# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1801 data_1 #[(Cu2L)2mbdpz] #------------------------------------------------------------------------------ _audit_creation_date '1999-03-26' _audit_creation_method 'by teXsan v1.8' #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton ' _publ_contact_author_name ' Paul E. Kruger ' _publ_contact_author_address ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; _publ_contact_author_phone ' 353 1 608 1422 ' _publ_contact_author_fax ' 353 1 671 2826 ' _publ_contact_author_email ' paul.kruger@tcd.ie ' loop_ _publ_author_name _publ_author_address ' Paul E. Kruger ' ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; ' Keith S. Murray ' ; Department of Chemistry Monash University Clayton Victoria Australia 3168 ; ' Boujemaa Moubaraki ' ; Department of Chemistry Monash University Clayton Victoria Australia 3168 ; 'Gary D. Fallon ' ; Department of Chemistry Monash University Clayton Victoria Australia 3168 ; _publ_section_title ; Tetranuclear Copper(II) Complexes Incorporating Short and Long Metal-Metal Separations: Synthesis, Structure and Magnetism. ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014 ; #------------------------------------------------------------------------------ _computing_data_collection 'Philis PW1100 Diffractomter Control' _computing_cell_refinement 'Philis PW1100 Diffractomter Control' _computing_data_reduction 'XPREP' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 14.495(3) _cell_length_b 17.395(2) _cell_length_c 16.334(2) _cell_angle_alpha 90 _cell_angle_beta 100.98(1) _cell_angle_gamma 90 _cell_volume 4043(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 8.5 _cell_measurement_theta_max 10.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'tabular' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_meas '1.72(1)' _chemical_formula_weight 1047.1 _chemical_formula_analytical ? _chemical_formula_sum 'C45 H44 Cu4 N8 O6 ' _chemical_formula_moiety 'C45 H44 Cu4 N8 O6 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2136.00 _exptl_absorpt_coefficient_mu 2.884 _exptl_absorpt_correction_type ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.798 _exptl_absorpt_correction_T_min 0.698 _exptl_special_details ; The scan width was (1.40+0.20tan\q)\% with an \w scan speed of 0.03\% per second. . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Philips PW1100' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 4 _diffrn_standards_decay_% '<1' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 1 1 1 5 2 1 1 5 _diffrn_reflns_number 6515 _reflns_number_total 3011 _reflns_number_gt 2287 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.180 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 59.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01309 _diffrn_orient_matrix_UB_12 -0.04193 _diffrn_orient_matrix_UB_13 -0.03809 _diffrn_orient_matrix_UB_21 -0.03412 _diffrn_orient_matrix_UB_22 0.02957 _diffrn_orient_matrix_UB_23 -0.04905 _diffrn_orient_matrix_UB_31 0.06003 _diffrn_orient_matrix_UB_32 0.02594 _diffrn_orient_matrix_UB_33 -0.00566 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 16 -2.019 0.589 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 180 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 176 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 24 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.20967(4) 0.16136(4) 0.52297(4) 0.0311(2) 1.000 . Uani d ? Cu(2) -0.01809(5) 0.10988(4) 0.45782(4) 0.0335(2) 1.000 . Uani d ? O(1) 0.1128(2) 0.1018(2) 0.4585(2) 0.039(1) 1.000 . Uani d ? O(2) 0.3163(2) 0.2211(2) 0.5755(2) 0.036(1) 1.000 . Uani d ? O(3) -0.1521(2) 0.1163(2) 0.4381(2) 0.043(1) 1.000 . Uani d ? N(1) -0.0248(3) 0.0249(3) 0.3777(2) 0.040(1) 1.000 . Uani d ? N(2) 0.2896(3) 0.0975(2) 0.4650(2) 0.038(1) 1.000 . Uani d ? N(3) 0.1110(2) 0.1958(2) 0.5873(2) 0.027(1) 1.000 . Uani d ? N(4) 0.0171(2) 0.1755(2) 0.5587(2) 0.028(1) 1.000 . Uani d ? C(1) -0.2143(3) 0.0690(3) 0.3954(3) 0.036(1) 1.000 . Uani d ? C(2) -0.3104(4) 0.0824(3) 0.3940(3) 0.044(2) 1.000 . Uani d ? C(3) -0.3787(4) 0.0354(3) 0.3516(4) 0.051(2) 1.000 . Uani d ? C(4) -0.3562(4) -0.0279(3) 0.3079(4) 0.054(2) 1.000 . Uani d ? C(5) -0.2649(4) -0.0429(3) 0.3087(3) 0.047(2) 1.000 . Uani d ? C(6) -0.1920(3) 0.0040(3) 0.3513(3) 0.036(1) 1.000 . Uani d ? C(7) -0.0971(4) -0.0153(3) 0.3460(3) 0.041(2) 1.000 . Uani d ? C(8) 0.0682(4) 0.0013(4) 0.3654(4) 0.066(2) 1.000 . Uani d ? C(9) 0.1381(4) 0.0543(5) 0.3987(5) 0.094(3) 1.000 . Uani d ? C(10) 0.2373(4) 0.0430(3) 0.4071(4) 0.054(2) 1.000 . Uani d ? C(11) 0.3792(4) 0.0971(3) 0.4787(3) 0.044(2) 1.000 . Uani d ? C(12) 0.4397(3) 0.1442(3) 0.5363(3) 0.039(1) 1.000 . Uani d ? C(13) 0.5378(4) 0.1316(4) 0.5476(4) 0.055(2) 1.000 . Uani d ? C(14) 0.5992(4) 0.1738(4) 0.6021(4) 0.067(2) 1.000 . Uani d ? C(15) 0.5665(4) 0.2294(4) 0.6490(4) 0.059(2) 1.000 . Uani d ? C(16) 0.4722(3) 0.2444(3) 0.6400(3) 0.044(2) 1.000 . Uani d ? C(17) 0.4059(3) 0.2023(3) 0.5835(3) 0.036(1) 1.000 . Uani d ? C(18) -0.1370(3) 0.1981(3) 0.6024(3) 0.043(2) 1.000 . Uani d ? C(19) -0.0326(3) 0.2044(3) 0.6139(3) 0.028(1) 1.000 . Uani d ? C(20) 0.0267(3) 0.2426(3) 0.6789(3) 0.025(1) 1.000 . Uani d ? C(21) 0.1160(3) 0.2358(3) 0.6583(3) 0.026(1) 1.000 . Uani d ? C(22) 0.2059(3) 0.2689(3) 0.7044(3) 0.039(1) 1.000 . Uani d ? C(23) 0.0000 0.2863(4) 0.7500 0.026(2) 1.000 ST Uani d ? H(1) -0.3282 0.1253 0.4234 0.052 1.000 . Uiso c ? H(2) -0.4429 0.0465 0.3514 0.062 1.000 . Uiso c ? H(3) -0.4044 -0.0602 0.2788 0.066 1.000 . Uiso c ? H(4) -0.2485 -0.0865 0.2794 0.057 1.000 . Uiso c ? H(5) -0.0868 -0.0607 0.3167 0.048 1.000 . Uiso c ? H(6) 0.0828 -0.0472 0.3916 0.078 1.000 . Uiso c ? H(7) 0.0670 -0.0034 0.3073 0.078 1.000 . Uiso c ? H(9) 0.2545 0.0484 0.3541 0.065 1.000 . Uiso c ? H(10) 0.2524 -0.0074 0.4279 0.065 1.000 . Uiso c ? H(11) 0.4081 0.0619 0.4470 0.053 1.000 . Uiso c ? H(12) 0.5609 0.0925 0.5162 0.067 1.000 . Uiso c ? H(13) 0.6648 0.1651 0.6083 0.080 1.000 . Uiso c ? H(14) 0.6101 0.2580 0.6882 0.070 1.000 . Uiso c ? H(15) 0.4511 0.2836 0.6724 0.052 1.000 . Uiso c ? H(16) -0.1579 0.2217 0.6481 0.051 1.000 . Uiso c ? H(17) -0.1653 0.2228 0.5521 0.051 1.000 . Uiso c ? H(18) -0.1542 0.1453 0.5999 0.051 1.000 . Uiso c ? H(19) 0.2500 0.2287 0.7203 0.047 1.000 . Uiso c ? H(20) 0.2303 0.3043 0.6697 0.047 1.000 . Uiso c ? H(21) 0.1945 0.2946 0.7528 0.047 1.000 . Uiso c ? H(22) 0.0520 0.3178 0.7727 0.031 1.000 . Uiso c ? 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 Cu(1) 0.0198(4) 0.0435(4) 0.0321(4) -0.0019(3) 0.0102(3) -0.0055(3) Cu(2) 0.0254(4) 0.0435(4) 0.0327(4) -0.0053(3) 0.0085(3) -0.0102(3) O(1) 0.026(2) 0.048(2) 0.046(2) -0.003(2) 0.013(2) -0.018(2) O(2) 0.018(2) 0.054(2) 0.036(2) 0.001(2) 0.008(1) -0.005(2) O(3) 0.030(2) 0.050(2) 0.048(2) -0.005(2) 0.006(2) -0.016(2) N(1) 0.035(2) 0.050(3) 0.038(2) -0.007(2) 0.012(2) -0.010(2) N(2) 0.028(2) 0.048(3) 0.040(2) -0.001(2) 0.014(2) -0.006(2) N(3) 0.021(2) 0.035(2) 0.027(2) -0.003(2) 0.007(2) -0.002(2) N(4) 0.019(2) 0.035(2) 0.031(2) -0.004(2) 0.008(2) -0.004(2) C(1) 0.036(3) 0.039(3) 0.031(3) -0.006(2) 0.002(2) 0.004(2) C(2) 0.034(3) 0.048(3) 0.048(3) -0.003(3) 0.004(2) 0.004(3) C(3) 0.029(3) 0.054(4) 0.065(4) -0.004(3) 0.000(3) 0.013(3) C(4) 0.043(4) 0.054(4) 0.060(4) -0.016(3) -0.008(3) -0.001(3) C(5) 0.048(3) 0.050(4) 0.039(3) -0.016(3) -0.002(3) -0.002(3) C(6) 0.034(3) 0.042(3) 0.030(3) -0.007(2) 0.001(2) -0.001(2) C(7) 0.042(3) 0.052(3) 0.027(3) -0.006(3) 0.005(2) -0.004(2) C(8) 0.052(4) 0.078(5) 0.078(5) -0.016(3) 0.037(3) -0.042(4) C(9) 0.026(3) 0.131(7) 0.123(6) 0.003(4) 0.009(4) -0.101(6) C(10) 0.043(3) 0.061(4) 0.065(4) -0.008(3) 0.027(3) -0.026(3) C(11) 0.035(3) 0.053(4) 0.051(3) 0.008(3) 0.021(3) -0.001(3) C(12) 0.022(3) 0.053(3) 0.043(3) 0.005(2) 0.010(2) 0.009(3) C(13) 0.025(3) 0.073(4) 0.071(4) 0.012(3) 0.017(3) 0.001(3) C(14) 0.018(3) 0.106(6) 0.075(4) 0.010(3) 0.006(3) 0.006(4) C(15) 0.027(3) 0.098(5) 0.047(3) -0.004(3) -0.004(3) 0.004(3) C(16) 0.026(3) 0.070(4) 0.035(3) -0.001(3) 0.006(2) 0.002(3) C(17) 0.023(3) 0.055(3) 0.030(3) 0.000(2) 0.008(2) 0.013(2) C(18) 0.023(3) 0.060(4) 0.047(3) -0.005(2) 0.011(2) -0.021(3) C(19) 0.022(2) 0.033(3) 0.029(2) -0.002(2) 0.008(2) -0.001(2) C(20) 0.023(2) 0.028(3) 0.025(2) 0.000(2) 0.009(2) 0.004(2) C(21) 0.023(2) 0.033(3) 0.021(2) -0.004(2) 0.005(2) 0.001(2) C(22) 0.022(3) 0.061(4) 0.036(3) -0.009(2) 0.009(2) -0.007(3) C(23) 0.020(3) 0.028(4) 0.030(3) 0.0000 0.006(3) 0.0000 #------------------------------------------------------------------------------ _refine_special_details ; The hydrogen atom on C(9) was not included in the least-squares calculations because of the apparent large out of plane thermal motion of this atom, probably caused by disorder. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2287 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_number_constraints 61 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_all 0.0655 _refine_ls_wR_factor_ref 0.0478 _refine_ls_goodness_of_fit_all 1.806 _refine_ls_goodness_of_fit_ref 1.536 _refine_ls_shift/su_max 0.0012 _refine_ls_shift/su_mean 0.0757 _refine_diff_density_min -0.42 _refine_diff_density_max 0.46 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Cu(1) O(1) 1.895(3) . . yes Cu(1) O(2) 1.923(3) . . yes Cu(1) N(2) 1.972(4) . . yes Cu(1) N(3) 2.020(4) . . yes Cu(2) O(1) 1.901(3) . . yes Cu(2) O(3) 1.910(3) . . yes Cu(2) N(1) 1.964(4) . . yes Cu(2) N(4) 1.989(4) . . yes O(1) C(9) 1.380(6) . . yes O(2) C(17) 1.322(5) . . yes O(3) C(1) 1.318(5) . . yes N(1) C(7) 1.284(6) . . yes N(1) C(8) 1.460(7) . . yes N(2) C(10) 1.448(6) . . yes N(2) C(11) 1.275(6) . . yes N(3) N(4) 1.397(5) . . yes N(3) C(21) 1.342(5) . . yes N(4) C(19) 1.354(5) . . yes C(1) C(2) 1.408(7) . . yes C(1) C(6) 1.413(7) . . yes C(2) C(3) 1.365(7) . . yes C(2) H(1) 0.95 . . no C(3) C(4) 1.385(8) . . yes C(3) H(2) 0.95 . . no C(4) C(5) 1.348(8) . . yes C(4) H(3) 0.95 . . no C(5) C(6) 1.408(7) . . yes C(5) H(4) 0.95 . . no C(6) C(7) 1.434(7) . . yes C(7) H(5) 0.95 . . no C(8) C(9) 1.400(8) . . yes C(8) H(6) 0.95 . . no C(8) H(7) 0.95 . . no C(9) C(10) 1.432(7) . . yes C(10) H(9) 0.95 . . no C(10) H(10) 0.95 . . no C(11) C(12) 1.418(7) . . yes C(11) H(11) 0.95 . . no C(12) C(13) 1.416(7) . . yes C(12) C(17) 1.414(7) . . yes C(13) C(14) 1.349(8) . . yes C(13) H(12) 0.95 . . no C(14) C(15) 1.372(9) . . yes C(14) H(13) 0.95 . . no C(15) C(16) 1.373(7) . . yes C(15) H(14) 0.95 . . no C(16) C(17) 1.404(7) . . yes C(16) H(15) 0.95 . . no C(18) C(19) 1.493(6) . . yes C(18) H(16) 0.95 . . no C(18) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(19) C(20) 1.399(6) . . yes C(20) C(21) 1.403(6) . . yes C(20) C(23) 1.499(5) . . yes C(21) C(22) 1.490(6) . . yes C(22) H(19) 0.95 . . no C(22) H(20) 0.95 . . no C(22) H(21) 0.95 . . no C(23) H(22) 0.95 . . no C(23) H(22) 0.95 . 2_556 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 O(1) Cu(1) O(2) 172.2(1) . . . yes O(1) Cu(1) N(2) 82.3(1) . . . yes O(1) Cu(1) N(3) 85.9(1) . . . yes O(2) Cu(1) N(2) 91.3(1) . . . yes O(2) Cu(1) N(3) 101.3(1) . . . yes N(2) Cu(1) N(3) 162.9(2) . . . yes O(1) Cu(2) O(3) 170.7(1) . . . yes O(1) Cu(2) N(1) 82.6(2) . . . yes O(1) Cu(2) N(4) 86.5(1) . . . yes O(3) Cu(2) N(1) 90.6(2) . . . yes O(3) Cu(2) N(4) 101.5(1) . . . yes N(1) Cu(2) N(4) 162.9(2) . . . yes Cu(1) O(1) Cu(2) 126.5(2) . . . yes Cu(1) O(1) C(9) 116.9(3) . . . yes Cu(2) O(1) C(9) 116.0(3) . . . yes Cu(1) O(2) C(17) 127.0(3) . . . yes Cu(2) O(3) C(1) 128.7(3) . . . yes Cu(2) N(1) C(7) 127.8(4) . . . yes Cu(2) N(1) C(8) 111.9(3) . . . yes C(7) N(1) C(8) 119.6(5) . . . yes Cu(1) N(2) C(10) 113.6(3) . . . yes Cu(1) N(2) C(11) 126.2(4) . . . yes C(10) N(2) C(11) 120.0(4) . . . yes Cu(1) N(3) N(4) 119.5(3) . . . yes Cu(1) N(3) C(21) 132.5(3) . . . yes N(4) N(3) C(21) 108.0(3) . . . yes Cu(2) N(4) N(3) 120.1(3) . . . yes Cu(2) N(4) C(19) 132.8(3) . . . yes N(3) N(4) C(19) 106.9(3) . . . yes O(3) C(1) C(2) 118.8(5) . . . yes O(3) C(1) C(6) 124.7(4) . . . yes C(2) C(1) C(6) 116.5(5) . . . yes C(1) C(2) C(3) 122.0(5) . . . yes C(1) C(2) H(1) 118.9 . . . no C(3) C(2) H(1) 119.1 . . . no C(2) C(3) C(4) 121.2(5) . . . yes C(2) C(3) H(2) 119.8 . . . no C(4) C(3) H(2) 119.1 . . . no C(3) C(4) C(5) 118.5(5) . . . yes C(3) C(4) H(3) 120.4 . . . no C(5) C(4) H(3) 121.1 . . . no C(4) C(5) C(6) 122.4(6) . . . yes C(4) C(5) H(4) 119.3 . . . no C(6) C(5) H(4) 118.3 . . . no C(1) C(6) C(5) 119.5(5) . . . yes C(1) C(6) C(7) 122.2(4) . . . yes C(5) C(6) C(7) 118.2(5) . . . yes N(1) C(7) C(6) 124.5(5) . . . yes N(1) C(7) H(5) 117.6 . . . no C(6) C(7) H(5) 117.9 . . . no N(1) C(8) C(9) 112.3(5) . . . yes N(1) C(8) H(6) 108.7 . . . no N(1) C(8) H(7) 108.7 . . . no C(9) C(8) H(6) 109.0 . . . no C(9) C(8) H(7) 108.5 . . . no H(6) C(8) H(7) 109.5 . . . no O(1) C(9) C(8) 113.5(5) . . . yes O(1) C(9) C(10) 114.2(5) . . . yes C(8) C(9) C(10) 125.9(6) . . . yes N(2) C(10) C(9) 111.4(4) . . . yes N(2) C(10) H(9) 109.5 . . . no N(2) C(10) H(10) 108.4 . . . no C(9) C(10) H(9) 109.4 . . . no C(9) C(10) H(10) 108.7 . . . no H(9) C(10) H(10) 109.5 . . . no N(2) C(11) C(12) 126.4(5) . . . yes N(2) C(11) H(11) 116.7 . . . no C(12) C(11) H(11) 116.9 . . . no C(11) C(12) C(13) 118.4(5) . . . yes C(11) C(12) C(17) 122.7(4) . . . yes C(13) C(12) C(17) 118.9(5) . . . yes C(12) C(13) C(14) 121.4(6) . . . yes C(12) C(13) H(12) 119.2 . . . no C(14) C(13) H(12) 119.4 . . . no C(13) C(14) C(15) 119.8(5) . . . yes C(13) C(14) H(13) 120.3 . . . no C(15) C(14) H(13) 119.8 . . . no C(14) C(15) C(16) 121.1(6) . . . yes C(14) C(15) H(14) 119.4 . . . no C(16) C(15) H(14) 119.5 . . . no C(15) C(16) C(17) 121.0(6) . . . yes C(15) C(16) H(15) 119.8 . . . no C(17) C(16) H(15) 119.3 . . . no O(2) C(17) C(12) 124.0(4) . . . yes O(2) C(17) C(16) 118.2(5) . . . yes C(12) C(17) C(16) 117.8(4) . . . yes C(19) C(18) H(16) 109.6 . . . no C(19) C(18) H(17) 109.6 . . . no C(19) C(18) H(18) 109.2 . . . no H(16) C(18) H(17) 109.5 . . . no H(16) C(18) H(18) 109.5 . . . no H(17) C(18) H(18) 109.5 . . . no N(4) C(19) C(18) 122.9(4) . . . yes N(4) C(19) C(20) 110.7(4) . . . yes C(18) C(19) C(20) 126.3(4) . . . yes C(19) C(20) C(21) 103.9(4) . . . yes C(19) C(20) C(23) 128.0(3) . . . yes C(21) C(20) C(23) 127.9(4) . . . yes N(3) C(21) C(20) 110.5(4) . . . yes N(3) C(21) C(22) 122.4(4) . . . yes C(20) C(21) C(22) 127.1(4) . . . yes C(21) C(22) H(19) 109.4 . . . no C(21) C(22) H(20) 109.8 . . . no C(21) C(22) H(21) 109.3 . . . no H(19) C(22) H(20) 109.5 . . . no H(19) C(22) H(21) 109.5 . . . no H(20) C(22) H(21) 109.5 . . . no C(20) C(23) C(20) 119.1(5) . . 2_556 yes C(20) C(23) H(22) 107.0 . . . no C(20) C(23) H(22) 107.1 . . 2_556 no C(20) C(23) H(22) 107.1 2_556 . . no C(20) C(23) H(22) 107.0 2_556 . 2_556 no H(22) C(23) H(22) 109.4 . . 2_556 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu(1) O(2) 2.585(3) . 7_556 no Cu(1) C(17) 3.217(5) . 7_556 no Cu(1) C(5) 3.407(5) . 3_556 no Cu(1) Cu(1) 3.431(1) . 7_556 no Cu(1) C(6) 3.572(5) . 3_556 no Cu(2) C(16) 3.135(5) . 7_556 no Cu(2) C(15) 3.300(6) . 7_556 no Cu(2) N(1) 3.530(4) . 3_556 no O(1) C(16) 3.242(7) . 7_556 no O(1) O(2) 3.328(5) . 7_556 no O(1) C(17) 3.477(6) . 7_556 no O(1) C(7) 3.578(6) . 3_556 no O(2) O(2) 2.997(6) . 7_556 no O(2) N(3) 3.367(5) . 7_556 no O(2) N(2) 3.516(5) . 7_556 no O(3) C(15) 3.382(7) . 7_556 no N(3) C(17) 3.274(6) . 7_556 no N(3) C(7) 3.344(6) . 3_556 no N(3) C(12) 3.434(6) . 7_556 no N(4) C(7) 3.294(7) . 3_556 no N(4) C(17) 3.485(6) . 7_556 no N(4) C(16) 3.562(6) . 7_556 no C(7) C(8) 3.568(8) . 2 no C(16) C(16) 3.53(1) . 2_656 no Cu(1) Cu(2) 3.391(1) . . no Cu(1) Cu(1) 3.431(1) . 7_556 no #------------------------------------------------------------------------------ #---END data_2 #[(Cu2L)2mdpz] #------------------------------------------------------------------------------ _computing_data_collection 'Philips PW1100 Diffractometer Control' _computing_cell_refinement 'Philips PW1100 Diffractometer Control' _computing_data_reduction 'XPREP' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 18.630(2) _cell_length_b 12.459(1) _cell_length_c 9.319(1) _cell_angle_alpha 81.546(8) _cell_angle_beta 86.965(6) _cell_angle_gamma 76.897(8) _cell_volume 2083.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.0 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark aqua' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_meas '1.65(1)' _chemical_formula_weight 1033.05 _chemical_formula_analytical ? _chemical_formula_sum 'C44 H42 Cu4 N8 O6 ' _chemical_formula_moiety 'C44 H42 Cu4 N8 O6 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1052.00 _exptl_absorpt_coefficient_mu 2.790 _exptl_absorpt_correction_type ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_correction_T_min 0.563 _exptl_special_details ; The scan width was (1.40+0.20tan\q)\% with an \w scan speed of 0.05\% per second . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Philips PW1100' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 4 _diffrn_standards_decay_% '<1' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 2 2 0 6 0 0 0 2 _diffrn_reflns_number 6546 _reflns_number_total 6185 _reflns_number_gt 4682 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 59.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03612 _diffrn_orient_matrix_UB_12 -0.03737 _diffrn_orient_matrix_UB_13 0.05905 _diffrn_orient_matrix_UB_21 -0.03343 _diffrn_orient_matrix_UB_22 0.01706 _diffrn_orient_matrix_UB_23 -0.08478 _diffrn_orient_matrix_UB_31 -0.02482 _diffrn_orient_matrix_UB_32 0.07237 _diffrn_orient_matrix_UB_33 0.03316 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 8 -2.019 0.589 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 88 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 84 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 12 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.50113(4) 0.10769(5) 0.33546(8) 0.0398(2) 1.000 . Uani d ? Cu(2) 0.44632(4) -0.06776(5) 0.14345(7) 0.0393(2) 1.000 . Uani d ? Cu(3) 0.05048(4) 0.58465(5) 0.06242(7) 0.0367(2) 1.000 . Uani d ? Cu(4) -0.01513(3) 0.41385(5) 0.32508(7) 0.0371(2) 1.000 . Uani d ? O(1) 0.5164(2) -0.0219(3) 0.2457(4) 0.051(1) 1.000 . Uani d ? O(2) 0.4925(2) 0.2306(3) 0.4356(4) 0.054(1) 1.000 . Uani d ? O(3) 0.3840(2) -0.1185(3) 0.0286(4) 0.054(1) 1.000 . Uani d ? O(4) -0.0181(2) 0.5535(2) 0.2098(4) 0.048(1) 1.000 . Uani d ? O(5) 0.1007(2) 0.6215(3) -0.1145(4) 0.047(1) 1.000 . Uani d ? O(6) -0.0206(2) 0.2809(3) 0.4473(3) 0.046(1) 1.000 . Uani d ? N(1) 0.6025(2) 0.0439(3) 0.3989(4) 0.042(1) 1.000 . Uani d ? N(2) 0.5299(2) -0.1882(3) 0.1122(4) 0.043(1) 1.000 . Uani d ? N(3) 0.3981(2) 0.1446(3) 0.2613(4) 0.037(1) 1.000 . Uani d ? N(4) 0.3741(2) 0.0676(3) 0.1922(4) 0.035(1) 1.000 . Uani d ? N(5) -0.0137(2) 0.7336(3) 0.0466(4) 0.043(1) 1.000 . Uani d ? N(6) -0.1006(2) 0.4991(3) 0.4210(4) 0.045(1) 1.000 . Uani d ? N(7) 0.1135(2) 0.4376(3) 0.1348(4) 0.034(1) 1.000 . Uani d ? N(8) 0.0848(2) 0.3634(3) 0.2350(4) 0.035(1) 1.000 . Uani d ? C(1) 0.5421(3) 0.2543(4) 0.5133(5) 0.045(1) 1.000 . Uani d ? C(2) 0.5236(3) 0.3544(4) 0.5730(6) 0.056(2) 1.000 . Uani d ? C(3) 0.5733(3) 0.3848(5) 0.6555(6) 0.061(2) 1.000 . Uani d ? C(4) 0.6416(3) 0.3187(5) 0.6837(6) 0.062(2) 1.000 . Uani d ? C(5) 0.6615(3) 0.2198(5) 0.6280(6) 0.058(2) 1.000 . Uani d ? C(6) 0.6130(3) 0.1856(4) 0.5423(5) 0.042(1) 1.000 . Uani d ? C(7) 0.6384(3) 0.0835(4) 0.4845(5) 0.046(1) 1.000 . Uani d ? C(8) 0.6352(3) -0.0595(5) 0.3415(7) 0.067(2) 1.000 . Uani d ? C(9) 0.5864(3) -0.0903(6) 0.257(1) 0.115(3) 1.000 . Uani d ? C(10) 0.5970(3) -0.1844(5) 0.1836(6) 0.060(2) 1.000 . Uani d ? C(11) 0.5303(3) -0.2669(4) 0.0367(5) 0.049(2) 1.000 . Uani d ? C(12) 0.4685(3) -0.2825(4) -0.0357(5) 0.044(1) 1.000 . Uani d ? C(13) 0.4784(3) -0.3759(5) -0.1085(6) 0.061(2) 1.000 . Uani d ? C(14) 0.4219(3) -0.3994(5) -0.1764(7) 0.066(2) 1.000 . Uani d ? C(15) 0.3536(3) -0.3272(5) -0.1758(7) 0.066(2) 1.000 . Uani d ? C(16) 0.3416(3) -0.2347(5) -0.1062(6) 0.059(2) 1.000 . Uani d ? C(17) 0.3987(3) -0.2086(4) -0.0344(5) 0.046(1) 1.000 . Uani d ? C(18) 0.3442(3) 0.3315(4) 0.3371(7) 0.060(2) 1.000 . Uani d ? C(19) 0.3408(2) 0.2311(4) 0.2692(5) 0.039(1) 1.000 . Uani d ? C(20) 0.2789(2) 0.2136(4) 0.2075(5) 0.037(1) 1.000 . Uani d ? C(21) 0.3016(2) 0.1099(4) 0.1618(5) 0.036(1) 1.000 . Uani d ? C(22) 0.2556(3) 0.0517(4) 0.0885(6) 0.053(2) 1.000 . Uani d ? C(23) 0.1080(3) 0.7226(4) -0.1686(5) 0.042(1) 1.000 . Uani d ? C(24) 0.1641(3) 0.7331(4) -0.2724(6) 0.053(2) 1.000 . Uani d ? C(25) 0.1746(3) 0.8362(5) -0.3344(7) 0.069(2) 1.000 . Uani d ? C(26) 0.1288(4) 0.9327(5) -0.2962(8) 0.082(2) 1.000 . Uani d ? C(27) 0.0736(4) 0.9248(5) -0.1981(7) 0.068(2) 1.000 . Uani d ? C(28) 0.0612(3) 0.8209(4) -0.1320(6) 0.048(2) 1.000 . Uani d ? C(29) 0.0001(3) 0.8197(4) -0.0330(6) 0.050(2) 1.000 . Uani d ? C(30) -0.0778(3) 0.7401(4) 0.1440(7) 0.066(2) 1.000 . Uani d ? C(31) -0.0748(4) 0.6382(5) 0.2351(8) 0.093(2) 1.000 . Uani d ? C(32) -0.1229(4) 0.6149(5) 0.3518(8) 0.084(2) 1.000 . Uani d ? C(33) -0.1336(3) 0.4657(4) 0.5359(6) 0.048(2) 1.000 . Uani d ? C(34) -0.1199(3) 0.3528(4) 0.6091(5) 0.044(1) 1.000 . Uani d ? C(35) -0.1639(3) 0.3283(5) 0.7319(6) 0.053(2) 1.000 . Uani d ? C(36) -0.1584(3) 0.2237(6) 0.8008(6) 0.063(2) 1.000 . Uani d ? C(37) -0.1080(3) 0.1374(5) 0.7464(6) 0.063(2) 1.000 . Uani d ? C(38) -0.0630(3) 0.1579(4) 0.6289(6) 0.055(2) 1.000 . Uani d ? C(39) -0.0665(3) 0.2661(4) 0.5569(5) 0.042(1) 1.000 . Uani d ? C(40) 0.2345(3) 0.4489(4) 0.0105(6) 0.049(1) 1.000 . Uani d ? C(41) 0.1856(2) 0.3927(3) 0.1129(5) 0.033(1) 1.000 . Uani d ? C(42) 0.2055(2) 0.2885(3) 0.1962(5) 0.035(1) 1.000 . Uani d ? C(43) 0.1410(2) 0.2731(3) 0.2699(5) 0.037(1) 1.000 . Uani d ? C(44) 0.1320(3) 0.1740(4) 0.3741(6) 0.053(2) 1.000 . Uani d ? H(1) 0.4761 0.4022 0.5564 0.067 1.000 . Uiso c ? H(2) 0.5591 0.4536 0.6933 0.073 1.000 . Uiso c ? H(3) 0.6748 0.3409 0.7418 0.075 1.000 . Uiso c ? H(4) 0.7089 0.1734 0.6476 0.069 1.000 . Uiso c ? H(5) 0.6859 0.0406 0.5116 0.056 1.000 . Uiso c ? H(6) 0.6780 -0.0488 0.2851 0.080 1.000 . Uiso c ? H(7) 0.6502 -0.1162 0.4217 0.080 1.000 . Uiso c ? H(9) 0.6103 -0.2509 0.2520 0.071 1.000 . Uiso c ? H(10) 0.6355 -0.1829 0.1130 0.071 1.000 . Uiso c ? H(11) 0.5759 -0.3187 0.0288 0.058 1.000 . Uiso c ? H(12) 0.5257 -0.4242 -0.1100 0.074 1.000 . Uiso c ? H(13) 0.4293 -0.4637 -0.2245 0.079 1.000 . Uiso c ? H(14) 0.3139 -0.3420 -0.2237 0.079 1.000 . Uiso c ? H(15) 0.2936 -0.1872 -0.1069 0.071 1.000 . Uiso c ? H(16) 0.3571 0.3095 0.4365 0.072 1.000 . Uiso c ? H(17) 0.3799 0.3675 0.2878 0.072 1.000 . Uiso c ? H(18) 0.2972 0.3818 0.3320 0.072 1.000 . Uiso c ? H(19) 0.2069 0.0960 0.0788 0.064 1.000 . Uiso c ? H(20) 0.2761 0.0392 -0.0042 0.064 1.000 . Uiso c ? H(21) 0.2540 -0.0179 0.1457 0.064 1.000 . Uiso c ? H(22) 0.1957 0.6677 -0.3004 0.064 1.000 . Uiso c ? H(23) 0.2138 0.8407 -0.4036 0.083 1.000 . Uiso c ? H(24) 0.1366 1.0033 -0.3388 0.099 1.000 . Uiso c ? H(25) 0.0421 0.9911 -0.1725 0.082 1.000 . Uiso c ? H(26) -0.0334 0.8890 -0.0249 0.060 1.000 . Uiso c ? H(27) -0.0791 0.7981 0.2011 0.079 1.000 . Uiso c ? H(28) -0.1210 0.7581 0.0871 0.079 1.000 . Uiso c ? H(30) -0.1719 0.6265 0.3179 0.100 1.000 . Uiso c ? H(31) -0.1229 0.6625 0.4232 0.100 1.000 . Uiso c ? H(32) -0.1700 0.5196 0.5772 0.058 1.000 . Uiso c ? H(33) -0.1985 0.3874 0.7676 0.063 1.000 . Uiso c ? H(34) -0.1882 0.2090 0.8842 0.075 1.000 . Uiso c ? H(35) -0.1046 0.0628 0.7916 0.075 1.000 . Uiso c ? H(36) -0.0284 0.0978 0.5959 0.065 1.000 . Uiso c ? H(37) 0.2828 0.4031 0.0114 0.058 1.000 . Uiso c ? H(38) 0.2157 0.4609 -0.0850 0.058 1.000 . Uiso c ? H(39) 0.2359 0.5182 0.0394 0.058 1.000 . Uiso c ? H(40) 0.1164 0.1960 0.4660 0.065 1.000 . Uiso c ? H(41) 0.0961 0.1412 0.3392 0.065 1.000 . Uiso c ? H(42) 0.1778 0.1213 0.3830 0.065 1.000 . Uiso c ? 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 Cu(1) 0.0285(4) 0.0396(4) 0.0477(4) -0.0008(3) -0.0037(3) -0.0043(3) Cu(2) 0.0301(4) 0.0368(4) 0.0458(4) 0.0026(3) 0.0005(3) -0.0052(3) Cu(3) 0.0320(4) 0.0291(4) 0.0455(4) -0.0009(3) -0.0025(3) -0.0021(3) Cu(4) 0.0298(4) 0.0328(4) 0.0459(4) -0.0019(3) 0.0040(3) -0.0058(3) O(1) 0.030(2) 0.047(2) 0.072(2) 0.007(2) -0.007(2) -0.021(2) O(2) 0.038(2) 0.051(2) 0.074(3) 0.002(2) -0.018(2) -0.024(2) O(3) 0.039(2) 0.050(2) 0.070(2) 0.007(2) -0.008(2) -0.021(2) O(4) 0.034(2) 0.032(2) 0.068(2) 0.003(1) 0.010(2) 0.002(2) O(5) 0.051(2) 0.036(2) 0.051(2) -0.006(2) 0.005(2) 0.000(2) O(6) 0.041(2) 0.043(2) 0.047(2) -0.002(2) 0.006(2) 0.002(2) N(1) 0.033(2) 0.045(2) 0.044(2) 0.001(2) 0.000(2) -0.005(2) N(2) 0.035(2) 0.048(2) 0.040(2) 0.002(2) 0.000(2) -0.007(2) N(3) 0.029(2) 0.035(2) 0.045(2) -0.001(2) -0.003(2) -0.006(2) N(4) 0.027(2) 0.031(2) 0.042(2) 0.002(2) 0.000(2) -0.002(2) N(5) 0.041(2) 0.035(2) 0.048(2) -0.001(2) -0.006(2) -0.002(2) N(6) 0.038(2) 0.042(2) 0.050(3) -0.001(2) 0.006(2) -0.010(2) N(7) 0.028(2) 0.032(2) 0.038(2) -0.003(2) 0.002(2) -0.003(2) N(8) 0.028(2) 0.034(2) 0.042(2) -0.003(2) 0.001(2) -0.005(2) C(1) 0.046(3) 0.045(3) 0.042(3) -0.010(2) 0.004(2) -0.001(2) C(2) 0.047(3) 0.053(3) 0.067(4) -0.006(3) -0.008(3) -0.016(3) C(3) 0.065(4) 0.056(3) 0.068(4) -0.018(3) 0.003(3) -0.022(3) C(4) 0.054(4) 0.076(4) 0.065(4) -0.020(3) -0.012(3) -0.020(3) C(5) 0.046(3) 0.074(4) 0.054(3) -0.013(3) -0.012(3) -0.007(3) C(6) 0.036(3) 0.051(3) 0.038(3) -0.010(2) -0.004(2) 0.001(2) C(7) 0.032(3) 0.058(3) 0.043(3) -0.003(2) -0.003(2) 0.005(3) C(8) 0.044(3) 0.075(4) 0.077(4) 0.013(3) -0.011(3) -0.028(3) C(9) 0.043(4) 0.101(5) 0.209(9) 0.038(3) -0.056(5) -0.112(6) C(10) 0.035(3) 0.073(4) 0.067(4) 0.010(3) -0.011(3) -0.024(3) C(11) 0.042(3) 0.054(3) 0.041(3) 0.007(2) 0.005(2) -0.007(3) C(12) 0.042(3) 0.045(3) 0.041(3) -0.002(2) 0.002(2) -0.010(2) C(13) 0.061(4) 0.060(4) 0.057(4) 0.002(3) 0.000(3) -0.018(3) C(14) 0.066(4) 0.060(4) 0.076(4) -0.007(3) -0.004(3) -0.033(3) C(15) 0.061(4) 0.062(4) 0.079(4) -0.016(3) -0.008(3) -0.021(3) C(16) 0.048(3) 0.056(3) 0.071(4) -0.001(3) -0.008(3) -0.012(3) C(17) 0.047(3) 0.051(3) 0.038(3) -0.009(2) 0.001(2) -0.004(2) C(18) 0.044(3) 0.050(3) 0.084(4) 0.006(3) -0.016(3) -0.025(3) C(19) 0.033(3) 0.032(2) 0.045(3) 0.003(2) -0.002(2) -0.003(2) C(20) 0.031(2) 0.034(2) 0.042(3) -0.003(2) -0.002(2) -0.001(2) C(21) 0.026(2) 0.034(2) 0.045(3) 0.000(2) 0.000(2) -0.001(2) C(22) 0.030(3) 0.047(3) 0.080(4) 0.003(2) -0.006(3) -0.019(3) C(23) 0.043(3) 0.046(3) 0.036(3) -0.012(2) -0.015(2) 0.004(2) C(24) 0.046(3) 0.057(3) 0.055(3) -0.012(3) -0.009(3) 0.002(3) C(25) 0.060(4) 0.076(4) 0.069(4) -0.024(3) 0.001(3) 0.011(3) C(26) 0.100(6) 0.064(4) 0.081(5) -0.034(4) -0.003(4) 0.019(4) C(27) 0.084(5) 0.043(3) 0.070(4) -0.005(3) -0.003(4) 0.007(3) C(28) 0.053(3) 0.037(3) 0.050(3) -0.007(2) -0.011(3) 0.005(2) C(29) 0.059(3) 0.034(3) 0.051(3) 0.001(2) -0.017(3) 0.003(2) C(30) 0.050(3) 0.042(3) 0.090(5) 0.011(3) 0.016(3) 0.002(3) C(31) 0.079(5) 0.049(4) 0.110(6) 0.033(3) 0.064(4) 0.025(4) C(32) 0.077(5) 0.046(3) 0.106(5) 0.017(3) 0.029(4) 0.004(3) C(33) 0.033(3) 0.057(3) 0.056(3) -0.005(2) 0.006(2) -0.022(3) C(34) 0.034(3) 0.058(3) 0.043(3) -0.014(2) -0.002(2) -0.012(3) C(35) 0.040(3) 0.078(4) 0.042(3) -0.018(3) 0.008(2) -0.012(3) C(36) 0.046(3) 0.097(5) 0.046(3) -0.025(3) 0.004(3) 0.000(3) C(37) 0.055(4) 0.074(4) 0.058(4) -0.026(3) -0.008(3) 0.014(3) C(38) 0.045(3) 0.056(3) 0.059(4) -0.008(3) 0.003(3) 0.002(3) C(39) 0.033(3) 0.053(3) 0.041(3) -0.010(2) -0.006(2) -0.007(2) C(40) 0.035(3) 0.048(3) 0.057(3) -0.001(2) 0.004(2) 0.000(3) C(41) 0.026(2) 0.033(2) 0.038(3) -0.002(2) 0.001(2) -0.008(2) C(42) 0.027(2) 0.032(2) 0.042(3) 0.001(2) -0.001(2) -0.007(2) C(43) 0.035(3) 0.031(2) 0.043(3) -0.003(2) -0.004(2) -0.006(2) C(44) 0.043(3) 0.030(3) 0.076(4) 0.004(2) 0.008(3) 0.004(3) #------------------------------------------------------------------------------ _refine_special_details ; The hydrogen atoms on C(9) and C(31) were not included in the least-squares calculations because of the apparent large out of plane thermal motion of these atoms, probably caused by disorder. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4682 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_all 0.0641 _refine_ls_wR_factor_ref 0.0492 _refine_ls_goodness_of_fit_all 1.761 _refine_ls_goodness_of_fit_ref 1.578 _refine_ls_shift/su_max 0.0028 _refine_ls_shift/su_mean 0.0785 _refine_diff_density_min -0.50 _refine_diff_density_max 0.41 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Cu(1) O(1) 1.884(3) . . yes Cu(1) O(2) 1.880(3) . . yes Cu(1) N(1) 1.961(4) . . yes Cu(1) N(3) 2.005(4) . . yes Cu(2) O(1) 1.889(3) . . yes Cu(2) O(3) 1.886(3) . . yes Cu(2) N(2) 1.945(4) . . yes Cu(2) N(4) 1.998(3) . . yes Cu(3) O(4) 1.884(3) . . yes Cu(3) O(5) 1.901(3) . . yes Cu(3) N(5) 1.957(4) . . yes Cu(3) N(7) 1.985(3) . . yes Cu(4) O(4) 1.897(3) . . yes Cu(4) O(6) 1.886(3) . . yes Cu(4) N(6) 1.954(4) . . yes Cu(4) N(8) 2.006(4) . . yes O(1) C(9) 1.388(6) . . yes O(2) C(1) 1.312(6) . . yes O(3) C(17) 1.310(6) . . yes O(4) C(31) 1.353(6) . . yes O(5) C(23) 1.320(5) . . yes O(6) C(39) 1.316(5) . . yes N(1) C(7) 1.285(6) . . yes N(1) C(8) 1.459(6) . . yes N(2) C(10) 1.459(6) . . yes N(2) C(11) 1.287(6) . . yes N(3) N(4) 1.394(5) . . yes N(3) C(19) 1.342(5) . . yes N(4) C(21) 1.362(5) . . yes N(5) C(29) 1.280(6) . . yes N(5) C(30) 1.456(6) . . yes N(6) C(32) 1.467(7) . . yes N(6) C(33) 1.270(6) . . yes N(7) N(8) 1.389(5) . . yes N(7) C(41) 1.350(5) . . yes N(8) C(43) 1.365(5) . . yes C(1) C(2) 1.406(7) . . yes C(1) C(6) 1.418(7) . . yes C(2) C(3) 1.381(7) . . yes C(2) H(1) 0.95 . . no C(3) C(4) 1.366(8) . . yes C(3) H(2) 0.95 . . no C(4) C(5) 1.374(7) . . yes C(4) H(3) 0.95 . . no C(5) C(6) 1.408(7) . . yes C(5) H(4) 0.95 . . no C(6) C(7) 1.427(7) . . yes C(7) H(5) 0.95 . . no C(8) C(9) 1.385(8) . . yes C(8) H(6) 0.96 . . no C(8) H(7) 0.96 . . no C(9) C(10) 1.412(8) . . yes C(10) H(9) 0.96 . . no C(10) H(10) 0.95 . . no C(11) C(12) 1.428(7) . . yes C(11) H(11) 0.95 . . no C(12) C(13) 1.403(7) . . yes C(12) C(17) 1.414(7) . . yes C(13) C(14) 1.363(8) . . yes C(13) H(12) 0.95 . . no C(14) C(15) 1.383(8) . . yes C(14) H(13) 0.95 . . no C(15) C(16) 1.374(7) . . yes C(15) H(14) 0.95 . . no C(16) C(17) 1.408(7) . . yes C(16) H(15) 0.95 . . no C(18) C(19) 1.497(7) . . yes C(18) H(16) 0.95 . . no C(18) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(19) C(20) 1.390(6) . . yes C(20) C(21) 1.387(6) . . yes C(20) C(42) 1.469(6) . . yes C(21) C(22) 1.490(7) . . yes C(22) H(19) 0.95 . . no C(22) H(20) 0.95 . . no C(22) H(21) 0.95 . . no C(23) C(24) 1.401(7) . . yes C(23) C(28) 1.408(7) . . yes C(24) C(25) 1.381(7) . . yes C(24) H(22) 0.95 . . no C(25) C(26) 1.389(9) . . yes C(25) H(23) 0.95 . . no C(26) C(27) 1.351(9) . . yes C(26) H(24) 0.95 . . no C(27) C(28) 1.411(7) . . yes C(27) H(25) 0.95 . . no C(28) C(29) 1.429(7) . . yes C(29) H(26) 0.95 . . no C(30) C(31) 1.411(7) . . yes C(30) H(27) 0.95 . . no C(30) H(28) 0.95 . . no C(31) C(32) 1.411(8) . . yes C(32) H(30) 0.95 . . no C(32) H(31) 0.95 . . no C(33) C(34) 1.443(7) . . yes C(33) H(32) 0.95 . . no C(34) C(35) 1.409(7) . . yes C(34) C(39) 1.418(7) . . yes C(35) C(36) 1.349(8) . . yes C(35) H(33) 0.95 . . no C(36) C(37) 1.395(8) . . yes C(36) H(34) 0.95 . . no C(37) C(38) 1.373(7) . . yes C(37) H(35) 0.95 . . no C(38) C(39) 1.404(7) . . yes C(38) H(36) 0.95 . . no C(40) C(41) 1.494(6) . . yes C(40) H(37) 0.95 . . no C(40) H(38) 0.95 . . no C(40) H(39) 0.95 . . no C(41) C(42) 1.394(6) . . yes C(42) C(43) 1.390(6) . . yes C(43) C(44) 1.490(6) . . yes C(44) H(40) 0.95 . . no C(44) H(41) 0.95 . . no C(44) H(42) 0.95 . . 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 O(1) Cu(1) O(2) 175.1(1) . . . yes O(1) Cu(1) N(1) 82.8(1) . . . yes O(1) Cu(1) N(3) 86.9(1) . . . yes O(2) Cu(1) N(1) 92.7(2) . . . yes O(2) Cu(1) N(3) 97.6(1) . . . yes N(1) Cu(1) N(3) 169.3(2) . . . yes O(1) Cu(2) O(3) 174.3(1) . . . yes O(1) Cu(2) N(2) 82.5(2) . . . yes O(1) Cu(2) N(4) 86.9(1) . . . yes O(3) Cu(2) N(2) 92.8(2) . . . yes O(3) Cu(2) N(4) 97.7(1) . . . yes N(2) Cu(2) N(4) 169.4(2) . . . yes O(4) Cu(3) O(5) 166.8(1) . . . yes O(4) Cu(3) N(5) 82.6(1) . . . yes O(4) Cu(3) N(7) 87.0(1) . . . yes O(5) Cu(3) N(5) 91.8(1) . . . yes O(5) Cu(3) N(7) 100.7(1) . . . yes N(5) Cu(3) N(7) 164.5(2) . . . yes O(4) Cu(4) O(6) 174.8(1) . . . yes O(4) Cu(4) N(6) 82.5(1) . . . yes O(4) Cu(4) N(8) 86.5(1) . . . yes O(6) Cu(4) N(6) 92.3(2) . . . yes O(6) Cu(4) N(8) 98.7(1) . . . yes N(6) Cu(4) N(8) 163.5(2) . . . yes Cu(1) O(1) Cu(2) 126.8(2) . . . yes Cu(1) O(1) C(9) 116.2(3) . . . yes Cu(2) O(1) C(9) 117.1(3) . . . yes Cu(1) O(2) C(1) 128.4(3) . . . yes Cu(2) O(3) C(17) 128.3(3) . . . yes Cu(3) O(4) Cu(4) 126.0(2) . . . yes Cu(3) O(4) C(31) 117.0(3) . . . yes Cu(4) O(4) C(31) 117.0(3) . . . yes Cu(3) O(5) C(23) 125.1(3) . . . yes Cu(4) O(6) C(39) 128.5(3) . . . yes Cu(1) N(1) C(7) 126.1(3) . . . yes Cu(1) N(1) C(8) 112.9(3) . . . yes C(7) N(1) C(8) 120.9(4) . . . yes Cu(2) N(2) C(10) 114.1(3) . . . yes Cu(2) N(2) C(11) 126.2(3) . . . yes C(10) N(2) C(11) 119.7(4) . . . yes Cu(1) N(3) N(4) 119.3(3) . . . yes Cu(1) N(3) C(19) 133.2(3) . . . yes N(4) N(3) C(19) 107.4(3) . . . yes Cu(2) N(4) N(3) 119.6(3) . . . yes Cu(2) N(4) C(21) 132.9(3) . . . yes N(3) N(4) C(21) 107.2(3) . . . yes Cu(3) N(5) C(29) 124.8(4) . . . yes Cu(3) N(5) C(30) 113.1(3) . . . yes C(29) N(5) C(30) 121.9(4) . . . yes Cu(4) N(6) C(32) 113.0(3) . . . yes Cu(4) N(6) C(33) 126.9(4) . . . yes C(32) N(6) C(33) 120.0(4) . . . yes Cu(3) N(7) N(8) 119.7(3) . . . yes Cu(3) N(7) C(41) 132.0(3) . . . yes N(8) N(7) C(41) 108.2(3) . . . yes Cu(4) N(8) N(7) 119.5(3) . . . yes Cu(4) N(8) C(43) 132.6(3) . . . yes N(7) N(8) C(43) 106.6(3) . . . yes O(2) C(1) C(2) 117.9(5) . . . yes O(2) C(1) C(6) 124.7(5) . . . yes C(2) C(1) C(6) 117.4(5) . . . yes C(1) C(2) C(3) 121.0(5) . . . yes C(1) C(2) H(1) 119.5 . . . no C(3) C(2) H(1) 119.5 . . . no C(2) C(3) C(4) 121.7(5) . . . yes C(2) C(3) H(2) 118.7 . . . no C(4) C(3) H(2) 119.6 . . . no C(3) C(4) C(5) 119.0(5) . . . yes C(3) C(4) H(3) 120.3 . . . no C(5) C(4) H(3) 120.7 . . . no C(4) C(5) C(6) 121.4(5) . . . yes C(4) C(5) H(4) 119.3 . . . no C(6) C(5) H(4) 119.3 . . . no C(1) C(6) C(5) 119.5(5) . . . yes C(1) C(6) C(7) 122.3(4) . . . yes C(5) C(6) C(7) 118.2(5) . . . yes N(1) C(7) C(6) 125.7(4) . . . yes N(1) C(7) H(5) 116.9 . . . no C(6) C(7) H(5) 117.5 . . . no N(1) C(8) C(9) 111.9(4) . . . yes N(1) C(8) H(6) 108.0 . . . no N(1) C(8) H(7) 108.0 . . . no C(9) C(8) H(6) 109.9 . . . no C(9) C(8) H(7) 110.3 . . . no H(6) C(8) H(7) 108.5 . . . no O(1) C(9) C(8) 116.0(5) . . . yes O(1) C(9) C(10) 114.8(5) . . . yes C(8) C(9) C(10) 129.1(5) . . . yes N(2) C(10) C(9) 111.4(4) . . . yes N(2) C(10) H(9) 108.3 . . . no N(2) C(10) H(10) 109.0 . . . no C(9) C(10) H(9) 109.5 . . . no C(9) C(10) H(10) 109.9 . . . no H(9) C(10) H(10) 108.7 . . . no N(2) C(11) C(12) 125.7(4) . . . yes N(2) C(11) H(11) 116.6 . . . no C(12) C(11) H(11) 117.7 . . . no C(11) C(12) C(13) 117.9(5) . . . yes C(11) C(12) C(17) 122.4(4) . . . yes C(13) C(12) C(17) 119.7(5) . . . yes C(12) C(13) C(14) 121.9(5) . . . yes C(12) C(13) H(12) 119.0 . . . no C(14) C(13) H(12) 119.1 . . . no C(13) C(14) C(15) 118.5(5) . . . yes C(13) C(14) H(13) 121.1 . . . no C(15) C(14) H(13) 120.4 . . . no C(14) C(15) C(16) 121.4(5) . . . yes C(14) C(15) H(14) 119.5 . . . no C(16) C(15) H(14) 119.1 . . . no C(15) C(16) C(17) 121.3(5) . . . yes C(15) C(16) H(15) 119.3 . . . no C(17) C(16) H(15) 119.4 . . . no O(3) C(17) C(12) 124.5(5) . . . yes O(3) C(17) C(16) 118.5(5) . . . yes C(12) C(17) C(16) 117.0(5) . . . yes C(19) C(18) H(16) 109.6 . . . no C(19) C(18) H(17) 109.9 . . . no C(19) C(18) H(18) 109.7 . . . no H(16) C(18) H(17) 109.3 . . . no H(16) C(18) H(18) 108.9 . . . no H(17) C(18) H(18) 109.4 . . . no N(3) C(19) C(18) 123.9(4) . . . yes N(3) C(19) C(20) 110.7(4) . . . yes C(18) C(19) C(20) 125.4(4) . . . yes C(19) C(20) C(21) 104.8(4) . . . yes C(19) C(20) C(42) 127.1(4) . . . yes C(21) C(20) C(42) 128.2(4) . . . yes N(4) C(21) C(20) 109.9(4) . . . yes N(4) C(21) C(22) 123.7(4) . . . yes C(20) C(21) C(22) 126.4(4) . . . yes C(21) C(22) H(19) 109.4 . . . no C(21) C(22) H(20) 109.7 . . . no C(21) C(22) H(21) 109.3 . . . no H(19) C(22) H(20) 109.8 . . . no H(19) C(22) H(21) 109.1 . . . no H(20) C(22) H(21) 109.5 . . . no O(5) C(23) C(24) 118.2(5) . . . yes O(5) C(23) C(28) 124.0(4) . . . yes C(24) C(23) C(28) 117.8(5) . . . yes C(23) C(24) C(25) 121.3(5) . . . yes C(23) C(24) H(22) 119.3 . . . no C(25) C(24) H(22) 119.4 . . . no C(24) C(25) C(26) 120.5(6) . . . yes C(24) C(25) H(23) 119.4 . . . no C(26) C(25) H(23) 120.1 . . . no C(25) C(26) C(27) 119.3(6) . . . yes C(25) C(26) H(24) 120.0 . . . no C(27) C(26) H(24) 120.7 . . . no C(26) C(27) C(28) 121.9(6) . . . yes C(26) C(27) H(25) 119.1 . . . no C(28) C(27) H(25) 119.0 . . . no C(23) C(28) C(27) 119.2(5) . . . yes C(23) C(28) C(29) 122.4(4) . . . yes C(27) C(28) C(29) 118.4(5) . . . yes N(5) C(29) C(28) 125.7(5) . . . yes N(5) C(29) H(26) 116.9 . . . no C(28) C(29) H(26) 117.5 . . . no N(5) C(30) C(31) 111.0(4) . . . yes N(5) C(30) H(27) 108.6 . . . no N(5) C(30) H(28) 108.6 . . . no C(31) C(30) H(27) 109.9 . . . no C(31) C(30) H(28) 109.8 . . . no H(27) C(30) H(28) 108.9 . . . no O(4) C(31) C(30) 116.1(5) . . . yes O(4) C(31) C(32) 116.1(5) . . . yes C(30) C(31) C(32) 127.8(5) . . . yes N(6) C(32) C(31) 111.2(5) . . . yes N(6) C(32) H(30) 108.2 . . . no N(6) C(32) H(31) 108.4 . . . no C(31) C(32) H(30) 110.0 . . . no C(31) C(32) H(31) 110.2 . . . no H(30) C(32) H(31) 108.7 . . . no N(6) C(33) C(34) 125.3(5) . . . yes N(6) C(33) H(32) 117.3 . . . no C(34) C(33) H(32) 117.4 . . . no C(33) C(34) C(35) 118.3(5) . . . yes C(33) C(34) C(39) 121.9(4) . . . yes C(35) C(34) C(39) 119.7(5) . . . yes C(34) C(35) C(36) 122.3(5) . . . yes C(34) C(35) H(33) 118.9 . . . no C(36) C(35) H(33) 118.8 . . . no C(35) C(36) C(37) 118.3(5) . . . yes C(35) C(36) H(34) 120.9 . . . no C(37) C(36) H(34) 120.7 . . . no C(36) C(37) C(38) 121.3(5) . . . yes C(36) C(37) H(35) 119.5 . . . no C(38) C(37) H(35) 119.2 . . . no C(37) C(38) C(39) 121.5(5) . . . yes C(37) C(38) H(36) 119.4 . . . no C(39) C(38) H(36) 119.0 . . . no O(6) C(39) C(34) 124.4(4) . . . yes O(6) C(39) C(38) 118.8(4) . . . yes C(34) C(39) C(38) 116.8(5) . . . yes C(41) C(40) H(37) 109.4 . . . no C(41) C(40) H(38) 109.3 . . . no C(41) C(40) H(39) 109.5 . . . no H(37) C(40) H(38) 109.4 . . . no H(37) C(40) H(39) 109.7 . . . no H(38) C(40) H(39) 109.5 . . . no N(7) C(41) C(40) 123.2(4) . . . yes N(7) C(41) C(42) 110.1(4) . . . yes C(40) C(41) C(42) 126.6(4) . . . yes C(20) C(42) C(41) 127.6(4) . . . yes C(20) C(42) C(43) 127.8(4) . . . yes C(41) C(42) C(43) 104.5(4) . . . yes N(8) C(43) C(42) 110.5(4) . . . yes N(8) C(43) C(44) 123.1(4) . . . yes C(42) C(43) C(44) 126.4(4) . . . yes C(43) C(44) H(40) 109.6 . . . no C(43) C(44) H(41) 109.5 . . . no C(43) C(44) H(42) 109.3 . . . no H(40) C(44) H(41) 109.6 . . . no H(40) C(44) H(42) 109.6 . . . no H(41) C(44) H(42) 109.3 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu(1) C(12) 3.387(5) . 2_655 no Cu(1) C(17) 3.523(5) . 2_655 no Cu(2) C(6) 3.329(5) . 2_656 no Cu(2) C(5) 3.499(5) . 2_656 no Cu(3) C(35) 3.375(5) . 2_566 no Cu(3) O(4) 3.417(4) . 2_565 no Cu(3) Cu(3) 3.477(1) . 2_565 no Cu(4) O(5) 2.737(3) . 2_565 no Cu(4) C(23) 3.216(5) . 2_565 no O(1) O(3) 3.563(5) . 2_655 no O(2) C(13) 3.393(7) . 2_655 no O(2) C(14) 3.524(7) . 2_655 no O(2) C(9) 3.56(1) . 2_656 no O(3) C(5) 3.401(7) . 2_656 no O(3) C(4) 3.476(7) . 2_656 no O(3) C(9) 3.55(1) . 2_655 no O(4) O(5) 3.186(5) . 2_565 no O(5) N(6) 3.417(5) . 2_565 no O(5) O(6) 3.447(5) . 2_565 no O(6) C(23) 3.149(5) . 2_565 no O(6) C(24) 3.254(6) . 2_565 no O(6) C(28) 3.547(6) . 2_565 no N(2) C(2) 3.568(7) . 2_656 no N(2) N(4) 3.596(5) . 2_655 no N(3) C(11) 3.331(6) . 2_655 no N(3) C(7) 3.589(6) . 2_656 no N(4) C(7) 3.336(6) . 2_656 no N(5) N(8) 3.483(5) . 2_565 no N(7) C(33) 3.524(6) . 2_566 no N(8) C(33) 3.512(6) . 2_566 no C(1) C(14) 3.498(8) . 2_655 no C(4) C(17) 3.467(7) . 2_656 no C(13) C(13) 3.39(1) . 2_645 no C(15) C(24) 3.574(8) . 1_545 no C(24) C(39) 3.291(7) . 2_565 no C(25) C(38) 3.512(8) . 2_565 no C(25) C(39) 3.517(8) . 2_565 no C(28) C(36) 3.571(7) . 2_566 no C(29) C(37) 3.597(7) . 2_566 no Cu(1) Cu(2) 3.373(1) . . no Cu(2) Cu(1) 3.373(1) . . no Cu(3) Cu(4) 3.3682(9) . . no Cu(3) Cu(3) 3.477(1) . 2_565 no Cu(4) Cu(3) 3.3682(9) . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------