Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'McKenzie, Christine J.' _publ_contact_author_address ; Department of Chemistry University of Southern Denmark Campusvej 55 DK-5230 Odense M Denmark ; _publ_contact_author_email chk@chem.sdu.dk _publ_contact_author_fax 004566158780 _publ_contact_author_phone 004565502518 loop_ _publ_author_name _publ_author_address J.K.Bjernemose ; Department of Chemistry University of Souhtern Denmark Campusvej 55 DK-5230 Odense M Denmark ; C.J.McKenzie ; Department of Chemistry University of Souhtern Denmark Campusvej 55 DK-5230 Odense M Denmark ; P.R.Raithby ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; S.J.Teat ; CLRC Daresbury Laboratory Daresbury Warrington WA4 4AD UK ; _publ_section_title ; Stuctural characterisation of a water intercalated \b-sheet and copper promoted monohydration of a dinitrile ; data_k01prr22 _database_code_CSD 207254 _audit_creation_date 2003-05-19T13:28:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_name_common '((Cu(cdc)!2$(OH!2$)) * H!2$O)!\\infty$' _chemical_formula_structural '{[Cu((NC)2CCONH2)2(OH2)] * H2O}' _chemical_formula_moiety 'Cu 2+, (C4 H2 N3 O -)2, H2 O, H2 O' _chemical_formula_sum 'C8 H8 Cu1 N6 O4' _chemical_formula_weight 315.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2230(5) _cell_length_b 7.4380(5) _cell_length_c 11.5910(11) _cell_angle_alpha 77.727(4) _cell_angle_beta 80.513(4) _cell_angle_gamma 74.160(6) _cell_volume 581.59(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9269 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'reddish brown' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 318 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.9 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.823 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_source 'fine focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.1135273 _diffrn_orient_matrix_UB_12 -0.0344702 _diffrn_orient_matrix_UB_13 -0.0832873 _diffrn_orient_matrix_UB_21 -0.0878271 _diffrn_orient_matrix_UB_22 -0.111014 _diffrn_orient_matrix_UB_23 -0.0125558 _diffrn_orient_matrix_UB_31 -0.0377672 _diffrn_orient_matrix_UB_32 0.0565264 _diffrn_orient_matrix_UB_33 -0.0573202 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\f and \w rotations' _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 9744 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2661 _reflns_number_gt 2397 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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_hydrogen_treatment_special ; All hydrogens on hetero atoms are unless otherwise stated located from the Fourier difference map and in the refinement restrained to have bondlengths of 1.00(1)\%A. Their thermal factors are set to 1.2*U~iso~ of the atom on which they are riding. All other hydrogen atoms are modelled as riding with SHELXL standard parameters for bondlengths, -angles and thermal factors. ; _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^)+(0.0301P)^2^+1.2192P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_number_reflns 2661 _refine_ls_number_parameters 198 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.624 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.08418(5) 1.02363(5) 0.74959(3) 0.01581(13) Uani 1 1 d . . . N11 N -0.1038(4) 0.8889(4) 0.8505(2) 0.0218(6) Uani 1 1 d . . . C12 C -0.2383(4) 0.8384(4) 0.8973(3) 0.0158(6) Uani 1 1 d . . . C13 C -0.4024(4) 0.7789(4) 0.9553(3) 0.0156(6) Uani 1 1 d . . . C14 C -0.5782(4) 0.8593(4) 0.9068(2) 0.0146(6) Uani 1 1 d . . . N15 N -0.7209(4) 0.9266(4) 0.8653(2) 0.0172(5) Uani 1 1 d . . . C16 C -0.3916(5) 0.6363(4) 1.0629(3) 0.0187(6) Uani 1 1 d . . . O17 O -0.5444(3) 0.5983(4) 1.1213(2) 0.0295(6) Uani 1 1 d . . . N18 N -0.2177(4) 0.5464(4) 1.0960(3) 0.0292(7) Uani 1 1 d D . . H181 H -0.151(5) 0.626(5) 1.105(4) 0.035 Uiso 1 1 d D . . H182 H -0.216(6) 0.452(4) 1.159(2) 0.035 Uiso 1 1 d D . . N21 N 0.2773(4) 1.1490(4) 0.6451(2) 0.0173(5) Uani 1 1 d . . . C22 C 0.4190(4) 1.1757(4) 0.5903(3) 0.0146(6) Uani 1 1 d . . . C23 C 0.5910(4) 1.2065(4) 0.5234(3) 0.0149(6) Uani 1 1 d . . . C24 C 0.7582(4) 1.1532(4) 0.5823(3) 0.0164(6) Uani 1 1 d . . . N25 N 0.8931(4) 1.1104(4) 0.6314(2) 0.0200(6) Uani 1 1 d . . . C26 C 0.6037(4) 1.2753(4) 0.3959(3) 0.0155(6) Uani 1 1 d . . . O27 O 0.7692(3) 1.2811(3) 0.3367(2) 0.0234(5) Uani 1 1 d . . . N28 N 0.4474(4) 1.3250(4) 0.3425(2) 0.0172(5) Uani 1 1 d D . . H281 H 0.334(3) 1.330(5) 0.387(3) 0.021 Uiso 1 1 d D . . H282 H 0.453(5) 1.388(5) 0.2678(14) 0.021 Uiso 1 1 d D . . O1W O -0.0560(3) 1.3017(4) 0.8223(2) 0.0290(6) Uani 1 1 d D . . H11W H -0.052(5) 1.399(4) 0.761(2) 0.035 Uiso 1 1 d D . . H12W H -0.177(2) 1.307(5) 0.856(3) 0.035 Uiso 1 1 d D . . O2W O -0.0455(4) 1.5656(4) 0.6081(2) 0.0308(6) Uani 1 1 d D . . H21W H -0.029(6) 1.540(6) 0.5355(18) 0.037 Uiso 1 1 d D . . H22W H 0.038(5) 1.630(5) 0.617(3) 0.037 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00851(19) 0.0241(2) 0.01358(19) 0.00420(14) -0.00308(13) -0.00669(14) N11 0.0120(12) 0.0312(15) 0.0192(13) 0.0072(11) -0.0045(10) -0.0076(11) C12 0.0136(14) 0.0178(14) 0.0143(14) 0.0029(11) -0.0056(11) -0.0033(12) C13 0.0123(14) 0.0184(14) 0.0154(14) 0.0041(11) -0.0030(11) -0.0070(12) C14 0.0160(14) 0.0184(14) 0.0095(13) 0.0010(11) 0.0009(11) -0.0084(12) N15 0.0124(12) 0.0243(13) 0.0143(12) 0.0036(10) -0.0030(10) -0.0082(10) C16 0.0201(15) 0.0190(15) 0.0169(15) 0.0031(12) -0.0065(12) -0.0070(13) O17 0.0191(12) 0.0364(14) 0.0254(12) 0.0094(10) 0.0007(10) -0.0077(11) N18 0.0200(14) 0.0284(16) 0.0369(17) 0.0200(13) -0.0180(13) -0.0135(12) N21 0.0138(12) 0.0224(13) 0.0153(12) 0.0026(10) -0.0035(10) -0.0072(10) C22 0.0140(14) 0.0172(14) 0.0124(13) 0.0011(11) -0.0064(11) -0.0035(11) C23 0.0112(13) 0.0192(14) 0.0133(14) 0.0027(11) -0.0027(11) -0.0055(11) C24 0.0142(14) 0.0213(15) 0.0118(13) 0.0040(11) 0.0013(11) -0.0084(12) N25 0.0138(12) 0.0302(15) 0.0148(12) 0.0051(11) -0.0034(10) -0.0091(11) C26 0.0135(14) 0.0174(14) 0.0158(14) 0.0002(11) -0.0025(11) -0.0061(11) O27 0.0137(11) 0.0355(13) 0.0187(11) 0.0014(10) -0.0015(9) -0.0069(10) N28 0.0082(11) 0.0305(14) 0.0092(11) 0.0059(10) -0.0010(9) -0.0060(10) O1W 0.0205(12) 0.0309(14) 0.0358(14) -0.0093(11) -0.0039(11) -0.0039(11) O2W 0.0233(13) 0.0290(13) 0.0397(15) -0.0016(11) -0.0051(11) -0.0085(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N11 1.984(3) . ? Cu1 N21 1.989(2) . ? Cu1 N15 1.989(2) 1_655 ? Cu1 N25 1.990(3) 1_455 ? Cu1 O1W 2.309(3) . ? N11 C12 1.148(4) . ? C12 C13 1.396(4) . ? C13 C14 1.401(4) . ? C13 C16 1.454(4) . ? C14 N15 1.151(4) . ? N15 Cu1 1.989(2) 1_455 ? C16 O17 1.264(4) . ? C16 N18 1.328(4) . ? N21 C22 1.154(4) . ? C22 C23 1.400(4) . ? C23 C24 1.407(4) . ? C23 C26 1.454(4) . ? C24 N25 1.145(4) . ? N25 Cu1 1.990(3) 1_655 ? C26 O27 1.283(4) . ? C26 N28 1.304(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 N11 Cu1 N21 177.56(12) . . ? N11 Cu1 N15 93.36(10) . 1_655 ? N21 Cu1 N15 86.67(10) . 1_655 ? N11 Cu1 N25 86.27(10) . 1_455 ? N21 Cu1 N25 93.59(10) . 1_455 ? N15 Cu1 N25 177.60(12) 1_655 1_455 ? N11 Cu1 O1W 93.13(11) . . ? N21 Cu1 O1W 89.30(10) . . ? N15 Cu1 O1W 94.52(10) 1_655 . ? N25 Cu1 O1W 87.87(11) 1_455 . ? C12 N11 Cu1 166.8(2) . . ? N11 C12 C13 179.2(4) . . ? C12 C13 C14 118.4(3) . . ? C12 C13 C16 121.0(3) . . ? C14 C13 C16 120.6(3) . . ? N15 C14 C13 178.8(3) . . ? C14 N15 Cu1 162.7(2) . 1_455 ? O17 C16 N18 121.7(3) . . ? O17 C16 C13 120.3(3) . . ? N18 C16 C13 118.0(3) . . ? C22 N21 Cu1 162.5(3) . . ? N21 C22 C23 179.4(3) . . ? C22 C23 C24 117.4(3) . . ? C22 C23 C26 122.3(3) . . ? C24 C23 C26 120.2(3) . . ? N25 C24 C23 179.2(3) . . ? C24 N25 Cu1 166.7(2) . 1_655 ? O27 C26 N28 120.8(3) . . ? O27 C26 C23 119.7(3) . . ? N28 C26 C23 119.5(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W O2W 0.901(10) 1.938(14) 2.823(4) 167(4) . O1W H12W O17 0.890(10) 1.934(17) 2.779(3) 158(3) 2_477 O2W H21W O2W 0.883(10) 1.927(15) 2.796(6) 167(4) 2_586 O2W H22W O27 0.894(10) 1.890(13) 2.768(3) 167(4) 2_686 N18 H181 O1W 0.890(10) 2.07(2) 2.893(4) 153(4) 2_577 N18 H182 O27 0.896(10) 2.184(15) 3.060(4) 166(4) 1_446 N28 H281 O2W 0.889(10) 2.01(2) 2.789(4) 146(3) 2_586 N28 H282 O17 0.893(10) 2.049(15) 2.916(3) 163(3) 1_664 _ccdc_chemical_compound_source_recrystallisation H~2~O data_bath33 _database_code_CSD 207255 _audit_creation_date 2003-05-19T15:55:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_name_common '(Cu(cyma)!2$) * H!2$O' _chemical_formula_structural '[Cu ((OCNH2)2CCN)2] * H2O' _chemical_formula_moiety 'Cu 2+, (C4 H4 N3 O2 -)2, H2 O' _chemical_formula_sum 'C8 H10 Cu N6 O5' _chemical_formula_weight 333.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.5923(5) _cell_length_b 11.2749(7) _cell_length_c 12.5768(8) _cell_angle_alpha 90 _cell_angle_beta 106.065(2) _cell_angle_gamma 90 _cell_volume 1170.83(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3031 _cell_measurement_theta_min 5.97 _cell_measurement_theta_max 29.04 _cell_measurement_wavelength 0.6893 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.899 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS v2.03' _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.928 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6893 _diffrn_source 'Daresbury SRS Station 9.8' _diffrn_radiation_probe x-ray _diffrn_radiation_type Synchrotron _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker AXS SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_unetI/netI 0.0226 _diffrn_reflns_number 4025 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 28.57 _diffrn_reflns_theta_full 28.57 _diffrn_measured_fraction_theta_full 0.96 _diffrn_measured_fraction_theta_max 0.96 _reflns_number_total 1579 _reflns_number_gt 1472 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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_hydrogen_treatment_special ; All hydrogens on hetero atoms are unless otherwise stated located from the Fourier difference map and in the refinement restrained to have bondlengths of 1.00(1)\%A. Their thermal factors are set to 1.2*U~iso~ of the atom on which they are riding. ; _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^)+(0.0544P)^2^+1.1221P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_number_reflns 1579 _refine_ls_number_parameters 109 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.848 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.216 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0 0 0.01884(13) Uani 1 2 d S . . C1 C 0.15049(19) 0.13100(14) -0.13850(13) 0.0171(3) Uani 1 1 d . . . C2 C 0.09135(19) 0.24032(14) -0.10652(13) 0.0163(3) Uani 1 1 d . . . C3 C -0.03346(19) 0.24758(14) -0.05175(13) 0.0173(3) Uani 1 1 d . . . C4 C 0.1566(2) 0.34702(15) -0.13333(14) 0.0203(3) Uani 1 1 d . . . N1 N 0.25997(19) 0.13372(13) -0.19648(13) 0.0225(3) Uani 1 1 d D . . N3 N -0.0993(2) 0.35371(13) -0.04231(15) 0.0255(3) Uani 1 1 d D . . N4 N 0.2147(2) 0.43336(15) -0.15198(16) 0.0325(4) Uani 1 1 d . . . O1 O 0.10325(16) 0.02897(12) -0.11517(11) 0.0212(3) Uani 1 1 d . . . H11 H 0.301(3) 0.2018(13) -0.2127(19) 0.025 Uiso 1 1 d D . . H12 H 0.290(3) 0.0814(17) -0.2412(16) 0.025 Uiso 1 1 d D . . O3 O -0.08627(15) 0.15838(11) -0.00957(11) 0.0216(3) Uani 1 1 d . . . H31 H -0.073(3) 0.4140(15) -0.0779(18) 0.026 Uiso 1 1 d D . . H32 H -0.1875(19) 0.354(2) -0.0184(18) 0.026 Uiso 1 1 d D . . O1W O 0 -0.19605(17) -0.25 0.0289(4) Uani 1 2 d SD . . H1W H 0.043(3) -0.1468(15) -0.1931(9) 0.035 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02299(19) 0.01222(18) 0.0264(2) 0.00407(9) 0.01532(14) 0.00268(9) C1 0.0183(7) 0.0167(7) 0.0170(7) 0.0012(5) 0.0058(6) -0.0004(5) C2 0.0170(7) 0.0143(7) 0.0189(7) 0.0016(5) 0.0071(6) -0.0005(5) C3 0.0158(7) 0.0157(7) 0.0211(7) 0.0022(5) 0.0062(6) 0.0009(5) C4 0.0206(7) 0.0185(7) 0.0243(8) -0.0003(6) 0.0105(6) 0.0008(6) N1 0.0262(7) 0.0192(7) 0.0275(7) -0.0009(5) 0.0167(6) -0.0003(5) N3 0.0260(7) 0.0162(7) 0.0400(9) 0.0061(6) 0.0188(7) 0.0055(5) N4 0.0399(9) 0.0203(7) 0.0469(10) 0.0012(7) 0.0277(8) -0.0044(7) O1 0.0280(6) 0.0140(5) 0.0270(6) 0.0022(5) 0.0166(5) 0.0003(5) O3 0.0230(6) 0.0146(5) 0.0327(6) 0.0057(4) 0.0166(5) 0.0026(4) O1W 0.0343(10) 0.0232(9) 0.0326(10) 0 0.0149(8) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 1.9243(12) . ? Cu1 O1 1.9243(12) 5 ? Cu1 O3 1.9245(12) . ? Cu1 O3 1.9245(12) 5 ? C1 O1 1.281(2) . ? C1 N1 1.341(2) . ? C1 C2 1.433(2) . ? C2 C4 1.407(2) . ? C2 C3 1.428(2) . ? C3 O3 1.2774(19) . ? C3 N3 1.343(2) . ? C4 N4 1.147(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 180.00(10) . 5 ? O1 Cu1 O3 92.59(5) . . ? O1 Cu1 O3 87.41(5) 5 . ? O1 Cu1 O3 87.41(5) . 5 ? O1 Cu1 O3 92.59(5) 5 5 ? O3 Cu1 O3 180.00(9) . 5 ? O1 C1 N1 117.37(15) . . ? O1 C1 C2 123.29(14) . . ? N1 C1 C2 119.33(14) . . ? C4 C2 C3 117.95(14) . . ? C4 C2 C1 118.20(14) . . ? C3 C2 C1 123.83(14) . . ? O3 C3 N3 117.27(15) . . ? O3 C3 C2 123.75(14) . . ? N3 C3 C2 118.98(14) . . ? N4 C4 C2 177.5(2) . . ? C1 O1 Cu1 124.50(11) . . ? C3 O3 Cu1 125.56(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O1 0.900(9) 2.208(13) 3.044(2) 154.3(14) . O1W H1W O3 0.900(9) 2.474(14) 3.1698(14) 134.3(17) 5 N1 H11 O1W 0.890(10) 2.219(15) 3.0263(19) 151(2) 3 N1 H12 N4 0.902(10) 2.136(12) 3.002(2) 161(2) 4_544 N3 H32 O3 0.889(10) 2.074(11) 2.953(2) 170(2) 7_455 _ccdc_chemical_compound_source_recrystallisation H~2~O