# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 _publ_contact_author_name 'Dr Randolf Kohn' _publ_contact_author_address ; Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_phone '# 44 1225 38 3305' _publ_contact_author_fax '# 44 1225 82 6231' _publ_contact_author_email r.d.kohn@bath.ac.uk _publ_requested_journal ChemComm _publ_requested_coeditor_name ; Zhida Pan, Mary F.Mahon, Gabriele Kociok-K\"ohn, ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; Trimethyltriazacyclohexane as bridging ligand for triangular Cu3 units and C-H hydride abstraction into a Cu6 cluster ; loop_ _publ_author_name _publ_author_address 'Randolf Dag Kohn' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Zhida Pan' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Mary F. Mahon' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Gabriele Kociok-Kohn' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; #============================================================================== data_pan24 _database_code_CSD 205861 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C24 H60 Cl4 Cu6 N12)(B F4)2(C H2 Cl2)2]' _chemical_formula_sum 'C26 H64 B2 Cl8 Cu6 F8 N12' _chemical_formula_weight 1383.35 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'P 1 21/n 1' 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 15.2550(12) _cell_length_b 8.3930(8) _cell_length_c 19.7430(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.893(3) _cell_angle_gamma 90.00 _cell_volume 2524.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.971 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6642 _exptl_absorpt_correction_T_max 0.7970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method \f-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7518 _diffrn_reflns_av_R_equivalents 0.1481 _diffrn_reflns_av_sigmaI/netI 0.2316 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4191 _reflns_number_gt 1603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'Collect, Nonius program suite version 1.9 (1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _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^)+(0.1248P)^2^+16.9545P] 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 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4191 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2489 _refine_ls_R_factor_gt 0.1071 _refine_ls_wR_factor_ref 0.3346 _refine_ls_wR_factor_gt 0.2557 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.29295(12) 0.5897(4) 0.54460(10) 0.0734(11) Uani 1 1 d . . . Cu2 Cu 0.46351(12) 0.6486(4) 0.52058(10) 0.0741(10) Uani 1 1 d . . . Cu3 Cu 0.33881(13) 0.8776(4) 0.52589(10) 0.0762(11) Uani 1 1 d . . . Cl1 Cl 0.3856(3) 0.3878(8) 0.5121(2) 0.081(2) Uani 1 1 d . . . Cl2 Cl 0.4202(3) 0.8213(8) 0.4362(2) 0.082(2) Uani 1 1 d . . . C1 C 0.3180(11) 0.786(3) 0.6640(8) 0.085(9) Uani 1 1 d . . . H1A H 0.3352 0.7944 0.7129 0.102 Uiso 1 1 calc R . . H1B H 0.2558 0.8187 0.6577 0.102 Uiso 1 1 calc R . . N1 N 0.3261(9) 0.624(3) 0.6433(7) 0.072(6) Uani 1 1 d . . . C11 C 0.2690(11) 0.527(3) 0.6834(9) 0.067(6) Uani 1 1 d . . . H11A H 0.2738 0.4153 0.6700 0.101 Uiso 1 1 calc R . . H11B H 0.2082 0.5630 0.6755 0.101 Uiso 1 1 calc R . . H11C H 0.2865 0.5387 0.7316 0.101 Uiso 1 1 calc R . . C2 C 0.4221(8) 0.588(3) 0.6624(8) 0.062(6) Uani 1 1 d . . . H2A H 0.4337 0.6075 0.7114 0.075 Uiso 1 1 calc R . . H2B H 0.4339 0.4735 0.6537 0.075 Uiso 1 1 calc R . . N2 N 0.4806(8) 0.684(3) 0.6244(7) 0.067(5) Uani 1 1 d . . . C21 C 0.5708(10) 0.642(3) 0.6478(8) 0.088(8) Uani 1 1 d . . . H21A H 0.6124 0.7091 0.6244 0.132 Uiso 1 1 calc R . . H21B H 0.5819 0.5299 0.6379 0.132 Uiso 1 1 calc R . . H21C H 0.5783 0.6603 0.6968 0.132 Uiso 1 1 calc R . . C3 C 0.4646(10) 0.852(4) 0.6425(9) 0.088(9) Uani 1 1 d . . . H3A H 0.4766 0.8668 0.6918 0.106 Uiso 1 1 calc R . . H3B H 0.5048 0.9216 0.6183 0.106 Uiso 1 1 calc R . . N3 N 0.3741(10) 0.896(3) 0.6245(7) 0.073(6) Uani 1 1 d . . . C31 C 0.3614(12) 1.057(3) 0.6450(10) 0.084(8) Uani 1 1 d . . . H31A H 0.3008 1.0895 0.6331 0.126 Uiso 1 1 calc R . . H31B H 0.4019 1.1267 0.6219 0.126 Uiso 1 1 calc R . . H31C H 0.3726 1.0661 0.6942 0.126 Uiso 1 1 calc R . . C4 C 0.1120(10) 0.666(3) 0.5272(9) 0.072(7) Uani 1 1 d . . . H4A H 0.0583 0.6902 0.4988 0.087 Uiso 1 1 calc R . . H4B H 0.0999 0.5736 0.5564 0.087 Uiso 1 1 calc R . . N4 N 0.1853(9) 0.629(3) 0.4836(8) 0.088(7) Uani 1 1 d . . . C41 C 0.1648(12) 0.481(4) 0.4410(9) 0.121(12) Uani 1 1 d . . . H41A H 0.1577 0.3894 0.4709 0.182 Uiso 1 1 calc R . . H41B H 0.2132 0.4608 0.4113 0.182 Uiso 1 1 calc R . . H41C H 0.1105 0.4981 0.4133 0.182 Uiso 1 1 calc R . . C5 C 0.1942(11) 0.765(3) 0.4390(10) 0.080(8) Uani 1 1 d . . . H5A H 0.1384 0.7809 0.4120 0.096 Uiso 1 1 calc R . . H5B H 0.2407 0.7425 0.4071 0.096 Uiso 1 1 calc R . . N5 N 0.2164(8) 0.912(3) 0.4768(8) 0.097(8) Uani 1 1 d . . . C51 C 0.2233(12) 1.042(3) 0.4312(11) 0.098(8) Uani 1 1 d . . . H51A H 0.2363 1.1394 0.4569 0.146 Uiso 1 1 calc R . . H51B H 0.1678 1.0543 0.4045 0.146 Uiso 1 1 calc R . . H51C H 0.2707 1.0206 0.4007 0.146 Uiso 1 1 calc R . . C6 C 0.1444(11) 0.930(3) 0.5250(9) 0.076(7) Uani 1 1 d . . . H6A H 0.1564 1.0257 0.5536 0.092 Uiso 1 1 calc R . . H6B H 0.0882 0.9484 0.4988 0.092 Uiso 1 1 calc R . . N6 N 0.1357(8) 0.797(3) 0.5671(8) 0.077(6) Uani 1 1 d . . . C61 C 0.0655(12) 0.825(3) 0.6159(10) 0.107(10) Uani 1 1 d . . . H61A H 0.0808 0.9183 0.6442 0.160 Uiso 1 1 calc R . . H61B H 0.0602 0.7314 0.6449 0.160 Uiso 1 1 calc R . . H61C H 0.0095 0.8447 0.5908 0.160 Uiso 1 1 calc R . . B B 0.5663(17) 0.220(4) 0.1480(13) 0.088(10) Uani 1 1 d . . . F1 F 0.5616(6) 0.069(2) 0.1775(6) 0.092(4) Uani 1 1 d . . . F2 F 0.6432(5) 0.2911(16) 0.1729(5) 0.079(4) Uani 1 1 d . . . F3 F 0.4945(7) 0.3062(18) 0.1709(6) 0.102(5) Uani 1 1 d . . . F4 F 0.5635(7) 0.2120(19) 0.0808(5) 0.103(5) Uani 1 1 d . . . C7 C 0.1024(17) 0.387(4) 0.2453(12) 0.121(11) Uani 1 1 d . . . H7A H 0.0815 0.3978 0.1972 0.146 Uiso 1 1 calc R . . H7B H 0.0646 0.4540 0.2731 0.146 Uiso 1 1 calc R . . Cl3 Cl 0.0958(5) 0.1790(13) 0.2717(4) 0.153(4) Uani 1 1 d . . . Cl4 Cl 0.2099(5) 0.4506(17) 0.2552(4) 0.204(6) 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 0.0328(11) 0.146(3) 0.0412(12) -0.0015(14) -0.0059(9) 0.0063(14) Cu2 0.0380(12) 0.145(3) 0.0389(12) 0.0003(15) 0.0015(9) 0.0017(15) Cu3 0.0431(12) 0.144(3) 0.0415(13) 0.0064(15) 0.0011(9) 0.0043(15) Cl1 0.035(2) 0.153(6) 0.054(3) -0.001(3) 0.0055(19) -0.007(3) Cl2 0.044(2) 0.163(6) 0.040(2) 0.012(3) 0.0091(19) 0.004(3) C1 0.038(9) 0.20(3) 0.015(8) -0.018(13) 0.015(7) -0.017(14) N1 0.038(8) 0.152(19) 0.025(7) -0.015(10) -0.004(6) -0.002(10) C11 0.050(10) 0.098(19) 0.053(11) 0.005(12) -0.002(9) -0.004(12) C2 0.018(7) 0.13(2) 0.041(9) -0.015(11) -0.004(7) -0.015(10) N2 0.030(7) 0.121(17) 0.050(9) -0.025(10) -0.006(7) 0.004(10) C21 0.028(8) 0.19(3) 0.043(10) 0.009(13) -0.006(7) 0.010(13) C3 0.019(8) 0.20(3) 0.045(11) 0.036(15) 0.004(7) -0.015(13) N3 0.061(10) 0.129(18) 0.031(8) -0.023(10) 0.014(7) 0.004(11) C31 0.047(11) 0.16(3) 0.049(12) 0.013(15) 0.001(9) -0.012(14) C4 0.035(9) 0.14(2) 0.042(10) -0.001(13) 0.000(8) 0.003(12) N4 0.038(8) 0.18(2) 0.044(9) -0.016(13) -0.013(7) 0.001(11) C41 0.056(12) 0.26(4) 0.043(12) -0.005(18) -0.018(10) -0.042(18) C5 0.042(11) 0.14(2) 0.051(12) 0.036(15) -0.014(9) -0.014(13) N5 0.024(7) 0.22(3) 0.043(9) 0.024(14) -0.002(7) 0.012(11) C51 0.056(12) 0.15(2) 0.081(15) 0.054(17) -0.017(11) 0.004(15) C6 0.044(10) 0.14(2) 0.049(11) 0.007(14) 0.001(9) 0.028(12) N6 0.034(8) 0.16(2) 0.039(8) 0.013(12) -0.005(7) 0.019(10) C61 0.051(11) 0.21(3) 0.061(13) 0.042(17) 0.018(10) 0.032(16) B 0.067(17) 0.13(3) 0.061(17) 0.015(19) -0.018(13) -0.019(19) F1 0.050(6) 0.164(14) 0.064(7) -0.008(9) 0.011(5) 0.001(8) F2 0.036(5) 0.137(11) 0.063(6) -0.006(7) -0.014(5) -0.021(6) F3 0.050(6) 0.166(14) 0.088(8) 0.003(9) -0.004(6) 0.006(8) F4 0.084(8) 0.185(15) 0.039(6) -0.032(7) -0.008(5) -0.029(9) C7 0.13(2) 0.16(3) 0.077(16) 0.031(18) -0.011(15) 0.01(2) Cl3 0.138(6) 0.239(11) 0.085(5) 0.018(6) 0.038(4) 0.034(7) Cl4 0.122(6) 0.386(17) 0.106(6) -0.047(8) 0.028(5) -0.086(9) _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 N1 2.009(13) . ? Cu1 N4 2.014(13) . ? Cu1 Cl1 2.318(6) . ? Cu1 Cu3 2.547(4) . ? Cu1 Cu2 2.714(3) . ? Cu2 N2 2.075(14) . ? Cu2 Cl2 2.280(6) . ? Cu2 Cl1 2.441(5) 3_666 ? Cu2 Cl1 2.493(7) . ? Cu2 Cu3 2.710(4) . ? Cu2 Cu2 2.866(6) 3_666 ? Cu3 N3 1.999(14) . ? Cu3 N5 2.081(13) . ? Cu3 Cl2 2.262(5) . ? Cl1 Cu2 2.441(5) 3_666 ? C1 N1 1.43(3) . ? C1 N3 1.51(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C11 1.45(2) . ? N1 C2 1.525(19) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C2 N2 1.44(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C21 1.47(2) . ? N2 C3 1.48(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C3 N3 1.46(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.43(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C4 N6 1.39(3) . ? C4 N4 1.48(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N4 C5 1.45(3) . ? N4 C41 1.52(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C5 N5 1.47(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? N5 C51 1.42(3) . ? N5 C6 1.50(2) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C6 N6 1.40(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N6 C61 1.49(2) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? B F4 1.33(3) . ? B F2 1.39(3) . ? B F1 1.40(3) . ? B F3 1.41(3) . ? C7 Cl4 1.72(3) . ? C7 Cl3 1.83(3) . ? C7 H7A 0.9900 . ? C7 H7B 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 N1 Cu1 N4 135.6(7) . . ? N1 Cu1 Cl1 104.2(6) . . ? N4 Cu1 Cl1 116.4(6) . . ? N1 Cu1 Cu3 87.1(6) . . ? N4 Cu1 Cu3 88.8(7) . . ? Cl1 Cu1 Cu3 118.53(17) . . ? N1 Cu1 Cu2 87.0(4) . . ? N4 Cu1 Cu2 128.7(5) . . ? Cl1 Cu1 Cu2 58.76(15) . . ? Cu3 Cu1 Cu2 61.91(10) . . ? N2 Cu2 Cl2 130.4(6) . . ? N2 Cu2 Cl1 101.9(4) . 3_666 ? Cl2 Cu2 Cl1 97.40(19) . 3_666 ? N2 Cu2 Cl1 103.1(6) . . ? Cl2 Cu2 Cl1 112.9(2) . . ? Cl1 Cu2 Cl1 108.99(17) 3_666 . ? N2 Cu2 Cu3 85.1(5) . . ? Cl2 Cu2 Cu3 53.08(15) . . ? Cl1 Cu2 Cu3 140.5(2) 3_666 . ? Cl1 Cu2 Cu3 106.98(15) . . ? N2 Cu2 Cu1 85.8(4) . . ? Cl2 Cu2 Cu1 89.89(14) . . ? Cl1 Cu2 Cu1 161.6(2) 3_666 . ? Cl1 Cu2 Cu1 52.66(14) . . ? Cu3 Cu2 Cu1 56.03(10) . . ? N2 Cu2 Cu2 111.9(6) . 3_666 ? Cl2 Cu2 Cu2 116.66(19) . 3_666 ? Cl1 Cu2 Cu2 55.33(17) 3_666 3_666 ? Cl1 Cu2 Cu2 53.66(15) . 3_666 ? Cu3 Cu2 Cu2 155.75(14) . 3_666 ? Cu1 Cu2 Cu2 106.30(16) . 3_666 ? N3 Cu3 N5 129.4(6) . . ? N3 Cu3 Cl2 130.3(5) . . ? N5 Cu3 Cl2 100.3(5) . . ? N3 Cu3 Cu1 89.6(6) . . ? N5 Cu3 Cu1 87.2(7) . . ? Cl2 Cu3 Cu1 94.6(2) . . ? N3 Cu3 Cu2 86.4(5) . . ? N5 Cu3 Cu2 134.1(7) . . ? Cl2 Cu3 Cu2 53.69(16) . . ? Cu1 Cu3 Cu2 62.06(10) . . ? Cu1 Cl1 Cu2 139.5(3) . 3_666 ? Cu1 Cl1 Cu2 68.6(2) . . ? Cu2 Cl1 Cu2 71.01(17) 3_666 . ? Cu3 Cl2 Cu2 73.24(16) . . ? N1 C1 N3 112.2(15) . . ? N1 C1 H1A 109.2 . . ? N3 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? N3 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 N1 C11 108.2(15) . . ? C1 N1 C2 102.4(15) . . ? C11 N1 C2 110.5(15) . . ? C1 N1 Cu1 113.0(13) . . ? C11 N1 Cu1 108.8(12) . . ? C2 N1 Cu1 113.7(11) . . ? 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 . . ? N2 C2 N1 111.9(15) . . ? N2 C2 H2A 109.2 . . ? N1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? N1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 N2 C21 107.3(16) . . ? C2 N2 C3 107.1(15) . . ? C21 N2 C3 108.3(15) . . ? C2 N2 Cu2 112.5(11) . . ? C21 N2 Cu2 110.2(11) . . ? C3 N2 Cu2 111.1(13) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C3 N2 110.5(18) . . ? N3 C3 H3A 109.5 . . ? N2 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C31 N3 C3 108.2(18) . . ? C31 N3 C1 110.2(16) . . ? C3 N3 C1 105.9(16) . . ? C31 N3 Cu3 108.3(14) . . ? C3 N3 Cu3 115.1(12) . . ? C1 N3 Cu3 109.0(11) . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C4 N4 108.3(16) . . ? N6 C4 H4A 110.0 . . ? N4 C4 H4A 110.0 . . ? N6 C4 H4B 110.0 . . ? N4 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C5 N4 C4 106.5(19) . . ? C5 N4 C41 109.1(17) . . ? C4 N4 C41 110.7(17) . . ? C5 N4 Cu1 113.2(12) . . ? C4 N4 Cu1 107.7(10) . . ? C41 N4 Cu1 109.6(14) . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C5 N5 112.1(18) . . ? N4 C5 H5A 109.2 . . ? N5 C5 H5A 109.2 . . ? N4 C5 H5B 109.2 . . ? N5 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C51 N5 C5 110.0(17) . . ? C51 N5 C6 114(2) . . ? C5 N5 C6 104.7(18) . . ? C51 N5 Cu3 107.9(13) . . ? C5 N5 Cu3 107.3(14) . . ? C6 N5 Cu3 112.9(11) . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N6 C6 N5 112.8(19) . . ? N6 C6 H6A 109.0 . . ? N5 C6 H6A 109.0 . . ? N6 C6 H6B 109.0 . . ? N5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C4 N6 C6 108.9(15) . . ? C4 N6 C61 108.4(17) . . ? C6 N6 C61 110.5(18) . . ? N6 C61 H61A 109.5 . . ? N6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? F4 B F2 111(2) . . ? F4 B F1 112(3) . . ? F2 B F1 108(2) . . ? F4 B F3 111(2) . . ? F2 B F3 109(2) . . ? F1 B F3 106(2) . . ? Cl4 C7 Cl3 109.1(14) . . ? Cl4 C7 H7A 109.9 . . ? Cl3 C7 H7A 109.9 . . ? Cl4 C7 H7B 109.9 . . ? Cl3 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.726 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.170 #============================================================================== #_eof # End of Crystallographic Information File data_pan21 _database_code_CSD 205862 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Cu6 C18 H46 Cl4 N9)(B F4)(C H2 Cl2)2' _chemical_formula_sum 'C20 H50 B Cl8 Cu6 F4 N9' _chemical_formula_weight 1168.34 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 14.9910(3) _cell_length_b 13.4050(4) _cell_length_c 20.3130(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4081.99(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 63158 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 3.641 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.3796 _exptl_absorpt_correction_T_max 0.8389 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method \f-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 49424 _diffrn_reflns_av_R_equivalents 0.1297 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.43 _reflns_number_total 4830 _reflns_number_gt 3596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'Collect, Nonius program suite version 1.9 (1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SHELXS-86 Program for Crystal Structure Solution. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1986. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _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^)+(0.0713P)^2^+7.4004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4830 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.93884(4) 0.15637(4) 0.33946(3) 0.03065(15) Uani 1 1 d . . . Cu2 Cu 0.80560(4) 0.15409(4) 0.42924(3) 0.03004(15) Uani 1 1 d . . . Cu3 Cu 0.96217(5) 0.2500 0.44198(4) 0.02935(18) Uani 1 2 d S . . Cu4 Cu 0.78620(5) 0.2500 0.31474(4) 0.0343(2) Uani 1 2 d S . . Cl1 Cl 0.97863(11) 0.2500 0.24304(8) 0.0371(3) Uani 1 2 d S . . Cl2 Cl 0.66378(10) 0.2500 0.41217(8) 0.0378(4) Uani 1 2 d S . . Cl3 Cl 1.04516(7) 0.10353(9) 0.41821(5) 0.0364(3) Uani 1 1 d . . . C1 C 0.8273(3) 0.0502(4) 0.2468(2) 0.0362(10) Uani 1 1 d . . . H1A H 0.8050 -0.0123 0.2267 0.043 Uiso 1 1 calc R . . H1B H 0.8580 0.0893 0.2122 0.043 Uiso 1 1 calc R . . N1 N 0.8902(2) 0.0266(3) 0.30013(19) 0.0336(8) Uani 1 1 d . . . C11 C 0.9655(3) -0.0322(4) 0.2721(3) 0.0428(12) Uani 1 1 d . . . H11A H 0.9956 0.0072 0.2381 0.064 Uiso 1 1 calc R . . H11B H 0.9424 -0.0939 0.2526 0.064 Uiso 1 1 calc R . . H11C H 1.0080 -0.0486 0.3072 0.064 Uiso 1 1 calc R . . C2 C 0.8449(3) -0.0328(3) 0.3507(2) 0.0396(11) Uani 1 1 d . . . H2A H 0.8874 -0.0490 0.3865 0.048 Uiso 1 1 calc R . . H2B H 0.8238 -0.0963 0.3313 0.048 Uiso 1 1 calc R . . N2 N 0.7687(3) 0.0227(3) 0.3779(2) 0.0381(9) Uani 1 1 d . . . C21 C 0.7209(4) -0.0463(4) 0.4233(3) 0.0558(15) Uani 1 1 d . . . H21A H 0.6694 -0.0119 0.4425 0.084 Uiso 1 1 calc R . . H21B H 0.7613 -0.0674 0.4585 0.084 Uiso 1 1 calc R . . H21C H 0.7004 -0.1049 0.3988 0.084 Uiso 1 1 calc R . . C3 C 0.7075(3) 0.0457(4) 0.3233(2) 0.0435(12) Uani 1 1 d . . . H3A H 0.6873 -0.0173 0.3026 0.052 Uiso 1 1 calc R . . H3B H 0.6543 0.0807 0.3406 0.052 Uiso 1 1 calc R . . N3 N 0.7514(2) 0.1085(3) 0.27354(19) 0.0353(8) Uani 1 1 d . . . C31 C 0.6883(3) 0.1217(4) 0.2176(3) 0.0474(13) Uani 1 1 d . . . H31A H 0.7160 0.1635 0.1837 0.071 Uiso 1 1 calc R . . H31B H 0.6336 0.1539 0.2334 0.071 Uiso 1 1 calc R . . H31C H 0.6736 0.0563 0.1989 0.071 Uiso 1 1 calc R . . C4 C 0.7617(4) 0.2500 0.5575(3) 0.0322(13) Uani 1 2 d S . . H4A H 0.7002 0.2500 0.5396 0.039 Uiso 1 2 calc SR . . H4B H 0.7579 0.2500 0.6061 0.039 Uiso 1 2 calc SR . . N4 N 0.8093(2) 0.1597(3) 0.53500(18) 0.0302(8) Uani 1 1 d . . . C41 C 0.7609(3) 0.0728(4) 0.5647(2) 0.0379(10) Uani 1 1 d . . . H41A H 0.7000 0.0701 0.5472 0.057 Uiso 1 1 calc R . . H41B H 0.7587 0.0806 0.6126 0.057 Uiso 1 1 calc R . . H41C H 0.7923 0.0109 0.5536 0.057 Uiso 1 1 calc R . . C5 C 0.8999(3) 0.1598(3) 0.5635(2) 0.0332(10) Uani 1 1 d . . . H5A H 0.8962 0.1590 0.6121 0.040 Uiso 1 1 calc R . . H5B H 0.9326 0.0994 0.5491 0.040 Uiso 1 1 calc R . . N5 N 0.9477(3) 0.2500 0.5414(2) 0.0304(11) Uani 1 2 d S . . C51 C 1.0377(5) 0.2500 0.5705(3) 0.0400(15) Uani 1 2 d S . . H51A H 1.0700 0.3098 0.5563 0.060 Uiso 0.50 1 calc PR . . H51B H 1.0702 0.1905 0.5560 0.060 Uiso 0.50 1 calc PR . . H51C H 1.0330 0.2497 0.6186 0.060 Uiso 1 2 calc SR . . B1 B 0.7066(6) 0.7500 0.2523(4) 0.0430(18) Uani 1 2 d S . . F1 F 0.7060(4) 0.7500 0.3190(2) 0.0601(13) Uani 1 2 d S . . F2 F 0.6681(4) 0.8330(3) 0.22743(19) 0.0890(15) Uani 1 1 d . . . F3 F 0.7940(4) 0.7500 0.2307(3) 0.116(3) Uani 1 2 d S . . C6 C 0.5175(7) 0.2500 0.6451(5) 0.084(3) Uani 1 2 d S . . H6A H 0.5722 0.2500 0.6725 0.100 Uiso 1 2 calc SR . . H6B H 0.4654 0.2500 0.6751 0.100 Uiso 1 2 calc SR . . Cl4 Cl 0.51531(15) 0.1421(2) 0.59692(12) 0.1085(8) Uani 1 1 d . . . C7 C 0.4387(8) 0.2245(14) 0.4291(6) 0.066(7) Uani 0.50 1 d P . . H7A H 0.4736 0.2512 0.4666 0.080 Uiso 1 2 calc SR . . H7B H 0.4615 0.2543 0.3878 0.080 Uiso 0.50 1 calc PR . . Cl5 Cl 0.3255(2) 0.2500 0.43906(18) 0.1228(15) Uani 1 2 d S . . Cl6 Cl 0.4455(3) 0.0938(3) 0.42633(19) 0.0848(12) Uani 0.50 1 d P . . H H 0.870(6) 0.2500 0.383(5) 0.08(3) Uiso 1 2 d S . . 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 0.0249(3) 0.0320(3) 0.0350(3) -0.0027(2) 0.0003(2) 0.0005(2) Cu2 0.0252(3) 0.0332(3) 0.0317(3) -0.0014(2) 0.0020(2) -0.0035(2) Cu3 0.0237(4) 0.0342(4) 0.0302(4) 0.000 0.0000(3) 0.000 Cu4 0.0264(4) 0.0385(4) 0.0379(4) 0.000 -0.0058(3) 0.000 Cl1 0.0356(8) 0.0438(9) 0.0318(7) 0.000 0.0048(6) 0.000 Cl2 0.0216(7) 0.0486(9) 0.0433(8) 0.000 0.0000(6) 0.000 Cl3 0.0300(5) 0.0391(6) 0.0401(6) 0.0001(5) -0.0015(4) 0.0094(5) C1 0.028(2) 0.043(3) 0.037(2) -0.008(2) -0.0031(18) -0.0011(19) N1 0.0260(18) 0.033(2) 0.042(2) -0.0041(16) -0.0001(15) 0.0044(15) C11 0.029(2) 0.039(3) 0.060(3) -0.016(2) 0.002(2) 0.005(2) C2 0.046(3) 0.031(2) 0.042(3) -0.0032(19) -0.001(2) -0.006(2) N2 0.039(2) 0.036(2) 0.039(2) -0.0056(17) 0.0088(17) -0.0100(17) C21 0.066(4) 0.050(3) 0.051(3) -0.008(3) 0.015(3) -0.032(3) C3 0.031(2) 0.051(3) 0.048(3) -0.014(2) 0.003(2) -0.013(2) N3 0.0255(18) 0.045(2) 0.0352(19) -0.0070(17) -0.0050(15) -0.0011(17) C31 0.036(3) 0.057(3) 0.049(3) -0.015(2) -0.015(2) 0.004(2) C4 0.031(3) 0.036(3) 0.030(3) 0.000 0.006(2) 0.000 N4 0.0253(18) 0.0327(19) 0.0326(19) 0.0000(15) 0.0037(14) -0.0031(15) C41 0.034(2) 0.036(2) 0.043(3) 0.006(2) 0.0055(19) -0.007(2) C5 0.031(2) 0.038(2) 0.031(2) 0.0033(18) 0.0009(17) 0.0026(19) N5 0.028(3) 0.033(3) 0.030(3) 0.000 -0.001(2) 0.000 C51 0.030(3) 0.051(4) 0.040(4) 0.000 -0.005(3) 0.000 B1 0.059(5) 0.032(4) 0.038(4) 0.000 0.002(4) 0.000 F1 0.096(4) 0.050(3) 0.034(2) 0.000 0.006(2) 0.000 F2 0.158(5) 0.048(2) 0.061(2) -0.0064(17) -0.035(3) 0.032(2) F3 0.068(4) 0.211(9) 0.069(4) 0.000 0.020(3) 0.000 C6 0.055(6) 0.131(10) 0.065(6) 0.000 -0.002(5) 0.000 Cl4 0.0629(12) 0.180(3) 0.0826(14) -0.0149(15) 0.0013(10) -0.0070(14) C7 0.045(6) 0.10(2) 0.052(6) -0.011(7) -0.004(4) -0.003(7) Cl5 0.0554(17) 0.221(5) 0.092(2) 0.000 0.0058(15) 0.000 Cl6 0.095(3) 0.091(3) 0.069(2) 0.0017(19) -0.0027(19) -0.038(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.048(4) . ? Cu1 Cl3 2.3668(12) . ? Cu1 Cl1 2.4014(14) . ? Cu1 Cu3 2.4566(8) . ? Cu1 Cu1 2.5103(11) 8_565 ? Cu1 Cu4 2.6577(8) . ? Cu1 Cu2 2.7049(8) . ? Cu1 H 1.84(7) . ? Cu2 N2 2.120(4) . ? Cu2 N4 2.150(4) . ? Cu2 Cl2 2.5087(14) . ? Cu2 Cu2 2.5713(11) 8_565 ? Cu2 Cu4 2.6734(9) . ? Cu2 Cu3 2.6887(8) . ? Cu2 H 1.87(7) . ? Cu3 N5 2.031(5) . ? Cu3 Cl3 2.3740(12) 8_565 ? Cu3 Cl3 2.3740(12) . ? Cu3 Cu1 2.4566(8) 8_565 ? Cu3 Cu2 2.6887(8) 8_565 ? Cu3 H 1.83(10) . ? Cu4 N3 2.138(4) . ? Cu4 N3 2.138(4) 8_565 ? Cu4 Cu1 2.6577(8) 8_565 ? Cu4 Cu2 2.6734(9) 8_565 ? Cu4 Cl2 2.6989(18) . ? Cu4 H 1.87(9) . ? Cl1 Cu1 2.4014(14) 8_565 ? Cl2 Cu2 2.5087(14) 8_565 ? C1 N1 1.472(6) . ? C1 N3 1.484(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.467(6) . ? N1 C11 1.489(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C2 N2 1.472(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.472(7) . ? N2 C21 1.491(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C3 N3 1.471(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.489(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C4 N4 1.477(5) 8_565 ? C4 N4 1.477(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N4 C5 1.477(6) . ? N4 C41 1.498(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C5 N5 1.476(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? N5 C51 1.473(8) . ? N5 C5 1.476(5) 8_565 ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? B1 F2 1.351(6) . ? B1 F2 1.351(6) 8_575 ? B1 F1 1.356(9) . ? B1 F3 1.383(11) . ? C6 Cl4 1.747(7) . ? C6 Cl4 1.747(7) 8_565 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 Cl5 1.742(12) . ? C7 Cl6 1.757(19) . ? C7 H7A 0.9900 . ? C7 H7B 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 N1 Cu1 Cl3 104.43(11) . . ? N1 Cu1 Cl1 102.36(11) . . ? Cl3 Cu1 Cl1 122.71(5) . . ? N1 Cu1 Cu3 144.61(11) . . ? Cl3 Cu1 Cu3 58.93(3) . . ? Cl1 Cu1 Cu3 112.89(3) . . ? N1 Cu1 Cu1 148.13(10) . 8_565 ? Cl3 Cu1 Cu1 107.41(3) . 8_565 ? Cl1 Cu1 Cu1 58.49(2) . 8_565 ? Cu3 Cu1 Cu1 59.274(15) . 8_565 ? N1 Cu1 Cu4 91.21(10) . . ? Cl3 Cu1 Cu4 148.09(4) . . ? Cl1 Cu1 Cu4 79.22(4) . . ? Cu3 Cu1 Cu4 92.38(3) . . ? Cu1 Cu1 Cu4 61.818(14) 8_565 . ? N1 Cu1 Cu2 89.47(11) . . ? Cl3 Cu1 Cu2 92.19(3) . . ? Cl1 Cu1 Cu2 137.66(4) . . ? Cu3 Cu1 Cu2 62.57(2) . . ? Cu1 Cu1 Cu2 90.646(15) 8_565 . ? Cu4 Cu1 Cu2 59.80(2) . . ? N1 Cu1 H 124(3) . . ? Cl3 Cu1 H 105(3) . . ? Cl1 Cu1 H 100(2) . . ? Cu3 Cu1 H 48(3) . . ? Cu1 Cu1 H 47(2) 8_565 . ? Cu4 Cu1 H 45(3) . . ? Cu2 Cu1 H 44(2) . . ? N2 Cu2 N4 121.81(15) . . ? N2 Cu2 Cl2 97.84(12) . . ? N4 Cu2 Cl2 98.16(11) . . ? N2 Cu2 Cu2 146.16(12) . 8_565 ? N4 Cu2 Cu2 88.00(10) . 8_565 ? Cl2 Cu2 Cu2 59.17(2) . 8_565 ? N2 Cu2 Cu4 86.73(11) . . ? N4 Cu2 Cu4 148.78(10) . . ? Cl2 Cu2 Cu4 62.68(4) . . ? Cu2 Cu2 Cu4 61.256(14) 8_565 . ? N2 Cu2 Cu3 132.25(11) . . ? N4 Cu2 Cu3 82.24(10) . . ? Cl2 Cu2 Cu3 120.54(3) . . ? Cu2 Cu2 Cu3 61.434(14) 8_565 . ? Cu4 Cu2 Cu3 87.06(3) . . ? N2 Cu2 Cu1 82.55(11) . . ? N4 Cu2 Cu1 130.88(10) . . ? Cl2 Cu2 Cu1 121.79(4) . . ? Cu2 Cu2 Cu1 89.354(15) 8_565 . ? Cu4 Cu2 Cu1 59.22(2) . . ? Cu3 Cu2 Cu1 54.19(2) . . ? N2 Cu2 H 117(2) . . ? N4 Cu2 H 118(3) . . ? Cl2 Cu2 H 91(3) . . ? Cu2 Cu2 H 47(2) 8_565 . ? Cu4 Cu2 H 44(3) . . ? Cu3 Cu2 H 43(3) . . ? Cu1 Cu2 H 43(2) . . ? N5 Cu3 Cl3 104.96(8) . 8_565 ? N5 Cu3 Cl3 104.96(8) . . ? Cl3 Cu3 Cl3 111.59(6) 8_565 . ? N5 Cu3 Cu1 145.87(6) . . ? Cl3 Cu3 Cu1 108.95(4) 8_565 . ? Cl3 Cu3 Cu1 58.64(3) . . ? N5 Cu3 Cu1 145.87(6) . 8_565 ? Cl3 Cu3 Cu1 58.64(3) 8_565 8_565 ? Cl3 Cu3 Cu1 108.95(4) . 8_565 ? Cu1 Cu3 Cu1 61.45(3) . 8_565 ? N5 Cu3 Cu2 90.15(13) . . ? Cl3 Cu3 Cu2 146.45(4) 8_565 . ? Cl3 Cu3 Cu2 92.43(3) . . ? Cu1 Cu3 Cu2 63.24(2) . . ? Cu1 Cu3 Cu2 92.20(3) 8_565 . ? N5 Cu3 Cu2 90.15(13) . 8_565 ? Cl3 Cu3 Cu2 92.43(3) 8_565 8_565 ? Cl3 Cu3 Cu2 146.45(4) . 8_565 ? Cu1 Cu3 Cu2 92.20(3) . 8_565 ? Cu1 Cu3 Cu2 63.24(2) 8_565 8_565 ? Cu2 Cu3 Cu2 57.13(3) . 8_565 ? N5 Cu3 H 125(3) . . ? Cl3 Cu3 H 105.1(15) 8_565 . ? Cl3 Cu3 H 105.1(15) . . ? Cu1 Cu3 H 48(2) . . ? Cu1 Cu3 H 48(2) 8_565 . ? Cu2 Cu3 H 44(2) . . ? Cu2 Cu3 H 44(2) 8_565 . ? N3 Cu4 N3 125.0(2) . 8_565 ? N3 Cu4 Cu1 134.68(10) . 8_565 ? N3 Cu4 Cu1 82.25(10) 8_565 8_565 ? N3 Cu4 Cu1 82.25(10) . . ? N3 Cu4 Cu1 134.68(10) 8_565 . ? Cu1 Cu4 Cu1 56.36(3) 8_565 . ? N3 Cu4 Cu2 142.55(11) . 8_565 ? N3 Cu4 Cu2 86.59(11) 8_565 8_565 ? Cu1 Cu4 Cu2 60.98(2) 8_565 8_565 ? Cu1 Cu4 Cu2 88.23(3) . 8_565 ? N3 Cu4 Cu2 86.59(11) . . ? N3 Cu4 Cu2 142.55(11) 8_565 . ? Cu1 Cu4 Cu2 88.23(3) 8_565 . ? Cu1 Cu4 Cu2 60.98(2) . . ? Cu2 Cu4 Cu2 57.49(3) 8_565 . ? N3 Cu4 Cl2 96.95(11) . . ? N3 Cu4 Cl2 96.95(11) 8_565 . ? Cu1 Cu4 Cl2 116.55(4) 8_565 . ? Cu1 Cu4 Cl2 116.55(4) . . ? Cu2 Cu4 Cl2 55.67(3) 8_565 . ? Cu2 Cu4 Cl2 55.67(3) . . ? N3 Cu4 H 117.0(3) . . ? N3 Cu4 H 117.0(3) 8_565 . ? Cu1 Cu4 H 44(2) 8_565 . ? Cu1 Cu4 H 44(2) . . ? Cu2 Cu4 H 44(2) 8_565 . ? Cu2 Cu4 H 44(2) . . ? Cl2 Cu4 H 85(3) . . ? Cu1 Cl1 Cu1 63.02(5) . 8_565 ? Cu2 Cl2 Cu2 61.66(4) 8_565 . ? Cu2 Cl2 Cu4 61.65(4) 8_565 . ? Cu2 Cl2 Cu4 61.65(4) . . ? Cu1 Cl3 Cu3 62.42(3) . . ? N1 C1 N3 109.6(4) . . ? N1 C1 H1A 109.8 . . ? N3 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? N3 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? C2 N1 C1 109.7(4) . . ? C2 N1 C11 109.3(4) . . ? C1 N1 C11 108.5(4) . . ? C2 N1 Cu1 110.6(3) . . ? C1 N1 Cu1 109.4(3) . . ? C11 N1 Cu1 109.2(3) . . ? 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 . . ? N1 C2 N2 110.3(4) . . ? N1 C2 H2A 109.6 . . ? N2 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? N2 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C3 N2 C2 107.9(4) . . ? C3 N2 C21 107.2(4) . . ? C2 N2 C21 107.0(4) . . ? C3 N2 Cu2 111.1(3) . . ? C2 N2 Cu2 113.7(3) . . ? C21 N2 Cu2 109.7(3) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C3 N2 111.0(4) . . ? N3 C3 H3A 109.4 . . ? N2 C3 H3A 109.4 . . ? N3 C3 H3B 109.4 . . ? N2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 N3 C1 107.0(4) . . ? C3 N3 C31 107.9(4) . . ? C1 N3 C31 105.7(4) . . ? C3 N3 Cu4 110.4(3) . . ? C1 N3 Cu4 115.1(3) . . ? C31 N3 Cu4 110.4(3) . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C4 N4 110.1(5) 8_565 . ? N4 C4 H4A 109.6 8_565 . ? N4 C4 H4A 109.6 . . ? N4 C4 H4B 109.6 8_565 . ? N4 C4 H4B 109.6 . . ? H4A C4 H4B 108.2 . . ? C5 N4 C4 108.8(4) . . ? C5 N4 C41 106.8(3) . . ? C4 N4 C41 106.2(3) . . ? C5 N4 Cu2 114.5(3) . . ? C4 N4 Cu2 109.0(3) . . ? C41 N4 Cu2 111.2(3) . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C5 N4 109.2(4) . . ? N5 C5 H5A 109.8 . . ? N4 C5 H5A 109.8 . . ? N5 C5 H5B 109.8 . . ? N4 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C51 N5 C5 108.8(3) . . ? C51 N5 C5 108.8(3) . 8_565 ? C5 N5 C5 110.0(5) . 8_565 ? C51 N5 Cu3 107.5(4) . . ? C5 N5 Cu3 110.8(3) . . ? C5 N5 Cu3 110.8(3) 8_565 . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? F2 B1 F2 110.9(8) . 8_575 ? F2 B1 F1 111.8(5) . . ? F2 B1 F1 111.8(5) 8_575 . ? F2 B1 F3 106.6(5) . . ? F2 B1 F3 106.6(5) 8_575 . ? F1 B1 F3 108.8(7) . . ? Cl4 C6 Cl4 111.7(6) . 8_565 ? Cl4 C6 H6A 109.3 . . ? Cl4 C6 H6A 109.3 8_565 . ? Cl4 C6 H6B 109.3 . . ? Cl4 C6 H6B 109.3 8_565 . ? H6A C6 H6B 107.9 . . ? Cl5 C7 Cl6 104.8(8) . . ? Cl5 C7 H7A 110.8 . . ? Cl6 C7 H7A 110.8 . . ? Cl5 C7 H7B 110.8 . . ? Cl6 C7 H7B 110.8 . . ? H7A C7 H7B 108.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.950 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.143 #============================================================================== #_eof # End of Crystallographic Information File