Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Barba-Behrens, Norah' 'Bernes, Sylvain' 'Contreras, Rosalinda' 'Escuer, Albert' 'Leigh, G.' 'Lopez-Sandoval, Horacio' 'Noth, H.' 'Vicente, Ramon' _publ_contact_author_name 'Prof Norah Barba-Behrens' _publ_contact_author_address ; Facultad de Quimica, Universidad Nacional Autonoma de Mexico, C.U., 04510, Mexico D.F., Mexico ; _publ_contact_author_phone '6223810' _publ_contact_author_fax '6162010' _publ_contact_author_email 'norah@servidor.unam.mx' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ? #=========================================================================== #========================================================================== # # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, Crystal Structure and Magnetic Properties of the Triangulo-tricopper(II) Complex [Cu3(cpse)3(H2O)3] 8.5 H2O ; data_noeth48 _database_code_CSD 174684 ################################################ # Complex [Cu~3~(cpse)~3~(H~2~O)~3] 8.5 H~2~O # ################################################ _audit_creation_method SHELXL-97 _audit_creation_date '2001-05-08' l _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 Cu3 N3 O20.50' _chemical_formula_weight 1061.55 _chemical_compound_source ? _exptl_crystal_preparation ; Crystal mounted on glass fiber with perfluorpolyetheroil ; 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 15.1559(1) _cell_length_b 15.1559(1) _cell_length_c 37.3630(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7432.51(14) _cell_formula_units_Z 6 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhombus _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 1.350 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.80545 _exptl_absorpt_correction_T_max 0.90769 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; 1200 frames measured in phi (0-360) with chi=0 and om=2th=25 65 frames measured in om (15-35) with chi=280, 2th=29 and phi=0 ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_source_power 1.5 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_detector 'Area CCD' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14234 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 29.13 _reflns_number_total 3010 _reflns_number_gt 2745 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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. H atoms for water molecules (O5 to O9) were found on difference maps and refined as remaining Hs (riding model). ; _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^)+(0.0347P)^2^+8.2073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom + difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(13) _refine_ls_number_reflns 3010 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _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 Cu1 Cu 0.79995(2) 0.47068(2) 0.104257(9) 0.02141(9) Uani 1 1 d . . . N1 N 0.94852(16) 0.51837(15) 0.09571(6) 0.0221(5) Uani 1 1 d . . . C1 C 0.9470(2) 0.6771(2) 0.10754(8) 0.0276(6) Uani 1 1 d . . . C2 C 0.9943(2) 0.62728(19) 0.08516(9) 0.0277(6) Uani 1 1 d . . . H2A H 0.9819 0.6320 0.0600 0.033 Uiso 1 1 calc R . . H2B H 1.0673 0.6623 0.0890 0.033 Uiso 1 1 calc R . . O2 O 0.99712(16) 0.76877(15) 0.11469(6) 0.0390(5) Uani 1 1 d . . . O3 O 0.85427(13) 0.61657(14) 0.11721(5) 0.0272(4) Uani 1 1 d . . . C3 C 0.94460(19) 0.45023(19) 0.06571(8) 0.0230(6) Uani 1 1 d . . . H3A H 0.9155 0.4656 0.0448 0.028 Uiso 1 1 calc R . . C4 C 0.86892(19) 0.34072(19) 0.07717(8) 0.0220(6) Uani 1 1 d . . . H4A H 0.9003 0.3205 0.0960 0.026 Uiso 1 1 calc R . . O4 O 0.77870(14) 0.33674(13) 0.09133(6) 0.0250(4) Uani 1 1 d . . . C5 C 1.0484(2) 0.4653(2) 0.05451(9) 0.0327(7) Uani 1 1 d . . . H5A H 1.0923 0.5349 0.0476 0.049 Uiso 1 1 calc R . . H5B H 1.0397 0.4214 0.0347 0.049 Uiso 1 1 calc R . . H5C H 1.0783 0.4489 0.0742 0.049 Uiso 1 1 calc R . . O5 O 0.77005(14) 0.44081(14) 0.16563(5) 0.0307(5) Uani 1 1 d . . . H51 H 0.7147 0.4223 0.1706 0.046 Uiso 1 1 d R . . H52 H 0.8115 0.4818 0.1813 0.046 Uiso 1 1 d R . . C6 C 0.9993(2) 0.5101(2) 0.12875(8) 0.0326(7) Uani 1 1 d . . . H6A H 1.0697 0.5334 0.1238 0.049 Uiso 1 1 calc R . . H6B H 0.9664 0.4403 0.1364 0.049 Uiso 1 1 calc R . . H6C H 0.9945 0.5512 0.1473 0.049 Uiso 1 1 calc R . . C7 C 0.8433(2) 0.26834(19) 0.04542(8) 0.0259(6) Uani 1 1 d . . . C8 C 0.7776(2) 0.2631(2) 0.01856(9) 0.0327(7) Uani 1 1 d . . . H8A H 0.7455 0.3014 0.0205 0.039 Uiso 1 1 calc R . . C9 C 0.7590(2) 0.2011(2) -0.01137(9) 0.0420(8) Uani 1 1 d . . . H9A H 0.7156 0.1991 -0.0293 0.050 Uiso 1 1 calc R . . C10 C 0.8055(3) 0.1428(3) -0.01415(11) 0.0480(9) Uani 1 1 d . . . H10A H 0.7942 0.1021 -0.0342 0.058 Uiso 1 1 calc R . . C11 C 0.8688(3) 0.1450(3) 0.01279(11) 0.0470(9) Uani 1 1 d . . . H11A H 0.8981 0.1040 0.0112 0.056 Uiso 1 1 calc R . . C12 C 0.8891(2) 0.2082(2) 0.04240(9) 0.0337(7) Uani 1 1 d . . . H12A H 0.9331 0.2104 0.0602 0.040 Uiso 1 1 calc R . . O6 O 1.3333 0.6667 0.08437(15) 0.0875(17) Uani 1 3 d S . . H61 H 1.3230 0.6179 0.0923 0.131 Uiso 0.67 1 d PR . . O7 O 0.74771(19) 0.6667 0.1667 0.0415(8) Uani 1 2 d S . . H71 H 0.8028 0.7192 0.1573 0.062 Uiso 1 1 d R . . O8 O 1.21755(19) 0.9072(2) 0.11801(8) 0.0633(8) Uani 1 1 d . . . H81 H 1.2375 0.9636 0.1346 0.095 Uiso 1 1 d R . . H82 H 1.1446 0.8656 0.1154 0.095 Uiso 1 1 d R . . O9 O 1.2535(3) 0.7490(3) 0.13270(14) 0.1240(17) Uani 1 1 d . . . H92 H 1.2644 0.7292 0.1513 0.186 Uiso 1 1 d R . . H91 H 1.2937 0.7296 0.1192 0.186 Uiso 1 1 d 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 0.01833(15) 0.01951(15) 0.02652(18) -0.00027(14) 0.00153(14) 0.00956(13) N1 0.0216(10) 0.0196(10) 0.0243(13) 0.0010(9) 0.0007(10) 0.0097(8) C1 0.0311(14) 0.0229(13) 0.0270(18) -0.0004(12) -0.0011(13) 0.0122(12) C2 0.0260(13) 0.0209(13) 0.0321(18) 0.0003(12) 0.0060(13) 0.0087(11) O2 0.0364(11) 0.0226(10) 0.0510(15) -0.0065(10) 0.0075(10) 0.0096(9) O3 0.0246(9) 0.0260(9) 0.0322(12) -0.0031(9) 0.0025(8) 0.0136(8) C3 0.0218(12) 0.0216(12) 0.0257(17) -0.0005(12) 0.0020(12) 0.0110(11) C4 0.0199(12) 0.0228(12) 0.0237(16) -0.0019(12) 0.0012(11) 0.0109(10) O4 0.0199(8) 0.0207(9) 0.0350(12) -0.0010(8) 0.0061(9) 0.0106(7) C5 0.0230(13) 0.0303(14) 0.041(2) -0.0012(14) 0.0083(13) 0.0109(12) O5 0.0277(9) 0.0270(9) 0.0306(11) -0.0011(9) 0.0002(8) 0.0084(8) C6 0.0302(14) 0.0354(15) 0.0335(19) -0.0036(14) -0.0037(14) 0.0173(13) C7 0.0213(12) 0.0219(13) 0.0291(17) -0.0005(12) 0.0042(12) 0.0069(10) C8 0.0275(13) 0.0275(14) 0.039(2) -0.0015(14) -0.0010(13) 0.0107(12) C9 0.0335(16) 0.0445(18) 0.031(2) -0.0050(16) -0.0068(15) 0.0066(14) C10 0.0368(17) 0.0427(18) 0.047(2) -0.0224(17) 0.0014(17) 0.0066(15) C11 0.0372(17) 0.0390(17) 0.065(3) -0.0201(18) 0.0020(18) 0.0190(15) C12 0.0331(15) 0.0350(15) 0.0364(18) -0.0099(15) -0.0047(14) 0.0196(13) O6 0.104(3) 0.104(3) 0.055(4) 0.000 0.000 0.0519(14) O7 0.0361(11) 0.0507(19) 0.042(2) -0.0089(16) -0.0045(8) 0.0253(10) O8 0.0408(14) 0.0648(18) 0.0657(19) -0.0126(15) 0.0172(14) 0.0124(13) O9 0.080(3) 0.066(2) 0.228(5) -0.007(3) 0.056(3) 0.0383(19) _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 O4 1.9504(17) . ? Cu1 O4 1.9527(18) 2_655 ? Cu1 O3 1.9952(18) . ? Cu1 N1 2.017(2) . ? Cu1 O5 2.337(2) . ? N1 C2 1.489(3) . ? N1 C6 1.493(4) . ? N1 C3 1.505(3) . ? C1 O2 1.234(3) . ? C1 O3 1.287(3) . ? C1 C2 1.524(4) . ? C3 C5 1.531(4) . ? C3 C4 1.533(3) . ? C4 O4 1.439(3) . ? C4 C7 1.528(4) . ? O4 Cu1 1.9527(18) 3_665 ? C7 C8 1.387(4) . ? C7 C12 1.399(4) . ? C8 C9 1.395(5) . ? C9 C10 1.382(5) . ? C10 C11 1.379(5) . ? C11 C12 1.393(4) . ? 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 O4 Cu1 O4 95.86(11) . 2_655 ? O4 Cu1 O3 167.28(7) . . ? O4 Cu1 O3 96.37(8) 2_655 . ? O4 Cu1 N1 84.70(8) . . ? O4 Cu1 N1 155.61(9) 2_655 . ? O3 Cu1 N1 82.72(8) . . ? O4 Cu1 O5 97.25(8) . . ? O4 Cu1 O5 96.79(8) 2_655 . ? O3 Cu1 O5 84.79(7) . . ? N1 Cu1 O5 107.36(8) . . ? C2 N1 C6 109.8(2) . . ? C2 N1 C3 113.6(2) . . ? C6 N1 C3 113.8(2) . . ? C2 N1 Cu1 104.89(15) . . ? C6 N1 Cu1 111.66(17) . . ? C3 N1 Cu1 102.59(15) . . ? O2 C1 O3 125.4(3) . . ? O2 C1 C2 119.9(2) . . ? O3 C1 C2 114.7(2) . . ? N1 C2 C1 109.3(2) . . ? C1 O3 Cu1 114.83(16) . . ? N1 C3 C5 114.6(2) . . ? N1 C3 C4 106.6(2) . . ? C5 C3 C4 113.2(2) . . ? O4 C4 C7 111.1(2) . . ? O4 C4 C3 109.2(2) . . ? C7 C4 C3 110.1(2) . . ? C4 O4 Cu1 112.86(14) . . ? C4 O4 Cu1 114.21(14) . 3_665 ? Cu1 O4 Cu1 131.12(10) . 3_665 ? C8 C7 C12 118.6(3) . . ? C8 C7 C4 121.4(2) . . ? C12 C7 C4 119.9(3) . . ? C7 C8 C9 121.1(3) . . ? C10 C9 C8 119.6(3) . . ? C11 C10 C9 120.0(3) . . ? C10 C11 C12 120.6(3) . . ? C11 C12 C7 120.0(3) . . ? 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 O4 Cu1 N1 C2 152.71(19) . . . . ? O4 Cu1 N1 C2 60.2(3) 2_655 . . . ? O3 Cu1 N1 C2 -29.13(17) . . . . ? O5 Cu1 N1 C2 -111.33(17) . . . . ? O4 Cu1 N1 C6 -88.45(18) . . . . ? O4 Cu1 N1 C6 179.07(19) 2_655 . . . ? O3 Cu1 N1 C6 89.71(18) . . . . ? O5 Cu1 N1 C6 7.51(19) . . . . ? O4 Cu1 N1 C3 33.76(16) . . . . ? O4 Cu1 N1 C3 -58.7(3) 2_655 . . . ? O3 Cu1 N1 C3 -148.08(17) . . . . ? O5 Cu1 N1 C3 129.72(15) . . . . ? C6 N1 C2 C1 -81.4(3) . . . . ? C3 N1 C2 C1 150.0(2) . . . . ? Cu1 N1 C2 C1 38.7(3) . . . . ? O2 C1 C2 N1 150.1(3) . . . . ? O3 C1 C2 N1 -30.5(4) . . . . ? O2 C1 O3 Cu1 -175.5(3) . . . . ? C2 C1 O3 Cu1 5.2(3) . . . . ? O4 Cu1 O3 C1 22.8(5) . . . . ? O4 Cu1 O3 C1 -141.0(2) 2_655 . . . ? N1 Cu1 O3 C1 14.4(2) . . . . ? O5 Cu1 O3 C1 122.7(2) . . . . ? C2 N1 C3 C5 70.5(3) . . . . ? C6 N1 C3 C5 -56.1(3) . . . . ? Cu1 N1 C3 C5 -176.9(2) . . . . ? C2 N1 C3 C4 -163.4(2) . . . . ? C6 N1 C3 C4 70.0(3) . . . . ? Cu1 N1 C3 C4 -50.8(2) . . . . ? N1 C3 C4 O4 46.0(3) . . . . ? C5 C3 C4 O4 173.0(2) . . . . ? N1 C3 C4 C7 168.3(2) . . . . ? C5 C3 C4 C7 -64.8(3) . . . . ? C7 C4 O4 Cu1 -139.11(18) . . . . ? C3 C4 O4 Cu1 -17.4(3) . . . . ? C7 C4 O4 Cu1 54.5(3) . . . 3_665 ? C3 C4 O4 Cu1 176.15(18) . . . 3_665 ? O4 Cu1 O4 C4 145.88(15) 2_655 . . . ? O3 Cu1 O4 C4 -18.0(5) . . . . ? N1 Cu1 O4 C4 -9.62(18) . . . . ? O5 Cu1 O4 C4 -116.49(18) . . . . ? O4 Cu1 O4 Cu1 -50.6(2) 2_655 . . 3_665 ? O3 Cu1 O4 Cu1 145.5(3) . . . 3_665 ? N1 Cu1 O4 Cu1 153.87(16) . . . 3_665 ? O5 Cu1 O4 Cu1 47.00(15) . . . 3_665 ? O4 C4 C7 C8 45.0(3) . . . . ? C3 C4 C7 C8 -76.1(3) . . . . ? O4 C4 C7 C12 -137.2(3) . . . . ? C3 C4 C7 C12 101.7(3) . . . . ? C12 C7 C8 C9 -1.5(4) . . . . ? C4 C7 C8 C9 176.3(3) . . . . ? C7 C8 C9 C10 1.0(5) . . . . ? C8 C9 C10 C11 0.9(5) . . . . ? C9 C10 C11 C12 -2.1(5) . . . . ? C10 C11 C12 C7 1.5(5) . . . . ? C8 C7 C12 C11 0.3(5) . . . . ? C4 C7 C12 C11 -177.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_distance_DA _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # # D H D-H H...A D-H...A D...A A symm publ O5 H51 0.763 2.063 154.11 2.769 O5 2_655 ? O5 H52 0.857 1.879 175.33 2.734 O2 11_565 ? O6 H61 0.736 2.133 149.20 2.791 O9 2_755 ? O8 H81 0.974 2.031 156.47 2.949 O7 2_765 ? O8 H82 0.965 1.968 172.50 2.927 O2 1_555 ? O9 H91 0.944 1.880 161.34 2.791 O6 1_555 ? _diffrn_measured_fraction_theta_max 0.720 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.720 _refine_diff_density_max 0.334 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.051 #============================================================================ data_fn169 _database_code_CSD 174685 ################################### # Complex [Cu(H-cpse)~2~] H~2~O # ################################### _audit_creation_method SHELXL-97 _audit_creation_date '2001-01-20' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 N2 O6 Cu1 H2 O' _chemical_formula_weight 526.07 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 27.5016(4) _cell_length_b 27.5016(4) _cell_length_c 6.72060(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5083.04(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS' _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_source_power 1.5 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_detector 'Area CCD' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62119 _diffrn_reflns_av_R_equivalents 0.1019 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5832 _reflns_number_gt 4098 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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. H atoms for the water molecule (O10) and the coordinated hydroxyl group (O4) were omitted. ; _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^)+(0.0897P)^2^+2.0320P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0133(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 5832 _refine_ls_number_parameters 308 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 O7 O 0.65708(18) 0.35568(15) 0.7143(6) 0.0747(12) Uani 1 1 d . . . H7 H 0.6756 0.3743 0.7718 0.112 Uiso 1 1 calc R . . O10 O 0.4538(4) 0.3458(5) 0.9330(17) 0.228(5) Uani 1 1 d . . . Cu1 Cu 0.614178(17) 0.266224(17) 0.33969(10) 0.0406(2) Uani 1 1 d . . . O5 O 0.53663(12) 0.27507(12) 0.8322(6) 0.0559(8) Uani 1 1 d . . . O2 O 0.70038(12) 0.27219(13) -0.1290(5) 0.0545(9) Uani 1 1 d . . . O3 O 0.64630(13) 0.29087(12) 0.1047(6) 0.0508(8) Uani 1 1 d . . . O4 O 0.56455(11) 0.21992(11) 0.1255(5) 0.0422(7) Uani 1 1 d . . . C16 C 0.6679(2) 0.35534(19) 0.5079(8) 0.0522(12) Uani 1 1 d . . . H16 H 0.6762 0.3220 0.4693 0.063 Uiso 1 1 calc R . . O6 O 0.58680(13) 0.24880(12) 0.5941(5) 0.0475(8) Uani 1 1 d . . . N1 N 0.65691(13) 0.20522(14) 0.3004(5) 0.0420(9) Uani 1 1 d . . . C2 C 0.69335(17) 0.21865(19) 0.1468(8) 0.0466(11) Uani 1 1 d . . . H2A H 0.6977 0.1914 0.0570 0.056 Uiso 1 1 calc R . . H2B H 0.7243 0.2248 0.2114 0.056 Uiso 1 1 calc R . . C1 C 0.67920(17) 0.26305(19) 0.0267(7) 0.0452(11) Uani 1 1 d . . . C3 C 0.62532(17) 0.16389(17) 0.2279(7) 0.0421(10) Uani 1 1 d . . . H3 H 0.6465 0.1376 0.1810 0.051 Uiso 1 1 calc R . . C7 C 0.56594(18) 0.14120(17) -0.0500(7) 0.0424(11) Uani 1 1 d . . . C13 C 0.56040(18) 0.28125(18) 0.6774(7) 0.0440(11) Uani 1 1 d . . . C6 C 0.6831(2) 0.1915(2) 0.4869(8) 0.0535(13) Uani 1 1 d . . . H6A H 0.6598 0.1828 0.5874 0.080 Uiso 1 1 calc R . . H6B H 0.7021 0.2186 0.5322 0.080 Uiso 1 1 calc R . . H6C H 0.7040 0.1643 0.4610 0.080 Uiso 1 1 calc R . . C5 C 0.5921(2) 0.14354(18) 0.3903(7) 0.0515(13) Uani 1 1 d . . . H5A H 0.6115 0.1320 0.4992 0.077 Uiso 1 1 calc R . . H5B H 0.5733 0.1172 0.3373 0.077 Uiso 1 1 calc R . . H5C H 0.5707 0.1687 0.4365 0.077 Uiso 1 1 calc R . . C17 C 0.6054(2) 0.4216(2) 0.4521(9) 0.0629(15) Uani 1 1 d . . . H17A H 0.5772 0.4304 0.3755 0.094 Uiso 1 1 calc R . . H17B H 0.6307 0.4450 0.4299 0.094 Uiso 1 1 calc R . . H17C H 0.5971 0.4211 0.5909 0.094 Uiso 1 1 calc R . . C11 C 0.5640(2) 0.0630(2) -0.2071(8) 0.0648(16) Uani 1 1 d . . . H11 H 0.5799 0.0346 -0.2452 0.078 Uiso 1 1 calc R . . N2 N 0.58400(15) 0.33301(14) 0.3886(6) 0.0474(10) Uani 1 1 d . . . C20 C 0.7286(2) 0.3911(3) 0.2641(11) 0.077(2) Uani 1 1 d . . . H20 H 0.7153 0.3709 0.1673 0.093 Uiso 1 1 calc R . . C15 C 0.62304(18) 0.37118(17) 0.3885(7) 0.0470(12) Uani 1 1 d . . . H15 H 0.6338 0.3744 0.2501 0.056 Uiso 1 1 calc R . . C8 C 0.51780(19) 0.1463(2) -0.0928(9) 0.0578(14) Uani 1 1 d . . . H8 H 0.5018 0.1744 -0.0531 0.069 Uiso 1 1 calc R . . C4 C 0.59502(17) 0.18231(17) 0.0502(6) 0.0405(10) Uani 1 1 d . . . H4 H 0.6172 0.1964 -0.0483 0.049 Uiso 1 1 calc R . . C10 C 0.5151(3) 0.0688(3) -0.2481(10) 0.0759(19) Uani 1 1 d . . . H10 H 0.4978 0.0444 -0.3126 0.091 Uiso 1 1 calc R . . C22 C 0.7860(2) 0.4520(2) 0.3506(17) 0.084(2) Uani 1 1 d . . . H22 H 0.8104 0.4739 0.3160 0.101 Uiso 1 1 calc R . . C18 C 0.5494(2) 0.3423(2) 0.2227(10) 0.0629(15) Uani 1 1 d . . . H18A H 0.5670 0.3438 0.0993 0.094 Uiso 1 1 calc R . . H18B H 0.5331 0.3727 0.2448 0.094 Uiso 1 1 calc R . . H18C H 0.5259 0.3165 0.2169 0.094 Uiso 1 1 calc R . . C12 C 0.5894(2) 0.09907(18) -0.1102(8) 0.0531(13) Uani 1 1 d . . . H12 H 0.6225 0.0952 -0.0850 0.064 Uiso 1 1 calc R . . C21 C 0.7652(3) 0.4228(3) 0.2117(14) 0.093(2) Uani 1 1 d . . . H21 H 0.7757 0.4241 0.0803 0.111 Uiso 1 1 calc R . . C9 C 0.4923(2) 0.1114(2) -0.1921(12) 0.0734(18) Uani 1 1 d . . . H9 H 0.4597 0.1162 -0.2219 0.088 Uiso 1 1 calc R . . C14 C 0.5565(2) 0.3301(2) 0.5785(10) 0.0663(17) Uani 1 1 d . . . H14A H 0.5226 0.3371 0.5526 0.080 Uiso 1 1 calc R . . H14B H 0.5687 0.3548 0.6688 0.080 Uiso 1 1 calc R . . C23 C 0.7697(3) 0.4483(3) 0.5469(16) 0.098(3) Uani 1 1 d . . . H23 H 0.7841 0.4676 0.6441 0.117 Uiso 1 1 calc R . . C19 C 0.7112(2) 0.3884(2) 0.4558(8) 0.0556(15) Uani 1 1 d . . . C24 C 0.7332(3) 0.4173(2) 0.6003(12) 0.0791(19) Uani 1 1 d . . . H24 H 0.7231 0.4155 0.7322 0.095 Uiso 1 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 O7 0.109(3) 0.072(3) 0.043(2) -0.003(2) -0.001(2) 0.019(2) O10 0.256(12) 0.299(14) 0.131(8) -0.010(9) -0.017(8) 0.062(11) Cu1 0.0447(3) 0.0399(3) 0.0374(3) 0.0019(3) 0.0044(3) 0.0009(2) O5 0.069(2) 0.064(2) 0.0350(16) 0.012(2) 0.005(2) 0.0134(16) O2 0.0488(17) 0.071(2) 0.043(2) 0.0034(18) 0.0081(17) -0.0003(15) O3 0.055(2) 0.0497(18) 0.0478(18) 0.0033(16) 0.0105(17) 0.0021(16) O4 0.0443(18) 0.0429(17) 0.0393(17) 0.0025(14) -0.0003(14) 0.0052(14) C16 0.065(3) 0.049(3) 0.043(3) 0.000(2) 0.001(2) 0.008(3) O6 0.059(2) 0.0449(18) 0.0390(17) 0.0057(15) 0.0019(17) 0.0086(16) N1 0.0433(19) 0.048(2) 0.035(2) 0.0011(16) -0.0080(16) -0.0017(15) C2 0.039(3) 0.057(3) 0.044(3) 0.000(2) 0.000(2) 0.004(2) C1 0.041(3) 0.054(3) 0.041(3) -0.006(2) 0.001(2) -0.008(2) C3 0.048(3) 0.042(2) 0.037(2) 0.001(2) -0.008(2) 0.002(2) C7 0.052(3) 0.044(3) 0.032(2) 0.0062(19) 0.000(2) -0.005(2) C13 0.049(3) 0.046(3) 0.037(3) 0.003(2) -0.004(2) 0.002(2) C6 0.057(3) 0.064(3) 0.039(3) 0.001(2) -0.015(2) 0.012(3) C5 0.073(3) 0.046(3) 0.036(3) 0.007(2) -0.002(2) -0.006(2) C17 0.076(4) 0.047(3) 0.066(4) 0.004(3) -0.001(3) 0.011(3) C11 0.093(4) 0.046(3) 0.055(4) 0.000(2) -0.011(3) 0.004(3) N2 0.051(2) 0.040(2) 0.051(3) 0.0032(17) 0.0092(19) 0.0017(16) C20 0.076(4) 0.076(4) 0.079(4) -0.030(4) 0.016(3) -0.029(4) C15 0.057(3) 0.044(2) 0.040(3) 0.0036(19) 0.005(2) 0.003(2) C8 0.050(3) 0.059(3) 0.064(3) -0.004(3) -0.004(2) -0.004(2) C4 0.046(3) 0.046(3) 0.030(2) 0.0041(19) -0.0018(19) 0.002(2) C10 0.097(5) 0.068(4) 0.062(4) 0.012(3) -0.026(4) -0.034(4) C22 0.063(3) 0.056(3) 0.134(7) -0.012(5) -0.016(6) -0.002(3) C18 0.054(3) 0.059(3) 0.075(4) 0.001(3) -0.008(3) 0.002(3) C12 0.068(3) 0.046(3) 0.045(3) 0.002(2) -0.009(2) -0.001(2) C21 0.094(5) 0.072(4) 0.112(6) -0.021(5) 0.026(5) -0.026(4) C9 0.060(3) 0.074(4) 0.086(5) -0.004(4) -0.016(4) -0.015(3) C14 0.078(4) 0.053(3) 0.068(4) 0.015(3) 0.038(3) 0.015(3) C23 0.093(6) 0.062(4) 0.138(8) -0.019(5) -0.061(6) -0.007(4) C19 0.058(3) 0.046(3) 0.063(4) -0.012(3) -0.014(3) 0.004(3) C24 0.097(5) 0.072(4) 0.068(4) -0.010(4) -0.021(4) 0.001(4) _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 O7 C16 1.419(6) . ? Cu1 O6 1.929(3) . ? Cu1 O3 1.932(4) . ? Cu1 N2 2.042(4) . ? Cu1 N1 2.065(4) . ? Cu1 O4 2.357(3) . ? O5 C13 1.241(6) . ? O2 C1 1.224(6) . ? O3 C1 1.296(6) . ? O4 C4 1.424(6) . ? C16 C19 1.537(8) . ? C16 C15 1.536(7) . ? O6 C13 1.279(6) . ? N1 C2 1.485(6) . ? N1 C6 1.494(6) . ? N1 C3 1.512(6) . ? C2 C1 1.514(7) . ? C3 C5 1.529(7) . ? C3 C4 1.542(6) . ? C7 C8 1.362(7) . ? C7 C12 1.387(7) . ? C7 C4 1.540(7) . ? C13 C14 1.502(7) . ? C17 C15 1.531(7) . ? C11 C10 1.383(9) . ? C11 C12 1.377(8) . ? N2 C14 1.485(7) . ? N2 C18 1.488(7) . ? N2 C15 1.501(6) . ? C20 C19 1.376(9) . ? C20 C21 1.378(9) . ? C8 C9 1.362(8) . ? C10 C9 1.379(10) . ? C22 C21 1.360(11) . ? C22 C23 1.397(13) . ? C23 C24 1.365(11) . ? C19 C24 1.394(9) . ? 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 O3 171.95(15) . . ? O6 Cu1 N2 85.54(15) . . ? O3 Cu1 N2 90.10(15) . . ? O6 Cu1 N1 97.69(14) . . ? O3 Cu1 N1 85.42(14) . . ? N2 Cu1 N1 169.24(15) . . ? O6 Cu1 O4 100.43(14) . . ? O3 Cu1 O4 87.43(14) . . ? N2 Cu1 O4 110.41(14) . . ? N1 Cu1 O4 79.20(12) . . ? C1 O3 Cu1 116.3(3) . . ? C4 O4 Cu1 105.6(2) . . ? O7 C16 C19 112.5(5) . . ? O7 C16 C15 109.8(5) . . ? C19 C16 C15 109.6(4) . . ? C13 O6 Cu1 115.9(3) . . ? C2 N1 C6 108.7(4) . . ? C2 N1 C3 110.5(4) . . ? C6 N1 C3 110.9(4) . . ? C2 N1 Cu1 105.7(3) . . ? C6 N1 Cu1 111.8(3) . . ? C3 N1 Cu1 109.0(3) . . ? N1 C2 C1 113.4(4) . . ? O2 C1 O3 123.8(5) . . ? O2 C1 C2 119.9(4) . . ? O3 C1 C2 116.1(4) . . ? N1 C3 C5 112.8(4) . . ? N1 C3 C4 108.3(4) . . ? C5 C3 C4 110.5(4) . . ? C8 C7 C12 118.5(5) . . ? C8 C7 C4 121.5(5) . . ? C12 C7 C4 119.9(4) . . ? O5 C13 O6 124.8(4) . . ? O5 C13 C14 117.2(4) . . ? O6 C13 C14 118.0(4) . . ? C10 C11 C12 120.3(6) . . ? C14 N2 C18 109.2(4) . . ? C14 N2 C15 113.7(4) . . ? C18 N2 C15 109.7(4) . . ? C14 N2 Cu1 107.2(3) . . ? C18 N2 Cu1 107.1(3) . . ? C15 N2 Cu1 109.8(3) . . ? C19 C20 C21 121.8(6) . . ? N2 C15 C16 112.1(4) . . ? N2 C15 C17 114.0(4) . . ? C16 C15 C17 111.5(4) . . ? C7 C8 C9 122.1(6) . . ? O4 C4 C3 106.4(3) . . ? O4 C4 C7 112.5(4) . . ? C3 C4 C7 112.2(4) . . ? C11 C10 C9 119.1(5) . . ? C21 C22 C23 118.0(7) . . ? C7 C12 C11 120.2(5) . . ? C22 C21 C20 120.5(8) . . ? C8 C9 C10 119.8(6) . . ? N2 C14 C13 113.1(4) . . ? C24 C23 C22 122.0(7) . . ? C20 C19 C24 118.1(6) . . ? C20 C19 C16 120.9(5) . . ? C24 C19 C16 121.0(6) . . ? C23 C24 C19 119.5(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_distance_DA _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # # D H D-H H...A D-H...A D...A A symm publ # O7 H7 0.820 2.510 127.02 3.075 O10 3_655 ? # _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.989 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.247 ######################################################## # End of Crystallographic Information File (CIF) # ########################################################