# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD Shinobu Itoh' _publ_contact_author_email SHINOBU@SCI.OSAKA-CU.AC.JP _publ_section_title ; Reaction of ?-Diketiminate Copper(II) Complexes and Na2S2 ; loop_ _publ_author_name 'Shinobu Itoh' 'Masayuki Inosako' 'Minoru Kubo' 'Atsushi Kunishita' 'Takashi Ogura' 'Chizu Shimokawa' ; H.Sugimoto ; 'Junji Teraoka' # Attachment 'B808678H.CIF' #============================================================================== data___3a _database_code_depnum_ccdc_archive 'CCDC 688667' #============================================================================== _audit_creation_date 2008-07-26 _audit_creation_method 'by CrystalStructure 3.8' # CHEMICAL DATA _chemical_formula_sum 'C31 H44 Cu N2 O2 ' _chemical_formula_moiety 'C31 H44 Cu N2 O2 ' _chemical_formula_weight 540.25 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 13.943(5) _cell_length_b 14.355(4) _cell_length_c 16.170(5) _cell_angle_alpha 90.0000 _cell_angle_beta 106.237(7) _cell_angle_gamma 90.0000 _cell_volume 3107.3(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5209 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156.00 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.578 _exptl_absorpt_correction_T_max 0.839 #============================================================================== # 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 15213 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed 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 3541 _reflns_number_gt 2304 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1403 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2331 _refine_ls_number_parameters 193 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0023Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.73 _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) ; 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 1.0000 0.34957(4) 0.7500 0.04755(19) Uani 1.00 2 d S . . O(1) O 0.9243(2) 0.2306(2) 0.7512(2) 0.1018(13) Uani 1.00 1 d . . . N(1) N 0.90533(18) 0.43757(18) 0.76756(17) 0.0402(7) Uani 1.00 1 d . . . C(1) C 1.000000(10) 0.5723(3) 0.750000(10) 0.0473(13) Uani 1.00 2 d S . . C(2) C 0.9176(2) 0.5288(2) 0.7674(2) 0.0412(8) Uani 1.00 1 d . . . C(3) C 0.8400(2) 0.5923(2) 0.7868(2) 0.0638(12) Uani 1.00 1 d . . . C(4) C 0.8145(2) 0.4003(2) 0.7803(2) 0.0426(9) Uani 1.00 1 d . . . C(5) C 0.8154(2) 0.3668(2) 0.8618(2) 0.0511(10) Uani 1.00 1 d . . . C(6) C 0.7261(3) 0.3307(2) 0.8715(2) 0.0632(12) Uani 1.00 1 d . . . C(7) C 0.6414(2) 0.3280(2) 0.8045(3) 0.0694(13) Uani 1.00 1 d . . . C(8) C 0.6425(2) 0.3593(2) 0.7246(3) 0.0646(12) Uani 1.00 1 d . . . C(9) C 0.7290(2) 0.3959(2) 0.7106(2) 0.0506(10) Uani 1.00 1 d . . . C(10) C 0.9069(3) 0.3702(3) 0.9378(2) 0.0700(13) Uani 1.00 1 d . . . C(11) C 0.9428(4) 0.2729(4) 0.9699(4) 0.117(2) Uani 1.00 1 d . . . C(12) C 0.8898(4) 0.4280(4) 1.0108(3) 0.113(2) Uani 1.00 1 d . . . C(13) C 0.7304(3) 0.4265(3) 0.6208(2) 0.0655(12) Uani 1.00 1 d . . . C(14) C 0.7410(5) 0.3411(4) 0.5676(3) 0.118(2) Uani 1.00 1 d . . . C(15) C 0.6381(4) 0.4828(4) 0.5741(3) 0.124(2) Uani 1.00 1 d . . . C(16) C 1.0000 0.1868(4) 0.7500 0.097(2) Uani 1.00 2 d S . . C(17) C 1.000000(10) 0.0826(4) 0.750000(10) 0.174(5) Uani 1.00 2 d S . . H(1) H 1.0000 0.6384 0.7500 0.058 Uiso 1.00 2 c R . . H(2) H 0.7896 0.6084 0.7331 0.082 Uiso 1.00 1 c R . . H(3) H 0.8724 0.6492 0.8145 0.081 Uiso 1.00 1 c R . . H(4) H 0.8077 0.5604 0.8255 0.081 Uiso 1.00 1 c R . . H(5) H 0.7244 0.3076 0.9261 0.081 Uiso 1.00 1 c R . . H(6) H 0.5814 0.3039 0.8129 0.088 Uiso 1.00 1 c R . . H(7) H 0.5831 0.3563 0.6783 0.077 Uiso 1.00 1 c R . . H(8) H 0.9615 0.4003 0.9183 0.086 Uiso 1.00 1 c R . . H(9) H 0.9113 0.2543 1.0145 0.139 Uiso 1.00 1 c R . . H(10) H 1.0155 0.2731 0.9941 0.138 Uiso 1.00 1 c R . . H(11) H 0.9242 0.2288 0.9218 0.138 Uiso 1.00 1 c R . . H(12) H 0.9062 0.4932 1.0027 0.136 Uiso 1.00 1 c R . . H(13) H 0.9327 0.4054 1.0660 0.136 Uiso 1.00 1 c R . . H(14) H 0.8197 0.4234 1.0107 0.136 Uiso 1.00 1 c R . . H(15) H 0.7904 0.4669 0.6269 0.077 Uiso 1.00 1 c R . . H(16) H 0.8121 0.3282 0.5761 0.145 Uiso 1.00 1 c R . . H(17) H 0.7089 0.3534 0.5065 0.145 Uiso 1.00 1 c R . . H(18) H 0.7093 0.2871 0.5863 0.145 Uiso 1.00 1 c R . . H(19) H 0.5863 0.4407 0.5406 0.145 Uiso 1.00 1 c R . . H(20) H 0.6563 0.5276 0.5353 0.145 Uiso 1.00 1 c R . . H(21) H 0.6126 0.5164 0.6163 0.145 Uiso 1.00 1 c R . . H(22) H 1.0208 0.0598 0.8095 0.241 Uiso 0.50 1 c R . . H(23) H 1.0466 0.0598 0.7191 0.241 Uiso 0.50 1 c R . . H(24) H 0.9326 0.0598 0.7214 0.241 Uiso 0.50 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) 0.0422(3) 0.0375(3) 0.0730(4) 0.0000 0.0326(3) 0.0000 O(1) 0.092(2) 0.0469(17) 0.199(3) -0.0110(15) 0.094(2) -0.0156(19) N(1) 0.0330(13) 0.0403(15) 0.0520(15) -0.0013(11) 0.0194(11) -0.0044(11) C(1) 0.044(2) 0.040(2) 0.060(2) 0.0000 0.018(2) 0.0000 C(2) 0.0391(17) 0.0425(18) 0.0452(18) 0.0028(14) 0.0170(14) -0.0041(13) C(3) 0.060(2) 0.044(2) 0.099(3) 0.0039(17) 0.042(2) -0.0067(19) C(4) 0.0376(17) 0.0380(18) 0.060(2) 0.0001(13) 0.0261(15) -0.0092(14) C(5) 0.0448(19) 0.055(2) 0.061(2) -0.0041(15) 0.0275(16) -0.0036(16) C(6) 0.055(2) 0.070(2) 0.077(2) -0.0099(18) 0.039(2) -0.0007(19) C(7) 0.044(2) 0.069(2) 0.107(3) -0.0141(18) 0.041(2) -0.009(2) C(8) 0.0401(19) 0.065(2) 0.088(2) -0.0094(18) 0.0170(19) -0.017(2) C(9) 0.0367(17) 0.055(2) 0.061(2) 0.0000(15) 0.0145(15) -0.0098(16) C(10) 0.055(2) 0.102(3) 0.058(2) -0.009(2) 0.0232(18) 0.006(2) C(11) 0.095(4) 0.133(5) 0.118(4) 0.027(3) 0.023(3) 0.038(3) C(12) 0.112(4) 0.160(6) 0.068(3) -0.027(4) 0.025(3) -0.025(3) C(13) 0.052(2) 0.082(2) 0.059(2) -0.001(2) 0.0091(18) -0.006(2) C(14) 0.140(5) 0.139(5) 0.083(3) -0.021(4) 0.044(3) -0.040(3) C(15) 0.096(4) 0.173(6) 0.094(4) 0.029(4) 0.013(3) 0.040(4) C(16) 0.117(5) 0.041(3) 0.176(7) 0.0000 0.110(5) 0.0000 C(17) 0.211(11) 0.040(3) 0.351(15) 0.0000 0.210(11) 0.0000 #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # 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) 2.011(3) yes . . Cu(1) O(1) 2.011(3) yes . 2_756 Cu(1) N(1) 1.905(2) yes . . Cu(1) N(1) 1.905(2) yes . 2_756 O(1) C(16) 1.233(4) yes . . N(1) C(2) 1.320(4) yes . . N(1) C(4) 1.442(4) yes . . C(1) C(2) 1.403(4) yes . . C(1) C(2) 1.403(4) yes . 2_756 C(2) C(3) 1.514(5) yes . . C(4) C(5) 1.399(5) yes . . C(4) C(9) 1.394(4) yes . . C(5) C(6) 1.396(5) yes . . C(5) C(10) 1.505(4) yes . . C(6) C(7) 1.361(5) yes . . C(7) C(8) 1.371(7) yes . . C(8) C(9) 1.391(5) yes . . C(9) C(13) 1.523(5) yes . . C(10) C(11) 1.525(7) yes . . C(10) C(12) 1.515(7) yes . . C(13) C(14) 1.527(7) yes . . C(13) C(15) 1.529(6) yes . . C(16) C(17) 1.496(9) yes . . C(1) H(1) 0.949 no . . C(3) H(2) 0.980 no . . C(3) H(3) 0.980 no . . C(3) H(4) 0.980 no . . C(6) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(8) H(7) 0.950 no . . C(10) H(8) 1.000 no . . C(11) H(9) 0.980 no . . C(11) H(10) 0.980 no . . C(11) H(11) 0.980 no . . C(12) H(12) 0.980 no . . C(12) H(13) 0.980 no . . C(12) H(14) 0.980 no . . C(13) H(15) 1.000 no . . C(14) H(16) 0.980 no . . C(14) H(17) 0.980 no . . C(14) H(18) 0.980 no . . C(15) H(19) 0.980 no . . C(15) H(20) 0.980 no . . C(15) H(21) 0.980 no . . C(17) H(22) 0.980 no . . C(17) H(22) 0.980 no . 2_756 C(17) H(23) 0.980 no . . C(17) H(23) 0.980 no . 2_756 C(17) H(24) 0.980 no . . C(17) H(24) 0.980 no . 2_756 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(1) 63.70(14) yes . . 2_756 O(1) Cu(1) N(1) 100.04(13) yes . . . O(1) Cu(1) N(1) 162.24(14) yes . . 2_756 O(1) Cu(1) N(1) 162.24(14) yes 2_756 . . O(1) Cu(1) N(1) 100.04(13) yes 2_756 . 2_756 N(1) Cu(1) N(1) 96.91(11) yes . . 2_756 Cu(1) O(1) C(16) 88.8(3) yes . . . Cu(1) N(1) C(2) 124.1(2) yes . . . Cu(1) N(1) C(4) 116.64(19) yes . . . C(2) N(1) C(4) 119.2(2) yes . . . C(2) C(1) C(2) 127.1(4) yes . . 2_756 N(1) C(2) C(1) 123.8(3) yes . . . N(1) C(2) C(3) 119.7(3) yes . . . C(1) C(2) C(3) 116.5(3) yes . . . N(1) C(4) C(5) 119.1(2) yes . . . N(1) C(4) C(9) 119.2(3) yes . . . C(5) C(4) C(9) 121.7(3) yes . . . C(4) C(5) C(6) 117.4(2) yes . . . C(4) C(5) C(10) 122.7(3) yes . . . C(6) C(5) C(10) 120.0(3) yes . . . C(5) C(6) C(7) 121.6(4) yes . . . C(6) C(7) C(8) 120.3(4) yes . . . C(7) C(8) C(9) 121.0(3) yes . . . C(4) C(9) C(8) 118.0(3) yes . . . C(4) C(9) C(13) 121.5(3) yes . . . C(8) C(9) C(13) 120.5(3) yes . . . C(5) C(10) C(11) 111.7(3) yes . . . C(5) C(10) C(12) 111.8(3) yes . . . C(11) C(10) C(12) 110.2(4) yes . . . C(9) C(13) C(14) 109.5(3) yes . . . C(9) C(13) C(15) 113.0(4) yes . . . C(14) C(13) C(15) 110.3(3) yes . . . O(1) C(16) O(1) 118.7(5) yes . . 2_756 O(1) C(16) C(17) 120.6(2) yes . . . O(1) C(16) C(17) 120.6(2) yes 2_756 . . C(2) C(1) H(1) 116.4 no . . . C(2) C(1) H(1) 116.4 no 2_756 . . C(2) C(3) H(2) 109.6 no . . . C(2) C(3) H(3) 109.3 no . . . C(2) C(3) H(4) 109.5 no . . . H(2) C(3) H(3) 109.5 no . . . H(2) C(3) H(4) 109.5 no . . . H(3) C(3) H(4) 109.5 no . . . C(5) C(6) H(5) 119.3 no . . . C(7) C(6) H(5) 119.2 no . . . C(6) C(7) H(6) 120.0 no . . . C(8) C(7) H(6) 119.7 no . . . C(7) C(8) H(7) 119.5 no . . . C(9) C(8) H(7) 119.5 no . . . C(5) C(10) H(8) 107.6 no . . . C(11) C(10) H(8) 107.3 no . . . C(12) C(10) H(8) 108.0 no . . . C(10) C(11) H(9) 109.2 no . . . C(10) C(11) H(10) 109.7 no . . . C(10) C(11) H(11) 109.5 no . . . H(9) C(11) H(10) 109.5 no . . . H(9) C(11) H(11) 109.5 no . . . H(10) C(11) H(11) 109.5 no . . . C(10) C(12) H(12) 109.0 no . . . C(10) C(12) H(13) 109.8 no . . . C(10) C(12) H(14) 109.6 no . . . H(12) C(12) H(13) 109.5 no . . . H(12) C(12) H(14) 109.5 no . . . H(13) C(12) H(14) 109.5 no . . . C(9) C(13) H(15) 107.9 no . . . C(14) C(13) H(15) 108.1 no . . . C(15) C(13) H(15) 107.9 no . . . C(13) C(14) H(16) 109.1 no . . . C(13) C(14) H(17) 109.5 no . . . C(13) C(14) H(18) 109.8 no . . . H(16) C(14) H(17) 109.5 no . . . H(16) C(14) H(18) 109.5 no . . . H(17) C(14) H(18) 109.5 no . . . C(13) C(15) H(19) 109.6 no . . . C(13) C(15) H(20) 109.3 no . . . C(13) C(15) H(21) 109.6 no . . . H(19) C(15) H(20) 109.5 no . . . H(19) C(15) H(21) 109.5 no . . . H(20) C(15) H(21) 109.5 no . . . C(16) C(17) H(22) 109.5 no . . . C(16) C(17) H(22) 109.5 no . . 2_756 C(16) C(17) H(23) 109.5 no . . . C(16) C(17) H(23) 109.5 no . . 2_756 C(16) C(17) H(24) 109.5 no . . . C(16) C(17) H(24) 109.5 no . . 2_756 H(22) C(17) H(22) 140.9 no . . 2_756 H(22) C(17) H(23) 109.4 no . . . H(22) C(17) H(23) 56.2 no . . 2_756 H(22) C(17) H(24) 109.4 no . . . H(22) C(17) H(24) 56.2 no . . 2_756 H(22) C(17) H(23) 56.2 no 2_756 . . H(22) C(17) H(23) 109.4 no 2_756 . 2_756 H(22) C(17) H(24) 56.2 no 2_756 . . H(22) C(17) H(24) 109.4 no 2_756 . 2_756 H(23) C(17) H(23) 140.9 no . . 2_756 H(23) C(17) H(24) 109.4 no . . . H(23) C(17) H(24) 56.2 no . . 2_756 H(23) C(17) H(24) 56.2 no 2_756 . . H(23) C(17) H(24) 109.4 no 2_756 . 2_756 H(24) C(17) H(24) 140.9 no . . 2_756 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Cu(1) N(1) C(2) -176.3(2) ? . . . . O(1) Cu(1) N(1) C(4) 2.7(2) ? . . . . N(1) Cu(1) O(1) C(16) -172.43(18) ? . . . . O(1) Cu(1) N(1) C(2) 161.0(3) ? . . 2_756 2_756 O(1) Cu(1) N(1) C(4) -20.0(5) ? . . 2_756 2_756 N(1) Cu(1) O(1) C(16) 25.2(5) ? 2_756 . . . O(1) Cu(1) N(1) C(2) 161.0(3) ? 2_756 . . . O(1) Cu(1) N(1) C(4) -20.0(5) ? 2_756 . . . N(1) Cu(1) O(1) C(16) 25.2(5) ? . . 2_756 . O(1) Cu(1) N(1) C(2) -176.3(2) ? 2_756 . 2_756 2_756 O(1) Cu(1) N(1) C(4) 2.7(2) ? 2_756 . 2_756 2_756 N(1) Cu(1) O(1) C(16) -172.43(18) ? 2_756 . 2_756 . N(1) Cu(1) N(1) C(2) -1.6(2) ? . . 2_756 2_756 N(1) Cu(1) N(1) C(4) 177.4(2) ? . . 2_756 2_756 N(1) Cu(1) N(1) C(2) -1.6(2) ? 2_756 . . . N(1) Cu(1) N(1) C(4) 177.4(2) ? 2_756 . . . Cu(1) N(1) C(2) C(1) 3.3(3) ? . . . . Cu(1) N(1) C(2) C(3) -176.7(2) ? . . . . Cu(1) N(1) C(4) C(5) 80.5(3) ? . . . . Cu(1) N(1) C(4) C(9) -97.5(3) ? . . . . C(2) N(1) C(4) C(5) -100.5(3) ? . . . . C(2) N(1) C(4) C(9) 81.5(3) ? . . . . C(4) N(1) C(2) C(1) -175.7(2) ? . . . . C(4) N(1) C(2) C(3) 4.3(4) ? . . . . C(2) C(1) C(2) N(1) -1.8(3) ? . . 2_756 2_756 C(2) C(1) C(2) C(3) 178.2(2) ? . . 2_756 2_756 C(2) C(1) C(2) N(1) -1.8(3) ? 2_756 . . . C(2) C(1) C(2) C(3) 178.2(2) ? 2_756 . . . N(1) C(4) C(5) C(6) -179.6(3) ? . . . . N(1) C(4) C(5) C(10) 1.6(5) ? . . . . N(1) C(4) C(9) C(8) 179.7(3) ? . . . . N(1) C(4) C(9) C(13) 2.1(5) ? . . . . C(5) C(4) C(9) C(8) 1.8(5) ? . . . . C(5) C(4) C(9) C(13) -175.9(3) ? . . . . C(9) C(4) C(5) C(6) -1.6(5) ? . . . . C(9) C(4) C(5) C(10) 179.6(3) ? . . . . C(4) C(5) C(6) C(7) 0.0(4) ? . . . . C(4) C(5) C(10) C(11) -116.7(4) ? . . . . C(4) C(5) C(10) C(12) 119.3(4) ? . . . . C(6) C(5) C(10) C(11) 64.6(5) ? . . . . C(6) C(5) C(10) C(12) -59.5(5) ? . . . . C(10) C(5) C(6) C(7) 178.9(4) ? . . . . C(5) C(6) C(7) C(8) 1.4(6) ? . . . . C(6) C(7) C(8) C(9) -1.2(6) ? . . . . C(7) C(8) C(9) C(4) -0.3(5) ? . . . . C(7) C(8) C(9) C(13) 177.3(3) ? . . . . C(4) C(9) C(13) C(14) 98.7(4) ? . . . . C(4) C(9) C(13) C(15) -137.9(4) ? . . . . C(8) C(9) C(13) C(14) -78.9(5) ? . . . . C(8) C(9) C(13) C(15) 44.5(5) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C(14) C(14) 3.464(8) ? . 7_656 O(1) H(2) 3.530 ? . 6_646 C(1) H(6) 3.568 ? . 5_555 C(1) H(6) 3.568 ? . 6_656 C(1) H(13) 2.877 ? . 3_767 C(1) H(13) 2.877 ? . 4_564 C(2) H(13) 3.060 ? . 3_767 C(2) H(13) 3.454 ? . 4_564 C(3) H(13) 3.391 ? . 3_767 C(6) H(2) 3.589 ? . 6_646 C(6) H(9) 3.246 ? . 7_657 C(7) H(1) 3.331 ? . 5_445 C(7) H(2) 3.400 ? . 6_646 C(7) H(3) 3.181 ? . 6_646 C(7) H(6) 3.175 ? . 2_656 C(7) H(7) 3.245 ? . 2_656 C(7) H(9) 3.421 ? . 7_657 C(7) H(24) 3.475 ? . 6_656 C(8) H(3) 3.076 ? . 6_646 C(8) H(6) 3.112 ? . 2_656 C(8) H(23) 3.165 ? . 5_455 C(8) H(24) 3.265 ? . 6_656 C(9) H(23) 3.495 ? . 5_455 C(10) H(12) 3.188 ? . 3_767 C(11) H(5) 3.434 ? . 7_657 C(12) H(8) 3.218 ? . 3_767 C(12) H(12) 3.125 ? . 3_767 C(12) H(15) 3.029 ? . 4_565 C(12) H(20) 3.448 ? . 4_565 C(13) H(14) 3.255 ? . 4_564 C(14) H(10) 3.449 ? . 8_454 C(14) H(16) 3.301 ? . 7_656 C(14) H(17) 3.192 ? . 7_656 C(14) H(18) 3.321 ? . 7_656 C(15) H(14) 3.275 ? . 4_564 C(15) H(19) 3.345 ? . 3_666 C(15) H(22) 3.464 ? . 6_656 C(15) H(23) 3.165 ? . 5_455 C(17) H(21) 3.152 ? . 5_545 C(17) H(21) 3.152 ? . 6_646 H(1) C(7) 3.331 ? . 5_555 H(1) C(7) 3.331 ? . 6_656 H(1) H(6) 2.705 ? . 5_555 H(1) H(6) 2.705 ? . 6_656 H(1) H(13) 2.927 ? . 3_767 H(1) H(13) 2.927 ? . 4_564 H(2) O(1) 3.530 ? . 6_656 H(2) C(6) 3.589 ? . 6_656 H(2) C(7) 3.400 ? . 6_656 H(2) H(6) 3.523 ? . 6_656 H(2) H(23) 3.404 ? . 5_455 H(2) H(24) 3.450 ? . 6_656 H(3) C(7) 3.181 ? . 6_656 H(3) C(8) 3.076 ? . 6_656 H(3) H(6) 3.214 ? . 6_656 H(3) H(7) 3.033 ? . 6_656 H(3) H(10) 3.249 ? . 3_767 H(3) H(13) 2.966 ? . 3_767 H(3) H(18) 2.970 ? . 6_656 H(4) H(13) 3.587 ? . 3_767 H(4) H(18) 3.589 ? . 6_656 H(4) H(23) 3.566 ? . 5_455 H(4) H(24) 3.222 ? . 6_656 H(5) C(11) 3.434 ? . 7_657 H(5) H(5) 2.829 ? . 7_657 H(5) H(9) 2.512 ? . 7_657 H(5) H(14) 3.574 ? . 7_657 H(5) H(20) 3.249 ? . 4_565 H(6) C(1) 3.568 ? . 5_445 H(6) C(7) 3.175 ? . 2_656 H(6) C(8) 3.112 ? . 2_656 H(6) H(1) 2.705 ? . 5_445 H(6) H(2) 3.523 ? . 6_646 H(6) H(3) 3.214 ? . 6_646 H(6) H(6) 2.590 ? . 2_656 H(6) H(7) 2.456 ? . 2_656 H(6) H(9) 2.888 ? . 7_657 H(7) C(7) 3.245 ? . 2_656 H(7) H(3) 3.033 ? . 6_646 H(7) H(6) 2.456 ? . 2_656 H(7) H(9) 3.424 ? . 8_454 H(7) H(10) 3.411 ? . 8_454 H(7) H(22) 3.291 ? . 6_656 H(7) H(23) 3.068 ? . 5_455 H(7) H(24) 3.378 ? . 6_656 H(8) C(12) 3.218 ? . 3_767 H(8) H(12) 2.461 ? . 3_767 H(8) H(13) 3.132 ? . 3_767 H(9) C(6) 3.246 ? . 7_657 H(9) C(7) 3.421 ? . 7_657 H(9) H(5) 2.512 ? . 7_657 H(9) H(6) 2.888 ? . 7_657 H(9) H(7) 3.424 ? . 8_555 H(9) H(20) 3.421 ? . 6_646 H(10) C(14) 3.449 ? . 8_555 H(10) H(3) 3.249 ? . 3_767 H(10) H(7) 3.411 ? . 8_555 H(10) H(12) 3.524 ? . 3_767 H(10) H(17) 3.210 ? . 8_555 H(10) H(18) 2.831 ? . 8_555 H(10) H(19) 3.248 ? . 8_555 H(11) H(19) 3.506 ? . 8_555 H(11) H(20) 3.242 ? . 6_646 H(11) H(21) 3.124 ? . 6_646 H(12) C(10) 3.188 ? . 3_767 H(12) C(12) 3.125 ? . 3_767 H(12) H(8) 2.461 ? . 3_767 H(12) H(10) 3.524 ? . 3_767 H(12) H(12) 2.650 ? . 3_767 H(12) H(13) 3.129 ? . 3_767 H(12) H(15) 2.963 ? . 4_565 H(12) H(16) 3.251 ? . 4_565 H(12) H(17) 3.538 ? . 4_565 H(13) C(1) 2.877 ? . 3_767 H(13) C(2) 3.060 ? . 3_767 H(13) C(2) 3.454 ? . 4_565 H(13) C(3) 3.391 ? . 3_767 H(13) H(1) 2.927 ? . 3_767 H(13) H(3) 2.966 ? . 3_767 H(13) H(4) 3.587 ? . 3_767 H(13) H(8) 3.132 ? . 3_767 H(13) H(12) 3.129 ? . 3_767 H(13) H(15) 3.059 ? . 4_565 H(14) C(13) 3.255 ? . 4_565 H(14) C(15) 3.275 ? . 4_565 H(14) H(5) 3.574 ? . 7_657 H(14) H(15) 2.569 ? . 4_565 H(14) H(17) 3.549 ? . 4_565 H(14) H(20) 2.520 ? . 4_565 H(15) C(12) 3.029 ? . 4_564 H(15) H(12) 2.963 ? . 4_564 H(15) H(13) 3.059 ? . 4_564 H(15) H(14) 2.569 ? . 4_564 H(16) C(14) 3.301 ? . 7_656 H(16) H(12) 3.251 ? . 4_564 H(16) H(16) 3.422 ? . 7_656 H(16) H(17) 2.906 ? . 7_656 H(16) H(18) 3.047 ? . 7_656 H(17) C(14) 3.192 ? . 7_656 H(17) H(10) 3.210 ? . 8_454 H(17) H(12) 3.538 ? . 4_564 H(17) H(14) 3.549 ? . 4_564 H(17) H(16) 2.906 ? . 7_656 H(17) H(17) 3.209 ? . 7_656 H(17) H(18) 2.929 ? . 7_656 H(18) C(14) 3.321 ? . 7_656 H(18) H(3) 2.970 ? . 6_646 H(18) H(4) 3.589 ? . 6_646 H(18) H(10) 2.831 ? . 8_454 H(18) H(16) 3.047 ? . 7_656 H(18) H(17) 2.929 ? . 7_656 H(18) H(18) 3.461 ? . 7_656 H(19) C(15) 3.345 ? . 3_666 H(19) H(10) 3.248 ? . 8_454 H(19) H(11) 3.506 ? . 8_454 H(19) H(19) 2.940 ? . 3_666 H(19) H(20) 3.291 ? . 3_666 H(19) H(21) 3.252 ? . 3_666 H(19) H(22) 3.591 ? . 8_454 H(19) H(23) 3.528 ? . 5_455 H(20) C(12) 3.448 ? . 4_564 H(20) H(5) 3.249 ? . 4_564 H(20) H(9) 3.421 ? . 6_656 H(20) H(11) 3.242 ? . 6_656 H(20) H(14) 2.520 ? . 4_564 H(20) H(19) 3.291 ? . 3_666 H(21) C(17) 3.152 ? . 5_455 H(21) H(11) 3.124 ? . 6_656 H(21) H(19) 3.252 ? . 3_666 H(21) H(22) 2.556 ? . 6_656 H(21) H(23) 2.203 ? . 5_455 H(21) H(24) 3.458 ? . 5_455 H(21) H(24) 2.932 ? . 6_656 H(22) C(15) 3.464 ? . 6_646 H(22) H(7) 3.291 ? . 6_646 H(22) H(19) 3.591 ? . 8_555 H(22) H(21) 2.556 ? . 6_646 H(23) C(8) 3.165 ? . 5_545 H(23) C(9) 3.495 ? . 5_545 H(23) C(15) 3.165 ? . 5_545 H(23) H(2) 3.404 ? . 5_545 H(23) H(4) 3.566 ? . 5_545 H(23) H(7) 3.068 ? . 5_545 H(23) H(19) 3.528 ? . 5_545 H(23) H(21) 2.203 ? . 5_545 H(24) C(7) 3.475 ? . 6_646 H(24) C(8) 3.265 ? . 6_646 H(24) H(2) 3.450 ? . 6_646 H(24) H(4) 3.222 ? . 6_646 H(24) H(7) 3.378 ? . 6_646 H(24) H(21) 3.458 ? . 5_545 H(24) H(21) 2.932 ? . 6_646 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #===END #============================================================================== data___4a _database_code_depnum_ccdc_archive 'CCDC 688668' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H36 Cu N2 O2 ' _chemical_formula_moiety 'C27 H36 Cu N2 O2 ' _chemical_formula_weight 484.14 _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 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 8.015(6) _cell_length_b 8.546(7) _cell_length_c 19.929(17) _cell_angle_alpha 88.52(2) _cell_angle_beta 83.23(2) _cell_angle_gamma 67.570(18) _cell_volume 1252.8(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3444 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 113.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 514.00 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.973 #============================================================================== # 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 9984 _diffrn_reflns_av_R_equivalents 0.077 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.968 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 3.0 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 5545 _reflns_number_gt 3586 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.1944 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3586 _refine_ls_number_parameters 325 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.23 _refine_diff_density_min -1.57 _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 0.31638(10) 0.38242(10) 0.27154(4) 0.02088(18) Uani 1.00 1 d . . . O(1) O 0.5351(6) 0.1750(5) 0.2918(2) 0.0317(12) Uani 1.00 1 d . . . O(2) O 0.3499(6) 0.3443(6) 0.3704(2) 0.0362(13) Uani 1.00 1 d . . . N(1) N 0.3510(6) 0.3772(6) 0.1745(2) 0.0197(12) Uani 1.00 1 d . . . N(2) N 0.0933(6) 0.5783(6) 0.2822(2) 0.0238(13) Uani 1.00 1 d . . . C(1) C 0.0857(8) 0.6312(8) 0.1634(3) 0.0253(15) Uani 1.00 1 d . . . C(2) C 0.2407(8) 0.4934(8) 0.1373(3) 0.0249(15) Uani 1.00 1 d . . . C(3) C 0.0186(8) 0.6699(7) 0.2316(3) 0.0210(14) Uani 1.00 1 d . . . C(4) C 0.2819(8) 0.4829(8) 0.0611(3) 0.0276(16) Uani 1.00 1 d . . . C(5) C -0.1490(8) 0.8328(8) 0.2468(3) 0.0291(16) Uani 1.00 1 d . . . C(6) C 0.5054(7) 0.2422(7) 0.1402(3) 0.0232(15) Uani 1.00 1 d . . . C(7) C 0.6772(8) 0.2514(8) 0.1356(3) 0.0250(15) Uani 1.00 1 d . . . C(8) C 0.8216(8) 0.1265(8) 0.0964(3) 0.0270(16) Uani 1.00 1 d . . . C(9) C 0.7952(8) -0.0031(8) 0.0637(3) 0.0262(15) Uani 1.00 1 d . . . C(10) C 0.6267(8) -0.0120(9) 0.0728(3) 0.0266(16) Uani 1.00 1 d . . . C(11) C 0.4793(8) 0.1055(8) 0.1112(2) 0.0225(14) Uani 1.00 1 d . . . C(12) C 0.7119(9) 0.3899(8) 0.1698(3) 0.0293(17) Uani 1.00 1 d . . . C(13) C 0.6707(12) 0.5507(10) 0.1294(4) 0.047(2) Uani 1.00 1 d . . . C(14) C 0.3002(8) 0.0857(9) 0.1221(3) 0.0275(16) Uani 1.00 1 d . . . C(15) C 0.2775(10) -0.0018(10) 0.1886(4) 0.042(2) Uani 1.00 1 d . . . C(16) C 0.0165(7) 0.6310(7) 0.3509(3) 0.0205(14) Uani 1.00 1 d . . . C(17) C -0.1224(7) 0.5803(7) 0.3817(3) 0.0221(15) Uani 1.00 1 d . . . C(18) C -0.1872(8) 0.6290(8) 0.4485(3) 0.0265(16) Uani 1.00 1 d . . . C(19) C -0.1156(8) 0.7201(7) 0.4854(3) 0.0244(15) Uani 1.00 1 d . . . C(20) C 0.0189(8) 0.7695(7) 0.4539(3) 0.0241(15) Uani 1.00 1 d . . . C(21) C 0.0894(7) 0.7256(7) 0.3860(3) 0.0216(15) Uani 1.00 1 d . . . C(22) C -0.1954(8) 0.4763(8) 0.3430(3) 0.0292(17) Uani 1.00 1 d . . . C(23) C -0.0733(9) 0.2852(9) 0.3401(4) 0.037(2) Uani 1.00 1 d . . . C(24) C 0.2376(9) 0.7724(9) 0.3509(3) 0.0321(18) Uani 1.00 1 d . . . C(25) C 0.3238(10) 0.8589(10) 0.3944(4) 0.041(2) Uani 1.00 1 d . . . C(26) C 0.4900(8) 0.2133(8) 0.3544(3) 0.0237(15) Uani 1.00 1 d . . . C(27) C 0.5975(8) 0.1111(9) 0.4073(3) 0.0285(16) Uani 1.00 1 d . . . H(1) H 0.0211 0.7077 0.1313 0.027 Uiso 1.00 1 c R . . H(2) H 0.3578 0.5427 0.0469 0.030 Uiso 1.00 1 c R . . H(3) H 0.1712 0.5313 0.0416 0.030 Uiso 1.00 1 c R . . H(4) H 0.3417 0.3675 0.0471 0.030 Uiso 1.00 1 c R . . H(5) H -0.2549 0.8074 0.2483 0.031 Uiso 1.00 1 c R . . H(6) H -0.1511 0.9125 0.2124 0.031 Uiso 1.00 1 c R . . H(7) H -0.1459 0.8791 0.2892 0.030 Uiso 1.00 1 c R . . H(8) H 0.9391 0.1307 0.0925 0.030 Uiso 1.00 1 c R . . H(9) H 0.8922 -0.0826 0.0351 0.027 Uiso 1.00 1 c R . . H(10) H 0.6115 -0.1043 0.0524 0.030 Uiso 1.00 1 c R . . H(11) H 0.6364 0.4171 0.2117 0.035 Uiso 1.00 1 c R . . H(12) H 0.8358 0.3483 0.1777 0.035 Uiso 1.00 1 c R . . H(13) H 0.7776 0.5447 0.1014 0.061 Uiso 1.00 1 c R . . H(14) H 0.6328 0.6452 0.1597 0.061 Uiso 1.00 1 c R . . H(15) H 0.5772 0.5633 0.1021 0.061 Uiso 1.00 1 c R . . H(16) H 0.2052 0.1945 0.1228 0.032 Uiso 1.00 1 c R . . H(17) H 0.2922 0.0191 0.0861 0.032 Uiso 1.00 1 c R . . H(18) H 0.3237 -0.1210 0.1813 0.048 Uiso 1.00 1 c R . . H(19) H 0.1529 0.0369 0.2063 0.048 Uiso 1.00 1 c R . . H(20) H 0.3438 0.0250 0.2199 0.048 Uiso 1.00 1 c R . . H(21) H -0.2831 0.5991 0.4697 0.029 Uiso 1.00 1 c R . . H(22) H -0.1592 0.7478 0.5317 0.026 Uiso 1.00 1 c R . . H(23) H 0.0677 0.8314 0.4791 0.025 Uiso 1.00 1 c R . . H(24) H -0.3135 0.4909 0.3636 0.034 Uiso 1.00 1 c R . . H(25) H -0.2022 0.5156 0.2980 0.034 Uiso 1.00 1 c R . . H(26) H 0.0160 0.2605 0.3018 0.044 Uiso 1.00 1 c R . . H(27) H -0.1457 0.2203 0.3373 0.044 Uiso 1.00 1 c R . . H(28) H -0.0152 0.2578 0.3801 0.044 Uiso 1.00 1 c R . . H(29) H 0.3308 0.6705 0.3329 0.038 Uiso 1.00 1 c R . . H(30) H 0.1921 0.8460 0.3150 0.038 Uiso 1.00 1 c R . . H(31) H 0.2612 0.9782 0.3932 0.050 Uiso 1.00 1 c R . . H(32) H 0.4481 0.8300 0.3778 0.050 Uiso 1.00 1 c R . . H(33) H 0.3144 0.8222 0.4395 0.050 Uiso 1.00 1 c R . . H(34) H 0.5531 0.0260 0.4218 0.033 Uiso 1.00 1 c R . . H(35) H 0.5864 0.1829 0.4445 0.033 Uiso 1.00 1 c R . . H(36) H 0.7217 0.0594 0.3893 0.033 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) 0.0134(3) 0.0211(4) 0.0210(3) 0.0006(2) 0.0009(2) -0.0019(2) O(1) 0.029(2) 0.028(2) 0.021(2) 0.008(2) -0.0038(19) -0.0028(19) O(2) 0.027(2) 0.037(2) 0.026(2) 0.008(2) 0.000(2) -0.002(2) N(1) 0.016(2) 0.018(2) 0.022(2) -0.003(2) -0.0014(19) -0.004(2) N(2) 0.020(2) 0.024(2) 0.024(2) -0.005(2) -0.000(2) 0.003(2) C(1) 0.021(3) 0.026(3) 0.022(3) 0.000(2) -0.007(2) 0.002(2) C(2) 0.019(2) 0.023(3) 0.027(3) -0.004(2) 0.002(2) 0.000(2) C(3) 0.021(2) 0.016(2) 0.023(3) -0.004(2) -0.003(2) 0.002(2) C(4) 0.026(3) 0.032(3) 0.018(3) -0.004(2) 0.001(2) 0.003(2) C(5) 0.025(3) 0.034(3) 0.017(2) -0.000(2) 0.003(2) -0.001(2) C(6) 0.015(2) 0.018(3) 0.029(3) 0.001(2) -0.001(2) -0.001(2) C(7) 0.022(3) 0.029(3) 0.021(2) -0.006(2) -0.000(2) -0.006(2) C(8) 0.016(2) 0.035(3) 0.023(3) -0.003(2) 0.004(2) -0.002(2) C(9) 0.019(2) 0.026(3) 0.023(3) 0.003(2) 0.001(2) -0.008(2) C(10) 0.026(3) 0.031(3) 0.019(2) -0.006(2) -0.003(2) -0.003(2) C(11) 0.024(3) 0.024(3) 0.014(2) -0.003(2) -0.002(2) -0.000(2) C(12) 0.027(3) 0.030(3) 0.030(3) -0.010(2) -0.000(2) -0.007(2) C(13) 0.052(5) 0.044(4) 0.056(5) -0.028(4) -0.010(4) 0.000(4) C(14) 0.020(3) 0.035(3) 0.025(3) -0.009(2) 0.003(2) 0.001(2) C(15) 0.028(3) 0.039(4) 0.053(4) -0.012(3) 0.014(3) -0.001(3) C(16) 0.015(2) 0.021(3) 0.020(2) -0.002(2) 0.004(2) -0.001(2) C(17) 0.014(2) 0.021(3) 0.029(3) -0.005(2) 0.003(2) -0.005(2) C(18) 0.014(2) 0.023(3) 0.036(3) -0.001(2) 0.004(2) -0.004(2) C(19) 0.026(3) 0.020(3) 0.018(2) -0.000(2) 0.004(2) -0.005(2) C(20) 0.023(3) 0.016(3) 0.025(3) 0.002(2) 0.001(2) -0.006(2) C(21) 0.014(2) 0.020(3) 0.027(3) -0.003(2) -0.006(2) 0.002(2) C(22) 0.016(2) 0.029(3) 0.040(3) -0.008(2) 0.005(2) -0.010(2) C(23) 0.028(3) 0.039(4) 0.043(4) -0.013(3) 0.002(3) -0.005(3) C(24) 0.024(3) 0.041(4) 0.029(3) -0.011(3) 0.001(2) -0.001(3) C(25) 0.034(3) 0.040(4) 0.052(4) -0.019(3) 0.004(3) -0.020(3) C(26) 0.015(2) 0.026(3) 0.030(3) -0.009(2) 0.002(2) 0.001(2) C(27) 0.026(3) 0.034(3) 0.021(3) -0.007(2) -0.003(2) 0.004(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # 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) 2.034(4) yes . . Cu(1) O(2) 2.021(4) yes . . Cu(1) N(1) 1.920(5) yes . . Cu(1) N(2) 1.921(4) yes . . O(1) C(26) 1.272(7) yes . . O(2) C(26) 1.261(6) yes . . N(1) C(2) 1.328(7) yes . . N(1) C(6) 1.443(6) yes . . N(2) C(3) 1.316(7) yes . . N(2) C(16) 1.442(7) yes . . C(1) C(2) 1.401(7) yes . . C(1) C(3) 1.401(8) yes . . C(2) C(4) 1.513(8) yes . . C(3) C(5) 1.527(7) yes . . C(6) C(7) 1.401(10) yes . . C(6) C(11) 1.412(10) yes . . C(7) C(8) 1.405(7) yes . . C(7) C(12) 1.510(11) yes . . C(8) C(9) 1.395(11) yes . . C(9) C(10) 1.372(10) yes . . C(10) C(11) 1.383(7) yes . . C(11) C(14) 1.499(10) yes . . C(12) C(13) 1.518(11) yes . . C(14) C(15) 1.532(10) yes . . C(16) C(17) 1.413(9) yes . . C(16) C(21) 1.402(10) yes . . C(17) C(18) 1.384(8) yes . . C(17) C(22) 1.505(11) yes . . C(18) C(19) 1.395(10) yes . . C(19) C(20) 1.381(10) yes . . C(20) C(21) 1.407(8) yes . . C(21) C(24) 1.487(10) yes . . C(22) C(23) 1.549(9) yes . . C(24) C(25) 1.529(13) yes . . C(26) C(27) 1.487(8) yes . . C(1) H(1) 0.950 no . . C(4) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(4) H(4) 0.950 no . . C(5) H(5) 0.950 no . . C(5) H(6) 0.950 no . . C(5) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(9) H(9) 0.950 no . . C(10) H(10) 0.950 no . . C(12) H(11) 0.950 no . . C(12) H(12) 0.950 no . . C(13) H(13) 0.950 no . . C(13) H(14) 0.950 no . . C(13) H(15) 0.950 no . . C(14) H(16) 0.950 no . . C(14) H(17) 0.950 no . . C(15) H(18) 0.950 no . . C(15) H(19) 0.950 no . . C(15) H(20) 0.950 no . . C(18) H(21) 0.950 no . . C(19) H(22) 0.950 no . . C(20) H(23) 0.950 no . . C(22) H(24) 0.950 no . . C(22) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(23) H(27) 0.950 no . . C(23) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(24) H(30) 0.950 no . . C(25) H(31) 0.950 no . . C(25) H(32) 0.950 no . . C(25) H(33) 0.950 no . . C(27) H(34) 0.950 no . . C(27) H(35) 0.950 no . . C(27) H(36) 0.950 no . . 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) 64.48(16) yes . . . O(1) Cu(1) N(1) 100.79(17) yes . . . O(1) Cu(1) N(2) 162.2(2) yes . . . O(2) Cu(1) N(1) 164.66(17) yes . . . O(2) Cu(1) N(2) 98.0(2) yes . . . N(1) Cu(1) N(2) 96.9(2) yes . . . Cu(1) O(1) C(26) 88.7(3) yes . . . Cu(1) O(2) C(26) 89.5(3) yes . . . Cu(1) N(1) C(2) 123.1(3) yes . . . Cu(1) N(1) C(6) 118.7(3) yes . . . C(2) N(1) C(6) 118.2(4) yes . . . Cu(1) N(2) C(3) 123.8(3) yes . . . Cu(1) N(2) C(16) 115.7(3) yes . . . C(3) N(2) C(16) 120.2(4) yes . . . C(2) C(1) C(3) 126.9(5) yes . . . N(1) C(2) C(1) 124.7(5) yes . . . N(1) C(2) C(4) 119.6(4) yes . . . C(1) C(2) C(4) 115.7(5) yes . . . N(2) C(3) C(1) 124.3(4) yes . . . N(2) C(3) C(5) 119.1(5) yes . . . C(1) C(3) C(5) 116.5(5) yes . . . N(1) C(6) C(7) 119.1(6) yes . . . N(1) C(6) C(11) 119.2(5) yes . . . C(7) C(6) C(11) 121.6(5) yes . . . C(6) C(7) C(8) 117.8(6) yes . . . C(6) C(7) C(12) 122.9(5) yes . . . C(8) C(7) C(12) 119.3(6) yes . . . C(7) C(8) C(9) 121.2(6) yes . . . C(8) C(9) C(10) 118.9(5) yes . . . C(9) C(10) C(11) 122.9(7) yes . . . C(6) C(11) C(10) 117.4(6) yes . . . C(6) C(11) C(14) 121.8(4) yes . . . C(10) C(11) C(14) 120.8(6) yes . . . C(7) C(12) C(13) 114.0(6) yes . . . C(11) C(14) C(15) 111.9(5) yes . . . N(2) C(16) C(17) 119.6(6) yes . . . N(2) C(16) C(21) 118.1(5) yes . . . C(17) C(16) C(21) 122.3(5) yes . . . C(16) C(17) C(18) 117.5(6) yes . . . C(16) C(17) C(22) 120.9(5) yes . . . C(18) C(17) C(22) 121.6(6) yes . . . C(17) C(18) C(19) 121.9(6) yes . . . C(18) C(19) C(20) 119.4(5) yes . . . C(19) C(20) C(21) 121.4(6) yes . . . C(16) C(21) C(20) 117.5(6) yes . . . C(16) C(21) C(24) 119.5(5) yes . . . C(20) C(21) C(24) 123.0(6) yes . . . C(17) C(22) C(23) 112.8(5) yes . . . C(21) C(24) C(25) 116.4(5) yes . . . O(1) C(26) O(2) 117.3(5) yes . . . O(1) C(26) C(27) 122.2(4) yes . . . O(2) C(26) C(27) 120.5(5) yes . . . C(2) C(1) H(1) 116.3 no . . . C(3) C(1) H(1) 116.8 no . . . C(2) C(4) H(2) 110.0 no . . . C(2) C(4) H(3) 109.2 no . . . C(2) C(4) H(4) 109.3 no . . . H(2) C(4) H(3) 109.5 no . . . H(2) C(4) H(4) 109.5 no . . . H(3) C(4) H(4) 109.5 no . . . C(3) C(5) H(5) 109.0 no . . . C(3) C(5) H(6) 110.0 no . . . C(3) C(5) H(7) 109.5 no . . . H(5) C(5) H(6) 109.5 no . . . H(5) C(5) H(7) 109.5 no . . . H(6) C(5) H(7) 109.5 no . . . C(7) C(8) H(8) 119.1 no . . . C(9) C(8) H(8) 119.8 no . . . C(8) C(9) H(9) 120.2 no . . . C(10) C(9) H(9) 120.9 no . . . C(9) C(10) H(10) 118.4 no . . . C(11) C(10) H(10) 118.7 no . . . C(7) C(12) H(11) 107.7 no . . . C(7) C(12) H(12) 108.6 no . . . C(13) C(12) H(11) 108.2 no . . . C(13) C(12) H(12) 108.8 no . . . H(11) C(12) H(12) 109.5 no . . . C(12) C(13) H(13) 109.1 no . . . C(12) C(13) H(14) 109.1 no . . . C(12) C(13) H(15) 110.2 no . . . H(13) C(13) H(14) 109.5 no . . . H(13) C(13) H(15) 109.5 no . . . H(14) C(13) H(15) 109.5 no . . . C(11) C(14) H(16) 108.9 no . . . C(11) C(14) H(17) 109.2 no . . . C(15) C(14) H(16) 109.0 no . . . C(15) C(14) H(17) 108.3 no . . . H(16) C(14) H(17) 109.5 no . . . C(14) C(15) H(18) 109.9 no . . . C(14) C(15) H(19) 110.2 no . . . C(14) C(15) H(20) 108.3 no . . . H(18) C(15) H(19) 109.5 no . . . H(18) C(15) H(20) 109.5 no . . . H(19) C(15) H(20) 109.5 no . . . C(17) C(18) H(21) 118.8 no . . . C(19) C(18) H(21) 119.3 no . . . C(18) C(19) H(22) 120.1 no . . . C(20) C(19) H(22) 120.4 no . . . C(19) C(20) H(23) 119.3 no . . . C(21) C(20) H(23) 119.2 no . . . C(17) C(22) H(24) 109.0 no . . . C(17) C(22) H(25) 108.3 no . . . C(23) C(22) H(24) 109.1 no . . . C(23) C(22) H(25) 108.1 no . . . H(24) C(22) H(25) 109.5 no . . . C(22) C(23) H(26) 110.0 no . . . C(22) C(23) H(27) 109.7 no . . . C(22) C(23) H(28) 108.6 no . . . H(26) C(23) H(27) 109.5 no . . . H(26) C(23) H(28) 109.5 no . . . H(27) C(23) H(28) 109.5 no . . . C(21) C(24) H(29) 106.8 no . . . C(21) C(24) H(30) 109.0 no . . . C(25) C(24) H(29) 107.5 no . . . C(25) C(24) H(30) 107.5 no . . . H(29) C(24) H(30) 109.5 no . . . C(24) C(25) H(31) 109.5 no . . . C(24) C(25) H(32) 110.2 no . . . C(24) C(25) H(33) 108.8 no . . . H(31) C(25) H(32) 109.5 no . . . H(31) C(25) H(33) 109.5 no . . . H(32) C(25) H(33) 109.5 no . . . C(26) C(27) H(34) 109.6 no . . . C(26) C(27) H(35) 109.3 no . . . C(26) C(27) H(36) 109.6 no . . . H(34) C(27) H(35) 109.5 no . . . H(34) C(27) H(36) 109.5 no . . . H(35) C(27) H(36) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Cu(1) O(2) C(26) -0.0(4) ? . . . . O(2) Cu(1) O(1) C(26) 0.0(4) ? . . . . O(1) Cu(1) N(1) C(2) -178.5(6) ? . . . . O(1) Cu(1) N(1) C(6) 0.6(5) ? . . . . N(1) Cu(1) O(1) C(26) 175.5(4) ? . . . . O(1) Cu(1) N(2) C(3) -179.5(7) ? . . . . O(1) Cu(1) N(2) C(16) 5.7(12) ? . . . . N(2) Cu(1) O(1) C(26) -9.5(10) ? . . . . O(2) Cu(1) N(1) C(2) -162.9(8) ? . . . . O(2) Cu(1) N(1) C(6) 16.3(13) ? . . . . N(1) Cu(1) O(2) C(26) -17.1(12) ? . . . . O(2) Cu(1) N(2) C(3) 171.8(6) ? . . . . O(2) Cu(1) N(2) C(16) -2.9(5) ? . . . . N(2) Cu(1) O(2) C(26) 177.1(4) ? . . . . N(1) Cu(1) N(2) C(3) -4.5(6) ? . . . . N(1) Cu(1) N(2) C(16) -179.2(5) ? . . . . N(2) Cu(1) N(1) C(2) 3.0(6) ? . . . . N(2) Cu(1) N(1) C(6) -177.8(5) ? . . . . Cu(1) O(1) C(26) O(2) -0.0(6) ? . . . . Cu(1) O(1) C(26) C(27) -179.1(7) ? . . . . Cu(1) O(2) C(26) O(1) 0.0(6) ? . . . . Cu(1) O(2) C(26) C(27) 179.2(6) ? . . . . Cu(1) N(1) C(2) C(1) -1.0(11) ? . . . . Cu(1) N(1) C(2) C(4) 177.9(5) ? . . . . Cu(1) N(1) C(6) C(7) -78.6(7) ? . . . . Cu(1) N(1) C(6) C(11) 102.3(6) ? . . . . C(2) N(1) C(6) C(7) 100.6(7) ? . . . . C(2) N(1) C(6) C(11) -78.5(8) ? . . . . C(6) N(1) C(2) C(1) 179.8(5) ? . . . . C(6) N(1) C(2) C(4) -1.2(10) ? . . . . Cu(1) N(2) C(3) C(1) 3.9(11) ? . . . . Cu(1) N(2) C(3) C(5) -174.1(5) ? . . . . Cu(1) N(2) C(16) C(17) -97.1(5) ? . . . . Cu(1) N(2) C(16) C(21) 80.0(6) ? . . . . C(3) N(2) C(16) C(17) 87.9(8) ? . . . . C(3) N(2) C(16) C(21) -94.9(7) ? . . . . C(16) N(2) C(3) C(1) 178.4(7) ? . . . . C(16) N(2) C(3) C(5) 0.5(10) ? . . . . C(2) C(1) C(3) N(2) -0.7(13) ? . . . . C(2) C(1) C(3) C(5) 177.3(7) ? . . . . C(3) C(1) C(2) N(1) -0.9(13) ? . . . . C(3) C(1) C(2) C(4) -179.8(5) ? . . . . N(1) C(6) C(7) C(8) -174.1(5) ? . . . . N(1) C(6) C(7) C(12) 5.0(9) ? . . . . N(1) C(6) C(11) C(10) 173.4(5) ? . . . . N(1) C(6) C(11) C(14) -7.4(8) ? . . . . C(7) C(6) C(11) C(10) -5.7(9) ? . . . . C(7) C(6) C(11) C(14) 173.5(5) ? . . . . C(11) C(6) C(7) C(8) 5.0(9) ? . . . . C(11) C(6) C(7) C(12) -176.0(5) ? . . . . C(6) C(7) C(8) C(9) -0.5(9) ? . . . . C(6) C(7) C(12) C(13) -84.3(8) ? . . . . C(8) C(7) C(12) C(13) 94.7(7) ? . . . . C(12) C(7) C(8) C(9) -179.6(5) ? . . . . C(7) C(8) C(9) C(10) -3.0(9) ? . . . . C(8) C(9) C(10) C(11) 2.3(9) ? . . . . C(9) C(10) C(11) C(6) 1.9(9) ? . . . . C(9) C(10) C(11) C(14) -177.2(5) ? . . . . C(6) C(11) C(14) C(15) -83.7(7) ? . . . . C(10) C(11) C(14) C(15) 95.5(7) ? . . . . N(2) C(16) C(17) C(18) 177.8(4) ? . . . . N(2) C(16) C(17) C(22) -1.9(7) ? . . . . N(2) C(16) C(21) C(20) -177.2(4) ? . . . . N(2) C(16) C(21) C(24) 1.9(7) ? . . . . C(17) C(16) C(21) C(20) -0.1(6) ? . . . . C(17) C(16) C(21) C(24) 179.0(5) ? . . . . C(21) C(16) C(17) C(18) 0.7(8) ? . . . . C(21) C(16) C(17) C(22) -178.9(5) ? . . . . C(16) C(17) C(18) C(19) -2.0(8) ? . . . . C(16) C(17) C(22) C(23) 81.1(7) ? . . . . C(18) C(17) C(22) C(23) -98.5(6) ? . . . . C(22) C(17) C(18) C(19) 177.6(5) ? . . . . C(17) C(18) C(19) C(20) 2.7(8) ? . . . . C(18) C(19) C(20) C(21) -2.0(8) ? . . . . C(19) C(20) C(21) C(16) 0.7(8) ? . . . . C(19) C(20) C(21) C(24) -178.3(5) ? . . . . C(16) C(21) C(24) C(25) -173.7(5) ? . . . . C(20) C(21) C(24) C(25) 5.3(8) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(5) 3.118(7) ? . 1_645 O(2) C(19) 3.396(7) ? . 2_566 C(5) O(1) 3.118(7) ? . 1_465 C(18) C(19) 3.400(8) ? . 2_566 C(19) O(2) 3.396(7) ? . 2_566 C(19) C(18) 3.400(8) ? . 2_566 C(19) C(19) 3.571(8) ? . 2_566 O(1) H(5) 3.036 ? . 1_645 O(1) H(6) 2.966 ? . 1_645 O(1) H(7) 2.825 ? . 1_645 O(1) H(27) 2.973 ? . 1_655 O(2) H(21) 3.187 ? . 2_566 O(2) H(22) 2.627 ? . 2_566 O(2) H(24) 3.369 ? . 1_655 O(2) H(31) 3.472 ? . 1_545 C(1) H(9) 3.555 ? . 1_465 C(1) H(13) 3.214 ? . 1_455 C(1) H(14) 3.596 ? . 1_455 C(1) H(18) 3.396 ? . 1_565 C(3) H(18) 3.584 ? . 1_565 C(4) H(2) 3.332 ? . 2_665 C(4) H(13) 3.357 ? . 2_665 C(4) H(15) 3.297 ? . 2_665 C(5) H(14) 3.411 ? . 1_455 C(5) H(19) 3.498 ? . 1_565 C(5) H(36) 3.310 ? . 1_465 C(6) H(6) 3.521 ? . 1_645 C(7) H(6) 3.138 ? . 1_645 C(8) H(1) 3.408 ? . 1_645 C(8) H(6) 2.886 ? . 1_645 C(8) H(9) 3.202 ? . 2_755 C(8) H(16) 3.439 ? . 1_655 C(8) H(17) 3.507 ? . 1_655 C(8) H(19) 3.487 ? . 1_655 C(9) H(1) 2.862 ? . 1_645 C(9) H(6) 3.074 ? . 1_645 C(9) H(8) 3.501 ? . 2_755 C(9) H(9) 3.295 ? . 2_755 C(9) H(17) 3.163 ? . 2_655 C(10) H(1) 3.470 ? . 1_645 C(10) H(6) 3.396 ? . 1_645 C(10) H(10) 3.225 ? . 2_655 C(10) H(13) 3.563 ? . 1_545 C(10) H(14) 3.352 ? . 1_545 C(10) H(17) 3.153 ? . 2_655 C(11) H(10) 3.425 ? . 2_655 C(12) H(25) 3.045 ? . 1_655 C(13) H(1) 3.548 ? . 1_655 C(13) H(3) 3.484 ? . 2_665 C(13) H(4) 3.574 ? . 2_665 C(13) H(5) 3.517 ? . 1_655 C(13) H(10) 3.184 ? . 1_565 C(13) H(18) 3.193 ? . 1_565 C(13) H(25) 3.596 ? . 1_655 C(14) H(8) 2.901 ? . 1_455 C(14) H(10) 3.478 ? . 2_655 C(14) H(12) 3.592 ? . 1_455 C(15) H(8) 3.329 ? . 1_455 C(15) H(14) 3.269 ? . 1_545 C(15) H(30) 2.934 ? . 1_545 C(16) H(36) 3.562 ? . 1_465 C(17) H(22) 3.432 ? . 2_566 C(17) H(32) 3.295 ? . 1_455 C(18) H(22) 3.407 ? . 2_566 C(18) H(32) 3.238 ? . 1_455 C(18) H(34) 3.302 ? . 1_465 C(18) H(35) 3.466 ? . 2_566 C(19) H(21) 3.515 ? . 2_566 C(19) H(28) 3.027 ? . 2_566 C(19) H(31) 3.350 ? . 2_576 C(19) H(34) 3.288 ? . 1_465 C(19) H(36) 3.345 ? . 1_465 C(20) H(21) 3.485 ? . 2_566 C(20) H(23) 3.479 ? . 2_576 C(20) H(28) 3.307 ? . 2_566 C(20) H(36) 3.086 ? . 1_465 C(21) H(36) 3.222 ? . 1_465 C(22) H(11) 3.214 ? . 1_455 C(22) H(12) 3.447 ? . 1_455 C(22) H(29) 3.546 ? . 1_455 C(22) H(32) 3.292 ? . 1_455 C(23) H(11) 3.533 ? . 1_455 C(23) H(12) 3.385 ? . 1_455 C(23) H(22) 3.281 ? . 2_566 C(23) H(30) 3.552 ? . 1_545 C(23) H(31) 3.217 ? . 1_545 C(23) H(35) 3.596 ? . 1_455 C(23) H(36) 3.054 ? . 1_455 C(24) H(18) 3.535 ? . 1_565 C(24) H(19) 3.582 ? . 1_565 C(24) H(20) 3.575 ? . 1_565 C(24) H(24) 3.518 ? . 1_655 C(25) H(21) 3.566 ? . 1_655 C(25) H(22) 3.409 ? . 2_576 C(25) H(24) 3.379 ? . 1_655 C(25) H(28) 3.485 ? . 1_565 C(25) H(34) 2.828 ? . 1_565 C(25) H(35) 3.353 ? . 2_666 C(26) H(7) 3.362 ? . 1_645 C(26) H(22) 3.201 ? . 2_566 C(26) H(24) 3.329 ? . 1_655 C(26) H(27) 2.923 ? . 1_655 C(26) H(31) 3.225 ? . 1_545 C(26) H(32) 3.433 ? . 1_545 C(27) H(7) 3.112 ? . 1_645 C(27) H(21) 3.549 ? . 2_566 C(27) H(22) 3.334 ? . 2_566 C(27) H(27) 2.789 ? . 1_655 C(27) H(31) 3.342 ? . 1_545 C(27) H(32) 3.159 ? . 1_545 C(27) H(33) 3.324 ? . 2_666 H(1) C(8) 3.408 ? . 1_465 H(1) C(9) 2.862 ? . 1_465 H(1) C(10) 3.470 ? . 1_465 H(1) C(13) 3.548 ? . 1_455 H(1) H(8) 3.502 ? . 1_465 H(1) H(9) 2.614 ? . 1_465 H(1) H(10) 3.591 ? . 1_465 H(1) H(13) 2.914 ? . 1_455 H(1) H(14) 3.336 ? . 1_455 H(1) H(18) 3.518 ? . 1_565 H(2) C(4) 3.332 ? . 2_665 H(2) H(2) 2.649 ? . 2_665 H(2) H(4) 3.189 ? . 2_665 H(2) H(13) 3.459 ? . 2_665 H(2) H(15) 3.053 ? . 2_665 H(3) C(13) 3.484 ? . 2_665 H(3) H(3) 3.579 ? . 2_565 H(3) H(9) 3.213 ? . 1_465 H(3) H(13) 3.199 ? . 1_455 H(3) H(13) 2.887 ? . 2_665 H(3) H(15) 3.230 ? . 2_665 H(4) C(13) 3.574 ? . 2_665 H(4) H(2) 3.189 ? . 2_665 H(4) H(10) 2.922 ? . 2_655 H(4) H(13) 3.201 ? . 2_665 H(4) H(15) 3.059 ? . 2_665 H(5) O(1) 3.036 ? . 1_465 H(5) C(13) 3.517 ? . 1_455 H(5) H(14) 2.702 ? . 1_455 H(5) H(20) 3.151 ? . 1_465 H(5) H(32) 3.255 ? . 1_455 H(5) H(36) 3.529 ? . 1_465 H(6) O(1) 2.966 ? . 1_465 H(6) C(6) 3.521 ? . 1_465 H(6) C(7) 3.138 ? . 1_465 H(6) C(8) 2.886 ? . 1_465 H(6) C(9) 3.074 ? . 1_465 H(6) C(10) 3.396 ? . 1_465 H(6) H(8) 3.179 ? . 1_465 H(6) H(9) 3.510 ? . 1_465 H(6) H(14) 3.591 ? . 1_455 H(6) H(19) 2.997 ? . 1_565 H(7) O(1) 2.825 ? . 1_465 H(7) C(26) 3.362 ? . 1_465 H(7) C(27) 3.112 ? . 1_465 H(7) H(19) 3.420 ? . 1_565 H(7) H(27) 3.093 ? . 1_565 H(7) H(34) 3.277 ? . 1_465 H(7) H(36) 2.428 ? . 1_465 H(8) C(9) 3.501 ? . 2_755 H(8) C(14) 2.901 ? . 1_655 H(8) C(15) 3.329 ? . 1_655 H(8) H(1) 3.502 ? . 1_645 H(8) H(6) 3.179 ? . 1_645 H(8) H(9) 2.699 ? . 2_755 H(8) H(16) 2.534 ? . 1_655 H(8) H(17) 2.608 ? . 1_655 H(8) H(19) 2.914 ? . 1_655 H(9) C(1) 3.555 ? . 1_645 H(9) C(8) 3.202 ? . 2_755 H(9) C(9) 3.295 ? . 2_755 H(9) H(1) 2.614 ? . 1_645 H(9) H(3) 3.213 ? . 1_645 H(9) H(6) 3.510 ? . 1_645 H(9) H(8) 2.699 ? . 2_755 H(9) H(9) 2.851 ? . 2_755 H(9) H(16) 3.568 ? . 2_655 H(9) H(17) 2.911 ? . 2_655 H(10) C(10) 3.225 ? . 2_655 H(10) C(11) 3.425 ? . 2_655 H(10) C(13) 3.184 ? . 1_545 H(10) C(14) 3.478 ? . 2_655 H(10) H(1) 3.591 ? . 1_645 H(10) H(4) 2.922 ? . 2_655 H(10) H(10) 2.999 ? . 2_655 H(10) H(13) 2.972 ? . 1_545 H(10) H(14) 2.959 ? . 1_545 H(10) H(15) 3.084 ? . 1_545 H(10) H(17) 2.927 ? . 2_655 H(11) C(22) 3.214 ? . 1_655 H(11) C(23) 3.533 ? . 1_655 H(11) H(24) 3.209 ? . 1_655 H(11) H(25) 2.600 ? . 1_655 H(11) H(26) 3.511 ? . 1_655 H(11) H(27) 3.272 ? . 1_655 H(12) C(14) 3.592 ? . 1_655 H(12) C(22) 3.447 ? . 1_655 H(12) C(23) 3.385 ? . 1_655 H(12) H(16) 2.835 ? . 1_655 H(12) H(19) 2.994 ? . 1_655 H(12) H(25) 2.748 ? . 1_655 H(12) H(26) 2.947 ? . 1_655 H(12) H(27) 3.337 ? . 1_655 H(13) C(1) 3.214 ? . 1_655 H(13) C(4) 3.357 ? . 2_665 H(13) C(10) 3.563 ? . 1_565 H(13) H(1) 2.914 ? . 1_655 H(13) H(2) 3.459 ? . 2_665 H(13) H(3) 3.199 ? . 1_655 H(13) H(3) 2.887 ? . 2_665 H(13) H(4) 3.201 ? . 2_665 H(13) H(10) 2.972 ? . 1_565 H(14) C(1) 3.596 ? . 1_655 H(14) C(5) 3.411 ? . 1_655 H(14) C(10) 3.352 ? . 1_565 H(14) C(15) 3.269 ? . 1_565 H(14) H(1) 3.336 ? . 1_655 H(14) H(5) 2.702 ? . 1_655 H(14) H(6) 3.591 ? . 1_655 H(14) H(10) 2.959 ? . 1_565 H(14) H(18) 2.516 ? . 1_565 H(14) H(20) 3.339 ? . 1_565 H(14) H(25) 3.186 ? . 1_655 H(15) C(4) 3.297 ? . 2_665 H(15) H(2) 3.053 ? . 2_665 H(15) H(3) 3.230 ? . 2_665 H(15) H(4) 3.059 ? . 2_665 H(15) H(10) 3.084 ? . 1_565 H(15) H(18) 3.030 ? . 1_565 H(16) C(8) 3.439 ? . 1_455 H(16) H(8) 2.534 ? . 1_455 H(16) H(9) 3.568 ? . 2_655 H(16) H(12) 2.835 ? . 1_455 H(17) C(8) 3.507 ? . 1_455 H(17) C(9) 3.163 ? . 2_655 H(17) C(10) 3.153 ? . 2_655 H(17) H(8) 2.608 ? . 1_455 H(17) H(9) 2.911 ? . 2_655 H(17) H(10) 2.927 ? . 2_655 H(18) C(1) 3.396 ? . 1_545 H(18) C(3) 3.584 ? . 1_545 H(18) C(13) 3.193 ? . 1_545 H(18) C(24) 3.535 ? . 1_545 H(18) H(1) 3.518 ? . 1_545 H(18) H(14) 2.516 ? . 1_545 H(18) H(15) 3.030 ? . 1_545 H(18) H(29) 3.463 ? . 1_545 H(18) H(30) 2.796 ? . 1_545 H(19) C(5) 3.498 ? . 1_545 H(19) C(8) 3.487 ? . 1_455 H(19) C(24) 3.582 ? . 1_545 H(19) H(6) 2.997 ? . 1_545 H(19) H(7) 3.420 ? . 1_545 H(19) H(8) 2.914 ? . 1_455 H(19) H(12) 2.994 ? . 1_455 H(19) H(30) 2.654 ? . 1_545 H(20) C(24) 3.575 ? . 1_545 H(20) H(5) 3.151 ? . 1_645 H(20) H(14) 3.339 ? . 1_545 H(20) H(30) 2.852 ? . 1_545 H(20) H(31) 3.481 ? . 1_545 H(20) H(32) 3.559 ? . 1_545 H(21) O(2) 3.187 ? . 2_566 H(21) C(19) 3.515 ? . 2_566 H(21) C(20) 3.485 ? . 2_566 H(21) C(25) 3.566 ? . 1_455 H(21) C(27) 3.549 ? . 2_566 H(21) H(23) 3.596 ? . 2_566 H(21) H(32) 3.063 ? . 1_455 H(21) H(33) 3.179 ? . 1_455 H(21) H(34) 3.521 ? . 1_465 H(21) H(35) 2.834 ? . 2_566 H(22) O(2) 2.627 ? . 2_566 H(22) C(17) 3.432 ? . 2_566 H(22) C(18) 3.407 ? . 2_566 H(22) C(23) 3.281 ? . 2_566 H(22) C(25) 3.409 ? . 2_576 H(22) C(26) 3.201 ? . 2_566 H(22) C(27) 3.334 ? . 2_566 H(22) H(28) 2.360 ? . 2_566 H(22) H(31) 2.612 ? . 2_576 H(22) H(33) 3.440 ? . 2_576 H(22) H(34) 3.535 ? . 1_465 H(22) H(34) 3.051 ? . 2_566 H(22) H(35) 3.223 ? . 2_566 H(23) C(20) 3.479 ? . 2_576 H(23) H(21) 3.596 ? . 2_566 H(23) H(23) 2.774 ? . 2_576 H(23) H(28) 2.913 ? . 2_566 H(23) H(31) 3.380 ? . 2_576 H(23) H(33) 3.596 ? . 2_576 H(23) H(35) 3.278 ? . 2_666 H(23) H(36) 3.399 ? . 1_465 H(24) O(2) 3.369 ? . 1_455 H(24) C(24) 3.518 ? . 1_455 H(24) C(25) 3.379 ? . 1_455 H(24) C(26) 3.329 ? . 1_455 H(24) H(11) 3.209 ? . 1_455 H(24) H(29) 2.807 ? . 1_455 H(24) H(32) 2.796 ? . 1_455 H(24) H(33) 3.452 ? . 1_455 H(24) H(35) 3.356 ? . 1_455 H(25) C(12) 3.045 ? . 1_455 H(25) C(13) 3.596 ? . 1_455 H(25) H(11) 2.600 ? . 1_455 H(25) H(12) 2.748 ? . 1_455 H(25) H(14) 3.186 ? . 1_455 H(25) H(29) 3.450 ? . 1_455 H(25) H(32) 3.321 ? . 1_455 H(26) H(11) 3.511 ? . 1_455 H(26) H(12) 2.947 ? . 1_455 H(26) H(30) 3.291 ? . 1_545 H(26) H(31) 3.162 ? . 1_545 H(27) O(1) 2.973 ? . 1_455 H(27) C(26) 2.923 ? . 1_455 H(27) C(27) 2.789 ? . 1_455 H(27) H(7) 3.093 ? . 1_545 H(27) H(11) 3.272 ? . 1_455 H(27) H(12) 3.337 ? . 1_455 H(27) H(30) 3.307 ? . 1_545 H(27) H(31) 3.428 ? . 1_545 H(27) H(35) 2.948 ? . 1_455 H(27) H(36) 2.209 ? . 1_455 H(28) C(19) 3.027 ? . 2_566 H(28) C(20) 3.307 ? . 2_566 H(28) C(25) 3.485 ? . 1_545 H(28) H(22) 2.360 ? . 2_566 H(28) H(23) 2.913 ? . 2_566 H(28) H(30) 3.477 ? . 1_545 H(28) H(31) 2.598 ? . 1_545 H(28) H(35) 3.579 ? . 1_455 H(28) H(36) 3.159 ? . 1_455 H(29) C(22) 3.546 ? . 1_655 H(29) H(18) 3.463 ? . 1_565 H(29) H(24) 2.807 ? . 1_655 H(29) H(25) 3.450 ? . 1_655 H(30) C(15) 2.934 ? . 1_565 H(30) C(23) 3.552 ? . 1_565 H(30) H(18) 2.796 ? . 1_565 H(30) H(19) 2.654 ? . 1_565 H(30) H(20) 2.852 ? . 1_565 H(30) H(26) 3.291 ? . 1_565 H(30) H(27) 3.307 ? . 1_565 H(30) H(28) 3.477 ? . 1_565 H(31) O(2) 3.472 ? . 1_565 H(31) C(19) 3.350 ? . 2_576 H(31) C(23) 3.217 ? . 1_565 H(31) C(26) 3.225 ? . 1_565 H(31) C(27) 3.342 ? . 1_565 H(31) H(20) 3.481 ? . 1_565 H(31) H(22) 2.612 ? . 2_576 H(31) H(23) 3.380 ? . 2_576 H(31) H(26) 3.162 ? . 1_565 H(31) H(27) 3.428 ? . 1_565 H(31) H(28) 2.598 ? . 1_565 H(31) H(34) 2.650 ? . 1_565 H(32) C(17) 3.295 ? . 1_655 H(32) C(18) 3.238 ? . 1_655 H(32) C(22) 3.292 ? . 1_655 H(32) C(26) 3.433 ? . 1_565 H(32) C(27) 3.159 ? . 1_565 H(32) H(5) 3.255 ? . 1_655 H(32) H(20) 3.559 ? . 1_565 H(32) H(21) 3.063 ? . 1_655 H(32) H(24) 2.796 ? . 1_655 H(32) H(25) 3.321 ? . 1_655 H(32) H(34) 2.367 ? . 1_565 H(32) H(35) 3.520 ? . 2_666 H(32) H(36) 3.482 ? . 1_565 H(33) C(27) 3.324 ? . 2_666 H(33) H(21) 3.179 ? . 1_655 H(33) H(22) 3.440 ? . 2_576 H(33) H(23) 3.596 ? . 2_576 H(33) H(24) 3.452 ? . 1_655 H(33) H(34) 3.029 ? . 1_565 H(33) H(34) 3.518 ? . 2_666 H(33) H(35) 2.525 ? . 2_666 H(33) H(36) 3.531 ? . 2_666 H(34) C(18) 3.302 ? . 1_645 H(34) C(19) 3.288 ? . 1_645 H(34) C(25) 2.828 ? . 1_545 H(34) H(7) 3.277 ? . 1_645 H(34) H(21) 3.521 ? . 1_645 H(34) H(22) 3.535 ? . 1_645 H(34) H(22) 3.051 ? . 2_566 H(34) H(31) 2.650 ? . 1_545 H(34) H(32) 2.367 ? . 1_545 H(34) H(33) 3.029 ? . 1_545 H(34) H(33) 3.518 ? . 2_666 H(34) H(34) 3.197 ? . 2_656 H(34) H(35) 3.479 ? . 2_656 H(35) C(18) 3.466 ? . 2_566 H(35) C(23) 3.596 ? . 1_655 H(35) C(25) 3.353 ? . 2_666 H(35) H(21) 2.834 ? . 2_566 H(35) H(22) 3.223 ? . 2_566 H(35) H(23) 3.278 ? . 2_666 H(35) H(24) 3.356 ? . 1_655 H(35) H(27) 2.948 ? . 1_655 H(35) H(28) 3.579 ? . 1_655 H(35) H(32) 3.520 ? . 2_666 H(35) H(33) 2.525 ? . 2_666 H(35) H(34) 3.479 ? . 2_656 H(36) C(5) 3.310 ? . 1_645 H(36) C(16) 3.562 ? . 1_645 H(36) C(19) 3.345 ? . 1_645 H(36) C(20) 3.086 ? . 1_645 H(36) C(21) 3.222 ? . 1_645 H(36) C(23) 3.054 ? . 1_655 H(36) H(5) 3.529 ? . 1_645 H(36) H(7) 2.428 ? . 1_645 H(36) H(23) 3.399 ? . 1_645 H(36) H(27) 2.209 ? . 1_655 H(36) H(28) 3.159 ? . 1_655 H(36) H(32) 3.482 ? . 1_545 H(36) H(33) 3.531 ? . 2_666 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================