# Supplementary Material (ESI) for Polymer Chemistry # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Polym.Chem. _journal_coden_Cambridge 1478 _publ_contact_author_name 'Xingqiang Lu' _publ_contact_author_address ; Shaanxi Key Laboratory of Degradable Medical Material Shaanxi Key Laboratory of Physico-inorganic Chemistry Northwest University Xi'an 710069 CHINA _pub1_contact_author_email lvxq@nwu.edu.cn _pub1_section_title Bulk ring-opening polymerization of L-lactide catalyzed by Ni and Ni-Ln complexes of the Salen-type Schiff-base ligand ; loop_ _publ_author_name 'Wenjuan Jin' 'Liqin Ding' 'Xingqiang Lu' 'Junfeng Hui' 'Daidi Fan' 'Jirong Song' data_1 _database_code_depnum_ccdc_archive 'CCDC 776507' #TrackingRef 'cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H24 N5 Ni O14 Sm' _chemical_formula_weight 779.51 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.276(2) _cell_length_b 26.738(5) _cell_length_c 9.1772(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.07(3) _cell_angle_gamma 90.00 _cell_volume 2759.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 2.867 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart CCD' _diffrn_measurement_method 'w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7443 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.1630 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.28 _reflns_number_total 3525 _reflns_number_gt 1614 _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^)+(0.0837P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 3525 _refine_ls_number_parameters 380 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.827 _refine_ls_shift/su_max 0.120 _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 Sm1 Sm 0.14585(11) 0.37876(3) 0.41702(13) 0.0648(4) Uani 1 1 d . . . Ni1 Ni 0.1966(2) 0.25396(9) 0.4827(3) 0.0615(7) Uani 1 1 d . . . O2 O 0.1607(9) 0.2947(4) 0.3232(14) 0.052(3) Uani 1 1 d . . . O3 O 0.2247(13) 0.3148(4) 0.5735(15) 0.067(4) Uani 1 1 d . . . N2 N 0.2290(15) 0.2133(8) 0.640(3) 0.075(7) Uani 1 1 d . . . N1 N 0.1697(13) 0.1949(5) 0.396(3) 0.081(7) Uani 1 1 d . . . O1 O 0.1036(12) 0.3635(5) 0.1356(14) 0.071(4) Uani 1 1 d . . . O4 O 0.2739(13) 0.4066(5) 0.6435(19) 0.087(5) Uani 1 1 d . . . O7 O 0.0283(19) 0.3842(8) 0.615(3) 0.150(13) Uani 1 1 d . . . C11 C 0.276(2) 0.2299(12) 0.768(4) 0.092(10) Uani 1 1 d . . . H11A H 0.2970 0.2056 0.8373 0.111 Uiso 1 1 calc R . . O8 O 0.3591(13) 0.3683(6) 0.3487(19) 0.083(5) Uani 1 1 d . . . C17 C 0.2730(17) 0.3203(8) 0.708(3) 0.063(6) Uani 1 1 d . . . O13 O 0.097(2) 0.4703(13) 0.459(5) 0.25(3) Uani 1 1 d . . . O5 O -0.0335(12) 0.3306(6) 0.474(2) 0.090(5) Uani 1 1 d . . . N4 N 0.3653(19) 0.4109(7) 0.294(2) 0.080(5) Uani 1 1 d . . . O9 O 0.4569(16) 0.4241(7) 0.250(2) 0.125(7) Uani 1 1 d . . . C16 C 0.3045(16) 0.3715(9) 0.750(2) 0.070(6) Uani 1 1 d . . . C10 C 0.198(3) 0.1615(10) 0.615(4) 0.121(12) Uani 1 1 d . . . H10A H 0.1179 0.1556 0.6425 0.146 Uiso 1 1 calc R . . H10B H 0.2515 0.1405 0.6761 0.146 Uiso 1 1 calc R . . O10 O 0.2753(17) 0.4383(6) 0.312(3) 0.119(7) Uani 1 1 d . . . C15 C 0.353(2) 0.3836(10) 0.883(3) 0.088(7) Uani 1 1 d . . . H15A H 0.3707 0.4169 0.9052 0.106 Uiso 1 1 calc R . . C8 C 0.1193(18) 0.1886(8) 0.259(3) 0.075(7) Uani 1 1 d . . . H8A H 0.1065 0.1561 0.2253 0.089 Uiso 1 1 calc R . . C7 C 0.1088(18) 0.2793(8) 0.199(2) 0.064(6) Uani 1 1 d . . . C12 C 0.2998(17) 0.2823(10) 0.813(3) 0.077(7) Uani 1 1 d . . . C6 C 0.0842(18) 0.2287(9) 0.161(3) 0.067(7) Uani 1 1 d . . . O11 O -0.0299(12) 0.4288(7) 0.323(2) 0.103(5) Uani 1 1 d . . . C9 C 0.206(2) 0.1478(9) 0.465(3) 0.095(7) Uani 1 1 d . . . H9A H 0.1521 0.1208 0.4356 0.115 Uiso 1 1 calc R . . H9B H 0.2864 0.1387 0.4440 0.115 Uiso 1 1 calc R . . C1 C 0.0797(19) 0.4052(8) 0.043(3) 0.084(7) Uani 1 1 d . . . H1A H 0.0660 0.3940 -0.0562 0.126 Uiso 1 1 calc R . . H1B H 0.1466 0.4275 0.0502 0.126 Uiso 1 1 calc R . . H1C H 0.0105 0.4224 0.0720 0.126 Uiso 1 1 calc R . . N3 N -0.035(3) 0.3562(14) 0.597(3) 0.154(17) Uani 1 1 d . . . O12 O -0.066(2) 0.5070(9) 0.356(4) 0.232(15) Uani 1 1 d . . . C18 C 0.287(3) 0.4586(8) 0.687(3) 0.122(10) Uani 1 1 d . . . H18A H 0.3376 0.4609 0.7749 0.183 Uiso 1 1 calc R . . H18B H 0.2101 0.4722 0.7034 0.183 Uiso 1 1 calc R . . H18C H 0.3210 0.4771 0.6106 0.183 Uiso 1 1 calc R . . C4 C 0.002(2) 0.2522(15) -0.071(3) 0.115(11) Uani 1 1 d . . . H4A H -0.0303 0.2432 -0.1632 0.139 Uiso 1 1 calc R . . C2 C 0.080(2) 0.3164(9) 0.092(3) 0.068(6) Uani 1 1 d . . . O6 O -0.1286(18) 0.3334(8) 0.650(2) 0.131(7) Uani 1 1 d . . . N5 N 0.027(5) 0.4698(7) 0.403(5) 0.19(2) Uani 1 1 d . . . C3 C 0.022(3) 0.3074(11) -0.039(3) 0.116(10) Uani 1 1 d . . . H3A H -0.0040 0.3327 -0.1029 0.139 Uiso 1 1 calc R . . C14 C 0.376(3) 0.3486(19) 0.985(5) 0.152(18) Uani 1 1 d . . . H14A H 0.4061 0.3576 1.0784 0.183 Uiso 1 1 calc R . . C13 C 0.354(2) 0.2991(16) 0.952(3) 0.118(12) Uani 1 1 d . . . H13A H 0.3755 0.2752 1.0226 0.142 Uiso 1 1 calc R . . C5 C 0.030(2) 0.2149(13) 0.027(3) 0.094(9) Uani 1 1 d . . . H5A H 0.0124 0.1816 0.0053 0.112 Uiso 1 1 calc R . . O14 O 0.100(3) 0.0626(9) 0.174(4) 0.197(13) Uani 1 1 d . . . C20 C 0.167(8) 0.012(5) 0.078(6) 0.46(2) Uani 1 1 d . . . C21 C 0.210(6) 0.0669(19) 0.004(8) 0.33(4) Uani 1 1 d . . . H21A H 0.2527 0.0601 -0.0809 0.494 Uiso 1 1 calc R . . H21B H 0.2601 0.0850 0.0741 0.494 Uiso 1 1 calc R . . H21C H 0.1408 0.0866 -0.0244 0.494 Uiso 1 1 calc R . . C19 C 0.097(5) -0.0063(17) 0.017(6) 0.28(3) Uani 1 1 d . . . H19A H 0.0710 -0.0344 0.0711 0.422 Uiso 1 1 calc R . . H19B H 0.1239 -0.0176 -0.0746 0.422 Uiso 1 1 calc R . . H19C H 0.0315 0.0165 -0.0021 0.422 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 Sm1 0.0717(6) 0.0547(6) 0.0657(6) -0.0022(8) -0.0113(4) -0.0018(8) Ni1 0.0681(15) 0.0531(16) 0.0616(16) 0.0033(13) -0.0075(12) -0.0014(12) O2 0.044(7) 0.050(7) 0.059(8) 0.004(6) -0.010(6) -0.010(6) O3 0.086(9) 0.060(8) 0.051(9) 0.008(7) -0.021(8) -0.006(7) N2 0.035(10) 0.100(17) 0.090(16) 0.064(13) -0.009(11) 0.012(10) N1 0.035(11) 0.056(10) 0.15(2) 0.041(12) -0.012(13) 0.013(7) O1 0.091(10) 0.068(10) 0.052(9) 0.006(7) -0.004(8) -0.001(8) O4 0.092(10) 0.058(9) 0.104(13) -0.036(10) -0.034(10) 0.007(8) O7 0.119(17) 0.089(13) 0.23(3) 0.002(14) -0.090(19) -0.032(11) C11 0.037(13) 0.12(3) 0.12(3) 0.06(2) 0.008(15) -0.002(14) O8 0.084(10) 0.061(10) 0.100(13) 0.004(9) -0.017(9) -0.010(8) C17 0.048(12) 0.077(16) 0.062(15) -0.006(13) -0.001(11) -0.024(11) O13 0.12(2) 0.25(4) 0.35(5) -0.05(3) -0.15(3) 0.002(18) O5 0.053(9) 0.111(13) 0.103(13) 0.017(11) -0.006(9) -0.028(9) N4 0.088(15) 0.059(14) 0.096(15) -0.006(11) 0.021(12) -0.033(12) O9 0.091(13) 0.151(17) 0.137(17) 0.009(14) 0.037(12) -0.043(12) C16 0.044(11) 0.107(18) 0.055(14) -0.013(14) -0.009(10) 0.016(11) C10 0.14(3) 0.063(19) 0.15(3) 0.05(2) -0.01(2) 0.005(18) O10 0.084(12) 0.072(11) 0.20(2) 0.018(13) -0.018(13) 0.020(10) C15 0.082(15) 0.11(2) 0.070(17) -0.023(16) -0.021(14) 0.016(14) C8 0.039(11) 0.071(16) 0.11(2) 0.020(15) -0.005(13) 0.033(10) C7 0.077(14) 0.061(14) 0.050(13) 0.012(11) -0.018(11) -0.016(11) C12 0.041(11) 0.09(2) 0.10(2) 0.022(17) -0.007(12) 0.009(12) C6 0.043(12) 0.052(14) 0.10(2) -0.002(14) 0.004(13) 0.002(10) O11 0.064(9) 0.135(15) 0.107(13) 0.034(12) -0.015(9) 0.030(9) C9 0.081(15) 0.093(19) 0.11(2) -0.010(17) 0.010(16) 0.011(13) C1 0.070(13) 0.076(15) 0.11(2) 0.050(15) 0.012(13) 0.014(12) N3 0.16(3) 0.25(4) 0.075(18) 0.13(2) 0.126(19) 0.16(3) O12 0.19(2) 0.094(16) 0.41(5) -0.09(2) 0.00(3) 0.028(16) C18 0.17(3) 0.081(17) 0.11(2) -0.033(15) -0.072(18) -0.006(17) C4 0.068(17) 0.19(4) 0.08(2) -0.06(2) 0.000(15) -0.007(19) C2 0.074(15) 0.074(17) 0.056(15) -0.004(12) -0.006(13) 0.009(13) O6 0.121(15) 0.170(19) 0.099(15) 0.010(13) -0.011(13) 0.028(13) N5 0.34(5) 0.000(9) 0.26(4) -0.023(15) 0.23(4) -0.023(17) C3 0.14(3) 0.10(2) 0.10(2) 0.005(19) -0.02(2) 0.051(19) C14 0.10(2) 0.25(5) 0.11(3) -0.08(4) -0.01(2) 0.02(3) C13 0.056(15) 0.25(4) 0.048(17) 0.07(2) 0.002(13) 0.06(2) C5 0.09(2) 0.12(2) 0.068(19) -0.023(18) -0.015(16) 0.010(16) O14 0.21(3) 0.14(2) 0.23(3) 0.01(2) -0.03(3) -0.10(2) C20 0.44(5) 0.78(10) 0.15(4) -0.01(8) -0.03(5) -0.529 C21 0.30(6) 0.26(6) 0.41(10) -0.26(7) -0.11(6) 0.07(5) C19 0.30(6) 0.20(4) 0.33(7) -0.10(5) -0.06(6) -0.12(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O3 2.366(12) . ? Sm1 O10 2.408(18) . ? Sm1 O2 2.418(12) . ? Sm1 O7 2.33(3) . ? Sm1 O5 2.484(14) . ? Sm1 O11 2.494(12) . ? Sm1 O13 2.54(3) . ? Sm1 O8 2.543(16) . ? Sm1 O4 2.556(14) . ? Sm1 O1 2.625(13) . ? Sm1 N3 2.78(2) . ? Sm1 N5 2.78(3) . ? Ni1 N1 1.79(2) . ? Ni1 N2 1.824(17) . ? Ni1 O3 1.844(12) . ? Ni1 O2 1.846(12) . ? O2 C7 1.31(2) . ? O3 C17 1.32(2) . ? N2 C11 1.33(4) . ? N2 C10 1.44(3) . ? N1 C8 1.35(3) . ? N1 C9 1.45(3) . ? O1 C2 1.34(2) . ? O1 C1 1.42(2) . ? O4 C16 1.38(2) . ? O4 C18 1.45(2) . ? O7 N3 1.04(4) . ? C11 C12 1.48(4) . ? O8 N4 1.25(2) . ? C17 C16 1.46(3) . ? C17 C12 1.42(3) . ? O13 N5 0.91(6) . ? O5 N3 1.32(3) . ? N4 O9 1.19(2) . ? N4 O10 1.27(2) . ? C16 C15 1.34(3) . ? C10 C9 1.44(4) . ? C15 C14 1.34(5) . ? C8 C6 1.43(3) . ? C7 C2 1.42(3) . ? C7 C6 1.42(3) . ? C12 C13 1.45(4) . ? C6 C5 1.38(4) . ? O11 N5 1.44(4) . ? N3 O6 1.33(3) . ? O12 N5 1.48(5) . ? C4 C5 1.36(4) . ? C4 C3 1.52(4) . ? C2 C3 1.35(3) . ? C14 C13 1.37(5) . ? O14 C20 1.81(13) . ? C20 C19 1.07(5) . ? C20 C21 1.69(10) . ? 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 O3 Sm1 O10 120.6(5) . . ? O3 Sm1 O2 60.7(4) . . ? O10 Sm1 O2 114.4(6) . . ? O3 Sm1 O7 77.4(7) . . ? O10 Sm1 O7 131.8(7) . . ? O2 Sm1 O7 113.2(5) . . ? O3 Sm1 O5 76.9(5) . . ? O10 Sm1 O5 162.3(5) . . ? O2 Sm1 O5 70.8(5) . . ? O7 Sm1 O5 49.6(6) . . ? O3 Sm1 O11 148.5(5) . . ? O10 Sm1 O11 89.8(6) . . ? O2 Sm1 O11 116.7(5) . . ? O7 Sm1 O11 75.8(7) . . ? O5 Sm1 O11 73.3(5) . . ? O3 Sm1 O13 132.8(10) . . ? O10 Sm1 O13 64.5(11) . . ? O2 Sm1 O13 165.9(8) . . ? O7 Sm1 O13 71.3(13) . . ? O5 Sm1 O13 106.0(10) . . ? O11 Sm1 O13 50.2(7) . . ? O3 Sm1 O8 75.4(5) . . ? O10 Sm1 O8 50.5(5) . . ? O2 Sm1 O8 73.7(4) . . ? O7 Sm1 O8 143.1(6) . . ? O5 Sm1 O8 142.5(6) . . ? O11 Sm1 O8 135.7(6) . . ? O13 Sm1 O8 111.3(9) . . ? O3 Sm1 O4 63.3(4) . . ? O10 Sm1 O4 79.1(7) . . ? O2 Sm1 O4 120.7(4) . . ? O7 Sm1 O4 70.5(6) . . ? O5 Sm1 O4 113.6(6) . . ? O11 Sm1 O4 121.0(6) . . ? O13 Sm1 O4 73.4(7) . . ? O8 Sm1 O4 75.1(5) . . ? O3 Sm1 O1 121.3(4) . . ? O10 Sm1 O1 77.4(6) . . ? O2 Sm1 O1 61.1(4) . . ? O7 Sm1 O1 134.8(6) . . ? O5 Sm1 O1 91.9(5) . . ? O11 Sm1 O1 70.0(6) . . ? O13 Sm1 O1 105.8(11) . . ? O8 Sm1 O1 81.3(5) . . ? O4 Sm1 O1 153.9(5) . . ? O3 Sm1 N3 75.2(5) . . ? O10 Sm1 N3 150.8(10) . . ? O2 Sm1 N3 94.7(9) . . ? O7 Sm1 N3 21.3(10) . . ? O5 Sm1 N3 28.3(9) . . ? O11 Sm1 N3 73.9(6) . . ? O13 Sm1 N3 86.6(13) . . ? O8 Sm1 N3 150.4(5) . . ? O4 Sm1 N3 88.7(10) . . ? O1 Sm1 N3 117.4(9) . . ? O3 Sm1 N5 145.1(9) . . ? O10 Sm1 N5 73.0(8) . . ? O2 Sm1 N5 147.6(12) . . ? O7 Sm1 N5 71.4(8) . . ? O5 Sm1 N5 93.7(8) . . ? O11 Sm1 N5 31.2(11) . . ? O13 Sm1 N5 19.0(12) . . ? O8 Sm1 N5 123.2(8) . . ? O4 Sm1 N5 91.5(12) . . ? O1 Sm1 N5 92.2(10) . . ? N3 Sm1 N5 81.0(8) . . ? N1 Ni1 N2 81.1(11) . . ? N1 Ni1 O3 179.7(9) . . ? N2 Ni1 O3 98.6(10) . . ? N1 Ni1 O2 98.4(9) . . ? N2 Ni1 O2 178.8(7) . . ? O3 Ni1 O2 81.9(5) . . ? N1 Ni1 Sm1 139.5(7) . . ? N2 Ni1 Sm1 137.8(8) . . ? O3 Ni1 Sm1 40.8(4) . . ? O2 Ni1 Sm1 42.5(4) . . ? C7 O2 Ni1 124.4(12) . . ? C7 O2 Sm1 124.2(12) . . ? Ni1 O2 Sm1 106.4(6) . . ? C17 O3 Ni1 124.5(13) . . ? C17 O3 Sm1 126.8(13) . . ? Ni1 O3 Sm1 108.6(6) . . ? C11 N2 C10 123(2) . . ? C11 N2 Ni1 123(2) . . ? C10 N2 Ni1 114(2) . . ? C8 N1 C9 113(2) . . ? C8 N1 Ni1 124.9(14) . . ? C9 N1 Ni1 122.5(19) . . ? C2 O1 C1 122.3(18) . . ? C2 O1 Sm1 117.2(12) . . ? C1 O1 Sm1 118.8(14) . . ? C16 O4 C18 116.2(17) . . ? C16 O4 Sm1 118.5(11) . . ? C18 O4 Sm1 122.8(12) . . ? N3 O7 Sm1 104(2) . . ? N2 C11 C12 128(3) . . ? N4 O8 Sm1 94.5(12) . . ? O3 C17 C16 115.3(19) . . ? O3 C17 C12 128(2) . . ? C16 C17 C12 117(2) . . ? N5 O13 Sm1 95(3) . . ? N3 O5 Sm1 88.5(18) . . ? O9 N4 O8 119(2) . . ? O9 N4 O10 126(2) . . ? O8 N4 O10 114.1(19) . . ? O9 N4 Sm1 177.5(16) . . ? O8 N4 Sm1 60.3(10) . . ? O10 N4 Sm1 54.2(11) . . ? C15 C16 O4 123(2) . . ? C15 C16 C17 123(2) . . ? O4 C16 C17 113.9(17) . . ? N2 C10 C9 112(2) . . ? N4 O10 Sm1 100.4(13) . . ? C16 C15 C14 121(3) . . ? N1 C8 C6 125(2) . . ? O2 C7 C2 116.8(18) . . ? O2 C7 C6 125.4(19) . . ? C2 C7 C6 118(2) . . ? C13 C12 C17 116(2) . . ? C13 C12 C11 127(3) . . ? C17 C12 C11 117(2) . . ? C7 C6 C5 123(2) . . ? C7 C6 C8 121(2) . . ? C5 C6 C8 116(2) . . ? N5 O11 Sm1 85(2) . . ? C10 C9 N1 99(2) . . ? O5 N3 O7 117(2) . . ? O5 N3 O6 98(4) . . ? O7 N3 O6 145(4) . . ? O5 N3 Sm1 63.2(11) . . ? O7 N3 Sm1 54(2) . . ? O6 N3 Sm1 161(3) . . ? C5 C4 C3 124(3) . . ? C3 C2 O1 120(2) . . ? C3 C2 C7 124(2) . . ? O1 C2 C7 114.8(19) . . ? O13 N5 O12 136(4) . . ? O13 N5 O11 129(4) . . ? O12 N5 O11 95(4) . . ? O13 N5 Sm1 66(3) . . ? O12 N5 Sm1 158(3) . . ? O11 N5 Sm1 63.4(11) . . ? C2 C3 C4 114(3) . . ? C13 C14 C15 120(3) . . ? C14 C13 C12 124(3) . . ? C4 C5 C6 117(3) . . ? C19 C20 O14 106(10) . . ? C19 C20 C21 114(8) . . ? O14 C20 C21 72(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.28 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.921 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.172