data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Liang Zhang' 'Zhi-Gang Ren' 'Hong-Xi Li' 'Jian-Ping Lang' _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email jplang@suda.edu.cn data_1 _database_code_depnum_ccdc_archive 'CCDC 787653' #TrackingRef 'JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C23 H32 Cl2 Cu2 N8), C2 H3 N' _chemical_formula_sum 'C48 H67 Cl4 Cu4 N17 O0' _chemical_formula_weight 1278.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.661(3) _cell_length_b 16.064(3) _cell_length_c 15.037(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.25(3) _cell_angle_gamma 90.00 _cell_volume 3133.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5382 _cell_measurement_theta_min 3.0671 _cell_measurement_theta_max 27.5165 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 1.555 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7188 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3708 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3583 _reflns_number_gt 2309 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+9.3098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3583 _refine_ls_number_parameters 179 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.2011 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.34257(5) 0.30136(4) 0.03265(5) 0.0411(3) Uani 1 1 d . . . Cl1 Cl 0.27098(11) 0.20484(9) 0.11700(9) 0.0457(4) Uani 1 1 d . . . N1 N 0.4958(3) 0.2776(3) 0.0555(3) 0.0376(10) Uani 1 1 d . . . C1 C 0.5969(6) 0.5596(4) 0.1631(5) 0.0646(19) Uani 1 1 d . . . H1A H 0.5956 0.6156 0.1406 0.097 Uiso 1 1 calc R . . H1B H 0.6458 0.5275 0.1435 0.097 Uiso 1 1 calc R . . H1C H 0.6165 0.5599 0.2302 0.097 Uiso 1 1 calc R . . N2 N 0.5712(3) 0.3208(3) 0.1205(3) 0.0372(10) Uani 1 1 d . . . C2 C 0.4922(5) 0.5217(4) 0.1240(4) 0.0440(13) Uani 1 1 d . . . N3 N 0.3709(3) 0.4206(3) 0.0921(3) 0.0360(10) Uani 1 1 d . . . C3 C 0.4003(6) 0.5559(4) 0.0719(4) 0.0525(16) Uani 1 1 d . . . H3 H 0.3890 0.6109 0.0522 0.063 Uiso 1 1 calc R . . N4 N 0.4723(3) 0.4401(3) 0.1352(3) 0.0363(10) Uani 1 1 d . . . C4 C 0.3266(5) 0.4924(4) 0.0540(4) 0.0454(14) Uani 1 1 d . . . C5 C 0.2153(5) 0.4955(4) 0.0019(5) 0.0640(19) Uani 1 1 d . . . H5A H 0.1925 0.4417 -0.0242 0.096 Uiso 1 1 calc R . . H5B H 0.2031 0.5358 -0.0476 0.096 Uiso 1 1 calc R . . H5C H 0.1778 0.5112 0.0437 0.096 Uiso 1 1 calc R . . C6 C 0.7639(4) 0.3287(5) 0.1918(5) 0.0600(18) Uani 1 1 d . . . H6A H 0.7629 0.3209 0.2548 0.090 Uiso 1 1 calc R . . H6B H 0.7681 0.3871 0.1798 0.090 Uiso 1 1 calc R . . H6C H 0.8226 0.3007 0.1838 0.090 Uiso 1 1 calc R . . C7 C 0.6666(4) 0.2934(4) 0.1244(4) 0.0414(13) Uani 1 1 d . . . N7 N 0.5000 -0.0497(10) 0.2500 0.074(4) Uani 0.50 2 d SPU . . C8 C 0.6519(4) 0.2332(4) 0.0580(4) 0.0475(14) Uani 1 1 d . . . H8 H 0.7029 0.2032 0.0431 0.057 Uiso 1 1 calc R . . C9 C 0.5458(5) 0.2253(4) 0.0165(4) 0.0436(13) Uani 1 1 d . . . C10 C 0.4855(6) 0.1700(5) -0.0626(6) 0.071(2) Uani 1 1 d . . . H10A H 0.4985 0.1127 -0.0443 0.106 Uiso 1 1 calc R . . H10B H 0.5065 0.1804 -0.1168 0.106 Uiso 1 1 calc R . . H10C H 0.4133 0.1815 -0.0770 0.106 Uiso 1 1 calc R . . C11 C 0.5424(4) 0.3756(3) 0.1853(4) 0.0351(11) Uani 1 1 d . . . H11 H 0.6054 0.4031 0.2241 0.042 Uiso 1 1 calc R . . C12 C 0.5000 0.3248(5) 0.2500 0.0362(16) Uani 1 2 d S . . H12A H 0.4456 0.2891 0.2121 0.043 Uiso 0.50 1 calc PR . . H12B H 0.5544 0.2891 0.2879 0.043 Uiso 0.50 1 calc PR . . C13 C 0.5000 0.0953(12) 0.2500 0.101(6) Uani 0.50 2 d SPU . . H13A H 0.4473 0.1152 0.2744 0.151 Uiso 0.25 1 calc PR . . H13B H 0.4868 0.1152 0.1871 0.151 Uiso 0.25 1 calc PR . . H13C H 0.5659 0.1152 0.2885 0.151 Uiso 0.25 1 calc PR . . C14 C 0.5000 0.0171(12) 0.2500 0.081(5) Uani 0.50 2 d SPU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0330(4) 0.0437(4) 0.0420(4) -0.0030(3) 0.0052(3) -0.0037(3) Cl1 0.0414(7) 0.0539(8) 0.0358(7) 0.0053(6) 0.0034(6) -0.0142(6) N1 0.031(2) 0.044(2) 0.038(2) -0.005(2) 0.0114(19) 0.0006(18) C1 0.070(5) 0.054(4) 0.070(5) -0.008(4) 0.023(4) -0.030(3) N2 0.028(2) 0.049(3) 0.033(2) -0.002(2) 0.0069(18) -0.0042(18) C2 0.059(4) 0.039(3) 0.039(3) -0.001(3) 0.023(3) -0.012(3) N3 0.034(2) 0.033(2) 0.036(2) 0.0006(19) 0.0034(18) 0.0011(17) C3 0.082(5) 0.035(3) 0.049(4) 0.004(3) 0.032(3) 0.001(3) N4 0.041(2) 0.034(2) 0.035(2) 0.0033(19) 0.0121(19) -0.0042(18) C4 0.056(4) 0.037(3) 0.042(3) 0.004(3) 0.013(3) 0.005(3) C5 0.061(4) 0.054(4) 0.065(4) 0.011(4) 0.003(3) 0.022(3) C6 0.030(3) 0.087(5) 0.060(4) 0.004(4) 0.009(3) -0.003(3) C7 0.030(3) 0.055(3) 0.041(3) 0.011(3) 0.013(2) 0.003(2) N7 0.090(10) 0.048(5) 0.058(8) 0.000 -0.013(7) 0.000 C8 0.037(3) 0.057(3) 0.054(4) 0.007(3) 0.020(3) 0.011(3) C9 0.046(3) 0.045(3) 0.044(3) -0.004(3) 0.019(3) 0.002(2) C10 0.063(4) 0.075(5) 0.072(5) -0.030(4) 0.017(4) 0.000(4) C11 0.032(3) 0.039(3) 0.033(3) -0.007(2) 0.007(2) -0.008(2) C12 0.031(4) 0.036(4) 0.037(4) 0.000 0.005(3) 0.000 C13 0.086(11) 0.046(6) 0.105(11) 0.000 -0.064(9) 0.000 C14 0.081(9) 0.045(5) 0.072(8) 0.000 -0.040(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.048(4) . ? Cu1 N3 2.098(4) . ? Cu1 Cl1 2.3007(17) 7 ? Cu1 Cl1 2.3971(16) . ? Cu1 Cu1 2.9202(14) 7 ? Cl1 Cu1 2.3007(17) 7 ? N1 C9 1.329(7) . ? N1 N2 1.367(6) . ? C1 C2 1.495(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? N2 C7 1.359(7) . ? N2 C11 1.455(7) . ? C2 N4 1.360(7) . ? C2 C3 1.368(9) . ? N3 C4 1.344(7) . ? N3 N4 1.369(6) . ? C3 C4 1.399(9) . ? C3 H3 0.9300 . ? N4 C11 1.451(7) . ? C4 C5 1.477(8) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.507(8) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.359(9) . ? N7 C14 1.07(2) . ? C8 C9 1.394(8) . ? C8 H8 0.9300 . ? C9 C10 1.506(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.518(7) . ? C11 H11 0.9800 . ? C12 C11 1.518(7) 2_655 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.26(3) . ? C13 H13A 0.9601 . ? C13 H13B 0.9601 . ? C13 H13C 0.9601 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 93.22(17) . . ? N1 Cu1 Cl1 119.77(14) . 7 ? N3 Cu1 Cl1 115.73(12) . 7 ? N1 Cu1 Cl1 110.85(14) . . ? N3 Cu1 Cl1 114.61(13) . . ? Cl1 Cu1 Cl1 103.16(5) 7 . ? N1 Cu1 Cu1 133.10(13) . 7 ? N3 Cu1 Cu1 133.15(13) . 7 ? Cl1 Cu1 Cu1 53.06(4) 7 7 ? Cl1 Cu1 Cu1 50.10(4) . 7 ? Cu1 Cl1 Cu1 76.83(5) 7 . ? C9 N1 N2 105.1(4) . . ? C9 N1 Cu1 133.0(4) . . ? N2 N1 Cu1 121.8(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 N2 N1 111.3(4) . . ? C7 N2 C11 128.6(4) . . ? N1 N2 C11 119.0(4) . . ? N4 C2 C3 105.9(5) . . ? N4 C2 C1 123.2(6) . . ? C3 C2 C1 130.9(6) . . ? C4 N3 N4 105.0(4) . . ? C4 N3 Cu1 127.1(4) . . ? N4 N3 Cu1 115.8(3) . . ? C2 C3 C4 107.1(5) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.4 . . ? C2 N4 N3 111.9(4) . . ? C2 N4 C11 128.9(5) . . ? N3 N4 C11 119.2(4) . . ? N3 C4 C3 110.0(5) . . ? N3 C4 C5 120.4(6) . . ? C3 C4 C5 129.5(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N2 106.3(5) . . ? C8 C7 C6 131.2(5) . . ? N2 C7 C6 122.6(5) . . ? C7 C8 C9 106.7(5) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N1 C9 C8 110.5(5) . . ? N1 C9 C10 119.5(5) . . ? C8 C9 C10 130.0(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 N2 111.0(4) . . ? N4 C11 C12 113.2(4) . . ? N2 C11 C12 110.0(4) . . ? N4 C11 H11 107.5 . . ? N2 C11 H11 107.5 . . ? C12 C11 H11 107.5 . . ? C11 C12 C11 114.9(6) 2_655 . ? C11 C12 H12A 108.5 2_655 . ? C11 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 2_655 . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N7 C14 C13 180.000(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 Cl1 Cu1 -129.40(14) . . . 7 ? N3 Cu1 Cl1 Cu1 126.69(13) . . . 7 ? Cl1 Cu1 Cl1 Cu1 0.0 7 . . 7 ? N3 Cu1 N1 C9 -157.8(5) . . . . ? Cl1 Cu1 N1 C9 -35.6(6) 7 . . . ? Cl1 Cu1 N1 C9 84.3(5) . . . . ? Cu1 Cu1 N1 C9 30.0(6) 7 . . . ? N3 Cu1 N1 N2 20.4(4) . . . . ? Cl1 Cu1 N1 N2 142.6(3) 7 . . . ? Cl1 Cu1 N1 N2 -97.5(4) . . . . ? Cu1 Cu1 N1 N2 -151.8(3) 7 . . . ? C9 N1 N2 C7 -2.3(6) . . . . ? Cu1 N1 N2 C7 179.0(4) . . . . ? C9 N1 N2 C11 -171.5(5) . . . . ? Cu1 N1 N2 C11 9.9(6) . . . . ? N1 Cu1 N3 C4 128.6(5) . . . . ? Cl1 Cu1 N3 C4 3.2(5) 7 . . . ? Cl1 Cu1 N3 C4 -116.7(5) . . . . ? Cu1 Cu1 N3 C4 -59.2(5) 7 . . . ? N1 Cu1 N3 N4 -7.9(4) . . . . ? Cl1 Cu1 N3 N4 -133.3(3) 7 . . . ? Cl1 Cu1 N3 N4 106.8(3) . . . . ? Cu1 Cu1 N3 N4 164.2(3) 7 . . . ? N4 C2 C3 C4 0.5(7) . . . . ? C1 C2 C3 C4 179.9(6) . . . . ? C3 C2 N4 N3 0.1(6) . . . . ? C1 C2 N4 N3 -179.4(5) . . . . ? C3 C2 N4 C11 -179.6(5) . . . . ? C1 C2 N4 C11 1.0(9) . . . . ? C4 N3 N4 C2 -0.7(6) . . . . ? Cu1 N3 N4 C2 144.7(4) . . . . ? C4 N3 N4 C11 179.0(5) . . . . ? Cu1 N3 N4 C11 -35.6(6) . . . . ? N4 N3 C4 C3 1.0(6) . . . . ? Cu1 N3 C4 C3 -139.2(4) . . . . ? N4 N3 C4 C5 -179.2(6) . . . . ? Cu1 N3 C4 C5 40.7(8) . . . . ? C2 C3 C4 N3 -0.9(7) . . . . ? C2 C3 C4 C5 179.3(6) . . . . ? N1 N2 C7 C8 2.1(6) . . . . ? C11 N2 C7 C8 169.9(5) . . . . ? N1 N2 C7 C6 -178.5(5) . . . . ? C11 N2 C7 C6 -10.6(9) . . . . ? N2 C7 C8 C9 -1.0(7) . . . . ? C6 C7 C8 C9 179.6(6) . . . . ? N2 N1 C9 C8 1.7(6) . . . . ? Cu1 N1 C9 C8 -179.9(4) . . . . ? N2 N1 C9 C10 -177.1(6) . . . . ? Cu1 N1 C9 C10 1.3(9) . . . . ? C7 C8 C9 N1 -0.4(7) . . . . ? C7 C8 C9 C10 178.2(7) . . . . ? C2 N4 C11 N2 -103.4(6) . . . . ? N3 N4 C11 N2 76.9(6) . . . . ? C2 N4 C11 C12 132.4(5) . . . . ? N3 N4 C11 C12 -47.3(6) . . . . ? C7 N2 C11 N4 133.1(5) . . . . ? N1 N2 C11 N4 -59.9(6) . . . . ? C7 N2 C11 C12 -100.9(5) . . . . ? N1 N2 C11 C12 66.1(5) . . . . ? N4 C11 C12 C11 -49.6(3) . . . 2_655 ? N2 C11 C12 C11 -174.3(4) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.908 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.093 #===END #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 787655' #TrackingRef 'JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C23 H32 Br2 Cu2 N8), C2 H3 N' _chemical_formula_sum 'C48 H67 Br4 Cu4 N17 O0' _chemical_formula_weight 1455.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.010(3) _cell_length_b 16.294(3) _cell_length_c 14.793(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.91(3) _cell_angle_gamma 90.00 _cell_volume 3230.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6160 _cell_measurement_theta_min 3.0396 _cell_measurement_theta_max 27.4894 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 3.816 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1643 _exptl_absorpt_correction_T_max 0.4580 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9159 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3683 _reflns_number_gt 2538 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+1.1490P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3683 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.34062(4) 0.29980(3) 0.03490(3) 0.03972(17) Uani 1 1 d . . . Br1 Br 0.27079(3) 0.19948(3) 0.12580(3) 0.04834(17) Uani 1 1 d . . . C4 C 0.6557(3) 0.2978(2) 0.1135(3) 0.0411(9) Uani 1 1 d . . . N4 N 0.4653(2) 0.43852(18) 0.1318(2) 0.0350(7) Uani 1 1 d . . . C11 C 0.5362(3) 0.3772(2) 0.1800(3) 0.0339(8) Uani 1 1 d . . . H11 H 0.5969 0.4059 0.2158 0.041 Uiso 1 1 calc R . . N3 N 0.3669(2) 0.41817(18) 0.0960(2) 0.0377(7) Uani 1 1 d . . . N2 N 0.5632(2) 0.32321(19) 0.1129(2) 0.0359(7) Uani 1 1 d . . . C12 C 0.5000 0.3265(3) 0.2500 0.0326(11) Uani 1 2 d S . . H12A H 0.4460 0.2914 0.2150 0.039 Uiso 0.50 1 calc PR . . H12B H 0.5540 0.2914 0.2850 0.039 Uiso 0.50 1 calc PR . . C2 C 0.5378(3) 0.2280(3) 0.0090(3) 0.0461(10) Uani 1 1 d . . . C3 C 0.6408(3) 0.2376(3) 0.0470(3) 0.0481(10) Uani 1 1 d . . . H3 H 0.6900 0.2084 0.0300 0.058 Uiso 1 1 calc R . . C7 C 0.3208(3) 0.4885(2) 0.0624(3) 0.0445(10) Uani 1 1 d . . . C9 C 0.4803(3) 0.5197(2) 0.1201(3) 0.0420(9) Uani 1 1 d . . . N1 N 0.4898(2) 0.2796(2) 0.0501(2) 0.0383(7) Uani 1 1 d . . . C10 C 0.5818(4) 0.5589(3) 0.1525(4) 0.0604(13) Uani 1 1 d . . . H10A H 0.6093 0.5515 0.2194 0.091 Uiso 1 1 calc R . . H10B H 0.5760 0.6165 0.1382 0.091 Uiso 1 1 calc R . . H10C H 0.6249 0.5337 0.1205 0.091 Uiso 1 1 calc R . . C8 C 0.3906(4) 0.5527(2) 0.0768(3) 0.0495(11) Uani 1 1 d . . . H8 H 0.3773 0.6074 0.0597 0.059 Uiso 1 1 calc R . . C5 C 0.7492(3) 0.3348(3) 0.1753(4) 0.0589(12) Uani 1 1 d . . . H5A H 0.8058 0.3072 0.1652 0.088 Uiso 1 1 calc R . . H5B H 0.7506 0.3292 0.2402 0.088 Uiso 1 1 calc R . . H5C H 0.7516 0.3920 0.1602 0.088 Uiso 1 1 calc R . . C6 C 0.2103(4) 0.4900(3) 0.0161(4) 0.0668(14) Uani 1 1 d . . . H6A H 0.1910 0.4420 -0.0225 0.100 Uiso 1 1 calc R . . H6B H 0.1930 0.5382 -0.0225 0.100 Uiso 1 1 calc R . . H6C H 0.1763 0.4908 0.0638 0.100 Uiso 1 1 calc R . . C1 C 0.4818(4) 0.1719(3) -0.0680(4) 0.0754(17) Uani 1 1 d . . . H1A H 0.5024 0.1163 -0.0517 0.113 Uiso 1 1 calc R . . H1B H 0.4953 0.1864 -0.1260 0.113 Uiso 1 1 calc R . . H1C H 0.4115 0.1768 -0.0759 0.113 Uiso 1 1 calc R . . C13 C 0.5000 -0.0200(12) -0.2500 0.084(5) Uiso 0.50 2 d SP . . N5 N 0.5000 0.0446(13) -0.2500 0.121(6) Uiso 0.50 2 d SP . . C14 C 0.4823(14) -0.0923(10) -0.2075(13) 0.051(4) Uiso 0.25 1 d P . . H14A H 0.4891 -0.0823 -0.1420 0.077 Uiso 0.25 1 calc PR . . H14B H 0.5296 -0.1333 -0.2129 0.077 Uiso 0.25 1 calc PR . . H14C H 0.4159 -0.1113 -0.2383 0.077 Uiso 0.25 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0334(3) 0.0417(3) 0.0409(3) -0.0014(2) 0.0058(2) -0.00542(19) Br1 0.0435(3) 0.0578(3) 0.0375(2) 0.00595(19) 0.00187(18) -0.02033(18) C4 0.028(2) 0.053(2) 0.044(2) 0.0137(19) 0.0125(17) 0.0043(17) N4 0.0346(17) 0.0330(15) 0.0359(16) 0.0003(13) 0.0078(14) -0.0057(13) C11 0.0281(19) 0.0403(19) 0.0338(19) -0.0050(16) 0.0097(15) -0.0067(15) N3 0.0314(17) 0.0337(16) 0.0448(18) 0.0029(15) 0.0062(14) -0.0003(13) N2 0.0279(16) 0.0472(18) 0.0334(16) -0.0017(14) 0.0098(13) -0.0023(13) C12 0.030(3) 0.035(3) 0.029(3) 0.000 0.004(2) 0.000 C2 0.043(2) 0.048(2) 0.054(3) -0.006(2) 0.025(2) -0.0025(19) C3 0.043(2) 0.046(2) 0.064(3) 0.006(2) 0.029(2) 0.0091(19) C7 0.052(3) 0.039(2) 0.043(2) 0.0055(19) 0.0143(19) 0.0055(19) C9 0.057(3) 0.037(2) 0.035(2) 0.0005(18) 0.0187(19) -0.0121(18) N1 0.0317(18) 0.0466(18) 0.0380(17) -0.0054(15) 0.0124(15) -0.0019(14) C10 0.062(3) 0.059(3) 0.063(3) -0.003(2) 0.023(3) -0.030(2) C8 0.068(3) 0.035(2) 0.047(3) 0.0073(19) 0.020(2) 0.000(2) C5 0.034(2) 0.082(3) 0.059(3) 0.005(3) 0.012(2) -0.002(2) C6 0.055(3) 0.058(3) 0.077(3) 0.009(3) 0.004(3) 0.017(2) C1 0.070(4) 0.076(3) 0.088(4) -0.040(3) 0.035(3) -0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.062(3) . ? Cu1 N3 2.116(3) . ? Cu1 Br1 2.4349(11) 7 ? Cu1 Br1 2.4905(8) . ? Cu1 Cu1 2.9364(11) 7 ? Br1 Cu1 2.4350(11) 7 ? C4 N2 1.358(5) . ? C4 C3 1.361(6) . ? C4 C5 1.490(6) . ? N4 C9 1.358(5) . ? N4 N3 1.366(4) . ? N4 C11 1.443(5) . ? C11 N2 1.456(5) . ? C11 C12 1.522(4) . ? C11 H11 0.9800 . ? N3 C7 1.338(5) . ? N2 N1 1.368(4) . ? C12 C11 1.522(4) 2_655 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C2 N1 1.329(5) . ? C2 C3 1.396(6) . ? C2 C1 1.494(7) . ? C3 H3 0.9300 . ? C7 C8 1.405(6) . ? C7 C6 1.500(6) . ? C9 C8 1.345(6) . ? C9 C10 1.505(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C8 H8 0.9300 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C13 N5 1.05(2) . ? C13 C14 1.39(2) 2_654 ? C13 C14 1.39(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 93.11(12) . . ? N1 Cu1 Br1 116.67(10) . 7 ? N3 Cu1 Br1 113.27(9) . 7 ? N1 Cu1 Br1 112.38(10) . . ? N3 Cu1 Br1 114.49(10) . . ? Br1 Cu1 Br1 106.82(2) 7 . ? N1 Cu1 Cu1 134.04(9) . 7 ? N3 Cu1 Cu1 132.77(9) . 7 ? Br1 Cu1 Cu1 54.28(3) 7 7 ? Br1 Cu1 Cu1 52.54(2) . 7 ? Cu1 Br1 Cu1 73.18(2) 7 . ? N2 C4 C3 105.7(4) . . ? N2 C4 C5 123.2(4) . . ? C3 C4 C5 131.1(4) . . ? C9 N4 N3 111.3(3) . . ? C9 N4 C11 128.9(3) . . ? N3 N4 C11 119.7(3) . . ? N4 C11 N2 111.1(3) . . ? N4 C11 C12 113.2(3) . . ? N2 C11 C12 109.9(3) . . ? N4 C11 H11 107.5 . . ? N2 C11 H11 107.5 . . ? C12 C11 H11 107.5 . . ? C7 N3 N4 105.0(3) . . ? C7 N3 Cu1 128.1(3) . . ? N4 N3 Cu1 114.7(2) . . ? C4 N2 N1 111.9(3) . . ? C4 N2 C11 128.1(3) . . ? N1 N2 C11 118.9(3) . . ? C11 C12 C11 114.3(4) 2_655 . ? C11 C12 H12A 108.7 2_655 . ? C11 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 2_655 . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? N1 C2 C3 110.3(4) . . ? N1 C2 C1 120.8(4) . . ? C3 C2 C1 128.9(4) . . ? C4 C3 C2 107.1(4) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? N3 C7 C8 110.0(4) . . ? N3 C7 C6 120.4(4) . . ? C8 C7 C6 129.6(4) . . ? C8 C9 N4 107.0(4) . . ? C8 C9 C10 130.3(4) . . ? N4 C9 C10 122.7(4) . . ? C2 N1 N2 105.0(3) . . ? C2 N1 Cu1 133.1(3) . . ? N2 N1 Cu1 121.9(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C8 C7 106.6(4) . . ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N5 C13 C14 147.9(9) . 2_654 ? N5 C13 C14 147.9(9) . . ? C14 C13 C14 64.3(17) 2_654 . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.886 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.089 #===END #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 787656' #TrackingRef 'JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 Cu2 I2 N8, C2 H3 N' _chemical_formula_sum 'C25 H3 Cu2 I2 N9 O0' _chemical_formula_weight 810.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.399(2) _cell_length_b 18.994(4) _cell_length_c 14.784(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.84(3) _cell_angle_gamma 90.00 _cell_volume 3189.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13506 _cell_measurement_theta_min 3.0515 _cell_measurement_theta_max 27.5204 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1779 _exptl_absorpt_correction_T_max 0.6376 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18059 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7241 _reflns_number_gt 5303 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7241 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.62105(6) 0.97330(3) 0.54365(5) 0.04164(18) Uani 1 1 d . . . Cu2 Cu 0.92228(7) 0.94742(4) 0.95455(5) 0.04402(19) Uani 1 1 d . . . I1 I 0.55446(3) 0.98267(2) 0.36741(2) 0.04967(14) Uani 1 1 d . . . I2 I 1.03222(4) 0.927318(18) 1.11361(3) 0.05040(14) Uani 1 1 d . . . C1 C 0.8533(4) 0.9158(3) 0.6661(3) 0.0335(10) Uani 1 1 d . . . C2 C 0.7768(5) 0.9322(3) 0.7443(3) 0.0345(11) Uani 1 1 d . . . C33 C 0.8352(5) 1.0765(3) 0.5506(4) 0.0392(12) Uani 1 1 d . . . C4 C 0.9576(5) 1.0770(3) 0.5745(4) 0.0433(13) Uani 1 1 d . . . C5 C 0.9817(5) 1.0141(3) 0.6194(4) 0.0372(12) Uani 1 1 d . . . C3 C 0.7494(5) 0.8667(3) 0.7986(3) 0.0340(11) Uani 1 1 d . . . C9 C 0.8450(5) 0.8016(3) 0.5771(4) 0.0401(12) Uani 1 1 d . . . C10 C 0.5699(5) 0.8803(3) 0.8872(4) 0.0443(13) Uani 1 1 d . . . C11 C 0.7592(6) 1.1328(3) 0.5021(5) 0.0564(16) Uani 1 1 d . . . C12 C 0.6618(5) 0.9331(3) 1.0079(4) 0.0460(13) Uani 1 1 d . . . C13 C 1.0948(5) 0.9862(3) 0.6640(4) 0.0508(15) Uani 1 1 d . . . C14 C 0.5510(5) 0.9078(3) 0.9703(4) 0.0492(14) Uani 1 1 d . . . C15 C 0.9711(5) 0.7812(3) 0.5973(4) 0.0502(15) Uani 1 1 d . . . C16 C 0.8798(5) 0.7589(3) 0.8142(4) 0.0427(13) Uani 1 1 d . . . C17 C 0.6909(7) 0.9684(4) 1.0981(4) 0.0625(18) Uani 1 1 d . . . C18 C 0.9967(6) 0.7491(3) 0.8407(4) 0.0506(14) Uani 1 1 d . . . C19 C 0.7546(6) 0.7665(3) 0.5301(4) 0.0479(14) Uani 1 1 d . . . C20 C 1.0403(5) 0.8156(3) 0.8709(4) 0.0462(14) Uani 1 1 d . . . C21 C 1.1630(6) 0.8352(4) 0.9072(5) 0.0636(18) Uani 1 1 d . . . C22 C 0.7878(6) 0.7062(3) 0.7761(5) 0.0581(17) Uani 1 1 d . . . C23 C 0.6545(6) 0.8095(3) 0.5315(4) 0.0470(14) Uani 1 1 d . . . C24 C 0.5291(6) 0.7974(3) 0.4910(6) 0.072(2) Uani 1 1 d . . . C25 C 0.4846(6) 0.8462(4) 0.8151(5) 0.0666(19) Uani 1 1 d . . . C30 C 0.3555(15) 0.6272(10) 0.6990(12) 0.206(8) Uiso 1 1 d . . . H30A H 0.3342 0.6021 0.7516 0.309 Uiso 1 1 calc R . . H30B H 0.4396 0.6302 0.7002 0.309 Uiso 1 1 calc R . . H30C H 0.3252 0.6028 0.6452 0.309 Uiso 1 1 calc R . . C31 C 0.3074(16) 0.6958(11) 0.6990(13) 0.178(6) Uiso 1 1 d . . . N1 N 0.8769(4) 0.9789(2) 0.6189(3) 0.0344(9) Uani 1 1 d . . . N2 N 0.7864(4) 1.0174(2) 0.5766(3) 0.0354(9) Uani 1 1 d . . . N7 N 0.6863(4) 0.8875(2) 0.8778(3) 0.0383(10) Uani 1 1 d . . . N8 N 0.7430(4) 0.9214(2) 0.9495(3) 0.0407(10) Uani 1 1 d . . . N6 N 0.9538(4) 0.8636(2) 0.8636(3) 0.0400(10) Uani 1 1 d . . . N5 N 0.8552(4) 0.8280(2) 0.8277(3) 0.0365(10) Uani 1 1 d . . . N3 N 0.7979(4) 0.8626(2) 0.6056(3) 0.0352(9) Uani 1 1 d . . . N4 N 0.6816(4) 0.8689(2) 0.5779(3) 0.0405(10) Uani 1 1 d . . . N9 N 0.2563(14) 0.7549(10) 0.6955(11) 0.217(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0393(4) 0.0414(4) 0.0436(4) -0.0011(3) 0.0003(3) 0.0007(3) Cu2 0.0478(4) 0.0420(4) 0.0413(4) -0.0019(3) -0.0018(3) -0.0008(3) I1 0.0407(2) 0.0733(3) 0.0350(2) -0.00248(17) 0.00253(16) 0.00968(18) I2 0.0685(3) 0.0373(2) 0.0426(2) 0.00293(15) -0.01229(19) -0.00875(18) C1 0.035(3) 0.036(3) 0.030(2) -0.002(2) 0.002(2) 0.001(2) C2 0.040(3) 0.034(3) 0.029(2) -0.002(2) 0.004(2) 0.003(2) C33 0.042(3) 0.034(3) 0.043(3) 0.002(2) 0.008(2) -0.003(2) C4 0.042(3) 0.042(3) 0.047(3) -0.008(2) 0.008(3) -0.005(2) C5 0.035(3) 0.040(3) 0.038(3) -0.011(2) 0.009(2) -0.003(2) C3 0.038(3) 0.031(2) 0.032(2) 0.001(2) 0.004(2) 0.002(2) C9 0.055(3) 0.030(3) 0.036(3) -0.001(2) 0.014(3) 0.007(2) C10 0.037(3) 0.042(3) 0.054(3) 0.010(3) 0.003(3) -0.002(2) C11 0.046(4) 0.045(3) 0.077(5) 0.015(3) 0.003(3) 0.002(3) C12 0.045(3) 0.049(3) 0.045(3) 0.005(3) 0.009(3) 0.008(3) C13 0.035(3) 0.060(4) 0.056(4) -0.002(3) -0.004(3) 0.000(3) C14 0.046(3) 0.053(3) 0.050(3) 0.009(3) 0.008(3) 0.005(3) C15 0.046(3) 0.049(3) 0.058(4) 0.008(3) 0.013(3) 0.018(3) C16 0.060(4) 0.033(3) 0.036(3) 0.001(2) 0.013(3) 0.003(3) C17 0.066(4) 0.079(5) 0.044(4) -0.007(3) 0.012(3) 0.010(4) C18 0.058(4) 0.040(3) 0.055(3) 0.002(3) 0.009(3) 0.011(3) C19 0.060(4) 0.042(3) 0.041(3) -0.008(2) 0.002(3) 0.003(3) C20 0.050(3) 0.043(3) 0.045(3) 0.006(2) 0.004(3) 0.011(3) C21 0.034(3) 0.067(4) 0.087(5) -0.002(4) -0.006(3) 0.006(3) C22 0.073(5) 0.035(3) 0.067(4) -0.002(3) 0.008(4) -0.011(3) C23 0.055(4) 0.036(3) 0.048(3) -0.006(2) -0.004(3) 0.001(3) C24 0.056(4) 0.052(4) 0.102(6) -0.023(4) -0.028(4) -0.004(3) C25 0.043(4) 0.080(5) 0.074(5) 0.002(4) -0.005(3) -0.009(3) N1 0.031(2) 0.038(2) 0.034(2) -0.0028(18) 0.0038(18) 0.0003(18) N2 0.032(2) 0.035(2) 0.039(2) 0.0019(18) 0.0026(19) -0.0001(18) N7 0.039(2) 0.042(2) 0.035(2) 0.0028(19) 0.0052(19) 0.000(2) N8 0.041(3) 0.047(3) 0.035(2) -0.0012(19) 0.005(2) 0.001(2) N6 0.038(3) 0.035(2) 0.046(2) 0.002(2) -0.001(2) 0.0018(19) N5 0.042(3) 0.026(2) 0.041(2) 0.0006(18) 0.003(2) -0.0001(18) N3 0.034(2) 0.038(2) 0.033(2) -0.0042(18) -0.0001(18) 0.0073(19) N4 0.038(2) 0.032(2) 0.051(3) -0.013(2) -0.002(2) 0.0021(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.083(4) . ? Cu1 N4 2.146(4) . ? Cu1 I1 2.6219(10) 3_676 ? Cu1 I1 2.6576(10) . ? Cu2 N8 2.098(5) . ? Cu2 N6 2.133(5) . ? Cu2 I2 2.5978(11) . ? Cu2 I2 2.6520(9) 3_777 ? Cu2 Cu2 2.9212(15) 3_777 ? I1 Cu1 2.6219(10) 3_676 ? I2 Cu2 2.6520(9) 3_777 ? C1 N1 1.423(7) . ? C1 N3 1.458(6) . ? C1 C2 1.537(7) . ? C2 C3 1.527(7) . ? C33 N2 1.323(7) . ? C33 C4 1.409(8) . ? C33 C11 1.518(8) . ? C4 C5 1.383(8) . ? C5 N1 1.369(7) . ? C5 C13 1.494(8) . ? C3 N5 1.446(6) . ? C3 N7 1.479(6) . ? C9 N3 1.358(6) . ? C9 C19 1.367(8) . ? C9 C15 1.496(8) . ? C10 N7 1.352(7) . ? C10 C14 1.368(8) . ? C10 C25 1.525(9) . ? C12 N8 1.337(7) . ? C12 C14 1.420(9) . ? C12 C17 1.503(9) . ? C16 N5 1.362(7) . ? C16 C18 1.370(8) . ? C16 C22 1.522(8) . ? C18 C20 1.415(9) . ? C19 C23 1.405(9) . ? C20 N6 1.342(7) . ? C20 C21 1.502(9) . ? C23 N4 1.342(7) . ? C23 C24 1.520(9) . ? C30 C31 1.41(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N9 1.26(2) . ? N1 N2 1.372(6) . ? N7 N8 1.356(6) . ? N6 N5 1.378(6) . ? N3 N4 1.359(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N4 92.88(16) . . ? N2 Cu1 I1 117.91(12) . 3_676 ? N4 Cu1 I1 114.84(13) . 3_676 ? N2 Cu1 I1 112.35(12) . . ? N4 Cu1 I1 110.67(13) . . ? I1 Cu1 I1 107.66(3) 3_676 . ? N8 Cu2 N6 90.98(17) . . ? N8 Cu2 I2 113.08(13) . . ? N6 Cu2 I2 111.54(12) . . ? N8 Cu2 I2 114.76(13) . 3_777 ? N6 Cu2 I2 112.39(12) . 3_777 ? I2 Cu2 I2 112.39(3) . 3_777 ? N8 Cu2 Cu2 136.78(13) . 3_777 ? N6 Cu2 Cu2 132.24(13) . 3_777 ? I2 Cu2 Cu2 57.08(3) . 3_777 ? I2 Cu2 Cu2 55.31(3) 3_777 3_777 ? Cu1 I1 Cu1 72.34(3) 3_676 . ? Cu2 I2 Cu2 67.61(3) . 3_777 ? N1 C1 N3 111.9(4) . . ? N1 C1 C2 109.9(4) . . ? N3 C1 C2 111.0(4) . . ? C3 C2 C1 112.6(4) . . ? N2 C33 C4 111.4(5) . . ? N2 C33 C11 119.7(5) . . ? C4 C33 C11 128.9(5) . . ? C5 C4 C33 105.5(5) . . ? N1 C5 C4 106.3(5) . . ? N1 C5 C13 123.3(5) . . ? C4 C5 C13 130.3(5) . . ? N5 C3 N7 110.4(4) . . ? N5 C3 C2 111.6(4) . . ? N7 C3 C2 109.5(4) . . ? N3 C9 C19 105.9(5) . . ? N3 C9 C15 123.9(5) . . ? C19 C9 C15 130.2(5) . . ? N7 C10 C14 106.5(5) . . ? N7 C10 C25 123.0(6) . . ? C14 C10 C25 130.5(6) . . ? N8 C12 C14 109.4(5) . . ? N8 C12 C17 122.3(6) . . ? C14 C12 C17 128.4(6) . . ? C10 C14 C12 106.2(5) . . ? N5 C16 C18 107.2(5) . . ? N5 C16 C22 123.0(5) . . ? C18 C16 C22 129.8(5) . . ? C16 C18 C20 106.0(5) . . ? C9 C19 C23 106.6(5) . . ? N6 C20 C18 110.3(5) . . ? N6 C20 C21 121.0(5) . . ? C18 C20 C21 128.7(5) . . ? N4 C23 C19 110.2(5) . . ? N4 C23 C24 119.8(5) . . ? C19 C23 C24 130.0(5) . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N9 C31 C30 175(2) . . ? N2 N1 C5 111.4(4) . . ? N2 N1 C1 120.5(4) . . ? C5 N1 C1 127.5(4) . . ? C33 N2 N1 105.4(4) . . ? C33 N2 Cu1 131.9(4) . . ? N1 N2 Cu1 121.5(3) . . ? C10 N7 N8 112.0(5) . . ? C10 N7 C3 127.0(5) . . ? N8 N7 C3 120.9(4) . . ? C12 N8 N7 105.9(5) . . ? C12 N8 Cu2 131.5(4) . . ? N7 N8 Cu2 122.6(3) . . ? C20 N6 N5 105.5(4) . . ? C20 N6 Cu2 128.2(4) . . ? N5 N6 Cu2 115.7(3) . . ? C16 N5 N6 111.0(4) . . ? C16 N5 C3 128.5(5) . . ? N6 N5 C3 119.8(4) . . ? N4 N3 C9 112.5(4) . . ? N4 N3 C1 119.0(4) . . ? C9 N3 C1 128.3(5) . . ? C23 N4 N3 104.8(4) . . ? C23 N4 Cu1 126.9(4) . . ? N3 N4 Cu1 116.0(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.937 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.170 #===END #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 787657' #TrackingRef 'JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H32 Cu2 N10 S2' _chemical_formula_sum 'C25 H32 Cu2 N10 S2' _chemical_formula_weight 663.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.747(4) _cell_length_b 8.0550(16) _cell_length_c 20.321(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.67(3) _cell_angle_gamma 90.00 _cell_volume 2907.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12340 _cell_measurement_theta_min 3.0102 _cell_measurement_theta_max 27.5087 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.641 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3929 _exptl_absorpt_correction_T_max 0.6388 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16148 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6523 _reflns_number_gt 5337 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0048(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6523 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.196 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.620092(18) 0.34714(4) 0.334269(17) 0.04059(13) Uani 1 1 d . . . Cu2 Cu 0.357621(18) 0.23846(4) 0.161481(16) 0.03823(12) Uani 1 1 d . . . C10 C 0.12224(14) 0.2411(3) 0.10526(13) 0.0335(5) Uani 1 1 d . . . C12 C 0.35831(17) -0.1412(3) 0.13605(14) 0.0396(6) Uani 1 1 d . . . C14 C 0.20666(13) 0.1107(3) 0.04315(11) 0.0249(5) Uani 1 1 d . . . H14 H 0.1592 0.0623 0.0137 0.030 Uiso 1 1 calc R . . C15 C 0.46380(15) 0.2151(3) 0.31167(13) 0.0336(5) Uani 1 1 d . . . C16 C 0.50983(15) 0.3876(3) 0.18665(14) 0.0362(6) Uani 1 1 d . . . C17 C 0.78176(13) 0.3790(3) 0.45489(12) 0.0266(5) Uani 1 1 d . . . H17 H 0.8331 0.3975 0.4862 0.032 Uiso 1 1 calc R . . C18 C 0.13662(16) 0.3472(3) 0.16056(14) 0.0375(6) Uani 1 1 d . . . H18 H 0.1018 0.3889 0.1802 0.045 Uiso 1 1 calc R . . C19 C 0.43961(19) -0.1549(4) 0.17774(17) 0.0581(9) Uani 1 1 d . . . H19A H 0.4682 -0.0765 0.1608 0.087 Uiso 1 1 calc R . . H19B H 0.4570 -0.2652 0.1736 0.087 Uiso 1 1 calc R . . H19C H 0.4459 -0.1317 0.2256 0.087 Uiso 1 1 calc R . . C20 C 0.84957(16) 0.2159(4) 0.38510(15) 0.0408(6) Uani 1 1 d . . . C21 C 0.66455(17) 0.7118(3) 0.37440(14) 0.0389(6) Uani 1 1 d . . . C22 C 0.23713(16) -0.1889(3) 0.08042(14) 0.0360(6) Uani 1 1 d . . . C23 C 0.25900(18) 0.4825(4) 0.24234(14) 0.0475(7) Uani 1 1 d . . . H23A H 0.3108 0.4826 0.2442 0.071 Uiso 1 1 calc R . . H23B H 0.2550 0.4358 0.2845 0.071 Uiso 1 1 calc R . . H23C H 0.2403 0.5943 0.2372 0.071 Uiso 1 1 calc R . . C24 C 0.74590(19) 0.1498(3) 0.29993(14) 0.0410(7) Uani 1 1 d . . . C25 C 0.05062(16) 0.1610(4) 0.06367(17) 0.0513(8) Uani 1 1 d . . . H25A H 0.0456 0.1675 0.0152 0.077 Uiso 1 1 calc R . . H25B H 0.0091 0.2171 0.0718 0.077 Uiso 1 1 calc R . . H25C H 0.0509 0.0467 0.0771 0.077 Uiso 1 1 calc R . . C26 C 0.92770(18) 0.2426(5) 0.43275(18) 0.0616(10) Uani 1 1 d . . . H26A H 0.9404 0.3581 0.4328 0.092 Uiso 1 1 calc R . . H26B H 0.9622 0.1779 0.4172 0.092 Uiso 1 1 calc R . . H26C H 0.9308 0.2091 0.4789 0.092 Uiso 1 1 calc R . . C27 C 0.30325(18) -0.2651(3) 0.11709(15) 0.0436(7) Uani 1 1 d . . . H27 H 0.3102 -0.3776 0.1274 0.052 Uiso 1 1 calc R . . C28 C 0.78607(16) 0.6894(3) 0.43397(13) 0.0371(6) Uani 1 1 d . . . C29 C 0.21370(15) 0.3808(3) 0.18179(12) 0.0320(5) Uani 1 1 d . . . C30 C 0.1604(2) -0.2582(4) 0.04963(18) 0.0519(8) Uani 1 1 d . . . H30A H 0.1621 -0.3767 0.0548 0.078 Uiso 1 1 calc R . . H30B H 0.1416 -0.2304 0.0012 0.078 Uiso 1 1 calc R . . H30C H 0.1277 -0.2124 0.0729 0.078 Uiso 1 1 calc R . . C31 C 0.5889(2) 0.7705(4) 0.33096(18) 0.0591(9) Uani 1 1 d . . . H31A H 0.5903 0.7993 0.2855 0.089 Uiso 1 1 calc R . . H31B H 0.5750 0.8663 0.3522 0.089 Uiso 1 1 calc R . . H31C H 0.5526 0.6839 0.3271 0.089 Uiso 1 1 calc R . . C32 C 0.73226(19) 0.7999(3) 0.40001(15) 0.0460(7) Uani 1 1 d . . . H32 H 0.7390 0.9129 0.3947 0.055 Uiso 1 1 calc R . . C33 C 0.82393(19) 0.1338(3) 0.32327(16) 0.0487(8) Uani 1 1 d . . . H33 H 0.8530 0.0778 0.3010 0.058 Uiso 1 1 calc R . . C34 C 0.6905(2) 0.0835(4) 0.23469(16) 0.0629(10) Uani 1 1 d . . . H34A H 0.6403 0.0999 0.2361 0.094 Uiso 1 1 calc R . . H34B H 0.6993 -0.0330 0.2308 0.094 Uiso 1 1 calc R . . H34C H 0.6964 0.1409 0.1954 0.094 Uiso 1 1 calc R . . C35 C 0.86874(18) 0.7114(4) 0.46807(17) 0.0555(8) Uani 1 1 d . . . H35A H 0.8837 0.6598 0.5130 0.083 Uiso 1 1 calc R . . H35B H 0.8804 0.8277 0.4731 0.083 Uiso 1 1 calc R . . H35C H 0.8953 0.6608 0.4400 0.083 Uiso 1 1 calc R . . C40 C 0.73873(13) 0.2845(3) 0.49610(11) 0.0247(4) Uani 1 1 d . . . H40A H 0.6974 0.2253 0.4633 0.030 Uiso 1 1 calc R . . H40B H 0.7723 0.2020 0.5247 0.030 Uiso 1 1 calc R . . N1 N 0.72257(12) 0.2350(2) 0.34549(10) 0.0317(5) Uani 1 1 d . . . N2 N 0.78734(12) 0.2757(3) 0.39770(10) 0.0312(4) Uani 1 1 d . . . N3 N 0.67537(11) 0.5518(2) 0.39222(10) 0.0300(4) Uani 1 1 d . . . N4 N 0.75040(11) 0.5399(2) 0.42907(10) 0.0276(4) Uani 1 1 d . . . N5 N 0.32888(11) 0.0064(3) 0.11189(10) 0.0317(4) Uani 1 1 d . . . N6 N 0.25485(11) -0.0250(2) 0.07745(10) 0.0276(4) Uani 1 1 d . . . N7 N 0.24630(11) 0.3031(2) 0.14094(10) 0.0279(4) Uani 1 1 d . . . N8 N 0.18900(11) 0.2181(2) 0.09385(10) 0.0263(4) Uani 1 1 d . . . N9 N 0.55932(13) 0.3929(3) 0.23748(12) 0.0476(6) Uani 1 1 d . . . N10 N 0.41310(14) 0.2134(3) 0.26136(12) 0.0455(6) Uani 1 1 d . . . S3 S 0.43782(4) 0.38171(9) 0.11383(3) 0.04256(18) Uani 1 1 d . . . S4 S 0.53723(4) 0.21630(10) 0.38344(3) 0.04278(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03052(19) 0.0530(2) 0.03184(19) 0.00192(14) 0.00104(14) -0.00719(14) Cu2 0.02883(19) 0.0509(2) 0.03002(19) -0.00222(13) 0.00253(14) -0.00813(14) C10 0.0284(13) 0.0439(14) 0.0293(13) 0.0018(10) 0.0111(10) 0.0023(10) C12 0.0451(16) 0.0479(16) 0.0273(13) 0.0039(11) 0.0138(12) 0.0171(12) C14 0.0233(11) 0.0305(11) 0.0207(10) -0.0035(9) 0.0067(9) -0.0026(9) C15 0.0318(13) 0.0423(14) 0.0274(12) 0.0014(10) 0.0103(11) -0.0090(11) C16 0.0315(13) 0.0454(14) 0.0327(14) 0.0052(11) 0.0119(11) -0.0088(11) C17 0.0210(11) 0.0368(12) 0.0211(11) 0.0007(9) 0.0055(9) -0.0006(9) C18 0.0390(14) 0.0412(14) 0.0385(14) 0.0007(11) 0.0213(12) 0.0061(11) C19 0.0503(19) 0.075(2) 0.0453(18) 0.0067(15) 0.0108(15) 0.0283(16) C20 0.0423(16) 0.0494(15) 0.0396(15) 0.0131(12) 0.0256(13) 0.0151(12) C21 0.0530(17) 0.0334(13) 0.0328(14) 0.0069(11) 0.0174(13) 0.0084(12) C22 0.0493(16) 0.0330(13) 0.0323(13) 0.0017(10) 0.0222(12) -0.0037(12) C23 0.067(2) 0.0445(15) 0.0345(15) -0.0133(12) 0.0212(14) -0.0119(14) C24 0.069(2) 0.0305(13) 0.0316(14) 0.0001(10) 0.0273(14) 0.0016(12) C25 0.0291(14) 0.082(2) 0.0448(17) -0.0076(15) 0.0142(13) -0.0060(14) C26 0.0348(17) 0.099(3) 0.056(2) 0.0192(18) 0.0218(15) 0.0230(16) C27 0.0602(19) 0.0345(14) 0.0414(15) 0.0096(11) 0.0238(14) 0.0093(13) C28 0.0477(16) 0.0392(14) 0.0279(13) -0.0036(11) 0.0168(12) -0.0154(12) C29 0.0474(15) 0.0281(11) 0.0230(11) 0.0001(9) 0.0148(11) 0.0004(10) C30 0.062(2) 0.0406(15) 0.0572(19) -0.0018(13) 0.0258(17) -0.0176(14) C31 0.060(2) 0.0584(19) 0.060(2) 0.0226(16) 0.0202(17) 0.0239(16) C32 0.068(2) 0.0302(13) 0.0445(16) 0.0019(12) 0.0242(15) -0.0063(14) C33 0.070(2) 0.0431(15) 0.0480(17) 0.0106(13) 0.0397(16) 0.0213(14) C34 0.100(3) 0.0577(19) 0.0363(16) -0.0193(14) 0.0290(18) -0.0187(19) C35 0.0522(19) 0.068(2) 0.0459(17) -0.0039(15) 0.0147(15) -0.0328(16) C40 0.0262(11) 0.0269(10) 0.0211(11) 0.0007(9) 0.0079(9) 0.0010(9) N1 0.0378(12) 0.0340(11) 0.0240(10) -0.0020(8) 0.0110(9) 0.0007(9) N2 0.0285(11) 0.0422(11) 0.0256(10) 0.0005(8) 0.0122(9) 0.0050(9) N3 0.0272(10) 0.0324(10) 0.0283(10) 0.0022(8) 0.0062(8) 0.0024(8) N4 0.0289(10) 0.0299(10) 0.0238(10) 0.0008(8) 0.0079(8) -0.0032(8) N5 0.0285(10) 0.0393(11) 0.0265(10) 0.0011(9) 0.0075(8) 0.0035(9) N6 0.0301(10) 0.0297(10) 0.0237(9) 0.0013(8) 0.0094(8) -0.0002(8) N7 0.0287(10) 0.0313(10) 0.0230(10) -0.0028(8) 0.0073(8) -0.0031(8) N8 0.0247(10) 0.0328(10) 0.0223(9) -0.0029(8) 0.0088(8) -0.0014(8) N9 0.0358(13) 0.0701(17) 0.0323(12) 0.0115(11) 0.0043(10) -0.0170(11) N10 0.0372(13) 0.0649(16) 0.0321(12) 0.0039(11) 0.0080(11) -0.0170(11) S3 0.0360(4) 0.0595(4) 0.0273(3) 0.0056(3) 0.0032(3) -0.0127(3) S4 0.0347(4) 0.0616(4) 0.0273(3) 0.0052(3) 0.0032(3) -0.0103(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N9 1.967(2) . ? Cu1 N1 2.068(2) . ? Cu1 N3 2.097(2) . ? Cu1 S4 2.3485(9) . ? Cu2 N10 1.972(2) . ? Cu2 N7 2.060(2) . ? Cu2 N5 2.110(2) . ? Cu2 S3 2.3370(9) . ? C10 N8 1.356(3) . ? C10 C18 1.368(4) . ? C10 C25 1.485(4) . ? C12 N5 1.336(3) . ? C12 C27 1.398(4) . ? C12 C19 1.492(4) . ? C14 N6 1.447(3) . ? C14 N8 1.462(3) . ? C14 C40 1.535(3) 4_565 ? C14 H14 0.9800 . ? C15 N10 1.152(3) . ? C15 S4 1.654(3) . ? C16 N9 1.147(3) . ? C16 S3 1.654(3) . ? C17 N4 1.451(3) . ? C17 N2 1.460(3) . ? C17 C40 1.538(3) . ? C17 H17 0.9800 . ? C18 C29 1.396(4) . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N2 1.360(3) . ? C20 C33 1.364(4) . ? C20 C26 1.490(4) . ? C21 N3 1.337(3) . ? C21 C32 1.401(4) . ? C21 C31 1.488(4) . ? C22 N6 1.368(3) . ? C22 C27 1.370(4) . ? C22 C30 1.482(4) . ? C23 C29 1.496(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N1 1.334(3) . ? C24 C33 1.392(5) . ? C24 C34 1.497(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27 0.9300 . ? C28 C32 1.357(4) . ? C28 N4 1.365(3) . ? C28 C35 1.492(4) . ? C29 N7 1.334(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C40 C14 1.535(3) 4_666 ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? N1 N2 1.372(3) . ? N3 N4 1.369(3) . ? N5 N6 1.363(3) . ? N7 N8 1.372(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9 Cu1 N1 114.36(10) . . ? N9 Cu1 N3 115.99(10) . . ? N1 Cu1 N3 90.39(8) . . ? N9 Cu1 S4 105.03(7) . . ? N1 Cu1 S4 118.33(6) . . ? N3 Cu1 S4 112.90(6) . . ? N10 Cu2 N7 113.63(10) . . ? N10 Cu2 N5 111.75(10) . . ? N7 Cu2 N5 92.29(8) . . ? N10 Cu2 S3 106.24(7) . . ? N7 Cu2 S3 122.39(6) . . ? N5 Cu2 S3 109.84(6) . . ? N8 C10 C18 106.0(2) . . ? N8 C10 C25 124.0(2) . . ? C18 C10 C25 130.0(2) . . ? N5 C12 C27 110.6(2) . . ? N5 C12 C19 120.1(3) . . ? C27 C12 C19 129.3(3) . . ? N6 C14 N8 110.78(18) . . ? N6 C14 C40 114.01(18) . 4_565 ? N8 C14 C40 109.62(18) . 4_565 ? N6 C14 H14 107.4 . . ? N8 C14 H14 107.4 . . ? C40 C14 H14 107.4 4_565 . ? N10 C15 S4 179.3(3) . . ? N9 C16 S3 179.2(3) . . ? N4 C17 N2 110.20(18) . . ? N4 C17 C40 114.63(18) . . ? N2 C17 C40 109.59(18) . . ? N4 C17 H17 107.4 . . ? N2 C17 H17 107.4 . . ? C40 C17 H17 107.4 . . ? C10 C18 C29 106.7(2) . . ? C10 C18 H18 126.7 . . ? C29 C18 H18 126.7 . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C33 105.9(3) . . ? N2 C20 C26 123.4(3) . . ? C33 C20 C26 130.7(3) . . ? N3 C21 C32 110.3(2) . . ? N3 C21 C31 120.0(3) . . ? C32 C21 C31 129.6(3) . . ? N6 C22 C27 105.4(2) . . ? N6 C22 C30 124.2(2) . . ? C27 C22 C30 130.4(2) . . ? C29 C23 H23A 109.5 . . ? C29 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C29 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 C33 110.7(3) . . ? N1 C24 C34 120.7(3) . . ? C33 C24 C34 128.6(3) . . ? C10 C25 H25A 109.5 . . ? C10 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C10 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 C12 106.9(2) . . ? C22 C27 H27 126.6 . . ? C12 C27 H27 126.6 . . ? C32 C28 N4 105.9(2) . . ? C32 C28 C35 130.6(3) . . ? N4 C28 C35 123.4(3) . . ? N7 C29 C18 110.6(2) . . ? N7 C29 C23 121.1(2) . . ? C18 C29 C23 128.3(2) . . ? C22 C30 H30A 109.5 . . ? C22 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C22 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C21 C31 H31A 109.5 . . ? C21 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C21 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 C21 107.1(2) . . ? C28 C32 H32 126.4 . . ? C21 C32 H32 126.4 . . ? C20 C33 C24 106.9(2) . . ? C20 C33 H33 126.5 . . ? C24 C33 H33 126.5 . . ? C24 C34 H34A 109.5 . . ? C24 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C24 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C28 C35 H35A 109.5 . . ? C28 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C28 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C14 C40 C17 116.44(18) 4_666 . ? C14 C40 H40A 108.2 4_666 . ? C17 C40 H40A 108.2 . . ? C14 C40 H40B 108.2 4_666 . ? C17 C40 H40B 108.2 . . ? H40A C40 H40B 107.3 . . ? C24 N1 N2 104.7(2) . . ? C24 N1 Cu1 130.4(2) . . ? N2 N1 Cu1 122.80(15) . . ? C20 N2 N1 111.7(2) . . ? C20 N2 C17 129.5(2) . . ? N1 N2 C17 118.73(19) . . ? C21 N3 N4 104.8(2) . . ? C21 N3 Cu1 126.95(18) . . ? N4 N3 Cu1 119.26(14) . . ? C28 N4 N3 111.8(2) . . ? C28 N4 C17 129.0(2) . . ? N3 N4 C17 119.14(18) . . ? C12 N5 N6 104.9(2) . . ? C12 N5 Cu2 126.89(18) . . ? N6 N5 Cu2 118.16(15) . . ? N5 N6 C22 112.2(2) . . ? N5 N6 C14 118.90(18) . . ? C22 N6 C14 128.9(2) . . ? C29 N7 N8 104.82(19) . . ? C29 N7 Cu2 128.97(17) . . ? N8 N7 Cu2 122.11(14) . . ? C10 N8 N7 111.84(19) . . ? C10 N8 C14 129.1(2) . . ? N7 N8 C14 118.93(18) . . ? C16 N9 Cu1 159.4(2) . . ? C15 N10 Cu2 157.8(2) . . ? C16 S3 Cu2 95.31(9) . . ? C15 S4 Cu1 96.00(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 C10 C18 C29 -1.6(3) . . . . ? C25 C10 C18 C29 178.0(3) . . . . ? N6 C22 C27 C12 1.2(3) . . . . ? C30 C22 C27 C12 -178.0(3) . . . . ? N5 C12 C27 C22 -0.7(3) . . . . ? C19 C12 C27 C22 178.5(3) . . . . ? C10 C18 C29 N7 1.5(3) . . . . ? C10 C18 C29 C23 -176.5(2) . . . . ? N4 C28 C32 C21 -0.7(3) . . . . ? C35 C28 C32 C21 176.4(3) . . . . ? N3 C21 C32 C28 0.5(3) . . . . ? C31 C21 C32 C28 -177.1(3) . . . . ? N2 C20 C33 C24 1.0(3) . . . . ? C26 C20 C33 C24 -178.7(3) . . . . ? N1 C24 C33 C20 -1.4(3) . . . . ? C34 C24 C33 C20 179.8(3) . . . . ? N4 C17 C40 C14 -37.4(3) . . . 4_666 ? N2 C17 C40 C14 -161.95(19) . . . 4_666 ? C33 C24 N1 N2 1.1(3) . . . . ? C34 C24 N1 N2 -179.9(2) . . . . ? C33 C24 N1 Cu1 164.50(18) . . . . ? C34 C24 N1 Cu1 -16.5(4) . . . . ? N9 Cu1 N1 C24 -20.3(3) . . . . ? N3 Cu1 N1 C24 -139.2(2) . . . . ? S4 Cu1 N1 C24 104.3(2) . . . . ? N9 Cu1 N1 N2 140.51(18) . . . . ? N3 Cu1 N1 N2 21.55(18) . . . . ? S4 Cu1 N1 N2 -94.92(17) . . . . ? C33 C20 N2 N1 -0.3(3) . . . . ? C26 C20 N2 N1 179.4(3) . . . . ? C33 C20 N2 C17 -177.0(2) . . . . ? C26 C20 N2 C17 2.7(4) . . . . ? C24 N1 N2 C20 -0.5(3) . . . . ? Cu1 N1 N2 C20 -165.47(17) . . . . ? C24 N1 N2 C17 176.6(2) . . . . ? Cu1 N1 N2 C17 11.6(3) . . . . ? N4 C17 N2 C20 114.6(3) . . . . ? C40 C17 N2 C20 -118.3(3) . . . . ? N4 C17 N2 N1 -61.9(3) . . . . ? C40 C17 N2 N1 65.1(3) . . . . ? C32 C21 N3 N4 -0.1(3) . . . . ? C31 C21 N3 N4 177.8(2) . . . . ? C32 C21 N3 Cu1 -146.42(19) . . . . ? C31 C21 N3 Cu1 31.5(4) . . . . ? N9 Cu1 N3 C21 11.4(2) . . . . ? N1 Cu1 N3 C21 128.9(2) . . . . ? S4 Cu1 N3 C21 -109.9(2) . . . . ? N9 Cu1 N3 N4 -130.66(17) . . . . ? N1 Cu1 N3 N4 -13.13(17) . . . . ? S4 Cu1 N3 N4 108.07(16) . . . . ? C32 C28 N4 N3 0.7(3) . . . . ? C35 C28 N4 N3 -176.7(2) . . . . ? C32 C28 N4 C17 178.4(2) . . . . ? C35 C28 N4 C17 1.0(4) . . . . ? C21 N3 N4 C28 -0.3(3) . . . . ? Cu1 N3 N4 C28 149.11(16) . . . . ? C21 N3 N4 C17 -178.3(2) . . . . ? Cu1 N3 N4 C17 -28.9(3) . . . . ? N2 C17 N4 C28 -104.7(3) . . . . ? C40 C17 N4 C28 131.1(2) . . . . ? N2 C17 N4 N3 72.9(2) . . . . ? C40 C17 N4 N3 -51.3(3) . . . . ? C27 C12 N5 N6 -0.1(3) . . . . ? C19 C12 N5 N6 -179.4(2) . . . . ? C27 C12 N5 Cu2 144.0(2) . . . . ? C19 C12 N5 Cu2 -35.3(4) . . . . ? N10 Cu2 N5 C12 -16.7(2) . . . . ? N7 Cu2 N5 C12 -133.3(2) . . . . ? S3 Cu2 N5 C12 101.0(2) . . . . ? N10 Cu2 N5 N6 123.28(17) . . . . ? N7 Cu2 N5 N6 6.67(17) . . . . ? S3 Cu2 N5 N6 -119.08(15) . . . . ? C12 N5 N6 C22 0.9(3) . . . . ? Cu2 N5 N6 C22 -146.97(16) . . . . ? C12 N5 N6 C14 -178.5(2) . . . . ? Cu2 N5 N6 C14 33.6(2) . . . . ? C27 C22 N6 N5 -1.3(3) . . . . ? C30 C22 N6 N5 177.9(2) . . . . ? C27 C22 N6 C14 178.0(2) . . . . ? C30 C22 N6 C14 -2.8(4) . . . . ? N8 C14 N6 N5 -74.4(2) . . . . ? C40 C14 N6 N5 49.8(3) 4_565 . . . ? N8 C14 N6 C22 106.3(3) . . . . ? C40 C14 N6 C22 -129.5(2) 4_565 . . . ? C18 C29 N7 N8 -0.7(3) . . . . ? C23 C29 N7 N8 177.4(2) . . . . ? C18 C29 N7 Cu2 -157.78(18) . . . . ? C23 C29 N7 Cu2 20.3(3) . . . . ? N10 Cu2 N7 C29 24.4(2) . . . . ? N5 Cu2 N7 C29 139.4(2) . . . . ? S3 Cu2 N7 C29 -105.3(2) . . . . ? N10 Cu2 N7 N8 -129.24(17) . . . . ? N5 Cu2 N7 N8 -14.26(17) . . . . ? S3 Cu2 N7 N8 101.05(16) . . . . ? C18 C10 N8 N7 1.3(3) . . . . ? C25 C10 N8 N7 -178.3(2) . . . . ? C18 C10 N8 C14 177.0(2) . . . . ? C25 C10 N8 C14 -2.7(4) . . . . ? C29 N7 N8 C10 -0.4(3) . . . . ? Cu2 N7 N8 C10 158.70(16) . . . . ? C29 N7 N8 C14 -176.56(19) . . . . ? Cu2 N7 N8 C14 -17.5(3) . . . . ? N6 C14 N8 C10 -111.4(3) . . . . ? C40 C14 N8 C10 121.9(2) 4_565 . . . ? N6 C14 N8 N7 64.0(2) . . . . ? C40 C14 N8 N7 -62.7(2) 4_565 . . . ? S3 C16 N9 Cu1 79(21) . . . . ? N1 Cu1 N9 C16 118.3(8) . . . . ? N3 Cu1 N9 C16 -138.5(8) . . . . ? S4 Cu1 N9 C16 -13.1(8) . . . . ? S4 C15 N10 Cu2 -50(24) . . . . ? N7 Cu2 N10 C15 -150.0(7) . . . . ? N5 Cu2 N10 C15 107.2(7) . . . . ? S3 Cu2 N10 C15 -12.6(7) . . . . ? N9 C16 S3 Cu2 -70(21) . . . . ? N10 Cu2 S3 C16 3.57(14) . . . . ? N7 Cu2 S3 C16 136.35(12) . . . . ? N5 Cu2 S3 C16 -117.45(12) . . . . ? N10 C15 S4 Cu1 59(24) . . . . ? N9 Cu1 S4 C15 2.07(13) . . . . ? N1 Cu1 S4 C15 -126.97(12) . . . . ? N3 Cu1 S4 C15 129.37(11) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.620 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.118 #===END #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 787658' #TrackingRef 'JPLangCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H32 Cu3 N12' _chemical_formula_sum 'C25 H32 Cu3 N12' _chemical_formula_weight 691.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_space_group_name_Hall ' -P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.738(2) _cell_length_b 7.8457(16) _cell_length_c 15.623(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.05(3) _cell_angle_gamma 90.00 _cell_volume 1428.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6935 _cell_measurement_theta_min 3.1305 _cell_measurement_theta_max 27.4816 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 2.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4815 _exptl_absorpt_correction_T_max 0.7287 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7906 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3252 _reflns_number_gt 2810 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3252 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.96168(2) 0.59605(4) 0.236342(19) 0.02792(13) Uani 1 1 d . . . N1 N 1.16219(17) 0.5632(2) 0.38451(12) 0.0233(4) Uani 1 1 d . . . C1 C 1.3045(3) 0.5022(4) 0.51337(18) 0.0423(7) Uani 1 1 d . . . H1A H 1.3692 0.5614 0.4955 0.063 Uiso 1 1 calc R . . H1B H 1.3075 0.3844 0.4973 0.063 Uiso 1 1 calc R . . H1C H 1.3066 0.5110 0.5748 0.063 Uiso 1 1 calc R . . Cu2 Cu 1.0000 1.0000 0.0000 0.03149(15) Uani 1 2 d S . . N2 N 1.05999(16) 0.6439(2) 0.35973(12) 0.0227(4) Uani 1 1 d . . . C2 C 1.1963(2) 0.5798(3) 0.47077(16) 0.0290(5) Uani 1 1 d . . . N3 N 1.13670(16) 0.3165(2) 0.29423(12) 0.0220(4) Uani 1 1 d . . . C3 C 1.1143(2) 0.6752(4) 0.50201(16) 0.0351(6) Uani 1 1 d . . . H3 H 1.1134 0.7093 0.5589 0.042 Uiso 1 1 calc R . . N4 N 1.03617(16) 0.3479(3) 0.24203(13) 0.0234(4) Uani 1 1 d . . . C4 C 1.0312(2) 0.7125(3) 0.43249(16) 0.0288(5) Uani 1 1 d . . . N5 N 0.99643(19) 0.7384(3) 0.13944(16) 0.0356(5) Uani 1 1 d . . . C5 C 0.9225(2) 0.8103(4) 0.4331(2) 0.0402(6) Uani 1 1 d . . . H5A H 0.9378 0.9298 0.4281 0.060 Uiso 1 1 calc R . . H5B H 0.8914 0.7891 0.4861 0.060 Uiso 1 1 calc R . . H5C H 0.8682 0.7749 0.3854 0.060 Uiso 1 1 calc R . . C6 C 1.2447(2) 0.0769(3) 0.37615(18) 0.0352(6) Uani 1 1 d . . . H6A H 1.3144 0.1058 0.3531 0.053 Uiso 1 1 calc R . . H6B H 1.2373 -0.0448 0.3784 0.053 Uiso 1 1 calc R . . H6C H 1.2470 0.1230 0.4333 0.053 Uiso 1 1 calc R . . N6 N 0.79902(19) 0.5825(3) 0.24902(15) 0.0349(5) Uani 1 1 d . . . C7 C 1.1449(2) 0.1494(3) 0.31999(15) 0.0261(5) Uani 1 1 d . . . C8 C 1.0485(2) 0.0718(3) 0.28147(17) 0.0302(5) Uani 1 1 d . . . H8 H 1.0295 -0.0427 0.2859 0.036 Uiso 1 1 calc R . . C9 C 0.9830(2) 0.1967(3) 0.23373(15) 0.0259(5) Uani 1 1 d . . . C10 C 0.8699(2) 0.1752(3) 0.1796(2) 0.0364(6) Uani 1 1 d . . . H10A H 0.8188 0.2643 0.1926 0.055 Uiso 1 1 calc R . . H10B H 0.8377 0.0666 0.1917 0.055 Uiso 1 1 calc R . . H10C H 0.8806 0.1807 0.1197 0.055 Uiso 1 1 calc R . . C11 C 1.21352(18) 0.4568(3) 0.32325(14) 0.0219(4) Uani 1 1 d . . . H11 H 1.2832 0.4065 0.3541 0.026 Uiso 1 1 calc R . . C12 C 0.9999(2) 0.8327(3) 0.08297(14) 0.0249(5) Uani 1 1 d . . . C13 C 1.2500 0.5640(4) 0.2500 0.0197(6) Uani 1 2 d S . . H13A H 1.1866 0.6368 0.2274 0.024 Uiso 0.50 1 calc PR . . H13B H 1.3134 0.6368 0.2726 0.024 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02191(18) 0.0280(2) 0.0327(2) 0.00151(11) -0.00109(13) 0.00278(11) N1 0.0227(9) 0.0278(9) 0.0191(9) 0.0005(8) 0.0018(7) 0.0020(8) C1 0.0436(16) 0.0540(18) 0.0254(13) 0.0010(13) -0.0111(12) 0.0017(14) Cu2 0.0368(3) 0.0308(2) 0.0264(2) 0.00648(17) 0.00200(18) -0.00563(18) N2 0.0213(9) 0.0252(9) 0.0220(9) 0.0010(8) 0.0047(8) 0.0018(8) C2 0.0342(13) 0.0308(12) 0.0209(11) 0.0000(10) -0.0007(10) -0.0019(10) N3 0.0208(9) 0.0205(9) 0.0248(9) 0.0027(8) 0.0036(7) -0.0003(8) C3 0.0463(15) 0.0385(14) 0.0215(12) -0.0052(10) 0.0077(11) 0.0006(12) N4 0.0198(9) 0.0239(9) 0.0264(10) -0.0006(8) 0.0016(7) 0.0000(8) C4 0.0321(12) 0.0284(12) 0.0278(12) -0.0049(10) 0.0117(10) -0.0041(10) N5 0.0309(11) 0.0368(11) 0.0388(12) -0.0041(10) 0.0032(9) -0.0051(9) C5 0.0351(14) 0.0421(15) 0.0460(16) -0.0084(13) 0.0161(12) 0.0040(13) C6 0.0379(15) 0.0317(13) 0.0361(14) 0.0109(11) 0.0050(12) 0.0099(11) N6 0.0281(10) 0.0423(12) 0.0344(12) 0.0009(10) 0.0045(9) -0.0007(9) C7 0.0318(12) 0.0219(11) 0.0260(11) 0.0039(9) 0.0091(10) 0.0050(10) C8 0.0374(14) 0.0205(11) 0.0342(13) 0.0025(10) 0.0108(11) -0.0008(10) C9 0.0256(11) 0.0236(11) 0.0296(12) -0.0024(9) 0.0073(9) -0.0016(10) C10 0.0273(12) 0.0314(13) 0.0493(16) -0.0054(12) 0.0001(12) -0.0063(11) C11 0.0184(10) 0.0251(11) 0.0218(11) 0.0000(9) 0.0011(8) 0.0015(9) C12 0.0291(12) 0.0238(11) 0.0217(11) 0.0055(9) 0.0020(9) -0.0049(9) C13 0.0174(14) 0.0199(14) 0.0220(15) 0.000 0.0027(12) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 1.946(2) . ? Cu1 N5 1.964(2) . ? Cu1 N4 2.132(2) . ? Cu1 N2 2.155(2) . ? N1 C2 1.364(3) . ? N1 N2 1.369(3) . ? N1 C11 1.455(3) . ? C1 C2 1.489(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? Cu2 C12 1.845(2) 3_775 ? Cu2 C12 1.845(2) . ? N2 C4 1.338(3) . ? C2 C3 1.357(4) . ? N3 N4 1.372(3) . ? N3 C7 1.372(3) . ? N3 C11 1.459(3) . ? C3 C4 1.399(4) . ? C3 H3 0.9300 . ? N4 C9 1.340(3) . ? C4 C5 1.490(4) . ? N5 C12 1.156(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.488(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? N6 N6 1.155(4) 2_655 ? C7 C8 1.359(4) . ? C8 C9 1.402(4) . ? C8 H8 0.9300 . ? C9 C10 1.493(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.523(3) . ? C11 H11 0.9800 . ? C13 C11 1.523(3) 2_755 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cu1 N5 114.11(10) . . ? N6 Cu1 N4 110.39(9) . . ? N5 Cu1 N4 115.38(9) . . ? N6 Cu1 N2 110.05(9) . . ? N5 Cu1 N2 116.84(9) . . ? N4 Cu1 N2 87.12(7) . . ? C2 N1 N2 112.1(2) . . ? C2 N1 C11 127.5(2) . . ? N2 N1 C11 119.88(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C12 Cu2 C12 180.00(10) 3_775 . ? C4 N2 N1 104.44(19) . . ? C4 N2 Cu1 131.83(16) . . ? N1 N2 Cu1 121.80(14) . . ? C3 C2 N1 105.8(2) . . ? C3 C2 C1 131.9(2) . . ? N1 C2 C1 122.2(2) . . ? N4 N3 C7 111.71(18) . . ? N4 N3 C11 120.22(18) . . ? C7 N3 C11 127.7(2) . . ? C2 C3 C4 107.1(2) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C9 N4 N3 104.79(18) . . ? C9 N4 Cu1 128.40(15) . . ? N3 N4 Cu1 120.47(14) . . ? N2 C4 C3 110.6(2) . . ? N2 C4 C5 121.2(2) . . ? C3 C4 C5 128.2(2) . . ? C12 N5 Cu1 169.2(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N6 N6 Cu1 174.7(3) 2_655 . ? C8 C7 N3 105.9(2) . . ? C8 C7 C6 130.0(2) . . ? N3 C7 C6 124.1(2) . . ? C7 C8 C9 107.1(2) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N4 C9 C8 110.4(2) . . ? N4 C9 C10 121.7(2) . . ? C8 C9 C10 127.8(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 N3 110.32(17) . . ? N1 C11 C13 110.75(19) . . ? N3 C11 C13 113.75(18) . . ? N1 C11 H11 107.2 . . ? N3 C11 H11 107.2 . . ? C13 C11 H11 107.2 . . ? N5 C12 Cu2 174.1(2) . . ? C11 C13 C11 113.0(3) 2_755 . ? C11 C13 H13A 109.0 2_755 . ? C11 C13 H13A 109.0 . . ? C11 C13 H13B 109.0 2_755 . ? C11 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 N2 C4 0.4(2) . . . . ? C11 N1 N2 C4 173.0(2) . . . . ? C2 N1 N2 Cu1 -165.50(16) . . . . ? C11 N1 N2 Cu1 7.1(3) . . . . ? N6 Cu1 N2 C4 -22.6(2) . . . . ? N5 Cu1 N2 C4 109.6(2) . . . . ? N4 Cu1 N2 C4 -133.3(2) . . . . ? N6 Cu1 N2 N1 138.90(16) . . . . ? N5 Cu1 N2 N1 -88.88(18) . . . . ? N4 Cu1 N2 N1 28.22(16) . . . . ? N2 N1 C2 C3 -0.6(3) . . . . ? C11 N1 C2 C3 -172.5(2) . . . . ? N2 N1 C2 C1 179.6(2) . . . . ? C11 N1 C2 C1 7.7(4) . . . . ? N1 C2 C3 C4 0.5(3) . . . . ? C1 C2 C3 C4 -179.7(3) . . . . ? C7 N3 N4 C9 -1.6(3) . . . . ? C11 N3 N4 C9 -175.05(19) . . . . ? C7 N3 N4 Cu1 152.68(15) . . . . ? C11 N3 N4 Cu1 -20.8(3) . . . . ? N6 Cu1 N4 C9 16.0(2) . . . . ? N5 Cu1 N4 C9 -115.2(2) . . . . ? N2 Cu1 N4 C9 126.4(2) . . . . ? N6 Cu1 N4 N3 -131.57(16) . . . . ? N5 Cu1 N4 N3 97.23(17) . . . . ? N2 Cu1 N4 N3 -21.23(16) . . . . ? N1 N2 C4 C3 -0.1(3) . . . . ? Cu1 N2 C4 C3 163.80(18) . . . . ? N1 N2 C4 C5 -179.0(2) . . . . ? Cu1 N2 C4 C5 -15.1(4) . . . . ? C2 C3 C4 N2 -0.3(3) . . . . ? C2 C3 C4 C5 178.5(3) . . . . ? N6 Cu1 N5 C12 18.2(12) . . . . ? N4 Cu1 N5 C12 147.6(11) . . . . ? N2 Cu1 N5 C12 -112.1(11) . . . . ? N5 Cu1 N6 N6 1(2) . . . 2_655 ? N4 Cu1 N6 N6 -131(2) . . . 2_655 ? N2 Cu1 N6 N6 134(2) . . . 2_655 ? N4 N3 C7 C8 1.5(3) . . . . ? C11 N3 C7 C8 174.4(2) . . . . ? N4 N3 C7 C6 179.3(2) . . . . ? C11 N3 C7 C6 -7.8(4) . . . . ? N3 C7 C8 C9 -0.8(3) . . . . ? C6 C7 C8 C9 -178.4(2) . . . . ? N3 N4 C9 C8 1.0(3) . . . . ? Cu1 N4 C9 C8 -150.45(17) . . . . ? N3 N4 C9 C10 -178.8(2) . . . . ? Cu1 N4 C9 C10 29.7(3) . . . . ? C7 C8 C9 N4 -0.1(3) . . . . ? C7 C8 C9 C10 179.7(2) . . . . ? C2 N1 C11 N3 110.7(3) . . . . ? N2 N1 C11 N3 -60.6(3) . . . . ? C2 N1 C11 C13 -122.4(2) . . . . ? N2 N1 C11 C13 66.2(2) . . . . ? N4 N3 C11 N1 69.6(2) . . . . ? C7 N3 C11 N1 -102.7(2) . . . . ? N4 N3 C11 C13 -55.5(3) . . . . ? C7 N3 C11 C13 132.1(2) . . . . ? Cu1 N5 C12 Cu2 48(3) . . . . ? C12 Cu2 C12 N5 -70(100) 3_775 . . . ? N1 C11 C13 C11 -170.76(19) . . . 2_755 ? N3 C11 C13 C11 -45.84(13) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.683 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.116 #===END