# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1994 #============================================================================== data_global #============================================================================== _audit_creation_date 14-12-98 _audit_creation_method from_MolEN_master_file_using_cif_in _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; Ulli Englert Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; _publ_contact_author_email 'ullrich.englert@ac.rwth-aachen.de' _publ_contact_author_fax '(0241) 8888288' _publ_contact_author_phone '(0241) 804666' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ?edit? ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synproportionation Reactions between Copper(II) Trihaloacetates Cu(CX3COO)2 , X = F, Cl, Br, and Copper in the Presence of Carbon Monoxide ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Calderazzo, Fausto' #<--'Last name, first name' ; Dipartimento di Chimica e Chimica Industriale Universit^ di Pisa Via Risorgimento 35 56126 Pisa Italy ; 'Della Pina, Fabrizio' #<--'Last name, first name' ; Dipartimento di Chimica e Chimica Industriale Universit^ di Pisa Via Risorgimento 35 56126 Pisa Italy ; 'Englert, Ulli' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'Pampaloni, Guido' #<--'Last name, first name' ; Dipartimento di Chimica e Chimica Industriale Universit^ di Pisa Via Risorgimento 35 56126 Pisa Italy ; 'Belli Dell'Amico, Daniela' #<--'Last name, first name' ; Dipartimento di Chimica e Chimica Industriale Universit^ di Pisa Via Risorgimento 35 56126 Pisa Italy; ; 'Passarelli, Vincenzo' #<--'Last name, first name' ; Dipartimento di Chimica e Chimica Industriale Universit^ di Pisa Via Risorgimento 35 56126 Pisa Italy; ; 'Alessio, Rocco' #<--'Last name, first name' ; Dipartimento di Chimica e Chimica Industriale Universit^ di Pisa Via Risorgimento 35 56126 Pisa Italy; ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; Backgrounds were obtained from analysis of the scan profile (Blessing, Coppens _& Becker, 1974) ; _publ_section_references ; Blessing, R.H., Coppens, P. & Becker, P. (1974). J. Appl. Cryst., 7, 488-492. Enraf-Nonius, CAD4 Operations Manual, Delft, 1977. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. International Tables for X-Ray Crystallography, T. Hahn E Vol. A, D. Reidel Publ. Comp., Dordrecht, (1983) Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ?none? ?none? ; data_GP31_12119 # 5. CRYSTAL DATA _chemical_compound_source 'see paper' _exptl_crystal_description rod _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _chemical_name_common ; polynuclear carbonyl derivative Cu4(CCl3COO)6(CHCl2COOH)(CO)2 ; _chemical_formula_sum 'C16 H2 Cl20 Cu4 O16' _chemical_formula_weight 1413.40 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_h-m 'P212121 ' _cell_length_a 11.695(4) _cell_length_b 17.567(7) _cell_length_c 22.437(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4610(3) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 13 _cell_formula_units_z 4.00 _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.038 _cell_measurement_temperature 203 _exptl_crystal_F_000 2728 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.494 _exptl_absorpt_correction_T_max 0.583 _diffrn_reflns_number 8809 _reflns_number_total 8076 _reflns_number_observed 4957 _reflns_observed_criterion >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -46.4 # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 7. REFINEMENT DATA _refine_ls_abs_structure_details ; inversion twin ; _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1633P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_abs_structure_Flack 0.39(4) _refine_ls_number_reflns 8071 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_obs 0.0910 _refine_ls_wR_factor_all 0.2706 _refine_ls_wR_factor_obs 0.2259 _refine_ls_goodness_of_fit_all 1.024 _refine_ls_goodness_of_fit_obs 1.116 _refine_ls_restrained_S_all 1.041 _refine_ls_restrained_S_obs 1.116 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.7279(2) 0.45393(11) 0.18073(9) 0.0523(6) Uani 1 d . . Cu2 Cu 0.7731(2) 0.56722(12) 0.29166(9) 0.0548(6) Uani 1 d . . Cu3 Cu 0.7891(2) 0.52419(8) 0.06305(8) 0.0361(4) Uani 1 d . . Cu4 Cu 0.7887(2) 0.50821(9) -0.09009(8) 0.0435(5) Uani 1 d . . Cl15 Cl 0.7141(5) 0.7290(2) 0.2492(2) 0.0658(12) Uani 1 d . . Cl16 Cl 0.7205(7) 0.7746(2) 0.1291(3) 0.089(2) Uani 1 d . . Cl17 Cl 0.9262(5) 0.7261(3) 0.1874(3) 0.091(2) Uani 1 d . . Cl25 Cl 0.7110(6) 0.7082(2) -0.2774(2) 0.084(2) Uani 1 d . . Cl26 Cl 0.7396(6) 0.7566(3) -0.1593(3) 0.092(2) Uani 1 d . . Cl27 Cl 0.9325(5) 0.6965(3) -0.2221(3) 0.085(2) Uani 1 d . . Cl35 Cl 0.4192(4) 0.4258(3) -0.0155(3) 0.080(2) Uani 1 d . . Cl36 Cl 0.3983(5) 0.5644(3) 0.0522(3) 0.092(2) Uani 1 d . . Cl37 Cl 0.4022(6) 0.5695(4) -0.0763(3) 0.101(2) Uani 1 d . . Cl45 Cl 1.1528(6) 0.5358(4) -0.1922(4) 0.129(3) Uani 1 d . . Cl46 Cl 1.1537(9) 0.4006(8) -0.1251(8) 0.229(8) Uani 1 d . . Cl47 Cl 1.1100(8) 0.3961(6) -0.2489(5) 0.175(5) Uani 1 d . . Cl55 Cl 1.1478(8) 0.5392(5) 0.1734(5) 0.156(4) Uani 1 d . . Cl56 Cl 1.1131(8) 0.3817(7) 0.1960(8) 0.256(9) Uani 1 d . . Cl57 Cl 1.1602(8) 0.4347(6) 0.0804(7) 0.188(6) Uani 1 d . . Cl65 Cl 0.8801(11) 0.2696(4) 0.0598(4) 0.151(4) Uani 1 d . . Cl66 Cl 0.6665(7) 0.2665(4) 0.0099(8) 0.190(6) Uani 1 d . . Cl67 Cl 0.8656(9) 0.2512(4) -0.0637(4) 0.135(3) Uani 1 d . . Cl75 Cl 1.1444(8) 0.6743(7) 0.0333(5) 0.158(4) Uani 1 d . . Cl76 Cl 0.9558(11) 0.7574(5) -0.0085(7) 0.182(5) Uani 1 d . . O1 O 0.5088(23) 0.4039(14) 0.1345(11) 0.161(12) Uani 1 d . . O2 O 0.9860(23) 0.6202(20) 0.3457(11) 0.208(17) Uani 1 d . . O11 O 0.7541(9) 0.5776(5) 0.1994(5) 0.041(3) Uani 1 d . . O13 O 0.7705(10) 0.6185(5) 0.1046(4) 0.042(3) Uani 1 d . . O21 O 0.7562(10) 0.5563(6) -0.2248(5) 0.054(3) Uani 1 d . . O23 O 0.7644(11) 0.6010(5) -0.1338(5) 0.054(3) Uani 1 d . . O31 O 0.6350(9) 0.5356(7) 0.0346(5) 0.050(3) Uani 1 d . . O33 O 0.6331(11) 0.5145(9) -0.0629(7) 0.077(4) Uani 1 d . . O41 O 0.8971(12) 0.4192(7) -0.1963(6) 0.069(4) Uani 1 d . . O43 O 0.9399(10) 0.4996(6) -0.1279(6) 0.057(3) Uani 1 d . . O51 O 0.8953(11) 0.4393(7) 0.1683(6) 0.060(3) Uani 1 d . . O53 O 0.9413(9) 0.5118(6) 0.0937(5) 0.048(3) Uani 1 d . . O61 O 0.7936(12) 0.4186(5) 0.0379(5) 0.057(3) Uani 1 d . . O63 O 0.8060(12) 0.4064(5) -0.0601(5) 0.058(3) Uani 1 d . . O71 O 0.8780(9) 0.5767(6) -0.0168(5) 0.045(2) Uani 1 d . . O73 O 1.0406(16) 0.6080(9) -0.0667(8) 0.104(6) Uani 1 d . . H73 H 1.0200(16) 0.5700(9) -0.0913(8) 0.135 Uiso 1 calc R . C1 C 0.5952(19) 0.4273(11) 0.1497(10) 0.070(6) Uani 1 d . . C2 C 0.9071(26) 0.5937(15) 0.3264(10) 0.096(9) Uani 1 d . . C12 C 0.7668(14) 0.6275(7) 0.1596(7) 0.039(4) Uani 1 d . . C14 C 0.7847(18) 0.7103(8) 0.1807(7) 0.054(4) Uani 1 d . . C22 C 0.7597(11) 0.6075(7) -0.1900(6) 0.031(3) Uani 1 d . . C24 C 0.7825(16) 0.6916(9) -0.2096(8) 0.056(4) Uani 1 d . . C32 C 0.5883(11) 0.5259(8) -0.0121(9) 0.041(3) Uani 1 d . . C34 C 0.4579(14) 0.5232(8) -0.0136(9) 0.055(4) Uani 1 d . . C42 C 0.9585(16) 0.4551(8) -0.1688(6) 0.044(4) Uani 1 d . . C44 C 1.0903(20) 0.4457(13) -0.1825(15) 0.108(11) Uani 1 d . . C52 C 0.9623(13) 0.4706(9) 0.1366(8) 0.043(4) Uani 1 d . . C54 C 1.0947(26) 0.4553(13) 0.1500(13) 0.115(11) Uani 1 d . . C62 C 0.8047(11) 0.3820(7) -0.0087(7) 0.037(3) Uani 1 d . . C64 C 0.8075(16) 0.2960(9) -0.0014(8) 0.058(5) Uani 1 d . . C72 C 0.9637(21) 0.6143(11) -0.0226(9) 0.071(6) Uani 1 d . . C74 C 0.9959(18) 0.6754(10) 0.0174(11) 0.073(5) Uani 1 d . . H74 H 0.9555(18) 0.6672(10) 0.0552(11) 0.095 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0615(14) 0.0569(11) 0.0385(11) -0.0022(8) 0.0020(10) -0.0124(10) Cu2 0.0634(15) 0.0594(11) 0.0417(12) -0.0025(8) -0.0007(11) -0.0138(11) Cu3 0.0438(11) 0.0311(7) 0.0334(9) -0.0001(6) -0.0028(8) -0.0060(8) Cu4 0.0532(12) 0.0445(9) 0.0330(10) -0.0007(7) 0.0061(9) -0.0131(9) Cl15 0.092(3) 0.041(2) 0.064(3) -0.015(2) 0.019(3) 0.002(2) Cl16 0.151(6) 0.035(2) 0.082(3) 0.009(2) 0.011(4) 0.016(3) Cl17 0.073(4) 0.069(3) 0.131(5) -0.038(3) 0.005(4) -0.029(3) Cl25 0.129(5) 0.049(2) 0.073(3) 0.011(2) -0.033(4) -0.005(3) Cl26 0.138(6) 0.048(2) 0.090(4) -0.012(2) 0.013(4) 0.008(3) Cl27 0.062(3) 0.071(3) 0.124(5) 0.014(3) 0.015(3) -0.012(3) Cl35 0.057(3) 0.056(2) 0.128(5) 0.005(3) 0.001(3) -0.021(2) Cl36 0.060(3) 0.091(4) 0.125(5) -0.007(3) 0.027(3) 0.014(3) Cl37 0.086(4) 0.102(4) 0.114(5) 0.026(4) -0.039(4) 0.023(3) Cl45 0.098(5) 0.099(5) 0.189(8) -0.063(5) 0.068(5) -0.045(4) Cl46 0.096(7) 0.244(14) 0.347(20) 0.124(14) -0.032(10) 0.055(8) Cl47 0.131(7) 0.161(8) 0.235(11) -0.135(8) 0.092(8) -0.062(6) Cl55 0.127(7) 0.117(6) 0.223(11) 0.000(6) -0.108(7) -0.030(5) Cl56 0.100(7) 0.222(11) 0.447(22) 0.249(14) -0.058(10) 0.012(7) Cl57 0.091(7) 0.159(8) 0.312(16) -0.004(10) 0.084(8) 0.036(6) Cl65 0.276(12) 0.073(4) 0.103(5) 0.013(4) -0.025(7) 0.071(6) Cl66 0.120(6) 0.064(4) 0.385(18) -0.001(7) 0.057(9) -0.033(4) Cl67 0.231(10) 0.065(3) 0.109(5) -0.025(4) 0.013(6) 0.051(5) Cl75 0.098(6) 0.202(10) 0.175(10) -0.071(8) -0.020(6) -0.033(6) Cl76 0.235(11) 0.069(4) 0.241(13) -0.029(6) -0.009(10) 0.036(6) O1 0.155(21) 0.169(21) 0.159(22) 0.071(17) -0.088(18) -0.087(18) O2 0.156(22) 0.328(39) 0.139(21) 0.081(23) -0.107(19) -0.152(26) O11 0.049(7) 0.031(4) 0.043(6) -0.004(4) 0.000(5) -0.001(4) O13 0.059(7) 0.035(5) 0.033(6) 0.003(4) 0.004(5) -0.002(5) O21 0.069(9) 0.056(6) 0.037(6) -0.011(5) 0.002(6) -0.020(6) O23 0.070(9) 0.037(5) 0.057(8) 0.006(5) -0.006(6) 0.003(5) O31 0.040(6) 0.067(7) 0.042(7) -0.014(5) -0.004(5) -0.005(5) O33 0.052(8) 0.114(11) 0.066(9) -0.019(8) 0.003(7) -0.024(8) O41 0.072(9) 0.064(8) 0.071(9) -0.024(7) -0.025(8) -0.007(7) O43 0.060(8) 0.048(6) 0.063(8) -0.010(6) 0.011(6) -0.003(5) O51 0.049(8) 0.063(7) 0.070(9) 0.017(6) -0.004(7) 0.004(6) O53 0.038(6) 0.046(6) 0.061(7) 0.015(5) -0.005(5) -0.012(5) O61 0.092(9) 0.025(4) 0.055(7) -0.003(5) 0.007(7) 0.000(6) O63 0.100(11) 0.032(5) 0.042(7) -0.006(5) -0.002(7) -0.008(6) O71 0.045(6) 0.053(6) 0.038(6) 0.010(5) -0.008(5) -0.021(5) O73 0.130(16) 0.100(11) 0.082(12) -0.020(9) 0.023(11) -0.059(11) C1 0.072(14) 0.054(10) 0.083(15) 0.018(10) -0.027(12) -0.017(10) C2 0.117(23) 0.113(20) 0.057(15) 0.025(12) -0.006(14) -0.045(17) C12 0.044(9) 0.026(6) 0.047(9) 0.011(6) -0.001(7) -0.002(6) C14 0.083(13) 0.036(7) 0.043(9) 0.005(6) -0.015(10) -0.015(8) C22 0.019(7) 0.044(7) 0.029(8) 0.001(6) -0.002(6) -0.004(5) C24 0.048(10) 0.049(8) 0.071(12) 0.020(8) 0.004(10) -0.008(8) C32 0.025(7) 0.040(7) 0.056(10) 0.002(7) 0.009(8) 0.002(6) C34 0.057(10) 0.032(7) 0.075(11) 0.008(7) -0.037(10) 0.002(7) C42 0.070(12) 0.032(7) 0.029(8) -0.007(6) -0.010(8) -0.002(7) C44 0.059(14) 0.081(15) 0.184(30) -0.044(17) 0.053(17) -0.013(12) C52 0.033(9) 0.042(8) 0.053(11) -0.002(8) -0.005(7) 0.000(7) C54 0.141(26) 0.077(15) 0.128(22) 0.080(16) 0.002(19) 0.028(15) C62 0.030(7) 0.032(6) 0.049(9) 0.003(7) -0.003(7) -0.008(5) C64 0.066(11) 0.043(8) 0.064(14) 0.007(7) 0.010(9) -0.003(8) C72 0.114(18) 0.054(10) 0.045(12) 0.013(8) 0.015(12) -0.008(11) C74 0.091(15) 0.058(11) 0.071(13) 0.000(10) 0.001(13) -0.033(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 Cu1 C1 1.77(2) . ? Cu1 O51 1.998(13) . ? Cu1 O21 2.131(11) 2_665 ? Cu1 O11 2.231(9) . ? Cu1 Cu3 2.997(3) . ? Cu2 C2 1.81(3) . ? Cu2 O41 2.026(14) 2_665 ? Cu2 O11 2.087(10) . ? Cu2 O21 2.226(11) 2_665 ? Cu2 Cu4 3.048(3) 2_665 ? Cu3 O13 1.912(9) . ? Cu3 O53 1.924(11) . ? Cu3 O31 1.925(11) . ? Cu3 O61 1.938(9) . ? Cu3 O71 2.267(11) . ? Cu4 O63 1.920(10) . ? Cu4 O23 1.922(10) . ? Cu4 O33 1.926(14) . ? Cu4 O43 1.969(12) . ? Cu4 O71 2.287(11) . ? Cu4 Cu2 3.048(3) 2_664 ? Cl15 C14 1.78(2) . ? Cl16 C14 1.78(2) . ? Cl17 C14 1.69(2) . ? Cl25 C24 1.76(2) . ? Cl26 C24 1.68(2) . ? Cl27 C24 1.78(2) . ? Cl35 C34 1.769(15) . ? Cl36 C34 1.78(2) . ? Cl37 C34 1.75(2) . ? Cl45 C44 1.76(2) . ? Cl46 C44 1.68(4) . ? Cl47 C44 1.74(3) . ? Cl55 C54 1.68(3) . ? Cl56 C54 1.67(2) . ? Cl57 C54 1.77(3) . ? Cl65 C64 1.68(2) . ? Cl66 C64 1.75(2) . ? Cl67 C64 1.74(2) . ? Cl75 C74 1.78(2) . ? Cl76 C74 1.62(2) . ? O1 C1 1.14(3) . ? O2 C2 1.12(3) . ? O11 C12 1.26(2) . ? O13 C12 1.24(2) . ? O21 C22 1.19(2) . ? O21 Cu1 2.131(11) 2_664 ? O21 Cu2 2.226(11) 2_664 ? O23 C22 1.26(2) . ? O31 C32 1.19(2) . ? O33 C32 1.27(2) . ? O41 C42 1.14(2) . ? O41 Cu2 2.026(14) 2_664 ? O43 C42 1.22(2) . ? O51 C52 1.19(2) . ? O53 C52 1.23(2) . ? O61 C62 1.23(2) . ? O63 C62 1.23(2) . ? O71 C72 1.21(2) . ? O73 C72 1.34(3) . ? C12 C14 1.54(2) . ? C22 C24 1.56(2) . ? C32 C34 1.53(2) . ? C42 C44 1.58(3) . ? C52 C54 1.60(3) . ? C62 C64 1.52(2) . ? C72 C74 1.45(3) . ? 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 C1 Cu1 O51 140.8(9) . . ? C1 Cu1 O21 116.5(8) . 2_665 ? O51 Cu1 O21 92.4(5) . 2_665 ? C1 Cu1 O11 116.9(7) . . ? O51 Cu1 O11 90.9(4) . . ? O21 Cu1 O11 83.4(4) 2_665 . ? C1 Cu1 Cu3 88.5(7) . . ? O51 Cu1 Cu3 72.3(4) . . ? O21 Cu1 Cu3 152.5(3) 2_665 . ? O11 Cu1 Cu3 74.4(3) . . ? C2 Cu2 O41 139.9(10) . 2_665 ? C2 Cu2 O11 119.6(8) . . ? O41 Cu2 O11 91.0(5) 2_665 . ? C2 Cu2 O21 117.0(10) . 2_665 ? O41 Cu2 O21 89.2(5) 2_665 2_665 ? O11 Cu2 O21 84.5(4) . 2_665 ? C2 Cu2 Cu4 86.8(7) . 2_665 ? O41 Cu2 Cu4 72.6(4) 2_665 2_665 ? O11 Cu2 Cu4 150.8(3) . 2_665 ? O21 Cu2 Cu4 71.6(3) 2_665 2_665 ? O13 Cu3 O53 91.7(5) . . ? O13 Cu3 O31 87.9(5) . . ? O53 Cu3 O31 178.3(5) . . ? O13 Cu3 O61 166.6(5) . . ? O53 Cu3 O61 88.3(5) . . ? O31 Cu3 O61 91.6(5) . . ? O13 Cu3 O71 94.9(4) . . ? O53 Cu3 O71 84.3(4) . . ? O31 Cu3 O71 97.4(4) . . ? O61 Cu3 O71 98.4(4) . . ? O13 Cu3 Cu1 84.3(3) . . ? O53 Cu3 Cu1 82.0(3) . . ? O31 Cu3 Cu1 96.3(4) . . ? O61 Cu3 Cu1 82.5(3) . . ? O71 Cu3 Cu1 166.3(3) . . ? O63 Cu4 O23 169.4(5) . . ? O63 Cu4 O33 92.5(6) . . ? O23 Cu4 O33 88.4(6) . . ? O63 Cu4 O43 89.1(5) . . ? O23 Cu4 O43 88.8(5) . . ? O33 Cu4 O43 172.8(6) . . ? O63 Cu4 O71 101.0(4) . . ? O23 Cu4 O71 89.3(4) . . ? O33 Cu4 O71 100.2(5) . . ? O43 Cu4 O71 86.4(4) . . ? O63 Cu4 Cu2 85.7(3) . 2_664 ? O23 Cu4 Cu2 83.7(4) . 2_664 ? O33 Cu4 Cu2 94.3(4) . 2_664 ? O43 Cu4 Cu2 78.9(4) . 2_664 ? O71 Cu4 Cu2 163.8(3) . 2_664 ? C12 O11 Cu2 138.5(9) . . ? C12 O11 Cu1 124.2(9) . . ? Cu2 O11 Cu1 96.6(4) . . ? C12 O13 Cu3 126.6(8) . . ? C22 O21 Cu1 135.3(10) . 2_664 ? C22 O21 Cu2 129.1(10) . 2_664 ? Cu1 O21 Cu2 95.5(4) 2_664 2_664 ? C22 O23 Cu4 126.1(9) . . ? C32 O31 Cu3 134.9(10) . . ? C32 O33 Cu4 133.2(12) . . ? C42 O41 Cu2 129.0(13) . 2_664 ? C42 O43 Cu4 122.1(12) . . ? C52 O51 Cu1 132.1(11) . . ? C52 O53 Cu3 122.1(10) . . ? C62 O61 Cu3 138.4(10) . . ? C62 O63 Cu4 130.6(9) . . ? C72 O71 Cu3 133.5(12) . . ? C72 O71 Cu4 126.2(12) . . ? Cu3 O71 Cu4 98.2(4) . . ? O1 C1 Cu1 172.3(20) . . ? O2 C2 Cu2 170.3(30) . . ? O13 C12 O11 128.1(13) . . ? O13 C12 C14 114.7(11) . . ? O11 C12 C14 117.1(13) . . ? C12 C14 Cl17 108.4(13) . . ? C12 C14 Cl15 112.1(11) . . ? Cl17 C14 Cl15 110.4(10) . . ? C12 C14 Cl16 110.0(11) . . ? Cl17 C14 Cl16 111.6(10) . . ? Cl15 C14 Cl16 104.3(10) . . ? O21 C22 O23 125.9(13) . . ? O21 C22 C24 122.3(14) . . ? O23 C22 C24 111.0(12) . . ? C22 C24 Cl26 113.7(12) . . ? C22 C24 Cl25 108.6(12) . . ? Cl26 C24 Cl25 108.9(10) . . ? C22 C24 Cl27 105.0(11) . . ? Cl26 C24 Cl27 111.6(11) . . ? Cl25 C24 Cl27 109.0(10) . . ? O31 C32 O33 128.3(13) . . ? O31 C32 C34 118.8(15) . . ? O33 C32 C34 112.9(16) . . ? C32 C34 Cl37 112.0(14) . . ? C32 C34 Cl35 106.7(10) . . ? Cl37 C34 Cl35 109.5(9) . . ? C32 C34 Cl36 111.1(12) . . ? Cl37 C34 Cl36 109.2(9) . . ? Cl35 C34 Cl36 108.2(11) . . ? O41 C42 O43 130.2(19) . . ? O41 C42 C44 117.1(17) . . ? O43 C42 C44 112.7(16) . . ? C42 C44 Cl46 109.4(19) . . ? C42 C44 Cl47 110.3(18) . . ? Cl46 C44 Cl47 111.1(16) . . ? C42 C44 Cl45 109.6(15) . . ? Cl46 C44 Cl45 109.5(17) . . ? Cl47 C44 Cl45 106.8(16) . . ? O51 C52 O53 127.3(15) . . ? O51 C52 C54 116.7(15) . . ? O53 C52 C54 116.0(15) . . ? C52 C54 Cl56 111.7(17) . . ? C52 C54 Cl55 105.6(15) . . ? Cl56 C54 Cl55 116.0(20) . . ? C52 C54 Cl57 106.7(18) . . ? Cl56 C54 Cl57 109.2(16) . . ? Cl55 C54 Cl57 107.0(15) . . ? O63 C62 O61 127.8(12) . . ? O63 C62 C64 116.5(13) . . ? O61 C62 C64 115.4(14) . . ? C62 C64 Cl65 111.9(12) . . ? C62 C64 Cl67 111.8(12) . . ? Cl65 C64 Cl67 109.3(11) . . ? C62 C64 Cl66 106.9(12) . . ? Cl65 C64 Cl66 106.1(11) . . ? Cl67 C64 Cl66 110.6(11) . . ? O71 C72 O73 126.2(19) . . ? O71 C72 C74 123.8(20) . . ? O73 C72 C74 110.0(19) . . ? C72 C74 Cl76 111.1(17) . . ? C72 C74 Cl75 111.8(17) . . ? Cl76 C74 Cl75 111.4(11) . . ? _refine_diff_density_max 2.082 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.219 #===END data_GP32_22119 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description platelet _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _chemical_name_common ; chloroacetato derivative Cu2(CCl3COO)4(CCl3COOH)2 ; _chemical_formula_sum 'C12 H2 Cl18 Cu2 O12' _chemical_formula_weight 1103.38 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P-1' _cell_length_a 9.354(4) _cell_length_b 9.650(1) _cell_length_c 10.875(5) _cell_angle_alpha 79.00(2) _cell_angle_beta 67.62(3) _cell_angle_gamma 73.08(2) _cell_volume 864.9(6) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 12 _cell_formula_units_z 1.00 _exptl_crystal_density_diffrn 2.12 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.687 _cell_measurement_temperature 203 _exptl_crystal_F_000 534 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 6832 _reflns_number_total 3384 _reflns_number_observed 2748 _reflns_observed_criterion >1.0\s(I) _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 45.0 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0.00 # 7. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_obs 0.069 _refine_ls_wR_factor_obs 0.075 _refine_ls_hydrogen_treatment riding _refine_ls_number_reflns 2748 _refine_ls_number_parameters 215 _refine_ls_number_restraints 4 _refine_ls_goodness_of_fit_obs 1.952 _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_shift/esd_max 0.022 _refine_diff_density_max 1.7142 _refine_diff_density_min -0.7309 _refine_ls_extinction_method none _atom_type_scat_source International_Tables_for_Xray_Crystallography # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution none _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Cu 0.39675(9) 0.43902(8) 0.10041(7) 0.0222(2) Ueq O11 0.3877(5) 0.6027(5) 0.1929(4) 0.031(1) Ueq C12 0.4623(7) 0.6985(7) 0.1369(6) 0.024(2) Ueq O13 0.5595(5) 0.7051(5) 0.0209(4) 0.030(1) Ueq C14 0.4234(8) 0.8277(7) 0.2199(6) 0.032(2) Ueq Cl15 0.5767(2) 0.9184(2) 0.1621(2) 0.0597(6) Ueq Cl16 0.3903(2) 0.7625(2) 0.3890(2) 0.0532(6) Ueq Cl17 0.2489(3) 0.9446(2) 0.2012(2) 0.0622(8) Ueq O21 0.5867(5) 0.3332(5) 0.1439(4) 0.035(1) Ueq C22 0.7227(7) 0.3566(7) 0.0766(6) 0.029(2) Ueq O23 0.2370(5) 0.5637(5) 0.0281(4) 0.034(1) Ueq C24 0.847(1) 0.288(1) 0.1423(8) 0.037(3) Ueq Cl25 0.8174(3) 0.1266(3) 0.2395(3) 0.0739(9) Ueq Cl26 1.0412(3) 0.2725(4) 0.0301(3) 0.073(1) Ueq Cl27 0.8140(4) 0.4136(4) 0.2584(3) 0.087(1) Ueq O31 0.2437(5) 0.3525(5) 0.2832(4) 0.031(1) Ueq C32 0.2256(8) 0.3652(7) 0.3964(7) 0.033(2) Ueq O33 0.2608(7) 0.4640(6) 0.4384(5) 0.056(2) Ueq C34 0.1645(7) 0.2527(7) 0.5088(6) 0.029(2) Ueq Cl35 0.0377(2) 0.1789(2) 0.4734(2) 0.0605(6) Ueq Cl36 0.0673(3) 0.3217(3) 0.6651(2) 0.0623(8) Ueq Cl37 0.3362(3) 0.1172(3) 0.5101(3) 0.0763(9) Ueq H 0.2808 0.5405 0.3783 0.0507 Uiso C24a 0.870(5) 0.233(5) 0.112(4) 0.05(1) Uiso Cl25a 0.793(3) 0.231(3) 0.291(3) 0.155(9) Uiso Cl26a 1.000(1) 0.344(1) 0.101(1) 0.062(3) Uiso Cl27a 0.948(2) 0.104(1) 0.016(1) 0.070(4) Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu 0.0216(3) 0.0268(3) 0.0164(3) -0.0078(2) -0.0044(2) 0.0006(3) O11 0.039(2) 0.033(2) 0.026(2) -0.019(2) -0.009(2) -0.000(2) C12 0.024(3) 0.025(3) 0.025(3) -0.006(2) -0.011(2) -0.001(2) O13 0.033(2) 0.032(2) 0.024(2) -0.012(2) -0.002(2) -0.006(2) C14 0.038(3) 0.037(3) 0.024(3) -0.018(2) -0.006(2) -0.001(3) Cl15 0.073(1) 0.0679(9) 0.048(1) -0.0511(7) -0.0009(8) -0.0153(8) Cl16 0.085(1) 0.060(1) 0.0268(7) -0.0433(7) -0.0145(7) -0.0033(7) Cl17 0.054(1) 0.043(1) 0.062(1) 0.008(1) -0.004(1) -0.007(1) O21 0.029(2) 0.043(3) 0.031(2) -0.010(2) -0.014(2) 0.008(2) C22 0.030(3) 0.030(3) 0.028(3) -0.005(2) -0.015(2) -0.001(2) O23 0.029(2) 0.040(3) 0.032(2) -0.007(2) -0.016(2) 0.005(2) C24 0.041(4) 0.033(4) 0.042(4) -0.012(3) -0.027(3) 0.015(4) Cl25 0.054(1) 0.057(1) 0.108(2) -0.023(1) -0.047(1) 0.053(1) Cl26 0.027(1) 0.097(2) 0.072(2) -0.003(1) -0.017(1) 0.025(2) Cl27 0.107(2) 0.100(2) 0.084(1) -0.018(1) -0.065(1) -0.021(1) O31 0.034(2) 0.038(2) 0.021(2) -0.018(2) -0.003(2) -0.000(2) C32 0.033(3) 0.033(3) 0.032(3) -0.010(3) -0.009(2) -0.001(3) O33 0.097(3) 0.051(3) 0.031(2) -0.049(2) -0.015(2) 0.003(2) C34 0.030(3) 0.029(3) 0.029(3) -0.012(2) -0.010(2) 0.000(3) Cl35 0.0667(9) 0.086(1) 0.044(1) -0.0565(7) -0.0125(7) 0.0062(9) Cl36 0.084(1) 0.067(1) 0.0264(9) -0.028(1) 0.0011(9) -0.0090(8) Cl37 0.058(1) 0.056(1) 0.095(2) 0.005(1) -0.031(1) 0.019(1) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cu Cu 2.648(1) ? Cu O11 1.995(3) ? Cu O13 1.949(3) ? Cu O21 1.956(3) ? Cu O23 1.945(3) ? Cu O31 2.143(3) ? O11 C12 1.244(5) ? C12 O13 1.245(5) ? C12 C14 1.555(7) ? C14 Cl15 1.747(5) ? C14 Cl16 1.764(5) ? C14 Cl17 1.754(6) ? O21 C22 1.265(6) ? C22 O23 1.240(6) ? C22 C24 1.522(9) ? C24 Cl25 1.739(8) ? C24 Cl26 1.738(9) ? C24 Cl27 1.79(1) ? O31 C32 1.202(6) ? C32 O33 1.300(6) ? C32 C34 1.524(7) ? O33 H 0.9000 ? C34 Cl35 1.734(5) ? C34 Cl36 1.750(5) ? C34 Cl37 1.754(5) ? C24a Cl25a 1.80(5) ? C24a Cl26a 1.80(4) ? C24a Cl27a 1.60(4) ? H O11 1.9440 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cu Cu O11 82.0(1) ? Cu Cu O13 85.9(1) ? Cu Cu O21 83.0(1) ? Cu Cu O23 85.6(1) ? Cu Cu O31 170.7(1) ? O11 Cu O13 167.9(1) ? O11 Cu O21 87.5(2) ? O11 Cu O23 90.5(2) ? O11 Cu O31 90.1(1) ? O13 Cu O21 90.1(2) ? O13 Cu O23 89.5(2) ? O13 Cu O31 101.8(1) ? O21 Cu O23 168.5(1) ? O21 Cu O31 91.8(1) ? O23 Cu O31 99.5(1) ? Cu O11 C12 123.4(3) ? O11 C12 O13 127.5(5) ? O11 C12 C14 115.8(4) ? O13 C12 C14 116.7(4) ? Cu O13 C12 121.1(3) ? C12 C14 Cl15 111.9(3) ? C12 C14 Cl16 109.4(3) ? C12 C14 Cl17 105.3(3) ? Cl15 C14 Cl16 109.5(3) ? Cl15 C14 Cl17 110.2(3) ? Cl16 C14 Cl17 110.5(3) ? Cu O21 C22 122.2(3) ? O21 C22 O23 128.8(5) ? O21 C22 C24 114.2(5) ? O23 C22 C24 116.8(5) ? Cu O23 C22 120.2(3) ? C22 C24 Cl25 112.9(5) ? C22 C24 Cl26 112.8(5) ? C22 C24 Cl27 104.6(5) ? Cl25 C24 Cl26 113.0(5) ? Cl25 C24 Cl27 105.2(5) ? Cl26 C24 Cl27 107.5(5) ? Cu O31 C32 129.2(3) ? O31 C32 O33 127.4(5) ? O31 C32 C34 120.4(5) ? O33 C32 C34 112.1(4) ? C32 O33 H 114.49 ? C32 C34 Cl35 110.3(4) ? C32 C34 Cl36 113.4(4) ? C32 C34 Cl37 104.4(4) ? Cl35 C34 Cl36 109.4(3) ? Cl35 C34 Cl37 109.4(3) ? Cl36 C34 Cl37 109.7(3) ? Cl25a C24a Cl26a 90(2) ? Cl25a C24a Cl27a 132(3) ? Cl26a C24a Cl27a 115(3) ? #===END