Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _audit_creation_method 'RAELSPUB and manual entry' _journal_coden_Cambridge 222 loop_ _publ_author_name 'Stephen Colbran' 'Paul V. Bernhardt' 'Donald C. Craig' 'David G. Lonnon' _publ_contact_author_name 'Dr Stephen Colbran' _publ_contact_author_address ; School of Chemical Sciences University of New South Wales Sydney NSW 2052 AUSTRALIA ; _publ_contact_author_email S.COLBRAN@UNSW.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Novel one-dimensional structures and solution behaviour of copper(II) bromide and chloride complexes of a new pentapyridyldiamine ligand ; _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' data_[Cu2(L)Br3]2[Cu2Br4] _database_code_depnum_ccdc_archive 'CCDC 225104' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety '2(C31 H31 Br3 Cu2 N7 1+),Cu2 Br4 2-' _chemical_formula_sum 'C62 H62 Br10 Cu6 N14' _chemical_formula_iupac ? _chemical_formula_weight 2183.6 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.084(3) _cell_length_b 10.628(4) _cell_length_c 19.583(7) _cell_angle_alpha 100.24(2) _cell_angle_beta 95.57(3) _cell_angle_gamma 105.44(2) _cell_volume 1772(1) _cell_formula_units_Z 1 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 18 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.05 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056.0 _exptl_absorpt_coefficient_mu 7.405 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.52 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6648 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 6214 _reflns_number_gt 3445 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.058 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3445 _refine_ls_number_parameters 415 _refine_ls_goodness_of_fit_ref 1.69 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 1.41 _refine_diff_density_min -1.67 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Cu1 0.34850(13) 0.04795(14) 0.18759(6) 0.0368(3) Uani Cu 1.0 Cu2 0.40517(14) 0.52865(14) 0.19135(6) 0.0411(4) Uani Cu 1.0 Br1 0.15102(12) 0.04091(13) 0.09724(6) 0.0493(3) Uani Br 1.0 Br2 0.66304(14) 0.51615(15) 0.18327(7) 0.0631(4) Uani Br 1.0 Br3 0.38171(15) 0.76850(12) 0.14759(6) 0.0564(4) Uani Br 1.0 N1 0.5262(9) 0.1012(8) 0.1380(4) 0.031(2) Uani N 1.0 N2 0.2150(9) -0.0150(8) 0.2566(5) 0.037(2) Uani N 1.0 N3 0.5249(9) 0.0962(8) 0.2716(4) 0.033(2) Uani N 1.0 N4 0.3478(10) 0.2998(8) 0.2716(4) 0.035(2) Uani N 1.0 N5 0.3086(10) 0.4322(8) 0.0943(4) 0.041(2) Uani N 1.0 N6 0.4425(10) 0.6235(9) 0.2916(4) 0.042(2) Uani N 1.0 N7 0.1755(9) 0.4850(8) 0.2083(4) 0.039(2) Uani N 1.0 C1 0.6518(11) 0.0537(11) 0.2409(5) 0.042(3) Uani C 1.0 C2 0.6612(11) 0.0903(10) 0.1709(5) 0.038(3) Uani C 1.0 C3 0.7890(11) 0.1019(11) 0.1388(6) 0.044(3) Uani C 1.0 C4 0.7860(13) 0.1276(12) 0.0728(6) 0.047(3) Uani C 1.0 C5 0.6545(13) 0.1470(12) 0.0396(6) 0.050(3) Uani C 1.0 C6 0.5273(12) 0.1318(11) 0.0743(6) 0.040(3) Uani C 1.0 C7 0.4652(12) 0.0201(11) 0.3240(5) 0.041(3) Uani C 1.0 C8 0.2919(12) -0.0047(10) 0.3204(5) 0.038(3) Uani C 1.0 C9 0.2170(14) -0.0288(12) 0.3764(6) 0.054(3) Uani C 1.0 C10 0.0636(17) -0.0655(15) 0.3687(8) 0.075(4) Uani C 1.0 C11 -0.0218(14) -0.0833(14) 0.3028(8) 0.072(4) Uani C 1.0 C12 0.0582(13) -0.0525(12) 0.2480(7) 0.056(3) Uani C 1.0 C13 0.5782(12) 0.2418(11) 0.3005(5) 0.041(3) Uani C 1.0 C14 0.4498(13) 0.2950(10) 0.3236(6) 0.041(3) Uani C 1.0 C15 0.4326(16) 0.3264(12) 0.3932(6) 0.056(3) Uani C 1.0 C16 0.3053(18) 0.3618(14) 0.4105(7) 0.070(4) Uani C 1.0 C17 0.1954(15) 0.3632(13) 0.3573(7) 0.057(3) Uani C 1.0 C18 0.2239(12) 0.3374(10) 0.2883(6) 0.039(3) Uani C 1.0 C19 0.1195(12) 0.3523(11) 0.2274(6) 0.046(3) Uani C 1.0 C20 0.0895(13) 0.4834(12) 0.1406(6) 0.055(3) Uani C 1.0 C21 0.1539(14) 0.4212(11) 0.0802(6) 0.047(3) Uani C 1.0 C22 0.0712(14) 0.3621(12) 0.0145(6) 0.056(3) Uani C 1.0 C23 0.1439(20) 0.3158(14) -0.0392(6) 0.070(4) Uani C 1.0 C24 0.2967(18) 0.3258(13) -0.0254(6) 0.066(4) Uani C 1.0 C25 0.3755(13) 0.3854(12) 0.0421(6) 0.050(3) Uani C 1.0 C26 0.1709(12) 0.5974(11) 0.2646(6) 0.045(3) Uani C 1.0 C27 0.3156(13) 0.6422(10) 0.3168(5) 0.041(3) Uani C 1.0 C28 0.3205(14) 0.7067(11) 0.3843(6) 0.050(3) Uani C 1.0 C29 0.4611(17) 0.7574(12) 0.4285(6) 0.057(3) Uani C 1.0 C30 0.5910(16) 0.7366(13) 0.4035(7) 0.064(4) Uani C 1.0 C31 0.5782(14) 0.6677(12) 0.3359(6) 0.052(3) Uani C 1.0 Cu3 0.92578(18) 0.36336(17) 0.47881(8) 0.0689(5) Uani Cu 1.0 Br4 0.88053(14) 0.53090(14) 0.41667(7) 0.0613(4) Uani Br 1.0 Br5 0.81880(16) 0.13517(14) 0.44908(7) 0.0659(4) Uani Br 1.0 H1C1 0.6304 -0.0451 0.2352 0.042 Uani H 1.0 H2C1 0.7519 0.0998 0.2728 0.042 Uani H 1.0 HC3 0.8854 0.0917 0.1636 0.044 Uani H 1.0 HC4 0.8786 0.1323 0.0485 0.047 Uani H 1.0 HC5 0.6516 0.1710 -0.0075 0.050 Uani H 1.0 HC6 0.4310 0.1443 0.0507 0.040 Uani H 1.0 H1C7 0.5173 0.0719 0.3720 0.041 Uani H 1.0 H2C7 0.4884 -0.0677 0.3148 0.041 Uani H 1.0 HC9 0.2783 -0.0186 0.4234 0.054 Uani H 1.0 HC10 0.0096 -0.0804 0.4099 0.075 Uani H 1.0 HC11 -0.1372 -0.1171 0.2951 0.072 Uani H 1.0 HC12 -0.0010 -0.0582 0.2012 0.056 Uani H 1.0 H1C13 0.6315 0.2735 0.2618 0.041 Uani H 1.0 H2C13 0.6549 0.2273 0.3363 0.041 Uani H 1.0 HC15 0.5133 0.3231 0.4309 0.056 Uani H 1.0 HC16 0.2920 0.3863 0.4608 0.070 Uani H 1.0 HC17 0.0971 0.3823 0.3679 0.057 Uani H 1.0 H1C19 0.1145 0.2806 0.1858 0.046 Uani H 1.0 H2C19 0.0138 0.3421 0.2404 0.046 Uani H 1.0 H1C20 0.0952 0.5773 0.1371 0.055 Uani H 1.0 H2C20 -0.0209 0.4311 0.1380 0.055 Uani H 1.0 HC22 -0.0420 0.3525 0.0056 0.056 Uani H 1.0 HC23 0.0851 0.2757 -0.0876 0.070 Uani H 1.0 HC24 0.3514 0.2908 -0.0630 0.066 Uani H 1.0 HC25 0.4881 0.3934 0.0518 0.050 Uani H 1.0 H1C26 0.0802 0.5672 0.2890 0.045 Uani H 1.0 H2C26 0.1602 0.6738 0.2432 0.045 Uani H 1.0 HC28 0.2236 0.7173 0.4016 0.050 Uani H 1.0 HC29 0.4679 0.8079 0.4775 0.057 Uani H 1.0 HC30 0.6938 0.7715 0.4343 0.064 Uani H 1.0 HC31 0.6722 0.6494 0.3189 0.052 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Cu1 0.0248(7) 0.0516(9) 0.0370(7) 0.0135(6) 0.0041(5) 0.0140(6) Cu Cu2 0.0380(8) 0.0449(9) 0.0423(8) 0.0151(7) 0.0079(6) 0.0088(7) Cu Br1 0.0319(6) 0.0746(9) 0.0428(6) 0.0234(6) -0.0005(5) 0.0072(6) Br Br2 0.0450(7) 0.090(1) 0.0629(8) 0.0270(7) 0.0171(6) 0.0234(8) Br Br3 0.0807(9) 0.0379(8) 0.0537(8) 0.0166(7) 0.0153(6) 0.0153(6) Br N1 0.028(5) 0.033(5) 0.035(5) 0.012(4) -0.001(4) 0.010(4) N N2 0.030(5) 0.028(5) 0.056(6) 0.010(4) 0.010(4) 0.013(4) N N3 0.031(5) 0.038(6) 0.040(5) 0.021(4) 0.007(4) 0.015(4) N N4 0.045(5) 0.023(5) 0.037(5) 0.008(4) 0.011(4) 0.004(4) N N5 0.045(6) 0.039(6) 0.039(5) 0.018(5) 0.001(4) 0.007(4) N N6 0.048(6) 0.046(6) 0.038(5) 0.019(5) 0.009(5) 0.016(5) N N7 0.039(5) 0.033(6) 0.045(5) 0.018(4) 0.004(4) 0.004(4) N C1 0.035(6) 0.051(8) 0.050(7) 0.026(6) 0.006(5) 0.013(6) C C2 0.031(6) 0.032(7) 0.044(6) 0.007(5) 0.006(5) -0.006(5) C C3 0.030(6) 0.044(7) 0.057(7) 0.013(6) 0.009(5) 0.005(6) C C4 0.042(7) 0.052(8) 0.049(7) 0.012(6) 0.019(6) 0.009(6) C C5 0.044(7) 0.050(8) 0.045(7) 0.002(6) 0.006(6) 0.000(6) C C6 0.037(7) 0.034(7) 0.046(7) 0.009(5) -0.003(5) 0.006(5) C C7 0.043(7) 0.048(8) 0.034(6) 0.018(6) 0.000(5) 0.013(6) C C8 0.055(7) 0.031(7) 0.039(6) 0.023(6) 0.015(6) 0.018(5) C C9 0.060(9) 0.053(8) 0.063(8) 0.030(7) 0.024(7) 0.023(7) C C10 0.083(9) 0.095(9) 0.086(9) 0.053(9) 0.049(9) 0.057(9) C C11 0.040(8) 0.076(9) 0.119(9) 0.019(7) 0.035(9) 0.052(9) C C12 0.042(8) 0.060(9) 0.083(9) 0.026(7) 0.021(7) 0.034(8) C C13 0.047(7) 0.038(7) 0.044(7) 0.020(6) 0.005(5) 0.012(6) C C14 0.052(7) 0.029(7) 0.043(7) 0.009(6) 0.008(6) 0.013(5) C C15 0.095(9) 0.051(8) 0.038(7) 0.040(8) 0.022(7) 0.017(6) C C16 0.110(9) 0.071(9) 0.052(8) 0.044(9) 0.041(9) 0.028(8) C C17 0.071(9) 0.060(9) 0.062(8) 0.037(7) 0.036(7) 0.026(7) C C18 0.045(7) 0.022(6) 0.055(7) 0.010(5) 0.020(6) 0.014(5) C C19 0.035(6) 0.033(7) 0.074(8) 0.008(6) 0.018(6) 0.019(6) C C20 0.057(8) 0.058(9) 0.063(8) 0.035(7) 0.000(6) 0.021(7) C C21 0.067(9) 0.040(7) 0.043(7) 0.019(6) 0.010(6) 0.025(6) C C22 0.068(9) 0.052(8) 0.043(7) 0.010(7) -0.011(7) 0.023(6) C C23 0.115(9) 0.057(9) 0.036(8) 0.022(9) 0.000(8) 0.013(7) C C24 0.108(9) 0.050(9) 0.042(8) 0.026(9) 0.015(8) 0.007(7) C C25 0.061(8) 0.048(8) 0.046(7) 0.020(7) 0.017(6) 0.010(6) C C26 0.039(7) 0.040(7) 0.059(7) 0.020(6) 0.008(6) 0.009(6) C C27 0.067(8) 0.032(7) 0.036(6) 0.027(6) 0.019(6) 0.014(5) C C28 0.069(9) 0.035(7) 0.054(8) 0.021(7) 0.018(7) 0.018(6) C C29 0.089(9) 0.046(8) 0.038(7) 0.031(8) 0.007(7) 0.001(6) C C30 0.085(9) 0.055(9) 0.052(8) 0.027(8) -0.015(7) 0.013(7) C C31 0.066(9) 0.046(8) 0.045(7) 0.017(7) 0.003(6) 0.013(6) C Cu3 0.059(1) 0.075(1) 0.073(1) 0.0207(9) 0.0177(9) 0.009(1) Cu Br4 0.0513(8) 0.070(1) 0.0607(8) 0.0225(7) -0.0052(6) 0.0101(7) Br Br5 0.075(1) 0.070(1) 0.0530(8) 0.0274(8) -0.0020(7) 0.0108(7) Br # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Br1 2.371(2) 1_555 1_555 no Cu1 Br3 3.037(2) 1_555 1_545 no Cu1 N1 1.971(8) 1_555 1_555 no Cu1 N2 1.989(8) 1_555 1_555 no Cu1 N3 2.070(8) 1_555 1_555 no Cu1 N4 2.883(8) 1_555 1_555 no Cu2 Br2 2.400(2) 1_555 1_555 no Cu2 Br3 2.882(2) 1_555 1_555 no Cu2 N4 3.082(8) 1_555 1_555 no Cu2 N5 1.985(8) 1_555 1_555 no Cu2 N6 1.992(8) 1_555 1_555 no Cu2 N7 2.086(8) 1_555 1_555 no Br3 Cu1 3.037(2) 1_555 1_565 no N1 C2 1.372(12) 1_555 1_555 no N1 C6 1.344(12) 1_555 1_555 no N2 C8 1.342(12) 1_555 1_555 no N2 C12 1.357(13) 1_555 1_555 no N3 C1 1.486(12) 1_555 1_555 no N3 C7 1.474(12) 1_555 1_555 no N3 C13 1.478(13) 1_555 1_555 no N4 C14 1.327(13) 1_555 1_555 no N4 C18 1.341(12) 1_555 1_555 no N5 C21 1.375(13) 1_555 1_555 no N5 C25 1.327(13) 1_555 1_555 no N6 C27 1.345(12) 1_555 1_555 no N6 C31 1.354(14) 1_555 1_555 no N7 C19 1.494(13) 1_555 1_555 no N7 C20 1.467(13) 1_555 1_555 no N7 C26 1.488(13) 1_555 1_555 no C1 C2 1.495(14) 1_555 1_555 no C2 C3 1.360(13) 1_555 1_555 no C3 C4 1.367(14) 1_555 1_555 no C4 C5 1.386(15) 1_555 1_555 no C5 C6 1.384(14) 1_555 1_555 no C7 C8 1.518(14) 1_555 1_555 no C8 C9 1.373(14) 1_555 1_555 no C9 C10 1.329(17) 1_555 1_555 no C10 C11 1.394(18) 1_555 1_555 no C11 C12 1.392(16) 1_555 1_555 no C13 C14 1.499(14) 1_555 1_555 no C14 C15 1.378(14) 1_555 1_555 no C15 C16 1.362(17) 1_555 1_555 no C16 C17 1.376(17) 1_555 1_555 no C17 C18 1.393(14) 1_555 1_555 no C18 C19 1.509(15) 1_555 1_555 no C20 C21 1.497(15) 1_555 1_555 no C21 C22 1.373(15) 1_555 1_555 no C22 C23 1.383(17) 1_555 1_555 no C23 C24 1.359(18) 1_555 1_555 no C24 C25 1.392(16) 1_555 1_555 no C26 C27 1.494(14) 1_555 1_555 no C27 C28 1.367(14) 1_555 1_555 no C28 C29 1.387(16) 1_555 1_555 no C29 C30 1.376(17) 1_555 1_555 no C30 C31 1.371(16) 1_555 1_555 no Cu3 Br4 2.426(2) 1_555 1_555 no Cu3 Br4 2.445(2) 1_555 2_766 no Cu3 Br5 2.302(2) 1_555 1_555 no Br4 Cu3 2.445(2) 1_555 2_766 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Cu1 Br3 101.01(6) 1_555 1_555 1_545 no Br1 Cu1 N1 97.9(2) 1_555 1_555 1_555 no Br1 Cu1 N2 98.3(3) 1_555 1_555 1_555 no Br1 Cu1 N3 168.0(2) 1_555 1_555 1_555 no Br1 Cu1 N4 95.6(2) 1_555 1_555 1_555 no Br3 Cu1 N1 85.1(2) 1_545 1_555 1_555 no Br3 Cu1 N2 88.6(2) 1_545 1_555 1_555 no Br3 Cu1 N3 90.8(2) 1_545 1_555 1_555 no Br3 Cu1 N4 160.8(2) 1_545 1_555 1_555 no N1 Cu1 N2 163.5(3) 1_555 1_555 1_555 no N1 Cu1 N3 81.1(3) 1_555 1_555 1_555 no N1 Cu1 N4 102.2(3) 1_555 1_555 1_555 no N2 Cu1 N3 83.8(3) 1_555 1_555 1_555 no N2 Cu1 N4 79.4(3) 1_555 1_555 1_555 no N3 Cu1 N4 73.1(3) 1_555 1_555 1_555 no Br2 Cu2 Br3 107.29(6) 1_555 1_555 1_555 no Br2 Cu2 N4 90.3(2) 1_555 1_555 1_555 no Br2 Cu2 N5 98.0(3) 1_555 1_555 1_555 no Br2 Cu2 N6 97.6(3) 1_555 1_555 1_555 no Br2 Cu2 N7 162.5(2) 1_555 1_555 1_555 no Br3 Cu2 N4 159.4(2) 1_555 1_555 1_555 no Br3 Cu2 N5 86.7(3) 1_555 1_555 1_555 no Br3 Cu2 N6 90.2(3) 1_555 1_555 1_555 no Br3 Cu2 N7 90.2(2) 1_555 1_555 1_555 no N4 Cu2 N5 101.7(3) 1_555 1_555 1_555 no N4 Cu2 N6 76.6(3) 1_555 1_555 1_555 no N4 Cu2 N7 72.5(3) 1_555 1_555 1_555 no N5 Cu2 N6 164.3(4) 1_555 1_555 1_555 no N5 Cu2 N7 82.4(3) 1_555 1_555 1_555 no N6 Cu2 N7 82.2(3) 1_555 1_555 1_555 no Cu1 Br3 Cu2 148.03(5) 1_565 1_555 1_555 no Cu1 N1 C2 113.6(6) 1_555 1_555 1_555 no Cu1 N1 C6 128.5(7) 1_555 1_555 1_555 no C2 N1 C6 117.4(8) 1_555 1_555 1_555 no Cu1 N2 C8 114.5(7) 1_555 1_555 1_555 no Cu1 N2 C12 127.0(8) 1_555 1_555 1_555 no C8 N2 C12 118.1(9) 1_555 1_555 1_555 no Cu1 N3 C1 104.3(6) 1_555 1_555 1_555 no Cu1 N3 C7 107.1(6) 1_555 1_555 1_555 no Cu1 N3 C13 111.2(6) 1_555 1_555 1_555 no C1 N3 C7 112.6(8) 1_555 1_555 1_555 no C1 N3 C13 109.2(8) 1_555 1_555 1_555 no C7 N3 C13 112.2(8) 1_555 1_555 1_555 no Cu1 N4 Cu2 113.3(3) 1_555 1_555 1_555 no Cu1 N4 C14 93.8(6) 1_555 1_555 1_555 no Cu1 N4 C18 127.0(7) 1_555 1_555 1_555 no Cu2 N4 C14 122.6(6) 1_555 1_555 1_555 no Cu2 N4 C18 85.5(6) 1_555 1_555 1_555 no C14 N4 C18 117.8(9) 1_555 1_555 1_555 no Cu2 N5 C21 113.7(7) 1_555 1_555 1_555 no Cu2 N5 C25 128.5(8) 1_555 1_555 1_555 no C21 N5 C25 117.7(9) 1_555 1_555 1_555 no Cu2 N6 C27 114.6(7) 1_555 1_555 1_555 no Cu2 N6 C31 127.4(8) 1_555 1_555 1_555 no C27 N6 C31 117.9(9) 1_555 1_555 1_555 no Cu2 N7 C19 112.7(6) 1_555 1_555 1_555 no Cu2 N7 C20 104.0(6) 1_555 1_555 1_555 no Cu2 N7 C26 105.0(6) 1_555 1_555 1_555 no C19 N7 C20 109.7(9) 1_555 1_555 1_555 no C19 N7 C26 112.5(8) 1_555 1_555 1_555 no C20 N7 C26 112.6(8) 1_555 1_555 1_555 no N3 C1 C2 109.1(8) 1_555 1_555 1_555 no N1 C2 C1 114.9(8) 1_555 1_555 1_555 no N1 C2 C3 121.5(10) 1_555 1_555 1_555 no C1 C2 C3 123.4(10) 1_555 1_555 1_555 no C2 C3 C4 120.1(10) 1_555 1_555 1_555 no C3 C4 C5 119.9(10) 1_555 1_555 1_555 no C4 C5 C6 117.3(11) 1_555 1_555 1_555 no N1 C6 C5 123.5(10) 1_555 1_555 1_555 no N3 C7 C8 111.2(8) 1_555 1_555 1_555 no N2 C8 C7 115.2(8) 1_555 1_555 1_555 no N2 C8 C9 122.1(10) 1_555 1_555 1_555 no C7 C8 C9 122.4(10) 1_555 1_555 1_555 no C8 C9 C10 120.4(12) 1_555 1_555 1_555 no C9 C10 C11 119.8(12) 1_555 1_555 1_555 no C10 C11 C12 118.1(11) 1_555 1_555 1_555 no N2 C12 C11 121.4(11) 1_555 1_555 1_555 no N3 C13 C14 112.1(8) 1_555 1_555 1_555 no N4 C14 C13 114.6(9) 1_555 1_555 1_555 no N4 C14 C15 122.7(10) 1_555 1_555 1_555 no C13 C14 C15 122.6(10) 1_555 1_555 1_555 no C14 C15 C16 119.8(12) 1_555 1_555 1_555 no C15 C16 C17 118.6(11) 1_555 1_555 1_555 no C16 C17 C18 118.7(11) 1_555 1_555 1_555 no N4 C18 C17 122.3(10) 1_555 1_555 1_555 no N4 C18 C19 115.2(9) 1_555 1_555 1_555 no C17 C18 C19 122.5(10) 1_555 1_555 1_555 no N7 C19 C18 112.3(8) 1_555 1_555 1_555 no N7 C20 C21 111.8(9) 1_555 1_555 1_555 no N5 C21 C20 114.4(10) 1_555 1_555 1_555 no N5 C21 C22 121.1(11) 1_555 1_555 1_555 no C20 C21 C22 124.5(12) 1_555 1_555 1_555 no C21 C22 C23 120.1(12) 1_555 1_555 1_555 no C22 C23 C24 118.9(12) 1_555 1_555 1_555 no C23 C24 C25 118.9(12) 1_555 1_555 1_555 no N5 C25 C24 123.2(11) 1_555 1_555 1_555 no N7 C26 C27 110.6(8) 1_555 1_555 1_555 no N6 C27 C26 115.5(9) 1_555 1_555 1_555 no N6 C27 C28 122.4(11) 1_555 1_555 1_555 no C26 C27 C28 122.0(10) 1_555 1_555 1_555 no C27 C28 C29 119.4(11) 1_555 1_555 1_555 no C28 C29 C30 118.5(11) 1_555 1_555 1_555 no C29 C30 C31 119.4(12) 1_555 1_555 1_555 no N6 C31 C30 122.2(11) 1_555 1_555 1_555 no Br4 Cu3 Br4 110.11(7) 1_555 1_555 2_766 no Br4 Cu3 Br5 128.73(8) 1_555 1_555 1_555 no Br4 Cu3 Br5 121.13(9) 2_766 1_555 1_555 no Cu3 Br4 Cu3 69.89(7) 1_555 1_555 2_766 no #===END data_[Cu2(L)Br2](ClO4).CH3CN _database_code_depnum_ccdc_archive 'CCDC 225105' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C31 H31 Br2 Cu2 N7 2+,2(Cl O4 1-),C2 H3 N' _chemical_formula_sum 'C33 H34 Br2 Cl2 Cu2 N8 O8' _chemical_formula_iupac ? _chemical_formula_weight 1028.5 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 11.643(5) _cell_length_b 22.669(5) _cell_length_c 15.249(6) _cell_angle_alpha 90 _cell_angle_beta 102.53(2) _cell_angle_gamma 90 _cell_volume 3929(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.74 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056.0 _exptl_absorpt_coefficient_mu 3.294 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.65 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6403 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 24 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 4 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 6149 _reflns_number_gt 3389 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.050 _refine_ls_wR_factor_ref 0.070 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3389 _refine_ls_number_parameters 458 _refine_ls_goodness_of_fit_ref 1.65 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.85 _refine_diff_density_min -0.84 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Cu1 0.16745(9) 0.21334(5) 0.85848(8) 0.0422(8) Uani Cu 1.0 Cu2 0.27704(9) 0.20991(5) 0.57251(8) 0.0394(7) Uani Cu 1.0 Br1 0.35979(9) 0.25432(5) 0.90444(8) 0.0576(4) Uani Br 1.0 Br2 0.09159(9) 0.25880(5) 0.53132(7) 0.0512(4) Uani Br 1.0 N1 0.0873(8) 0.2849(4) 0.7966(5) 0.046(2) Uani N 1.0 N2 0.2017(7) 0.1329(4) 0.9144(5) 0.044(2) Uani N 1.0 N3 0.0095(6) 0.1754(3) 0.8041(5) 0.038(2) Uani N 1.0 N4 0.2125(7) 0.1399(3) 0.7140(5) 0.040(2) Uani N 1.0 N5 0.3699(7) 0.2763(4) 0.6365(5) 0.044(2) Uani N 1.0 N6 0.2271(8) 0.1319(3) 0.5154(5) 0.043(2) Uani N 1.0 N7 0.4265(6) 0.1633(4) 0.6270(5) 0.045(2) Uani N 1.0 C1 -0.0789(9) 0.2223(5) 0.7948(8) 0.058(3) Uani C 1.0 C2 -0.0299(9) 0.2785(4) 0.7643(7) 0.047(3) Uani C 1.0 C3 -0.0967(12) 0.3224(6) 0.7167(9) 0.080(4) Uani C 1.0 C4 -0.0451(14) 0.3721(6) 0.6997(9) 0.079(4) Uani C 1.0 C5 0.0725(14) 0.3815(5) 0.7323(9) 0.074(4) Uani C 1.0 C6 0.1375(11) 0.3368(5) 0.7803(8) 0.063(3) Uani C 1.0 C7 -0.0096(9) 0.1294(5) 0.8680(7) 0.051(3) Uani C 1.0 C8 0.1041(10) 0.1009(4) 0.9091(6) 0.050(3) Uani C 1.0 C9 0.1088(13) 0.0440(6) 0.9440(9) 0.078(4) Uani C 1.0 C10 0.2147(16) 0.0194(6) 0.9853(9) 0.094(5) Uani C 1.0 C11 0.3157(13) 0.0536(7) 0.9881(8) 0.086(4) Uani C 1.0 C12 0.3059(10) 0.1098(5) 0.9533(7) 0.061(3) Uani C 1.0 C13 0.0082(8) 0.1494(4) 0.7122(6) 0.043(3) Uani C 1.0 C14 0.1097(9) 0.1119(5) 0.7113(6) 0.043(3) Uani C 1.0 C15 0.1043(10) 0.0499(5) 0.7098(7) 0.058(3) Uani C 1.0 C16 0.2017(12) 0.0175(5) 0.7150(9) 0.072(4) Uani C 1.0 C17 0.3068(11) 0.0456(5) 0.7183(8) 0.063(3) Uani C 1.0 C18 0.3091(9) 0.1064(5) 0.7167(6) 0.045(3) Uani C 1.0 C19 0.4189(9) 0.1393(5) 0.7169(7) 0.052(3) Uani C 1.0 C20 0.5239(8) 0.2078(6) 0.6383(8) 0.064(3) Uani C 1.0 C21 0.4836(9) 0.2644(5) 0.6691(7) 0.045(3) Uani C 1.0 C22 0.5587(11) 0.3030(7) 0.7252(9) 0.081(4) Uani C 1.0 C23 0.5162(14) 0.3588(7) 0.7413(9) 0.082(4) Uani C 1.0 C24 0.4020(13) 0.3716(5) 0.7038(8) 0.074(4) Uani C 1.0 C25 0.3300(10) 0.3298(5) 0.6544(7) 0.061(3) Uani C 1.0 C26 0.4353(9) 0.1167(5) 0.5614(8) 0.058(3) Uani C 1.0 C27 0.3169(10) 0.0946(5) 0.5196(7) 0.050(3) Uani C 1.0 C28 0.2936(14) 0.0362(6) 0.4849(8) 0.084(4) Uani C 1.0 C29 0.1819(17) 0.0187(6) 0.4494(9) 0.096(5) Uani C 1.0 C30 0.0896(13) 0.0592(6) 0.4485(8) 0.077(4) Uani C 1.0 C31 0.1169(10) 0.1144(5) 0.4809(7) 0.052(3) Uani C 1.0 Cl1A 0.7036(2) 0.0425(1) 0.7647(2) 0.060(4) Uani Cl 1.0 O1A 0.7232(6) 0.0975(2) 0.7284(6) 0.144(7) Uani O 1.0 O2A 0.8106(4) 0.0121(3) 0.7898(5) 0.110(4) Uani O 1.0 O3A 0.6252(6) 0.0096(3) 0.7002(5) 0.129(6) Uani O 1.0 O4A 0.6553(7) 0.0509(4) 0.8405(4) 0.176(5) Uani O 1.0 Cl1B 0.7636(5) 0.1521(3) 0.4761(4) 0.076(6) Uani Cl 0.68 O1B 0.7532(11) 0.1918(5) 0.5444(8) 0.142(9) Uani O 0.68 O2B 0.7760(13) 0.1835(6) 0.3994(6) 0.131(9) Uani O 0.68 O3B 0.6625(9) 0.1167(6) 0.4551(8) 0.141(9) Uani O 0.68 O4B 0.8627(9) 0.1162(6) 0.5054(8) 0.125(5) Uani O 0.68 Cl1B' 0.7612(14) 0.1462(8) 0.4467(10) 0.085(6) Uani Cl 0.32 O1B' 0.8073(31) 0.1918(15) 0.4025(19) 0.150(9) Uani O 0.32 O2B' 0.6516(18) 0.1634(15) 0.4622(23) 0.148(9) Uani O 0.32 O3B' 0.8386(21) 0.1344(13) 0.5291(13) 0.089(5) Uani O 0.32 O4B' 0.7475(32) 0.0953(12) 0.3932(18) 0.186(9) Uani O 0.32 N1An 0.6857(32) 0.1845(12) -0.0495(22) 0.247(9) Uani N 1.0 C1An 0.6614(26) 0.1491(15) 0.0032(22) 0.177(9) Uani C 1.0 C2An 0.6409(30) 0.1107(15) 0.0563(21) 0.188(9) Uani C 1.0 H1C1 -0.1002 0.2291 0.8541 0.058 Uani H 1.0 H2C1 -0.1507 0.2103 0.7495 0.058 Uani H 1.0 HC3 -0.1835 0.3171 0.6949 0.080 Uani H 1.0 HC4 -0.0931 0.4033 0.6622 0.079 Uani H 1.0 HC5 0.1101 0.4197 0.7217 0.074 Uani H 1.0 HC6 0.2239 0.3426 0.8036 0.063 Uani H 1.0 H1C7 -0.0653 0.0991 0.8355 0.051 Uani H 1.0 H2C7 -0.0438 0.1478 0.9163 0.051 Uani H 1.0 HC9 0.0346 0.0208 0.9390 0.078 Uani H 1.0 HC10 0.2194 -0.0211 1.0121 0.094 Uani H 1.0 HC11 0.3950 0.0371 1.0154 0.086 Uani H 1.0 HC12 0.3786 0.1340 0.9572 0.061 Uani H 1.0 H1C13 0.0007 0.1891 0.6830 0.043 Uani H 1.0 H2C13 -0.0719 0.1320 0.7075 0.043 Uani H 1.0 HC15 0.0267 0.0298 0.7046 0.058 Uani H 1.0 HC16 0.1978 -0.0265 0.7166 0.072 Uani H 1.0 HC17 0.3806 0.0223 0.7217 0.063 Uani H 1.0 H1C19 0.4239 0.1730 0.7598 0.052 Uani H 1.0 H2C19 0.4870 0.1121 0.7378 0.052 Uani H 1.0 H1C20 0.5470 0.2139 0.5795 0.064 Uani H 1.0 H2C20 0.5932 0.1932 0.6838 0.064 Uani H 1.0 HC22 0.6412 0.2911 0.7534 0.081 Uani H 1.0 HC23 0.5682 0.3884 0.7792 0.082 Uani H 1.0 HC24 0.3701 0.4116 0.7122 0.074 Uani H 1.0 HC25 0.2451 0.3394 0.6310 0.061 Uani H 1.0 H1C26 0.4841 0.0834 0.5928 0.058 Uani H 1.0 H2C26 0.4733 0.1331 0.5138 0.058 Uani H 1.0 HC28 0.3602 0.0080 0.4868 0.084 Uani H 1.0 HC29 0.1653 -0.0220 0.4244 0.096 Uani H 1.0 HC30 0.0059 0.0475 0.4244 0.077 Uani H 1.0 HC31 0.0516 0.1433 0.4790 0.052 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Cu1 0.042(1) 0.044(1) 0.040(1) -0.0046(6) 0.0062(6) 0.0012(6) Cu Cu2 0.0376(9) 0.043(1) 0.037(1) 0.0030(5) 0.0051(5) -0.0005(6) Cu Br1 0.0456(6) 0.0762(9) 0.0524(7) -0.0127(6) 0.0135(5) -0.0128(6) Br Br2 0.0451(6) 0.0596(7) 0.0493(7) 0.0060(5) 0.0110(5) 0.0084(6) Br N1 0.061(6) 0.044(5) 0.037(5) 0.005(4) 0.017(4) 0.005(4) N N2 0.057(6) 0.044(5) 0.029(5) 0.006(5) 0.007(4) 0.001(4) N N3 0.041(5) 0.042(5) 0.032(5) -0.001(4) 0.009(4) 0.003(4) N N4 0.041(5) 0.052(5) 0.024(4) 0.000(4) 0.002(3) 0.005(4) N N5 0.045(5) 0.050(6) 0.039(5) -0.002(4) 0.010(4) 0.002(4) N N6 0.061(6) 0.037(5) 0.036(5) -0.003(5) 0.019(4) -0.001(4) N N7 0.039(5) 0.055(5) 0.040(5) 0.014(4) 0.012(4) 0.008(4) N C1 0.047(6) 0.071(7) 0.058(8) 0.016(6) 0.016(6) -0.004(6) C C2 0.055(7) 0.047(7) 0.042(7) 0.014(5) 0.018(5) 0.013(5) C C3 0.085(9) 0.088(9) 0.073(9) 0.037(8) 0.030(8) 0.031(8) C C4 0.108(9) 0.057(9) 0.082(9) 0.029(8) 0.045(9) 0.022(7) C C5 0.128(9) 0.036(7) 0.074(9) 0.001(8) 0.058(9) 0.008(7) C C6 0.097(9) 0.046(7) 0.052(7) -0.025(7) 0.026(7) 0.004(6) C C7 0.054(7) 0.055(7) 0.045(7) -0.013(5) 0.015(5) 0.006(6) C C8 0.082(8) 0.038(6) 0.030(6) -0.002(6) 0.012(6) -0.002(5) C C9 0.109(9) 0.063(9) 0.065(9) -0.004(8) 0.023(8) 0.023(7) C C10 0.150(9) 0.070(9) 0.057(9) -0.001(9) 0.012(9) 0.021(8) C C11 0.108(9) 0.095(9) 0.050(8) 0.059(9) 0.005(8) 0.010(8) C C12 0.073(9) 0.069(8) 0.036(7) 0.020(7) 0.000(6) 0.004(6) C C13 0.044(6) 0.049(7) 0.035(6) 0.000(5) 0.009(5) 0.000(5) C C14 0.051(7) 0.051(7) 0.030(6) -0.009(5) 0.015(5) -0.003(5) C C15 0.075(9) 0.048(7) 0.053(7) -0.018(6) 0.018(6) -0.015(6) C C16 0.109(9) 0.035(7) 0.078(9) 0.004(8) 0.037(8) -0.006(7) C C17 0.092(9) 0.040(7) 0.065(8) 0.004(7) 0.035(7) 0.002(6) C C18 0.049(6) 0.058(7) 0.033(6) 0.006(6) 0.017(5) 0.009(5) C C19 0.050(7) 0.058(8) 0.049(7) 0.019(5) 0.016(5) 0.015(6) C C20 0.029(6) 0.102(9) 0.063(8) -0.004(6) 0.012(5) 0.029(7) C C21 0.048(7) 0.046(6) 0.043(6) -0.004(5) 0.014(5) 0.006(5) C C22 0.060(8) 0.108(9) 0.066(9) -0.043(8) -0.007(7) 0.013(8) C C23 0.098(9) 0.082(9) 0.060(9) -0.031(9) 0.001(8) -0.013(8) C C24 0.107(9) 0.058(8) 0.055(8) -0.015(8) 0.015(8) -0.021(7) C C25 0.073(8) 0.072(8) 0.041(7) -0.009(7) 0.015(6) -0.010(6) C C26 0.054(7) 0.062(7) 0.063(8) 0.018(6) 0.026(6) -0.006(6) C C27 0.074(8) 0.043(7) 0.040(7) 0.011(6) 0.025(6) 0.003(5) C C28 0.135(9) 0.072(9) 0.050(8) 0.022(9) 0.032(9) -0.012(7) C C29 0.157(9) 0.059(9) 0.063(9) -0.029(9) 0.002(9) -0.022(7) C C30 0.110(9) 0.069(9) 0.050(8) -0.024(9) 0.014(8) -0.012(7) C C31 0.069(8) 0.049(7) 0.037(6) -0.021(6) 0.009(6) -0.007(5) C Cl1A 0.059(4) 0.054(4) 0.062(6) 0.007(2) 0.000(2) 0.004(2) Cl O1A 0.096(6) 0.080(5) 0.247(9) -0.005(4) 0.017(6) 0.067(4) O O2A 0.070(4) 0.093(7) 0.149(9) 0.026(4) -0.011(3) 0.014(5) O O3A 0.109(5) 0.083(6) 0.158(9) 0.014(4) -0.052(5) -0.041(5) O O4A 0.207(9) 0.251(9) 0.083(4) 0.104(9) 0.058(6) 0.025(6) O Cl1B 0.050(7) 0.120(8) 0.063(5) 0.003(7) 0.019(4) 0.034(5) Cl O1B 0.145(9) 0.173(9) 0.114(7) 0.046(9) 0.041(7) -0.003(5) O O2B 0.115(9) 0.194(9) 0.074(5) -0.054(9) 0.000(6) 0.064(7) O O3B 0.094(9) 0.216(9) 0.099(9) -0.062(8) -0.013(6) 0.075(9) O O4B 0.086(8) 0.164(8) 0.123(9) 0.047(7) 0.022(8) 0.030(6) O Cl1B' 0.065(7) 0.130(8) 0.062(5) -0.004(6) 0.019(4) 0.032(5) Cl O1B' 0.128(9) 0.232(9) 0.079(7) -0.075(9) 0.001(7) 0.074(9) O O2B' 0.053(9) 0.246(9) 0.144(9) 0.026(8) 0.017(4) 0.063(9) O O3B' 0.056(7) 0.130(7) 0.078(6) 0.009(6) 0.013(5) 0.040(5) O O4B' 0.264(9) 0.179(9) 0.103(9) -0.013(9) 0.017(9) -0.018(9) O N1An 0.337(9) 0.167(9) 0.287(9) 0.001(9) 0.176(9) 0.006(9) N C1An 0.142(9) 0.210(9) 0.184(9) -0.028(9) 0.048(9) -0.114(9) C C2An 0.183(9) 0.227(9) 0.171(9) 0.046(9) 0.079(9) -0.047(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Br1 2.385(1) 1_555 1_555 no Cu1 N1 2.003(8) 1_555 1_555 no Cu1 N2 2.016(8) 1_555 1_555 no Cu1 N3 2.037(7) 1_555 1_555 no Cu1 N4 2.898(8) 1_555 1_555 no Cu1 Br2 3.022(2) 1_555 4_555 no Cu2 Br2 2.387(1) 1_555 1_555 no Cu2 N4 2.906(7) 1_555 1_555 no Cu2 N5 1.981(8) 1_555 1_555 no Cu2 N6 2.001(8) 1_555 1_555 no Cu2 N7 2.051(7) 1_555 1_555 no Cu2 Br1 3.037(2) 1_555 4_554 no Br1 Cu2 3.037(2) 1_555 4_555 no Br2 Cu1 3.022(2) 1_555 4_554 no N1 C2 1.353(12) 1_555 1_555 no N1 C6 1.360(12) 1_555 1_555 no N2 C8 1.336(12) 1_555 1_555 no N2 C12 1.335(12) 1_555 1_555 no N3 C1 1.465(12) 1_555 1_555 no N3 C7 1.477(12) 1_555 1_555 no N3 C13 1.517(11) 1_555 1_555 no N4 C14 1.348(11) 1_555 1_555 no N4 C18 1.351(11) 1_555 1_555 no N5 C21 1.337(12) 1_555 1_555 no N5 C25 1.348(13) 1_555 1_555 no N6 C27 1.336(12) 1_555 1_555 no N6 C31 1.336(12) 1_555 1_555 no N7 C19 1.497(12) 1_555 1_555 no N7 C20 1.499(13) 1_555 1_555 no N7 C26 1.474(12) 1_555 1_555 no C1 C2 1.510(15) 1_555 1_555 no C2 C3 1.371(15) 1_555 1_555 no C3 C4 1.329(17) 1_555 1_555 no C4 C5 1.368(18) 1_555 1_555 no C5 C6 1.376(16) 1_555 1_555 no C7 C8 1.485(14) 1_555 1_555 no C8 C9 1.392(15) 1_555 1_555 no C9 C10 1.375(19) 1_555 1_555 no C10 C11 1.402(19) 1_555 1_555 no C11 C12 1.375(17) 1_555 1_555 no C13 C14 1.459(13) 1_555 1_555 no C14 C15 1.405(13) 1_555 1_555 no C15 C16 1.339(15) 1_555 1_555 no C16 C17 1.370(15) 1_555 1_555 no C17 C18 1.380(14) 1_555 1_555 no C18 C19 1.479(13) 1_555 1_555 no C20 C21 1.476(15) 1_555 1_555 no C21 C22 1.391(15) 1_555 1_555 no C22 C23 1.400(18) 1_555 1_555 no C23 C24 1.359(18) 1_555 1_555 no C24 C25 1.376(15) 1_555 1_555 no C26 C27 1.475(15) 1_555 1_555 no C27 C28 1.430(16) 1_555 1_555 no C28 C29 1.355(20) 1_555 1_555 no C29 C30 1.412(19) 1_555 1_555 no C30 C31 1.357(15) 1_555 1_555 no Cl1A O1A 1.403(3) 1_555 1_555 no N1An C1An 1.212(35) 1_555 1_555 no C1An C2An 1.247(38) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Cu1 N1 97.8(3) 1_555 1_555 1_555 no Br1 Cu1 N2 98.1(2) 1_555 1_555 1_555 no Br1 Cu1 N3 172.5(2) 1_555 1_555 1_555 no Br1 Cu1 N4 97.7(2) 1_555 1_555 1_555 no Br1 Cu1 Br2 95.50(5) 1_555 1_555 4_555 no N1 Cu1 N2 164.0(4) 1_555 1_555 1_555 no N1 Cu1 N3 82.1(3) 1_555 1_555 1_555 no N1 Cu1 N4 104.5(3) 1_555 1_555 1_555 no N1 Cu1 Br2 92.7(2) 1_555 1_555 4_555 no N2 Cu1 N3 82.5(3) 1_555 1_555 1_555 no N2 Cu1 N4 75.5(3) 1_555 1_555 1_555 no N2 Cu1 Br2 83.6(2) 1_555 1_555 4_555 no N3 Cu1 N4 75.2(3) 1_555 1_555 1_555 no N3 Cu1 Br2 92.0(2) 1_555 1_555 4_555 no N4 Cu1 Br2 156.6(2) 1_555 1_555 4_555 no Br2 Cu2 N4 94.8(2) 1_555 1_555 1_555 no Br2 Cu2 N5 98.2(2) 1_555 1_555 1_555 no Br2 Cu2 N6 97.8(3) 1_555 1_555 1_555 no Br2 Cu2 N7 170.2(2) 1_555 1_555 1_555 no Br2 Cu2 Br1 95.07(5) 1_555 1_555 4_554 no N4 Cu2 N5 104.5(3) 1_555 1_555 1_555 no N4 Cu2 N6 75.1(3) 1_555 1_555 1_555 no N4 Cu2 N7 75.6(3) 1_555 1_555 1_555 no N4 Cu2 Br1 162.4(2) 1_555 1_555 4_554 no N5 Cu2 N6 164.0(4) 1_555 1_555 1_555 no N5 Cu2 N7 82.4(3) 1_555 1_555 1_555 no N5 Cu2 Br1 88.5(2) 1_555 1_555 4_554 no N6 Cu2 N7 82.1(3) 1_555 1_555 1_555 no N6 Cu2 Br1 89.1(2) 1_555 1_555 4_554 no N7 Cu2 Br1 94.7(2) 1_555 1_555 4_554 no Cu1 Br1 Cu2 84.40(5) 1_555 1_555 4_555 no Cu2 Br2 Cu1 84.70(5) 1_555 1_555 4_554 no Cu1 N1 C2 114.5(7) 1_555 1_555 1_555 no Cu1 N1 C6 127.7(8) 1_555 1_555 1_555 no C2 N1 C6 117.8(9) 1_555 1_555 1_555 no Cu1 N2 C8 112.2(7) 1_555 1_555 1_555 no Cu1 N2 C12 128.3(8) 1_555 1_555 1_555 no C8 N2 C12 119.5(9) 1_555 1_555 1_555 no Cu1 N3 C1 106.6(6) 1_555 1_555 1_555 no Cu1 N3 C7 106.3(6) 1_555 1_555 1_555 no Cu1 N3 C13 111.6(5) 1_555 1_555 1_555 no C1 N3 C7 111.8(8) 1_555 1_555 1_555 no C1 N3 C13 109.1(7) 1_555 1_555 1_555 no C7 N3 C13 111.3(7) 1_555 1_555 1_555 no Cu1 N4 Cu2 111.7(3) 1_555 1_555 1_555 no Cu1 N4 C14 89.3(5) 1_555 1_555 1_555 no Cu1 N4 C18 126.0(6) 1_555 1_555 1_555 no Cu2 N4 C14 127.3(6) 1_555 1_555 1_555 no Cu2 N4 C18 88.9(5) 1_555 1_555 1_555 no C14 N4 C18 117.6(8) 1_555 1_555 1_555 no Cu2 N5 C21 114.9(7) 1_555 1_555 1_555 no Cu2 N5 C25 127.4(7) 1_555 1_555 1_555 no C21 N5 C25 117.5(9) 1_555 1_555 1_555 no Cu2 N6 C27 112.8(7) 1_555 1_555 1_555 no Cu2 N6 C31 126.7(7) 1_555 1_555 1_555 no C27 N6 C31 120.3(9) 1_555 1_555 1_555 no Cu2 N7 C19 110.1(5) 1_555 1_555 1_555 no Cu2 N7 C20 104.7(6) 1_555 1_555 1_555 no Cu2 N7 C26 105.8(6) 1_555 1_555 1_555 no C19 N7 C20 109.4(8) 1_555 1_555 1_555 no C19 N7 C26 112.8(8) 1_555 1_555 1_555 no C20 N7 C26 113.5(8) 1_555 1_555 1_555 no N3 C1 C2 109.7(8) 1_555 1_555 1_555 no N1 C2 C1 113.4(8) 1_555 1_555 1_555 no N1 C2 C3 121.8(11) 1_555 1_555 1_555 no C1 C2 C3 124.5(11) 1_555 1_555 1_555 no C2 C3 C4 119.3(13) 1_555 1_555 1_555 no C3 C4 C5 121.4(12) 1_555 1_555 1_555 no C4 C5 C6 118.1(11) 1_555 1_555 1_555 no N1 C6 C5 121.7(11) 1_555 1_555 1_555 no N3 C7 C8 109.7(8) 1_555 1_555 1_555 no N2 C8 C7 117.3(9) 1_555 1_555 1_555 no N2 C8 C9 121.2(11) 1_555 1_555 1_555 no C7 C8 C9 121.5(11) 1_555 1_555 1_555 no C8 C9 C10 120.5(13) 1_555 1_555 1_555 no C9 C10 C11 116.9(12) 1_555 1_555 1_555 no C10 C11 C12 120.2(12) 1_555 1_555 1_555 no N2 C12 C11 121.7(12) 1_555 1_555 1_555 no N3 C13 C14 112.9(8) 1_555 1_555 1_555 no N4 C14 C13 116.1(9) 1_555 1_555 1_555 no N4 C14 C15 120.6(10) 1_555 1_555 1_555 no C13 C14 C15 123.3(9) 1_555 1_555 1_555 no C14 C15 C16 120.8(10) 1_555 1_555 1_555 no C15 C16 C17 119.1(10) 1_555 1_555 1_555 no C16 C17 C18 118.9(11) 1_555 1_555 1_555 no N4 C18 C17 122.9(10) 1_555 1_555 1_555 no N4 C18 C19 115.4(9) 1_555 1_555 1_555 no C17 C18 C19 121.6(10) 1_555 1_555 1_555 no N7 C19 C18 113.9(8) 1_555 1_555 1_555 no N7 C20 C21 109.7(8) 1_555 1_555 1_555 no N5 C21 C20 114.4(9) 1_555 1_555 1_555 no N5 C21 C22 122.8(11) 1_555 1_555 1_555 no C20 C21 C22 122.7(11) 1_555 1_555 1_555 no C21 C22 C23 118.5(12) 1_555 1_555 1_555 no C22 C23 C24 118.0(12) 1_555 1_555 1_555 no C23 C24 C25 120.5(12) 1_555 1_555 1_555 no N5 C25 C24 122.3(11) 1_555 1_555 1_555 no N7 C26 C27 109.9(8) 1_555 1_555 1_555 no N6 C27 C26 117.1(9) 1_555 1_555 1_555 no N6 C27 C28 119.0(11) 1_555 1_555 1_555 no C26 C27 C28 124.0(11) 1_555 1_555 1_555 no C27 C28 C29 120.5(13) 1_555 1_555 1_555 no C28 C29 C30 118.4(12) 1_555 1_555 1_555 no C29 C30 C31 118.6(13) 1_555 1_555 1_555 no N6 C31 C30 123.1(11) 1_555 1_555 1_555 no O1A Cl1A O2A 109.47 1_555 1_555 1_555 no N1An C1An C2An 176.6(38) 1_555 1_555 1_555 no #===END data_[Cu2(L)Br3](ClO4) _database_code_depnum_ccdc_archive 'CCDC 225106' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C31 H31 Br3 Cu2 N7 1+,Cl O4 1-' _chemical_formula_sum 'C31 H31 Br3 Cl Cu2 N7 O4' _chemical_formula_iupac ? _chemical_formula_weight 967.9 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.896(4) _cell_length_b 10.771(6) _cell_length_c 19.092(9) _cell_angle_alpha 96.06(3) _cell_angle_beta 96.45(3) _cell_angle_gamma 103.43(3) _cell_volume 1752(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 9 _cell_measurement_theta_max 10 _cell_measurement_temperature 294 _exptl_crystal_description lath _exptl_crystal_colour blue _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.83 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956.0 _exptl_absorpt_coefficient_mu 4.729 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.79 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6363 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 6160 _reflns_number_gt 3679 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.058 _refine_ls_wR_factor_ref 0.068 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3679 _refine_ls_number_parameters 410 _refine_ls_goodness_of_fit_ref 1.83 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 1.27 _refine_diff_density_min -1.54 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Cu1 0.21906(13) 0.09760(12) 0.18816(6) 0.0406(3) Uani Cu 1.0 Cu2 0.28065(13) 0.57746(12) 0.19536(6) 0.0392(3) Uani Cu 1.0 Br1 -0.04604(14) 0.11633(14) 0.18218(7) 0.0706(4) Uani Br 1.0 Br2 0.43035(14) 0.54059(14) 0.10466(7) 0.0666(4) Uani Br 1.0 Br3 0.21301(14) 0.82808(10) 0.15160(6) 0.0571(3) Uani Br 1.0 N1 0.2512(9) 0.1254(7) 0.0894(4) 0.042(2) Uani N 1.0 N2 0.2501(9) 0.0709(7) 0.2896(4) 0.035(2) Uani N 1.0 N3 0.4605(8) 0.1457(7) 0.2024(4) 0.037(2) Uani N 1.0 N4 0.3324(9) 0.3748(7) 0.2707(4) 0.038(2) Uani N 1.0 N5 0.0722(8) 0.4907(7) 0.1401(4) 0.036(2) Uani N 1.0 N6 0.4533(8) 0.6783(7) 0.2717(5) 0.041(2) Uani N 1.0 N7 0.1477(8) 0.5786(7) 0.2770(4) 0.035(2) Uani N 1.0 C1 0.5059(11) 0.1020(10) 0.1340(5) 0.047(3) Uani C 1.0 C2 0.3969(12) 0.1313(9) 0.0748(5) 0.040(2) Uani C 1.0 C3 0.4364(14) 0.1507(11) 0.0082(6) 0.057(3) Uani C 1.0 C4 0.3245(17) 0.1644(12) -0.0452(6) 0.068(4) Uani C 1.0 C5 0.1757(16) 0.1592(11) -0.0305(6) 0.062(3) Uani C 1.0 C6 0.1454(12) 0.1406(10) 0.0364(6) 0.049(3) Uani C 1.0 C7 0.5086(10) 0.0715(9) 0.2601(5) 0.038(2) Uani C 1.0 C8 0.3961(11) 0.0617(8) 0.3128(5) 0.036(2) Uani C 1.0 C9 0.4365(12) 0.0404(9) 0.3819(6) 0.045(3) Uani C 1.0 C10 0.3249(15) 0.0234(10) 0.4261(6) 0.055(3) Uani C 1.0 C11 0.1770(13) 0.0318(11) 0.4023(6) 0.053(3) Uani C 1.0 C12 0.1415(11) 0.0573(10) 0.3346(6) 0.045(3) Uani C 1.0 C13 0.5305(11) 0.2891(10) 0.2224(5) 0.044(3) Uani C 1.0 C14 0.4700(12) 0.3457(9) 0.2848(5) 0.043(3) Uani C 1.0 C15 0.5464(13) 0.3578(10) 0.3537(6) 0.055(3) Uani C 1.0 C16 0.4761(17) 0.3958(11) 0.4084(6) 0.072(4) Uani C 1.0 C17 0.3293(15) 0.4192(10) 0.3959(5) 0.056(3) Uani C 1.0 C18 0.2650(12) 0.4140(9) 0.3250(5) 0.041(2) Uani C 1.0 C19 0.1153(12) 0.4520(10) 0.3052(5) 0.047(3) Uani C 1.0 C20 -0.0017(11) 0.5978(10) 0.2428(6) 0.045(3) Uani C 1.0 C21 -0.0467(10) 0.5170(9) 0.1710(5) 0.036(2) Uani C 1.0 C22 -0.1971(11) 0.4810(11) 0.1370(6) 0.051(3) Uani C 1.0 C23 -0.2272(13) 0.4146(13) 0.0708(7) 0.064(4) Uani C 1.0 C24 -0.1085(15) 0.3772(10) 0.0400(6) 0.057(3) Uani C 1.0 C25 0.0450(12) 0.4203(10) 0.0765(6) 0.047(3) Uani C 1.0 C26 0.2307(12) 0.6846(9) 0.3323(5) 0.042(2) Uani C 1.0 C27 0.4027(11) 0.7047(9) 0.3340(6) 0.045(3) Uani C 1.0 C28 0.5072(13) 0.7549(11) 0.3965(6) 0.060(3) Uani C 1.0 C29 0.6631(15) 0.7817(12) 0.3926(8) 0.079(4) Uani C 1.0 C30 0.7130(14) 0.7616(14) 0.3279(9) 0.089(5) Uani C 1.0 C31 0.6049(12) 0.7070(11) 0.2679(7) 0.063(3) Uani C 1.0 Cl1 0.8812(3) 0.2287(3) 0.4605(2) 0.076(5) Uani Cl 1.0 O1 0.7611(8) 0.2665(8) 0.4880(4) 0.108(6) Uani O 1.0 O2 1.0079(9) 0.2538(10) 0.5121(4) 0.190(3) Uani O 1.0 O3 0.9192(11) 0.2948(10) 0.4052(5) 0.196(9) Uani O 1.0 O4 0.8366(10) 0.0996(7) 0.4368(6) 0.144(8) Uani O 1.0 H1C1 0.4972 0.0072 0.1295 0.047 Uani H 1.0 H2C1 0.6159 0.1486 0.1314 0.047 Uani H 1.0 HC3 0.5454 0.1548 -0.0015 0.057 Uani H 1.0 HC4 0.3518 0.1779 -0.0937 0.068 Uani H 1.0 HC5 0.0923 0.1688 -0.0677 0.062 Uani H 1.0 HC6 0.0374 0.1381 0.0472 0.049 Uani H 1.0 H1C7 0.6155 0.1172 0.2847 0.038 Uani H 1.0 H2C7 0.5096 -0.0170 0.2385 0.038 Uani H 1.0 HC9 0.5458 0.0376 0.3992 0.045 Uani H 1.0 HC10 0.3512 0.0050 0.4756 0.055 Uani H 1.0 HC11 0.0950 0.0193 0.4345 0.053 Uani H 1.0 HC12 0.0342 0.0659 0.3181 0.045 Uani H 1.0 H1C13 0.5051 0.3127 0.1740 0.044 Uani H 1.0 H2C13 0.6374 0.2734 0.2276 0.044 Uani H 1.0 HC15 0.6512 0.3388 0.3625 0.055 Uani H 1.0 HC16 0.5304 0.4071 0.4582 0.072 Uani H 1.0 HC17 0.2716 0.4390 0.4360 0.056 Uani H 1.0 H1C19 0.0461 0.3846 0.2678 0.047 Uani H 1.0 H2C19 0.0620 0.4596 0.3483 0.047 Uani H 1.0 H1C20 0.0110 0.6907 0.2370 0.045 Uani H 1.0 H2C20 -0.0850 0.5714 0.2731 0.045 Uani H 1.0 HC22 -0.2836 0.5035 0.1608 0.051 Uani H 1.0 HC23 -0.3353 0.3925 0.0441 0.064 Uani H 1.0 HC24 -0.1308 0.3211 -0.0070 0.057 Uani H 1.0 HC25 0.1336 0.3978 0.0544 0.047 Uani H 1.0 H1C26 0.2019 0.6634 0.3795 0.042 Uani H 1.0 H2C26 0.2003 0.7652 0.3220 0.042 Uani H 1.0 HC28 0.4681 0.7709 0.4429 0.060 Uani H 1.0 HC29 0.7405 0.8156 0.4366 0.079 Uani H 1.0 HC30 0.8269 0.7862 0.3239 0.089 Uani H 1.0 HC31 0.6421 0.6891 0.2212 0.063 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Cu1 0.0370(7) 0.0472(8) 0.0369(7) 0.0101(5) 0.0013(5) 0.0080(6) Cu Cu2 0.0282(6) 0.0448(8) 0.0403(7) 0.0037(5) 0.0042(5) -0.0004(6) Cu Br1 0.0498(7) 0.090(1) 0.0692(9) 0.0194(7) -0.0016(6) 0.0044(7) Br Br2 0.0490(7) 0.098(1) 0.0590(8) 0.0248(7) 0.0134(6) 0.0200(7) Br Br3 0.0735(8) 0.0356(6) 0.0545(7) 0.0075(5) -0.0067(6) 0.0017(5) Br N1 0.054(5) 0.032(5) 0.034(5) 0.010(4) -0.006(4) 0.000(4) N N2 0.044(5) 0.030(5) 0.032(4) 0.010(4) 0.003(4) 0.004(4) N N3 0.040(4) 0.035(5) 0.035(5) 0.014(4) -0.001(4) 0.002(4) N N4 0.043(5) 0.031(5) 0.036(5) 0.005(4) -0.002(4) 0.008(4) N N5 0.038(4) 0.027(4) 0.038(5) 0.005(3) -0.002(4) 0.005(4) N N6 0.030(4) 0.035(5) 0.055(6) 0.009(4) -0.005(4) -0.002(4) N N7 0.036(4) 0.032(5) 0.038(5) 0.007(4) 0.008(4) 0.003(4) N C1 0.047(6) 0.049(7) 0.046(6) 0.014(5) 0.004(5) 0.003(5) C C2 0.050(6) 0.036(6) 0.037(6) 0.012(5) 0.012(5) 0.004(5) C C3 0.069(8) 0.047(7) 0.045(7) 0.000(6) 0.009(6) -0.001(5) C C4 0.099(9) 0.055(8) 0.043(7) 0.011(7) -0.001(7) 0.000(6) C C5 0.091(9) 0.043(7) 0.049(8) 0.018(7) -0.007(7) 0.005(6) C C6 0.060(7) 0.039(6) 0.045(7) 0.013(5) -0.001(5) 0.004(5) C C7 0.034(5) 0.035(6) 0.048(6) 0.014(4) 0.003(4) 0.009(5) C C8 0.051(6) 0.021(5) 0.037(6) 0.011(4) 0.002(5) 0.005(4) C C9 0.060(7) 0.030(6) 0.043(6) 0.013(5) -0.002(5) 0.004(5) C C10 0.082(8) 0.044(7) 0.040(7) 0.014(6) 0.005(6) 0.008(5) C C11 0.059(7) 0.051(7) 0.053(7) 0.010(6) 0.019(6) 0.016(6) C C12 0.047(6) 0.039(6) 0.051(7) 0.011(5) 0.013(5) 0.008(5) C C13 0.040(6) 0.043(6) 0.051(7) 0.012(5) 0.003(5) 0.015(5) C C14 0.052(6) 0.023(5) 0.045(6) 0.001(5) -0.007(5) 0.004(5) C C15 0.062(7) 0.037(6) 0.062(8) 0.022(5) -0.019(6) -0.001(6) C C16 0.118(9) 0.043(7) 0.047(8) 0.036(7) -0.032(7) -0.007(6) C C17 0.100(9) 0.031(6) 0.037(6) 0.024(6) -0.001(6) 0.003(5) C C18 0.059(6) 0.019(5) 0.041(6) 0.001(4) 0.003(5) 0.008(4) C C19 0.058(7) 0.047(7) 0.037(6) 0.010(5) 0.010(5) 0.014(5) C C20 0.034(5) 0.055(7) 0.051(7) 0.017(5) 0.014(5) 0.004(5) C C21 0.031(5) 0.029(5) 0.051(6) 0.010(4) 0.010(4) 0.007(5) C C22 0.036(6) 0.052(7) 0.059(7) 0.000(5) 0.004(5) 0.014(6) C C23 0.042(7) 0.082(9) 0.060(8) -0.004(6) -0.005(6) 0.027(7) C C24 0.081(8) 0.041(7) 0.037(6) -0.003(6) -0.011(6) 0.009(5) C C25 0.051(6) 0.043(6) 0.043(6) 0.002(5) 0.000(5) 0.011(5) C C26 0.057(6) 0.030(6) 0.037(6) 0.013(5) 0.000(5) -0.007(5) C C27 0.045(6) 0.031(6) 0.054(7) 0.013(5) -0.008(5) -0.005(5) C C28 0.062(8) 0.053(7) 0.063(8) 0.031(6) -0.016(6) -0.014(6) C C29 0.065(9) 0.058(9) 0.098(9) 0.026(7) -0.032(8) -0.035(8) C C30 0.042(7) 0.079(9) 0.127(9) 0.011(7) -0.014(8) -0.030(9) C C31 0.034(6) 0.060(8) 0.089(9) 0.010(5) -0.001(6) -0.009(7) C Cl1 0.051(5) 0.094(9) 0.092(7) 0.022(6) 0.016(2) 0.040(2) Cl O1 0.091(7) 0.156(9) 0.105(9) 0.069(7) 0.029(4) 0.041(4) O O2 0.096(5) 0.276(9) 0.182(9) 0.078(8) -0.050(6) -0.038(8) O O3 0.183(9) 0.244(9) 0.253(9) 0.111(9) 0.144(8) 0.192(9) O O4 0.120(9) 0.100(8) 0.213(9) 0.037(8) 0.020(6) 0.013(5) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Br1 2.404(2) 1_555 1_555 no Cu1 Br3 2.900(2) 1_555 1_545 no Cu1 N1 1.982(8) 1_555 1_555 no Cu1 N2 1.987(7) 1_555 1_555 no Cu1 N3 2.068(7) 1_555 1_555 no Cu2 Br2 2.355(2) 1_555 1_555 no Cu2 Br3 3.076(2) 1_555 1_555 no Cu2 N5 1.993(7) 1_555 1_555 no Cu2 N6 2.013(8) 1_555 1_555 no Cu2 N7 2.060(7) 1_555 1_555 no Br3 Cu1 2.900(2) 1_555 1_565 no N1 C2 1.344(12) 1_555 1_555 no N1 C6 1.352(12) 1_555 1_555 no N2 C8 1.353(11) 1_555 1_555 no N2 C12 1.357(12) 1_555 1_555 no N3 C1 1.471(12) 1_555 1_555 no N3 C7 1.508(11) 1_555 1_555 no N3 C13 1.515(12) 1_555 1_555 no N4 C14 1.338(12) 1_555 1_555 no N4 C18 1.334(12) 1_555 1_555 no N5 C21 1.339(11) 1_555 1_555 no N5 C25 1.327(12) 1_555 1_555 no N6 C27 1.344(13) 1_555 1_555 no N6 C31 1.324(12) 1_555 1_555 no N7 C19 1.496(12) 1_555 1_555 no N7 C20 1.482(12) 1_555 1_555 no N7 C26 1.464(11) 1_555 1_555 no C1 C2 1.513(14) 1_555 1_555 no C2 C3 1.381(14) 1_555 1_555 no C3 C4 1.387(16) 1_555 1_555 no C4 C5 1.374(17) 1_555 1_555 no C5 C6 1.360(15) 1_555 1_555 no C7 C8 1.491(13) 1_555 1_555 no C8 C9 1.386(13) 1_555 1_555 no C9 C10 1.366(15) 1_555 1_555 no C10 C11 1.369(15) 1_555 1_555 no C11 C12 1.367(14) 1_555 1_555 no C13 C14 1.492(14) 1_555 1_555 no C14 C15 1.389(14) 1_555 1_555 no C15 C16 1.351(17) 1_555 1_555 no C16 C17 1.386(17) 1_555 1_555 no C17 C18 1.399(14) 1_555 1_555 no C18 C19 1.502(14) 1_555 1_555 no C20 C21 1.503(13) 1_555 1_555 no C21 C22 1.368(13) 1_555 1_555 no C22 C23 1.350(16) 1_555 1_555 no C23 C24 1.382(17) 1_555 1_555 no C24 C25 1.410(14) 1_555 1_555 no C26 C27 1.491(14) 1_555 1_555 no C27 C28 1.400(14) 1_555 1_555 no C28 C29 1.362(17) 1_555 1_555 no C29 C30 1.372(20) 1_555 1_555 no C30 C31 1.389(17) 1_555 1_555 no Cl1 O1 1.366(5) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Cu1 Br3 108.2(1) 1_555 1_555 1_545 no Br1 Cu1 N1 98.4(2) 1_555 1_555 1_555 no Br1 Cu1 N2 97.6(2) 1_555 1_555 1_555 no Br1 Cu1 N3 161.3(2) 1_555 1_555 1_555 no Br3 Cu1 N1 89.2(2) 1_545 1_555 1_555 no Br3 Cu1 N2 87.5(2) 1_545 1_555 1_555 no Br3 Cu1 N3 90.6(2) 1_545 1_555 1_555 no N1 Cu1 N2 163.9(3) 1_555 1_555 1_555 no N1 Cu1 N3 81.4(3) 1_555 1_555 1_555 no N2 Cu1 N3 82.9(3) 1_555 1_555 1_555 no Br2 Cu2 Br3 96.7(1) 1_555 1_555 1_555 no Br2 Cu2 N5 97.0(2) 1_555 1_555 1_555 no Br2 Cu2 N6 99.3(2) 1_555 1_555 1_555 no Br2 Cu2 N7 170.6(2) 1_555 1_555 1_555 no Br3 Cu2 N5 85.5(2) 1_555 1_555 1_555 no Br3 Cu2 N6 90.9(2) 1_555 1_555 1_555 no Br3 Cu2 N7 92.4(2) 1_555 1_555 1_555 no N5 Cu2 N6 163.7(3) 1_555 1_555 1_555 no N5 Cu2 N7 81.2(3) 1_555 1_555 1_555 no N6 Cu2 N7 83.0(3) 1_555 1_555 1_555 no Cu1 Br3 Cu2 149.7(1) 1_565 1_555 1_555 no Cu1 N1 C2 114.9(6) 1_555 1_555 1_555 no Cu1 N1 C6 127.7(7) 1_555 1_555 1_555 no C2 N1 C6 117.3(9) 1_555 1_555 1_555 no Cu1 N2 C8 113.5(6) 1_555 1_555 1_555 no Cu1 N2 C12 127.1(6) 1_555 1_555 1_555 no C8 N2 C12 119.4(8) 1_555 1_555 1_555 no Cu1 N3 C1 106.0(5) 1_555 1_555 1_555 no Cu1 N3 C7 105.6(5) 1_555 1_555 1_555 no Cu1 N3 C13 112.9(5) 1_555 1_555 1_555 no C1 N3 C7 111.4(7) 1_555 1_555 1_555 no C1 N3 C13 109.5(7) 1_555 1_555 1_555 no C7 N3 C13 111.3(7) 1_555 1_555 1_555 no C14 N4 C18 118.5(8) 1_555 1_555 1_555 no Cu2 N5 C21 113.3(6) 1_555 1_555 1_555 no Cu2 N5 C25 126.5(7) 1_555 1_555 1_555 no C21 N5 C25 120.1(8) 1_555 1_555 1_555 no Cu2 N6 C27 112.9(6) 1_555 1_555 1_555 no Cu2 N6 C31 127.0(8) 1_555 1_555 1_555 no C27 N6 C31 119.8(9) 1_555 1_555 1_555 no Cu2 N7 C19 111.6(6) 1_555 1_555 1_555 no Cu2 N7 C20 103.8(6) 1_555 1_555 1_555 no Cu2 N7 C26 107.7(6) 1_555 1_555 1_555 no C19 N7 C20 108.5(7) 1_555 1_555 1_555 no C19 N7 C26 111.8(7) 1_555 1_555 1_555 no C20 N7 C26 113.1(7) 1_555 1_555 1_555 no N3 C1 C2 108.3(8) 1_555 1_555 1_555 no N1 C2 C1 114.8(8) 1_555 1_555 1_555 no N1 C2 C3 121.3(10) 1_555 1_555 1_555 no C1 C2 C3 123.6(10) 1_555 1_555 1_555 no C2 C3 C4 119.9(11) 1_555 1_555 1_555 no C3 C4 C5 119.1(12) 1_555 1_555 1_555 no C4 C5 C6 117.8(11) 1_555 1_555 1_555 no N1 C6 C5 124.6(11) 1_555 1_555 1_555 no N3 C7 C8 109.8(7) 1_555 1_555 1_555 no N2 C8 C7 117.1(8) 1_555 1_555 1_555 no N2 C8 C9 120.9(9) 1_555 1_555 1_555 no C7 C8 C9 122.0(9) 1_555 1_555 1_555 no C8 C9 C10 119.1(10) 1_555 1_555 1_555 no C9 C10 C11 119.8(10) 1_555 1_555 1_555 no C10 C11 C12 120.0(10) 1_555 1_555 1_555 no N2 C12 C11 120.8(9) 1_555 1_555 1_555 no N3 C13 C14 113.1(8) 1_555 1_555 1_555 no N4 C14 C13 115.7(8) 1_555 1_555 1_555 no N4 C14 C15 122.5(10) 1_555 1_555 1_555 no C13 C14 C15 121.6(10) 1_555 1_555 1_555 no C14 C15 C16 118.5(10) 1_555 1_555 1_555 no C15 C16 C17 120.5(10) 1_555 1_555 1_555 no C16 C17 C18 117.4(11) 1_555 1_555 1_555 no N4 C18 C17 122.2(10) 1_555 1_555 1_555 no N4 C18 C19 115.7(8) 1_555 1_555 1_555 no C17 C18 C19 122.1(10) 1_555 1_555 1_555 no N7 C19 C18 110.4(8) 1_555 1_555 1_555 no N7 C20 C21 109.3(7) 1_555 1_555 1_555 no N5 C21 C20 115.3(8) 1_555 1_555 1_555 no N5 C21 C22 121.9(9) 1_555 1_555 1_555 no C20 C21 C22 122.6(9) 1_555 1_555 1_555 no C21 C22 C23 119.2(10) 1_555 1_555 1_555 no C22 C23 C24 119.9(10) 1_555 1_555 1_555 no C23 C24 C25 118.3(11) 1_555 1_555 1_555 no N5 C25 C24 120.2(10) 1_555 1_555 1_555 no N7 C26 C27 110.3(8) 1_555 1_555 1_555 no N6 C27 C26 116.6(8) 1_555 1_555 1_555 no N6 C27 C28 121.4(10) 1_555 1_555 1_555 no C26 C27 C28 121.9(10) 1_555 1_555 1_555 no C27 C28 C29 118.6(12) 1_555 1_555 1_555 no C28 C29 C30 119.3(11) 1_555 1_555 1_555 no C29 C30 C31 119.9(12) 1_555 1_555 1_555 no N6 C31 C30 120.8(12) 1_555 1_555 1_555 no O1 Cl1 O2 109.5 1_555 1_555 1_555 no #===END data_[Cu2(L)Cl3]Cl.6H2O _database_code_depnum_ccdc_archive 'CCDC 225107' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C31 H31 Cl3 Cu2 N7 1+,Cl 1-,6(H2 O)' _chemical_formula_sum 'C31 H43 Cl4 Cu2 N7 O6' _chemical_formula_iupac ? _chemical_formula_weight 878.6 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,-y,1/2+z 3 -x,-y,-z 4 -x,y,1/2-z 5 1/2+x,1/2+y,z 6 1/2+x,1/2-y,1/2+z 7 1/2-x,1/2-y,-z 8 1/2-x,1/2+y,1/2-z _cell_length_a 25.159(15) _cell_length_b 16.587(5) _cell_length_c 21.312(11) _cell_angle_alpha 90 _cell_angle_beta 113.12(2) _cell_angle_gamma 90 _cell_volume 8179(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 18 _cell_measurement_theta_max 20 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.43 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3616.0 _exptl_absorpt_coefficient_mu 4.122 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.78 # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 7171 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 65 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 4 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 6962 _reflns_number_gt 4122 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.057 _refine_ls_wR_factor_ref 0.079 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4122 _refine_ls_number_parameters 464 _refine_ls_goodness_of_fit_ref 1.77 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 1.21 _refine_diff_density_min -1.05 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description Cl/O1 0.66Cl+0.34O Cl/O2 0.34Cl+0.66O loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Cu1 0.36965(4) 0.52867(6) 0.52465(5) 0.0464(3) Uani Cu 1.0 Cu2 0.34404(4) 0.36253(6) 0.23329(4) 0.0441(3) Uani Cu 1.0 Cl1 0.45338(7) 0.46025(11) 0.55711(8) 0.0532(5) Uani Cl 1.0 Cl2 0.39114(7) 0.40946(12) 0.15329(8) 0.0585(5) Uani Cl 1.0 Cl3 0.26537(8) 0.29410(13) 0.16412(9) 0.0705(6) Uani Cl 1.0 N1 0.3956(2) 0.6310(3) 0.4975(3) 0.046(1) Uani N 1.0 N2 0.3221(2) 0.4419(4) 0.5425(3) 0.052(2) Uani N 1.0 N3 0.2914(2) 0.5876(3) 0.4860(3) 0.046(1) Uani N 1.0 N4 0.3239(2) 0.4752(4) 0.3980(3) 0.046(1) Uani N 1.0 N5 0.3052(3) 0.4689(4) 0.2319(3) 0.052(2) Uani N 1.0 N6 0.3977(3) 0.2682(4) 0.2654(3) 0.052(1) Uani N 1.0 N7 0.4051(2) 0.4121(3) 0.3201(3) 0.047(1) Uani N 1.0 C1 0.3059(3) 0.6752(5) 0.4999(4) 0.056(2) Uani C 1.0 C2 0.3595(3) 0.6928(5) 0.4891(4) 0.053(2) Uani C 1.0 C3 0.3723(4) 0.7697(5) 0.4745(5) 0.079(3) Uani C 1.0 C4 0.4231(5) 0.7811(6) 0.4650(6) 0.101(3) Uani C 1.0 C5 0.4608(4) 0.7165(6) 0.4732(5) 0.082(3) Uani C 1.0 C6 0.4453(3) 0.6420(5) 0.4885(4) 0.058(2) Uani C 1.0 C7 0.2576(3) 0.5546(5) 0.5229(4) 0.055(2) Uani C 1.0 C8 0.2696(3) 0.4664(5) 0.5354(3) 0.052(2) Uani C 1.0 C9 0.2309(4) 0.4122(6) 0.5437(4) 0.071(2) Uani C 1.0 C10 0.2459(4) 0.3337(6) 0.5594(5) 0.082(3) Uani C 1.0 C11 0.3002(5) 0.3089(5) 0.5661(5) 0.083(3) Uani C 1.0 C12 0.3369(3) 0.3643(5) 0.5568(4) 0.065(2) Uani C 1.0 C13 0.2617(3) 0.5745(5) 0.4103(3) 0.058(2) Uani C 1.0 C14 0.2704(3) 0.4917(4) 0.3887(3) 0.048(2) Uani C 1.0 C15 0.2251(3) 0.4381(5) 0.3598(4) 0.063(2) Uani C 1.0 C16 0.2376(4) 0.3624(6) 0.3414(4) 0.075(2) Uani C 1.0 C17 0.2928(4) 0.3441(5) 0.3503(4) 0.061(2) Uani C 1.0 C18 0.3353(3) 0.4031(5) 0.3774(3) 0.050(2) Uani C 1.0 C19 0.3960(3) 0.3893(5) 0.3830(4) 0.059(2) Uani C 1.0 C20 0.4011(3) 0.4998(5) 0.3088(4) 0.067(2) Uani C 1.0 C21 0.3402(4) 0.5257(5) 0.2700(4) 0.060(2) Uani C 1.0 C22 0.3233(5) 0.6023(5) 0.2742(5) 0.081(3) Uani C 1.0 C23 0.2644(7) 0.6218(7) 0.2380(6) 0.110(4) Uani C 1.0 C24 0.2284(5) 0.5654(8) 0.2004(5) 0.098(4) Uani C 1.0 C25 0.2497(4) 0.4871(6) 0.1974(4) 0.075(3) Uani C 1.0 C26 0.4609(3) 0.3776(5) 0.3225(4) 0.056(2) Uani C 1.0 C27 0.4513(3) 0.2893(5) 0.3082(3) 0.056(2) Uani C 1.0 C28 0.4946(4) 0.2332(7) 0.3357(4) 0.083(3) Uani C 1.0 C29 0.4818(5) 0.1530(7) 0.3194(6) 0.099(4) Uani C 1.0 C30 0.4284(6) 0.1314(6) 0.2756(7) 0.107(4) Uani C 1.0 C31 0.3858(4) 0.1905(5) 0.2476(5) 0.081(3) Uani C 1.0 Cl/OW1 0.5718(8) -0.0077(9) 0.5511(12) 0.674(9) Uani Cl/O1 1.0 Cl/OW2 0.8985(3) 0.4793(5) 0.5812(4) 0.205(4) Uani Cl/O2 1.0 OW1 0.9979(15) 0.1769(20) 0.1788(11) 0.309(9) Uani O 0.5 OW2 0.9490(8) 0.0990(11) 0.2017(7) 0.143(6) Uani O 0.5 OW3 0.9398(8) 0.5657(10) 0.7077(14) 0.432(9) Uani O 1.0 OW4 0.1060(4) 0.3182(5) 0.5621(6) 0.178(4) Uani O 1.0 OW5 0.9283(6) 0.3143(9) 0.0894(10) 0.310(8) Uani O 1.0 OW6 1.0885(15) 0.2656(16) 0.2634(19) 0.326(9) Uani O 0.5 OW6' 1.0676(15) 0.4202(17) 0.1656(22) 0.326(9) Uani O 0.5 H1C1 0.3120 0.6879 0.5482 0.056 Uani H 1.0 H2C1 0.2735 0.7088 0.4682 0.056 Uani H 1.0 HC3 0.3457 0.8158 0.4710 0.079 Uani H 1.0 HC4 0.4328 0.8355 0.4523 0.101 Uani H 1.0 HC5 0.4983 0.7243 0.4680 0.082 Uani H 1.0 HC6 0.4714 0.5950 0.4931 0.058 Uani H 1.0 H1C7 0.2154 0.5627 0.4950 0.055 Uani H 1.0 H2C7 0.2685 0.5831 0.5676 0.055 Uani H 1.0 HC9 0.1915 0.4310 0.5381 0.071 Uani H 1.0 HC10 0.2182 0.2948 0.5660 0.082 Uani H 1.0 HC11 0.3126 0.2516 0.5776 0.083 Uani H 1.0 HC12 0.3760 0.3463 0.5607 0.065 Uani H 1.0 H1C13 0.2774 0.6143 0.3866 0.058 Uani H 1.0 H2C13 0.2194 0.5837 0.3964 0.058 Uani H 1.0 HC15 0.1846 0.4535 0.3524 0.063 Uani H 1.0 HC16 0.2062 0.3215 0.3216 0.075 Uani H 1.0 HC17 0.3027 0.2898 0.3377 0.061 Uani H 1.0 H1C19 0.4054 0.3307 0.3923 0.059 Uani H 1.0 H2C19 0.4229 0.4220 0.4220 0.059 Uani H 1.0 H1C20 0.4249 0.5151 0.2825 0.067 Uani H 1.0 H2C20 0.4165 0.5277 0.3540 0.067 Uani H 1.0 HC22 0.3515 0.6438 0.3021 0.081 Uani H 1.0 HC23 0.2501 0.6774 0.2406 0.110 Uani H 1.0 HC24 0.1866 0.5782 0.1744 0.098 Uani H 1.0 HC25 0.2227 0.4448 0.1689 0.075 Uani H 1.0 H1C26 0.4922 0.3862 0.3687 0.056 Uani H 1.0 H2C26 0.4721 0.4038 0.2872 0.056 Uani H 1.0 HC28 0.5344 0.2502 0.3667 0.083 Uani H 1.0 HC29 0.5121 0.1109 0.3403 0.099 Uani H 1.0 HC30 0.4194 0.0734 0.2631 0.107 Uani H 1.0 HC31 0.3464 0.1748 0.2143 0.081 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Cu1 0.0426(5) 0.0511(6) 0.0485(6) 0.0071(5) 0.0212(4) 0.0038(5) Cu Cu2 0.0447(5) 0.0507(6) 0.0369(5) -0.0002(5) 0.0161(4) -0.0016(5) Cu Cl1 0.0480(9) 0.062(1) 0.049(1) 0.0138(8) 0.0183(8) -0.0001(9) Cl Cl2 0.054(1) 0.084(1) 0.0434(9) -0.0006(9) 0.0260(8) 0.0098(9) Cl Cl3 0.065(1) 0.082(1) 0.055(1) -0.024(1) 0.0135(9) -0.005(1) Cl N1 0.052(3) 0.047(3) 0.046(3) 0.007(3) 0.027(3) 0.001(3) N N2 0.058(4) 0.058(4) 0.042(3) -0.003(3) 0.022(3) -0.001(3) N N3 0.047(3) 0.050(4) 0.044(3) 0.010(3) 0.021(3) 0.001(3) N N4 0.049(3) 0.058(4) 0.034(3) 0.005(3) 0.018(3) -0.005(3) N N5 0.058(4) 0.066(4) 0.042(3) 0.016(3) 0.031(3) 0.010(3) N N6 0.064(4) 0.051(4) 0.047(3) 0.005(3) 0.030(3) -0.002(3) N N7 0.047(3) 0.053(4) 0.044(3) -0.001(3) 0.020(3) -0.014(3) N C1 0.058(4) 0.060(5) 0.054(5) 0.012(4) 0.027(4) 0.000(4) C C2 0.058(4) 0.054(5) 0.050(4) 0.012(4) 0.023(4) 0.006(4) C C3 0.076(6) 0.056(6) 0.104(7) 0.014(4) 0.035(5) 0.023(5) C C4 0.094(7) 0.071(7) 0.140(9) -0.005(6) 0.047(7) 0.039(7) C C5 0.072(6) 0.089(7) 0.094(7) -0.015(5) 0.040(5) 0.017(6) C C6 0.056(4) 0.062(5) 0.060(5) 0.000(4) 0.028(4) 0.004(4) C C7 0.050(4) 0.071(5) 0.056(5) 0.004(4) 0.035(4) 0.000(4) C C8 0.054(4) 0.074(5) 0.037(4) 0.002(4) 0.027(3) -0.003(4) C C9 0.068(5) 0.096(7) 0.057(5) -0.011(5) 0.032(4) -0.003(5) C C10 0.090(7) 0.084(7) 0.085(7) -0.025(6) 0.047(6) -0.002(5) C C11 0.113(8) 0.059(6) 0.090(7) -0.009(6) 0.052(6) 0.009(5) C C12 0.076(6) 0.057(5) 0.066(5) 0.006(4) 0.030(4) 0.011(4) C C13 0.056(4) 0.074(5) 0.037(4) 0.018(4) 0.012(3) 0.007(4) C C14 0.047(4) 0.063(5) 0.034(4) 0.007(4) 0.017(3) 0.000(3) C C15 0.061(5) 0.080(6) 0.052(5) 0.002(5) 0.026(4) -0.004(4) C C16 0.072(6) 0.092(7) 0.069(6) -0.021(5) 0.037(5) -0.013(5) C C17 0.085(6) 0.061(5) 0.049(4) -0.012(4) 0.038(4) -0.010(4) C C18 0.052(4) 0.066(5) 0.029(3) 0.006(4) 0.014(3) 0.006(3) C C19 0.058(4) 0.079(6) 0.041(4) 0.014(4) 0.020(3) -0.012(4) C C20 0.072(5) 0.050(5) 0.078(6) -0.014(4) 0.029(5) -0.014(4) C C21 0.082(6) 0.051(5) 0.065(5) 0.009(5) 0.049(5) 0.007(4) C C22 0.135(9) 0.051(6) 0.088(7) 0.019(6) 0.076(7) 0.018(5) C C23 0.191(9) 0.076(8) 0.095(8) 0.063(8) 0.091(9) 0.030(6) C C24 0.115(9) 0.119(9) 0.073(7) 0.071(8) 0.050(7) 0.028(6) C C25 0.076(6) 0.106(8) 0.048(5) 0.028(5) 0.032(4) 0.015(5) C C26 0.040(4) 0.075(6) 0.048(4) 0.004(4) 0.010(3) -0.016(4) C C27 0.058(5) 0.076(6) 0.039(4) 0.021(4) 0.024(4) 0.000(4) C C28 0.083(6) 0.110(8) 0.056(5) 0.044(6) 0.027(5) 0.003(5) C C29 0.112(9) 0.096(9) 0.097(8) 0.052(7) 0.049(7) 0.024(7) C C30 0.163(9) 0.053(6) 0.139(9) 0.027(8) 0.095(9) 0.011(7) C C31 0.110(8) 0.052(5) 0.091(7) 0.004(5) 0.051(6) -0.012(5) C Cl/OW1 0.791(9) 0.296(9) 0.875(9) 0.179(9) 0.261(9) 0.136(9) Cl Cl/OW2 0.104(5) 0.202(7) 0.240(8) 0.048(4) -0.006(4) 0.046(6) Cl OW1 0.412(9) 0.357(9) 0.108(9) 0.092(9) 0.050(9) -0.068(9) O OW2 0.182(9) 0.185(9) 0.074(9) -0.035(9) 0.063(9) -0.005(9) O OW3 0.358(9) 0.262(9) 0.624(9) -0.112(9) 0.137(9) 0.107(9) O OW4 0.107(6) 0.140(8) 0.289(9) -0.019(5) 0.078(7) 0.043(8) O OW5 0.247(9) 0.258(9) 0.477(9) -0.090(9) 0.198(9) -0.166(9) O OW6 0.356(9) 0.212(9) 0.458(9) -0.073(9) 0.210(9) -0.160(9) O OW6 0.356(9) 0.212(9) 0.458(9) -0.073(9) 0.210(9) -0.160(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cl1 2.249(2) 1_555 1_555 no Cu1 Cl2 2.774(2) 1_555 2_565 no Cu1 N1 1.984(6) 1_555 1_555 no Cu1 N2 2.001(6) 1_555 1_555 no Cu1 N3 2.059(5) 1_555 1_555 no Cu1 N4 2.638(5) 1_555 1_555 no Cu2 Cl2 2.550(2) 1_555 1_555 no Cu2 Cl3 2.255(2) 1_555 1_555 no Cu2 N5 2.012(6) 1_555 1_555 no Cu2 N6 2.004(6) 1_555 1_555 no Cu2 N7 2.055(5) 1_555 1_555 no N1 C2 1.334(8) 1_555 1_555 no N1 C6 1.350(8) 1_555 1_555 no N2 C8 1.333(8) 1_555 1_555 no N2 C12 1.341(9) 1_555 1_555 no N3 C1 1.498(9) 1_555 1_555 no N3 C7 1.472(8) 1_555 1_555 no N3 C13 1.504(8) 1_555 1_555 no N4 C14 1.311(8) 1_555 1_555 no N4 C18 1.342(8) 1_555 1_555 no N5 C21 1.327(9) 1_555 1_555 no N5 C25 1.332(9) 1_555 1_555 no N6 C27 1.343(9) 1_555 1_555 no N6 C31 1.344(10) 1_555 1_555 no N7 C19 1.494(9) 1_555 1_555 no N7 C20 1.472(9) 1_555 1_555 no N7 C26 1.500(8) 1_555 1_555 no C1 C2 1.485(9) 1_555 1_555 no C2 C3 1.381(10) 1_555 1_555 no C3 C4 1.384(12) 1_555 1_555 no C4 C5 1.395(12) 1_555 1_555 no C5 C6 1.372(11) 1_555 1_555 no C7 C8 1.496(10) 1_555 1_555 no C8 C9 1.386(10) 1_555 1_555 no C9 C10 1.360(12) 1_555 1_555 no C10 C11 1.380(12) 1_555 1_555 no C11 C12 1.372(11) 1_555 1_555 no C13 C14 1.491(10) 1_555 1_555 no C14 C15 1.386(10) 1_555 1_555 no C15 C16 1.389(11) 1_555 1_555 no C16 C17 1.359(11) 1_555 1_555 no C17 C18 1.396(10) 1_555 1_555 no C18 C19 1.503(9) 1_555 1_555 no C20 C21 1.490(11) 1_555 1_555 no C21 C22 1.355(11) 1_555 1_555 no C22 C23 1.411(15) 1_555 1_555 no C23 C24 1.331(16) 1_555 1_555 no C24 C25 1.416(12) 1_555 1_555 no C26 C27 1.496(10) 1_555 1_555 no C27 C28 1.375(10) 1_555 1_555 no C28 C29 1.380(14) 1_555 1_555 no C29 C30 1.348(15) 1_555 1_555 no C30 C31 1.402(14) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Cu1 Cl2 95.00(6) 1_555 1_555 2_565 no Cl1 Cu1 N1 98.3(2) 1_555 1_555 1_555 no Cl1 Cu1 N2 97.8(2) 1_555 1_555 1_555 no Cl1 Cu1 N3 174.8(2) 1_555 1_555 1_555 no Cl1 Cu1 N4 97.2(1) 1_555 1_555 1_555 no Cl2 Cu1 N1 90.8(2) 2_565 1_555 1_555 no Cl2 Cu1 N2 88.7(2) 2_565 1_555 1_555 no Cl2 Cu1 N3 90.2(2) 2_565 1_555 1_555 no Cl2 Cu1 N4 166.7(1) 2_565 1_555 1_555 no N1 Cu1 N2 163.8(2) 1_555 1_555 1_555 no N1 Cu1 N3 81.4(2) 1_555 1_555 1_555 no N1 Cu1 N4 92.9(2) 1_555 1_555 1_555 no N2 Cu1 N3 82.4(2) 1_555 1_555 1_555 no N2 Cu1 N4 84.2(2) 1_555 1_555 1_555 no N3 Cu1 N4 77.7(2) 1_555 1_555 1_555 no Cl2 Cu2 Cl3 103.62(7) 1_555 1_555 1_555 no Cl2 Cu2 N5 94.2(2) 1_555 1_555 1_555 no Cl2 Cu2 N6 92.2(2) 1_555 1_555 1_555 no Cl2 Cu2 N7 95.8(2) 1_555 1_555 1_555 no Cl3 Cu2 N5 97.8(2) 1_555 1_555 1_555 no Cl3 Cu2 N6 97.5(2) 1_555 1_555 1_555 no Cl3 Cu2 N7 160.6(2) 1_555 1_555 1_555 no N5 Cu2 N6 161.5(2) 1_555 1_555 1_555 no N5 Cu2 N7 81.3(2) 1_555 1_555 1_555 no N6 Cu2 N7 80.8(2) 1_555 1_555 1_555 no Cu1 N1 C2 114.3(5) 1_555 1_555 1_555 no Cu1 N1 C6 126.0(5) 1_555 1_555 1_555 no C2 N1 C6 119.8(6) 1_555 1_555 1_555 no Cu1 N2 C8 113.6(5) 1_555 1_555 1_555 no Cu1 N2 C12 126.9(5) 1_555 1_555 1_555 no C8 N2 C12 119.5(7) 1_555 1_555 1_555 no Cu1 N3 C1 105.1(4) 1_555 1_555 1_555 no Cu1 N3 C7 105.8(4) 1_555 1_555 1_555 no Cu1 N3 C13 110.7(4) 1_555 1_555 1_555 no C1 N3 C7 113.7(5) 1_555 1_555 1_555 no C1 N3 C13 109.4(5) 1_555 1_555 1_555 no C7 N3 C13 111.8(5) 1_555 1_555 1_555 no Cu1 N4 C14 95.3(4) 1_555 1_555 1_555 no Cu1 N4 C18 124.7(4) 1_555 1_555 1_555 no C14 N4 C18 118.4(6) 1_555 1_555 1_555 no Cu2 N5 C21 114.3(5) 1_555 1_555 1_555 no Cu2 N5 C25 127.2(6) 1_555 1_555 1_555 no C21 N5 C25 118.5(7) 1_555 1_555 1_555 no Cu2 N6 C27 113.0(5) 1_555 1_555 1_555 no Cu2 N6 C31 127.3(6) 1_555 1_555 1_555 no C27 N6 C31 119.6(7) 1_555 1_555 1_555 no Cu2 N7 C19 112.6(4) 1_555 1_555 1_555 no Cu2 N7 C20 105.6(4) 1_555 1_555 1_555 no Cu2 N7 C26 103.7(4) 1_555 1_555 1_555 no C19 N7 C20 111.9(5) 1_555 1_555 1_555 no C19 N7 C26 110.1(5) 1_555 1_555 1_555 no C20 N7 C26 112.7(6) 1_555 1_555 1_555 no N3 C1 C2 109.0(6) 1_555 1_555 1_555 no N1 C2 C1 116.2(6) 1_555 1_555 1_555 no N1 C2 C3 122.2(7) 1_555 1_555 1_555 no C1 C2 C3 121.5(7) 1_555 1_555 1_555 no C2 C3 C4 118.0(8) 1_555 1_555 1_555 no C3 C4 C5 119.9(8) 1_555 1_555 1_555 no C4 C5 C6 118.6(8) 1_555 1_555 1_555 no N1 C6 C5 121.4(7) 1_555 1_555 1_555 no N3 C7 C8 109.9(5) 1_555 1_555 1_555 no N2 C8 C7 116.1(6) 1_555 1_555 1_555 no N2 C8 C9 120.2(8) 1_555 1_555 1_555 no C7 C8 C9 123.6(7) 1_555 1_555 1_555 no C8 C9 C10 120.7(8) 1_555 1_555 1_555 no C9 C10 C11 118.7(8) 1_555 1_555 1_555 no C10 C11 C12 118.6(8) 1_555 1_555 1_555 no N2 C12 C11 122.3(8) 1_555 1_555 1_555 no N3 C13 C14 113.2(6) 1_555 1_555 1_555 no N4 C14 C13 114.4(6) 1_555 1_555 1_555 no N4 C14 C15 123.3(7) 1_555 1_555 1_555 no C13 C14 C15 122.2(7) 1_555 1_555 1_555 no C14 C15 C16 117.9(7) 1_555 1_555 1_555 no C15 C16 C17 119.6(8) 1_555 1_555 1_555 no C16 C17 C18 118.5(8) 1_555 1_555 1_555 no N4 C18 C17 122.2(7) 1_555 1_555 1_555 no N4 C18 C19 116.8(6) 1_555 1_555 1_555 no C17 C18 C19 121.1(7) 1_555 1_555 1_555 no N7 C19 C18 113.5(6) 1_555 1_555 1_555 no N7 C20 C21 111.4(6) 1_555 1_555 1_555 no N5 C21 C20 115.2(7) 1_555 1_555 1_555 no N5 C21 C22 123.7(8) 1_555 1_555 1_555 no C20 C21 C22 121.1(9) 1_555 1_555 1_555 no C21 C22 C23 117.9(10) 1_555 1_555 1_555 no C22 C23 C24 119.3(10) 1_555 1_555 1_555 no C23 C24 C25 119.4(10) 1_555 1_555 1_555 no N5 C25 C24 121.1(9) 1_555 1_555 1_555 no N7 C26 C27 107.0(6) 1_555 1_555 1_555 no N6 C27 C26 115.6(6) 1_555 1_555 1_555 no N6 C27 C28 121.9(8) 1_555 1_555 1_555 no C26 C27 C28 122.5(8) 1_555 1_555 1_555 no C27 C28 C29 118.5(9) 1_555 1_555 1_555 no C28 C29 C30 120.1(10) 1_555 1_555 1_555 no C29 C30 C31 119.7(10) 1_555 1_555 1_555 no N6 C31 C30 120.1(9) 1_555 1_555 1_555 no #===END