Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Kojima, Masaaki' 'Akashi, H.' 'Hirotsu, Masakazu' 'Kambe, Takashi' 'Kashino, Setsuo' 'Nakajima, Kiyohiko' 'Saimiya, Hiromi' 'Tokii, Tadashi' _publ_contact_author_name 'Prof Masaaki Kojima' _publ_contact_author_address ; Department of Chemistry, Faculty of Science, Okayama University, Tsushima, Okayama 700-8530, Japan ; _publ_requested_journal 'J. Chem. Soc. Dalton Trans' _publ_requested_coeditor_name ? ? _publ_contact_author_phone ? '+81-86-251-7842' _publ_contact_author_fax ? '+81-86-251-7842' _publ_contact_author_email ? 'kojima@cc.okayama-u.ac.jp' #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Antiferromagnetism induced by successive protonation of terminal phenol groups of a bis(µ-phenoxide)-bridged dicopper(II,II) complex ; #============================================================================== _publ_section_references ; Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; #============================================================================== data_compound1 #[Cu(HL1)2 2](NO3) .H2O______ _database_code_CSD 179771 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 ' _computing_publication_material 'teXsan for Windows version 1.06 ' #------------------------------------------------------------------------------ _cell_length_a 22.438(10) _cell_length_b 19.620(10) _cell_length_c 17.301(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7618(6) _cell_formula_units_Z 8 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.6 _cell_measurement_theta_max 11.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbca' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall '-P2ac2ab' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2+x,1/2-y,-z' '-x,1/2+y,1/2-z' '1/2-x,-y,1/2+z' '-x,-y, -z' '1/2-x,1/2+y,+z' '+x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 867.90 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H48 Cu2 N6 O11 ' _chemical_formula_moiety 'C36 H44 Cu2 N6 O11 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3616.00 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type 'omega scans' _exptl_absorpt_process_details 'North,Phillips & Matthews, 1968' _exptl_absorpt_correction_T_max 0.624 _exptl_absorpt_correction_T_min 0.493 _exptl_special_details ; The scan width was (1.26+0.30tan q) ¥ % with an ¥ w ¥ scan speed of 4 % per minute ¥ (up to 2 scans to achieve I/ s(I) > 10). ¥ Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method 'w-2 q' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 -3 -1 2 -3 1 3 -3 _diffrn_reflns_number 6983 _reflns_number_total 6983 _reflns_number_gt 5305 _reflns_threshold_expression 'I>0.85 s(I)' _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.105 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04207 _diffrn_orient_matrix_UB_12 0.01508 _diffrn_orient_matrix_UB_13 -0.00843 _diffrn_orient_matrix_UB_21 0.01321 _diffrn_orient_matrix_UB_22 0.04867 _diffrn_orient_matrix_UB_23 0.00094 _diffrn_orient_matrix_UB_31 0.00644 _diffrn_orient_matrix_UB_32 -0.00141 _diffrn_orient_matrix_UB_33 -0.05717 #------------------------------------------------------------------------------ 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 C 0 288 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 384 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 48 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 88 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cu 0 16 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.11144(4) 0.19818(5) 0.23462(6) 0.0324(3) 1.000 . Uani d ? Cu(2) 0.21671(4) 0.29488(5) 0.26065(5) 0.0307(3) 1.000 . Uani d ? O(1) 0.1992(2) 0.2024(3) 0.2274(3) 0.0391(15) 1.000 . Uani d ? O(2) 0.1074(3) 0.1300(3) 0.3476(3) 0.0440(18) 1.000 . Uani d ? O(3) 0.1324(2) 0.2803(3) 0.2898(3) 0.0365(15) 1.000 . Uani d ? O(4) 0.2527(3) 0.2603(3) 0.3784(4) 0.056(2) 1.000 . Uani d ? O(5) 0.1081(4) 0.1801(4) 0.4931(4) 0.103(3) 1.000 . Uani d ? O(6) 0.1507(4) 0.0869(5) 0.5162(6) 0.118(4) 1.000 . Uani d ? O(7) 0.1318(4) 0.1571(6) 0.6063(5) 0.134(4) 1.000 . Uani d ? O(8) 0.3880(4) 0.0498(6) 0.5464(7) 0.143(5) 1.000 . Uani d ? O(9) 0.3187(4) 0.0447(5) 0.4710(6) 0.120(4) 1.000 . Uani d ? O(10) 0.3927(5) 0.1054(5) 0.4425(7) 0.148(5) 1.000 . Uani d ? O(11) 0.2438(3) 0.1319(4) 0.4108(4) 0.076(3) 1.000 . Uani d ? N(1) 0.1078(3) 0.1129(3) 0.1705(4) 0.0317(18) 1.000 . Uani d ? N(2) 0.0238(3) 0.2184(3) 0.2015(4) 0.041(2) 1.000 . Uani d ? N(3) 0.2190(3) 0.3925(3) 0.2998(4) 0.0363(19) 1.000 . Uani d ? N(4) 0.2817(3) 0.3231(3) 0.1836(4) 0.041(2) 1.000 . Uani d ? N(5) 0.1304(4) 0.1420(6) 0.5388(6) 0.077(4) 1.000 . Uani d ? N(6) 0.3679(5) 0.0680(5) 0.4856(6) 0.077(4) 1.000 . Uani d ? C(1) 0.2371(4) 0.1545(4) 0.1987(5) 0.036(2) 1.000 . Uani d ? C(2) 0.2936(4) 0.1454(4) 0.2297(5) 0.046(3) 1.000 . Uani d ? C(3) 0.3317(4) 0.0973(5) 0.1960(6) 0.049(3) 1.000 . Uani d ? C(4) 0.3150(4) 0.0562(5) 0.1356(6) 0.052(3) 1.000 . Uani d ? C(5) 0.2584(4) 0.0626(4) 0.1079(5) 0.046(3) 1.000 . Uani d ? C(6) 0.2182(4) 0.1121(4) 0.1389(5) 0.039(3) 1.000 . Uani d ? C(7) 0.1547(4) 0.1197(4) 0.1086(5) 0.047(3) 1.000 . Uani d ? C(8) 0.1169(4) 0.0485(4) 0.2165(4) 0.042(3) 1.000 . Uani d ? C(9) 0.0709(3) 0.0365(4) 0.2790(5) 0.037(2) 1.000 . Uani d ? C(10) 0.0300(4) -0.0169(4) 0.2724(5) 0.052(3) 1.000 . Uani d ? C(11) -0.0102(4) -0.0294(5) 0.3288(6) 0.059(3) 1.000 . Uani d ? C(12) -0.0131(4) 0.0099(5) 0.3926(5) 0.048(3) 1.000 . Uani d ? C(13) 0.0275(4) 0.0621(4) 0.3998(5) 0.047(3) 1.000 . Uani d ? C(14) 0.0688(4) 0.0749(4) 0.3450(5) 0.035(2) 1.000 . Uani d ? C(15) 0.0478(4) 0.1126(4) 0.1312(5) 0.040(3) 1.000 . Uani d ? C(16) 0.0247(4) 0.1851(5) 0.1234(5) 0.049(3) 1.000 . Uani d ? C(17) 0.0111(4) 0.2918(4) 0.1882(5) 0.053(3) 1.000 . Uani d ? C(18) -0.0240(3) 0.1878(5) 0.2509(5) 0.053(3) 1.000 . Uani d ? C(19) 0.0989(4) 0.3218(5) 0.3334(5) 0.043(3) 1.000 . Uani d ? C(20) 0.0531(4) 0.2961(5) 0.3812(4) 0.045(3) 1.000 . Uani d ? C(21) 0.0169(4) 0.3397(6) 0.4196(5) 0.063(3) 1.000 . Uani d ? C(22) 0.0277(4) 0.4122(5) 0.4181(5) 0.057(3) 1.000 . Uani d ? C(23) 0.0749(4) 0.4360(5) 0.3748(5) 0.048(3) 1.000 . Uani d ? C(24) 0.1104(4) 0.3935(4) 0.3306(5) 0.038(2) 1.000 . Uani d ? C(25) 0.1599(4) 0.4217(4) 0.2842(5) 0.039(3) 1.000 . Uani d ? C(26) 0.2350(4) 0.3997(4) 0.3843(5) 0.044(3) 1.000 . Uani d ? C(27) 0.2928(4) 0.3689(4) 0.4087(5) 0.037(2) 1.000 . Uani d ? C(28) 0.3388(4) 0.4086(5) 0.4339(5) 0.055(3) 1.000 . Uani d ? C(29) 0.3905(5) 0.3789(6) 0.4614(6) 0.069(4) 1.000 . Uani d ? C(30) 0.3962(4) 0.3109(6) 0.4626(6) 0.060(3) 1.000 . Uani d ? C(31) 0.3505(4) 0.2685(5) 0.4361(5) 0.050(3) 1.000 . Uani d ? C(32) 0.2983(4) 0.2974(5) 0.4092(5) 0.045(3) 1.000 . Uani d ? C(33) 0.2646(4) 0.4300(4) 0.2540(5) 0.043(3) 1.000 . Uani d ? C(34) 0.2685(4) 0.3980(4) 0.1746(5) 0.042(3) 1.000 . Uani d ? C(35) 0.2752(4) 0.2919(5) 0.1059(5) 0.056(3) 1.000 . Uani d ? C(36) 0.3437(4) 0.3138(5) 0.2123(6) 0.056(3) 1.000 . Uani d ? H(1) 0.3713 0.0900 0.2152 0.052 1.000 . Uiso c ? H(2) 0.3597 0.2185 0.4370 0.072 1.000 . Uiso c ? H(3) 0.0796 0.4847 0.3759 0.060 1.000 . Uiso c ? H(4) -0.0438 -0.0001 0.4316 0.057 1.000 . Uiso c ? H(5) 0.2427 0.0336 0.0652 0.058 1.000 . Uiso c ? H(6) 0.4354 0.2921 0.4841 0.074 1.000 . Uiso c ? H(7) -0.0388 -0.0684 0.3230 0.062 1.000 . Uiso c ? H(8) 0.0441 0.2473 0.3846 0.057 1.000 . Uiso c ? H(9) 0.3066 0.1722 0.2741 0.055 1.000 . Uiso c ? H(10) 0.0304 -0.0472 0.2258 0.063 1.000 . Uiso c ? H(11) 0.3412 0.4586 0.4344 0.074 1.000 . Uiso c ? H(12) 0.0013 0.4430 0.4481 0.058 1.000 . Uiso c ? H(13) 0.3434 0.0241 0.1107 0.057 1.000 . Uiso c ? H(14) 0.0251 0.0892 0.4480 0.059 1.000 . Uiso c ? H(15) -0.0163 0.3248 0.4547 0.065 1.000 . Uiso c ? H(16) 0.4265 0.4080 0.4808 0.077 1.000 . Uiso c ? H(17) 0.2009 0.3778 0.4144 0.052 1.000 . Uiso c ? H(18) 0.2304 0.4480 0.3987 0.052 1.000 . Uiso c ? H(19) 0.3025 0.4288 0.2796 0.047 1.000 . Uiso c ? H(20) 0.2534 0.4782 0.2507 0.047 1.000 . Uiso c ? H(21) 0.1485 0.4152 0.2314 0.047 1.000 . Uiso c ? H(22) 0.1600 0.4706 0.2935 0.047 1.000 . Uiso c ? H(23) 0.1479 0.1642 0.0834 0.046 1.000 . Uiso c ? H(24) 0.1450 0.0863 0.0682 0.046 1.000 . Uiso c ? H(25) 0.2311 0.4040 0.1474 0.050 1.000 . Uiso c ? H(26) 0.2986 0.4207 0.1436 0.050 1.000 . Uiso c ? H(27) 0.0188 0.0858 0.1614 0.046 1.000 . Uiso c ? H(28) 0.0494 0.0902 0.0811 0.046 1.000 . Uiso c ? H(29) 0.0481 0.2095 0.0866 0.060 1.000 . Uiso c ? H(30) -0.0166 0.1846 0.1011 0.060 1.000 . Uiso c ? H(31) 0.1555 0.0504 0.2376 0.046 1.000 . Uiso c ? H(32) 0.1165 0.0109 0.1785 0.046 1.000 . Uiso c ? H(33) 0.0083 0.3002 0.1319 0.064 1.000 . Uiso c ? H(34) 0.0390 0.3190 0.2094 0.064 1.000 . Uiso c ? H(35) -0.0284 0.3015 0.2078 0.064 1.000 . Uiso c ? H(36) 0.3727 0.3094 0.1670 0.064 1.000 . Uiso c ? H(37) 0.3500 0.2741 0.2416 0.064 1.000 . Uiso c ? H(38) 0.3591 0.3524 0.2401 0.064 1.000 . Uiso c ? H(39) 0.2824 0.3245 0.0647 0.065 1.000 . Uiso c ? H(40) 0.2395 0.2700 0.0983 0.065 1.000 . Uiso c ? H(41) 0.3077 0.2568 0.0976 0.065 1.000 . Uiso c ? H(42) -0.0544 0.1691 0.2187 0.062 1.000 . Uiso c ? H(43) -0.0398 0.2223 0.2823 0.062 1.000 . Uiso c ? H(44) -0.0067 0.1528 0.2810 0.062 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) 0.0295(5) 0.0339(6) 0.0337(5) -0.0005(4) -0.0020(5) -0.0035(5) Cu(2) 0.0293(5) 0.0324(5) 0.0304(5) -0.0016(4) 0.0012(5) -0.0028(5) O(1) 0.030(3) 0.039(3) 0.048(3) -0.003(3) 0.000(3) -0.014(3) O(2) 0.051(4) 0.044(4) 0.037(3) -0.014(3) -0.007(3) 0.005(3) O(3) 0.033(3) 0.031(3) 0.046(3) -0.005(2) 0.010(3) -0.011(3) O(4) 0.065(5) 0.055(4) 0.048(4) -0.006(3) -0.017(3) 0.005(3) O(5) 0.166(9) 0.069(5) 0.074(5) 0.022(5) -0.055(6) 0.001(4) O(6) 0.104(8) 0.098(7) 0.153(10) 0.016(6) -0.019(7) 0.025(7) O(7) 0.089(7) 0.273(13) 0.041(5) 0.047(8) 0.005(5) 0.016(7) O(8) 0.083(7) 0.182(11) 0.164(11) -0.017(7) 0.005(8) 0.014(9) O(9) 0.080(6) 0.105(7) 0.174(10) -0.024(6) -0.045(7) 0.014(7) O(10) 0.169(10) 0.080(7) 0.195(12) -0.021(6) 0.071(9) 0.059(7) O(11) 0.067(5) 0.074(5) 0.086(6) -0.004(4) -0.004(4) 0.021(4) N(1) 0.026(4) 0.038(4) 0.031(4) -0.007(3) -0.002(3) -0.006(3) N(2) 0.038(4) 0.047(4) 0.037(4) -0.001(3) -0.008(3) 0.001(3) N(3) 0.037(4) 0.038(4) 0.034(4) 0.004(3) 0.000(3) 0.001(3) N(4) 0.042(4) 0.043(4) 0.038(4) 0.002(3) 0.012(4) -0.002(3) N(5) 0.069(7) 0.115(9) 0.046(6) -0.021(7) -0.026(5) 0.030(7) N(6) 0.095(9) 0.061(7) 0.074(8) 0.044(6) -0.036(7) -0.020(6) C(1) 0.042(5) 0.025(4) 0.040(5) -0.007(4) 0.006(4) 0.001(4) C(2) 0.040(5) 0.048(5) 0.050(5) -0.004(4) -0.008(5) 0.001(5) C(3) 0.034(5) 0.045(6) 0.067(7) 0.007(4) 0.001(5) 0.003(5) C(4) 0.032(5) 0.051(6) 0.072(7) 0.001(5) 0.023(5) 0.005(5) C(5) 0.057(6) 0.035(5) 0.045(5) -0.002(4) 0.024(5) -0.005(4) C(6) 0.040(5) 0.049(5) 0.029(5) -0.004(4) 0.001(4) 0.005(4) C(7) 0.058(6) 0.043(5) 0.040(5) -0.011(5) 0.004(5) -0.003(4) C(8) 0.056(6) 0.037(5) 0.034(5) 0.021(4) -0.014(5) -0.003(4) C(9) 0.031(4) 0.035(5) 0.045(6) 0.007(4) -0.003(4) 0.021(4) C(10) 0.064(6) 0.037(5) 0.056(6) 0.003(5) -0.012(6) -0.001(5) C(11) 0.053(6) 0.060(6) 0.063(7) -0.029(5) 0.005(6) 0.021(6) C(12) 0.047(6) 0.051(6) 0.047(6) -0.005(5) 0.011(5) 0.012(5) C(13) 0.062(6) 0.050(6) 0.029(5) 0.005(5) 0.006(5) 0.008(4) C(14) 0.035(5) 0.036(5) 0.035(5) 0.003(4) -0.011(4) -0.001(4) C(15) 0.037(5) 0.042(5) 0.041(5) -0.002(4) -0.004(4) -0.012(4) C(16) 0.041(5) 0.061(6) 0.046(5) -0.001(5) -0.014(4) -0.002(5) C(17) 0.063(6) 0.031(5) 0.066(6) 0.018(5) -0.022(5) 0.002(5) C(18) 0.023(4) 0.068(6) 0.068(7) 0.003(4) -0.001(5) -0.010(5) C(19) 0.033(5) 0.065(6) 0.030(5) 0.010(4) -0.004(4) -0.002(4) C(20) 0.031(5) 0.074(6) 0.030(4) -0.001(5) 0.009(4) -0.006(5) C(21) 0.053(6) 0.108(9) 0.028(5) 0.003(6) 0.008(5) 0.010(6) C(22) 0.057(7) 0.074(7) 0.041(6) 0.033(6) -0.018(5) -0.013(5) C(23) 0.039(5) 0.063(6) 0.041(6) 0.008(5) -0.007(5) -0.011(5) C(24) 0.032(5) 0.049(5) 0.032(5) 0.015(4) -0.008(4) -0.007(4) C(25) 0.040(5) 0.039(5) 0.038(5) 0.006(4) -0.003(4) 0.007(4) C(26) 0.061(6) 0.039(5) 0.032(5) 0.002(4) 0.003(5) -0.010(4) C(27) 0.040(5) 0.045(5) 0.026(4) 0.007(4) -0.010(4) -0.011(4) C(28) 0.049(6) 0.068(7) 0.047(6) -0.008(5) -0.007(5) -0.016(5) C(29) 0.045(6) 0.112(10) 0.049(6) -0.006(7) -0.010(5) -0.017(7) C(30) 0.045(6) 0.091(8) 0.045(6) 0.023(6) 0.004(5) -0.001(6) C(31) 0.057(6) 0.064(6) 0.030(5) 0.025(5) 0.006(5) 0.004(5) C(32) 0.041(5) 0.069(6) 0.025(4) 0.007(5) -0.001(4) 0.006(5) C(33) 0.045(5) 0.047(5) 0.036(5) -0.006(4) 0.006(4) 0.003(4) C(34) 0.033(5) 0.049(5) 0.043(5) -0.001(4) 0.006(4) 0.010(4) C(35) 0.069(7) 0.050(6) 0.050(6) -0.004(5) 0.013(5) -0.004(5) C(36) 0.032(5) 0.054(6) 0.082(7) 0.007(4) 0.009(5) 0.007(5) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _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) + 0.00181¦Fo¦^2^]' _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 5305 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.1060 _refine_ls_wR_factor_all 0.1080 _refine_ls_wR_factor_ref 0.1080 _refine_ls_goodness_of_fit_all 1.469 _refine_ls_goodness_of_fit_ref 1.470 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -0.72 _refine_diff_density_max 0.69 #============================================================================== # MOLECULAR GEOMETRY _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 CU1 CU2 3.0629(18) . . ? CU1 O1 1.975(6) . . ? CU1 O2 2.371(7) . . ? CU1 O3 1.931(6) . . ? CU1 N1 2.009(7) . . ? CU1 N2 2.088(8) . . ? CU2 O1 1.943(6) . . ? CU2 O3 1.980(6) . . ? CU2 O4 2.294(7) . . ? CU2 N3 2.032(8) . . ? CU2 N4 2.053(8) . . ? O1 C1 1.361(11) . . ? O2 C14 1.386(11) . . ? O3 C19 1.341(11) . . ? O4 C32 1.364(12) . . ? O5 N5 1.198(12) . . ? O6 N5 1.235(15) . . ? O7 N5 1.205(14) . . ? O8 N6 1.199(15) . . ? O9 N6 1.222(14) . . ? O10 N6 1.185(15) . . ? N1 C7 1.507(12) . . ? N1 C8 1.509(12) . . ? N1 C15 1.507(11) . . ? N2 C16 1.502(13) . . ? N2 C17 1.485(12) . . ? N2 C18 1.495(12) . . ? N3 C25 1.472(11) . . ? N3 C26 1.512(12) . . ? N3 C33 1.488(12) . . ? N4 C34 1.506(12) . . ? N4 C35 1.484(13) . . ? N4 C36 1.489(13) . . ? C1 C2 1.389(13) . . ? C1 C6 1.393(13) . . ? C2 C3 1.401(14) . . ? C2 H9 0.98 . . no C3 C4 1.371(15) . . ? C3 H1 0.96 . . no C4 C5 1.361(14) . . ? C4 H13 1.00 . . no C5 C6 1.430(13) . . ? C5 H5 1.00 . . no C6 C7 1.526(13) . . ? C7 H23 0.99 . . no C7 H24 0.98 . . no C8 C9 1.512(14) . . ? C8 H31 0.94 . . no C8 H32 0.99 . . no C9 C10 1.397(14) . . ? C9 C14 1.370(13) . . ? C10 C11 1.353(15) . . ? C10 H10 1.00 . . no C11 C12 1.347(14) . . ? C11 H7 1.00 . . no C12 C13 1.377(14) . . ? C12 H4 0.98 . . no C13 C14 1.350(13) . . ? C13 H14 0.99 . . no C15 C16 1.521(14) . . ? C15 H27 0.99 . . no C15 H28 0.97 . . no C16 H29 0.95 . . no C16 H30 1.00 . . no C17 H33 0.99 . . no C17 H34 0.90 . . no C17 H35 0.97 . . no C18 H42 0.95 . . no C18 H43 0.94 . . no C18 H44 0.95 . . no C19 C20 1.411(13) . . ?? C19 C24 1.431(14) . . ? C20 C21 1.354(14) . . ? C20 H8 0.98 . . no C21 C22 1.443(16) . . ? C21 H15 1.01 . . no C22 C23 1.378(15) . . ? C22 H12 0.99 . . no C23 C24 1.385(13) . . ? C23 H3 0.96 . . no C24 C25 1.478(13) . . ? C25 H21 0.96 . . no C25 H22 0.97 . . no C26 C27 1.492(13) . . ? C26 H17 1.02 . . no C26 H18 0.98 . . no C27 C28 1.365(13) . . ? C27 C32 1.410(14) . . ? C28 C29 1.382(15) . . ? C28 H11 0.98 . . no C29 C30 1.339(16) . . ? C29 H16 1.05 . . no C30 C31 1.398(16) . . ? C30 H6 1.02 . . no C31 C32 1.382(14) . . ? C31 H2 1.00 . . no C33 C34 1.513(14) . . ? C33 H19 0.96 . . no C33 H20 0.98 . . no C34 H25 0.97 . . no C34 H26 0.97 . . no C35 H39 0.97 . . no C35 H40 0.92 . . no C35 H41 1.01 . . no C36 H36 1.02 . . no C36 H37 0.94 . . no C36 H38 0.96 . . 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 O1 CU1 O2 96.5(3) . . . ? O1 CU1 O3 75.8(3) . . . ? O1 CU1 N1 92.3(3) . . . ? O1 CU1 N2 156.1(3) . . . ? O2 CU1 O3 94.2(3) . . . ? O2 CU1 N1 89.1(3) . . . ? O2 CU1 N2 107.3(3) . . . ? O3 CU1 N1 167.9(3) . . . ? O3 CU1 N2 101.9(3) . . . ? N1 CU1 N2 88.2(3) . . . ? O1 CU2 O3 75.4(2) . . . ? O1 CU2 O4 93.4(3) . . . ? O1 CU2 N3 169.6(3) . . . ? O1 CU2 N4 101.7(3) . . . ? O3 CU2 O4 93.9(3) . . . ? O3 CU2 N3 94.3(3) . . . ? O3 CU2 N4 152.1(3) . . . ? O4 CU2 N3 88.5(3) . . . ? O4 CU2 N4 114.0(3) . . . ? N3 CU2 N4 86.8(3) . . . ? CU1 O1 CU2 102.8(3) . . . ? CU1 O1 C1 128.1(6) . . . ? CU2 O1 C1 128.8(6) . . . ? CU1 O2 C14 115.9(6) . . . ? CU1 O3 CU2 103.1(3) . . . ? CU1 O3 C19 130.5(6) . . . ? CU2 O3 C19 126.3(6) . . . ? CU2 O4 C32 117.0(6) . . . ? CU1 N1 C7 106.9(5) . . . ? CU1 N1 C8 113.6(5) . . . ? CU1 N1 C15 106.8(5) . . . ? CU1 N2 C16 98.7(6) . . . ? CU1 N2 C17 114.0(6) . . . ? CU1 N2 C18 116.2(6) . . . ? CU2 N3 C25 106.5(6) . . . ? CU2 N3 C26 114.6(6) . . . ? CU2 N3 C33 107.8(6) . . . ? CU2 N4 C34 100.9(6) . . . ? CU2 N4 C35 114.0(7) . . . ? CU2 N4 C36 114.4(6) . . . ? O5 N5 O6 119.5(13) . . . ? O5 N5 O7 119.7(16) . . . ? O8 N6 O9 114.2(17) . . . ? O8 N6 O10 124.0(18) . . . ? O1 C1 C2 121.3(9) . . . ? C1 C2 C3 118.9(10) . . . ? C1 C2 H9 120.6 . . . no C3 C2 H9 120.6 . . . no C2 C3 C4 123.1(10) . . . ? C2 C3 H1 121.4 . . . no C4 C3 H1 115.4 . . . no C4 C5 C6 121.3(10) . . . ? C4 C5 H5 122.5 . . . no C6 C5 H5 116.2 . . . no C5 C6 C7 121.8(9) . . . ? C5 C6 H23 129.0 . . . no C7 C6 H23 25.6 . . . no N1 C7 C6 113.5(8) . . . ? N1 C7 H23 106.5 . . . no N1 C7 H24 107.1 . . . no C6 C7 H23 112.4 . . . no C6 C7 H24 112.7 . . . no N1 C8 C9 114.5(8) . . . ? N1 C8 H31 107.2 . . . no N1 C8 H32 105.8 . . . no C9 C8 H31 111.0 . . . no C9 C8 H32 110.7 . . . no C8 C9 C10 120.5(10) . . . ? C8 C9 C14 122.3(9) . . . ? C9 C10 C11 121.0(11) . . . ? C9 C10 H10 120.4 . . . no C11 C10 H10 118.6 . . . no C10 C11 C12 121.3(10) . . . ? C10 C11 H7 119.5 . . . no C12 C11 H7 119.2 . . . no C11 C12 C13 117.9(10) . . . ? C11 C12 H4 118.8 . . . no C13 C12 H4 123.3 . . . no C12 C13 C14 121.9(10) . . . ? C12 C13 H14 116.0 . . . no C14 C13 H14 122.0 . . . no O2 C14 C9 115.8(9) . . . ? O2 C14 C13 123.5(9) . . . ? C9 C14 C13 120.5(10) . . . ? N1 C15 C16 110.0(7) . . . ? N1 C15 H27 110.7 . . . no N1 C15 H28 111.8 . . . no C16 C15 H27 108.7 . . . no C16 C15 H28 110.8 . . . no N2 C16 C15 109.4(8) . . . ? N2 C16 H29 112.9 . . . no N2 C16 H30 109.7 . . . no C15 C16 H29 109.9 . . . no C15 C16 H30 110.0 . . . no H29 C16 H30 104.9 . . . no N2 C17 H33 109.1 . . . no N2 C17 H34 112.2 . . . no N2 C17 H35 108.2 . . . no H33 C17 H34 110.1 . . . no H33 C17 H35 104.8 . . . no H34 C17 H35 112.1 . . . no N2 C18 H42 109.5 . . . no N2 C18 H43 108.2 . . . no N2 C18 H44 108.3 . . . no H42 C18 H43 110.2 . . . no H42 C18 H44 109.5 . . . no H43 C18 H44 111.0 . . . no O3 C19 C20 121.4(10) . . . ? O3 C19 C24 118.4(9) . . . ? C19 C20 C21 119.9(11) . . . ? C19 C20 H8 122.3 . . . no C21 C20 H8 117.6 . . . no C20 C21 C22 120.8(11) . . . ? C20 C21 H15 123.9 . . . no C22 C21 H15 115.1 . . . no C21 C22 C23 118.3(10) . . . ? C21 C22 H12 119.3 . . . no C23 C22 H12 122.3 . . . no C22 C23 C24 122.5(11) . . . ? C22 C23 H3 114.3 . . . no C24 C23 H3 123.1 . . . no C19 C24 C23 118.0(10) . . . ? C19 C24 C25 121.6(9) . . . ? C23 C24 C25 120.4(10) . . . ? N3 C25 H21 111.3 . . . no N3 C25 H22 110.6 . . . no C24 C25 H21 105.5 . . . no C24 C25 H22 106.4 . . . no N3 C26 C27 116.1(8) . . . ? N3 C26 H17 106.1 . . . no N3 C26 H18 108.1 . . . no C27 C26 H17 109.7 . . . no C27 C26 H18 114.1 . . . no H17 C26 H18 101.5 . . . no C26 C27 C28 121.2(10) . . . ? C26 C27 C32 118.8(9) . . . ? C28 C27 C32 120.0(10) . . . ? C27 C28 C29 120.3(11) . . . ? C27 C28 H11 127.9 . . . no C29 C28 H11 111.8 . . . no C28 C29 C30 120.3(12) . . . ? C28 C29 H16 121.9 . . . no C30 C29 H16 117.8 . . . no C29 C30 C31 121.2(11) . . . ? C29 C30 H6 116.5 . . . no C31 C30 H6 122.3 . . . no C30 C31 C32 119.2(11) . . . ? C30 C31 H2 115.2 . . . no C32 C31 H2 125.6 . . . no O4 C32 C27 117.5(9) . . . ? O4 C32 C31 123.3(11) . . . ? C27 C32 C31 119.0(11) . . . ? N3 C33 C34 108.5(8) . . . ? N3 C33 H19 110.6 . . . no N3 C33 H20 109.3 . . . no C34 C33 H19 111.1 . . . no C34 C33 H20 111.2 . . . no N4 C34 C33 108.8(8) . . . ? N4 C34 H25 109.9 . . . no N4 C34 H26 111.5 . . . no C33 C34 H25 110.0 . . . no C33 C34 H26 110.5 . . . no H25 C34 H26 106.2 . . . no N4 C35 H39 112.1 . . . no N4 C35 H40 114.2 . . . no N4 C35 H41 109.8 . . . no H39 C35 H40 110.4 . . . no H39 C35 H41 102.8 . . . no H40 C35 H41 106.8 . . . no N4 C36 H36 110.5 . . . no N4 C36 H37 114.9 . . . no N4 C36 H38 113.8 . . . no H36 C36 H37 104.4 . . . no H36 C36 H38 102.8 . . . no H37 C36 H38 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 ? ? ? ? ? ? #------------------------------------------------------------------------------ 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 ? ? ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================= #------------------------------------------------------------------------------ data_compound2 #[Cu2(L)2] _database_code_CSD 179770 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C36 H44 Cu2 N4 O4 ' _chemical_formula_moiety '[Cu2(L)2]' _chemical_formula_weight 723.86 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.608(1) _cell_length_b 9.692(2) _cell_length_c 9.180(1) _cell_angle_alpha 104.337(7) _cell_angle_beta 102.475(5) _cell_angle_gamma 87.414(6) _cell_volume 808.6(2) _cell_formula_units_Z 1 _cell_measurement_reflns_used 5376 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 298.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.767 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K a' _diffrn_radiarion_monochromator 'graphite' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4699 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9519 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9519 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3521 _reflns_number_gt 3110 _reflns_threshold_expression 'F^2^>2.0 s(F^2^)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.0849 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3110 _refine_ls_number_parameters 208 _refine_ls_goodness_of_fit_ref 2.644 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[ s^2^(Fo) + 0.00063¦Fo¦^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.86 _refine_diff_density_min -0.58 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.16881(5) 0.49241(5) 0.05462(5) 0.0333(1) Uani 1.00 d . . . O(1) O -0.0289(3) 0.3705(3) 0.0163(3) 0.0390(7) Uani 1.00 d . . . O(2) O 0.2460(4) 0.4468(3) -0.1292(4) 0.0491(9) Uani 1.00 d . . . N(1) N 0.2889(4) 0.3393(4) 0.1442(4) 0.0384(9) Uani 1.00 d . . . N(2) N 0.1968(4) 0.6069(4) 0.2850(4) 0.0438(9) Uani 1.00 d . . . C(1) C -0.0430(4) 0.2754(4) 0.0950(4) 0.0358(9) Uani 1.00 d . . . C(2) C -0.1714(5) 0.2507(5) 0.1323(6) 0.046(1) Uani 1.00 d . . . C(3) C -0.1817(5) 0.1521(5) 0.2154(6) 0.052(1) Uani 1.00 d . . . C(4) C -0.0639(6) 0.0726(5) 0.2618(6) 0.057(1) Uani 1.00 d . . . C(5) C 0.0619(5) 0.0940(5) 0.2239(6) 0.049(1) Uani 1.00 d . . . C(6) C 0.0766(5) 0.1917(4) 0.1403(5) 0.039(1) Uani 1.00 d . . . C(7) C 0.2119(5) 0.2005(4) 0.0885(5) 0.042(1) Uani 1.00 d . . . C(8) C 0.3125(5) 0.3312(5) -0.1787(5) 0.045(1) Uani 1.00 d . . . C(9) C 0.2931(5) 0.2673(6) -0.3395(5) 0.056(1) Uani 1.00 d . . . C(10) C 0.3600(6) 0.1402(6) -0.3927(6) 0.063(2) Uani 1.00 d . . . C(11) C 0.4497(6) 0.0750(6) -0.2946(7) 0.063(2) Uani 1.00 d . . . C(12) C 0.4743(5) 0.1351(5) -0.1370(6) 0.052(1) Uani 1.00 d . . . C(13) C 0.4060(4) 0.2618(5) -0.0791(5) 0.043(1) Uani 1.00 d . . . C(14) C 0.4283(4) 0.3250(5) 0.0912(5) 0.046(1) Uani 1.00 d . . . C(15) C 0.3195(5) 0.3882(5) 0.3133(5) 0.050(1) Uani 1.00 d . . . C(16) C 0.3271(6) 0.5441(7) 0.3639(7) 0.069(2) Uani 1.00 d . . . C(17) C 0.0719(7) 0.5979(9) 0.3525(7) 0.084(2) Uani 1.00 d . . . C(18) C 0.236(1) 0.7525(7) 0.3032(8) 0.106(3) Uani 1.00 d . . . H(1) H -0.2535 0.3027 0.0999 0.0553 Uiso 1.00 calc . . . H(2) H -0.2699 0.1385 0.2411 0.0625 Uiso 1.00 calc . . . H(3) H -0.0707 0.0047 0.3189 0.0683 Uiso 1.00 calc . . . H(4) H 0.1424 0.0398 0.2560 0.0591 Uiso 1.00 calc . . . H(5) H 0.1900 0.1788 -0.0207 0.0504 Uiso 1.00 calc . . . H(6) H 0.2745 0.1307 0.1222 0.0504 Uiso 1.00 calc . . . H(7) H 0.2337 0.3121 -0.4110 0.0666 Uiso 1.00 calc . . . H(8) H 0.3427 0.0979 -0.5001 0.0756 Uiso 1.00 calc . . . H(9) H 0.4952 -0.0111 -0.3334 0.0752 Uiso 1.00 calc . . . H(10) H 0.5376 0.0904 -0.0682 0.0624 Uiso 1.00 calc . . . H(11) H 0.4710 0.4166 0.1149 0.0549 Uiso 1.00 calc . . . H(12) H 0.4897 0.2651 0.1437 0.0549 Uiso 1.00 calc . . . H(13) H 0.2459 0.3551 0.3509 0.0596 Uiso 1.00 calc . . . H(14) H 0.4081 0.3501 0.3539 0.0596 Uiso 1.00 calc . . . H(15) H 0.4088 0.5770 0.3395 0.0834 Uiso 1.00 calc . . . H(16) H 0.3340 0.5725 0.4720 0.0834 Uiso 1.00 calc . . . H(17) H 0.0923 0.6471 0.4581 0.1002 Uiso 1.00 calc . . . H(18) H -0.0081 0.6399 0.2994 0.1002 Uiso 1.00 calc . . . H(19) H 0.0512 0.5008 0.3434 0.1002 Uiso 1.00 calc . . . H(20) H 0.2632 0.7976 0.4096 0.1275 Uiso 1.00 calc . . . H(21) H 0.3132 0.7555 0.2548 0.1275 Uiso 1.00 calc . . . H(22) H 0.1566 0.8008 0.2573 0.1275 Uiso 1.00 calc . . . 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) 0.0286(3) 0.0378(3) 0.0350(3) 0.0013(2) 0.0044(2) 0.0140(2) O(1) 0.030(1) 0.043(1) 0.048(2) -0.002(1) 0.005(1) 0.022(1) O(2) 0.054(2) 0.054(2) 0.047(2) 0.014(1) 0.022(2) 0.020(1) N(1) 0.034(2) 0.048(2) 0.035(2) 0.005(1) 0.005(1) 0.015(1) N(2) 0.045(2) 0.041(2) 0.040(2) -0.004(1) 0.004(2) 0.004(1) C(1) 0.038(2) 0.030(2) 0.039(2) -0.004(1) 0.006(2) 0.008(1) C(2) 0.039(2) 0.043(2) 0.060(3) -0.003(2) 0.011(2) 0.017(2) C(3) 0.051(3) 0.049(2) 0.060(3) -0.010(2) 0.015(2) 0.016(2) C(4) 0.067(3) 0.051(3) 0.060(3) -0.010(2) 0.009(2) 0.030(2) C(5) 0.054(3) 0.043(2) 0.055(3) 0.005(2) 0.008(2) 0.022(2) C(6) 0.041(2) 0.036(2) 0.041(2) 0.002(2) 0.009(2) 0.012(2) C(7) 0.039(2) 0.045(2) 0.044(2) 0.005(2) 0.009(2) 0.015(2) C(8) 0.037(2) 0.057(2) 0.046(2) 0.003(2) 0.018(2) 0.015(2) C(9) 0.048(3) 0.080(3) 0.042(2) 0.005(2) 0.016(2) 0.016(2) C(10) 0.060(3) 0.080(4) 0.047(3) -0.007(3) 0.026(2) 0.000(2) C(11) 0.060(3) 0.057(3) 0.073(4) 0.001(2) 0.036(3) 0.001(2) C(12) 0.045(2) 0.050(2) 0.070(3) 0.008(2) 0.028(2) 0.018(2) C(13) 0.031(2) 0.049(2) 0.051(2) 0.002(2) 0.014(2) 0.012(2) C(14) 0.028(2) 0.062(3) 0.048(2) 0.005(2) 0.005(2) 0.019(2) C(15) 0.048(3) 0.066(3) 0.035(2) 0.010(2) 0.003(2) 0.017(2) C(16) 0.059(3) 0.083(4) 0.058(3) -0.006(3) 0.002(3) 0.011(3) C(17) 0.063(4) 0.118(5) 0.057(3) -0.014(3) 0.018(3) -0.009(3) C(18) 0.182(9) 0.068(4) 0.069(4) -0.054(5) 0.034(5) 0.000(3) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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) 2.199(3) . . yes Cu(1) O(1) 1.971(3) . 2_565 yes Cu(1) O(2) 1.932(3) . . yes Cu(1) N(1) 2.062(3) . . yes Cu(1) N(2) 2.096(3) . . yes O(1) C(1) 1.331(5) . . yes O(2) C(8) 1.296(5) . . yes N(1) C(7) 1.485(6) . . yes N(1) C(14) 1.509(5) . . yes N(1) C(15) 1.474(5) . . yes N(2) C(16) 1.490(7) . . yes N(2) C(17) 1.480(7) . . yes N(2) C(18) 1.437(7) . . yes C(1) C(2) 1.396(6) . . yes C(1) C(6) 1.424(5) . . yes C(2) C(3) 1.380(6) . . yes C(3) C(4) 1.390(7) . . yes C(4) C(5) 1.365(7) . . yes C(5) C(6) 1.387(6) . . yes C(6) C(7) 1.490(6) . . yes C(8) C(9) 1.426(7) . . yes C(8) C(13) 1.410(6) . . yes C(9) C(10) 1.392(7) . . yes C(10) C(11) 1.360(8) . . yes C(11) C(12) 1.391(8) . . yes C(12) C(13) 1.406(6) . . yes C(13) C(14) 1.503(6) . . yes C(15) C(16) 1.467(8) . . yes #------------------------------------------------------------------------------ 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(1) 80.3(1) . 1_555 2_565 yes O(1) Cu(1) O(2) 110.1(1) . 1_555 1_555 yes O(1) Cu(1) N(1) 91.6(1) . 1_555 1_555 yes O(1) Cu(1) N(2) 103.4(1) . 1_555 1_555 yes O(1) Cu(1) O(2) 94.8(1) 2_565 1_555 1_555 yes O(1) Cu(1) N(1) 170.5(1) 2_565 1_555 1_555 yes O(1) Cu(1) N(2) 92.5(1) 2_565 1_555 1_555 yes O(2) Cu(1) N(1) 92.7(1) . 1_555 1_555 yes O(2) Cu(1) N(2) 146.4(2) . 1_555 1_555 yes N(1) Cu(1) N(2) 84.4(1) . 1_555 1_555 yes Cu(1) O(1) Cu(1) 99.7(1) . 1_555 2_565 yes Cu(1) O(1) C(1) 123.0(2) . 1_555 1_555 yes Cu(1) O(1) C(1) 129.3(3) 2_565 1_555 1_555 yes Cu(1) O(2) C(8) 126.1(3) . 1_555 1_555 yes Cu(1) N(1) C(7) 110.0(2) . 1_555 1_555 yes Cu(1) N(1) C(14) 108.5(3) . 1_555 1_555 yes Cu(1) N(1) C(15) 108.2(3) . 1_555 1_555 yes C(7) N(1) C(14) 109.4(3) . 1_555 1_555 yes C(7) N(1) C(15) 112.1(4) . 1_555 1_555 yes C(14) N(1) C(15) 108.6(3) . 1_555 1_555 yes Cu(1) N(2) C(16) 104.0(3) . 1_555 1_555 yes Cu(1) N(2) C(17) 113.1(3) . 1_555 1_555 yes Cu(1) N(2) C(18) 111.2(4) . 1_555 1_555 yes C(16) N(2) C(17) 112.5(5) . 1_555 1_555 yes C(16) N(2) C(18) 104.4(5) . 1_555 1_555 yes C(17) N(2) C(18) 111.1(5) . 1_555 1_555 yes O(1) C(1) C(2) 123.0(4) . 1_555 1_555 yes O(1) C(1) C(6) 119.2(4) . 1_555 1_555 yes C(2) C(1) C(6) 117.8(4) . 1_555 1_555 yes C(1) C(2) C(3) 121.4(4) . 1_555 1_555 yes C(2) C(3) C(4) 120.4(4) . 1_555 1_555 yes C(3) C(4) C(5) 118.8(4) . 1_555 1_555 yes C(4) C(5) C(6) 122.5(4) . 1_555 1_555 yes C(1) C(6) C(5) 119.0(4) . 1_555 1_555 yes C(1) C(6) C(7) 120.6(4) . 1_555 1_555 yes C(5) C(6) C(7) 120.3(4) . 1_555 1_555 yes N(1) C(7) C(6) 116.8(3) . 1_555 1_555 yes O(2) C(8) C(9) 120.7(4) . 1_555 1_555 yes O(2) C(8) C(13) 122.7(4) . 1_555 1_555 yes C(9) C(8) C(13) 116.7(4) . 1_555 1_555 yes C(8) C(9) C(10) 120.8(5) . 1_555 1_555 yes C(9) C(10) C(11) 121.6(5) . 1_555 1_555 yes C(10) C(11) C(12) 119.6(4) . 1_555 1_555 yes C(11) C(12) C(13) 120.3(5) . 1_555 1_555 yes C(8) C(13) C(12) 121.1(4) . 1_555 1_555 yes C(8) C(13) C(14) 118.3(4) . 1_555 1_555 yes C(12) C(13) C(14) 120.6(4) . 1_555 1_555 yes N(1) C(14) C(13) 111.3(3) . 1_555 1_555 yes N(1) C(15) C(16) 111.5(4) . 1_555 1_555 yes N(2) C(16) C(15) 109.9(4) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Cu(1) O(1) Cu(1) O(1) 0.0 1_555 1_555 2_565 2_565 yes Cu(1) O(1) Cu(1) O(2) -109.6(1) 1_555 1_555 2_565 2_565 yes Cu(1) O(1) Cu(1) N(2) 103.2(1) 1_555 1_555 2_565 2_565 yes Cu(1) O(1) C(1) C(2) 146.9(3) 1_555 1_555 1_555 1_555 yes Cu(1) O(1) C(1) C(6) -34.8(5) 1_555 1_555 1_555 1_555 yes Cu(1) O(1) Cu(1) O(1) 0.0 1_555 2_565 2_565 1_555 yes Cu(1) O(1) Cu(1) O(2) 91.6(1) 1_555 2_565 2_565 2_565 yes Cu(1) O(1) Cu(1) N(1) -175.0(1) 1_555 2_565 2_565 2_565 yes Cu(1) O(1) Cu(1) N(2) -90.3(1) 1_555 2_565 2_565 2_565 yes Cu(1) O(1) C(1) C(2) -4.8(6) 1_555 2_565 2_565 2_565 yes Cu(1) O(1) C(1) C(6) 176.9(3) 1_555 2_565 2_565 2_565 yes Cu(1) O(2) C(8) C(9) 142.9(4) 1_555 1_555 1_555 1_555 yes Cu(1) O(2) C(8) C(13) -36.7(6) 1_555 1_555 1_555 1_555 yes Cu(1) N(1) C(7) C(6) -65.5(4) 1_555 1_555 1_555 1_555 yes Cu(1) N(1) C(14) C(13) -68.1(4) 1_555 1_555 1_555 1_555 yes Cu(1) N(1) C(15) C(16) -30.1(5) 1_555 1_555 1_555 1_555 yes Cu(1) N(2) C(16) C(15) -45.2(5) 1_555 1_555 1_555 1_555 yes O(1) Cu(1) O(1) Cu(1) 0.0 1_555 1_555 2_565 2_565 yes O(1) Cu(1) O(1) C(1) -148.5(4) 1_555 1_555 2_565 2_565 yes O(1) Cu(1) O(2) C(8) -75.6(4) 1_555 1_555 1_555 1_555 yes O(1) Cu(1) N(2) C(16) 112.7(3) 1_555 1_555 1_555 1_555 yes O(1) Cu(1) N(2) C(17) -9.6(4) 1_555 1_555 1_555 1_555 yes O(1) Cu(1) N(2) C(18) -135.5(5) 1_555 1_555 1_555 1_555 yes O(1) Cu(1) O(1) Cu(1) 0.0 1_555 2_565 2_565 1_555 yes O(1) Cu(1) O(1) C(1) 151.2(4) 1_555 2_565 2_565 2_565 yes O(1) Cu(1) O(2) C(8) 157.0(4) 1_555 2_565 2_565 2_565 yes O(1) Cu(1) N(1) C(7) -54.5(8) 1_555 2_565 2_565 2_565 yes O(1) Cu(1) N(1) C(14) -174.1(7) 1_555 2_565 2_565 2_565 yes O(1) Cu(1) N(1) C(15) 68.3(8) 1_555 2_565 2_565 2_565 yes O(1) Cu(1) N(2) C(16) 166.6(3) 1_555 2_565 2_565 2_565 yes O(1) Cu(1) N(2) C(17) -71.1(4) 1_555 2_565 2_565 2_565 yes O(1) Cu(1) N(2) C(18) 54.8(5) 1_555 2_565 2_565 2_565 yes O(1) C(1) C(2) C(3) -179.4(4) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(6) C(5) 179.2(4) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(6) C(7) -5.5(6) 1_555 1_555 1_555 1_555 yes O(2) Cu(1) O(1) C(1) 117.3(3) 1_555 1_555 1_555 1_555 yes O(2) Cu(1) O(1) C(1) -38.9(3) 1_555 1_555 2_565 2_565 yes O(2) Cu(1) N(1) C(7) -87.5(3) 1_555 1_555 1_555 1_555 yes O(2) Cu(1) N(1) C(14) 32.1(3) 1_555 1_555 1_555 1_555 yes O(2) Cu(1) N(1) C(15) 149.7(3) 1_555 1_555 1_555 1_555 yes O(2) Cu(1) N(2) C(16) -64.2(4) 1_555 1_555 1_555 1_555 yes O(2) Cu(1) N(2) C(17) 173.5(4) 1_555 1_555 1_555 1_555 yes O(2) Cu(1) N(2) C(18) 47.6(6) 1_555 1_555 1_555 1_555 yes O(2) C(8) C(9) C(10) -177.5(5) 1_555 1_555 1_555 1_555 yes O(2) C(8) C(13) C(12) 178.8(4) 1_555 1_555 1_555 1_555 yes O(2) C(8) C(13) C(14) 0.2(6) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) O(1) C(1) 23.8(3) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) O(2) C(8) 17.2(4) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(2) C(16) 22.4(3) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(2) C(17) -99.9(4) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(2) C(18) 134.2(5) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(6) C(1) 64.5(5) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(6) C(5) -120.3(4) 1_555 1_555 1_555 1_555 yes N(1) C(14) C(13) C(8) 57.0(5) 1_555 1_555 1_555 1_555 yes N(1) C(14) C(13) C(12) -121.7(4) 1_555 1_555 1_555 1_555 yes N(1) C(15) C(16) N(2) 52.1(6) 1_555 1_555 1_555 1_555 yes N(2) Cu(1) O(1) C(1) -60.9(3) 1_555 1_555 1_555 1_555 yes N(2) Cu(1) O(1) C(1) 108.3(3) 1_555 1_555 2_565 2_565 yes N(2) Cu(1) O(2) C(8) 101.2(4) 1_555 1_555 1_555 1_555 yes N(2) Cu(1) N(1) C(7) 126.1(3) 1_555 1_555 1_555 1_555 yes N(2) Cu(1) N(1) C(14) -114.3(3) 1_555 1_555 1_555 1_555 yes N(2) Cu(1) N(1) C(15) 3.3(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -1.2(8) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) 1.4(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) -2.4(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(7) 172.8(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 0.1(8) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 2.4(6) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -0.2(8) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) -173.9(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) N(1) C(14) 175.4(3) 1_555 1_555 1_555 1_555 yes C(6) C(7) N(1) C(15) 55.0(5) 1_555 1_555 1_555 1_555 yes C(7) N(1) C(14) C(13) 51.9(4) 1_555 1_555 1_555 1_555 yes C(7) N(1) C(15) C(16) -151.5(4) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -2.2(8) 1_555 1_555 1_555 1_555 yes C(8) C(13) C(12) C(11) -0.6(7) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(13) C(12) -0.8(7) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(13) C(14) -179.4(4) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) 0.8(8) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(13) 2.2(7) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(13) 0.6(8) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 178.0(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) N(1) C(15) 174.5(4) 1_555 1_555 1_555 1_555 yes C(14) N(1) C(15) C(16) 87.5(5) 1_555 1_555 1_555 1_555 yes C(15) C(16) N(2) C(17) 77.5(5) 1_555 1_555 1_555 1_555 yes C(15) C(16) N(2) C(18) -161.9(5) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 C(11) C(18) 3.544(10) . 2_665 ? #------------------------------------------------------------------------------ #============================================================================== data_compound3 #[Cu2(L)(HL)]ClO4.CH3OH.H2O________ _database_code_CSD 179772 _audit_creation_date '2002-02-05' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C74 H102 Cl2 Cu4 N8 O20 ' _chemical_formula_moiety '[Cu2(L)(HL)]ClO4.CH3OH.H2O ' _chemical_formula_weight 1748.75 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/a' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z' 'x+1/2,-y+1/2,z' #------------------------------------------------------------------------------ _cell_length_a 17.012(1) _cell_length_b 17.596(1) _cell_length_c 26.692(2) _cell_angle_alpha 90 _cell_angle_beta 101.7114(8) _cell_angle_gamma 90 _cell_volume 7824.0(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 27119 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.885 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K¥a' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 32725 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.8721 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.8707 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 16152 _reflns_number_gt 9496 _reflns_threshold_expression F^2^>2.0¥s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.1970 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 15658 _refine_ls_number_parameters 973 _refine_ls_goodness_of_fit_ref 1.300 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.002Fo^2^ + 1.000¥s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0060 _refine_diff_density_max 3.95 _refine_diff_density_min -3.19 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.174 0.200 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cu' 'Cu' 0.284 1.430 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.75796(4) 0.14458(4) 0.42898(3) 0.0283(2) Uani 1.00 1 d . . . Cu2 Cu 0.83967(4) 0.15135(4) 0.33431(3) 0.0266(2) Uani 1.00 1 d . . . Cu3 Cu 0.80712(5) -0.14797(4) 0.06251(3) 0.0349(2) Uani 1.00 1 d . . . Cu4 Cu 0.94913(5) -0.15923(4) 0.15640(3) 0.0324(2) Uani 1.00 1 d . . . Cl1 Cl 0.9748(1) -0.3495(1) -0.13381(7) 0.0458(5) Uani 1.00 1 d . . . Cl2 Cl 1.0439(1) 0.35282(9) 0.61918(7) 0.0438(4) Uani 1.00 1 d . . . O1 O 0.7938(2) 0.0788(2) 0.3773(1) 0.028(1) Uani 1.00 1 d . . . O2 O 0.8695(2) 0.1107(2) 0.4863(1) 0.033(1) Uani 1.00 1 d . . . O3 O 0.8086(3) 0.2180(2) 0.3929(1) 0.031(1) Uani 1.00 1 d . . . O4 O 0.9537(2) 0.1264(2) 0.3629(1) 0.029(1) Uani 1.00 1 d . . . O5 O 0.8764(3) -0.0843(2) 0.1159(1) 0.033(1) Uani 1.00 1 d . . . O6 O 0.8788(3) -0.1087(3) 0.0060(2) 0.044(1) Uani 1.00 1 d . . . O7 O 0.8857(3) -0.2219(2) 0.0946(2) 0.040(1) Uani 1.00 1 d . . . O8 O 1.0462(3) -0.1290(2) 0.1304(2) 0.040(1) Uani 1.00 1 d . . . O9 O 0.9283(4) -0.2840(3) -0.1470(3) 0.086(2) Uani 1.00 1 d . . . O17 O 1.0030(2) 0.1369(2) 0.4614(1) 0.032(1) Uani 1.00 1 d . . . O11 O 1.0179(5) -0.3582(5) -0.1742(3) 0.120(3) Uani 1.00 1 d . . . O12 O 0.9208(6) -0.4114(4) -0.1330(4) 0.130(4) Uani 1.00 1 d . . . O13 O 1.086(1) 0.4103(6) 0.6481(7) 0.253(9) Uani 1.00 1 d . . . O14 O 0.9664(5) 0.365(1) 0.6197(6) 0.246(7) Uani 1.00 1 d . . . O15 O 1.0630(7) 0.3440(8) 0.5715(3) 0.201(6) Uani 1.00 1 d . . . O16 O 1.056(1) 0.2897(5) 0.6429(4) 0.232(7) Uani 1.00 1 d . . . O20 O 1.001(1) 0.4939(7) 0.7269(5) 0.291(8) Uani 1.00 1 d . . . O18 O 1.0274(3) -0.1398(2) 0.0317(2) 0.039(1) Uani 1.00 1 d . . . O19 O 0.8407(8) 0.4007(6) 0.7207(4) 0.172(5) Uani 1.00 1 d . . . O10 O 1.0288(4) -0.3393(5) -0.0871(2) 0.103(3) Uani 1.00 1 d . . . N1 N 0.6993(3) 0.0595(3) 0.4581(2) 0.033(1) Uani 1.00 1 d . . . N2 N 0.6715(3) 0.2157(3) 0.4448(2) 0.030(1) Uani 1.00 1 d . . . N3 N 0.8670(3) 0.2435(3) 0.2951(2) 0.030(1) Uani 1.00 1 d . . . N4 N 0.7502(3) 0.1299(3) 0.2695(2) 0.030(1) Uani 1.00 1 d . . . N5 N 0.7283(3) -0.0632(3) 0.0369(2) 0.036(1) Uani 1.00 1 d . . . N6 N 0.7117(4) -0.2212(3) 0.0468(2) 0.043(2) Uani 1.00 1 d . . . N7 N 1.0010(3) -0.2538(3) 0.1918(2) 0.035(1) Uani 1.00 1 d . . . N8 N 0.9070(3) -0.1382(3) 0.2221(2) 0.035(1) Uani 1.00 1 d . . . C1 C 0.7995(4) 0.0022(3) 0.3816(2) 0.029(1) Uani 1.00 1 d . . . C2 C 0.8646(4) -0.0374(3) 0.3705(2) 0.031(2) Uani 1.00 1 d . . . C3 C 0.8671(4) -0.1156(3) 0.3737(2) 0.034(2) Uani 1.00 1 d . . . C4 C 0.8069(5) -0.1564(3) 0.3887(3) 0.044(2) Uani 1.00 1 d . . . C5 C 0.7432(4) -0.1181(3) 0.4016(3) 0.041(2) Uani 1.00 1 d . . . C6 C 0.7388(4) -0.0380(3) 0.3993(2) 0.033(2) Uani 1.00 1 d . . . C7 C 0.6710(4) 0.0038(3) 0.4159(3) 0.036(2) Uani 1.00 1 d . . . C8 C 0.7498(4) 0.0186(4) 0.5038(2) 0.036(2) Uani 1.00 1 d . . . C9 C 0.7914(4) 0.0703(3) 0.5446(2) 0.035(2) Uani 1.00 1 d . . . C10 C 0.7723(4) 0.0758(4) 0.5928(3) 0.046(2) Uani 1.00 1 d . . . C11 C 0.8143(6) 0.1247(5) 0.6300(3) 0.059(3) Uani 1.00 1 d . . . C12 C 0.8785(5) 0.1676(4) 0.6202(3) 0.053(2) Uani 1.00 1 d . . . C13 C 0.8994(4) 0.1630(4) 0.5725(3) 0.040(2) Uani 1.00 1 d . . . C14 C 0.8549(4) 0.1148(3) 0.5353(2) 0.032(2) Uani 1.00 1 d . . . C15 C 0.6286(4) 0.0943(4) 0.4739(3) 0.040(2) Uani 1.00 1 d . . . C16 C 0.6014(4) 0.1638(4) 0.4421(3) 0.037(2) Uani 1.00 1 d . . . C17 C 0.6923(4) 0.2539(4) 0.4961(3) 0.041(2) Uani 1.00 1 d . . . C18 C 0.6488(4) 0.2766(3) 0.4051(2) 0.038(2) Uani 1.00 1 d . . . C19 C 0.8470(4) 0.2851(3) 0.4069(2) 0.033(2) Uani 1.00 1 d . . . C20 C 0.8732(4) 0.3065(3) 0.4572(2) 0.036(2) Uani 1.00 1 d . . . C21 C 0.9082(4) 0.3778(4) 0.4693(3) 0.044(2) Uani 1.00 1 d . . . C22 C 0.9150(4) 0.4279(3) 0.4309(3) 0.043(2) Uani 1.00 1 d . . . C23 C 0.8907(4) 0.4072(3) 0.3805(3) 0.042(2) Uani 1.00 1 d . . . C24 C 0.8565(4) 0.3347(3) 0.3675(2) 0.033(2) Uani 1.00 1 d . . . C25 C 0.8272(4) 0.3134(3) 0.3121(2) 0.034(2) Uani 1.00 1 d . . . C26 C 0.9563(4) 0.2572(3) 0.3028(2) 0.031(2) Uani 1.00 1 d . . . C27 C 1.0029(4) 0.1874(3) 0.2956(2) 0.030(2) Uani 1.00 1 d . . . C28 C 1.0531(4) 0.1847(4) 0.2599(2) 0.035(2) Uani 1.00 1 d . . . C29 C 1.1044(4) 0.1230(4) 0.2584(3) 0.037(2) Uani 1.00 1 d . . . C30 C 1.1053(4) 0.0646(4) 0.2928(3) 0.037(2) Uani 1.00 1 d . . . C31 C 1.0551(4) 0.0652(3) 0.3283(2) 0.032(2) Uani 1.00 1 d . . . C32 C 1.0037(3) 0.1261(3) 0.3296(2) 0.026(1) Uani 1.00 1 d . . . C33 C 0.7487(4) 0.1949(3) 0.2341(2) 0.031(2) Uani 1.00 1 d . . . C34 C 0.8335(4) 0.2278(3) 0.2404(2) 0.035(2) Uani 1.00 1 d . . . C35 C 0.6697(4) 0.1184(4) 0.2798(3) 0.044(2) Uani 1.00 1 d . . . C36 C 0.7764(5) 0.0606(4) 0.2461(3) 0.049(2) Uani 1.00 1 d . . . C37 C 0.8754(4) -0.0072(3) 0.1172(2) 0.033(2) Uani 1.00 1 d . . . C38 C 0.9459(4) 0.0338(3) 0.1334(2) 0.037(2) Uani 1.00 1 d . . . C39 C 0.9433(5) 0.1137(4) 0.1354(3) 0.042(2) Uani 1.00 1 d . . . C40 C 0.8701(5) 0.1513(4) 0.1208(2) 0.043(2) Uani 1.00 1 d . . . C41 C 0.8007(4) 0.1102(4) 0.1038(3) 0.041(2) Uani 1.00 1 d . . . C42 C 0.8016(4) 0.0313(4) 0.1016(2) 0.033(2) Uani 1.00 1 d . . . C43 C 0.7251(4) -0.0109(4) 0.0820(3) 0.040(2) Uani 1.00 1 d . . . C44 C 0.7476(4) -0.0170(4) -0.0061(2) 0.039(2) Uani 1.00 1 d . . . C45 C 0.7628(4) -0.0650(3) -0.0496(2) 0.036(2) Uani 1.00 1 d . . . C46 C 0.7105(4) -0.0652(4) -0.0973(3) 0.042(2) Uani 1.00 1 d . . . C47 C 0.7285(5) -0.1085(4) -0.1371(3) 0.047(2) Uani 1.00 1 d . . . C48 C 0.7992(5) -0.1503(4) -0.1292(3) 0.049(2) Uani 1.00 1 d . . . C49 C 0.8521(4) -0.1505(4) -0.0820(3) 0.040(2) Uani 1.00 1 d . . . C50 C 0.8335(4) -0.1078(4) -0.0426(2) 0.036(2) Uani 1.00 1 d . . . C51 C 0.6475(4) -0.1004(4) 0.0196(3) 0.045(2) Uani 1.00 1 d . . . C52 C 0.6419(4) -0.1710(4) 0.0501(3) 0.044(2) Uani 1.00 1 d . . . C53 C 0.6988(5) -0.2567(4) -0.0046(3) 0.053(2) Uani 1.00 1 d . . . C54 C 0.7175(5) -0.2819(4) 0.0859(3) 0.047(2) Uani 1.00 1 d . . . C55 C 0.9116(4) -0.2896(4) 0.0801(3) 0.042(2) Uani 1.00 1 d . . . C56 C 0.9058(5) -0.3076(4) 0.0282(3) 0.048(2) Uani 1.00 1 d . . . C57 C 0.9334(5) -0.3794(4) 0.0148(3) 0.055(2) Uani 1.00 1 d . . . C58 C 0.9609(6) -0.4315(4) 0.0517(3) 0.061(3) Uani 1.00 1 d . . . C59 C 0.9697(5) -0.4118(4) 0.1036(3) 0.051(2) Uani 1.00 1 d . . . C60 C 0.9456(4) -0.3411(3) 0.1178(3) 0.041(2) Uani 1.00 1 d . . . C61 C 0.9510(4) -0.3227(4) 0.1733(3) 0.042(2) Uani 1.00 1 d . . . C62 C 1.0850(5) -0.2651(4) 0.1836(3) 0.044(2) Uani 1.00 1 d . . . C63 C 1.1358(4) -0.1943(4) 0.1957(2) 0.038(2) Uani 1.00 1 d . . . C64 C 1.2076(4) -0.1956(4) 0.2335(3) 0.043(2) Uani 1.00 1 d . . . C65 C 1.2586(4) -0.1317(5) 0.2416(3) 0.052(2) Uani 1.00 1 d . . . C66 C 1.2353(4) -0.0692(4) 0.2102(3) 0.050(2) Uani 1.00 1 d . . . C67 C 1.1667(4) -0.0662(4) 0.1728(3) 0.044(2) Uani 1.00 1 d . . . C68 C 1.1149(4) -0.1288(4) 0.1659(2) 0.037(2) Uani 1.00 1 d . . . C69 C 1.0035(5) -0.2431(4) 0.2480(3) 0.042(2) Uani 1.00 1 d . . . C70 C 0.9240(4) -0.2081(3) 0.2539(2) 0.038(2) Uani 1.00 1 d . . . C71 C 0.9562(4) -0.0734(4) 0.2492(2) 0.039(2) Uani 1.00 1 d . . . C72 C 0.8218(4) -0.1209(4) 0.2142(3) 0.040(2) Uani 1.00 1 d . . . C73 C 1.0576(4) 0.0746(4) 0.4753(3) 0.039(2) Uani 1.00 1 d . . . C74 C 1.0716(4) -0.0766(4) 0.0180(3) 0.051(2) Uani 1.00 1 d . . . H1 H 0.9074 -0.0105 0.3608 0.0374 Uiso 1.00 1 c . . . H2 H 0.9114 -0.1419 0.3654 0.0411 Uiso 1.00 1 c . . . H3 H 0.8089 -0.2103 0.3899 0.0528 Uiso 1.00 1 c . . . H4 H 0.7019 -0.1458 0.4125 0.0491 Uiso 1.00 1 c . . . H5 H 0.6371 -0.0323 0.4274 0.0430 Uiso 1.00 1 c . . . H6 H 0.6414 0.0305 0.3872 0.0430 Uiso 1.00 1 c . . . H7 H 0.7156 -0.0139 0.5181 0.0434 Uiso 1.00 1 c . . . H8 H 0.7892 -0.0110 0.4920 0.0434 Uiso 1.00 1 c . . . H9 H 0.7300 0.0455 0.6005 0.0550 Uiso 1.00 1 c . . . H10 H 0.7992 0.1290 0.6622 0.0719 Uiso 1.00 1 c . . . H11 H 0.9076 0.1997 0.6458 0.0629 Uiso 1.00 1 c . . . H12 H 0.9429 0.1917 0.5652 0.0474 Uiso 1.00 1 c . . . H13 H 0.5862 0.0584 0.4693 0.0478 Uiso 1.00 1 c . . . H14 H 0.6429 0.1084 0.5089 0.0478 Uiso 1.00 1 c . . . H15 H 0.5604 0.1891 0.4552 0.0446 Uiso 1.00 1 c . . . H16 H 0.5813 0.1496 0.4076 0.0446 Uiso 1.00 1 c . . . H17 H 0.7066 0.2167 0.5219 0.0496 Uiso 1.00 1 c . . . H18 H 0.7358 0.2878 0.4966 0.0496 Uiso 1.00 1 c . . . H19 H 0.6468 0.2817 0.5018 0.0496 Uiso 1.00 1 c . . . H20 H 0.6927 0.3101 0.4062 0.0461 Uiso 1.00 1 c . . . H21 H 0.6349 0.2539 0.3723 0.0461 Uiso 1.00 1 c . . . H22 H 0.6040 0.3042 0.4119 0.0461 Uiso 1.00 1 c . . . H23 H 0.8674 0.2724 0.4838 0.0434 Uiso 1.00 1 c . . . H24 H 0.9275 0.3918 0.5041 0.0524 Uiso 1.00 1 c . . . H25 H 0.9365 0.4772 0.4393 0.0515 Uiso 1.00 1 c . . . H26 H 0.8970 0.4417 0.3542 0.0506 Uiso 1.00 1 c . . . H27 H 0.8369 0.3551 0.2917 0.0404 Uiso 1.00 1 c . . . H28 H 0.7711 0.3041 0.3068 0.0404 Uiso 1.00 1 c . . . H29 H 0.9654 0.2943 0.2787 0.0375 Uiso 1.00 1 c . . . H30 H 0.9750 0.2756 0.3365 0.0375 Uiso 1.00 1 c . . . H31 H 1.0520 0.2255 0.2363 0.0423 Uiso 1.00 1 c . . . H32 H 1.1382 0.1214 0.2340 0.0442 Uiso 1.00 1 c . . . H33 H 1.1409 0.0230 0.2925 0.0437 Uiso 1.00 1 c . . . H34 H 1.0561 0.0239 0.3515 0.0384 Uiso 1.00 1 c . . . H35 H 0.8317 0.2737 0.2216 0.0423 Uiso 1.00 1 c . . . H36 H 0.8672 0.1923 0.2280 0.0423 Uiso 1.00 1 c . . . H37 H 0.7309 0.1781 0.1998 0.0378 Uiso 1.00 1 c . . . H38 H 0.7133 0.2329 0.2418 0.0378 Uiso 1.00 1 c . . . H39 H 0.6532 0.1630 0.2947 0.0527 Uiso 1.00 1 c . . . H40 H 0.6332 0.1077 0.2486 0.0527 Uiso 1.00 1 c . . . H41 H 0.6707 0.0768 0.3026 0.0527 Uiso 1.00 1 c . . . H42 H 0.7770 0.0188 0.2688 0.0576 Uiso 1.00 1 c . . . H43 H 0.7397 0.0500 0.2149 0.0576 Uiso 1.00 1 c . . . H44 H 0.8283 0.0682 0.2395 0.0576 Uiso 1.00 1 c . . . H45 H 0.9956 0.0079 0.1429 0.0440 Uiso 1.00 1 c . . . H46 H 0.9915 0.1418 0.1466 0.0507 Uiso 1.00 1 c . . . H47 H 0.8680 0.2053 0.1227 0.0510 Uiso 1.00 1 c . . . H48 H 0.7514 0.1367 0.0934 0.0494 Uiso 1.00 1 c . . . H49 H 0.6835 0.0253 0.0714 0.0477 Uiso 1.00 1 c . . . H50 H 0.7129 -0.0408 0.1090 0.0477 Uiso 1.00 1 c . . . H51 H 0.7039 0.0159 -0.0185 0.0471 Uiso 1.00 1 c . . . H52 H 0.7944 0.0122 0.0067 0.0471 Uiso 1.00 1 c . . . H53 H 0.6629 -0.0357 -0.1027 0.0501 Uiso 1.00 1 c . . . H54 H 0.6929 -0.1096 -0.1694 0.0562 Uiso 1.00 1 c . . . H55 H 0.8117 -0.1794 -0.1566 0.0591 Uiso 1.00 1 c . . . H56 H 0.9000 -0.1796 -0.0771 0.0480 Uiso 1.00 1 c . . . H57 H 0.6066 -0.0658 0.0243 0.0543 Uiso 1.00 1 c . . . H58 H 0.6404 -0.1131 -0.0156 0.0543 Uiso 1.00 1 c . . . H59 H 0.5932 -0.1966 0.0368 0.0534 Uiso 1.00 1 c . . . H60 H 0.6436 -0.1578 0.0849 0.0534 Uiso 1.00 1 c . . . H61 H 0.6502 -0.2851 -0.0104 0.0634 Uiso 1.00 1 c . . . H62 H 0.6952 -0.2182 -0.0299 0.0634 Uiso 1.00 1 c . . . H63 H 0.7423 -0.2896 -0.0065 0.0634 Uiso 1.00 1 c . . . H64 H 0.6693 -0.3108 0.0800 0.0561 Uiso 1.00 1 c . . . H65 H 0.7615 -0.3145 0.0839 0.0561 Uiso 1.00 1 c . . . H66 H 0.7257 -0.2598 0.1190 0.0561 Uiso 1.00 1 c . . . H67 H 0.8837 -0.2722 0.0024 0.0583 Uiso 1.00 1 c . . . H68 H 0.9322 -0.3908 -0.0202 0.0654 Uiso 1.00 1 c . . . H69 H 0.9747 -0.4810 0.0425 0.0738 Uiso 1.00 1 c . . . H70 H 0.9919 -0.4474 0.1291 0.0608 Uiso 1.00 1 c . . . H71 H 0.9739 -0.3652 0.1930 0.0503 Uiso 1.00 1 c . . . H72 H 0.8983 -0.3143 0.1787 0.0503 Uiso 1.00 1 c . . . H73 H 1.1095 -0.3052 0.2053 0.0530 Uiso 1.00 1 c . . . H74 H 1.0829 -0.2787 0.1490 0.0530 Uiso 1.00 1 c . . . H75 H 1.2214 -0.2402 0.2535 0.0515 Uiso 1.00 1 c . . . H76 H 1.3064 -0.1316 0.2673 0.0625 Uiso 1.00 1 c . . . H77 H 1.2691 -0.0256 0.2149 0.0608 Uiso 1.00 1 c . . . H78 H 1.1545 -0.0223 0.1520 0.0521 Uiso 1.00 1 c . . . H79 H 1.0108 -0.2906 0.2650 0.0501 Uiso 1.00 1 c . . . H80 H 1.0465 -0.2100 0.2622 0.0501 Uiso 1.00 1 c . . . H81 H 0.9270 -0.1954 0.2889 0.0463 Uiso 1.00 1 c . . . H82 H 0.8823 -0.2439 0.2434 0.0463 Uiso 1.00 1 c . . . H83 H 1.0114 -0.0858 0.2542 0.0471 Uiso 1.00 1 c . . . H84 H 0.9457 -0.0288 0.2290 0.0471 Uiso 1.00 1 c . . . H85 H 0.9419 -0.0652 0.2814 0.0471 Uiso 1.00 1 c . . . H86 H 0.8075 -0.1124 0.2464 0.0481 Uiso 1.00 1 c . . . H87 H 0.8108 -0.0763 0.1938 0.0481 Uiso 1.00 1 c . . . H88 H 0.7918 -0.1622 0.1974 0.0481 Uiso 1.00 1 c . . . H92 H 1.1265 -0.0906 0.0216 0.0609 Uiso 1.00 1 c . . . H93 H 1.0505 -0.0623 -0.0162 0.0609 Uiso 1.00 1 c . . . H94 H 1.0677 -0.0351 0.0403 0.0609 Uiso 1.00 1 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 Cu1 0.0272(4) 0.0343(4) 0.0267(4) 0.0067(3) 0.0128(3) 0.0051(3) Cu2 0.0274(4) 0.0307(4) 0.0231(3) 0.0043(3) 0.0086(3) 0.0044(3) Cu3 0.0350(4) 0.0428(4) 0.0291(4) -0.0131(4) 0.0113(3) -0.0057(3) Cu4 0.0384(4) 0.0349(4) 0.0267(4) -0.0036(3) 0.0134(3) -0.0062(3) Cl1 0.0426(9) 0.0533(9) 0.0404(9) 0.0059(8) 0.0060(7) 0.0050(7) Cl2 0.0415(9) 0.0400(8) 0.048(1) -0.0014(7) 0.0041(8) 0.0145(7) O1 0.029(2) 0.029(2) 0.027(2) 0.003(2) 0.011(2) 0.005(2) O2 0.026(2) 0.053(2) 0.021(2) 0.005(2) 0.005(2) 0.008(2) O3 0.038(2) 0.026(2) 0.032(2) 0.004(2) 0.017(2) -0.001(2) O4 0.023(2) 0.040(2) 0.025(2) 0.005(2) 0.011(2) 0.007(2) O5 0.033(2) 0.039(2) 0.029(2) -0.010(2) 0.007(2) -0.007(2) O6 0.036(3) 0.075(3) 0.023(2) -0.014(2) 0.010(2) -0.002(2) O7 0.042(3) 0.040(2) 0.039(3) -0.007(2) 0.014(2) -0.017(2) O8 0.038(2) 0.051(3) 0.033(2) -0.003(2) 0.012(2) -0.001(2) O9 0.089(5) 0.065(4) 0.096(5) 0.033(4) -0.004(4) 0.015(3) O17 0.025(2) 0.041(2) 0.029(2) 0.003(2) 0.007(2) 0.007(2) O11 0.079(5) 0.22(1) 0.065(5) 0.022(6) 0.031(5) -0.004(5) O12 0.19(1) 0.056(4) 0.158(8) -0.042(5) 0.060(8) 0.010(4) O13 0.34(2) 0.114(8) 0.34(2) -0.07(1) 0.15(2) -0.05(1) O14 0.043(5) 0.43(2) 0.25(2) 0.047(9) 0.007(8) -0.15(1) O15 0.16(1) 0.41(2) 0.045(5) -0.03(1) 0.045(6) 0.036(8) O16 0.46(2) 0.115(7) 0.152(9) 0.13(1) 0.15(1) 0.094(7) O20 0.42(2) 0.26(1) 0.27(1) 0.29(2) 0.27(2) 0.18(1) O18 0.038(2) 0.040(2) 0.044(3) -0.004(2) 0.015(2) 0.002(2) O19 0.20(1) 0.161(9) 0.134(9) 0.046(8) -0.027(9) 0.026(7) O10 0.055(4) 0.205(8) 0.039(3) 0.008(5) -0.014(3) 0.021(4) N1 0.025(3) 0.043(3) 0.033(3) 0.009(2) 0.014(2) 0.010(2) N2 0.030(3) 0.039(3) 0.023(2) 0.011(2) 0.008(2) 0.002(2) N3 0.031(3) 0.033(2) 0.029(3) 0.002(2) 0.013(2) 0.006(2) N4 0.034(3) 0.033(2) 0.025(3) 0.007(2) 0.009(2) 0.004(2) N5 0.033(3) 0.051(3) 0.025(3) -0.018(2) 0.009(2) 0.001(2) N6 0.048(4) 0.053(3) 0.030(3) -0.014(3) 0.014(3) -0.003(2) N7 0.041(3) 0.040(3) 0.029(3) 0.005(2) 0.015(2) -0.007(2) N8 0.042(3) 0.035(3) 0.030(3) -0.006(2) 0.015(2) -0.009(2) C1 0.032(3) 0.032(3) 0.023(3) 0.001(2) 0.009(2) 0.005(2) C2 0.036(3) 0.036(3) 0.022(3) 0.002(3) 0.009(3) -0.001(2) C3 0.045(4) 0.032(3) 0.028(3) 0.004(3) 0.015(3) -0.002(2) C4 0.060(5) 0.037(3) 0.038(4) 0.005(3) 0.016(3) 0.002(3) C5 0.049(4) 0.034(3) 0.043(4) -0.005(3) 0.016(3) 0.008(3) C6 0.030(3) 0.038(3) 0.030(3) -0.001(3) 0.007(3) 0.002(2) C7 0.031(3) 0.040(3) 0.038(4) -0.005(3) 0.009(3) 0.010(3) C8 0.029(3) 0.046(3) 0.036(3) 0.009(3) 0.011(3) 0.018(3) C9 0.038(4) 0.044(3) 0.027(3) 0.012(3) 0.014(3) 0.007(3) C10 0.043(4) 0.070(5) 0.029(4) 0.011(4) 0.020(3) 0.012(3) C11 0.084(6) 0.067(5) 0.034(4) 0.016(5) 0.028(4) 0.009(3) C12 0.067(5) 0.060(4) 0.032(4) 0.007(4) 0.010(4) -0.001(3) C13 0.041(4) 0.048(4) 0.032(3) 0.005(3) 0.012(3) 0.004(3) C14 0.034(3) 0.042(3) 0.021(3) 0.008(3) 0.009(3) 0.005(2) C15 0.033(4) 0.050(4) 0.043(4) 0.008(3) 0.021(3) 0.015(3) C16 0.023(3) 0.055(4) 0.037(4) 0.013(3) 0.011(3) 0.009(3) C17 0.047(4) 0.048(4) 0.032(3) 0.013(3) 0.016(3) -0.001(3) C18 0.041(4) 0.041(3) 0.034(3) 0.017(3) 0.011(3) 0.007(3) C19 0.036(4) 0.033(3) 0.035(3) 0.004(3) 0.017(3) -0.003(2) C20 0.040(4) 0.035(3) 0.033(3) 0.010(3) 0.007(3) -0.001(2) C21 0.047(4) 0.043(3) 0.042(4) 0.015(3) 0.011(3) -0.013(3) C22 0.040(4) 0.030(3) 0.057(5) 0.005(3) 0.009(3) -0.008(3) C23 0.042(4) 0.032(3) 0.057(5) 0.007(3) 0.023(4) 0.002(3) C24 0.036(3) 0.028(3) 0.036(3) 0.010(3) 0.011(3) 0.003(2) C25 0.037(3) 0.028(3) 0.037(3) 0.008(3) 0.010(3) 0.013(2) C26 0.026(3) 0.035(3) 0.036(3) 0.003(2) 0.011(3) 0.006(2) C27 0.030(3) 0.039(3) 0.022(3) -0.004(3) 0.009(2) 0.001(2) C28 0.037(4) 0.044(3) 0.027(3) -0.009(3) 0.013(3) 0.002(3) C29 0.033(3) 0.046(3) 0.036(4) -0.004(3) 0.018(3) -0.009(3) C30 0.027(3) 0.043(3) 0.043(4) 0.002(3) 0.015(3) -0.009(3) C31 0.027(3) 0.036(3) 0.036(3) -0.002(3) 0.011(3) 0.001(2) C32 0.020(3) 0.036(3) 0.024(3) 0.003(2) 0.010(2) 0.002(2) C33 0.028(3) 0.036(3) 0.030(3) 0.009(3) 0.005(3) 0.006(2) C34 0.042(4) 0.040(3) 0.024(3) 0.001(3) 0.007(3) 0.011(2) C35 0.041(4) 0.059(4) 0.032(4) -0.003(3) 0.007(3) 0.004(3) C36 0.077(5) 0.040(3) 0.030(4) 0.020(4) 0.014(4) 0.002(3) C37 0.038(3) 0.031(3) 0.029(3) -0.011(3) 0.007(3) -0.009(2) C38 0.040(4) 0.042(3) 0.029(3) -0.002(3) 0.008(3) -0.005(3) C39 0.056(4) 0.043(3) 0.030(3) -0.014(3) 0.010(3) -0.004(3) C40 0.063(5) 0.040(3) 0.026(3) -0.002(3) 0.011(3) 0.000(3) C41 0.051(4) 0.046(4) 0.029(3) 0.001(3) 0.014(3) -0.000(3) C42 0.031(3) 0.047(3) 0.023(3) -0.002(3) 0.012(3) 0.001(2) C43 0.039(4) 0.049(4) 0.034(4) -0.001(3) 0.016(3) 0.003(3) C44 0.045(4) 0.050(4) 0.027(3) -0.016(3) 0.015(3) 0.000(3) C45 0.040(4) 0.041(3) 0.026(3) -0.015(3) 0.007(3) -0.002(2) C46 0.050(4) 0.042(3) 0.031(3) -0.011(3) 0.004(3) 0.001(3) C47 0.054(5) 0.045(4) 0.037(4) -0.010(3) -0.000(3) -0.001(3) C48 0.072(5) 0.050(4) 0.028(3) -0.016(4) 0.015(4) -0.006(3) C49 0.045(4) 0.046(4) 0.032(3) -0.009(3) 0.015(3) 0.002(3) C50 0.037(4) 0.047(3) 0.025(3) -0.019(3) 0.009(3) -0.002(3) C51 0.032(4) 0.061(4) 0.041(4) -0.017(3) 0.004(3) 0.008(3) C52 0.034(4) 0.062(4) 0.037(4) -0.016(3) 0.010(3) 0.002(3) C53 0.065(5) 0.065(4) 0.031(4) -0.032(4) 0.015(4) -0.013(3) C54 0.054(5) 0.052(4) 0.036(4) -0.028(3) 0.014(3) -0.005(3) C55 0.053(4) 0.039(3) 0.042(4) -0.026(3) 0.029(3) -0.016(3) C56 0.060(5) 0.050(4) 0.045(4) -0.026(4) 0.030(4) -0.021(3) C57 0.062(5) 0.057(4) 0.059(5) -0.036(4) 0.041(4) -0.033(4) C58 0.087(6) 0.045(4) 0.067(5) -0.026(4) 0.050(5) -0.026(4) C59 0.067(5) 0.040(4) 0.054(5) -0.014(4) 0.036(4) -0.010(3) C60 0.051(4) 0.035(3) 0.044(4) -0.010(3) 0.029(3) -0.011(3) C61 0.050(4) 0.034(3) 0.047(4) -0.006(3) 0.020(3) -0.003(3) C62 0.054(4) 0.045(4) 0.039(4) 0.001(3) 0.021(3) -0.009(3) C63 0.041(4) 0.045(3) 0.033(3) 0.007(3) 0.019(3) -0.008(3) C64 0.046(4) 0.046(4) 0.039(4) 0.014(3) 0.015(3) -0.004(3) C65 0.036(4) 0.072(5) 0.049(5) 0.000(4) 0.012(3) -0.014(4) C66 0.040(4) 0.058(4) 0.054(5) -0.010(4) 0.013(4) -0.014(4) C67 0.036(4) 0.048(4) 0.047(4) -0.010(3) 0.010(3) -0.006(3) C68 0.036(3) 0.047(3) 0.032(3) 0.000(3) 0.016(3) -0.005(3) C69 0.055(4) 0.044(4) 0.031(3) 0.002(3) 0.017(3) -0.002(3) C70 0.054(4) 0.036(3) 0.030(3) -0.007(3) 0.019(3) -0.007(3) C71 0.040(4) 0.048(4) 0.032(3) -0.004(3) 0.012(3) -0.015(3) C72 0.039(4) 0.048(4) 0.039(4) -0.002(3) 0.020(3) -0.007(3) C73 0.039(4) 0.041(3) 0.035(4) 0.012(3) 0.005(3) 0.010(3) C74 0.042(4) 0.052(4) 0.061(5) -0.005(3) 0.013(4) 0.020(3) #============================================================================== _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'DirectMethod' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics 'ORTEP3' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 . Cu2 . 3.1239(9) yes Cu1 . O1 . 1.989(4) yes Cu1 . O2 . 2.261(4) yes Cu1 . O3 . 1.917(4) yes Cu1 . N1 . 2.038(5) yes Cu1 . N2 . 2.040(5) yes Cu2 . O1 . 1.980(4) yes Cu2 . O3 . 2.105(4) yes Cu2 . O4 . 1.985(4) yes Cu2 . N3 . 2.034(4) yes Cu2 . N4 . 2.094(5) yes Cu3 . Cu4 . 3.1141(11) yes Cu3 . O5 . 1.998(4) yes Cu3 . O6 . 2.232(4) yes Cu3 . O7 . 1.936(5) yes Cu3 . N5 . 2.030(6) yes Cu3 . N6 . 2.049(5) yes Cu4 . O5 . 1.972(4) yes Cu4 . O7 . 2.093(4) yes Cu4 . O8 . 1.989(4) yes Cu4 . N7 . 2.025(5) yes Cu4 . N8 . 2.059(5) yes Cl1 . O9 . 1.402(6) yes Cl1 . O11 . 1.429(7) yes Cl1 . O12 . 1.429(7) yes Cl1 . O10 . 1.402(6) yes Cl2 . O13 . 1.383(14) yes Cl2 . O14 . 1.338(8) yes Cl2 . O15 . 1.385(8) yes Cl2 . O16 . 1.274(7) yes O1 . C1 . 1.354(6) yes O2 . C14 . 1.382(7) yes O3 . C19 . 1.364(7) yes O4 . C32 . 1.349(6) yes O5 . C37 . 1.359(6) yes O6 . C50 . 1.369(7) yes O7 . C55 . 1.353(7) yes O8 . C68 . 1.347(8) yes O17 . C73 . 1.436(7) yes O18 . C74 . 1.430(7) yes N1 . C7 . 1.498(8) yes N1 . C8 . 1.522(7) yes N1 . C15 . 1.484(7) yes N2 . C16 . 1.494(8) yes N2 . C17 . 1.500(8) yes N2 . C18 . 1.501(7) yes N3 . C25 . 1.517(7) yes N3 . C26 . 1.510(7) yes N3 . C34 . 1.481(8) yes N4 . C33 . 1.481(7) yes N4 . C35 . 1.464(8) yes N4 . C36 . 1.479(7) yes N5 . C43 . 1.525(8) yes N5 . C44 . 1.496(7) yes N5 . C51 . 1.508(8) yes N6 . C52 . 1.497(9) yes N6 . C53 . 1.482(8) yes N6 . C54 . 1.483(8) yes N7 . C61 . 1.505(8) yes N7 . C62 . 1.502(8) yes N7 . C69 . 1.504(8) yes N8 . C70 . 1.488(8) yes N8 . C71 . 1.508(8) yes N8 . C72 . 1.454(8) yes C1 . C2 . 1.389(8) yes C1 . C6 . 1.409(8) yes C2 . C3 . 1.379(8) yes C2 . H1 . 0.949 no C3 . C4 . 1.376(9) yes C3 . H2 . 0.948 no C4 . C5 . 1.378(9) yes C4 . H3 . 0.950 no C5 . C6 . 1.412(8) yes C5 . H4 . 0.948 no C6 . C7 . 1.508(8) yes C7 . H5 . 0.951 no C7 . H6 . 0.949 no C8 . C9 . 1.483(9) yes C8 . H7 . 0.951 no C8 . H8 . 0.950 no C9 . C10 . 1.393(8) yes C9 . C14 . 1.398(8) yes C10 . C11 . 1.396(11) yes C10 . H9 . 0.951(7) no C11 . C12 . 1.395(11) yes C11 . H10 . 0.948(7) no C12 . C13 . 1.391(9) yes C12 . H11 . 0.947 no C13 . C14 . 1.404(9) yes C13 . H12 . 0.949 no C15 . C16 . 1.505(8) yes C15 . H13 . 0.948 no C15 . H14 . 0.950 no C16 . H15 . 0.951 no C16 . H16 . 0.949 no C17 . H17 . 0.947 no C17 . H18 . 0.948 no C17 . H19 . 0.953 no C18 . H20 . 0.948 no C18 . H21 . 0.949 no C18 . H22 . 0.952 no C19 . C20 . 1.379(9) yes C19 . C24 . 1.400(8) yes C20 . C21 . 1.400(9) yes C20 . H23 . 0.949 no C21 . C22 . 1.37(1) yes C21 . H24 . 0.954 no C22 . C23 . 1.37(1) yes C22 . H25 . 0.950 no C23 . C24 . 1.416(8) yes C23 . H26 . 0.950 no C24 . C25 . 1.508(9) yes C25 . H27 . 0.949 no C25 . H28 . 0.951 no C26 . C27 . 1.494(8) yes C26 . H29 . 0.950 no C26 . H30 . 0.946 no C27 . C28 . 1.404(8) yes C27 . C32 . 1.409(8) yes C28 . C29 . 1.399(9) yes C28 . H31 . 0.952 no C29 . C30 . 1.375(9) yes C29 . H32 . 0.953 no C30 . C31 . 1.399(8) yes C30 . H33 . 0.953 no C31 . C32 . 1.388(8) yes C31 . H34 . 0.952 no C33 . C34 . 1.532(9) yes C33 . H37 . 0.950 no C33 . H38 . 0.949 no C34 . H35 . 0.950 no C34 . H36 . 0.952 no C35 . H39 . 0.948 no C35 . H40 . 0.950 no C35 . H41 . 0.951 no C36 . H42 . 0.952 no C36 . H43 . 0.953 no C36 . H44 . 0.945 no C37 . C38 . 1.389(8) yes C37 . C42 . 1.413(9) yes C38 . C39 . 1.410(8) yes C38 . H45 . 0.949 no C39 . C40 . 1.39(1) yes C39 . H46 . 0.951 no C40 . C41 . 1.38(1) yes C40 . H47 . 0.952 no C41 . C42 . 1.391(8) yes C41 . H48 . 0.950 no C42 . C43 . 1.497(9) yes C43 . H49 . 0.953 no C43 . H50 . 0.948 no C44 . C45 . 1.500(8) yes C44 . H51 . 0.947 no C44 . H52 . 0.951 no C45 . C46 . 1.398(9) yes C45 . C50 . 1.399(9) yes C46 . C47 . 1.390(9) yes C46 . H53 . 0.948 no C47 . C48 . 1.389(11) yes C47 . H54 . 0.949 no C48 . C49 . 1.39(1) yes C48 . H55 . 0.951 no C49 . C50 . 1.382(8) yes C49 . H56 . 0.949 no C51 . C52 . 1.499(9) yes C51 . H57 . 0.952 no C51 . H58 . 0.948 no C52 . H59 . 0.947 no C52 . H60 . 0.952 no C53 . H61 . 0.952 no C53 . H62 . 0.951 no C53 . H63 . 0.948 no C54 . H64 . 0.950 no C54 . H65 . 0.952 no C54 . H66 . 0.952 no C55 . C56 . 1.406(9) yes C55 . C60 . 1.39(1) yes C56 . C57 . 1.42(1) yes C56 . H67 . 0.948 no C57 . C58 . 1.357(12) yes C57 . H68 . 0.951 no C58 . C59 . 1.41(1) yes C58 . H69 . 0.948 no C59 . C60 . 1.385(8) yes C59 . H70 . 0.946 no C60 . C61 . 1.501(9) yes C61 . H71 . 0.952 no C61 . H72 . 0.949 no C62 . C63 . 1.513(9) yes C62 . H73 . 0.953 no C62 . H74 . 0.948 no C63 . C64 . 1.42(1) yes C63 . C68 . 1.405(9) yes C64 . C65 . 1.41(1) yes C64 . H75 . 0.953 no C65 . C66 . 1.392(11) yes C65 . H76 . 0.952 no C66 . C67 . 1.37(1) yes C66 . H77 . 0.951 no C67 . C68 . 1.400(9) yes C67 . H78 . 0.949 no C69 . C70 . 1.523(9) yes C69 . H79 . 0.948 no C69 . H80 . 0.951 no C70 . H81 . 0.951 no C70 . H82 . 0.948 no C71 . H83 . 0.948 no C71 . H84 . 0.949 no C71 . H85 . 0.950 no C72 . H86 . 0.949 no C72 . H87 . 0.952 no C72 . H88 . 0.948 no C74 . H92 . 0.952 no C74 . H93 . 0.943 no C74 . H94 . 0.954 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cu2 . Cu1 . O1 . 38.0(1) yes Cu2 . Cu1 . O2 . 96.1(1) yes O1 . Cu1 . O2 . 88.97(15) yes Cu2 . Cu1 . O3 . 41.27(11) yes O1 . Cu1 . O3 . 79.11(15) yes O2 . Cu1 . O3 . 96.65(16) yes Cu2 . Cu1 . N1 . 132.01(14) yes O1 . Cu1 . N1 . 94.58(17) yes O2 . Cu1 . N1 . 87.55(17) yes O3 . Cu1 . N1 . 172.32(19) yes Cu2 . Cu1 . N2 . 127.03(13) yes O1 . Cu1 . N2 . 146.78(18) yes O2 . Cu1 . N2 . 124.24(17) yes O3 . Cu1 . N2 . 96.18(17) yes N1 . Cu1 . N2 . 86.69(19) yes Cu1 . Cu2 . O1 . 38.20(11) yes Cu1 . Cu2 . O3 . 36.9(1) yes O1 . Cu2 . O3 . 74.99(15) yes Cu1 . Cu2 . O4 . 103.97(11) yes O1 . Cu2 . O4 . 95.95(15) yes O3 . Cu2 . O4 . 102.17(17) yes Cu1 . Cu2 . N3 . 129.23(13) yes O1 . Cu2 . N3 . 166.05(17) yes O3 . Cu2 . N3 . 93.23(16) yes O4 . Cu2 . N3 . 93.81(18) yes Cu1 . Cu2 . N4 . 107.06(13) yes O1 . Cu2 . N4 . 93.27(17) yes O3 . Cu2 . N4 . 117.66(17) yes O4 . Cu2 . N4 . 140.15(17) yes N3 . Cu2 . N4 . 85.55(19) yes Cu4 . Cu3 . O5 . 38.05(12) yes Cu4 . Cu3 . O6 . 97.02(12) yes O5 . Cu3 . O6 . 89.10(16) yes Cu4 . Cu3 . O7 . 41.27(12) yes O5 . Cu3 . O7 . 78.86(17) yes O6 . Cu3 . O7 . 94.79(18) yes Cu4 . Cu3 . N5 . 132.02(15) yes O5 . Cu3 . N5 . 94.72(19) yes O6 . Cu3 . N5 . 87.63(18) yes O7 . Cu3 . N5 . 173.08(19) yes Cu4 . Cu3 . N6 . 125.31(16) yes O5 . Cu3 . N6 . 145.80(18) yes O6 . Cu3 . N6 . 125.10(19) yes O7 . Cu3 . N6 . 96.6(2) yes N5 . Cu3 . N6 . 87.2(2) yes Cu3 . Cu4 . O5 . 38.65(11) yes Cu3 . Cu4 . O7 . 37.60(12) yes O5 . Cu4 . O7 . 75.81(17) yes Cu3 . Cu4 . O8 . 105.40(14) yes O5 . Cu4 . O8 . 95.91(17) yes O7 . Cu4 . O8 . 101.36(18) yes Cu3 . Cu4 . N7 . 128.40(15) yes O5 . Cu4 . N7 . 165.89(19) yes O7 . Cu4 . N7 . 92.34(19) yes O8 . Cu4 . N7 . 93.9(2) yes Cu3 . Cu4 . N8 . 109.11(16) yes O5 . Cu4 . N8 . 93.39(19) yes O7 . Cu4 . N8 . 123.64(19) yes O8 . Cu4 . N8 . 134.95(19) yes N7 . Cu4 . N8 . 86.8(2) yes O9 . Cl1 . O11 . 104.4(5) yes O9 . Cl1 . O12 . 107.4(5) yes O11 . Cl1 . O12 . 111.1(5) yes O9 . Cl1 . O10 . 110.6(5) yes O11 . Cl1 . O10 . 109.9(4) yes O12 . Cl1 . O10 . 113.0(5) yes O13 . Cl2 . O14 . 106.6(9) yes O13 . Cl2 . O15 . 113.7(8) yes O14 . Cl2 . O15 . 116.2(9) yes O13 . Cl2 . O16 . 110.5(11) yes O14 . Cl2 . O16 . 100.6(11) yes O15 . Cl2 . O16 . 108.4(8) yes Cu1 . O1 . Cu2 . 103.81(16) yes Cu1 . O1 . C1 . 123.1(3) yes Cu2 . O1 . C1 . 131.4(3) yes Cu1 . O2 . C14 . 109.8(3) yes Cu1 . O3 . Cu2 . 101.80(16) yes Cu1 . O3 . C19 . 133.2(4) yes Cu2 . O3 . C19 . 120.5(3) yes Cu2 . O4 . C32 . 116.4(3) yes Cu3 . O5 . Cu4 . 103.30(18) yes Cu3 . O5 . C37 . 124.7(4) yes Cu4 . O5 . C37 . 131.5(4) yes Cu3 . O6 . C50 . 111.4(4) yes Cu3 . O7 . Cu4 . 101.14(17) yes Cu3 . O7 . C55 . 134.5(4) yes Cu4 . O7 . C55 . 122.9(4) yes Cu4 . O8 . C68 . 114.8(4) yes Cu1 . N1 . C7 . 107.5(3) yes Cu1 . N1 . C8 . 114.4(4) yes C7 . N1 . C8 . 109.7(5) yes Cu1 . N1 . C15 . 107.0(3) yes C7 . N1 . C15 . 109.2(5) yes C8 . N1 . C15 . 109.1(4) yes Cu1 . N2 . C16 . 102.5(3) yes Cu1 . N2 . C17 . 114.7(4) yes C16 . N2 . C17 . 110.9(5) yes Cu1 . N2 . C18 . 112.6(3) yes C16 . N2 . C18 . 108.3(5) yes C17 . N2 . C18 . 107.6(5) yes Cu2 . N3 . C25 . 109.2(3) yes Cu2 . N3 . C26 . 112.7(3) yes C25 . N3 . C26 . 109.1(4) yes Cu2 . N3 . C34 . 106.0(3) yes C25 . N3 . C34 . 109.9(5) yes C26 . N3 . C34 . 109.9(4) yes Cu2 . N4 . C33 . 107.7(4) yes Cu2 . N4 . C35 . 114.8(4) yes C33 . N4 . C35 . 109.4(5) yes Cu2 . N4 . C36 . 105.5(4) yes C33 . N4 . C36 . 109.6(4) yes C35 . N4 . C36 . 109.8(5) yes Cu3 . N5 . C43 . 107.7(4) yes Cu3 . N5 . C44 . 115.2(4) yes C43 . N5 . C44 . 109.1(5) yes Cu3 . N5 . C51 . 106.4(4) yes C43 . N5 . C51 . 109.1(5) yes C44 . N5 . C51 . 109.2(5) yes Cu3 . N6 . C52 . 102.8(4) yes Cu3 . N6 . C53 . 114.7(4) yes C52 . N6 . C53 . 109.5(6) yes Cu3 . N6 . C54 . 111.9(4) yes C52 . N6 . C54 . 108.9(5) yes C53 . N6 . C54 . 108.9(5) yes Cu4 . N7 . C61 . 110.2(4) yes Cu4 . N7 . C62 . 112.2(4) yes C61 . N7 . C62 . 109.7(5) yes Cu4 . N7 . C69 . 106.5(4) yes C61 . N7 . C69 . 109.1(5) yes C62 . N7 . C69 . 109.1(5) yes Cu4 . N8 . C70 . 106.0(3) yes Cu4 . N8 . C71 . 106.8(3) yes C70 . N8 . C71 . 109.1(5) yes Cu4 . N8 . C72 . 115.0(4) yes C70 . N8 . C72 . 109.2(5) yes C71 . N8 . C72 . 110.5(5) yes O1 . C1 . C2 . 121.8(5) yes O1 . C1 . C6 . 118.9(5) yes C2 . C1 . C6 . 119.3(5) yes C1 . C2 . C3 . 120.3(5) yes C1 . C2 . H1 . 119.8 no C3 . C2 . H1 . 119.9 no C2 . C3 . C4 . 121.5(6) yes C2 . C3 . H2 . 119.3 no C4 . C3 . H2 . 119.2 no C3 . C4 . C5 . 119.1(5) yes C3 . C4 . H3 . 120.5 no C5 . C4 . H3 . 120.4 no C4 . C5 . C6 . 121.0(6) yes C4 . C5 . H4 . 119.6 no C6 . C5 . H4 . 119.4 no C1 . C6 . C5 . 118.7(5) yes C1 . C6 . C7 . 120.6(5) yes C5 . C6 . C7 . 120.7(5) yes N1 . C7 . C6 . 113.1(5) yes N1 . C7 . H5 . 108.4 no C6 . C7 . H5 . 108.6 no N1 . C7 . H6 . 108.6 no C6 . C7 . H6 . 108.5 no H5 . C7 . H6 . 109.5 no N1 . C8 . C9 . 113.9(5) yes N1 . C8 . H7 . 108.3 no C9 . C8 . H7 . 108.3 no N1 . C8 . H8 . 108.4 no C9 . C8 . H8 . 108.4 no H7 . C8 . H8 . 109.4 no C8 . C9 . C10 . 123.7(6) yes C8 . C9 . C14 . 118.9(5) yes C10 . C9 . C14 . 117.4(6) yes C9 . C10 . C11 . 121.2(7) yes C9 . C10 . H9 . 119.3 no C11 . C10 . H9 . 119.5 no C10 . C11 . C12 . 120.5(6) yes C10 . C11 . H10 . 119.9 no C12 . C11 . H10 . 119.6 no C11 . C12 . C13 . 119.7(7) yes C11 . C12 . H11 . 120.2 no C13 . C12 . H11 . 120.2 no C12 . C13 . C14 . 118.8(6) yes C12 . C13 . H12 . 120.8 no C14 . C13 . H12 . 120.4 no O2 . C14 . C9 . 115.7(5) yes O2 . C14 . C13 . 121.9(5) yes C9 . C14 . C13 . 122.4(5) yes N1 . C15 . C16 . 110.5(5) yes N1 . C15 . H13 . 109.1 no C16 . C15 . H13 . 109.3 no N1 . C15 . H14 . 109.1 no C16 . C15 . H14 . 109.3 no H13 . C15 . H14 . 109.6 no N2 . C16 . C15 . 108.5(5) yes N2 . C16 . H15 . 109.5 no C15 . C16 . H15 . 109.8 no N2 . C16 . H16 . 109.5 no C15 . C16 . H16 . 110.0 no H15 . C16 . H16 . 109.5 no N2 . C17 . H17 . 109.4 no N2 . C17 . H18 . 109.5 no H17 . C17 . H18 . 109.9 no N2 . C17 . H19 . 109.2 no H17 . C17 . H19 . 109.5 no H18 . C17 . H19 . 109.4 no N2 . C18 . H20 . 109.5 no N2 . C18 . H21 . 109.4 no H20 . C18 . H21 . 109.7 no N2 . C18 . H22 . 109.3 no H20 . C18 . H22 . 109.5 no H21 . C18 . H22 . 109.4 no O3 . C19 . C20 . 123.0(5) yes O3 . C19 . C24 . 117.2(6) yes C20 . C19 . C24 . 119.8(6) yes C19 . C20 . C21 . 120.5(6) yes C19 . C20 . H23 . 119.6 no C21 . C20 . H23 . 119.9 no C20 . C21 . C22 . 120.1(6) yes C20 . C21 . H24 . 120.2 no C22 . C21 . H24 . 119.8 no C21 . C22 . C23 . 120.4(6) yes C21 . C22 . H25 . 119.8 no C23 . C22 . H25 . 119.9 no C22 . C23 . C24 . 120.4(6) yes C22 . C23 . H26 . 119.9 no C24 . C23 . H26 . 119.8 no C19 . C24 . C23 . 118.9(6) yes C19 . C24 . C25 . 121.0(5) yes C23 . C24 . C25 . 120.1(5) yes N3 . C25 . C24 . 114.6(5) yes N3 . C25 . H27 . 108.3 no C24 . C25 . H27 . 108.1 no N3 . C25 . H28 . 108.2 no C24 . C25 . H28 . 108.1 no H27 . C25 . H28 . 109.4 no N3 . C26 . C27 . 113.3(5) yes N3 . C26 . H29 . 108.3 no C27 . C26 . H29 . 108.3 no N3 . C26 . H30 . 108.6 no C27 . C26 . H30 . 108.6 no H29 . C26 . H30 . 109.7 no C26 . C27 . C28 . 121.8(5) yes C26 . C27 . C32 . 118.9(5) yes C28 . C27 . C32 . 118.9(5) yes C27 . C28 . C29 . 121.0(6) yes C27 . C28 . H31 . 119.4 no C29 . C28 . H31 . 119.6 no C28 . C29 . C30 . 118.9(5) yes C28 . C29 . H32 . 120.7 no C30 . C29 . H32 . 120.5 no C29 . C30 . C31 . 121.5(5) yes C29 . C30 . H33 . 119.4 no C31 . C30 . H33 . 119.1 no C30 . C31 . C32 . 119.7(5) yes C30 . C31 . H34 . 120.3 no C32 . C31 . H34 . 120.0 no O4 . C32 . C27 . 119.7(5) yes O4 . C32 . C31 . 120.3(5) yes C27 . C32 . C31 . 120.0(5) yes N4 . C33 . C34 . 109.1(5) yes N4 . C33 . H37 . 109.6 no C34 . C33 . H37 . 109.5 no N4 . C33 . H38 . 109.6 no C34 . C33 . H38 . 109.5 no H37 . C33 . H38 . 109.5 no N3 . C34 . C33 . 110.2(5) yes N3 . C34 . H35 . 109.2 no C33 . C34 . H35 . 109.6 no N3 . C34 . H36 . 109.1 no C33 . C34 . H36 . 109.5 no H35 . C34 . H36 . 109.3 no N4 . C35 . H39 . 109.4 no N4 . C35 . H40 . 109.4 no H39 . C35 . H40 . 109.6 no N4 . C35 . H41 . 109.4 no H39 . C35 . H41 . 109.6 no H40 . C35 . H41 . 109.4 no N4 . C36 . H42 . 109.4 no N4 . C36 . H43 . 109.3 no H42 . C36 . H43 . 109.1 no N4 . C36 . H44 . 109.6 no H42 . C36 . H44 . 109.8 no H43 . C36 . H44 . 109.7 no O5 . C37 . C38 . 120.8(6) yes O5 . C37 . C42 . 119.0(5) yes C38 . C37 . C42 . 120.2(5) yes C37 . C38 . C39 . 119.9(6) yes C37 . C38 . H45 . 120.1 no C39 . C38 . H45 . 120.1 no C38 . C39 . C40 . 119.7(6) yes C38 . C39 . H46 . 120.0 no C40 . C39 . H46 . 120.3 no C39 . C40 . C41 . 120.0(6) yes C39 . C40 . H47 . 119.9 no C41 . C40 . H47 . 120.1 no C40 . C41 . C42 . 121.4(6) yes C40 . C41 . H48 . 119.0 no C42 . C41 . H48 . 119.6 no C37 . C42 . C41 . 118.8(6) yes C37 . C42 . C43 . 121.6(5) yes C41 . C42 . C43 . 119.6(6) yes N5 . C43 . C42 . 114.0(5) yes N5 . C43 . H49 . 108.2 no C42 . C43 . H49 . 108.3 no N5 . C43 . H50 . 108.3 no C42 . C43 . H50 . 108.5 no H49 . C43 . H50 . 109.4 no N5 . C44 . C45 . 112.8(5) yes N5 . C44 . H51 . 108.7 no C45 . C44 . H51 . 108.7 no N5 . C44 . H52 . 108.3 no C45 . C44 . H52 . 108.7 no H51 . C44 . H52 . 109.6 no C44 . C45 . C46 . 122.0(6) yes C44 . C45 . C50 . 118.5(6) yes C46 . C45 . C50 . 119.4(6) yes C45 . C46 . C47 . 119.9(7) yes C45 . C46 . H53 . 120.1 no C47 . C46 . H53 . 120.0 no C46 . C47 . C48 . 119.6(7) yes C46 . C47 . H54 . 120.4 no C48 . C47 . H54 . 120.0 no C47 . C48 . C49 . 121.2(6) yes C47 . C48 . H55 . 119.4 no C49 . C48 . H55 . 119.4 no C48 . C49 . C50 . 118.9(7) yes C48 . C49 . H56 . 120.5 no C50 . C49 . H56 . 120.7 no O6 . C50 . C45 . 115.9(5) yes O6 . C50 . C49 . 122.9(6) yes C45 . C50 . C49 . 120.9(6) yes N5 . C51 . C52 . 110.4(6) yes N5 . C51 . H57 . 109.1 no C52 . C51 . H57 . 109.3 no N5 . C51 . H58 . 109.3 no C52 . C51 . H58 . 109.4 no H57 . C51 . H58 . 109.4 no N6 . C52 . C51 . 108.6(5) yes N6 . C52 . H59 . 109.9 no C51 . C52 . H59 . 109.7 no N6 . C52 . H60 . 109.6 no C51 . C52 . H60 . 109.5 no H59 . C52 . H60 . 109.6 no N6 . C53 . H61 . 109.5 no N6 . C53 . H62 . 109.5 no H61 . C53 . H62 . 109.2 no N6 . C53 . H63 . 109.6 no H61 . C53 . H63 . 109.5 no H62 . C53 . H63 . 109.5 no N6 . C54 . H64 . 109.8 no N6 . C54 . H65 . 109.6 no H64 . C54 . H65 . 109.3 no N6 . C54 . H66 . 109.6 no H64 . C54 . H66 . 109.4 no H65 . C54 . H66 . 109.2 no O7 . C55 . C56 . 121.2(7) yes O7 . C55 . C60 . 118.6(5) yes C56 . C55 . C60 . 120.2(6) yes C55 . C56 . C57 . 119.3(7) yes C55 . C56 . H67 . 120.4 no C57 . C56 . H67 . 120.4 no C56 . C57 . C58 . 120.2(6) yes C56 . C57 . H68 . 119.6 no C58 . C57 . H68 . 120.2 no C57 . C58 . C59 . 120.0(7) yes C57 . C58 . H69 . 120.1 no C59 . C58 . H69 . 119.9 no C58 . C59 . C60 . 120.8(8) yes C58 . C59 . H70 . 119.5 no C60 . C59 . H70 . 119.7 no C55 . C60 . C59 . 119.3(6) yes C55 . C60 . C61 . 120.4(5) yes C59 . C60 . C61 . 120.1(6) yes N7 . C61 . C60 . 114.5(5) yes N7 . C61 . H71 . 108.1 no C60 . C61 . H71 . 108.2 no N7 . C61 . H72 . 108.3 no C60 . C61 . H72 . 108.3 no H71 . C61 . H72 . 109.4 no N7 . C62 . C63 . 112.2(5) yes N7 . C62 . H73 . 108.7 no C63 . C62 . H73 . 108.6 no N7 . C62 . H74 . 109.1 no C63 . C62 . H74 . 108.9 no H73 . C62 . H74 . 109.3 no C62 . C63 . C64 . 120.8(6) yes C62 . C63 . C68 . 119.1(6) yes C64 . C63 . C68 . 119.9(6) yes C63 . C64 . C65 . 120.8(6) yes C63 . C64 . H75 . 119.4 no C65 . C64 . H75 . 119.8 no C64 . C65 . C66 . 116.6(7) yes C64 . C65 . H76 . 121.5 no C66 . C65 . H76 . 121.9 no C65 . C66 . C67 . 124.3(7) yes C65 . C66 . H77 . 117.8 no C67 . C66 . H77 . 117.9 no C66 . C67 . C68 . 119.1(7) yes C66 . C67 . H78 . 120.6 no C68 . C67 . H78 . 120.4 no O8 . C68 . C63 . 118.7(6) yes O8 . C68 . C67 . 121.9(6) yes C63 . C68 . C67 . 119.4(7) yes N7 . C69 . C70 . 107.9(6) yes N7 . C69 . H79 . 109.9 no C70 . C69 . H79 . 109.8 no N7 . C69 . H80 . 109.8 no C70 . C69 . H80 . 109.7 no H79 . C69 . H80 . 109.6 no N8 . C70 . C69 . 110.4(5) yes N8 . C70 . H81 . 109.3 no C69 . C70 . H81 . 109.0 no N8 . C70 . H82 . 109.5 no C69 . C70 . H82 . 109.2 no H81 . C70 . H82 . 109.5 no N8 . C71 . H83 . 109.3 no N8 . C71 . H84 . 109.3 no H83 . C71 . H84 . 109.8 no N8 . C71 . H85 . 109.2 no H83 . C71 . H85 . 109.6 no H84 . C71 . H85 . 109.6 no N8 . C72 . H86 . 109.4 no N8 . C72 . H87 . 109.3 no H86 . C72 . H87 . 109.4 no N8 . C72 . H88 . 109.4 no H86 . C72 . H88 . 109.7 no H87 . C72 . H88 . 109.5 no O18 . C74 . H92 . 109.2 no O18 . C74 . H93 . 109.8 no H92 . C74 . H93 . 109.9 no O18 . C74 . H94 . 109.2 no H92 . C74 . H94 . 109.0 no H93 . C74 . H94 . 109.7 no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================