H 0.3093 -0.0939 0.2947 0.060 Uiso 1 1 calc R . . H1B H 0.1984 -0.1134 0.4122 0.060 Uiso 1 1 calc R . . C2 C 0.2029(5) 0.01100(16) 0.3634(4) 0.0451(7) Uani 1 1 d . . . H2A H 0.0942 0.0244 0.3946 0.060 Uiso 1 1 calc R . . H2B H 0.3267 0.0230 0.4608 0.060 Uiso 1 1 calc R . . C3 C 0.1452(4) 0.15093(16) 0.2331(4) 0.0401(6) Uani 1 1 d . . . H3 H 0.0152 0.1544 0.2379 0.060 Uiso 1 1 calc R . . C4 C 0.1363(4) 0.20092(16) 0.0792(4) 0.0442(7) Uani 1 1 d . . . H4A H 0.1254 0.2592 0.1023 0.060 Uiso 1 1 calc R . . H4B H 0.2612 0.1937 0.0689 0.060 Uiso 1 1 calc R . . C5 C -0.0312(4) 0.17974(16) -0.0922(3) 0.0419(6) Uani 1 1 d . . . H5A H -0.1554 0.1805 -0.0793 0.060 Uiso 1 1 calc R . . H5B H -0.0384 0.2225 -0.1742 0.060 Uiso 1 1 calc R . . C6 C -0.1604(4) -0.10154(18) 0.2113(4) 0.0475(7) Uani 1 1 d . . . H6A H -0.1602 -0.0531 0.2765 0.060 Uiso 1 1 calc R . . H6B H -0.1497 -0.1502 0.2791 0.060 Uiso 1 1 calc R . . H6C H -0.2818 -0.1036 0.1096 0.060 Uiso 1 1 calc R . . C7 C 0.2999(4) 0.18970(19) 0.3967(4) 0.0535(8) Uani 1 1 d . . . H7A H 0.2974 0.1618 0.4947 0.060 Uiso 1 1 calc R . . H7B H 0.2700 0.2474 0.4009 0.060 Uiso 1 1 calc R . . H7C H 0.4294 0.1842 0.3971 0.060 Uiso 1 1 calc R . . 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 Cu1 0.0431(3) 0.0293(3) 0.0311(3) 0.00144(17) 0.01711(19) -0.00035(18) N1 0.0401(12) 0.0332(11) 0.0365(11) 0.0035(9) 0.0206(10) 0.0033(9) N2 0.0390(11) 0.0346(11) 0.0359(11) -0.0010(9) 0.0200(9) 0.0005(9) N3 0.0532(15) 0.0528(14) 0.0538(15) -0.0036(11) 0.0311(12) -0.0029(11) N4 0.0375(12) 0.0341(12) 0.0509(14) 0.0011(10) 0.0204(11) -0.0004(9) N5 0.0623(16) 0.0563(16) 0.0530(15) -0.0061(12) 0.0331(13) 0.0012(12) C1 0.0496(15) 0.0452(16) 0.0329(14) 0.0073(11) 0.0147(12) 0.0040(12) C2 0.0559(17) 0.0485(17) 0.0336(14) 0.0015(11) 0.0210(13) -0.0023(13) C3 0.0444(14) 0.0355(14) 0.0459(16) -0.0094(11) 0.0243(12) -0.0010(11) C4 0.0519(16) 0.0309(13) 0.0544(17) -0.0034(12) 0.0264(14) -0.0029(12) C5 0.0517(16) 0.0295(13) 0.0499(17) 0.0054(12) 0.0263(14) 0.0057(11) C6 0.0574(18) 0.0437(16) 0.0557(17) 0.0059(13) 0.0377(15) 0.0027(13) C7 0.0573(18) 0.0509(17) 0.0536(18) -0.0153(14) 0.0242(16) -0.0073(14) _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 Cu1 N2 2.045(2) . ? Cu1 N2 2.045(2) 3 ? Cu1 N1 2.090(2) 3 ? Cu1 N1 2.090(2) . ? N1 C1 1.481(3) . ? N1 C6 1.484(3) . ? N1 C5 1.486(3) 3 ? N2 C2 1.483(3) . ? N2 C3 1.497(3) . ? N2 H1N2 0.9100 . ? N3 N4 1.186(3) . ? N4 N5 1.172(3) . ? C1 C2 1.512(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.524(4) . ? C3 C7 1.530(4) . ? C3 H3 0.9800 . ? C4 C5 1.518(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.486(3) 3 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 N2 Cu1 N2 180.0 . 3 ? N2 Cu1 N1 93.27(8) . 3 ? N2 Cu1 N1 86.73(8) 3 3 ? N2 Cu1 N1 86.73(8) . . ? N2 Cu1 N1 93.27(8) 3 . ? N1 Cu1 N1 180.0 3 . ? C1 N1 C6 109.6(2) . . ? C1 N1 C5 109.1(2) . 3 ? C6 N1 C5 108.8(2) . 3 ? C1 N1 Cu1 102.31(15) . . ? C6 N1 Cu1 114.51(16) . . ? C5 N1 Cu1 112.25(15) 3 . ? C2 N2 C3 112.3(2) . . ? C2 N2 Cu1 106.70(16) . . ? C3 N2 Cu1 117.97(17) . . ? C2 N2 H1N2 106.4 . . ? C3 N2 H1N2 106.4 . . ? Cu1 N2 H1N2 106.4 . . ? N5 N4 N3 179.8(3) . . ? N1 C1 C2 110.3(2) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 109.0(2) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N2 C3 C4 110.5(2) . . ? N2 C3 C7 112.4(2) . . ? C4 C3 C7 109.0(2) . . ? N2 C3 H3 108.3 . . ? C4 C3 H3 108.3 . . ? C7 C3 H3 108.3 . . ? C5 C4 C3 116.4(2) . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4B 108.2 . . ? C3 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? N1 C5 C4 114.5(2) 3 . ? N1 C5 H5A 108.6 3 . ? C4 C5 H5A 108.6 . . ? N1 C5 H5B 108.6 3 . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.403 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.066 #------------------------------------END--------------------------------------- data_[CuL1(H2O)2](NO2)2,3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H36 Cu N6 O6' _chemical_formula_weight 448.03 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.596(1) _cell_length_b 12.157(1) _cell_length_c 9.698(1) _cell_angle_alpha 90.00 _cell_angle_beta 108.10(1) _cell_angle_gamma 90.00 _cell_volume 1075.4(2) _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 blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 478 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1898 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1898 _reflns_number_gt 1460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'NRCVAX (Gabe, et al., 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'NRCVAX (Gabe, et al., 1989)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0942P)^2^+0.2721P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom method' _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 1898 _refine_ls_number_parameters 126 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Cu1 Cu 0.0000 0.0000 0.0000 0.0481(2) Uani 1 2 d S . . OW1 O -0.0845(4) -0.2042(3) 0.0106(3) 0.0922(10) Uani 1 1 d . . . H1OW H -0.1837 -0.2215 -0.0400 0.060 Uiso 1 1 d . . . H2OW H -0.0659 -0.2337 0.1000 0.060 Uiso 1 1 d . . . N1 N 0.1570(3) -0.0659(2) -0.0785(3) 0.0540(7) Uani 1 1 d . . . N2 N 0.1436(3) -0.0260(2) 0.2008(3) 0.0555(7) Uani 1 1 d . . . H1N2 H 0.1090 -0.0854 0.2371 0.060 Uiso 1 1 calc R . . C1 C 0.2516(4) -0.1290(3) 0.0454(4) 0.0688(10) Uani 1 1 d . . . H1A H 0.3420 -0.1488 0.0267 0.060 Uiso 1 1 calc R . . H1B H 0.2023 -0.1963 0.0574 0.060 Uiso 1 1 calc R . . C2 C 0.2856(4) -0.0615(4) 0.1815(4) 0.0701(10) Uani 1 1 d . . . H2A H 0.3414 -0.1049 0.2642 0.060 Uiso 1 1 calc R . . H2B H 0.3435 0.0023 0.1738 0.060 Uiso 1 1 calc R . . C3 C 0.1640(5) 0.0625(3) 0.3121(4) 0.0651(10) Uani 1 1 d . . . H3 H 0.2012 0.1280 0.2763 0.060 Uiso 1 1 calc R . . C4 C 0.0187(5) 0.0909(4) 0.3305(4) 0.0702(10) Uani 1 1 d . . . H4A H 0.0361 0.1404 0.4126 0.060 Uiso 1 1 calc R . . H4B H -0.0238 0.0241 0.3548 0.060 Uiso 1 1 calc R . . C5 C -0.0923(5) 0.1433(3) 0.2028(4) 0.0670(10) Uani 1 1 d . . . H5A H -0.0460 0.2039 0.1687 0.060 Uiso 1 1 calc R . . H5B H -0.1709 0.1735 0.2343 0.060 Uiso 1 1 calc R . . C6 C 0.2478(5) 0.0169(3) -0.1242(5) 0.0719(11) Uani 1 1 d . . . H6A H 0.2997 0.0610 -0.0423 0.060 Uiso 1 1 calc R . . H6B H 0.1855 0.0632 -0.1981 0.060 Uiso 1 1 calc R . . H6C H 0.3167 -0.0200 -0.1618 0.060 Uiso 1 1 calc R . . C7 C 0.2744(6) 0.0302(4) 0.4570(5) 0.0862(13) Uani 1 1 d . . . H7A H 0.2428 -0.0363 0.4915 0.060 Uiso 1 1 calc R . . H7B H 0.2813 0.0880 0.5262 0.060 Uiso 1 1 calc R . . H7C H 0.3687 0.0187 0.4445 0.060 Uiso 1 1 calc R . . N3 N 0.0427(5) -0.2739(4) 0.3830(6) 0.1049(15) Uani 1 1 d . . . O1 O 0.1371(5) -0.2439(4) 0.3399(5) 0.1266(15) Uani 1 1 d . . . O2 O -0.0670(6) -0.2444(6) 0.3123(7) 0.195(3) Uani 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 Cu1 0.0513(4) 0.0523(4) 0.0411(3) 0.0009(2) 0.0151(2) 0.0067(2) OW1 0.089(2) 0.115(3) 0.0728(19) 0.0088(18) 0.0251(16) -0.0132(19) N1 0.0586(16) 0.0511(16) 0.0573(17) -0.0019(13) 0.0254(14) 0.0037(13) N2 0.0627(18) 0.0548(16) 0.0469(16) 0.0045(12) 0.0138(14) -0.0018(13) C1 0.066(2) 0.070(2) 0.072(2) 0.009(2) 0.0248(19) 0.0183(19) C2 0.063(2) 0.081(3) 0.064(2) 0.010(2) 0.0166(19) 0.012(2) C3 0.079(2) 0.062(2) 0.051(2) -0.0034(17) 0.0142(18) -0.0102(19) C4 0.085(3) 0.075(2) 0.053(2) -0.0129(19) 0.025(2) -0.004(2) C5 0.079(2) 0.060(2) 0.069(2) -0.0114(18) 0.033(2) 0.0031(19) C6 0.074(3) 0.079(3) 0.070(3) 0.0019(19) 0.033(2) -0.005(2) C7 0.097(3) 0.098(3) 0.053(2) -0.007(2) 0.008(2) -0.005(3) N3 0.074(3) 0.124(4) 0.124(4) 0.052(3) 0.041(3) 0.020(3) O1 0.112(3) 0.144(4) 0.129(3) 0.053(3) 0.045(3) 0.005(3) O2 0.109(4) 0.300(8) 0.180(5) 0.121(5) 0.052(4) 0.010(4) _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 Cu1 N2 2.031(3) . ? Cu1 N2 2.031(3) 3 ? Cu1 N1 2.050(3) 3 ? Cu1 N1 2.050(3) . ? OW1 H1OW 0.949(3) . ? OW1 H2OW 0.903(3) . ? N1 C1 1.477(4) . ? N1 C6 1.486(5) . ? N1 C5 1.503(5) 3 ? N2 C3 1.492(5) . ? N2 C2 1.497(5) . ? N2 H1N2 0.9100 . ? C1 C2 1.501(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.500(6) . ? C3 C7 1.526(6) . ? C3 H3 0.9800 . ? C4 C5 1.501(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.503(5) 3 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? N3 O2 1.122(6) . ? N3 O1 1.168(5) . ? 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 N2 Cu1 N2 180.00(16) . 3 ? N2 Cu1 N1 93.57(12) . 3 ? N2 Cu1 N1 86.43(12) 3 3 ? N2 Cu1 N1 86.43(12) . . ? N2 Cu1 N1 93.57(12) 3 . ? N1 Cu1 N1 180.0 3 . ? H1OW OW1 H2OW 106.0(3) . . ? C1 N1 C6 109.0(3) . . ? C1 N1 C5 108.9(3) . 3 ? C6 N1 C5 108.6(3) . 3 ? C1 N1 Cu1 103.8(2) . . ? C6 N1 Cu1 114.4(2) . . ? C5 N1 Cu1 112.0(2) 3 . ? C3 N2 C2 112.3(3) . . ? C3 N2 Cu1 118.6(2) . . ? C2 N2 Cu1 107.3(2) . . ? C3 N2 H1N2 105.9 . . ? C2 N2 H1N2 105.9 . . ? Cu1 N2 H1N2 105.9 . . ? N1 C1 C2 110.0(3) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 108.1(3) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C4 109.5(3) . . ? N2 C3 C7 112.2(3) . . ? C4 C3 C7 110.8(4) . . ? N2 C3 H3 108.1 . . ? C4 C3 H3 108.1 . . ? C7 C3 H3 108.1 . . ? C3 C4 C5 116.5(3) . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? C5 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? C4 C5 N1 114.0(3) . 3 ? C4 C5 H5A 108.8 . . ? N1 C5 H5A 108.8 3 . ? C4 C5 H5B 108.8 . . ? N1 C5 H5B 108.8 3 . ? H5A C5 H5B 107.7 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 N3 O1 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.618 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.067 #--------------------------------------END------------------------------------ data_[CuL1(H2O)2]Cl2,4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H36 Cl2 Cu N4 O2' _chemical_formula_weight 426.91 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' 'O' 'O' 0.0106 0.0060 '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' 'Cu' 'Cu' 0.3201 1.2651 '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 P21/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 8.973(1) _cell_length_b 11.864(4) _cell_length_c 9.614(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.93(2) _cell_angle_gamma 90.00 _cell_volume 979.1(5) _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 blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 454 _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2846 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2846 _reflns_number_gt 2366 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'NRCVAX (Gabe, et al., 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'NRCVAX (Gabe, et al., 1989)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+1.1745P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom method' _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 2846 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.272 _refine_ls_restrained_S_all 1.272 _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 Cu1 Cu 0.0000 0.0000 0.5000 0.02430(10) Uani 1 2 d S . . OW1 O -0.0917(2) 0.2159(2) 0.5011(2) 0.0548(6) Uani 1 1 d . . . H1OW H -0.2005 0.2325 0.4568 0.060 Uiso 1 1 d . . . H2OW H -0.0474 0.2562 0.5867 0.060 Uiso 1 1 d . . . N1 N 0.1747(2) 0.06380(16) 0.4244(2) 0.0257(4) Uani 1 1 d . . . N2 N 0.1472(2) 0.02354(16) 0.7029(2) 0.0253(4) Uani 1 1 d . . . H1N2 H 0.1106 0.0847 0.7397 0.060 Uiso 1 1 calc R . . C1 C 0.2740(3) 0.1268(2) 0.5512(3) 0.0326(5) Uani 1 1 d . . . H1A H 0.2234 0.1970 0.5625 0.060 Uiso 1 1 calc R . . H1B H 0.3731 0.1446 0.5349 0.060 Uiso 1 1 calc R . . C2 C 0.3014(3) 0.0573(2) 0.6877(3) 0.0325(5) Uani 1 1 d . . . H2A H 0.3622 -0.0092 0.6815 0.060 Uiso 1 1 calc R . . H2B H 0.3584 0.1010 0.7716 0.060 Uiso 1 1 calc R . . C3 C 0.1601(3) -0.0687(2) 0.8116(2) 0.0288(5) Uani 1 1 d . . . H3 H 0.1968 -0.1369 0.7743 0.060 Uiso 1 1 calc R . . C4 C 0.0008(3) -0.0930(2) 0.8301(3) 0.0332(5) Uani 1 1 d . . . H4A H 0.0139 -0.1440 0.9117 0.060 Uiso 1 1 calc R . . H4B H -0.0417 -0.0231 0.8546 0.060 Uiso 1 1 calc R . . C5 C -0.1166(3) -0.1439(2) 0.6989(3) 0.0326(5) Uani 1 1 d . . . H5A H -0.0690 -0.2079 0.6655 0.060 Uiso 1 1 calc R . . H5B H -0.2045 -0.1718 0.7282 0.060 Uiso 1 1 calc R . . C6 C 0.2700(3) -0.0246(2) 0.3811(3) 0.0357(5) Uani 1 1 d . . . H6A H 0.2038 -0.0714 0.3071 0.060 Uiso 1 1 calc R . . H6B H 0.3206 -0.0700 0.4642 0.060 Uiso 1 1 calc R . . H6C H 0.3472 0.0104 0.3442 0.060 Uiso 1 1 calc R . . C7 C 0.2755(3) -0.0398(3) 0.9586(3) 0.0441(7) Uani 1 1 d . . . H7A H 0.3793 -0.0390 0.9496 0.060 Uiso 1 1 calc R . . H7B H 0.2687 -0.0954 1.0290 0.060 Uiso 1 1 calc R . . H7C H 0.2511 0.0330 0.9894 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.04401(8) 0.25490(6) 0.83772(7) 0.03972(15) Uani 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 Cu1 0.02192(17) 0.02999(19) 0.02136(17) 0.00048(16) 0.00685(13) -0.00543(16) OW1 0.0384(11) 0.0846(17) 0.0411(11) -0.0096(11) 0.0112(9) 0.0021(11) N1 0.0237(9) 0.0266(9) 0.0275(9) 0.0009(7) 0.0087(7) -0.0023(7) N2 0.0242(8) 0.0273(10) 0.0251(8) -0.0010(7) 0.0082(7) -0.0005(7) C1 0.0297(11) 0.0332(12) 0.0353(12) -0.0030(10) 0.0101(10) -0.0108(10) C2 0.0248(11) 0.0397(13) 0.0317(11) -0.0032(10) 0.0064(9) -0.0059(10) C3 0.0305(11) 0.0306(11) 0.0253(10) 0.0030(9) 0.0083(9) 0.0052(9) C4 0.0354(12) 0.0394(13) 0.0275(11) 0.0083(10) 0.0137(10) 0.0027(10) C5 0.0329(12) 0.0317(12) 0.0353(12) 0.0083(10) 0.0132(10) -0.0036(10) C6 0.0329(12) 0.0385(14) 0.0383(13) -0.0007(10) 0.0146(10) 0.0060(10) C7 0.0427(15) 0.0555(17) 0.0282(12) 0.0037(12) 0.0011(11) -0.0005(13) Cl1 0.0398(3) 0.0395(3) 0.0399(3) -0.0106(3) 0.0117(3) -0.0013(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 Cu1 N2 2.0317(19) . ? Cu1 N2 2.0317(19) 3_556 ? Cu1 N1 2.0553(18) . ? Cu1 N1 2.0553(18) 3_556 ? OW1 H1OW 0.965(2) . ? OW1 H2OW 0.934(2) . ? N1 C1 1.486(3) . ? N1 C6 1.487(3) . ? N1 C5 1.490(3) 3_556 ? N2 C2 1.488(3) . ? N2 C3 1.494(3) . ? N2 H1N2 0.9100 . ? C1 C2 1.508(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.519(3) . ? C3 C7 1.528(3) . ? C3 H3 0.9800 . ? C4 C5 1.513(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.490(3) 3_556 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 N2 Cu1 N2 179.998(2) . 3_556 ? N2 Cu1 N1 86.52(8) . . ? N2 Cu1 N1 93.48(8) 3_556 . ? N2 Cu1 N1 93.48(8) . 3_556 ? N2 Cu1 N1 86.52(8) 3_556 3_556 ? N1 Cu1 N1 180.0 . 3_556 ? H1OW OW1 H2OW 113.6(2) . . ? C1 N1 C6 109.17(19) . . ? C1 N1 C5 108.63(19) . 3_556 ? C6 N1 C5 108.92(19) . 3_556 ? C1 N1 Cu1 103.40(13) . . ? C6 N1 Cu1 113.52(15) . . ? C5 N1 Cu1 112.94(14) 3_556 . ? C2 N2 C3 112.41(18) . . ? C2 N2 Cu1 107.81(14) . . ? C3 N2 Cu1 117.83(14) . . ? C2 N2 H1N2 106.0 . . ? C3 N2 H1N2 106.0 . . ? Cu1 N2 H1N2 106.0 . . ? N1 C1 C2 110.24(19) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 108.19(19) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C4 109.73(18) . . ? N2 C3 C7 112.1(2) . . ? C4 C3 C7 110.0(2) . . ? N2 C3 H3 108.3 . . ? C4 C3 H3 108.3 . . ? C7 C3 H3 108.3 . . ? C5 C4 C3 115.4(2) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? N1 C5 C4 113.9(2) 3_556 . ? N1 C5 H5A 108.8 3_556 . ? C4 C5 H5A 108.8 . . ? N1 C5 H5B 108.8 3_556 . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.494 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.074 #--------------------------------------END------------------------------------ data_[CuL1(H2O)2]Br2,5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H36 Br2 Cu N4 O2' _chemical_formula_weight 515.83 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' 'O' 'O' 0.0106 0.0060 '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' 'Br' 'Br' -0.2901 2.4595 '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 monoclinic _symmetry_space_group_name_H-M P21/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 9.245(1) _cell_length_b 12.115(1) _cell_length_c 9.749(1) _cell_angle_alpha 90.00 _cell_angle_beta 107.24(1) _cell_angle_gamma 90.00 _cell_volume 1042.8(2) _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 blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 4.892 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3026 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 29.98 _reflns_number_total 3026 _reflns_number_gt 1936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'NRCVAX (Gabe, et al., 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'NRCVAX (Gabe, et al., 1989)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1453P)^2^+88.8890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.003(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3026 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1703 _refine_ls_R_factor_gt 0.1140 _refine_ls_wR_factor_ref 0.5437 _refine_ls_wR_factor_gt 0.5270 _refine_ls_goodness_of_fit_ref 1.299 _refine_ls_restrained_S_all 1.299 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.5000 0.0315(10) Uani 1 2 d S . . OW1 O -0.094(2) 0.211(2) 0.495(2) 0.070(6) Uani 1 1 d . . . H1OW H -0.2000 0.2452 0.4159 0.060 Uiso 1 1 d . . . H2OW H -0.1400 0.2335 0.5669 0.060 Uiso 1 1 d . . . N1 N 0.167(2) 0.0658(14) 0.4249(18) 0.031(3) Uani 1 1 d . . . N2 N 0.1448(18) 0.0258(14) 0.7002(17) 0.029(3) Uani 1 1 d . . . H1N2 H 0.1080 0.0851 0.7364 0.060 Uiso 1 1 calc R . . C1 C 0.260(3) 0.130(2) 0.550(3) 0.042(5) Uani 1 1 d . . . H1A H 0.2058 0.1966 0.5612 0.060 Uiso 1 1 calc R . . H1B H 0.3541 0.1524 0.5328 0.060 Uiso 1 1 calc R . . C2 C 0.294(2) 0.061(2) 0.686(2) 0.043(5) Uani 1 1 d . . . H2A H 0.3538 -0.0035 0.6779 0.060 Uiso 1 1 calc R . . H2B H 0.3493 0.1034 0.7687 0.060 Uiso 1 1 calc R . . C3 C 0.162(3) -0.0658(18) 0.810(2) 0.035(4) Uani 1 1 d . . . H3 H 0.2003 -0.1320 0.7745 0.060 Uiso 1 1 calc R . . C4 C 0.008(3) -0.091(2) 0.828(2) 0.043(5) Uani 1 1 d . . . H4A H 0.0224 -0.1409 0.9088 0.060 Uiso 1 1 calc R . . H4B H -0.0340 -0.0231 0.8522 0.060 Uiso 1 1 calc R . . C5 C -0.107(2) -0.1418(19) 0.700(3) 0.042(5) Uani 1 1 d . . . H5A H -0.0620 -0.2053 0.6687 0.060 Uiso 1 1 calc R . . H5B H -0.1921 -0.1681 0.7308 0.060 Uiso 1 1 calc R . . C6 C 0.261(3) -0.020(2) 0.381(3) 0.047(6) Uani 1 1 d . . . H6A H 0.1975 -0.0667 0.3094 0.060 Uiso 1 1 calc R . . H6B H 0.3135 -0.0630 0.4636 0.060 Uiso 1 1 calc R . . H6C H 0.3340 0.0160 0.3433 0.060 Uiso 1 1 calc R . . C7 C 0.272(4) -0.033(3) 0.954(3) 0.063(8) Uani 1 1 d . . . H7A H 0.3733 -0.0309 0.9459 0.060 Uiso 1 1 calc R . . H7B H 0.2672 -0.0854 1.0258 0.060 Uiso 1 1 calc R . . H7C H 0.2459 0.0391 0.9806 0.060 Uiso 1 1 calc R . . Br1 Br 0.0347(3) 0.2601(2) 0.8391(3) 0.0458(9) Uani 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 Cu1 0.0324(18) 0.039(2) 0.0258(16) 0.0010(13) 0.0120(13) -0.0065(14) OW1 0.055(12) 0.106(18) 0.055(12) -0.004(12) 0.024(10) 0.019(12) N1 0.033(8) 0.029(8) 0.034(8) -0.001(7) 0.015(7) -0.002(7) N2 0.030(8) 0.028(8) 0.030(8) -0.005(6) 0.011(6) 0.000(6) C1 0.033(10) 0.043(12) 0.052(13) -0.015(10) 0.013(9) -0.022(9) C2 0.029(10) 0.068(16) 0.034(11) -0.002(11) 0.010(8) -0.009(10) C3 0.043(11) 0.034(10) 0.028(9) -0.003(8) 0.010(8) -0.005(9) C4 0.045(12) 0.053(14) 0.034(11) 0.013(10) 0.018(9) 0.004(11) C5 0.032(10) 0.038(11) 0.061(14) 0.013(10) 0.024(10) -0.001(9) C6 0.050(13) 0.049(14) 0.053(14) 0.002(11) 0.030(11) 0.010(11) C7 0.063(17) 0.09(2) 0.027(11) 0.006(13) 0.007(11) 0.006(17) Br1 0.0454(14) 0.0463(14) 0.0474(14) -0.0133(10) 0.0164(10) -0.0024(10) _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 Cu1 N2 2.037(16) 3_556 ? Cu1 N2 2.037(16) . ? Cu1 N1 2.054(16) 3_556 ? Cu1 N1 2.054(16) . ? OW1 H1OW 1.13(2) . ? OW1 H2OW 0.96(2) . ? N1 C1 1.49(3) . ? N1 C6 1.49(3) . ? N1 C5 1.50(3) 3_556 ? N2 C2 1.49(3) . ? N2 C3 1.52(3) . ? N2 H1N2 0.9100 . ? C1 C2 1.53(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.52(3) . ? C3 C7 1.53(3) . ? C3 H3 0.9800 . ? C4 C5 1.51(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.50(3) 3_556 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 N2 Cu1 N2 180.0(8) 3_556 . ? N2 Cu1 N1 86.1(7) 3_556 3_556 ? N2 Cu1 N1 93.9(7) . 3_556 ? N2 Cu1 N1 93.9(7) 3_556 . ? N2 Cu1 N1 86.1(7) . . ? N1 Cu1 N1 179.998(1) 3_556 . ? H1OW OW1 H2OW 85.0(15) . . ? C1 N1 C6 110.5(19) . . ? C1 N1 C5 109.1(18) . 3_556 ? C6 N1 C5 107.4(17) . 3_556 ? C1 N1 Cu1 103.1(12) . . ? C6 N1 Cu1 113.4(14) . . ? C5 N1 Cu1 113.4(13) 3_556 . ? C2 N2 C3 111.6(17) . . ? C2 N2 Cu1 108.5(12) . . ? C3 N2 Cu1 117.6(12) . . ? C2 N2 H1N2 106.1 . . ? C3 N2 H1N2 106.1 . . ? Cu1 N2 H1N2 106.1 . . ? N1 C1 C2 109.8(18) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 106.4(18) . . ? N2 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? N2 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? N2 C3 C4 109.0(18) . . ? N2 C3 C7 111(2) . . ? C4 C3 C7 110(2) . . ? N2 C3 H3 109.0 . . ? C4 C3 H3 109.0 . . ? C7 C3 H3 109.0 . . ? C5 C4 C3 116.4(18) . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4B 108.2 . . ? C3 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? N1 C5 C4 114.9(19) 3_556 . ? N1 C5 H5A 108.5 3_556 . ? C4 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 3_556 . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.562 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.373 #------------------------------------END------------------------------------- data_[CuL1(H2O)2]I2,6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H36 Cu I2 N4 O2' _chemical_formula_weight 609.81 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' '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 P21/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 8.5634(3) _cell_length_b 13.1899(5) _cell_length_c 10.2121(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.266(1) _cell_angle_gamma 90.00 _cell_volume 1122.68(7) _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 blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 3.735 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'SMART CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6408 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.04 _reflns_number_total 2463 _reflns_number_gt 2285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART CCD (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'NRCVAX (Gabe, et al., 1989)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+1.7662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom method' _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 2463 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_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_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 Cu1 Cu 0.0000 0.0000 0.0000 0.03029(11) Uani 1 2 d S . . OW1 O 0.1764(4) -0.1221(2) -0.1261(3) 0.0779(9) Uani 1 1 d . . . H1OW H 0.1003 -0.1407 -0.2200 0.060 Uiso 1 1 d . . . H2OW H 0.2105 -0.1750 -0.0800 0.060 Uiso 1 1 d . . . N1 N 0.1188(3) 0.11657(18) -0.0668(2) 0.0356(5) Uani 1 1 d . . . N2 N -0.1648(3) 0.01177(18) -0.1787(2) 0.0351(5) Uani 1 1 d . . . H1N2 H -0.1477 -0.0426 -0.2286 0.060 Uiso 1 1 calc R . . C1 C 0.0571(4) 0.1148(3) -0.2148(3) 0.0466(7) Uani 1 1 d . . . H1A H 0.1057 0.0590 -0.2528 0.060 Uiso 1 1 calc R . . H1B H 0.0861 0.1774 -0.2532 0.060 Uiso 1 1 calc R . . C2 C -0.1224(4) 0.1029(3) -0.2500(3) 0.0461(7) Uani 1 1 d . . . H2A H -0.1725 0.1628 -0.2226 0.060 Uiso 1 1 calc R . . H2B H -0.1606 0.0947 -0.3464 0.060 Uiso 1 1 calc R . . C3 C -0.3391(4) 0.0082(3) -0.1760(3) 0.0430(7) Uani 1 1 d . . . H3 H -0.3614 0.0646 -0.1206 0.060 Uiso 1 1 calc R . . C4 C -0.3746(4) -0.0896(3) -0.1117(4) 0.0504(8) Uani 1 1 d . . . H4A H -0.3402 -0.1457 -0.1599 0.060 Uiso 1 1 calc R . . H4B H -0.4898 -0.0954 -0.1228 0.060 Uiso 1 1 calc R . . C5 C -0.2958(4) -0.1007(3) 0.0368(4) 0.0479(8) Uani 1 1 d . . . H5A H -0.3180 -0.0402 0.0834 0.060 Uiso 1 1 calc R . . H5B H -0.3445 -0.1576 0.0725 0.060 Uiso 1 1 calc R . . C6 C 0.0852(4) 0.2169(3) -0.0132(4) 0.0515(8) Uani 1 1 d . . . H6A H 0.1101 0.2146 0.0834 0.060 Uiso 1 1 calc R . . H6B H -0.0261 0.2333 -0.0459 0.060 Uiso 1 1 calc R . . H6C H 0.1500 0.2677 -0.0424 0.060 Uiso 1 1 calc R . . C7 C -0.4489(5) 0.0184(4) -0.3159(4) 0.0664(11) Uani 1 1 d . . . H7A H -0.5580 0.0068 -0.3109 0.060 Uiso 1 1 calc R . . H7B H -0.4186 -0.0304 -0.3752 0.060 Uiso 1 1 calc R . . H7C H -0.4392 0.0855 -0.3498 0.060 Uiso 1 1 calc R . . I1 I -0.10942(3) -0.179014(18) -0.42421(2) 0.05154(9) Uani 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 Cu1 0.0310(2) 0.0340(2) 0.0258(2) 0.00315(17) 0.00615(17) -0.00468(18) OW1 0.081(2) 0.0563(17) 0.078(2) 0.0112(15) -0.0189(16) -0.0060(15) N1 0.0375(12) 0.0328(12) 0.0390(13) 0.0025(10) 0.0141(10) -0.0020(10) N2 0.0369(12) 0.0374(13) 0.0303(12) -0.0019(9) 0.0061(9) 0.0046(10) C1 0.059(2) 0.0486(18) 0.0372(15) 0.0099(13) 0.0217(14) -0.0005(15) C2 0.0558(19) 0.0484(18) 0.0321(14) 0.0098(13) 0.0059(13) 0.0044(15) C3 0.0334(15) 0.0479(18) 0.0439(17) -0.0083(13) 0.0008(12) 0.0054(13) C4 0.0302(15) 0.0502(19) 0.068(2) -0.0067(17) 0.0055(14) -0.0047(13) C5 0.0367(16) 0.0507(18) 0.063(2) 0.0042(16) 0.0246(15) -0.0048(14) C6 0.055(2) 0.0370(16) 0.062(2) -0.0023(15) 0.0132(17) 0.0002(15) C7 0.048(2) 0.080(3) 0.060(2) -0.007(2) -0.0105(18) 0.0121(19) I1 0.06086(15) 0.05158(14) 0.04347(13) -0.01097(9) 0.01466(10) -0.00180(10) _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 Cu1 N2 2.041(2) . ? Cu1 N2 2.041(2) 3 ? Cu1 N1 2.045(2) . ? Cu1 N1 2.045(2) 3 ? OW1 H1OW 1.057(3) . ? OW1 H2OW 0.855(3) . ? N1 C1 1.483(4) . ? N1 C6 1.485(4) . ? N1 C5 1.490(4) 3 ? N2 C2 1.493(4) . ? N2 C3 1.501(4) . ? N2 H1N2 0.9100 . ? C1 C2 1.504(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.509(5) . ? C3 C7 1.526(5) . ? C3 H3 0.9800 . ? C4 C5 1.519(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.490(4) 3 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 N2 Cu1 N2 180.0 . 3 ? N2 Cu1 N1 86.52(10) . . ? N2 Cu1 N1 93.48(10) 3 . ? N2 Cu1 N1 93.48(10) . 3 ? N2 Cu1 N1 86.52(10) 3 3 ? N1 Cu1 N1 180.0 . 3 ? H1OW OW1 H2OW 111.8(3) . . ? C1 N1 C6 109.6(3) . . ? C1 N1 C5 108.4(2) . 3 ? C6 N1 C5 108.8(3) . 3 ? C1 N1 Cu1 103.88(18) . . ? C6 N1 Cu1 113.2(2) . . ? C5 N1 Cu1 112.70(19) 3 . ? C2 N2 C3 112.9(2) . . ? C2 N2 Cu1 107.57(18) . . ? C3 N2 Cu1 117.87(19) . . ? C2 N2 H1N2 105.9 . . ? C3 N2 H1N2 105.9 . . ? Cu1 N2 H1N2 105.9 . . ? N1 C1 C2 110.5(2) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 108.5(2) . . ? N2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C4 109.6(2) . . ? N2 C3 C7 112.4(3) . . ? C4 C3 C7 110.0(3) . . ? N2 C3 H3 108.3 . . ? C4 C3 H3 108.3 . . ? C7 C3 H3 108.3 . . ? C3 C4 C5 115.4(3) . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 . . ? C5 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? N1 C5 C4 114.6(3) 3 . ? N1 C5 H5A 108.6 3 . ? C4 C5 H5A 108.6 . . ? N1 C5 H5B 108.6 3 . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.922 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.079 #--------------------------------END------------------------------------------