Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Barbara Sieklucka' 'Robert Podgajny' 'Tomasz Korzeniak' 'Maria Balanda' 'Tadeusz Wasiutynski' 'William Errington' 'Terence J Kemp' 'N. Alcock' _publ_contact_author_name 'Dr Barbara Sieklucka' _publ_contact_author_address ; Faculty of Chemistry Jagiellonian University Ingardena 3 Krakow 30 060 POLAND ; _publ_contact_author_email 'SIEKLUCK@CHEMIA.UJ.EDU.PL' _publ_section_title ; 2-D soft ferromagnet based on [Wv(CN)8]3- and Cu II with a Tc of 34 K ; data_w15new _database_code_CSD 182458 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9.60 H9.20 Cu N9 O1.80 W' _chemical_formula_weight 526.7 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.3792(6) _cell_length_b 32.096(2) _cell_length_c 7.0160(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1661.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5488 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description plates _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 8.220 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 5385 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 29.15 _reflns_number_total 2073 _reflns_number_gt 1954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _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 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0568P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0034(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2073 _refine_ls_number_parameters 111 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.004 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 W1 W 0.0000 0.145428(8) 0.30805(7) 0.00771(8) Uani 1 2 d S . . Cu1 Cu 0.0000 0.31481(3) 0.3051(5) 0.00807(18) Uani 1 2 d S . . N1 N 0.0000 0.2490(2) 0.317(3) 0.0184(17) Uani 1 2 d S . . C1 C 0.0000 0.2129(2) 0.307(4) 0.0153(15) Uani 1 2 d SU . . N2 N 0.2930(10) 0.1766(2) -0.0171(10) 0.0196(15) Uiso 1 1 d . . . C2 C 0.1907(12) 0.1664(3) 0.0914(12) 0.0185(18) Uiso 1 1 d . . . N3 N 0.3316(11) 0.1728(2) 0.5945(11) 0.0234(17) Uiso 1 1 d . . . C3 C 0.2188(12) 0.1626(3) 0.4936(13) 0.0192(19) Uiso 1 1 d . . . N4 N 0.0000 0.0815(4) 0.6769(18) 0.054(4) Uani 1 2 d S . . C4 C 0.0000 0.1037(4) 0.5526(17) 0.025(3) Uani 1 2 d S . . N5 N 0.2774(16) 0.0690(3) 0.1922(18) 0.068(3) Uani 1 1 d . . . C5 C 0.1779(13) 0.0955(3) 0.2329(13) 0.032(2) Uani 1 1 d . . . C001 C -0.558(3) 0.0255(7) 0.821(9) 0.068(7) Uiso 0.50 1 d P . . C002 C -0.062(4) 0.0100(10) 0.869(5) 0.020(7) Uiso 0.25 1 d P . . C003 C -0.5000 0.004(2) 0.688(10) 0.10(2) Uiso 0.50 2 d SP . . C004 C 0.0000 -0.0002(10) 0.792(9) 0.049(8) Uiso 0.50 2 d SP . . C005 C -0.613(7) 0.0371(17) 0.955(7) 0.056(12) Uiso 0.25 1 d P . . C006 C -0.138(6) -0.0088(13) 1.277(8) 0.050(12) Uiso 0.25 1 d P . . C007 C -0.706(8) 0.004(3) 0.552(17) 0.072(16) Uiso 0.25 1 d P . . C008 C -0.606(9) 0.009(2) 0.608(9) 0.067(16) Uiso 0.25 1 d P . . C009 C -0.5000 -0.088(2) 0.855(12) 0.14(3) Uiso 0.50 2 d SP . . C010 C -0.5000 0.0054(10) 0.954(5) 0.028(6) Uiso 0.50 2 d SP . . C011 C -0.5000 -0.0371(18) 0.855(9) 0.11(2) Uiso 0.50 2 d SP . . 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 W1 0.00663(13) 0.01002(14) 0.00648(14) -0.0003(4) 0.000 0.000 Cu1 0.0062(3) 0.0130(4) 0.0050(4) 0.0011(13) 0.000 0.000 N1 0.020(3) 0.017(3) 0.019(4) 0.010(8) 0.000 0.000 C1 0.018(3) 0.012(3) 0.016(3) -0.005(7) 0.000 0.000 N4 0.076(10) 0.052(8) 0.033(7) 0.024(6) 0.000 0.000 C4 0.030(6) 0.021(5) 0.025(6) 0.012(4) 0.000 0.000 N5 0.074(7) 0.035(5) 0.095(8) -0.001(5) 0.029(6) 0.032(5) C5 0.027(4) 0.022(4) 0.047(5) -0.001(3) 0.006(4) 0.011(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 W1 C5 2.138(8) 4 ? W1 C5 2.138(8) . y W1 C3 2.146(9) . y W1 C3 2.146(9) 4 ? W1 C1 2.165(7) . y W1 C4 2.177(11) . y W1 C2 2.178(9) 4 ? W1 C2 2.178(9) . y Cu1 N3 1.971(8) 7_454 y Cu1 N3 1.971(8) 6_554 ? Cu1 N2 1.992(8) 6 y Cu1 N2 1.992(8) 7_455 ? Cu1 N1 2.115(7) . y N1 C1 1.160(11) . ? N2 C2 1.121(11) . ? N2 Cu1 1.992(8) 6_554 ? N3 C3 1.141(12) . ? N3 Cu1 1.971(8) 6 ? N4 C4 1.125(17) . ? N5 C5 1.159(12) . ? C001 C001 0.85(4) 4_455 ? C001 C005 1.09(7) . ? C001 C010 1.22(6) . ? C001 C003 1.24(8) . ? C001 C005 1.62(6) 4_455 ? C001 C008 1.63(8) . ? C001 C008 1.99(8) 4_455 ? C002 C004 0.78(5) . ? C002 C006 0.85(5) 3_554 ? C002 C002 0.91(7) 4 ? C002 C006 1.61(6) 2_554 ? C003 C008 0.97(7) . ? C003 C008 0.97(7) 4_455 ? C003 C001 1.24(8) 4_455 ? C003 C010 1.67(7) 2_454 ? C003 C011 1.76(9) . ? C003 C007 1.79(9) . ? C003 C007 1.79(9) 4_455 ? C003 C010 1.87(7) . ? C004 C002 0.78(5) 4 ? C004 C006 1.06(5) 2_554 ? C004 C006 1.06(5) 3_554 ? C005 C010 1.32(6) . ? C005 C001 1.62(6) 4_455 ? C005 C007 1.65(12) 3 ? C005 C005 1.67(11) 4_455 ? C005 C008 1.82(9) 3 ? C006 C002 0.85(5) 3 ? C006 C004 1.06(5) 2 ? C006 C002 1.61(6) 2 ? C006 C007 1.96(11) 2_455 ? C006 C006 2.03(9) 4 ? C007 C008 0.85(9) . ? C007 C005 1.65(12) 3_554 ? C007 C010 1.70(7) 2_454 ? C007 C006 1.96(11) 2_454 ? C008 C010 1.41(6) 2_454 ? C008 C008 1.56(13) 4_455 ? C008 C005 1.82(9) 3_554 ? C008 C001 1.99(8) 4_455 ? C009 C011 1.65(8) . ? C010 C001 1.22(6) 4_455 ? C010 C005 1.32(6) 4_455 ? C010 C008 1.41(6) 2_455 ? C010 C008 1.41(6) 3 ? C010 C011 1.53(7) . ? C010 C003 1.67(7) 2_455 ? C010 C007 1.70(7) 2_455 ? C010 C007 1.70(7) 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 C5 W1 C5 75.8(5) 4 . ? C5 W1 C3 143.5(4) 4 . ? C5 W1 C3 83.1(4) . . ? C5 W1 C3 83.1(4) 4 4 ? C5 W1 C3 143.5(4) . 4 ? C3 W1 C3 97.6(5) . 4 ? C5 W1 C1 138.5(4) 4 . ? C5 W1 C1 138.5(4) . . ? C3 W1 C1 75.2(6) . . ? C3 W1 C1 75.2(6) 4 . ? C5 W1 C4 74.5(4) 4 . ? C5 W1 C4 74.5(4) . . ? C3 W1 C4 71.3(3) . . ? C3 W1 C4 71.3(3) 4 . ? C1 W1 C4 128.2(8) . . ? C5 W1 C2 70.3(3) 4 4 ? C5 W1 C2 117.1(3) . 4 ? C3 W1 C2 146.1(3) . 4 ? C3 W1 C2 81.8(3) 4 4 ? C1 W1 C2 71.9(6) . 4 ? C4 W1 C2 137.7(3) . 4 ? C5 W1 C2 117.1(3) 4 . ? C5 W1 C2 70.3(3) . . ? C3 W1 C2 81.8(3) . . ? C3 W1 C2 146.1(3) 4 . ? C1 W1 C2 71.9(6) . . ? C4 W1 C2 137.7(3) . . ? C2 W1 C2 80.5(5) 4 . ? N3 Cu1 N3 78.2(5) 7_454 6_554 ? N3 Cu1 N2 157.7(3) 7_454 6 ? N3 Cu1 N2 87.6(3) 6_554 6 ? N3 Cu1 N2 87.6(3) 7_454 7_455 ? N3 Cu1 N2 157.7(3) 6_554 7_455 ? N2 Cu1 N2 100.1(5) 6 7_455 ? N3 Cu1 N1 103.3(5) 7_454 . ? N3 Cu1 N1 103.3(5) 6_554 . ? N2 Cu1 N1 96.5(4) 6 . ? N2 Cu1 N1 96.5(4) 7_455 . ? C1 N1 Cu1 174(2) . . ? N1 C1 W1 176(2) . . ? C2 N2 Cu1 169.3(7) . 6_554 ? N2 C2 W1 177.9(8) . . ? C3 N3 Cu1 169.4(8) . 6 ? N3 C3 W1 177.7(9) . . ? N4 C4 W1 178.8(12) . . ? N5 C5 W1 178.5(10) . . ? C001 C001 C005 112(3) 4_455 . ? C001 C001 C010 69.4(13) 4_455 . ? C005 C001 C010 70(5) . . ? C001 C001 C003 69.9(18) 4_455 . ? C005 C001 C003 166(6) . . ? C010 C001 C003 99(3) . . ? C001 C001 C005 39(2) 4_455 4_455 ? C005 C001 C005 73(5) . 4_455 ? C010 C001 C005 53(3) . 4_455 ? C003 C001 C005 107(3) . 4_455 ? C001 C001 C008 103(2) 4_455 . ? C005 C001 C008 145(4) . . ? C010 C001 C008 127(4) . . ? C003 C001 C008 37(3) . . ? C005 C001 C008 141(4) 4_455 . ? C001 C001 C008 53(2) 4_455 4_455 ? C005 C001 C008 165(4) . 4_455 ? C010 C001 C008 103(3) . 4_455 ? C003 C001 C008 23(3) . 4_455 ? C005 C001 C008 91(3) 4_455 4_455 ? C008 C001 C008 50(4) . 4_455 ? C004 C002 C006 81(5) . 3_554 ? C004 C002 C002 54(3) . 4 ? C006 C002 C002 131(4) 3_554 4 ? C004 C002 C006 35(3) . 2_554 ? C006 C002 C006 107(5) 3_554 2_554 ? C002 C002 C006 24(2) 4 2_554 ? C008 C003 C008 107(10) . 4_455 ? C008 C003 C001 128(8) . 4_455 ? C008 C003 C001 94(6) 4_455 4_455 ? C008 C003 C001 94(6) . . ? C008 C003 C001 128(8) 4_455 . ? C001 C003 C001 40(4) 4_455 . ? C008 C003 C010 57(6) . 2_454 ? C008 C003 C010 57(6) 4_455 2_454 ? C001 C003 C010 147(5) 4_455 2_454 ? C001 C003 C010 147(5) . 2_454 ? C008 C003 C011 120(6) . . ? C008 C003 C011 120(6) 4_455 . ? C001 C003 C011 85(5) 4_455 . ? C001 C003 C011 85(5) . . ? C010 C003 C011 122(5) 2_454 . ? C008 C003 C007 9(6) . . ? C008 C003 C007 112(7) 4_455 . ? C001 C003 C007 133(6) 4_455 . ? C001 C003 C007 96(4) . . ? C010 C003 C007 59(4) 2_454 . ? C011 C003 C007 111(4) . . ? C008 C003 C007 112(7) . 4_455 ? C008 C003 C007 9(6) 4_455 4_455 ? C001 C003 C007 96(4) 4_455 4_455 ? C001 C003 C007 133(6) . 4_455 ? C010 C003 C007 59(4) 2_454 4_455 ? C011 C003 C007 111(4) . 4_455 ? C007 C003 C007 116(7) . 4_455 ? C008 C003 C010 125(6) . . ? C008 C003 C010 125(6) 4_455 . ? C001 C003 C010 40(3) 4_455 . ? C001 C003 C010 40(3) . . ? C010 C003 C010 172(5) 2_454 . ? C011 C003 C010 50(3) . . ? C007 C003 C010 122(4) . . ? C007 C003 C010 122(4) 4_455 . ? C002 C004 C002 72(6) 4 . ? C002 C004 C006 52(4) 4 2_554 ? C002 C004 C006 121(6) . 2_554 ? C002 C004 C006 121(6) 4 3_554 ? C002 C004 C006 52(4) . 3_554 ? C006 C004 C006 147(6) 2_554 3_554 ? C001 C005 C010 60(4) . . ? C001 C005 C001 29(2) . 4_455 ? C010 C005 C001 48(3) . 4_455 ? C001 C005 C007 104(6) . 3 ? C010 C005 C007 69(4) . 3 ? C001 C005 C007 112(4) 4_455 3 ? C001 C005 C005 68(3) . 4_455 ? C010 C005 C005 51(3) . 4_455 ? C001 C005 C005 39(2) 4_455 4_455 ? C007 C005 C005 115(3) 3 4_455 ? C001 C005 C008 103(5) . 3 ? C010 C005 C008 50(3) . 3 ? C001 C005 C008 98(4) 4_455 3 ? C007 C005 C008 28(3) 3 3 ? C005 C005 C008 88(3) 4_455 3 ? C002 C006 C004 47(5) 3 2 ? C002 C006 C002 25(3) 3 2 ? C004 C006 C002 25(3) 2 2 ? C002 C006 C007 175(6) 3 2_455 ? C004 C006 C007 128(6) 2 2_455 ? C002 C006 C007 150(4) 2 2_455 ? C002 C006 C006 49(4) 3 4 ? C004 C006 C006 17(3) 2 4 ? C002 C006 C006 24(2) 2 4 ? C007 C006 C006 126(3) 2_455 4 ? C008 C007 C005 88(9) . 3_554 ? C008 C007 C010 56(6) . 2_454 ? C005 C007 C010 46(3) 3_554 2_454 ? C008 C007 C003 11(7) . . ? C005 C007 C003 82(5) 3_554 . ? C010 C007 C003 57(3) 2_454 . ? C008 C007 C006 97(10) . 2_454 ? C005 C007 C006 130(6) 3_554 2_454 ? C010 C007 C006 150(6) 2_454 2_454 ? C003 C007 C006 94(6) . 2_454 ? C007 C008 C003 160(10) . . ? C007 C008 C010 94(9) . 2_454 ? C003 C008 C010 87(6) . 2_454 ? C007 C008 C008 151(9) . 4_455 ? C003 C008 C008 37(5) . 4_455 ? C010 C008 C008 56(3) 2_454 4_455 ? C007 C008 C001 132(10) . . ? C003 C008 C001 50(5) . . ? C010 C008 C001 134(5) 2_454 . ? C008 C008 C001 77(2) 4_455 . ? C007 C008 C005 65(9) . 3_554 ? C003 C008 C005 104(7) . 3_554 ? C010 C008 C005 46(3) 2_454 3_554 ? C008 C008 C005 92(3) 4_455 3_554 ? C001 C008 C005 145(5) . 3_554 ? C007 C008 C001 157(10) . 4_455 ? C003 C008 C001 29(5) . 4_455 ? C010 C008 C001 109(4) 2_454 4_455 ? C008 C008 C001 53(2) 4_455 4_455 ? C001 C008 C001 24.7(17) . 4_455 ? C005 C008 C001 133(4) 3_554 4_455 ? C001 C010 C001 41(3) 4_455 . ? C001 C010 C005 79(3) 4_455 . ? C001 C010 C005 51(3) . . ? C001 C010 C005 51(3) 4_455 4_455 ? C001 C010 C005 79(3) . 4_455 ? C005 C010 C005 79(5) . 4_455 ? C001 C010 C008 125(3) 4_455 2_455 ? C001 C010 C008 163(4) . 2_455 ? C005 C010 C008 127(5) . 2_455 ? C005 C010 C008 84(4) 4_455 2_455 ? C001 C010 C008 163(4) 4_455 3 ? C001 C010 C008 125(3) . 3 ? C005 C010 C008 84(4) . 3 ? C005 C010 C008 127(5) 4_455 3 ? C008 C010 C008 67(6) 2_455 3 ? C001 C010 C011 97(4) 4_455 . ? C001 C010 C011 97(4) . . ? C005 C010 C011 134(3) . . ? C005 C010 C011 134(3) 4_455 . ? C008 C010 C011 94(4) 2_455 . ? C008 C010 C011 94(4) 3 . ? C001 C010 C003 148(3) 4_455 2_455 ? C001 C010 C003 148(3) . 2_455 ? C005 C010 C003 98(3) . 2_455 ? C005 C010 C003 98(3) 4_455 2_455 ? C008 C010 C003 36(3) 2_455 2_455 ? C008 C010 C003 36(3) 3 2_455 ? C011 C010 C003 107(3) . 2_455 ? C001 C010 C007 96(4) 4_455 2_455 ? C001 C010 C007 136(4) . 2_455 ? C005 C010 C007 135(5) . 2_455 ? C005 C010 C007 65(4) 4_455 2_455 ? C008 C010 C007 30(4) 2_455 2_455 ? C008 C010 C007 97(5) 3 2_455 ? C011 C010 C007 91(4) . 2_455 ? C003 C010 C007 64(4) 2_455 2_455 ? C001 C010 C007 136(4) 4_455 3 ? C001 C010 C007 96(4) . 3 ? C005 C010 C007 65(4) . 3 ? C005 C010 C007 135(5) 4_455 3 ? C008 C010 C007 97(5) 2_455 3 ? C008 C010 C007 30(4) 3 3 ? C011 C010 C007 91(4) . 3 ? C003 C010 C007 64(4) 2_455 3 ? C007 C010 C007 127(8) 2_455 3 ? C001 C010 C003 41(3) 4_455 . ? C001 C010 C003 41(3) . . ? C005 C010 C003 91(4) . . ? C005 C010 C003 91(4) 4_455 . ? C008 C010 C003 139(4) 2_455 . ? C008 C010 C003 139(4) 3 . ? C011 C010 C003 61(4) . . ? C003 C010 C003 168(2) 2_455 . ? C007 C010 C003 114(4) 2_455 . ? C007 C010 C003 114(4) 3 . ? C010 C011 C009 153(6) . . ? C010 C011 C003 69(3) . . ? C009 C011 C003 138(6) . . ? 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 N3 Cu1 N1 C1 40.4(3) 7_454 . . . ? N3 Cu1 N1 C1 -40.4(3) 6_554 . . . ? N2 Cu1 N1 C1 -129.5(3) 6 . . . ? N2 Cu1 N1 C1 129.5(3) 7_455 . . . ? Cu1 N1 C1 W1 180.00(6) . . . . ? C5 W1 C1 N1 112.1(10) 4 . . . ? C5 W1 C1 N1 -112.1(10) . . . . ? C3 W1 C1 N1 -51.1(4) . . . . ? C3 W1 C1 N1 51.1(3) 4 . . . ? C4 W1 C1 N1 0.00(10) . . . . ? C2 W1 C1 N1 137.2(3) 4 . . . ? C2 W1 C1 N1 -137.2(3) . . . . ? Cu1 N2 C2 W1 27(26) 6_554 . . . ? C5 W1 C2 N2 -106(23) 4 . . . ? C5 W1 C2 N2 -44(23) . . . . ? C3 W1 C2 N2 41(22) . . . . ? C3 W1 C2 N2 133(22) 4 . . . ? C1 W1 C2 N2 118(23) . . . . ? C4 W1 C2 N2 -9(23) . . . . ? C2 W1 C2 N2 -168(100) 4 . . . ? Cu1 N3 C3 W1 80(23) 6 . . . ? C5 W1 C3 N3 -124(22) 4 . . . ? C5 W1 C3 N3 -178(100) . . . . ? C3 W1 C3 N3 -35(22) 4 . . . ? C1 W1 C3 N3 37(22) . . . . ? C4 W1 C3 N3 -102(22) . . . . ? C2 W1 C3 N3 51(22) 4 . . . ? C2 W1 C3 N3 111(22) . . . . ? C5 W1 C4 N4 39.6(3) 4 . . . ? C5 W1 C4 N4 -39.6(3) . . . . ? C3 W1 C4 N4 -127.4(3) . . . . ? C3 W1 C4 N4 127.4(3) 4 . . . ? C1 W1 C4 N4 180.00(14) . . . . ? C2 W1 C4 N4 73.9(5) 4 . . . ? C2 W1 C4 N4 -73.9(5) . . . . ? C5 W1 C5 N5 169(37) 4 . . . ? C3 W1 C5 N5 -41(37) . . . . ? C3 W1 C5 N5 -134(37) 4 . . . ? C1 W1 C5 N5 18(37) . . . . ? C4 W1 C5 N5 -113(37) . . . . ? C2 W1 C5 N5 111(37) 4 . . . ? C2 W1 C5 N5 43(37) . . . . ? C001 C001 C003 C008 -152(7) 4_455 . . . ? C005 C001 C003 C008 108(19) . . . . ? C010 C001 C003 C008 144(6) . . . . ? C005 C001 C003 C008 -161(6) 4_455 . . . ? C008 C001 C003 C008 -114(15) 4_455 . . . ? C001 C001 C003 C008 -37(8) 4_455 . . 4_455 ? C005 C001 C003 C008 -138(18) . . . 4_455 ? C010 C001 C003 C008 -101(9) . . . 4_455 ? C005 C001 C003 C008 -47(11) 4_455 . . 4_455 ? C008 C001 C003 C008 114(15) . . . 4_455 ? C005 C001 C003 C001 -100(18) . . . 4_455 ? C010 C001 C003 C001 -64(2) . . . 4_455 ? C005 C001 C003 C001 -10(4) 4_455 . . 4_455 ? C008 C001 C003 C001 152(7) . . . 4_455 ? C008 C001 C003 C001 37(8) 4_455 . . 4_455 ? C001 C001 C003 C010 -124(8) 4_455 . . 2_454 ? C005 C001 C003 C010 136(19) . . . 2_454 ? C010 C001 C003 C010 172(6) . . . 2_454 ? C005 C001 C003 C010 -134(6) 4_455 . . 2_454 ? C008 C001 C003 C010 28(5) . . . 2_454 ? C008 C001 C003 C010 -87(14) 4_455 . . 2_454 ? C001 C001 C003 C011 88.3(18) 4_455 . . . ? C005 C001 C003 C011 -12(18) . . . . ? C010 C001 C003 C011 24.2(16) . . . . ? C005 C001 C003 C011 78(3) 4_455 . . . ? C008 C001 C003 C011 -120(6) . . . . ? C008 C001 C003 C011 125(9) 4_455 . . . ? C001 C001 C003 C007 -161(5) 4_455 . . . ? C005 C001 C003 C007 99(19) . . . . ? C010 C001 C003 C007 135(4) . . . . ? C005 C001 C003 C007 -171(5) 4_455 . . . ? C008 C001 C003 C007 -9(6) . . . . ? C008 C001 C003 C007 -123(11) 4_455 . . . ? C001 C001 C003 C007 -27(6) 4_455 . . 4_455 ? C005 C001 C003 C007 -127(18) . . . 4_455 ? C010 C001 C003 C007 -91(8) . . . 4_455 ? C005 C001 C003 C007 -37(9) 4_455 . . 4_455 ? C008 C001 C003 C007 125(12) . . . 4_455 ? C008 C001 C003 C007 10(7) 4_455 . . 4_455 ? C001 C001 C003 C010 64(2) 4_455 . . . ? C005 C001 C003 C010 -36(18) . . . . ? C005 C001 C003 C010 54(3) 4_455 . . . ? C008 C001 C003 C010 -144(6) . . . . ? C008 C001 C003 C010 101(9) 4_455 . . . ? C006 C002 C004 C002 159(4) 3_554 . . 4 ? C006 C002 C004 C002 19(4) 2_554 . . 4 ? C006 C002 C004 C006 140(8) 3_554 . . 2_554 ? C002 C002 C004 C006 -19(4) 4 . . 2_554 ? C002 C002 C004 C006 -159(4) 4 . . 3_554 ? C006 C002 C004 C006 -140(9) 2_554 . . 3_554 ? C001 C001 C005 C010 -56(2) 4_455 . . . ? C003 C001 C005 C010 39(18) . . . . ? C005 C001 C005 C010 -56(2) 4_455 . . . ? C008 C001 C005 C010 126(8) . . . . ? C008 C001 C005 C010 -61(18) 4_455 . . . ? C010 C001 C005 C001 56(2) . . . 4_455 ? C003 C001 C005 C001 95(18) . . . 4_455 ? C005 C001 C005 C001 0.00(2) 4_455 . . 4_455 ? C008 C001 C005 C001 -177(9) . . . 4_455 ? C008 C001 C005 C001 -5(17) 4_455 . . 4_455 ? C001 C001 C005 C007 -111(4) 4_455 . . 3 ? C010 C001 C005 C007 -55(4) . . . 3 ? C003 C001 C005 C007 -16(20) . . . 3 ? C005 C001 C005 C007 -111(4) 4_455 . . 3 ? C008 C001 C005 C007 71(10) . . . 3 ? C008 C001 C005 C007 -116(17) 4_455 . . 3 ? C001 C001 C005 C005 0.000(13) 4_455 . . 4_455 ? C010 C001 C005 C005 56(2) . . . 4_455 ? C003 C001 C005 C005 95(18) . . . 4_455 ? C008 C001 C005 C005 -177(9) . . . 4_455 ? C008 C001 C005 C005 -5(17) 4_455 . . 4_455 ? C001 C001 C005 C008 -83(4) 4_455 . . 3 ? C010 C001 C005 C008 -26(3) . . . 3 ? C003 C001 C005 C008 12(20) . . . 3 ? C005 C001 C005 C008 -83(4) 4_455 . . 3 ? C008 C001 C005 C008 100(8) . . . 3 ? C008 C001 C005 C008 -88(18) 4_455 . . 3 ? C008 C003 C007 C008 -57(34) 4_455 . . . ? C001 C003 C007 C008 61(36) 4_455 . . . ? C001 C003 C007 C008 78(36) . . . . ? C010 C003 C007 C008 -80(35) 2_454 . . . ? C011 C003 C007 C008 165(36) . . . . ? C007 C003 C007 C008 -66(37) 4_455 . . . ? C010 C003 C007 C008 110(36) . . . . ? C008 C003 C007 C005 122(37) . . . 3_554 ? C008 C003 C007 C005 65(9) 4_455 . . 3_554 ? C001 C003 C007 C005 -177(8) 4_455 . . 3_554 ? C001 C003 C007 C005 -160(6) . . . 3_554 ? C010 C003 C007 C005 42(3) 2_454 . . 3_554 ? C011 C003 C007 C005 -73(6) . . . 3_554 ? C007 C003 C007 C005 56(9) 4_455 . . 3_554 ? C010 C003 C007 C005 -128(6) . . . 3_554 ? C008 C003 C007 C010 80(35) . . . 2_454 ? C008 C003 C007 C010 23(8) 4_455 . . 2_454 ? C001 C003 C007 C010 140(8) 4_455 . . 2_454 ? C001 C003 C007 C010 157(5) . . . 2_454 ? C011 C003 C007 C010 -115(5) . . . 2_454 ? C007 C003 C007 C010 13(8) 4_455 . . 2_454 ? C010 C003 C007 C010 -170(6) . . . 2_454 ? C008 C003 C007 C006 -108(37) . . . 2_454 ? C008 C003 C007 C006 -166(8) 4_455 . . 2_454 ? C001 C003 C007 C006 -48(9) 4_455 . . 2_454 ? C001 C003 C007 C006 -31(6) . . . 2_454 ? C010 C003 C007 C006 172(6) 2_454 . . 2_454 ? C011 C003 C007 C006 57(6) . . . 2_454 ? C007 C003 C007 C006 -175(5) 4_455 . . 2_454 ? C010 C003 C007 C006 2(8) . . . 2_454 ? C005 C007 C008 C003 -57(36) 3_554 . . . ? C010 C007 C008 C003 -93(35) 2_454 . . . ? C006 C007 C008 C003 73(36) 2_454 . . . ? C005 C007 C008 C010 36(5) 3_554 . . 2_454 ? C003 C007 C008 C010 93(35) . . . 2_454 ? C006 C007 C008 C010 166(4) 2_454 . . 2_454 ? C005 C007 C008 C008 39(18) 3_554 . . 4_455 ? C010 C007 C008 C008 3(14) 2_454 . . 4_455 ? C003 C007 C008 C008 96(40) . . . 4_455 ? C006 C007 C008 C008 169(13) 2_454 . . 4_455 ? C005 C007 C008 C001 -142(10) 3_554 . . . ? C010 C007 C008 C001 -179(13) 2_454 . . . ? C003 C007 C008 C001 -85(35) . . . . ? C006 C007 C008 C001 -13(14) 2_454 . . . ? C010 C007 C008 C005 -36(5) 2_454 . . 3_554 ? C003 C007 C008 C005 57(36) . . . 3_554 ? C006 C007 C008 C005 130(7) 2_454 . . 3_554 ? C005 C007 C008 C001 -143(23) 3_554 . . 4_455 ? C010 C007 C008 C001 -179(100) 2_454 . . 4_455 ? C003 C007 C008 C001 -86(40) . . . 4_455 ? C006 C007 C008 C001 -14(28) 2_454 . . 4_455 ? C008 C003 C008 C007 126(32) 4_455 . . . ? C001 C003 C008 C007 -126(34) 4_455 . . . ? C001 C003 C008 C007 -103(35) . . . . ? C010 C003 C008 C007 95(36) 2_454 . . . ? C011 C003 C008 C007 -16(39) . . . . ? C007 C003 C008 C007 117(36) 4_455 . . . ? C010 C003 C008 C007 -76(38) . . . . ? C008 C003 C008 C010 31(11) 4_455 . . 2_454 ? C001 C003 C008 C010 140(7) 4_455 . . 2_454 ? C001 C003 C008 C010 162(4) . . . 2_454 ? C011 C003 C008 C010 -111(6) . . . 2_454 ? C007 C003 C008 C010 -95(36) . . . 2_454 ? C007 C003 C008 C010 23(7) 4_455 . . 2_454 ? C010 C003 C008 C010 -170(6) . . . 2_454 ? C001 C003 C008 C008 108(14) 4_455 . . 4_455 ? C001 C003 C008 C008 131(11) . . . 4_455 ? C010 C003 C008 C008 -31(11) 2_454 . . 4_455 ? C011 C003 C008 C008 -142(14) . . . 4_455 ? C007 C003 C008 C008 -126(32) . . . 4_455 ? C007 C003 C008 C008 -8(6) 4_455 . . 4_455 ? C010 C003 C008 C008 159(16) . . . 4_455 ? C008 C003 C008 C001 -131(11) 4_455 . . . ? C001 C003 C008 C001 -23(5) 4_455 . . . ? C010 C003 C008 C001 -162(4) 2_454 . . . ? C011 C003 C008 C001 87(7) . . . . ? C007 C003 C008 C001 103(35) . . . . ? C007 C003 C008 C001 -140(9) 4_455 . . . ? C010 C003 C008 C001 27(5) . . . . ? C008 C003 C008 C005 74(10) 4_455 . . 3_554 ? C001 C003 C008 C005 -177(7) 4_455 . . 3_554 ? C001 C003 C008 C005 -154(5) . . . 3_554 ? C010 C003 C008 C005 43(3) 2_454 . . 3_554 ? C011 C003 C008 C005 -67(8) . . . 3_554 ? C007 C003 C008 C005 -51(34) . . . 3_554 ? C007 C003 C008 C005 66(8) 4_455 . . 3_554 ? C010 C003 C008 C005 -127(7) . . . 3_554 ? C008 C003 C008 C001 -108(14) 4_455 . . 4_455 ? C001 C003 C008 C001 23(5) . . . 4_455 ? C010 C003 C008 C001 -140(7) 2_454 . . 4_455 ? C011 C003 C008 C001 110(11) . . . 4_455 ? C007 C003 C008 C001 126(34) . . . 4_455 ? C007 C003 C008 C001 -117(12) 4_455 . . 4_455 ? C010 C003 C008 C001 50(7) . . . 4_455 ? C001 C001 C008 C007 -179(13) 4_455 . . . ? C005 C001 C008 C007 -2(19) . . . . ? C010 C001 C008 C007 107(13) . . . . ? C003 C001 C008 C007 154(17) . . . . ? C005 C001 C008 C007 -178(12) 4_455 . . . ? C008 C001 C008 C007 -179(100) 4_455 . . . ? C001 C001 C008 C003 27(7) 4_455 . . . ? C005 C001 C008 C003 -155(10) . . . . ? C010 C001 C008 C003 -46(8) . . . . ? C005 C001 C008 C003 29(9) 4_455 . . . ? C008 C001 C008 C003 27(7) 4_455 . . . ? C001 C001 C008 C010 3(7) 4_455 . . 2_454 ? C005 C001 C008 C010 -180(7) . . . 2_454 ? C010 C001 C008 C010 -71(8) . . . 2_454 ? C003 C001 C008 C010 -25(6) . . . 2_454 ? C005 C001 C008 C010 4(11) 4_455 . . 2_454 ? C008 C001 C008 C010 3(7) 4_455 . . 2_454 ? C001 C001 C008 C008 0.000(15) 4_455 . . 4_455 ? C005 C001 C008 C008 177(9) . . . 4_455 ? C010 C001 C008 C008 -74(3) . . . 4_455 ? C003 C001 C008 C008 -27(7) . . . 4_455 ? C005 C001 C008 C008 2(5) 4_455 . . 4_455 ? C001 C001 C008 C005 75(8) 4_455 . . 3_554 ? C005 C001 C008 C005 -108(10) . . . 3_554 ? C010 C001 C008 C005 1(10) . . . 3_554 ? C003 C001 C008 C005 47(8) . . . 3_554 ? C005 C001 C008 C005 76(10) 4_455 . . 3_554 ? C008 C001 C008 C005 75(8) 4_455 . . 3_554 ? C005 C001 C008 C001 177(9) . . . 4_455 ? C010 C001 C008 C001 -74(3) . . . 4_455 ? C003 C001 C008 C001 -27(7) . . . 4_455 ? C005 C001 C008 C001 2(5) 4_455 . . 4_455 ? C008 C001 C008 C001 0.00(3) 4_455 . . 4_455 ? C005 C001 C010 C001 -125(3) . . . 4_455 ? C003 C001 C010 C001 65(2) . . . 4_455 ? C005 C001 C010 C001 -40(3) 4_455 . . 4_455 ? C008 C001 C010 C001 90(3) . . . 4_455 ? C008 C001 C010 C001 42(3) 4_455 . . 4_455 ? C001 C001 C010 C005 125(3) 4_455 . . . ? C003 C001 C010 C005 -171(4) . . . . ? C005 C001 C010 C005 84(5) 4_455 . . . ? C008 C001 C010 C005 -145(5) . . . . ? C008 C001 C010 C005 166(4) 4_455 . . . ? C001 C001 C010 C005 40(3) 4_455 . . 4_455 ? C005 C001 C010 C005 -84(5) . . . 4_455 ? C003 C001 C010 C005 105(3) . . . 4_455 ? C008 C001 C010 C005 131(4) . . . 4_455 ? C008 C001 C010 C005 82(3) 4_455 . . 4_455 ? C001 C001 C010 C008 37(14) 4_455 . . 2_455 ? C005 C001 C010 C008 -88(15) . . . 2_455 ? C003 C001 C010 C008 101(14) . . . 2_455 ? C005 C001 C010 C008 -3(14) 4_455 . . 2_455 ? C008 C001 C010 C008 127(13) . . . 2_455 ? C008 C001 C010 C008 79(16) 4_455 . . 2_455 ? C001 C001 C010 C008 168(5) 4_455 . . 3 ? C005 C001 C010 C008 43(6) . . . 3 ? C003 C001 C010 C008 -128(5) . . . 3 ? C005 C001 C010 C008 127(6) 4_455 . . 3 ? C008 C001 C010 C008 -102(6) . . . 3 ? C008 C001 C010 C008 -151(4) 4_455 . . 3 ? C001 C001 C010 C011 -92.7(15) 4_455 . . . ? C005 C001 C010 C011 143(3) . . . . ? C003 C001 C010 C011 -28(2) . . . . ? C005 C001 C010 C011 -133(3) 4_455 . . . ? C008 C001 C010 C011 -2(4) . . . . ? C008 C001 C010 C011 -51(2) 4_455 . . . ? C001 C001 C010 C003 127(4) 4_455 . . 2_455 ? C005 C001 C010 C003 3(5) . . . 2_455 ? C003 C001 C010 C003 -168(3) . . . 2_455 ? C005 C001 C010 C003 87(5) 4_455 . . 2_455 ? C008 C001 C010 C003 -142(5) . . . 2_455 ? C008 C001 C010 C003 169(4) 4_455 . . 2_455 ? C001 C001 C010 C007 7(6) 4_455 . . 2_455 ? C005 C001 C010 C007 -118(7) . . . 2_455 ? C003 C001 C010 C007 71(7) . . . 2_455 ? C005 C001 C010 C007 -34(7) 4_455 . . 2_455 ? C008 C001 C010 C007 97(7) . . . 2_455 ? C008 C001 C010 C007 48(7) 4_455 . . 2_455 ? C001 C001 C010 C007 175(4) 4_455 . . 3 ? C005 C001 C010 C007 51(5) . . . 3 ? C003 C001 C010 C007 -120(5) . . . 3 ? C005 C001 C010 C007 135(5) 4_455 . . 3 ? C008 C001 C010 C007 -94(6) . . . 3 ? C008 C001 C010 C007 -143(4) 4_455 . . 3 ? C001 C001 C010 C003 -65(2) 4_455 . . . ? C005 C001 C010 C003 171(4) . . . . ? C005 C001 C010 C003 -105(3) 4_455 . . . ? C008 C001 C010 C003 26(4) . . . . ? C008 C001 C010 C003 -23(3) 4_455 . . . ? C001 C005 C010 C001 33(3) . . . 4_455 ? C007 C005 C010 C001 155(5) 3 . . 4_455 ? C005 C005 C010 C001 -52(3) 4_455 . . 4_455 ? C008 C005 C010 C001 179(4) 3 . . 4_455 ? C001 C005 C010 C001 -33(3) 4_455 . . . ? C007 C005 C010 C001 121(5) 3 . . . ? C005 C005 C010 C001 -85(3) 4_455 . . . ? C008 C005 C010 C001 146(4) 3 . . . ? C001 C005 C010 C005 85(3) . . . 4_455 ? C001 C005 C010 C005 52(3) 4_455 . . 4_455 ? C007 C005 C010 C005 -153(5) 3 . . 4_455 ? C008 C005 C010 C005 -129(4) 3 . . 4_455 ? C001 C005 C010 C008 159(4) . . . 2_455 ? C001 C005 C010 C008 125(5) 4_455 . . 2_455 ? C007 C005 C010 C008 -80(7) 3 . . 2_455 ? C005 C005 C010 C008 73(4) 4_455 . . 2_455 ? C008 C005 C010 C008 -56(6) 3 . . 2_455 ? C001 C005 C010 C008 -146(4) . . . 3 ? C001 C005 C010 C008 -179(4) 4_455 . . 3 ? C007 C005 C010 C008 -24(5) 3 . . 3 ? C005 C005 C010 C008 129(4) 4_455 . . 3 ? C001 C005 C010 C011 -56(6) . . . . ? C001 C005 C010 C011 -90(6) 4_455 . . . ? C007 C005 C010 C011 65(6) 3 . . . ? C005 C005 C010 C011 -141(6) 4_455 . . . ? C008 C005 C010 C011 89(5) 3 . . . ? C001 C005 C010 C003 -179(3) . . . 2_455 ? C001 C005 C010 C003 148(3) 4_455 . . 2_455 ? C007 C005 C010 C003 -57(5) 3 . . 2_455 ? C005 C005 C010 C003 96(3) 4_455 . . 2_455 ? C008 C005 C010 C003 -33(3) 3 . . 2_455 ? C001 C005 C010 C007 120(7) . . . 2_455 ? C001 C005 C010 C007 87(7) 4_455 . . 2_455 ? C007 C005 C010 C007 -118(10) 3 . . 2_455 ? C005 C005 C010 C007 35(6) 4_455 . . 2_455 ? C008 C005 C010 C007 -94(8) 3 . . 2_455 ? C001 C005 C010 C007 -121(5) . . . 3 ? C001 C005 C010 C007 -155(5) 4_455 . . 3 ? C005 C005 C010 C007 153(5) 4_455 . . 3 ? C008 C005 C010 C007 24(5) 3 . . 3 ? C001 C005 C010 C003 -6(3) . . . . ? C001 C005 C010 C003 -39(3) 4_455 . . . ? C007 C005 C010 C003 115(5) 3 . . . ? C005 C005 C010 C003 -91(3) 4_455 . . . ? C008 C005 C010 C003 140(4) 3 . . . ? C008 C003 C010 C001 -110(11) . . . 4_455 ? C008 C003 C010 C001 45(9) 4_455 . . 4_455 ? C001 C003 C010 C001 -65(4) . . . 4_455 ? C010 C003 C010 C001 148(2) 2_454 . . 4_455 ? C011 C003 C010 C001 148(2) . . . 4_455 ? C007 C003 C010 C001 -120(8) . . . 4_455 ? C007 C003 C010 C001 56(6) 4_455 . . 4_455 ? C008 C003 C010 C001 -45(9) . . . . ? C008 C003 C010 C001 110(11) 4_455 . . . ? C001 C003 C010 C001 65(4) 4_455 . . . ? C010 C003 C010 C001 -148(2) 2_454 . . . ? C011 C003 C010 C001 -148(2) . . . . ? C007 C003 C010 C001 -56(6) . . . . ? C007 C003 C010 C001 120(8) 4_455 . . . ? C008 C003 C010 C005 -38(10) . . . . ? C008 C003 C010 C005 117(9) 4_455 . . . ? C001 C003 C010 C005 72(3) 4_455 . . . ? C001 C003 C010 C005 7(3) . . . . ? C010 C003 C010 C005 -141(3) 2_454 . . . ? C011 C003 C010 C005 -141(3) . . . . ? C007 C003 C010 C005 -49(7) . . . . ? C007 C003 C010 C005 127(6) 4_455 . . . ? C008 C003 C010 C005 -117(9) . . . 4_455 ? C008 C003 C010 C005 38(10) 4_455 . . 4_455 ? C001 C003 C010 C005 -7(3) 4_455 . . 4_455 ? C001 C003 C010 C005 -72(3) . . . 4_455 ? C010 C003 C010 C005 141(3) 2_454 . . 4_455 ? C011 C003 C010 C005 141(3) . . . 4_455 ? C007 C003 C010 C005 -127(6) . . . 4_455 ? C007 C003 C010 C005 49(7) 4_455 . . 4_455 ? C008 C003 C010 C008 161(4) . . . 2_455 ? C008 C003 C010 C008 -44(16) 4_455 . . 2_455 ? C001 C003 C010 C008 -89(7) 4_455 . . 2_455 ? C001 C003 C010 C008 -154(6) . . . 2_455 ? C010 C003 C010 C008 58(6) 2_454 . . 2_455 ? C011 C003 C010 C008 58(6) . . . 2_455 ? C007 C003 C010 C008 150(6) . . . 2_455 ? C007 C003 C010 C008 -34(11) 4_455 . . 2_455 ? C008 C003 C010 C008 44(16) . . . 3 ? C008 C003 C010 C008 -161(4) 4_455 . . 3 ? C001 C003 C010 C008 154(6) 4_455 . . 3 ? C001 C003 C010 C008 89(7) . . . 3 ? C010 C003 C010 C008 -58(6) 2_454 . . 3 ? C011 C003 C010 C008 -58(6) . . . 3 ? C007 C003 C010 C008 34(11) . . . 3 ? C007 C003 C010 C008 -150(6) 4_455 . . 3 ? C008 C003 C010 C011 103(9) . . . . ? C008 C003 C010 C011 -103(9) 4_455 . . . ? C001 C003 C010 C011 -148(2) 4_455 . . . ? C001 C003 C010 C011 148(2) . . . . ? C010 C003 C010 C011 0.00(4) 2_454 . . . ? C007 C003 C010 C011 92(6) . . . . ? C007 C003 C010 C011 -92(6) 4_455 . . . ? C008 C003 C010 C003 103(9) . . . 2_455 ? C008 C003 C010 C003 -103(9) 4_455 . . 2_455 ? C001 C003 C010 C003 -148(2) 4_455 . . 2_455 ? C001 C003 C010 C003 148(2) . . . 2_455 ? C010 C003 C010 C003 0.00(6) 2_454 . . 2_455 ? C011 C003 C010 C003 0.00(5) . . . 2_455 ? C007 C003 C010 C003 92(6) . . . 2_455 ? C007 C003 C010 C003 -92(6) 4_455 . . 2_455 ? C008 C003 C010 C007 -180(9) . . . 2_455 ? C008 C003 C010 C007 -25(12) 4_455 . . 2_455 ? C001 C003 C010 C007 -70(5) 4_455 . . 2_455 ? C001 C003 C010 C007 -135(5) . . . 2_455 ? C010 C003 C010 C007 78(5) 2_454 . . 2_455 ? C011 C003 C010 C007 78(5) . . . 2_455 ? C007 C003 C010 C007 170(3) . . . 2_455 ? C007 C003 C010 C007 -14(11) 4_455 . . 2_455 ? C008 C003 C010 C007 25(12) . . . 3 ? C008 C003 C010 C007 180(9) 4_455 . . 3 ? C001 C003 C010 C007 135(5) 4_455 . . 3 ? C001 C003 C010 C007 70(5) . . . 3 ? C010 C003 C010 C007 -78(5) 2_454 . . 3 ? C011 C003 C010 C007 -78(5) . . . 3 ? C007 C003 C010 C007 14(11) . . . 3 ? C007 C003 C010 C007 -170(3) 4_455 . . 3 ? C001 C010 C011 C009 159.3(14) 4_455 . . . ? C001 C010 C011 C009 -159.3(14) . . . . ? C005 C010 C011 C009 -119(5) . . . . ? C005 C010 C011 C009 119(5) 4_455 . . . ? C008 C010 C011 C009 34(3) 2_455 . . . ? C008 C010 C011 C009 -34(3) 3 . . . ? C003 C010 C011 C009 0.00(2) 2_455 . . . ? C007 C010 C011 C009 64(4) 2_455 . . . ? C007 C010 C011 C009 -64(4) 3 . . . ? C003 C010 C011 C009 180.00(2) . . . . ? C001 C010 C011 C003 -20.7(14) 4_455 . . . ? C001 C010 C011 C003 20.7(14) . . . . ? C005 C010 C011 C003 61(5) . . . . ? C005 C010 C011 C003 -61(5) 4_455 . . . ? C008 C010 C011 C003 -146(3) 2_455 . . . ? C008 C010 C011 C003 146(3) 3 . . . ? C003 C010 C011 C003 180.000(8) 2_455 . . . ? C007 C010 C011 C003 -116(4) 2_455 . . . ? C007 C010 C011 C003 116(4) 3 . . . ? C008 C003 C011 C010 -112(8) . . . . ? C008 C003 C011 C010 112(8) 4_455 . . . ? C001 C003 C011 C010 20.1(17) 4_455 . . . ? C001 C003 C011 C010 -20.1(17) . . . . ? C010 C003 C011 C010 180.000(10) 2_454 . . . ? C007 C003 C011 C010 -115(5) . . . . ? C007 C003 C011 C010 115(5) 4_455 . . . ? C008 C003 C011 C009 68(8) . . . . ? C008 C003 C011 C009 -68(8) 4_455 . . . ? C001 C003 C011 C009 -159.9(17) 4_455 . . . ? C001 C003 C011 C009 159.9(17) . . . . ? C010 C003 C011 C009 0.000(14) 2_454 . . . ? C007 C003 C011 C009 65(5) . . . . ? C007 C003 C011 C009 -65(5) 4_455 . . . ? C010 C003 C011 C009 180.000(19) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 1.725 _refine_diff_density_min -7.975 _refine_diff_density_rms 0.315 data_cutet _database_code_CSD 182459 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H23 Cl2 Cu N5 O8' _chemical_formula_weight 451.75 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.2510(9) _cell_length_b 15.2479(14) _cell_length_c 13.8062(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.737(3) _cell_angle_gamma 90.00 _cell_volume 1716.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3784 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 26.99 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 1.631 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6764 _exptl_absorpt_correction_T_max 0.8539 _exptl_absorpt_process_details ;SADABS (Sheldrick, 1996) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area-detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5021 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2720 _reflns_number_gt 2516 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction SAINT _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+3.1717P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(2) _refine_ls_number_reflns 2720 _refine_ls_number_parameters 218 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.085 _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 0.79121(5) 0.16366(3) 0.61686(4) 0.02709(15) Uani 1 1 d . . . Cl1 Cl 0.7918(2) 0.15121(7) 0.12976(14) 0.0378(4) Uani 1 1 d . . . Cl2 Cl 0.38810(18) 0.10118(9) 0.35474(12) 0.0445(3) Uani 1 1 d D . . N1 N 0.7968(6) 0.2956(3) 0.5833(4) 0.0425(11) Uani 1 1 d . . . H1A H 0.7086 0.3239 0.6026 0.051 Uiso 1 1 calc R . . H1B H 0.8915 0.3209 0.6151 0.051 Uiso 1 1 calc R . . N2 N 0.8350(6) 0.1452(3) 0.4785(4) 0.0371(11) Uani 1 1 d . . . H2 H 0.7376 0.1295 0.4391 0.045 Uiso 1 1 calc R . . N3 N 0.9695(6) 0.0717(3) 0.6537(4) 0.0373(10) Uani 1 1 d . . . H3 H 0.9207 0.0167 0.6541 0.045 Uiso 1 1 calc R . . N4 N 0.7929(7) 0.1740(3) 0.7621(4) 0.0365(11) Uani 1 1 d . . . H4 H 0.8311 0.2294 0.7825 0.044 Uiso 1 1 calc R . . N5 N 0.5469(6) 0.1184(4) 0.6130(4) 0.0462(12) Uani 1 1 d . . . H5A H 0.4730 0.1615 0.5900 0.055 Uiso 1 1 calc R . . H5B H 0.5276 0.0700 0.5731 0.055 Uiso 1 1 calc R . . O11 O 0.8446(8) 0.1048(4) 0.2185(4) 0.0710(16) Uani 1 1 d . . . O12 O 0.9264(8) 0.1536(5) 0.0757(5) 0.087(2) Uani 1 1 d . . . O13 O 0.7425(9) 0.2349(3) 0.1530(5) 0.091(2) Uani 1 1 d . . . O14 O 0.6591(8) 0.1056(5) 0.0748(6) 0.089(2) Uani 1 1 d . . . O21 O 0.2861(12) 0.0884(4) 0.2658(5) 0.126(4) Uani 1 1 d D . . O22 O 0.3435(19) 0.1688(5) 0.4140(7) 0.168(6) Uani 1 1 d D . . O23 O 0.5171(12) 0.1440(11) 0.3266(8) 0.198(7) Uani 1 1 d D . . O24 O 0.430(2) 0.0309(4) 0.4058(6) 0.242(10) Uani 1 1 d D . . C1 C 0.7905(8) 0.3025(5) 0.4774(5) 0.0503(15) Uani 1 1 d . . . H1A' H 0.8345 0.3600 0.4604 0.060 Uiso 1 1 calc R . . H1B' H 0.6756 0.2978 0.4443 0.060 Uiso 1 1 calc R . . C2 C 0.8930(8) 0.2286(4) 0.4437(5) 0.0451(13) Uani 1 1 d . . . H2A H 0.8820 0.2282 0.3713 0.054 Uiso 1 1 calc R . . H2B H 1.0101 0.2373 0.4706 0.054 Uiso 1 1 calc R . . C3 C 0.9559(8) 0.0706(4) 0.4803(5) 0.0453(14) Uani 1 1 d . . . H3A H 0.8970 0.0139 0.4741 0.054 Uiso 1 1 calc R . . H3B H 1.0181 0.0762 0.4247 0.054 Uiso 1 1 calc R . . C4 C 1.0717(7) 0.0739(4) 0.5758(5) 0.0399(12) Uani 1 1 d . . . H4A H 1.1469 0.0229 0.5814 0.048 Uiso 1 1 calc R . . H4B H 1.1377 0.1283 0.5800 0.048 Uiso 1 1 calc R . . C5 C 1.0445(7) 0.0944(4) 0.7546(4) 0.0419(13) Uani 1 1 d . . . H5A' H 1.1095 0.1490 0.7548 0.050 Uiso 1 1 calc R . . H5B' H 1.1178 0.0467 0.7834 0.050 Uiso 1 1 calc R . . C6 C 0.9059(7) 0.1068(4) 0.8122(4) 0.0390(12) Uani 1 1 d . . . H6A H 0.8467 0.0507 0.8163 0.047 Uiso 1 1 calc R . . H6B H 0.9489 0.1263 0.8797 0.047 Uiso 1 1 calc R . . C7 C 0.6209(9) 0.1637(5) 0.7826(5) 0.0521(16) Uani 1 1 d . . . H7A H 0.5626 0.2205 0.7728 0.063 Uiso 1 1 calc R . . H7B H 0.6223 0.1453 0.8515 0.063 Uiso 1 1 calc R . . C8 C 0.5327(8) 0.0958(6) 0.7146(5) 0.0559(18) Uani 1 1 d . . . H8A H 0.5813 0.0373 0.7307 0.067 Uiso 1 1 calc R . . H8B H 0.4157 0.0936 0.7228 0.067 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 0.0323(3) 0.0293(3) 0.0205(3) -0.0004(3) 0.00682(19) -0.0020(3) Cl1 0.0410(6) 0.0297(6) 0.0420(10) -0.0015(6) 0.0038(6) 0.0073(6) Cl2 0.0506(8) 0.0463(7) 0.0358(7) -0.0008(6) 0.0039(6) -0.0153(6) N1 0.053(3) 0.036(2) 0.040(3) 0.007(2) 0.012(2) 0.003(2) N2 0.042(3) 0.048(3) 0.023(2) -0.011(2) 0.011(2) -0.015(2) N3 0.044(2) 0.027(2) 0.043(3) 0.0002(19) 0.016(2) -0.0012(17) N4 0.051(3) 0.029(2) 0.031(3) -0.0005(18) 0.010(2) 0.0018(18) N5 0.037(3) 0.068(3) 0.036(3) 0.000(2) 0.014(2) -0.010(2) O11 0.097(4) 0.062(3) 0.054(3) 0.010(2) 0.011(3) 0.033(3) O12 0.063(3) 0.135(6) 0.069(4) -0.009(4) 0.031(3) -0.010(3) O13 0.156(7) 0.035(3) 0.080(4) -0.009(3) 0.011(4) 0.040(3) O14 0.073(4) 0.104(5) 0.083(5) -0.023(4) -0.010(3) -0.031(3) O21 0.196(8) 0.087(4) 0.068(5) 0.028(4) -0.073(5) -0.043(5) O22 0.320(17) 0.086(5) 0.084(6) -0.004(5) -0.013(8) 0.089(8) O23 0.098(6) 0.400(19) 0.101(7) -0.015(10) 0.033(6) -0.127(9) O24 0.56(3) 0.043(3) 0.068(5) -0.003(4) -0.131(10) 0.043(7) C1 0.050(3) 0.059(4) 0.040(4) 0.019(3) 0.002(3) 0.003(3) C2 0.060(4) 0.050(3) 0.028(3) 0.005(2) 0.017(3) -0.010(3) C3 0.055(3) 0.042(3) 0.044(3) -0.019(3) 0.024(3) -0.015(3) C4 0.043(3) 0.035(3) 0.046(3) -0.005(2) 0.023(3) 0.000(2) C5 0.042(3) 0.047(3) 0.035(3) 0.015(2) 0.001(2) 0.002(2) C6 0.045(3) 0.044(3) 0.025(3) 0.005(2) 0.000(2) -0.004(2) C7 0.058(4) 0.071(4) 0.032(3) 0.003(3) 0.022(3) 0.019(3) C8 0.036(3) 0.096(5) 0.039(4) 0.012(4) 0.016(3) -0.006(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 N4 2.009(6) . ? Cu1 N2 2.017(5) . ? Cu1 N3 2.041(5) . ? Cu1 N1 2.067(5) . ? Cu1 N5 2.124(5) . ? Cl1 O13 1.392(5) . ? Cl1 O14 1.416(5) . ? Cl1 O11 1.425(5) . ? Cl1 O12 1.429(7) . ? Cl2 O24 1.300(6) . ? Cl2 O23 1.355(7) . ? Cl2 O21 1.392(5) . ? Cl2 O22 1.400(8) . ? N1 C1 1.460(8) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.466(8) . ? N2 C3 1.510(9) . ? N2 H2 0.9300 . ? N3 C4 1.464(7) . ? N3 C5 1.478(8) . ? N3 H3 0.9300 . ? N4 C6 1.484(7) . ? N4 C7 1.497(9) . ? N4 H4 0.9300 . ? N5 C8 1.467(8) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? C1 C2 1.524(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.501(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.508(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? 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 N4 Cu1 N2 168.8(2) . . ? N4 Cu1 N3 84.8(2) . . ? N2 Cu1 N3 85.0(2) . . ? N4 Cu1 N1 98.6(2) . . ? N2 Cu1 N1 84.9(2) . . ? N3 Cu1 N1 133.2(2) . . ? N4 Cu1 N5 85.0(2) . . ? N2 Cu1 N5 103.7(2) . . ? N3 Cu1 N5 115.4(2) . . ? N1 Cu1 N5 111.4(2) . . ? O13 Cl1 O14 110.2(5) . . ? O13 Cl1 O11 108.6(4) . . ? O14 Cl1 O11 109.1(4) . . ? O13 Cl1 O12 112.0(5) . . ? O14 Cl1 O12 109.4(4) . . ? O11 Cl1 O12 107.6(4) . . ? O24 Cl2 O23 113.5(11) . . ? O24 Cl2 O21 115.9(5) . . ? O23 Cl2 O21 102.1(6) . . ? O24 Cl2 O22 111.2(6) . . ? O23 Cl2 O22 95.7(9) . . ? O21 Cl2 O22 116.2(6) . . ? C1 N1 Cu1 107.2(4) . . ? C1 N1 H1A 110.3 . . ? Cu1 N1 H1A 110.3 . . ? C1 N1 H1B 110.3 . . ? Cu1 N1 H1B 110.3 . . ? H1A N1 H1B 108.5 . . ? C2 N2 C3 114.2(5) . . ? C2 N2 Cu1 107.7(4) . . ? C3 N2 Cu1 107.6(4) . . ? C2 N2 H2 109.1 . . ? C3 N2 H2 109.1 . . ? Cu1 N2 H2 109.1 . . ? C4 N3 C5 118.9(5) . . ? C4 N3 Cu1 106.0(4) . . ? C5 N3 Cu1 104.8(3) . . ? C4 N3 H3 108.9 . . ? C5 N3 H3 108.9 . . ? Cu1 N3 H3 108.9 . . ? C6 N4 C7 112.7(5) . . ? C6 N4 Cu1 108.7(4) . . ? C7 N4 Cu1 108.5(4) . . ? C6 N4 H4 109.0 . . ? C7 N4 H4 109.0 . . ? Cu1 N4 H4 109.0 . . ? C8 N5 Cu1 105.4(4) . . ? C8 N5 H5A 110.7 . . ? Cu1 N5 H5A 110.7 . . ? C8 N5 H5B 110.7 . . ? Cu1 N5 H5B 110.7 . . ? H5A N5 H5B 108.8 . . ? N1 C1 C2 108.4(5) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 108.5(5) . . ? 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 . . ? C4 C3 N2 108.6(4) . . ? C4 C3 H3A 110.0 . . ? N2 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? N2 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N3 C4 C3 106.4(5) . . ? N3 C4 H4A 110.4 . . ? C3 C4 H4A 110.4 . . ? N3 C4 H4B 110.4 . . ? C3 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? N3 C5 C6 106.6(5) . . ? N3 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? N3 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? N4 C6 C5 108.4(5) . . ? N4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? N4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N4 C7 C8 109.7(5) . . ? N4 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N4 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N5 C8 C7 109.4(6) . . ? N5 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? N5 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? 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 N4 Cu1 N1 C1 -178.1(4) . . . . ? N2 Cu1 N1 C1 12.6(4) . . . . ? N3 Cu1 N1 C1 90.9(5) . . . . ? N5 Cu1 N1 C1 -90.1(4) . . . . ? N4 Cu1 N2 C2 -92.6(12) . . . . ? N3 Cu1 N2 C2 -118.0(4) . . . . ? N1 Cu1 N2 C2 16.3(4) . . . . ? N5 Cu1 N2 C2 127.1(4) . . . . ? N4 Cu1 N2 C3 31.0(12) . . . . ? N3 Cu1 N2 C3 5.6(3) . . . . ? N1 Cu1 N2 C3 139.9(4) . . . . ? N5 Cu1 N2 C3 -109.3(4) . . . . ? N4 Cu1 N3 C4 -151.1(4) . . . . ? N2 Cu1 N3 C4 24.1(4) . . . . ? N1 Cu1 N3 C4 -54.1(5) . . . . ? N5 Cu1 N3 C4 126.9(4) . . . . ? N4 Cu1 N3 C5 -24.6(4) . . . . ? N2 Cu1 N3 C5 150.6(4) . . . . ? N1 Cu1 N3 C5 72.4(5) . . . . ? N5 Cu1 N3 C5 -106.6(4) . . . . ? N2 Cu1 N4 C6 -30.3(13) . . . . ? N3 Cu1 N4 C6 -4.9(4) . . . . ? N1 Cu1 N4 C6 -137.9(4) . . . . ? N5 Cu1 N4 C6 111.2(4) . . . . ? N2 Cu1 N4 C7 -153.1(10) . . . . ? N3 Cu1 N4 C7 -127.7(4) . . . . ? N1 Cu1 N4 C7 99.3(4) . . . . ? N5 Cu1 N4 C7 -11.6(4) . . . . ? N4 Cu1 N5 C8 -15.9(5) . . . . ? N2 Cu1 N5 C8 157.0(5) . . . . ? N3 Cu1 N5 C8 66.0(5) . . . . ? N1 Cu1 N5 C8 -113.2(5) . . . . ? Cu1 N1 C1 C2 -38.1(6) . . . . ? C3 N2 C2 C1 -161.0(5) . . . . ? Cu1 N2 C2 C1 -41.5(6) . . . . ? N1 C1 C2 N2 54.1(7) . . . . ? C2 N2 C3 C4 85.5(6) . . . . ? Cu1 N2 C3 C4 -34.0(5) . . . . ? C5 N3 C4 C3 -166.1(5) . . . . ? Cu1 N3 C4 C3 -48.5(5) . . . . ? N2 C3 C4 N3 55.6(6) . . . . ? C4 N3 C5 C6 167.2(5) . . . . ? Cu1 N3 C5 C6 49.1(5) . . . . ? C7 N4 C6 C5 153.8(5) . . . . ? Cu1 N4 C6 C5 33.6(5) . . . . ? N3 C5 C6 N4 -55.8(6) . . . . ? C6 N4 C7 C8 -83.1(6) . . . . ? Cu1 N4 C7 C8 37.2(6) . . . . ? Cu1 N5 C8 C7 40.3(6) . . . . ? N4 C7 C8 N5 -53.1(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O12 0.92 2.33 3.139(8) 147.1 4_455 N1 H1A O21 0.92 2.61 3.091(9) 112.8 4 N2 H2 O23 0.93 2.22 3.099(12) 158.2 . N3 H3 O11 0.93 2.19 3.063(7) 156.5 2 N4 H4 O22 0.93 2.38 3.170(10) 142.9 4 N5 H5A O22 0.92 2.50 3.091(11) 121.9 . N5 H5B O24 0.92 2.40 3.172(9) 141.0 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.763 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.084