Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yuan-Gen Yao' _publ_contact_author_email YYG@FJIRSM.AC.CN _publ_section_title ; Nanosized lanthanide oxide rods in I1O3 hybrid organic-inorganic frameworks involving in situ ligand synthesis ; loop_ _publ_author_name 'Yuan-Gen Yao.' 'Lan-Fen Chen.' 'Jian-Kai Cheng.' 'Zhao-Ji Li.' ; Ye-Yan Qin ; 'Guo-Qiang Ren.' 'Pei-Xiu Yin.' 'Jian Zhang.' # Attachment 'merge-cif.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 662586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10.67 Cu Dy2 N4 O12.83' _chemical_formula_weight 780.77 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, 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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -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' '-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' _cell_length_a 27.420(5) _cell_length_b 27.420(5) _cell_length_c 7.0011(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4558.5(17) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2079 _cell_measurement_theta_min 2.5731 _cell_measurement_theta_max 27.4449 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.1100 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3261 _exptl_absorpt_coefficient_mu 8.410 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.714 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4448 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.45 _reflns_number_total 2320 _reflns_number_gt 2054 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+100.0597P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2320 _refine_ls_number_parameters 153 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.001 _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 Dy1 Dy 0.747316(10) 0.341477(10) 0.11686(3) 0.01159(10) Uani 1 1 d . . . Cu1 Cu 1.0000 0.5000 0.0000 0.0505(4) Uani 1 2 d S . . C1 C 0.8389(2) 0.4344(2) -0.2100(7) 0.0160(10) Uani 1 1 d . . . C2 C 0.8884(2) 0.4505(3) -0.1032(8) 0.0224(12) Uani 1 1 d . . . C3 C 0.9430(3) 0.5091(3) -0.3489(10) 0.042(2) Uani 1 1 d . . . H3 H 0.9782 0.5335 -0.4007 0.050 Uiso 1 1 calc R . . C4 C 0.8948(3) 0.4950(3) -0.4506(9) 0.0318(16) Uani 1 1 d . . . H4 H 0.8979 0.5114 -0.5695 0.038 Uiso 1 1 calc R . . C5 C 0.8907(2) 0.4302(3) 0.0930(8) 0.0232(12) Uani 1 1 d . . . O1W O 0.8499(4) 0.5371(4) 0.1349(13) 0.084(2) Uani 1 1 d D . . H1WA H 0.870(5) 0.569(3) 0.09(2) 0.125 Uiso 1 1 d D . . H1WB H 0.821(4) 0.537(5) 0.18(2) 0.125 Uiso 1 1 d D . . O1 O 0.78863(15) 0.39875(16) -0.1584(5) 0.0160(8) Uani 1 1 d . . . O2 O 0.84631(17) 0.39762(19) 0.1767(6) 0.0245(9) Uani 1 1 d . . . O2W O 1.0026(10) 0.4173(7) -0.174(3) 0.104(7) Uani 0.53 1 d P . . O2W' O 0.9929(6) 0.3760(9) -0.169(3) 0.084(6) Uani 0.47 1 d P . . O3 O 0.93897(19) 0.4493(2) 0.1655(7) 0.0415(14) Uani 1 1 d . . . O4 O 0.6667 0.3333 0.0141(14) 0.033(2) Uani 1 3 d S . . H4A H 0.6667 0.3333 -0.1073 0.049 Uiso 1 3 d SR . . O5 O 0.75042(16) 0.42456(15) 0.2191(5) 0.0140(7) Uani 1 1 d . . . H5A H 0.7211 0.4162 0.2844 0.021 Uiso 1 1 d R . . O6 O 0.6667 0.3333 0.3333 0.026(5) Uani 0.50 6 d SP . . N1 N 0.8439(2) 0.4586(2) -0.3842(7) 0.0214(10) Uani 1 1 d . . . N2 N 0.9387(2) 0.4873(3) -0.1752(8) 0.0325(14) Uani 1 1 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 Dy1 0.01170(14) 0.01106(13) 0.01224(14) -0.00097(8) -0.00258(8) 0.00587(10) Cu1 0.0074(5) 0.0824(11) 0.0334(7) 0.0265(7) -0.0035(5) 0.0013(6) C1 0.016(3) 0.018(3) 0.014(2) -0.003(2) -0.002(2) 0.009(2) C2 0.012(3) 0.028(3) 0.019(3) 0.003(2) -0.002(2) 0.003(2) C3 0.019(3) 0.050(5) 0.031(4) 0.018(3) 0.000(3) -0.001(3) C4 0.017(3) 0.040(4) 0.023(3) 0.017(3) 0.002(2) 0.002(3) C5 0.017(3) 0.030(3) 0.016(3) 0.002(2) -0.002(2) 0.007(3) O1W 0.078(6) 0.100(7) 0.067(5) -0.005(5) 0.011(4) 0.041(5) O1 0.0085(17) 0.0207(19) 0.0140(18) 0.0019(15) 0.0003(14) 0.0037(15) O2 0.0135(19) 0.034(2) 0.020(2) 0.0059(18) 0.0005(16) 0.0075(18) O2W 0.152(19) 0.057(10) 0.105(13) 0.014(10) 0.054(13) 0.053(12) O2W' 0.033(8) 0.091(13) 0.084(12) 0.007(11) -0.004(7) -0.002(9) O3 0.014(2) 0.065(4) 0.027(2) 0.018(2) -0.0033(18) 0.006(2) O4 0.0046(18) 0.0046(18) 0.089(7) 0.000 0.000 0.0023(9) O5 0.0150(18) 0.0138(18) 0.0128(17) -0.0006(14) 0.0025(14) 0.0068(15) O6 0.028(7) 0.028(7) 0.023(10) 0.000 0.000 0.014(3) N1 0.013(2) 0.023(3) 0.020(2) 0.005(2) -0.0019(19) 0.004(2) N2 0.010(2) 0.046(3) 0.025(3) 0.010(2) 0.000(2) 0.001(2) _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 Dy1 O4 2.228(3) . ? Dy1 O5 2.334(4) 17 ? Dy1 O5 2.348(4) . ? Dy1 O1 2.384(4) . ? Dy1 O2 2.395(4) . ? Dy1 O5 2.415(4) 3_665 ? Dy1 N1 2.538(5) 17_554 ? Dy1 O6 2.5956(7) . ? Dy1 O1 2.599(4) 17_554 ? Dy1 C1 3.016(5) 17_554 ? Dy1 Dy1 3.6522(8) 3_665 ? Dy1 Dy1 3.6522(8) 2_655 ? Cu1 O3 1.936(5) . ? Cu1 O3 1.936(5) 10_765 ? Cu1 N2 1.966(5) . ? Cu1 N2 1.966(5) 10_765 ? C1 O1 1.281(7) . ? C1 N1 1.361(7) . ? C1 C2 1.413(8) . ? C1 Dy1 3.015(5) 18_544 ? C2 N2 1.335(7) . ? C2 C5 1.495(8) . ? C3 N2 1.334(9) . ? C3 C4 1.376(9) . ? C3 H3 0.9300 . ? C4 N1 1.330(7) . ? C4 H4 0.9300 . ? C5 O2 1.239(7) . ? C5 O3 1.262(7) . ? O1W H1WA 0.83(8) . ? O1W H1WB 0.85(13) . ? O1 Dy1 2.599(4) 18_544 ? O2W O2W' 1.03(2) . ? O4 Dy1 2.228(3) 3_665 ? O4 Dy1 2.228(3) 2_655 ? O4 H4A 0.8499 . ? O5 Dy1 2.334(4) 18_545 ? O5 Dy1 2.415(4) 2_655 ? O5 H5A 0.8502 . ? O6 Dy1 2.5967(5) 3_665 ? O6 Dy1 2.5958(7) 17 ? O6 Dy1 2.5967(5) 18_545 ? O6 Dy1 2.5980(7) 16_655 ? O6 Dy1 2.5978(7) 2_655 ? N1 Dy1 2.538(5) 18_544 ? 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 Dy1 O5 116.1(3) . 17 ? O4 Dy1 O5 75.43(14) . . ? O5 Dy1 O5 76.17(11) 17 . ? O4 Dy1 O1 85.8(2) . . ? O5 Dy1 O1 141.89(13) 17 . ? O5 Dy1 O1 80.37(13) . . ? O4 Dy1 O2 150.47(12) . . ? O5 Dy1 O2 74.12(13) 17 . ? O5 Dy1 O2 80.99(14) . . ? O1 Dy1 O2 72.86(13) . . ? O4 Dy1 O5 74.09(14) . 3_665 ? O5 Dy1 O5 74.89(11) 17 3_665 ? O5 Dy1 O5 122.00(17) . 3_665 ? O1 Dy1 O5 143.15(12) . 3_665 ? O2 Dy1 O5 134.61(13) . 3_665 ? O4 Dy1 N1 130.72(17) . 17_554 ? O5 Dy1 N1 94.21(14) 17 17_554 ? O5 Dy1 N1 152.88(15) . 17_554 ? O1 Dy1 N1 93.21(15) . 17_554 ? O2 Dy1 N1 71.95(16) . 17_554 ? O5 Dy1 N1 78.17(15) 3_665 17_554 ? O4 Dy1 O6 54.5(2) . . ? O5 Dy1 O6 61.60(9) 17 . ? O5 Dy1 O6 61.43(9) . . ? O1 Dy1 O6 129.21(9) . . ? O2 Dy1 O6 126.59(10) . . ? O5 Dy1 O6 60.64(9) 3_665 . ? N1 Dy1 O6 135.77(12) 17_554 . ? O4 Dy1 O1 82.2(2) . 17_554 ? O5 Dy1 O1 138.80(12) 17 17_554 ? O5 Dy1 O1 144.81(12) . 17_554 ? O1 Dy1 O1 71.06(5) . 17_554 ? O2 Dy1 O1 108.66(14) . 17_554 ? O5 Dy1 O1 75.80(12) 3_665 17_554 ? N1 Dy1 O1 51.58(13) 17_554 17_554 ? O6 Dy1 O1 124.11(9) . 17_554 ? O4 Dy1 C1 106.3(2) . 17_554 ? O5 Dy1 C1 118.60(14) 17 17_554 ? O5 Dy1 C1 160.06(14) . 17_554 ? O1 Dy1 C1 79.97(14) . 17_554 ? O2 Dy1 C1 90.08(15) . 17_554 ? O5 Dy1 C1 76.70(14) 3_665 17_554 ? N1 Dy1 C1 26.64(15) 17_554 17_554 ? O6 Dy1 C1 136.13(10) . 17_554 ? O1 Dy1 C1 25.00(13) 17_554 17_554 ? O4 Dy1 Dy1 34.95(12) . 3_665 ? O5 Dy1 Dy1 95.78(9) 17 3_665 ? O5 Dy1 Dy1 96.81(9) . 3_665 ? O1 Dy1 Dy1 116.64(9) . 3_665 ? O2 Dy1 Dy1 169.90(10) . 3_665 ? O5 Dy1 Dy1 39.27(9) 3_665 3_665 ? N1 Dy1 Dy1 109.49(12) 17_554 3_665 ? O6 Dy1 Dy1 45.313(7) . 3_665 ? O1 Dy1 Dy1 78.82(9) 17_554 3_665 ? C1 Dy1 Dy1 94.92(11) 17_554 3_665 ? O4 Dy1 Dy1 34.95(12) . 2_655 ? O5 Dy1 Dy1 96.85(9) 17 2_655 ? O5 Dy1 Dy1 40.61(9) . 2_655 ? O1 Dy1 Dy1 83.90(9) . 2_655 ? O2 Dy1 Dy1 120.30(11) . 2_655 ? O5 Dy1 Dy1 95.59(9) 3_665 2_655 ? N1 Dy1 Dy1 165.43(11) 17_554 2_655 ? O6 Dy1 Dy1 45.343(7) . 2_655 ? O1 Dy1 Dy1 114.29(8) 17_554 2_655 ? C1 Dy1 Dy1 139.28(11) 17_554 2_655 ? Dy1 Dy1 Dy1 60.0 3_665 2_655 ? O3 Cu1 O3 180.0(4) . 10_765 ? O3 Cu1 N2 83.7(2) . . ? O3 Cu1 N2 96.3(2) 10_765 . ? O3 Cu1 N2 96.3(2) . 10_765 ? O3 Cu1 N2 83.7(2) 10_765 10_765 ? N2 Cu1 N2 180.0(4) . 10_765 ? O1 C1 N1 115.5(5) . . ? O1 C1 C2 126.1(5) . . ? N1 C1 C2 118.4(5) . . ? O1 C1 Dy1 59.0(3) . 18_544 ? N1 C1 Dy1 56.7(3) . 18_544 ? C2 C1 Dy1 173.5(4) . 18_544 ? N2 C2 C1 120.3(5) . . ? N2 C2 C5 114.1(5) . . ? C1 C2 C5 125.6(5) . . ? N2 C3 C4 119.3(6) . . ? N2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? N1 C4 C3 122.0(6) . . ? N1 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? O2 C5 O3 123.9(5) . . ? O2 C5 C2 119.6(5) . . ? O3 C5 C2 116.5(5) . . ? H1WA O1W H1WB 106(12) . . ? C1 O1 Dy1 135.0(3) . . ? C1 O1 Dy1 96.0(3) . 18_544 ? Dy1 O1 Dy1 128.83(15) . 18_544 ? C5 O2 Dy1 140.3(4) . . ? C5 O3 Cu1 114.1(4) . . ? Dy1 O4 Dy1 110.1(2) . 3_665 ? Dy1 O4 Dy1 110.1(2) . 2_655 ? Dy1 O4 Dy1 110.1(2) 3_665 2_655 ? Dy1 O4 H4A 108.8 . . ? Dy1 O4 H4A 108.8 3_665 . ? Dy1 O4 H4A 108.8 2_655 . ? Dy1 O5 Dy1 104.08(14) 18_545 . ? Dy1 O5 Dy1 102.05(14) 18_545 2_655 ? Dy1 O5 Dy1 100.11(14) . 2_655 ? Dy1 O5 H5A 52.0 18_545 . ? Dy1 O5 H5A 109.3 . . ? Dy1 O5 H5A 50.0 2_655 . ? Dy1 O6 Dy1 89.414(14) . 3_665 ? Dy1 O6 Dy1 90.684(14) . 17 ? Dy1 O6 Dy1 90.656(14) 3_665 17 ? Dy1 O6 Dy1 90.654(14) . 18_545 ? Dy1 O6 Dy1 180.0 3_665 18_545 ? Dy1 O6 Dy1 89.393(14) 17 18_545 ? Dy1 O6 Dy1 180.0 . 16_655 ? Dy1 O6 Dy1 90.606(14) 3_665 16_655 ? Dy1 O6 Dy1 89.374(14) 17 16_655 ? Dy1 O6 Dy1 89.336(14) 18_545 16_655 ? Dy1 O6 Dy1 89.374(14) . 2_655 ? Dy1 O6 Dy1 89.364(14) 3_665 2_655 ? Dy1 O6 Dy1 180.0 17 2_655 ? Dy1 O6 Dy1 90.602(14) 18_545 2_655 ? Dy1 O6 Dy1 90.578(14) 16_655 2_655 ? C4 N1 C1 119.3(5) . . ? C4 N1 Dy1 143.9(4) . 18_544 ? C1 N1 Dy1 96.7(3) . 18_544 ? C3 N2 C2 120.6(5) . . ? C3 N2 Cu1 127.8(4) . . ? C2 N2 Cu1 111.5(4) . . ? 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 O5 H5A O5 0.85 2.06 2.888(5) 165.8 18_545 O4 H4A O4 0.85 1.68 2.53(2) 180.0 16_654 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.241 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.187 #=================================================END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 662587' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10.67 Cu Ho2 N4 O12.83' _chemical_formula_weight 785.63 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, 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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -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' '-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' _cell_length_a 27.3601(8) _cell_length_b 27.3601(8) _cell_length_c 6.9815(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4526.0(3) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4424 _cell_measurement_theta_min 2.5787 _cell_measurement_theta_max 27.4565 _exptl_crystal_description Prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.0900 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3279 _exptl_absorpt_coefficient_mu 8.908 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.592 _exptl_absorpt_correction_T_max 0.641 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11900 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0168 _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 2.58 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2308 _reflns_number_gt 2188 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+169.7845P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2308 _refine_ls_number_parameters 153 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _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 Ho1 Ho 0.413866(9) 0.674776(9) 0.44994(3) 0.01257(9) Uani 1 1 d . . . Cu1 Cu 0.6667 0.8333 0.3333 0.0508(4) Uani 1 2 d S . . C1 C 0.5051(2) 0.7676(2) 0.1230(8) 0.0185(10) Uani 1 1 d . . . C2 C 0.5548(2) 0.7839(3) 0.2303(8) 0.0251(12) Uani 1 1 d . . . C3 C 0.6096(3) 0.8427(3) -0.0167(11) 0.044(2) Uani 1 1 d . . . H3 H 0.6448 0.8674 -0.0684 0.053 Uiso 1 1 calc R . . C4 C 0.5611(3) 0.8283(3) -0.1191(10) 0.0368(17) Uani 1 1 d . . . H4 H 0.5641 0.8443 -0.2390 0.044 Uiso 1 1 calc R . . C5 C 0.5570(2) 0.7640(3) 0.4265(9) 0.0261(12) Uani 1 1 d . . . O1 O 0.45446(15) 0.73165(16) 0.1750(5) 0.0174(7) Uani 1 1 d . . . O1W O 0.5371(4) 0.6874(4) 0.8670(13) 0.083(2) Uani 1 1 d D . . H1WB H 0.555(5) 0.715(4) 0.787(16) 0.125 Uiso 1 1 d D . . H1WA H 0.565(4) 0.690(6) 0.931(17) 0.125 Uiso 1 1 d D . . O2 O 0.51270(17) 0.73094(19) 0.5113(6) 0.0274(9) Uani 1 1 d . . . O2W O 0.6592(6) 0.7069(7) 0.167(3) 0.090(5) Uani 0.55 1 d P . . O2W' O 0.6704(10) 0.7499(7) 0.164(3) 0.094(7) Uani 0.45 1 d P . . O3 O 0.60550(19) 0.7823(3) 0.4997(7) 0.0453(14) Uani 1 1 d . . . O4 O 0.3333 0.6667 0.3465(14) 0.032(2) Uani 1 3 d S . . H4A H 0.3333 0.6667 0.2247 0.049 Uiso 1 3 d SR . . O5 O 0.34098(14) 0.58382(15) 0.5531(5) 0.0135(7) Uani 1 1 d . . . H5A H 0.3169 0.5875 0.6188 0.020 Uiso 1 1 d R . . O6 O 0.3333 0.6667 0.6667 0.033(5) Uani 0.50 6 d SP . . N1 N 0.51006(19) 0.7920(2) -0.0512(7) 0.0227(10) Uani 1 1 d . . . N2 N 0.6053(2) 0.8208(3) 0.1569(8) 0.0350(13) Uani 1 1 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 Ho1 0.01291(12) 0.01219(12) 0.01302(13) -0.00095(8) -0.00264(8) 0.00658(9) Cu1 0.0092(5) 0.0806(10) 0.0350(7) 0.0239(7) -0.0035(4) 0.0019(6) C1 0.016(2) 0.019(2) 0.019(3) -0.003(2) -0.002(2) 0.008(2) C2 0.014(3) 0.035(3) 0.021(3) 0.003(2) -0.001(2) 0.008(2) C3 0.015(3) 0.055(5) 0.036(4) 0.019(3) 0.001(3) -0.001(3) C4 0.018(3) 0.046(4) 0.026(3) 0.014(3) -0.001(2) 0.000(3) C5 0.015(3) 0.033(3) 0.024(3) 0.002(2) -0.001(2) 0.008(2) O1 0.0111(16) 0.0225(19) 0.0149(18) 0.0003(14) 0.0010(13) 0.0057(15) O1W 0.098(6) 0.091(6) 0.069(5) 0.015(4) 0.007(5) 0.054(5) O2 0.0141(19) 0.037(2) 0.025(2) 0.0029(18) 0.0010(16) 0.0082(18) O2W 0.046(7) 0.067(9) 0.117(13) 0.015(9) -0.009(8) -0.002(7) O2W' 0.134(18) 0.044(9) 0.100(14) 0.009(9) 0.054(13) 0.041(11) O3 0.013(2) 0.070(4) 0.031(3) 0.015(2) -0.0043(18) 0.005(2) O4 0.0050(17) 0.0050(17) 0.087(7) 0.000 0.000 0.0025(9) O5 0.0121(16) 0.0159(17) 0.0122(17) 0.0006(13) 0.0006(13) 0.0068(14) O6 0.033(7) 0.033(7) 0.033(12) 0.000 0.000 0.017(4) N1 0.014(2) 0.025(2) 0.021(2) 0.0028(19) -0.0030(18) 0.0039(19) N2 0.016(2) 0.049(3) 0.028(3) 0.010(2) -0.002(2) 0.007(2) _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 Ho1 O4 2.222(3) . ? Ho1 O5 2.323(4) 15_556 ? Ho1 O5 2.337(3) 2_665 ? Ho1 O1 2.369(4) . ? Ho1 O2 2.388(4) . ? Ho1 O5 2.393(3) . ? Ho1 N1 2.521(5) 14_455 ? Ho1 O1 2.582(4) 14_455 ? Ho1 O6 2.5905(3) . ? Ho1 C1 2.998(5) 14_455 ? Ho1 Ho1 3.6395(4) 3_565 ? Ho1 Ho1 3.6395(4) 2_665 ? Cu1 O3 1.939(5) 16_665 ? Cu1 O3 1.939(5) . ? Cu1 N2 1.969(5) 16_665 ? Cu1 N2 1.969(5) . ? C1 O1 1.287(7) . ? C1 N1 1.362(7) . ? C1 C2 1.414(8) . ? C1 Ho1 2.998(5) 15 ? C2 N2 1.340(8) . ? C2 C5 1.487(8) . ? C3 N2 1.332(9) . ? C3 C4 1.380(9) . ? C3 H3 0.9300 . ? C4 N1 1.331(8) . ? C4 H4 0.9300 . ? C5 O2 1.242(7) . ? C5 O3 1.267(7) . ? O1 Ho1 2.582(4) 15 ? O1W H1WB 0.87(10) . ? O1W H1WA 0.86(14) . ? O2W O2W' 1.06(2) . ? O4 Ho1 2.222(3) 2_665 ? O4 Ho1 2.222(3) 3_565 ? O4 H4A 0.8500 . ? O5 Ho1 2.323(4) 14_456 ? O5 Ho1 2.337(3) 3_565 ? O5 H5A 0.8499 . ? O6 Ho1 2.5883(3) 2_665 ? O6 Ho1 2.5882(3) 13_566 ? O6 Ho1 2.5893(2) 15_556 ? O6 Ho1 2.5904(3) 14_456 ? O6 Ho1 2.5893(2) 3_565 ? N1 Ho1 2.521(5) 15 ? 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 Ho1 O5 115.8(3) . 15_556 ? O4 Ho1 O5 75.15(14) . 2_665 ? O5 Ho1 O5 75.68(10) 15_556 2_665 ? O4 Ho1 O1 85.3(2) . . ? O5 Ho1 O1 142.22(12) 15_556 . ? O5 Ho1 O1 80.70(13) 2_665 . ? O4 Ho1 O2 150.45(12) . . ? O5 Ho1 O2 74.18(13) 15_556 . ? O5 Ho1 O2 81.27(14) 2_665 . ? O1 Ho1 O2 73.41(14) . . ? O4 Ho1 O5 74.03(14) . . ? O5 Ho1 O5 74.61(10) 15_556 . ? O5 Ho1 O5 121.13(16) 2_665 . ? O1 Ho1 O5 143.15(12) . . ? O2 Ho1 O5 134.60(14) . . ? O4 Ho1 N1 130.90(17) . 14_455 ? O5 Ho1 N1 94.60(14) 15_556 14_455 ? O5 Ho1 N1 153.01(14) 2_665 14_455 ? O1 Ho1 N1 93.30(15) . 14_455 ? O2 Ho1 N1 71.82(16) . 14_455 ? O5 Ho1 N1 78.74(15) . 14_455 ? O4 Ho1 O1 81.8(2) . 14_455 ? O5 Ho1 O1 139.36(12) 15_556 14_455 ? O5 Ho1 O1 144.63(12) 2_665 14_455 ? O1 Ho1 O1 70.85(5) . 14_455 ? O2 Ho1 O1 109.12(14) . 14_455 ? O5 Ho1 O1 76.19(12) . 14_455 ? N1 Ho1 O1 52.08(13) 14_455 14_455 ? O4 Ho1 O6 54.7(2) . . ? O5 Ho1 O6 61.09(9) 15_556 . ? O5 Ho1 O6 60.93(9) 2_665 . ? O1 Ho1 O6 128.99(9) . . ? O2 Ho1 O6 126.28(11) . . ? O5 Ho1 O6 60.27(8) . . ? N1 Ho1 O6 135.91(12) 14_455 . ? O1 Ho1 O6 123.98(8) 14_455 . ? O4 Ho1 C1 106.2(2) . 14_455 ? O5 Ho1 C1 119.05(14) 15_556 14_455 ? O5 Ho1 C1 160.45(14) 2_665 14_455 ? O1 Ho1 C1 80.00(14) . 14_455 ? O2 Ho1 C1 90.30(15) . 14_455 ? O5 Ho1 C1 77.10(13) . 14_455 ? N1 Ho1 C1 26.84(15) 14_455 14_455 ? O1 Ho1 C1 25.29(13) 14_455 14_455 ? O6 Ho1 C1 136.17(10) . 14_455 ? O4 Ho1 Ho1 35.02(12) . 3_565 ? O5 Ho1 Ho1 95.47(9) 15_556 3_565 ? O5 Ho1 Ho1 96.33(9) 2_665 3_565 ? O1 Ho1 Ho1 116.29(9) . 3_565 ? O2 Ho1 Ho1 169.64(10) . 3_565 ? O5 Ho1 Ho1 39.13(8) . 3_565 ? N1 Ho1 Ho1 109.77(12) 14_455 3_565 ? O1 Ho1 Ho1 78.65(8) 14_455 3_565 ? O6 Ho1 Ho1 45.359(1) . 3_565 ? C1 Ho1 Ho1 94.93(10) 14_455 3_565 ? O4 Ho1 Ho1 35.02(12) . 2_665 ? O5 Ho1 Ho1 96.37(9) 15_556 2_665 ? O5 Ho1 Ho1 40.26(9) 2_665 2_665 ? O1 Ho1 Ho1 83.64(9) . 2_665 ? O2 Ho1 Ho1 120.18(11) . 2_665 ? O5 Ho1 Ho1 95.31(8) . 2_665 ? N1 Ho1 Ho1 165.66(11) 14_455 2_665 ? O1 Ho1 Ho1 113.98(8) 14_455 2_665 ? O6 Ho1 Ho1 45.329(1) . 2_665 ? C1 Ho1 Ho1 139.26(11) 14_455 2_665 ? Ho1 Ho1 Ho1 60.0 3_565 2_665 ? O3 Cu1 O3 179.996(2) 16_665 . ? O3 Cu1 N2 84.0(2) 16_665 16_665 ? O3 Cu1 N2 96.0(2) . 16_665 ? O3 Cu1 N2 96.0(2) 16_665 . ? O3 Cu1 N2 84.0(2) . . ? N2 Cu1 N2 179.997(1) 16_665 . ? O1 C1 N1 115.5(5) . . ? O1 C1 C2 126.2(5) . . ? N1 C1 C2 118.3(5) . . ? O1 C1 Ho1 59.0(3) . 15 ? N1 C1 Ho1 56.7(3) . 15 ? C2 C1 Ho1 173.3(4) . 15 ? N2 C2 C1 120.1(5) . . ? N2 C2 C5 114.3(5) . . ? C1 C2 C5 125.6(5) . . ? N2 C3 C4 119.2(6) . . ? N2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? N1 C4 C3 121.9(6) . . ? N1 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? O2 C5 O3 123.0(6) . . ? O2 C5 C2 120.1(5) . . ? O3 C5 C2 116.9(5) . . ? C1 O1 Ho1 134.6(3) . . ? C1 O1 Ho1 95.7(3) . 15 ? Ho1 O1 Ho1 129.49(15) . 15 ? H1WB O1W H1WA 100(13) . . ? C5 O2 Ho1 139.7(4) . . ? C5 O3 Cu1 113.5(4) . . ? Ho1 O4 Ho1 110.0(2) 2_665 3_565 ? Ho1 O4 Ho1 110.0(2) 2_665 . ? Ho1 O4 Ho1 110.0(2) 3_565 . ? Ho1 O4 H4A 109.0 2_665 . ? Ho1 O4 H4A 109.0 3_565 . ? Ho1 O4 H4A 109.0 . . ? Ho1 O5 Ho1 104.49(14) 14_456 3_565 ? Ho1 O5 Ho1 102.74(13) 14_456 . ? Ho1 O5 Ho1 100.62(13) 3_565 . ? Ho1 O5 H5A 53.6 14_456 . ? Ho1 O5 H5A 50.9 3_565 . ? Ho1 O5 H5A 109.3 . . ? Ho1 O6 Ho1 90.746(1) 2_665 13_566 ? Ho1 O6 Ho1 90.726(1) 2_665 15_556 ? Ho1 O6 Ho1 89.330(1) 13_566 15_556 ? Ho1 O6 Ho1 180.0 2_665 14_456 ? Ho1 O6 Ho1 89.302(1) 13_566 14_456 ? Ho1 O6 Ho1 89.283(1) 15_556 14_456 ? Ho1 O6 Ho1 89.322(1) 2_665 3_565 ? Ho1 O6 Ho1 90.718(1) 13_566 3_565 ? Ho1 O6 Ho1 180.0 15_556 3_565 ? Ho1 O6 Ho1 90.668(1) 14_456 3_565 ? Ho1 O6 Ho1 89.302(1) 2_665 . ? Ho1 O6 Ho1 180.0 13_566 . ? Ho1 O6 Ho1 90.680(1) 15_556 . ? Ho1 O6 Ho1 90.650(1) 14_456 . ? Ho1 O6 Ho1 89.272(1) 3_565 . ? C4 N1 C1 119.6(5) . . ? C4 N1 Ho1 143.9(4) . 15 ? C1 N1 Ho1 96.5(3) . 15 ? C3 N2 C2 120.8(5) . . ? C3 N2 Cu1 128.0(4) . . ? C2 N2 Cu1 111.1(4) . . ? 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 O4 H4A O4 0.85 1.66 2.51(2) 180.0 13_565 O5 H5A O5 0.85 2.03 2.859(5) 166.4 14_456 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.924 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.166 #=================================================END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 662588' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10.67 Cu Er2 N4 O12.83' _chemical_formula_weight 790.29 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, 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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -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' '-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' _cell_length_a 27.294(4) _cell_length_b 27.294(4) _cell_length_c 6.9565(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4488.1(12) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4334 _cell_measurement_theta_min 3.0523 _cell_measurement_theta_max 27.4719 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3297 _exptl_absorpt_coefficient_mu 9.465 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.623 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8065 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2288 _reflns_number_gt 2098 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+82.5678P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2288 _refine_ls_number_parameters 153 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Er1 Er 0.747263(9) 0.341704(9) 0.11645(3) 0.01071(10) Uani 1 1 d . . . Cu1 Cu 1.0000 0.5000 0.0000 0.0483(4) Uani 1 2 d S . . O1 O 0.78788(14) 0.39840(15) -0.1586(5) 0.0151(7) Uani 1 1 d . . . O1W O 0.8707(4) 0.3548(4) 0.5347(11) 0.078(2) Uani 1 1 d D . . H1WA H 0.880(7) 0.384(3) 0.475(15) 0.118 Uiso 1 1 d D . . H1WB H 0.861(7) 0.360(5) 0.642(9) 0.118 Uiso 1 1 d D . . O2 O 0.84571(16) 0.39787(18) 0.1785(6) 0.0236(8) Uani 1 1 d . . . O3 O 0.93860(19) 0.4494(2) 0.1673(7) 0.0412(13) Uani 1 1 d . . . O6 O 0.6667 0.3333 0.3333 0.030(5) Uani 0.50 6 d SP . . O5 O 0.75692(15) 0.34114(14) 0.4457(5) 0.0126(7) Uani 1 1 d . . . H5A H 0.7883 0.3458 0.4793 0.019 Uiso 1 1 d R . . N1 N 0.84315(19) 0.4587(2) -0.3853(7) 0.0204(9) Uani 1 1 d . . . N2 N 0.9385(2) 0.4874(3) -0.1773(8) 0.0315(13) Uani 1 1 d . . . C1 C 0.8378(2) 0.4342(2) -0.2103(8) 0.0150(9) Uani 1 1 d . . . C2 C 0.8880(2) 0.4507(3) -0.1031(8) 0.0219(11) Uani 1 1 d . . . C3 C 0.9420(3) 0.5095(3) -0.3500(10) 0.0387(18) Uani 1 1 d . . . H3 H 0.9771 0.5348 -0.4017 0.046 Uiso 1 1 calc R . . C4 C 0.8934(3) 0.4947(3) -0.4530(9) 0.0317(15) Uani 1 1 d . . . H4 H 0.8963 0.5107 -0.5734 0.038 Uiso 1 1 calc R . . C5 C 0.8896(2) 0.4305(3) 0.0954(8) 0.0235(12) Uani 1 1 d . . . O4 O 0.6667 0.3333 0.0159(15) 0.032(2) Uani 1 3 d S . . H4A H 0.6667 0.3333 -0.1063 0.048 Uiso 1 3 d SR . . O2W O 0.9971(10) 0.5836(7) -0.825(3) 0.093(6) Uani 0.50 1 d P . . O2W' O 1.0082(6) 0.6234(8) -0.835(3) 0.090(6) Uani 0.50 1 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 Er1 0.01107(13) 0.01056(13) 0.01077(15) -0.00085(7) -0.00238(7) 0.00562(9) Cu1 0.0076(5) 0.0797(10) 0.0311(6) 0.0243(6) -0.0029(4) 0.0019(5) O1 0.0068(15) 0.0196(17) 0.0140(18) -0.0012(14) -0.0003(12) 0.0030(14) O1W 0.105(7) 0.089(6) 0.051(4) 0.013(4) 0.010(4) 0.056(5) O2 0.0111(17) 0.032(2) 0.020(2) 0.0040(17) 0.0003(15) 0.0050(16) O3 0.013(2) 0.066(4) 0.025(2) 0.015(2) -0.0028(17) 0.005(2) O6 0.033(7) 0.033(7) 0.024(11) 0.000 0.000 0.017(4) O5 0.0118(16) 0.0134(17) 0.0122(17) 0.0009(12) 0.0014(13) 0.0060(14) N1 0.011(2) 0.022(2) 0.019(2) 0.0012(18) -0.0045(17) 0.0018(18) N2 0.012(2) 0.045(3) 0.023(3) 0.012(2) 0.0003(19) 0.003(2) C1 0.010(2) 0.018(2) 0.015(2) -0.0021(19) -0.0019(18) 0.0060(19) C2 0.012(2) 0.030(3) 0.017(3) 0.000(2) -0.003(2) 0.005(2) C3 0.013(3) 0.051(4) 0.029(3) 0.019(3) 0.005(2) -0.002(3) C4 0.022(3) 0.039(4) 0.023(3) 0.013(3) -0.001(2) 0.007(3) C5 0.016(3) 0.033(3) 0.017(3) 0.002(2) 0.000(2) 0.009(2) O4 0.0071(18) 0.0071(18) 0.082(7) 0.000 0.000 0.0036(9) O2W 0.135(17) 0.044(8) 0.095(13) 0.010(9) 0.045(12) 0.042(10) O2W' 0.048(8) 0.081(12) 0.080(11) -0.001(10) -0.002(7) -0.014(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 Er1 O4 2.209(3) . ? Er1 O5 2.307(4) . ? Er1 O5 2.326(3) 18_545 ? Er1 O1 2.360(4) . ? Er1 O2 2.374(4) . ? Er1 O5 2.387(3) 17 ? Er1 N1 2.513(4) 17_554 ? Er1 O1 2.576(4) 17_554 ? Er1 O6 2.5805(5) . ? Er1 C1 2.980(5) 17_554 ? Er1 Er1 3.6286(6) 3_665 ? Er1 Er1 3.6286(6) 2_655 ? Cu1 O3 1.938(5) 10_765 ? Cu1 O3 1.938(5) . ? Cu1 N2 1.969(5) . ? Cu1 N2 1.969(5) 10_765 ? O1 C1 1.269(6) . ? O1 Er1 2.576(4) 18_544 ? O1W H1WA 0.82(8) . ? O1W H1WB 0.83(9) . ? O2 C5 1.223(7) . ? O3 C5 1.270(7) . ? O6 Er1 2.5829(5) 16_655 ? O6 Er1 2.5817(3) 18_545 ? O6 Er1 2.5817(3) 3_665 ? O6 Er1 2.5827(4) 2_655 ? O6 Er1 2.5807(3) 17 ? O5 Er1 2.327(3) 17 ? O5 Er1 2.386(3) 18_545 ? O5 H5A 0.8354 . ? N1 C4 1.311(8) . ? N1 C1 1.361(7) . ? N1 Er1 2.513(4) 18_544 ? N2 C3 1.326(8) . ? N2 C2 1.339(7) . ? C1 C2 1.420(7) . ? C1 Er1 2.979(5) 18_544 ? C2 C5 1.496(8) . ? C3 C4 1.379(9) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? O4 Er1 2.209(3) 3_665 ? O4 Er1 2.209(3) 2_655 ? O4 H4A 0.8499 . ? O2W O2W' 0.97(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 O4 Er1 O5 115.2(3) . . ? O4 Er1 O5 74.96(14) . 18_545 ? O5 Er1 O5 75.43(11) . 18_545 ? O4 Er1 O1 85.9(2) . . ? O5 Er1 O1 142.35(12) . . ? O5 Er1 O1 81.14(13) 18_545 . ? O4 Er1 O2 150.63(12) . . ? O5 Er1 O2 74.19(13) . . ? O5 Er1 O2 81.31(14) 18_545 . ? O1 Er1 O2 73.45(13) . . ? O4 Er1 O5 73.75(14) . 17 ? O5 Er1 O5 74.28(11) . 17 ? O5 Er1 O5 120.64(17) 18_545 17 ? O1 Er1 O5 143.34(12) . 17 ? O2 Er1 O5 134.50(13) . 17 ? O4 Er1 N1 131.12(17) . 17_554 ? O5 Er1 N1 94.52(14) . 17_554 ? O5 Er1 N1 153.18(14) 18_545 17_554 ? O1 Er1 N1 93.33(15) . 17_554 ? O2 Er1 N1 71.98(16) . 17_554 ? O5 Er1 N1 78.73(15) 17 17_554 ? O4 Er1 O1 82.3(2) . 17_554 ? O5 Er1 O1 139.16(11) . 17_554 ? O5 Er1 O1 145.03(12) 18_545 17_554 ? O1 Er1 O1 70.95(5) . 17_554 ? O2 Er1 O1 109.30(13) . 17_554 ? O5 Er1 O1 76.26(12) 17 17_554 ? N1 Er1 O1 52.04(13) 17_554 17_554 ? O4 Er1 O6 54.2(2) . . ? O5 Er1 O6 60.94(9) . . ? O5 Er1 O6 60.71(9) 18_545 . ? O1 Er1 O6 129.19(9) . . ? O2 Er1 O6 126.16(10) . . ? O5 Er1 O6 60.01(9) 17 . ? N1 Er1 O6 135.67(12) 17_554 . ? O1 Er1 O6 123.87(8) 17_554 . ? O4 Er1 C1 106.4(2) . 17_554 ? O5 Er1 C1 119.17(13) . 17_554 ? O5 Er1 C1 160.76(13) 18_545 17_554 ? O1 Er1 C1 79.84(13) . 17_554 ? O2 Er1 C1 90.52(15) . 17_554 ? O5 Er1 C1 77.28(13) 17 17_554 ? N1 Er1 C1 27.03(15) 17_554 17_554 ? O1 Er1 C1 25.07(13) 17_554 17_554 ? O6 Er1 C1 136.05(10) . 17_554 ? O4 Er1 Er1 34.77(12) . 3_665 ? O5 Er1 Er1 95.31(9) . 3_665 ? O5 Er1 Er1 96.23(9) 18_545 3_665 ? O1 Er1 Er1 116.41(8) . 3_665 ? O2 Er1 Er1 169.50(10) . 3_665 ? O5 Er1 Er1 39.06(8) 17 3_665 ? N1 Er1 Er1 109.59(11) 17_554 3_665 ? O1 Er1 Er1 78.55(8) 17_554 3_665 ? O6 Er1 Er1 45.352(1) . 3_665 ? C1 Er1 Er1 94.77(10) 17_554 3_665 ? O4 Er1 Er1 34.77(12) . 2_655 ? O5 Er1 Er1 96.28(9) . 2_655 ? O5 Er1 Er1 40.27(9) 18_545 2_655 ? O1 Er1 Er1 83.84(9) . 2_655 ? O2 Er1 Er1 120.20(11) . 2_655 ? O5 Er1 Er1 95.13(8) 17 2_655 ? N1 Er1 Er1 165.64(11) 17_554 2_655 ? O1 Er1 Er1 114.04(8) 17_554 2_655 ? O6 Er1 Er1 45.382(1) . 2_655 ? C1 Er1 Er1 139.11(10) 17_554 2_655 ? Er1 Er1 Er1 60.0 3_665 2_655 ? O3 Cu1 O3 180.0(5) 10_765 . ? O3 Cu1 N2 96.1(2) 10_765 . ? O3 Cu1 N2 83.9(2) . . ? O3 Cu1 N2 83.9(2) 10_765 10_765 ? O3 Cu1 N2 96.1(2) . 10_765 ? N2 Cu1 N2 180.0(4) . 10_765 ? C1 O1 Er1 134.9(3) . . ? C1 O1 Er1 95.5(3) . 18_544 ? Er1 O1 Er1 129.28(14) . 18_544 ? H1WA O1W H1WB 105(12) . . ? C5 O2 Er1 139.9(4) . . ? C5 O3 Cu1 114.4(4) . . ? Er1 O6 Er1 89.264(11) 16_655 18_545 ? Er1 O6 Er1 180.0 16_655 . ? Er1 O6 Er1 90.732(11) 18_545 . ? Er1 O6 Er1 90.684(11) 16_655 3_665 ? Er1 O6 Er1 180.0 18_545 3_665 ? Er1 O6 Er1 89.332(11) . 3_665 ? Er1 O6 Er1 90.662(11) 16_655 2_655 ? Er1 O6 Er1 90.682(11) 18_545 2_655 ? Er1 O6 Er1 89.296(11) . 2_655 ? Er1 O6 Er1 89.276(11) 3_665 2_655 ? Er1 O6 Er1 89.296(11) 16_655 17 ? Er1 O6 Er1 89.314(11) 18_545 17 ? Er1 O6 Er1 90.746(11) . 17 ? Er1 O6 Er1 90.734(11) 3_665 17 ? Er1 O6 Er1 180.0 2_655 17 ? Er1 O5 Er1 104.91(14) . 17 ? Er1 O5 Er1 103.01(14) . 18_545 ? Er1 O5 Er1 100.68(13) 17 18_545 ? Er1 O5 H5A 112.9 . . ? Er1 O5 H5A 119.1 17 . ? Er1 O5 H5A 114.4 18_545 . ? C4 N1 C1 120.3(5) . . ? C4 N1 Er1 143.7(4) . 18_544 ? C1 N1 Er1 96.0(3) . 18_544 ? C3 N2 C2 120.1(5) . . ? C3 N2 Cu1 128.9(4) . . ? C2 N2 Cu1 111.0(4) . . ? O1 C1 N1 116.2(4) . . ? O1 C1 C2 126.1(5) . . ? N1 C1 C2 117.7(5) . . ? O1 C1 Er1 59.4(3) . 18_544 ? N1 C1 Er1 57.0(3) . 18_544 ? C2 C1 Er1 173.2(4) . 18_544 ? N2 C2 C1 120.3(5) . . ? N2 C2 C5 114.9(5) . . ? C1 C2 C5 124.7(5) . . ? N2 C3 C4 119.9(6) . . ? N2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? N1 C4 C3 121.7(6) . . ? N1 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? O2 C5 O3 124.0(6) . . ? O2 C5 C2 120.4(5) . . ? O3 C5 C2 115.7(5) . . ? Er1 O4 Er1 110.5(2) . 3_665 ? Er1 O4 Er1 110.5(2) . 2_655 ? Er1 O4 Er1 110.5(2) 3_665 2_655 ? Er1 O4 H4A 108.5 . . ? Er1 O4 H4A 108.5 3_665 . ? Er1 O4 H4A 108.5 2_655 . ? 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 O4 H4A O4 0.85 1.69 2.54(2) 180.0 16_654 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.047 _refine_diff_density_min -1.359 _refine_diff_density_rms 0.247 #End of Crystallographic Information File