Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chaudhuri, Nirmalendu Ray' 'Diaz, Carmen' 'Konar, Sanjit' 'Mukherjee, Partha Sarathi' 'Ribas, Joan' 'Zangrando, Enniop' _publ_contact_author_name 'Prof Nirmalendu Ray Chaudhuri' _publ_contact_author_address ; Prof Nirmalendu Ray Chaudhuri Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICNRC@MAHENDRA.IACS.RES.IN' _publ_section_title ; Synthesis, crystal structure and magneto-structural correlation of two bi-bridging 1D copper(II) chains ; data_complex-1 _database_code_CSD 185893 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-oxalate-bis[1-(aminoethyl)pyrrolidine-copper(II)]- 0.5(squarate) perchlorate hydrated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C2 O4 2-) 2(C6 H14 N2 Cu 2+) 0.5(C4 O4 2-) (Cl O4 1-) 0.25(O H2)' _chemical_formula_sum 'C16 H28.50 Cl Cu2 N4 O10.25' _chemical_formula_weight 603.46 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' 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.081(3) _cell_length_b 13.402(4) _cell_length_c 16.185(5) _cell_angle_alpha 65.85(3) _cell_angle_beta 91.23(3) _cell_angle_gamma 82.25(3) _cell_volume 1188.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 619 _exptl_absorpt_coefficient_mu 1.961 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6659 _exptl_absorpt_correction_T_max 1.0512 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8216 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.97 _reflns_number_total 5046 _reflns_number_gt 3143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'Shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.02 (Farrugia, 1999)' _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^ > 2sigma(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. ; _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^)+(0.0878P)^2^+1.2165P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5046 _refine_ls_number_parameters 318 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1725 _refine_ls_wR_factor_gt 0.1581 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.002 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 Cu1 Cu 0.14818(11) 0.27985(6) 0.24859(5) 0.0416(3) Uani 1 1 d . . . Cu2 Cu 0.83638(11) 0.52884(6) 0.22336(5) 0.0421(3) Uani 1 1 d . . . O1 O 0.5386(6) 0.2616(3) 0.2631(3) 0.0520(11) Uani 1 1 d . . . O2 O 0.2044(6) 0.4280(3) 0.2413(3) 0.0436(10) Uani 1 1 d . . . O3 O 0.4548(7) 0.5401(3) 0.2249(3) 0.0526(11) Uani 1 1 d . . . O4 O 0.7868(6) 0.3752(3) 0.2454(3) 0.0441(10) Uani 1 1 d . . . O5 O 0.8268(7) 0.5721(4) 0.0919(3) 0.0509(11) Uani 1 1 d . . . O6 O 1.1486(7) 0.3354(3) 0.1162(3) 0.0473(10) Uani 1 1 d . . . N1 N 0.1567(9) 0.2108(4) 0.3845(4) 0.0497(13) Uani 1 1 d . . . H1A H 0.2650 0.2330 0.4085 0.060 Uiso 1 1 calc R . . H1B H 0.0257 0.2310 0.4025 0.060 Uiso 1 1 calc R . . N2 N 0.1003(8) 0.1277(4) 0.2566(4) 0.0456(12) Uani 1 1 d . . . N3 N 0.8714(9) 0.6873(4) 0.2073(4) 0.0532(13) Uani 1 1 d . . . N4 N 0.8817(10) 0.4897(5) 0.3571(4) 0.0586(15) Uani 1 1 d . . . H4A H 0.7688 0.4563 0.3855 0.070 Uiso 1 1 calc R . . H4B H 1.0093 0.4419 0.3805 0.070 Uiso 1 1 calc R . . C5 C 0.2007(12) 0.0895(6) 0.4147(5) 0.0596(18) Uani 1 1 d . . . H5A H 0.1643 0.0526 0.4770 0.072 Uiso 1 1 calc R . . H5B H 0.3567 0.0652 0.4115 0.072 Uiso 1 1 calc R . . C6 C 0.0566(13) 0.0630(6) 0.3522(5) 0.0612(19) Uani 1 1 d . . . H6A H 0.0883 -0.0155 0.3668 0.073 Uiso 1 1 calc R . . H6B H -0.0991 0.0810 0.3603 0.073 Uiso 1 1 calc R . . C2 C 0.4012(9) 0.4500(5) 0.2374(4) 0.0417(14) Uani 1 1 d . . . C1 C 0.5923(10) 0.3521(5) 0.2496(4) 0.0417(14) Uani 1 1 d . . . C7 C 0.9979(15) 0.6677(7) 0.2943(6) 0.078(2) Uani 1 1 d . . . H7A H 0.9964 0.7373 0.2996 0.093 Uiso 1 1 calc R . . H7B H 1.1515 0.6363 0.2948 0.093 Uiso 1 1 calc R . . C8 C 0.8916(16) 0.5893(7) 0.3728(5) 0.078(2) Uani 1 1 d . . . H8A H 0.9792 0.5705 0.4294 0.094 Uiso 1 1 calc R . . H8B H 0.7429 0.6233 0.3763 0.094 Uiso 1 1 calc R . . C3 C 0.9262(9) 0.5295(5) 0.0442(4) 0.0399(13) Uani 1 1 d . . . C4 C 1.0640(10) 0.4264(5) 0.0548(4) 0.0433(14) Uani 1 1 d . . . C9 C -0.0805(11) 0.1299(6) 0.1919(5) 0.0555(17) Uani 1 1 d . . . H9A H -0.0754 0.1887 0.1323 0.067 Uiso 1 1 calc R . . H9B H -0.2254 0.1411 0.2134 0.067 Uiso 1 1 calc R . . C10 C -0.0361(14) 0.0177(6) 0.1885(6) 0.073(2) Uani 1 1 d . . . H10A H -0.1094 -0.0356 0.2354 0.088 Uiso 1 1 calc R . . H10B H -0.0891 0.0227 0.1298 0.088 Uiso 1 1 calc R . . C11 C 0.2141(13) -0.0155(6) 0.2045(6) 0.070(2) Uani 1 1 d . . . H11A H 0.2773 -0.0149 0.1498 0.084 Uiso 1 1 calc R . . H11B H 0.2540 -0.0891 0.2530 0.084 Uiso 1 1 calc R . . C12 C 0.2973(11) 0.0715(6) 0.2309(5) 0.0585(18) Uani 1 1 d . . . H12A H 0.4104 0.0364 0.2816 0.070 Uiso 1 1 calc R . . H12B H 0.3608 0.1246 0.1801 0.070 Uiso 1 1 calc R . . C13 C 1.0002(13) 0.7496(6) 0.1309(6) 0.071(2) Uani 1 1 d . . . H13A H 1.1054 0.6991 0.1165 0.085 Uiso 1 1 calc R . . H13B H 1.0814 0.7979 0.1464 0.085 Uiso 1 1 calc R . . C14 C 0.8273(17) 0.8171(7) 0.0506(6) 0.085(3) Uani 1 1 d . . . H14A H 0.8414 0.7898 0.0036 0.102 Uiso 1 1 calc R . . H14B H 0.8442 0.8947 0.0248 0.102 Uiso 1 1 calc R . . C15 C 0.6011(15) 0.8012(9) 0.0914(7) 0.089(3) Uani 1 1 d . . . H15A H 0.5003 0.8710 0.0690 0.107 Uiso 1 1 calc R . . H15B H 0.5329 0.7488 0.0762 0.107 Uiso 1 1 calc R . . C16 C 0.6541(13) 0.7584(7) 0.1898(7) 0.072(2) Uani 1 1 d . . . H16A H 0.5421 0.7160 0.2226 0.087 Uiso 1 1 calc R . . H16B H 0.6628 0.8184 0.2079 0.087 Uiso 1 1 calc R . . O1W O 0.600(5) 0.341(3) 0.027(2) 0.110(9) Uiso 0.25 1 d P . . Cl Cl 0.5972(3) 0.25957(17) 0.52386(13) 0.0700(5) Uani 1 1 d D . . O7 O 0.4601(12) 0.3491(5) 0.4536(5) 0.115(2) Uani 1 1 d D A . O8 O 0.797(2) 0.2336(13) 0.4987(10) 0.216(12) Uani 0.707(18) 1 d PDU A 1 O9 O 0.479(2) 0.1704(9) 0.5557(11) 0.184(10) Uani 0.707(18) 1 d PDU A 1 O10 O 0.624(2) 0.2906(13) 0.5961(8) 0.168(8) Uani 0.707(18) 1 d PDU A 1 O8A O 0.651(3) 0.1809(15) 0.4847(14) 0.099(7) Uani 0.293(18) 1 d PDU A 2 O9A O 0.494(3) 0.2115(18) 0.5997(11) 0.099(7) Uani 0.293(18) 1 d PDU A 2 O10A O 0.799(3) 0.2876(16) 0.5399(15) 0.099(7) Uani 0.293(18) 1 d PDU A 2 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 0.0446(5) 0.0351(4) 0.0400(5) -0.0105(3) 0.0034(3) -0.0066(3) Cu2 0.0456(5) 0.0393(5) 0.0417(5) -0.0163(3) 0.0059(3) -0.0089(3) O1 0.040(2) 0.039(2) 0.076(3) -0.023(2) 0.001(2) -0.0043(18) O2 0.033(2) 0.041(2) 0.054(3) -0.018(2) 0.0037(17) -0.0059(17) O3 0.050(3) 0.037(2) 0.069(3) -0.021(2) 0.005(2) -0.0072(19) O4 0.029(2) 0.045(2) 0.057(3) -0.018(2) 0.0086(17) -0.0102(17) O5 0.063(3) 0.044(3) 0.040(2) -0.015(2) 0.006(2) 0.001(2) O6 0.056(3) 0.037(2) 0.041(2) -0.010(2) 0.0009(19) -0.0011(19) N1 0.048(3) 0.049(3) 0.048(3) -0.015(3) 0.002(2) -0.008(2) N2 0.042(3) 0.042(3) 0.049(3) -0.015(2) 0.009(2) -0.007(2) N3 0.058(3) 0.043(3) 0.060(4) -0.022(3) 0.006(3) -0.011(2) N4 0.064(4) 0.055(4) 0.058(4) -0.024(3) 0.008(3) -0.010(3) C5 0.071(5) 0.046(4) 0.047(4) -0.005(3) 0.005(3) -0.003(3) C6 0.079(5) 0.040(4) 0.055(4) -0.007(3) 0.012(4) -0.020(3) C2 0.038(3) 0.039(3) 0.043(3) -0.012(3) 0.008(2) -0.008(2) C1 0.044(4) 0.039(3) 0.038(3) -0.012(3) 0.004(2) -0.007(3) C7 0.090(6) 0.070(5) 0.085(6) -0.041(5) -0.008(5) -0.025(4) C8 0.116(7) 0.067(5) 0.049(5) -0.026(4) 0.001(4) -0.004(5) C3 0.041(3) 0.040(3) 0.036(3) -0.012(3) 0.005(2) -0.010(2) C4 0.046(3) 0.042(4) 0.038(3) -0.012(3) 0.001(3) -0.009(3) C9 0.058(4) 0.048(4) 0.062(5) -0.025(3) 0.004(3) -0.008(3) C10 0.094(6) 0.053(5) 0.088(6) -0.044(4) 0.005(5) -0.018(4) C11 0.080(5) 0.052(4) 0.078(6) -0.032(4) 0.009(4) -0.001(4) C12 0.060(4) 0.049(4) 0.062(5) -0.021(3) 0.009(3) -0.001(3) C13 0.061(5) 0.047(4) 0.106(7) -0.029(4) 0.026(4) -0.018(3) C14 0.137(8) 0.044(4) 0.060(5) -0.008(4) 0.020(5) -0.013(5) C15 0.084(6) 0.088(7) 0.089(7) -0.039(6) -0.007(5) 0.011(5) C16 0.065(5) 0.053(5) 0.098(7) -0.031(4) 0.011(4) -0.004(4) Cl 0.0805(13) 0.0704(13) 0.0514(11) -0.0163(9) 0.0047(9) -0.0159(10) O7 0.146(6) 0.081(5) 0.089(5) -0.017(4) -0.029(4) 0.007(4) O8 0.165(13) 0.204(17) 0.187(15) -0.010(13) 0.136(12) 0.060(12) O9 0.174(13) 0.100(9) 0.205(17) 0.022(9) -0.095(12) -0.083(9) O10 0.146(13) 0.272(19) 0.123(10) -0.135(12) -0.042(9) 0.009(11) O8A 0.050(10) 0.123(13) 0.125(13) -0.052(10) 0.005(7) -0.020(7) O9A 0.050(10) 0.123(13) 0.125(13) -0.052(10) 0.005(7) -0.020(7) O10A 0.050(10) 0.123(13) 0.125(13) -0.052(10) 0.005(7) -0.020(7) _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 O6 1.959(4) 1_455 ? Cu1 N1 2.003(5) . ? Cu1 O2 2.017(4) . ? Cu1 N2 2.051(5) . ? Cu1 O1 2.350(4) . ? Cu1 O4 2.377(4) 1_455 ? Cu2 O5 1.960(4) . ? Cu2 O4 2.007(4) . ? Cu2 N4 2.011(6) . ? Cu2 N3 2.072(5) . ? Cu2 O3 2.307(4) . ? Cu2 O2 2.398(4) 1_655 ? O1 C1 1.233(7) . ? O2 C2 1.267(7) . ? O2 Cu2 2.398(4) 1_455 ? O3 C2 1.230(7) . ? O4 C1 1.259(7) . ? O4 Cu1 2.377(4) 1_655 ? O5 C3 1.256(7) . ? O6 C4 1.248(7) . ? O6 Cu1 1.959(4) 1_655 ? N1 C5 1.475(9) . ? N2 C6 1.483(8) . ? N2 C12 1.486(8) . ? N2 C9 1.491(8) . ? N3 C16 1.469(9) . ? N3 C13 1.487(9) . ? N3 C7 1.496(10) . ? N4 C8 1.466(10) . ? C5 C6 1.503(10) . ? C2 C1 1.574(8) . ? C7 C8 1.504(12) . ? C3 C4 1.458(9) . ? C3 C4 1.469(8) 2_765 ? C4 C3 1.469(8) 2_765 ? C9 C10 1.515(10) . ? C10 C11 1.512(11) . ? C11 C12 1.536(10) . ? C13 C14 1.528(12) . ? C14 C15 1.541(12) . ? C15 C16 1.466(13) . ? Cl O8 1.334(8) . ? Cl O9A 1.346(13) . ? Cl O10A 1.380(12) . ? Cl O9 1.400(9) . ? Cl O10 1.405(9) . ? Cl O7 1.414(6) . ? Cl O8A 1.444(13) . ? 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 O6 Cu1 N1 175.34(19) 1_455 . ? O6 Cu1 O2 89.92(18) 1_455 . ? N1 Cu1 O2 94.2(2) . . ? O6 Cu1 N2 90.20(19) 1_455 . ? N1 Cu1 N2 85.7(2) . . ? O2 Cu1 N2 178.42(18) . . ? O6 Cu1 O1 90.56(18) 1_455 . ? N1 Cu1 O1 88.2(2) . . ? O2 Cu1 O1 76.23(15) . . ? N2 Cu1 O1 102.19(18) . . ? O6 Cu1 O4 94.92(16) 1_455 1_455 ? N1 Cu1 O4 88.26(19) . 1_455 ? O2 Cu1 O4 76.06(15) . 1_455 ? N2 Cu1 O4 105.49(17) . 1_455 ? O1 Cu1 O4 151.73(15) . 1_455 ? O5 Cu2 O4 91.14(18) . . ? O5 Cu2 N4 173.3(2) . . ? O4 Cu2 N4 92.5(2) . . ? O5 Cu2 N3 91.8(2) . . ? O4 Cu2 N3 175.93(19) . . ? N4 Cu2 N3 84.9(2) . . ? O5 Cu2 O3 93.11(18) . . ? O4 Cu2 O3 76.82(15) . . ? N4 Cu2 O3 93.2(2) . . ? N3 Cu2 O3 100.22(19) . . ? O5 Cu2 O2 89.99(17) . 1_655 ? O4 Cu2 O2 75.72(15) . 1_655 ? N4 Cu2 O2 85.5(2) . 1_655 ? N3 Cu2 O2 107.07(19) . 1_655 ? O3 Cu2 O2 152.42(15) . 1_655 ? C1 O1 Cu1 109.2(4) . . ? C2 O2 Cu1 119.8(4) . . ? C2 O2 Cu2 136.3(4) . 1_455 ? Cu1 O2 Cu2 103.28(16) . 1_455 ? C2 O3 Cu2 109.8(4) . . ? C1 O4 Cu2 120.1(4) . . ? C1 O4 Cu1 135.5(4) . 1_655 ? Cu2 O4 Cu1 104.35(16) . 1_655 ? C3 O5 Cu2 132.7(4) . . ? C4 O6 Cu1 130.6(4) . 1_655 ? C5 N1 Cu1 107.5(4) . . ? C6 N2 C12 111.1(5) . . ? C6 N2 C9 111.4(5) . . ? C12 N2 C9 101.8(5) . . ? C6 N2 Cu1 105.8(4) . . ? C12 N2 Cu1 111.8(4) . . ? C9 N2 Cu1 115.1(4) . . ? C16 N3 C13 104.5(6) . . ? C16 N3 C7 114.1(6) . . ? C13 N3 C7 108.0(6) . . ? C16 N3 Cu2 111.4(4) . . ? C13 N3 Cu2 116.1(4) . . ? C7 N3 Cu2 103.1(4) . . ? C8 N4 Cu2 110.5(5) . . ? N1 C5 C6 106.9(6) . . ? N2 C6 C5 109.7(6) . . ? O3 C2 O2 125.9(6) . . ? O3 C2 C1 117.8(5) . . ? O2 C2 C1 116.2(5) . . ? O1 C1 O4 126.7(6) . . ? O1 C1 C2 117.8(5) . . ? O4 C1 C2 115.5(5) . . ? N3 C7 C8 109.2(7) . . ? N4 C8 C7 107.3(6) . . ? O5 C3 C4 139.5(6) . . ? O5 C3 C4 130.1(5) . 2_765 ? C4 C3 C4 90.3(5) . 2_765 ? O6 C4 C3 139.6(6) . . ? O6 C4 C3 130.7(6) . 2_765 ? C3 C4 C3 89.7(5) . 2_765 ? N2 C9 C10 105.1(6) . . ? C11 C10 C9 105.0(6) . . ? C10 C11 C12 104.9(6) . . ? N2 C12 C11 106.5(6) . . ? N3 C13 C14 105.5(6) . . ? C13 C14 C15 104.6(7) . . ? C16 C15 C14 104.8(7) . . ? C15 C16 N3 104.7(7) . . ? O8 Cl O9A 132.7(10) . . ? O8 Cl O10A 50.9(10) . . ? O9A Cl O10A 113.5(10) . . ? O8 Cl O9 112.8(8) . . ? O9A Cl O9 46.0(10) . . ? O10A Cl O9 140.5(9) . . ? O8 Cl O10 109.5(8) . . ? O9A Cl O10 60.6(10) . . ? O10A Cl O10 61.4(9) . . ? O9 Cl O10 106.1(8) . . ? O8 Cl O7 113.3(6) . . ? O9A Cl O7 113.7(8) . . ? O10A Cl O7 111.8(8) . . ? O9 Cl O7 107.7(5) . . ? O10 Cl O7 107.0(6) . . ? O8 Cl O8A 54.4(9) . . ? O9A Cl O8A 108.7(9) . . ? O10A Cl O8A 104.8(9) . . ? O9 Cl O8A 66.0(9) . . ? O10 Cl O8A 149.5(9) . . ? O7 Cl O8A 103.4(8) . . ? 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 O6 Cu1 O1 C1 82.5(4) 1_455 . . . ? N1 Cu1 O1 C1 -102.0(4) . . . . ? O2 Cu1 O1 C1 -7.3(4) . . . . ? N2 Cu1 O1 C1 172.8(4) . . . . ? O4 Cu1 O1 C1 -19.0(6) 1_455 . . . ? O6 Cu1 O2 C2 -83.2(5) 1_455 . . . ? N1 Cu1 O2 C2 94.6(5) . . . . ? N2 Cu1 O2 C2 11(7) . . . . ? O1 Cu1 O2 C2 7.4(4) . . . . ? O4 Cu1 O2 C2 -178.3(5) 1_455 . . . ? O6 Cu1 O2 Cu2 89.73(19) 1_455 . . 1_455 ? N1 Cu1 O2 Cu2 -92.5(2) . . . 1_455 ? N2 Cu1 O2 Cu2 -176(71) . . . 1_455 ? O1 Cu1 O2 Cu2 -179.7(2) . . . 1_455 ? O4 Cu1 O2 Cu2 -5.36(15) 1_455 . . 1_455 ? O5 Cu2 O3 C2 89.9(4) . . . . ? O4 Cu2 O3 C2 -0.5(4) . . . . ? N4 Cu2 O3 C2 -92.3(4) . . . . ? N3 Cu2 O3 C2 -177.7(4) . . . . ? O2 Cu2 O3 C2 -6.0(6) 1_655 . . . ? O5 Cu2 O4 C1 -92.4(5) . . . . ? N4 Cu2 O4 C1 93.2(5) . . . . ? N3 Cu2 O4 C1 44(3) . . . . ? O3 Cu2 O4 C1 0.5(4) . . . . ? O2 Cu2 O4 C1 177.9(5) 1_655 . . . ? O5 Cu2 O4 Cu1 84.27(19) . . . 1_655 ? N4 Cu2 O4 Cu1 -90.1(2) . . . 1_655 ? N3 Cu2 O4 Cu1 -139(3) . . . 1_655 ? O3 Cu2 O4 Cu1 177.2(2) . . . 1_655 ? O2 Cu2 O4 Cu1 -5.42(15) 1_655 . . 1_655 ? O4 Cu2 O5 C3 -51.0(6) . . . . ? N4 Cu2 O5 C3 71.7(19) . . . . ? N3 Cu2 O5 C3 131.8(6) . . . . ? O3 Cu2 O5 C3 -127.8(6) . . . . ? O2 Cu2 O5 C3 24.8(6) 1_655 . . . ? O6 Cu1 N1 C5 -9(3) 1_455 . . . ? O2 Cu1 N1 C5 -159.9(4) . . . . ? N2 Cu1 N1 C5 18.5(4) . . . . ? O1 Cu1 N1 C5 -83.8(4) . . . . ? O4 Cu1 N1 C5 124.2(4) 1_455 . . . ? O6 Cu1 N2 C6 -171.6(4) 1_455 . . . ? N1 Cu1 N2 C6 10.5(4) . . . . ? O2 Cu1 N2 C6 94(7) . . . . ? O1 Cu1 N2 C6 97.7(4) . . . . ? O4 Cu1 N2 C6 -76.5(4) 1_455 . . . ? O6 Cu1 N2 C12 67.2(4) 1_455 . . . ? N1 Cu1 N2 C12 -110.6(5) . . . . ? O2 Cu1 N2 C12 -27(7) . . . . ? O1 Cu1 N2 C12 -23.4(5) . . . . ? O4 Cu1 N2 C12 162.4(4) 1_455 . . . ? O6 Cu1 N2 C9 -48.3(4) 1_455 . . . ? N1 Cu1 N2 C9 133.9(4) . . . . ? O2 Cu1 N2 C9 -143(7) . . . . ? O1 Cu1 N2 C9 -138.9(4) . . . . ? O4 Cu1 N2 C9 46.9(5) 1_455 . . . ? O5 Cu2 N3 C16 85.8(5) . . . . ? O4 Cu2 N3 C16 -51(3) . . . . ? N4 Cu2 N3 C16 -100.0(5) . . . . ? O3 Cu2 N3 C16 -7.7(5) . . . . ? O2 Cu2 N3 C16 176.3(5) 1_655 . . . ? O5 Cu2 N3 C13 -33.7(5) . . . . ? O4 Cu2 N3 C13 -170(3) . . . . ? N4 Cu2 N3 C13 140.5(5) . . . . ? O3 Cu2 N3 C13 -127.1(5) . . . . ? O2 Cu2 N3 C13 56.9(5) 1_655 . . . ? O5 Cu2 N3 C7 -151.5(5) . . . . ? O4 Cu2 N3 C7 72(3) . . . . ? N4 Cu2 N3 C7 22.7(5) . . . . ? O3 Cu2 N3 C7 115.0(5) . . . . ? O2 Cu2 N3 C7 -61.0(5) 1_655 . . . ? O5 Cu2 N4 C8 66.1(19) . . . . ? O4 Cu2 N4 C8 -171.3(5) . . . . ? N3 Cu2 N4 C8 5.6(5) . . . . ? O3 Cu2 N4 C8 -94.4(5) . . . . ? O2 Cu2 N4 C8 113.2(5) 1_655 . . . ? Cu1 N1 C5 C6 -43.5(6) . . . . ? C12 N2 C6 C5 83.8(7) . . . . ? C9 N2 C6 C5 -163.5(6) . . . . ? Cu1 N2 C6 C5 -37.7(7) . . . . ? N1 C5 C6 N2 55.1(8) . . . . ? Cu2 O3 C2 O2 -179.5(5) . . . . ? Cu2 O3 C2 C1 0.4(7) . . . . ? Cu1 O2 C2 O3 173.3(5) . . . . ? Cu2 O2 C2 O3 3.4(10) 1_455 . . . ? Cu1 O2 C2 C1 -6.6(7) . . . . ? Cu2 O2 C2 C1 -176.6(4) 1_455 . . . ? Cu1 O1 C1 O4 -174.6(5) . . . . ? Cu1 O1 C1 C2 6.3(6) . . . . ? Cu2 O4 C1 O1 -179.6(5) . . . . ? Cu1 O4 C1 O1 5.0(10) 1_655 . . . ? Cu2 O4 C1 C2 -0.5(7) . . . . ? Cu1 O4 C1 C2 -175.9(4) 1_655 . . . ? O3 C2 C1 O1 179.2(6) . . . . ? O2 C2 C1 O1 -0.8(8) . . . . ? O3 C2 C1 O4 0.0(8) . . . . ? O2 C2 C1 O4 179.9(5) . . . . ? C16 N3 C7 C8 73.4(8) . . . . ? C13 N3 C7 C8 -170.9(6) . . . . ? Cu2 N3 C7 C8 -47.5(7) . . . . ? Cu2 N4 C8 C7 -33.0(8) . . . . ? N3 C7 C8 N4 54.8(9) . . . . ? Cu2 O5 C3 C4 11.9(12) . . . . ? Cu2 O5 C3 C4 -170.4(4) . . . 2_765 ? Cu1 O6 C4 C3 -3.3(11) 1_655 . . . ? Cu1 O6 C4 C3 176.4(4) 1_655 . . 2_765 ? O5 C3 C4 O6 -2.0(14) . . . . ? C4 C3 C4 O6 179.7(9) 2_765 . . . ? O5 C3 C4 C3 178.3(10) . . . 2_765 ? C4 C3 C4 C3 0.000(1) 2_765 . . 2_765 ? C6 N2 C9 C10 -77.4(7) . . . . ? C12 N2 C9 C10 41.1(7) . . . . ? Cu1 N2 C9 C10 162.2(5) . . . . ? N2 C9 C10 C11 -31.0(8) . . . . ? C9 C10 C11 C12 8.5(9) . . . . ? C6 N2 C12 C11 83.0(7) . . . . ? C9 N2 C12 C11 -35.6(7) . . . . ? Cu1 N2 C12 C11 -159.0(5) . . . . ? C10 C11 C12 N2 16.9(8) . . . . ? C16 N3 C13 C14 -29.7(8) . . . . ? C7 N3 C13 C14 -151.5(7) . . . . ? Cu2 N3 C13 C14 93.4(6) . . . . ? N3 C13 C14 C15 8.0(9) . . . . ? C13 C14 C15 C16 16.5(9) . . . . ? C14 C15 C16 N3 -35.4(9) . . . . ? C13 N3 C16 C15 41.0(8) . . . . ? C7 N3 C16 C15 158.7(7) . . . . ? Cu2 N3 C16 C15 -85.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.535 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.098 ############ END data_complex-2 _database_code_CSD 185894 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-pyrazine-oxalate-tetraaquo-dicopper(II) diperchlorate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C4 H4 N2) (C2 O4 2-) 4(H2 O) Cu2] 2(CL O4 1-)' _chemical_formula_sum 'C6 H12 Cl2 Cu2 N2 O16' _chemical_formula_weight 566.16 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' 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 10.644(4) _cell_length_b 10.254(4) _cell_length_c 8.363(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.96(2) _cell_angle_gamma 90.00 _cell_volume 912.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 2.707 _exptl_absorpt_correction_type 'refdelf' _exptl_absorpt_correction_T_min 0.5482 _exptl_absorpt_correction_T_max 1.0721 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1890 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.68 _reflns_number_total 1135 _reflns_number_gt 1008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'Shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.02 (Farrugia, 1999)' _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^ > 2sigma(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. ; _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^)+(0.0978P)^2^+1.9281P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1135 _refine_ls_number_parameters 85 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.28656(7) 0.0000 0.15070(9) 0.0472(4) Uani 1 2 d S . . O1 O 0.4066(3) 0.1304(3) 0.0595(4) 0.0525(8) Uani 1 1 d . . . O2 O 0.1658(4) -0.1427(5) 0.1993(7) 0.0788(12) Uani 1 1 d D . . H1O H 0.078(3) -0.130(8) 0.223(12) 0.118 Uiso 1 1 d D . . H2O H 0.167(7) -0.232(4) 0.159(11) 0.118 Uiso 1 1 d D . . N1 N 0.4105(5) 0.0000 0.3767(7) 0.0477(11) Uani 1 2 d S . . C1 C 0.4557(4) 0.1100(4) 0.4388(6) 0.0514(10) Uani 1 1 d . . . H1 H 0.4268 0.1893 0.3987 0.062 Uiso 1 1 calc R . . C2 C 0.5000 0.0754(5) 0.0000 0.0462(12) Uani 1 2 d S . . Cl Cl 0.17371(14) 0.0000 0.7072(2) 0.0525(5) Uani 1 2 d SD . . O10 O 0.0997(8) 0.0000 0.8415(13) 0.129(4) Uani 1 2 d SD . . O11 O 0.2983(9) 0.0000 0.7610(17) 0.211(13) Uani 0.83(3) 2 d SPD . . O12 O 0.1602(15) 0.1084(8) 0.6141(13) 0.192(9) Uani 0.83(3) 1 d PD . . O13 O 0.254(3) 0.102(3) 0.706(3) 0.112(17) Uiso 0.17(3) 1 d PD . . O14 O 0.095(3) 0.0000 0.574(2) 0.112(17) Uiso 0.17(3) 2 d SPD . . 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 Cu 0.0504(5) 0.0368(5) 0.0546(6) 0.000 0.0031(3) 0.000 O1 0.0634(18) 0.0354(14) 0.0590(19) 0.0006(12) 0.0122(14) 0.0024(13) O2 0.068(2) 0.059(2) 0.110(4) 0.000(2) 0.006(2) -0.0068(18) N1 0.047(2) 0.045(3) 0.051(3) 0.000 -0.002(2) 0.000 C1 0.059(2) 0.040(2) 0.056(3) 0.0025(17) -0.003(2) 0.0041(18) C2 0.061(3) 0.033(3) 0.044(3) 0.000 0.002(2) 0.000 Cl 0.0486(8) 0.0409(8) 0.0680(10) 0.000 -0.0016(6) 0.000 O10 0.103(6) 0.158(9) 0.128(9) 0.000 0.055(6) 0.000 O11 0.060(6) 0.45(4) 0.121(11) 0.000 -0.017(6) 0.000 O12 0.37(2) 0.077(6) 0.127(8) 0.039(5) 0.058(11) 0.097(9) _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 Cu O2 1.994(4) . ? Cu O2 1.994(4) 6 ? Cu O1 2.008(3) . ? Cu O1 2.008(3) 6 ? Cu N1 2.287(6) . ? O1 C2 1.253(4) . ? N1 C1 1.329(5) . ? N1 C1 1.329(5) 6 ? C1 C1 1.380(9) 2_656 ? C2 O1 1.253(4) 2_655 ? C2 C2 1.547(11) 5_655 ? Cl O13 1.345(15) . ? Cl O13 1.345(15) 6 ? Cl O12 1.363(7) 6 ? Cl O12 1.363(7) . ? Cl O14 1.383(15) . ? Cl O10 1.383(8) . ? Cl O11 1.393(10) . ? 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 O2 Cu O2 94.4(3) . 6 ? O2 Cu O1 169.2(2) . . ? O2 Cu O1 90.31(19) 6 . ? O2 Cu O1 90.31(19) . 6 ? O2 Cu O1 169.2(2) 6 6 ? O1 Cu O1 83.46(18) . 6 ? O2 Cu N1 101.34(19) . . ? O2 Cu N1 101.34(19) 6 . ? O1 Cu N1 87.26(15) . . ? O1 Cu N1 87.26(15) 6 . ? C2 O1 Cu 111.4(3) . . ? C1 N1 C1 116.2(6) . 6 ? C1 N1 Cu 121.5(3) . . ? C1 N1 Cu 121.5(3) 6 . ? N1 C1 C1 121.9(3) . 2_656 ? O1 C2 O1 126.6(5) 2_655 . ? O1 C2 C2 116.7(3) 2_655 5_655 ? O1 C2 C2 116.7(3) . 5_655 ? O13 Cl O13 101(4) . 6 ? O13 Cl O12 133.5(14) . 6 ? O13 Cl O12 55.0(15) 6 6 ? O13 Cl O12 55.0(15) . . ? O13 Cl O12 133.5(14) 6 . ? O12 Cl O12 109.3(11) 6 . ? O13 Cl O14 111.8(13) . . ? O13 Cl O14 111.8(13) 6 . ? O12 Cl O14 58.9(7) 6 . ? O12 Cl O14 58.9(7) . . ? O13 Cl O10 112.0(12) . . ? O13 Cl O10 112.0(12) 6 . ? O12 Cl O10 114.0(5) 6 . ? O12 Cl O10 114.0(5) . . ? O14 Cl O10 107.9(12) . . ? O13 Cl O11 53.4(18) . . ? O13 Cl O11 53.4(18) 6 . ? O12 Cl O11 106.0(7) 6 . ? O12 Cl O11 106.0(7) . . ? O14 Cl O11 145.3(13) . . ? O10 Cl O11 106.8(7) . . ? 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 O2 Cu O1 C2 -59.3(9) . . . . ? O2 Cu O1 C2 -175.2(3) 6 . . . ? O1 Cu O1 C2 -4.0(3) 6 . . . ? N1 Cu O1 C2 83.5(3) . . . . ? O2 Cu N1 C1 -143.4(5) . . . . ? O2 Cu N1 C1 -46.5(5) 6 . . . ? O1 Cu N1 C1 43.3(5) . . . . ? O1 Cu N1 C1 126.9(5) 6 . . . ? O2 Cu N1 C1 46.5(5) . . . 6 ? O2 Cu N1 C1 143.4(5) 6 . . 6 ? O1 Cu N1 C1 -126.9(5) . . . 6 ? O1 Cu N1 C1 -43.3(5) 6 . . 6 ? C1 N1 C1 C1 -0.1(11) 6 . . 2_656 ? Cu N1 C1 C1 -170.7(5) . . . 2_656 ? Cu O1 C2 O1 -176.6(3) . . . 2_655 ? Cu O1 C2 C2 3.4(3) . . . 5_655 ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.794 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.151 ##### END ##