Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _audit_creation_method ; MolEN (An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands) ; _journal_coden_Cambridge 186 loop_ _publ_author_name 'Triki, S.' 'Gomez-Garcia, Carlos J.' 'Pala, Jean-Sala' 'Thetiot, F.' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr S Triki' _publ_contact_author_address ; Chimie, Electrochimie Moleculaires, Chimie Analytique Universite de Bretagne Occidentale BP 809 Brest 29285 Cedex FRANCE ; _publ_contact_author_phone '(33)298016146' _publ_contact_author_fax '(33)298017001' _publ_contact_author_email triki@univ-brest.fr _publ_requested_journal 'Dalton Transactions' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM _publ_section_title ; New Polymeric Compounds with 2,2-dicyano-1-ethoxyethenolate (dcne-) Bridging Ligand: Syntheses, Structural Characterization and Magnetic Properties of [M(dcne)2(H2O)2] (M = MnII, FeII, CoII, NiII and ZnII) and [Cu(dcne)2(H2O)] ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. ; data_Co(dcne)2(H2O)2 #(compound 3) _database_code_CSD 169972 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12H14N4O6Co' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12H14N4O6Co' _chemical_formula_weight 369.20 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Co ? 0.299 0.973 International_Tables_Vol_IV_Table_2.3.1 # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 14.0331(8) _cell_length_b 15.415(1) _cell_length_c 7.9596(5) _cell_angle_alpha 90 _cell_angle_beta 110.870(5) _cell_angle_gamma 90 _cell_volume 1608.8(4) _cell_formula_units_z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.52 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD-(Enraf-Nonius) _diffrn_measurement_method \q/2\q _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 3284 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.500 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1859 _reflns_number_gt 1538 _reflns_threshold_expression >2.0\s(I) _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _diffrn_measurement_method 'CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0004 Fo^4^)' _refine_ls_hydrogen_treatment refxyz_U=1.3_x_bonding_atom _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1538 _refine_ls_number_parameters 113 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.047 _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_all 0.050 _refine_ls_wR_factor_ref 0.040 _refine_ls_goodness_of_fit_all 1.598 _refine_ls_goodness_of_fit_ref 1.293 _refine_ls_shift/su_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.252 _refine_diff_density_min -0.329 # 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_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CO 0.0000 0.35250(2) 0.2500 0.0174(2) 0.500 Uij ? ? Co O1 0.0705(1) 0.45435(8) 0.1720(2) 0.0306(8) 1.000 Uij ? ? O O2 0.3136(1) 0.06193(9) 0.0499(2) 0.0318(8) 1.000 Uij ? ? O O3 0.1671(1) 0.12870(8) -0.1136(2) 0.0275(9) 1.000 Uij ? ? O N1 0.0929(1) 0.2619(1) 0.1821(2) 0.026(1) 1.000 Uij ? ? N N2 0.3861(1) 0.1488(1) 0.4894(2) 0.024(1) 1.000 Uij ? ? N C1 0.1567(1) 0.2157(1) 0.1796(2) 0.019(1) 1.000 Uij ? ? C C2 0.3199(2) 0.1536(1) 0.3551(3) 0.018(1) 1.000 Uij ? ? C C3 0.2379(2) 0.1604(1) 0.1896(3) 0.017(1) 1.000 Uij ? ? C C4 0.2445(2) 0.1128(1) 0.0390(3) 0.023(1) 1.000 Uij ? ? C C5 0.1693(2) 0.0828(2) -0.2721(3) 0.041(2) 1.000 Uij ? ? C C6 0.0842(2) 0.1093(2) -0.4265(3) 0.051(2) 1.000 Uij ? ? C H01 0.098(1) 0.452(1) 0.105(2) 0.050(7) 1.000 Uiso ? ? H H02 0.105(1) 0.486(1) 0.246(3) 0.058(7) 1.000 Uiso ? ? H H1 0.1655 0.0221 -0.2548 0.0658 1.000 Uiso calc C5 H H2 0.2310 0.0959 -0.2906 0.0658 1.000 Uiso calc C5 H H3 0.0858 0.0793 -0.5298 0.0803 1.000 Uiso calc C6 H H4 0.0225 0.0962 -0.4081 0.0803 1.000 Uiso calc C6 H H5 0.0879 0.1700 -0.4440 0.0803 1.000 Uiso calc C6 H 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 _atom_site_aniso_type_symbol CO 0.0157(3) 0.0188(2) 0.0179(2) 0.0000 0.0030(2) 0.0000 Co O1 0.034(1) 0.0326(8) 0.0256(7) -0.0123(7) 0.0169(6) -0.0079(6) O O2 0.034(1) 0.0431(8) 0.0219(7) 0.0205(8) 0.0108(6) 0.0039(6) O O3 0.034(1) 0.0357(8) 0.0172(7) 0.0129(7) -0.0003(7) -0.0035(6) O N1 0.025(1) 0.0310(9) 0.0226(9) 0.0091(9) -0.0013(9) -0.0077(7) N N2 0.024(1) 0.0262(9) 0.0207(8) 0.0042(8) 0.0040(9) -0.0021(7) N C1 0.018(2) 0.023(1) 0.0158(9) -0.006(1) 0.000(1) -0.0029(8) C C2 0.013(2) 0.017(1) 0.025(1) 0.002(1) 0.0106(9) -0.0026(8) C C3 0.011(2) 0.022(1) 0.0183(9) 0.0086(9) 0.003(1) 0.0009(8) C C4 0.024(2) 0.023(1) 0.021(1) 0.003(1) 0.005(1) 0.0041(9) C C5 0.070(2) 0.054(1) 0.019(1) 0.024(1) 0.005(1) -0.009(1) C C6 0.086(2) 0.060(2) 0.026(1) 0.011(2) 0.004(1) -0.004(1) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CO O1 2.066(1) . . ? CO O1 2.066(1) . 2_555 ? CO N1 2.108(2) . . ? CO N1 2.108(2) . 2_555 ? CO N2 2.120(1) . 7_556 ? CO N2 2.120(1) . 8_454 ? O1 H01 0.76(2) . . ? O1 H02 0.79(2) . . ? O2 C4 1.225(3) . . ? O2 H01 2.05(2) . 7_555 ? O2 H02 2.00(2) . 6_545 ? O3 C4 1.333(2) . . ? O3 C5 1.457(3) . . ? N1 C1 1.149(3) . . ? N2 C2 1.142(2) . . ? C1 C3 1.403(3) . . ? C2 C3 1.411(2) . . ? C3 C4 1.436(3) . . ? C5 C6 1.435(3) . . ? H01 H02 1.21(3) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 CO O1 81.07(6) . . 2_555 ? O1 CO N1 91.18(7) . . . ? O1 CO N1 170.68(6) . . 2_555 ? O1 CO N2 91.51(6) . . 7_556 ? O1 CO N2 89.29(6) . . 8_454 ? O1 CO N1 170.68(6) . 2_555 . ? O1 CO N1 91.18(7) . 2_555 2_555 ? O1 CO N2 89.29(6) . 2_555 7_556 ? O1 CO N2 91.51(6) . 2_555 8_454 ? N1 CO N1 96.98(7) . . 2_555 ? N1 CO N2 85.72(7) . . 7_556 ? N1 CO N2 93.59(7) . . 8_454 ? N1 CO N2 93.59(7) . 2_555 7_556 ? N1 CO N2 85.72(7) . 2_555 8_454 ? N2 CO N2 178.96(6) . 7_556 8_454 ? CO O1 H01 125(1) . . . ? CO O1 H02 119(1) . . . ? H01 O1 H02 102(2) . . . ? C4 O2 H01 131.1(5) . . 7_555 ? C4 O2 H02 129.7(7) . . 6_545 ? H01 O2 H02 97.9(8) . 7_555 6_545 ? C4 O3 C5 116.0(2) . . . ? CO N1 C1 166.2(1) . . . ? CO N2 C2 174.2(2) . 7_556 . ? N1 C1 C3 176.0(2) . . . ? N2 C2 C3 179.5(2) . . . ? C1 C3 C2 118.3(2) . . . ? C1 C3 C4 123.8(2) . . . ? C2 C3 C4 117.9(2) . . . ? O2 C4 O3 123.4(2) . . . ? O2 C4 C3 123.5(2) . . . ? O3 C4 C3 113.1(2) . . . ? O3 C5 C6 109.6(2) . . . ? O1 H01 O2 172(1) . . 7_555 ? O1 H01 H02 39(1) . . . ? O2 H01 H02 136(1) . 7_555 . ? O1 H02 O2 173(2) . . 6_555 ? O1 H02 H01 37(1) . . . ? O2 H02 H01 147(1) . 6_555 . ? data_Zn(dcne)2(H2O)2 #(compound 5) _database_code_CSD 169973 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12H14N4O6Zn' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12H14N4O6Zn' _chemical_formula_weight 375.64 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Zn ? 0.222 1.431 International_Tables_Vol_IV_Table_2.3.1 # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 14.1182(4) _cell_length_b 15.5441(4) _cell_length_c 7.9715(2) _cell_angle_alpha 90 _cell_angle_beta 110.874(2) _cell_angle_gamma 90 _cell_volume 1634.6(2) _cell_formula_units_z 4 _cell_measurement_temperature 290 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.53 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 290 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD_(Enraf-Nonius) _diffrn_measurement_method \q/2\q _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 4589 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI 0.250 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.03 _reflns_number_total 2374 _reflns_number_gt 1672 _reflns_threshold_expression >4.0\s(I) _computing_data_collection 'KappaCCD_(Enraf-Nonius)' _computing_cell_refinement KappaCCD_(Enraf-Nonius) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0036 Fo^4^)' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1672 _refine_ls_number_parameters 113 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_all 0.046 _refine_ls_wR_factor_ref 0.046 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_ref 1.232 _refine_ls_shift/su_max 0.012 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.262 _refine_diff_density_min -0.277 # 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_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol ZN 0.0000 0.35186(2) 0.2500 0.0247(1) 0.500 Uij ? ? Zn O1 -0.0712(1) 0.4539(1) 0.3276(2) 0.0415(7) 1.000 Uij ? ? O O2 0.1872(1) 0.4371(1) 0.9507(2) 0.0460(8) 1.000 Uij ? ? O O3 0.3335(1) 0.3727(1) 1.1116(2) 0.0423(8) 1.000 Uij ? ? O N1 0.4070(1) 0.2399(1) 0.8187(3) 0.0380(8) 1.000 Uij ? ? N N2 0.1141(1) 0.3501(1) 0.5126(2) 0.0348(8) 1.000 Uij ? ? N C1 0.3427(1) 0.2848(1) 0.8202(2) 0.0300(8) 1.000 Uij ? ? C C2 0.1804(2) 0.3456(1) 0.6465(3) 0.0290(8) 1.000 Uij ? ? C C3 0.2613(2) 0.3396(1) 0.8098(3) 0.0291(8) 1.000 Uij ? ? C C4 0.2561(2) 0.3877(1) 0.9602(3) 0.0319(8) 1.000 Uij ? ? C C5 0.3328(3) 0.4183(2) 1.2700(3) 0.063(2) 1.000 Uij ? ? C C6 0.4128(4) 0.3907(3) 1.4240(4) 0.078(2) 1.000 Uij ? ? C H01 -0.105(2) 0.492(2) 0.244(3) 0.059(9) 1.000 Uiso ? ? H H02 -0.099(2) 0.450(2) 0.396(4) 0.07(1) 1.000 Uiso ? ? H H1 0.2707 0.4092 1.2855 0.0971 1.000 Uiso calc C5 H H2 0.3418 0.4784 1.2543 0.0971 1.000 Uiso calc C5 H H3 0.4101 0.4218 1.5251 0.1198 1.000 Uiso calc C6 H H4 0.4041 0.3311 1.4410 0.1198 1.000 Uiso calc C6 H H5 0.4752 0.4003 1.4098 0.1198 1.000 Uiso calc C6 H 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 _atom_site_aniso_type_symbol ZN 0.0205(1) 0.0269(1) 0.0275(1) 0.0000 0.0054(1) 0.0000 Zn O1 0.0430(7) 0.0433(8) 0.0384(6) 0.0158(6) 0.0220(5) 0.0080(6) O O2 0.0509(8) 0.0570(9) 0.0336(7) 0.0249(7) 0.0175(6) 0.0026(7) O O3 0.0502(9) 0.0554(8) 0.0272(7) 0.0217(7) 0.0016(6) -0.0070(6) O N1 0.0337(8) 0.0437(9) 0.0373(8) 0.0123(7) 0.0038(7) -0.0100(7) N N2 0.0329(8) 0.0405(9) 0.0317(8) 0.0073(7) 0.0045(7) -0.0032(7) N C1 0.0303(8) 0.0319(9) 0.0279(8) 0.0008(8) 0.0060(7) -0.0050(7) C C2 0.0273(8) 0.0286(9) 0.0312(8) 0.0031(7) 0.0104(6) -0.0024(7) C C3 0.0285(8) 0.032(1) 0.0271(8) 0.0066(7) 0.0071(7) -0.0011(7) C C4 0.0352(9) 0.0344(9) 0.0267(7) 0.0068(8) 0.0098(7) 0.0010(7) C C5 0.093(2) 0.086(2) 0.031(1) 0.039(2) 0.007(1) -0.013(1) C C6 0.123(3) 0.094(2) 0.041(1) 0.020(3) 0.007(2) -0.010(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ZN O1 2.086(2) . . ? ZN O1 2.086(2) . 2_555 ? ZN N1 2.139(2) . 7_556 ? ZN N1 2.139(2) . 8_454 ? ZN N2 2.139(2) . . ? ZN N2 2.139(2) . 2_555 ? O1 H01 0.89(3) . . ? O1 H02 0.78(4) . . ? O2 C4 1.220(3) . . ? O2 H01 1.92(3) . 3_566 ? O2 H02 2.05(4) . 2_556 ? O3 C4 1.329(2) . . ? O3 C5 1.451(4) . . ? N1 C1 1.148(3) . . ? N2 C2 1.143(2) . . ? C1 C3 1.409(3) . . ? C2 C3 1.396(2) . . ? C3 C4 1.437(3) . . ? C5 C6 1.406(4) . . ? H01 H02 1.35(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 ZN O1 80.97(7) . . 2_555 ? O1 ZN N1 171.09(7) . . 7_556 ? O1 ZN N1 91.54(7) . . 8_454 ? O1 ZN N2 89.63(6) . . . ? O1 ZN N2 91.47(6) . . 2_555 ? O1 ZN N1 91.54(7) . 2_555 7_556 ? O1 ZN N1 171.09(7) . 2_555 8_454 ? O1 ZN N2 91.47(6) . 2_555 . ? O1 ZN N2 89.63(6) . 2_555 2_555 ? N1 ZN N1 96.31(8) . 7_556 8_454 ? N1 ZN N2 85.71(7) . 7_556 . ? N1 ZN N2 93.32(7) . 7_556 2_555 ? N1 ZN N2 93.32(7) . 8_454 . ? N1 ZN N2 85.71(7) . 8_454 2_555 ? N2 ZN N2 178.55(7) . . 2_555 ? ZN O1 H01 117(1) . . . ? ZN O1 H02 124(2) . . . ? H01 O1 H02 108(3) . . . ? C4 O2 H01 130(1) . . 3_566 ? C4 O2 H02 132.0(8) . . 2_556 ? H01 O2 H02 95(1) . 3_566 2_556 ? C4 O3 C5 116.6(2) . . . ? ZN N1 C1 165.4(2) . 7_556 . ? ZN N2 C2 174.0(2) . . . ? N1 C1 C3 176.3(2) . . . ? N2 C2 C3 179.7(8) . . . ? C1 C3 C2 118.3(2) . . . ? C1 C3 C4 123.3(2) . . . ? C2 C3 C4 118.3(2) . . . ? O2 C4 O3 123.1(2) . . . ? O2 C4 C3 123.5(2) . . . ? O3 C4 C3 113.4(2) . . . ? O3 C5 C6 111.0(3) . . . ? O1 H01 O2 173(2) . . 3_566 ? O1 H01 H02 33(1) . . . ? O2 H01 H02 145(2) . 3_566 . ? O1 H02 O2 172(2) . . 2_556 ? O1 H02 H01 38(1) . . . ? O2 H02 H01 136(2) . 2_556 . ? #===END data_cu(dcne)2(H2O) #(compound 6) _database_code_CSD 169974 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12H12N4O5Cu' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12H12N4O5Cu' _chemical_formula_weight 355.79 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Cu ? 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1 # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.8978(6) _cell_length_b 15.8015(9) _cell_length_c 7.3402(5) _cell_angle_alpha 90 _cell_angle_beta 105.963(5) _cell_angle_gamma 90 _cell_volume 1438.3(3) _cell_formula_units_z 4 _cell_measurement_temperature 273 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD_(Enraf-Nonius) _diffrn_measurement_method \q/2\q _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 2838 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.500 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1644 _reflns_number_gt 1158 _reflns_threshold_expression >2.0\s(I) _computing_data_collection 'KappaCCD_(Enraf-Nonius)' _computing_cell_refinement KappaCCD_(Enraf-Nonius) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0004 Fo^4^)' _refine_ls_hydrogen_treatment refxyz_U=1.3_x_bonding_atom _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1158 _refine_ls_number_parameters 101 _refine_ls_number_restraints 8 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.063 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_all 0.060 _refine_ls_wR_factor_ref 0.040 _refine_ls_goodness_of_fit_all 1.643 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_shift/su_max 0.006 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.146 _refine_diff_density_min -0.266 # 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_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CU 0.0000 0.14878(3) 0.7500 0.0226(2) 0.500 Uij ? ? Cu O1 0.0000 0.0265(2) 0.7500 0.026(2) 0.500 Uij ? ? O O2 -0.1684(1) 0.0565(1) 0.0172(3) 0.0237(9) 1.000 Uij ? ? O O3 -0.3229(1) 0.1223(1) -0.1323(2) 0.0174(8) 1.000 Uij ? ? O N1 -0.3912(2) 0.2658(1) 0.1805(3) 0.021(1) 1.000 Uij ? ? N N2 -0.0963(2) 0.1480(2) 0.4908(3) 0.026(1) 1.000 Uij ? ? N C1 -0.3258(2) 0.2175(2) 0.1757(3) 0.016(1) 1.000 Uij ? ? C C2 -0.1612(2) 0.1517(2) 0.3492(4) 0.019(1) 1.000 Uij ? ? C C3 -0.2435(2) 0.1583(2) 0.1796(4) 0.017(1) 1.000 Uij ? ? C C4 -0.2390(2) 0.1076(2) 0.0194(4) 0.017(1) 1.000 Uij ? ? C C5 -0.3241(2) 0.0747(2) -0.3019(4) 0.023(1) 1.000 Uij ? ? C C6 -0.4164(2) 0.1064(2) -0.4563(4) 0.031(2) 1.000 Uij ? ? C H01 0.0580 -0.0052 0.8242 0.0507 1.000 Uiso ? ? H H1 -0.3330 0.0161 -0.2815 0.0306 1.000 Uiso calc C5 H H2 -0.2585 0.0833 -0.3345 0.0306 1.000 Uiso calc C5 H H3 -0.4195 0.0765 -0.5699 0.0436 1.000 Uiso calc C6 H H4 -0.4816 0.0979 -0.4222 0.0436 1.000 Uiso calc C6 H H5 -0.4071 0.1651 -0.4753 0.0436 1.000 Uiso calc C6 H 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 _atom_site_aniso_type_symbol CU 0.0360(3) 0.0168(2) 0.0191(2) 0.0000 -0.0101(2) 0.0000 Cu O1 0.029(1) 0.016(1) 0.040(2) 0.0000 -0.019(1) 0.0000 O O2 0.0229(8) 0.0228(9) 0.026(1) 0.0103(8) 0.0005(7) -0.002(1) O O3 0.0169(8) 0.0229(9) 0.0137(9) 0.0046(8) 0.0010(7) -0.0023(8) O N1 0.0188(9) 0.029(1) 0.016(1) 0.001(1) 0.0018(8) -0.004(1) N N2 0.036(1) 0.022(1) 0.023(1) 0.005(1) -0.007(1) -0.002(1) N C1 0.019(1) 0.021(1) 0.010(1) -0.008(1) -0.000(1) 0.000(1) C C2 0.025(1) 0.012(1) 0.022(1) 0.001(1) 0.004(1) -0.003(1) C C3 0.017(1) 0.018(1) 0.016(1) 0.004(1) 0.0007(9) -0.000(1) C C4 0.015(1) 0.019(1) 0.018(1) -0.002(1) 0.0019(9) 0.004(1) C C5 0.027(1) 0.026(1) 0.018(1) 0.002(1) 0.008(1) -0.005(1) C C6 0.035(2) 0.044(2) 0.019(2) 0.006(1) 0.003(1) -0.005(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CU O1 1.932(3) . . ? CU O1 1.932(3) . 2_556 ? CU N1 2.108(2) . 7_456 ? CU N1 2.108(2) . 8_555 ? CU N2 1.965(2) . . ? CU N2 1.965(2) . 2_556 ? O1 H01 0.939(1) . . ? O1 H01 0.939(1) . 2_556 ? O2 C4 1.222(3) . . ? O2 H01 1.769(2) . 3_556 ? O3 C4 1.342(3) . . ? O3 C5 1.451(3) . . ? N1 C1 1.146(3) . . ? N2 C2 1.143(3) . . ? C1 C3 1.410(3) . . ? C2 C3 1.400(3) . . ? C3 C4 1.436(4) . . ? C5 C6 1.487(3) . . ? H01 H01 1.5891 . 2_556 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 CU N1 129.80(6) . . 7_456 ? O1 CU N1 129.80(6) . . 8_555 ? O1 CU N2 89.65(7) . . . ? O1 CU N2 89.65(7) . . 2_556 ? N1 CU N1 100.39(9) . 7_456 8_555 ? N1 CU N2 87.29(9) . 7_456 . ? N1 CU N2 93.15(9) . 7_456 2_556 ? N1 CU N2 93.15(9) . 8_555 . ? N1 CU N2 87.29(9) . 8_555 2_556 ? N2 CU N2 179.3(1) . . 2_556 ? CU O1 H01 122.2(1) . . . ? CU O1 H01 122.2(1) . . 2_556 ? H01 O1 H01 115.6(3) . . 2_556 ? C4 O2 H01 139.7(2) . . 3_556 ? C4 O3 C5 116.0(2) . . . ? CU N1 C1 168.2(2) . 7_456 . ? CU N2 C2 171.9(2) . . . ? N1 C1 C3 177.2(3) . . . ? N2 C2 C3 177.5(3) . . . ? C1 C3 C2 116.8(2) . . . ? C1 C3 C4 123.5(2) . . . ? C2 C3 C4 119.7(2) . . . ? O2 C4 O3 122.5(2) . . . ? O2 C4 C3 125.3(2) . . . ? O3 C4 C3 112.3(2) . . . ? O3 C5 C6 107.3(2) . . . ? O1 H01 O2 173.9(1) . . 3_556 ? O1 H01 H01 32.2(1) . . 2_556 ? O2 H01 H01 152.43(6) . 3_556 2_556 ? #===END