#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2013-04-14 at 22:19:37 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : agsg6_0m struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2013-04-14 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ AUTHOR DETAILS -------------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Barcel\'o-Oliver, Miquel' _publ_contact_author_address ; Department of Chemistry, University of the Balearic Islands, campus UIB, cta. Valldemossa km 7.5, Ed. Mateu Orfila Palma de Mallorca E-07122, SPAIN ; _publ_contact_author_email miquel.barcelo@uib.es _publ_contact_author_fax '0034971173426' _publ_contact_author_phone '0034971173199' # Insert blank lines between references _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of G\"ottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_agsg6_0m _audit_creation_date 2013-04-14T22:19:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H26 Cu1 N4 O11 U1' _chemical_formula_sum 'C22 H26 Cu N4 O11 U' _chemical_formula_weight 824.04 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.155(4) _cell_length_b 12.610(5) _cell_length_c 18.864(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2653.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4611 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.963 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1287 _exptl_absorpt_correction_T_max 0.2754 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_unetI/netI 0.099 _diffrn_reflns_number 11885 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.26 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 4611 _reflns_number_gt 3653 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.03' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. TWIN/BASF refinement was needed for account a racemic twin, due to Flack's parameter was not 0 between 2 Esd's ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4611 _refine_ls_number_parameters 357 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1421 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.045(14) _refine_diff_density_max 1.933 _refine_diff_density_min -3.145 _refine_diff_density_rms 0.226 _iucr_refine_instructions_details ; TITL agsg6_0m in P 21 21 21 CELL 0.71073 11.1545 12.6097 18.8640 90.000 90.000 90.000 ZERR 4.00 0.0042 0.0047 0.0072 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CU U UNIT 88 104 16 44 4 4 MERG 2 TWIN ISOR 0.01 C13 BOND -0.5 FMAP 2 SIZE 0.20 0.30 0.40 ACTA BOND -0.5 rem BOND $H CONF L.S. 4 TEMP 21.00 WGHT 0.077100 BASF 0.04502 FVAR 0.06069 U1 6 0.827708 0.513526 0.160517 11.00000 0.02184 0.03780 = 0.03071 -0.00012 0.00130 -0.00056 CU1 5 0.521920 0.537983 0.154336 11.00000 0.02382 0.04815 = 0.03514 -0.00064 0.00466 -0.00032 O9 4 1.027277 0.600805 0.178999 11.00000 0.03649 0.05479 = 0.04829 -0.00764 0.00308 -0.00532 O31 4 0.661395 0.626495 0.132243 11.00000 0.02387 0.04639 = 0.03269 0.00189 -0.00701 0.01097 O21 4 0.792606 0.522162 0.250753 11.00000 0.02189 0.05969 = 0.03347 -0.00024 -0.01112 -0.00828 O20 4 0.861011 0.505695 0.070305 11.00000 0.01518 0.04457 = 0.04193 0.00277 -0.01343 -0.00830 O11 4 0.639688 0.423887 0.140859 11.00000 0.02677 0.03889 = 0.03668 -0.00182 0.00494 -0.01705 O5 4 0.847462 0.315912 0.168482 11.00000 0.04675 0.03743 = 0.06338 0.01220 -0.01428 -0.00091 O8 4 0.876408 0.706453 0.163769 11.00000 0.02759 0.04207 = 0.06002 -0.00330 0.00038 -0.00216 O6 4 1.011320 0.399870 0.177217 11.00000 0.03205 0.03898 = 0.07402 0.00543 -0.00808 0.00346 O51 4 0.450303 0.522378 0.034315 11.00000 0.08214 0.08514 = 0.02437 0.00221 -0.01876 0.01713 N19 3 0.409075 0.430819 0.192809 11.00000 0.02041 0.07358 = 0.03177 0.00752 0.00891 0.01670 N4 3 0.990615 0.696777 0.172958 11.00000 0.05243 0.04543 = 0.02803 -0.01010 0.00139 -0.00342 C13 1 0.404179 0.335661 0.171459 11.00000 0.02391 0.04726 = 0.05892 0.01034 -0.00784 -0.01403 C1 1 0.640987 0.707697 0.086584 11.00000 0.03154 0.04716 = 0.02164 -0.00255 -0.00276 0.01239 O7 4 1.011968 0.227659 0.173121 11.00000 0.05738 0.04121 = 0.08624 -0.00085 -0.00753 0.00959 C11 1 0.331067 0.461497 0.253247 11.00000 0.04335 0.10505 = 0.06239 0.01398 0.01802 -0.02008 AFIX 23 H11A 2 0.248477 0.463816 0.237225 11.00000 -1.20000 H11B 2 0.336785 0.407653 0.289815 11.00000 -1.20000 AFIX 0 O10 4 1.058702 0.772112 0.172920 11.00000 0.06354 0.05595 = 0.07721 0.00664 -0.00397 -0.03288 C5 1 0.526601 0.853426 0.041085 11.00000 0.05665 0.05256 = 0.03285 -0.00565 -0.01140 0.02035 AFIX 43 H5 2 0.458760 0.896223 0.042794 11.00000 -1.20000 AFIX 0 C19 1 0.599873 0.341871 0.102541 11.00000 0.02648 0.04735 = 0.03316 0.00785 -0.00704 -0.01257 C3 1 0.712021 0.809689 -0.013197 11.00000 0.04413 0.05119 = 0.03525 0.01036 0.00042 -0.00359 AFIX 43 H3 2 0.769142 0.820070 -0.048433 11.00000 -1.20000 AFIX 0 C9 1 0.341266 0.662236 0.236457 11.00000 0.05643 0.08238 = 0.03257 -0.01019 0.02159 0.03209 AFIX 23 H9A 2 0.261007 0.659588 0.216741 11.00000 -1.20000 H9B 2 0.347500 0.725709 0.265271 11.00000 -1.20000 AFIX 0 C4 1 0.611823 0.873867 -0.011199 11.00000 0.07232 0.05271 = 0.04252 0.00617 -0.02650 0.00343 AFIX 43 H4 2 0.601552 0.928754 -0.043564 11.00000 -1.20000 AFIX 0 C7 1 0.445669 0.757728 0.145774 11.00000 0.02949 0.04562 = 0.03748 -0.01423 -0.01263 0.00281 N3 3 0.962020 0.311254 0.172183 11.00000 0.02126 0.05077 = 0.05261 -0.00982 -0.00546 0.00636 C21 1 0.379471 0.494358 -0.081754 11.00000 0.06706 0.10088 = 0.06195 -0.03500 -0.01399 0.01016 AFIX 137 H21A 2 0.306031 0.478072 -0.057557 11.00000 -1.50000 H21B 2 0.400472 0.436615 -0.112509 11.00000 -1.50000 H21C 2 0.369175 0.557721 -0.109301 11.00000 -1.50000 AFIX 0 N23 3 0.431551 0.667495 0.176992 11.00000 0.00757 0.07860 = 0.02957 -0.01836 0.00385 -0.00147 C2 1 0.728746 0.730808 0.035956 11.00000 0.02941 0.04996 = 0.04858 0.00361 0.01775 0.00351 AFIX 43 H2 2 0.799682 0.692056 0.035582 11.00000 -1.20000 AFIX 0 C10 1 0.362386 0.563382 0.283478 11.00000 0.02883 0.13461 = 0.03899 0.00674 0.01399 -0.00495 AFIX 23 H10A 2 0.446554 0.561505 0.296342 11.00000 -1.20000 H10B 2 0.316959 0.572380 0.326910 11.00000 -1.20000 AFIX 0 C12 1 0.313325 0.259509 0.198766 11.00000 0.04474 0.08367 = 0.07924 0.02570 -0.00996 -0.02114 AFIX 137 H12A 2 0.279266 0.286564 0.241861 11.00000 -1.50000 H12B 2 0.350946 0.192428 0.207947 11.00000 -1.50000 H12C 2 0.251153 0.250410 0.164105 11.00000 -1.50000 AFIX 0 C16 1 0.525742 0.171513 0.017852 11.00000 0.04005 0.04443 = 0.10889 -0.02761 -0.00949 -0.01439 AFIX 43 H16 2 0.499902 0.116123 -0.010891 11.00000 -1.20000 AFIX 0 C22 1 0.597905 0.512282 -0.055442 11.00000 0.06078 0.09926 = 0.07282 -0.01483 0.00130 -0.01533 AFIX 137 H22A 2 0.653171 0.500151 -0.017282 11.00000 -1.50000 H22B 2 0.614098 0.579992 -0.076647 11.00000 -1.50000 H22C 2 0.606932 0.457550 -0.090411 11.00000 -1.50000 AFIX 0 C8 1 0.368532 0.851958 0.165797 11.00000 0.03093 0.06213 = 0.06283 -0.02243 0.00074 0.01439 AFIX 137 H8B 2 0.286400 0.837206 0.154221 11.00000 -1.50000 H8C 2 0.394854 0.913398 0.140089 11.00000 -1.50000 H8A 2 0.375459 0.864985 0.215770 11.00000 -1.50000 AFIX 0 C15 1 0.449811 0.214174 0.069308 11.00000 0.02252 0.07688 = 0.07591 0.01553 -0.02375 -0.02058 AFIX 43 H15 2 0.373106 0.186439 0.074750 11.00000 -1.20000 AFIX 0 C18 1 0.675930 0.297328 0.049867 11.00000 0.04019 0.05064 = 0.03637 0.00153 0.00887 0.00778 AFIX 43 H18 2 0.751661 0.325884 0.042068 11.00000 -1.20000 AFIX 0 C6 1 0.537308 0.773064 0.090549 11.00000 0.03544 0.04602 = 0.04401 -0.01196 0.00213 0.00043 C14 1 0.486600 0.297364 0.112617 11.00000 0.04701 0.04539 = 0.03962 0.00133 -0.02042 -0.01438 C17 1 0.637519 0.211866 0.010356 11.00000 0.06127 0.05996 = 0.05118 -0.01519 -0.00364 -0.00394 AFIX 43 H17 2 0.689616 0.181200 -0.022222 11.00000 -1.20000 AFIX 0 C20 1 0.477464 0.511017 -0.028485 11.00000 0.05641 0.05484 = 0.05573 0.00672 -0.02858 0.00422 HKLF 4 REM agsg6_0m in P 21 21 21 REM R1 = 0.0568 for 3653 Fo > 4sig(Fo) and 0.0773 for all 4611 data REM 357 parameters refined using 6 restraints END WGHT 0.0770 0.0000 REM Highest difference peak 1.933, deepest hole -3.145, 1-sigma level 0.226 Q1 1 0.8336 0.5884 0.1602 11.00000 0.05 1.93 Q2 1 0.8258 0.5139 0.2148 11.00000 0.05 1.72 Q3 1 0.8301 0.4432 0.1603 11.00000 0.05 1.67 Q4 1 0.8259 0.5137 0.1064 11.00000 0.05 1.64 Q5 1 0.7433 0.5778 0.1673 11.00000 0.05 1.32 Q6 1 0.7563 0.4375 0.1177 11.00000 0.05 1.12 Q7 1 0.7478 0.5976 0.1352 11.00000 0.05 1.07 Q8 1 0.9086 0.5992 0.1295 11.00000 0.05 1.06 Q9 1 0.9092 0.4352 0.1268 11.00000 0.05 1.06 Q10 1 0.9085 0.4321 0.2006 11.00000 0.05 1.06 Q11 1 0.9159 0.5812 0.1806 11.00000 0.05 1.03 Q12 1 0.7443 0.4407 0.1769 11.00000 0.05 0.97 Q13 1 0.7584 0.4395 0.2052 11.00000 0.05 0.95 Q14 1 0.7505 0.4562 0.1594 11.00000 0.05 0.92 Q15 1 0.5214 0.5322 0.2149 11.00000 0.05 0.92 Q16 1 0.8997 0.5953 0.1932 11.00000 0.05 0.91 Q17 1 0.8758 0.5806 0.2267 11.00000 0.05 0.90 Q18 1 0.8260 0.5154 0.2808 11.00000 0.05 0.89 Q19 1 0.8950 0.4613 0.1564 11.00000 0.05 0.76 Q20 1 0.5713 0.5934 0.1580 11.00000 0.05 0.75 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.82771(5) 0.51353(4) 0.16052(3) 0.03012(17) Uani 1 1 d . . . Cu1 Cu 0.52192(15) 0.53798(12) 0.15434(10) 0.0357(4) Uani 1 1 d . . . O9 O 1.0273(9) 0.6008(8) 0.1790(6) 0.047(3) Uani 1 1 d . . . O31 O 0.6614(9) 0.6265(7) 0.1322(5) 0.034(2) Uani 1 1 d . . . O21 O 0.7926(7) 0.5222(8) 0.2508(5) 0.038(2) Uani 1 1 d . . . O20 O 0.8610(7) 0.5057(8) 0.0703(5) 0.034(2) Uani 1 1 d . . . O11 O 0.6397(8) 0.4239(7) 0.1409(5) 0.034(3) Uani 1 1 d . . . O5 O 0.8475(10) 0.3159(7) 0.1685(6) 0.049(3) Uani 1 1 d . . . O8 O 0.8764(9) 0.7065(7) 0.1638(7) 0.043(3) Uani 1 1 d . . . O6 O 1.0113(9) 0.3999(8) 0.1772(6) 0.048(3) Uani 1 1 d . . . O51 O 0.4503(11) 0.5224(10) 0.0343(6) 0.064(3) Uani 1 1 d . . . N19 N 0.4091(10) 0.4308(11) 0.1928(6) 0.042(3) Uani 1 1 d . . . N4 N 0.9906(13) 0.6968(10) 0.1730(7) 0.042(3) Uani 1 1 d . . . C13 C 0.4042(14) 0.3357(12) 0.1715(11) 0.043(4) Uani 1 1 d U . . C1 C 0.6410(12) 0.7077(11) 0.0866(7) 0.033(4) Uani 1 1 d . . . O7 O 1.0120(11) 0.2277(8) 0.1731(7) 0.062(3) Uani 1 1 d . . . C11 C 0.3311(18) 0.4615(15) 0.2532(10) 0.070(5) Uani 1 1 d . . . H11A H 0.2485 0.4638 0.2372 0.084 Uiso 1 1 calc R . . H11B H 0.3368 0.4077 0.2898 0.084 Uiso 1 1 calc R . . O10 O 1.0587(11) 0.7721(9) 0.1729(7) 0.066(4) Uani 1 1 d . . . C5 C 0.5266(16) 0.8534(12) 0.0411(8) 0.047(4) Uani 1 1 d . . . H5 H 0.4588 0.8962 0.0428 0.057 Uiso 1 1 calc R . . C19 C 0.5999(13) 0.3419(11) 0.1025(8) 0.036(4) Uani 1 1 d . . . C3 C 0.7120(14) 0.8097(12) -0.0132(8) 0.044(4) Uani 1 1 d . . . H3 H 0.7691 0.8201 -0.0484 0.052 Uiso 1 1 calc R . . C9 C 0.3413(17) 0.6622(13) 0.2365(8) 0.057(5) Uani 1 1 d . . . H9A H 0.261 0.6596 0.2167 0.069 Uiso 1 1 calc R . . H9B H 0.3475 0.7257 0.2653 0.069 Uiso 1 1 calc R . . C4 C 0.6118(16) 0.8739(13) -0.0112(9) 0.056(5) Uani 1 1 d . . . H4 H 0.6016 0.9288 -0.0436 0.067 Uiso 1 1 calc R . . C7 C 0.4457(13) 0.7577(12) 0.1458(8) 0.038(4) Uani 1 1 d . . . N3 N 0.9620(11) 0.3113(10) 0.1722(8) 0.042(4) Uani 1 1 d . . . C21 C 0.3795(16) 0.4944(18) -0.0818(10) 0.077(6) Uani 1 1 d . . . H21A H 0.306 0.4781 -0.0576 0.115 Uiso 1 1 calc R . . H21B H 0.4005 0.4366 -0.1125 0.115 Uiso 1 1 calc R . . H21C H 0.3692 0.5577 -0.1093 0.115 Uiso 1 1 calc R . . N23 N 0.4316(10) 0.6675(11) 0.1770(7) 0.039(3) Uani 1 1 d . . . C2 C 0.7287(14) 0.7308(12) 0.0360(9) 0.043(4) Uani 1 1 d . . . H2 H 0.7997 0.6921 0.0356 0.051 Uiso 1 1 calc R . . C10 C 0.3624(14) 0.5634(17) 0.2835(9) 0.067(6) Uani 1 1 d . . . H10A H 0.4466 0.5615 0.2963 0.081 Uiso 1 1 calc R . . H10B H 0.317 0.5724 0.3269 0.081 Uiso 1 1 calc R . . C12 C 0.3133(17) 0.2595(15) 0.1988(11) 0.069(6) Uani 1 1 d . . . H12A H 0.2793 0.2866 0.2419 0.104 Uiso 1 1 calc R . . H12B H 0.3509 0.1924 0.2079 0.104 Uiso 1 1 calc R . . H12C H 0.2512 0.2504 0.1641 0.104 Uiso 1 1 calc R . . C16 C 0.5257(16) 0.1715(13) 0.0179(12) 0.064(6) Uani 1 1 d . . . H16 H 0.4999 0.1161 -0.0109 0.077 Uiso 1 1 calc R . . C22 C 0.5979(16) 0.5123(18) -0.0554(10) 0.078(6) Uani 1 1 d . . . H22A H 0.6532 0.5002 -0.0173 0.116 Uiso 1 1 calc R . . H22B H 0.6141 0.58 -0.0766 0.116 Uiso 1 1 calc R . . H22C H 0.6069 0.4575 -0.0904 0.116 Uiso 1 1 calc R . . C8 C 0.3685(13) 0.8520(12) 0.1658(10) 0.052(4) Uani 1 1 d . . . H8B H 0.2864 0.8372 0.1542 0.078 Uiso 1 1 calc R . . H8C H 0.3949 0.9134 0.1401 0.078 Uiso 1 1 calc R . . H8A H 0.3755 0.865 0.2158 0.078 Uiso 1 1 calc R . . C15 C 0.4498(14) 0.2142(14) 0.0693(10) 0.058(5) Uani 1 1 d . . . H15 H 0.3731 0.1864 0.0748 0.07 Uiso 1 1 calc R . . C18 C 0.6759(17) 0.2973(11) 0.0499(7) 0.042(4) Uani 1 1 d . . . H18 H 0.7517 0.3259 0.0421 0.051 Uiso 1 1 calc R . . C6 C 0.5373(13) 0.7731(12) 0.0905(8) 0.042(4) Uani 1 1 d . . . C14 C 0.4866(15) 0.2974(12) 0.1126(8) 0.044(4) Uani 1 1 d . . . C17 C 0.6375(16) 0.2119(13) 0.0104(9) 0.057(5) Uani 1 1 d . . . H17 H 0.6896 0.1812 -0.0222 0.069 Uiso 1 1 calc R . . C20 C 0.4775(15) 0.5110(13) -0.0285(9) 0.056(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0218(3) 0.0378(3) 0.0307(3) -0.0001(2) 0.0013(3) -0.0006(2) Cu1 0.0238(9) 0.0482(10) 0.0351(11) -0.0006(8) 0.0047(9) -0.0003(7) O9 0.036(7) 0.055(7) 0.048(8) -0.008(5) 0.003(6) -0.005(5) O31 0.024(5) 0.046(5) 0.033(5) 0.002(4) -0.007(5) 0.011(5) O21 0.022(5) 0.060(6) 0.033(6) 0.000(4) -0.011(4) -0.008(4) O20 0.015(4) 0.045(5) 0.042(6) 0.003(5) -0.013(4) -0.008(4) O11 0.027(6) 0.039(5) 0.037(6) -0.002(4) 0.005(4) -0.017(4) O5 0.047(7) 0.037(5) 0.063(8) 0.012(5) -0.014(7) -0.001(5) O8 0.028(6) 0.042(5) 0.060(8) -0.003(6) 0.000(6) -0.002(4) O6 0.032(6) 0.039(6) 0.074(9) 0.005(5) -0.008(6) 0.003(5) O51 0.082(9) 0.085(9) 0.024(6) 0.002(6) -0.019(6) 0.017(7) N19 0.020(7) 0.074(9) 0.032(8) 0.008(6) 0.009(6) 0.017(6) N4 0.052(9) 0.045(7) 0.028(8) -0.010(6) 0.001(7) -0.003(7) C13 0.024(7) 0.047(7) 0.059(9) 0.010(7) -0.008(7) -0.014(6) C1 0.032(10) 0.047(8) 0.022(8) -0.003(6) -0.003(7) 0.012(6) O7 0.057(8) 0.041(6) 0.086(10) -0.001(6) -0.008(8) 0.010(6) C11 0.043(11) 0.105(15) 0.062(12) 0.014(10) 0.018(11) -0.020(12) O10 0.064(8) 0.056(7) 0.077(10) 0.007(6) -0.004(7) -0.033(6) C5 0.057(12) 0.053(10) 0.033(10) -0.006(7) -0.011(9) 0.020(8) C19 0.026(8) 0.047(8) 0.033(9) 0.008(6) -0.007(7) -0.013(7) C3 0.044(10) 0.051(9) 0.035(10) 0.010(7) 0.000(8) -0.004(7) C9 0.056(12) 0.082(11) 0.033(9) -0.010(8) 0.022(10) 0.032(10) C4 0.072(13) 0.053(10) 0.043(11) 0.006(8) -0.027(10) 0.003(9) C7 0.029(8) 0.046(9) 0.037(10) -0.014(7) -0.013(7) 0.003(7) N3 0.021(7) 0.051(8) 0.053(10) -0.010(7) -0.005(7) 0.006(6) C21 0.067(12) 0.101(14) 0.062(13) -0.035(13) -0.014(10) 0.010(12) N23 0.008(6) 0.079(10) 0.030(8) -0.018(6) 0.004(5) -0.001(6) C2 0.029(8) 0.050(9) 0.049(11) 0.004(8) 0.018(8) 0.004(7) C10 0.029(11) 0.135(17) 0.039(11) 0.007(11) 0.014(8) -0.005(10) C12 0.045(12) 0.084(13) 0.079(14) 0.026(10) -0.010(11) -0.021(11) C16 0.040(11) 0.044(9) 0.109(18) -0.028(10) -0.009(11) -0.014(8) C22 0.061(13) 0.099(15) 0.073(14) -0.015(12) 0.001(10) -0.015(13) C8 0.031(8) 0.062(10) 0.063(12) -0.022(9) 0.001(8) 0.014(7) C15 0.023(9) 0.077(12) 0.076(14) 0.016(10) -0.024(9) -0.021(8) C18 0.040(9) 0.051(8) 0.036(9) 0.002(6) 0.009(10) 0.008(9) C6 0.035(9) 0.046(9) 0.044(10) -0.012(7) 0.002(8) 0.000(7) C14 0.047(10) 0.045(9) 0.040(10) 0.001(7) -0.020(8) -0.014(8) C17 0.061(13) 0.060(11) 0.051(12) -0.015(8) -0.004(9) -0.004(9) C20 0.056(11) 0.055(10) 0.056(11) 0.007(9) -0.029(9) 0.004(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O20 1.745(9) . ? U1 O21 1.750(9) . ? U1 O31 2.399(9) . ? U1 O11 2.411(8) . ? U1 O8 2.493(9) . ? U1 O5 2.506(9) . ? U1 O9 2.508(10) . ? U1 O6 2.520(10) . ? U1 N4 2.949(13) . ? U1 N3 2.966(13) . ? U1 Cu1 3.427(2) . ? Cu1 O31 1.960(10) . ? Cu1 O11 1.965(9) . ? Cu1 N23 1.966(13) . ? Cu1 N19 1.984(13) . ? Cu1 O51 2.409(11) . ? O9 N4 1.282(16) . ? O31 C1 1.357(16) . ? O11 C19 1.338(16) . ? O5 N3 1.281(15) . ? O8 N4 1.291(16) . ? O6 N3 1.249(16) . ? O51 C20 1.231(19) . ? N19 C13 1.27(2) . ? N19 C11 1.49(2) . ? N4 O10 1.216(16) . ? C13 C12 1.49(2) . ? C13 C14 1.52(3) . ? C1 C2 1.398(19) . ? C1 C6 1.422(19) . ? O7 N3 1.192(16) . ? C11 C10 1.45(3) . ? C5 C6 1.38(2) . ? C5 C4 1.39(2) . ? C19 C14 1.40(2) . ? C19 C18 1.42(2) . ? C3 C2 1.37(2) . ? C3 C4 1.38(2) . ? C9 N23 1.509(19) . ? C9 C10 1.55(2) . ? C7 N23 1.29(2) . ? C7 C6 1.47(2) . ? C7 C8 1.515(19) . ? C21 C20 1.50(2) . ? C16 C17 1.35(2) . ? C16 C15 1.40(2) . ? C22 C20 1.44(2) . ? C15 C14 1.39(2) . ? C18 C17 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O20 U1 O21 179.3(4) . . ? O20 U1 O31 88.9(3) . . ? O21 U1 O31 90.4(4) . . ? O20 U1 O11 90.5(3) . . ? O21 U1 O11 89.1(3) . . ? O31 U1 O11 64.6(3) . . ? O20 U1 O8 91.9(4) . . ? O21 U1 O8 87.9(4) . . ? O31 U1 O8 66.1(3) . . ? O11 U1 O8 130.6(3) . . ? O20 U1 O5 89.1(4) . . ? O21 U1 O5 91.3(4) . . ? O31 U1 O5 132.2(3) . . ? O11 U1 O5 67.6(3) . . ? O8 U1 O5 161.7(3) . . ? O20 U1 O9 88.4(3) . . ? O21 U1 O9 92.1(4) . . ? O31 U1 O9 117.2(4) . . ? O11 U1 O9 177.8(3) . . ? O8 U1 O9 51.3(3) . . ? O5 U1 O9 110.5(4) . . ? O20 U1 O6 85.2(4) . . ? O21 U1 O6 95.5(4) . . ? O31 U1 O6 173.8(3) . . ? O11 U1 O6 117.4(3) . . ? O8 U1 O6 112.0(3) . . ? O5 U1 O6 49.9(3) . . ? O9 U1 O6 60.7(3) . . ? O20 U1 N4 89.5(4) . . ? O21 U1 N4 90.7(4) . . ? O31 U1 N4 91.7(4) . . ? O11 U1 N4 156.3(4) . . ? O8 U1 N4 25.7(3) . . ? O5 U1 N4 136.1(4) . . ? O9 U1 N4 25.6(4) . . ? O6 U1 N4 86.3(4) . . ? O20 U1 N3 85.2(4) . . ? O21 U1 N3 95.4(4) . . ? O31 U1 N3 156.6(3) . . ? O11 U1 N3 92.7(3) . . ? O8 U1 N3 136.6(3) . . ? O5 U1 N3 25.3(3) . . ? O9 U1 N3 85.3(3) . . ? O6 U1 N3 24.6(3) . . ? N4 U1 N3 110.9(4) . . ? O20 U1 Cu1 100.6(2) . . ? O21 U1 Cu1 78.7(3) . . ? O31 U1 Cu1 33.8(2) . . ? O11 U1 Cu1 34.0(2) . . ? O8 U1 Cu1 97.5(2) . . ? O5 U1 Cu1 100.3(2) . . ? O9 U1 Cu1 148.1(2) . . ? O6 U1 Cu1 149.8(2) . . ? N4 U1 Cu1 123.1(3) . . ? N3 U1 Cu1 125.6(2) . . ? O31 Cu1 O11 81.9(4) . . ? O31 Cu1 N23 88.9(4) . . ? O11 Cu1 N23 168.3(4) . . ? O31 Cu1 N19 165.8(4) . . ? O11 Cu1 N19 88.4(4) . . ? N23 Cu1 N19 99.3(5) . . ? O31 Cu1 O51 96.3(4) . . ? O11 Cu1 O51 92.3(4) . . ? N23 Cu1 O51 95.9(5) . . ? N19 Cu1 O51 94.5(5) . . ? O31 Cu1 U1 43.0(3) . . ? O11 Cu1 U1 43.4(2) . . ? N23 Cu1 U1 125.3(4) . . ? N19 Cu1 U1 123.9(3) . . ? O51 Cu1 U1 110.8(3) . . ? N4 O9 U1 96.8(9) . . ? C1 O31 Cu1 115.6(9) . . ? C1 O31 U1 136.0(9) . . ? Cu1 O31 U1 103.2(4) . . ? C19 O11 Cu1 114.5(9) . . ? C19 O11 U1 137.3(9) . . ? Cu1 O11 U1 102.6(4) . . ? N3 O5 U1 97.8(8) . . ? N4 O8 U1 97.2(7) . . ? N3 O6 U1 98.1(8) . . ? C20 O51 Cu1 146.3(11) . . ? C13 N19 C11 117.7(15) . . ? C13 N19 Cu1 123.8(11) . . ? C11 N19 Cu1 118.4(11) . . ? O10 N4 O9 122.5(15) . . ? O10 N4 O8 122.8(13) . . ? O9 N4 O8 114.6(12) . . ? O10 N4 U1 175.4(11) . . ? O9 N4 U1 57.6(7) . . ? O8 N4 U1 57.0(6) . . ? N19 C13 C12 122.0(18) . . ? N19 C13 C14 120.5(14) . . ? C12 C13 C14 117.4(16) . . ? O31 C1 C2 118.2(12) . . ? O31 C1 C6 122.7(13) . . ? C2 C1 C6 119.0(13) . . ? C10 C11 N19 113.1(15) . . ? C6 C5 C4 123.7(15) . . ? O11 C19 C14 122.5(14) . . ? O11 C19 C18 119.0(13) . . ? C14 C19 C18 118.5(14) . . ? C2 C3 C4 121.1(16) . . ? N23 C9 C10 111.1(13) . . ? C3 C4 C5 117.6(15) . . ? N23 C7 C6 121.6(14) . . ? N23 C7 C8 120.6(14) . . ? C6 C7 C8 117.9(14) . . ? O7 N3 O6 125.7(13) . . ? O7 N3 O5 120.5(13) . . ? O6 N3 O5 113.7(12) . . ? O7 N3 U1 175.7(12) . . ? O6 N3 U1 57.2(7) . . ? O5 N3 U1 56.8(6) . . ? C7 N23 C9 117.3(13) . . ? C7 N23 Cu1 124.8(11) . . ? C9 N23 Cu1 117.9(11) . . ? C3 C2 C1 121.1(15) . . ? C11 C10 C9 116.9(15) . . ? C17 C16 C15 119.1(16) . . ? C14 C15 C16 121.3(15) . . ? C17 C18 C19 120.1(17) . . ? C5 C6 C1 117.4(14) . . ? C5 C6 C7 120.9(15) . . ? C1 C6 C7 121.7(14) . . ? C15 C14 C19 119.4(16) . . ? C15 C14 C13 119.3(15) . . ? C19 C14 C13 121.3(13) . . ? C16 C17 C18 121.6(18) . . ? O51 C20 C22 124.7(15) . . ? O51 C20 C21 118.8(16) . . ? C22 C20 C21 116.5(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O20 U1 Cu1 O31 -71.8(5) . . . . ? O21 U1 Cu1 O31 108.0(5) . . . . ? O11 U1 Cu1 O31 -146.6(6) . . . . ? O8 U1 Cu1 O31 21.6(5) . . . . ? O5 U1 Cu1 O31 -162.7(5) . . . . ? O9 U1 Cu1 O31 32.4(6) . . . . ? O6 U1 Cu1 O31 -170.6(6) . . . . ? N4 U1 Cu1 O31 24.6(5) . . . . ? N3 U1 Cu1 O31 -163.4(5) . . . . ? O20 U1 Cu1 O11 74.9(5) . . . . ? O21 U1 Cu1 O11 -105.4(5) . . . . ? O31 U1 Cu1 O11 146.6(6) . . . . ? O8 U1 Cu1 O11 168.2(5) . . . . ? O5 U1 Cu1 O11 -16.1(5) . . . . ? O9 U1 Cu1 O11 179.1(6) . . . . ? O6 U1 Cu1 O11 -24.0(7) . . . . ? N4 U1 Cu1 O11 171.2(5) . . . . ? N3 U1 Cu1 O11 -16.8(5) . . . . ? O20 U1 Cu1 N23 -109.1(6) . . . . ? O21 U1 Cu1 N23 70.7(6) . . . . ? O31 U1 Cu1 N23 -37.3(6) . . . . ? O11 U1 Cu1 N23 176.1(6) . . . . ? O8 U1 Cu1 N23 -15.7(6) . . . . ? O5 U1 Cu1 N23 160.0(6) . . . . ? O9 U1 Cu1 N23 -4.9(7) . . . . ? O6 U1 Cu1 N23 152.1(7) . . . . ? N4 U1 Cu1 N23 -12.7(6) . . . . ? N3 U1 Cu1 N23 159.3(7) . . . . ? O20 U1 Cu1 N19 115.5(6) . . . . ? O21 U1 Cu1 N19 -64.8(6) . . . . ? O31 U1 Cu1 N19 -172.8(6) . . . . ? O11 U1 Cu1 N19 40.6(6) . . . . ? O8 U1 Cu1 N19 -151.2(5) . . . . ? O5 U1 Cu1 N19 24.5(5) . . . . ? O9 U1 Cu1 N19 -140.3(7) . . . . ? O6 U1 Cu1 N19 16.7(7) . . . . ? N4 U1 Cu1 N19 -148.2(5) . . . . ? N3 U1 Cu1 N19 23.8(6) . . . . ? O20 U1 Cu1 O51 4.7(5) . . . . ? O21 U1 Cu1 O51 -175.6(5) . . . . ? O31 U1 Cu1 O51 76.4(5) . . . . ? O11 U1 Cu1 O51 -70.2(5) . . . . ? O8 U1 Cu1 O51 98.0(4) . . . . ? O5 U1 Cu1 O51 -86.3(4) . . . . ? O9 U1 Cu1 O51 108.9(6) . . . . ? O6 U1 Cu1 O51 -94.1(6) . . . . ? N4 U1 Cu1 O51 101.0(4) . . . . ? N3 U1 Cu1 O51 -87.0(5) . . . . ? O20 U1 O9 N4 92.2(9) . . . . ? O21 U1 O9 N4 -87.2(8) . . . . ? O31 U1 O9 N4 4.2(9) . . . . ? O8 U1 O9 N4 -1.5(8) . . . . ? O5 U1 O9 N4 -179.4(8) . . . . ? O6 U1 O9 N4 177.6(10) . . . . ? N3 U1 O9 N4 177.5(8) . . . . ? Cu1 U1 O9 N4 -15.4(11) . . . . ? O11 Cu1 O31 C1 136.1(9) . . . . ? N23 Cu1 O31 C1 -51.1(9) . . . . ? N19 Cu1 O31 C1 -176.4(17) . . . . ? O51 Cu1 O31 C1 44.7(9) . . . . ? U1 Cu1 O31 C1 158.5(10) . . . . ? O11 Cu1 O31 U1 -22.4(4) . . . . ? N23 Cu1 O31 U1 150.3(5) . . . . ? N19 Cu1 O31 U1 25(2) . . . . ? O51 Cu1 O31 U1 -113.9(4) . . . . ? O20 U1 O31 C1 -40.7(12) . . . . ? O21 U1 O31 C1 139.4(12) . . . . ? O11 U1 O31 C1 -131.7(12) . . . . ? O8 U1 O31 C1 51.9(12) . . . . ? O5 U1 O31 C1 -128.4(12) . . . . ? O9 U1 O31 C1 46.9(12) . . . . ? N4 U1 O31 C1 48.8(12) . . . . ? N3 U1 O31 C1 -116.0(14) . . . . ? Cu1 U1 O31 C1 -151.7(14) . . . . ? O20 U1 O31 Cu1 111.0(4) . . . . ? O21 U1 O31 Cu1 -68.9(4) . . . . ? O11 U1 O31 Cu1 19.9(3) . . . . ? O8 U1 O31 Cu1 -156.5(5) . . . . ? O5 U1 O31 Cu1 23.2(6) . . . . ? O9 U1 O31 Cu1 -161.4(4) . . . . ? N4 U1 O31 Cu1 -159.6(4) . . . . ? N3 U1 O31 Cu1 35.7(11) . . . . ? O31 Cu1 O11 C19 -135.9(9) . . . . ? N23 Cu1 O11 C19 -174(2) . . . . ? N19 Cu1 O11 C19 54.5(10) . . . . ? O51 Cu1 O11 C19 -39.9(9) . . . . ? U1 Cu1 O11 C19 -158.2(11) . . . . ? O31 Cu1 O11 U1 22.3(4) . . . . ? N23 Cu1 O11 U1 -16(3) . . . . ? N19 Cu1 O11 U1 -147.3(5) . . . . ? O51 Cu1 O11 U1 118.3(4) . . . . ? O20 U1 O11 C19 41.7(13) . . . . ? O21 U1 O11 C19 -138.9(13) . . . . ? O31 U1 O11 C19 130.3(13) . . . . ? O8 U1 O11 C19 134.6(12) . . . . ? O5 U1 O11 C19 -47.0(12) . . . . ? O6 U1 O11 C19 -43.1(14) . . . . ? N4 U1 O11 C19 131.5(13) . . . . ? N3 U1 O11 C19 -43.5(13) . . . . ? Cu1 U1 O11 C19 150.1(15) . . . . ? O20 U1 O11 Cu1 -108.4(5) . . . . ? O21 U1 O11 Cu1 71.0(5) . . . . ? O31 U1 O11 Cu1 -19.8(3) . . . . ? O8 U1 O11 Cu1 -15.5(6) . . . . ? O5 U1 O11 Cu1 162.8(5) . . . . ? O6 U1 O11 Cu1 166.7(4) . . . . ? N4 U1 O11 Cu1 -18.6(10) . . . . ? N3 U1 O11 Cu1 166.4(4) . . . . ? O20 U1 O5 N3 80.7(9) . . . . ? O21 U1 O5 N3 -99.9(9) . . . . ? O31 U1 O5 N3 168.4(8) . . . . ? O11 U1 O5 N3 171.7(10) . . . . ? O8 U1 O5 N3 -12.4(16) . . . . ? O9 U1 O5 N3 -7.2(10) . . . . ? O6 U1 O5 N3 -3.8(9) . . . . ? N4 U1 O5 N3 -7.5(12) . . . . ? Cu1 U1 O5 N3 -178.7(9) . . . . ? O20 U1 O8 N4 -84.9(9) . . . . ? O21 U1 O8 N4 95.8(9) . . . . ? O31 U1 O8 N4 -172.9(10) . . . . ? O11 U1 O8 N4 -177.1(8) . . . . ? O5 U1 O8 N4 7.8(17) . . . . ? O9 U1 O8 N4 1.5(8) . . . . ? O6 U1 O8 N4 0.7(10) . . . . ? N3 U1 O8 N4 0.1(13) . . . . ? Cu1 U1 O8 N4 174.2(9) . . . . ? O20 U1 O6 N3 -88.9(10) . . . . ? O21 U1 O6 N3 91.0(10) . . . . ? O11 U1 O6 N3 -0.8(11) . . . . ? O8 U1 O6 N3 -179.0(10) . . . . ? O5 U1 O6 N3 3.9(9) . . . . ? O9 U1 O6 N3 -179.7(12) . . . . ? N4 U1 O6 N3 -178.7(10) . . . . ? Cu1 U1 O6 N3 14.0(13) . . . . ? O31 Cu1 O51 C20 39(2) . . . . ? O11 Cu1 O51 C20 -43(2) . . . . ? N23 Cu1 O51 C20 129(2) . . . . ? N19 Cu1 O51 C20 -131(2) . . . . ? U1 Cu1 O51 C20 -2(2) . . . . ? O31 Cu1 N19 C13 -81(2) . . . . ? O11 Cu1 N19 C13 -33.8(13) . . . . ? N23 Cu1 N19 C13 155.1(13) . . . . ? O51 Cu1 N19 C13 58.4(14) . . . . ? U1 Cu1 N19 C13 -60.3(14) . . . . ? O31 Cu1 N19 C11 95(2) . . . . ? O11 Cu1 N19 C11 142.1(12) . . . . ? N23 Cu1 N19 C11 -29.0(13) . . . . ? O51 Cu1 N19 C11 -125.7(12) . . . . ? U1 Cu1 N19 C11 115.6(11) . . . . ? U1 O9 N4 O10 -174.5(13) . . . . ? U1 O9 N4 O8 2.5(13) . . . . ? U1 O8 N4 O10 174.5(13) . . . . ? U1 O8 N4 O9 -2.6(13) . . . . ? O20 U1 N4 O9 -87.3(8) . . . . ? O21 U1 N4 O9 93.4(8) . . . . ? O31 U1 N4 O9 -176.2(8) . . . . ? O11 U1 N4 O9 -177.3(8) . . . . ? O8 U1 N4 O9 177.3(14) . . . . ? O5 U1 N4 O9 0.8(11) . . . . ? O6 U1 N4 O9 -2.1(9) . . . . ? N3 U1 N4 O9 -2.7(8) . . . . ? Cu1 U1 N4 O9 170.4(7) . . . . ? O20 U1 N4 O8 95.4(9) . . . . ? O21 U1 N4 O8 -83.9(9) . . . . ? O31 U1 N4 O8 6.5(9) . . . . ? O11 U1 N4 O8 5.4(14) . . . . ? O5 U1 N4 O8 -176.5(8) . . . . ? O9 U1 N4 O8 -177.3(14) . . . . ? O6 U1 N4 O8 -179.3(9) . . . . ? N3 U1 N4 O8 -179.9(9) . . . . ? Cu1 U1 N4 O8 -6.9(10) . . . . ? C11 N19 C13 C12 8(2) . . . . ? Cu1 N19 C13 C12 -176.3(12) . . . . ? C11 N19 C13 C14 -176.5(15) . . . . ? Cu1 N19 C13 C14 -1(2) . . . . ? Cu1 O31 C1 C2 -140.8(12) . . . . ? U1 O31 C1 C2 8(2) . . . . ? Cu1 O31 C1 C6 42.5(16) . . . . ? U1 O31 C1 C6 -168.3(9) . . . . ? C13 N19 C11 C10 167.0(16) . . . . ? Cu1 N19 C11 C10 -9(2) . . . . ? Cu1 O11 C19 C14 -44.1(17) . . . . ? U1 O11 C19 C14 168.2(10) . . . . ? Cu1 O11 C19 C18 136.5(11) . . . . ? U1 O11 C19 C18 -11(2) . . . . ? C2 C3 C4 C5 -2(2) . . . . ? C6 C5 C4 C3 0(2) . . . . ? U1 O6 N3 O7 176.3(16) . . . . ? U1 O6 N3 O5 -6.4(15) . . . . ? U1 O5 N3 O7 -176.1(15) . . . . ? U1 O5 N3 O6 6.4(15) . . . . ? O20 U1 N3 O6 89.0(10) . . . . ? O21 U1 N3 O6 -91.4(10) . . . . ? O31 U1 N3 O6 165.1(8) . . . . ? O11 U1 N3 O6 179.3(10) . . . . ? O8 U1 N3 O6 1.4(13) . . . . ? O5 U1 N3 O6 -173.0(16) . . . . ? O9 U1 N3 O6 0.3(10) . . . . ? N4 U1 N3 O6 1.4(10) . . . . ? Cu1 U1 N3 O6 -171.4(8) . . . . ? O20 U1 N3 O5 -98.0(9) . . . . ? O21 U1 N3 O5 81.6(9) . . . . ? O31 U1 N3 O5 -22.0(16) . . . . ? O11 U1 N3 O5 -7.7(9) . . . . ? O8 U1 N3 O5 174.4(7) . . . . ? O9 U1 N3 O5 173.3(9) . . . . ? O6 U1 N3 O5 173.0(16) . . . . ? N4 U1 N3 O5 174.4(9) . . . . ? Cu1 U1 N3 O5 1.6(11) . . . . ? C6 C7 N23 C9 175.7(14) . . . . ? C8 C7 N23 C9 -4(2) . . . . ? C6 C7 N23 Cu1 -3(2) . . . . ? C8 C7 N23 Cu1 178.1(10) . . . . ? C10 C9 N23 C7 -161.8(14) . . . . ? C10 C9 N23 Cu1 16.6(18) . . . . ? O31 Cu1 N23 C7 33.5(12) . . . . ? O11 Cu1 N23 C7 71(3) . . . . ? N19 Cu1 N23 C7 -158.2(12) . . . . ? O51 Cu1 N23 C7 -62.7(12) . . . . ? U1 Cu1 N23 C7 57.9(13) . . . . ? O31 Cu1 N23 C9 -144.8(11) . . . . ? O11 Cu1 N23 C9 -107(2) . . . . ? N19 Cu1 N23 C9 23.5(12) . . . . ? O51 Cu1 N23 C9 119.0(11) . . . . ? U1 Cu1 N23 C9 -120.4(10) . . . . ? C4 C3 C2 C1 5(2) . . . . ? O31 C1 C2 C3 177.9(14) . . . . ? C6 C1 C2 C3 -5(2) . . . . ? N19 C11 C10 C9 67(2) . . . . ? N23 C9 C10 C11 -72(2) . . . . ? C17 C16 C15 C14 0(3) . . . . ? O11 C19 C18 C17 179.1(14) . . . . ? C14 C19 C18 C17 0(2) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? C4 C5 C6 C7 178.1(14) . . . . ? O31 C1 C6 C5 179.9(13) . . . . ? C2 C1 C6 C5 3(2) . . . . ? O31 C1 C6 C7 1(2) . . . . ? C2 C1 C6 C7 -175.6(14) . . . . ? N23 C7 C6 C5 157.3(15) . . . . ? C8 C7 C6 C5 -23(2) . . . . ? N23 C7 C6 C1 -24(2) . . . . ? C8 C7 C6 C1 155.4(13) . . . . ? C16 C15 C14 C19 3(3) . . . . ? C16 C15 C14 C13 -175.5(16) . . . . ? O11 C19 C14 C15 178.1(14) . . . . ? C18 C19 C14 C15 -3(2) . . . . ? O11 C19 C14 C13 -4(2) . . . . ? C18 C19 C14 C13 175.5(14) . . . . ? N19 C13 C14 C15 -152.3(16) . . . . ? C12 C13 C14 C15 24(2) . . . . ? N19 C13 C14 C19 30(2) . . . . ? C12 C13 C14 C19 -154.4(15) . . . . ? C15 C16 C17 C18 -3(3) . . . . ? C19 C18 C17 C16 3(3) . . . . ? Cu1 O51 C20 C22 -7(3) . . . . ? Cu1 O51 C20 C21 172.9(15) . . . . ? # END of CIF