Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Tomoaki Tanase' 'Ajay Sah' _publ_contact_author_name 'Tomoaki Tanase' _publ_contact_author_address ; Department of Chemistry Nara Women's University Kitauoya-higashi-machi Nara 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_requested_journal 'Dalton Transactions' _publ_section_title ; Amine mediated proton transfer reaction and C-Cl bond activation of solvent chloroform by trinuclear copper(II) complex of a glucopyranosylamine derived ligand ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #============================================================================== #===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 #============================================================================== #============================================================================= data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 286668' #============================================================================= # CHEMICAL DATA _chemical_formula_sum 'C47 H79 Cl3 Cu3 N4 O16 ' _chemical_formula_moiety '[Cu3(L1)2(EtNH2)2(MeOH)2].2MeOH.CHCl3 ' _chemical_formula_weight 1253.16 _chemical_melting_point ? #============================================================================= # 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 8.0925(5) _cell_length_b 12.2513(11) _cell_length_c 14.9817(11) _cell_angle_alpha 91.958(4) _cell_angle_beta 98.528(3) _cell_angle_gamma 96.609(4) _cell_volume 1457.17(19) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3781 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 655.00 _exptl_absorpt_coefficient_mu 1.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.773 #============================================================================= # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 13283 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.900 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 #============================================================================= # 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 5908 _reflns_number_gt 5693 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1070 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5141 _refine_ls_number_parameters 661 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0657P)^2^+1.0710P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0218 _refine_diff_density_max 0.71 _refine_diff_density_min -0.72 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.08(2) 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) ; 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 0.82434(6) 0.66638(4) 0.09136(4) 0.0229(2) Uani 1.00 1 d . . . CU(2) Cu 0.66183(9) 0.89996(6) 0.20388(5) 0.02200(15) Uani 1.00 1 d . . . CU(3) Cu 0.51057(6) 1.13769(4) 0.31927(4) 0.0255(2) Uani 1.00 1 d . . . CL(1) Cl 1.1642(4) 0.9274(2) -0.3264(2) 0.1059(11) Uani 1.00 1 d . . . CL(2) Cl 1.2368(4) 0.8503(4) -0.50199(19) 0.1289(16) Uani 1.00 1 d . . . CL(3) Cl 1.2220(3) 0.7062(2) -0.35671(17) 0.0726(5) Uani 1.00 1 d . . . O(1) O 0.8788(5) 0.5630(3) 0.0044(2) 0.0322(9) Uani 1.00 1 d . . . O(2) O 0.7754(4) 0.7697(3) 0.1871(2) 0.0243(7) Uani 1.00 1 d . . . O(3) O 0.6400(4) 0.8549(3) 0.3242(2) 0.0249(7) Uani 1.00 1 d . . . O(4) O 0.7302(5) 0.7540(3) 0.5043(2) 0.0262(8) Uani 1.00 1 d . . . O(5) O 0.8359(4) 0.5510(3) 0.3423(2) 0.0244(7) Uani 1.00 1 d . . . O(6) O 0.7980(5) 0.5965(3) 0.5787(2) 0.0327(9) Uani 1.00 1 d . . . O(7) O 0.4371(5) 1.2334(3) 0.4046(2) 0.0319(9) Uani 1.00 1 d . . . O(8) O 0.5996(5) 1.0463(3) 0.2286(2) 0.0263(8) Uani 1.00 1 d . . . O(9) O 0.6224(4) 0.9251(2) 0.0762(2) 0.0254(7) Uani 1.00 1 d . . . O(10) O 0.6060(5) 1.0501(3) -0.0936(2) 0.0275(8) Uani 1.00 1 d . . . O(11) O 0.4504(5) 1.2373(3) 0.0635(2) 0.0286(8) Uani 1.00 1 d . . . O(12) O 0.5048(6) 1.1959(3) -0.1726(2) 0.0356(10) Uani 1.00 1 d . . . O(13) O 0.5277(5) 0.6103(3) 0.0640(2) 0.0364(8) Uani 1.00 1 d . . . O(14) O 0.2521(5) 1.0223(4) 0.2915(4) 0.0624(15) Uani 1.00 1 d . . . O(15) O 0.3891(4) 0.7817(3) -0.0155(2) 0.0344(8) Uani 1.00 1 d . . . O(16) O 0.3038(5) 0.8071(3) 0.2893(2) 0.0389(9) Uani 1.00 1 d . . . N(1) N 0.8818(5) 0.5700(4) 0.1891(3) 0.0227(9) Uani 1.00 1 d . . . N(2) N 0.4794(6) 1.2413(4) 0.2245(3) 0.0287(11) Uani 1.00 1 d . . . N(3) N 0.8229(5) 0.7805(3) 0.0000(2) 0.0265(9) Uani 1.00 1 d . . . N(4) N 0.5989(7) 1.0507(4) 0.4194(3) 0.0398(12) Uani 1.00 1 d . . . C(1) C 0.8781(6) 0.6250(4) 0.2757(3) 0.0225(9) Uani 1.00 1 d . . . C(2) C 0.7477(6) 0.7043(4) 0.2602(3) 0.0232(11) Uani 1.00 1 d . . . C(3) C 0.7518(6) 0.7762(4) 0.3441(3) 0.0230(11) Uani 1.00 1 d . . . C(4) C 0.7134(6) 0.6989(4) 0.4167(3) 0.0215(9) Uani 1.00 1 d . . . C(5) C 0.8401(6) 0.6125(4) 0.4246(3) 0.0241(11) Uani 1.00 1 d . . . C(6) C 0.7968(7) 0.5341(4) 0.4969(3) 0.0314(11) Uani 1.00 1 d . . . C(7) C 0.6840(6) 0.6770(4) 0.5685(3) 0.0301(11) Uani 1.00 1 d . . . C(8) C 0.6958(9) 0.7397(5) 0.6576(4) 0.0387(14) Uani 1.00 1 d . . . C(9) C 0.9256(7) 0.4739(5) 0.1830(4) 0.0242(12) Uani 1.00 1 d . . . C(10) C 0.9455(6) 0.4148(4) 0.1008(3) 0.0247(11) Uani 1.00 1 d . . . C(11) C 0.9178(6) 0.4645(4) 0.0142(3) 0.0237(11) Uani 1.00 1 d . . . C(12) C 0.9398(6) 0.3980(5) -0.0650(4) 0.0286(12) Uani 1.00 1 d . . . C(13) C 0.9878(7) 0.2944(5) -0.0524(4) 0.0331(12) Uani 1.00 1 d . . . C(14) C 1.0186(8) 0.2501(5) 0.0332(4) 0.0339(13) Uani 1.00 1 d . . . C(15) C 0.9966(7) 0.3109(5) 0.1073(4) 0.0279(12) Uani 1.00 1 d . . . C(16) C 0.9117(7) 0.4446(5) -0.1584(3) 0.0338(13) Uani 1.00 1 d . . . C(17) C 1.0415(9) 0.5457(6) -0.1631(4) 0.0472(16) Uani 1.00 1 d . . . C(18) C 0.7324(8) 0.4765(5) -0.1812(4) 0.0362(13) Uani 1.00 1 d . . . C(19) C 0.9313(8) 0.3600(6) -0.2329(4) 0.0429(14) Uani 1.00 1 d . . . C(20) C 0.5429(6) 1.2060(4) 0.1439(3) 0.0244(10) Uani 1.00 1 d . . . C(21) C 0.5321(7) 1.0820(4) 0.1437(3) 0.0233(11) Uani 1.00 1 d . . . C(22) C 0.6227(6) 1.0400(4) 0.0695(3) 0.0230(11) Uani 1.00 1 d . . . C(23) C 0.5284(6) 1.0770(4) -0.0163(3) 0.0243(10) Uani 1.00 1 d . . . C(24) C 0.5250(7) 1.2021(4) -0.0125(3) 0.0239(11) Uani 1.00 1 d . . . C(25) C 0.4269(8) 1.2344(4) -0.0985(4) 0.0351(12) Uani 1.00 1 d . . . C(26) C 0.5118(7) 1.0811(4) -0.1736(3) 0.0334(11) Uani 1.00 1 d . . . C(27) C 0.5978(11) 1.0523(6) -0.2514(4) 0.0483(18) Uani 1.00 1 d . . . C(28) C 0.4224(7) 1.3359(4) 0.2310(4) 0.0259(12) Uani 1.00 1 d . . . C(29) C 0.3737(6) 1.3814(4) 0.3100(3) 0.0246(11) Uani 1.00 1 d . . . C(30) C 0.3838(6) 1.3309(4) 0.3941(4) 0.0252(11) Uani 1.00 1 d . . . C(31) C 0.3381(6) 1.3887(4) 0.4697(4) 0.0273(12) Uani 1.00 1 d . . . C(32) C 0.2831(6) 1.4907(4) 0.4577(3) 0.0278(11) Uani 1.00 1 d . . . C(33) C 0.2759(7) 1.5428(5) 0.3748(4) 0.0293(12) Uani 1.00 1 d . . . C(34) C 0.3196(7) 1.4883(5) 0.3014(4) 0.0268(12) Uani 1.00 1 d . . . C(35) C 0.3514(7) 1.3362(4) 0.5636(4) 0.0323(12) Uani 1.00 1 d . . . C(36) C 0.2275(10) 1.2319(6) 0.5578(5) 0.0544(19) Uani 1.00 1 d . . . C(37) C 0.5304(8) 1.3154(5) 0.5962(4) 0.0381(14) Uani 1.00 1 d . . . C(38) C 0.3034(9) 1.4158(5) 0.6362(4) 0.0439(15) Uani 1.00 1 d . . . C(39) C 0.9869(7) 0.8439(5) -0.0054(4) 0.0413(13) Uani 1.00 1 d . . . C(40) C 0.9784(9) 0.9200(6) -0.0854(5) 0.0556(18) Uani 1.00 1 d . . . C(41) C 0.4569(8) 0.5098(5) 0.0169(4) 0.0432(14) Uani 1.00 1 d . . . C(42) C 0.7691(9) 1.1002(5) 0.4666(5) 0.0482(15) Uani 1.00 1 d . . . C(43) C 0.8260(12) 1.0404(8) 0.5471(6) 0.075(2) Uani 1.00 1 d . . . C(44) C 0.0919(11) 1.0484(8) 0.2841(10) 0.092(3) Uani 1.00 1 d . . . C(45) C 0.3891(8) 0.7824(5) -0.1093(4) 0.0433(14) Uani 1.00 1 d . . . C(46) C 0.2725(8) 0.7722(5) 0.1967(4) 0.0435(14) Uani 1.00 1 d . . . C(47) C 1.1424(8) 0.8195(6) -0.4081(4) 0.0513(16) Uani 1.00 1 d . . . H(1) H 0.4183 1.3777 0.1800 0.030 Uiso 1.00 1 c R . . H(2) H 0.9500 0.4366 0.2386 0.029 Uiso 1.00 1 c R . . H(3) H 0.3133 1.5228 0.2453 0.033 Uiso 1.00 1 c R . . H(4) H 0.2465 1.6153 0.3694 0.034 Uiso 1.00 1 c R . . H(5) H 0.2503 1.5296 0.5070 0.034 Uiso 1.00 1 c R . . H(6) H 1.0204 0.2826 0.1650 0.036 Uiso 1.00 1 c R . . H(7) H 1.0537 0.1793 0.0379 0.044 Uiso 1.00 1 c R . . H(8) H 1.0039 0.2544 -0.1047 0.041 Uiso 1.00 1 c R . . H(9) H 0.6583 1.2365 0.1480 0.030 Uiso 1.00 1 c R . . H(10) H 0.4189 1.0520 0.1311 0.028 Uiso 1.00 1 c R . . H(11) H 0.7371 1.0755 0.0791 0.029 Uiso 1.00 1 c R . . H(12) H 0.4183 1.0425 -0.0243 0.029 Uiso 1.00 1 c R . . H(13) H 0.6383 1.2382 -0.0074 0.031 Uiso 1.00 1 c R . . H(14) H 0.4028 1.0442 -0.1801 0.040 Uiso 1.00 1 c R . . H(15) H 0.9881 0.6655 0.2973 0.028 Uiso 1.00 1 c R . . H(16) H 0.6427 0.6636 0.2466 0.027 Uiso 1.00 1 c R . . H(17) H 0.8630 0.8142 0.3618 0.027 Uiso 1.00 1 c R . . H(18) H 0.6047 0.6627 0.4023 0.028 Uiso 1.00 1 c R . . H(19) H 0.9512 0.6498 0.4429 0.030 Uiso 1.00 1 c R . . H(20) H 0.5736 0.6431 0.5497 0.037 Uiso 1.00 1 c R . . H(21) H 0.4283 1.3113 -0.0989 0.041 Uiso 1.00 1 c R . . H(22) H 0.3151 1.1993 -0.1053 0.041 Uiso 1.00 1 c R . . H(23) H 0.8818 0.4853 0.5051 0.040 Uiso 1.00 1 c R . . H(24) H 0.6918 0.4959 0.4787 0.040 Uiso 1.00 1 c R . . H(25) H 0.6034 0.9743 -0.2553 0.054 Uiso 1.00 1 c R . . H(26) H 0.5386 1.0730 -0.3061 0.054 Uiso 1.00 1 c R . . H(27) H 0.7113 1.0885 -0.2435 0.054 Uiso 1.00 1 c R . . H(28) H 0.8087 0.7734 0.6763 0.047 Uiso 1.00 1 c R . . H(29) H 0.6224 0.7946 0.6521 0.047 Uiso 1.00 1 c R . . H(30) H 0.6658 0.6902 0.7017 0.047 Uiso 1.00 1 c R . . H(31) H 0.3793 1.4841 0.6411 0.054 Uiso 1.00 1 c R . . H(32) H 0.1929 1.4320 0.6197 0.054 Uiso 1.00 1 c R . . H(33) H 0.3163 1.3844 0.6934 0.054 Uiso 1.00 1 c R . . H(34) H 0.1211 1.2478 0.5424 0.063 Uiso 1.00 1 c R . . H(35) H 0.2598 1.1820 0.5147 0.063 Uiso 1.00 1 c R . . H(36) H 0.2448 1.2003 0.6160 0.063 Uiso 1.00 1 c R . . H(37) H 0.5404 1.2827 0.6530 0.043 Uiso 1.00 1 c R . . H(38) H 0.5689 1.2678 0.5535 0.043 Uiso 1.00 1 c R . . H(39) H 0.6065 1.3834 0.6027 0.043 Uiso 1.00 1 c R . . H(40) H 1.1531 0.5225 -0.1507 0.058 Uiso 1.00 1 c R . . H(41) H 1.0268 0.5732 -0.2209 0.058 Uiso 1.00 1 c R . . H(42) H 1.0321 0.5995 -0.1184 0.058 Uiso 1.00 1 c R . . H(43) H 0.7166 0.5315 -0.1374 0.042 Uiso 1.00 1 c R . . H(44) H 0.7179 0.5053 -0.2393 0.042 Uiso 1.00 1 c R . . H(45) H 0.6547 0.4137 -0.1792 0.042 Uiso 1.00 1 c R . . H(46) H 0.8525 0.2977 -0.2321 0.052 Uiso 1.00 1 c R . . H(47) H 0.9185 0.3912 -0.2898 0.052 Uiso 1.00 1 c R . . H(48) H 1.0437 0.3380 -0.2208 0.052 Uiso 1.00 1 c R . . H(49) H 0.8504 1.0974 0.4272 0.063 Uiso 1.00 1 c R . . H(50) H 0.7665 1.1738 0.4869 0.063 Uiso 1.00 1 c R . . H(51) H 1.0251 0.8870 0.0505 0.049 Uiso 1.00 1 c R . . H(52) H 1.0673 0.7930 -0.0111 0.049 Uiso 1.00 1 c R . . H(53) H 0.7498 1.0435 0.5881 0.087 Uiso 1.00 1 c R . . H(54) H 0.8303 0.9655 0.5281 0.087 Uiso 1.00 1 c R . . H(55) H 0.9353 1.0721 0.5736 0.087 Uiso 1.00 1 c R . . H(56) H 1.0899 0.9593 -0.0854 0.067 Uiso 1.00 1 c R . . H(57) H 0.9467 0.8776 -0.1398 0.067 Uiso 1.00 1 c R . . H(58) H 0.9034 0.9714 -0.0784 0.067 Uiso 1.00 1 c R . . H(59) H 0.5525 1.0422 0.4737 0.063 Uiso 1.00 1 c R . . H(60) H 0.5921 0.9772 0.3995 0.063 Uiso 1.00 1 c R . . H(61) H 0.7588 0.8206 0.0131 0.063 Uiso 1.00 1 c R . . H(62) H 0.7635 0.7653 -0.0657 0.063 Uiso 1.00 1 c R . . H(63) H 1.0279 0.7979 -0.4275 0.063 Uiso 1.00 1 c R . . H(64) H 0.2529 0.9422 0.3023 0.063 Uiso 1.00 1 c R . . H(65) H 0.4194 0.8142 0.3000 0.063 Uiso 1.00 1 c R . . H(66) H 0.4548 0.6632 0.0400 0.063 Uiso 1.00 1 c R . . H(67) H 0.0943 1.1262 0.2764 0.117 Uiso 1.00 1 c R . . H(68) H 0.0254 1.0088 0.2357 0.117 Uiso 1.00 1 c R . . H(69) H 0.0495 1.0330 0.3394 0.117 Uiso 1.00 1 c R . . H(70) H 0.3484 0.4903 0.0283 0.054 Uiso 1.00 1 c R . . H(71) H 0.4592 0.5168 -0.0461 0.054 Uiso 1.00 1 c R . . H(72) H 0.5267 0.4531 0.0366 0.054 Uiso 1.00 1 c R . . H(73) H 0.1577 0.7623 0.1769 0.052 Uiso 1.00 1 c R . . H(74) H 0.3267 0.8283 0.1631 0.052 Uiso 1.00 1 c R . . H(75) H 0.3215 0.7064 0.1884 0.052 Uiso 1.00 1 c R . . H(76) H 0.4690 0.8414 0.0200 0.063 Uiso 1.00 1 c R . . H(77) H 0.5026 0.7739 -0.1217 0.054 Uiso 1.00 1 c R . . H(78) H 0.3150 0.7236 -0.1389 0.054 Uiso 1.00 1 c R . . H(79) H 0.3616 0.8504 -0.1313 0.054 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) 0.0295(3) 0.0222(3) 0.0181(3) 0.0065(2) 0.0042(2) 0.0024(2) CU(2) 0.0285(2) 0.0206(2) 0.0175(2) 0.00680(19) 0.00214(19) 0.00306(17) CU(3) 0.0377(4) 0.0198(3) 0.0199(3) 0.0077(2) 0.0041(2) 0.0012(2) CL(1) 0.144(2) 0.0642(15) 0.0903(19) 0.0148(15) -0.0388(18) -0.0336(12) CL(2) 0.0868(18) 0.227(4) 0.0585(14) -0.055(2) 0.0129(12) 0.0436(19) CL(3) 0.0725(13) 0.0767(14) 0.0697(13) 0.0171(10) 0.0081(10) 0.0010(10) O(1) 0.047(2) 0.027(2) 0.024(2) 0.0091(18) 0.0065(18) 0.0017(18) O(2) 0.0344(19) 0.0223(17) 0.0176(17) 0.0081(14) 0.0044(14) 0.0043(14) O(3) 0.036(2) 0.0229(18) 0.0182(17) 0.0130(15) 0.0030(14) 0.0030(13) O(4) 0.034(2) 0.025(2) 0.0195(19) 0.0035(16) 0.0055(15) 0.0029(16) O(5) 0.0355(19) 0.0199(17) 0.0190(17) 0.0063(14) 0.0044(14) 0.0055(14) O(6) 0.045(2) 0.033(2) 0.021(2) 0.0096(18) 0.0058(17) 0.0083(16) O(7) 0.057(2) 0.0193(19) 0.022(2) 0.0099(18) 0.0112(18) 0.0025(16) O(8) 0.039(2) 0.0227(19) 0.0187(17) 0.0102(15) 0.0027(15) 0.0033(14) O(9) 0.036(2) 0.0203(18) 0.0213(18) 0.0074(15) 0.0049(15) 0.0026(13) O(10) 0.041(2) 0.027(2) 0.0160(19) 0.0088(16) 0.0066(16) 0.0031(16) O(11) 0.040(2) 0.0242(19) 0.0248(19) 0.0120(16) 0.0090(16) 0.0045(15) O(12) 0.061(2) 0.031(2) 0.0177(19) 0.0113(19) 0.0105(18) 0.0040(16) O(13) 0.0325(19) 0.031(2) 0.044(2) 0.0065(16) -0.0022(16) -0.0029(16) O(14) 0.037(2) 0.038(2) 0.113(4) 0.004(2) 0.017(2) -0.004(2) O(15) 0.0329(19) 0.032(2) 0.036(2) 0.0014(15) -0.0007(15) 0.0049(16) O(16) 0.036(2) 0.046(2) 0.036(2) 0.0069(17) 0.0104(17) 0.0087(18) N(1) 0.024(2) 0.022(2) 0.023(2) 0.0061(17) 0.0037(17) -0.0012(18) N(2) 0.038(2) 0.025(2) 0.024(2) 0.005(2) 0.008(2) -0.005(2) N(3) 0.025(2) 0.032(2) 0.024(2) 0.0070(18) 0.0060(17) 0.0073(18) N(4) 0.057(3) 0.039(2) 0.026(2) 0.022(2) 0.004(2) 0.002(2) C(1) 0.030(2) 0.022(2) 0.016(2) 0.0030(19) 0.0022(18) 0.0030(18) C(2) 0.023(2) 0.027(2) 0.019(2) 0.002(2) 0.0004(19) 0.003(2) C(3) 0.026(2) 0.024(2) 0.019(2) 0.005(2) 0.0010(19) 0.001(2) C(4) 0.021(2) 0.022(2) 0.022(2) 0.0039(18) 0.0032(18) 0.0011(18) C(5) 0.026(2) 0.024(2) 0.022(2) 0.001(2) 0.0028(19) 0.005(2) C(6) 0.040(3) 0.029(2) 0.027(2) 0.007(2) 0.009(2) 0.007(2) C(7) 0.034(2) 0.035(2) 0.023(2) 0.003(2) 0.009(2) 0.006(2) C(8) 0.055(3) 0.041(3) 0.024(3) 0.010(2) 0.013(2) 0.006(2) C(9) 0.024(2) 0.029(3) 0.019(2) 0.004(2) -0.001(2) 0.001(2) C(10) 0.023(2) 0.031(3) 0.019(2) 0.002(2) 0.000(2) 0.000(2) C(11) 0.021(2) 0.026(2) 0.025(2) 0.0053(19) 0.0078(19) -0.006(2) C(12) 0.022(2) 0.033(3) 0.032(2) 0.004(2) 0.009(2) -0.002(2) C(13) 0.027(2) 0.034(3) 0.039(3) 0.008(2) 0.009(2) -0.013(2) C(14) 0.032(3) 0.033(3) 0.037(3) 0.013(2) 0.001(2) 0.000(2) C(15) 0.023(2) 0.029(3) 0.031(3) 0.010(2) -0.001(2) -0.004(2) C(16) 0.042(3) 0.034(3) 0.026(2) -0.002(2) 0.012(2) -0.004(2) C(17) 0.052(3) 0.057(4) 0.031(3) -0.014(3) 0.017(2) -0.002(2) C(18) 0.041(3) 0.040(3) 0.025(2) 0.004(2) -0.001(2) -0.001(2) C(19) 0.044(3) 0.055(3) 0.032(3) 0.009(2) 0.012(2) -0.001(2) C(20) 0.031(2) 0.020(2) 0.023(2) 0.0004(19) 0.007(2) 0.0013(18) C(21) 0.030(2) 0.022(2) 0.018(2) 0.007(2) 0.001(2) 0.003(2) C(22) 0.026(2) 0.018(2) 0.026(2) 0.0057(19) 0.006(2) -0.001(2) C(23) 0.028(2) 0.023(2) 0.023(2) 0.0030(19) 0.007(2) 0.0015(18) C(24) 0.032(2) 0.021(2) 0.021(2) 0.007(2) 0.008(2) 0.0023(19) C(25) 0.049(3) 0.031(2) 0.030(2) 0.016(2) 0.011(2) 0.005(2) C(26) 0.048(3) 0.029(2) 0.023(2) 0.008(2) 0.003(2) 0.004(2) C(27) 0.081(5) 0.046(4) 0.021(3) 0.014(3) 0.014(3) 0.001(2) C(28) 0.034(2) 0.018(2) 0.027(3) 0.007(2) 0.003(2) 0.002(2) C(29) 0.029(2) 0.019(2) 0.027(2) 0.006(2) 0.004(2) -0.002(2) C(30) 0.025(2) 0.025(2) 0.024(2) 0.001(2) 0.000(2) 0.006(2) C(31) 0.019(2) 0.025(2) 0.036(3) -0.0004(19) 0.002(2) 0.006(2) C(32) 0.020(2) 0.034(2) 0.028(2) 0.003(2) 0.002(2) -0.006(2) C(33) 0.028(2) 0.028(2) 0.033(3) 0.011(2) 0.003(2) -0.007(2) C(34) 0.030(2) 0.025(3) 0.026(3) 0.007(2) 0.001(2) 0.003(2) C(35) 0.043(3) 0.028(2) 0.029(2) 0.002(2) 0.017(2) 0.003(2) C(36) 0.067(4) 0.042(3) 0.053(4) -0.014(3) 0.022(3) 0.008(3) C(37) 0.056(3) 0.037(3) 0.024(2) 0.017(2) 0.006(2) 0.004(2) C(38) 0.063(4) 0.041(3) 0.035(3) 0.016(3) 0.025(3) -0.000(2) C(39) 0.029(2) 0.048(3) 0.049(3) 0.005(2) 0.010(2) 0.019(2) C(40) 0.043(3) 0.064(4) 0.064(4) 0.005(3) 0.016(3) 0.033(3) C(41) 0.055(3) 0.034(3) 0.037(3) -0.004(2) 0.004(2) 0.001(2) C(42) 0.046(3) 0.044(3) 0.053(4) 0.004(2) 0.006(2) 0.004(2) C(43) 0.072(5) 0.074(5) 0.066(5) -0.006(4) -0.021(4) 0.014(4) C(44) 0.048(4) 0.053(5) 0.179(12) 0.011(3) 0.022(5) 0.007(6) C(45) 0.050(3) 0.039(3) 0.036(3) -0.005(2) -0.002(2) 0.003(2) C(46) 0.041(3) 0.047(3) 0.038(3) -0.002(2) -0.002(2) 0.009(2) C(47) 0.043(3) 0.064(4) 0.042(3) -0.010(3) 0.005(2) -0.012(3) #============================================================================= _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.7.0' _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) 1.919(4) ? . . CU(1) O(2) 1.994(3) ? . . CU(1) O(13) 2.390(3) ? . . CU(1) N(1) 1.949(5) ? . . CU(1) N(3) 1.989(4) ? . . CU(2) O(2) 1.958(4) ? . . CU(2) O(3) 1.931(3) ? . . CU(2) O(8) 1.956(4) ? . . CU(2) O(9) 1.933(3) ? . . CU(3) O(7) 1.910(4) ? . . CU(3) O(8) 1.997(4) ? . . CU(3) O(14) 2.360(4) ? . . CU(3) N(2) 1.944(5) ? . . CU(3) N(4) 1.965(5) ? . . CL(1) C(47) 1.746(8) ? . . CL(2) C(47) 1.730(8) ? . . CL(3) C(47) 1.751(8) ? . . O(1) C(11) 1.290(7) ? . . O(2) C(2) 1.408(6) ? . . O(3) C(3) 1.406(7) ? . . O(4) C(4) 1.436(6) ? . . O(4) C(7) 1.429(6) ? . . O(5) C(1) 1.423(6) ? . . O(5) C(5) 1.417(6) ? . . O(6) C(6) 1.420(7) ? . . O(6) C(7) 1.423(7) ? . . O(7) C(30) 1.322(7) ? . . O(8) C(21) 1.412(6) ? . . O(9) C(22) 1.416(6) ? . . O(10) C(23) 1.443(6) ? . . O(10) C(26) 1.410(6) ? . . O(11) C(20) 1.411(6) ? . . O(11) C(24) 1.441(7) ? . . O(12) C(25) 1.445(8) ? . . O(12) C(26) 1.414(7) ? . . O(13) C(41) 1.415(7) ? . . O(14) C(44) 1.360(11) ? . . O(15) C(45) 1.406(7) ? . . O(16) C(46) 1.415(7) ? . . N(1) C(1) 1.447(6) ? . . N(1) C(9) 1.273(8) ? . . N(2) C(20) 1.452(7) ? . . N(2) C(28) 1.301(8) ? . . N(3) C(39) 1.473(7) ? . . N(4) C(42) 1.502(8) ? . . C(1) C(2) 1.514(7) ? . . C(2) C(3) 1.503(7) ? . . C(3) C(4) 1.510(7) ? . . C(4) C(5) 1.552(7) ? . . C(5) C(6) 1.524(8) ? . . C(7) C(8) 1.502(8) ? . . C(9) C(10) 1.445(8) ? . . C(10) C(11) 1.450(8) ? . . C(10) C(15) 1.385(8) ? . . C(11) C(12) 1.461(8) ? . . C(12) C(13) 1.380(9) ? . . C(12) C(16) 1.526(8) ? . . C(13) C(14) 1.408(9) ? . . C(14) C(15) 1.361(9) ? . . C(16) C(17) 1.539(9) ? . . C(16) C(18) 1.538(9) ? . . C(16) C(19) 1.535(9) ? . . C(20) C(21) 1.511(7) ? . . C(21) C(22) 1.526(8) ? . . C(22) C(23) 1.506(7) ? . . C(23) C(24) 1.535(7) ? . . C(24) C(25) 1.501(8) ? . . C(26) C(27) 1.496(10) ? . . C(28) C(29) 1.417(8) ? . . C(29) C(30) 1.420(8) ? . . C(29) C(34) 1.432(8) ? . . C(30) C(31) 1.431(8) ? . . C(31) C(32) 1.382(8) ? . . C(31) C(35) 1.561(8) ? . . C(32) C(33) 1.412(8) ? . . C(33) C(34) 1.378(9) ? . . C(35) C(36) 1.523(9) ? . . C(35) C(37) 1.512(9) ? . . C(35) C(38) 1.557(9) ? . . C(39) C(40) 1.542(10) ? . . C(42) C(43) 1.475(12) ? . . O(13) H(66) 0.969 ? . . O(14) H(64) 1.000 ? . . O(15) H(76) 0.999 ? . . O(16) H(65) 0.919 ? . . N(3) H(61) 0.795 ? . . N(3) H(62) 1.031 ? . . N(4) H(59) 0.949 ? . . N(4) H(60) 0.931 ? . . C(1) H(15) 0.973 ? . . C(2) H(16) 0.925 ? . . C(3) H(17) 0.960 ? . . C(4) H(18) 0.930 ? . . C(5) H(19) 0.957 ? . . C(6) H(23) 0.959 ? . . C(6) H(24) 0.920 ? . . C(7) H(20) 0.939 ? . . C(8) H(28) 0.955 ? . . C(8) H(29) 0.946 ? . . C(8) H(30) 0.951 ? . . C(9) H(2) 0.970 ? . . C(13) H(8) 0.944 ? . . C(14) H(7) 0.945 ? . . C(15) H(6) 0.944 ? . . C(17) H(40) 0.972 ? . . C(17) H(41) 0.935 ? . . C(17) H(42) 0.941 ? . . C(18) H(43) 0.957 ? . . C(18) H(44) 0.948 ? . . C(18) H(45) 0.940 ? . . C(19) H(46) 0.938 ? . . C(19) H(47) 0.943 ? . . C(19) H(48) 0.971 ? . . C(20) H(9) 0.957 ? . . C(21) H(10) 0.936 ? . . C(22) H(11) 0.964 ? . . C(23) H(12) 0.930 ? . . C(24) H(13) 0.962 ? . . C(25) H(21) 0.942 ? . . C(25) H(22) 0.946 ? . . C(26) H(14) 0.933 ? . . C(27) H(25) 0.962 ? . . C(27) H(26) 0.944 ? . . C(27) H(27) 0.961 ? . . C(28) H(1) 0.934 ? . . C(32) H(5) 0.953 ? . . C(33) H(4) 0.948 ? . . C(34) H(3) 0.952 ? . . C(36) H(34) 0.904 ? . . C(36) H(35) 0.959 ? . . C(36) H(36) 0.963 ? . . C(37) H(37) 0.950 ? . . C(37) H(38) 0.960 ? . . C(37) H(39) 0.970 ? . . C(38) H(31) 0.974 ? . . C(38) H(32) 0.937 ? . . C(38) H(33) 0.948 ? . . C(39) H(51) 0.965 ? . . C(39) H(52) 0.961 ? . . C(40) H(56) 0.973 ? . . C(40) H(57) 0.937 ? . . C(40) H(58) 0.938 ? . . C(41) H(70) 0.925 ? . . C(41) H(71) 0.953 ? . . C(41) H(72) 0.971 ? . . C(42) H(49) 0.950 ? . . C(42) H(50) 0.946 ? . . C(43) H(53) 0.935 ? . . C(43) H(54) 0.958 ? . . C(43) H(55) 0.947 ? . . C(44) H(67) 0.962 ? . . C(44) H(68) 0.922 ? . . C(44) H(69) 0.961 ? . . C(45) H(77) 0.980 ? . . C(45) H(78) 0.935 ? . . C(45) H(79) 0.944 ? . . C(46) H(73) 0.925 ? . . C(46) H(74) 0.968 ? . . C(46) H(75) 0.951 ? . . C(47) H(63) 0.933 ? . . 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(1) CU(1) O(2) 176.81(17) ? . . . O(1) CU(1) O(13) 95.68(16) ? . . . O(1) CU(1) N(1) 91.2(2) ? . . . O(1) CU(1) N(3) 89.62(19) ? . . . O(2) CU(1) O(13) 85.80(14) ? . . . O(2) CU(1) N(1) 85.82(18) ? . . . O(2) CU(1) N(3) 93.05(17) ? . . . O(13) CU(1) N(1) 97.74(17) ? . . . O(13) CU(1) N(3) 95.88(16) ? . . . N(1) CU(1) N(3) 166.21(18) ? . . . O(2) CU(2) O(3) 88.00(16) ? . . . O(2) CU(2) O(8) 167.19(15) ? . . . O(2) CU(2) O(9) 93.74(16) ? . . . O(3) CU(2) O(8) 92.83(16) ? . . . O(3) CU(2) O(9) 164.50(15) ? . . . O(8) CU(2) O(9) 88.87(16) ? . . . O(7) CU(3) O(8) 175.94(17) ? . . . O(7) CU(3) O(14) 94.1(2) ? . . . O(7) CU(3) N(2) 92.0(2) ? . . . O(7) CU(3) N(4) 89.1(2) ? . . . O(8) CU(3) O(14) 89.65(18) ? . . . O(8) CU(3) N(2) 85.7(2) ? . . . O(8) CU(3) N(4) 92.3(2) ? . . . O(14) CU(3) N(2) 101.6(2) ? . . . O(14) CU(3) N(4) 92.3(2) ? . . . N(2) CU(3) N(4) 166.0(2) ? . . . CU(1) O(1) C(11) 129.8(3) ? . . . CU(1) O(2) CU(2) 141.89(19) ? . . . CU(1) O(2) C(2) 105.4(3) ? . . . CU(2) O(2) C(2) 105.5(3) ? . . . CU(2) O(3) C(3) 106.6(3) ? . . . C(4) O(4) C(7) 109.7(3) ? . . . C(1) O(5) C(5) 108.5(3) ? . . . C(6) O(6) C(7) 112.4(4) ? . . . CU(3) O(7) C(30) 129.9(3) ? . . . CU(2) O(8) CU(3) 143.3(2) ? . . . CU(2) O(8) C(21) 105.4(3) ? . . . CU(3) O(8) C(21) 105.1(3) ? . . . CU(2) O(9) C(22) 106.2(3) ? . . . C(23) O(10) C(26) 110.4(4) ? . . . C(20) O(11) C(24) 109.2(4) ? . . . C(25) O(12) C(26) 112.4(4) ? . . . CU(1) O(13) C(41) 122.3(3) ? . . . CU(3) O(14) C(44) 129.8(4) ? . . . CU(1) N(1) C(1) 110.5(3) ? . . . CU(1) N(1) C(9) 127.7(4) ? . . . C(1) N(1) C(9) 121.7(4) ? . . . CU(3) N(2) C(20) 111.7(3) ? . . . CU(3) N(2) C(28) 126.6(4) ? . . . C(20) N(2) C(28) 121.5(5) ? . . . CU(1) N(3) C(39) 115.9(3) ? . . . CU(3) N(4) C(42) 112.6(4) ? . . . O(5) C(1) N(1) 113.0(4) ? . . . O(5) C(1) C(2) 109.5(4) ? . . . N(1) C(1) C(2) 106.8(4) ? . . . O(2) C(2) C(1) 110.5(4) ? . . . O(2) C(2) C(3) 110.1(4) ? . . . C(1) C(2) C(3) 110.5(4) ? . . . O(3) C(3) C(2) 108.5(4) ? . . . O(3) C(3) C(4) 116.1(4) ? . . . C(2) C(3) C(4) 105.8(4) ? . . . O(4) C(4) C(3) 112.8(4) ? . . . O(4) C(4) C(5) 106.7(3) ? . . . C(3) C(4) C(5) 109.2(4) ? . . . O(5) C(5) C(4) 112.7(4) ? . . . O(5) C(5) C(6) 109.1(4) ? . . . C(4) C(5) C(6) 108.3(4) ? . . . O(6) C(6) C(5) 108.7(4) ? . . . O(4) C(7) O(6) 110.2(4) ? . . . O(4) C(7) C(8) 107.5(4) ? . . . O(6) C(7) C(8) 108.5(4) ? . . . N(1) C(9) C(10) 126.3(5) ? . . . C(9) C(10) C(11) 120.8(5) ? . . . C(9) C(10) C(15) 118.3(5) ? . . . C(11) C(10) C(15) 120.9(5) ? . . . O(1) C(11) C(10) 123.8(5) ? . . . O(1) C(11) C(12) 119.4(5) ? . . . C(10) C(11) C(12) 116.7(5) ? . . . C(11) C(12) C(13) 118.4(5) ? . . . C(11) C(12) C(16) 119.7(5) ? . . . C(13) C(12) C(16) 121.9(5) ? . . . C(12) C(13) C(14) 123.3(6) ? . . . C(13) C(14) C(15) 118.8(6) ? . . . C(10) C(15) C(14) 121.9(5) ? . . . C(12) C(16) C(17) 110.1(4) ? . . . C(12) C(16) C(18) 111.2(5) ? . . . C(12) C(16) C(19) 111.6(5) ? . . . C(17) C(16) C(18) 109.9(5) ? . . . C(17) C(16) C(19) 107.6(5) ? . . . C(18) C(16) C(19) 106.4(4) ? . . . O(11) C(20) N(2) 113.0(4) ? . . . O(11) C(20) C(21) 109.7(3) ? . . . N(2) C(20) C(21) 106.5(4) ? . . . O(8) C(21) C(20) 111.6(4) ? . . . O(8) C(21) C(22) 110.7(4) ? . . . C(20) C(21) C(22) 109.6(4) ? . . . O(9) C(22) C(21) 108.0(4) ? . . . O(9) C(22) C(23) 116.2(4) ? . . . C(21) C(22) C(23) 104.2(4) ? . . . O(10) C(23) C(22) 111.3(4) ? . . . O(10) C(23) C(24) 107.1(4) ? . . . C(22) C(23) C(24) 111.4(4) ? . . . O(11) C(24) C(23) 111.2(4) ? . . . O(11) C(24) C(25) 109.7(4) ? . . . C(23) C(24) C(25) 109.3(4) ? . . . O(12) C(25) C(24) 107.6(5) ? . . . O(10) C(26) O(12) 111.6(4) ? . . . O(10) C(26) C(27) 108.3(5) ? . . . O(12) C(26) C(27) 107.1(5) ? . . . N(2) C(28) C(29) 125.2(5) ? . . . C(28) C(29) C(30) 124.6(5) ? . . . C(28) C(29) C(34) 115.0(5) ? . . . C(30) C(29) C(34) 120.3(5) ? . . . O(7) C(30) C(29) 121.7(5) ? . . . O(7) C(30) C(31) 119.6(5) ? . . . C(29) C(30) C(31) 118.7(5) ? . . . C(30) C(31) C(32) 118.9(5) ? . . . C(30) C(31) C(35) 119.8(5) ? . . . C(32) C(31) C(35) 121.3(5) ? . . . C(31) C(32) C(33) 123.0(5) ? . . . C(32) C(33) C(34) 118.8(5) ? . . . C(29) C(34) C(33) 120.3(5) ? . . . C(31) C(35) C(36) 109.8(4) ? . . . C(31) C(35) C(37) 110.6(5) ? . . . C(31) C(35) C(38) 110.8(5) ? . . . C(36) C(35) C(37) 112.3(5) ? . . . C(36) C(35) C(38) 106.9(5) ? . . . C(37) C(35) C(38) 106.5(4) ? . . . N(3) C(39) C(40) 112.4(4) ? . . . N(4) C(42) C(43) 111.9(6) ? . . . CL(1) C(47) CL(2) 114.8(4) ? . . . CL(1) C(47) CL(3) 108.3(3) ? . . . CL(2) C(47) CL(3) 110.3(4) ? . . . CU(1) O(13) H(66) 118.0 ? . . . C(41) O(13) H(66) 104.3 ? . . . CU(3) O(14) H(64) 118.2 ? . . . C(44) O(14) H(64) 109.9 ? . . . C(45) O(15) H(76) 114.0 ? . . . C(46) O(16) H(65) 100.8 ? . . . CU(1) N(3) H(61) 105.3 ? . . . CU(1) N(3) H(62) 122.8 ? . . . C(39) N(3) H(61) 110.0 ? . . . C(39) N(3) H(62) 105.9 ? . . . H(61) N(3) H(62) 94.4 ? . . . CU(3) N(4) H(59) 124.6 ? . . . CU(3) N(4) H(60) 109.8 ? . . . C(42) N(4) H(59) 94.1 ? . . . C(42) N(4) H(60) 115.0 ? . . . H(59) N(4) H(60) 99.9 ? . . . O(5) C(1) H(15) 108.7 ? . . . N(1) C(1) H(15) 109.1 ? . . . C(2) C(1) H(15) 109.7 ? . . . O(2) C(2) H(16) 108.8 ? . . . C(1) C(2) H(16) 108.1 ? . . . C(3) C(2) H(16) 108.8 ? . . . O(3) C(3) H(17) 108.3 ? . . . C(2) C(3) H(17) 109.6 ? . . . C(4) C(3) H(17) 108.4 ? . . . O(4) C(4) H(18) 108.6 ? . . . C(3) C(4) H(18) 110.4 ? . . . C(5) C(4) H(18) 109.1 ? . . . O(5) C(5) H(19) 109.0 ? . . . C(4) C(5) H(19) 108.7 ? . . . C(6) C(5) H(19) 109.1 ? . . . O(6) C(6) H(23) 109.8 ? . . . O(6) C(6) H(24) 109.9 ? . . . C(5) C(6) H(23) 107.6 ? . . . C(5) C(6) H(24) 109.6 ? . . . H(23) C(6) H(24) 111.2 ? . . . O(4) C(7) H(20) 109.9 ? . . . O(6) C(7) H(20) 110.3 ? . . . C(8) C(7) H(20) 110.3 ? . . . C(7) C(8) H(28) 109.6 ? . . . C(7) C(8) H(29) 110.0 ? . . . C(7) C(8) H(30) 109.2 ? . . . H(28) C(8) H(29) 109.4 ? . . . H(28) C(8) H(30) 108.9 ? . . . H(29) C(8) H(30) 109.7 ? . . . N(1) C(9) H(2) 117.4 ? . . . C(10) C(9) H(2) 116.3 ? . . . C(12) C(13) H(8) 116.3 ? . . . C(14) C(13) H(8) 120.4 ? . . . C(13) C(14) H(7) 119.6 ? . . . C(15) C(14) H(7) 121.6 ? . . . C(10) C(15) H(6) 118.9 ? . . . C(14) C(15) H(6) 119.2 ? . . . C(16) C(17) H(40) 108.0 ? . . . C(16) C(17) H(41) 110.3 ? . . . C(16) C(17) H(42) 109.7 ? . . . H(40) C(17) H(41) 108.9 ? . . . H(40) C(17) H(42) 108.4 ? . . . H(41) C(17) H(42) 111.5 ? . . . C(16) C(18) H(43) 108.9 ? . . . C(16) C(18) H(44) 109.7 ? . . . C(16) C(18) H(45) 108.9 ? . . . H(43) C(18) H(44) 109.1 ? . . . H(43) C(18) H(45) 109.7 ? . . . H(44) C(18) H(45) 110.5 ? . . . C(16) C(19) H(46) 109.5 ? . . . C(16) C(19) H(47) 110.5 ? . . . C(16) C(19) H(48) 108.6 ? . . . H(46) C(19) H(47) 111.1 ? . . . H(46) C(19) H(48) 108.8 ? . . . H(47) C(19) H(48) 108.3 ? . . . O(11) C(20) H(9) 109.4 ? . . . N(2) C(20) H(9) 108.8 ? . . . C(21) C(20) H(9) 109.3 ? . . . O(8) C(21) H(10) 107.7 ? . . . C(20) C(21) H(10) 109.1 ? . . . C(22) C(21) H(10) 108.0 ? . . . O(9) C(22) H(11) 109.6 ? . . . C(21) C(22) H(11) 108.6 ? . . . C(23) C(22) H(11) 109.9 ? . . . O(10) C(23) H(12) 109.4 ? . . . C(22) C(23) H(12) 108.8 ? . . . C(24) C(23) H(12) 108.8 ? . . . O(11) C(24) H(13) 109.2 ? . . . C(23) C(24) H(13) 109.1 ? . . . C(25) C(24) H(13) 108.2 ? . . . O(12) C(25) H(21) 109.8 ? . . . O(12) C(25) H(22) 108.4 ? . . . C(24) C(25) H(21) 110.7 ? . . . C(24) C(25) H(22) 109.7 ? . . . H(21) C(25) H(22) 110.5 ? . . . O(10) C(26) H(14) 109.2 ? . . . O(12) C(26) H(14) 109.6 ? . . . C(27) C(26) H(14) 111.0 ? . . . C(26) C(27) H(25) 109.9 ? . . . C(26) C(27) H(26) 110.5 ? . . . C(26) C(27) H(27) 110.8 ? . . . H(25) C(27) H(26) 109.0 ? . . . H(25) C(27) H(27) 107.6 ? . . . H(26) C(27) H(27) 109.0 ? . . . N(2) C(28) H(1) 116.6 ? . . . C(29) C(28) H(1) 118.1 ? . . . C(31) C(32) H(5) 119.9 ? . . . C(33) C(32) H(5) 117.1 ? . . . C(32) C(33) H(4) 121.5 ? . . . C(34) C(33) H(4) 119.6 ? . . . C(29) C(34) H(3) 120.7 ? . . . C(33) C(34) H(3) 119.0 ? . . . C(35) C(36) H(34) 110.2 ? . . . C(35) C(36) H(35) 106.7 ? . . . C(35) C(36) H(36) 106.8 ? . . . H(34) C(36) H(35) 112.7 ? . . . H(34) C(36) H(36) 112.4 ? . . . H(35) C(36) H(36) 107.6 ? . . . C(35) C(37) H(37) 111.6 ? . . . C(35) C(37) H(38) 110.7 ? . . . C(35) C(37) H(39) 111.1 ? . . . H(37) C(37) H(38) 108.6 ? . . . H(37) C(37) H(39) 107.8 ? . . . H(38) C(37) H(39) 106.9 ? . . . C(35) C(38) H(31) 109.2 ? . . . C(35) C(38) H(32) 110.5 ? . . . C(35) C(38) H(33) 110.0 ? . . . H(31) C(38) H(32) 108.6 ? . . . H(31) C(38) H(33) 107.7 ? . . . H(32) C(38) H(33) 110.8 ? . . . N(3) C(39) H(51) 108.9 ? . . . N(3) C(39) H(52) 108.5 ? . . . C(40) C(39) H(51) 109.7 ? . . . C(40) C(39) H(52) 109.9 ? . . . H(51) C(39) H(52) 107.2 ? . . . C(39) C(40) H(56) 108.5 ? . . . C(39) C(40) H(57) 109.6 ? . . . C(39) C(40) H(58) 109.8 ? . . . H(56) C(40) H(57) 108.6 ? . . . H(56) C(40) H(58) 108.6 ? . . . H(57) C(40) H(58) 111.7 ? . . . O(13) C(41) H(70) 110.5 ? . . . O(13) C(41) H(71) 109.1 ? . . . O(13) C(41) H(72) 108.6 ? . . . H(70) C(41) H(71) 111.3 ? . . . H(70) C(41) H(72) 109.7 ? . . . H(71) C(41) H(72) 107.5 ? . . . N(4) C(42) H(49) 110.2 ? . . . N(4) C(42) H(50) 110.8 ? . . . C(43) C(42) H(49) 107.3 ? . . . C(43) C(42) H(50) 106.7 ? . . . H(49) C(42) H(50) 109.8 ? . . . C(42) C(43) H(53) 109.3 ? . . . C(42) C(43) H(54) 108.1 ? . . . C(42) C(43) H(55) 109.3 ? . . . H(53) C(43) H(54) 110.0 ? . . . H(53) C(43) H(55) 111.0 ? . . . H(54) C(43) H(55) 109.0 ? . . . O(14) C(44) H(67) 108.6 ? . . . O(14) C(44) H(68) 110.0 ? . . . O(14) C(44) H(69) 108.7 ? . . . H(67) C(44) H(68) 110.8 ? . . . H(67) C(44) H(69) 107.6 ? . . . H(68) C(44) H(69) 111.0 ? . . . O(15) C(45) H(77) 108.9 ? . . . O(15) C(45) H(78) 110.4 ? . . . O(15) C(45) H(79) 110.5 ? . . . H(77) C(45) H(78) 108.2 ? . . . H(77) C(45) H(79) 107.5 ? . . . H(78) C(45) H(79) 111.3 ? . . . O(16) C(46) H(73) 109.5 ? . . . O(16) C(46) H(74) 108.4 ? . . . O(16) C(46) H(75) 109.5 ? . . . H(73) C(46) H(74) 110.0 ? . . . H(73) C(46) H(75) 111.6 ? . . . H(74) C(46) H(75) 107.9 ? . . . CL(1) C(47) H(63) 108.7 ? . . . CL(2) C(47) H(63) 108.2 ? . . . CL(3) C(47) H(63) 106.2 ? . . . #============================================================================= #===END of compound 6 #=========================================================== #------------------------------------------------------------------------------ data_trans-[CuCl2(dmen)2].H2O_(compound13c) _database_code_depnum_ccdc_archive 'CCDC 297891' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C8 H26 Cl2 Cu N4 O ' _chemical_formula_moiety 'C8 H26 Cl2 Cu N4 O ' _chemical_formula_weight 328.77 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' _symmetry_Int_Tables_number 5 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,-z 1/2+x,1/2+y,z 1/2-x,1/2+y,-z _cell_length_a 10.668(8) _cell_length_b 8.306(6) _cell_length_c 9.478(7) _cell_angle_alpha 90 _cell_angle_beta 122.187(2) _cell_angle_gamma 90 _cell_volume 710.7(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 674 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 26.7 _cell_measurement_temperature 153.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 1587 _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.58 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _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) 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 592 _reflns_number_gt 558 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1484 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 558 _refine_ls_number_parameters 75 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0445P)^2^+6.1836P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0351 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2580 Friedel Pairs' _refine_ls_abs_structure_Flack 0.08(6) _refine_diff_density_max 0.56 _refine_diff_density_min -0.56 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) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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 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 0.5000 0.1894(2) 1.0000 0.0227(6) Uani 1.00 d S . . Cl(1) Cl 0.8113(2) 0.1915(6) 1.1168(2) 0.0273(6) Uani 1.00 d . . . O(1) O 1.0000 0.103(3) 1.5000 0.093(6) Uani 1.00 d S . . N(1) N 0.518(1) 0.028(2) 1.170(1) 0.029(3) Uani 1.00 d . . . N(2) N 0.525(1) 0.360(2) 1.172(1) 0.035(3) Uani 1.00 d . . . C(1) C 0.636(2) -0.106(3) 1.226(3) 0.062(6) Uani 1.00 d . . . C(2) C 0.494(1) 0.122(2) 1.290(1) 0.040(3) Uani 1.00 d . . . C(3) C 0.580(1) 0.277(2) 1.329(1) 0.044(3) Uani 1.00 d . . . C(4) C 0.642(2) 0.462(2) 1.231(2) 0.048(5) Uani 1.00 d . . . H(1) H 0.3942 0.1451 1.2443 0.0507 Uiso 1.00 calc . . . H(2) H 0.5328 0.0633 1.3924 0.0507 Uiso 1.00 calc . . . H(3) H 0.6833 0.2539 1.3781 0.0540 Uiso 1.00 calc . . . H(4) H 0.5667 0.3411 1.4010 0.0540 Uiso 1.00 calc . . . H(5) H 0.6208 -0.1847 1.2875 0.0861 Uiso 1.00 calc . . . H(6) H 0.6319 -0.1509 1.1335 0.0861 Uiso 1.00 calc . . . H(7) H 0.7316 -0.0570 1.2981 0.0861 Uiso 1.00 calc . . . H(8) H 0.7323 0.4093 1.2720 0.0614 Uiso 1.00 calc . . . H(9) H 0.6261 0.5351 1.1420 0.0614 Uiso 1.00 calc . . . H(10) H 0.6481 0.5299 1.3174 0.0614 Uiso 1.00 calc . . . H(11) H 0.4283 -0.0340 1.1091 0.0385 Uiso 1.00 calc . . . H(12) H 0.4343 0.4113 1.1371 0.0406 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) 0.0331(8) 0.0223(9) 0.0159(7) 0.0000 0.0151(5) 0.0000 Cl(1) 0.0197(9) 0.035(1) 0.0269(9) 0.000(2) 0.0120(7) 0.001(2) O(1) 0.12(1) 0.08(1) 0.034(6) 0.0000 0.014(7) 0.0000 N(1) 0.037(7) 0.030(7) 0.022(6) 0.002(6) 0.017(6) 0.000(6) N(2) 0.037(7) 0.038(8) 0.025(6) 0.012(6) 0.014(5) -0.007(6) C(1) 0.031(8) 0.05(1) 0.09(1) 0.003(6) 0.019(8) 0.042(8) C(2) 0.047(6) 0.056(7) 0.027(5) -0.006(6) 0.025(4) 0.002(5) C(3) 0.040(6) 0.062(7) 0.033(5) -0.004(6) 0.021(4) -0.017(5) C(4) 0.037(8) 0.06(1) 0.045(8) 0.010(7) 0.017(7) -0.025(7) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL93 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ORTEP-II #------------------------------------------------------------------------------ _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) Cl(1) 2.887(3) . . yes Cu(1) Cl(1) 2.887(3) . 2_657 yes Cu(1) N(1) 2.02(1) . . yes Cu(1) N(1) 2.02(1) . 2_657 yes Cu(1) N(2) 2.06(1) . . yes Cu(1) N(2) 2.06(1) . 2_657 yes N(1) C(1) 1.55(2) . . yes N(1) C(2) 1.51(2) . . yes N(2) C(3) 1.45(2) . . yes N(2) C(4) 1.35(2) . . yes C(2) C(3) 1.50(2) . . 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 Cl(1) Cu(1) Cl(1) 179.3(2) . . 2_657 yes Cl(1) Cu(1) N(1) 95.6(4) . . . yes Cl(1) Cu(1) N(1) 84.9(4) . . 2_657 yes Cl(1) Cu(1) N(2) 93.0(4) . . . yes Cl(1) Cu(1) N(2) 86.5(4) . . 2_657 yes Cl(1) Cu(1) N(1) 84.9(4) 2_657 . . yes Cl(1) Cu(1) N(1) 95.6(4) 2_657 . 2_657 yes Cl(1) Cu(1) N(2) 86.5(4) 2_657 . . yes Cl(1) Cu(1) N(2) 93.0(4) 2_657 . 2_657 yes N(1) Cu(1) N(1) 96.9(8) . . 2_657 yes N(1) Cu(1) N(2) 84.9(6) . . . yes N(1) Cu(1) N(2) 177.3(6) . . 2_657 yes N(1) Cu(1) N(2) 177.3(6) 2_657 . . yes N(1) Cu(1) N(2) 84.9(6) 2_657 . 2_657 yes N(2) Cu(1) N(2) 93.2(8) . . 2_657 yes Cu(1) N(1) C(1) 117(1) . . . yes Cu(1) N(1) C(2) 105.7(9) . . . yes C(1) N(1) C(2) 123(1) . . . yes Cu(1) N(2) C(3) 107.1(10) . . . yes Cu(1) N(2) C(4) 117(1) . . . yes C(3) N(2) C(4) 95(1) . . . yes N(1) C(2) C(3) 107(1) . . . yes N(2) C(3) C(2) 107.1(9) . . . yes N(1) Cu(1) N(1) 96.9(8) . . 2_657 yes N(1) Cu(1) N(2) 84.9(6) . . . yes N(1) Cu(1) N(2) 177.3(6) . . 2_657 yes N(1) Cu(1) Cl(1) 95.6(4) . . . yes N(1) Cu(1) Cl(1) 84.9(4) . . 2_657 yes N(1) Cu(1) N(2) 177.3(6) 2_657 . . yes N(1) Cu(1) N(2) 84.9(6) 2_657 . 2_657 yes N(1) Cu(1) Cl(1) 84.9(4) 2_657 . . yes N(1) Cu(1) Cl(1) 95.6(4) 2_657 . 2_657 yes N(2) Cu(1) N(2) 93.2(8) . . 2_657 yes N(2) Cu(1) Cl(1) 93.0(4) . . . yes N(2) Cu(1) Cl(1) 86.5(4) . . 2_657 yes N(2) Cu(1) Cl(1) 86.5(4) 2_657 . . yes N(2) Cu(1) Cl(1) 93.0(4) 2_657 . 2_657 yes Cl(1) Cu(1) Cl(1) 179.3(2) . . 2_657 yes #------------------------------------------------------------------------------ #===END of compound 13c #------------------------------------------------------------------------------ #============================================================================= #===CIF END #============================================================================= #============================================================================= #===END of compound 5 #=========================================================== #============================================================================== data_[Cu(HL1)(EtNH2)]_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 611610' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C21 H32 Cu N2 O6 ' _chemical_formula_moiety 'C21 H32 Cu N2 O6 ' _chemical_formula_weight 472.04 _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 6.612(4) _cell_length_b 12.230(6) _cell_length_c 14.089(7) _cell_angle_alpha 77.465(10) _cell_angle_beta 82.337(14) _cell_angle_gamma 88.386(16) _cell_volume 1102.3(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1789 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description rectangl. _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498.00 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.921 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 8224 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.813 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _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) 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 9568 _reflns_number_gt 8224 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.1926 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4120 _refine_ls_number_parameters 544 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1015P)^2^+4.6768P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0146 _refine_diff_density_max 1.03 _refine_diff_density_min -1.54 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2580 Friedel Pairs' _refine_ls_abs_structure_Flack 0.00(2) 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 -1.75630(12) 0.22502(9) 0.46509(6) 0.0287(3) Uani 1.00 1 d . . . CU(2) Cu -0.90037(12) -0.10535(9) 0.72869(6) 0.0283(3) Uani 1.00 1 d . . . O(1) O -1.9462(15) 0.3336(8) 0.4134(6) 0.033(2) Uani 1.00 1 d . . . O(2) O -1.5457(14) 0.1174(8) 0.5109(6) 0.033(2) Uani 1.00 1 d . . . O(3) O -1.2490(12) -0.0681(6) 0.5299(5) 0.0381(17) Uani 1.00 1 d . . . O(4) O -0.9544(15) -0.0558(8) 0.3563(7) 0.033(2) Uani 1.00 1 d . . . O(5) O -1.3541(13) 0.1258(7) 0.2555(6) 0.033(2) Uani 1.00 1 d . . . O(6) O -0.8918(12) -0.0191(7) 0.1856(5) 0.0408(18) Uani 1.00 1 d . . . O(7) O -0.7175(14) -0.2232(8) 0.7856(7) 0.031(2) Uani 1.00 1 d . . . O(8) O -1.1321(14) -0.0117(8) 0.6854(6) 0.0277(19) Uani 1.00 1 d . . . O(9) O -1.5844(11) 0.0530(6) 0.6971(4) 0.0318(14) Uani 1.00 1 d . . . O(10) O -1.6934(13) 0.1818(8) 0.8419(6) 0.0286(19) Uani 1.00 1 d . . . O(11) O -1.2650(12) 0.0162(7) 0.9376(5) 0.0292(18) Uani 1.00 1 d . . . O(12) O -1.6733(12) 0.2029(7) 1.0026(5) 0.0380(17) Uani 1.00 1 d . . . N(1) N -1.6137(16) 0.2267(9) 0.3339(7) 0.032(2) Uani 1.00 1 d . . . N(2) N -1.0003(16) -0.0769(9) 0.8570(7) 0.032(2) Uani 1.00 1 d . . . N(3) N -1.8946(16) 0.2024(9) 0.6030(7) 0.030(2) Uani 1.00 1 d . . . N(4) N -0.7903(18) -0.1044(9) 0.5887(7) 0.032(2) Uani 1.00 1 d . . . C(1) C -1.4190(16) 0.1707(8) 0.3405(7) 0.032(2) Uani 1.00 1 d . . . C(2) C -1.4443(16) 0.0770(9) 0.4312(6) 0.029(2) Uani 1.00 1 d . . . C(3) C -1.236(2) 0.0270(11) 0.4478(9) 0.032(2) Uani 1.00 1 d . . . C(4) C -1.1558(19) -0.0134(10) 0.3552(8) 0.033(2) Uani 1.00 1 d . . . C(5) C -1.1569(17) 0.0803(9) 0.2650(7) 0.036(2) Uani 1.00 1 d . . . C(6) C -1.083(2) 0.0328(12) 0.1755(9) 0.039(3) Uani 1.00 1 d . . . C(7) C -0.887(2) -0.0982(12) 0.2725(10) 0.038(3) Uani 1.00 1 d . . . C(8) C -0.678(2) -0.1427(14) 0.2762(11) 0.049(4) Uani 1.00 1 d . . . C(9) C -1.678(2) 0.2703(11) 0.2528(9) 0.032(2) Uani 1.00 1 d . . . C(10) C -1.852(2) 0.3400(12) 0.2424(10) 0.035(3) Uani 1.00 1 d . . . C(11) C -1.971(2) 0.3754(12) 0.3214(10) 0.030(2) Uani 1.00 1 d . . . C(12) C -2.130(2) 0.4588(12) 0.2981(9) 0.035(3) Uani 1.00 1 d . . . C(13) C -2.168(3) 0.4894(19) 0.2013(14) 0.068(5) Uani 1.00 1 d . . . C(14) C -2.056(3) 0.4476(18) 0.1249(13) 0.071(6) Uani 1.00 1 d . . . C(15) C -1.897(2) 0.3794(15) 0.1429(12) 0.051(4) Uani 1.00 1 d . . . C(16) C -2.247(2) 0.5096(12) 0.3773(11) 0.038(3) Uani 1.00 1 d . . . C(17) C -2.380(2) 0.4238(16) 0.4533(14) 0.057(4) Uani 1.00 1 d . . . C(18) C -2.091(2) 0.5644(12) 0.4260(12) 0.044(3) Uani 1.00 1 d . . . C(19) C -2.385(3) 0.6050(17) 0.3365(14) 0.063(5) Uani 1.00 1 d . . . C(20) C -1.1458(15) 0.0124(8) 0.8463(7) 0.030(2) Uani 1.00 1 d . . . C(21) C -1.2772(17) -0.0077(9) 0.7694(7) 0.031(2) Uani 1.00 1 d . . . C(22) C -1.439(2) 0.0839(11) 0.7517(9) 0.026(2) Uani 1.00 1 d . . . C(23) C -1.5500(16) 0.0907(10) 0.8522(8) 0.029(2) Uani 1.00 1 d . . . C(24) C -1.4053(15) 0.1076(8) 0.9226(7) 0.030(2) Uani 1.00 1 d . . . C(25) C -1.5279(19) 0.1137(11) 1.0197(8) 0.033(2) Uani 1.00 1 d . . . C(26) C -1.802(2) 0.1869(12) 0.9351(8) 0.035(3) Uani 1.00 1 d . . . C(27) C -1.949(2) 0.2807(13) 0.9218(10) 0.039(3) Uani 1.00 1 d . . . C(28) C -0.9654(19) -0.1325(12) 0.9404(10) 0.033(2) Uani 1.00 1 d . . . C(29) C -0.814(2) -0.2213(12) 0.9553(9) 0.034(3) Uani 1.00 1 d . . . C(30) C -0.701(2) -0.2600(12) 0.8752(10) 0.033(3) Uani 1.00 1 d . . . C(31) C -0.557(2) -0.3508(12) 0.9018(11) 0.041(3) Uani 1.00 1 d . . . C(32) C -0.535(3) -0.3910(16) 0.9968(12) 0.063(5) Uani 1.00 1 d . . . C(33) C -0.648(3) -0.3510(18) 1.0748(10) 0.074(6) Uani 1.00 1 d . . . C(34) C -0.786(3) -0.2678(17) 1.0532(11) 0.054(4) Uani 1.00 1 d . . . C(35) C -0.428(2) -0.3996(12) 0.8181(11) 0.042(3) Uani 1.00 1 d . . . C(36) C -0.566(2) -0.4505(13) 0.7635(12) 0.050(4) Uani 1.00 1 d . . . C(37) C -0.298(2) -0.3066(14) 0.7481(12) 0.046(3) Uani 1.00 1 d . . . C(38) C -0.281(3) -0.4919(19) 0.8609(14) 0.075(6) Uani 1.00 1 d . . . C(39) C -1.996(2) 0.2999(11) 0.6375(8) 0.033(2) Uani 1.00 1 d . . . C(40) C -1.848(2) 0.3862(13) 0.6430(11) 0.048(3) Uani 1.00 1 d . . . C(41) C -0.677(2) -0.2009(13) 0.5593(11) 0.044(3) Uani 1.00 1 d . . . C(42) C -0.826(2) -0.2908(14) 0.5597(12) 0.050(3) Uani 1.00 1 d . . . H(1) H -2.2787 0.5425 0.1870 0.080 Uiso 1.00 1 c R . . H(2) H -2.0928 0.4701 0.0596 0.083 Uiso 1.00 1 c R . . H(3) H -1.8094 0.3575 0.0916 0.055 Uiso 1.00 1 c R . . H(4) H -1.6055 0.2517 0.1960 0.038 Uiso 1.00 1 c R . . H(5) H -0.4469 -0.4504 1.0138 0.080 Uiso 1.00 1 c R . . H(6) H -0.6237 -0.3782 1.1394 0.090 Uiso 1.00 1 c R . . H(7) H -0.8619 -0.2395 1.1053 0.071 Uiso 1.00 1 c R . . H(8) H -1.0423 -0.1177 0.9981 0.042 Uiso 1.00 1 c R . . H(9) H -0.6736 -0.1970 0.3342 0.062 Uiso 1.00 1 c R . . H(10) H -0.6404 -0.1750 0.2206 0.062 Uiso 1.00 1 c R . . H(11) H -0.5884 -0.0825 0.2734 0.062 Uiso 1.00 1 c R . . H(12) H -1.7582 0.3533 0.6880 0.051 Uiso 1.00 1 c R . . H(13) H -1.7746 0.4119 0.5800 0.051 Uiso 1.00 1 c R . . H(14) H -1.9216 0.4452 0.6644 0.051 Uiso 1.00 1 c R . . H(15) H -1.9995 0.5059 0.4545 0.052 Uiso 1.00 1 c R . . H(16) H -2.0136 0.6182 0.3792 0.052 Uiso 1.00 1 c R . . H(17) H -2.1599 0.5949 0.4770 0.052 Uiso 1.00 1 c R . . H(18) H -2.4437 0.4575 0.5038 0.061 Uiso 1.00 1 c R . . H(19) H -2.4838 0.3979 0.4215 0.061 Uiso 1.00 1 c R . . H(20) H -2.3007 0.3617 0.4796 0.061 Uiso 1.00 1 c R . . H(21) H -2.3071 0.6588 0.2909 0.071 Uiso 1.00 1 c R . . H(22) H -2.4827 0.5728 0.3053 0.071 Uiso 1.00 1 c R . . H(23) H -2.4529 0.6328 0.3888 0.071 Uiso 1.00 1 c R . . H(24) H -1.8823 0.3503 0.8943 0.045 Uiso 1.00 1 c R . . H(25) H -2.0422 0.2689 0.8766 0.045 Uiso 1.00 1 c R . . H(26) H -2.0292 0.2848 0.9820 0.045 Uiso 1.00 1 c R . . H(27) H -0.2066 -0.2772 0.7831 0.054 Uiso 1.00 1 c R . . H(28) H -0.2219 -0.3367 0.6976 0.054 Uiso 1.00 1 c R . . H(29) H -0.3850 -0.2492 0.7206 0.054 Uiso 1.00 1 c R . . H(30) H -0.6590 -0.3956 0.7353 0.059 Uiso 1.00 1 c R . . H(31) H -0.4888 -0.4793 0.7118 0.059 Uiso 1.00 1 c R . . H(32) H -0.6436 -0.5109 0.8063 0.059 Uiso 1.00 1 c R . . H(33) H -0.3584 -0.5520 0.9046 0.093 Uiso 1.00 1 c R . . H(34) H -0.2064 -0.5210 0.8090 0.093 Uiso 1.00 1 c R . . H(35) H -0.1896 -0.4634 0.8956 0.093 Uiso 1.00 1 c R . . H(36) H -0.9008 -0.3149 0.6252 0.060 Uiso 1.00 1 c R . . H(37) H -0.9266 -0.2647 0.5165 0.060 Uiso 1.00 1 c R . . H(38) H -0.7617 -0.3553 0.5419 0.060 Uiso 1.00 1 c R . . H(39) H -2.0864 0.3318 0.5914 0.042 Uiso 1.00 1 c R . . H(40) H -2.0704 0.2733 0.6995 0.042 Uiso 1.00 1 c R . . H(41) H -0.6077 -0.1782 0.4933 0.050 Uiso 1.00 1 c R . . H(42) H -0.5807 -0.2289 0.6017 0.050 Uiso 1.00 1 c R . . H(43) H -1.0745 0.0907 0.1189 0.049 Uiso 1.00 1 c R . . H(44) H -1.1794 -0.0223 0.1705 0.049 Uiso 1.00 1 c R . . H(45) H -1.4418 0.1282 1.0637 0.043 Uiso 1.00 1 c R . . H(46) H -1.5982 0.0449 1.0461 0.043 Uiso 1.00 1 c R . . H(47) H -1.3196 0.2209 0.3466 0.039 Uiso 1.00 1 c R . . H(48) H -1.5276 0.0201 0.4201 0.036 Uiso 1.00 1 c R . . H(49) H -1.1492 0.0823 0.4580 0.035 Uiso 1.00 1 c R . . H(50) H -1.2404 -0.0732 0.3505 0.040 Uiso 1.00 1 c R . . H(51) H -1.0677 0.1378 0.2679 0.042 Uiso 1.00 1 c R . . H(52) H -0.9754 -0.1586 0.2724 0.042 Uiso 1.00 1 c R . . H(53) H -1.0754 0.0822 0.8220 0.035 Uiso 1.00 1 c R . . H(54) H -1.3440 -0.0789 0.7922 0.035 Uiso 1.00 1 c R . . H(55) H -1.3769 0.1533 0.7205 0.031 Uiso 1.00 1 c R . . H(56) H -1.6231 0.0225 0.8796 0.034 Uiso 1.00 1 c R . . H(57) H -1.3298 0.1756 0.8967 0.035 Uiso 1.00 1 c R . . H(58) H -1.8729 0.1187 0.9605 0.042 Uiso 1.00 1 c R . . H(59) H -2.0104 0.1437 0.6228 0.038 Uiso 1.00 1 c R . . H(60) H -1.8183 0.1947 0.6644 0.038 Uiso 1.00 1 c R . . H(61) H -0.9039 -0.0909 0.5522 0.038 Uiso 1.00 1 c R . . H(62) H -0.7003 -0.0409 0.5670 0.038 Uiso 1.00 1 c R . . H(63) H -1.2039 -0.0530 0.6000 0.038 Uiso 1.00 1 c R . . H(64) H -1.5915 0.0959 0.6280 0.038 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) 0.0312(7) 0.0363(7) 0.0193(6) 0.0073(6) 0.0007(5) -0.0108(5) CU(2) 0.0314(7) 0.0367(7) 0.0177(6) 0.0081(6) -0.0003(5) -0.0105(5) O(1) 0.043(6) 0.042(5) 0.020(4) 0.010(4) -0.007(4) -0.015(3) O(2) 0.035(5) 0.043(4) 0.020(4) 0.013(3) 0.007(3) -0.016(3) O(3) 0.057(4) 0.037(3) 0.021(3) 0.015(3) -0.010(3) -0.007(2) O(4) 0.038(5) 0.038(4) 0.027(4) 0.016(4) -0.005(3) -0.019(3) O(5) 0.033(4) 0.041(4) 0.021(3) 0.015(3) 0.009(3) -0.007(3) O(6) 0.036(4) 0.054(4) 0.028(3) 0.023(3) 0.004(3) -0.008(3) O(7) 0.034(5) 0.034(4) 0.024(4) 0.011(3) 0.003(3) -0.012(3) O(8) 0.033(4) 0.038(4) 0.012(3) 0.009(3) -0.001(3) -0.009(3) O(9) 0.040(3) 0.041(3) 0.019(2) 0.006(3) -0.012(2) -0.012(2) O(10) 0.021(4) 0.046(5) 0.019(4) 0.011(3) -0.002(3) -0.008(3) O(11) 0.031(4) 0.043(4) 0.015(3) 0.014(3) -0.004(2) -0.011(3) O(12) 0.034(4) 0.056(4) 0.033(3) 0.011(3) -0.007(3) -0.026(3) N(1) 0.032(5) 0.040(5) 0.023(4) 0.005(4) 0.008(3) -0.015(3) N(2) 0.030(5) 0.043(5) 0.022(4) 0.007(4) 0.001(3) -0.011(3) N(3) 0.029(5) 0.037(5) 0.022(4) 0.007(4) 0.005(3) -0.007(3) N(4) 0.042(6) 0.038(5) 0.016(4) 0.008(4) 0.002(3) -0.010(3) C(1) 0.041(5) 0.032(4) 0.023(4) 0.000(4) 0.005(3) -0.014(3) C(2) 0.037(5) 0.037(5) 0.013(3) 0.011(4) 0.002(3) -0.010(3) C(3) 0.039(7) 0.037(6) 0.021(5) 0.008(5) 0.001(4) -0.015(5) C(4) 0.035(6) 0.046(6) 0.020(4) 0.015(4) -0.001(4) -0.017(4) C(5) 0.040(5) 0.041(5) 0.023(4) 0.013(4) 0.002(3) -0.007(4) C(6) 0.031(6) 0.055(7) 0.025(5) 0.014(5) 0.008(4) -0.007(5) C(7) 0.033(6) 0.052(7) 0.030(5) 0.016(5) -0.003(4) -0.015(5) C(8) 0.039(7) 0.070(9) 0.042(7) 0.039(7) -0.010(5) -0.021(6) C(9) 0.044(7) 0.036(5) 0.016(5) 0.003(5) 0.001(4) -0.011(4) C(10) 0.045(8) 0.041(7) 0.022(6) 0.014(6) -0.008(5) -0.012(5) C(11) 0.028(6) 0.044(7) 0.022(6) 0.002(5) -0.000(4) -0.015(5) C(12) 0.043(7) 0.041(6) 0.020(5) 0.007(5) -0.001(4) -0.007(4) C(13) 0.068(10) 0.099(13) 0.051(9) 0.056(10) -0.033(8) -0.039(9) C(14) 0.081(11) 0.100(13) 0.047(9) 0.061(10) -0.034(8) -0.042(9) C(15) 0.062(10) 0.061(9) 0.033(8) 0.036(8) -0.005(6) -0.021(6) C(16) 0.041(8) 0.043(7) 0.037(7) 0.011(6) -0.008(5) -0.020(6) C(17) 0.050(9) 0.064(10) 0.058(10) 0.009(7) 0.014(7) -0.031(8) C(18) 0.050(8) 0.037(7) 0.050(8) 0.011(6) 0.000(6) -0.025(6) C(19) 0.074(13) 0.074(11) 0.049(10) 0.039(10) -0.011(9) -0.031(8) C(20) 0.033(5) 0.030(4) 0.027(4) 0.011(4) 0.004(3) -0.015(3) C(21) 0.035(5) 0.032(5) 0.027(4) 0.007(4) 0.003(3) -0.015(4) C(22) 0.026(6) 0.039(6) 0.018(5) 0.003(4) -0.004(4) -0.014(4) C(23) 0.019(5) 0.047(6) 0.025(4) 0.010(4) 0.000(3) -0.021(4) C(24) 0.034(5) 0.034(4) 0.027(4) 0.010(4) -0.005(3) -0.019(3) C(25) 0.031(6) 0.053(7) 0.018(4) 0.015(5) -0.005(4) -0.018(4) C(26) 0.033(6) 0.059(7) 0.020(5) 0.020(5) -0.004(4) -0.024(5) C(27) 0.036(6) 0.054(7) 0.029(6) 0.005(5) 0.001(4) -0.019(5) C(28) 0.018(5) 0.055(7) 0.026(5) 0.012(5) 0.002(4) -0.011(5) C(29) 0.038(7) 0.045(7) 0.019(6) 0.016(6) -0.005(5) -0.010(5) C(30) 0.039(7) 0.037(7) 0.029(7) 0.007(5) -0.011(5) -0.016(5) C(31) 0.038(7) 0.049(7) 0.044(8) 0.026(5) -0.018(5) -0.025(6) C(32) 0.082(12) 0.080(11) 0.029(7) 0.042(9) -0.009(7) -0.020(7) C(33) 0.106(14) 0.101(13) 0.014(5) 0.055(11) -0.020(6) -0.007(6) C(34) 0.066(10) 0.083(11) 0.018(6) 0.029(9) -0.018(6) -0.017(6) C(35) 0.054(9) 0.038(7) 0.035(8) 0.019(6) -0.007(6) -0.013(6) C(36) 0.060(10) 0.049(8) 0.043(8) -0.013(7) 0.002(7) -0.017(7) C(37) 0.032(7) 0.064(9) 0.053(8) 0.005(6) -0.011(6) -0.031(7) C(38) 0.100(16) 0.088(13) 0.044(10) 0.066(12) -0.021(10) -0.029(9) C(39) 0.045(7) 0.036(5) 0.019(5) 0.008(5) 0.005(4) -0.015(4) C(40) 0.059(9) 0.047(7) 0.040(7) 0.004(6) 0.005(6) -0.020(6) C(41) 0.036(7) 0.059(8) 0.042(7) 0.009(6) -0.005(5) -0.028(6) C(42) 0.057(9) 0.055(8) 0.040(7) -0.001(6) -0.011(6) -0.011(6) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.7.0' _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) 1.898(10) ? . . CU(1) O(2) 1.964(9) ? . . CU(1) N(1) 1.956(10) ? . . CU(1) N(3) 1.999(10) ? . . CU(2) O(7) 1.960(9) ? . . CU(2) O(8) 1.969(9) ? . . CU(2) N(2) 1.941(11) ? . . CU(2) N(4) 2.007(10) ? . . O(1) C(11) 1.316(16) ? . . O(2) C(2) 1.406(14) ? . . O(3) C(3) 1.447(13) ? . . O(4) C(4) 1.416(16) ? . . O(4) C(7) 1.405(18) ? . . O(5) C(1) 1.434(14) ? . . O(5) C(5) 1.415(14) ? . . O(6) C(6) 1.409(15) ? . . O(6) C(7) 1.390(15) ? . . O(7) C(30) 1.263(17) ? . . O(8) C(21) 1.429(13) ? . . O(9) C(22) 1.415(16) ? . . O(10) C(23) 1.438(14) ? . . O(10) C(26) 1.422(15) ? . . O(11) C(20) 1.426(12) ? . . O(11) C(24) 1.430(13) ? . . O(12) C(25) 1.436(15) ? . . O(12) C(26) 1.403(16) ? . . N(1) C(1) 1.445(15) ? . . N(1) C(9) 1.276(17) ? . . N(2) C(20) 1.431(14) ? . . N(2) C(28) 1.270(16) ? . . N(3) C(39) 1.493(18) ? . . N(4) C(41) 1.49(2) ? . . C(1) C(2) 1.514(12) ? . . C(2) C(3) 1.515(18) ? . . C(3) C(4) 1.519(19) ? . . C(4) C(5) 1.516(14) ? . . C(5) C(6) 1.517(18) ? . . C(7) C(8) 1.47(2) ? . . C(9) C(10) 1.42(2) ? . . C(10) C(11) 1.42(2) ? . . C(10) C(15) 1.45(2) ? . . C(11) C(12) 1.46(2) ? . . C(12) C(13) 1.39(2) ? . . C(12) C(16) 1.51(2) ? . . C(13) C(14) 1.40(2) ? . . C(14) C(15) 1.34(2) ? . . C(16) C(17) 1.53(2) ? . . C(16) C(18) 1.55(2) ? . . C(16) C(19) 1.52(2) ? . . C(20) C(21) 1.539(16) ? . . C(21) C(22) 1.532(17) ? . . C(22) C(23) 1.523(16) ? . . C(23) C(24) 1.515(16) ? . . C(24) C(25) 1.510(15) ? . . C(26) C(27) 1.48(2) ? . . C(28) C(29) 1.46(2) ? . . C(29) C(30) 1.43(2) ? . . C(29) C(34) 1.41(2) ? . . C(30) C(31) 1.46(2) ? . . C(31) C(32) 1.35(2) ? . . C(31) C(35) 1.58(2) ? . . C(32) C(33) 1.41(2) ? . . C(33) C(34) 1.36(2) ? . . C(35) C(36) 1.50(2) ? . . C(35) C(37) 1.53(2) ? . . C(35) C(38) 1.54(2) ? . . C(39) C(40) 1.49(2) ? . . C(41) C(42) 1.49(2) ? . . O(3) H(63) 1.123 ? . . O(9) H(64) 1.007 ? . . N(3) H(59) 1.033 ? . . N(3) H(60) 1.044 ? . . N(4) H(61) 0.957 ? . . N(4) H(62) 0.962 ? . . C(1) H(47) 0.937 ? . . C(2) H(48) 0.951 ? . . C(3) H(49) 0.947 ? . . C(4) H(50) 0.952 ? . . C(5) H(51) 0.941 ? . . C(6) H(43) 0.941 ? . . C(6) H(44) 0.961 ? . . C(7) H(52) 0.957 ? . . C(8) H(9) 0.938 ? . . C(8) H(10) 0.952 ? . . C(8) H(11) 0.948 ? . . C(9) H(4) 0.945 ? . . C(13) H(1) 0.978 ? . . C(14) H(2) 0.964 ? . . C(15) H(3) 0.945 ? . . C(17) H(18) 0.943 ? . . C(17) H(19) 0.962 ? . . C(17) H(20) 0.948 ? . . C(18) H(15) 0.975 ? . . C(18) H(16) 0.931 ? . . C(18) H(17) 0.941 ? . . C(19) H(21) 0.926 ? . . C(19) H(22) 0.967 ? . . C(19) H(23) 0.934 ? . . C(20) H(53) 0.957 ? . . C(21) H(54) 0.959 ? . . C(22) H(55) 0.945 ? . . C(23) H(56) 0.954 ? . . C(24) H(57) 0.958 ? . . C(25) H(45) 0.943 ? . . C(25) H(46) 0.950 ? . . C(26) H(58) 0.945 ? . . C(27) H(24) 0.951 ? . . C(27) H(25) 0.975 ? . . C(27) H(26) 0.947 ? . . C(28) H(8) 0.950 ? . . C(32) H(5) 0.931 ? . . C(33) H(6) 0.933 ? . . C(34) H(7) 0.954 ? . . C(36) H(30) 0.955 ? . . C(36) H(31) 0.958 ? . . C(36) H(32) 0.958 ? . . C(37) H(27) 0.954 ? . . C(37) H(28) 0.952 ? . . C(37) H(29) 0.942 ? . . C(38) H(33) 0.962 ? . . C(38) H(34) 0.953 ? . . C(38) H(35) 0.941 ? . . C(39) H(39) 0.953 ? . . C(39) H(40) 0.937 ? . . C(40) H(12) 0.942 ? . . C(40) H(13) 0.945 ? . . C(40) H(14) 0.941 ? . . C(41) H(41) 0.966 ? . . C(41) H(42) 0.937 ? . . C(42) H(36) 0.977 ? . . C(42) H(37) 0.963 ? . . C(42) H(38) 0.950 ? . . 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(1) CU(1) O(2) 176.0(3) ? . . . O(1) CU(1) N(1) 91.4(4) ? . . . O(1) CU(1) N(3) 94.4(4) ? . . . O(2) CU(1) N(1) 85.1(4) ? . . . O(2) CU(1) N(3) 89.2(4) ? . . . N(1) CU(1) N(3) 172.7(4) ? . . . O(7) CU(2) O(8) 167.2(3) ? . . . O(7) CU(2) N(2) 91.5(4) ? . . . O(7) CU(2) N(4) 95.4(4) ? . . . O(8) CU(2) N(2) 84.6(4) ? . . . O(8) CU(2) N(4) 90.4(4) ? . . . N(2) CU(2) N(4) 169.5(4) ? . . . CU(1) O(1) C(11) 129.5(9) ? . . . CU(1) O(2) C(2) 109.4(6) ? . . . C(4) O(4) C(7) 112.0(10) ? . . . C(1) O(5) C(5) 107.4(8) ? . . . C(6) O(6) C(7) 114.3(8) ? . . . CU(2) O(7) C(30) 127.6(9) ? . . . CU(2) O(8) C(21) 108.5(6) ? . . . C(23) O(10) C(26) 110.0(8) ? . . . C(20) O(11) C(24) 108.8(7) ? . . . C(25) O(12) C(26) 111.7(10) ? . . . CU(1) N(1) C(1) 110.3(7) ? . . . CU(1) N(1) C(9) 126.3(9) ? . . . C(1) N(1) C(9) 123.4(10) ? . . . CU(2) N(2) C(20) 109.1(7) ? . . . CU(2) N(2) C(28) 128.1(10) ? . . . C(20) N(2) C(28) 122.4(11) ? . . . CU(1) N(3) C(39) 119.0(7) ? . . . CU(2) N(4) C(41) 122.3(8) ? . . . O(5) C(1) N(1) 111.4(9) ? . . . O(5) C(1) C(2) 109.9(8) ? . . . N(1) C(1) C(2) 107.4(8) ? . . . O(2) C(2) C(1) 109.7(9) ? . . . O(2) C(2) C(3) 114.1(9) ? . . . C(1) C(2) C(3) 108.5(8) ? . . . O(3) C(3) C(2) 112.0(9) ? . . . O(3) C(3) C(4) 108.3(10) ? . . . C(2) C(3) C(4) 105.8(10) ? . . . O(4) C(4) C(3) 112.8(11) ? . . . O(4) C(4) C(5) 107.8(8) ? . . . C(3) C(4) C(5) 111.0(10) ? . . . O(5) C(5) C(4) 112.2(8) ? . . . O(5) C(5) C(6) 108.7(9) ? . . . C(4) C(5) C(6) 108.1(10) ? . . . O(6) C(6) C(5) 110.0(10) ? . . . O(4) C(7) O(6) 113.0(11) ? . . . O(4) C(7) C(8) 110.8(13) ? . . . O(6) C(7) C(8) 109.1(10) ? . . . N(1) C(9) C(10) 125.2(12) ? . . . C(9) C(10) C(11) 123.9(13) ? . . . C(9) C(10) C(15) 115.4(13) ? . . . C(11) C(10) C(15) 120.6(13) ? . . . O(1) C(11) C(10) 122.0(12) ? . . . O(1) C(11) C(12) 120.2(12) ? . . . C(10) C(11) C(12) 117.7(12) ? . . . C(11) C(12) C(13) 117.8(14) ? . . . C(11) C(12) C(16) 120.5(12) ? . . . C(13) C(12) C(16) 121.7(14) ? . . . C(12) C(13) C(14) 123.2(18) ? . . . C(13) C(14) C(15) 120.0(18) ? . . . C(10) C(15) C(14) 120.2(16) ? . . . C(12) C(16) C(17) 112.5(13) ? . . . C(12) C(16) C(18) 108.0(12) ? . . . C(12) C(16) C(19) 112.5(13) ? . . . C(17) C(16) C(18) 111.2(14) ? . . . C(17) C(16) C(19) 107.5(13) ? . . . C(18) C(16) C(19) 105.0(14) ? . . . O(11) C(20) N(2) 111.4(7) ? . . . O(11) C(20) C(21) 112.3(8) ? . . . N(2) C(20) C(21) 106.4(9) ? . . . O(8) C(21) C(20) 103.9(8) ? . . . O(8) C(21) C(22) 114.4(8) ? . . . C(20) C(21) C(22) 110.8(9) ? . . . O(9) C(22) C(21) 110.3(10) ? . . . O(9) C(22) C(23) 107.5(9) ? . . . C(21) C(22) C(23) 106.5(9) ? . . . O(10) C(23) C(22) 109.5(8) ? . . . O(10) C(23) C(24) 108.9(10) ? . . . C(22) C(23) C(24) 112.5(9) ? . . . O(11) C(24) C(23) 110.6(9) ? . . . O(11) C(24) C(25) 108.9(8) ? . . . C(23) C(24) C(25) 108.8(9) ? . . . O(12) C(25) C(24) 108.2(8) ? . . . O(10) C(26) O(12) 112.9(10) ? . . . O(10) C(26) C(27) 108.6(10) ? . . . O(12) C(26) C(27) 109.0(12) ? . . . N(2) C(28) C(29) 124.4(12) ? . . . C(28) C(29) C(30) 121.9(12) ? . . . C(28) C(29) C(34) 116.2(13) ? . . . C(30) C(29) C(34) 121.9(14) ? . . . O(7) C(30) C(29) 125.8(13) ? . . . O(7) C(30) C(31) 118.6(13) ? . . . C(29) C(30) C(31) 115.6(12) ? . . . C(30) C(31) C(32) 119.9(15) ? . . . C(30) C(31) C(35) 119.1(12) ? . . . C(32) C(31) C(35) 121.0(14) ? . . . C(31) C(32) C(33) 123.4(18) ? . . . C(32) C(33) C(34) 118.5(15) ? . . . C(29) C(34) C(33) 120.7(15) ? . . . C(31) C(35) C(36) 110.2(13) ? . . . C(31) C(35) C(37) 109.8(13) ? . . . C(31) C(35) C(38) 111.1(13) ? . . . C(36) C(35) C(37) 110.4(13) ? . . . C(36) C(35) C(38) 107.8(15) ? . . . C(37) C(35) C(38) 107.5(14) ? . . . N(3) C(39) C(40) 112.1(12) ? . . . N(4) C(41) C(42) 108.9(12) ? . . . C(3) O(3) H(63) 116.5 ? . . . C(22) O(9) H(64) 119.6 ? . . . CU(1) N(3) H(59) 116.2 ? . . . CU(1) N(3) H(60) 124.3 ? . . . C(39) N(3) H(59) 101.1 ? . . . C(39) N(3) H(60) 84.3 ? . . . H(59) N(3) H(60) 105.9 ? . . . CU(2) N(4) H(61) 106.6 ? . . . CU(2) N(4) H(62) 106.4 ? . . . C(41) N(4) H(61) 106.7 ? . . . C(41) N(4) H(62) 106.3 ? . . . H(61) N(4) H(62) 107.9 ? . . . O(5) C(1) H(47) 108.7 ? . . . N(1) C(1) H(47) 110.1 ? . . . C(2) C(1) H(47) 109.3 ? . . . O(2) C(2) H(48) 107.4 ? . . . C(1) C(2) H(48) 108.9 ? . . . C(3) C(2) H(48) 108.0 ? . . . O(3) C(3) H(49) 110.0 ? . . . C(2) C(3) H(49) 109.9 ? . . . C(4) C(3) H(49) 110.8 ? . . . O(4) C(4) H(50) 107.0 ? . . . C(3) C(4) H(50) 108.3 ? . . . C(5) C(4) H(50) 109.8 ? . . . O(5) C(5) H(51) 108.9 ? . . . C(4) C(5) H(51) 109.9 ? . . . C(6) C(5) H(51) 109.0 ? . . . O(6) C(6) H(43) 110.7 ? . . . O(6) C(6) H(44) 108.7 ? . . . C(5) C(6) H(43) 109.5 ? . . . C(5) C(6) H(44) 108.7 ? . . . H(43) C(6) H(44) 109.2 ? . . . O(4) C(7) H(52) 107.5 ? . . . O(6) C(7) H(52) 108.2 ? . . . C(8) C(7) H(52) 108.2 ? . . . C(7) C(8) H(9) 109.6 ? . . . C(7) C(8) H(10) 108.4 ? . . . C(7) C(8) H(11) 108.5 ? . . . H(9) C(8) H(10) 110.3 ? . . . H(9) C(8) H(11) 110.6 ? . . . H(10) C(8) H(11) 109.4 ? . . . N(1) C(9) H(4) 116.2 ? . . . C(10) C(9) H(4) 118.6 ? . . . C(12) C(13) H(1) 117.1 ? . . . C(14) C(13) H(1) 119.6 ? . . . C(13) C(14) H(2) 119.1 ? . . . C(15) C(14) H(2) 120.9 ? . . . C(10) C(15) H(3) 118.2 ? . . . C(14) C(15) H(3) 121.6 ? . . . C(16) C(17) H(18) 110.0 ? . . . C(16) C(17) H(19) 108.6 ? . . . C(16) C(17) H(20) 110.3 ? . . . H(18) C(17) H(19) 109.0 ? . . . H(18) C(17) H(20) 110.3 ? . . . H(19) C(17) H(20) 108.7 ? . . . C(16) C(18) H(15) 108.1 ? . . . C(16) C(18) H(16) 110.3 ? . . . C(16) C(18) H(17) 109.5 ? . . . H(15) C(18) H(16) 108.9 ? . . . H(15) C(18) H(17) 108.1 ? . . . H(16) C(18) H(17) 111.9 ? . . . C(16) C(19) H(21) 109.3 ? . . . C(16) C(19) H(22) 106.4 ? . . . C(16) C(19) H(23) 108.5 ? . . . H(21) C(19) H(22) 110.1 ? . . . H(21) C(19) H(23) 113.0 ? . . . H(22) C(19) H(23) 109.3 ? . . . O(11) C(20) H(53) 108.5 ? . . . N(2) C(20) H(53) 109.3 ? . . . C(21) C(20) H(53) 109.0 ? . . . O(8) C(21) H(54) 109.3 ? . . . C(20) C(21) H(54) 109.3 ? . . . C(22) C(21) H(54) 108.9 ? . . . O(9) C(22) H(55) 111.8 ? . . . C(21) C(22) H(55) 110.3 ? . . . C(23) C(22) H(55) 110.2 ? . . . O(10) C(23) H(56) 108.7 ? . . . C(22) C(23) H(56) 108.9 ? . . . C(24) C(23) H(56) 108.3 ? . . . O(11) C(24) H(57) 108.8 ? . . . C(23) C(24) H(57) 110.0 ? . . . C(25) C(24) H(57) 109.7 ? . . . O(12) C(25) H(45) 109.5 ? . . . O(12) C(25) H(46) 109.4 ? . . . C(24) C(25) H(45) 110.5 ? . . . C(24) C(25) H(46) 109.3 ? . . . H(45) C(25) H(46) 110.1 ? . . . O(10) C(26) H(58) 108.3 ? . . . O(12) C(26) H(58) 108.6 ? . . . C(27) C(26) H(58) 109.5 ? . . . C(26) C(27) H(24) 111.5 ? . . . C(26) C(27) H(25) 109.5 ? . . . C(26) C(27) H(26) 111.2 ? . . . H(24) C(27) H(25) 107.3 ? . . . H(24) C(27) H(26) 109.7 ? . . . H(25) C(27) H(26) 107.6 ? . . . N(2) C(28) H(8) 119.7 ? . . . C(29) C(28) H(8) 115.9 ? . . . C(31) C(32) H(5) 119.8 ? . . . C(33) C(32) H(5) 116.7 ? . . . C(32) C(33) H(6) 120.9 ? . . . C(34) C(33) H(6) 120.5 ? . . . C(29) C(34) H(7) 120.1 ? . . . C(33) C(34) H(7) 119.1 ? . . . C(35) C(36) H(30) 110.3 ? . . . C(35) C(36) H(31) 110.7 ? . . . C(35) C(36) H(32) 110.9 ? . . . H(30) C(36) H(31) 108.4 ? . . . H(30) C(36) H(32) 108.4 ? . . . H(31) C(36) H(32) 108.1 ? . . . C(35) C(37) H(27) 109.7 ? . . . C(35) C(37) H(28) 109.2 ? . . . C(35) C(37) H(29) 109.2 ? . . . H(27) C(37) H(28) 109.0 ? . . . H(27) C(37) H(29) 109.8 ? . . . H(28) C(37) H(29) 110.0 ? . . . C(35) C(38) H(33) 109.2 ? . . . C(35) C(38) H(34) 109.5 ? . . . C(35) C(38) H(35) 110.8 ? . . . H(33) C(38) H(34) 108.2 ? . . . H(33) C(38) H(35) 109.2 ? . . . H(34) C(38) H(35) 109.9 ? . . . N(3) C(39) H(39) 107.0 ? . . . N(3) C(39) H(40) 108.2 ? . . . C(40) C(39) H(39) 109.2 ? . . . C(40) C(39) H(40) 110.0 ? . . . H(39) C(39) H(40) 110.3 ? . . . C(39) C(40) H(12) 108.3 ? . . . C(39) C(40) H(13) 108.7 ? . . . C(39) C(40) H(14) 107.7 ? . . . H(12) C(40) H(13) 110.6 ? . . . H(12) C(40) H(14) 110.9 ? . . . H(13) C(40) H(14) 110.6 ? . . . N(4) C(41) H(41) 109.9 ? . . . N(4) C(41) H(42) 111.4 ? . . . C(42) C(41) H(41) 107.6 ? . . . C(42) C(41) H(42) 109.9 ? . . . H(41) C(41) H(42) 109.1 ? . . . C(41) C(42) H(36) 110.0 ? . . . C(41) C(42) H(37) 112.0 ? . . . C(41) C(42) H(38) 112.8 ? . . . H(36) C(42) H(37) 106.1 ? . . . H(36) C(42) H(38) 107.2 ? . . . H(37) C(42) H(38) 108.3 ? . . .