# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H22 Cl2 Dy N O9' _chemical_formula_weight 497.66 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' Dy Dy -0.1892 4.4098 '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 9.118(2) _cell_length_b 15.223(4) _cell_length_c 12.154(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.432(5) _cell_angle_gamma 90.00 _cell_volume 1590.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description strip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 5.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0974 _exptl_absorpt_correction_T_max 0.3025 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8705 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3395 _reflns_number_gt 2560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0612P)^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 _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3395 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _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 0.74577(3) 0.009940(19) 0.25298(2) 0.01167(12) Uani 1 1 d . . . Cl1 Cl 0.78104(18) 0.17959(10) 0.32655(13) 0.0209(3) Uani 1 1 d . . . Cl2 Cl 1.29600(18) -0.56679(10) 0.37105(12) 0.0207(3) Uani 1 1 d . . . O1 O 0.5894(5) -0.0833(3) 0.0984(3) 0.0148(9) Uani 1 1 d . . . O1W O 0.8935(5) 0.0174(3) 0.1293(4) 0.0225(10) Uani 1 1 d . . . H1WB H 0.9785 -0.0101 0.1412 0.027 Uiso 1 1 d R . . H1WA H 0.8531 0.0507 0.0710 0.027 Uiso 1 1 d R . . O2 O 0.4114(4) -0.0914(3) -0.0823(3) 0.0143(9) Uani 1 1 d . . . O2W O 0.5082(5) 0.0121(3) 0.2863(4) 0.0209(10) Uani 1 1 d . . . H2WA H 0.4785 0.0584 0.3117 0.025 Uiso 1 1 d R . . H2WB H 0.4512 -0.0336 0.2729 0.025 Uiso 1 1 d R . . O3 O 1.0174(5) 0.0099(3) 0.3623(3) 0.0174(10) Uani 1 1 d . . . O3W O 0.7921(5) -0.1383(3) 0.2955(4) 0.0245(10) Uani 1 1 d . . . H3WA H 0.8438 -0.1543 0.3645 0.029 Uiso 1 1 d R . . H3WB H 0.7574 -0.1764 0.2421 0.029 Uiso 1 1 d R . . O4 O 1.2013(5) 0.0076(3) 0.5381(3) 0.0149(9) Uani 1 1 d . . . O4W O 1.0888(5) -0.4066(3) 0.0492(4) 0.0242(10) Uani 1 1 d . . . H4WA H 1.1484 -0.4420 0.0303 0.029 Uiso 1 1 d R . . O5W O 0.8923(6) -0.2316(3) 0.4909(4) 0.0240(10) Uani 1 1 d . . . H5WA H 0.8408 -0.2788 0.4861 0.029 Uiso 1 1 d R . . H5WB H 0.9658 -0.2194 0.5534 0.029 Uiso 1 1 d R . . N1 N 0.8035(7) -0.2427(3) -0.1335(5) 0.0178(12) Uani 1 1 d . . . C1 C 0.4999(6) -0.0517(4) 0.0043(4) 0.0138(13) Uani 1 1 d . . . C2 C 1.0637(8) 0.0053(4) 0.4705(5) 0.0165(13) Uani 1 1 d . . . C3 C 0.8747(8) -0.2178(5) -0.2246(5) 0.0256(15) Uani 1 1 d . . . H3A H 0.8290 -0.1625 -0.2617 0.038 Uiso 1 1 calc R . . H3B H 0.8542 -0.2642 -0.2837 0.038 Uiso 1 1 calc R . . H3C H 0.9872 -0.2104 -0.1876 0.038 Uiso 1 1 calc R . . C4 C 0.6323(8) -0.2548(4) -0.1903(6) 0.0252(16) Uani 1 1 d . . . H4A H 0.5851 -0.1992 -0.2251 0.038 Uiso 1 1 calc R . . H4B H 0.5865 -0.2736 -0.1317 0.038 Uiso 1 1 calc R . . H4C H 0.6130 -0.2997 -0.2513 0.038 Uiso 1 1 calc R . . C5 C 0.8296(8) -0.1698(4) -0.0451(6) 0.0263(16) Uani 1 1 d . . . H5A H 0.7754 -0.1167 -0.0835 0.040 Uiso 1 1 calc R . . H5B H 0.9412 -0.1576 -0.0113 0.040 Uiso 1 1 calc R . . H5C H 0.7891 -0.1875 0.0168 0.040 Uiso 1 1 calc R . . C6 C 0.8703(7) -0.3285(4) -0.0741(5) 0.0172(13) Uani 1 1 d . . . H6A H 0.8237 -0.3411 -0.0129 0.021 Uiso 1 1 calc R . . H6B H 0.8392 -0.3764 -0.1323 0.021 Uiso 1 1 calc R . . C7 C 1.0460(7) -0.3293(4) -0.0189(6) 0.0240(15) Uani 1 1 d . . . H7A H 1.0952 -0.3285 -0.0802 0.029 Uiso 1 1 calc R . . H7B H 1.0811 -0.2767 0.0310 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01193(19) 0.01309(19) 0.00917(18) -0.00003(10) 0.00244(13) -0.00002(11) Cl1 0.0294(9) 0.0146(7) 0.0174(7) -0.0006(6) 0.0061(6) -0.0016(7) Cl2 0.0185(8) 0.0273(9) 0.0155(7) -0.0033(6) 0.0047(6) 0.0008(7) O1 0.016(2) 0.016(2) 0.009(2) -0.0002(16) 0.0004(17) 0.0004(18) O1W 0.013(2) 0.037(3) 0.016(2) 0.0066(19) 0.0025(19) 0.007(2) O2 0.015(2) 0.015(2) 0.011(2) -0.0011(16) 0.0014(17) 0.0001(17) O2W 0.021(3) 0.022(2) 0.023(3) -0.0043(18) 0.010(2) -0.0035(19) O3 0.016(2) 0.026(3) 0.009(2) -0.0010(16) 0.0031(18) -0.0011(19) O3W 0.034(3) 0.014(2) 0.017(2) -0.0003(18) -0.002(2) 0.004(2) O4 0.012(2) 0.019(2) 0.011(2) -0.0011(16) 0.0010(18) 0.0000(18) O4W 0.025(3) 0.028(3) 0.023(2) 0.008(2) 0.012(2) 0.010(2) O5W 0.027(3) 0.020(2) 0.022(2) 0.0046(18) 0.004(2) -0.002(2) N1 0.025(3) 0.013(3) 0.018(3) 0.0016(19) 0.010(2) 0.002(2) C1 0.005(3) 0.025(4) 0.012(3) -0.003(2) 0.003(2) -0.002(3) C2 0.027(4) 0.008(3) 0.014(3) -0.001(2) 0.006(3) 0.002(3) C3 0.030(4) 0.028(4) 0.023(4) 0.006(3) 0.015(3) -0.002(3) C4 0.015(4) 0.030(4) 0.030(4) 0.000(3) 0.006(3) 0.001(3) C5 0.034(4) 0.016(3) 0.027(4) -0.007(3) 0.008(3) 0.000(3) C6 0.020(3) 0.014(3) 0.022(3) -0.002(2) 0.013(3) -0.002(3) C7 0.021(3) 0.025(4) 0.029(4) 0.003(3) 0.011(3) 0.000(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 Dy1 O3W 2.321(4) . ? Dy1 O1W 2.331(4) . ? Dy1 O2W 2.333(4) . ? Dy1 O3 2.389(4) . ? Dy1 O1 2.407(4) . ? Dy1 O2 2.432(4) 3_655 ? Dy1 O4 2.437(4) 3_756 ? Dy1 Cl1 2.7169(16) . ? O1 C1 1.259(6) . ? O1W H1WB 0.8500 . ? O1W H1WA 0.8500 . ? O2 C1 1.248(6) . ? O2 Dy1 2.432(4) 3_655 ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3 C2 1.242(7) . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? O4 C2 1.251(8) . ? O4 Dy1 2.437(4) 3_756 ? O4W C7 1.417(7) . ? O4W H4WA 0.8500 . ? O5W H5WA 0.8501 . ? O5W H5WB 0.8499 . ? N1 C4 1.494(9) . ? N1 C3 1.506(7) . ? N1 C5 1.507(7) . ? N1 C6 1.519(7) . ? C1 C1 1.579(13) 3_655 ? C2 C2 1.563(13) 3_756 ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.517(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? 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 O3W Dy1 O1W 95.14(15) . . ? O3W Dy1 O2W 94.91(15) . . ? O1W Dy1 O2W 151.71(17) . . ? O3W Dy1 O3 78.36(15) . . ? O1W Dy1 O3 69.15(15) . . ? O2W Dy1 O3 138.94(15) . . ? O3W Dy1 O1 67.48(14) . . ? O1W Dy1 O1 81.09(14) . . ? O2W Dy1 O1 78.49(14) . . ? O3 Dy1 O1 132.00(13) . . ? O3W Dy1 O2 134.18(14) . 3_655 ? O1W Dy1 O2 74.22(14) . 3_655 ? O2W Dy1 O2 79.82(14) . 3_655 ? O3 Dy1 O2 132.99(13) . 3_655 ? O1 Dy1 O2 66.87(14) . 3_655 ? O3W Dy1 O4 72.75(14) . 3_756 ? O1W Dy1 O4 136.11(15) . 3_756 ? O2W Dy1 O4 72.18(15) . 3_756 ? O3 Dy1 O4 67.12(14) . 3_756 ? O1 Dy1 O4 127.52(13) . 3_756 ? O2 Dy1 O4 143.22(13) 3_655 3_756 ? O3W Dy1 Cl1 149.06(11) . . ? O1W Dy1 Cl1 97.77(11) . . ? O2W Dy1 Cl1 86.83(11) . . ? O3 Dy1 Cl1 80.19(10) . . ? O1 Dy1 Cl1 142.37(10) . . ? O2 Dy1 Cl1 76.58(10) 3_655 . ? O4 Dy1 Cl1 78.49(10) 3_756 . ? C1 O1 Dy1 121.4(4) . . ? Dy1 O1W H1WB 123.8 . . ? Dy1 O1W H1WA 112.6 . . ? H1WB O1W H1WA 123.6 . . ? C1 O2 Dy1 120.4(4) . 3_655 ? Dy1 O2W H2WA 120.1 . . ? Dy1 O2W H2WB 119.9 . . ? H2WA O2W H2WB 120.0 . . ? C2 O3 Dy1 120.9(4) . . ? Dy1 O3W H3WA 120.0 . . ? Dy1 O3W H3WB 120.1 . . ? H3WA O3W H3WB 120.0 . . ? C2 O4 Dy1 119.3(4) . 3_756 ? C7 O4W H4WA 116.4 . . ? H5WA O5W H5WB 120.0 . . ? C4 N1 C3 109.4(5) . . ? C4 N1 C5 108.3(5) . . ? C3 N1 C5 109.5(5) . . ? C4 N1 C6 107.8(5) . . ? C3 N1 C6 111.3(5) . . ? C5 N1 C6 110.6(5) . . ? O2 C1 O1 128.6(6) . . ? O2 C1 C1 116.1(6) . 3_655 ? O1 C1 C1 115.3(6) . 3_655 ? O3 C2 O4 127.4(6) . . ? O3 C2 C2 116.7(7) . 3_756 ? O4 C2 C2 115.9(7) . 3_756 ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 N1 114.5(5) . . ? C7 C6 H6A 108.6 . . ? N1 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? N1 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O4W C7 C6 108.0(5) . . ? O4W C7 H7A 110.1 . . ? C6 C7 H7A 110.1 . . ? O4W C7 H7B 110.1 . . ? C6 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3W Dy1 O1 C1 -176.8(4) . . . . ? O1W Dy1 O1 C1 -77.4(4) . . . . ? O2W Dy1 O1 C1 82.9(4) . . . . ? O3 Dy1 O1 C1 -128.6(4) . . . . ? O2 Dy1 O1 C1 -0.8(4) 3_655 . . . ? O4 Dy1 O1 C1 139.6(4) 3_756 . . . ? Cl1 Dy1 O1 C1 13.8(5) . . . . ? O3W Dy1 O3 C2 -79.0(4) . . . . ? O1W Dy1 O3 C2 -179.2(4) . . . . ? O2W Dy1 O3 C2 5.0(5) . . . . ? O1 Dy1 O3 C2 -123.6(4) . . . . ? O2 Dy1 O3 C2 139.7(4) 3_655 . . . ? O4 Dy1 O3 C2 -3.0(4) 3_756 . . . ? Cl1 Dy1 O3 C2 78.6(4) . . . . ? Dy1 O2 C1 O1 -179.3(4) 3_655 . . . ? Dy1 O2 C1 C1 0.9(7) 3_655 . . 3_655 ? Dy1 O1 C1 O2 -179.2(4) . . . . ? Dy1 O1 C1 C1 0.7(7) . . . 3_655 ? Dy1 O3 C2 O4 -177.4(4) . . . . ? Dy1 O3 C2 C2 3.0(8) . . . 3_756 ? Dy1 O4 C2 O3 -177.3(4) 3_756 . . . ? Dy1 O4 C2 C2 2.4(8) 3_756 . . 3_756 ? C4 N1 C6 C7 176.0(5) . . . . ? C3 N1 C6 C7 56.1(7) . . . . ? C5 N1 C6 C7 -65.9(6) . . . . ? N1 C6 C7 O4W 170.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.976 _refine_diff_density_min -2.426 _refine_diff_density_rms 0.247 _database_code_depnum_ccdc_archive 'CCDC 942168' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H22 Cl2 Er N O9' _chemical_formula_weight 502.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -9.4367 3.9380 '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 9.0957(2) _cell_length_b 15.1667(3) _cell_length_c 12.0825(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.627(2) _cell_angle_gamma 90.00 _cell_volume 1569.96(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description strip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 13.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0321 _exptl_absorpt_correction_T_max 0.0954 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4795 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.86 _diffrn_reflns_theta_max 61.17 _reflns_number_total 2355 _reflns_number_gt 2141 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0530P)^2^+8.9737P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00223(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2355 _refine_ls_number_parameters 185 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 0.791 _refine_ls_restrained_S_all 0.790 _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 0.74581(3) 0.009718(17) 0.25300(2) 0.00866(15) Uani 1 1 d . . . Cl1 Cl 0.78169(12) 0.17866(7) 0.32462(9) 0.0165(3) Uani 1 1 d . . . Cl2 Cl 1.29560(12) -0.56627(7) 0.37089(9) 0.0167(3) Uani 1 1 d . . . O1 O 0.5895(3) -0.08304(19) 0.0989(2) 0.0135(7) Uani 1 1 d . . . O1W O 0.8908(4) 0.0164(2) 0.1295(3) 0.0202(8) Uani 1 1 d . . . H1WB H 0.9757 -0.0111 0.1413 0.024 Uiso 1 1 d R . . H1WA H 0.8504 0.0497 0.0711 0.024 Uiso 1 1 d R . . O2 O 0.4110(3) -0.09152(19) -0.0821(2) 0.0126(7) Uani 1 1 d . . . O2W O 0.5101(4) 0.0119(2) 0.2861(3) 0.0158(7) Uani 1 1 d . . . H2WA H 0.4804 0.0583 0.3115 0.019 Uiso 1 1 d R . . H2WB H 0.4531 -0.0337 0.2727 0.019 Uiso 1 1 d R . . O3 O 1.0177(4) 0.0094(2) 0.3615(3) 0.0160(7) Uani 1 1 d . . . O3W O 0.7931(4) -0.1376(2) 0.2956(3) 0.0203(7) Uani 1 1 d . . . H3WA H 0.8449 -0.1537 0.3646 0.024 Uiso 1 1 d R . . H3WB H 0.7585 -0.1758 0.2422 0.024 Uiso 1 1 d R . . O4 O 1.2028(3) 0.00751(18) 0.5392(3) 0.0108(7) Uani 1 1 d . . . O4W O 1.0879(4) -0.4072(2) 0.0499(3) 0.0210(7) Uani 1 1 d . . . H4WA H 1.1476 -0.4426 0.0310 0.025 Uiso 1 1 d R . . O5W O 0.8912(4) -0.2312(2) 0.4902(3) 0.0205(7) Uani 1 1 d . . . H5WA H 0.8397 -0.2785 0.4854 0.025 Uiso 1 1 d R . . H5WB H 0.9648 -0.2190 0.5527 0.025 Uiso 1 1 d R . . N1 N 0.8037(4) -0.2424(2) -0.1321(3) 0.0141(8) Uani 1 1 d U . . C1 C 0.5000(4) -0.0510(3) 0.0050(3) 0.0102(9) Uani 1 1 d . . . C2 C 1.0635(5) 0.0049(3) 0.4704(4) 0.0102(10) Uani 1 1 d . . . C3 C 0.8751(6) -0.2185(4) -0.2237(4) 0.0248(11) Uani 1 1 d . . . H3A H 0.8251 -0.1651 -0.2651 0.037 Uiso 1 1 calc R . . H3B H 0.8597 -0.2671 -0.2799 0.037 Uiso 1 1 calc R . . H3C H 0.9871 -0.2078 -0.1857 0.037 Uiso 1 1 calc R . . C4 C 0.6301(6) -0.2538(3) -0.1921(5) 0.0242(12) Uani 1 1 d . . . H4A H 0.5843 -0.1979 -0.2279 0.036 Uiso 1 1 calc R . . H4B H 0.5823 -0.2719 -0.1341 0.036 Uiso 1 1 calc R . . H4C H 0.6112 -0.2991 -0.2531 0.036 Uiso 1 1 calc R . . C5 C 0.8296(6) -0.1704(3) -0.0442(4) 0.0231(11) Uani 1 1 d U . . H5A H 0.7787 -0.1164 -0.0833 0.035 Uiso 1 1 calc R . . H5B H 0.9419 -0.1598 -0.0076 0.035 Uiso 1 1 calc R . . H5C H 0.7853 -0.1874 0.0162 0.035 Uiso 1 1 calc R . . C6 C 0.8695(5) -0.3291(3) -0.0738(4) 0.0139(9) Uani 1 1 d . . . H6A H 0.8240 -0.3419 -0.0117 0.017 Uiso 1 1 calc R . . H6B H 0.8368 -0.3768 -0.1329 0.017 Uiso 1 1 calc R . . C7 C 1.0467(5) -0.3299(3) -0.0194(4) 0.0220(11) Uani 1 1 d . . . H7A H 1.0949 -0.3304 -0.0817 0.026 Uiso 1 1 calc R . . H7B H 1.0834 -0.2769 0.0300 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0086(2) 0.0084(2) 0.0096(2) -0.00005(9) 0.00379(13) 0.00008(9) Cl1 0.0221(6) 0.0097(5) 0.0169(5) -0.0007(4) 0.0056(4) -0.0013(4) Cl2 0.0132(5) 0.0214(6) 0.0157(6) -0.0025(4) 0.0054(4) 0.0006(4) O1 0.0162(16) 0.0104(15) 0.0122(16) 0.0005(13) 0.0025(13) 0.0011(12) O1W 0.0149(17) 0.033(2) 0.0166(18) 0.0069(14) 0.0097(14) 0.0071(14) O2 0.0135(15) 0.0121(16) 0.0098(15) -0.0022(13) 0.0008(12) -0.0004(12) O2W 0.0101(16) 0.0192(17) 0.0195(18) -0.0062(13) 0.0067(14) -0.0037(12) O3 0.0139(17) 0.0244(18) 0.0115(19) 0.0013(13) 0.0065(14) 0.0008(13) O3W 0.0293(18) 0.0103(16) 0.0134(16) 0.0008(13) -0.0031(14) 0.0029(14) O4 0.0074(16) 0.0137(16) 0.0107(16) 0.0019(12) 0.0024(13) -0.0005(11) O4W 0.0223(17) 0.0195(17) 0.0281(19) 0.0067(14) 0.0175(14) 0.0114(14) O5W 0.0194(18) 0.0144(16) 0.0242(19) 0.0037(14) 0.0025(15) 0.0010(13) N1 0.0134(11) 0.0142(12) 0.0152(12) 0.0003(8) 0.0057(9) -0.0006(8) C1 0.012(2) 0.010(2) 0.012(2) -0.0007(17) 0.007(2) -0.0010(16) C2 0.013(2) 0.007(2) 0.013(3) 0.0001(16) 0.007(2) -0.0003(16) C3 0.029(3) 0.028(3) 0.023(3) 0.006(2) 0.016(2) 0.000(2) C4 0.011(2) 0.034(3) 0.027(3) -0.003(2) 0.005(2) -0.001(2) C5 0.0233(13) 0.0218(14) 0.0242(14) -0.0009(9) 0.0079(9) 0.0007(9) C6 0.016(2) 0.011(2) 0.019(2) 0.0000(18) 0.0101(19) -0.0020(18) C7 0.015(2) 0.021(3) 0.029(3) 0.005(2) 0.007(2) 0.002(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 Er1 O3W 2.301(3) . ? Er1 O1W 2.302(3) . ? Er1 O2W 2.310(3) . ? Er1 O3 2.378(3) . ? Er1 O1 2.385(3) . ? Er1 O2 2.421(3) 3_655 ? Er1 O4 2.409(3) 3_756 ? Er1 Cl1 2.6890(10) . ? O1 C1 1.252(5) . ? O1W H1WB 0.8474 . ? O1W H1WA 0.8449 . ? O2 C1 1.252(5) . ? O2 Er1 2.421(3) 3_655 ? O2W H2WA 0.8470 . ? O2W H2WB 0.8469 . ? O3 C2 1.242(6) . ? O3W H3WA 0.8441 . ? O3W H3WB 0.8453 . ? O4 C2 1.261(5) . ? O4 Er1 2.409(3) 3_756 ? O4W C7 1.416(6) . ? O4W H4WA 0.8476 . ? O5W H5WA 0.8472 . ? O5W H5WB 0.8443 . ? N1 C4 1.510(6) . ? N1 C5 1.485(6) . ? N1 C3 1.503(6) . ? N1 C6 1.516(6) . ? C1 C1 1.551(9) 3_655 ? C2 C2 1.556(9) 3_756 ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.523(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? 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 O3W Er1 O1W 94.76(12) . . ? O3W Er1 O2W 95.18(11) . . ? O1W Er1 O2W 151.51(12) . . ? O3W Er1 O3 78.04(11) . . ? O1W Er1 O3 68.98(11) . . ? O2W Er1 O3 139.34(11) . . ? O3W Er1 O1 67.63(10) . . ? O1W Er1 O1 80.87(11) . . ? O2W Er1 O1 78.40(11) . . ? O3 Er1 O1 131.75(10) . . ? O3W Er1 O2 134.51(10) . 3_655 ? O1W Er1 O2 74.11(11) . 3_655 ? O2W Er1 O2 79.91(11) . 3_655 ? O3 Er1 O2 132.61(10) . 3_655 ? O1 Er1 O2 67.08(10) . 3_655 ? O3W Er1 O4 72.86(10) . 3_756 ? O1W Er1 O4 136.69(11) . 3_756 ? O2W Er1 O4 71.80(11) . 3_756 ? O3 Er1 O4 67.88(10) . 3_756 ? O1 Er1 O4 127.28(10) . 3_756 ? O2 Er1 O4 142.86(10) 3_655 3_756 ? O3W Er1 Cl1 149.31(8) . . ? O1W Er1 Cl1 97.62(9) . . ? O2W Er1 Cl1 87.12(8) . . ? O3 Er1 Cl1 80.41(8) . . ? O1 Er1 Cl1 142.13(7) . . ? O2 Er1 Cl1 76.06(7) 3_655 . ? O4 Er1 Cl1 78.92(7) 3_756 . ? C1 O1 Er1 120.9(3) . . ? Er1 O1W H1WB 123.9 . . ? Er1 O1W H1WA 112.6 . . ? H1WB O1W H1WA 123.5 . . ? C1 O2 Er1 119.6(3) . 3_655 ? Er1 O2W H2WA 120.2 . . ? Er1 O2W H2WB 119.9 . . ? H2WA O2W H2WB 119.9 . . ? C2 O3 Er1 120.0(3) . . ? Er1 O3W H3WA 120.1 . . ? Er1 O3W H3WB 120.1 . . ? H3WA O3W H3WB 119.8 . . ? C2 O4 Er1 118.9(3) . 3_756 ? C7 O4W H4WA 115.5 . . ? H5WA O5W H5WB 120.0 . . ? C4 N1 C5 108.5(4) . . ? C4 N1 C3 108.4(4) . . ? C5 N1 C3 110.2(4) . . ? C4 N1 C6 108.0(3) . . ? C5 N1 C6 111.2(4) . . ? C3 N1 C6 110.5(4) . . ? O2 C1 O1 127.7(4) . . ? O2 C1 C1 116.2(4) . 3_655 ? O1 C1 C1 116.2(4) . 3_655 ? O3 C2 O4 127.0(4) . . ? O3 C2 C2 117.1(5) . 3_756 ? O4 C2 C2 115.9(5) . 3_756 ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 N1 113.8(4) . . ? C7 C6 H6A 108.8 . . ? N1 C6 H6A 108.8 . . ? C7 C6 H6B 108.8 . . ? N1 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O4W C7 C6 107.1(4) . . ? O4W C7 H7A 110.3 . . ? C6 C7 H7A 110.3 . . ? O4W C7 H7B 110.3 . . ? C6 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3W Er1 O1 C1 -176.5(3) . . . . ? O1W Er1 O1 C1 -77.5(3) . . . . ? O2W Er1 O1 C1 82.9(3) . . . . ? O3 Er1 O1 C1 -128.4(3) . . . . ? O2 Er1 O1 C1 -1.0(3) 3_655 . . . ? O4 Er1 O1 C1 139.0(3) 3_756 . . . ? Cl1 Er1 O1 C1 13.2(4) . . . . ? O3W Er1 O3 C2 -79.3(3) . . . . ? O1W Er1 O3 C2 -179.2(3) . . . . ? O2W Er1 O3 C2 4.7(4) . . . . ? O1 Er1 O3 C2 -124.0(3) . . . . ? O2 Er1 O3 C2 139.6(3) 3_655 . . . ? O4 Er1 O3 C2 -3.1(3) 3_756 . . . ? Cl1 Er1 O3 C2 78.8(3) . . . . ? Er1 O2 C1 O1 -179.1(3) 3_655 . . . ? Er1 O2 C1 C1 0.5(5) 3_655 . . 3_655 ? Er1 O1 C1 O2 -179.4(3) . . . . ? Er1 O1 C1 C1 1.1(5) . . . 3_655 ? Er1 O3 C2 O4 -177.0(3) . . . . ? Er1 O3 C2 C2 2.8(6) . . . 3_756 ? Er1 O4 C2 O3 -177.2(3) 3_756 . . . ? Er1 O4 C2 C2 3.0(6) 3_756 . . 3_756 ? C4 N1 C6 C7 174.5(4) . . . . ? C5 N1 C6 C7 -66.6(5) . . . . ? C3 N1 C6 C7 56.1(5) . . . . ? N1 C6 C7 O4W 169.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 61.17 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.895 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.141 #_eof #End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 942169'