# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_date 2004-10-26 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? _publ_contact_author_name 'Tomoaki Tanase' _publ_contact_author_address ; Department of Chemistry Nara Women's University Kitauoya-higashi-machi Nara Nara prefecture 630-8285 JAPAN ; _publ_contact_author_email tanase@cc.nara-wu.ac.jp _publ_contact_author_fax +81-742-20-3399 _publ_contact_author_phone +81-742-20-3399 _publ_section_title ; Trinuclear coordinatively labile Cu(II) complex of 4,6-O-ethylidene-beta-D-glucopyranosylamine derived Schiff base ligand and its reactivity towards primary alcohols and amines ; loop_ _publ_author_name 'Tomoaki Tanase' 'Merii Kato' 'Ajay Sah' data_Complex_2a _database_code_depnum_ccdc_archive 'CCDC 250717' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C40 H56 Cu3 N2 O14 ' _chemical_formula_moiety 'C40 H56 Cu3 N2 O14 ' _chemical_formula_weight 979.53 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 6.4406(2) _cell_length_b 14.9072(5) _cell_length_c 42.412(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4072.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7675 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036.00 _exptl_absorpt_coefficient_mu 1.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 0.922 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 22509 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_max 27.25 _diffrn_measured_fraction_theta_max 0.6845 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.7605 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 44 #============================================================================== # 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 17330 _reflns_number_gt 13172 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0500 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 13250 _refine_ls_number_parameters 593 _refine_ls_goodness_of_fit_ref 0.409 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0090 _refine_diff_density_max 2.32 _refine_diff_density_min -1.75 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 13743 Friedel Pairs' _refine_ls_abs_structure_Flack 0.04(1) 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 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; 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 Cu(1) Cu -0.48757(10) -0.34120(4) -0.07628(2) 0.0225(2) Uani 1.00 1 d . . . Cu(2) Cu -0.11198(10) -0.22180(4) -0.12655(2) 0.0232(2) Uani 1.00 1 d . . . Cu(3) Cu 0.30691(10) -0.10237(4) -0.16741(2) 0.0212(2) Uani 1.00 1 d . . . O(1) O -0.6646(5) -0.4315(2) -0.05968(8) 0.0232(11) Uani 1.00 1 d . . . O(2) O -0.3227(5) -0.2447(2) -0.09482(8) 0.0215(11) Uani 1.00 1 d . . . O(3) O -0.1729(5) -0.0965(2) -0.12336(8) 0.0222(10) Uani 1.00 1 d . . . O(4) O -0.3100(5) 0.0792(2) -0.09199(8) 0.0228(11) Uani 1.00 1 d . . . O(5) O -0.6895(5) -0.0855(2) -0.06232(8) 0.0252(11) Uani 1.00 1 d . . . O(6) O -0.5785(6) 0.1533(2) -0.06580(8) 0.0287(12) Uani 1.00 1 d . . . O(7) O 0.4566(5) -0.0122(2) -0.18881(8) 0.0229(11) Uani 1.00 1 d . . . O(8) O 0.1427(5) -0.1986(2) -0.14930(8) 0.0232(11) Uani 1.00 1 d . . . O(9) O -0.0900(5) -0.3451(2) -0.13849(7) 0.0239(11) Uani 1.00 1 d . . . O(10) O 0.1275(6) -0.5227(2) -0.15236(8) 0.0254(11) Uani 1.00 1 d . . . O(11) O 0.4726(6) -0.3570(2) -0.19054(7) 0.0245(11) Uani 1.00 1 d . . . O(12) O 0.3928(6) -0.5976(2) -0.17894(8) 0.0341(12) Uani 1.00 1 d . . . O(13) O -0.3112(6) -0.4236(2) -0.09908(9) 0.0276(12) Uani 1.00 1 d . . . O(14) O 0.1359(5) -0.0195(2) -0.14349(8) 0.0246(11) Uani 1.00 1 d . . . N(1) N -0.6565(7) -0.2462(2) -0.05836(10) 0.020(1) Uani 1.00 1 d . . . N(2) N 0.4861(7) -0.1968(3) -0.18329(9) 0.0176(13) Uani 1.00 1 d . . . C(1) C -0.5499(7) -0.1593(3) -0.06128(12) 0.020(2) Uani 1.00 1 d . . . C(2) C -0.4319(7) -0.1630(3) -0.09177(12) 0.020(2) Uani 1.00 1 d . . . C(3) C -0.2884(8) -0.0843(3) -0.09537(13) 0.024(2) Uani 1.00 1 d . . . C(4) C -0.4272(7) -0.0022(3) -0.09412(12) 0.020(2) Uani 1.00 1 d . . . C(5) C -0.5661(8) -0.0044(3) -0.06444(12) 0.022(2) Uani 1.00 1 d . . . C(6) C -0.7073(8) 0.0759(3) -0.06521(12) 0.028(2) Uani 1.00 1 d . . . C(7) C -0.4398(8) 0.1545(3) -0.09205(12) 0.024(2) Uani 1.00 1 d . . . C(8) C -0.3053(9) 0.2349(3) -0.09038(13) 0.042(2) Uani 1.00 1 d . . . C(9) C -0.8330(8) -0.2556(3) -0.04693(12) 0.023(2) Uani 1.00 1 d . . . C(10) C -0.9352(8) -0.3379(3) -0.03904(11) 0.018(2) Uani 1.00 1 d . . . C(11) C -0.8364(8) -0.4221(3) -0.04449(11) 0.018(2) Uani 1.00 1 d . . . C(12) C -0.9389(7) -0.5019(3) -0.03230(11) 0.018(2) Uani 1.00 1 d . . . C(13) C -1.1273(8) -0.4906(3) -0.01826(11) 0.022(2) Uani 1.00 1 d . . . C(14) C -1.2269(8) -0.4062(4) -0.01470(11) 0.024(2) Uani 1.00 1 d . . . C(15) C -1.1308(8) -0.3320(4) -0.02455(11) 0.024(2) Uani 1.00 1 d . . . C(16) C -0.8383(8) -0.5969(3) -0.03525(12) 0.025(2) Uani 1.00 1 d . . . C(17) C -0.8242(8) -0.6212(3) -0.06999(11) 0.022(2) Uani 1.00 1 d . . . C(18) C -0.6250(8) -0.5954(3) -0.01948(13) 0.035(2) Uani 1.00 1 d . . . C(19) C -0.9630(8) -0.6679(3) -0.01807(11) 0.030(2) Uani 1.00 1 d . . . C(20) C 0.4272(7) -0.2831(3) -0.17029(12) 0.021(2) Uani 1.00 1 d . . . C(21) C 0.1941(8) -0.2790(3) -0.16446(11) 0.017(1) Uani 1.00 1 d . . . C(22) C 0.1236(8) -0.3614(3) -0.14608(11) 0.016(2) Uani 1.00 1 d . . . C(23) C 0.1733(8) -0.4389(3) -0.16707(13) 0.023(2) Uani 1.00 1 d . . . C(24) C 0.4081(8) -0.4382(3) -0.17475(12) 0.020(2) Uani 1.00 1 d . . . C(25) C 0.4652(8) -0.5185(3) -0.19443(12) 0.028(2) Uani 1.00 1 d . . . C(26) C 0.1774(9) -0.5956(3) -0.17258(12) 0.028(2) Uani 1.00 1 d . . . C(27) C 0.1223(10) -0.6791(3) -0.15576(12) 0.047(2) Uani 1.00 1 d . . . C(28) C 0.6523(8) -0.1856(3) -0.19944(11) 0.020(2) Uani 1.00 1 d . . . C(29) C 0.7244(8) -0.1019(4) -0.21134(12) 0.022(2) Uani 1.00 1 d . . . C(30) C 0.6216(8) -0.0197(3) -0.20633(11) 0.019(2) Uani 1.00 1 d . . . C(31) C 0.7074(9) 0.0617(4) -0.21944(12) 0.023(2) Uani 1.00 1 d . . . C(32) C 0.8926(9) 0.0534(3) -0.23755(12) 0.030(2) Uani 1.00 1 d . . . C(33) C 0.9957(9) -0.0301(4) -0.24111(12) 0.030(2) Uani 1.00 1 d . . . C(34) C 0.9105(8) -0.1042(4) -0.22856(11) 0.022(2) Uani 1.00 1 d . . . C(35) C 0.6109(8) 0.1540(4) -0.21545(12) 0.024(2) Uani 1.00 1 d . . . C(36) C 0.6117(8) 0.1770(3) -0.17965(11) 0.030(2) Uani 1.00 1 d . . . C(37) C 0.3882(8) 0.1550(4) -0.22782(11) 0.026(2) Uani 1.00 1 d . . . C(38) C 0.7280(8) 0.2270(3) -0.23213(11) 0.029(2) Uani 1.00 1 d . . . C(39) C -0.3200(8) -0.5186(3) -0.10065(12) 0.030(2) Uani 1.00 1 d . . . C(40) C 0.0826(8) 0.0680(3) -0.15308(12) 0.031(2) Uani 1.00 1 d . . . H(1) H -0.237(7) -0.401(3) -0.1144(11) 0.0328 Uiso 1.00 1 c . . . H(2) H -0.013(8) -0.057(3) -0.1374(10) 0.0299 Uiso 1.00 1 c . . . H(3) H -0.9090 -0.2020 -0.0431 0.027 Uiso 1.00 1 c R . . H(4) H -1.1971 -0.5423 -0.0105 0.027 Uiso 1.00 1 c R . . H(5) H -1.3592 -0.4023 -0.0049 0.029 Uiso 1.00 1 c R . . H(6) H -1.1971 -0.2755 -0.0222 0.029 Uiso 1.00 1 c R . . H(7) H 0.7318 -0.2376 -0.2041 0.024 Uiso 1.00 1 c R . . H(8) H 0.9502 0.1052 -0.2472 0.036 Uiso 1.00 1 c R . . H(9) H 1.1230 -0.0332 -0.2524 0.036 Uiso 1.00 1 c R . . H(10) H 0.9802 -0.1598 -0.2313 0.026 Uiso 1.00 1 c R . . H(11) H -0.2809 0.2514 -0.0691 0.050 Uiso 1.00 1 c R . . H(12) H -0.3748 0.2823 -0.1010 0.050 Uiso 1.00 1 c R . . H(13) H -0.1765 0.2233 -0.1005 0.050 Uiso 1.00 1 c R . . H(14) H -0.9470 -0.6512 -0.0765 0.027 Uiso 1.00 1 c R . . H(15) H -0.7079 -0.6594 -0.0731 0.027 Uiso 1.00 1 c R . . H(16) H -0.8070 -0.5681 -0.0821 0.027 Uiso 1.00 1 c R . . H(17) H -0.5229 -0.5789 -0.0345 0.042 Uiso 1.00 1 c R . . H(18) H -0.5933 -0.6531 -0.0113 0.043 Uiso 1.00 1 c R . . H(19) H -0.6264 -0.5529 -0.0028 0.042 Uiso 1.00 1 c R . . H(20) H -0.9169 -0.6728 0.0031 0.035 Uiso 1.00 1 c R . . H(21) H -0.9473 -0.7241 -0.0284 0.035 Uiso 1.00 1 c R . . H(22) H -1.1051 -0.6508 -0.0183 0.036 Uiso 1.00 1 c R . . H(23) H 0.2380 -0.6990 -0.1438 0.056 Uiso 1.00 1 c R . . H(24) H 0.0848 -0.7240 -0.1706 0.056 Uiso 1.00 1 c R . . H(25) H 0.0085 -0.6677 -0.1421 0.056 Uiso 1.00 1 c R . . H(26) H 0.4854 0.1569 -0.1705 0.036 Uiso 1.00 1 c R . . H(27) H 0.6233 0.2402 -0.1771 0.036 Uiso 1.00 1 c R . . H(28) H 0.7254 0.1484 -0.1696 0.036 Uiso 1.00 1 c R . . H(29) H 0.3888 0.1722 -0.2494 0.031 Uiso 1.00 1 c R . . H(30) H 0.3086 0.1968 -0.2160 0.031 Uiso 1.00 1 c R . . H(31) H 0.3287 0.0970 -0.2258 0.031 Uiso 1.00 1 c R . . H(32) H 0.8323 0.2509 -0.2187 0.035 Uiso 1.00 1 c R . . H(33) H 0.6325 0.2730 -0.2376 0.035 Uiso 1.00 1 c R . . H(34) H 0.7905 0.2038 -0.2507 0.035 Uiso 1.00 1 c R . . H(35) H -0.2391 -0.5442 -0.0842 0.036 Uiso 1.00 1 c R . . H(36) H -0.2664 -0.5371 -0.1205 0.036 Uiso 1.00 1 c R . . H(37) H -0.4599 -0.5380 -0.0987 0.036 Uiso 1.00 1 c R . . H(38) H 0.1848 0.1081 -0.1452 0.038 Uiso 1.00 1 c R . . H(39) H -0.0496 0.0842 -0.1449 0.038 Uiso 1.00 1 c R . . H(40) H 0.0799 0.0713 -0.1754 0.038 Uiso 1.00 1 c R . . H(41) H -0.7926 0.0768 -0.0469 0.034 Uiso 1.00 1 c R . . H(42) H -0.7924 0.0742 -0.0835 0.034 Uiso 1.00 1 c R . . H(43) H 0.6119 -0.5213 -0.1965 0.034 Uiso 1.00 1 c R . . H(44) H 0.4037 -0.5138 -0.2147 0.034 Uiso 1.00 1 c R . . H(45) H -0.4562 -0.1519 -0.0442 0.024 Uiso 1.00 1 c R . . H(46) H -0.5297 -0.1604 -0.1085 0.025 Uiso 1.00 1 c R . . H(47) H -0.1951 -0.0832 -0.0780 0.029 Uiso 1.00 1 c R . . H(48) H -0.5122 -0.0004 -0.1124 0.024 Uiso 1.00 1 c R . . H(49) H -0.4806 -0.0009 -0.0462 0.026 Uiso 1.00 1 c R . . H(50) H -0.5189 0.1547 -0.1110 0.029 Uiso 1.00 1 c R . . H(51) H 0.4957 -0.2915 -0.1507 0.025 Uiso 1.00 1 c R . . H(52) H 0.1266 -0.2796 -0.1844 0.020 Uiso 1.00 1 c R . . H(53) H 0.2026 -0.3660 -0.1272 0.019 Uiso 1.00 1 c R . . H(54) H 0.0964 -0.4340 -0.1861 0.027 Uiso 1.00 1 c R . . H(55) H 0.4814 -0.4422 -0.1554 0.025 Uiso 1.00 1 c R . . H(56) H 0.1010 -0.5915 -0.1917 0.034 Uiso 1.00 1 c R . . 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) 0.0234(4) 0.0161(3) 0.0281(4) -0.0003(3) 0.0069(4) 0.0010(3) Cu(2) 0.0234(4) 0.0177(3) 0.0285(4) -0.0007(3) 0.0096(4) -0.0013(3) Cu(3) 0.0211(4) 0.0163(3) 0.0261(4) -0.0005(3) 0.0067(4) 0.0004(3) O(1) 0.019(2) 0.019(2) 0.031(2) 0.006(2) 0.013(2) 0.004(2) O(2) 0.018(2) 0.014(2) 0.033(2) 0.003(2) 0.010(2) -0.002(2) O(3) 0.022(2) 0.018(2) 0.026(2) -0.003(2) 0.016(2) -0.005(2) O(4) 0.026(2) 0.012(2) 0.031(2) -0.002(2) 0.014(2) -0.001(2) O(5) 0.025(2) 0.016(2) 0.034(2) -0.001(2) 0.014(2) 0.008(2) O(6) 0.047(3) 0.016(2) 0.023(2) 0.004(2) 0.017(2) -0.003(2) O(7) 0.024(3) 0.018(2) 0.027(2) -0.002(2) 0.014(2) 0.005(2) O(8) 0.022(2) 0.013(2) 0.035(2) -0.002(2) 0.011(2) 0.002(2) O(9) 0.031(2) 0.016(2) 0.024(2) -0.006(2) 0.011(2) -0.003(2) O(10) 0.039(3) 0.010(2) 0.027(2) -0.002(2) 0.015(2) 0.000(2) O(11) 0.034(3) 0.019(2) 0.021(2) 0.003(2) 0.017(2) 0.001(2) O(12) 0.038(3) 0.017(2) 0.047(3) 0.007(2) 0.016(2) -0.001(2) O(13) 0.030(3) 0.014(2) 0.038(3) -0.002(2) 0.019(2) -0.001(2) O(14) 0.019(2) 0.015(2) 0.040(3) -0.000(2) 0.012(2) 0.001(2) N(1) 0.023(3) 0.014(2) 0.023(3) 0.005(2) 0.009(2) 0.002(2) N(2) 0.018(3) 0.015(2) 0.020(3) -0.001(2) 0.001(2) 0.000(2) C(1) 0.019(4) 0.013(3) 0.029(3) 0.005(3) 0.009(3) -0.012(3) C(2) 0.025(4) 0.015(3) 0.021(3) 0.005(3) -0.003(3) 0.000(3) C(3) 0.017(3) 0.019(3) 0.036(4) -0.002(3) 0.004(3) -0.004(3) C(4) 0.014(3) 0.026(3) 0.021(3) 0.002(3) 0.000(3) -0.002(3) C(5) 0.030(4) 0.011(3) 0.025(3) -0.005(2) 0.010(3) -0.001(2) C(6) 0.039(4) 0.026(3) 0.020(4) -0.003(3) 0.020(3) -0.002(3) C(7) 0.025(4) 0.022(3) 0.025(4) 0.002(3) 0.005(3) 0.002(3) C(8) 0.049(4) 0.016(3) 0.060(5) 0.002(3) 0.017(4) -0.009(3) C(9) 0.020(4) 0.020(3) 0.028(4) 0.002(3) 0.004(3) -0.005(2) C(10) 0.017(4) 0.024(3) 0.012(3) -0.003(3) -0.002(2) -0.003(3) C(11) 0.012(3) 0.028(3) 0.013(3) -0.002(3) -0.004(3) 0.007(2) C(12) 0.010(3) 0.028(3) 0.017(3) 0.001(2) 0.005(3) 0.001(3) C(13) 0.028(4) 0.023(3) 0.016(3) -0.009(3) 0.001(3) -0.003(2) C(14) 0.026(4) 0.036(4) 0.010(3) 0.001(3) -0.001(3) -0.010(3) C(15) 0.024(4) 0.028(3) 0.020(3) -0.000(3) 0.002(3) 0.006(3) C(16) 0.021(4) 0.020(3) 0.035(4) -0.013(3) 0.001(3) -0.000(3) C(17) 0.023(3) 0.017(3) 0.027(3) 0.002(3) 0.010(3) 0.004(2) C(18) 0.019(3) 0.018(3) 0.069(5) 0.005(3) -0.009(3) 0.015(3) C(19) 0.034(4) 0.021(3) 0.034(4) 0.002(3) 0.007(3) 0.012(3) C(20) 0.021(4) 0.021(3) 0.020(3) -0.004(3) 0.006(3) 0.000(3) C(21) 0.018(3) 0.015(3) 0.016(3) 0.001(3) 0.000(3) -0.003(3) C(22) 0.017(3) 0.021(3) 0.011(3) -0.004(3) 0.006(3) -0.001(2) C(23) 0.023(4) 0.016(3) 0.029(4) -0.000(2) 0.003(3) -0.004(3) C(24) 0.032(4) 0.013(3) 0.017(3) 0.002(3) -0.001(3) 0.002(2) C(25) 0.032(4) 0.018(3) 0.034(4) 0.003(3) 0.019(3) 0.000(3) C(26) 0.039(4) 0.023(3) 0.022(4) 0.000(3) 0.004(3) -0.008(3) C(27) 0.073(5) 0.019(3) 0.048(4) -0.008(3) 0.034(4) -0.008(3) C(28) 0.017(4) 0.032(3) 0.012(3) -0.005(3) 0.004(3) -0.005(2) C(29) 0.013(3) 0.020(3) 0.034(4) 0.001(3) 0.007(3) 0.003(3) C(30) 0.022(3) 0.033(3) 0.003(3) 0.003(3) 0.003(3) 0.001(2) C(31) 0.023(4) 0.033(3) 0.015(3) -0.003(3) -0.003(3) 0.001(3) C(32) 0.039(4) 0.025(3) 0.027(4) -0.006(3) 0.010(3) 0.009(3) C(33) 0.024(4) 0.039(4) 0.026(4) -0.005(3) 0.016(3) -0.008(3) C(34) 0.019(3) 0.022(3) 0.026(4) 0.006(3) 0.011(3) -0.001(3) C(35) 0.021(3) 0.026(3) 0.024(4) -0.008(3) 0.003(3) 0.002(3) C(36) 0.022(4) 0.027(3) 0.041(4) -0.004(3) -0.014(3) -0.004(3) C(37) 0.026(3) 0.029(3) 0.023(4) -0.010(3) 0.009(3) 0.007(3) C(38) 0.038(4) 0.034(4) 0.017(4) -0.013(3) 0.008(3) 0.013(3) C(39) 0.036(4) 0.020(3) 0.034(4) -0.002(3) 0.008(3) 0.001(3) C(40) 0.032(4) 0.027(3) 0.034(4) 0.010(3) 0.020(3) 0.003(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) O(1) 1.900(3) ? . . Cu(1) O(2) 1.953(3) ? . . Cu(1) O(13) 1.932(4) ? . . Cu(1) N(1) 1.941(4) ? . . Cu(2) O(2) 1.941(3) ? . . Cu(2) O(3) 1.913(3) ? . . Cu(2) O(8) 1.934(3) ? . . Cu(2) O(9) 1.911(3) ? . . Cu(3) O(7) 1.887(3) ? . . Cu(3) O(8) 1.941(3) ? . . Cu(3) O(14) 1.941(3) ? . . Cu(3) N(2) 1.940(4) ? . . O(1) C(11) 1.288(6) ? . . O(2) C(2) 1.412(6) ? . . O(3) C(3) 1.413(6) ? . . O(4) C(4) 1.432(6) ? . . O(4) C(7) 1.400(6) ? . . O(5) C(1) 1.422(6) ? . . O(5) C(5) 1.449(6) ? . . O(6) C(6) 1.422(6) ? . . O(6) C(7) 1.427(6) ? . . O(7) C(30) 1.302(6) ? . . O(8) C(21) 1.400(5) ? . . O(9) C(22) 1.434(6) ? . . O(10) C(23) 1.427(6) ? . . O(10) C(26) 1.421(6) ? . . O(11) C(20) 1.427(6) ? . . O(11) C(24) 1.445(6) ? . . O(12) C(25) 1.429(6) ? . . O(12) C(26) 1.414(7) ? . . O(13) C(39) 1.419(6) ? . . O(14) C(40) 1.409(6) ? . . N(1) C(1) 1.470(6) ? . . N(1) C(9) 1.244(7) ? . . N(2) C(20) 1.451(6) ? . . N(2) C(28) 1.282(7) ? . . C(1) C(2) 1.501(7) ? . . C(2) C(3) 1.501(7) ? . . C(3) C(4) 1.517(7) ? . . C(4) C(5) 1.545(7) ? . . C(5) C(6) 1.503(7) ? . . C(7) C(8) 1.480(7) ? . . C(9) C(10) 1.433(7) ? . . C(10) C(11) 1.427(7) ? . . C(10) C(15) 1.404(7) ? . . C(11) C(12) 1.456(7) ? . . C(12) C(13) 1.362(7) ? . . C(12) C(16) 1.562(7) ? . . C(13) C(14) 1.421(7) ? . . C(14) C(15) 1.334(7) ? . . C(16) C(17) 1.520(7) ? . . C(16) C(18) 1.528(7) ? . . C(16) C(19) 1.515(7) ? . . C(20) C(21) 1.523(7) ? . . C(21) C(22) 1.523(6) ? . . C(22) C(23) 1.493(7) ? . . C(23) C(24) 1.547(7) ? . . C(24) C(25) 1.504(7) ? . . C(26) C(27) 1.478(7) ? . . C(28) C(29) 1.423(7) ? . . C(29) C(30) 1.410(7) ? . . C(29) C(34) 1.404(7) ? . . C(30) C(31) 1.445(7) ? . . C(31) C(32) 1.424(8) ? . . C(31) C(35) 1.518(8) ? . . C(32) C(33) 1.418(7) ? . . C(33) C(34) 1.343(7) ? . . C(35) C(36) 1.557(7) ? . . C(35) C(37) 1.527(7) ? . . C(35) C(38) 1.501(7) ? . . O(13) H(1) 0.87(5) ? . . O(14) H(2) 1.13(5) ? . . C(1) H(45) 0.9500 ? . . C(2) H(46) 0.9500 ? . . C(3) H(47) 0.9499 ? . . C(4) H(48) 0.9500 ? . . C(5) H(49) 0.9501 ? . . C(6) H(41) 0.9499 ? . . C(6) H(42) 0.9500 ? . . C(7) H(50) 0.9502 ? . . C(8) H(11) 0.9500 ? . . C(8) H(12) 0.9501 ? . . C(8) H(13) 0.9500 ? . . C(9) H(3) 0.9501 ? . . C(13) H(4) 0.9500 ? . . C(14) H(5) 0.9500 ? . . C(15) H(6) 0.9499 ? . . C(17) H(14) 0.9500 ? . . C(17) H(15) 0.9501 ? . . C(17) H(16) 0.9499 ? . . C(18) H(17) 0.9499 ? . . C(18) H(18) 0.9501 ? . . C(18) H(19) 0.9499 ? . . C(19) H(20) 0.9502 ? . . C(19) H(21) 0.9501 ? . . C(19) H(22) 0.9500 ? . . C(20) H(51) 0.9500 ? . . C(21) H(52) 0.9501 ? . . C(22) H(53) 0.9501 ? . . C(23) H(54) 0.9500 ? . . C(24) H(55) 0.9501 ? . . C(25) H(43) 0.9500 ? . . C(25) H(44) 0.9500 ? . . C(26) H(56) 0.9500 ? . . C(27) H(23) 0.9500 ? . . C(27) H(24) 0.9499 ? . . C(27) H(25) 0.9501 ? . . C(28) H(7) 0.9499 ? . . C(32) H(8) 0.9501 ? . . C(33) H(9) 0.9501 ? . . C(34) H(10) 0.9499 ? . . C(36) H(26) 0.9499 ? . . C(36) H(27) 0.9501 ? . . C(36) H(28) 0.9500 ? . . C(37) H(29) 0.9501 ? . . C(37) H(30) 0.9499 ? . . C(37) H(31) 0.9500 ? . . C(38) H(32) 0.9499 ? . . C(38) H(33) 0.9500 ? . . C(38) H(34) 0.9500 ? . . C(39) H(35) 0.9499 ? . . C(39) H(36) 0.9499 ? . . C(39) H(37) 0.9499 ? . . C(40) H(38) 0.9499 ? . . C(40) H(39) 0.9499 ? . . C(40) H(40) 0.9498 ? . . H(8) C(32) 0.9501 ? . . H(49) C(5) 0.9501 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Cu(1) O(1) 176.0(1) ? . . . O(13) Cu(1) O(1) 95.0(1) ? . . . N(1) Cu(1) O(1) 92.1(2) ? . . . Cu(1) O(1) C(11) 128.6(3) ? . . . O(13) Cu(1) O(2) 87.0(1) ? . . . N(1) Cu(1) O(2) 85.7(2) ? . . . Cu(1) O(2) C(2) 109.1(3) ? . . . Cu(1) O(2) Cu(2) 142.0(2) ? . . . N(1) Cu(1) O(13) 171.6(2) ? . . . Cu(1) O(13) C(39) 129.4(3) ? . . . Cu(1) N(1) C(1) 110.4(3) ? . . . Cu(1) N(1) C(9) 125.6(3) ? . . . Cu(2) O(2) C(2) 105.1(3) ? . . . O(3) Cu(2) O(2) 88.8(1) ? . . . O(8) Cu(2) O(2) 165.9(1) ? . . . O(9) Cu(2) O(2) 93.8(1) ? . . . O(8) Cu(2) O(3) 92.0(1) ? . . . O(9) Cu(2) O(3) 166.5(1) ? . . . Cu(2) O(3) C(3) 107.0(3) ? . . . O(9) Cu(2) O(8) 88.7(1) ? . . . Cu(2) O(8) C(21) 106.0(3) ? . . . Cu(2) O(8) Cu(3) 142.4(2) ? . . . Cu(2) O(9) C(22) 107.1(3) ? . . . O(8) Cu(3) O(7) 174.5(1) ? . . . O(14) Cu(3) O(7) 95.0(1) ? . . . N(2) Cu(3) O(7) 92.6(2) ? . . . Cu(3) O(7) C(30) 129.1(3) ? . . . O(14) Cu(3) O(8) 87.4(1) ? . . . Cu(3) O(8) C(21) 108.8(3) ? . . . N(2) Cu(3) O(8) 85.7(2) ? . . . N(2) Cu(3) O(14) 168.6(2) ? . . . Cu(3) O(14) C(40) 125.2(3) ? . . . Cu(3) N(2) C(20) 110.9(3) ? . . . Cu(3) N(2) C(28) 126.0(3) ? . . . O(1) C(11) C(10) 124.1(4) ? . . . O(1) C(11) C(12) 118.6(4) ? . . . O(2) C(2) C(1) 111.2(4) ? . . . O(2) C(2) C(3) 111.0(4) ? . . . O(3) C(3) C(2) 108.0(4) ? . . . O(3) C(3) C(4) 116.3(4) ? . . . O(4) C(4) C(3) 112.1(4) ? . . . O(4) C(4) C(5) 105.8(4) ? . . . C(7) O(4) C(4) 111.4(4) ? . . . O(4) C(7) O(6) 111.2(4) ? . . . O(4) C(7) C(8) 107.4(4) ? . . . O(5) C(1) N(1) 112.9(4) ? . . . O(5) C(1) C(2) 108.7(4) ? . . . C(5) O(5) C(1) 107.5(4) ? . . . O(5) C(5) C(4) 112.7(4) ? . . . O(5) C(5) C(6) 109.5(4) ? . . . O(6) C(6) C(5) 107.1(4) ? . . . C(7) O(6) C(6) 112.9(4) ? . . . O(6) C(7) C(8) 109.8(4) ? . . . O(7) C(30) C(29) 123.0(4) ? . . . O(7) C(30) C(31) 117.4(4) ? . . . O(8) C(21) C(22) 112.6(4) ? . . . O(8) C(21) C(20) 110.0(4) ? . . . O(9) C(22) C(21) 105.3(4) ? . . . O(9) C(22) C(23) 118.1(4) ? . . . O(10) C(23) C(22) 111.9(4) ? . . . O(10) C(23) C(24) 107.4(4) ? . . . C(26) O(10) C(23) 111.0(4) ? . . . O(10) C(26) O(12) 110.7(4) ? . . . O(10) C(26) C(27) 107.4(4) ? . . . O(11) C(20) C(21) 109.3(4) ? . . . O(11) C(20) N(2) 113.7(4) ? . . . C(24) O(11) C(20) 108.0(3) ? . . . O(11) C(24) C(23) 112.6(4) ? . . . O(11) C(24) C(25) 109.8(4) ? . . . O(12) C(25) C(24) 108.8(4) ? . . . C(26) O(12) C(25) 113.0(4) ? . . . O(12) C(26) C(27) 108.0(4) ? . . . N(1) C(1) C(2) 106.1(4) ? . . . C(9) N(1) C(1) 123.9(4) ? . . . N(1) C(9) C(10) 127.4(5) ? . . . N(2) C(20) C(21) 106.5(4) ? . . . C(28) N(2) C(20) 122.4(4) ? . . . N(2) C(28) C(29) 125.1(5) ? . . . C(1) C(2) C(3) 111.8(4) ? . . . C(2) C(3) C(4) 105.3(4) ? . . . C(3) C(4) C(5) 110.7(4) ? . . . C(4) C(5) C(6) 108.4(4) ? . . . C(9) C(10) C(11) 120.7(4) ? . . . C(9) C(10) C(15) 117.5(5) ? . . . C(10) C(11) C(12) 117.3(4) ? . . . C(15) C(10) C(11) 121.7(5) ? . . . C(10) C(15) C(14) 120.1(5) ? . . . C(11) C(12) C(13) 117.3(4) ? . . . C(11) C(12) C(16) 121.6(4) ? . . . C(16) C(12) C(13) 121.1(4) ? . . . C(12) C(13) C(14) 123.9(5) ? . . . C(12) C(16) C(17) 108.6(4) ? . . . C(12) C(16) C(18) 109.0(4) ? . . . C(12) C(16) C(19) 112.0(4) ? . . . C(13) C(14) C(15) 119.4(5) ? . . . C(18) C(16) C(17) 112.0(4) ? . . . C(19) C(16) C(17) 109.4(4) ? . . . C(19) C(16) C(18) 106.0(4) ? . . . C(20) C(21) C(22) 110.1(4) ? . . . C(21) C(22) C(23) 104.8(4) ? . . . C(22) C(23) C(24) 109.3(4) ? . . . C(23) C(24) C(25) 110.6(4) ? . . . C(28) C(29) C(30) 123.8(5) ? . . . C(28) C(29) C(34) 116.2(5) ? . . . C(29) C(30) C(31) 119.5(5) ? . . . C(34) C(29) C(30) 120.0(5) ? . . . C(29) C(34) C(33) 122.4(5) ? . . . C(30) C(31) C(35) 124.1(5) ? . . . C(30) C(31) C(32) 117.0(5) ? . . . C(35) C(31) C(32) 118.9(5) ? . . . C(31) C(32) C(33) 121.8(5) ? . . . C(31) C(35) C(36) 107.9(4) ? . . . C(31) C(35) C(37) 110.8(4) ? . . . C(31) C(35) C(38) 113.4(4) ? . . . C(32) C(33) C(34) 119.2(5) ? . . . C(37) C(35) C(36) 109.6(4) ? . . . C(38) C(35) C(36) 107.3(4) ? . . . C(38) C(35) C(37) 107.6(4) ? . . . Cu(1) O(13) H(1) 116(3) ? . . . Cu(3) O(14) H(2) 106(2) ? . . . O(2) C(2) H(46) 107.2940 ? . . . O(3) C(3) H(47) 108.6068 ? . . . O(4) C(4) H(48) 109.3754 ? . . . O(4) C(7) H(50) 108.9280 ? . . . O(5) C(1) H(45) 109.5524 ? . . . O(5) C(5) H(49) 108.2008 ? . . . O(6) C(6) H(42) 110.0934 ? . . . O(6) C(6) H(41) 109.8571 ? . . . O(6) C(7) H(50) 108.8378 ? . . . O(8) C(21) H(52) 107.9487 ? . . . O(9) C(22) H(53) 109.7105 ? . . . O(10) C(23) H(54) 109.3117 ? . . . O(10) C(26) H(56) 110.4334 ? . . . O(11) C(20) H(51) 109.3393 ? . . . O(11) C(24) H(55) 108.0366 ? . . . O(12) C(25) H(44) 109.9635 ? . . . O(12) C(25) H(43) 109.3288 ? . . . O(12) C(26) H(56) 110.2893 ? . . . H(1) O(13) C(39) 111(3) ? . . . O(13) C(39) H(35) 110.1631 ? . . . O(13) C(39) H(37) 109.8065 ? . . . O(13) C(39) H(36) 108.4343 ? . . . H(2) O(14) C(40) 108(2) ? . . . O(14) C(40) H(38) 108.1377 ? . . . O(14) C(40) H(40) 109.9342 ? . . . O(14) C(40) H(39) 110.3470 ? . . . N(1) C(1) H(45) 109.6129 ? . . . N(1) C(9) H(3) 116.2446 ? . . . N(2) C(20) H(51) 109.1104 ? . . . N(2) C(28) H(7) 117.1400 ? . . . H(45) C(1) C(2) 109.8485 ? . . . C(1) C(2) H(46) 107.8507 ? . . . H(46) C(2) C(3) 107.4711 ? . . . C(2) C(3) H(47) 109.0209 ? . . . H(47) C(3) C(4) 109.3201 ? . . . C(3) C(4) H(48) 109.4979 ? . . . H(48) C(4) C(5) 109.3884 ? . . . C(4) C(5) H(49) 108.9876 ? . . . C(5) C(6) H(42) 110.2253 ? . . . H(49) C(5) C(6) 109.0112 ? . . . C(5) C(6) H(41) 110.1223 ? . . . H(42) C(6) H(41) 109.4530 ? . . . C(7) C(8) H(11) 110.6465 ? . . . C(7) C(8) H(12) 107.7034 ? . . . C(7) C(8) H(13) 110.0500 ? . . . H(50) C(7) C(8) 110.5981 ? . . . H(12) C(8) H(11) 109.4802 ? . . . H(13) C(8) H(11) 109.4682 ? . . . H(13) C(8) H(12) 109.4637 ? . . . H(3) C(9) C(10) 116.3601 ? . . . C(10) C(15) H(6) 120.2440 ? . . . C(12) C(13) H(4) 118.1902 ? . . . C(13) C(14) H(5) 120.3317 ? . . . H(4) C(13) C(14) 117.8846 ? . . . C(14) C(15) H(6) 119.6227 ? . . . H(5) C(14) C(15) 120.2109 ? . . . C(16) C(17) H(15) 108.9345 ? . . . C(16) C(17) H(16) 109.3800 ? . . . C(16) C(17) H(14) 110.1029 ? . . . C(16) C(18) H(17) 109.3811 ? . . . C(16) C(18) H(19) 109.0936 ? . . . C(16) C(18) H(18) 109.9375 ? . . . C(16) C(19) H(20) 110.0680 ? . . . C(16) C(19) H(21) 109.8149 ? . . . C(16) C(19) H(22) 108.5287 ? . . . H(15) C(17) H(14) 109.4635 ? . . . H(16) C(17) H(14) 109.4741 ? . . . H(16) C(17) H(15) 109.4702 ? . . . H(19) C(18) H(17) 109.4650 ? . . . H(18) C(18) H(17) 109.4754 ? . . . H(19) C(18) H(18) 109.4735 ? . . . H(21) C(19) H(20) 109.4742 ? . . . H(22) C(19) H(20) 109.4656 ? . . . H(22) C(19) H(21) 109.4715 ? . . . C(20) C(21) H(52) 107.8329 ? . . . H(51) C(20) C(21) 108.7186 ? . . . H(52) C(21) C(22) 108.1370 ? . . . C(21) C(22) H(53) 109.2361 ? . . . H(53) C(22) C(23) 109.3227 ? . . . C(22) C(23) H(54) 109.6444 ? . . . H(54) C(23) C(24) 109.2705 ? . . . C(23) C(24) H(55) 107.6533 ? . . . C(24) C(25) H(44) 109.9806 ? . . . H(55) C(24) C(25) 108.0469 ? . . . C(24) C(25) H(43) 109.3286 ? . . . H(44) C(25) H(43) 109.4676 ? . . . C(26) C(27) H(23) 109.4928 ? . . . C(26) C(27) H(24) 109.6447 ? . . . C(26) C(27) H(25) 109.2847 ? . . . H(56) C(26) C(27) 109.9473 ? . . . H(24) C(27) H(23) 109.4658 ? . . . H(25) C(27) H(23) 109.4648 ? . . . H(25) C(27) H(24) 109.4743 ? . . . H(7) C(28) C(29) 117.7027 ? . . . C(29) C(34) H(10) 119.1841 ? . . . C(31) C(32) H(8) 119.2165 ? . . . C(32) C(33) H(9) 120.0290 ? . . . H(8) C(32) C(33) 118.9895 ? . . . C(33) C(34) H(10) 118.4503 ? . . . H(9) C(33) C(34) 120.7792 ? . . . C(35) C(36) H(26) 108.9996 ? . . . C(35) C(36) H(28) 110.0659 ? . . . C(35) C(36) H(27) 109.3457 ? . . . C(35) C(37) H(30) 109.3758 ? . . . C(35) C(37) H(31) 109.8141 ? . . . C(35) C(37) H(29) 109.2231 ? . . . C(35) C(38) H(32) 110.2197 ? . . . C(35) C(38) H(33) 108.2692 ? . . . C(35) C(38) H(34) 109.9188 ? . . . H(28) C(36) H(26) 109.4743 ? . . . H(27) C(36) H(26) 109.4706 ? . . . H(28) C(36) H(27) 109.4694 ? . . . H(30) C(37) H(29) 109.4706 ? . . . H(31) C(37) H(29) 109.4679 ? . . . H(31) C(37) H(30) 109.4753 ? . . . H(33) C(38) H(32) 109.4636 ? . . . H(34) C(38) H(32) 109.4687 ? . . . H(34) C(38) H(33) 109.4804 ? . . . H(37) C(39) H(35) 109.4869 ? . . . H(36) C(39) H(35) 109.4624 ? . . . H(37) C(39) H(36) 109.4687 ? . . . H(40) C(40) H(38) 109.4566 ? . . . H(39) C(40) H(38) 109.4839 ? . . . H(40) C(40) H(39) 109.4594 ? . . . #============================================================================== #===END #============================================================================== data_Complex_3 _database_code_depnum_ccdc_archive 'CCDC 250718' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C56 H88 Cu3 N2 O18 ' _chemical_formula_moiety 'C56 H88 Cu3 N2 O18 ' _chemical_formula_weight 1267.95 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z #------------------------------------------------------------------------------ _cell_length_a 8.14870(10) _cell_length_b 12.23590(10) _cell_length_c 16.9972(3) _cell_angle_alpha 72.113(8) _cell_angle_beta 78.973(9) _cell_angle_gamma 65.529(6) _cell_volume 1463.92(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3631 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 669.00 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.944 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 7377 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 27.09 _diffrn_measured_fraction_theta_max 0.7118 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.7894 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 #============================================================================== # 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 6056 _reflns_number_gt 5296 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0560 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5309 _refine_ls_number_parameters 509 _refine_ls_goodness_of_fit_ref 0.788 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0230 _refine_diff_density_max 1.14 _refine_diff_density_min -0.81 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1454 Friedel Pairs' _refine_ls_abs_structure_Flack 0.02(3) 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 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; 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 Cu(1) Cu -0.1759(2) 0.0707(2) -0.65274(12) 0.0205(3) Uani 1.00 1 d . . . Cu(2) Cu -0.2162(2) 0.3856(2) -0.77252(13) 0.0225(3) Uani 1.00 1 d . . . Cu(3) Cu -0.3349(2) 0.7067(2) -0.89512(12) 0.0214(4) Uani 1.00 1 d . . . O(1) O -0.1472(7) -0.0728(6) -0.5631(4) 0.023(2) Uani 1.00 1 d . . . O(2) O -0.1754(8) 0.2122(6) -0.7459(4) 0.024(2) Uani 1.00 1 d . . . O(3) O -0.1328(7) 0.3788(5) -0.8844(4) 0.022(2) Uani 1.00 1 d . . . O(4) O -0.0684(8) 0.2974(6) -1.0421(5) 0.029(2) Uani 1.00 1 d . . . O(5) O 0.0106(8) 0.0025(6) -0.8808(4) 0.023(2) Uani 1.00 1 d . . . O(6) O 0.0523(9) 0.1304(7) -1.1049(4) 0.026(2) Uani 1.00 1 d . . . O(7) O -0.3518(8) 0.8494(6) -0.9826(4) 0.024(2) Uani 1.00 1 d . . . O(8) O -0.3287(8) 0.5647(6) -0.8024(4) 0.016(2) Uani 1.00 1 d . . . O(9) O -0.2475(7) 0.3894(5) -0.6582(4) 0.023(2) Uani 1.00 1 d . . . O(10) O -0.4255(8) 0.4788(6) -0.5034(4) 0.021(2) Uani 1.00 1 d . . . O(11) O -0.4977(8) 0.7707(6) -0.6662(4) 0.023(2) Uani 1.00 1 d . . . O(12) O -0.5533(8) 0.6445(6) -0.4424(4) 0.030(2) Uani 1.00 1 d . . . O(13) O -0.2353(9) 0.1805(7) -0.5782(4) 0.032(2) Uani 1.00 1 d . . . O(14) O -0.2637(8) 0.5966(6) -0.9678(4) 0.021(2) Uani 1.00 1 d . . . O(15) O -0.4836(7) 0.1197(6) -0.6733(5) 0.035(2) Uani 1.00 1 d . . . O(16) O -0.0201(8) 0.6582(6) -0.8714(5) 0.031(2) Uani 1.00 1 d . . . O(17) O 0.326(2) 0.5421(10) -1.0949(7) 0.107(4) Uiso 1.00 1 d . . . O(18) O -0.789(2) -0.968(2) -0.3572(10) 0.172(6) Uiso 1.00 1 d . . . N(1) N -0.0898(10) -0.0263(8) -0.7353(5) 0.023(2) Uani 1.00 1 d . . . N(2) N -0.4569(10) 0.8056(7) -0.8144(5) 0.019(2) Uani 1.00 1 d . . . C(1) C -0.1129(11) 0.0557(7) -0.8174(5) 0.021(2) Uiso 1.00 1 d . . . C(2) C -0.0828(11) 0.1681(7) -0.8159(5) 0.018(2) Uiso 1.00 1 d . . . C(3) C -0.1431(12) 0.2713(8) -0.8950(6) 0.020(2) Uiso 1.00 1 d . . . C(4) C -0.0206(10) 0.2164(7) -0.9625(5) 0.019(2) Uiso 1.00 1 d . . . C(5) C -0.0347(11) 0.0935(8) -0.9584(5) 0.021(2) Uiso 1.00 1 d . . . C(6) C 0.0969(11) 0.0403(8) -1.0262(6) 0.024(2) Uiso 1.00 1 d . . . C(7) C 0.0569(11) 0.2468(8) -1.1065(5) 0.028(2) Uiso 1.00 1 d . . . C(8) C 0.0018(13) 0.3356(10) -1.1852(7) 0.038(3) Uiso 1.00 1 d . . . C(9) C -0.0356(11) -0.1444(8) -0.7218(6) 0.020(2) Uiso 1.00 1 d . . . C(10) C -0.0176(11) -0.2295(9) -0.6411(6) 0.018(2) Uiso 1.00 1 d . . . C(11) C -0.0687(12) -0.1923(10) -0.5622(7) 0.023(2) Uiso 1.00 1 d . . . C(12) C -0.0367(11) -0.2843(9) -0.4888(6) 0.022(2) Uiso 1.00 1 d . . . C(13) C 0.0409(11) -0.4060(9) -0.4918(6) 0.028(2) Uiso 1.00 1 d . . . C(14) C 0.0904(11) -0.4445(9) -0.5630(6) 0.028(2) Uiso 1.00 1 d . . . C(15) C 0.0595(12) -0.3557(9) -0.6371(7) 0.023(2) Uiso 1.00 1 d . . . C(16) C -0.0950(11) -0.2485(9) -0.4053(6) 0.025(2) Uiso 1.00 1 d . . . C(17) C -0.0498(13) -0.3648(10) -0.3297(7) 0.042(3) Uiso 1.00 1 d . . . C(18) C -0.3043(11) -0.1762(9) -0.3979(6) 0.035(2) Uiso 1.00 1 d . . . C(19) C 0.0049(12) -0.1684(9) -0.3981(6) 0.034(2) Uiso 1.00 1 d . . . C(20) C -0.4929(11) 0.7280(7) -0.7353(5) 0.020(2) Uiso 1.00 1 d . . . C(21) C -0.3436(10) 0.6004(7) -0.7300(5) 0.015(2) Uiso 1.00 1 d . . . C(22) C -0.3801(12) 0.5070(8) -0.6534(6) 0.018(2) Uiso 1.00 1 d . . . C(23) C -0.3815(10) 0.5531(7) -0.5808(5) 0.017(2) Uiso 1.00 1 d . . . C(24) C -0.5268(11) 0.6852(7) -0.5888(5) 0.018(2) Uiso 1.00 1 d . . . C(25) C -0.5279(12) 0.7312(8) -0.5175(6) 0.026(2) Uiso 1.00 1 d . . . C(26) C -0.4187(11) 0.5226(7) -0.4372(5) 0.027(2) Uiso 1.00 1 d . . . C(27) C -0.4618(13) 0.4387(10) -0.3557(7) 0.037(3) Uiso 1.00 1 d . . . C(28) C -0.5001(11) 0.9217(8) -0.8279(6) 0.019(2) Uiso 1.00 1 d . . . C(29) C -0.4796(11) 1.0046(9) -0.9065(6) 0.022(2) Uiso 1.00 1 d . . . C(30) C -0.4131(11) 0.9663(10) -0.9785(7) 0.022(2) Uiso 1.00 1 d . . . C(31) C -0.4151(11) 1.0614(9) -1.0576(6) 0.025(2) Uiso 1.00 1 d . . . C(32) C -0.4757(11) 1.1828(9) -1.0539(6) 0.027(2) Uiso 1.00 1 d . . . C(33) C -0.5416(11) 1.2186(9) -0.9760(6) 0.027(2) Uiso 1.00 1 d . . . C(34) C -0.5427(11) 1.1335(9) -0.9073(6) 0.021(2) Uiso 1.00 1 d . . . C(35) C -0.3553(12) 1.0250(9) -1.1410(6) 0.029(2) Uiso 1.00 1 d . . . C(36) C -0.4698(12) 0.9616(9) -1.1547(6) 0.034(2) Uiso 1.00 1 d . . . C(37) C -0.1517(11) 0.9393(8) -1.1445(6) 0.028(2) Uiso 1.00 1 d . . . C(38) C -0.3807(13) 1.1417(10) -1.2131(7) 0.044(3) Uiso 1.00 1 d . . . C(39) C -0.3426(13) 0.1732(10) -0.5044(7) 0.037(3) Uiso 1.00 1 d . . . C(40) C -0.1459(13) 0.6079(11) -1.0428(7) 0.039(3) Uiso 1.00 1 d . . . C(41) C -0.5681(12) 0.0405(10) -0.6186(7) 0.032(3) Uiso 1.00 1 d . . . C(42) C -0.765(1) 0.0992(11) -0.6414(8) 0.048(3) Uiso 1.00 1 d . . . C(43) C -0.793(2) 0.234(1) -0.6822(10) 0.075(4) Uiso 1.00 1 d . . . C(44) C -0.6148(13) 0.2439(10) -0.6850(7) 0.042(3) Uiso 1.00 1 d . . . C(45) C 0.0651(12) 0.7351(10) -0.9292(7) 0.033(3) Uiso 1.00 1 d . . . C(46) C 0.2562(13) 0.6854(10) -0.9066(7) 0.040(3) Uiso 1.00 1 d . . . C(47) C 0.295(2) 0.5478(12) -0.8673(9) 0.056(3) Uiso 1.00 1 d . . . C(48) C 0.1175(12) 0.5325(9) -0.8507(7) 0.036(3) Uiso 1.00 1 d . . . C(49) C 0.248(2) 0.599(2) -1.1753(10) 0.099(5) Uiso 1.00 1 d . . . C(50) C 0.334(2) 0.6862(12) -1.2182(8) 0.067(3) Uiso 1.00 1 d . . . C(51) C 0.498(3) 0.644(2) -1.1776(13) 0.134(7) Uiso 1.00 1 d . . . C(52) C 0.497(2) 0.5374(12) -1.1009(8) 0.062(3) Uiso 1.00 1 d . . . C(53) C -0.716(3) -0.859(2) -0.360(1) 0.142(8) Uiso 1.00 1 d . . . C(54) C -0.968(3) -0.865(3) -0.399(2) 0.202(12) Uiso 1.00 1 d . . . C(55) C -0.982(3) -0.744(2) -0.4143(13) 0.132(7) Uiso 1.00 1 d . . . C(56) C -0.802(2) -0.749(1) -0.4001(10) 0.088(4) Uiso 1.00 1 d . . . H(1) H -0.0043 -0.1777 -0.7687 0.025 Uiso 1.00 1 c R . . H(2) H 0.0618 -0.4682 -0.4408 0.034 Uiso 1.00 1 c R . . H(3) H 0.1453 -0.5304 -0.5614 0.033 Uiso 1.00 1 c R . . H(4) H 0.0914 -0.3814 -0.6871 0.027 Uiso 1.00 1 c R . . H(5) H -0.5502 0.9572 -0.7821 0.022 Uiso 1.00 1 c R . . H(6) H -0.4738 1.2447 -1.1037 0.033 Uiso 1.00 1 c R . . H(7) H -0.5853 1.3035 -0.9756 0.032 Uiso 1.00 1 c R . . H(8) H -0.5852 1.1571 -0.8566 0.026 Uiso 1.00 1 c R . . H(9) H -0.0797 0.3168 -1.2069 0.045 Uiso 1.00 1 c R . . H(10) H 0.1061 0.3302 -1.2225 0.045 Uiso 1.00 1 c R . . H(11) H -0.0554 0.4177 -1.1783 0.045 Uiso 1.00 1 c R . . H(12) H -0.1496 -0.3900 -0.3137 0.051 Uiso 1.00 1 c R . . H(13) H -0.0259 -0.3443 -0.2846 0.051 Uiso 1.00 1 c R . . H(14) H 0.0539 -0.4310 -0.3438 0.051 Uiso 1.00 1 c R . . H(15) H -0.3335 -0.0898 -0.4210 0.042 Uiso 1.00 1 c R . . H(16) H -0.3471 -0.1902 -0.3411 0.042 Uiso 1.00 1 c R . . H(17) H -0.3608 -0.2053 -0.4265 0.042 Uiso 1.00 1 c R . . H(18) H 0.1145 -0.2215 -0.3727 0.041 Uiso 1.00 1 c R . . H(19) H -0.0693 -0.1124 -0.3656 0.041 Uiso 1.00 1 c R . . H(20) H 0.0309 -0.1228 -0.4519 0.041 Uiso 1.00 1 c R . . H(21) H -0.5882 0.4704 -0.3411 0.044 Uiso 1.00 1 c R . . H(22) H -0.3984 0.4355 -0.3131 0.044 Uiso 1.00 1 c R . . H(23) H -0.4253 0.3572 -0.3620 0.044 Uiso 1.00 1 c R . . H(24) H -0.4144 0.8745 -1.1322 0.041 Uiso 1.00 1 c R . . H(25) H -0.4793 0.9783 -1.2124 0.041 Uiso 1.00 1 c R . . H(26) H -0.5869 0.9923 -1.1278 0.041 Uiso 1.00 1 c R . . H(27) H -0.0804 0.9883 -1.1659 0.034 Uiso 1.00 1 c R . . H(28) H -0.1303 0.8862 -1.1792 0.034 Uiso 1.00 1 c R . . H(29) H -0.1223 0.8924 -1.0895 0.034 Uiso 1.00 1 c R . . H(30) H -0.4983 1.1745 -1.2321 0.053 Uiso 1.00 1 c R . . H(31) H -0.2935 1.1213 -1.2576 0.053 Uiso 1.00 1 c R . . H(32) H -0.3655 1.2016 -1.1936 0.053 Uiso 1.00 1 c R . . H(33) H -0.4648 0.2247 -0.5152 0.045 Uiso 1.00 1 c R . . H(34) H -0.3037 0.2005 -0.4674 0.045 Uiso 1.00 1 c R . . H(35) H -0.3326 0.0899 -0.4802 0.045 Uiso 1.00 1 c R . . H(36) H -0.2158 0.6624 -1.0882 0.047 Uiso 1.00 1 c R . . H(37) H -0.0803 0.5289 -1.0540 0.047 Uiso 1.00 1 c R . . H(38) H -0.0641 0.6406 -1.0355 0.047 Uiso 1.00 1 c R . . H(39) H -0.2334 0.0805 -0.8307 0.025 Uiso 1.00 1 c R . . H(40) H 0.0430 0.1454 -0.8134 0.022 Uiso 1.00 1 c R . . H(41) H -0.2646 0.2880 -0.9023 0.024 Uiso 1.00 1 c R . . H(42) H 0.1006 0.2013 -0.9557 0.023 Uiso 1.00 1 c R . . H(43) H -0.1540 0.1095 -0.9689 0.025 Uiso 1.00 1 c R . . H(44) H 0.1756 0.2349 -1.0979 0.033 Uiso 1.00 1 c R . . H(45) H -0.6055 0.7222 -0.7355 0.024 Uiso 1.00 1 c R . . H(46) H -0.2329 0.6058 -0.7254 0.018 Uiso 1.00 1 c R . . H(47) H -0.4962 0.5072 -0.6548 0.021 Uiso 1.00 1 c R . . H(48) H -0.2665 0.5549 -0.5800 0.020 Uiso 1.00 1 c R . . H(49) H -0.6415 0.6818 -0.5882 0.021 Uiso 1.00 1 c R . . H(50) H -0.3022 0.5230 -0.4378 0.032 Uiso 1.00 1 c R . . H(51) H 0.0877 -0.0342 -1.0273 0.029 Uiso 1.00 1 c R . . H(52) H 0.2168 0.0231 -1.0160 0.029 Uiso 1.00 1 c R . . H(53) H -0.6246 0.8096 -0.5203 0.031 Uiso 1.00 1 c R . . H(54) H -0.4166 0.7397 -0.5189 0.031 Uiso 1.00 1 c R . . H(55) H -0.5105 -0.0412 -0.6261 0.039 Uiso 1.00 1 c R . . H(56) H -0.5633 0.0380 -0.5626 0.039 Uiso 1.00 1 c R . . H(57) H -0.7806 0.0604 -0.6783 0.058 Uiso 1.00 1 c R . . H(58) H -0.8452 0.0927 -0.5934 0.058 Uiso 1.00 1 c R . . H(59) H -0.8263 0.2556 -0.7371 0.090 Uiso 1.00 1 c R . . H(60) H -0.8836 0.2869 -0.6517 0.090 Uiso 1.00 1 c R . . H(61) H -0.6159 0.2776 -0.6414 0.051 Uiso 1.00 1 c R . . H(62) H -0.5886 0.2946 -0.7366 0.051 Uiso 1.00 1 c R . . H(63) H 0.0617 0.7326 -0.9842 0.040 Uiso 1.00 1 c R . . H(64) H 0.0051 0.8183 -0.9247 0.040 Uiso 1.00 1 c R . . H(65) H 0.3347 0.6963 -0.9549 0.048 Uiso 1.00 1 c R . . H(66) H 0.2684 0.7242 -0.8687 0.048 Uiso 1.00 1 c R . . H(67) H 0.3723 0.4996 -0.9041 0.067 Uiso 1.00 1 c R . . H(68) H 0.3511 0.5220 -0.8171 0.067 Uiso 1.00 1 c R . . H(69) H 0.1010 0.4928 -0.7939 0.043 Uiso 1.00 1 c R . . H(70) H 0.1121 0.4847 -0.8842 0.043 Uiso 1.00 1 c R . . H(73) H 0.2744 0.5385 -1.2045 0.118 Uiso 1.00 1 c R . . H(74) H 0.1212 0.6403 -1.1672 0.119 Uiso 1.00 1 c R . . H(75) H 0.3600 0.6865 -1.2752 0.081 Uiso 1.00 1 c R . . H(76) H 0.2567 0.7673 -1.2132 0.081 Uiso 1.00 1 c R . . H(77) H 0.5995 0.6135 -1.2142 0.160 Uiso 1.00 1 c R . . H(78) H 0.5043 0.7110 -1.1627 0.160 Uiso 1.00 1 c R . . H(79) H 0.5140 0.5540 -1.0527 0.075 Uiso 1.00 1 c R . . H(80) H 0.5852 0.4591 -1.1063 0.074 Uiso 1.00 1 c R . . H(81) H -0.7130 -0.8595 -0.3040 0.170 Uiso 1.00 1 c R . . H(82) H -0.5966 -0.8829 -0.3853 0.170 Uiso 1.00 1 c R . . H(83) H -0.9741 -0.8803 -0.4495 0.243 Uiso 1.00 1 c R . . H(84) H -1.0674 -0.8741 -0.3615 0.243 Uiso 1.00 1 c R . . H(85) H -1.0083 -0.7015 -0.4703 0.158 Uiso 1.00 1 c R . . H(86) H -1.0746 -0.7023 -0.3783 0.158 Uiso 1.00 1 c R . . H(87) H -0.8189 -0.6942 -0.3671 0.106 Uiso 1.00 1 c R . . H(88) H -0.7379 -0.7263 -0.4512 0.105 Uiso 1.00 1 c R . . 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) 0.0254(6) 0.0152(7) 0.0176(7) -0.0061(5) 0.0003(5) -0.0032(6) Cu(2) 0.0321(8) 0.0147(4) 0.0198(5) -0.0093(5) 0.0015(6) -0.0049(4) Cu(3) 0.0281(6) 0.0167(7) 0.0176(8) -0.0083(5) -0.0005(5) -0.0027(6) O(1) 0.025(3) 0.017(4) 0.022(4) -0.005(3) 0.005(3) -0.004(3) O(2) 0.025(3) 0.017(4) 0.030(5) -0.010(3) 0.004(3) -0.009(4) O(3) 0.034(3) 0.019(3) 0.016(3) -0.013(3) 0.000(3) -0.006(3) O(4) 0.030(3) 0.016(4) 0.033(5) -0.005(3) -0.004(3) -0.003(4) O(5) 0.032(3) 0.023(4) 0.018(5) -0.014(3) 0.004(3) -0.011(4) O(6) 0.049(4) 0.026(4) 0.006(4) -0.016(3) -0.002(3) -0.003(4) O(7) 0.040(4) 0.016(4) 0.012(4) -0.008(3) -0.006(3) 0.001(3) O(8) 0.031(3) 0.016(4) 0.001(4) -0.008(3) -0.002(3) -0.001(3) O(9) 0.026(3) 0.015(3) 0.025(4) -0.005(3) -0.001(3) -0.006(3) O(10) 0.039(4) 0.021(4) 0.001(4) -0.011(3) -0.001(3) -0.001(3) O(11) 0.030(3) 0.011(4) 0.020(5) -0.007(3) -0.001(3) 0.002(3) O(12) 0.039(4) 0.016(4) 0.027(5) -0.005(3) 0.001(3) -0.005(4) O(13) 0.047(4) 0.025(5) 0.022(5) -0.013(3) 0.005(3) -0.007(4) O(14) 0.030(3) 0.022(4) 0.011(4) -0.010(3) 0.000(3) -0.005(4) O(15) 0.016(3) 0.021(4) 0.053(5) -0.006(3) 0.000(3) 0.005(4) O(16) 0.023(3) 0.019(4) 0.044(5) -0.008(3) -0.002(3) 0.003(4) N(1) 0.023(4) 0.022(5) 0.023(5) -0.009(3) -0.001(4) -0.002(4) N(2) 0.027(4) 0.017(4) 0.007(4) -0.007(3) -0.002(3) 0.001(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) O(1) 1.900(7) ? . . Cu(1) O(2) 1.956(7) ? . . Cu(1) O(13) 1.979(9) ? . . Cu(1) O(15) 2.394(7) ? . . Cu(1) N(1) 1.96(1) ? . . Cu(2) O(2) 1.923(8) ? . . Cu(2) O(3) 1.907(6) ? . . Cu(2) O(8) 1.932(6) ? . . Cu(2) O(9) 1.924(7) ? . . Cu(3) O(7) 1.888(7) ? . . Cu(3) O(8) 1.944(6) ? . . Cu(3) O(14) 1.944(8) ? . . Cu(3) O(16) 2.466(7) ? . . Cu(3) N(2) 1.959(9) ? . . O(1) C(11) 1.33(1) ? . . O(2) C(2) 1.41(1) ? . . O(3) C(3) 1.42(1) ? . . O(4) C(4) 1.42(1) ? . . O(4) C(7) 1.44(1) ? . . O(5) C(1) 1.44(1) ? . . O(5) C(5) 1.435(9) ? . . O(6) C(6) 1.44(1) ? . . O(6) C(7) 1.43(1) ? . . O(7) C(30) 1.33(1) ? . . O(8) C(21) 1.40(1) ? . . O(9) C(22) 1.41(1) ? . . O(10) C(23) 1.428(9) ? . . O(10) C(26) 1.41(1) ? . . O(11) C(20) 1.41(1) ? . . O(11) C(24) 1.46(1) ? . . O(12) C(25) 1.43(1) ? . . O(12) C(26) 1.427(9) ? . . O(13) C(39) 1.39(1) ? . . O(14) C(40) 1.45(1) ? . . O(15) C(41) 1.43(1) ? . . O(15) C(44) 1.43(1) ? . . O(16) C(45) 1.43(1) ? . . O(16) C(48) 1.46(1) ? . . O(17) C(49) 1.46(2) ? . . O(17) C(52) 1.36(2) ? . . O(18) C(53) 1.66(4) ? . . O(18) C(54) 1.60(3) ? . . N(1) C(1) 1.44(1) ? . . N(1) C(9) 1.28(1) ? . . N(2) C(20) 1.45(1) ? . . N(2) C(28) 1.27(1) ? . . C(1) C(2) 1.50(1) ? . . C(2) C(3) 1.53(1) ? . . C(3) C(4) 1.50(1) ? . . C(4) C(5) 1.53(1) ? . . C(5) C(6) 1.52(1) ? . . C(7) C(8) 1.45(1) ? . . C(9) C(10) 1.44(1) ? . . C(10) C(11) 1.48(2) ? . . C(10) C(15) 1.39(1) ? . . C(11) C(12) 1.38(1) ? . . C(12) C(13) 1.37(1) ? . . C(12) C(16) 1.54(2) ? . . C(13) C(14) 1.36(2) ? . . C(14) C(15) 1.37(1) ? . . C(16) C(17) 1.56(1) ? . . C(16) C(18) 1.56(1) ? . . C(16) C(19) 1.55(2) ? . . C(20) C(21) 1.52(1) ? . . C(21) C(22) 1.52(1) ? . . C(22) C(23) 1.50(1) ? . . C(23) C(24) 1.54(1) ? . . C(24) C(25) 1.48(1) ? . . C(26) C(27) 1.53(1) ? . . C(28) C(29) 1.44(1) ? . . C(29) C(30) 1.38(2) ? . . C(29) C(34) 1.44(2) ? . . C(30) C(31) 1.48(1) ? . . C(31) C(32) 1.38(2) ? . . C(31) C(35) 1.54(2) ? . . C(32) C(33) 1.46(2) ? . . C(33) C(34) 1.31(1) ? . . C(35) C(36) 1.52(2) ? . . C(35) C(37) 1.55(1) ? . . C(35) C(38) 1.54(1) ? . . C(41) C(42) 1.53(1) ? . . C(42) C(43) 1.51(2) ? . . C(43) C(44) 1.50(2) ? . . C(45) C(46) 1.50(1) ? . . C(46) C(47) 1.53(2) ? . . C(47) C(48) 1.50(2) ? . . C(49) C(50) 1.45(3) ? . . C(50) C(51) 1.44(3) ? . . C(51) C(50) 1.44(3) ? . . C(51) C(52) 1.54(2) ? . . C(52) C(51) 1.54(2) ? . . C(53) C(56) 1.27(2) ? . . C(54) C(55) 1.37(4) ? . . C(55) C(56) 1.51(3) ? . . C(1) H(39) 0.9500 ? . . C(2) H(40) 0.9500 ? . . C(3) H(41) 0.9500 ? . . C(4) H(42) 0.9500 ? . . C(5) H(43) 0.9500 ? . . C(6) H(51) 0.9499 ? . . C(6) H(52) 0.9500 ? . . C(7) H(44) 0.9500 ? . . C(8) H(9) 0.9500 ? . . C(8) H(10) 0.9500 ? . . C(8) H(11) 0.9500 ? . . C(9) H(1) 0.9500 ? . . C(13) H(2) 0.9500 ? . . C(14) H(3) 0.9500 ? . . C(15) H(4) 0.9501 ? . . C(17) H(12) 0.9499 ? . . C(17) H(13) 0.9500 ? . . C(17) H(14) 0.9499 ? . . C(18) H(15) 0.9500 ? . . C(18) H(16) 0.9499 ? . . C(18) H(17) 0.9499 ? . . C(19) H(18) 0.9500 ? . . C(19) H(19) 0.9500 ? . . C(19) H(20) 0.9500 ? . . C(20) H(45) 0.9500 ? . . C(21) H(46) 0.9500 ? . . C(22) H(47) 0.9500 ? . . C(23) H(48) 0.9500 ? . . C(24) H(49) 0.9500 ? . . C(25) H(53) 0.9500 ? . . C(25) H(54) 0.9500 ? . . C(26) H(50) 0.9500 ? . . C(27) H(21) 0.9500 ? . . C(27) H(22) 0.9500 ? . . C(27) H(23) 0.9500 ? . . C(28) H(5) 0.9501 ? . . C(32) H(6) 0.9500 ? . . C(33) H(7) 0.9500 ? . . C(34) H(8) 0.9500 ? . . C(36) H(24) 0.9501 ? . . C(36) H(25) 0.9500 ? . . C(36) H(26) 0.9500 ? . . C(37) H(27) 0.9500 ? . . C(37) H(28) 0.9501 ? . . C(37) H(29) 0.9500 ? . . C(38) H(30) 0.9500 ? . . C(38) H(31) 0.9500 ? . . C(38) H(32) 0.9501 ? . . C(39) H(33) 0.9500 ? . . C(39) H(34) 0.9500 ? . . C(39) H(35) 0.9500 ? . . C(40) H(36) 0.9501 ? . . C(40) H(37) 0.9500 ? . . C(40) H(38) 0.9500 ? . . C(41) H(55) 0.9500 ? . . C(41) H(56) 0.9500 ? . . C(42) H(57) 0.9499 ? . . C(42) H(58) 0.9500 ? . . C(43) H(59) 0.9500 ? . . C(43) H(60) 0.9500 ? . . C(44) H(61) 0.9500 ? . . C(44) H(62) 0.9500 ? . . C(45) H(63) 0.9500 ? . . C(45) H(64) 0.9500 ? . . C(46) H(65) 0.9501 ? . . C(46) H(66) 0.9500 ? . . C(47) H(67) 0.9501 ? . . C(47) H(68) 0.9501 ? . . C(48) H(69) 0.9499 ? . . C(48) H(70) 0.9501 ? . . C(49) H(73) 0.9500 ? . . C(49) H(74) 0.9500 ? . . C(50) H(75) 0.9500 ? . . C(50) H(76) 0.9500 ? . . C(51) H(77) 0.9501 ? . . C(51) H(78) 0.9500 ? . . C(52) H(79) 0.9500 ? . . C(52) H(80) 0.9499 ? . . C(53) H(81) 0.9500 ? . . C(53) H(82) 0.9500 ? . . C(54) H(83) 0.9501 ? . . C(54) H(84) 0.9500 ? . . C(55) H(85) 0.9501 ? . . C(55) H(86) 0.9500 ? . . C(56) H(87) 0.9501 ? . . C(56) H(88) 0.9500 ? . . H(2) C(13) 0.9500 ? . . H(67) C(47) 0.9501 ? . . H(77) C(51) 0.9501 ? . . H(78) C(51) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Cu(1) O(1) 173.5(3) ? . . . O(13) Cu(1) O(1) 93.0(3) ? . . . O(15) Cu(1) O(1) 97.2(3) ? . . . N(1) Cu(1) O(1) 92.7(3) ? . . . Cu(1) O(1) C(11) 130.2(7) ? . . . O(13) Cu(1) O(2) 87.9(3) ? . . . O(15) Cu(1) O(2) 89.2(3) ? . . . N(1) Cu(1) O(2) 85.6(3) ? . . . Cu(1) O(2) C(2) 108.9(5) ? . . . Cu(1) O(2) Cu(2) 142.4(4) ? . . . O(15) Cu(1) O(13) 95.1(3) ? . . . N(1) Cu(1) O(13) 171.1(4) ? . . . Cu(1) O(13) C(39) 125.1(8) ? . . . N(1) Cu(1) O(15) 91.0(3) ? . . . Cu(1) O(15) C(41) 116.7(5) ? . . . Cu(1) O(15) C(44) 121.4(7) ? . . . Cu(1) N(1) C(1) 109.9(6) ? . . . Cu(1) N(1) C(9) 127.2(7) ? . . . Cu(2) O(2) C(2) 107.4(5) ? . . . O(3) Cu(2) O(2) 88.5(3) ? . . . O(8) Cu(2) O(2) 163.0(3) ? . . . O(9) Cu(2) O(2) 93.6(3) ? . . . O(8) Cu(2) O(3) 92.9(3) ? . . . O(9) Cu(2) O(3) 167.4(3) ? . . . Cu(2) O(3) C(3) 107.3(5) ? . . . O(9) Cu(2) O(8) 88.7(3) ? . . . Cu(2) O(8) C(21) 105.6(4) ? . . . Cu(2) O(8) Cu(3) 140.5(3) ? . . . Cu(2) O(9) C(22) 106.7(5) ? . . . O(8) Cu(3) O(7) 177.1(3) ? . . . O(14) Cu(3) O(7) 94.3(3) ? . . . O(16) Cu(3) O(7) 94.3(3) ? . . . N(2) Cu(3) O(7) 92.3(3) ? . . . Cu(3) O(7) C(30) 128.1(7) ? . . . O(14) Cu(3) O(8) 87.8(3) ? . . . Cu(3) O(8) C(21) 107.2(5) ? . . . O(16) Cu(3) O(8) 87.5(3) ? . . . N(2) Cu(3) O(8) 85.2(3) ? . . . O(16) Cu(3) O(14) 93.4(3) ? . . . N(2) Cu(3) O(14) 166.1(4) ? . . . Cu(3) O(14) C(40) 123.4(8) ? . . . N(2) Cu(3) O(16) 98.2(3) ? . . . Cu(3) O(16) C(45) 115.6(5) ? . . . Cu(3) O(16) C(48) 124.2(7) ? . . . Cu(3) N(2) C(20) 110.6(6) ? . . . Cu(3) N(2) C(28) 125.9(6) ? . . . O(1) C(11) C(10) 119.8(8) ? . . . O(1) C(11) C(12) 121(1) ? . . . O(2) C(2) C(1) 111.3(7) ? . . . O(2) C(2) C(3) 109.8(6) ? . . . O(3) C(3) C(2) 107.2(9) ? . . . O(3) C(3) C(4) 117.2(8) ? . . . O(4) C(4) C(3) 111.3(6) ? . . . O(4) C(4) C(5) 108.0(8) ? . . . C(7) O(4) C(4) 110.8(5) ? . . . O(4) C(7) O(6) 110.0(7) ? . . . O(4) C(7) C(8) 107.4(6) ? . . . O(5) C(1) N(1) 114.1(6) ? . . . O(5) C(1) C(2) 108.2(7) ? . . . C(5) O(5) C(1) 107.1(5) ? . . . O(5) C(5) C(4) 113.8(8) ? . . . O(5) C(5) C(6) 108.0(6) ? . . . O(6) C(6) C(5) 108.8(6) ? . . . C(7) O(6) C(6) 112.6(8) ? . . . O(6) C(7) C(8) 110(1) ? . . . O(7) C(30) C(29) 124.5(9) ? . . . O(7) C(30) C(31) 116(1) ? . . . O(8) C(21) C(22) 111.7(8) ? . . . O(8) C(21) C(20) 109.7(7) ? . . . O(9) C(22) C(21) 106.5(6) ? . . . O(9) C(22) C(23) 117.2(7) ? . . . O(10) C(23) C(22) 112.8(8) ? . . . O(10) C(23) C(24) 106.2(6) ? . . . C(26) O(10) C(23) 110.8(8) ? . . . O(10) C(26) O(12) 110.2(7) ? . . . O(10) C(26) C(27) 109.1(9) ? . . . O(11) C(20) C(21) 110.3(7) ? . . . O(11) C(20) N(2) 114.4(8) ? . . . C(24) O(11) C(20) 111.2(7) ? . . . O(11) C(24) C(23) 111.7(6) ? . . . O(11) C(24) C(25) 109.9(8) ? . . . O(12) C(25) C(24) 108.7(9) ? . . . C(26) O(12) C(25) 112.0(6) ? . . . O(12) C(26) C(27) 107.1(7) ? . . . C(44) O(15) C(41) 107.1(7) ? . . . O(15) C(41) C(42) 105.2(8) ? . . . O(15) C(44) C(43) 105(1) ? . . . C(48) O(16) C(45) 107.2(6) ? . . . O(16) C(45) C(46) 106.7(8) ? . . . O(16) C(48) C(47) 105.6(9) ? . . . O(17) C(49) C(50) 104(1) ? . . . C(52) O(17) C(49) 111(1) ? . . . O(17) C(52) C(51) 102(1) ? . . . C(54) O(18) C(53) 90(1) ? . . . O(18) C(53) C(56) 117(2) ? . . . O(18) C(54) C(55) 115(2) ? . . . N(1) C(1) C(2) 107.4(8) ? . . . C(9) N(1) C(1) 122.6(9) ? . . . N(1) C(9) C(10) 124(1) ? . . . N(2) C(20) C(21) 105.7(6) ? . . . C(28) N(2) C(20) 123.5(8) ? . . . N(2) C(28) C(29) 125.8(9) ? . . . C(1) C(2) C(3) 110.6(9) ? . . . C(2) C(3) C(4) 103.8(6) ? . . . C(3) C(4) C(5) 109.9(7) ? . . . C(4) C(5) C(6) 107.4(7) ? . . . C(9) C(10) C(11) 124.5(9) ? . . . C(9) C(10) C(15) 117(1) ? . . . C(10) C(11) C(12) 118.5(9) ? . . . C(15) C(10) C(11) 117.8(8) ? . . . C(10) C(15) C(14) 122(1) ? . . . C(11) C(12) C(13) 119(1) ? . . . C(11) C(12) C(16) 119.7(9) ? . . . C(16) C(12) C(13) 121.2(8) ? . . . C(12) C(13) C(14) 124.5(9) ? . . . C(12) C(16) C(18) 109.9(8) ? . . . C(12) C(16) C(19) 110.1(8) ? . . . C(12) C(16) C(17) 112.2(8) ? . . . C(13) C(14) C(15) 118(1) ? . . . C(18) C(16) C(17) 106.7(7) ? . . . C(19) C(16) C(17) 107.4(9) ? . . . C(19) C(16) C(18) 110.5(8) ? . . . C(20) C(21) C(22) 110.2(6) ? . . . C(21) C(22) C(23) 105.8(9) ? . . . C(22) C(23) C(24) 109.8(6) ? . . . C(23) C(24) C(25) 109.9(7) ? . . . C(28) C(29) C(30) 122(1) ? . . . C(28) C(29) C(34) 116.0(9) ? . . . C(29) C(30) C(31) 118(1) ? . . . C(34) C(29) C(30) 121.0(9) ? . . . C(29) C(34) C(33) 121(1) ? . . . C(30) C(31) C(35) 120.8(9) ? . . . C(30) C(31) C(32) 117(1) ? . . . C(35) C(31) C(32) 121.7(8) ? . . . C(31) C(32) C(33) 122.0(8) ? . . . C(31) C(35) C(36) 110.9(8) ? . . . C(31) C(35) C(37) 110.8(8) ? . . . C(31) C(35) C(38) 110.1(9) ? . . . C(32) C(33) C(34) 119(1) ? . . . C(37) C(35) C(36) 110.3(9) ? . . . C(38) C(35) C(36) 107.3(9) ? . . . C(38) C(35) C(37) 107.4(7) ? . . . C(41) C(42) C(43) 103(1) ? . . . C(42) C(43) C(44) 106.5(9) ? . . . C(45) C(46) C(47) 102(1) ? . . . C(46) C(47) C(48) 107.3(8) ? . . . C(49) C(50) C(51) 105(1) ? . . . C(50) C(51) C(52) 108(1) ? . . . C(53) C(56) C(55) 106(1) ? . . . C(54) C(55) C(56) 107(1) ? . . . O(2) C(2) H(40) 108.3974 ? . . . O(3) C(3) H(41) 109.2586 ? . . . O(4) C(4) H(42) 109.0714 ? . . . O(4) C(7) H(44) 109.3136 ? . . . O(5) C(1) H(39) 109.0687 ? . . . O(5) C(5) H(43) 109.3164 ? . . . O(6) C(6) H(52) 109.5274 ? . . . O(6) C(6) H(51) 109.6724 ? . . . O(6) C(7) H(44) 109.5021 ? . . . O(8) C(21) H(46) 108.5318 ? . . . O(9) C(22) H(47) 109.0685 ? . . . O(10) C(23) H(48) 109.5908 ? . . . O(10) C(26) H(50) 110.1498 ? . . . O(11) C(20) H(45) 108.8839 ? . . . O(11) C(24) H(49) 108.2061 ? . . . O(12) C(25) H(54) 110.0223 ? . . . O(12) C(25) H(53) 109.3704 ? . . . O(12) C(26) H(50) 110.1624 ? . . . O(13) C(39) H(33) 109.1902 ? . . . O(13) C(39) H(35) 109.9789 ? . . . O(13) C(39) H(34) 109.2075 ? . . . O(14) C(40) H(36) 109.7250 ? . . . O(14) C(40) H(38) 108.7855 ? . . . O(14) C(40) H(37) 110.0798 ? . . . O(15) C(41) H(55) 110.6219 ? . . . O(15) C(41) H(56) 110.2972 ? . . . O(15) C(44) H(61) 110.2635 ? . . . O(15) C(44) H(62) 110.3944 ? . . . O(16) C(45) H(63) 110.2275 ? . . . O(16) C(45) H(64) 109.9107 ? . . . O(16) C(48) H(69) 110.4877 ? . . . O(16) C(48) H(70) 110.5198 ? . . . O(17) C(49) H(73) 110.6996 ? . . . O(17) C(49) H(74) 109.3286 ? . . . O(17) C(52) H(79) 108.4526 ? . . . O(17) C(52) H(80) 112.3682 ? . . . O(18) C(53) H(81) 107.2234 ? . . . O(18) C(53) H(82) 105.9540 ? . . . O(18) C(54) H(83) 108.3883 ? . . . O(18) C(54) H(84) 106.6173 ? . . . N(1) C(1) H(39) 108.8937 ? . . . N(1) C(9) H(1) 117.4102 ? . . . N(2) C(20) H(45) 108.6138 ? . . . N(2) C(28) H(5) 117.2982 ? . . . H(39) C(1) C(2) 109.0838 ? . . . C(1) C(2) H(40) 108.3558 ? . . . H(40) C(2) C(3) 108.2951 ? . . . C(2) C(3) H(41) 109.5173 ? . . . H(41) C(3) C(4) 109.5145 ? . . . C(3) C(4) H(42) 109.3460 ? . . . H(42) C(4) C(5) 109.2760 ? . . . C(4) C(5) H(43) 109.1206 ? . . . H(43) C(5) C(6) 109.0702 ? . . . C(5) C(6) H(52) 109.6958 ? . . . C(5) C(6) H(51) 109.7168 ? . . . H(52) C(6) H(51) 109.4591 ? . . . C(7) C(8) H(9) 109.4773 ? . . . C(7) C(8) H(10) 108.6921 ? . . . C(7) C(8) H(11) 110.5158 ? . . . H(44) C(7) C(8) 110.3192 ? . . . H(10) C(8) H(9) 109.7076 ? . . . H(11) C(8) H(9) 109.4713 ? . . . H(11) C(8) H(10) 108.9599 ? . . . H(1) C(9) C(10) 117.8572 ? . . . C(10) C(15) H(4) 119.0196 ? . . . C(12) C(13) H(2) 118.0378 ? . . . C(13) C(14) H(3) 120.8669 ? . . . H(2) C(13) C(14) 117.4800 ? . . . C(14) C(15) H(4) 118.8145 ? . . . H(3) C(14) C(15) 121.0809 ? . . . C(16) C(17) H(12) 109.6960 ? . . . C(16) C(17) H(13) 109.3224 ? . . . C(16) C(17) H(14) 110.0952 ? . . . C(16) C(18) H(15) 110.2613 ? . . . C(16) C(18) H(17) 109.4100 ? . . . C(16) C(18) H(16) 109.2392 ? . . . C(16) C(19) H(19) 109.7355 ? . . . C(16) C(19) H(20) 109.4234 ? . . . C(16) C(19) H(18) 109.0542 ? . . . H(13) C(17) H(12) 109.2547 ? . . . H(14) C(17) H(12) 109.4751 ? . . . H(14) C(17) H(13) 108.9785 ? . . . H(17) C(18) H(15) 109.4876 ? . . . H(16) C(18) H(15) 109.1612 ? . . . H(17) C(18) H(16) 109.2637 ? . . . H(19) C(19) H(18) 109.6618 ? . . . H(20) C(19) H(18) 109.4713 ? . . . H(20) C(19) H(19) 109.4800 ? . . . C(20) C(21) H(46) 108.1473 ? . . . H(45) C(20) C(21) 108.7681 ? . . . H(46) C(21) C(22) 108.4464 ? . . . C(21) C(22) H(47) 109.0392 ? . . . H(47) C(22) C(23) 108.9823 ? . . . C(22) C(23) H(48) 109.1850 ? . . . H(48) C(23) C(24) 109.1637 ? . . . C(23) C(24) H(49) 108.3915 ? . . . H(49) C(24) C(25) 108.5893 ? . . . C(24) C(25) H(54) 109.7972 ? . . . C(24) C(25) H(53) 109.4344 ? . . . H(54) C(25) H(53) 109.4642 ? . . . C(26) C(27) H(21) 109.4762 ? . . . C(26) C(27) H(22) 109.7501 ? . . . C(26) C(27) H(23) 109.4436 ? . . . H(50) C(26) C(27) 110.0866 ? . . . H(22) C(27) H(21) 109.6489 ? . . . H(23) C(27) H(21) 109.4706 ? . . . H(23) C(27) H(22) 109.0369 ? . . . H(5) C(28) C(29) 116.8533 ? . . . C(29) C(34) H(8) 119.2122 ? . . . C(31) C(32) H(6) 118.6849 ? . . . C(32) C(33) H(7) 120.0107 ? . . . H(6) C(32) C(33) 119.3400 ? . . . C(33) C(34) H(8) 119.2868 ? . . . H(7) C(33) C(34) 120.4803 ? . . . C(35) C(36) H(24) 109.3371 ? . . . C(35) C(36) H(26) 109.3069 ? . . . C(35) C(36) H(25) 109.5892 ? . . . C(35) C(37) H(28) 109.6507 ? . . . C(35) C(37) H(29) 107.6886 ? . . . C(35) C(37) H(27) 109.8286 ? . . . C(35) C(38) H(30) 110.4406 ? . . . C(35) C(38) H(31) 109.6808 ? . . . C(35) C(38) H(32) 108.0074 ? . . . H(26) C(36) H(24) 109.4734 ? . . . H(25) C(36) H(24) 109.4841 ? . . . H(26) C(36) H(25) 109.6360 ? . . . H(28) C(37) H(27) 109.3661 ? . . . H(29) C(37) H(27) 109.4694 ? . . . H(29) C(37) H(28) 110.8162 ? . . . H(31) C(38) H(30) 109.0308 ? . . . H(32) C(38) H(30) 109.4741 ? . . . H(32) C(38) H(31) 110.1984 ? . . . H(35) C(39) H(33) 109.4756 ? . . . H(34) C(39) H(33) 109.6538 ? . . . H(35) C(39) H(34) 109.3215 ? . . . H(38) C(40) H(36) 109.4707 ? . . . H(37) C(40) H(36) 109.0600 ? . . . H(38) C(40) H(37) 109.7070 ? . . . H(55) C(41) C(42) 111.0454 ? . . . H(56) C(41) C(42) 110.1962 ? . . . C(41) C(42) H(57) 110.4358 ? . . . C(41) C(42) H(58) 111.1420 ? . . . H(56) C(41) H(55) 109.4555 ? . . . H(57) C(42) C(43) 111.7097 ? . . . H(58) C(42) C(43) 110.5912 ? . . . C(42) C(43) H(59) 109.7730 ? . . . C(42) C(43) H(60) 110.9183 ? . . . H(58) C(42) H(57) 109.4542 ? . . . C(43) C(44) H(61) 109.6196 ? . . . C(43) C(44) H(62) 111.6599 ? . . . H(59) C(43) C(44) 109.2885 ? . . . H(60) C(43) C(44) 110.8404 ? . . . H(60) C(43) H(59) 109.4617 ? . . . H(62) C(44) H(61) 109.4573 ? . . . H(63) C(45) C(46) 110.8261 ? . . . H(64) C(45) C(46) 109.6614 ? . . . C(45) C(46) H(65) 110.3864 ? . . . C(45) C(46) H(66) 111.8540 ? . . . H(64) C(45) H(63) 109.4603 ? . . . H(65) C(46) C(47) 110.7805 ? . . . H(66) C(46) C(47) 111.4170 ? . . . C(46) C(47) H(67) 110.2767 ? . . . C(46) C(47) H(68) 109.7496 ? . . . H(66) C(46) H(65) 109.4643 ? . . . C(47) C(48) H(69) 110.0375 ? . . . C(47) C(48) H(70) 110.6683 ? . . . H(67) C(47) C(48) 109.7483 ? . . . H(68) C(47) C(48) 110.3230 ? . . . H(68) C(47) H(67) 109.4637 ? . . . H(70) C(48) H(69) 109.4559 ? . . . H(73) C(49) C(50) 111.1398 ? . . . H(74) C(49) C(50) 111.6491 ? . . . C(49) C(50) H(75) 110.2761 ? . . . C(49) C(50) H(76) 109.8879 ? . . . H(74) C(49) H(73) 109.4640 ? . . . H(75) C(50) C(51) 111.2052 ? . . . H(76) C(50) C(51) 110.1762 ? . . . C(50) C(51) H(77) 109.3858 ? . . . C(50) C(51) H(78) 110.1256 ? . . . H(76) C(50) H(75) 109.4588 ? . . . H(77) C(51) C(52) 108.5015 ? . . . H(78) C(51) C(52) 111.2832 ? . . . C(51) C(52) H(79) 110.5439 ? . . . C(51) C(52) H(80) 113.1652 ? . . . H(78) C(51) H(77) 109.4588 ? . . . H(80) C(52) H(79) 109.4540 ? . . . H(81) C(53) C(56) 109.4638 ? . . . H(82) C(53) C(56) 106.5367 ? . . . C(53) C(56) H(87) 108.0237 ? . . . C(53) C(56) H(88) 111.4632 ? . . . H(82) C(53) H(81) 109.4608 ? . . . H(83) C(54) C(55) 108.8967 ? . . . H(84) C(54) C(55) 108.2638 ? . . . C(54) C(55) H(85) 110.2828 ? . . . C(54) C(55) H(86) 110.6146 ? . . . H(84) C(54) H(83) 109.4566 ? . . . H(85) C(55) C(56) 108.9818 ? . . . H(86) C(55) C(56) 109.8720 ? . . . C(55) C(56) H(87) 110.3887 ? . . . C(55) C(56) H(88) 110.9445 ? . . . H(86) C(55) H(85) 109.4608 ? . . . H(88) C(56) H(87) 109.4616 ? . . . #============================================================================== #===END #============================================================================== data_Complex_4 _database_code_depnum_ccdc_archive 'CCDC 250719' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H32 Cu N2 O2 ' _chemical_formula_moiety 'C24 H32 Cu N2 O2 ' _chemical_formula_weight 444.07 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.830(4) _cell_length_b 10.858(3) _cell_length_c 17.007(5) _cell_angle_alpha 90 _cell_angle_beta 102.255(4) _cell_angle_gamma 90 _cell_volume 2315.3(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3496 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.1 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description cubic _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940.00 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.398 _exptl_absorpt_correction_T_max 0.749 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 12529 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_max 26.71 _diffrn_measured_fraction_theta_max 0.4710 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.5517 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 #============================================================================== # 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 5674 _reflns_number_gt 5073 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.1060 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5096 _refine_ls_number_parameters 294 _refine_ls_goodness_of_fit_ref 1.603 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0040 _refine_diff_density_max 1.1770 _refine_diff_density_min -1.62 _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 C C 0.003 0.002 ; 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) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; 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 Cu(1) Cu 0.57130(5) 0.57231(6) 0.69054(5) 0.0447(3) Uani 1.00 1 d . . . O(1) O 0.4257(3) 0.6073(3) 0.6369(3) 0.0474(13) Uani 1.00 1 d . . . O(2) O 0.7118(3) 0.6135(3) 0.7520(3) 0.044(1) Uani 1.00 1 d . . . N(1) N 0.6211(4) 0.5767(4) 0.5888(4) 0.046(2) Uani 1.00 1 d . . . N(2) N 0.5276(4) 0.5027(4) 0.7848(4) 0.047(2) Uani 1.00 1 d . . . C(1) C 0.7264(4) 0.5226(5) 0.5857(5) 0.056(2) Uani 1.00 1 d . . . C(2) C 0.5657(5) 0.6308(5) 0.5249(5) 0.046(2) Uani 1.00 1 d . . . C(3) C 0.4635(4) 0.6914(5) 0.5135(4) 0.046(2) Uani 1.00 1 d . . . C(4) C 0.3980(4) 0.6822(5) 0.5742(4) 0.037(2) Uani 1.00 1 d . . . C(5) C 0.2971(4) 0.7457(5) 0.5611(4) 0.040(2) Uani 1.00 1 d . . . C(6) C 0.2694(5) 0.8200(5) 0.4916(4) 0.044(2) Uani 1.00 1 d . . . C(7) C 0.3318(4) 0.8283(5) 0.4331(5) 0.050(2) Uani 1.00 1 d . . . C(8) C 0.4259(4) 0.7631(5) 0.4461(4) 0.047(2) Uani 1.00 1 d . . . C(9) C 0.2209(4) 0.7351(5) 0.6200(5) 0.056(2) Uani 1.00 1 d . . . C(10) C 0.1236(4) 0.8228(5) 0.5996(5) 0.065(3) Uani 1.00 1 d . . . C(11) C 0.1760(4) 0.6015(5) 0.6104(4) 0.051(2) Uani 1.00 1 d . . . C(12) C 0.2765(5) 0.7558(6) 0.7077(5) 0.064(2) Uani 1.00 1 d . . . C(13) C 0.4319(4) 0.4211(5) 0.7728(5) 0.058(2) Uani 1.00 1 d . . . C(14) C 0.5784(5) 0.5270(5) 0.8606(5) 0.054(2) Uani 1.00 1 d . . . C(15) C 0.6759(5) 0.5995(5) 0.8853(5) 0.049(2) Uani 1.00 1 d . . . C(16) C 0.7386(5) 0.6425(5) 0.8287(5) 0.045(2) Uani 1.00 1 d . . . C(17) C 0.8364(4) 0.7074(5) 0.8604(4) 0.044(2) Uani 1.00 1 d . . . C(18) C 0.8629(5) 0.7349(6) 0.9437(5) 0.054(2) Uani 1.00 1 d . . . C(19) C 0.7981(5) 0.6957(6) 0.9982(5) 0.068(3) Uani 1.00 1 d . . . C(20) C 0.7071(5) 0.6267(6) 0.9660(5) 0.057(3) Uani 1.00 1 d . . . C(21) C 0.9116(4) 0.7444(5) 0.8036(4) 0.048(2) Uani 1.00 1 d . . . C(22) C 1.0085(4) 0.8214(5) 0.8471(5) 0.073(3) Uani 1.00 1 d . . . C(23) C 0.9567(5) 0.6229(5) 0.7745(4) 0.054(2) Uani 1.00 1 d . . . C(24) C 0.8536(4) 0.8261(5) 0.7328(4) 0.048(2) Uani 1.00 1 d . . . H(1) H 0.2046 0.8652 0.4832 0.051 Uiso 1.00 1 c R . . H(2) H 0.3102 0.8791 0.3871 0.061 Uiso 1.00 1 c R . . H(3) H 0.4671 0.7661 0.4059 0.058 Uiso 1.00 1 c R . . H(4) H 0.9252 0.7815 0.9647 0.065 Uiso 1.00 1 c R . . H(5) H 0.8170 0.7174 1.0535 0.083 Uiso 1.00 1 c R . . H(6) H 0.6670 0.5960 1.0027 0.070 Uiso 1.00 1 c R . . H(7) H 0.5965 0.6292 0.4789 0.057 Uiso 1.00 1 c R . . H(8) H 0.5497 0.4910 0.9023 0.068 Uiso 1.00 1 c R . . H(9) H 0.7811 0.5827 0.5995 0.069 Uiso 1.00 1 c R . . H(10) H 0.7243 0.4934 0.5328 0.070 Uiso 1.00 1 c R . . H(11) H 0.7406 0.4560 0.6226 0.069 Uiso 1.00 1 c R . . H(12) H 0.1420 0.8976 0.6281 0.082 Uiso 1.00 1 c R . . H(13) H 0.0641 0.7866 0.6158 0.082 Uiso 1.00 1 c R . . H(14) H 0.1057 0.8391 0.5434 0.082 Uiso 1.00 1 c R . . H(15) H 0.1122 0.5978 0.5701 0.064 Uiso 1.00 1 c R . . H(16) H 0.1616 0.5768 0.6606 0.064 Uiso 1.00 1 c R . . H(17) H 0.2277 0.5480 0.5963 0.064 Uiso 1.00 1 c R . . H(18) H 0.3049 0.6810 0.7323 0.078 Uiso 1.00 1 c R . . H(19) H 0.2269 0.7888 0.7364 0.078 Uiso 1.00 1 c R . . H(20) H 0.3327 0.8131 0.7087 0.078 Uiso 1.00 1 c R . . H(21) H 0.3693 0.4685 0.7712 0.070 Uiso 1.00 1 c R . . H(22) H 0.4402 0.3636 0.8158 0.070 Uiso 1.00 1 c R . . H(23) H 0.4261 0.3781 0.7234 0.070 Uiso 1.00 1 c R . . H(24) H 0.9913 0.9066 0.8434 0.083 Uiso 1.00 1 c R . . H(25) H 1.0678 0.8066 0.8232 0.084 Uiso 1.00 1 c R . . H(26) H 1.0259 0.7977 0.9021 0.084 Uiso 1.00 1 c R . . H(27) H 1.0207 0.5977 0.8099 0.066 Uiso 1.00 1 c R . . H(28) H 0.9703 0.6375 0.7225 0.066 Uiso 1.00 1 c R . . H(29) H 0.9044 0.5601 0.7713 0.066 Uiso 1.00 1 c R . . H(30) H 0.8222 0.7755 0.6885 0.058 Uiso 1.00 1 c R . . H(31) H 0.9041 0.8798 0.7172 0.058 Uiso 1.00 1 c R . . H(32) H 0.7997 0.8733 0.7493 0.058 Uiso 1.00 1 c R . . 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) 0.0456(5) 0.0365(4) 0.0557(7) -0.0016(3) 0.0193(4) -0.0013(4) O(1) 0.047(2) 0.048(2) 0.050(3) 0.001(2) 0.017(2) -0.002(2) O(2) 0.045(2) 0.044(2) 0.047(4) -0.008(2) 0.016(2) -0.010(2) N(1) 0.040(3) 0.041(3) 0.063(5) -0.015(2) 0.020(3) -0.010(3) N(2) 0.047(3) 0.040(3) 0.060(5) -0.005(2) 0.029(3) 0.000(3) C(1) 0.054(4) 0.048(3) 0.072(6) -0.005(3) 0.028(4) -0.028(4) C(2) 0.062(4) 0.039(3) 0.041(5) -0.017(3) 0.018(4) -0.018(3) C(3) 0.046(4) 0.041(3) 0.056(5) -0.011(3) 0.025(4) 0.001(4) C(4) 0.044(3) 0.037(3) 0.029(5) -0.010(3) 0.004(3) 0.001(3) C(5) 0.046(3) 0.032(3) 0.042(5) -0.003(3) 0.011(3) 0.006(3) C(6) 0.047(3) 0.034(3) 0.046(5) -0.007(3) 0.002(3) -0.001(3) C(7) 0.047(4) 0.035(3) 0.071(6) -0.004(3) 0.021(4) -0.010(3) C(8) 0.047(4) 0.045(4) 0.053(5) -0.017(3) 0.019(3) -0.005(4) C(9) 0.040(3) 0.030(3) 0.100(7) -0.001(3) 0.018(4) 0.002(4) C(10) 0.056(4) 0.044(4) 0.106(8) -0.003(3) 0.040(4) -0.001(4) C(11) 0.041(3) 0.047(4) 0.071(6) -0.012(3) 0.024(3) -0.009(3) C(12) 0.047(4) 0.049(4) 0.099(7) 0.011(3) 0.022(4) -0.003(4) C(13) 0.054(4) 0.049(4) 0.073(6) 0.004(3) 0.019(4) 0.020(4) C(14) 0.067(4) 0.041(3) 0.063(6) 0.013(3) 0.032(4) 0.019(4) C(15) 0.049(4) 0.045(4) 0.056(6) 0.018(3) 0.017(4) 0.000(4) C(16) 0.055(4) 0.030(3) 0.056(6) 0.015(3) 0.027(4) 0.006(3) C(17) 0.046(4) 0.037(3) 0.049(5) 0.005(3) 0.011(3) -0.008(3) C(18) 0.057(4) 0.050(4) 0.054(6) 0.010(3) 0.012(4) 0.005(4) C(19) 0.055(4) 0.069(5) 0.084(7) 0.021(4) 0.023(5) -0.014(4) C(20) 0.050(4) 0.050(4) 0.073(7) 0.015(3) 0.019(4) -0.004(4) C(21) 0.052(4) 0.033(3) 0.059(5) -0.000(3) 0.010(4) -0.006(3) C(22) 0.041(4) 0.048(4) 0.119(8) 0.009(3) -0.008(4) -0.002(4) C(23) 0.059(4) 0.054(4) 0.053(6) 0.007(3) 0.022(4) 0.007(3) C(24) 0.051(4) 0.029(3) 0.065(5) 0.003(3) 0.015(3) -0.005(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) O(1) 1.934(4) ? . . Cu(1) O(2) 1.934(4) ? . . Cu(1) N(1) 1.968(6) ? . . Cu(1) N(2) 1.959(6) ? . . O(1) C(4) 1.328(7) ? . . O(2) C(16) 1.314(9) ? . . N(1) C(1) 1.484(8) ? . . N(1) C(2) 1.304(8) ? . . N(2) C(13) 1.492(7) ? . . N(2) C(14) 1.34(1) ? . . C(2) C(3) 1.443(8) ? . . C(3) C(4) 1.47(1) ? . . C(3) C(8) 1.385(9) ? . . C(4) C(5) 1.442(7) ? . . C(5) C(6) 1.413(9) ? . . C(5) C(9) 1.54(1) ? . . C(6) C(7) 1.41(1) ? . . C(7) C(8) 1.376(8) ? . . C(9) C(10) 1.550(8) ? . . C(9) C(11) 1.556(8) ? . . C(9) C(12) 1.53(1) ? . . C(14) C(15) 1.462(8) ? . . C(15) C(16) 1.46(1) ? . . C(15) C(20) 1.38(1) ? . . C(16) C(17) 1.441(8) ? . . C(17) C(18) 1.42(1) ? . . C(17) C(21) 1.56(1) ? . . C(18) C(19) 1.43(1) ? . . C(19) C(20) 1.397(9) ? . . C(21) C(22) 1.550(8) ? . . C(21) C(23) 1.562(9) ? . . C(21) C(24) 1.553(8) ? . . C(1) H(9) 0.9500 ? . . C(1) H(10) 0.9500 ? . . C(1) H(11) 0.9500 ? . . C(2) H(7) 0.9499 ? . . C(6) H(1) 0.9500 ? . . C(7) H(2) 0.9500 ? . . C(8) H(3) 0.9500 ? . . C(10) H(12) 0.9500 ? . . C(10) H(13) 0.9499 ? . . C(10) H(14) 0.9500 ? . . C(11) H(15) 0.9500 ? . . C(11) H(16) 0.9501 ? . . C(11) H(17) 0.9501 ? . . C(12) H(18) 0.9500 ? . . C(12) H(19) 0.9500 ? . . C(12) H(20) 0.9500 ? . . C(13) H(21) 0.9500 ? . . C(13) H(22) 0.9500 ? . . C(13) H(23) 0.9500 ? . . C(14) H(8) 0.9500 ? . . C(18) H(4) 0.9501 ? . . C(19) H(5) 0.9501 ? . . C(20) H(6) 0.9500 ? . . C(22) H(24) 0.9500 ? . . C(22) H(25) 0.9500 ? . . C(22) H(26) 0.9499 ? . . C(23) H(27) 0.9500 ? . . C(23) H(28) 0.9500 ? . . C(23) H(29) 0.9500 ? . . C(24) H(30) 0.9500 ? . . C(24) H(31) 0.9501 ? . . C(24) H(32) 0.9499 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Cu(1) O(1) 154.9(2) ? . . . N(1) Cu(1) O(1) 92.4(2) ? . . . N(2) Cu(1) O(1) 92.7(2) ? . . . Cu(1) O(1) C(4) 124.5(4) ? . . . N(1) Cu(1) O(2) 91.7(2) ? . . . N(2) Cu(1) O(2) 92.5(2) ? . . . Cu(1) O(2) C(16) 127.5(4) ? . . . N(2) Cu(1) N(1) 158.7(2) ? . . . Cu(1) N(1) C(1) 119.2(4) ? . . . Cu(1) N(1) C(2) 121.5(5) ? . . . Cu(1) N(2) C(13) 119.2(4) ? . . . Cu(1) N(2) C(14) 123.0(4) ? . . . O(1) C(4) C(3) 120.7(5) ? . . . O(1) C(4) C(5) 119.7(6) ? . . . O(2) C(16) C(15) 121.0(5) ? . . . O(2) C(16) C(17) 120.8(7) ? . . . C(2) N(1) C(1) 119.2(6) ? . . . N(1) C(2) C(3) 129.5(7) ? . . . C(14) N(2) C(13) 117.8(6) ? . . . N(2) C(14) C(15) 126.5(7) ? . . . C(2) C(3) C(4) 121.0(6) ? . . . C(2) C(3) C(8) 121.0(7) ? . . . C(3) C(4) C(5) 119.3(5) ? . . . C(8) C(3) C(4) 118.0(5) ? . . . C(3) C(8) C(7) 124.2(7) ? . . . C(4) C(5) C(9) 122.4(5) ? . . . C(4) C(5) C(6) 117.4(6) ? . . . C(9) C(5) C(6) 120.2(5) ? . . . C(5) C(6) C(7) 123.3(5) ? . . . C(5) C(9) C(11) 105.8(5) ? . . . C(5) C(9) C(12) 113.2(5) ? . . . C(5) C(9) C(10) 113.6(6) ? . . . C(6) C(7) C(8) 117.7(6) ? . . . C(11) C(9) C(10) 106.6(4) ? . . . C(12) C(9) C(10) 108.4(6) ? . . . C(12) C(9) C(11) 109.0(6) ? . . . C(14) C(15) C(16) 122.7(7) ? . . . C(14) C(15) C(20) 116.9(7) ? . . . C(15) C(16) C(17) 117.9(7) ? . . . C(20) C(15) C(16) 120.4(6) ? . . . C(15) C(20) C(19) 123.2(7) ? . . . C(16) C(17) C(21) 119.9(6) ? . . . C(16) C(17) C(18) 118.9(7) ? . . . C(21) C(17) C(18) 121.2(5) ? . . . C(17) C(18) C(19) 122.3(6) ? . . . C(17) C(21) C(23) 107.4(5) ? . . . C(17) C(21) C(24) 111.8(5) ? . . . C(17) C(21) C(22) 112.5(6) ? . . . C(18) C(19) C(20) 117.1(7) ? . . . C(23) C(21) C(22) 107.1(4) ? . . . C(24) C(21) C(22) 105.4(5) ? . . . C(24) C(21) C(23) 112.7(5) ? . . . N(1) C(1) H(9) 110.5059 ? . . . N(1) C(1) H(11) 109.0593 ? . . . N(1) C(1) H(10) 108.8359 ? . . . N(1) C(2) H(7) 115.4926 ? . . . N(2) C(13) H(21) 110.4223 ? . . . N(2) C(13) H(23) 108.6969 ? . . . N(2) C(13) H(22) 109.2861 ? . . . N(2) C(14) H(8) 116.7423 ? . . . H(11) C(1) H(9) 109.4718 ? . . . H(10) C(1) H(9) 109.4723 ? . . . H(11) C(1) H(10) 109.4771 ? . . . H(7) C(2) C(3) 115.0155 ? . . . C(3) C(8) H(3) 117.7550 ? . . . C(5) C(6) H(1) 118.5228 ? . . . C(6) C(7) H(2) 120.6635 ? . . . H(1) C(6) C(7) 118.1891 ? . . . C(7) C(8) H(3) 118.0521 ? . . . H(2) C(7) C(8) 121.5881 ? . . . C(9) C(10) H(12) 108.0570 ? . . . C(9) C(10) H(13) 109.8036 ? . . . C(9) C(10) H(14) 110.5364 ? . . . C(9) C(11) H(16) 107.9001 ? . . . C(9) C(11) H(17) 109.5256 ? . . . C(9) C(11) H(15) 110.9702 ? . . . C(9) C(12) H(18) 111.0687 ? . . . C(9) C(12) H(20) 107.9410 ? . . . C(9) C(12) H(19) 109.3839 ? . . . H(13) C(10) H(12) 109.4740 ? . . . H(14) C(10) H(12) 109.4774 ? . . . H(14) C(10) H(13) 109.4689 ? . . . H(16) C(11) H(15) 109.4660 ? . . . H(17) C(11) H(15) 109.4722 ? . . . H(17) C(11) H(16) 109.4789 ? . . . H(20) C(12) H(18) 109.4738 ? . . . H(19) C(12) H(18) 109.4676 ? . . . H(20) C(12) H(19) 109.4774 ? . . . H(23) C(13) H(21) 109.4721 ? . . . H(22) C(13) H(21) 109.4708 ? . . . H(23) C(13) H(22) 109.4744 ? . . . H(8) C(14) C(15) 116.7566 ? . . . C(15) C(20) H(6) 119.7689 ? . . . C(17) C(18) H(4) 119.5161 ? . . . C(18) C(19) H(5) 120.3055 ? . . . H(4) C(18) C(19) 118.1978 ? . . . C(19) C(20) H(6) 116.9740 ? . . . H(5) C(19) C(20) 122.5543 ? . . . C(21) C(22) H(24) 109.9585 ? . . . C(21) C(22) H(25) 109.7378 ? . . . C(21) C(22) H(26) 108.7153 ? . . . C(21) C(23) H(28) 107.8978 ? . . . C(21) C(23) H(29) 108.7215 ? . . . C(21) C(23) H(27) 111.7615 ? . . . C(21) C(24) H(30) 109.7586 ? . . . C(21) C(24) H(32) 109.7699 ? . . . C(21) C(24) H(31) 108.8821 ? . . . H(25) C(22) H(24) 109.4710 ? . . . H(26) C(22) H(24) 109.4710 ? . . . H(26) C(22) H(25) 109.4710 ? . . . H(28) C(23) H(27) 109.4780 ? . . . H(29) C(23) H(27) 109.4679 ? . . . H(29) C(23) H(28) 109.4760 ? . . . H(32) C(24) H(30) 109.4698 ? . . . H(31) C(24) H(30) 109.4730 ? . . . H(32) C(24) H(31) 109.4723 ? . . . #============================================================================== #===END #============================================================================== data_Complex_5 _database_code_depnum_ccdc_archive 'CCDC 250720' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C5 H25 Cl2 Cu N5 ' _chemical_formula_moiety 'C5 H25 Cl2 Cu N5 ' _chemical_formula_weight 289.74 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 14.0065(10) _cell_length_b 11.6044(11) _cell_length_c 8.5136(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1383.8(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2274 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612.00 _exptl_absorpt_coefficient_mu 1.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.824 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 7810 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_theta_max 48.76 _diffrn_measured_fraction_theta_max 0.1546 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.7004 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # 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 1158 _reflns_number_gt 1021 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0480 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1023 _refine_ls_number_parameters 70 _refine_ls_goodness_of_fit_ref 0.735 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.95 _refine_diff_density_min -0.47 _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 C C 0.003 0.002 ; 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) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; 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 Cu(1) Cu 0.13043(4) 0.2500 0.78432(7) 0.0194(2) Uani 1.00 2 d S . . Cl(1) Cl 0.35125(6) 0.01282(8) 0.65351(12) 0.0271(3) Uani 1.00 1 d . . . N(1) N 0.1307(2) 0.0754(3) 0.7816(3) 0.0242(9) Uani 1.00 1 d . . . N(2) N 0.2219(3) 0.2500 0.9998(5) 0.0242(12) Uani 1.00 2 d S . . N(3) N 0.2228(3) 0.2500 0.5947(5) 0.0264(13) Uani 1.00 2 d S . . N(4) N -0.0063(3) 0.2500 0.8781(5) 0.0245(12) Uani 1.00 2 d S . . C(1) C 0.0793(3) 0.0165(3) 0.6549(5) 0.0373(12) Uani 1.00 1 d . . . C(2) C 0.3242(4) 0.2500 0.9697(7) 0.030(2) Uani 1.00 2 d S . . C(3) C 0.1848(5) 0.2500 0.4312(6) 0.048(2) Uani 1.00 2 d S . . C(4) C -0.0102(4) 0.2500 1.0517(6) 0.033(2) Uani 1.00 2 d S . . H(1) H 0.1140 0.0361 0.5658 0.046 Uiso 1.00 1 c R . . H(2) H 0.0134 0.0625 0.6341 0.046 Uiso 1.00 1 c R . . H(3) H 0.0804 -0.0695 0.6691 0.046 Uiso 1.00 1 c R . . H(4) H 0.1059 0.0475 0.8754 0.029 Uiso 1.00 1 c R . . H(5) H 0.1868 0.0516 0.7846 0.029 Uiso 1.00 1 c R . . H(6) H 0.2031 0.3163 1.0543 0.029 Uiso 1.00 1 c R . . H(7) H 0.3599 0.2500 1.0572 0.036 Uiso 1.00 2 c R . . H(8) H 0.3417 0.1807 0.9091 0.037 Uiso 1.00 1 c R . . H(9) H -0.0382 0.1817 0.8470 0.029 Uiso 1.00 1 c R . . H(10) H -0.0750 0.2500 1.0850 0.040 Uiso 1.00 2 c R . . H(11) H 0.0197 0.3135 1.0850 0.040 Uiso 1.00 1 c R . . H(12) H 0.2604 0.3152 0.6098 0.032 Uiso 1.00 1 c R . . H(13) H 0.2305 0.2500 0.3699 0.060 Uiso 1.00 2 c R . . H(14) H 0.1454 0.1825 0.4125 0.060 Uiso 1.00 1 c R . . 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) 0.0231(4) 0.0155(4) 0.0196(4) 0.0000 0.0000(3) 0.0000 Cl(1) 0.0309(5) 0.0209(5) 0.0296(6) 0.0016(4) 0.0015(4) -0.0044(4) N(1) 0.031(2) 0.017(2) 0.024(2) -0.0004(13) 0.0061(13) -0.001(1) N(2) 0.030(2) 0.020(2) 0.023(3) 0.0000 -0.006(2) 0.0000 N(3) 0.032(3) 0.019(2) 0.028(3) 0.0000 0.005(2) 0.0000 N(4) 0.026(2) 0.014(2) 0.033(3) 0.0000 -0.000(2) 0.0000 C(1) 0.040(2) 0.031(2) 0.040(3) -0.007(2) 0.007(2) -0.016(2) C(2) 0.029(3) 0.030(3) 0.032(3) 0.0000 -0.010(3) 0.0000 C(3) 0.089(5) 0.040(4) 0.014(4) 0.0000 -0.001(3) 0.0000 C(4) 0.033(3) 0.032(3) 0.035(4) 0.0000 0.006(3) 0.0000 #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) N(1) 2.027(3) ? . . Cu(1) N(1) 2.027(3) ? . 55503 Cu(1) N(2) 2.238(4) ? . . Cu(1) N(2) 2.238(4) ? . 55503 Cu(1) N(3) 2.069(4) ? . . Cu(1) N(4) 2.074(4) ? . . N(1) C(1) 1.466(5) ? . . N(2) Cu(1) 2.238(4) ? . . N(2) Cu(1) 2.238(4) ? . 55503 N(2) C(2) 1.456(7) ? . . N(2) C(2) 1.456(7) ? . 55503 N(3) C(3) 1.490(7) ? . . N(4) C(4) 1.479(7) ? . . C(2) N(2) 1.456(7) ? . . C(2) N(2) 1.456(7) ? . 55503 N(1) H(4) 0.9287 ? . . N(1) H(5) 0.8333 ? . . N(2) H(6) 0.9363 ? . . N(2) H(6) 0.9363 ? . 55503 N(3) H(12) 0.9301 ? . . N(3) H(12) 0.9301 ? . 55503 N(4) H(9) 0.9478 ? . . N(4) H(9) 0.9478 ? . 55503 C(1) H(1) 0.9291 ? . . C(1) H(2) 1.0803 ? . . C(1) H(3) 1.0048 ? . . C(2) H(7) 0.8971 ? . . C(2) H(8) 0.9862 ? . . C(2) H(8) 0.9862 ? . 55503 C(3) H(13) 0.8254 ? . . C(3) H(14) 0.9716 ? . . C(3) H(14) 0.9716 ? . 55503 C(4) H(10) 0.9506 ? . . C(4) H(11) 0.8938 ? . . C(4) H(11) 0.8938 ? . 55503 H(6) N(2) 0.9363 ? . . H(6) N(2) 0.9363 ? . 55503 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Cu(1) N(1) 178.7(1) ? 55503 . . N(2) Cu(1) N(1) 90.48(8) ? . . . N(3) Cu(1) N(1) 89.44(8) ? . . . N(4) Cu(1) N(1) 90.34(8) ? . . . Cu(1) N(1) C(1) 118.3(2) ? . . . N(2) Cu(1) N(1) 90.48(8) ? . . 55503 N(3) Cu(1) N(1) 89.44(8) ? . . 55503 N(4) Cu(1) N(1) 90.34(8) ? . . 55503 Cu(1) N(1) C(1) 118.3(2) ? . 55503 55503 N(3) Cu(1) N(2) 106.4(2) ? . . . N(4) Cu(1) N(2) 102.3(2) ? . . . Cu(1) N(2) C(2) 114.8(3) ? . . . N(4) Cu(1) N(3) 151.3(2) ? . . . Cu(1) N(3) C(3) 120.4(4) ? . . . Cu(1) N(4) C(4) 114.8(3) ? . . . Cu(1) N(1) H(4) 109.7473 ? . . . Cu(1) N(1) H(5) 109.4367 ? . . . Cu(1) N(1) H(4) 109.7473 ? . 55503 55503 Cu(1) N(1) H(5) 109.4367 ? . 55503 55503 Cu(1) N(2) H(6) 104.1265 ? . . . Cu(1) N(2) H(6) 104.1265 ? . . 55503 Cu(1) N(3) H(12) 104.2383 ? . . . Cu(1) N(3) H(12) 104.2383 ? . . 55503 Cu(1) N(4) H(9) 109.1452 ? . . . Cu(1) N(4) H(9) 109.1452 ? . . 55503 N(1) C(1) H(1) 103.2508 ? . . . N(1) C(1) H(2) 108.0168 ? . . . H(4) N(1) C(1) 106.6729 ? . . . H(5) N(1) C(1) 109.3257 ? . . . N(1) C(1) H(3) 111.4602 ? . . . H(5) N(1) H(4) 102.1528 ? . . . H(6) N(2) C(2) 111.4317 ? . . . H(6) N(2) C(2) 111.4317 ? 55503 . . N(2) C(2) H(8) 109.6749 ? . . . N(2) C(2) H(8) 109.6749 ? . . 55503 N(2) C(2) H(7) 113.6313 ? . . . H(6) N(2) H(6) 110.5119 ? 55503 . . H(12) N(3) C(3) 109.3263 ? . . . H(12) N(3) C(3) 109.3263 ? 55503 . . N(3) C(3) H(14) 110.8861 ? . . . N(3) C(3) H(14) 110.8862 ? . . 55503 N(3) C(3) H(13) 108.3105 ? . . . H(12) N(3) H(12) 108.8041 ? 55503 . . H(9) N(4) C(4) 105.1339 ? . . . H(9) N(4) C(4) 105.1339 ? 55503 . . N(4) C(4) H(11) 107.4305 ? . . . N(4) C(4) H(11) 107.4305 ? . . 55503 N(4) C(4) H(10) 109.4522 ? . . . H(9) N(4) H(9) 113.5647 ? 55503 . . H(2) C(1) H(1) 101.0578 ? . . . H(3) C(1) H(1) 109.4716 ? . . . H(3) C(1) H(2) 121.6322 ? . . . H(8) C(2) H(7) 107.2414 ? . . . H(8) C(2) H(7) 107.2414 ? 55503 . . H(8) C(2) H(8) 109.2630 ? 55503 . . H(14) C(3) H(13) 109.6512 ? . . . H(14) C(3) H(13) 109.6512 ? 55503 . . H(14) C(3) H(14) 107.4480 ? 55503 . . H(11) C(4) H(10) 110.6456 ? . . . H(11) C(4) H(10) 110.6456 ? 55503 . . H(11) C(4) H(11) 111.1167 ? 55503 . . #============================================================================== #===END #==============================================================================