Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _audit_creation_method Xtal3.6 _audit_creation_date 04-08-17 _audit_update_record ? _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Leonard F Lindoy' _publ_contact_author_address ; School of Chemistry University of Sydney F11 Darlington NSW 2006 AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_section_title ; A study of the complexation and extraction of Cu(II) sulfate and Ni(II) sulfate by N3O2-donor macrocycles ; loop_ _publ_author_name 'Leonard F. Lindoy' 'Stuart G. Galbraith' 'Vesna Gasperov' 'Brendan R. Rumbel' 'Brian W. Skelton' ; P.Tasker ; 'Allan H. White' _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_lln3o2 _database_code_depnum_ccdc_archive 'CCDC 251651' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C21 H31 Cl2 Cu1 N3 O12' _chemical_formula_moiety ? _chemical_formula_weight 651.94 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 16.921(2) _cell_length_b 10.6010(10) _cell_length_c 16.233(2) _cell_angle_alpha 90.00000 _cell_angle_beta 111.143(2) _cell_angle_gamma 90.00000 _cell_volume 2715.9(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7253 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.5 _cell_measurement_temperature 159(2) _exptl_absorpt_coefficient_mu 1.067 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .15 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .661 _exptl_absorpt_correction_T_max .914 _diffrn_reflns_number 31835 _reflns_number_total 6946 _reflns_Friedel_coverage 0 _reflns_number_gt 4773 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29. _diffrn_reflns_theta_full 29. _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .061 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .054 _refine_ls_wR_factor_ref .059 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_number_reflns 4773 _refine_ls_number_parameters 365 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .013 _refine_diff_density_min -.48 _refine_diff_density_max .986 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 84 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 124 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 48 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .29775(3) .17201(4) .21953(3) .0273(2) Uani ? ? 1.00000 ? ? Cl1 .16681(7) .01706(9) .43216(6) .0376(5) Uani ? ? 1.00000 ? ? O101 .1690(2) .1424(3) .4655(2) .069(2) Uani ? ? 1.00000 ? ? O102 .1328(7) -.0684(6) .4685(7) .146(7) Uani ? ? .753(9) ? ? O103 .2560(3) -.0187(5) .4532(3) .071(3) Uani ? ? .753(9) ? ? O104 .1333(6) .0181(7) .3394(3) .116(5) Uani ? ? .753(9) ? ? O102' .2076(12) -.0787(15) .4912(11) .068(5) Uiso ? ? .247(9) ? ? O103' .1873(12) .0165(18) .3594(13) .069(6) Uiso ? ? .247(9) ? ? O104' .0746(12) -.009(2) .3990(13) .089(7) Uiso ? ? .247(9) ? ? Cl2 .50727(6) .14266(8) .15841(6) .0320(4) Uani ? ? 1.00000 ? ? O201 .42578(17) .1803(3) .1589(2) .0440(15) Uani ? ? 1.00000 ? ? O202 .5200(2) .1945(3) .08297(19) .0483(16) Uani ? ? 1.00000 ? ? O203 .5119(2) .0086(3) .1585(2) .0555(17) Uani ? ? 1.00000 ? ? O204 .57149(18) .1909(3) .23743(19) .0463(15) Uani ? ? 1.00000 ? ? O1 .26529(18) .3194(2) .14214(17) .0392(13) Uani ? ? 1.00000 ? ? N1 .3220(2) .0181(3) .2966(2) .0316(14) Uani ? ? 1.00000 ? ? C2 .4134(3) .0015(4) .3483(3) .0392(19) Uani ? ? 1.00000 ? ? C3 .4493(3) .1082(4) .4134(3) .039(2) Uani ? ? 1.00000 ? ? C4 .4486(3) .2363(4) .3710(2) .0334(18) Uani ? ? 1.00000 ? ? N5 .3608(2) .2846(3) .3239(2) .0291(14) Uani ? ? 1.00000 ? ? C6 .3181(3) .3165(4) .3887(2) .0330(18) Uani ? ? 1.00000 ? ? C7 .2753(3) .4409(3) .3702(3) .0321(18) Uani ? ? 1.00000 ? ? C71 .3128(3) .5468(4) .4173(3) .039(2) Uani ? ? 1.00000 ? ? C72 .2739(3) .6641(4) .4010(3) .044(2) Uani ? ? 1.00000 ? ? C73 .1957(3) .6745(4) .3337(3) .047(2) Uani ? ? 1.00000 ? ? C74 .1562(3) .5712(4) .2837(3) .039(2) Uani ? ? 1.00000 ? ? C8 .1958(3) .4536(3) .3030(3) .0358(19) Uani ? ? 1.00000 ? ? O9 .16113(18) .3433(2) .26188(18) .0381(13) Uani ? ? 1.00000 ? ? C10 .0800(3) .3473(4) .1917(3) .040(2) Uani ? ? 1.00000 ? ? C11 .0476(3) .2154(4) .1766(3) .038(2) Uani ? ? 1.00000 ? ? O12 .10109(17) .1456(2) .14180(17) .0337(13) Uani ? ? 1.00000 ? ? C13 .0783(2) .0230(3) .1182(2) .0302(17) Uani ? ? 1.00000 ? ? C131 .0176(3) -.0425(4) .1397(3) .036(2) Uani ? ? 1.00000 ? ? C132 .0006(3) -.1676(4) .1142(3) .040(2) Uani ? ? 1.00000 ? ? C133 .0435(3) -.2274(4) .0674(3) .039(2) Uani ? ? 1.00000 ? ? C134 .1034(2) -.1606(3) .0446(2) .0335(18) Uani ? ? 1.00000 ? ? C14 .1211(2) -.0348(3) .0691(2) .0283(16) Uani ? ? 1.00000 ? ? C15 .1839(2) .0383(3) .0429(2) .0293(16) Uani ? ? 1.00000 ? ? N16 .2690(2) .0493(3) .1150(2) .0286(14) Uani ? ? 1.00000 ? ? C17 .3047(2) -.0745(3) .1541(3) .0317(17) Uani ? ? 1.00000 ? ? C18 .2870(3) -.0921(3) .2383(3) .0336(18) Uani ? ? 1.00000 ? ? O301 .3655(2) .5036(3) .1275(2) .075(2) Uani ? ? 1.00000 ? ? H1 .28833 .02307 .33409 .03900 Uiso ? ? 1.00000 ? ? H2a .44423 .00221 .30778 .05000 Uiso ? ? 1.00000 ? ? H2b .42416 -.07722 .37809 .05000 Uiso ? ? 1.00000 ? ? H3a .50565 .08760 .45236 .05100 Uiso ? ? 1.00000 ? ? H3b .41475 .11384 .45024 .05100 Uiso ? ? 1.00000 ? ? H4a .47696 .22794 .32969 .04100 Uiso ? ? 1.00000 ? ? H4b .47963 .29604 .41525 .04100 Uiso ? ? 1.00000 ? ? H5 .37921 .36321 .31178 .03600 Uiso ? ? 1.00000 ? ? H6a .35896 .31738 .44715 .04100 Uiso ? ? 1.00000 ? ? H6b .27674 .25257 .38536 .04100 Uiso ? ? 1.00000 ? ? H71 .36796 .53898 .46317 .04900 Uiso ? ? 1.00000 ? ? H72 .30176 .73664 .43654 .05300 Uiso ? ? 1.00000 ? ? H73 .16795 .75433 .31994 .05900 Uiso ? ? 1.00000 ? ? H74 .10167 .58029 .23597 .04900 Uiso ? ? 1.00000 ? ? H10a .08637 .37908 .13778 .04900 Uiso ? ? 1.00000 ? ? H10b .04230 .40313 .20518 .04900 Uiso ? ? 1.00000 ? ? H11a -.01099 .21292 .13665 .04500 Uiso ? ? 1.00000 ? ? H11b .04869 .17923 .23177 .04500 Uiso ? ? 1.00000 ? ? H131 -.01293 -.00122 .17150 .04500 Uiso ? ? 1.00000 ? ? H132 -.04210 -.21295 .12966 .04600 Uiso ? ? 1.00000 ? ? H133 .03002 -.31435 .04902 .05100 Uiso ? ? 1.00000 ? ? H134 .13545 -.20286 .01317 .04200 Uiso ? ? 1.00000 ? ? H15a .16192 .12315 .02644 .03600 Uiso ? ? 1.00000 ? ? H15b .18992 .00058 -.00761 .03600 Uiso ? ? 1.00000 ? ? H16 .31167 .08433 .09221 .03300 Uiso ? ? 1.00000 ? ? H17a .36501 -.07646 .16668 .03800 Uiso ? ? 1.00000 ? ? H17b .27987 -.14107 .11230 .03800 Uiso ? ? 1.00000 ? ? H18a .22633 -.09797 .22383 .04200 Uiso ? ? 1.00000 ? ? H18b .31166 -.16849 .26729 .04200 Uiso ? ? 1.00000 ? ? H1a .29893 .38588 .14512 .05700 Uiso ? ? 1.00000 ? ? H1b .22211 .31901 .09247 .05700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 .0386(3) .0211(2) .0222(2) .0018(2) .01073(19) .00296(18) Cl1 .0512(6) .0272(5) .0290(5) .0001(4) .0077(4) -.0035(4) O101 .087(3) .0449(19) .055(2) .0210(18) .001(2) -.0170(16) O102 .204(10) .058(4) .263(11) -.005(5) .189(9) .034(5) O103 .068(4) .081(4) .062(3) .021(3) .022(3) -.016(3) O104 .154(8) .117(5) .034(3) .054(5) -.017(4) -.020(3) Cl2 .0337(5) .0294(5) .0326(5) -.0006(4) .0115(4) -.0017(4) O201 .0372(16) .0457(17) .0519(18) .0002(14) .0195(14) -.0016(14) O202 .058(2) .0549(19) .0382(17) .0015(15) .0241(15) .0063(14) O203 .064(2) .0270(15) .077(2) .0005(15) .0283(19) -.0028(15) O204 .0439(17) .0493(18) .0379(16) -.0087(14) .0052(14) -.0031(14) O1 .0525(17) .0279(14) .0306(14) -.0018(13) .0071(13) .0108(12) N1 .0411(19) .0255(15) .0284(16) .0036(14) .0129(15) .0054(13) C2 .050(3) .028(2) .031(2) .0066(18) .0045(19) .0044(16) C3 .051(3) .030(2) .029(2) .0046(18) .0060(19) .0041(16) C4 .042(2) .0289(19) .028(2) .0029(17) .0100(17) .0024(15) N5 .0405(19) .0237(14) .0259(16) -.0008(13) .0154(14) .0021(12) C6 .044(2) .032(2) .0259(19) -.0028(18) .0161(17) -.0009(16) C7 .044(2) .0282(19) .033(2) -.0041(17) .0252(19) -.0021(16) C71 .049(3) .037(2) .043(2) -.0111(19) .031(2) -.0082(18) C72 .054(3) .030(2) .063(3) -.011(2) .040(3) -.012(2) C73 .066(3) .0225(18) .073(3) .000(2) .051(3) -.001(2) C74 .050(3) .031(2) .048(2) .0046(19) .030(2) .0055(18) C8 .052(3) .0271(19) .039(2) -.0018(18) .030(2) -.0031(16) O9 .0466(17) .0277(14) .0371(15) .0021(12) .0114(13) -.0049(12) C10 .045(2) .038(2) .037(2) .005(2) .016(2) -.0038(18) C11 .038(2) .044(2) .034(2) .0026(18) .0171(19) -.0082(18) O12 .0413(16) .0322(14) .0334(14) -.0048(12) .0204(13) -.0070(11) C13 .036(2) .032(2) .0205(18) -.0002(16) .0076(16) -.0004(15) C131 .040(2) .042(2) .028(2) -.0046(18) .0143(18) .0017(17) C132 .042(2) .045(2) .030(2) -.011(2) .0108(18) .0092(18) C133 .045(3) .032(2) .033(2) -.0059(18) .0059(19) .0023(17) C134 .038(2) .030(2) .030(2) -.0001(17) .0092(17) -.0009(16) C14 .031(2) .0300(19) .0226(18) -.0010(16) .0087(16) .0027(14) C15 .040(2) .0284(18) .0217(17) -.0013(16) .0137(16) -.0014(14) N16 .0341(17) .0246(15) .0275(16) -.0010(13) .0115(14) -.0021(12) C17 .037(2) .0239(18) .035(2) .0020(16) .0147(18) -.0005(15) C18 .040(2) .0215(17) .037(2) .0008(16) .0113(18) .0040(15) O301 .080(3) .059(2) .072(3) -.023(2) .009(2) .007(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 O201 . . 2.685(4) ? Cu1 O1 . . 1.956(3) ? Cu1 N1 . . 2.006(3) ? Cu1 N5 . . 2.032(3) ? Cu1 N16 . . 2.052(3) ? Cl1 O101 . . 1.429(3) ? Cl1 O102 . . 1.321(10) ? Cl1 O103 . . 1.472(5) ? Cl1 O104 . . 1.404(5) ? Cl1 O102' . . 1.396(15) ? Cl1 O103' . . 1.35(2) ? Cl1 O104' . . 1.48(2) ? Cl2 O201 . . 1.438(3) ? Cl2 O202 . . 1.427(4) ? Cl2 O203 . . 1.423(3) ? Cl2 O204 . . 1.443(3) ? O1 H1a . . .896 ? O1 H1b . . .871 ? N1 C2 . . 1.481(5) ? N1 C18 . . 1.485(5) ? N1 H1 . . .974 ? C2 C3 . . 1.518(5) ? C2 H2a . . .975 ? C2 H2b . . .949 ? C3 C4 . . 1.520(6) ? C3 H3a . . .960 ? C3 H3b . . .978 ? C4 N5 . . 1.495(5) ? C4 H4a . . .960 ? C4 H4b . . .960 ? N5 C6 . . 1.514(6) ? N5 H5 . . .935 ? C6 C7 . . 1.482(5) ? C6 H6a . . .951 ? C6 H6b . . .962 ? C7 C71 . . 1.378(5) ? C7 C8 . . 1.401(5) ? C71 C72 . . 1.388(6) ? C71 H71 . . .964 ? C72 C73 . . 1.383(6) ? C72 H72 . . .975 ? C73 C74 . . 1.383(6) ? C73 H73 . . .955 ? C74 C8 . . 1.396(5) ? C74 H74 . . .971 ? C8 O9 . . 1.369(4) ? O9 C10 . . 1.435(4) ? C10 C11 . . 1.490(6) ? C10 H10a . . .979 ? C10 H10b . . .951 ? C11 O12 . . 1.433(6) ? C11 H11a . . .969 ? C11 H11b . . .969 ? O12 C13 . . 1.371(4) ? C13 C131 . . 1.384(6) ? C13 C14 . . 1.397(6) ? C131 C132 . . 1.388(6) ? C131 H131 . . .958 ? C132 C133 . . 1.379(7) ? C132 H132 . . .973 ? C133 C134 . . 1.392(7) ? C133 H133 . . .971 ? C134 C14 . . 1.394(5) ? C134 H134 . . .977 ? C14 C15 . . 1.494(6) ? C15 N16 . . 1.497(4) ? C15 H15a . . .973 ? C15 H15b . . .950 ? N16 C17 . . 1.488(4) ? N16 H16 . . .995 ? C17 C18 . . 1.511(7) ? C17 H17a . . .967 ? C17 H17b . . .964 ? C18 H18a . . .970 ? C18 H18b . . .953 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O201 Cu1 O1 . . . 79.34(11) ? O201 Cu1 N1 . . . 104.15(12) ? O201 Cu1 N5 . . . 92.09(12) ? O201 Cu1 N16 . . . 72.52(12) ? O1 Cu1 N1 . . . 175.81(13) ? O1 Cu1 N5 . . . 90.43(11) ? O1 Cu1 N16 . . . 92.73(11) ? N1 Cu1 N5 . . . 91.73(12) ? N1 Cu1 N16 . . . 86.21(12) ? N5 Cu1 N16 . . . 163.38(14) ? O101 Cl1 O102 . . . 115.1(5) ? O101 Cl1 O103 . . . 105.5(3) ? O101 Cl1 O104 . . . 110.1(3) ? O101 Cl1 O102' . . . 118.5(7) ? O101 Cl1 O103' . . . 110.9(8) ? O101 Cl1 O104' . . . 101.1(9) ? O102 Cl1 O103 . . . 107.2(5) ? O102 Cl1 O104 . . . 114.3(5) ? O103 Cl1 O104 . . . 103.6(5) ? O102' Cl1 O103' . . . 112.3(12) ? O102' Cl1 O104' . . . 107.9(11) ? O103' Cl1 O104' . . . 104.6(12) ? O201 Cl2 O202 . . . 109.81(18) ? O201 Cl2 O203 . . . 109.2(2) ? O201 Cl2 O204 . . . 108.25(19) ? O202 Cl2 O203 . . . 111.1(2) ? O202 Cl2 O204 . . . 109.16(19) ? O203 Cl2 O204 . . . 109.24(17) ? Cu1 O201 Cl2 . . . 153.49(18) ? Cu1 O1 H1a . . . 124.6 ? Cu1 O1 H1b . . . 122.5 ? H1a O1 H1b . . . 111.0 ? Cu1 N1 C2 . . . 112.8(3) ? Cu1 N1 C18 . . . 107.3(2) ? Cu1 N1 H1 . . . 108.1 ? C2 N1 C18 . . . 111.2(3) ? C2 N1 H1 . . . 112.3 ? C18 N1 H1 . . . 104.6 ? N1 C2 C3 . . . 112.4(3) ? N1 C2 H2a . . . 108.7 ? N1 C2 H2b . . . 111.2 ? C3 C2 H2a . . . 106.7 ? C3 C2 H2b . . . 110.2 ? H2a C2 H2b . . . 107.5 ? C2 C3 C4 . . . 114.5(3) ? C2 C3 H3a . . . 110.0 ? C2 C3 H3b . . . 107.1 ? C4 C3 H3a . . . 110.3 ? C4 C3 H3b . . . 108.3 ? H3a C3 H3b . . . 106.4 ? C3 C4 N5 . . . 112.5(3) ? C3 C4 H4a . . . 108.0 ? C3 C4 H4b . . . 109.7 ? N5 C4 H4a . . . 109.3 ? N5 C4 H4b . . . 109.4 ? H4a C4 H4b . . . 107.9 ? Cu1 N5 C4 . . . 110.6(2) ? Cu1 N5 C6 . . . 118.2(2) ? Cu1 N5 H5 . . . 117.6 ? C4 N5 C6 . . . 110.8(3) ? C4 N5 H5 . . . 93.8 ? C6 N5 H5 . . . 103.0 ? N5 C6 C7 . . . 112.2(3) ? N5 C6 H6a . . . 109.8 ? N5 C6 H6b . . . 108.8 ? C7 C6 H6a . . . 108.7 ? C7 C6 H6b . . . 108.8 ? H6a C6 H6b . . . 108.4 ? C6 C7 C71 . . . 121.2(3) ? C6 C7 C8 . . . 120.4(3) ? C71 C7 C8 . . . 118.3(3) ? C7 C71 C72 . . . 122.2(4) ? C7 C71 H71 . . . 118.8 ? C72 C71 H71 . . . 119.0 ? C71 C72 C73 . . . 118.3(4) ? C71 C72 H72 . . . 119.9 ? C73 C72 H72 . . . 121.8 ? C72 C73 C74 . . . 121.6(4) ? C72 C73 H73 . . . 120.3 ? C74 C73 H73 . . . 118.2 ? C73 C74 C8 . . . 118.9(4) ? C73 C74 H74 . . . 120.6 ? C8 C74 H74 . . . 120.6 ? C7 C8 C74 . . . 120.7(3) ? C7 C8 O9 . . . 114.8(3) ? C74 C8 O9 . . . 124.5(3) ? C8 O9 C10 . . . 118.7(3) ? O9 C10 C11 . . . 107.0(3) ? O9 C10 H10a . . . 109.7 ? O9 C10 H10b . . . 111.4 ? C11 C10 H10a . . . 109.2 ? C11 C10 H10b . . . 112.6 ? H10a C10 H10b . . . 106.9 ? C10 C11 O12 . . . 107.6(4) ? C10 C11 H11a . . . 111.2 ? C10 C11 H11b . . . 109.6 ? O12 C11 H11a . . . 111.2 ? O12 C11 H11b . . . 110.9 ? H11a C11 H11b . . . 106.3 ? C11 O12 C13 . . . 116.5(3) ? O12 C13 C131 . . . 124.4(4) ? O12 C13 C14 . . . 115.0(4) ? C131 C13 C14 . . . 120.6(3) ? C13 C131 C132 . . . 119.8(4) ? C13 C131 H131 . . . 120.0 ? C132 C131 H131 . . . 120.2 ? C131 C132 C133 . . . 120.6(4) ? C131 C132 H132 . . . 119.2 ? C133 C132 H132 . . . 120.2 ? C132 C133 C134 . . . 119.4(4) ? C132 C133 H133 . . . 119.6 ? C134 C133 H133 . . . 120.9 ? C133 C134 C14 . . . 120.9(4) ? C133 C134 H134 . . . 120.0 ? C14 C134 H134 . . . 119.0 ? C13 C14 C134 . . . 118.7(4) ? C13 C14 C15 . . . 120.2(3) ? C134 C14 C15 . . . 121.1(4) ? C14 C15 N16 . . . 113.5(3) ? C14 C15 H15a . . . 108.5 ? C14 C15 H15b . . . 109.6 ? N16 C15 H15a . . . 107.9 ? N16 C15 H15b . . . 109.6 ? H15a C15 H15b . . . 107.5 ? Cu1 N16 C15 . . . 124.8(2) ? Cu1 N16 C17 . . . 105.5(2) ? Cu1 N16 H16 . . . 94.79 ? C15 N16 C17 . . . 113.1(3) ? C15 N16 H16 . . . 111.1 ? C17 N16 H16 . . . 104.5 ? N16 C17 C18 . . . 108.2(3) ? N16 C17 H17a . . . 110.1 ? N16 C17 H17b . . . 109.8 ? C18 C17 H17a . . . 110.1 ? C18 C17 H17b . . . 111.6 ? H17a C17 H17b . . . 106.9 ? N1 C18 C17 . . . 108.4(3) ? N1 C18 H18a . . . 110.4 ? N1 C18 H18b . . . 110.5 ? C17 C18 H18a . . . 109.1 ? C17 C18 H18b . . . 111.0 ? H18a C18 H18b . . . 107.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1348 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min -21 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 8.785 _diffrn_reflns_av_sigmaI/netI .096 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .09 _refine_ls_wR_factor_all .063 _refine_ls_goodness_of_fit_all 1.126 _refine_ls_shift/su_mean .002 #===END #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_llvg4 _database_code_depnum_ccdc_archive 'CCDC 251652' _audit_creation_method Xtal3.6 _audit_creation_date 99-05-25 _audit_update_record ? _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C20 H41 N3 Ni1 O13 S1' _chemical_formula_moiety ? _chemical_formula_weight 622.31 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 25.092(2) _cell_length_b 38.474(3) _cell_length_c 11.6660(10) _cell_angle_alpha 90.00000 _cell_angle_beta 97.7320(10) _cell_angle_gamma 90.00000 _cell_volume 11159.8(16) _cell_formula_units_Z 16 _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25 _cell_measurement_temperature 293(2) _exptl_absorpt_coefficient_mu .837 _exptl_crystal_description prism _exptl_crystal_size_max .40 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .27 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .682 _exptl_absorpt_correction_T_max .894 _diffrn_reflns_number 121685 _reflns_number_total 19565 _reflns_Friedel_coverage 0 _reflns_number_gt 16596 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .047 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .079 _refine_ls_wR_factor_ref .099 _refine_ls_goodness_of_fit_ref 1.98 _refine_ls_number_reflns 16596 _refine_ls_number_parameters 1422 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .068 _refine_diff_density_min -.835 _refine_diff_density_max 2.232 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 320 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 656 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ni ? 0 16 .285 1.113 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 48 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 208 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 16 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 .59366(2) .182768(17) .56181(6) .0164(3) Uani ? ? 1.00000 ? ? Ni2 .90185(2) .933683(17) .44919(6) .0167(3) Uani ? ? 1.00000 ? ? Ni3 .60884(3) .681182(17) .56428(6) .0175(3) Uani ? ? 1.00000 ? ? Ni4 .10514(2) .931259(17) .07357(6) .0164(3) Uani ? ? 1.00000 ? ? O1 .57914(14) .23536(9) .5303(3) .0228(18) Uani ? ? 1.00000 ? ? O10 .51136(15) .17347(11) .5159(3) .031(2) Uani ? ? 1.00000 ? ? O10' .57860(14) .19121(10) .7324(3) .0210(18) Uani ? ? 1.00000 ? ? N10 .61068(16) .13031(11) .5864(4) .019(2) Uani ? ? 1.00000 ? ? C11 .6018(2) .11420(13) .4697(5) .019(2) Uani ? ? 1.00000 ? ? C12 .6272(2) .13702(14) .3858(5) .022(3) Uani ? ? 1.00000 ? ? N13 .60535(17) .17261(12) .3890(4) .021(2) Uani ? ? 1.00000 ? ? C14 .6382(2) .19913(14) .3368(5) .023(3) Uani ? ? 1.00000 ? ? C141 .6636(2) .18712(14) .2331(5) .022(3) Uani ? ? 1.00000 ? ? C142 .6342(2) .18723(16) .1231(5) .029(3) Uani ? ? 1.00000 ? ? C143 .6583(3) .17867(17) .0270(5) .035(3) Uani ? ? 1.00000 ? ? C144 .7126(3) .17054(17) .0402(5) .036(3) Uani ? ? 1.00000 ? ? C145 .7427(2) .16994(17) .1496(6) .032(3) Uani ? ? 1.00000 ? ? C146 .7171(2) .17762(14) .2463(5) .026(3) Uani ? ? 1.00000 ? ? O15 .74247(15) .17539(11) .3581(3) .030(2) Uani ? ? 1.00000 ? ? C16 .7987(2) .17885(17) .3773(6) .035(3) Uani ? ? 1.00000 ? ? C11' .6662(2) .12524(14) .6446(5) .021(3) Uani ? ? 1.00000 ? ? C12' .6874(2) .15833(14) .7042(5) .024(3) Uani ? ? 1.00000 ? ? N13' .67744(16) .18765(11) .6224(4) .018(2) Uani ? ? 1.00000 ? ? C14' .6980(2) .22149(14) .6726(5) .023(3) Uani ? ? 1.00000 ? ? C141' .7551(2) .22096(13) .7318(5) .021(2) Uani ? ? 1.00000 ? ? C142' .7672(2) .22852(14) .8476(5) .029(3) Uani ? ? 1.00000 ? ? C143' .8193(3) .22780(17) .9044(6) .038(3) Uani ? ? 1.00000 ? ? C144' .8611(2) .22020(14) .8441(6) .033(3) Uani ? ? 1.00000 ? ? C145' .8507(2) .21173(16) .7268(5) .030(3) Uani ? ? 1.00000 ? ? C146' .7987(2) .21283(14) .6707(5) .022(3) Uani ? ? 1.00000 ? ? O15' .78471(15) .20508(11) .5543(3) .031(2) Uani ? ? 1.00000 ? ? C16' .8169(3) .18097(18) .5046(6) .041(4) Uani ? ? 1.00000 ? ? O2 .91223(14) .98610(9) .4822(3) .0212(18) Uani ? ? 1.00000 ? ? O20 .98337(14) .92368(10) .5069(4) .029(2) Uani ? ? 1.00000 ? ? O20' .91984(14) .94088(10) .2804(3) .025(2) Uani ? ? 1.00000 ? ? N20 .88810(16) .88075(11) .4246(4) .019(2) Uani ? ? 1.00000 ? ? C21 .8970(2) .86492(14) .5425(5) .024(3) Uani ? ? 1.00000 ? ? C22 .8693(2) .88658(15) .6255(5) .024(3) Uani ? ? 1.00000 ? ? N23 .88610(16) .92366(11) .6203(4) .018(2) Uani ? ? 1.00000 ? ? C24 .8467(2) .94787(14) .6640(5) .024(3) Uani ? ? 1.00000 ? ? C241 .8277(2) .93771(14) .7765(5) .021(3) Uani ? ? 1.00000 ? ? C242 .8630(2) .93089(19) .8760(6) .037(3) Uani ? ? 1.00000 ? ? C243 .8453(3) .9232(2) .9802(5) .049(4) Uani ? ? 1.00000 ? ? C244 .7917(3) .92283(18) .9877(6) .038(3) Uani ? ? 1.00000 ? ? C245 .7552(2) .92969(18) .8927(6) .039(4) Uani ? ? 1.00000 ? ? C246 .7730(2) .93608(17) .7873(5) .033(3) Uani ? ? 1.00000 ? ? O25 .73553(18) .94643(12) .6966(4) .041(2) Uani ? ? 1.00000 ? ? C26 .7086(3) .91894(18) .6333(6) .040(4) Uani ? ? 1.00000 ? ? C21' .8330(2) .87512(15) .3629(5) .028(3) Uani ? ? 1.00000 ? ? C22' .8123(2) .90760(15) .3011(5) .025(3) Uani ? ? 1.00000 ? ? N23' .81911(17) .93713(11) .3812(4) .021(2) Uani ? ? 1.00000 ? ? C24' .7977(2) .97049(14) .3326(5) .023(3) Uani ? ? 1.00000 ? ? C241' .7388(2) .96941(14) .2792(5) .023(3) Uani ? ? 1.00000 ? ? C242' .7233(2) .97992(16) .1665(5) .031(3) Uani ? ? 1.00000 ? ? C243' .6696(3) .97993(16) .1164(6) .036(3) Uani ? ? 1.00000 ? ? C244' .6310(2) .96820(17) .1811(6) .036(3) Uani ? ? 1.00000 ? ? C245' .6442(2) .95792(16) .2951(6) .032(3) Uani ? ? 1.00000 ? ? C246' .6984(2) .95769(14) .3435(5) .024(3) Uani ? ? 1.00000 ? ? O25' .71599(15) .94750(12) .4542(3) .035(2) Uani ? ? 1.00000 ? ? C26' .6784(2) .93156(15) .5210(5) .028(3) Uani ? ? 1.00000 ? ? O3 .59820(15) .73479(10) .5370(3) .027(2) Uani ? ? 1.00000 ? ? O30 .52750(14) .67250(10) .5056(3) .026(2) Uani ? ? 1.00000 ? ? O30' .59152(15) .68792(10) .7329(3) .027(2) Uani ? ? 1.00000 ? ? N30 .62239(16) .62820(11) .5850(4) .018(2) Uani ? ? 1.00000 ? ? C31 .6135(2) .61327(13) .4674(5) .020(2) Uani ? ? 1.00000 ? ? C32 .6410(2) .63592(14) .3860(5) .024(3) Uani ? ? 1.00000 ? ? N33 .62382(17) .67259(12) .3914(4) .023(2) Uani ? ? 1.00000 ? ? C34 .6624(2) .69754(15) .3496(5) .028(3) Uani ? ? 1.00000 ? ? C341 .6823(2) .68719(13) .2377(5) .022(3) Uani ? ? 1.00000 ? ? C342 .6462(2) .68058(18) .1378(5) .035(3) Uani ? ? 1.00000 ? ? C343 .6639(3) .67262(18) .0324(5) .036(3) Uani ? ? 1.00000 ? ? C344 .7185(3) .67199(16) .0272(6) .036(3) Uani ? ? 1.00000 ? ? C345 .7547(2) .67880(17) .1205(7) .040(4) Uani ? ? 1.00000 ? ? C346 .7365(2) .68625(14) .2269(6) .030(3) Uani ? ? 1.00000 ? ? O35 .77448(17) .69610(11) .3194(4) .040(2) Uani ? ? 1.00000 ? ? C36 .8028(2) .66828(16) .3797(5) .032(3) Uani ? ? 1.00000 ? ? C31' .6771(2) .62202(14) .6458(5) .023(3) Uani ? ? 1.00000 ? ? C32' .6982(2) .65419(14) .7105(5) .023(3) Uani ? ? 1.00000 ? ? N33' .69133(17) .68395(11) .6321(4) .020(2) Uani ? ? 1.00000 ? ? C34' .7134(2) .71738(14) .6833(5) .024(3) Uani ? ? 1.00000 ? ? C341' .7717(2) .71610(14) .7357(5) .025(3) Uani ? ? 1.00000 ? ? C342' .7870(2) .72555(14) .8503(5) .030(3) Uani ? ? 1.00000 ? ? C343' .8414(3) .72462(16) .8994(6) .039(3) Uani ? ? 1.00000 ? ? C344' .8801(3) .71492(17) .8335(7) .043(4) Uani ? ? 1.00000 ? ? C345' .8663(2) .70459(16) .7206(6) .033(3) Uani ? ? 1.00000 ? ? C346' .8129(2) .70539(15) .6712(5) .026(3) Uani ? ? 1.00000 ? ? O35' .79495(16) .69451(11) .5590(4) .031(2) Uani ? ? 1.00000 ? ? C36' .8327(2) .68112(17) .4907(6) .034(3) Uani ? ? 1.00000 ? ? O4 .09144(15) .98387(10) .0468(3) .025(2) Uani ? ? 1.00000 ? ? O40 .02325(15) .92067(11) .0287(3) .029(2) Uani ? ? 1.00000 ? ? O40' .09133(14) .93918(9) .2449(3) .0196(17) Uani ? ? 1.00000 ? ? N40 .12177(16) .87877(11) .0962(4) .017(2) Uani ? ? 1.00000 ? ? C41 .1123(2) .86317(15) -.0215(5) .024(3) Uani ? ? 1.00000 ? ? C42 .1366(2) .88608(13) -.1061(5) .021(3) Uani ? ? 1.00000 ? ? N43 .11589(17) .92208(11) -.0995(4) .019(2) Uani ? ? 1.00000 ? ? C44 .1485(2) .94882(14) -.1522(5) .021(3) Uani ? ? 1.00000 ? ? C441 .1747(2) .93719(14) -.2544(5) .021(3) Uani ? ? 1.00000 ? ? C442 .1466(2) .93662(15) -.3642(5) .027(3) Uani ? ? 1.00000 ? ? C443 .1715(3) .9272(2) -.4598(5) .040(4) Uani ? ? 1.00000 ? ? C444 .2255(3) .91800(17) -.4422(6) .036(3) Uani ? ? 1.00000 ? ? C445 .2546(2) .91825(16) -.3318(6) .033(3) Uani ? ? 1.00000 ? ? C446 .2284(2) .92638(14) -.2393(5) .023(3) Uani ? ? 1.00000 ? ? O45 .25294(15) .92462(11) -.1246(3) .031(2) Uani ? ? 1.00000 ? ? C46 .3095(2) .92576(16) -.1039(6) .034(3) Uani ? ? 1.00000 ? ? C41' .1779(2) .87378(14) .1544(5) .024(3) Uani ? ? 1.00000 ? ? C42' .1987(2) .90627(14) .2141(5) .023(3) Uani ? ? 1.00000 ? ? N43' .18935(17) .93604(11) .1335(4) .021(2) Uani ? ? 1.00000 ? ? C44' .2088(2) .96976(15) .1846(5) .026(3) Uani ? ? 1.00000 ? ? C441' .2665(2) .96915(14) .2470(5) .026(3) Uani ? ? 1.00000 ? ? C442' .2774(3) .97589(16) .3644(5) .034(3) Uani ? ? 1.00000 ? ? C443' .3290(3) .97523(15) .4220(6) .037(3) Uani ? ? 1.00000 ? ? C444' .3714(3) .96708(17) .3614(6) .040(3) Uani ? ? 1.00000 ? ? C445' .3618(2) .96082(16) .2456(6) .036(3) Uani ? ? 1.00000 ? ? C446' .3095(2) .96110(15) .1880(5) .027(3) Uani ? ? 1.00000 ? ? O45' .29763(16) .95572(10) .0702(3) .028(2) Uani ? ? 1.00000 ? ? C46' .3256(2) .92707(16) .0237(6) .038(3) Uani ? ? 1.00000 ? ? S1 .51126(5) .76941(3) .75542(11) .0187(6) Uani ? ? 1.00000 ? ? O11 .47122(18) .74876(11) .6875(4) .027(2) Uani ? ? .879(4) ? ? O12 .56529(19) .75438(12) .7498(6) .046(3) Uani ? ? .879(4) ? ? O13 .5015(2) .76873(12) .8761(4) .038(3) Uani ? ? .879(4) ? ? O14 .51194(17) .80542(11) .7136(4) .026(2) Uani ? ? .879(4) ? ? O11' .4525(11) .7535(7) .708(2) .018(6) Uiso ? ? .121(4) ? ? O12' .522(2) .7683(13) .633(4) .065(13) Uiso ? ? .121(4) ? ? O13' .5464(15) .7456(10) .817(3) .043(9) Uiso ? ? .121(4) ? ? O14' .491(2) .8028(14) .808(5) .076(15) Uiso ? ? .121(4) ? ? S2 -.00196(5) 1.01925(3) .24498(10) .0150(6) Uani ? ? 1.00000 ? ? O21 -.0235(2) 1.02324(12) .3560(4) .030(3) Uani ? ? .831(4) ? ? O22 .00337(18) 1.05405(11) .1960(4) .023(2) Uani ? ? .831(4) ? ? O23 -.03788(18) .99733(11) .1666(4) .022(2) Uani ? ? .831(4) ? ? O24 .05204(17) 1.00318(12) .2685(5) .033(3) Uani ? ? .831(4) ? ? O21' -.0016(9) 1.0182(6) .112(2) .029(5) Uiso ? ? .169(4) ? ? O22' -.0032(9) 1.0563(6) .278(2) .026(5) Uiso ? ? .169(4) ? ? O23' -.0525(10) 1.0021(7) .271(2) .038(6) Uiso ? ? .169(4) ? ? O24' .0402(9) .9989(6) .309(2) .030(5) Uiso ? ? .169(4) ? ? S3 .50274(5) .88449(4) .24076(13) .0239(7) Uani ? ? 1.00000 ? ? O31 .46741(16) .90608(10) .3020(4) .033(2) Uani ? ? 1.00000 ? ? O32 .46901(15) .86062(9) .1615(4) .026(2) Uani ? ? 1.00000 ? ? O33 .53833(16) .86330(10) .3255(4) .030(2) Uani ? ? 1.00000 ? ? O34 .53552(16) .90589(10) .1728(4) .034(2) Uani ? ? 1.00000 ? ? S4 .00805(5) .86681(4) .27565(13) .0247(7) Uani ? ? 1.00000 ? ? O41 -.02840(15) .88820(12) .1929(4) .033(2) Uani ? ? 1.00000 ? ? O42 -.02468(16) .84442(10) .3411(4) .031(2) Uani ? ? 1.00000 ? ? O43 .04218(16) .84520(10) .2114(4) .031(2) Uani ? ? 1.00000 ? ? O44 .04213(15) .89062(10) .3557(4) .029(2) Uani ? ? 1.00000 ? ? O01 -.0092(2) .80187(12) .0463(4) .043(3) Uani ? ? 1.00000 ? ? O02 .0126(2) .87464(13) .7527(4) .047(3) Uani ? ? 1.00000 ? ? O03 .0308(2) .79584(13) .4832(4) .050(3) Uani ? ? 1.00000 ? ? O04 .4986(2) .87636(12) .7602(4) .046(3) Uani ? ? 1.00000 ? ? O05 .5215(2) .95028(12) .4673(4) .046(3) Uani ? ? 1.00000 ? ? O06 .4810(2) .95370(12) .0290(4) .047(3) Uani ? ? 1.00000 ? ? O07 -.0204(2) .73744(13) .1509(5) .054(3) Uani ? ? 1.00000 ? ? O08 .4691(2) 1.01531(14) .1448(5) .058(3) Uani ? ? 1.00000 ? ? O09 .0446(2) .76607(13) -.1262(5) .054(3) Uani ? ? 1.00000 ? ? O010 .5329(2) 1.01624(14) .3655(5) .058(3) Uani ? ? 1.00000 ? ? O011 .8863(2) .79233(13) .7072(5) .055(3) Uani ? ? 1.00000 ? ? O012 .3755(3) 1.04337(16) .1994(6) .070(4) Uani ? ? 1.00000 ? ? O013 .5716(2) .91027(19) .6465(6) .084(4) Uani ? ? 1.00000 ? ? O014 .9385(2) .83877(16) -.1371(5) .067(4) Uani ? ? 1.00000 ? ? O015 .0753(2) .85557(17) .5866(6) .072(4) Uani ? ? 1.00000 ? ? O016 .4352(3) .8948(2) -.0711(6) .023(4) Uani ? ? .50000 ? ? O017 .4272(7) .9298(4) -.2009(17) .041(10) Uani ? ? .25000 ? ? O018 .0832(8) .8179(5) .7117(18) .051(12) Uani ? ? .25000 ? ? H1a .56668 .23548 .45697 .03700 Uiso ? ? 1.00000 ? ? H1b .55366 .24530 .56801 .03700 Uiso ? ? 1.00000 ? ? H10a .49517 .17965 .45472 .05000 Uiso ? ? 1.00000 ? ? H10b .48509 .16666 .56167 .05000 Uiso ? ? 1.00000 ? ? H10'a .55912 .21392 .74865 .03500 Uiso ? ? 1.00000 ? ? H10'b .56077 .18296 .76835 .03500 Uiso ? ? 1.00000 ? ? H10 .58696 .12069 .63253 .02600 Uiso ? ? 1.00000 ? ? H11a .61757 .09176 .47199 .02800 Uiso ? ? 1.00000 ? ? H11b .56424 .11238 .44441 .02800 Uiso ? ? 1.00000 ? ? H12a .61953 .12767 .30954 .02900 Uiso ? ? 1.00000 ? ? H12b .66517 .13755 .40737 .02900 Uiso ? ? 1.00000 ? ? H13 .57203 .17137 .34368 .02900 Uiso ? ? 1.00000 ? ? H14a .61522 .21869 .31395 .03100 Uiso ? ? 1.00000 ? ? H14b .66584 .20678 .39570 .03100 Uiso ? ? 1.00000 ? ? H142 .59703 .19387 .11377 .03700 Uiso ? ? 1.00000 ? ? H143 .63771 .17803 -.04902 .04600 Uiso ? ? 1.00000 ? ? H144 .72988 .16578 -.02604 .04800 Uiso ? ? 1.00000 ? ? H145 .78054 .16355 .15876 .04200 Uiso ? ? 1.00000 ? ? H16a .81569 .15937 .34494 .04500 Uiso ? ? 1.00000 ? ? H16b .80990 .19951 .34150 .04500 Uiso ? ? 1.00000 ? ? H11'a .66725 .10685 .70086 .02900 Uiso ? ? 1.00000 ? ? H11'b .68908 .11834 .58851 .02900 Uiso ? ? 1.00000 ? ? H12'a .72521 .15664 .72843 .03200 Uiso ? ? 1.00000 ? ? H12'b .66958 .16282 .76902 .03200 Uiso ? ? 1.00000 ? ? H13' .69763 .18509 .56175 .02600 Uiso ? ? 1.00000 ? ? H14'a .69522 .23829 .61113 .03000 Uiso ? ? 1.00000 ? ? H14'b .67504 .22873 .72712 .03000 Uiso ? ? 1.00000 ? ? H142' .73835 .23488 .89048 .03700 Uiso ? ? 1.00000 ? ? H143' .82643 .23220 .98632 .05000 Uiso ? ? 1.00000 ? ? H144' .89717 .22052 .88317 .04500 Uiso ? ? 1.00000 ? ? H145' .87967 .20500 .68480 .04200 Uiso ? ? 1.00000 ? ? H16'a .85398 .18708 .52063 .05300 Uiso ? ? 1.00000 ? ? H16'b .81288 .15821 .53942 .05300 Uiso ? ? 1.00000 ? ? H2a .93165 .99521 .43394 .03600 Uiso ? ? 1.00000 ? ? H2b .93187 .99549 .55849 .03500 Uiso ? ? 1.00000 ? ? H20a 1.00847 .91095 .48054 .04700 Uiso ? ? 1.00000 ? ? H20b 1.00000 .94191 .53992 .04700 Uiso ? ? 1.00000 ? ? H20'a .93982 .95935 .25725 .04100 Uiso ? ? 1.00000 ? ? H20'b .93972 .92411 .25616 .04100 Uiso ? ? 1.00000 ? ? H21a .93441 .86364 .56911 .03200 Uiso ? ? 1.00000 ? ? H21b .88250 .84179 .53870 .03200 Uiso ? ? 1.00000 ? ? H22a .83104 .88508 .60474 .03300 Uiso ? ? 1.00000 ? ? H22b .87816 .87799 .70238 .03300 Uiso ? ? 1.00000 ? ? H23 .91832 .92534 .66897 .02600 Uiso ? ? 1.00000 ? ? H24a .81588 .94938 .60625 .03200 Uiso ? ? 1.00000 ? ? H24b .86290 .97030 .67358 .03200 Uiso ? ? 1.00000 ? ? H242 .90104 .93164 .87211 .04800 Uiso ? ? 1.00000 ? ? H243 .87105 .91710 1.04594 .05900 Uiso ? ? 1.00000 ? ? H244 .77981 .91787 1.06013 .04900 Uiso ? ? 1.00000 ? ? H245 .71740 .92991 .89892 .04800 Uiso ? ? 1.00000 ? ? H26a .68506 .90738 .67844 .04900 Uiso ? ? 1.00000 ? ? H26b .73507 .90181 .61561 .04900 Uiso ? ? 1.00000 ? ? H20' .91282 .87178 .38087 .02800 Uiso ? ? 1.00000 ? ? H21'a .80954 .86895 .41843 .03600 Uiso ? ? 1.00000 ? ? H21'b .83332 .85656 .30932 .03600 Uiso ? ? 1.00000 ? ? H22'a .83204 .91163 .23807 .03300 Uiso ? ? 1.00000 ? ? H22'b .77524 .90474 .27164 .03300 Uiso ? ? 1.00000 ? ? H23' .80198 .93702 .44668 .02800 Uiso ? ? 1.00000 ? ? H24'a .81881 .97738 .27482 .03200 Uiso ? ? 1.00000 ? ? H24'b .80150 .98726 .39336 .03200 Uiso ? ? 1.00000 ? ? H242' .75023 .98710 .11980 .04200 Uiso ? ? 1.00000 ? ? H243' .65995 .98761 .03812 .04600 Uiso ? ? 1.00000 ? ? H244' .59410 .96753 .14558 .04800 Uiso ? ? 1.00000 ? ? H245' .61677 .95131 .34003 .04300 Uiso ? ? 1.00000 ? ? H26'a .65925 .91349 .47954 .03900 Uiso ? ? 1.00000 ? ? H26'b .65271 .94909 .53857 .03900 Uiso ? ? 1.00000 ? ? H3a .58664 .74607 .58942 .04400 Uiso ? ? 1.00000 ? ? H3b .57874 .74359 .46250 .04400 Uiso ? ? 1.00000 ? ? H30a .50670 .66140 .54465 .04100 Uiso ? ? 1.00000 ? ? H30b .50908 .68702 .47291 .04100 Uiso ? ? 1.00000 ? ? H30'a .57895 .70984 .75127 .04300 Uiso ? ? 1.00000 ? ? H30'b .56729 .67726 .75525 .04300 Uiso ? ? 1.00000 ? ? H30 .59801 .61876 .62973 .02600 Uiso ? ? 1.00000 ? ? H31a .57597 .61219 .44069 .02800 Uiso ? ? 1.00000 ? ? H31b .62802 .59034 .46918 .02800 Uiso ? ? 1.00000 ? ? H32a .67915 .63469 .40736 .03300 Uiso ? ? 1.00000 ? ? H32b .63259 .62761 .30860 .03300 Uiso ? ? 1.00000 ? ? H33 .59146 .67456 .34314 .03000 Uiso ? ? 1.00000 ? ? H34a .69315 .69970 .40838 .04000 Uiso ? ? 1.00000 ? ? H34b .64577 .71997 .33967 .04000 Uiso ? ? 1.00000 ? ? H342 .60813 .68145 .14107 .04500 Uiso ? ? 1.00000 ? ? H343 .63893 .66742 -.03507 .04700 Uiso ? ? 1.00000 ? ? H344 .73129 .66681 -.04512 .04800 Uiso ? ? 1.00000 ? ? H345 .79221 .67784 .11599 .05400 Uiso ? ? 1.00000 ? ? H36a .82729 .65860 .33205 .04300 Uiso ? ? 1.00000 ? ? H36b .77785 .65065 .39451 .04300 Uiso ? ? 1.00000 ? ? H31'a .70011 .61583 .59054 .03100 Uiso ? ? 1.00000 ? ? H31'b .67603 .60321 .69894 .03100 Uiso ? ? 1.00000 ? ? H32'a .67903 .65812 .77396 .03200 Uiso ? ? 1.00000 ? ? H32'b .73548 .65120 .73857 .03200 Uiso ? ? 1.00000 ? ? H33' .71069 .67830 .57201 .02800 Uiso ? ? 1.00000 ? ? H34'a .69188 .72416 .74084 .03300 Uiso ? ? 1.00000 ? ? H34'b .70910 .73458 .62272 .03300 Uiso ? ? 1.00000 ? ? H342' .76002 .73336 .89683 .04400 Uiso ? ? 1.00000 ? ? H343' .85117 .73079 .97974 .05200 Uiso ? ? 1.00000 ? ? H344' .91721 .71515 .86731 .05300 Uiso ? ? 1.00000 ? ? H345' .89355 .69645 .67477 .04300 Uiso ? ? 1.00000 ? ? H36'a .85200 .66192 .53126 .04200 Uiso ? ? 1.00000 ? ? H36'b .85822 .69822 .47654 .04200 Uiso ? ? 1.00000 ? ? H4a .06920 .98964 .08652 .03900 Uiso ? ? 1.00000 ? ? H4b .08728 .98717 -.02027 .03900 Uiso ? ? 1.00000 ? ? H40a -.00003 .90908 .06097 .04600 Uiso ? ? 1.00000 ? ? H40b .00763 .92601 -.04096 .04600 Uiso ? ? 1.00000 ? ? H40'a .07305 .92176 .27090 .03300 Uiso ? ? 1.00000 ? ? H40'b .06751 .95588 .26211 .03300 Uiso ? ? 1.00000 ? ? H40 .09902 .86899 .14307 .02400 Uiso ? ? 1.00000 ? ? H41a .12841 .84044 -.01969 .03200 Uiso ? ? 1.00000 ? ? H41b .07457 .86061 -.04566 .03200 Uiso ? ? 1.00000 ? ? H42a .12786 .87729 -.18289 .03100 Uiso ? ? 1.00000 ? ? H42b .17488 .88627 -.08708 .03100 Uiso ? ? 1.00000 ? ? H43 .08213 .92135 -.14343 .02500 Uiso ? ? 1.00000 ? ? H44a .12557 .96795 -.17587 .02900 Uiso ? ? 1.00000 ? ? H44b .17614 .95633 -.09342 .02900 Uiso ? ? 1.00000 ? ? H442 .10945 .94300 -.37499 .03600 Uiso ? ? 1.00000 ? ? H443 .15161 .92718 -.53591 .05200 Uiso ? ? 1.00000 ? ? H444 .24304 .91192 -.50723 .04800 Uiso ? ? 1.00000 ? ? H445 .29187 .91230 -.32079 .04300 Uiso ? ? 1.00000 ? ? H46a .32450 .90558 -.13580 .04600 Uiso ? ? 1.00000 ? ? H46b .32277 .94588 -.13889 .04600 Uiso ? ? 1.00000 ? ? H41'a .17897 .85508 .20804 .03200 Uiso ? ? 1.00000 ? ? H41'b .20063 .86779 .09685 .03200 Uiso ? ? 1.00000 ? ? H42'a .23597 .90403 .24142 .03300 Uiso ? ? 1.00000 ? ? H42'b .17980 .91014 .27943 .03300 Uiso ? ? 1.00000 ? ? H43' .20751 .93222 .07065 .02700 Uiso ? ? 1.00000 ? ? H44'a .20674 .98652 .12430 .03600 Uiso ? ? 1.00000 ? ? H44'b .18540 .97644 .23862 .03600 Uiso ? ? 1.00000 ? ? H442' .24794 .98050 .40745 .04400 Uiso ? ? 1.00000 ? ? H443' .33531 .98050 .50355 .04800 Uiso ? ? 1.00000 ? ? H444' .40741 .96601 .40233 .05200 Uiso ? ? 1.00000 ? ? H445' .39157 .95614 .20193 .04700 Uiso ? ? 1.00000 ? ? H46'a .36332 .93007 .04310 .05300 Uiso ? ? 1.00000 ? ? H46'b .31571 .90557 .05862 .05300 Uiso ? ? 1.00000 ? ? H01a .00000 .82622 .09131 .06400 Uiso ? ? 1.00000 ? ? H01b -.02024 .78083 .07455 .06400 Uiso ? ? 1.00000 ? ? H02a -.01084 .86098 .75747 .07200 Uiso ? ? 1.00000 ? ? H02b -.00314 .89453 .74691 .07200 Uiso ? ? 1.00000 ? ? H03a .02945 .77510 .43702 .07300 Uiso ? ? 1.00000 ? ? H03b .00757 .81016 .43113 .07300 Uiso ? ? 1.00000 ? ? H04a .50311 .85678 .76886 .06300 Uiso ? ? 1.00000 ? ? H04b .48208 .87822 .72808 .06300 Uiso ? ? 1.00000 ? ? H05a .50073 .93030 .40590 .07300 Uiso ? ? 1.00000 ? ? H05b .51143 .97676 .41487 .07300 Uiso ? ? 1.00000 ? ? H06a .49978 .93600 .08062 .07200 Uiso ? ? 1.00000 ? ? H06b .48126 .97151 .08015 .07200 Uiso ? ? 1.00000 ? ? H07b -.01262 .71795 .11954 .07900 Uiso ? ? 1.00000 ? ? H07a -.04831 .73798 .13402 .07900 Uiso ? ? 1.00000 ? ? H08a .44685 1.02937 .11678 .08600 Uiso ? ? 1.00000 ? ? H08b .48449 1.02809 .09069 .08600 Uiso ? ? 1.00000 ? ? H09a .01341 .77854 -.16778 .07900 Uiso ? ? 1.00000 ? ? H09b .04748 .77684 -.05465 .07900 Uiso ? ? 1.00000 ? ? H010a .51137 1.02565 .42240 .08800 Uiso ? ? 1.00000 ? ? H010b .53618 .99359 .38012 .08800 Uiso ? ? 1.00000 ? ? H013a .54864 .91652 .56500 .12400 Uiso ? ? 1.00000 ? ? H013b .56671 .92966 .71565 .12400 Uiso ? ? 1.00000 ? ? 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 Ni1 .0149(3) .0209(3) .0137(3) .0016(3) .0024(2) .0001(3) Ni2 .0123(3) .0202(3) .0181(4) -.0018(2) .0040(3) -.0019(3) Ni3 .0169(3) .0188(3) .0170(4) .0045(3) .0034(3) .0025(3) Ni4 .0146(3) .0200(3) .0156(3) .0031(2) .0051(3) .0009(3) O1 .024(2) .022(2) .021(2) .0115(15) .0009(15) .0013(16) O10 .020(2) .048(3) .024(2) -.0028(18) -.0020(16) .0045(19) O10' .0193(18) .030(2) .0149(19) .0020(15) .0056(14) -.0014(15) N10 .016(2) .027(2) .015(2) -.0029(18) .0029(17) .0026(19) C11 .023(3) .016(3) .020(3) -.003(2) .005(2) .000(2) C12 .021(3) .023(3) .022(3) .000(2) .006(2) -.002(2) N13 .017(2) .025(2) .020(2) .0020(18) .0021(18) .0060(19) C14 .025(3) .025(3) .022(3) .002(2) .008(2) .000(2) C141 .023(3) .025(3) .018(3) -.002(2) .007(2) .002(2) C142 .027(3) .044(4) .018(3) .009(3) .005(2) .005(3) C143 .042(4) .041(4) .020(3) .009(3) .004(3) .002(3) C144 .047(4) .039(4) .026(3) .018(3) .020(3) -.000(3) C145 .026(3) .038(3) .034(3) .007(3) .011(3) -.004(3) C146 .035(3) .016(3) .027(3) .007(2) .008(2) .000(2) O15 .026(2) .035(2) .027(2) .0046(17) .0018(17) .0062(18) C16 .022(3) .043(4) .040(4) .004(3) .005(3) -.014(3) C11' .019(3) .021(3) .022(3) .001(2) .004(2) .004(2) C12' .022(3) .026(3) .022(3) .003(2) .001(2) .002(2) N13' .016(2) .020(2) .018(2) .0001(17) .0033(17) .0001(18) C14' .022(3) .019(3) .027(3) .002(2) .003(2) -.005(2) C141' .026(3) .011(2) .024(3) -.000(2) -.000(2) -.004(2) C142' .034(3) .018(3) .033(3) .002(2) -.001(3) -.007(2) C143' .042(4) .039(4) .028(3) .002(3) -.009(3) -.005(3) C144' .030(3) .016(3) .051(4) .001(2) -.008(3) -.001(3) C145' .023(3) .038(3) .031(3) -.002(2) .004(2) .008(3) C146' .023(3) .022(3) .022(3) -.005(2) .001(2) .003(2) O15' .024(2) .049(3) .020(2) .0045(18) .0060(16) .0027(19) C16' .031(3) .046(4) .043(4) .014(3) -.006(3) -.015(3) O2 .0212(18) .022(2) .021(2) -.0037(15) .0044(15) .0041(15) O20 .0157(18) .035(2) .037(2) -.0001(16) .0020(17) -.0090(19) O20' .0202(19) .031(2) .027(2) -.0015(16) .0106(16) -.0024(17) N20 .014(2) .023(2) .021(2) -.0019(17) .0031(17) -.0010(19) C21 .019(3) .026(3) .028(3) -.001(2) .004(2) .005(2) C22 .023(3) .028(3) .022(3) -.002(2) .005(2) .007(2) N23 .018(2) .019(2) .018(2) .0007(17) .0055(17) .0005(18) C24 .029(3) .023(3) .022(3) .005(2) .010(2) -.002(2) C241 .023(3) .022(3) .018(3) -.006(2) .006(2) -.004(2) C242 .020(3) .061(4) .029(3) -.014(3) .005(2) -.001(3) C243 .041(4) .090(6) .014(3) -.025(4) -.000(3) .004(3) C244 .038(4) .051(4) .028(3) -.005(3) .016(3) -.002(3) C245 .029(3) .050(4) .043(4) -.008(3) .021(3) .008(3) C246 .020(3) .042(4) .034(4) -.005(3) -.004(2) .012(3) O25 .041(3) .041(3) .040(3) -.010(2) .000(2) .006(2) C26 .049(4) .045(4) .027(3) -.022(3) .011(3) .000(3) C21' .017(3) .034(3) .031(3) -.002(2) -.001(2) -.007(3) C22' .018(3) .029(3) .028(3) -.004(2) .002(2) -.002(2) N23' .016(2) .024(2) .022(2) .0007(18) .0016(18) -.005(2) C24' .016(2) .025(3) .026(3) -.002(2) .001(2) .001(2) C241' .022(3) .023(3) .025(3) .006(2) .002(2) -.004(2) C242' .032(3) .031(3) .030(3) -.004(3) -.001(3) .007(3) C243' .043(4) .026(3) .035(4) .000(3) -.010(3) .009(3) C244' .024(3) .035(3) .044(4) -.002(3) -.005(3) .004(3) C245' .021(3) .034(3) .041(4) .002(2) .003(3) -.009(3) C246' .023(3) .020(3) .030(3) .002(2) .004(2) -.004(2) O25' .021(2) .064(3) .019(2) -.012(2) .0047(16) -.004(2) C26' .018(3) .033(3) .035(3) -.003(2) .007(2) .010(3) O3 .032(2) .025(2) .024(2) .0046(16) .0041(17) .0044(17) O30 .0214(19) .031(2) .026(2) .0027(16) .0032(16) .0106(17) O30' .025(2) .032(2) .024(2) .0017(16) .0067(16) .0005(17) N30 .015(2) .024(2) .016(2) -.0001(17) .0038(17) .0013(18) C31 .019(3) .017(3) .023(3) .001(2) .000(2) -.000(2) C32 .023(3) .027(3) .022(3) .001(2) .005(2) .000(2) N33 .020(2) .031(3) .017(2) .0047(19) .0005(18) .002(2) C34 .037(3) .025(3) .021(3) -.002(2) .006(2) .006(2) C341 .032(3) .014(3) .021(3) .001(2) .005(2) .005(2) C342 .027(3) .057(4) .021(3) .010(3) .006(2) .001(3) C343 .041(4) .045(4) .022(3) .016(3) .001(3) .008(3) C344 .047(4) .032(3) .032(4) .013(3) .020(3) .001(3) C345 .026(3) .038(4) .058(5) .001(3) .015(3) -.013(3) C346 .027(3) .017(3) .046(4) .003(2) -.000(3) -.012(3) O35 .033(2) .035(2) .050(3) .0023(19) -.002(2) -.009(2) C36 .034(3) .033(3) .030(3) .008(3) .010(3) .006(3) C31' .022(3) .021(3) .026(3) .007(2) .000(2) .005(2) C32' .022(3) .019(3) .026(3) .005(2) .000(2) .006(2) N33' .022(2) .017(2) .022(2) .0008(18) .0032(18) -.0002(18) C34' .024(3) .018(3) .030(3) .001(2) .006(2) -.007(2) C341' .031(3) .016(3) .027(3) -.000(2) -.001(2) -.002(2) C342' .040(3) .019(3) .031(3) -.006(2) .003(3) -.001(2) C343' .051(4) .027(3) .035(4) -.008(3) -.011(3) -.003(3) C344' .031(3) .037(4) .056(5) -.013(3) -.012(3) .006(3) C345' .031(3) .027(3) .040(4) -.004(2) .004(3) .006(3) C346' .025(3) .031(3) .023(3) -.006(2) .004(2) .003(2) O35' .025(2) .042(2) .027(2) .0073(18) .0044(17) -.0028(19) C36' .021(3) .043(4) .039(4) .004(3) -.000(3) -.006(3) O4 .030(2) .024(2) .022(2) .0086(16) .0081(16) .0019(16) O40 .0193(19) .047(3) .022(2) .0014(17) .0038(16) .0090(18) O40' .0223(18) .0176(18) .020(2) .0051(14) .0086(15) .0026(15) N40 .015(2) .016(2) .021(2) .0013(16) .0065(17) .0012(18) C41 .021(3) .031(3) .021(3) -.001(2) .004(2) -.002(2) C42 .026(3) .016(3) .024(3) .003(2) .010(2) -.004(2) N43 .021(2) .020(2) .017(2) .0020(17) .0067(17) -.0002(18) C44 .027(3) .020(3) .018(3) .004(2) .010(2) .002(2) C441 .019(3) .024(3) .022(3) .007(2) .008(2) .002(2) C442 .026(3) .028(3) .027(3) .010(2) .006(2) .003(2) C443 .046(4) .060(4) .014(3) .013(3) .006(3) -.004(3) C444 .043(4) .038(4) .033(4) .006(3) .023(3) .004(3) C445 .029(3) .034(3) .038(4) .008(3) .014(3) .005(3) C446 .026(3) .023(3) .021(3) .004(2) .007(2) .003(2) O45 .021(2) .047(3) .025(2) .0010(18) .0024(16) -.0025(19) C46 .022(3) .030(3) .052(4) .010(2) .013(3) -.006(3) C41' .020(3) .019(3) .031(3) -.002(2) .001(2) .004(2) C42' .020(3) .025(3) .024(3) .003(2) .001(2) .002(2) N43' .016(2) .023(2) .022(2) .0034(17) .0026(18) .0008(19) C44' .024(3) .027(3) .027(3) -.000(2) .003(2) -.004(2) C441' .028(3) .019(3) .030(3) -.006(2) .002(2) .004(2) C442' .043(4) .028(3) .030(3) .001(3) -.000(3) -.006(3) C443' .047(4) .021(3) .037(4) -.004(3) -.011(3) -.007(3) C444' .035(3) .036(4) .045(4) -.008(3) -.009(3) .013(3) C445' .022(3) .033(3) .050(4) -.013(2) -.004(3) .006(3) C446' .024(3) .025(3) .029(3) .000(2) -.001(2) .009(2) O45' .031(2) .025(2) .028(2) .0058(16) .0060(17) .0017(17) C46' .031(3) .029(3) .053(4) .007(3) -.002(3) -.010(3) S1 .0211(6) .0227(7) .0129(6) -.0028(5) .0041(5) -.0019(5) O11 .033(2) .022(2) .026(2) -.0020(19) .001(2) .005(2) O12 .023(2) .019(2) .097(5) -.001(2) .009(3) -.006(3) O13 .073(4) .029(3) .016(2) -.027(2) .021(2) -.006(2) O14 .027(2) .018(2) .031(3) -.0060(17) -.002(2) .0088(19) S2 .0170(6) .0108(6) .0177(6) .0016(4) .0040(5) .0004(5) O21 .049(3) .021(2) .024(3) -.013(2) .020(2) -.005(2) O22 .030(2) .017(2) .023(2) -.0063(18) .004(2) .0035(19) O23 .034(2) .016(2) .015(2) -.0055(18) -.0035(19) -.0021(18) O24 .015(2) .022(2) .060(4) .0062(18) .003(2) -.004(2) S3 .0218(7) .0190(7) .0329(8) -.0031(5) .0109(6) -.0023(6) O31 .031(2) .029(2) .043(3) -.0037(17) .022(2) -.009(2) O32 .030(2) .019(2) .032(2) -.0041(16) .0101(17) -.0012(17) O33 .033(2) .024(2) .034(2) -.0020(17) .0106(18) -.0008(18) O34 .030(2) .025(2) .051(3) -.0047(17) .028(2) .002(2) S4 .0225(7) .0238(7) .0307(8) -.0001(5) .0146(6) -.0019(6) O41 .024(2) .049(3) .029(2) .0004(18) .0099(17) -.009(2) O42 .029(2) .021(2) .048(3) -.0003(16) .025(2) .0014(19) O43 .030(2) .027(2) .041(3) -.0025(17) .0222(19) -.0041(19) O44 .030(2) .027(2) .031(2) -.0032(17) .0108(17) -.0044(18) O01 .055(3) .037(3) .038(3) .003(2) .007(2) -.003(2) O02 .053(3) .044(3) .041(3) -.002(2) -.009(2) .006(2) O03 .058(3) .044(3) .048(3) -.009(2) .002(2) .004(2) O04 .064(3) .028(2) .041(3) -.001(2) -.014(2) .004(2) O05 .058(3) .042(3) .038(3) .001(2) .005(2) -.009(2) O06 .060(3) .034(3) .050(3) -.002(2) .014(2) .007(2) O07 .077(4) .038(3) .051(3) -.004(3) .023(3) -.009(2) O08 .078(4) .051(3) .048(3) .014(3) .024(3) .009(3) O09 .067(3) .048(3) .048(3) .009(3) .015(3) -.007(2) O010 .067(4) .054(3) .056(4) .002(3) .018(3) -.003(3) O011 .061(3) .048(3) .054(3) .001(3) .003(3) .009(3) O012 .074(4) .065(4) .069(4) -.006(3) .006(3) .013(3) O013 .054(4) .101(5) .092(5) .001(3) -.003(3) .036(4) O014 .049(3) .082(4) .070(4) -.001(3) .004(3) .020(3) O015 .067(4) .078(4) .072(4) .010(3) .012(3) -.005(3) O016 .015(3) .029(4) .025(4) .004(3) .002(3) -.003(3) O017 .042(10) .030(9) .054(12) -.022(8) .015(9) -.021(9) O018 .047(12) .058(13) .047(12) -.008(10) .000(9) -.011(10) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ni1 O1 . . 2.080(4) ? Ni1 O10 . . 2.093(4) ? Ni1 O10' . . 2.101(4) ? Ni1 N10 . . 2.075(4) ? Ni1 N13 . . 2.113(5) ? Ni1 N13' . . 2.134(4) ? Ni2 O2 . . 2.063(4) ? Ni2 O20 . . 2.101(4) ? Ni2 O20' . . 2.096(4) ? Ni2 N20 . . 2.079(4) ? Ni2 N23 . . 2.122(5) ? Ni2 N23' . . 2.124(4) ? Ni3 O3 . . 2.099(4) ? Ni3 O30 . . 2.090(4) ? Ni3 O30' . . 2.087(4) ? Ni3 N30 . . 2.075(4) ? Ni3 N33 . . 2.127(5) ? Ni3 N33' . . 2.117(4) ? Ni4 O4 . . 2.070(4) ? Ni4 O40 . . 2.091(4) ? Ni4 O40' . . 2.096(4) ? Ni4 N40 . . 2.072(4) ? Ni4 N43 . . 2.103(4) ? Ni4 N43' . . 2.142(4) ? O1 H1a . . .870 ? O1 H1b . . .908 ? O10 H10a . . .808 ? O10 H10b . . .939 ? O10' H10'a . . 1.031 ? O10' H10'b . . .726 ? N10 C11 . . 1.486(7) ? N10 C11' . . 1.478(6) ? N10 H10 . . .931 ? C11 C12 . . 1.517(8) ? C11 H11a . . .949 ? C11 H11b . . .951 ? C12 N13 . . 1.477(7) ? C12 H12a . . .955 ? C12 H12b . . .953 ? N13 C14 . . 1.492(7) ? N13 H13 . . .928 ? C14 C141 . . 1.513(8) ? C14 H14a . . .963 ? C14 H14b . . .955 ? C141 C142 . . 1.391(7) ? C141 C146 . . 1.381(8) ? C142 C143 . . 1.383(9) ? C142 H142 . . .958 ? C143 C144 . . 1.386(9) ? C143 H143 . . .965 ? C144 C145 . . 1.394(8) ? C144 H144 . . .953 ? C145 C146 . . 1.403(9) ? C145 H145 . . .972 ? C146 O15 . . 1.374(7) ? O15 C16 . . 1.405(7) ? C16 C16' . . 1.496(9) ? C16 H16a . . .964 ? C16 H16b . . .958 ? C11' C12' . . 1.513(7) ? C11' H11'a . . .963 ? C11' H11'b . . .963 ? C12' N13' . . 1.477(7) ? C12' H12'a . . .955 ? C12' H12'b . . .945 ? N13' C14' . . 1.491(7) ? N13' H13' . . .929 ? C14' C141' . . 1.503(7) ? C14' H14'a . . .961 ? C14' H14'b . . .955 ? C141' C142' . . 1.375(8) ? C141' C146' . . 1.419(8) ? C142' C143' . . 1.385(8) ? C142' H142' . . .965 ? C143' C144' . . 1.372(10) ? C143' H143' . . .963 ? C144' C145' . . 1.396(9) ? C144' H144' . . .956 ? C145' C146' . . 1.381(7) ? C145' H145' . . .965 ? C146' O15' . . 1.388(7) ? O15' C16' . . 1.405(8) ? C16' H16'a . . .954 ? C16' H16'b . . .976 ? O2 H2a . . .866 ? O2 H2b . . 1.024 ? O20 H20a . . .885 ? O20 H20b . . .878 ? O20' H20'a . . .931 ? O20' H20'b . . .885 ? N20 C21 . . 1.494(7) ? N20 C21' . . 1.485(6) ? N20 H20' . . .921 ? C21 C22 . . 1.516(8) ? C21 H21a . . .948 ? C21 H21b . . .961 ? C22 N23 . . 1.491(7) ? C22 H22a . . .961 ? C22 H22b . . .953 ? N23 C24 . . 1.497(7) ? N23 H23 . . .926 ? C24 C241 . . 1.507(8) ? C24 H24a . . .956 ? C24 H24b . . .954 ? C241 C242 . . 1.387(8) ? C241 C246 . . 1.397(8) ? C242 C243 . . 1.382(10) ? C242 H242 . . .961 ? C243 C244 . . 1.360(10) ? C243 H243 . . .962 ? C244 C245 . . 1.366(9) ? C244 H244 . . .953 ? C245 C246 . . 1.385(10) ? C245 H245 . . .960 ? C246 O25 . . 1.377(7) ? O25 C26 . . 1.408(8) ? C26 C26' . . 1.503(9) ? C26 H26a . . .953 ? C26 H26b . . .977 ? C21' C22' . . 1.500(8) ? C21' H21'a . . .962 ? C21' H21'b . . .950 ? C22' N23' . . 1.466(7) ? C22' H22'a . . .954 ? C22' H22'b . . .953 ? N23' C24' . . 1.475(7) ? N23' H23' . . .926 ? C24' C241' . . 1.526(7) ? C24' H24'a . . .949 ? C24' H24'b . . .953 ? C241' C242' . . 1.380(8) ? C241' C246' . . 1.415(8) ? C242' C243' . . 1.395(9) ? C242' H242' . . .963 ? C243' C244' . . 1.382(10) ? C243' H243' . . .959 ? C244' C245' . . 1.384(9) ? C244' H244' . . .962 ? C245' C246' . . 1.401(7) ? C245' H245' . . .953 ? C246' O25' . . 1.364(7) ? O25' C26' . . 1.439(7) ? C26' H26'a . . .942 ? C26' H26'b . . .974 ? O3 H3a . . .833 ? O3 H3b . . .997 ? O30 H30a . . .852 ? O30 H30b . . .790 ? O30' H30'a . . .935 ? O30' H30'b . . .805 ? N30 C31 . . 1.476(7) ? N30 C31' . . 1.477(6) ? N30 H30 . . .930 ? C31 C32 . . 1.522(8) ? C31 H31a . . .953 ? C31 H31b . . .953 ? C32 N33 . . 1.479(7) ? C32 H32a . . .956 ? C32 H32b . . .954 ? N33 C34 . . 1.491(8) ? N33 H33 . . .927 ? C34 C341 . . 1.512(8) ? C34 H34a . . .965 ? C34 H34b . . .959 ? C341 C342 . . 1.400(8) ? C341 C346 . . 1.383(8) ? C342 C343 . . 1.397(9) ? C342 H342 . . .961 ? C343 C344 . . 1.380(10) ? C343 H343 . . .960 ? C344 C345 . . 1.345(9) ? C344 H344 . . .962 ? C345 C346 . . 1.408(10) ? C345 H345 . . .951 ? C346 O35 . . 1.392(7) ? O35 C36 . . 1.418(7) ? C36 C36' . . 1.490(9) ? C36 H36a . . .958 ? C36 H36b . . .955 ? C31' C32' . . 1.509(7) ? C31' H31'a . . .952 ? C31' H31'b . . .956 ? C32' N33' . . 1.461(7) ? C32' H32'a . . .948 ? C32' H32'b . . .955 ? N33' C34' . . 1.493(7) ? N33' H33' . . .931 ? C34' C341' . . 1.507(7) ? C34' H34'a . . .953 ? C34' H34'b . . .964 ? C341' C342' . . 1.389(8) ? C341' C346' . . 1.420(8) ? C342' C343' . . 1.408(9) ? C342' H342' . . .970 ? C343' C344' . . 1.371(10) ? C343' H343' . . .966 ? C344' C345' . . 1.375(10) ? C344' H344' . . .960 ? C345' C346' . . 1.385(8) ? C345' H345' . . .975 ? C346' O35' . . 1.390(7) ? O35' C36' . . 1.413(8) ? C36' H36'a . . .971 ? C36' H36'b . . .949 ? O4 H4a . . .804 ? O4 H4b . . .785 ? O40 H40a . . .861 ? O40 H40b . . .877 ? O40' H40'a . . .888 ? O40' H40'b . . .918 ? N40 C41 . . 1.488(7) ? N40 C41' . . 1.490(6) ? N40 H40 . . .922 ? C41 C42 . . 1.512(8) ? C41 H41a . . .963 ? C41 H41b . . .955 ? C42 N43 . . 1.485(7) ? C42 H42a . . .955 ? C42 H42b . . .956 ? N43 C44 . . 1.497(7) ? N43 H43 . . .929 ? C44 C441 . . 1.505(8) ? C44 H44a . . .952 ? C44 H44b . . .952 ? C441 C442 . . 1.376(8) ? C441 C446 . . 1.399(7) ? C442 C443 . . 1.398(9) ? C442 H442 . . .956 ? C443 C444 . . 1.388(9) ? C443 H443 . . .958 ? C444 C445 . . 1.392(9) ? C444 H444 . . .956 ? C445 C446 . . 1.373(9) ? C445 H445 . . .955 ? C446 O45 . . 1.398(7) ? O45 C46 . . 1.407(7) ? C46 C46' . . 1.490(10) ? C46 H46a . . .960 ? C46 H46b . . .956 ? C41' C42' . . 1.491(8) ? C41' H41'a . . .952 ? C41' H41'b . . .966 ? C42' N43' . . 1.480(7) ? C42' H42'a . . .950 ? C42' H42'b . . .962 ? N43' C44' . . 1.483(7) ? N43' H43' . . .925 ? C44' C441' . . 1.529(8) ? C44' H44'a . . .951 ? C44' H44'b . . .953 ? C441' C442' . . 1.385(9) ? C441' C446' . . 1.393(9) ? C442' C443' . . 1.376(9) ? C442' H442' . . .965 ? C443' C444' . . 1.391(10) ? C443' H443' . . .964 ? C444' C445' . . 1.361(10) ? C444' H444' . . .964 ? C445' C446' . . 1.391(8) ? C445' H445' . . .976 ? C446' O45' . . 1.382(7) ? O45' C46' . . 1.450(8) ? C46' H46'a . . .951 ? C46' H46'b . . .969 ? S1 O11 . . 1.433(4) ? S1 O12 . . 1.483(5) ? S1 O13 . . 1.461(5) ? S1 O14 . . 1.470(4) ? S1 O11' . . 1.62(3) ? S1 O12' . . 1.49(5) ? S1 O13' . . 1.40(4) ? S1 O14' . . 1.54(6) ? S2 O21 . . 1.476(5) ? S2 O22 . . 1.469(4) ? S2 O23 . . 1.462(4) ? S2 O24 . . 1.481(4) ? S2 O21' . . 1.55(2) ? S2 O22' . . 1.48(2) ? S2 O23' . . 1.50(3) ? S2 O24' . . 1.44(2) ? S3 O31 . . 1.469(5) ? S3 O32 . . 1.485(4) ? S3 O33 . . 1.484(4) ? S3 O34 . . 1.469(5) ? S4 O41 . . 1.486(4) ? S4 O42 . . 1.473(4) ? S4 O43 . . 1.469(5) ? S4 O44 . . 1.493(4) ? O01 H01a . . 1.084 ? O01 H01b . . .930 ? O02 H02a . . .796 ? O02 H02b . . .859 ? O03 H03a . . .961 ? O03 H03b . . .957 ? O04 H04a . . .767 ? O04 H04b . . .524 ? O05 H05a . . 1.129 ? O05 H05b . . 1.198 ? O06 H06a . . .986 ? O06 H06b . . .908 ? O07 H07b . . .868 ? O07 H07a . . .703 ? O08 H08a . . .814 ? O08 H08b . . .924 ? O09 H09a . . .987 ? O09 H09b . . .926 ? O010 H010a . . .980 ? O010 H010b . . .890 ? O013 H013a . . 1.070 ? O013 H013b . . 1.118 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O1 Ni1 O10 . . . 88.72(15) ? O1 Ni1 O10' . . . 88.14(15) ? O1 Ni1 N10 . . . 177.01(17) ? O1 Ni1 N13 . . . 93.13(16) ? O1 Ni1 N13' . . . 96.56(15) ? O10 Ni1 O10' . . . 88.38(15) ? O10 Ni1 N10 . . . 92.68(16) ? O10 Ni1 N13 . . . 89.03(16) ? O10 Ni1 N13' . . . 173.58(17) ? O10' Ni1 N10 . . . 94.54(16) ? O10' Ni1 N13 . . . 177.08(15) ? O10' Ni1 N13' . . . 88.14(15) ? N10 Ni1 N13 . . . 84.25(17) ? N10 Ni1 N13' . . . 82.22(16) ? N13 Ni1 N13' . . . 94.31(16) ? O2 Ni2 O20 . . . 91.50(15) ? O2 Ni2 O20' . . . 90.47(15) ? O2 Ni2 N20 . . . 176.19(17) ? O2 Ni2 N23 . . . 92.13(16) ? O2 Ni2 N23' . . . 95.81(15) ? O20 Ni2 O20' . . . 90.10(15) ? O20 Ni2 N20 . . . 90.06(16) ? O20 Ni2 N23 . . . 87.80(16) ? O20 Ni2 N23' . . . 172.45(17) ? O20' Ni2 N20 . . . 93.00(17) ? O20' Ni2 N23 . . . 176.70(16) ? O20' Ni2 N23' . . . 87.95(16) ? N20 Ni2 N23 . . . 84.46(17) ? N20 Ni2 N23' . . . 82.76(16) ? N23 Ni2 N23' . . . 93.80(17) ? O3 Ni3 O30 . . . 90.50(15) ? O3 Ni3 O30' . . . 89.00(16) ? O3 Ni3 N30 . . . 176.89(17) ? O3 Ni3 N33 . . . 92.52(17) ? O3 Ni3 N33' . . . 96.05(15) ? O30 Ni3 O30' . . . 90.60(15) ? O30 Ni3 N30 . . . 91.07(15) ? O30 Ni3 N33 . . . 87.36(16) ? O30 Ni3 N33' . . . 173.18(16) ? O30' Ni3 N30 . . . 93.67(16) ? O30' Ni3 N33 . . . 177.47(17) ? O30' Ni3 N33' . . . 87.61(16) ? N30 Ni3 N33 . . . 84.87(18) ? N30 Ni3 N33' . . . 82.49(16) ? N33 Ni3 N33' . . . 94.24(17) ? O4 Ni4 O40 . . . 90.87(16) ? O4 Ni4 O40' . . . 87.51(15) ? O4 Ni4 N40 . . . 177.40(16) ? O4 Ni4 N43 . . . 93.40(16) ? O4 Ni4 N43' . . . 95.84(16) ? O40 Ni4 O40' . . . 89.11(15) ? O40 Ni4 N40 . . . 90.94(16) ? O40 Ni4 N43 . . . 88.59(16) ? O40 Ni4 N43' . . . 172.40(17) ? O40' Ni4 N40 . . . 94.39(16) ? O40' Ni4 N43 . . . 177.54(16) ? O40' Ni4 N43' . . . 87.63(16) ? N40 Ni4 N43 . . . 84.78(17) ? N40 Ni4 N43' . . . 82.48(16) ? N43 Ni4 N43' . . . 94.55(17) ? Ni1 O1 H1a . . . 102.1 ? Ni1 O1 H1b . . . 116.2 ? H1a O1 H1b . . . 106.9 ? Ni1 O10 H10a . . . 122.5 ? Ni1 O10 H10b . . . 130.2 ? H10a O10 H10b . . . 106.0 ? Ni1 O10' H10'a . . . 117.1 ? Ni1 O10' H10'b . . . 133.0 ? H10'a O10' H10'b . . . 85.4 ? Ni1 N10 C11 . . . 106.0(3) ? Ni1 N10 C11' . . . 110.8(3) ? Ni1 N10 H10 . . . 109.3 ? C11 N10 C11' . . . 112.4(4) ? C11 N10 H10 . . . 109.6 ? C11' N10 H10 . . . 108.6 ? N10 C11 C12 . . . 109.0(4) ? N10 C11 H11a . . . 110.0 ? N10 C11 H11b . . . 109.6 ? C12 C11 H11a . . . 109.6 ? C12 C11 H11b . . . 109.1 ? H11a C11 H11b . . . 109.5 ? C11 C12 N13 . . . 109.4(4) ? C11 C12 H12a . . . 109.5 ? C11 C12 H12b . . . 109.5 ? N13 C12 H12a . . . 110.1 ? N13 C12 H12b . . . 109.6 ? H12a C12 H12b . . . 108.8 ? Ni1 N13 C12 . . . 107.1(3) ? Ni1 N13 C14 . . . 114.7(3) ? Ni1 N13 H13 . . . 108.8 ? C12 N13 C14 . . . 113.4(4) ? C12 N13 H13 . . . 104.3 ? C14 N13 H13 . . . 107.9 ? N13 C14 C141 . . . 115.6(4) ? N13 C14 H14a . . . 107.7 ? N13 C14 H14b . . . 107.7 ? C141 C14 H14a . . . 108.5 ? C141 C14 H14b . . . 109.1 ? H14a C14 H14b . . . 107.9 ? C14 C141 C142 . . . 120.6(5) ? C14 C141 C146 . . . 119.9(5) ? C142 C141 C146 . . . 119.4(5) ? C141 C142 C143 . . . 120.8(5) ? C141 C142 H142 . . . 119.5 ? C143 C142 H142 . . . 119.7 ? C142 C143 C144 . . . 119.6(5) ? C142 C143 H143 . . . 120.9 ? C144 C143 H143 . . . 119.5 ? C143 C144 C145 . . . 120.7(6) ? C143 C144 H144 . . . 120.1 ? C145 C144 H144 . . . 119.2 ? C144 C145 C146 . . . 118.8(5) ? C144 C145 H145 . . . 120.5 ? C146 C145 H145 . . . 120.7 ? C141 C146 C145 . . . 120.7(5) ? C141 C146 O15 . . . 116.2(5) ? C145 C146 O15 . . . 123.1(5) ? C146 O15 C16 . . . 118.2(5) ? O15 C16 C16' . . . 109.2(5) ? O15 C16 H16a . . . 110.6 ? O15 C16 H16b . . . 110.9 ? C16' C16 H16a . . . 109.9 ? C16' C16 H16b . . . 108.7 ? H16a C16 H16b . . . 107.7 ? N10 C11' C12' . . . 110.6(4) ? N10 C11' H11'a . . . 110.3 ? N10 C11' H11'b . . . 109.6 ? C12' C11' H11'a . . . 109.2 ? C12' C11' H11'b . . . 109.8 ? H11'a C11' H11'b . . . 107.2 ? C11' C12' N13' . . . 109.1(4) ? C11' C12' H12'a . . . 110.7 ? C11' C12' H12'b . . . 110.3 ? N13' C12' H12'a . . . 108.6 ? N13' C12' H12'b . . . 108.7 ? H12'a C12' H12'b . . . 109.5 ? Ni1 N13' C12' . . . 102.7(3) ? Ni1 N13' C14' . . . 118.7(3) ? Ni1 N13' H13' . . . 110.6 ? C12' N13' C14' . . . 113.1(4) ? C12' N13' H13' . . . 110.4 ? C14' N13' H13' . . . 101.4 ? N13' C14' C141' . . . 115.2(4) ? N13' C14' H14'a . . . 107.9 ? N13' C14' H14'b . . . 108.0 ? C141' C14' H14'a . . . 108.7 ? C141' C14' H14'b . . . 108.7 ? H14'a C14' H14'b . . . 108.1 ? C14' C141' C142' . . . 121.3(5) ? C14' C141' C146' . . . 121.6(5) ? C142' C141' C146' . . . 117.2(5) ? C141' C142' C143' . . . 122.4(6) ? C141' C142' H142' . . . 118.8 ? C143' C142' H142' . . . 118.8 ? C142' C143' C144' . . . 119.8(6) ? C142' C143' H143' . . . 120.6 ? C144' C143' H143' . . . 119.5 ? C143' C144' C145' . . . 119.8(5) ? C143' C144' H144' . . . 119.5 ? C145' C144' H144' . . . 120.7 ? C144' C145' C146' . . . 119.9(6) ? C144' C145' H145' . . . 120.4 ? C146' C145' H145' . . . 119.7 ? C141' C146' C145' . . . 120.8(5) ? C141' C146' O15' . . . 115.4(4) ? C145' C146' O15' . . . 123.8(5) ? C146' O15' C16' . . . 117.5(4) ? C16 C16' O15' . . . 109.3(5) ? C16 C16' H16'a . . . 111.5 ? C16 C16' H16'b . . . 109.2 ? O15' C16' H16'a . . . 110.9 ? O15' C16' H16'b . . . 108.9 ? H16'a C16' H16'b . . . 106.9 ? Ni2 O2 H2a . . . 110.0 ? Ni2 O2 H2b . . . 122.8 ? H2a O2 H2b . . . 100.1 ? Ni2 O20 H20a . . . 134.2 ? Ni2 O20 H20b . . . 112.3 ? H20a O20 H20b . . . 106.0 ? Ni2 O20' H20'a . . . 124.5 ? Ni2 O20' H20'b . . . 114.0 ? H20'a O20' H20'b . . . 96.6 ? Ni2 N20 C21 . . . 105.7(3) ? Ni2 N20 C21' . . . 109.6(3) ? Ni2 N20 H20' . . . 109.4 ? C21 N20 C21' . . . 113.7(4) ? C21 N20 H20' . . . 109.2 ? C21' N20 H20' . . . 109.2 ? N20 C21 C22 . . . 109.9(4) ? N20 C21 H21a . . . 110.0 ? N20 C21 H21b . . . 109.0 ? C22 C21 H21a . . . 109.7 ? C22 C21 H21b . . . 109.6 ? H21a C21 H21b . . . 108.7 ? C21 C22 N23 . . . 110.1(5) ? C21 C22 H22a . . . 109.6 ? C21 C22 H22b . . . 110.0 ? N23 C22 H22a . . . 109.0 ? N23 C22 H22b . . . 109.8 ? H22a C22 H22b . . . 108.3 ? Ni2 N23 C22 . . . 107.6(3) ? Ni2 N23 C24 . . . 115.0(3) ? Ni2 N23 H23 . . . 107.9 ? C22 N23 C24 . . . 112.2(4) ? C22 N23 H23 . . . 105.6 ? C24 N23 H23 . . . 108.1 ? N23 C24 C241 . . . 115.8(4) ? N23 C24 H24a . . . 107.8 ? N23 C24 H24b . . . 108.2 ? C241 C24 H24a . . . 108.0 ? C241 C24 H24b . . . 108.2 ? H24a C24 H24b . . . 108.6 ? C24 C241 C242 . . . 122.5(5) ? C24 C241 C246 . . . 121.3(5) ? C242 C241 C246 . . . 116.2(5) ? C241 C242 C243 . . . 122.1(6) ? C241 C242 H242 . . . 118.8 ? C243 C242 H242 . . . 119.1 ? C242 C243 C244 . . . 119.8(6) ? C242 C243 H243 . . . 119.5 ? C244 C243 H243 . . . 120.7 ? C243 C244 C245 . . . 120.5(6) ? C243 C244 H244 . . . 119.3 ? C245 C244 H244 . . . 120.2 ? C244 C245 C246 . . . 119.5(6) ? C244 C245 H245 . . . 120.1 ? C246 C245 H245 . . . 120.4 ? C241 C246 C245 . . . 121.8(5) ? C241 C246 O25 . . . 119.7(6) ? C245 C246 O25 . . . 117.7(5) ? C246 O25 C26 . . . 114.5(5) ? O25 C26 C26' . . . 111.3(5) ? O25 C26 H26a . . . 110.5 ? O25 C26 H26b . . . 109.1 ? C26' C26 H26a . . . 110.7 ? C26' C26 H26b . . . 108.1 ? H26a C26 H26b . . . 106.9 ? N20 C21' C22' . . . 110.6(4) ? N20 C21' H21'a . . . 108.9 ? N20 C21' H21'b . . . 109.8 ? C22' C21' H21'a . . . 108.9 ? C22' C21' H21'b . . . 110.1 ? H21'a C21' H21'b . . . 108.5 ? C21' C22' N23' . . . 109.6(4) ? C21' C22' H22'a . . . 108.9 ? C21' C22' H22'b . . . 109.6 ? N23' C22' H22'a . . . 109.7 ? N23' C22' H22'b . . . 110.1 ? H22'a C22' H22'b . . . 108.8 ? Ni2 N23' C22' . . . 102.4(3) ? Ni2 N23' C24' . . . 119.0(3) ? Ni2 N23' H23' . . . 103.3 ? C22' N23' C24' . . . 115.1(4) ? C22' N23' H23' . . . 119.7 ? C24' N23' H23' . . . 97.8 ? N23' C24' C241' . . . 114.6(4) ? N23' C24' H24'a . . . 107.9 ? N23' C24' H24'b . . . 108.0 ? C241' C24' H24'a . . . 108.6 ? C241' C24' H24'b . . . 108.4 ? H24'a C24' H24'b . . . 109.3 ? C24' C241' C242' . . . 120.9(5) ? C24' C241' C246' . . . 121.1(5) ? C242' C241' C246' . . . 118.0(5) ? C241' C242' C243' . . . 122.1(6) ? C241' C242' H242' . . . 119.6 ? C243' C242' H242' . . . 118.3 ? C242' C243' C244' . . . 118.7(6) ? C242' C243' H243' . . . 120.3 ? C244' C243' H243' . . . 121.0 ? C243' C244' C245' . . . 121.6(5) ? C243' C244' H244' . . . 118.5 ? C245' C244' H244' . . . 119.9 ? C244' C245' C246' . . . 118.9(6) ? C244' C245' H245' . . . 120.5 ? C246' C245' H245' . . . 120.6 ? C241' C246' C245' . . . 120.7(5) ? C241' C246' O25' . . . 115.4(5) ? C245' C246' O25' . . . 123.8(5) ? C246' O25' C26' . . . 118.9(4) ? C26 C26' O25' . . . 108.7(5) ? C26 C26' H26'a . . . 111.9 ? C26 C26' H26'b . . . 108.1 ? O25' C26' H26'a . . . 111.3 ? O25' C26' H26'b . . . 108.6 ? H26'a C26' H26'b . . . 108.2 ? Ni3 O3 H3a . . . 116.7 ? Ni3 O3 H3b . . . 120.2 ? H3a O3 H3b . . . 106.6 ? Ni3 O30 H30a . . . 123.1 ? Ni3 O30 H30b . . . 121.8 ? H30a O30 H30b . . . 104.6 ? Ni3 O30' H30'a . . . 116.6 ? Ni3 O30' H30'b . . . 120.3 ? H30'a O30' H30'b . . . 95.3 ? Ni3 N30 C31 . . . 105.8(3) ? Ni3 N30 C31' . . . 109.9(3) ? Ni3 N30 H30 . . . 109.8 ? C31 N30 C31' . . . 113.4(4) ? C31 N30 H30 . . . 110.0 ? C31' N30 H30 . . . 107.8 ? N30 C31 C32 . . . 109.5(4) ? N30 C31 H31a . . . 109.9 ? N30 C31 H31b . . . 109.3 ? C32 C31 H31a . . . 109.4 ? C32 C31 H31b . . . 109.8 ? H31a C31 H31b . . . 108.9 ? C31 C32 N33 . . . 111.1(5) ? C31 C32 H32a . . . 109.3 ? C31 C32 H32b . . . 109.7 ? N33 C32 H32a . . . 108.9 ? N33 C32 H32b . . . 109.3 ? H32a C32 H32b . . . 108.5 ? Ni3 N33 C32 . . . 106.2(3) ? Ni3 N33 C34 . . . 114.6(3) ? Ni3 N33 H33 . . . 108.1 ? C32 N33 C34 . . . 113.2(4) ? C32 N33 H33 . . . 106.8 ? C34 N33 H33 . . . 107.6 ? N33 C34 C341 . . . 114.7(4) ? N33 C34 H34a . . . 108.4 ? N33 C34 H34b . . . 109.1 ? C341 C34 H34a . . . 108.1 ? C341 C34 H34b . . . 108.8 ? H34a C34 H34b . . . 107.6 ? C34 C341 C342 . . . 120.9(5) ? C34 C341 C346 . . . 121.9(5) ? C342 C341 C346 . . . 117.0(6) ? C341 C342 C343 . . . 121.7(6) ? C341 C342 H342 . . . 119.8 ? C343 C342 H342 . . . 118.6 ? C342 C343 C344 . . . 118.6(6) ? C342 C343 H343 . . . 121.2 ? C344 C343 H343 . . . 120.2 ? C343 C344 C345 . . . 121.7(6) ? C343 C344 H344 . . . 119.5 ? C345 C344 H344 . . . 118.9 ? C344 C345 C346 . . . 119.4(6) ? C344 C345 H345 . . . 120.8 ? C346 C345 H345 . . . 119.8 ? C341 C346 C345 . . . 121.6(5) ? C341 C346 O35 . . . 120.0(6) ? C345 C346 O35 . . . 118.1(5) ? C346 O35 C36 . . . 115.1(4) ? O35 C36 C36' . . . 109.9(5) ? O35 C36 H36a . . . 108.9 ? O35 C36 H36b . . . 109.2 ? C36' C36 H36a . . . 110.3 ? C36' C36 H36b . . . 110.1 ? H36a C36 H36b . . . 108.4 ? N30 C31' C32' . . . 110.5(4) ? N30 C31' H31'a . . . 108.9 ? N30 C31' H31'b . . . 109.2 ? C32' C31' H31'a . . . 109.8 ? C32' C31' H31'b . . . 109.6 ? H31'a C31' H31'b . . . 108.8 ? C31' C32' N33' . . . 109.0(4) ? C31' C32' H32'a . . . 109.9 ? C31' C32' H32'b . . . 109.6 ? N33' C32' H32'a . . . 109.5 ? N33' C32' H32'b . . . 109.7 ? H32'a C32' H32'b . . . 109.2 ? Ni3 N33' C32' . . . 102.9(3) ? Ni3 N33' C34' . . . 119.0(3) ? Ni3 N33' H33' . . . 106.8 ? C32' N33' C34' . . . 114.7(4) ? C32' N33' H33' . . . 105.0 ? C34' N33' H33' . . . 107.4 ? N33' C34' C341' . . . 115.0(4) ? N33' C34' H34'a . . . 107.6 ? N33' C34' H34'b . . . 107.4 ? C341' C34' H34'a . . . 109.5 ? C341' C34' H34'b . . . 109.1 ? H34'a C34' H34'b . . . 108.0 ? C34' C341' C342' . . . 120.7(5) ? C34' C341' C346' . . . 122.0(5) ? C342' C341' C346' . . . 117.3(5) ? C341' C342' C343' . . . 120.8(6) ? C341' C342' H342' . . . 119.7 ? C343' C342' H342' . . . 119.4 ? C342' C343' C344' . . . 120.1(6) ? C342' C343' H343' . . . 119.6 ? C344' C343' H343' . . . 120.3 ? C343' C344' C345' . . . 120.6(6) ? C343' C344' H344' . . . 119.2 ? C345' C344' H344' . . . 120.2 ? C344' C345' C346' . . . 119.9(6) ? C344' C345' H345' . . . 120.8 ? C346' C345' H345' . . . 119.3 ? C341' C346' C345' . . . 121.2(5) ? C341' C346' O35' . . . 114.8(5) ? C345' C346' O35' . . . 123.9(5) ? C346' O35' C36' . . . 118.9(4) ? C36 C36' O35' . . . 108.3(5) ? C36 C36' H36'a . . . 109.3 ? C36 C36' H36'b . . . 110.5 ? O35' C36' H36'a . . . 109.3 ? O35' C36' H36'b . . . 111.4 ? H36'a C36' H36'b . . . 107.9 ? Ni4 O4 H4a . . . 107.3 ? Ni4 O4 H4b . . . 107.8 ? H4a O4 H4b . . . 121.4 ? Ni4 O40 H40a . . . 133.9 ? Ni4 O40 H40b . . . 119.2 ? H40a O40 H40b . . . 106.4 ? Ni4 O40' H40'a . . . 112.0 ? Ni4 O40' H40'b . . . 120.4 ? H40'a O40' H40'b . . . 94.1 ? Ni4 N40 C41 . . . 105.7(3) ? Ni4 N40 C41' . . . 110.2(3) ? Ni4 N40 H40 . . . 110.1 ? C41 N40 C41' . . . 113.1(4) ? C41 N40 H40 . . . 110.3 ? C41' N40 H40 . . . 107.4 ? N40 C41 C42 . . . 109.8(4) ? N40 C41 H41a . . . 109.3 ? N40 C41 H41b . . . 110.1 ? C42 C41 H41a . . . 109.8 ? C42 C41 H41b . . . 109.8 ? H41a C41 H41b . . . 108.0 ? C41 C42 N43 . . . 109.6(5) ? C41 C42 H42a . . . 110.1 ? C41 C42 H42b . . . 109.5 ? N43 C42 H42a . . . 109.9 ? N43 C42 H42b . . . 109.2 ? H42a C42 H42b . . . 108.5 ? Ni4 N43 C42 . . . 107.3(3) ? Ni4 N43 C44 . . . 115.3(3) ? Ni4 N43 H43 . . . 108.0 ? C42 N43 C44 . . . 113.9(4) ? C42 N43 H43 . . . 104.1 ? C44 N43 H43 . . . 107.6 ? N43 C44 C441 . . . 116.2(4) ? N43 C44 H44a . . . 107.9 ? N43 C44 H44b . . . 107.3 ? C441 C44 H44a . . . 108.1 ? C441 C44 H44b . . . 108.0 ? H44a C44 H44b . . . 109.1 ? C44 C441 C442 . . . 121.3(5) ? C44 C441 C446 . . . 120.2(5) ? C442 C441 C446 . . . 118.5(5) ? C441 C442 C443 . . . 121.3(5) ? C441 C442 H442 . . . 119.1 ? C443 C442 H442 . . . 119.7 ? C442 C443 C444 . . . 118.7(5) ? C442 C443 H443 . . . 120.4 ? C444 C443 H443 . . . 120.9 ? C443 C444 C445 . . . 121.0(6) ? C443 C444 H444 . . . 119.3 ? C445 C444 H444 . . . 119.7 ? C444 C445 C446 . . . 118.8(6) ? C444 C445 H445 . . . 120.3 ? C446 C445 H445 . . . 120.8 ? C441 C446 C445 . . . 121.5(5) ? C441 C446 O45 . . . 115.4(5) ? C445 C446 O45 . . . 123.1(5) ? C446 O45 C46 . . . 117.8(5) ? O45 C46 C46' . . . 107.7(5) ? O45 C46 H46a . . . 110.4 ? O45 C46 H46b . . . 110.7 ? C46' C46 H46a . . . 110.3 ? C46' C46 H46b . . . 109.6 ? H46a C46 H46b . . . 108.2 ? N40 C41' C42' . . . 110.8(4) ? N40 C41' H41'a . . . 109.8 ? N40 C41' H41'b . . . 108.9 ? C42' C41' H41'a . . . 110.4 ? C42' C41' H41'b . . . 108.8 ? H41'a C41' H41'b . . . 108.0 ? C41' C42' N43' . . . 109.6(4) ? C41' C42' H42'a . . . 110.4 ? C41' C42' H42'b . . . 108.7 ? N43' C42' H42'a . . . 110.4 ? N43' C42' H42'b . . . 109.3 ? H42'a C42' H42'b . . . 108.4 ? Ni4 N43' C42' . . . 101.9(3) ? Ni4 N43' C44' . . . 117.6(3) ? Ni4 N43' H43' . . . 107.3 ? C42' N43' C44' . . . 113.9(4) ? C42' N43' H43' . . . 109.1 ? C44' N43' H43' . . . 106.7 ? N43' C44' C441' . . . 114.7(4) ? N43' C44' H44'a . . . 108.3 ? N43' C44' H44'b . . . 107.6 ? C441' C44' H44'a . . . 108.5 ? C441' C44' H44'b . . . 108.5 ? H44'a C44' H44'b . . . 109.2 ? C44' C441' C442' . . . 121.2(5) ? C44' C441' C446' . . . 121.0(5) ? C442' C441' C446' . . . 117.8(5) ? C441' C442' C443' . . . 121.9(6) ? C441' C442' H442' . . . 119.0 ? C443' C442' H442' . . . 119.1 ? C442' C443' C444' . . . 119.3(6) ? C442' C443' H443' . . . 119.8 ? C444' C443' H443' . . . 121.0 ? C443' C444' C445' . . . 120.0(6) ? C443' C444' H444' . . . 119.2 ? C445' C444' H444' . . . 120.9 ? C444' C445' C446' . . . 120.5(6) ? C444' C445' H445' . . . 120.4 ? C446' C445' H445' . . . 119.1 ? C441' C446' C445' . . . 120.5(6) ? C441' C446' O45' . . . 116.5(5) ? C445' C446' O45' . . . 122.9(6) ? C446' O45' C46' . . . 115.8(4) ? C46 C46' O45' . . . 108.7(5) ? C46 C46' H46'a . . . 111.7 ? C46 C46' H46'b . . . 109.9 ? O45' C46' H46'a . . . 109.6 ? O45' C46' H46'b . . . 109.1 ? H46'a C46' H46'b . . . 107.8 ? O11 S1 O12 . . . 109.7(3) ? O11 S1 O13 . . . 109.1(3) ? O11 S1 O14 . . . 112.2(2) ? O12 S1 O13 . . . 107.9(3) ? O12 S1 O14 . . . 107.5(3) ? O13 S1 O14 . . . 110.3(3) ? O11' S1 O12' . . . 87(2) ? O11' S1 O13' . . . 114.0(19) ? O11' S1 O14' . . . 97(2) ? O12' S1 O13' . . . 107(3) ? O12' S1 O14' . . . 121(3) ? O13' S1 O14' . . . 124(3) ? O21 S2 O22 . . . 108.0(3) ? O21 S2 O23 . . . 109.9(3) ? O21 S2 O24 . . . 108.3(3) ? O22 S2 O23 . . . 111.3(2) ? O22 S2 O24 . . . 108.9(3) ? O23 S2 O24 . . . 110.3(3) ? O21' S2 O22' . . . 106.7(13) ? O21' S2 O23' . . . 108.0(13) ? O21' S2 O24' . . . 113.6(13) ? O22' S2 O23' . . . 109.1(14) ? O22' S2 O24' . . . 115.4(12) ? O23' S2 O24' . . . 103.8(14) ? O31 S3 O32 . . . 108.8(2) ? O31 S3 O33 . . . 109.6(3) ? O31 S3 O34 . . . 111.3(2) ? O32 S3 O33 . . . 108.4(2) ? O32 S3 O34 . . . 108.9(2) ? O33 S3 O34 . . . 109.7(2) ? O41 S4 O42 . . . 108.9(2) ? O41 S4 O43 . . . 109.4(2) ? O41 S4 O44 . . . 108.5(2) ? O42 S4 O43 . . . 109.7(2) ? O42 S4 O44 . . . 110.3(2) ? O43 S4 O44 . . . 110.0(2) ? H01a O01 H01b . . . 129.4 ? H02a O02 H02b . . . 105.0 ? H03a O03 H03b . . . 98.6 ? H04a O04 H04b . . . 108.5 ? H05a O05 H05b . . . 102.0 ? H06a O06 H06b . . . 99.2 ? H07b O07 H07a . . . 100.3 ? H08a O08 H08b . . . 72.5 ? H09a O09 H09b . . . 100.8 ? H010a O010 H010b . . . 106.1 ? H013a O013 H013b . . . 113.2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 5280 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 45 _reflns_limit_l_min -13 _reflns_limit_l_max 13 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 20.796 _diffrn_reflns_av_sigmaI/netI .037 _diffrn_reflns_theta_min .98 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .092 _refine_ls_wR_factor_all .102 _refine_ls_goodness_of_fit_all 1.958 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_llvg27 _database_code_depnum_ccdc_archive 'CCDC 255535' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C20 H42.3 Cu1 N3 O13.67 S1' _chemical_formula_moiety ? _chemical_formula_weight 637.92 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 12.010(2) _cell_length_b 13.212(2) _cell_length_c 28.428(4) _cell_angle_alpha 79.278(2) _cell_angle_beta 80.110(2) _cell_angle_gamma 85.473(2) _cell_volume 4361.1(12) _cell_formula_units_Z 6 _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.3 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu .89 _exptl_crystal_description prism _exptl_crystal_size_max .4 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .7 _exptl_absorpt_correction_T_max .881 _diffrn_reflns_number 41956 _reflns_number_total 21102 _reflns_Friedel_coverage ? _reflns_number_gt 16903 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.5 _diffrn_reflns_theta_full 28.5 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .053 _refine_ls_wR_factor_ref .063 _refine_ls_goodness_of_fit_ref 1.3 _refine_ls_number_reflns 16903 _refine_ls_number_parameters 1393 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .047 _refine_diff_density_min -.837 _refine_diff_density_max 1.355 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 120 .002014 .002014 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 254 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Cu ? 0 6 .263001 1.266 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 18 .004028 .002991 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' O ? 0 82 .007996 .005981 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' S ? 0 6 .109985 .124023 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .63090(3) .51826(3) .085970(10) .0206(2) Uani ? ? 1.00000 ? ? Cu2 -.04252(3) .20408(3) .752750(10) .0199(2) Uani ? ? 1.00000 ? ? Cu3 .30790(3) .85461(3) .415080(10) .0193(2) Uani ? ? 1.00000 ? ? O1 .6860(2) .4979(2) .01844(8) .0270(15) Uani ? ? 1.00000 ? ? N10 .5667(2) .54531(19) .15237(9) .0222(15) Uani ? ? 1.00000 ? ? C11 .5237(3) .4501(2) .18432(11) .026(2) Uani ? ? 1.00000 ? ? C12 .4806(3) .3848(3) .15293(12) .027(2) Uani ? ? 1.00000 ? ? N13 .5649(2) .37803(19) .10838(9) .0228(16) Uani ? ? 1.00000 ? ? C14 .6484(3) .2877(2) .11377(12) .026(2) Uani ? ? 1.00000 ? ? C141 .7135(3) .2813(2) .15521(10) .0229(18) Uani ? ? 1.00000 ? ? C142 .6821(3) .2134(2) .19863(11) .026(2) Uani ? ? 1.00000 ? ? C143 .7420(3) .2039(2) .23711(11) .029(2) Uani ? ? 1.00000 ? ? C144 .8360(3) .2614(2) .23230(12) .030(2) Uani ? ? 1.00000 ? ? C145 .8692(3) .3296(2) .18946(11) .027(2) Uani ? ? 1.00000 ? ? C146 .8078(2) .3390(2) .15150(10) .0225(18) Uani ? ? 1.00000 ? ? O15 .83825(18) .40999(16) .10921(8) .0287(14) Uani ? ? 1.00000 ? ? C16 .9461(3) .3881(2) .08000(12) .027(2) Uani ? ? 1.00000 ? ? C11' .6512(3) .5990(3) .16970(11) .027(2) Uani ? ? 1.00000 ? ? C12' .6991(3) .6804(3) .12772(12) .028(2) Uani ? ? 1.00000 ? ? N13' .7380(2) .63023(19) .08492(9) .0212(15) Uani ? ? 1.00000 ? ? C14' .7770(3) .7044(2) .03984(11) .0237(19) Uani ? ? 1.00000 ? ? C141' .8945(2) .7383(2) .03844(10) .0214(17) Uani ? ? 1.00000 ? ? C142' .9194(3) .8403(2) .03583(11) .026(2) Uani ? ? 1.00000 ? ? C143' 1.0297(3) .8671(2) .03429(11) .028(2) Uani ? ? 1.00000 ? ? C144' 1.1169(3) .7918(3) .03467(11) .027(2) Uani ? ? 1.00000 ? ? C145' 1.0940(3) .6887(2) .03781(11) .0248(19) Uani ? ? 1.00000 ? ? C146' .9837(2) .6632(2) .04005(10) .0213(17) Uani ? ? 1.00000 ? ? O15' .95237(16) .56359(15) .04277(7) .0222(13) Uani ? ? 1.00000 ? ? C16' 1.0167(3) .4816(2) .06794(12) .025(2) Uani ? ? 1.00000 ? ? O2 .01096(18) .18307(19) .68502(8) .0235(14) Uani ? ? 1.00000 ? ? N20 -.1031(2) .23193(19) .81941(9) .0221(15) Uani ? ? 1.00000 ? ? C21 -.1414(3) .1360(3) .85225(11) .027(2) Uani ? ? 1.00000 ? ? C22 -.1856(3) .0693(3) .82206(12) .028(2) Uani ? ? 1.00000 ? ? N23 -.1037(2) .0629(2) .77685(9) .0237(16) Uani ? ? 1.00000 ? ? C24 -.0190(3) -.0263(2) .78149(11) .027(2) Uani ? ? 1.00000 ? ? C241 .0484(3) -.0318(2) .82222(10) .0226(18) Uani ? ? 1.00000 ? ? C242 .0199(3) -.1001(2) .86562(11) .027(2) Uani ? ? 1.00000 ? ? C243 .0807(3) -.1083(2) .90336(11) .028(2) Uani ? ? 1.00000 ? ? C244 .1733(3) -.0488(2) .89824(11) .029(2) Uani ? ? 1.00000 ? ? C245 .2042(3) .0199(2) .85528(12) .028(2) Uani ? ? 1.00000 ? ? C246 .1414(3) .0279(2) .81779(10) .0229(18) Uani ? ? 1.00000 ? ? O25 .16921(18) .09960(16) .77546(8) .0291(14) Uani ? ? 1.00000 ? ? C26 .2745(3) .0775(2) .74499(12) .027(2) Uani ? ? 1.00000 ? ? C21' -.0186(3) .2885(3) .83536(11) .028(2) Uani ? ? 1.00000 ? ? C22' .0256(3) .3697(3) .79240(12) .029(2) Uani ? ? 1.00000 ? ? N23' .0638(2) .31807(19) .74990(9) .0215(15) Uani ? ? 1.00000 ? ? C24' .1010(3) .3918(2) .70446(11) .0230(18) Uani ? ? 1.00000 ? ? C241' .2184(2) .4267(2) .70318(10) .0214(17) Uani ? ? 1.00000 ? ? C242' .2418(3) .5283(2) .70216(11) .0247(19) Uani ? ? 1.00000 ? ? C243' .3525(3) .5556(2) .70115(11) .027(2) Uani ? ? 1.00000 ? ? C244' .4393(3) .4816(3) .70077(11) .027(2) Uani ? ? 1.00000 ? ? C245' .4178(3) .3785(2) .70220(10) .0244(18) Uani ? ? 1.00000 ? ? C246' .3084(2) .3521(2) .70419(10) .0208(17) Uani ? ? 1.00000 ? ? O25' .27840(17) .25219(15) .70640(7) .0219(13) Uani ? ? 1.00000 ? ? C26' .3445(3) .1708(2) .73143(12) .025(2) Uani ? ? 1.00000 ? ? O3 .36734(18) .83241(18) .34795(7) .0233(14) Uani ? ? 1.00000 ? ? N30 .2369(2) .88441(19) .48013(9) .0206(15) Uani ? ? 1.00000 ? ? C31 .1923(3) .7895(2) .51227(11) .0250(19) Uani ? ? 1.00000 ? ? C32 .1536(3) .7225(3) .48033(12) .027(2) Uani ? ? 1.00000 ? ? N33 .2419(2) .71497(19) .43716(9) .0215(15) Uani ? ? 1.00000 ? ? C34 .3268(3) .6257(2) .44442(11) .0241(19) Uani ? ? 1.00000 ? ? C341 .3887(2) .6233(2) .48667(10) .0210(17) Uani ? ? 1.00000 ? ? C342 .3537(3) .5585(2) .53071(11) .0248(19) Uani ? ? 1.00000 ? ? C343 .4098(3) .5533(2) .56996(11) .028(2) Uani ? ? 1.00000 ? ? C344 .5032(3) .6110(2) .56573(11) .028(2) Uani ? ? 1.00000 ? ? C345 .5403(3) .6754(2) .52231(11) .025(2) Uani ? ? 1.00000 ? ? C346 .4820(2) .6816(2) .48330(10) .0201(17) Uani ? ? 1.00000 ? ? O35 .51572(17) .74955(16) .44026(8) .0274(14) Uani ? ? 1.00000 ? ? C36 .6247(3) .7254(2) .41315(12) .027(2) Uani ? ? 1.00000 ? ? C31' .3179(3) .9391(2) .49906(11) .025(2) Uani ? ? 1.00000 ? ? C32' .3704(3) 1.0185(2) .45728(11) .026(2) Uani ? ? 1.00000 ? ? N33' .4149(2) .96615(18) .41542(8) .0201(15) Uani ? ? 1.00000 ? ? C34' .4576(3) 1.0394(2) .37048(11) .0234(18) Uani ? ? 1.00000 ? ? C341' .5742(2) 1.0736(2) .37124(10) .0207(17) Uani ? ? 1.00000 ? ? C342' .5968(3) 1.1754(2) .37097(11) .0249(19) Uani ? ? 1.00000 ? ? C343' .7067(3) 1.2026(2) .37152(11) .028(2) Uani ? ? 1.00000 ? ? C344' .7947(3) 1.1282(3) .37179(11) .027(2) Uani ? ? 1.00000 ? ? C345' .7738(3) 1.0250(2) .37263(11) .0241(18) Uani ? ? 1.00000 ? ? C346' .6639(2) .9991(2) .37323(10) .0211(17) Uani ? ? 1.00000 ? ? O35' .63455(17) .89947(15) .37418(7) .0219(13) Uani ? ? 1.00000 ? ? C36' .6965(3) .8178(2) .40106(12) .025(2) Uani ? ? 1.00000 ? ? S1 .47785(7) .69240(6) .00974(3) .0282(5) Uani ? ? 1.00000 ? ? O11 .4936(2) .6368(2) .05838(8) .0409(17) Uani ? ? 1.00000 ? ? O12 .4955(3) .8031(2) .00671(11) .050(2) Uani ? ? 1.00000 ? ? O13 .56196(19) .65079(19) -.02767(8) .0338(16) Uani ? ? 1.00000 ? ? O14 .36419(19) .68035(18) .00060(9) .0359(17) Uani ? ? 1.00000 ? ? S2 -.21016(6) .36538(5) .68136(3) .0223(4) Uani ? ? 1.00000 ? ? O21 -.1872(2) .3104(2) .72885(8) .0410(17) Uani ? ? 1.00000 ? ? O22 -.2023(2) .47623(18) .67862(9) .0415(18) Uani ? ? 1.00000 ? ? O23 -.12523(18) .32931(17) .64249(7) .0273(14) Uani ? ? 1.00000 ? ? O24 -.32311(19) .3435(2) .67441(11) .045(2) Uani ? ? 1.00000 ? ? S3 .15217(6) 1.01815(6) .33614(3) .0237(5) Uani ? ? 1.00000 ? ? O31 .1714(2) .9712(2) .38569(8) .0399(17) Uani ? ? 1.00000 ? ? O32 .1665(2) 1.12904(19) .32868(10) .046(2) Uani ? ? 1.00000 ? ? O33 .23575(18) .97139(17) .30005(7) .0281(14) Uani ? ? 1.00000 ? ? O34 .03757(19) .99918(18) .33036(9) .0342(16) Uani ? ? 1.00000 ? ? O01 .1643(3) .1980(2) .50658(9) .050(2) Uani ? ? 1.00000 ? ? O02 .3308(3) .3478(2) .35517(12) .058(2) Uani ? ? 1.00000 ? ? O03 1.1831(3) .4879(3) .15247(12) .077(3) Uani ? ? 1.00000 ? ? O04 1.0199(2) .3029(2) .30075(11) .051(2) Uani ? ? 1.00000 ? ? O05 .9763(3) -.0353(3) .46151(13) .070(3) Uani ? ? 1.00000 ? ? O06 .6757(3) 1.0330(2) .00645(12) .058(2) Uani ? ? 1.00000 ? ? O07 1.1709(3) .2191(2) .40876(10) .070(3) Uani ? ? 1.00000 ? ? O08 .5073(3) .9006(3) .17795(12) .077(3) Uani ? ? 1.00000 ? ? O09 1.0263(3) .5090(2) .42736(10) .059(2) Uani ? ? 1.00000 ? ? O010 .8665(3) .5910(3) .49287(12) .058(2) Uani ? ? 1.00000 ? ? O011 .5431(3) .9104(2) .07620(11) .060(3) Uani ? ? 1.00000 ? ? O012 .6279(3) .9310(3) -.06972(12) .070(3) Uani ? ? 1.00000 ? ? O013 .4143(4) 1.0593(4) .22992(14) .101(4) Uani ? ? 1.00000 ? ? O014 1.2057(3) .4198(2) .24689(10) .056(2) Uani ? ? 1.00000 ? ? O015 .9720(3) .3392(2) .39542(12) .064(3) Uani ? ? 1.00000 ? ? O016 .7680(3) .6660(3) -.09922(13) .075(3) Uani ? ? 1.00000 ? ? O017 .4061(3) .7192(3) .20766(14) .097(3) Uani ? ? 1.00000 ? ? O018 .3193(3) .6487(3) .13644(13) .088(3) Uani ? ? 1.00000 ? ? O019 .3498(4) .2493(4) .27350(14) .102(4) Uani ? ? 1.00000 ? ? O020 .3125(6) 1.1631(3) .15132(17) .136(6) Uani ? ? 1.00000 ? ? H1a .670(4) .440(4) .0144(18) .069(16) Uiso ? ? 1.00000 ? ? H1b .651(4) .537(4) .0029(16) .047(13) Uiso ? ? 1.00000 ? ? H10 .511(3) .587(3) .1474(12) .022(8) Uiso ? ? 1.00000 ? ? H11a .464(3) .468(3) .2097(13) .030(9) Uiso ? ? 1.00000 ? ? H11b .582(3) .417(3) .1992(12) .024(8) Uiso ? ? 1.00000 ? ? H12a .420(3) .416(3) .1430(12) .026(9) Uiso ? ? 1.00000 ? ? H12b .463(3) .312(3) .1701(13) .028(9) Uiso ? ? 1.00000 ? ? H13 .526(3) .366(3) .0876(13) .025(9) Uiso ? ? 1.00000 ? ? H14a .697(3) .291(3) .0840(14) .037(10) Uiso ? ? 1.00000 ? ? H14b .610(3) .231(3) .1180(14) .039(10) Uiso ? ? 1.00000 ? ? H142 .621(3) .178(3) .2008(13) .033(10) Uiso ? ? 1.00000 ? ? H143 .712(3) .156(3) .2662(13) .031(9) Uiso ? ? 1.00000 ? ? H144 .882(3) .255(3) .2581(13) .027(9) Uiso ? ? 1.00000 ? ? H145 .933(3) .366(3) .1863(12) .024(9) Uiso ? ? 1.00000 ? ? H16a .926(3) .370(3) .0510(13) .032(9) Uiso ? ? 1.00000 ? ? H16b .987(3) .329(3) .0977(12) .022(8) Uiso ? ? 1.00000 ? ? H11'a .709(3) .553(3) .1776(12) .023(8) Uiso ? ? 1.00000 ? ? H11'b .617(3) .626(3) .1964(15) .043(11) Uiso ? ? 1.00000 ? ? H12'a .759(3) .719(3) .1351(14) .038(10) Uiso ? ? 1.00000 ? ? H12'b .645(3) .730(3) .1200(13) .029(9) Uiso ? ? 1.00000 ? ? H13' .799(3) .589(3) .0896(12) .023(8) Uiso ? ? 1.00000 ? ? H14'a .725(3) .761(3) .0380(12) .022(8) Uiso ? ? 1.00000 ? ? H14'b .770(3) .672(3) .0158(13) .026(9) Uiso ? ? 1.00000 ? ? H142' .867(3) .890(3) .0344(12) .027(9) Uiso ? ? 1.00000 ? ? H143' 1.044(3) .930(3) .0339(12) .022(8) Uiso ? ? 1.00000 ? ? H144' 1.192(3) .811(3) .0329(14) .041(11) Uiso ? ? 1.00000 ? ? H145' 1.151(3) .638(3) .0385(13) .030(9) Uiso ? ? 1.00000 ? ? H16'a 1.087(3) .471(2) .0481(11) .019(8) Uiso ? ? 1.00000 ? ? H16'b 1.033(3) .500(2) .0966(12) .023(8) Uiso ? ? 1.00000 ? ? H2a -.005(4) .128(4) .6806(16) .047(13) Uiso ? ? 1.00000 ? ? H2b -.024(4) .225(3) .6713(15) .043(13) Uiso ? ? 1.00000 ? ? H20 -.159(3) .273(3) .8145(13) .027(9) Uiso ? ? 1.00000 ? ? H21a -.082(3) .106(3) .8649(12) .022(8) Uiso ? ? 1.00000 ? ? H21b -.204(3) .150(3) .8792(14) .040(10) Uiso ? ? 1.00000 ? ? H22a -.201(3) .001(3) .8379(14) .035(10) Uiso ? ? 1.00000 ? ? H22b -.250(3) .103(3) .8118(13) .033(10) Uiso ? ? 1.00000 ? ? H23 -.140(3) .054(3) .7572(13) .025(9) Uiso ? ? 1.00000 ? ? H24a -.059(3) -.090(3) .7867(13) .035(10) Uiso ? ? 1.00000 ? ? H24b .030(3) -.025(3) .7512(14) .033(10) Uiso ? ? 1.00000 ? ? H242 -.046(3) -.143(3) .8694(14) .037(10) Uiso ? ? 1.00000 ? ? H243 .060(3) -.150(3) .9319(14) .034(10) Uiso ? ? 1.00000 ? ? H244 .221(3) -.060(3) .9219(14) .041(11) Uiso ? ? 1.00000 ? ? H245 .267(3) .060(3) .8498(14) .040(10) Uiso ? ? 1.00000 ? ? H26a .254(3) .059(3) .7156(13) .032(9) Uiso ? ? 1.00000 ? ? H26b .320(3) .021(3) .7612(12) .024(8) Uiso ? ? 1.00000 ? ? H21'a -.055(3) .319(3) .8636(13) .029(9) Uiso ? ? 1.00000 ? ? H21'b .042(3) .241(3) .8423(12) .022(8) Uiso ? ? 1.00000 ? ? H22'a -.039(3) .423(3) .7842(12) .026(9) Uiso ? ? 1.00000 ? ? H22'b .089(3) .409(3) .7979(14) .046(11) Uiso ? ? 1.00000 ? ? H23' .127(3) .267(3) .7561(13) .033(9) Uiso ? ? 1.00000 ? ? H24'a .098(3) .357(2) .6793(12) .018(8) Uiso ? ? 1.00000 ? ? H24'b .048(3) .451(3) .7021(12) .027(9) Uiso ? ? 1.00000 ? ? H242' .183(3) .577(3) .7025(13) .035(10) Uiso ? ? 1.00000 ? ? H243' .365(3) .623(3) .6983(13) .036(10) Uiso ? ? 1.00000 ? ? H244' .507(3) .500(3) .6966(12) .023(8) Uiso ? ? 1.00000 ? ? H245' .471(3) .327(2) .7013(11) .018(8) Uiso ? ? 1.00000 ? ? H26'a .415(3) .157(2) .7086(12) .023(8) Uiso ? ? 1.00000 ? ? H26'b .366(3) .192(3) .7559(13) .029(9) Uiso ? ? 1.00000 ? ? H3a .355(4) .773(4) .3422(16) .056(13) Uiso ? ? 1.00000 ? ? H3b .328(3) .877(3) .3321(13) .029(10) Uiso ? ? 1.00000 ? ? H30 .180(3) .925(3) .4738(12) .023(8) Uiso ? ? 1.00000 ? ? H31a .131(3) .809(3) .5344(13) .029(9) Uiso ? ? 1.00000 ? ? H31b .250(3) .757(2) .5293(11) .018(8) Uiso ? ? 1.00000 ? ? H32a .089(3) .752(2) .4675(12) .022(8) Uiso ? ? 1.00000 ? ? H32b .134(3) .655(3) .4996(13) .034(10) Uiso ? ? 1.00000 ? ? H33 .208(3) .699(2) .4122(12) .021(8) Uiso ? ? 1.00000 ? ? H34a .378(3) .628(3) .4151(13) .028(9) Uiso ? ? 1.00000 ? ? H34b .291(3) .564(3) .4484(12) .024(8) Uiso ? ? 1.00000 ? ? H342 .288(3) .517(3) .5344(12) .026(9) Uiso ? ? 1.00000 ? ? H343 .386(3) .515(3) .5983(15) .045(11) Uiso ? ? 1.00000 ? ? H344 .545(3) .603(3) .5895(14) .033(10) Uiso ? ? 1.00000 ? ? H345 .606(3) .717(3) .5187(13) .033(10) Uiso ? ? 1.00000 ? ? H36a .605(3) .706(3) .3842(14) .039(10) Uiso ? ? 1.00000 ? ? H36b .666(3) .670(3) .4309(12) .025(8) Uiso ? ? 1.00000 ? ? H31'a .375(3) .890(2) .5099(11) .019(8) Uiso ? ? 1.00000 ? ? H31'b .279(3) .970(2) .5247(11) .014(7) Uiso ? ? 1.00000 ? ? H32'a .425(3) 1.056(3) .4659(13) .035(10) Uiso ? ? 1.00000 ? ? H32'b .314(3) 1.071(3) .4480(12) .021(8) Uiso ? ? 1.00000 ? ? H33' .474(3) .921(2) .4218(11) .020(8) Uiso ? ? 1.00000 ? ? H34'a .406(3) 1.094(2) .3688(11) .013(7) Uiso ? ? 1.00000 ? ? H34'b .459(3) 1.007(3) .3436(13) .029(9) Uiso ? ? 1.00000 ? ? H342' .542(3) 1.223(2) .3715(11) .018(8) Uiso ? ? 1.00000 ? ? H343' .724(3) 1.270(3) .3720(13) .031(9) Uiso ? ? 1.00000 ? ? H344' .874(3) 1.146(3) .3711(12) .028(9) Uiso ? ? 1.00000 ? ? H345' .835(3) .976(2) .3711(11) .020(8) Uiso ? ? 1.00000 ? ? H36'a .770(3) .801(3) .3807(12) .027(9) Uiso ? ? 1.00000 ? ? H36'b .712(3) .838(2) .4294(12) .019(8) Uiso ? ? 1.00000 ? ? H01a .16567 .20009 .47527 .07600 Uiso ? ? 1.00000 ? ? H01b .15667 .26175 .51246 .07600 Uiso ? ? 1.00000 ? ? H02a .29080 .41201 .34598 .09100 Uiso ? ? 1.00000 ? ? H02b .34735 .32801 .32064 .09100 Uiso ? ? 1.00000 ? ? H03a 1.16451 .41341 .15734 .11400 Uiso ? ? 1.00000 ? ? H03b 1.21055 .50366 .17847 .11400 Uiso ? ? 1.00000 ? ? H04a 1.05582 .34986 .29048 .07400 Uiso ? ? 1.00000 ? ? H04b 1.05875 .24347 .30319 .07400 Uiso ? ? 1.00000 ? ? H05a 1.02377 -.02717 .43233 .10200 Uiso ? ? 1.00000 ? ? H05b .93564 -.07006 .45634 .10200 Uiso ? ? 1.00000 ? ? H06a .70727 .97914 -.01771 .09100 Uiso ? ? 1.00000 ? ? H06b .62053 1.09505 .00511 .09100 Uiso ? ? 1.00000 ? ? H07a 1.10508 .22532 .42308 .10400 Uiso ? ? 1.00000 ? ? H07b 1.17382 .17643 .38703 .10400 Uiso ? ? 1.00000 ? ? H08a .47879 .82973 .18485 .12300 Uiso ? ? 1.00000 ? ? H08b .48046 .95037 .19674 .12300 Uiso ? ? 1.00000 ? ? H09a 1.05241 .55122 .40003 .08600 Uiso ? ? 1.00000 ? ? H09b .96853 .56046 .44196 .08600 Uiso ? ? 1.00000 ? ? H011a .45077 .89813 .08620 .09500 Uiso ? ? 1.00000 ? ? H011b .59820 .95717 .04804 .09500 Uiso ? ? 1.00000 ? ? H012a .58001 .88129 -.04341 .10500 Uiso ? ? 1.00000 ? ? H012b .69313 .89600 -.05174 .10500 Uiso ? ? 1.00000 ? ? H013a .46620 1.08250 .20197 .15000 Uiso ? ? 1.00000 ? ? H013b .39157 .99795 .22411 .15000 Uiso ? ? 1.00000 ? ? H014a 1.18666 .46449 .26724 .08100 Uiso ? ? 1.00000 ? ? H014b 1.24906 .35900 .25350 .08100 Uiso ? ? 1.00000 ? ? H015a 1.00000 .42000 .39993 .09700 Uiso ? ? 1.00000 ? ? H015b .98333 .34110 .35606 .09700 Uiso ? ? 1.00000 ? ? H016a .73773 .74092 -.11379 .11800 Uiso ? ? 1.00000 ? ? H016b .81935 .64487 -.13828 .11800 Uiso ? ? 1.00000 ? ? H017a .35447 .68588 .19022 .14700 Uiso ? ? 1.00000 ? ? H017b .34992 .73931 .23123 .14700 Uiso ? ? 1.00000 ? ? H019a .40631 .30221 .26664 .16100 Uiso ? ? 1.00000 ? ? H019b .38044 .20122 .25470 .16100 Uiso ? ? 1.00000 ? ? H020a .34664 1.14738 .18917 .21400 Uiso ? ? 1.00000 ? ? H020b .23526 1.18822 .15261 .21400 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 .01918(17) .02287(18) .02004(17) -.00176(13) -.00412(13) -.00315(13) Cu2 .01905(17) .02333(18) .01767(17) -.00086(13) -.00374(13) -.00366(13) Cu3 .01925(17) .02141(17) .01721(16) -.00361(13) -.00315(13) -.00222(13) O1 .0284(12) .0296(12) .0241(11) -.0030(10) -.0067(9) -.0045(9) N10 .0175(11) .0239(12) .0242(12) .0011(10) -.0029(10) -.0032(10) C11 .0229(15) .0282(15) .0232(14) -.0014(12) -.0008(12) -.0013(12) C12 .0208(15) .0317(17) .0279(16) -.0044(12) -.0024(12) -.0006(13) N13 .0212(12) .0260(13) .0230(12) -.0011(10) -.0088(10) -.0039(10) C14 .0297(16) .0227(15) .0289(16) -.0006(12) -.0108(13) -.0052(12) C141 .0257(14) .0206(14) .0233(14) .0030(11) -.0069(11) -.0056(11) C142 .0280(16) .0210(14) .0288(16) -.0004(12) -.0048(13) -.0017(12) C143 .0389(18) .0239(15) .0225(15) .0059(13) -.0043(13) -.0012(12) C144 .0393(18) .0281(16) .0256(15) .0098(13) -.0132(14) -.0085(12) C145 .0270(16) .0248(15) .0307(16) .0025(12) -.0106(13) -.0078(12) C146 .0234(14) .0194(13) .0235(14) .0019(11) -.0042(11) -.0019(11) O15 .0235(11) .0280(11) .0296(11) .0016(9) -.0015(9) .0041(9) C16 .0284(16) .0239(15) .0264(15) .0009(12) .0007(12) -.0055(12) C11' .0274(16) .0315(16) .0227(15) -.0037(13) -.0023(12) -.0093(12) C12' .0305(16) .0264(15) .0269(15) -.0029(13) -.0008(13) -.0098(12) N13' .0180(11) .0225(12) .0223(12) .0015(9) -.0031(9) -.0026(9) C14' .0218(14) .0243(15) .0245(15) .0000(11) -.0051(12) -.0021(12) C141' .0220(14) .0245(14) .0177(13) -.0025(11) -.0025(11) -.0035(11) C142' .0295(16) .0245(15) .0214(14) -.0005(12) -.0025(12) -.0015(11) C143' .0363(17) .0234(15) .0242(15) -.0084(13) -.0040(13) -.0021(12) C144' .0260(15) .0341(17) .0208(14) -.0110(13) -.0007(12) -.0033(12) C145' .0225(14) .0293(16) .0226(14) -.0024(12) -.0012(11) -.0060(12) C146' .0240(14) .0223(14) .0178(13) -.0032(11) -.0015(11) -.0051(11) O15' .0211(10) .0201(10) .0262(10) -.0012(8) -.0046(8) -.0053(8) C16' .0213(14) .0245(15) .0283(15) .0024(11) -.0033(12) -.0047(12) O2 .0227(11) .0263(12) .0227(11) -.0004(9) -.0056(9) -.0063(9) N20 .0201(12) .0249(13) .0204(12) .0025(10) -.0029(9) -.0035(10) C21 .0254(15) .0339(17) .0192(14) -.0007(13) -.0011(12) -.0019(12) C22 .0230(15) .0346(17) .0257(15) -.0058(13) -.0020(12) -.0005(13) N23 .0241(13) .0302(13) .0191(12) -.0026(10) -.0100(10) -.0038(10) C24 .0324(16) .0244(15) .0256(15) -.0008(12) -.0106(13) -.0054(12) C241 .0269(15) .0211(14) .0206(13) .0009(11) -.0067(11) -.0042(11) C242 .0307(16) .0216(14) .0272(15) -.0018(12) -.0032(13) -.0019(12) C243 .0393(18) .0232(15) .0205(14) .0041(13) -.0047(13) .0000(12) C244 .0382(18) .0287(16) .0241(15) .0081(13) -.0133(13) -.0078(12) C245 .0264(15) .0249(15) .0347(17) -.0001(12) -.0104(13) -.0055(13) C246 .0257(14) .0194(13) .0231(14) .0013(11) -.0050(11) -.0024(11) O25 .0250(11) .0272(11) .0290(11) .0013(9) -.0001(9) .0061(9) C26 .0280(16) .0224(15) .0275(15) .0011(12) .0001(12) -.0048(12) C21' .0299(16) .0331(17) .0228(15) -.0029(13) -.0042(13) -.0093(13) C22' .0318(17) .0292(16) .0271(16) -.0029(13) -.0033(13) -.0116(13) N23' .0189(11) .0240(12) .0216(12) -.0005(9) -.0031(9) -.0047(10) C24' .0214(14) .0235(14) .0231(14) -.0006(11) -.0046(11) -.0011(11) C241' .0226(14) .0235(14) .0171(13) -.0026(11) -.0012(11) -.0019(11) C242' .0273(15) .0230(14) .0225(14) .0006(12) -.0033(12) -.0022(11) C243' .0352(17) .0220(15) .0236(15) -.0083(12) -.0032(12) -.0014(12) C244' .0261(16) .0320(16) .0219(14) -.0100(13) -.0026(12) -.0016(12) C245' .0220(14) .0288(15) .0206(14) -.0007(12) -.0007(11) -.0030(12) C246' .0250(14) .0210(13) .0161(12) -.0027(11) -.0016(11) -.0033(10) O25' .0234(10) .0192(10) .0235(10) -.0006(8) -.0046(8) -.0039(8) C26' .0234(15) .0236(15) .0274(15) .0014(11) -.0030(12) -.0034(12) O3 .0236(11) .0258(11) .0206(10) -.0021(9) -.0031(8) -.0046(9) N30 .0170(11) .0215(12) .0230(12) -.0008(9) -.0050(9) -.0011(9) C31 .0253(15) .0269(15) .0208(14) -.0054(12) .0011(12) -.0018(12) C32 .0209(14) .0306(16) .0276(15) -.0071(12) -.0020(12) -.0026(13) N33 .0219(12) .0244(12) .0189(11) -.0040(9) -.0070(10) -.0013(9) C34 .0286(15) .0209(14) .0253(15) -.0025(12) -.0100(12) -.0046(11) C341 .0243(14) .0189(13) .0207(13) -.0002(10) -.0072(11) -.0029(10) C342 .0259(15) .0206(14) .0261(15) -.0027(11) -.0034(12) .0001(11) C343 .0373(17) .0236(15) .0209(14) .0026(13) -.0037(13) -.0012(12) C344 .0354(17) .0274(15) .0238(15) .0050(13) -.0126(13) -.0087(12) C345 .0254(15) .0228(14) .0299(16) .0004(11) -.0097(12) -.0060(12) C346 .0219(13) .0176(13) .0205(13) .0003(10) -.0044(11) -.0018(10) O35 .0226(10) .0269(11) .0278(11) -.0022(8) -.0022(9) .0061(9) C36 .0306(16) .0230(15) .0260(15) -.0022(12) .0021(13) -.0056(12) C31' .0273(15) .0280(15) .0213(14) -.0050(12) -.0042(12) -.0067(12) C32' .0304(16) .0244(15) .0252(15) -.0050(12) -.0027(12) -.0081(12) N33' .0182(11) .0222(12) .0196(11) -.0024(9) -.0036(9) -.0018(9) C34' .0248(15) .0244(15) .0199(14) -.0037(12) -.0049(11) .0013(11) C341' .0233(14) .0228(14) .0151(12) -.0055(11) -.0007(10) -.0011(10) C342' .0312(16) .0213(14) .0209(14) -.0034(12) -.0019(12) -.0017(11) C343' .0379(17) .0235(15) .0227(14) -.0120(13) -.0039(13) -.0024(12) C344' .0268(16) .0328(16) .0226(14) -.0116(13) -.0007(12) -.0030(12) C345' .0205(14) .0293(15) .0219(14) -.0050(12) .0000(11) -.0041(12) C346' .0247(14) .0219(14) .0165(12) -.0056(11) -.0004(11) -.0036(10) O35' .0251(10) .0184(9) .0232(10) -.0032(8) -.0047(8) -.0043(8) C36' .0227(14) .0229(14) .0290(16) .0001(11) -.0014(12) -.0035(12) S1 .0290(4) .0287(4) .0287(4) -.0034(3) -.0144(3) .0005(3) O11 .0331(13) .0587(16) .0255(12) .0162(12) -.0087(10) .0027(11) O12 .0641(19) .0355(14) .0556(17) -.0149(13) -.0197(15) -.0068(12) O13 .0313(12) .0421(13) .0261(11) -.0046(10) -.0087(10) .0039(10) O14 .0285(12) .0360(13) .0498(15) .0030(10) -.0190(11) -.0141(11) S2 .0202(3) .0218(3) .0255(3) -.0016(3) -.0092(3) -.0005(3) O21 .0344(13) .0562(16) .0221(11) .0213(12) .0002(10) .0053(11) O22 .0601(17) .0258(12) .0407(14) -.0102(11) -.0079(12) -.0077(10) O23 .0296(11) .0333(12) .0191(10) -.0044(9) -.0063(9) -.0014(9) O24 .0200(11) .0425(14) .082(2) .0036(10) -.0178(12) -.0310(14) S3 .0270(4) .0220(3) .0247(3) .0002(3) -.0110(3) -.0047(3) O31 .0386(13) .0580(16) .0225(11) .0192(12) -.0114(10) -.0090(11) O32 .0569(17) .0266(13) .0568(17) -.0066(11) -.0104(14) -.0106(12) O33 .0284(11) .0341(12) .0214(10) -.0010(9) -.0057(9) -.0026(9) O34 .0262(11) .0365(13) .0453(14) .0031(9) -.0124(10) -.0171(11) O01 .0583(18) .0596(18) .0327(14) .0068(14) -.0157(13) -.0096(13) O02 .066(2) .0462(16) .073(2) -.0020(14) -.0449(17) -.0092(15) O03 .063(2) .124(3) .0476(18) .039(2) -.0232(16) -.029(2) O04 .0485(16) .0451(16) .066(2) .0004(13) -.0250(15) -.0101(14) O05 .058(2) .069(2) .071(2) -.0035(17) .0170(17) -.0010(18) O06 .0446(16) .0478(17) .084(2) -.0060(13) -.0261(16) -.0037(16) O07 .131(3) .0494(18) .0342(15) .0015(19) -.0218(18) -.0149(13) O08 .0481(19) .122(3) .052(2) .003(2) -.0089(15) .007(2) O09 .082(2) .0457(16) .0394(15) -.0138(15) .0155(15) -.0037(13) O010 .0496(17) .066(2) .063(2) -.0161(15) .0008(15) -.0257(16) O011 .079(2) .0551(18) .0480(17) -.0054(16) -.0173(16) -.0045(14) O012 .078(2) .071(2) .057(2) -.0059(18) -.0003(18) -.0091(17) O013 .116(3) .128(4) .059(2) -.080(3) .004(2) -.005(2) O014 .090(2) .0408(15) .0403(15) .0026(15) -.0215(15) -.0094(12) O015 .076(2) .0487(17) .059(2) -.0217(16) .0172(17) -.0075(15) O016 .064(2) .100(3) .061(2) .014(2) -.0080(17) -.022(2) O017 .072(2) .109(3) .072(2) .028(2) .034(2) .026(2) O018 .075(2) .092(3) .064(2) .043(2) .0230(18) .016(2) O019 .113(3) .118(4) .061(2) .050(3) .003(2) -.020(2) O020 .256(7) .068(3) .079(3) -.014(4) -.021(4) -.004(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 O1 . . 1.981(2) ? Cu1 N10 . . 1.998(3) ? Cu1 N13 . . 2.021(3) ? Cu1 N13' . . 2.028(3) ? Cu1 O11 . . 2.317(2) ? Cu2 O2 . . 1.986(2) ? Cu2 N20 . . 2.000(3) ? Cu2 N23 . . 2.014(3) ? Cu2 N23' . . 2.032(3) ? Cu2 O21 . . 2.263(2) ? Cu3 O3 . . 1.986(2) ? Cu3 N30 . . 1.994(3) ? Cu3 N33 . . 2.014(2) ? Cu3 N33' . . 2.032(3) ? Cu3 O31 . . 2.314(3) ? O1 H1a . . .83(6) ? O1 H1b . . .77(4) ? N10 C11 . . 1.481(4) ? N10 C11' . . 1.480(5) ? N10 H10 . . .84(3) ? C11 C12 . . 1.524(5) ? C11 H11a . . .98(3) ? C11 H11b . . .92(3) ? C12 N13 . . 1.492(4) ? C12 H12a . . .87(4) ? C12 H12b . . 1.01(3) ? N13 C14 . . 1.500(4) ? N13 H13 . . .86(4) ? C14 C141 . . 1.508(5) ? C14 H14a . . .94(4) ? C14 H14b . . .89(4) ? C141 C142 . . 1.397(4) ? C141 C146 . . 1.394(4) ? C142 C143 . . 1.391(5) ? C142 H142 . . .89(4) ? C143 C144 . . 1.383(5) ? C143 H143 . . .98(3) ? C144 C145 . . 1.391(4) ? C144 H144 . . .98(4) ? C145 C146 . . 1.390(5) ? C145 H145 . . .92(4) ? C146 O15 . . 1.393(3) ? O15 C16 . . 1.453(4) ? C16 C16' . . 1.507(4) ? C16 H16a . . .97(4) ? C16 H16b . . .99(3) ? C11' C12' . . 1.515(4) ? C11' H11'a . . .91(3) ? C11' H11'b . . .92(4) ? C12' N13' . . 1.481(4) ? C12' H12'a . . .98(4) ? C12' H12'b . . .91(4) ? N13' C14' . . 1.491(4) ? N13' H13' . . .89(3) ? C14' C141' . . 1.506(4) ? C14' H14'a . . .93(3) ? C14' H14'b . . .89(4) ? C141' C142' . . 1.389(4) ? C141' C146' . . 1.402(4) ? C142' C143' . . 1.390(5) ? C142' H142' . . .87(3) ? C143' C144' . . 1.386(4) ? C143' H143' . . .86(4) ? C144' C145' . . 1.395(5) ? C144' H144' . . .94(4) ? C145' C146' . . 1.381(4) ? C145' H145' . . .92(3) ? C146' O15' . . 1.382(4) ? O15' C16' . . 1.433(4) ? C16' H16'a . . .95(3) ? C16' H16'b . . .94(4) ? O2 H2a . . .80(5) ? O2 H2b . . .76(4) ? N20 C21 . . 1.482(4) ? N20 C21' . . 1.482(5) ? N20 H20 . . .84(3) ? C21 C22 . . 1.519(5) ? C21 H21a . . .89(3) ? C21 H21b . . 1.01(4) ? C22 N23 . . 1.490(4) ? C22 H22a . . .95(4) ? C22 H22b . . .93(4) ? N23 C24 . . 1.497(4) ? N23 H23 . . .79(4) ? C24 C241 . . 1.511(5) ? C24 H24a . . .98(4) ? C24 H24b . . .96(4) ? C241 C242 . . 1.394(4) ? C241 C246 . . 1.392(4) ? C242 C243 . . 1.382(5) ? C242 H242 . . .99(4) ? C243 C244 . . 1.384(5) ? C243 H243 . . .90(3) ? C244 C245 . . 1.392(4) ? C244 H244 . . .94(4) ? C245 C246 . . 1.392(5) ? C245 H245 . . .94(4) ? C246 O25 . . 1.394(3) ? O25 C26 . . 1.447(4) ? C26 C26' . . 1.501(4) ? C26 H26a . . .99(4) ? C26 H26b . . .98(3) ? C21' C22' . . 1.518(4) ? C21' H21'a . . .99(4) ? C21' H21'b . . .94(3) ? C22' N23' . . 1.484(4) ? C22' H22'a . . 1.03(3) ? C22' H22'b . . 1.00(4) ? N23' C24' . . 1.490(4) ? N23' H23' . . .99(4) ? C24' C241' . . 1.509(4) ? C24' H24'a . . .93(4) ? C24' H24'b . . .96(3) ? C241' C242' . . 1.387(4) ? C241' C246' . . 1.405(4) ? C242' C243' . . 1.399(5) ? C242' H242' . . .92(4) ? C243' C244' . . 1.372(4) ? C243' H243' . . .90(4) ? C244' C245' . . 1.398(5) ? C244' H244' . . .86(4) ? C245' C246' . . 1.375(4) ? C245' H245' . . .90(3) ? C246' O25' . . 1.383(4) ? O25' C26' . . 1.437(4) ? C26' H26'a . . 1.00(3) ? C26' H26'b . . .88(4) ? O3 H3a . . .87(5) ? O3 H3b . . .84(4) ? N30 C31 . . 1.486(4) ? N30 C31' . . 1.480(5) ? N30 H30 . . .85(3) ? C31 C32 . . 1.528(5) ? C31 H31a . . .93(3) ? C31 H31b . . .94(3) ? C32 N33 . . 1.491(4) ? C32 H32a . . .94(3) ? C32 H32b . . .98(4) ? N33 C34 . . 1.504(4) ? N33 H33 . . .94(4) ? C34 C341 . . 1.512(5) ? C34 H34a . . .95(3) ? C34 H34b . . .93(4) ? C341 C342 . . 1.398(4) ? C341 C346 . . 1.390(4) ? C342 C343 . . 1.388(5) ? C342 H342 . . .97(4) ? C343 C344 . . 1.381(5) ? C343 H343 . . .88(4) ? C344 C345 . . 1.388(4) ? C344 H344 . . .90(4) ? C345 C346 . . 1.397(5) ? C345 H345 . . .98(4) ? C346 O35 . . 1.395(3) ? O35 C36 . . 1.445(4) ? C36 C36' . . 1.504(4) ? C36 H36a . . .98(4) ? C36 H36b . . .97(3) ? C31' C32' . . 1.514(4) ? C31' H31'a . . .96(3) ? C31' H31'b . . .94(3) ? C32' N33' . . 1.486(4) ? C32' H32'a . . .94(4) ? C32' H32'b . . .96(3) ? N33' C34' . . 1.492(3) ? N33' H33' . . .92(3) ? C34' C341' . . 1.510(4) ? C34' H34'a . . .91(3) ? C34' H34'b . . .94(4) ? C341' C342' . . 1.392(4) ? C341' C346' . . 1.402(4) ? C342' C343' . . 1.398(5) ? C342' H342' . . .88(3) ? C343' C344' . . 1.385(4) ? C343' H343' . . .94(4) ? C344' C345' . . 1.401(5) ? C344' H344' . . .99(4) ? C345' C346' . . 1.385(4) ? C345' H345' . . .94(3) ? C346' O35' . . 1.384(4) ? O35' C36' . . 1.436(4) ? C36' H36'a . . 1.00(3) ? C36' H36'b . . .95(4) ? S1 O11 . . 1.475(2) ? S1 O12 . . 1.479(3) ? S1 O13 . . 1.488(2) ? S1 O14 . . 1.459(3) ? S2 O21 . . 1.469(2) ? S2 O22 . . 1.462(3) ? S2 O23 . . 1.490(2) ? S2 O24 . . 1.462(3) ? S3 O31 . . 1.478(2) ? S3 O32 . . 1.460(3) ? S3 O33 . . 1.492(2) ? S3 O34 . . 1.460(3) ? O01 H01a . . .883 ? O01 H01b . . .883 ? O02 H02a . . .957 ? O02 H02b . . 1.045 ? O03 H03a . . 1.005 ? O03 H03b . . .922 ? O04 H04a . . .767 ? O04 H04b . . .878 ? O05 H05a . . .916 ? O05 H05b . . .746 ? O06 H06a . . 1.083 ? O06 H06b . . 1.012 ? O07 H07a . . .830 ? O07 H07b . . .906 ? O08 H08a . . .996 ? O08 H08b . . .927 ? O09 H09a . . .892 ? O09 H09b . . 1.023 ? O011 H011a . . 1.113 ? O011 H011b . . 1.077 ? O012 H012a . . 1.025 ? O012 H012b . . 1.040 ? O013 H013a . . .940 ? O013 H013b . . .926 ? O014 H014a . . .892 ? O014 H014b . . .929 ? O015 H015a . . 1.180 ? O015 H015b . . 1.099 ? O016 H016a . . 1.062 ? O016 H016b . . 1.242 ? O017 H017a . . 1.027 ? O017 H017b . . .926 ? O019 H019a . . .983 ? O019 H019b . . .920 ? O020 H020a . . 1.193 ? O020 H020b . . .957 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O1 Cu1 N10 . . . 176.02(11) ? O1 Cu1 N13 . . . 95.22(11) ? O1 Cu1 N13' . . . 95.65(10) ? O1 Cu1 O11 . . . 89.44(9) ? N10 Cu1 N13 . . . 85.85(10) ? N10 Cu1 N13' . . . 84.82(10) ? N10 Cu1 O11 . . . 86.58(9) ? N13 Cu1 N13' . . . 155.45(11) ? N13 Cu1 O11 . . . 109.57(10) ? N13' Cu1 O11 . . . 92.48(10) ? O2 Cu2 N20 . . . 176.50(10) ? O2 Cu2 N23 . . . 95.74(10) ? O2 Cu2 N23' . . . 95.12(10) ? O2 Cu2 O21 . . . 90.73(9) ? N20 Cu2 N23 . . . 85.78(10) ? N20 Cu2 N23' . . . 84.72(10) ? N20 Cu2 O21 . . . 85.81(9) ? N23 Cu2 N23' . . . 154.63(10) ? N23 Cu2 O21 . . . 107.10(10) ? N23' Cu2 O21 . . . 95.61(10) ? O3 Cu3 N30 . . . 174.92(10) ? O3 Cu3 N33 . . . 95.03(10) ? O3 Cu3 N33' . . . 96.03(9) ? O3 Cu3 O31 . . . 89.62(8) ? N30 Cu3 N33 . . . 86.04(10) ? N30 Cu3 N33' . . . 84.94(10) ? N30 Cu3 O31 . . . 85.34(9) ? N33 Cu3 N33' . . . 154.83(10) ? N33 Cu3 O31 . . . 109.06(10) ? N33' Cu3 O31 . . . 93.57(10) ? Cu1 O1 H1a . . . 111(3) ? Cu1 O1 H1b . . . 105(3) ? H1a O1 H1b . . . 106(5) ? Cu1 N10 C11 . . . 110.9(2) ? Cu1 N10 C11' . . . 108.37(17) ? Cu1 N10 H10 . . . 103(2) ? C11 N10 C11' . . . 116.6(2) ? C11 N10 H10 . . . 108(2) ? C11' N10 H10 . . . 109(3) ? N10 C11 C12 . . . 107.8(2) ? N10 C11 H11a . . . 109(2) ? N10 C11 H11b . . . 108(2) ? C12 C11 H11a . . . 112(2) ? C12 C11 H11b . . . 112(2) ? H11a C11 H11b . . . 107(3) ? C11 C12 N13 . . . 110.4(3) ? C11 C12 H12a . . . 109(3) ? C11 C12 H12b . . . 114(2) ? N13 C12 H12a . . . 106(2) ? N13 C12 H12b . . . 108(2) ? H12a C12 H12b . . . 109(3) ? Cu1 N13 C12 . . . 106.9(2) ? Cu1 N13 C14 . . . 116.19(19) ? Cu1 N13 H13 . . . 110(2) ? C12 N13 C14 . . . 114.1(2) ? C12 N13 H13 . . . 105(2) ? C14 N13 H13 . . . 105(2) ? N13 C14 C141 . . . 114.6(3) ? N13 C14 H14a . . . 107(2) ? N13 C14 H14b . . . 107(2) ? C141 C14 H14a . . . 112(3) ? C141 C14 H14b . . . 109(3) ? H14a C14 H14b . . . 107(4) ? C14 C141 C142 . . . 120.1(3) ? C14 C141 C146 . . . 122.2(2) ? C142 C141 C146 . . . 117.7(3) ? C141 C142 C143 . . . 121.5(3) ? C141 C142 H142 . . . 117(2) ? C143 C142 H142 . . . 122(2) ? C142 C143 C144 . . . 119.7(3) ? C142 C143 H143 . . . 115(2) ? C144 C143 H143 . . . 125(2) ? C143 C144 C145 . . . 120.1(3) ? C143 C144 H144 . . . 121.7(19) ? C145 C144 H144 . . . 118.2(19) ? C144 C145 C146 . . . 119.6(3) ? C144 C145 H145 . . . 119(2) ? C146 C145 H145 . . . 121(2) ? C141 C146 C145 . . . 121.5(2) ? C141 C146 O15 . . . 118.7(3) ? C145 C146 O15 . . . 119.8(3) ? C146 O15 C16 . . . 116.0(2) ? O15 C16 C16' . . . 110.4(3) ? O15 C16 H16a . . . 105(2) ? O15 C16 H16b . . . 109.7(18) ? C16' C16 H16a . . . 111(2) ? C16' C16 H16b . . . 110(2) ? H16a C16 H16b . . . 110(3) ? N10 C11' C12' . . . 107.0(3) ? N10 C11' H11'a . . . 109(2) ? N10 C11' H11'b . . . 110(3) ? C12' C11' H11'a . . . 108(2) ? C12' C11' H11'b . . . 113(2) ? H11'a C11' H11'b . . . 110(3) ? C11' C12' N13' . . . 108.3(3) ? C11' C12' H12'a . . . 114(2) ? C11' C12' H12'b . . . 111(2) ? N13' C12' H12'a . . . 112(2) ? N13' C12' H12'b . . . 108(2) ? H12'a C12' H12'b . . . 104(3) ? Cu1 N13' C12' . . . 108.59(18) ? Cu1 N13' C14' . . . 122.0(2) ? Cu1 N13' H13' . . . 97(2) ? C12' N13' C14' . . . 113.4(2) ? C12' N13' H13' . . . 110(2) ? C14' N13' H13' . . . 104(2) ? N13' C14' C141' . . . 112.2(2) ? N13' C14' H14'a . . . 108.2(18) ? N13' C14' H14'b . . . 105(2) ? C141' C14' H14'a . . . 111(2) ? C141' C14' H14'b . . . 115(2) ? H14'a C14' H14'b . . . 106(3) ? C14' C141' C142' . . . 123.4(3) ? C14' C141' C146' . . . 118.5(3) ? C142' C141' C146' . . . 118.1(3) ? C141' C142' C143' . . . 120.9(3) ? C141' C142' H142' . . . 122(3) ? C143' C142' H142' . . . 117(2) ? C142' C143' C144' . . . 120.1(3) ? C142' C143' H143' . . . 121(2) ? C144' C143' H143' . . . 119(2) ? C143' C144' C145' . . . 120.2(3) ? C143' C144' H144' . . . 120(2) ? C145' C144' H144' . . . 120(2) ? C144' C145' C146' . . . 119.1(3) ? C144' C145' H145' . . . 121(2) ? C146' C145' H145' . . . 119(2) ? C141' C146' C145' . . . 121.8(3) ? C141' C146' O15' . . . 114.7(3) ? C145' C146' O15' . . . 123.5(3) ? C146' O15' C16' . . . 117.5(2) ? C16 C16' O15' . . . 107.0(3) ? C16 C16' H16'a . . . 113(2) ? C16 C16' H16'b . . . 110.3(19) ? O15' C16' H16'a . . . 109.2(18) ? O15' C16' H16'b . . . 110(2) ? H16'a C16' H16'b . . . 107(3) ? Cu2 O2 H2a . . . 112(3) ? Cu2 O2 H2b . . . 101(3) ? H2a O2 H2b . . . 108(5) ? Cu2 N20 C21 . . . 110.7(2) ? Cu2 N20 C21' . . . 108.70(17) ? Cu2 N20 H20 . . . 102(2) ? C21 N20 C21' . . . 116.2(2) ? C21 N20 H20 . . . 110(2) ? C21' N20 H20 . . . 108(3) ? N20 C21 C22 . . . 107.5(2) ? N20 C21 H21a . . . 107(2) ? N20 C21 H21b . . . 112(2) ? C22 C21 H21a . . . 112(2) ? C22 C21 H21b . . . 109(2) ? H21a C21 H21b . . . 109(3) ? C21 C22 N23 . . . 110.3(3) ? C21 C22 H22a . . . 115(3) ? C21 C22 H22b . . . 108(3) ? N23 C22 H22a . . . 108(2) ? N23 C22 H22b . . . 105(2) ? H22a C22 H22b . . . 110(3) ? Cu2 N23 C22 . . . 106.9(2) ? Cu2 N23 C24 . . . 117.0(2) ? Cu2 N23 H23 . . . 106(2) ? C22 N23 C24 . . . 114.1(2) ? C22 N23 H23 . . . 106(2) ? C24 N23 H23 . . . 106(2) ? N23 C24 C241 . . . 114.7(3) ? N23 C24 H24a . . . 109(2) ? N23 C24 H24b . . . 109(2) ? C241 C24 H24a . . . 108(2) ? C241 C24 H24b . . . 111(2) ? H24a C24 H24b . . . 105(3) ? C24 C241 C242 . . . 120.0(3) ? C24 C241 C246 . . . 122.2(2) ? C242 C241 C246 . . . 117.8(3) ? C241 C242 C243 . . . 121.6(3) ? C241 C242 H242 . . . 119(2) ? C243 C242 H242 . . . 120(2) ? C242 C243 C244 . . . 119.9(3) ? C242 C243 H243 . . . 122(3) ? C244 C243 H243 . . . 118(3) ? C243 C244 C245 . . . 119.9(3) ? C243 C244 H244 . . . 121(2) ? C245 C244 H244 . . . 119(2) ? C244 C245 C246 . . . 119.5(3) ? C244 C245 H245 . . . 123(2) ? C246 C245 H245 . . . 118(2) ? C241 C246 C245 . . . 121.4(3) ? C241 C246 O25 . . . 118.9(3) ? C245 C246 O25 . . . 119.7(3) ? C246 O25 C26 . . . 115.7(2) ? O25 C26 C26' . . . 110.3(3) ? O25 C26 H26a . . . 107(2) ? O25 C26 H26b . . . 112.1(18) ? C26' C26 H26a . . . 110(2) ? C26' C26 H26b . . . 108(2) ? H26a C26 H26b . . . 111(3) ? N20 C21' C22' . . . 106.9(3) ? N20 C21' H21'a . . . 109(2) ? N20 C21' H21'b . . . 107(2) ? C22' C21' H21'a . . . 112.0(19) ? C22' C21' H21'b . . . 108.3(18) ? H21'a C21' H21'b . . . 113(3) ? C21' C22' N23' . . . 108.2(3) ? C21' C22' H22'a . . . 110.0(17) ? C21' C22' H22'b . . . 114(2) ? N23' C22' H22'a . . . 108(2) ? N23' C22' H22'b . . . 110(2) ? H22'a C22' H22'b . . . 106(3) ? Cu2 N23' C22' . . . 108.54(18) ? Cu2 N23' C24' . . . 122.5(2) ? Cu2 N23' H23' . . . 91(2) ? C22' N23' C24' . . . 113.0(2) ? C22' N23' H23' . . . 110(2) ? C24' N23' H23' . . . 108.5(19) ? N23' C24' C241' . . . 111.3(2) ? N23' C24' H24'a . . . 105.8(18) ? N23' C24' H24'b . . . 109.3(18) ? C241' C24' H24'a . . . 112(2) ? C241' C24' H24'b . . . 110(2) ? H24'a C24' H24'b . . . 109(3) ? C24' C241' C242' . . . 123.5(3) ? C24' C241' C246' . . . 118.4(3) ? C242' C241' C246' . . . 118.1(3) ? C241' C242' C243' . . . 120.7(3) ? C241' C242' H242' . . . 119(2) ? C243' C242' H242' . . . 121(2) ? C242' C243' C244' . . . 119.9(3) ? C242' C243' H243' . . . 118(2) ? C244' C243' H243' . . . 122(2) ? C243' C244' C245' . . . 120.5(3) ? C243' C244' H244' . . . 119(2) ? C245' C244' H244' . . . 120(2) ? C244' C245' C246' . . . 119.1(3) ? C244' C245' H245' . . . 125(2) ? C246' C245' H245' . . . 116(2) ? C241' C246' C245' . . . 121.6(3) ? C241' C246' O25' . . . 114.9(3) ? C245' C246' O25' . . . 123.5(3) ? C246' O25' C26' . . . 117.0(2) ? C26 C26' O25' . . . 107.2(3) ? C26 C26' H26'a . . . 110(2) ? C26 C26' H26'b . . . 115(2) ? O25' C26' H26'a . . . 107.9(18) ? O25' C26' H26'b . . . 110(2) ? H26'a C26' H26'b . . . 107(3) ? Cu3 O3 H3a . . . 115(3) ? Cu3 O3 H3b . . . 101(3) ? H3a O3 H3b . . . 108(4) ? Cu3 N30 C31 . . . 110.8(2) ? Cu3 N30 C31' . . . 108.77(17) ? Cu3 N30 H30 . . . 103(2) ? C31 N30 C31' . . . 115.9(2) ? C31 N30 H30 . . . 107(2) ? C31' N30 H30 . . . 110(3) ? N30 C31 C32 . . . 107.6(2) ? N30 C31 H31a . . . 108(2) ? N30 C31 H31b . . . 108.0(19) ? C32 C31 H31a . . . 111(2) ? C32 C31 H31b . . . 113(2) ? H31a C31 H31b . . . 109(3) ? C31 C32 N33 . . . 110.3(3) ? C31 C32 H32a . . . 111(2) ? C31 C32 H32b . . . 110(2) ? N33 C32 H32a . . . 105(2) ? N33 C32 H32b . . . 113(2) ? H32a C32 H32b . . . 108(3) ? Cu3 N33 C32 . . . 107.2(2) ? Cu3 N33 C34 . . . 115.34(18) ? Cu3 N33 H33 . . . 108.9(18) ? C32 N33 C34 . . . 114.4(2) ? C32 N33 H33 . . . 109.2(19) ? C34 N33 H33 . . . 102(2) ? N33 C34 C341 . . . 114.5(3) ? N33 C34 H34a . . . 107(2) ? N33 C34 H34b . . . 110(2) ? C341 C34 H34a . . . 111(2) ? C341 C34 H34b . . . 109(2) ? H34a C34 H34b . . . 105(3) ? C34 C341 C342 . . . 119.6(3) ? C34 C341 C346 . . . 122.5(2) ? C342 C341 C346 . . . 117.9(3) ? C341 C342 C343 . . . 121.1(3) ? C341 C342 H342 . . . 120(2) ? C343 C342 H342 . . . 119(2) ? C342 C343 C344 . . . 120.2(3) ? C342 C343 H343 . . . 121(3) ? C344 C343 H343 . . . 118(3) ? C343 C344 C345 . . . 120.0(3) ? C343 C344 H344 . . . 121(2) ? C345 C344 H344 . . . 118(2) ? C344 C345 C346 . . . 119.4(3) ? C344 C345 H345 . . . 121(2) ? C346 C345 H345 . . . 119(2) ? C341 C346 C345 . . . 121.4(2) ? C341 C346 O35 . . . 118.8(3) ? C345 C346 O35 . . . 119.8(3) ? C346 O35 C36 . . . 116.0(2) ? O35 C36 C36' . . . 110.5(3) ? O35 C36 H36a . . . 103(2) ? O35 C36 H36b . . . 112.4(19) ? C36' C36 H36a . . . 112(2) ? C36' C36 H36b . . . 108(2) ? H36a C36 H36b . . . 112(3) ? N30 C31' C32' . . . 107.0(3) ? N30 C31' H31'a . . . 108(2) ? N30 C31' H31'b . . . 109(2) ? C32' C31' H31'a . . . 109.9(18) ? C32' C31' H31'b . . . 111.7(17) ? H31'a C31' H31'b . . . 111(3) ? C31' C32' N33' . . . 108.6(3) ? C31' C32' H32'a . . . 113(2) ? C31' C32' H32'b . . . 109.6(18) ? N33' C32' H32'a . . . 114(2) ? N33' C32' H32'b . . . 109(2) ? H32'a C32' H32'b . . . 103(3) ? Cu3 N33' C32' . . . 108.17(17) ? Cu3 N33' C34' . . . 121.9(2) ? Cu3 N33' H33' . . . 94(2) ? C32' N33' C34' . . . 113.0(2) ? C32' N33' H33' . . . 111(2) ? C34' N33' H33' . . . 106.3(18) ? N33' C34' C341' . . . 112.0(2) ? N33' C34' H34'a . . . 106.1(17) ? N33' C34' H34'b . . . 109(2) ? C341' C34' H34'a . . . 111(2) ? C341' C34' H34'b . . . 110(2) ? H34'a C34' H34'b . . . 109(3) ? C34' C341' C342' . . . 123.2(3) ? C34' C341' C346' . . . 118.6(3) ? C342' C341' C346' . . . 118.2(3) ? C341' C342' C343' . . . 120.6(3) ? C341' C342' H342' . . . 120(2) ? C343' C342' H342' . . . 119(2) ? C342' C343' C344' . . . 120.1(3) ? C342' C343' H343' . . . 123(2) ? C344' C343' H343' . . . 117(2) ? C343' C344' C345' . . . 120.3(3) ? C343' C344' H344' . . . 121(2) ? C345' C344' H344' . . . 118(2) ? C344' C345' C346' . . . 118.8(3) ? C344' C345' H345' . . . 119(2) ? C346' C345' H345' . . . 122(2) ? C341' C346' C345' . . . 121.9(3) ? C341' C346' O35' . . . 114.8(3) ? C345' C346' O35' . . . 123.2(2) ? C346' O35' C36' . . . 116.8(2) ? C36 C36' O35' . . . 107.0(3) ? C36 C36' H36'a . . . 109(2) ? C36 C36' H36'b . . . 111.5(18) ? O35' C36' H36'a . . . 109.9(19) ? O35' C36' H36'b . . . 110.1(18) ? H36'a C36' H36'b . . . 109(3) ? O11 S1 O12 . . . 108.94(18) ? O11 S1 O13 . . . 109.52(14) ? O11 S1 O14 . . . 110.71(14) ? O12 S1 O13 . . . 109.24(15) ? O12 S1 O14 . . . 109.42(16) ? O13 S1 O14 . . . 108.99(15) ? Cu1 O11 S1 . . . 133.06(14) ? O21 S2 O22 . . . 109.59(16) ? O21 S2 O23 . . . 109.19(13) ? O21 S2 O24 . . . 109.84(15) ? O22 S2 O23 . . . 109.49(13) ? O22 S2 O24 . . . 109.98(16) ? O23 S2 O24 . . . 108.74(16) ? Cu2 O21 S2 . . . 133.24(13) ? O31 S3 O32 . . . 109.14(17) ? O31 S3 O33 . . . 109.39(13) ? O31 S3 O34 . . . 109.39(14) ? O32 S3 O33 . . . 109.55(14) ? O32 S3 O34 . . . 109.78(15) ? O33 S3 O34 . . . 109.58(15) ? Cu3 O31 S3 . . . 132.97(14) ? H01a O01 H01b . . . 108.7 ? H02a O02 H02b . . . 96.2 ? H03a O03 H03b . . . 112.6 ? H04a O04 H04b . . . 114.3 ? H05a O05 H05b . . . 99.0 ? H06a O06 H06b . . . 134.7 ? H07a O07 H07b . . . 109.9 ? H08a O08 H08b . . . 123.2 ? H09a O09 H09b . . . 97.3 ? H011a O011 H011b . . . 137.4 ? H012a O012 H012b . . . 82.5 ? H013a O013 H013b . . . 103.6 ? H014a O014 H014b . . . 124.3 ? H015a O015 H015b . . . 105.3 ? H016a O016 H016b . . . 96.2 ? H017a O017 H017b . . . 96.9 ? H019a O019 H019b . . . 104.4 ? H020a O020 H020b . . . 115.3 ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2026 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min -17 _reflns_limit_k_max 18 _reflns_limit_l_min -36 _reflns_limit_l_max 39 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 12.586 _diffrn_reflns_av_sigmaI/netI .047 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all .067 _refine_ls_wR_factor_all .067 _refine_ls_goodness_of_fit_all 1.24 _refine_ls_shift/su_mean .002 #===END