# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2297 data_cupapno3 _manuscript_identification_number_B0079831 # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, crystal structures and magnetic properties of one- and two-dimensional pap-containing copper(II) complexes (pap = pyrazino[2,3-f][4,7]-phenanthroline) ; loop_ _publ_author_name _publ_author_address 'Hilde Grove' ; Department of Chemistry University of Bergen N-5007 Bergen Norway ; 'Jorunn Sletten' ; Department of Chemistry University of Bergen N-5007 Bergen Norway ; 'Miguel Julve' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Juan Cano' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu2 (C14 H8 N 4)2 (H2O)2 (NO3)3]n (NO3)n' _chemical_formula_analytical ? _chemical_formula_sum 'C14 H12 Cu2 N8 O14' _chemical_formula_weight 643.40 _chemical_melting_point ? _chemical_compound_source 'synthesized by H. Grove' 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 monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0172(2) _cell_length_b 8.85050(10) _cell_length_c 24.3125(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.7700(10) _cell_angle_gamma 90.00 _cell_volume 2144.56(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.0 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method ? _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 2.078 _exptl_absorpt_correction_type 'empirical, SADABS' _exptl_absorpt_correction_T_min 0.705166 _exptl_absorpt_correction_T_max 0.862236 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '2K SMART CCD' _diffrn_measurement_method '\w-scan' _diffrn_standards_number '50 first frames remeasured at end of experiment' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 18577 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 30.49 _reflns_number_total 6462 _reflns_number_observed 4620 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, version 4.0' _computing_cell_refinement 'SAINT, version 4.0' _computing_data_reduction 'SAINT, version 4.0' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, version 4.3, 1992' _computing_publication_material 'CIFTAB, Sheldrick, 1993' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+1.8964P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom if bonded to C, difmap if bonded to O' _refine_ls_hydrogen_treatment 'riding model for C-bonded, isotropic refinement for O-bonded H' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6461 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_obs 0.0377 _refine_ls_wR_factor_all 0.0762 _refine_ls_wR_factor_obs 0.0668 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.31934(3) 0.63796(3) 0.189154(12) 0.01950(7) Uani 1 d . . Cu2 Cu 0.80836(3) 0.12975(3) 0.145965(11) 0.01876(7) Uani 1 d . . O1 O 0.2427(2) 0.5802(2) 0.25641(9) 0.0312(4) Uani 1 d . . H10 H 0.2690(37) 0.6003(42) 0.2845(15) 0.055(12) Uiso 1 d . . H11 H 0.1878(31) 0.5125(35) 0.2574(12) 0.033(9) Uiso 1 d . . O2 O 0.9384(2) 0.0088(2) 0.10802(8) 0.0264(4) Uani 1 d . . H20 H 0.9385(35) -0.0765(44) 0.1086(15) 0.054(12) Uiso 1 d . . H21 H 1.0136(33) 0.0394(35) 0.1158(13) 0.038(9) Uiso 1 d . . O3 O 0.1452(2) 0.7455(2) 0.16318(7) 0.0257(4) Uani 1 d . . O4 O 0.1191(2) 0.5182(2) 0.12965(8) 0.0327(4) Uani 1 d . . O5 O -0.0400(2) 0.6853(2) 0.11294(9) 0.0397(5) Uani 1 d . . O6 O 0.7850(2) -0.0363(2) 0.19864(7) 0.0244(4) Uani 1 d . . O7 O 0.6534(2) -0.0922(2) 0.12500(8) 0.0371(5) Uani 1 d . . O8 O 0.6850(2) -0.2550(2) 0.19261(8) 0.0316(4) Uani 1 d . . O9 O 0.9768(2) 0.1903(2) 0.20969(7) 0.0245(4) Uani 1 d . . O10 O 0.9275(2) 0.4297(2) 0.20918(7) 0.0272(4) Uani 1 d . . O11 O 1.0886(2) 0.3420(2) 0.26780(7) 0.0247(4) Uani 1 d . . O12 O 0.6435(2) 0.7708(3) -0.10547(9) 0.0447(5) Uani 1 d . . O13 O 0.8164(2) 0.8808(2) -0.13436(8) 0.0379(5) Uani 1 d . . O14 O 0.8002(2) 0.8586(2) -0.04670(7) 0.0362(5) Uani 1 d . . N1 N 0.3947(2) 0.6912(2) 0.11813(8) 0.0191(4) Uani 1 d . . N2 N 0.4589(2) 0.4700(2) 0.19043(8) 0.0179(4) Uani 1 d . . N3 N 0.6575(2) 0.2576(2) 0.17175(8) 0.0177(4) Uani 1 d . . N4 N 0.8025(2) 0.2870(2) 0.08590(8) 0.0201(4) Uani 1 d . . N5 N 0.0722(2) 0.6463(2) 0.13474(9) 0.0259(4) Uani 1 d . . N6 N 0.7050(2) -0.1317(2) 0.17166(9) 0.0236(4) Uani 1 d . . N7 N 0.9948(2) 0.3218(2) 0.22770(8) 0.0192(4) Uani 1 d . . N8 N 0.7520(2) 0.8357(2) -0.09516(9) 0.0246(4) Uani 1 d . . C1 C 0.3588(2) 0.8037(3) 0.08314(10) 0.0229(5) Uani 1 d . . H1 H 0.2897(2) 0.8680(3) 0.09086(10) 0.027 Uiso 1 calc R . C2 C 0.4224(2) 0.8276(3) 0.03510(10) 0.0232(5) Uani 1 d . . H2 H 0.3944(2) 0.9060(3) 0.01123(10) 0.028 Uiso 1 calc R . C3 C 0.5266(2) 0.7350(3) 0.02308(10) 0.0223(5) Uani 1 d . . H3 H 0.5694(2) 0.7509(3) -0.00866(10) 0.027 Uiso 1 calc R . C4 C 0.5673(2) 0.6163(2) 0.05956(9) 0.0183(4) Uani 1 d . . C5 C 0.4971(2) 0.5990(2) 0.10632(9) 0.0169(4) Uani 1 d . . C6 C 0.5298(2) 0.4796(2) 0.14560(9) 0.0164(4) Uani 1 d . . C7 C 0.4871(2) 0.3544(3) 0.22436(9) 0.0199(4) Uani 1 d . . H7 H 0.4409(2) 0.3444(3) 0.25549(9) 0.024 Uiso 1 calc R . C8 C 0.5861(2) 0.2454(3) 0.21438(10) 0.0206(5) Uani 1 d . . H8 H 0.6008(2) 0.1638(3) 0.23833(10) 0.025 Uiso 1 calc R . C9 C 0.6298(2) 0.3779(2) 0.13704(9) 0.0168(4) Uani 1 d . . C10 C 0.7054(2) 0.3933(2) 0.09005(9) 0.0177(4) Uani 1 d . . C11 C 0.6771(2) 0.5108(3) 0.05146(9) 0.0183(5) Uani 1 d . . C12 C 0.7564(2) 0.5168(3) 0.00703(10) 0.0223(5) Uani 1 d . . H12 H 0.7426(2) 0.5923(3) -0.01954(10) 0.027 Uiso 1 calc R . C13 C 0.8550(2) 0.4095(3) 0.00322(10) 0.0244(5) Uani 1 d . . H13 H 0.9079(2) 0.4126(3) -0.02609(10) 0.029 Uiso 1 calc R . C14 C 0.8758(2) 0.2959(3) 0.04331(10) 0.0248(5) Uani 1 d . . H14 H 0.9429(2) 0.2247(3) 0.04006(10) 0.030 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02015(14) 0.02076(14) 0.01804(14) 0.00056(12) 0.00415(11) 0.00079(12) Cu2 0.01762(14) 0.01922(14) 0.01924(15) 0.00174(12) 0.00082(11) 0.00128(11) O1 0.0326(11) 0.0406(11) 0.0209(10) -0.0022(9) 0.0052(8) -0.0180(9) O2 0.0225(10) 0.0243(10) 0.0324(11) -0.0018(8) 0.0034(8) 0.0021(8) O3 0.0242(9) 0.0285(9) 0.0245(9) -0.0060(7) 0.0024(7) 0.0013(7) O4 0.0370(11) 0.0266(9) 0.0347(11) -0.0015(8) 0.0051(9) 0.0021(8) O5 0.0273(10) 0.0436(11) 0.0457(13) -0.0013(10) -0.0090(9) 0.0026(9) O6 0.0256(9) 0.0212(8) 0.0255(9) -0.0004(7) -0.0016(7) -0.0052(7) O7 0.0417(11) 0.0365(11) 0.0300(11) 0.0038(9) -0.0119(9) -0.0122(9) O8 0.0375(11) 0.0222(9) 0.0351(11) 0.0033(8) 0.0030(9) -0.0069(8) O9 0.0248(9) 0.0203(8) 0.0275(9) -0.0062(7) -0.0022(7) 0.0003(7) O10 0.0291(9) 0.0216(8) 0.0298(10) 0.0025(8) -0.0023(8) 0.0056(7) O11 0.0274(9) 0.0233(9) 0.0215(9) 0.0006(7) -0.0068(7) -0.0048(7) O12 0.0359(11) 0.0588(14) 0.0393(12) -0.0050(11) 0.0035(9) -0.0247(10) O13 0.0312(10) 0.0610(13) 0.0221(9) 0.0074(10) 0.0049(8) -0.0118(10) O14 0.0390(11) 0.0480(12) 0.0212(9) 0.0015(9) 0.0006(8) -0.0108(9) N1 0.0198(10) 0.0164(9) 0.0211(10) 0.0008(8) 0.0021(8) -0.0004(7) N2 0.0202(10) 0.0184(9) 0.0153(9) -0.0006(7) 0.0021(8) -0.0052(7) N3 0.0178(9) 0.0176(9) 0.0173(10) 0.0026(7) -0.0006(7) -0.0003(7) N4 0.0168(9) 0.0241(10) 0.0194(10) -0.0009(8) 0.0010(8) 0.0010(8) N5 0.0240(10) 0.0318(11) 0.0224(11) 0.0014(9) 0.0047(8) 0.0016(9) N6 0.0214(10) 0.0216(10) 0.0280(11) -0.0013(9) 0.0028(8) -0.0030(8) N7 0.0189(9) 0.0203(9) 0.0187(9) 0.0008(8) 0.0033(7) -0.0013(8) N8 0.0267(11) 0.0221(10) 0.0257(11) 0.0028(8) 0.0056(9) 0.0004(8) C1 0.0230(12) 0.0183(11) 0.0268(13) 0.0020(10) -0.0001(10) 0.0015(9) C2 0.0270(13) 0.0200(11) 0.0216(12) 0.0057(9) -0.0021(10) -0.0003(9) C3 0.0251(12) 0.0226(11) 0.0191(12) 0.0041(9) 0.0021(10) -0.0030(10) C4 0.0199(11) 0.0183(11) 0.0164(11) 0.0003(9) 0.0001(8) -0.0025(9) C5 0.0184(10) 0.0152(10) 0.0167(11) 0.0005(8) -0.0006(8) -0.0027(8) C6 0.0177(11) 0.0171(10) 0.0144(11) -0.0002(8) 0.0007(8) -0.0029(8) C7 0.0226(11) 0.0223(11) 0.0152(10) 0.0015(9) 0.0031(8) -0.0046(10) C8 0.0230(12) 0.0217(11) 0.0170(11) 0.0036(9) 0.0009(9) -0.0022(9) C9 0.0194(10) 0.0170(10) 0.0134(10) 0.0004(9) -0.0008(8) -0.0033(9) C10 0.0159(10) 0.0201(11) 0.0171(11) -0.0006(9) 0.0016(8) -0.0023(8) C11 0.0197(11) 0.0199(11) 0.0152(11) 0.0008(9) 0.0012(9) -0.0038(9) C12 0.0242(12) 0.0244(12) 0.0182(12) 0.0029(9) 0.0020(9) -0.0040(10) C13 0.0218(12) 0.0327(13) 0.0194(12) -0.0001(10) 0.0054(10) -0.0030(10) C14 0.0193(12) 0.0320(13) 0.0236(13) 0.0002(11) 0.0048(10) 0.0012(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.943(2) . ? Cu1 N1 2.009(2) . ? Cu1 O3 2.031(2) . ? Cu1 N2 2.039(2) . ? Cu1 O11 2.239(2) 2_655 ? Cu1 O4 2.580(2) . ? Cu2 O6 1.978(2) . ? Cu2 O2 1.984(2) . ? Cu2 N4 2.014(2) . ? Cu2 N3 2.036(2) . ? Cu2 O9 2.238(2) . ? Cu2 O7 2.524(2) . ? O1 H10 0.73(4) . ? O1 H11 0.82(3) . ? O2 H20 0.75(4) . ? O2 H21 0.81(3) . ? O3 N5 1.297(3) . ? O4 N5 1.238(3) . ? O5 N5 1.243(3) . ? O6 N6 1.297(2) . ? O7 N6 1.248(3) . ? O8 N6 1.228(3) . ? O9 N7 1.250(2) . ? O10 N7 1.228(2) . ? O11 N7 1.297(2) . ? O11 Cu1 2.239(2) 2_645 ? O12 N8 1.232(3) . ? O13 N8 1.268(3) . ? O14 N8 1.244(3) . ? N1 C1 1.335(3) . ? N1 C5 1.363(3) . ? N2 C7 1.327(3) . ? N2 C6 1.362(3) . ? N3 C8 1.322(3) . ? N3 C9 1.369(3) . ? N4 C14 1.331(3) . ? N4 C10 1.364(3) . ? C1 C2 1.402(3) . ? C1 H1 0.93 . ? C2 C3 1.381(3) . ? C2 H2 0.93 . ? C3 C4 1.409(3) . ? C3 H3 0.93 . ? C4 C5 1.404(3) . ? C4 C11 1.472(3) . ? C5 C6 1.440(3) . ? C6 C9 1.378(3) . ? C7 C8 1.421(3) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C10 1.439(3) . ? C10 C11 1.410(3) . ? C11 C12 1.405(3) . ? C12 C13 1.380(3) . ? C12 H12 0.93 . ? C13 C14 1.401(3) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? 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 N1 177.82(9) . . ? O1 Cu1 O3 89.15(8) . . ? N1 Cu1 O3 90.48(7) . . ? O1 Cu1 N2 97.11(8) . . ? N1 Cu1 N2 82.38(8) . . ? O3 Cu1 N2 155.85(7) . . ? O1 Cu1 O11 89.88(8) . 2_655 ? N1 Cu1 O11 92.29(7) . 2_655 ? O3 Cu1 O11 93.89(7) . 2_655 ? N2 Cu1 O11 109.36(7) . 2_655 ? O1 Cu1 O4 90.76(8) . . ? N1 Cu1 O4 87.28(7) . . ? O3 Cu1 O4 54.77(6) . . ? N2 Cu1 O4 101.67(7) . . ? O11 Cu1 O4 148.64(6) 2_655 . ? O6 Cu2 O2 91.50(8) . . ? O6 Cu2 N4 170.38(7) . . ? O2 Cu2 N4 90.47(8) . . ? O6 Cu2 N3 94.24(7) . . ? O2 Cu2 N3 170.14(8) . . ? N4 Cu2 N3 82.58(8) . . ? O6 Cu2 O9 81.92(7) . . ? O2 Cu2 O9 88.06(7) . . ? N4 Cu2 O9 107.56(7) . . ? N3 Cu2 O9 100.67(7) . . ? O6 Cu2 O7 56.10(6) . . ? O2 Cu2 O7 84.58(8) . . ? N4 Cu2 O7 114.77(7) . . ? N3 Cu2 O7 91.98(7) . . ? O9 Cu2 O7 137.03(6) . . ? Cu1 O1 H10 126.0(29) . . ? Cu1 O1 H11 122.9(21) . . ? H10 O1 H11 109.4(35) . . ? Cu2 O2 H20 122.0(27) . . ? Cu2 O2 H21 110.6(22) . . ? H20 O2 H21 109.5(34) . . ? N5 O3 Cu1 105.59(14) . . ? N5 O4 Cu1 81.35(14) . . ? N6 O6 Cu2 105.29(14) . . ? N6 O7 Cu2 81.07(13) . . ? N7 O9 Cu2 122.50(14) . . ? N7 O11 Cu1 118.26(13) . 2_645 ? C1 N1 C5 118.2(2) . . ? C1 N1 Cu1 128.5(2) . . ? C5 N1 Cu1 113.36(15) . . ? C7 N2 C6 116.8(2) . . ? C7 N2 Cu1 132.4(2) . . ? C6 N2 Cu1 110.73(14) . . ? C8 N3 C9 117.0(2) . . ? C8 N3 Cu2 132.3(2) . . ? C9 N3 Cu2 110.67(14) . . ? C14 N4 C10 118.0(2) . . ? C14 N4 Cu2 128.9(2) . . ? C10 N4 Cu2 113.08(15) . . ? O4 N5 O5 123.2(2) . . ? O4 N5 O3 118.3(2) . . ? O5 N5 O3 118.4(2) . . ? O8 N6 O7 123.8(2) . . ? O8 N6 O6 119.1(2) . . ? O7 N6 O6 117.1(2) . . ? O10 N7 O9 122.8(2) . . ? O10 N7 O11 119.9(2) . . ? O9 N7 O11 117.4(2) . . ? O12 N8 O14 121.3(2) . . ? O12 N8 O13 119.9(2) . . ? O14 N8 O13 118.8(2) . . ? N1 C1 C2 121.8(2) . . ? N1 C1 H1 119.08(14) . . ? C2 C1 H1 119.08(14) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 H2 119.89(14) . . ? C1 C2 H2 119.89(14) . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3 120.46(14) . . ? C4 C3 H3 120.46(14) . . ? C5 C4 C3 117.0(2) . . ? C5 C4 C11 118.8(2) . . ? C3 C4 C11 124.2(2) . . ? N1 C5 C4 123.6(2) . . ? N1 C5 C6 115.2(2) . . ? C4 C5 C6 121.2(2) . . ? N2 C6 C9 121.7(2) . . ? N2 C6 C5 118.4(2) . . ? C9 C6 C5 120.0(2) . . ? N2 C7 C8 121.7(2) . . ? N2 C7 H7 119.14(13) . . ? C8 C7 H7 119.14(13) . . ? N3 C8 C7 121.3(2) . . ? N3 C8 H8 119.33(13) . . ? C7 C8 H8 119.33(13) . . ? N3 C9 C6 121.4(2) . . ? N3 C9 C10 118.2(2) . . ? C6 C9 C10 120.4(2) . . ? N4 C10 C11 123.8(2) . . ? N4 C10 C9 115.4(2) . . ? C11 C10 C9 120.8(2) . . ? C12 C11 C10 116.7(2) . . ? C12 C11 C4 124.5(2) . . ? C10 C11 C4 118.8(2) . . ? C13 C12 C11 119.3(2) . . ? C13 C12 H12 120.36(14) . . ? C11 C12 H12 120.36(14) . . ? C12 C13 C14 120.3(2) . . ? C12 C13 H13 119.84(14) . . ? C14 C13 H13 119.84(14) . . ? N4 C14 C13 121.9(2) . . ? N4 C14 H14 119.04(14) . . ? C13 C14 H14 119.04(14) . . ? _refine_diff_density_max 0.483 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.086 _Operators_for_generating_equivalent_atoms: ; $1 -x+3/2, y-1/2, -z+1/2 $2 -x+3/2, y+1/2, -z+1/2 $3 x-1/2, -y+3/2, z+1/2 $4 x-1, y, z $5 x+1, y-1, z $6 -x+2, -y+1, -z $7 -x+1/2, y+1/2, -z+1/2 $8 x, y+1, z $9 x-1, y+1, z ; _Cu...Cu_and_Cu...O_distances ; Distance CUCU 6.809 (0.000) Cu1 - Cu2 5.194 (0.000) Cu1 - Cu2_$2 5.576 (0.000) Cu1 - Cu1_$7 6.714 (0.000) Cu1 - Cu2_$8 6.721 (0.000) Cu1 - Cu2_$9 6.816 (0.000) Cu1 - Cu2_$4 6.909 (0.000) Cu2 - Cu2_$1 Distance CU.O 4.237 (0.002) Cu1 - O10_$2 3.235 (0.002) Cu2 - O10 ; _hydrogen_bonding ; Distance O..O 2.706 (0.003) O1 - O13_$3 2.644 (0.003) O1 - O11_$4 2.873 (0.003) O2 - O5_$5 2.661 (0.003) O2 - O13_$6 Distance H..O 1.989 (0.037) H10 - O13_$3 1.838 (0.033) H11 - O11_$4 2.121 (0.039) H20 - O5_$5 1.856 (0.033) H21 - O13_$6 Angle OH.O 167.82 ( 3.96) O1 - H10 - O13_$3 169.44 ( 3.02) O1 - H11 - O11_$4 174.14 ( 3.66) O2 - H20 - O5_$5 177.25 ( 3.11) O2 - H21 - O13_$6 ; _least-squares_planes_and_angles_between_planes ; Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 4.810 (0.006) x + 6.509 (0.004) y + 10.391 (0.017) z = 7.431 (0.001) * 0.194 (0.001) N1 * -0.186 (0.001) N2 * 0.177 (0.001) O1 * -0.185 (0.001) O3 0.223 (0.001) Cu1 -2.138 (0.002) O4 2.441 (0.002) O11_$2 Rms deviation of fitted atoms = 0.186 6.554 (0.005) x + 4.116 (0.005) y + 12.828 (0.014) z = 7.558 (0.003) Angle to previous plane (with approximate esd) = 19.73 ( 0.09 ) * 0.015 (0.001) N3 * -0.015 (0.001) N4 * 0.015 (0.001) O2 * -0.014 (0.001) O6 0.146 (0.001) Cu2 -2.052 (0.002) O7 2.317 (0.002) O9 Rms deviation of fitted atoms = 0.015 6.052 (0.002) x + 5.249 (0.002) y + 11.398 (0.006) z = 7.347 (0.001) Angle to previous plane (with approximate esd) = 8.70 ( 0.08 ) * 0.016 (0.002) N1 * 0.067 (0.002) N2 * -0.058 (0.002) N3 * -0.005 (0.002) N4 * -0.010 (0.002) C1 * -0.047 (0.002) C2 * -0.039 (0.002) C3 * -0.001 (0.002) C4 * 0.017 (0.002) C5 * 0.036 (0.002) C6 * 0.018 (0.002) C7 * -0.069 (0.002) C8 * 0.009 (0.002) C9 * 0.013 (0.002) C10 * 0.018 (0.002) C11 * 0.023 (0.002) C12 * 0.013 (0.002) C13 * 0.000 (0.002) C14 0.090 (0.001) Cu1 -0.110 (0.001) Cu2 Rms deviation of fitted atoms = 0.033 4.810 (0.006) x + 6.509 (0.004) y + 10.391 (0.017) z = 7.431 (0.001) Angle to previous plane (with approximate esd) = 11.27 ( 0.08 ) * 0.194 (0.001) N1 * -0.186 (0.001) N2 * 0.177 (0.001) O1 * -0.185 (0.001) O3 0.223 (0.001) Cu1 -2.138 (0.002) O4 2.441 (0.002) O11_$2 Rms deviation of fitted atoms = 0.186 6.554 (0.005) x - 4.116 (0.005) y + 12.828 (0.014) z = 6.629 (0.006) Angle to previous plane (with approximate esd) = 75.09 ( 0.05 ) * -0.015 (0.001) N3_$2 * 0.015 (0.001) N4_$2 * -0.015 (0.001) O2_$2 * 0.014 (0.001) O6_$2 Rms deviation of fitted atoms = 0.015 - 7.297 (0.008) x - 1.467 (0.010) y - 17.862 (0.018) z = 2.381 (0.012) Angle to previous plane (with approximate esd) = 80.96 ( 0.06 ) * 0.002 (0.002) N7_$2 * -0.001 (0.001) O9_$2 * -0.001 (0.001) O10_$2 * -0.001 (0.001) O11_$2 -0.397 (0.004) Cu1 -0.180 (0.004) Cu2_$2 Rms deviation of fitted atoms = 0.001 4.810 (0.006) x + 6.509 (0.004) y + 10.391 (0.017) z = 7.431 (0.001) Angle to previous plane (with approximate esd) = 84.84 ( 0.07 ) * 0.194 (0.001) N1 * -0.186 (0.001) N2 * 0.177 (0.001) O1 * -0.185 (0.001) O3 0.223 (0.001) Cu1 -2.138 (0.002) O4 2.441 (0.002) O11_$2 Rms deviation of fitted atoms = 0.186 6.072 (0.007) x + 5.384 (0.007) y + 10.910 (0.020) z = 7.408 (0.003) Angle to previous plane (with approximate esd) = 10.45 ( 0.13 ) * -0.001 (0.002) N1 * 0.005 (0.002) C1 * -0.004 (0.002) C2 * -0.001 (0.002) C3 * 0.005 (0.002) C4 * -0.004 (0.002) C5 Rms deviation of fitted atoms = 0.004 6.080 (0.007) x + 5.262 (0.006) y + 11.272 (0.019) z = 7.374 (0.002) Angle to previous plane (with approximate esd) = 1.17 ( 0.15 ) * -0.010 (0.002) C4 * -0.001 (0.002) C5 * 0.012 (0.002) C6 * -0.012 (0.002) C9 * 0.000 (0.002) C10 * 0.011 (0.002) C11 -0.044 (0.004) C3 -0.005 (0.003) N1 0.036 (0.003) N2 -0.085 (0.003) N3 -0.016 (0.003) N4 0.024 (0.004) C12 Rms deviation of fitted atoms = 0.009 6.318 (0.007) x + 4.906 (0.006) y + 11.596 (0.020) z = 7.407 (0.001) Angle to previous plane (with approximate esd) = 2.83 ( 0.14 ) * 0.006 (0.001) N2 * 0.002 (0.001) N3 * -0.019 (0.002) C6 * 0.011 (0.002) C7 * -0.015 (0.002) C8 * 0.015 (0.001) C9 Rms deviation of fitted atoms = 0.012 6.080 (0.007) x + 5.262 (0.006) y + 11.272 (0.019) z = 7.374 (0.002) Angle to previous plane (with approximate esd) = 2.83 ( 0.14 ) * -0.010 (0.002) C4 * -0.001 (0.002) C5 * 0.012 (0.002) C6 * -0.012 (0.002) C9 * 0.000 (0.002) C10 * 0.011 (0.002) C11 Rms deviation of fitted atoms = 0.009 6.089 (0.008) x + 5.180 (0.007) y + 11.496 (0.020) z = 7.363 (0.004) Angle to previous plane (with approximate esd) = 0.76 ( 0.15 ) * -0.003 (0.002) N4 * 0.004 (0.002) C10 * -0.003 (0.002) C11 * 0.000 (0.002) C12 * 0.001 (0.002) C13 * 0.000 (0.002) C14 Rms deviation of fitted atoms = 0.003 ; "#===END" data_cupapcl _manuscript_identification_number_B0079831 # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, crystal structures and magnetic properties of one- and two-dimensional pap-containing copper(II) complexes (pap = pyrazino[2,3-f][4,7]-phenanthroline) ; loop_ _publ_author_name _publ_author_address 'Hilde Grove' ; Department of Chemistry University of Bergen N-5007 Bergen Norway ; 'Jorunn Sletten' ; Department of Chemistry University of Bergen N-5007 Bergen Norway ; 'Miguel Julve' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Juan Cano' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu4 (C14 H8 N4)4 Cl7]n Cln . 15nH2O _chemical_formula_analytical ? _chemical_formula_sum 'C56 H62 Cl8 Cu4 N16 O15' _chemical_formula_weight 1736.98 _chemical_melting_point ? _chemical_compound_source 'synthesized by H. Grove' 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 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.954(2) _cell_length_b 12.0954(14) _cell_length_c 21.334(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.300(2) _cell_angle_gamma 90.00 _cell_volume 3563.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1852 _cell_measurement_theta_min 3 _cell_measurement_theta_max 19 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method ? _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 1.551 _exptl_absorpt_correction_type 'empirical, SADABS' _exptl_absorpt_correction_T_min 0.759038 _exptl_absorpt_correction_T_max 0.894322 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'SMART 2K CCD'? _diffrn_measurement_method \w _diffrn_standards_number '50 first frames remeasured at end of experiment' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15937 _diffrn_reflns_av_R_equivalents 0.1261 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 21.99 _reflns_number_total 4376 _reflns_number_observed 2011 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, version 4.0' _computing_cell_refinement 'SAINT, version 4.0' _computing_data_reduction 'SAINT, version 4.0' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, version 4.3, 1992' _computing_publication_material 'CIFTAB (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 55 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1628P)^2^+21.7452P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom for those bonded to C, those bonded to O not found' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4321 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2245 _refine_ls_R_factor_obs 0.1073 _refine_ls_wR_factor_all 0.3475 _refine_ls_wR_factor_obs 0.2690 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.246 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 1.246 _refine_ls_shift/esd_max 0.011 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.3883(2) 0.2770(2) 0.18353(10) 0.0348(8) Uani 1 d . . Cu2 Cu 0.8201(2) 0.2613(2) 0.02720(10) 0.0358(8) Uani 1 d . . Cl1 Cl 0.2792(5) 0.3220(5) 0.0982(3) 0.079(2) Uani 1 d . . Cl2 Cl 0.2500 0.1967(7) 0.2500 0.068(3) Uani 1 d S . Cl3 Cl 0.7642(4) 0.2922(4) -0.0767(2) 0.054(2) Uani 1 d . . Cl4 Cl 0.9749(10) 0.1586(11) -0.0013(6) 0.206(6) Uani 1 d . . Cl5 Cl 0.7500 0.2763(15) 0.2500 0.164(6) Uani 1 d S . O1 O 1.1163(11) 0.1288(15) 0.0999(8) 0.091(6) Uani 1 d . . O2 O 0.7388(17) 0.6711(21) 0.3601(12) 0.164(10) Uani 1 d . . O3 O 0.4643(17) -0.3467(17) 0.0720(11) 0.148(9) Uani 1 d . . O4 O 0.5923(15) -0.3097(17) 0.1764(12) 0.141(9) Uani 1 d . . O5 O 0.6657(18) 0.5151(25) 0.2782(11) 0.190(12) Uani 1 d . . O6 O 0.2500 0.8609(43) 0.2500 0.251(22) Uiso 1 d S . O7 O 0.7292(28) 0.0304(28) 0.2277(17) 0.105(13) Uiso 0.50 d P . O8 O 1.1056(28) 0.1448(33) -0.2165(19) 0.119(14) Uiso 0.50 d P . O91 O 0.9619(11) 0.0890(13) -0.1428(7) 0.029(4) Uiso 0.70 d P . O92 O 1.0633(25) 0.1358(27) -0.1257(17) 0.025(9) Uiso 0.30 d P . N1 N 0.3907(10) 0.4248(11) 0.2258(6) 0.031(4) Uani 1 d . . N2 N 0.4810(10) 0.2401(12) 0.2666(7) 0.032(4) Uani 1 d . . N3 N 0.6006(9) 0.2351(11) 0.3839(6) 0.027(4) Uani 1 d . . N4 N 0.6176(10) 0.4113(12) 0.4576(7) 0.037(4) Uani 1 d . . N5 N 0.4200(11) 0.1283(11) 0.1462(7) 0.034(4) Uani 1 d . . N6 N 0.5242(10) 0.3139(11) 0.1365(6) 0.030(4) Uani 1 d . . N7 N 0.6891(10) 0.3084(11) 0.0768(7) 0.030(4) Uani 1 d . . N8 N 0.7502(11) 0.1150(12) 0.0294(7) 0.036(4) Uani 1 d . . C1 C 0.3451(13) 0.5217(14) 0.2013(9) 0.035(5) Uiso 1 d . . H1 H 0.3061(13) 0.5195(14) 0.1621(9) 0.052 Uiso 1 calc R . C2 C 0.3564(13) 0.6185(15) 0.2333(9) 0.039(5) Uiso 1 d . . H2 H 0.3279(13) 0.6829(15) 0.2155(9) 0.059 Uiso 1 calc R . C3 C 0.4107(13) 0.6206(16) 0.2925(9) 0.040(5) Uiso 1 d . . H3 H 0.4171(13) 0.6869(16) 0.3148(9) 0.061 Uiso 1 calc R . C4 C 0.4550(12) 0.5293(14) 0.3193(8) 0.031(5) Uiso 1 d . . C5 C 0.4415(11) 0.4310(13) 0.2830(8) 0.021(4) Uiso 1 d . . C6 C 0.4897(11) 0.3340(13) 0.3043(8) 0.022(4) Uiso 1 d . . C7 C 0.5302(12) 0.1533(15) 0.2862(8) 0.029(5) Uiso 1 d . . H7 H 0.5264(12) 0.0912(15) 0.2603(8) 0.043 Uiso 1 calc R . C8 C 0.5901(12) 0.1493(15) 0.3461(8) 0.032(5) Uiso 1 d . . H8 H 0.6226(12) 0.0841(15) 0.3587(8) 0.047 Uiso 1 calc R . C9 C 0.5491(11) 0.3287(13) 0.3620(7) 0.017(4) Uiso 1 d . . C10 C 0.5622(12) 0.4252(14) 0.4018(8) 0.026(4) Uiso 1 d . . C11 C 0.5134(12) 0.5210(14) 0.3817(8) 0.030(5) Uiso 1 d . . C12 C 0.5303(13) 0.6125(15) 0.4227(9) 0.038(5) Uiso 1 d . . H12 H 0.5005(13) 0.6798(15) 0.4112(9) 0.057 Uiso 1 calc R . C13 C 0.5908(12) 0.6033(15) 0.4799(9) 0.036(5) Uiso 1 d . . H13 H 0.6024(12) 0.6636(15) 0.5070(9) 0.055 Uiso 1 calc R . C14 C 0.6331(12) 0.5030(14) 0.4955(9) 0.030(5) Uiso 1 d . . H14 H 0.6743(12) 0.4966(14) 0.5337(9) 0.046 Uiso 1 calc R . C21 C 0.3629(13) 0.0388(15) 0.1524(9) 0.039(5) Uiso 1 d . . H21 H 0.3080(13) 0.0436(15) 0.1723(9) 0.058 Uiso 1 calc R . C22 C 0.3916(14) -0.0623(17) 0.1267(10) 0.052(6) Uiso 1 d . . H22 H 0.3535(14) -0.1243(17) 0.1307(10) 0.079 Uiso 1 calc R . C23 C 0.4697(12) -0.0752(15) 0.0971(8) 0.034(5) Uiso 1 d . . H23 H 0.4859(12) -0.1430(15) 0.0810(8) 0.051 Uiso 1 calc R . C24 C 0.5257(13) 0.0211(14) 0.0921(9) 0.034(5) Uiso 1 d . . C25 C 0.4989(12) 0.1216(13) 0.1175(8) 0.023(4) Uiso 1 d . . C26 C 0.5541(12) 0.2196(14) 0.1118(8) 0.027(4) Uiso 1 d . . C27 C 0.5785(12) 0.4016(15) 0.1320(8) 0.034(5) Uiso 1 d . . H27 H 0.5615(12) 0.4674(15) 0.1501(8) 0.051 Uiso 1 calc R . C28 C 0.6581(12) 0.4006(15) 0.1022(8) 0.030(5) Uiso 1 d . . H28 H 0.6922(12) 0.4661(15) 0.0993(8) 0.045 Uiso 1 calc R . C29 C 0.6378(12) 0.2166(14) 0.0816(8) 0.031(5) Uiso 1 d . . C30 C 0.6684(14) 0.1137(15) 0.0568(9) 0.037(5) Uiso 1 d . . C31 C 0.6124(13) 0.0159(14) 0.0618(9) 0.033(5) Uiso 1 d . . C32 C 0.6492(14) -0.0796(17) 0.0382(9) 0.050(6) Uiso 1 d . . H32 H 0.6188(14) -0.1471(17) 0.0421(9) 0.076 Uiso 1 calc R . C33 C 0.7313(15) -0.0742(19) 0.0087(10) 0.060(6) Uiso 1 d . . H33 H 0.7535(15) -0.1372(19) -0.0097(10) 0.090 Uiso 1 calc R . C34 C 0.7800(14) 0.0243(16) 0.0065(9) 0.040(5) Uiso 1 d . . H34 H 0.8364(14) 0.0257(16) -0.0120(9) 0.059 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0375(15) 0.033(2) 0.0310(15) -0.0029(11) -0.0047(11) 0.0029(11) Cu2 0.0407(15) 0.039(2) 0.0251(14) -0.0001(11) -0.0028(11) -0.0079(11) Cl1 0.096(5) 0.047(4) 0.078(5) -0.008(3) -0.046(4) 0.011(3) Cl2 0.046(5) 0.068(6) 0.094(7) 0.000 0.025(5) 0.000 Cl3 0.080(4) 0.047(4) 0.030(3) 0.002(2) -0.014(3) -0.016(3) Cl4 0.242(14) 0.188(12) 0.184(12) 0.018(9) 0.011(11) -0.067(10) Cl5 0.096(9) 0.278(20) 0.109(11) 0.000 -0.013(8) 0.000 O1 0.057(11) 0.128(16) 0.091(14) -0.018(11) 0.016(10) -0.001(10) O2 0.143(21) 0.174(24) 0.173(26) 0.058(20) 0.019(18) 0.022(18) O3 0.166(21) 0.110(18) 0.152(22) -0.033(15) -0.028(17) 0.045(15) O4 0.128(18) 0.096(17) 0.189(24) -0.029(15) -0.014(16) 0.008(13) O5 0.176(25) 0.270(35) 0.116(21) 0.007(20) -0.007(19) -0.084(22) N1 0.042(10) 0.033(10) 0.016(9) -0.006(7) -0.003(7) 0.004(7) N2 0.030(9) 0.038(10) 0.030(9) 0.002(8) 0.007(7) 0.008(7) N3 0.028(8) 0.029(9) 0.020(8) -0.003(7) -0.009(7) -0.003(7) N4 0.045(10) 0.044(11) 0.022(9) -0.004(7) -0.002(8) -0.002(8) N5 0.045(10) 0.028(10) 0.025(9) 0.009(7) -0.012(8) 0.010(7) N6 0.037(9) 0.021(9) 0.032(10) -0.012(7) 0.010(8) -0.010(7) N7 0.037(9) 0.013(9) 0.038(10) 0.001(7) 0.003(7) -0.012(7) N8 0.045(11) 0.036(10) 0.027(9) -0.005(7) 0.001(8) 0.000(8) _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 N1 2.000(13) . ? Cu1 N5 2.041(14) . ? Cu1 N2 2.086(14) . ? Cu1 Cl1 2.264(6) . ? Cu1 N6 2.314(14) . ? Cu1 Cl2 2.734(4) . ? Cu2 N4 2.018(15) 2_655 ? Cu2 N8 2.024(15) . ? Cu2 N3 2.077(12) 2_655 ? Cu2 Cl3 2.271(5) . ? Cu2 N7 2.311(15) . ? Cu2 Cl4 2.64(2) . ? Cl2 Cu1 2.734(4) 2 ? O7 O7 1.04(7) 2_655 ? N1 C5 1.32(2) . ? N1 C1 1.40(2) . ? N2 C7 1.29(2) . ? N2 C6 1.39(2) . ? N3 C8 1.31(2) . ? N3 C9 1.39(2) . ? N3 Cu2 2.077(12) 2_655 ? N4 C10 1.33(2) . ? N4 C14 1.37(2) . ? N4 Cu2 2.018(15) 2_655 ? N5 C25 1.34(2) . ? N5 C21 1.36(2) . ? N6 C27 1.31(2) . ? N6 C26 1.35(2) . ? N7 C29 1.33(2) . ? N7 C28 1.34(2) . ? N8 C34 1.29(2) . ? N8 C30 1.36(2) . ? C1 C2 1.35(2) . ? C1 H1 0.93 . ? C2 C3 1.38(2) . ? C2 H2 0.93 . ? C3 C4 1.35(2) . ? C3 H3 0.93 . ? C4 C5 1.42(2) . ? C4 C11 1.46(2) . ? C5 C6 1.40(2) . ? C6 C9 1.38(2) . ? C7 C8 1.42(2) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C10 1.44(2) . ? C10 C11 1.38(2) . ? C11 C12 1.41(2) . ? C12 C13 1.38(2) . ? C12 H12 0.93 . ? C13 C14 1.37(2) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C21 C22 1.42(3) . ? C21 H21 0.93 . ? C22 C23 1.34(2) . ? C22 H22 0.93 . ? C23 C24 1.42(2) . ? C23 H23 0.93 . ? C24 C25 1.40(2) . ? C24 C31 1.45(2) . ? C25 C26 1.43(2) . ? C26 C29 1.41(2) . ? C27 C28 1.36(2) . ? C27 H27 0.93 . ? C28 H28 0.93 . ? C29 C30 1.44(2) . ? C30 C31 1.43(2) . ? C31 C32 1.39(2) . ? C32 C33 1.39(3) . ? C32 H32 0.93 . ? C33 C34 1.37(3) . ? C33 H33 0.93 . ? C34 H34 0.93 . ? 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 N1 Cu1 N5 166.7(6) . . ? N1 Cu1 N2 80.8(5) . . ? N5 Cu1 N2 90.0(5) . . ? N1 Cu1 Cl1 96.5(4) . . ? N5 Cu1 Cl1 93.2(4) . . ? N2 Cu1 Cl1 175.5(4) . . ? N1 Cu1 N6 93.6(5) . . ? N5 Cu1 N6 76.3(5) . . ? N2 Cu1 N6 87.9(5) . . ? Cl1 Cu1 N6 95.9(4) . . ? N1 Cu1 Cl2 92.9(4) . . ? N5 Cu1 Cl2 95.6(5) . . ? N2 Cu1 Cl2 83.2(4) . . ? Cl1 Cu1 Cl2 93.4(2) . . ? N6 Cu1 Cl2 168.0(4) . . ? N4 Cu2 N8 168.5(6) 2_655 . ? N4 Cu2 N3 80.2(5) 2_655 2_655 ? N8 Cu2 N3 92.3(5) . 2_655 ? N4 Cu2 Cl3 95.1(4) 2_655 . ? N8 Cu2 Cl3 93.9(4) . . ? N3 Cu2 Cl3 168.0(4) 2_655 . ? N4 Cu2 N7 93.2(5) 2_655 . ? N8 Cu2 N7 77.9(5) . . ? N3 Cu2 N7 88.4(5) 2_655 . ? Cl3 Cu2 N7 102.9(4) . . ? N4 Cu2 Cl4 96.4(5) 2_655 . ? N8 Cu2 Cl4 90.4(5) . . ? N3 Cu2 Cl4 78.0(5) 2_655 . ? Cl3 Cu2 Cl4 91.7(3) . . ? N7 Cu2 Cl4 161.8(4) . . ? Cu1 Cl2 Cu1 138.4(3) . 2 ? C5 N1 C1 116.8(14) . . ? C5 N1 Cu1 116.0(11) . . ? C1 N1 Cu1 127.2(11) . . ? C7 N2 C6 118.7(15) . . ? C7 N2 Cu1 133.3(12) . . ? C6 N2 Cu1 108.0(10) . . ? C8 N3 C9 115.7(14) . . ? C8 N3 Cu2 132.9(12) . 2_655 ? C9 N3 Cu2 111.4(10) . 2_655 ? C10 N4 C14 116.5(15) . . ? C10 N4 Cu2 116.0(11) . 2_655 ? C14 N4 Cu2 127.2(12) . 2_655 ? C25 N5 C21 121.9(15) . . ? C25 N5 Cu1 118.1(11) . . ? C21 N5 Cu1 120.0(13) . . ? C27 N6 C26 116.2(15) . . ? C27 N6 Cu1 134.7(12) . . ? C26 N6 Cu1 109.0(10) . . ? C29 N7 C28 117.0(15) . . ? C29 N7 Cu2 107.4(11) . . ? C28 N7 Cu2 135.5(11) . . ? C34 N8 C30 119.4(17) . . ? C34 N8 Cu2 123.4(14) . . ? C30 N8 Cu2 117.3(12) . . ? C2 C1 N1 121.6(17) . . ? C2 C1 H1 119.2(12) . . ? N1 C1 H1 119.2(9) . . ? C1 C2 C3 119.2(18) . . ? C1 C2 H2 120.4(12) . . ? C3 C2 H2 120.4(11) . . ? C4 C3 C2 122.1(18) . . ? C4 C3 H3 119.0(11) . . ? C2 C3 H3 119.0(11) . . ? C3 C4 C5 116.0(16) . . ? C3 C4 C11 127.1(17) . . ? C5 C4 C11 116.9(15) . . ? N1 C5 C6 114.9(14) . . ? N1 C5 C4 124.3(15) . . ? C6 C5 C4 120.6(15) . . ? C9 C6 N2 118.0(14) . . ? C9 C6 C5 121.8(15) . . ? N2 C6 C5 120.2(15) . . ? N2 C7 C8 122.3(17) . . ? N2 C7 H7 118.8(10) . . ? C8 C7 H7 118.8(10) . . ? N3 C8 C7 121.7(17) . . ? N3 C8 H8 119.1(10) . . ? C7 C8 H8 119.1(10) . . ? C6 C9 N3 123.5(14) . . ? C6 C9 C10 119.8(15) . . ? N3 C9 C10 116.7(14) . . ? N4 C10 C11 125.5(16) . . ? N4 C10 C9 115.5(15) . . ? C11 C10 C9 118.8(16) . . ? C10 C11 C12 115.8(17) . . ? C10 C11 C4 121.8(16) . . ? C12 C11 C4 122.2(16) . . ? C13 C12 C11 120.7(17) . . ? C13 C12 H12 119.7(11) . . ? C11 C12 H12 119.7(11) . . ? C14 C13 C12 118.1(18) . . ? C14 C13 H13 120.9(11) . . ? C12 C13 H13 120.9(11) . . ? C13 C14 N4 123.2(17) . . ? C13 C14 H14 118.4(11) . . ? N4 C14 H14 118.4(10) . . ? N5 C21 C22 116.4(18) . . ? N5 C21 H21 121.8(11) . . ? C22 C21 H21 121.8(12) . . ? C23 C22 C21 125.0(20) . . ? C23 C22 H22 117.5(12) . . ? C21 C22 H22 117.5(12) . . ? C22 C23 C24 115.7(18) . . ? C22 C23 H23 122.1(12) . . ? C24 C23 H23 122.1(11) . . ? C25 C24 C23 120.2(17) . . ? C25 C24 C31 119.6(16) . . ? C23 C24 C31 120.1(16) . . ? N5 C25 C24 120.8(15) . . ? N5 C25 C26 118.6(15) . . ? C24 C25 C26 120.6(17) . . ? N6 C26 C29 121.5(15) . . ? N6 C26 C25 117.9(16) . . ? C29 C26 C25 120.5(16) . . ? N6 C27 C28 123.1(18) . . ? N6 C27 H27 118.5(10) . . ? C28 C27 H27 118.5(11) . . ? N7 C28 C27 122.0(17) . . ? N7 C28 H28 119.0(10) . . ? C27 C28 H28 119.0(11) . . ? N7 C29 C26 120.1(16) . . ? N7 C29 C30 120.0(16) . . ? C26 C29 C30 119.9(16) . . ? N8 C30 C31 122.9(17) . . ? N8 C30 C29 117.5(16) . . ? C31 C30 C29 119.6(17) . . ? C32 C31 C30 115.3(18) . . ? C32 C31 C24 125.0(17) . . ? C30 C31 C24 119.7(16) . . ? C33 C32 C31 119.9(20) . . ? C33 C32 H32 120.0(13) . . ? C31 C32 H32 120.0(12) . . ? C34 C33 C32 120.1(21) . . ? C34 C33 H33 120.0(13) . . ? C32 C33 H33 120.0(13) . . ? N8 C34 C33 122.3(20) . . ? N8 C34 H34 118.8(12) . . ? C33 C34 H34 118.8(13) . . ? _refine_diff_density_max 1.380 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.177 _Operators_for_generating_equivalent_atoms: ; $1 -x+1/2, y, -z+1/2 $2 -x+3/2, y, -z+1/2 $3 x+1, y, z $4 -x+2, -y, -z $5 -x+3/2, y+1, -z+1/2 $6 -x+1, -y, -z $7 x-1/2, -y, z+1/2 $8 -x+1, -y+1, -z $9 -x+2, -y+1, -z ; _possible_hydrogen_bond_interactions ; Distance O.CL 2.730 (0.021) O1 - Cl4 3.263 (0.018) O1 - Cl1_$3 3.272 (0.024) O3 - Cl3_$6 3.209 (0.035) O5 - Cl5 3.019 (0.037) O7 - Cl5 Distance O..O 3.043 (0.023) O1 - O91_$4 2.598 (0.033) O2 - O4_$5 2.671 (0.037) O2 - O5 2.684 (0.031) O3 - O4 3.019 (0.046) O4 - O8_$7 2.793 (0.052) O5 - O5_$2 3.078 (0.056) O7 - O8_$7 2.804 (0.043) O8 - O91 ; _Cu...Cu_distances ; Distance CUCU 5.110 (0.005) Cu1 - Cu1_$1 7.297 (0.003) Cu1 - Cu2 7.489 (0.003) Cu1 - Cu2_$8 6.887 (0.003) Cu1 - Cu2_$2 10.082 (0.004) Cu1 - Cu1_$2 7.849 (0.004) Cu2 - Cu2_$9 9.978 (0.005) Cu2 - Cu2_$2 ; _C...C-distances_across_tetranuclear_unit ; Distance C..C 6.539 (0.033) C7 - C7_$2 6.353 (0.024) C7 - C8_$2 6.482 (0.035) C8 - C8_$2 6.427 (0.033) C27 - C27_$2 6.297 (0.023) C27 - C28_$2 6.457 (0.033) C28 - C28_$2 9.505 (0.025) C2 - C13_$2 9.619 (0.025) C2 - C12_$2 9.606 (0.025) C3 - C12_$2 9.689 (0.025) C3 - C13_$2 8.741 (0.028) C33 - C22_$2 8.832 (0.027) C33 - C23_$2 8.888 (0.027) C32 - C22_$2 8.768 (0.026) C32 - C23_$2 ; _Least-squares_planes ; Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 11.488 (0.031) x - 4.340 (0.060) y - 11.821 (0.070) z = 7.777 (0.056) * 0.100 (0.006) Cl1_$2 * -0.119 (0.007) N1_$2 * 0.128 (0.007) N2_$2 * -0.109 (0.006) N5_$2 Rms deviation of fitted atoms = 0.115 11.488 (0.031) x + 4.340 (0.060) y - 11.821 (0.070) z = 3.544 (0.025) Angle to previous plane (with approximate esd) = 42.06 ( 0.32 ) * -0.100 (0.006) Cl1 * 0.119 (0.007) N1 * -0.128 (0.007) N2 * 0.109 (0.006) N5 -0.050 (0.007) Cu1 -2.774 (0.007) Cl2 2.227 (0.016) N6 Rms deviation of fitted atoms = 0.115 11.875 (0.035) x - 4.943 (0.060) y - 9.584 (0.063) z = 8.217 (0.044) Angle to previous plane (with approximate esd) = 45.65 ( 0.32 ) * 0.149 (0.006) Cl3 * -0.159 (0.006) N8 * 0.188 (0.007) N3_$2 * -0.179 (0.007) N4_$2 -0.031 (0.007) Cu2 -2.295 (0.016) N7 2.588 (0.017) Cl4 Rms deviation of fitted atoms = 0.169 11.488 (0.031) x - 4.340 (0.060) y - 11.821 (0.070) z = 7.777 (0.056) Angle to previous plane (with approximate esd) = 7.10 ( 0.58 ) * 0.100 (0.006) Cl1_$2 * -0.119 (0.007) N1_$2 * 0.128 (0.007) N2_$2 * -0.109 (0.006) N5_$2 Rms deviation of fitted atoms = 0.115 11.875 (0.035) x + 4.943 (0.060) y - 9.584 (0.063) z = 4.803 (0.044) Angle to previous plane (with approximate esd) = 45.65 ( 0.32 ) * -0.149 (0.006) Cl3_$2 * 0.159 (0.006) N8_$2 * -0.188 (0.007) N3 * 0.179 (0.007) N4 Rms deviation of fitted atoms = 0.169 12.079 (0.013) x + 3.282 (0.023) y - 11.550 (0.033) z = 3.554 (0.019) Angle to previous plane (with approximate esd) = 9.49 ( 0.42 ) * -0.048 (0.013) N1 * -0.035 (0.013) N2 * 0.039 (0.013) N3 * -0.028 (0.014) N4 * 0.002 (0.015) C1 * 0.088 (0.015) C2 * 0.066 (0.016) C3 * -0.008 (0.016) C4 * -0.075 (0.015) C5 * -0.056 (0.015) C6 * 0.048 (0.014) C7 * 0.067 (0.015) C8 * -0.023 (0.014) C9 * -0.008 (0.016) C10 * -0.051 (0.017) C11 * -0.020 (0.016) C12 * 0.020 (0.015) C13 * 0.022 (0.015) C14 -0.073 (0.009) Cu1 0.056 (0.008) Cu2_$2 Rms deviation of fitted atoms = 0.046 11.488 (0.031) x + 4.340 (0.060) y - 11.821 (0.070) z = 3.544 (0.025) Angle to previous plane (with approximate esd) = 5.68 ( 0.41 ) * -0.100 (0.006) Cl1 * 0.119 (0.007) N1 * -0.128 (0.007) N2 * 0.109 (0.006) N5 -0.050 (0.007) Cu1 -2.774 (0.007) Cl2 2.227 (0.016) N6 Rms deviation of fitted atoms = 0.115 5.959 (0.025) x - 2.505 (0.024) y + 17.267 (0.026) z = 4.688 (0.014) Angle to previous plane (with approximate esd) = 83.69 ( 0.21 ) * 0.018 (0.013) N5 * 0.006 (0.013) N6 * -0.029 (0.013) N7 * 0.002 (0.014) N8 * 0.008 (0.015) C21 * -0.010 (0.016) C22 * -0.024 (0.015) C23 * -0.017 (0.017) C24 * 0.009 (0.016) C25 * -0.006 (0.016) C26 * 0.033 (0.014) C27 * -0.005 (0.014) C28 * -0.020 (0.016) C29 * -0.009 (0.017) C30 * -0.011 (0.017) C31 * 0.039 (0.017) C32 * 0.005 (0.017) C33 * 0.012 (0.016) C34 0.101 (0.009) Cu1 0.014 (0.009) Cu2 Rms deviation of fitted atoms = 0.018 11.875 (0.035) x - 4.943 (0.060) y - 9.584 (0.063) z = 8.217 (0.044) Angle to previous plane (with approximate esd) = 80.93 ( 0.21 ) * 0.149 (0.006) Cl3 * -0.159 (0.006) N8 * 0.188 (0.007) N3_$2 * -0.179 (0.007) N4_$2 -0.031 (0.007) Cu2 -2.295 (0.016) N7 2.588 (0.017) Cl4 Rms deviation of fitted atoms = 0.169 12.079 (0.013) x - 3.282 (0.023) y - 11.550 (0.033) z = 8.790 (0.023) Angle to previous plane (with approximate esd) = 9.49 ( 0.41 ) * 0.048 (0.013) N1_$2 * 0.035 (0.013) N2_$2 * -0.039 (0.013) N3_$2 * 0.028 (0.014) N4_$2 * -0.002 (0.015) C1_$2 * -0.088 (0.015) C2_$2 * -0.066 (0.016) C3_$2 * 0.008 (0.016) C4_$2 * 0.075 (0.015) C5_$2 * 0.056 (0.015) C6_$2 * -0.048 (0.014) C7_$2 * -0.067 (0.015) C8_$2 * 0.023 (0.014) C9_$2 * 0.008 (0.016) C10_$2 * 0.051 (0.017) C11_$2 * 0.020 (0.016) C12_$2 * -0.020 (0.015) C13_$2 * -0.022 (0.015) C14_$2 Rms deviation of fitted atoms = 0.046 12.079 (0.013) x + 3.282 (0.023) y - 11.550 (0.033) z = 3.554 (0.019) Angle to previous plane (with approximate esd) = 31.49 ( 0.15 ) * -0.048 (0.013) N1 * -0.035 (0.013) N2 * 0.039 (0.013) N3 * -0.028 (0.014) N4 * 0.002 (0.015) C1 * 0.088 (0.015) C2 * 0.066 (0.016) C3 * -0.008 (0.016) C4 * -0.075 (0.015) C5 * -0.056 (0.015) C6 * 0.048 (0.014) C7 * 0.067 (0.015) C8 * -0.023 (0.014) C9 * -0.008 (0.016) C10 * -0.051 (0.017) C11 * -0.020 (0.016) C12 * 0.020 (0.015) C13 * 0.022 (0.015) C14 -0.073 (0.009) Cu1 0.056 (0.008) Cu2_$2 Rms deviation of fitted atoms = 0.046 5.959 (0.025) x - 2.505 (0.024) y + 17.267 (0.026) z = 4.688 (0.014) Angle to previous plane (with approximate esd) = 86.74 ( 0.13 ) * 0.018 (0.013) N5 * 0.006 (0.013) N6 * -0.029 (0.013) N7 * 0.002 (0.014) N8 * 0.008 (0.015) C21 * -0.010 (0.016) C22 * -0.024 (0.015) C23 * -0.017 (0.017) C24 * 0.009 (0.016) C25 * -0.006 (0.016) C26 * 0.033 (0.014) C27 * -0.005 (0.014) C28 * -0.020 (0.016) C29 * -0.009 (0.017) C30 * -0.011 (0.017) C31 * 0.039 (0.017) C32 * 0.005 (0.017) C33 * 0.012 (0.016) C34 0.101 (0.009) Cu1 0.014 (0.009) Cu2 Rms deviation of fitted atoms = 0.018 5.959 (0.025) x + 2.505 (0.024) y + 17.267 (0.026) z = 12.884 (0.014) Angle to previous plane (with approximate esd) = 23.90 ( 0.20 ) * -0.018 (0.013) N5_$2 * -0.006 (0.013) N6_$2 * 0.029 (0.013) N7_$2 * -0.002 (0.013) N8_$2 * -0.008 (0.015) C21_$2 * 0.010 (0.016) C22_$2 * 0.024 (0.015) C23_$2 * 0.017 (0.017) C24_$2 * -0.009 (0.016) C25_$2 * 0.006 (0.016) C26_$2 * -0.033 (0.014) C27_$2 * 0.005 (0.014) C28_$2 * 0.020 (0.016) C29_$2 * 0.009 (0.017) C30_$2 * 0.011 (0.017) C31_$2 * -0.039 (0.017) C32_$2 * -0.005 (0.017) C33_$2 * -0.012 (0.016) C34_$2 Rms deviation of fitted atoms = 0.018 ; "#===END" data_cupapsq _manuscript_identification_number_B0079831 # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, crystal structures and magnetic properties of one- and two-dimensional pap-containing copper(II) complexes (pap = pyrazino[2,3-f][4,7]-phenanthroline) ; loop_ _publ_author_name _publ_author_address 'Hilde Grove' ; Department of Chemistry University of Bergen N-5007 Bergen Norway ; 'Jorunn Sletten' ; Department of Chemistry University of Bergen N-5007 Bergen Norway ; 'Miguel Julve' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Juan Cano' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu4 (C14 H8 N4)4 (H2 O)4 (C4 O4)2]n (C4 O4)n (N O3)2n . 12n(H2 O)' _chemical_formula_analytical ? _chemical_formula_sum 'C68 H64 Cu4 N18 O34' _chemical_formula_weight 1931.52 _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' '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 'I 41 / a m d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z+1/2' 'x, -y, -z' 'y+1/4, x+3/4, -z+1/4' '-y+1/4, -x+1/4, -z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1/2' 'y+3/4, x+5/4, -z+3/4' '-y+3/4, -x+3/4, -z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z-1/2' '-x, y, z' '-y-1/4, -x-3/4, z-1/4' 'y-1/4, x-1/4, z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' '-y+1/4, -x-1/4, z+1/4' 'y+1/4, x+1/4, z-1/4' _cell_length_a 24.5977(13) _cell_length_b 24.5977(13) _cell_length_c 25.800(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15610.4(16) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description cube _exptl_crystal_colour brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method ? _exptl_crystal_F_000 7888 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type 'empirical, SADABS' _exptl_absorpt_correction_T_min 0.717843 _exptl_absorpt_correction_T_max 0.801481 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '2K SMART CCD' _diffrn_measurement_method \w _diffrn_standards_number '50 first frames remeasured at end of experiment' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46418 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3626 _reflns_number_observed 2409 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, version 4.0' _computing_cell_refinement 'SAINT, version 4.0' _computing_data_reduction 'SAINT, version 4.0' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, version 4.3, 1992' _computing_publication_material 'CIFTAB, Sheldrick, 1993' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 29 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2002P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom if bound to C, difmap if bound to O of coordinated water' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3597 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1337 _refine_ls_R_factor_obs 0.0932 _refine_ls_wR_factor_all 0.3437 _refine_ls_wR_factor_obs 0.3067 _refine_ls_goodness_of_fit_all 1.305 _refine_ls_goodness_of_fit_obs 1.469 _refine_ls_restrained_S_all 1.330 _refine_ls_restrained_S_obs 1.469 _refine_ls_shift/esd_max 0.787 _refine_ls_shift/esd_mean 0.028 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.35262(4) 0.39100(4) 0.40964(4) 0.0417(5) Uani 1 d . . C1 C 0.3592(4) 0.4221(4) 0.2980(4) 0.069(3) Uani 1 d . . H1 H 0.3215(4) 0.4214(4) 0.3001(4) 0.103 Uiso 1 calc R . C2 C 0.3814(5) 0.4342(4) 0.2517(4) 0.067(3) Uani 1 d . . H2 H 0.3595(5) 0.4411(4) 0.2230(4) 0.101 Uiso 1 calc R . C3 C 0.4376(6) 0.4361(3) 0.2479(4) 0.076(3) Uani 1 d . . H3 H 0.4536(6) 0.4447(3) 0.2163(4) 0.115 Uiso 1 calc R . C4 C 0.4715(3) 0.4250(3) 0.2921(3) 0.052(2) Uani 1 d . . C5 C 0.4424(4) 0.4125(3) 0.3388(3) 0.049(2) Uani 1 d . . C6 C 0.4716(3) 0.4002(3) 0.3845(3) 0.043(2) Uani 1 d . . C7 C 0.4724(3) 0.3751(3) 0.4693(3) 0.043(2) Uani 1 d . . H7 H 0.4543(3) 0.3661(3) 0.4998(3) 0.065 Uiso 1 calc R . C8 C 0.3641(3) 0.2790(3) 0.3499(3) 0.049(2) Uani 1 d . . H8 H 0.3702(3) 0.2976(3) 0.3191(3) 0.073 Uiso 1 calc R . C9 C 0.3439(3) 0.2788(3) 0.4365(3) 0.035(2) Uani 1 d . . C10 C 0.3327(3) 0.3078(3) 0.4838(3) 0.035(2) Uani 1 d . . C11 C 0.3220(3) 0.2793(3) 0.5296(3) 0.041(2) Uani 1 d . . C12 C 0.3107(3) 0.3119(3) 0.5739(3) 0.043(2) Uani 1 d . . H12 H 0.3037(3) 0.2953(3) 0.6055(3) 0.064 Uiso 1 calc R . C13 C 0.3100(3) 0.3653(4) 0.5704(3) 0.056(2) Uani 1 d . . H13 H 0.3024(3) 0.3859(4) 0.5998(3) 0.084 Uiso 1 calc R . C14 C 0.3208(3) 0.3920(3) 0.5228(3) 0.050(2) Uani 1 d . . H14 H 0.3196(3) 0.4298(3) 0.5207(3) 0.075 Uiso 1 calc R . C22 C 0.2306(4) 0.4231(4) 0.3795(3) 0.053(2) Uani 1 d . . C23 C 0.2308(3) 0.4808(3) 0.3750 0.042(3) Uani 1 d S . C24 C 0.1717(4) 0.4217(4) 0.3750 0.066(4) Uani 1 d S . C51 C 0.4705(3) 0.5107(3) 0.4734(2) 0.036(2) Uani 1 d . . N1 N 0.3866(3) 0.4112(3) 0.3405(2) 0.049(2) Uani 1 d . . N2 N 0.4431(3) 0.3874(2) 0.4279(3) 0.043(2) Uani 1 d . . N3 N 0.3556(2) 0.3067(2) 0.3932(2) 0.0406(15) Uani 1 d . . N4 N 0.3329(2) 0.3618(3) 0.4800(2) 0.0406(15) Uani 1 d . . O1 O 0.3425(2) 0.4697(2) 0.4326(2) 0.0537(15) Uani 1 d . . H15 H 0.3152(2) 0.4910(2) 0.4121(2) 0.081 Uiso 1 d R . H16 H 0.3736(2) 0.4879(2) 0.4355(2) 0.081 Uiso 1 d R . O2 O 0.2656(3) 0.3857(2) 0.3843(3) 0.065(2) Uani 1 d . . O3 O 0.2667(2) 0.5167(2) 0.3750 0.059(2) Uani 1 d S . O4 O 0.1351(3) 0.3851(3) 0.3750 0.108(5) Uani 1 d S . O5 O 0.4340(2) 0.5239(2) 0.4415(2) 0.0510(14) Uani 1 d . . O11 O 0.2328(5) 0.2705(5) 0.3874(5) 0.078(4) Uiso 0.50 d P . O12 O 0.1904(22) 0.3114(20) 0.2932(22) 0.374(28) Uiso 0.50 d P . O13 O 0.4583(12) 0.3418(14) 0.5870(12) 0.204(13) Uiso 0.50 d P . O14 O 0.2500 0.3610(11) 0.2500 0.233(10) Uiso 1 d S . O15 O 0.1025(15) 0.2724(17) 0.4057(13) 0.262(19) Uiso 0.50 d P . O16 O 0.1348(13) 0.3007(12) 0.2768(12) 0.189(12) Uiso 0.50 d P . 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 0.0482(7) 0.0318(6) 0.0450(7) -0.0002(4) -0.0057(4) 0.0011(4) C1 0.094(8) 0.059(6) 0.054(6) 0.003(5) -0.019(5) 0.003(5) C2 0.090(8) 0.058(6) 0.053(6) 0.011(4) -0.019(5) 0.006(5) C3 0.142(11) 0.040(5) 0.048(5) 0.008(4) -0.007(6) 0.005(6) C4 0.077(5) 0.027(4) 0.050(5) -0.001(3) -0.011(4) 0.001(4) C5 0.081(7) 0.027(4) 0.040(4) -0.002(3) -0.003(4) -0.005(4) C6 0.054(5) 0.027(4) 0.046(5) -0.009(3) -0.001(4) 0.007(3) C7 0.066(5) 0.028(4) 0.036(4) 0.002(3) 0.001(3) -0.001(3) C8 0.066(6) 0.047(4) 0.034(4) 0.007(3) 0.005(4) 0.002(4) C9 0.038(4) 0.033(4) 0.035(4) 0.002(3) -0.002(3) 0.006(3) C10 0.030(4) 0.031(4) 0.043(4) -0.003(3) 0.002(3) -0.001(3) C11 0.023(4) 0.055(4) 0.044(4) -0.001(3) 0.000(3) 0.001(3) C12 0.042(4) 0.048(5) 0.039(4) -0.009(3) 0.015(3) -0.003(3) C13 0.049(5) 0.070(6) 0.050(5) -0.024(4) 0.015(4) -0.007(4) C14 0.043(5) 0.043(5) 0.064(6) -0.016(4) -0.001(4) -0.004(3) C22 0.062(6) 0.052(5) 0.045(4) 0.002(4) -0.010(4) 0.000(4) C23 0.044(4) 0.044(4) 0.038(5) 0.006(3) -0.006(3) 0.004(5) C24 0.061(5) 0.061(5) 0.076(9) 0.019(5) -0.019(5) -0.009(7) C51 0.049(4) 0.029(4) 0.029(3) -0.001(3) 0.004(3) 0.000(3) N1 0.059(5) 0.039(4) 0.049(4) 0.005(3) -0.013(3) 0.001(3) N2 0.051(4) 0.032(3) 0.046(4) -0.003(3) 0.010(3) -0.007(3) N3 0.053(4) 0.028(3) 0.042(3) 0.006(3) 0.001(3) 0.001(3) N4 0.034(3) 0.045(4) 0.042(3) -0.009(3) 0.002(3) -0.007(3) O1 0.047(3) 0.050(3) 0.063(4) 0.007(3) -0.007(3) -0.001(3) O2 0.062(4) 0.047(4) 0.087(5) -0.001(3) -0.021(3) 0.007(3) O3 0.042(3) 0.042(3) 0.091(6) 0.007(3) -0.007(3) 0.005(4) O4 0.084(5) 0.084(5) 0.156(13) 0.050(6) -0.050(6) -0.031(6) O5 0.057(3) 0.058(4) 0.038(3) 0.008(2) -0.008(3) 0.001(3) _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 N4 2.011(6) . ? Cu1 N1 2.032(7) . ? Cu1 O1 2.040(6) . ? Cu1 N3 2.118(6) . ? Cu1 O2 2.242(6) . ? Cu1 N2 2.278(7) . ? C1 N1 1.312(11) . ? C1 C2 1.347(14) . ? C1 H1 0.93 . ? C2 C3 1.386(15) . ? C2 H2 0.93 . ? C3 C4 1.438(13) . ? C3 H3 0.93 . ? C4 C4 1.40(2) 22_655 ? C4 C5 1.435(11) . ? C5 N1 1.374(11) . ? C5 C6 1.414(11) . ? C6 N2 1.356(10) . ? C6 C6 1.40(2) 22_655 ? C7 N2 1.323(10) . ? C7 C7 1.36(2) 22_655 ? C7 H7 0.93 . ? C8 N3 1.326(10) . ? C8 C8 1.42(2) 29 ? C8 H8 0.93 . ? C9 N3 1.343(9) . ? C9 C9 1.415(14) 29 ? C9 C10 1.440(10) . ? C10 N4 1.331(9) . ? C10 C11 1.397(10) . ? C11 C12 1.424(10) . ? C11 C11 1.44(2) 29 ? C12 C13 1.316(12) . ? C12 H12 0.93 . ? C13 C14 1.419(12) . ? C13 H13 0.93 . ? C14 N4 1.364(10) . ? C14 H14 0.93 . ? C22 O2 1.267(10) . ? C22 C23 1.425(12) . ? C22 C24 1.453(13) . ? C23 O3 1.249(13) . ? C23 C22 1.425(12) 15_445 ? C24 O4 1.28(2) . ? C24 C22 1.453(13) 15_445 ? C51 O5 1.260(8) . ? C51 C51 1.450(14) 22_655 ? C51 C51 1.471(12) 6_566 ? O1 H15 1.00 . ? O1 H16 0.89 . ? O12 O16 1.46(5) . ? 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 N4 Cu1 N1 168.2(3) . . ? N4 Cu1 O1 92.8(2) . . ? N1 Cu1 O1 94.1(2) . . ? N4 Cu1 N3 80.7(2) . . ? N1 Cu1 N3 92.9(3) . . ? O1 Cu1 N3 172.6(2) . . ? N4 Cu1 O2 90.7(2) . . ? N1 Cu1 O2 98.6(3) . . ? O1 Cu1 O2 91.4(2) . . ? N3 Cu1 O2 85.2(2) . . ? N4 Cu1 N2 92.0(2) . . ? N1 Cu1 N2 77.8(3) . . ? O1 Cu1 N2 95.5(2) . . ? N3 Cu1 N2 88.3(2) . . ? O2 Cu1 N2 172.4(2) . . ? N1 C1 C2 125.3(10) . . ? N1 C1 H1 117.3(6) . . ? C2 C1 H1 117.3(6) . . ? C1 C2 C3 118.3(9) . . ? C1 C2 H2 120.9(6) . . ? C3 C2 H2 120.9(5) . . ? C2 C3 C4 121.0(9) . . ? C2 C3 H3 119.5(5) . . ? C4 C3 H3 119.5(6) . . ? C4 C4 C3 125.4(6) 22_655 . ? C4 C4 C5 119.9(5) 22_655 . ? C3 C4 C5 114.6(9) . . ? N1 C5 C6 118.4(7) . . ? N1 C5 C4 122.0(7) . . ? C6 C5 C4 119.6(8) . . ? N2 C6 C6 121.0(5) . 22_655 ? N2 C6 C5 118.5(8) . . ? C6 C6 C5 120.5(5) 22_655 . ? N2 C7 C7 122.9(4) . 22_655 ? N2 C7 H7 118.6(4) . . ? C7 C7 H7 118.525(7) 22_655 . ? N3 C8 C8 121.0(4) . 29 ? N3 C8 H8 119.5(4) . . ? C8 C8 H8 119.530(6) 29 . ? N3 C9 C9 120.8(4) . 29 ? N3 C9 C10 119.5(6) . . ? C9 C9 C10 119.7(4) 29 . ? N4 C10 C11 124.3(6) . . ? N4 C10 C9 115.5(6) . . ? C11 C10 C9 120.1(6) . . ? C10 C11 C12 115.6(7) . . ? C10 C11 C11 120.1(4) . 29 ? C12 C11 C11 124.3(4) . 29 ? C13 C12 C11 120.7(7) . . ? C13 C12 H12 119.7(5) . . ? C11 C12 H12 119.7(4) . . ? C12 C13 C14 121.2(7) . . ? C12 C13 H13 119.4(5) . . ? C14 C13 H13 119.4(5) . . ? N4 C14 C13 119.3(7) . . ? N4 C14 H14 120.4(5) . . ? C13 C14 H14 120.4(5) . . ? O2 C22 C23 136.8(9) . . ? O2 C22 C24 132.0(8) . . ? C23 C22 C24 91.2(7) . . ? O3 C23 C22 135.0(5) . 15_445 ? O3 C23 C22 135.0(5) . . ? C22 C23 C22 89.9(10) 15_445 . ? O4 C24 C22 136.1(5) . 15_445 ? O4 C24 C22 136.1(5) . . ? C22 C24 C22 87.8(10) 15_445 . ? O5 C51 C51 135.4(4) . 22_655 ? O5 C51 C51 134.6(4) . 6_566 ? C51 C51 C51 90.000(1) 22_655 6_566 ? C1 N1 C5 118.7(8) . . ? C1 N1 Cu1 124.9(7) . . ? C5 N1 Cu1 116.4(5) . . ? C7 N2 C6 116.1(7) . . ? C7 N2 Cu1 135.0(5) . . ? C6 N2 Cu1 108.9(5) . . ? C8 N3 C9 118.2(6) . . ? C8 N3 Cu1 132.7(5) . . ? C9 N3 Cu1 109.1(5) . . ? C10 N4 C14 118.8(7) . . ? C10 N4 Cu1 115.1(5) . . ? C14 N4 Cu1 126.0(5) . . ? Cu1 O1 H15 115.1(2) . . ? Cu1 O1 H16 113.5(2) . . ? H15 O1 H16 111.0 . . ? C22 O2 Cu1 129.4(6) . . ? _refine_diff_density_max 2.467 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.191 _operators_to_generate_equivalent_atoms ; $1 1-X, Y, Z $2 X, 0.5-Y, Z $3 -0.25+Y, 0.25+X, 0.75-Z $4 X, 1-Y, 1-Z $5 1-X, 0.5-Y,Z $6 1-X, 1-Y, 1-Z ; _possible_hydrogen_bonds ; Distance O..O 2.650 (0.006) O1 - O3 2.626 (0.008) O1 - O5 2.946 (0.013) O2 - O11 3.096 (0.052) O4 - O12 2.991 (0.041) O4 - O15 Distance H..O 1.655 (0.006) H15 - O3 1.738 (0.008) H16 - O5 Angle OHO 171.01 ( 0.31) O1 - H15 - O3 179.54 ( 0.41) O1 - H16 - O5 ; _Cu---Cu_distances ; 7.250 (0.002) Cu1 - Cu1_$1 6.936 (0.002) Cu1 - Cu1_$2 7.576 (0.002) Cu1 - Cu1_$3 10.034 (0.002) Cu1 - Cu1_$5 7.106 (0.002) Cu1 - Cu1_$4 10.152 (0.002) Cu1 - Cu1_$6 ; _Least-squares_planes_(x,y,z_in_crystal_coordinates)_and_deviations_from_them ; (* indicates atom used to define plane) 23.085 (0.020) x + 0.248 (0.049) y - 8.903 (0.056) z = 11.336 (0.040) * 0.107 (0.003) O1_$1 * -0.104 (0.003) N1_$1 * 0.116 (0.003) N3_$1 * -0.119 (0.003) N4_$1 Rms deviation of fitted atoms = 0.112 23.085 (0.020) x - 0.248 (0.049) y + 8.903 (0.056) z = 11.750 (0.025) Angle to previous plane (with approximate esd) = 40.39 ( 0.12 ) * -0.107 (0.003) O1 * 0.104 (0.003) N1 * -0.116 (0.003) N3 * 0.119 (0.003) N4 -0.059 (0.003) Cu1 -2.292 (0.007) O2 2.194 (0.008) N2 Rms deviation of fitted atoms = 0.112 23.085 (0.020) x + 0.248 (0.049) y + 8.903 (0.056) z = 11.873 (0.018) Angle to previous plane (with approximate esd) = 1.15 ( 0.21 ) * -0.107 (0.003) O1_$2 * 0.104 (0.003) N1_$2 * -0.116 (0.003) N3_$2 * 0.119 (0.003) N4_$2 Rms deviation of fitted atoms = 0.112 23.085 (0.020) x - 0.248 (0.049) y + 8.903 (0.056) z = 11.750 (0.025) Angle to previous plane (with approximate esd) = 1.15 ( 0.21 ) * -0.107 (0.003) O1 * 0.104 (0.003) N1 * -0.116 (0.003) N3 * 0.119 (0.003) N4 Rms deviation of fitted atoms = 0.112 - 0.248 (0.049) x + 23.085 (0.020) y - 8.903 (0.056) z = 10.906 (0.032) Angle to previous plane (with approximate esd) = 82.07 ( 0.17 ) * -0.107 (0.003) O1_$3 * 0.104 (0.003) N1_$3 * -0.116 (0.003) N3_$3 * 0.119 (0.003) N4_$3 Rms deviation of fitted atoms = 0.112 0.000 (0.000) x + 23.813 (0.008) y + 6.466 (0.033) z = 11.992 (0.009) Angle to previous plane (with approximate esd) = 34.71 ( 0.10 ) * 0.002 (0.006) N1 * 0.000 (0.005) N2 * -0.014 (0.009) C1 * -0.024 (0.008) C2 * -0.003 (0.008) C3 * 0.017 (0.007) C4 * 0.022 (0.007) C5 * 0.026 (0.006) C6 * -0.025 (0.005) C7 * 0.002 (0.006) N1_$1 * 0.000 (0.005) N2_$1 * -0.014 (0.009) C1_$1 * -0.024 (0.008) C2_$1 * -0.003 (0.008) C3_$1 * 0.017 (0.007) C4_$1 * 0.022 (0.007) C5_$1 * 0.026 (0.006) C6_$1 * -0.025 (0.005) C7_$1 -0.032 (0.003) Cu1 Rms deviation of fitted atoms = 0.018 23.085 (0.020) x - 0.248 (0.049) y + 8.903 (0.056) z = 11.750 (0.025) Angle to previous plane (with approximate esd) = 85.60 ( 0.12 ) * -0.107 (0.003) O1 * 0.104 (0.003) N1 * -0.116 (0.003) N3 * 0.119 (0.003) N4 Rms deviation of fitted atoms = 0.112 23.948 (0.008) x + 0.000 (0.001) y + 5.891 (0.033) z = 10.804 (0.014) Angle to previous plane (with approximate esd) = 7.01 ( 0.14 ) * 0.028 (0.006) N3 * -0.004 (0.006) N4 * -0.023 (0.006) C8 * 0.002 (0.006) C9 * 0.015 (0.007) C10 * 0.028 (0.006) C11 * 0.017 (0.006) C12 * -0.019 (0.007) C13 * -0.042 (0.008) C14 * 0.028 (0.006) N3_$2 * -0.004 (0.006) N4_$2 * -0.023 (0.006) C8_$2 * 0.002 (0.006) C9_$2 * 0.015 (0.007) C10_$2 * 0.028 (0.006) C11_$2 * 0.017 (0.006) C12_$2 * -0.019 (0.007) C13_$2 * -0.042 (0.008) C14_$2 Rms deviation of fitted atoms = 0.023 - 1.853 (0.047) x + 1.853 (0.047) y + 25.653 (0.008) z = 10.083 (0.009) Angle to previous plane (with approximate esd) = 81.16 ( 0.13 ) * -0.004 (0.003) O2 * 0.000 (0.000) O3 * 0.000 (0.000) O4 * 0.004 (0.003) O2_$3 * 0.008 (0.007) C22 * 0.000 (0.000) C23 * 0.000 (0.000) C24 * -0.008 (0.007) C22_$3 0.497 (0.010) Cu1 Rms deviation of fitted atoms = 0.004 23.085 (0.020) x - 0.248 (0.049) y + 8.903 (0.056) z = 11.750 (0.025) Angle to previous plane (with approximate esd) = 74.24 ( 0.17 ) * -0.107 (0.003) O1 * 0.104 (0.003) N1 * -0.116 (0.003) N3 * 0.119 (0.003) N4 Rms deviation of fitted atoms = 0.112 - 1.991 (0.134) x + 1.991 (0.134) y + 25.631 (0.023) z = 10.109 (0.025) Angle to previous plane (with approximate esd) = 74.57 ( 0.33 ) * 0.000 (0.000) C22 * 0.000 (0.000) C23 * 0.000 (0.000) C24 * 0.000 (0.000) C22_$3 -0.022 (0.019) O2 0.000 (0.000) O3 0.000 (0.000) O4 0.022 (0.019) O2_$3 0.467 (0.029) Cu1 Rms deviation of fitted atoms = 0.000 - 0.000 (0.000) x + 22.926 (0.028) y + 9.349 (0.075) z = 16.137 (0.024) Angle to previous plane (with approximate esd) = 64.19 ( 0.37 ) * 0.002 (0.003) O5 * -0.004 (0.006) C51 * 0.002 (0.003) O5_$1 * -0.004 (0.006) C51_$1 * -0.002 (0.003) O5_$4 * 0.004 (0.006) C51_$4 * -0.002 (0.003) O5_$6 * 0.004 (0.006) C51_$6 Rms deviation of fitted atoms = 0.003 ; "#===END"