# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Parimal Bharadwaj' _publ_contact_author_email PKB@IITK.AC.IN _publ_section_title ; Coordination polymers with pyridine-2,4, 6-tricarboxylic acid and alkaline-earth/lanthanides/transition metals: Synthesis and X-ray structures ; loop_ _publ_author_name 'Parimal Bharadwaj' 'Madhab C Das' 'Sujit Kumar Ghosh' E.C.Sanudo # Attachment 'CIFs.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 697859' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H6 Cd O7' _chemical_formula_weight 254.47 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.998(4) _cell_length_b 6.592(3) _cell_length_c 8.459(4) _cell_angle_alpha 74.674(5) _cell_angle_beta 74.278(4) _cell_angle_gamma 81.171(5) _cell_volume 309.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 244 _exptl_absorpt_coefficient_mu 3.514 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6033 _exptl_absorpt_correction_T_max 0.6985 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2034 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1458 _reflns_number_gt 1451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0553P)^2^+0.4090P] 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 1458 _refine_ls_number_parameters 115 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.128 _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 Cd1 Cd 0.95077(3) 0.19148(3) 0.29424(2) 0.00618(13) Uani 1 1 d . . . O1 O 0.7789(4) -0.0566(4) 0.5363(3) 0.0094(5) Uani 1 1 d . . . O2 O 0.5437(4) 0.2246(4) 0.3340(3) 0.0102(5) Uani 1 1 d . . . O3 O 0.8798(4) 0.2514(4) 0.0248(3) 0.0095(5) Uani 1 1 d . . . O4 O 1.0848(5) -0.1070(4) 0.1919(3) 0.0093(5) Uani 1 1 d . . . OW1 O 1.2773(4) 0.3563(4) 0.1124(3) 0.0103(5) Uani 1 1 d D . . OW2 O 0.8467(5) 0.4988(5) 0.3842(4) 0.0134(6) Uani 1 1 d D . . OW3 O 1.5642(5) -0.2368(5) 0.2010(4) 0.0186(6) Uani 1 1 d D . . C2 C 1.0598(6) -0.1033(5) 0.0474(4) 0.0083(6) Uani 1 1 d . . . C1 C 0.5672(6) -0.0816(5) 0.5598(4) 0.0067(6) Uani 1 1 d . . . H2W3 H 1.424(4) -0.217(12) 0.211(9) 0.042(18) Uiso 1 1 d D . . H1W2 H 0.934(11) 0.591(9) 0.364(9) 0.041(19) Uiso 1 1 d D . . H1W3 H 1.594(15) -0.283(13) 0.116(7) 0.07(3) Uiso 1 1 d D . . H2W2 H 0.731(8) 0.557(10) 0.352(9) 0.05(2) Uiso 1 1 d D . . H1W1 H 1.358(8) 0.347(9) 0.178(6) 0.05(4) Uiso 1 1 d D . . H2W1 H 1.258(18) 0.487(4) 0.080(13) 0.08(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.00581(17) 0.00718(17) 0.00539(17) -0.00008(11) -0.00247(11) -0.00056(10) O1 0.0060(10) 0.0126(12) 0.0078(10) 0.0016(9) -0.0015(9) -0.0030(9) O2 0.0088(11) 0.0108(11) 0.0101(11) 0.0020(9) -0.0037(9) -0.0038(9) O3 0.0126(11) 0.0084(11) 0.0080(11) -0.0027(9) -0.0045(9) 0.0027(9) O4 0.0112(12) 0.0106(12) 0.0072(11) -0.0018(10) -0.0055(10) 0.0009(9) OW1 0.0080(11) 0.0113(12) 0.0105(11) 0.0026(9) -0.0059(9) -0.0003(9) OW2 0.0137(13) 0.0113(13) 0.0172(14) -0.0061(11) -0.0050(11) 0.0001(10) OW3 0.0135(13) 0.0224(13) 0.0224(16) -0.0078(11) -0.0085(12) 0.0029(10) C2 0.0085(14) 0.0098(15) 0.0069(14) -0.0011(12) -0.0039(12) 0.0010(11) C1 0.0058(14) 0.0094(14) 0.0059(13) -0.0014(12) -0.0037(11) -0.0001(11) _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 Cd1 OW2 2.290(3) . ? Cd1 O4 2.303(3) . ? Cd1 OW1 2.349(3) . ? Cd1 O3 2.352(3) . ? Cd1 O1 2.352(3) . ? Cd1 O2 2.356(3) . ? Cd1 O1 2.370(3) 2_756 ? O1 C1 1.260(4) . ? O1 Cd1 2.370(3) 2_756 ? O2 C1 1.249(4) 2_656 ? O3 C2 1.242(4) 2_755 ? O4 C2 1.265(4) . ? OW1 H1W1 0.82(5) . ? OW1 H2W1 0.83(2) . ? OW2 H1W2 0.82(7) . ? OW2 H2W2 0.82(6) . ? OW3 H2W3 0.82(2) . ? OW3 H1W3 0.82(6) . ? C2 O3 1.242(4) 2_755 ? C2 C2 1.564(7) 2_755 ? C1 O2 1.249(4) 2_656 ? C1 C1 1.559(7) 2_656 ? 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 OW2 Cd1 O4 175.24(9) . . ? OW2 Cd1 OW1 86.03(11) . . ? O4 Cd1 OW1 89.28(10) . . ? OW2 Cd1 O3 108.21(10) . . ? O4 Cd1 O3 71.38(9) . . ? OW1 Cd1 O3 76.38(10) . . ? OW2 Cd1 O1 101.42(11) . . ? O4 Cd1 O1 82.33(10) . . ? OW1 Cd1 O1 151.13(9) . . ? O3 Cd1 O1 125.72(9) . . ? OW2 Cd1 O2 78.19(10) . . ? O4 Cd1 O2 106.02(9) . . ? OW1 Cd1 O2 139.35(9) . . ? O3 Cd1 O2 73.54(9) . . ? O1 Cd1 O2 69.38(9) . . ? OW2 Cd1 O1 94.77(10) . 2_756 ? O4 Cd1 O1 83.66(10) . 2_756 ? OW1 Cd1 O1 81.04(10) . 2_756 ? O3 Cd1 O1 146.24(9) . 2_756 ? O1 Cd1 O1 70.63(11) . 2_756 ? O2 Cd1 O1 136.94(9) . 2_756 ? C1 O1 Cd1 118.1(2) . . ? C1 O1 Cd1 132.3(2) . 2_756 ? Cd1 O1 Cd1 109.37(11) . 2_756 ? C1 O2 Cd1 117.6(2) 2_656 . ? C2 O3 Cd1 116.6(2) 2_755 . ? C2 O4 Cd1 117.3(2) . . ? Cd1 OW1 H1W1 101(4) . . ? Cd1 OW1 H2W1 116(7) . . ? H1W1 OW1 H2W1 100(8) . . ? Cd1 OW2 H1W2 124(5) . . ? Cd1 OW2 H2W2 108(5) . . ? H1W2 OW2 H2W2 106(7) . . ? H2W3 OW3 H1W3 96(8) . . ? O3 C2 O4 125.3(3) 2_755 . ? O3 C2 C2 117.3(4) 2_755 2_755 ? O4 C2 C2 117.4(4) . 2_755 ? O2 C1 O1 126.9(3) 2_656 . ? O2 C1 C1 117.1(4) 2_656 2_656 ? O1 C1 C1 116.0(4) . 2_656 ? 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 OW2 Cd1 O1 C1 83.6(3) . . . . ? O4 Cd1 O1 C1 -99.4(3) . . . . ? OW1 Cd1 O1 C1 -173.7(2) . . . . ? O3 Cd1 O1 C1 -38.9(3) . . . . ? O2 Cd1 O1 C1 11.0(2) . . . . ? O1 Cd1 O1 C1 174.7(3) 2_756 . . . ? OW2 Cd1 O1 Cd1 -91.08(12) . . . 2_756 ? O4 Cd1 O1 Cd1 85.95(11) . . . 2_756 ? OW1 Cd1 O1 Cd1 11.6(2) . . . 2_756 ? O3 Cd1 O1 Cd1 146.37(10) . . . 2_756 ? O2 Cd1 O1 Cd1 -163.68(13) . . . 2_756 ? O1 Cd1 O1 Cd1 0.0 2_756 . . 2_756 ? OW2 Cd1 O2 C1 -118.9(3) . . . 2_656 ? O4 Cd1 O2 C1 63.4(3) . . . 2_656 ? OW1 Cd1 O2 C1 171.8(2) . . . 2_656 ? O3 Cd1 O2 C1 127.9(3) . . . 2_656 ? O1 Cd1 O2 C1 -11.7(2) . . . 2_656 ? O1 Cd1 O2 C1 -34.6(3) 2_756 . . 2_656 ? OW2 Cd1 O3 C2 175.8(2) . . . 2_755 ? O4 Cd1 O3 C2 0.8(2) . . . 2_755 ? OW1 Cd1 O3 C2 94.7(3) . . . 2_755 ? O1 Cd1 O3 C2 -64.7(3) . . . 2_755 ? O2 Cd1 O3 C2 -113.0(2) . . . 2_755 ? O1 Cd1 O3 C2 45.2(3) 2_756 . . 2_755 ? OW1 Cd1 O4 C2 -76.2(3) . . . . ? O3 Cd1 O4 C2 -0.3(2) . . . . ? O1 Cd1 O4 C2 131.5(3) . . . . ? O2 Cd1 O4 C2 65.6(3) . . . . ? O1 Cd1 O4 C2 -157.3(3) 2_756 . . . ? Cd1 O4 C2 O3 -179.2(3) . . . 2_755 ? Cd1 O4 C2 C2 0.0(5) . . . 2_755 ? Cd1 O1 C1 O2 169.1(3) . . . 2_656 ? Cd1 O1 C1 O2 -17.7(5) 2_756 . . 2_656 ? Cd1 O1 C1 C1 -9.5(5) . . . 2_656 ? Cd1 O1 C1 C1 163.7(2) 2_756 . . 2_656 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.553 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.274 #===END of CIF for Complex 1 ===================== data_complex2 _database_code_depnum_ccdc_archive 'CCDC 697860' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 Cd4 N4 O34' _chemical_formula_weight 1426.24 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.403(5) _cell_length_b 17.963(6) _cell_length_c 13.090(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.904(8) _cell_angle_gamma 90.00 _cell_volume 2352.5(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description 'rectangular parallelopipeds' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 1.892 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6810 _exptl_absorpt_correction_T_max 0.7392 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15459 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.30 _reflns_number_total 5821 _reflns_number_gt 5118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.1499P)^2^+4.2423P] 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 5821 _refine_ls_number_parameters 366 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.2143 _refine_ls_wR_factor_gt 0.1851 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.046 _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 Cd1 Cd 0.16101(8) 0.06143(4) 0.06158(6) 0.0174(3) Uani 1 1 d . . . Cd2 Cd 0.55056(9) 0.17792(5) 0.23825(10) 0.0337(3) Uani 1 1 d D . . OW6 O 0.4751(12) 0.3827(7) 0.3299(12) 0.000(2) Uiso 0.50 1 d PD . . OW2 O 0.5431(6) 0.1427(3) 0.4288(4) 0.0000(10) Uiso 1 1 d D . . O7 O 0.3220(8) 0.1466(5) 0.1652(8) 0.0242(18) Uani 1 1 d . . . O5 O -0.0852(8) 0.0510(4) 0.0253(7) 0.0176(15) Uani 1 1 d . . . O3 O 0.6698(9) 0.2931(5) 0.2781(10) 0.037(2) Uani 1 1 d . . . O6 O -0.2764(8) 0.1133(4) 0.0067(7) 0.0197(15) Uani 1 1 d . . . OW4 O 0.3652(9) 0.0322(5) 0.0239(8) 0.0258(18) Uani 1 1 d D . . O1 O 0.5946(9) 0.0506(5) 0.2012(8) 0.0272(19) Uani 1 1 d . . . O8 O 0.3644(9) 0.2650(6) 0.2089(10) 0.041(3) Uani 1 1 d . . . OW3 O 0.1306(9) 0.1147(5) -0.1043(7) 0.0242(17) Uani 1 1 d D . . O2 O 0.7564(9) -0.0367(5) 0.2360(8) 0.0258(18) Uani 1 1 d . . . O4 O 0.8710(8) 0.3459(4) 0.3194(7) 0.0204(16) Uani 1 1 d . . . N2 N 0.0609(9) 0.1701(5) 0.0977(7) 0.0166(17) Uani 1 1 d . . . N1 N 0.7744(9) 0.1575(5) 0.2734(8) 0.0197(18) Uani 1 1 d . . . OW7 O 0.5425(15) 0.4658(10) 0.1459(13) 0.064(4) Uani 1 1 d D . . OW5 O 0.2114(11) -0.0123(5) 0.2080(8) 0.032(2) Uani 1 1 d D . . C14 C -0.1514(11) 0.1091(6) 0.0288(9) 0.018(2) Uani 1 1 d . . . C3 C 1.0470(12) 0.1318(7) 0.3478(9) 0.021(2) Uani 1 1 d . . . O10 O -0.1075(14) 0.3891(7) 0.0768(11) 0.024(3) Uani 1 1 d . . . H11 H -0.1889 0.3863 0.0522 0.049 Uiso 1 1 calc R . . OW1 O 0.5369(11) 0.1997(6) 0.0573(12) 0.045(3) Uani 1 1 d D . . C6 C 0.7152(12) 0.0289(6) 0.2334(10) 0.021(2) Uani 1 1 d . . . C13 C -0.0711(11) 0.1797(6) 0.0637(8) 0.0153(19) Uani 1 1 d . . . C8 C 0.7958(12) 0.2905(6) 0.3005(9) 0.021(2) Uani 1 1 d . . . C2 C 0.9563(12) 0.0736(6) 0.3087(9) 0.021(2) Uani 1 1 d . . . H2 H 0.9872 0.0252 0.3061 0.025 Uiso 1 1 calc R . . C4 C 0.9959(11) 0.2033(6) 0.3449(9) 0.019(2) Uani 1 1 d . . . H4 H 1.0528 0.2433 0.3687 0.023 Uiso 1 1 calc R . . C9 C 0.1386(11) 0.2299(6) 0.1321(9) 0.019(2) Uani 1 1 d . . . O9 O 1.1941(14) 0.1170(8) 0.3944(13) 0.028(4) Uani 1 1 d . . . H9 H 1.2087 0.0723 0.3908 0.044 Uiso 1 1 calc R . . C12 C -0.1291(11) 0.2496(6) 0.0588(8) 0.0165(19) Uani 1 1 d . . . H12 H -0.2215 0.2548 0.0351 0.020 Uiso 1 1 calc R . . C5 C 0.8589(11) 0.2146(6) 0.3061(9) 0.017(2) Uani 1 1 d . . . C10 C 0.0882(11) 0.3018(6) 0.1297(9) 0.018(2) Uani 1 1 d . . . H10 H 0.1448 0.3419 0.1542 0.022 Uiso 1 1 calc R . . C11 C -0.0484(11) 0.3122(6) 0.0897(9) 0.018(2) Uani 1 1 d . . . C1 C 0.8212(11) 0.0886(6) 0.2741(9) 0.019(2) Uani 1 1 d . . . C16 C 0.2871(12) 0.2132(7) 0.1720(10) 0.025(2) Uani 1 1 d . . . OW6' O 0.4845(12) 0.3887(7) 0.3011(12) 0.000(3) Uiso 0.50 1 d PD . . H1W3 H 0.055(7) 0.128(9) -0.141(10) 0.03(4) Uiso 1 1 d D . . H2W3 H 0.17(2) 0.10(2) -0.149(11) 0.06(5) Uiso 1 1 d D . . H1W5 H 0.198(17) -0.056(3) 0.191(13) 0.05(4) Uiso 1 1 d D . . H2W5 H 0.279(8) -0.006(8) 0.256(8) 0.04(3) Uiso 1 1 d D . . H2W7 H 0.52(2) 0.506(7) 0.113(17) 0.06(7) Uiso 1 1 d D . . H1W7 H 0.49(14) 0.46(5) 0.19(11) 0.07(6) Uiso 1 1 d D . . H2W6 H 0.521(13) 0.419(5) 0.344(6) 0.04(4) Uiso 1 1 d D . . H1W6 H 0.519(14) 0.348(4) 0.319(9) 0.05(6) Uiso 1 1 d D . . H1W2 H 0.54(2) 0.178(2) 0.463(6) 0.05(6) Uiso 1 1 d D . . H2W4 H 0.435(11) 0.031(10) 0.072(11) 0.05(6) Uiso 1 1 d D . . H1W4 H 0.35(2) -0.011(4) 0.004(17) 0.05(8) Uiso 1 1 d D . . H2W2 H 0.471(12) 0.122(11) 0.411(3) 0.04(2) Uiso 1 1 d D . . H2W1 H 0.602(10) 0.187(11) 0.036(5) 0.05(6) Uiso 1 1 d D . . H1W1 H 0.54(3) 0.243(2) 0.037(6) 0.05(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0124(4) 0.0115(4) 0.0260(5) -0.0028(3) 0.0014(3) 0.0009(2) Cd2 0.0118(5) 0.0184(5) 0.0663(8) -0.0158(4) 0.0029(4) -0.0009(3) O7 0.013(4) 0.016(4) 0.041(5) -0.003(3) 0.003(3) 0.001(3) O5 0.014(4) 0.010(3) 0.028(4) -0.004(3) 0.004(3) 0.000(3) O3 0.015(4) 0.018(4) 0.069(7) -0.014(4) -0.003(4) 0.002(3) O6 0.013(4) 0.016(4) 0.028(4) -0.004(3) 0.003(3) 0.001(3) OW4 0.017(4) 0.017(4) 0.039(5) -0.007(4) -0.001(3) 0.001(3) O1 0.019(4) 0.018(4) 0.042(5) -0.006(4) 0.004(4) 0.000(3) O8 0.015(4) 0.025(5) 0.076(8) -0.019(5) -0.001(4) -0.002(4) OW3 0.016(4) 0.028(4) 0.028(4) 0.003(4) 0.005(3) 0.006(3) O2 0.025(4) 0.016(4) 0.037(5) -0.004(3) 0.010(4) -0.001(3) O4 0.019(4) 0.016(4) 0.024(4) -0.001(3) 0.003(3) -0.002(3) N2 0.015(4) 0.014(4) 0.020(4) -0.004(3) 0.004(3) -0.002(3) N1 0.013(4) 0.017(4) 0.027(5) -0.001(4) 0.002(4) -0.001(3) OW7 0.049(8) 0.066(10) 0.069(10) -0.004(8) 0.004(7) 0.009(7) OW5 0.041(6) 0.017(4) 0.029(5) 0.002(3) -0.009(4) -0.004(4) C14 0.016(5) 0.013(5) 0.025(5) -0.001(4) 0.006(4) 0.000(4) C3 0.021(5) 0.018(5) 0.023(5) 0.001(4) 0.002(4) 0.001(4) O10 0.035(8) 0.022(6) 0.015(8) -0.004(6) 0.006(6) 0.002(5) OW1 0.028(5) 0.022(5) 0.093(9) 0.005(5) 0.028(6) 0.007(4) C6 0.018(5) 0.017(5) 0.030(6) -0.001(4) 0.007(4) -0.003(4) C13 0.016(5) 0.014(5) 0.014(4) -0.002(4) 0.002(4) -0.002(4) C8 0.018(5) 0.019(5) 0.024(5) -0.003(4) 0.002(4) 0.000(4) C2 0.020(5) 0.018(5) 0.025(5) 0.003(4) 0.006(4) 0.003(4) C4 0.015(5) 0.019(5) 0.022(5) 0.001(4) 0.002(4) -0.001(4) C9 0.016(5) 0.017(5) 0.023(5) -0.004(4) 0.005(4) -0.003(4) O9 0.040(7) 0.021(8) 0.016(10) -0.007(7) -0.003(7) 0.002(6) C12 0.014(5) 0.018(5) 0.016(5) -0.002(4) 0.002(4) 0.001(4) C5 0.017(5) 0.013(5) 0.022(5) -0.003(4) 0.006(4) -0.001(4) C10 0.019(5) 0.014(5) 0.022(5) -0.006(4) 0.005(4) -0.005(4) C11 0.019(5) 0.016(5) 0.021(5) 0.000(4) 0.006(4) 0.002(4) C1 0.016(5) 0.015(5) 0.025(5) 0.001(4) 0.005(4) -0.002(4) C16 0.016(5) 0.022(6) 0.034(6) -0.007(5) 0.004(5) 0.000(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 Cd1 OW5 2.270(9) . ? Cd1 OW3 2.314(9) . ? Cd1 N2 2.321(9) . ? Cd1 O5 2.346(8) 3 ? Cd1 OW4 2.368(9) . ? Cd1 O7 2.396(9) . ? Cd1 O5 2.481(8) . ? Cd2 N1 2.277(10) . ? Cd2 OW1 2.365(15) . ? Cd2 O7 2.375(8) . ? Cd2 O3 2.395(9) . ? Cd2 O1 2.409(9) . ? Cd2 O8 2.436(10) . ? Cd2 OW2 2.595(5) . ? Cd2 C16 2.713(12) . ? OW6 H2W6 0.80(3) . ? OW6 H1W6 0.80(3) . ? OW2 H1W2 0.80(3) . ? OW2 H2W2 0.81(12) . ? O7 C16 1.260(15) . ? O5 C14 1.259(13) . ? O5 Cd1 2.346(8) 3 ? O3 C8 1.262(15) . ? O6 C14 1.254(13) . ? OW4 H2W4 0.82(14) . ? OW4 H1W4 0.82(8) . ? O1 C6 1.270(15) . ? O8 C16 1.238(15) . ? OW3 H1W3 0.84(11) . ? OW3 H2W3 0.84(18) . ? O2 C6 1.253(15) . ? O4 C8 1.248(14) . ? N2 C13 1.333(14) . ? N2 C9 1.347(14) . ? N1 C1 1.328(15) . ? N1 C5 1.343(14) . ? OW7 H2W7 0.84(14) . ? OW7 H1W7 0.9(12) . ? OW5 H1W5 0.82(3) . ? OW5 H2W5 0.81(10) . ? C14 C13 1.518(14) . ? C3 C4 1.386(16) . ? C3 C2 1.407(16) . ? C3 O9 1.508(18) . ? O10 C11 1.503(16) . ? O10 H11 0.8200 . ? OW1 H2W1 0.83(10) . ? OW1 H1W1 0.83(10) . ? C6 C1 1.525(15) . ? C13 C12 1.388(15) . ? C8 C5 1.506(15) . ? C2 C1 1.380(16) . ? C2 H2 0.9300 . ? C4 C5 1.391(15) . ? C4 H4 0.9300 . ? C9 C10 1.390(15) . ? C9 C16 1.519(16) . ? O9 H9 0.8200 . ? C12 C11 1.395(15) . ? C12 H12 0.9300 . ? C10 C11 1.386(16) . ? C10 H10 0.9300 . ? OW6' H2W6 0.80(3) . ? OW6' H1W6 0.81(3) . ? 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 OW5 Cd1 OW3 167.0(4) . . ? OW5 Cd1 N2 109.3(4) . . ? OW3 Cd1 N2 83.7(3) . . ? OW5 Cd1 O5 82.9(3) . 3 ? OW3 Cd1 O5 87.7(3) . 3 ? N2 Cd1 O5 135.5(3) . 3 ? OW5 Cd1 OW4 91.9(4) . . ? OW3 Cd1 OW4 78.2(3) . . ? N2 Cd1 OW4 135.0(3) . . ? O5 Cd1 OW4 84.8(3) 3 . ? OW5 Cd1 O7 86.0(3) . . ? OW3 Cd1 O7 99.3(3) . . ? N2 Cd1 O7 68.3(3) . . ? O5 Cd1 O7 156.1(3) 3 . ? OW4 Cd1 O7 74.4(3) . . ? OW5 Cd1 O5 96.0(3) . . ? OW3 Cd1 O5 89.0(3) . . ? N2 Cd1 O5 66.7(3) . . ? O5 Cd1 O5 69.5(3) 3 . ? OW4 Cd1 O5 151.8(3) . . ? O7 Cd1 O5 132.9(3) . . ? N1 Cd2 OW1 90.4(4) . . ? N1 Cd2 O7 154.1(3) . . ? OW1 Cd2 O7 81.8(4) . . ? N1 Cd2 O3 69.8(3) . . ? OW1 Cd2 O3 87.8(4) . . ? O7 Cd2 O3 133.9(3) . . ? N1 Cd2 O1 69.3(3) . . ? OW1 Cd2 O1 85.3(4) . . ? O7 Cd2 O1 85.4(3) . . ? O3 Cd2 O1 138.5(3) . . ? N1 Cd2 O8 149.4(3) . . ? OW1 Cd2 O8 84.8(4) . . ? O7 Cd2 O8 54.8(3) . . ? O3 Cd2 O8 79.7(3) . . ? O1 Cd2 O8 139.9(3) . . ? N1 Cd2 OW2 93.7(3) . . ? OW1 Cd2 OW2 173.2(3) . . ? O7 Cd2 OW2 92.2(3) . . ? O3 Cd2 OW2 98.7(3) . . ? O1 Cd2 OW2 91.1(3) . . ? O8 Cd2 OW2 94.4(3) . . ? N1 Cd2 C16 171.9(4) . . ? OW1 Cd2 C16 82.1(4) . . ? O7 Cd2 C16 27.7(3) . . ? O3 Cd2 C16 106.6(3) . . ? O1 Cd2 C16 112.9(3) . . ? O8 Cd2 C16 27.1(3) . . ? OW2 Cd2 C16 94.0(3) . . ? H2W6 OW6 H1W6 109(5) . . ? Cd2 OW2 H1W2 113(3) . . ? Cd2 OW2 H2W2 96(5) . . ? H1W2 OW2 H2W2 111.00 . . ? C16 O7 Cd2 91.3(7) . . ? C16 O7 Cd1 118.5(7) . . ? Cd2 O7 Cd1 147.8(4) . . ? C14 O5 Cd1 128.1(7) . 3 ? C14 O5 Cd1 118.5(7) . . ? Cd1 O5 Cd1 110.5(3) 3 . ? C8 O3 Cd2 117.5(8) . . ? Cd1 OW4 H2W4 120(10) . . ? Cd1 OW4 H1W4 101(10) . . ? H2W4 OW4 H1W4 106.00 . . ? C6 O1 Cd2 116.7(7) . . ? C16 O8 Cd2 89.0(8) . . ? Cd1 OW3 H1W3 122(10) . . ? Cd1 OW3 H2W3 124(10) . . ? H1W3 OW3 H2W3 105(16) . . ? C13 N2 C9 118.5(9) . . ? C13 N2 Cd1 121.3(7) . . ? C9 N2 Cd1 118.5(7) . . ? C1 N1 C5 120.2(10) . . ? C1 N1 Cd2 120.3(7) . . ? C5 N1 Cd2 119.0(7) . . ? H2W7 OW7 H1W7 107.00 . . ? Cd1 OW5 H1W5 110(10) . . ? Cd1 OW5 H2W5 122(10) . . ? H1W5 OW5 H2W5 113(10) . . ? O6 C14 O5 125.8(10) . . ? O6 C14 C13 118.0(9) . . ? O5 C14 C13 116.2(9) . . ? C4 C3 C2 117.7(11) . . ? C4 C3 O9 120.9(11) . . ? C2 C3 O9 121.4(11) . . ? C11 O10 H11 109.5 . . ? Cd2 OW1 H2W1 117(3) . . ? Cd2 OW1 H1W1 118(3) . . ? H2W1 OW1 H1W1 93.00 . . ? O2 C6 O1 126.6(11) . . ? O2 C6 C1 116.3(10) . . ? O1 C6 C1 117.0(10) . . ? N2 C13 C12 121.8(10) . . ? N2 C13 C14 115.1(9) . . ? C12 C13 C14 123.1(10) . . ? O4 C8 O3 124.9(11) . . ? O4 C8 C5 118.1(10) . . ? O3 C8 C5 117.1(10) . . ? C1 C2 C3 119.7(11) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C3 C4 C5 119.5(11) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N2 C9 C10 123.1(10) . . ? N2 C9 C16 114.7(10) . . ? C10 C9 C16 122.2(10) . . ? C3 O9 H9 109.5 . . ? C13 C12 C11 119.8(10) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? N1 C5 C4 121.3(10) . . ? N1 C5 C8 116.0(10) . . ? C4 C5 C8 122.7(10) . . ? C11 C10 C9 118.4(10) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C12 118.3(10) . . ? C10 C11 O10 120.8(10) . . ? C12 C11 O10 120.8(10) . . ? N1 C1 C2 121.5(10) . . ? N1 C1 C6 115.1(10) . . ? C2 C1 C6 123.4(10) . . ? O8 C16 O7 124.9(12) . . ? O8 C16 C9 118.5(11) . . ? O7 C16 C9 116.6(10) . . ? O8 C16 Cd2 63.9(7) . . ? O7 C16 Cd2 61.0(6) . . ? C9 C16 Cd2 177.5(8) . . ? H2W6 OW6' H1W6 108(5) . . ? 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 N1 Cd2 O7 C16 -162.4(9) . . . . ? OW1 Cd2 O7 C16 -88.7(8) . . . . ? O3 Cd2 O7 C16 -9.9(10) . . . . ? O1 Cd2 O7 C16 -174.7(8) . . . . ? O8 Cd2 O7 C16 0.7(8) . . . . ? OW2 Cd2 O7 C16 94.4(8) . . . . ? N1 Cd2 O7 Cd1 -3.7(14) . . . . ? OW1 Cd2 O7 Cd1 69.9(8) . . . . ? O3 Cd2 O7 Cd1 148.7(7) . . . . ? O1 Cd2 O7 Cd1 -16.0(8) . . . . ? O8 Cd2 O7 Cd1 159.3(10) . . . . ? OW2 Cd2 O7 Cd1 -106.9(8) . . . . ? C16 Cd2 O7 Cd1 158.6(14) . . . . ? OW5 Cd1 O7 C16 -127.3(10) . . . . ? OW3 Cd1 O7 C16 64.7(10) . . . . ? N2 Cd1 O7 C16 -14.6(9) . . . . ? O5 Cd1 O7 C16 170.3(9) 3 . . . ? OW4 Cd1 O7 C16 139.6(10) . . . . ? O5 Cd1 O7 C16 -32.7(11) . . . . ? OW5 Cd1 O7 Cd2 77.2(8) . . . . ? OW3 Cd1 O7 Cd2 -90.8(8) . . . . ? N2 Cd1 O7 Cd2 -170.2(9) . . . . ? O5 Cd1 O7 Cd2 14.8(14) 3 . . . ? OW4 Cd1 O7 Cd2 -15.9(8) . . . . ? O5 Cd1 O7 Cd2 171.8(6) . . . . ? OW5 Cd1 O5 C14 117.6(8) . . . . ? OW3 Cd1 O5 C14 -74.5(8) . . . . ? N2 Cd1 O5 C14 9.1(8) . . . . ? O5 Cd1 O5 C14 -162.4(10) 3 . . . ? OW4 Cd1 O5 C14 -136.8(8) . . . . ? O7 Cd1 O5 C14 27.4(10) . . . . ? OW5 Cd1 O5 Cd1 -80.1(4) . . . 3 ? OW3 Cd1 O5 Cd1 87.9(4) . . . 3 ? N2 Cd1 O5 Cd1 171.5(5) . . . 3 ? O5 Cd1 O5 Cd1 0.0 3 . . 3 ? OW4 Cd1 O5 Cd1 25.5(8) . . . 3 ? O7 Cd1 O5 Cd1 -170.3(3) . . . 3 ? N1 Cd2 O3 C8 -0.7(10) . . . . ? OW1 Cd2 O3 C8 -92.0(11) . . . . ? O7 Cd2 O3 C8 -168.3(9) . . . . ? O1 Cd2 O3 C8 -11.6(14) . . . . ? O8 Cd2 O3 C8 -177.1(11) . . . . ? OW2 Cd2 O3 C8 90.0(10) . . . . ? C16 Cd2 O3 C8 -173.1(10) . . . . ? N1 Cd2 O1 C6 10.9(9) . . . . ? OW1 Cd2 O1 C6 103.1(9) . . . . ? O7 Cd2 O1 C6 -174.8(9) . . . . ? O3 Cd2 O1 C6 21.9(12) . . . . ? O8 Cd2 O1 C6 179.3(9) . . . . ? OW2 Cd2 O1 C6 -82.6(9) . . . . ? C16 Cd2 O1 C6 -177.5(9) . . . . ? N1 Cd2 O8 C16 164.8(8) . . . . ? OW1 Cd2 O8 C16 82.9(9) . . . . ? O7 Cd2 O8 C16 -0.7(8) . . . . ? O3 Cd2 O8 C16 171.6(10) . . . . ? O1 Cd2 O8 C16 6.6(13) . . . . ? OW2 Cd2 O8 C16 -90.3(9) . . . . ? OW5 Cd1 N2 C13 -101.7(8) . . . . ? OW3 Cd1 N2 C13 78.2(8) . . . . ? O5 Cd1 N2 C13 -2.0(10) 3 . . . ? OW4 Cd1 N2 C13 144.6(8) . . . . ? O7 Cd1 N2 C13 -179.1(9) . . . . ? O5 Cd1 N2 C13 -13.4(8) . . . . ? OW5 Cd1 N2 C9 93.2(9) . . . . ? OW3 Cd1 N2 C9 -86.8(8) . . . . ? O5 Cd1 N2 C9 -167.0(7) 3 . . . ? OW4 Cd1 N2 C9 -20.4(10) . . . . ? O7 Cd1 N2 C9 15.9(8) . . . . ? O5 Cd1 N2 C9 -178.4(9) . . . . ? OW1 Cd2 N1 C1 -95.2(9) . . . . ? O7 Cd2 N1 C1 -23.4(14) . . . . ? O3 Cd2 N1 C1 177.3(10) . . . . ? O1 Cd2 N1 C1 -10.4(9) . . . . ? O8 Cd2 N1 C1 -175.6(9) . . . . ? OW2 Cd2 N1 C1 79.4(9) . . . . ? OW1 Cd2 N1 C5 92.9(9) . . . . ? O7 Cd2 N1 C5 164.6(8) . . . . ? O3 Cd2 N1 C5 5.4(8) . . . . ? O1 Cd2 N1 C5 177.7(10) . . . . ? O8 Cd2 N1 C5 12.5(14) . . . . ? OW2 Cd2 N1 C5 -92.5(9) . . . . ? Cd1 O5 C14 O6 17.0(17) 3 . . . ? Cd1 O5 C14 O6 175.8(9) . . . . ? Cd1 O5 C14 C13 -163.4(7) 3 . . . ? Cd1 O5 C14 C13 -4.5(13) . . . . ? Cd2 O1 C6 O2 169.0(10) . . . . ? Cd2 O1 C6 C1 -10.4(14) . . . . ? C9 N2 C13 C12 2.7(16) . . . . ? Cd1 N2 C13 C12 -162.3(8) . . . . ? C9 N2 C13 C14 -178.6(10) . . . . ? Cd1 N2 C13 C14 16.4(12) . . . . ? O6 C14 C13 N2 172.6(10) . . . . ? O5 C14 C13 N2 -7.1(14) . . . . ? O6 C14 C13 C12 -8.7(16) . . . . ? O5 C14 C13 C12 171.6(10) . . . . ? Cd2 O3 C8 O4 177.4(9) . . . . ? Cd2 O3 C8 C5 -3.4(15) . . . . ? C4 C3 C2 C1 -3.2(17) . . . . ? O9 C3 C2 C1 175.1(12) . . . . ? C2 C3 C4 C5 1.4(17) . . . . ? O9 C3 C4 C5 -177.0(12) . . . . ? C13 N2 C9 C10 -2.7(16) . . . . ? Cd1 N2 C9 C10 162.7(9) . . . . ? C13 N2 C9 C16 178.4(10) . . . . ? Cd1 N2 C9 C16 -16.2(13) . . . . ? N2 C13 C12 C11 0.3(16) . . . . ? C14 C13 C12 C11 -178.3(10) . . . . ? C1 N1 C5 C4 -2.4(17) . . . . ? Cd2 N1 C5 C4 169.5(8) . . . . ? C1 N1 C5 C8 179.0(10) . . . . ? Cd2 N1 C5 C8 -9.0(13) . . . . ? C3 C4 C5 N1 1.4(17) . . . . ? C3 C4 C5 C8 179.9(11) . . . . ? O4 C8 C5 N1 -172.6(10) . . . . ? O3 C8 C5 N1 8.2(16) . . . . ? O4 C8 C5 C4 8.9(17) . . . . ? O3 C8 C5 C4 -170.3(12) . . . . ? N2 C9 C10 C11 -0.2(17) . . . . ? C16 C9 C10 C11 178.6(11) . . . . ? C9 C10 C11 C12 3.1(16) . . . . ? C9 C10 C11 O10 -175.0(11) . . . . ? C13 C12 C11 C10 -3.2(16) . . . . ? C13 C12 C11 O10 174.9(11) . . . . ? C5 N1 C1 C2 0.5(17) . . . . ? Cd2 N1 C1 C2 -171.3(9) . . . . ? C5 N1 C1 C6 -179.1(10) . . . . ? Cd2 N1 C1 C6 9.1(14) . . . . ? C3 C2 C1 N1 2.3(18) . . . . ? C3 C2 C1 C6 -178.2(11) . . . . ? O2 C6 C1 N1 -178.0(11) . . . . ? O1 C6 C1 N1 1.4(16) . . . . ? O2 C6 C1 C2 2.4(17) . . . . ? O1 C6 C1 C2 -178.2(11) . . . . ? Cd2 O8 C16 O7 1.3(15) . . . . ? Cd2 O8 C16 C9 -179.0(10) . . . . ? Cd2 O7 C16 O8 -1.3(16) . . . . ? Cd1 O7 C16 O8 -168.6(12) . . . . ? Cd2 O7 C16 C9 179.0(10) . . . . ? Cd1 O7 C16 C9 11.7(15) . . . . ? Cd1 O7 C16 Cd2 -167.3(8) . . . . ? N2 C9 C16 O8 -177.1(12) . . . . ? C10 C9 C16 O8 4.0(19) . . . . ? N2 C9 C16 O7 2.6(16) . . . . ? C10 C9 C16 O7 -176.2(11) . . . . ? OW1 Cd2 C16 O8 -93.9(10) . . . . ? O7 Cd2 C16 O8 178.8(14) . . . . ? O3 Cd2 C16 O8 -8.6(10) . . . . ? O1 Cd2 C16 O8 -175.4(9) . . . . ? OW2 Cd2 C16 O8 91.7(9) . . . . ? OW1 Cd2 C16 O7 87.3(8) . . . . ? O3 Cd2 C16 O7 172.5(8) . . . . ? O1 Cd2 C16 O7 5.8(9) . . . . ? O8 Cd2 C16 O7 -178.8(14) . . . . ? OW2 Cd2 C16 O7 -87.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.703 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.330 #===END of CIF for Complex 2 ===================== data_complex3 _database_code_depnum_ccdc_archive 'CCDC 697861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H34 N4 Ni3 O22' _chemical_formula_weight 858.64 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.472(3) _cell_length_b 8.752(4) _cell_length_c 11.646(4) _cell_angle_alpha 92.638(5) _cell_angle_beta 101.187(4) _cell_angle_gamma 90.541(5) _cell_volume 746.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description needles _exptl_crystal_colour Green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 1.977 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7173 _exptl_absorpt_correction_T_max 0.7973 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4983 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.34 _reflns_number_total 3537 _reflns_number_gt 3266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0560P)^2^+0.2761P] 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 3537 _refine_ls_number_parameters 267 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.029 _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 Ni1 Ni 0.0000 1.0000 0.5000 0.00954(10) Uani 1 2 d S . . Ni2 Ni 0.74884(3) 0.28398(3) 0.846015(19) 0.00943(9) Uani 1 1 d . . . O1 O 0.62640(18) 0.21260(16) 0.66886(11) 0.0128(3) Uani 1 1 d . . . O2 O 0.42844(18) 0.28586(16) 0.51200(11) 0.0129(3) Uani 1 1 d . . . O3 O 0.79369(18) 0.43422(16) 0.99517(11) 0.0128(3) Uani 1 1 d . . . O4 O 0.72769(17) 0.66615(16) 1.05991(11) 0.0132(3) Uani 1 1 d . . . O5 O 0.31716(19) 0.96450(16) 0.73899(12) 0.0172(3) Uani 1 1 d . . . O6 O 0.13529(18) 0.82511(16) 0.59603(12) 0.0125(3) Uani 1 1 d . . . OW1 O 0.54493(18) 0.15603(16) 0.89812(12) 0.0126(3) Uani 1 1 d D . . OW2 O 0.95921(19) 0.37754(17) 0.77386(12) 0.0130(3) Uani 1 1 d D . . OW3 O 0.8772(2) 0.6033(2) 0.63257(18) 0.0338(4) Uani 1 1 d D . . OW4 O -0.10463(19) 0.83137(17) 0.37653(12) 0.0136(3) Uani 1 1 d D . . OW5 O -0.22409(19) 0.96928(17) 0.57389(12) 0.0139(3) Uani 1 1 d D . . N1 N 0.5843(2) 0.45584(18) 0.79254(13) 0.0094(3) Uani 1 1 d . . . N2 N 0.9360(2) 0.12982(19) 0.92694(14) 0.0114(3) Uani 1 1 d . . . C1 C 0.7126(2) 0.5585(2) 0.98313(15) 0.0107(3) Uani 1 1 d . . . C2 C 0.5859(2) 0.5778(2) 0.86589(15) 0.0107(3) Uani 1 1 d . . . C3 C 0.4837(2) 0.7045(2) 0.83299(15) 0.0110(3) Uani 1 1 d . . . H3 H 0.4883 0.7902 0.8838 0.013 Uiso 1 1 calc R . . C4 C 0.3728(2) 0.7007(2) 0.72107(16) 0.0110(3) Uani 1 1 d . . . C5 C 0.2671(2) 0.8419(2) 0.68248(15) 0.0107(3) Uani 1 1 d . . . C6 C 0.3676(2) 0.5695(2) 0.64714(16) 0.0110(3) Uani 1 1 d . . . H6 H 0.2901 0.5629 0.5742 0.013 Uiso 1 1 calc R . . C7 C 0.4808(2) 0.4493(2) 0.68506(15) 0.0100(3) Uani 1 1 d . . . C8 C 0.5115(2) 0.3041(2) 0.61495(16) 0.0111(3) Uani 1 1 d . . . C9 C 0.9482(3) 0.1361(2) 1.05619(16) 0.0154(4) Uani 1 1 d . . . H9A H 0.8303 0.1078 1.0729 0.018 Uiso 1 1 calc R . . H9B H 0.9767 0.2403 1.0866 0.018 Uiso 1 1 calc R . . C10 C 1.0915(3) 0.0311(2) 1.11877(16) 0.0150(4) Uani 1 1 d . . . H10A H 1.2112 0.0668 1.1101 0.018 Uiso 1 1 calc R . . H10B H 1.0883 0.0359 1.2017 0.018 Uiso 1 1 calc R . . H1N2 H 1.035(4) 0.166(3) 0.916(2) 0.020(6) Uiso 1 1 d . . . H1W1 H 0.496(3) 0.095(3) 0.8485(18) 0.018(6) Uiso 1 1 d D . . H2W5 H -0.294(3) 0.900(3) 0.544(2) 0.026(7) Uiso 1 1 d D . . H2W1 H 0.465(3) 0.210(3) 0.913(2) 0.016(6) Uiso 1 1 d D . . H2W2 H 1.047(3) 0.391(4) 0.826(2) 0.033(8) Uiso 1 1 d D . . H1W5 H -0.272(4) 1.045(3) 0.598(2) 0.032(8) Uiso 1 1 d D . . H1W4 H -0.170(4) 0.887(3) 0.331(2) 0.034(8) Uiso 1 1 d D . . H2W3 H 0.953(4) 0.660(3) 0.616(3) 0.043(9) Uiso 1 1 d D . . H1W2 H 0.935(4) 0.452(3) 0.733(2) 0.041(9) Uiso 1 1 d D . . H1W3 H 0.786(3) 0.633(4) 0.590(2) 0.039(9) Uiso 1 1 d D . . H2W4 H -0.045(4) 0.774(3) 0.340(2) 0.034(8) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00842(17) 0.00955(17) 0.01033(16) 0.00006(12) 0.00104(12) 0.00195(12) Ni2 0.00777(14) 0.00991(14) 0.01057(13) 0.00065(9) 0.00151(9) 0.00229(9) O1 0.0095(6) 0.0109(7) 0.0117(6) 0.0006(5) 0.0018(5) 0.0034(5) O2 0.0126(6) 0.0141(7) 0.0118(6) -0.0015(5) 0.0021(5) -0.0006(5) O3 0.0113(6) 0.0129(7) 0.0132(6) 0.0001(5) 0.0000(5) 0.0030(5) O4 0.0103(6) 0.0151(7) 0.0137(6) -0.0031(5) 0.0018(5) 0.0012(5) O5 0.0174(7) 0.0129(7) 0.0180(7) -0.0020(5) -0.0036(5) 0.0022(5) O6 0.0100(6) 0.0126(7) 0.0136(6) 0.0017(5) -0.0015(5) 0.0015(5) OW1 0.0094(6) 0.0130(7) 0.0149(6) -0.0022(5) 0.0018(5) 0.0005(5) OW2 0.0090(6) 0.0158(7) 0.0136(6) 0.0024(5) 0.0004(5) 0.0000(5) OW3 0.0170(8) 0.0321(10) 0.0489(11) 0.0269(9) -0.0075(7) -0.0075(7) OW4 0.0133(7) 0.0128(7) 0.0141(6) -0.0006(5) 0.0015(5) 0.0040(5) OW5 0.0113(7) 0.0124(7) 0.0185(7) -0.0038(6) 0.0054(5) 0.0004(5) N1 0.0071(7) 0.0105(7) 0.0107(7) 0.0016(6) 0.0014(5) 0.0020(5) N2 0.0091(8) 0.0128(8) 0.0129(7) 0.0028(6) 0.0027(6) 0.0017(6) C1 0.0066(8) 0.0138(9) 0.0120(8) 0.0022(7) 0.0024(6) 0.0001(6) C2 0.0085(8) 0.0118(9) 0.0118(8) 0.0001(7) 0.0025(6) -0.0008(6) C3 0.0086(8) 0.0119(9) 0.0125(8) 0.0003(7) 0.0025(6) 0.0013(6) C4 0.0079(8) 0.0121(9) 0.0134(8) 0.0019(7) 0.0029(6) 0.0011(6) C5 0.0093(8) 0.0121(9) 0.0114(8) 0.0020(7) 0.0031(6) 0.0018(6) C6 0.0086(8) 0.0126(9) 0.0124(8) 0.0012(7) 0.0032(6) 0.0006(6) C7 0.0078(8) 0.0122(9) 0.0100(8) 0.0004(6) 0.0021(6) 0.0000(6) C8 0.0084(8) 0.0122(9) 0.0135(8) 0.0004(7) 0.0045(6) -0.0004(6) C9 0.0177(10) 0.0158(10) 0.0121(8) 0.0008(7) 0.0012(7) 0.0066(7) C10 0.0161(9) 0.0136(9) 0.0142(8) 0.0004(7) 0.0002(7) 0.0048(7) _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 Ni1 OW5 2.0466(17) 2_576 ? Ni1 OW5 2.0466(17) . ? Ni1 OW4 2.0503(16) 2_576 ? Ni1 OW4 2.0503(16) . ? Ni1 O6 2.0889(15) . ? Ni1 O6 2.0889(15) 2_576 ? Ni2 N1 1.9965(18) . ? Ni2 N2 2.0750(18) . ? Ni2 OW1 2.0815(16) . ? Ni2 OW2 2.0974(17) . ? Ni2 O3 2.1010(15) . ? Ni2 O1 2.1499(15) . ? O1 C8 1.274(2) . ? O2 C8 1.241(2) . ? O3 C1 1.251(2) . ? O4 C1 1.257(2) . ? O5 C5 1.248(2) . ? O6 C5 1.267(2) . ? OW1 H1W1 0.799(17) . ? OW1 H2W1 0.805(17) . ? OW2 H2W2 0.810(18) . ? OW2 H1W2 0.824(18) . ? OW3 H2W3 0.804(18) . ? OW3 H1W3 0.808(18) . ? OW4 H1W4 0.829(17) . ? OW4 H2W4 0.831(18) . ? OW5 H2W5 0.815(17) . ? OW5 H1W5 0.819(17) . ? N1 C2 1.335(2) . ? N1 C7 1.336(2) . ? N2 C10 1.480(3) 2_757 ? N2 C9 1.489(2) . ? N2 H1N2 0.84(3) . ? C1 C2 1.520(2) . ? C2 C3 1.379(3) . ? C3 C4 1.401(2) . ? C3 H3 0.9300 . ? C4 C6 1.399(3) . ? C4 C5 1.511(3) . ? C6 C7 1.390(3) . ? C6 H6 0.9300 . ? C7 C8 1.522(3) . ? C9 C10 1.517(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.480(3) 2_757 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? 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 OW5 Ni1 OW5 180.0 2_576 . ? OW5 Ni1 OW4 87.99(6) 2_576 2_576 ? OW5 Ni1 OW4 92.01(6) . 2_576 ? OW5 Ni1 OW4 92.01(6) 2_576 . ? OW5 Ni1 OW4 87.99(6) . . ? OW4 Ni1 OW4 180.0 2_576 . ? OW5 Ni1 O6 89.04(6) 2_576 . ? OW5 Ni1 O6 90.96(6) . . ? OW4 Ni1 O6 93.88(7) 2_576 . ? OW4 Ni1 O6 86.12(7) . . ? OW5 Ni1 O6 90.96(6) 2_576 2_576 ? OW5 Ni1 O6 89.04(6) . 2_576 ? OW4 Ni1 O6 86.12(7) 2_576 2_576 ? OW4 Ni1 O6 93.88(7) . 2_576 ? O6 Ni1 O6 180.000(1) . 2_576 ? N1 Ni2 N2 170.13(6) . . ? N1 Ni2 OW1 94.05(7) . . ? N2 Ni2 OW1 88.04(7) . . ? N1 Ni2 OW2 91.63(7) . . ? N2 Ni2 OW2 87.85(7) . . ? OW1 Ni2 OW2 169.53(6) . . ? N1 Ni2 O3 78.08(6) . . ? N2 Ni2 O3 92.15(7) . . ? OW1 Ni2 O3 94.98(6) . . ? OW2 Ni2 O3 94.79(6) . . ? N1 Ni2 O1 76.56(6) . . ? N2 Ni2 O1 113.21(6) . . ? OW1 Ni2 O1 87.03(6) . . ? OW2 Ni2 O1 85.75(6) . . ? O3 Ni2 O1 154.63(5) . . ? C8 O1 Ni2 115.65(12) . . ? C1 O3 Ni2 115.30(12) . . ? C5 O6 Ni1 126.18(13) . . ? Ni2 OW1 H1W1 113.0(18) . . ? Ni2 OW1 H2W1 110.8(19) . . ? H1W1 OW1 H2W1 106(3) . . ? Ni2 OW2 H2W2 108(2) . . ? Ni2 OW2 H1W2 117(2) . . ? H2W2 OW2 H1W2 114(3) . . ? H2W3 OW3 H1W3 100(3) . . ? Ni1 OW4 H1W4 97(2) . . ? Ni1 OW4 H2W4 126(2) . . ? H1W4 OW4 H2W4 110(3) . . ? Ni1 OW5 H2W5 116(2) . . ? Ni1 OW5 H1W5 118(2) . . ? H2W5 OW5 H1W5 116(3) . . ? C2 N1 C7 121.70(16) . . ? C2 N1 Ni2 117.92(12) . . ? C7 N1 Ni2 120.34(13) . . ? C10 N2 C9 109.28(15) 2_757 . ? C10 N2 Ni2 115.79(12) 2_757 . ? C9 N2 Ni2 111.62(12) . . ? C10 N2 H1N2 111.0(18) 2_757 . ? C9 N2 H1N2 105.9(18) . . ? Ni2 N2 H1N2 102.6(18) . . ? O3 C1 O4 125.13(17) . . ? O3 C1 C2 116.31(16) . . ? O4 C1 C2 118.56(17) . . ? N1 C2 C3 121.35(16) . . ? N1 C2 C1 112.22(16) . . ? C3 C2 C1 126.42(17) . . ? C2 C3 C4 118.30(17) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C6 C4 C3 119.47(18) . . ? C6 C4 C5 121.97(17) . . ? C3 C4 C5 118.52(17) . . ? O5 C5 O6 125.84(18) . . ? O5 C5 C4 117.02(16) . . ? O6 C5 C4 117.15(17) . . ? C7 C6 C4 118.58(17) . . ? C7 C6 H6 120.7 . . ? C4 C6 H6 120.7 . . ? N1 C7 C6 120.47(17) . . ? N1 C7 C8 112.13(16) . . ? C6 C7 C8 127.35(16) . . ? O2 C8 O1 125.85(18) . . ? O2 C8 C7 118.83(17) . . ? O1 C8 C7 115.30(16) . . ? N2 C9 C10 112.95(16) . . ? N2 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N2 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N2 C10 C9 112.59(16) 2_757 . ? N2 C10 H10A 109.1 2_757 . ? C9 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 2_757 . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? 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 N1 Ni2 O1 C8 -0.91(12) . . . . ? N2 Ni2 O1 C8 -179.43(12) . . . . ? OW1 Ni2 O1 C8 93.98(14) . . . . ? OW2 Ni2 O1 C8 -93.61(13) . . . . ? O3 Ni2 O1 C8 -1.4(2) . . . . ? N1 Ni2 O3 C1 -3.81(13) . . . . ? N2 Ni2 O3 C1 174.86(13) . . . . ? OW1 Ni2 O3 C1 -96.92(14) . . . . ? OW2 Ni2 O3 C1 86.84(14) . . . . ? O1 Ni2 O3 C1 -3.3(2) . . . . ? OW5 Ni1 O6 C5 72.69(16) 2_576 . . . ? OW5 Ni1 O6 C5 -107.31(16) . . . . ? OW4 Ni1 O6 C5 -15.23(16) 2_576 . . . ? OW4 Ni1 O6 C5 164.77(16) . . . . ? OW1 Ni2 N1 C2 97.57(14) . . . . ? OW2 Ni2 N1 C2 -91.23(14) . . . . ? O3 Ni2 N1 C2 3.32(13) . . . . ? O1 Ni2 N1 C2 -176.47(14) . . . . ? OW1 Ni2 N1 C7 -84.47(14) . . . . ? OW2 Ni2 N1 C7 86.73(14) . . . . ? O3 Ni2 N1 C7 -178.71(15) . . . . ? O1 Ni2 N1 C7 1.50(13) . . . . ? OW1 Ni2 N2 C10 60.21(13) . . . 2_757 ? OW2 Ni2 N2 C10 -110.16(14) . . . 2_757 ? O3 Ni2 N2 C10 155.12(13) . . . 2_757 ? O1 Ni2 N2 C10 -25.72(15) . . . 2_757 ? OW1 Ni2 N2 C9 -65.66(13) . . . . ? OW2 Ni2 N2 C9 123.97(13) . . . . ? O3 Ni2 N2 C9 29.25(13) . . . . ? O1 Ni2 N2 C9 -151.59(12) . . . . ? Ni2 O3 C1 O4 -176.73(14) . . . . ? Ni2 O3 C1 C2 3.6(2) . . . . ? C7 N1 C2 C3 -1.5(3) . . . . ? Ni2 N1 C2 C3 176.41(13) . . . . ? C7 N1 C2 C1 179.59(15) . . . . ? Ni2 N1 C2 C1 -2.48(19) . . . . ? O3 C1 C2 N1 -0.9(2) . . . . ? O4 C1 C2 N1 179.42(16) . . . . ? O3 C1 C2 C3 -179.73(17) . . . . ? O4 C1 C2 C3 0.6(3) . . . . ? N1 C2 C3 C4 1.9(3) . . . . ? C1 C2 C3 C4 -179.37(16) . . . . ? C2 C3 C4 C6 0.6(3) . . . . ? C2 C3 C4 C5 -177.25(16) . . . . ? Ni1 O6 C5 O5 14.2(3) . . . . ? Ni1 O6 C5 C4 -166.07(12) . . . . ? C6 C4 C5 O5 -160.65(18) . . . . ? C3 C4 C5 O5 17.1(2) . . . . ? C6 C4 C5 O6 19.6(3) . . . . ? C3 C4 C5 O6 -162.61(17) . . . . ? C3 C4 C6 C7 -3.4(3) . . . . ? C5 C4 C6 C7 174.40(15) . . . . ? C2 N1 C7 C6 -1.4(3) . . . . ? Ni2 N1 C7 C6 -179.30(13) . . . . ? C2 N1 C7 C8 176.12(15) . . . . ? Ni2 N1 C7 C8 -1.8(2) . . . . ? C4 C6 C7 N1 3.8(3) . . . . ? C4 C6 C7 C8 -173.31(17) . . . . ? Ni2 O1 C8 O2 178.60(14) . . . . ? Ni2 O1 C8 C7 0.29(19) . . . . ? N1 C7 C8 O2 -177.56(16) . . . . ? C6 C7 C8 O2 -0.2(3) . . . . ? N1 C7 C8 O1 0.9(2) . . . . ? C6 C7 C8 O1 178.21(17) . . . . ? C10 N2 C9 C10 53.8(2) 2_757 . . . ? Ni2 N2 C9 C10 -176.79(13) . . . . ? N2 C9 C10 N2 -55.6(2) . . . 2_757 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.642 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.103 #===END of CIF for Complex 3 ===================== data_complex4 _database_code_depnum_ccdc_archive 'CCDC 697862' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Mn3 N2 O16' _chemical_formula_weight 653.10 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.434(3) _cell_length_b 8.585(4) _cell_length_c 9.880(3) _cell_angle_alpha 110.107(5) _cell_angle_beta 95.052(4) _cell_angle_gamma 102.072(5) _cell_volume 493.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description cubic _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 325 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7682 _exptl_absorpt_correction_T_max 0.8260 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3245 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2434 _reflns_number_gt 2094 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0350P)^2^+2.5056P] 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 2334 _refine_ls_number_parameters 185 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.114 _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 Mn1 Mn 0.06464(15) 0.06079(11) 0.33009(10) 0.0184(3) Uani 1 1 d . . . Mn2 Mn -0.5000 0.5000 0.0000 0.0204(3) Uani 1 2 d S . . O3 O -0.0499(7) 0.8366(5) 0.3997(5) 0.0212(9) Uani 1 1 d . . . O4 O -0.2203(8) 0.6217(6) 0.1889(5) 0.0258(10) Uani 1 1 d . . . OW1 O 0.0477(8) -0.1490(6) 0.1158(5) 0.0232(9) Uani 1 1 d D . . O2 O -0.6050(7) 0.0303(6) 0.3575(5) 0.0229(9) Uani 1 1 d . . . O6 O -0.8732(9) 0.1921(6) 0.1623(5) 0.0313(11) Uani 1 1 d . . . OW2 O -0.4326(9) 0.2535(6) -0.0547(6) 0.0317(11) Uani 1 1 d D . . O1 O -0.2886(7) 0.0229(5) 0.2820(5) 0.0222(9) Uani 1 1 d . . . O5 O -0.7251(8) 0.4339(6) 0.1280(5) 0.0273(10) Uani 1 1 d . . . C5 C -0.2112(9) 0.5674(7) 0.4077(6) 0.0163(11) Uani 1 1 d . . . N1 N -0.1863(8) 0.6457(6) 0.5538(5) 0.0169(9) Uani 1 1 d . . . C6 C -0.1558(9) 0.6847(7) 0.3251(6) 0.0165(11) Uani 1 1 d . . . C8 C -0.7880(10) 0.3492(8) 0.2059(6) 0.0182(11) Uani 1 1 d . . . C4 C -0.2823(9) 0.3907(8) 0.3376(7) 0.0194(11) Uani 1 1 d . . . H4 H -0.2916 0.3393 0.2369 0.023 Uiso 1 1 calc R . . C2 C -0.3220(10) 0.3728(8) 0.5712(7) 0.0207(12) Uani 1 1 d . . . H2 H -0.3628 0.3102 0.6292 0.025 Uiso 1 1 calc R . . C7 C -0.4173(10) 0.1007(7) 0.3492(7) 0.0200(12) Uani 1 1 d . . . C3 C -0.3395(9) 0.2915(7) 0.4212(7) 0.0190(11) Uani 1 1 d . . . C1 C -0.2417(9) 0.5508(8) 0.6332(7) 0.0195(11) Uani 1 1 d . . . H1W2 H -0.315(6) 0.236(9) -0.071(7) 0.05(6) Uiso 1 1 d D . . H2W2 H -0.517(11) 0.163(6) -0.110(8) 0.03(2) Uiso 1 1 d D . . H1W1 H 0.002(16) -0.143(13) 0.038(6) 0.05(3) Uiso 1 1 d D . . H2W1 H -0.027(10) -0.238(5) 0.116(8) 0.016(17) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0179(5) 0.0156(5) 0.0200(5) 0.0057(3) 0.0035(3) 0.0026(3) Mn2 0.0241(7) 0.0179(6) 0.0171(6) 0.0064(5) 0.0047(5) 0.0010(5) O3 0.026(2) 0.016(2) 0.018(2) 0.0061(16) 0.0012(16) -0.0013(17) O4 0.037(3) 0.020(2) 0.016(2) 0.0068(17) 0.0022(18) 0.0001(19) OW1 0.028(2) 0.019(2) 0.019(2) 0.0081(17) 0.0018(18) -0.0026(18) O2 0.0111(19) 0.023(2) 0.033(2) 0.0078(19) 0.0048(17) 0.0014(16) O6 0.047(3) 0.022(2) 0.020(2) 0.0057(19) 0.002(2) 0.004(2) OW2 0.028(3) 0.018(2) 0.041(3) 0.000(2) 0.005(2) 0.007(2) O1 0.019(2) 0.016(2) 0.026(2) 0.0008(17) 0.0039(17) 0.0036(17) O5 0.034(3) 0.031(2) 0.021(2) 0.0157(19) 0.0169(19) 0.002(2) C5 0.016(3) 0.017(3) 0.015(3) 0.005(2) 0.004(2) 0.002(2) N1 0.018(2) 0.012(2) 0.019(2) 0.0045(18) 0.0032(18) 0.0018(18) C6 0.020(3) 0.013(2) 0.019(3) 0.010(2) 0.003(2) 0.004(2) C8 0.018(3) 0.018(3) 0.016(3) 0.004(2) 0.005(2) 0.004(2) C4 0.015(3) 0.020(3) 0.017(3) 0.004(2) 0.002(2) -0.002(2) C2 0.019(3) 0.021(3) 0.021(3) 0.005(2) 0.013(2) 0.002(2) C7 0.021(3) 0.013(3) 0.021(3) 0.004(2) 0.000(2) 0.001(2) C3 0.015(3) 0.015(3) 0.021(3) 0.003(2) 0.002(2) 0.000(2) C1 0.014(3) 0.020(3) 0.022(3) 0.004(2) 0.001(2) 0.004(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 Mn1 O2 2.200(5) 1_655 ? Mn1 O1 2.211(5) . ? Mn1 OW1 2.234(5) . ? Mn1 O3 2.264(4) 1_545 ? Mn1 N1 2.304(5) 2_566 ? Mn1 O6 2.322(5) 1_655 ? Mn1 O3 2.525(5) 2_566 ? Mn2 O5 2.119(4) 2_465 ? Mn2 O5 2.119(4) . ? Mn2 OW2 2.144(5) . ? Mn2 OW2 2.144(5) 2_465 ? Mn2 O4 2.257(5) 2_465 ? Mn2 O4 2.257(5) . ? O3 C6 1.260(7) . ? O3 Mn1 2.264(4) 1_565 ? O3 Mn1 2.525(5) 2_566 ? O4 C6 1.258(7) . ? OW1 H1W1 0.82(7) . ? OW1 H2W1 0.81(5) . ? O2 C7 1.255(7) . ? O2 Mn1 2.200(5) 1_455 ? O6 C8 1.247(8) . ? O6 Mn1 2.322(5) 1_455 ? OW2 H1W2 0.82(2) . ? OW2 H2W2 0.82(6) . ? O1 C7 1.264(8) . ? O5 C8 1.266(7) . ? C5 N1 1.344(7) . ? C5 C4 1.386(8) . ? C5 C6 1.509(8) . ? N1 C1 1.332(8) . ? N1 Mn1 2.304(5) 2_566 ? C8 C1 1.497(8) 2_466 ? C4 C3 1.397(9) . ? C4 H4 0.9300 . ? C2 C3 1.387(8) . ? C2 C1 1.395(8) . ? C2 H2 0.9300 . ? C7 C3 1.494(8) . ? C1 C8 1.497(8) 2_466 ? 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 O2 Mn1 O1 166.12(17) 1_655 . ? O2 Mn1 OW1 80.19(18) 1_655 . ? O1 Mn1 OW1 89.81(17) . . ? O2 Mn1 O3 89.21(17) 1_655 1_545 ? O1 Mn1 O3 79.89(17) . 1_545 ? OW1 Mn1 O3 82.47(17) . 1_545 ? O2 Mn1 N1 91.43(18) 1_655 2_566 ? O1 Mn1 N1 102.37(17) . 2_566 ? OW1 Mn1 N1 140.96(18) . 2_566 ? O3 Mn1 N1 135.87(17) 1_545 2_566 ? O2 Mn1 O6 93.66(19) 1_655 1_655 ? O1 Mn1 O6 92.71(19) . 1_655 ? OW1 Mn1 O6 73.60(17) . 1_655 ? O3 Mn1 O6 155.00(17) 1_545 1_655 ? N1 Mn1 O6 68.94(18) 2_566 1_655 ? O2 Mn1 O3 94.59(17) 1_655 2_566 ? O1 Mn1 O3 89.53(16) . 2_566 ? OW1 Mn1 O3 151.15(16) . 2_566 ? O3 Mn1 O3 69.03(17) 1_545 2_566 ? N1 Mn1 O3 66.94(16) 2_566 2_566 ? O6 Mn1 O3 135.24(16) 1_655 2_566 ? O5 Mn2 O5 180.0 2_465 . ? O5 Mn2 OW2 90.0(2) 2_465 . ? O5 Mn2 OW2 90.0(2) . . ? O5 Mn2 OW2 90.0(2) 2_465 2_465 ? O5 Mn2 OW2 90.0(2) . 2_465 ? OW2 Mn2 OW2 180.000(1) . 2_465 ? O5 Mn2 O4 94.33(19) 2_465 2_465 ? O5 Mn2 O4 85.67(19) . 2_465 ? OW2 Mn2 O4 87.97(19) . 2_465 ? OW2 Mn2 O4 92.03(19) 2_465 2_465 ? O5 Mn2 O4 85.67(19) 2_465 . ? O5 Mn2 O4 94.33(19) . . ? OW2 Mn2 O4 92.03(19) . . ? OW2 Mn2 O4 87.97(19) 2_465 . ? O4 Mn2 O4 180.00(19) 2_465 . ? C6 O3 Mn1 130.3(4) . 1_565 ? C6 O3 Mn1 115.7(4) . 2_566 ? Mn1 O3 Mn1 110.97(17) 1_565 2_566 ? C6 O4 Mn2 148.3(4) . . ? Mn1 OW1 H1W1 121(7) . . ? Mn1 OW1 H2W1 109(5) . . ? H1W1 OW1 H2W1 105(9) . . ? C7 O2 Mn1 139.7(4) . 1_455 ? C8 O6 Mn1 120.0(4) . 1_455 ? Mn2 OW2 H1W2 124(5) . . ? Mn2 OW2 H2W2 124(6) . . ? H1W2 OW2 H2W2 102(8) . . ? C7 O1 Mn1 132.6(4) . . ? C8 O5 Mn2 149.6(5) . . ? N1 C5 C4 122.4(5) . . ? N1 C5 C6 115.5(5) . . ? C4 C5 C6 122.1(5) . . ? C1 N1 C5 118.7(5) . . ? C1 N1 Mn1 119.0(4) . 2_566 ? C5 N1 Mn1 122.2(4) . 2_566 ? O4 C6 O3 126.5(5) . . ? O4 C6 C5 116.9(5) . . ? O3 C6 C5 116.6(5) . . ? O6 C8 O5 126.7(6) . . ? O6 C8 C1 117.0(5) . 2_466 ? O5 C8 C1 116.2(5) . 2_466 ? C5 C4 C3 118.6(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C3 C2 C1 118.5(6) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? O2 C7 O1 125.0(6) . . ? O2 C7 C3 118.2(5) . . ? O1 C7 C3 116.8(5) . . ? C2 C3 C4 118.9(5) . . ? C2 C3 C7 121.0(6) . . ? C4 C3 C7 120.1(5) . . ? N1 C1 C2 122.7(6) . . ? N1 C1 C8 114.5(5) . 2_466 ? C2 C1 C8 122.8(6) . 2_466 ? 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 O5 Mn2 O4 C6 162.5(8) 2_465 . . . ? O5 Mn2 O4 C6 -17.5(8) . . . . ? OW2 Mn2 O4 C6 -107.7(8) . . . . ? OW2 Mn2 O4 C6 72.3(8) 2_465 . . . ? O2 Mn1 O1 C7 140.3(7) 1_655 . . . ? OW1 Mn1 O1 C7 -176.0(6) . . . . ? O3 Mn1 O1 C7 101.6(6) 1_545 . . . ? N1 Mn1 O1 C7 -33.4(6) 2_566 . . . ? O6 Mn1 O1 C7 -102.5(6) 1_655 . . . ? O3 Mn1 O1 C7 32.8(6) 2_566 . . . ? OW2 Mn2 O5 C8 28.1(9) . . . . ? OW2 Mn2 O5 C8 -151.9(9) 2_465 . . . ? O4 Mn2 O5 C8 116.0(9) 2_465 . . . ? O4 Mn2 O5 C8 -64.0(9) . . . . ? C4 C5 N1 C1 -3.3(9) . . . . ? C6 C5 N1 C1 176.9(5) . . . . ? C4 C5 N1 Mn1 179.3(4) . . . 2_566 ? C6 C5 N1 Mn1 -0.5(7) . . . 2_566 ? Mn2 O4 C6 O3 -117.6(8) . . . . ? Mn2 O4 C6 C5 62.2(10) . . . . ? Mn1 O3 C6 O4 1.4(10) 1_565 . . . ? Mn1 O3 C6 O4 159.4(5) 2_566 . . . ? Mn1 O3 C6 C5 -178.4(4) 1_565 . . . ? Mn1 O3 C6 C5 -20.3(6) 2_566 . . . ? N1 C5 C6 O4 -165.0(5) . . . . ? C4 C5 C6 O4 15.2(9) . . . . ? N1 C5 C6 O3 14.8(8) . . . . ? C4 C5 C6 O3 -165.0(6) . . . . ? Mn1 O6 C8 O5 172.3(5) 1_455 . . . ? Mn1 O6 C8 C1 -8.3(8) 1_455 . . 2_466 ? Mn2 O5 C8 O6 -72.9(11) . . . . ? Mn2 O5 C8 C1 107.7(8) . . . 2_466 ? N1 C5 C4 C3 3.1(9) . . . . ? C6 C5 C4 C3 -177.2(5) . . . . ? Mn1 O2 C7 O1 -132.2(6) 1_455 . . . ? Mn1 O2 C7 C3 46.6(9) 1_455 . . . ? Mn1 O1 C7 O2 -142.6(5) . . . . ? Mn1 O1 C7 C3 38.6(8) . . . . ? C1 C2 C3 C4 -1.8(9) . . . . ? C1 C2 C3 C7 178.0(6) . . . . ? C5 C4 C3 C2 -0.4(9) . . . . ? C5 C4 C3 C7 179.8(5) . . . . ? O2 C7 C3 C2 61.8(8) . . . . ? O1 C7 C3 C2 -119.4(7) . . . . ? O2 C7 C3 C4 -118.4(7) . . . . ? O1 C7 C3 C4 60.4(8) . . . . ? C5 N1 C1 C2 0.9(9) . . . . ? Mn1 N1 C1 C2 178.4(4) 2_566 . . . ? C5 N1 C1 C8 -178.8(5) . . . 2_466 ? Mn1 N1 C1 C8 -1.3(7) 2_566 . . 2_466 ? C3 C2 C1 N1 1.7(9) . . . . ? C3 C2 C1 C8 -178.7(5) . . . 2_466 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.641 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.286 #===END of CIF for Complex 4 ===================== data_complex5 _database_code_depnum_ccdc_archive 'CCDC 697863' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Mg3 N2 O20' _chemical_formula_weight 633.27 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0000 '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 19.708(4) _cell_length_b 6.799(5) _cell_length_c 19.461(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.873(5) _cell_angle_gamma 90.00 _cell_volume 2326.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9496 _exptl_absorpt_correction_T_max 0.9630 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7341 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2876 _reflns_number_gt 2583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0726P)^2^+4.0731P] 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 2876 _refine_ls_number_parameters 434 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.124 _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 C1 C 0.8602(4) 0.2097(10) 0.2262(4) 0.0213(12) Uani 1 1 d . . . C2 C 0.7859(3) 0.2035(10) 0.2172(3) 0.0193(11) Uani 1 1 d . . . H2 H 0.7451 0.1771 0.1695 0.023 Uiso 1 1 calc R . . C3 C 0.7741(3) 0.2385(9) 0.2827(3) 0.0175(11) Uani 1 1 d D . . C4 C 0.8367(4) 0.2828(10) 0.3522(3) 0.0245(12) Uani 1 1 d . . . H4 H 0.8305 0.3085 0.3959 0.025 Uiso 1 1 calc R . . C5 C 0.9085(3) 0.2884(9) 0.3557(3) 0.0252(11) Uani 1 1 d . . . C6 C 0.9830(3) 0.3352(9) 0.4254(3) 0.0250(11) Uani 1 1 d . . . C7 C 0.6941(4) 0.2229(10) 0.2754(4) 0.0232(12) Uani 1 1 d D . . C8 C 0.8826(4) 0.1708(10) 0.1626(4) 0.0243(13) Uani 1 1 d . . . C9 C 1.2475(4) 0.2405(10) 0.3114(4) 0.0265(14) Uani 1 1 d . . . C10 C 1.2451(4) 0.2130(10) 0.2395(4) 0.0246(13) Uani 1 1 d . . . H10 H 1.1990 0.1903 0.1963 0.030 Uiso 1 1 calc R . . C13 C 0.8775(4) 0.2067(9) -0.1301(4) 0.0245(13) Uani 1 1 d . . . C14 C 1.1818(5) 0.2365(13) 0.3307(5) 0.0271(17) Uani 1 1 d . . . C15 C 1.3125(4) 0.1859(10) 0.1563(4) 0.0232(12) Uani 1 1 d D . . C16 C 0.9438(4) 0.1517(11) -0.0552(4) 0.0279(14) Uani 1 1 d . . . N1 N 0.8117(4) 0.2206(9) -0.1258(3) 0.0267(12) Uani 1 1 d . . . N2 N 0.9195(3) 0.2495(8) 0.2945(3) 0.0213(10) Uani 1 1 d . . . O1 O 0.9521(3) 0.1571(9) 0.1850(3) 0.0248(11) Uani 1 1 d . . . O2 O 0.8300(3) 0.1556(9) 0.0961(3) 0.0353(13) Uani 1 1 d . . . O3 O 0.6411(3) 0.1714(9) 0.2126(3) 0.0314(12) Uani 1 1 d . . . O4 O 0.6858(3) 0.2620(10) 0.3341(3) 0.0326(12) Uani 1 1 d . . . O5 O 0.9810(3) 0.3682(8) 0.4887(3) 0.0259(10) Uani 1 1 d . . . O6 O 1.0408(3) 0.3353(8) 0.4153(3) 0.0271(10) Uani 1 1 d . . . O7 O 0.6977(4) 0.2516(12) -0.0982(5) 0.0374(19) Uani 1 1 d . . . O8 O 1.1171(4) 0.2182(12) 0.2737(5) 0.029(2) Uani 1 1 d . . . O9 O 1.2514(3) 0.2117(11) 0.0976(3) 0.0436(15) Uani 1 1 d . . . O10 O 1.3725(3) 0.1336(9) 0.1567(3) 0.0346(12) Uani 1 1 d . . . O11 O 0.9278(3) 0.1290(9) 0.0015(3) 0.0354(12) Uani 1 1 d . . . O12 O 1.0077(3) 0.1309(9) -0.0516(3) 0.0274(12) Uani 1 1 d . . . OW1 O 0.5427(4) -0.1164(9) 0.1205(3) 0.0378(13) Uani 1 1 d D . . OW2 O 0.6121(4) 0.4211(10) 0.0733(3) 0.0413(13) Uani 1 1 d D . . OW3 O 0.4937(3) 0.3262(9) 0.1146(3) 0.0367(13) Uani 1 1 d D . . OW4 O 0.6445(3) 0.0248(9) 0.0593(3) 0.0330(12) Uani 1 1 d D . . OW5 O 1.0570(4) -0.0394(9) 0.3431(4) 0.0390(13) Uani 1 1 d D . . OW6 O 1.0204(3) 0.5356(9) 0.2663(3) 0.0346(12) Uani 1 1 d D . . OW7 O 0.7779(4) -0.0928(9) -0.0238(3) 0.0448(15) Uani 1 1 d D . . OW8 O 0.8562(3) 0.4833(8) 0.0177(3) 0.0350(12) Uani 1 1 d D . . Mg1 Mg 1.03090(13) 0.2444(4) 0.30339(13) 0.0235(5) Uani 1 1 d D . . Mg2 Mg 0.57237(12) 0.1554(4) 0.09789(12) 0.0236(5) Uani 1 1 d D . . Mg3 Mg 0.81447(14) 0.1934(4) -0.01242(13) 0.0276(5) Uani 1 1 d D . . C11 C 1.3122(4) 0.2201(9) 0.2335(4) 0.0214(12) Uani 1 1 d D . . C12 C 0.8798(4) 0.2401(10) -0.1999(4) 0.0236(13) Uani 1 1 d . . . H12 H 0.9259 0.2358 -0.2022 0.028 Uiso 1 1 calc R . . H1W2 H 0.584(2) 0.484(7) 0.035(3) 0.05(2) Uiso 1 1 d D . . H1W3 H 0.458(5) 0.38(2) 0.0775(18) 0.06(9) Uiso 1 1 d D . . H1W5 H 1.092(4) -0.100(7) 0.342(5) 0.04(3) Uiso 1 1 d D . . H1W6 H 0.979(3) 0.563(19) 0.230(5) 0.06(4) Uiso 1 1 d D . . H1W7 H 0.778(8) -0.174(14) 0.008(6) 0.06(4) Uiso 1 1 d D . . H1W8 H 0.87(2) 0.56(2) -0.004(15) 0.05(4) Uiso 1 1 d D . . H2W2 H 0.653(3) 0.419(7) 0.071(6) 0.05(6) Uiso 1 1 d D . . H2W3 H 0.499(3) 0.399(11) 0.151(3) 0.04(2) Uiso 1 1 d D . . H2W5 H 1.048(5) -0.090(12) 0.377(4) 0.04(3) Uiso 1 1 d D . . H2W6 H 1.053(4) 0.599(13) 0.261(5) 0.04(3) Uiso 1 1 d D . . H2W7 H 0.746(6) -0.140(19) -0.065(4) 0.06(4) Uiso 1 1 d D . . H2W8 H 0.853(11) 0.555(12) 0.051(9) 0.05(8) Uiso 1 1 d D . . H1W4 H 0.679(4) -0.056(11) 0.075(4) 0.04(3) Uiso 1 1 d D . . H2W1 H 0.511(9) -0.20(2) 0.096(10) 0.04(8) Uiso 1 1 d D . . H2W4 H 0.635(6) 0.050(15) 0.015(2) 0.05(3) Uiso 1 1 d D . . H1W1 H 0.563(13) -0.16(3) 0.165(4) 0.05(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(3) 0.025(3) 0.017(3) -0.004(2) 0.011(2) -0.008(2) C2 0.021(2) 0.031(3) 0.017(3) 0.001(2) 0.012(2) -0.003(2) C3 0.019(3) 0.023(3) 0.017(3) -0.001(2) 0.013(2) -0.002(2) C4 0.035(3) 0.025(3) 0.015(3) -0.004(2) 0.012(2) 0.003(2) C5 0.035(3) 0.025(3) 0.011(2) -0.002(2) 0.005(2) -0.004(2) C6 0.032(2) 0.027(3) 0.015(2) -0.002(2) 0.009(2) -0.002(2) C7 0.022(3) 0.024(3) 0.026(3) 0.000(2) 0.013(3) 0.000(2) C8 0.031(3) 0.029(3) 0.019(3) -0.004(2) 0.012(3) -0.009(3) C9 0.036(4) 0.022(3) 0.028(3) 0.003(3) 0.021(3) 0.003(3) C10 0.023(3) 0.022(3) 0.030(3) 0.000(3) 0.013(3) 0.002(2) C13 0.037(4) 0.013(3) 0.025(3) 0.001(2) 0.016(3) -0.004(2) C14 0.027(4) 0.036(4) 0.019(5) 0.003(3) 0.012(4) -0.002(3) C15 0.020(3) 0.025(3) 0.023(3) 0.002(2) 0.008(2) 0.005(2) C16 0.033(4) 0.026(3) 0.025(3) -0.004(3) 0.015(3) -0.003(3) N1 0.038(3) 0.027(3) 0.024(3) -0.001(2) 0.022(3) -0.004(2) N2 0.022(2) 0.027(3) 0.017(2) -0.0054(19) 0.0099(19) -0.0049(19) O1 0.025(2) 0.031(3) 0.021(2) -0.006(2) 0.0116(19) -0.002(2) O2 0.038(3) 0.053(3) 0.020(2) -0.012(2) 0.018(2) -0.019(3) O3 0.021(2) 0.048(3) 0.017(2) 0.001(2) 0.0011(18) -0.001(2) O4 0.021(2) 0.055(4) 0.028(3) -0.001(2) 0.017(2) 0.001(2) O5 0.021(2) 0.037(3) 0.018(2) -0.0053(19) 0.0075(17) -0.0013(19) O6 0.027(2) 0.033(3) 0.018(2) -0.005(2) 0.0088(18) -0.003(2) O7 0.049(4) 0.022(5) 0.036(5) -0.004(4) 0.017(4) 0.002(4) O8 0.025(4) 0.031(4) 0.026(6) 0.011(4) 0.007(4) 0.002(3) O9 0.035(3) 0.070(4) 0.018(2) -0.001(3) 0.005(2) 0.017(3) O10 0.031(3) 0.048(3) 0.027(2) -0.004(2) 0.014(2) 0.002(2) O11 0.045(3) 0.044(3) 0.025(2) 0.007(2) 0.023(2) 0.008(2) O12 0.037(3) 0.026(3) 0.019(2) -0.003(2) 0.012(2) 0.003(2) OW1 0.045(3) 0.035(3) 0.029(3) 0.002(2) 0.013(2) -0.012(2) OW2 0.038(3) 0.044(3) 0.034(3) 0.011(3) 0.009(2) 0.001(3) OW3 0.042(3) 0.039(3) 0.029(3) -0.002(2) 0.017(2) 0.011(3) OW4 0.025(2) 0.053(3) 0.019(2) 0.000(2) 0.0077(19) 0.009(2) OW5 0.048(3) 0.034(3) 0.053(4) 0.002(3) 0.038(3) 0.004(3) OW6 0.029(3) 0.034(3) 0.043(3) -0.002(2) 0.018(2) -0.003(2) OW7 0.075(4) 0.036(3) 0.023(3) -0.007(2) 0.023(3) -0.019(3) OW8 0.046(3) 0.033(3) 0.031(3) -0.002(2) 0.021(2) -0.003(2) Mg1 0.0222(10) 0.0301(11) 0.0210(10) -0.0037(9) 0.0123(9) -0.0011(9) Mg2 0.0215(10) 0.0321(11) 0.0146(9) 0.0006(9) 0.0059(8) -0.0004(9) Mg3 0.0328(12) 0.0319(13) 0.0189(10) 0.0014(9) 0.0124(9) 0.0001(10) C11 0.024(3) 0.012(3) 0.028(3) 0.004(2) 0.012(3) -0.001(2) C12 0.029(3) 0.013(3) 0.024(3) 0.002(2) 0.011(3) -0.003(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 C1 N2 1.343(8) . ? C1 C2 1.396(8) . ? C1 C8 1.513(9) . ? C2 C3 1.414(8) . ? C2 H2 0.9300 . ? C3 C4 1.391(8) . ? C3 C7 1.522(8) . ? C4 C5 1.385(9) . ? C4 H4 0.9300 . ? C5 N2 1.331(8) . ? C5 C6 1.516(8) . ? C6 O6 1.241(7) . ? C6 O5 1.271(7) . ? C7 O3 1.245(8) . ? C7 O4 1.253(8) . ? C8 O1 1.239(8) . ? C8 O2 1.244(9) . ? C9 N1 1.329(10) 4 ? C9 C10 1.390(10) . ? C9 C14 1.504(10) . ? C10 C11 1.382(9) . ? C10 H10 0.9300 . ? C13 N1 1.341(10) . ? C13 C12 1.398(9) . ? C13 C16 1.499(10) . ? C14 O8 1.262(12) . ? C14 O7 1.275(12) 4 ? C14 Mg1 2.774(8) . ? C15 O10 1.232(8) . ? C15 O9 1.242(8) . ? C15 C11 1.521(9) . ? C16 O12 1.239(9) . ? C16 O11 1.286(8) . ? N1 C9 1.329(10) 4_454 ? N1 Mg3 2.191(6) . ? N2 Mg1 2.123(5) . ? O1 Mg1 2.200(5) . ? O2 Mg3 2.008(5) . ? O3 Mg2 2.025(5) . ? O5 Mg2 2.080(5) 4 ? O6 Mg1 2.185(5) . ? O7 C14 1.275(12) 4_454 ? O7 Mg3 2.183(8) . ? O8 Mg1 2.034(7) . ? O11 Mg3 2.171(6) . ? OW1 Mg2 2.046(6) . ? OW1 H2W1 0.82(14) . ? OW1 H1W1 0.83(9) . ? OW2 Mg2 2.108(7) . ? OW2 H1W2 0.82(5) . ? OW2 H2W2 0.83(8) . ? OW3 Mg2 2.077(6) . ? OW3 H1W3 0.83(8) . ? OW3 H2W3 0.83(6) . ? OW4 Mg2 2.082(6) . ? OW4 H1W4 0.82(8) . ? OW4 H2W4 0.81(6) . ? OW5 Mg1 2.056(7) . ? OW5 H1W5 0.81(8) . ? OW5 H2W5 0.83(8) . ? OW6 Mg1 2.085(6) . ? OW6 H1W6 0.82(9) . ? OW6 H2W6 0.82(9) . ? OW7 Mg3 2.052(7) . ? OW7 H1W7 0.83(10) . ? OW7 H2W7 0.83(8) . ? OW8 Mg3 2.114(6) . ? OW8 H1W8 0.8(3) . ? OW8 H2W8 0.84(14) . ? Mg2 O5 2.080(5) 4_454 ? C11 C12 1.401(10) 4 ? C12 C11 1.401(10) 4_454 ? C12 H12 0.9300 . ? 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 N2 C1 C2 121.6(6) . . ? N2 C1 C8 113.5(5) . . ? C2 C1 C8 124.8(6) . . ? C1 C2 C3 118.2(5) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 118.5(5) . . ? C4 C3 C7 122.2(5) . . ? C2 C3 C7 119.2(5) . . ? C5 C4 C3 119.4(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N2 C5 C4 121.8(5) . . ? N2 C5 C6 111.0(5) . . ? C4 C5 C6 127.2(5) . . ? O6 C6 O5 126.0(5) . . ? O6 C6 C5 116.5(5) . . ? O5 C6 C5 117.5(5) . . ? O3 C7 O4 123.8(6) . . ? O3 C7 C3 119.0(6) . . ? O4 C7 C3 117.1(6) . . ? O1 C8 O2 128.9(6) . . ? O1 C8 C1 114.3(6) . . ? O2 C8 C1 116.8(6) . . ? N1 C9 C10 122.5(7) 4 . ? N1 C9 C14 110.1(6) 4 . ? C10 C9 C14 127.4(7) . . ? C11 C10 C9 118.8(7) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? N1 C13 C12 120.4(7) . . ? N1 C13 C16 113.5(6) . . ? C12 C13 C16 126.1(7) . . ? O8 C14 O7 128.1(7) . 4 ? O8 C14 C9 115.1(8) . . ? O7 C14 C9 116.9(8) 4 . ? O7 C14 Mg1 85.7(5) 4 . ? C9 C14 Mg1 157.2(6) . . ? O10 C15 O9 125.0(7) . . ? O10 C15 C11 118.0(6) . . ? O9 C15 C11 117.0(6) . . ? O12 C16 O11 125.1(7) . . ? O12 C16 C13 120.0(6) . . ? O11 C16 C13 114.9(7) . . ? C9 N1 C13 120.1(6) 4_454 . ? C9 N1 Mg3 121.5(5) 4_454 . ? C13 N1 Mg3 118.2(5) . . ? C5 N2 C1 120.3(5) . . ? C5 N2 Mg1 120.7(4) . . ? C1 N2 Mg1 118.9(4) . . ? C8 O1 Mg1 119.5(4) . . ? C8 O2 Mg3 138.0(5) . . ? C7 O3 Mg2 160.6(5) . . ? C6 O5 Mg2 125.8(4) . 4 ? C6 O6 Mg1 118.9(4) . . ? C14 O7 Mg3 120.0(5) 4_454 . ? C14 O8 Mg1 112.5(6) . . ? C16 O11 Mg3 120.4(5) . . ? Mg2 OW1 H2W1 136(10) . . ? Mg2 OW1 H1W1 119(10) . . ? H2W1 OW1 H1W1 104(19) . . ? Mg2 OW2 H1W2 119(2) . . ? Mg2 OW2 H2W2 118(3) . . ? H1W2 OW2 H2W2 104(7) . . ? Mg2 OW3 H1W3 120(3) . . ? Mg2 OW3 H2W3 130(3) . . ? H1W3 OW3 H2W3 102(8) . . ? Mg2 OW4 H1W4 138(6) . . ? Mg2 OW4 H2W4 115(6) . . ? H1W4 OW4 H2W4 107(9) . . ? Mg1 OW5 H1W5 122(3) . . ? Mg1 OW5 H2W5 126(5) . . ? H1W5 OW5 H2W5 107(9) . . ? Mg1 OW6 H1W6 115(8) . . ? Mg1 OW6 H2W6 126(7) . . ? H1W6 OW6 H2W6 108(9) . . ? Mg3 OW7 H1W7 132(9) . . ? Mg3 OW7 H2W7 123(10) . . ? H1W7 OW7 H2W7 102(10) . . ? Mg3 OW8 H1W8 131(17) . . ? Mg3 OW8 H2W8 127(11) . . ? H1W8 OW8 H2W8 101(19) . . ? O8 Mg1 OW5 85.7(3) . . ? O8 Mg1 OW6 87.1(3) . . ? OW5 Mg1 OW6 171.9(3) . . ? O8 Mg1 N2 160.7(3) . . ? OW5 Mg1 N2 96.9(2) . . ? OW6 Mg1 N2 91.1(2) . . ? O8 Mg1 O6 126.7(3) . . ? OW5 Mg1 O6 89.8(2) . . ? OW6 Mg1 O6 91.5(2) . . ? N2 Mg1 O6 72.6(2) . . ? O8 Mg1 O1 87.9(3) . . ? OW5 Mg1 O1 94.5(3) . . ? OW6 Mg1 O1 88.9(2) . . ? N2 Mg1 O1 72.84(19) . . ? O6 Mg1 O1 145.4(2) . . ? O8 Mg1 C14 24.8(3) . . ? OW5 Mg1 C14 81.1(3) . . ? OW6 Mg1 C14 90.9(3) . . ? N2 Mg1 C14 174.3(3) . . ? O6 Mg1 C14 102.0(2) . . ? O1 Mg1 C14 112.5(3) . . ? O3 Mg2 OW1 85.7(3) . . ? O3 Mg2 OW3 88.4(2) . . ? OW1 Mg2 OW3 99.5(3) . . ? O3 Mg2 O5 165.9(2) . 4_454 ? OW1 Mg2 O5 87.1(2) . 4_454 ? OW3 Mg2 O5 80.8(2) . 4_454 ? O3 Mg2 OW4 101.3(2) . . ? OW1 Mg2 OW4 90.1(3) . . ? OW3 Mg2 OW4 166.9(3) . . ? O5 Mg2 OW4 90.9(2) 4_454 . ? O3 Mg2 OW2 94.1(2) . . ? OW1 Mg2 OW2 174.2(3) . . ? OW3 Mg2 OW2 86.3(3) . . ? O5 Mg2 OW2 94.2(2) 4_454 . ? OW4 Mg2 OW2 84.2(3) . . ? O2 Mg3 OW7 82.6(2) . . ? O2 Mg3 OW8 88.4(2) . . ? OW7 Mg3 OW8 171.0(2) . . ? O2 Mg3 O11 100.6(2) . . ? OW7 Mg3 O11 96.5(3) . . ? OW8 Mg3 O11 84.5(3) . . ? O2 Mg3 O7 115.8(3) . . ? OW7 Mg3 O7 83.8(3) . . ? OW8 Mg3 O7 100.7(3) . . ? O11 Mg3 O7 143.3(3) . . ? O2 Mg3 N1 173.0(3) . . ? OW7 Mg3 N1 97.1(2) . . ? OW8 Mg3 N1 91.7(2) . . ? O11 Mg3 N1 72.4(2) . . ? O7 Mg3 N1 71.1(3) . . ? C10 C11 C12 118.3(6) . 4 ? C10 C11 C15 120.6(6) . . ? C12 C11 C15 121.1(6) 4 . ? C13 C12 C11 119.7(7) . 4_454 ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 4_454 . ? 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 N2 C1 C2 C3 -0.6(10) . . . . ? C8 C1 C2 C3 178.4(6) . . . . ? C1 C2 C3 C4 1.8(9) . . . . ? C1 C2 C3 C7 -177.1(6) . . . . ? C2 C3 C4 C5 -1.0(9) . . . . ? C7 C3 C4 C5 177.8(6) . . . . ? C3 C4 C5 N2 -1.0(10) . . . . ? C3 C4 C5 C6 179.5(6) . . . . ? N2 C5 C6 O6 1.7(8) . . . . ? C4 C5 C6 O6 -178.8(7) . . . . ? N2 C5 C6 O5 -177.5(6) . . . . ? C4 C5 C6 O5 2.1(10) . . . . ? C4 C3 C7 O3 -175.8(6) . . . . ? C2 C3 C7 O3 3.0(10) . . . . ? C4 C3 C7 O4 3.7(10) . . . . ? C2 C3 C7 O4 -177.5(6) . . . . ? N2 C1 C8 O1 8.6(9) . . . . ? C2 C1 C8 O1 -170.5(7) . . . . ? N2 C1 C8 O2 -171.9(7) . . . . ? C2 C1 C8 O2 9.0(11) . . . . ? N1 C9 C10 C11 2.2(10) 4 . . . ? C14 C9 C10 C11 -179.3(7) . . . . ? N1 C9 C14 O8 173.9(7) 4 . . . ? C10 C9 C14 O8 -4.7(12) . . . . ? N1 C9 C14 O7 -7.3(10) 4 . . 4 ? C10 C9 C14 O7 174.1(8) . . . 4 ? N1 C9 C14 Mg1 162.8(12) 4 . . . ? C10 C9 C14 Mg1 -15.8(19) . . . . ? N1 C13 C16 O12 178.8(6) . . . . ? C12 C13 C16 O12 -0.4(11) . . . . ? N1 C13 C16 O11 -0.9(9) . . . . ? C12 C13 C16 O11 179.9(7) . . . . ? C12 C13 N1 C9 2.3(10) . . . 4_454 ? C16 C13 N1 C9 -177.0(6) . . . 4_454 ? C12 C13 N1 Mg3 -174.4(5) . . . . ? C16 C13 N1 Mg3 6.3(8) . . . . ? C4 C5 N2 C1 2.3(10) . . . . ? C6 C5 N2 C1 -178.1(6) . . . . ? C4 C5 N2 Mg1 -176.7(5) . . . . ? C6 C5 N2 Mg1 2.9(7) . . . . ? C2 C1 N2 C5 -1.4(10) . . . . ? C8 C1 N2 C5 179.5(6) . . . . ? C2 C1 N2 Mg1 177.6(5) . . . . ? C8 C1 N2 Mg1 -1.6(8) . . . . ? O2 C8 O1 Mg1 169.0(6) . . . . ? C1 C8 O1 Mg1 -11.6(8) . . . . ? O1 C8 O2 Mg3 -26.0(14) . . . . ? C1 C8 O2 Mg3 154.6(6) . . . . ? O4 C7 O3 Mg2 134.6(13) . . . . ? C3 C7 O3 Mg2 -45.9(19) . . . . ? O6 C6 O5 Mg2 -20.6(10) . . . 4 ? C5 C6 O5 Mg2 158.5(4) . . . 4 ? O5 C6 O6 Mg1 173.8(5) . . . . ? C5 C6 O6 Mg1 -5.3(8) . . . . ? O7 C14 O8 Mg1 7.7(12) 4 . . . ? C9 C14 O8 Mg1 -173.7(5) . . . . ? O12 C16 O11 Mg3 175.2(6) . . . . ? C13 C16 O11 Mg3 -5.1(8) . . . . ? C14 O8 Mg1 OW5 -78.0(6) . . . . ? C14 O8 Mg1 OW6 98.3(6) . . . . ? C14 O8 Mg1 N2 -176.6(8) . . . . ? C14 O8 Mg1 O6 8.5(8) . . . . ? C14 O8 Mg1 O1 -172.7(6) . . . . ? C5 N2 Mg1 O8 -179.8(8) . . . . ? C1 N2 Mg1 O8 1.2(11) . . . . ? C5 N2 Mg1 OW5 83.5(5) . . . . ? C1 N2 Mg1 OW5 -95.5(5) . . . . ? C5 N2 Mg1 OW6 -95.4(5) . . . . ? C1 N2 Mg1 OW6 85.7(5) . . . . ? C5 N2 Mg1 O6 -4.1(5) . . . . ? C1 N2 Mg1 O6 176.9(5) . . . . ? C5 N2 Mg1 O1 176.1(6) . . . . ? C1 N2 Mg1 O1 -2.9(5) . . . . ? C6 O6 Mg1 O8 -176.7(5) . . . . ? C6 O6 Mg1 OW5 -92.2(5) . . . . ? C6 O6 Mg1 OW6 95.8(5) . . . . ? C6 O6 Mg1 N2 5.1(5) . . . . ? C6 O6 Mg1 O1 5.5(8) . . . . ? C6 O6 Mg1 C14 -173.0(5) . . . . ? C8 O1 Mg1 O8 -170.3(6) . . . . ? C8 O1 Mg1 OW5 104.2(6) . . . . ? C8 O1 Mg1 OW6 -83.1(6) . . . . ? C8 O1 Mg1 N2 8.4(6) . . . . ? C8 O1 Mg1 O6 8.0(8) . . . . ? C8 O1 Mg1 C14 -173.6(6) . . . . ? O7 C14 Mg1 O8 -174.0(10) 4 . . . ? C9 C14 Mg1 O8 14.9(12) . . . . ? O8 C14 Mg1 OW5 99.1(7) . . . . ? O7 C14 Mg1 OW5 -74.9(5) 4 . . . ? C9 C14 Mg1 OW5 113.9(15) . . . . ? O8 C14 Mg1 OW6 -81.3(7) . . . . ? O7 C14 Mg1 OW6 104.7(5) 4 . . . ? C9 C14 Mg1 OW6 -66.4(15) . . . . ? O8 C14 Mg1 O6 -173.0(6) . . . . ? O7 C14 Mg1 O6 13.0(6) 4 . . . ? C9 C14 Mg1 O6 -158.2(14) . . . . ? O8 C14 Mg1 O1 7.9(7) . . . . ? O7 C14 Mg1 O1 -166.1(5) 4 . . . ? C9 C14 Mg1 O1 22.7(15) . . . . ? C7 O3 Mg2 OW1 158.1(16) . . . . ? C7 O3 Mg2 OW3 -102.2(16) . . . . ? C7 O3 Mg2 O5 -142.0(14) . . . 4_454 ? C7 O3 Mg2 OW4 68.9(16) . . . . ? C7 O3 Mg2 OW2 -16.0(16) . . . . ? C8 O2 Mg3 OW7 124.2(9) . . . . ? C8 O2 Mg3 OW8 -55.2(8) . . . . ? C8 O2 Mg3 O11 28.9(9) . . . . ? C8 O2 Mg3 O7 -156.3(8) . . . . ? C16 O11 Mg3 O2 -174.6(6) . . . . ? C16 O11 Mg3 OW7 101.7(6) . . . . ? C16 O11 Mg3 OW8 -87.3(6) . . . . ? C16 O11 Mg3 O7 13.3(9) . . . . ? C16 O11 Mg3 N1 6.3(6) . . . . ? C14 O7 Mg3 O2 -175.0(7) 4_454 . . . ? C14 O7 Mg3 OW7 -96.3(7) 4_454 . . . ? C14 O7 Mg3 OW8 91.5(7) 4_454 . . . ? C14 O7 Mg3 O11 -3.7(10) 4_454 . . . ? C14 O7 Mg3 N1 3.4(7) 4_454 . . . ? C9 N1 Mg3 OW7 82.1(6) 4_454 . . . ? C13 N1 Mg3 OW7 -101.3(5) . . . . ? C9 N1 Mg3 OW8 -99.6(6) 4_454 . . . ? C13 N1 Mg3 OW8 77.0(5) . . . . ? C9 N1 Mg3 O11 176.7(6) 4_454 . . . ? C13 N1 Mg3 O11 -6.6(5) . . . . ? C9 N1 Mg3 O7 1.1(6) 4_454 . . . ? C13 N1 Mg3 O7 177.8(6) . . . . ? C9 C10 C11 C12 -1.6(9) . . . 4 ? C9 C10 C11 C15 178.5(6) . . . . ? O10 C15 C11 C10 -158.0(7) . . . . ? O9 C15 C11 C10 21.4(10) . . . . ? O10 C15 C11 C12 22.2(10) . . . 4 ? O9 C15 C11 C12 -158.4(7) . . . 4 ? N1 C13 C12 C11 -2.7(10) . . . 4_454 ? C16 C13 C12 C11 176.4(6) . . . 4_454 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.691 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.125 #===END of CIF for Complex 5 ===================== data_complex6 _database_code_depnum_ccdc_archive 'CCDC 697864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 Mg3 N2 O24' _chemical_formula_weight 705.33 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.274(5) _cell_length_b 8.955(4) _cell_length_c 11.032(5) _cell_angle_alpha 74.722(6) _cell_angle_beta 74.713(6) _cell_angle_gamma 79.032(7) _cell_volume 663.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.3 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 366 _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9643 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4259 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3290 _reflns_number_gt 2463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.1718P)^2^+1.2720P] 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 3076 _refine_ls_number_parameters 253 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.2473 _refine_ls_wR_factor_gt 0.1758 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.113 _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 Mg1 Mg 0.70669(17) 0.36294(14) 0.67703(12) 0.0171(4) Uani 1 1 d . . . Mg2 Mg 1.0000 -0.5000 1.0000 0.0179(4) Uani 1 2 d S . . O2 O 0.7467(4) 0.3469(3) 0.4729(3) 0.0213(6) Uani 1 1 d . . . O1 O 0.7635(4) 0.1897(3) 0.3410(3) 0.0236(6) Uani 1 1 d . . . OW2 O 1.0030(4) 0.3450(3) 0.6575(3) 0.0202(6) Uani 1 1 d D . . OW6 O 1.2213(4) 0.0785(4) 0.7511(3) 0.0267(7) Uani 1 1 d D . . O5 O 0.7097(4) 0.2238(3) 0.8760(3) 0.0213(6) Uani 1 1 d . . . O3 O 0.7242(4) -0.3915(3) 0.5763(3) 0.0208(6) Uani 1 1 d . . . O6 O 0.7324(4) -0.0190(3) 1.0013(3) 0.0237(6) Uani 1 1 d . . . O4 O 0.6255(4) -0.4461(3) 0.7867(3) 0.0211(6) Uani 1 1 d . . . OW1 O 0.4135(4) 0.3870(3) 0.6882(3) 0.0224(6) Uani 1 1 d D . . OW3 O 0.7081(4) -0.4599(4) 1.0197(3) 0.0232(6) Uani 1 1 d D . . OW4 O 1.0115(4) -0.2775(3) 1.0113(3) 0.0251(6) Uani 1 1 d D . . N1 N 0.7170(4) 0.1214(4) 0.6763(3) 0.0170(6) Uani 1 1 d . . . OW5 O 0.9735(4) -0.5776(4) 1.1942(3) 0.0237(6) Uani 1 1 d D . . C4 C 0.6792(5) -0.1399(5) 0.7960(4) 0.0208(8) Uani 1 1 d . . . H4 H 0.6630 -0.2118 0.8748 0.035 Uiso 1 1 calc R . . C6 C 0.7462(5) 0.2158(4) 0.4495(4) 0.0203(7) Uani 1 1 d . . . C2 C 0.7081(5) -0.0716(4) 0.5656(4) 0.0191(7) Uani 1 1 d . . . H2 H 0.7155 -0.0987 0.4885 0.033 Uiso 1 1 calc R . . C1 C 0.7213(5) 0.0816(4) 0.5667(4) 0.0196(7) Uani 1 1 d . . . C3 C 0.6838(5) -0.1828(5) 0.6812(4) 0.0195(7) Uani 1 1 d . . . C8 C 0.7117(5) 0.0771(4) 0.8995(4) 0.0189(7) Uani 1 1 d . . . C7 C 0.6762(5) -0.3497(5) 0.6821(4) 0.0206(8) Uani 1 1 d . . . C5 C 0.6996(5) 0.0133(4) 0.7871(4) 0.0190(7) Uani 1 1 d . . . H1W4 H 0.931(10) -0.198(7) 1.009(9) 0.08(3) Uiso 1 1 d D . . H1W1 H 0.375(9) 0.464(5) 0.637(5) 0.049(18) Uiso 1 1 d D . . H1W2 H 1.076(6) 0.357(6) 0.587(3) 0.057(13) Uiso 1 1 d D . . H1W3 H 0.668(10) -0.459(10) 0.956(4) 0.08(3) Uiso 1 1 d D . . H2W4 H 1.094(7) -0.245(8) 1.033(7) 0.06(2) Uiso 1 1 d D . . H2W1 H 0.357(10) 0.317(6) 0.687(8) 0.07(2) Uiso 1 1 d D . . H2W3 H 0.618(7) -0.482(9) 1.081(4) 0.08(3) Uiso 1 1 d D . . H2W2 H 1.056(7) 0.262(4) 0.692(4) 0.051(12) Uiso 1 1 d D . . H2W6 H 1.227(8) 0.046(6) 0.828(2) 0.041(14) Uiso 1 1 d D . . H1W6 H 1.234(11) -0.006(5) 0.729(7) 0.06(2) Uiso 1 1 d D . . H1W5 H 0.911(10) -0.651(6) 1.234(7) 0.07(2) Uiso 1 1 d D . . H2W5 H 0.958(11) -0.518(7) 1.243(6) 0.07(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0139(6) 0.0195(7) 0.0199(7) -0.0055(5) -0.0032(5) -0.0060(5) Mg2 0.0132(9) 0.0206(9) 0.0220(9) -0.0066(7) -0.0036(6) -0.0050(6) O2 0.0218(14) 0.0238(14) 0.0218(13) -0.0052(10) -0.0057(10) -0.0097(10) O1 0.0298(15) 0.0243(14) 0.0194(13) -0.0070(11) -0.0029(11) -0.0107(11) OW2 0.0145(13) 0.0249(14) 0.0205(14) -0.0034(11) -0.0023(10) -0.0059(10) OW6 0.0298(16) 0.0270(15) 0.0259(16) -0.0089(12) -0.0111(12) 0.0012(12) O5 0.0181(13) 0.0213(13) 0.0271(14) -0.0075(11) -0.0060(10) -0.0047(10) O3 0.0195(13) 0.0212(13) 0.0226(14) -0.0063(10) -0.0011(10) -0.0079(10) O6 0.0269(15) 0.0239(14) 0.0217(14) -0.0055(11) -0.0069(11) -0.0042(11) O4 0.0229(14) 0.0213(13) 0.0206(13) -0.0028(10) -0.0049(10) -0.0095(10) OW1 0.0144(13) 0.0261(15) 0.0273(15) -0.0044(11) -0.0056(10) -0.0051(11) OW3 0.0141(13) 0.0338(15) 0.0225(14) -0.0072(11) -0.0014(10) -0.0071(11) OW4 0.0235(15) 0.0215(14) 0.0347(16) -0.0084(12) -0.0110(12) -0.0046(11) N1 0.0140(14) 0.0178(14) 0.0221(15) -0.0090(12) -0.0038(11) -0.0028(11) OW5 0.0204(14) 0.0306(15) 0.0231(14) -0.0073(12) -0.0024(11) -0.0121(12) C4 0.0174(18) 0.0265(19) 0.0200(18) -0.0043(14) -0.0036(13) -0.0083(14) C6 0.0176(17) 0.0228(18) 0.0223(18) -0.0065(14) -0.0025(13) -0.0079(13) C2 0.0175(17) 0.0197(17) 0.0235(18) -0.0093(14) -0.0059(13) -0.0028(13) C1 0.0148(16) 0.0216(18) 0.0231(18) -0.0038(14) -0.0019(13) -0.0092(13) C3 0.0155(17) 0.0251(18) 0.0197(18) -0.0071(14) -0.0025(13) -0.0058(14) C8 0.0168(17) 0.0217(17) 0.0221(18) -0.0111(14) -0.0021(13) -0.0060(13) C7 0.0153(17) 0.0298(19) 0.0207(18) -0.0073(14) -0.0069(13) -0.0058(14) C5 0.0146(17) 0.0242(18) 0.0196(17) -0.0048(14) -0.0046(13) -0.0053(13) _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 Mg1 OW1 2.076(3) . ? Mg1 OW2 2.088(3) . ? Mg1 N1 2.152(3) . ? Mg1 O3 2.198(3) 1_565 ? Mg1 O5 2.224(3) . ? Mg1 O2 2.233(3) . ? Mg1 O4 2.251(3) 1_565 ? Mg1 C7 2.555(4) 1_565 ? Mg2 OW5 2.039(3) 2_747 ? Mg2 OW5 2.039(3) . ? Mg2 OW3 2.047(3) . ? Mg2 OW3 2.047(3) 2_747 ? Mg2 OW4 2.048(3) 2_747 ? Mg2 OW4 2.048(3) . ? O2 C6 1.267(5) . ? O1 C6 1.250(5) . ? OW2 H1W2 0.81(2) . ? OW2 H2W2 0.82(4) . ? OW6 H2W6 0.83(2) . ? OW6 H1W6 0.84(5) . ? O5 C8 1.268(5) . ? O3 C7 1.261(5) . ? O3 Mg1 2.198(3) 1_545 ? O6 C8 1.247(5) . ? O4 C7 1.260(5) . ? O4 Mg1 2.251(3) 1_545 ? OW1 H1W1 0.82(5) . ? OW1 H2W1 0.82(6) . ? OW3 H1W3 0.83(5) . ? OW3 H2W3 0.82(5) . ? OW4 H1W4 0.83(7) . ? OW4 H2W4 0.83(6) . ? N1 C5 1.337(5) . ? N1 C1 1.339(5) . ? OW5 H1W5 0.83(7) . ? OW5 H2W5 0.83(7) . ? C4 C5 1.383(5) . ? C4 C3 1.408(5) . ? C4 H4 0.9300 . ? C6 C1 1.513(5) . ? C2 C3 1.389(5) . ? C2 C1 1.397(5) . ? C2 H2 0.9300 . ? C3 C7 1.503(6) . ? C8 C5 1.524(5) . ? C7 Mg1 2.555(4) 1_545 ? 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 OW1 Mg1 OW2 177.45(13) . . ? OW1 Mg1 N1 87.56(12) . . ? OW2 Mg1 N1 93.36(12) . . ? OW1 Mg1 O3 92.32(12) . 1_565 ? OW2 Mg1 O3 85.73(11) . 1_565 ? N1 Mg1 O3 151.39(13) . 1_565 ? OW1 Mg1 O5 98.56(12) . . ? OW2 Mg1 O5 83.98(11) . . ? N1 Mg1 O5 72.38(12) . . ? O3 Mg1 O5 135.63(11) 1_565 . ? OW1 Mg1 O2 86.48(12) . . ? OW2 Mg1 O2 91.54(11) . . ? N1 Mg1 O2 72.22(11) . . ? O3 Mg1 O2 79.21(11) 1_565 . ? O5 Mg1 O2 143.97(12) . . ? OW1 Mg1 O4 84.07(12) . 1_565 ? OW2 Mg1 O4 96.30(12) . 1_565 ? N1 Mg1 O4 149.02(12) . 1_565 ? O3 Mg1 O4 59.00(11) 1_565 1_565 ? O5 Mg1 O4 79.44(11) . 1_565 ? O2 Mg1 O4 136.56(12) . 1_565 ? OW1 Mg1 C7 89.69(12) . 1_565 ? OW2 Mg1 C7 89.42(12) . 1_565 ? N1 Mg1 C7 177.13(13) . 1_565 ? O3 Mg1 C7 29.57(11) 1_565 1_565 ? O5 Mg1 C7 107.24(12) . 1_565 ? O2 Mg1 C7 108.44(12) . 1_565 ? O4 Mg1 C7 29.53(11) 1_565 1_565 ? OW5 Mg2 OW5 180.000(1) 2_747 . ? OW5 Mg2 OW3 87.88(11) 2_747 . ? OW5 Mg2 OW3 92.12(12) . . ? OW5 Mg2 OW3 92.12(12) 2_747 2_747 ? OW5 Mg2 OW3 87.88(11) . 2_747 ? OW3 Mg2 OW3 180.0 . 2_747 ? OW5 Mg2 OW4 91.01(12) 2_747 2_747 ? OW5 Mg2 OW4 88.99(12) . 2_747 ? OW3 Mg2 OW4 87.65(12) . 2_747 ? OW3 Mg2 OW4 92.35(12) 2_747 2_747 ? OW5 Mg2 OW4 88.99(12) 2_747 . ? OW5 Mg2 OW4 91.01(12) . . ? OW3 Mg2 OW4 92.35(12) . . ? OW3 Mg2 OW4 87.65(12) 2_747 . ? OW4 Mg2 OW4 180.000(1) 2_747 . ? C6 O2 Mg1 119.0(2) . . ? Mg1 OW2 H1W2 121(4) . . ? Mg1 OW2 H2W2 117(4) . . ? H1W2 OW2 H2W2 99(5) . . ? H2W6 OW6 H1W6 100(6) . . ? C8 O5 Mg1 118.9(2) . . ? C7 O3 Mg1 91.1(2) . 1_545 ? C7 O4 Mg1 88.7(2) . 1_545 ? Mg1 OW1 H1W1 114(5) . . ? Mg1 OW1 H2W1 124(5) . . ? H1W1 OW1 H2W1 105(7) . . ? Mg2 OW3 H1W3 117(5) . . ? Mg2 OW3 H2W3 133(5) . . ? H1W3 OW3 H2W3 104(3) . . ? Mg2 OW4 H1W4 132(7) . . ? Mg2 OW4 H2W4 128(5) . . ? H1W4 OW4 H2W4 99(8) . . ? C5 N1 C1 119.8(3) . . ? C5 N1 Mg1 120.1(2) . . ? C1 N1 Mg1 119.8(2) . . ? Mg2 OW5 H1W5 120(6) . . ? Mg2 OW5 H2W5 122(5) . . ? H1W5 OW5 H2W5 108(7) . . ? C5 C4 C3 117.5(3) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? O1 C6 O2 126.1(4) . . ? O1 C6 C1 118.8(3) . . ? O2 C6 C1 115.1(3) . . ? C3 C2 C1 119.1(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? N1 C1 C2 121.2(3) . . ? N1 C1 C6 113.4(3) . . ? C2 C1 C6 125.4(3) . . ? C2 C3 C4 119.3(3) . . ? C2 C3 C7 120.1(3) . . ? C4 C3 C7 120.4(3) . . ? O6 C8 O5 127.0(3) . . ? O6 C8 C5 117.5(3) . . ? O5 C8 C5 115.4(3) . . ? O4 C7 O3 120.8(4) . . ? O4 C7 C3 120.5(3) . . ? O3 C7 C3 118.7(3) . . ? O4 C7 Mg1 61.7(2) . 1_545 ? O3 C7 Mg1 59.3(2) . 1_545 ? C3 C7 Mg1 173.2(3) . 1_545 ? N1 C5 C4 123.1(3) . . ? N1 C5 C8 112.4(3) . . ? C4 C5 C8 124.5(3) . . ? 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 OW1 Mg1 O2 C6 -84.7(3) . . . . ? OW2 Mg1 O2 C6 96.9(3) . . . . ? N1 Mg1 O2 C6 3.9(3) . . . . ? O3 Mg1 O2 C6 -177.7(3) 1_565 . . . ? O5 Mg1 O2 C6 15.1(4) . . . . ? O4 Mg1 O2 C6 -162.2(3) 1_565 . . . ? C7 Mg1 O2 C6 -173.2(3) 1_565 . . . ? OW1 Mg1 O5 C8 83.2(3) . . . . ? OW2 Mg1 O5 C8 -96.9(3) . . . . ? N1 Mg1 O5 C8 -1.4(3) . . . . ? O3 Mg1 O5 C8 -174.5(2) 1_565 . . . ? O2 Mg1 O5 C8 -12.6(4) . . . . ? O4 Mg1 O5 C8 165.5(3) 1_565 . . . ? C7 Mg1 O5 C8 175.6(3) 1_565 . . . ? OW1 Mg1 N1 C5 -92.7(3) . . . . ? OW2 Mg1 N1 C5 89.7(3) . . . . ? O3 Mg1 N1 C5 176.9(3) 1_565 . . . ? O5 Mg1 N1 C5 7.1(3) . . . . ? O2 Mg1 N1 C5 -179.8(3) . . . . ? O4 Mg1 N1 C5 -18.5(4) 1_565 . . . ? OW2 Mg1 N1 C1 -97.1(3) . . . . ? O3 Mg1 N1 C1 -9.9(4) 1_565 . . . ? O5 Mg1 N1 C1 -179.7(3) . . . . ? O2 Mg1 N1 C1 -6.6(3) . . . . ? O4 Mg1 N1 C1 154.8(3) 1_565 . . . ? Mg1 O2 C6 O1 178.7(3) . . . . ? Mg1 O2 C6 C1 -1.1(4) . . . . ? C5 N1 C1 C2 -0.1(5) . . . . ? Mg1 N1 C1 C2 -173.4(3) . . . . ? C5 N1 C1 C6 -178.6(3) . . . . ? Mg1 N1 C1 C6 8.1(4) . . . . ? C3 C2 C1 N1 2.2(6) . . . . ? C3 C2 C1 C6 -179.5(3) . . . . ? O1 C6 C1 N1 175.8(3) . . . . ? O2 C6 C1 N1 -4.4(5) . . . . ? O1 C6 C1 C2 -2.7(6) . . . . ? O2 C6 C1 C2 177.1(3) . . . . ? C1 C2 C3 C4 -2.0(5) . . . . ? C1 C2 C3 C7 -177.8(3) . . . . ? C5 C4 C3 C2 0.0(5) . . . . ? C5 C4 C3 C7 175.8(3) . . . . ? Mg1 O5 C8 O6 172.4(3) . . . . ? Mg1 O5 C8 C5 -3.5(4) . . . . ? Mg1 O4 C7 O3 6.3(4) 1_545 . . . ? Mg1 O4 C7 C3 -172.7(3) 1_545 . . . ? Mg1 O3 C7 O4 -6.4(4) 1_545 . . . ? Mg1 O3 C7 C3 172.5(3) 1_545 . . . ? C2 C3 C7 O4 -169.2(3) . . . . ? C4 C3 C7 O4 15.0(6) . . . . ? C2 C3 C7 O3 11.8(5) . . . . ? C4 C3 C7 O3 -163.9(3) . . . . ? C1 N1 C5 C4 -2.1(5) . . . . ? Mg1 N1 C5 C4 171.1(3) . . . . ? C1 N1 C5 C8 175.9(3) . . . . ? Mg1 N1 C5 C8 -10.8(4) . . . . ? C3 C4 C5 N1 2.2(6) . . . . ? C3 C4 C5 C8 -175.7(3) . . . . ? O6 C8 C5 N1 -167.2(3) . . . . ? O5 C8 C5 N1 9.1(5) . . . . ? O6 C8 C5 C4 10.8(6) . . . . ? O5 C8 C5 C4 -172.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.678 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.174 #===END of CIF for Complex 6 ===================== data_complex7 _database_code_depnum_ccdc_archive 'CCDC 697865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Ca3 N2 O16' _chemical_formula_weight 608.52 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.714(2) _cell_length_b 8.773(3) _cell_length_c 10.070(3) _cell_angle_alpha 108.977(5) _cell_angle_beta 97.689(4) _cell_angle_gamma 100.447(5) _cell_volume 539.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 310 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 0.9193 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3605 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2561 _reflns_number_gt 2057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0000P)^2^+5.0161P] 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 2561 _refine_ls_number_parameters 181 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1729 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.109 _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 Ca2 Ca -0.44458(16) 0.05846(13) 0.33046(11) 0.0181(2) Uani 1 1 d . . . Ca1 Ca 0.0000 0.5000 1.0000 0.0204(3) Uani 1 2 d S . . O3 O 0.0995(6) 0.9533(5) 0.6388(5) 0.0286(9) Uani 1 1 d . . . O1 O -0.4415(6) 0.1770(4) 0.5983(4) 0.0222(8) Uani 1 1 d . . . OW1 O -0.4663(7) -0.1584(5) 0.1087(4) 0.025 Uani 1 1 d D . . O2 O -0.2905(7) 0.3820(5) 0.8059(4) 0.0277(9) Uani 1 1 d . . . O4 O -0.1955(6) 0.9686(5) 0.7160(4) 0.0262(9) Uani 1 1 d . . . N1 N -0.3145(7) 0.3660(5) 0.4519(5) 0.0189(9) Uani 1 1 d . . . O5 O -0.3848(7) 0.2089(5) 0.1712(4) 0.0308(10) Uani 1 1 d . . . O6 O -0.2148(7) 0.4336(5) 1.1387(4) 0.0290(9) Uani 1 1 d . . . C5 C -0.2558(8) 0.4559(7) 0.3734(6) 0.0197(10) Uani 1 1 d . . . OW2 O -0.0775(8) 0.7606(6) 1.0654(6) 0.037 Uani 1 1 d D . . C8 C -0.3442(8) 0.3243(7) 0.6730(6) 0.0199(10) Uani 1 1 d . . . C1 C -0.2892(8) 0.4388(7) 0.5928(6) 0.0192(10) Uani 1 1 d . . . C3 C -0.1589(7) 0.7037(6) 0.5787(5) 0.0170(10) Uani 1 1 d . . . C4 C -0.1751(8) 0.6269(6) 0.4328(6) 0.0178(10) Uani 1 1 d . . . C6 C -0.2889(8) 0.3582(7) 0.2149(6) 0.0225(11) Uani 1 1 d . . . C7 C -0.0772(8) 0.8904(6) 0.6497(5) 0.0188(10) Uani 1 1 d . . . C2 C -0.2165(8) 0.6116(7) 0.6611(6) 0.0210(11) Uani 1 1 d . . . H4 H -0.134(9) 0.678(8) 0.369(7) 0.022(16) Uiso 1 1 d . . . H2 H -0.214(9) 0.667(8) 0.769(7) 0.024(16) Uiso 1 1 d . . . H1W1 H -0.533(8) -0.246(4) 0.110(6) 0.020(15) Uiso 1 1 d D . . H2W1 H -0.504(13) -0.158(11) 0.027(4) 0.06(3) Uiso 1 1 d D . . H1W2 H 0.018(8) 0.835(7) 1.123(6) 0.05(2) Uiso 1 1 d D . . H2W2 H -0.194(6) 0.774(9) 1.075(8) 0.04(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca2 0.0178(5) 0.0164(5) 0.0185(5) 0.0048(4) 0.0042(4) 0.0024(4) Ca1 0.0230(7) 0.0199(7) 0.0161(7) 0.0060(6) 0.0053(6) 0.0001(6) O3 0.0197(19) 0.025(2) 0.038(2) 0.0102(18) 0.0054(17) -0.0006(16) O1 0.028(2) 0.0167(18) 0.0186(18) 0.0071(15) 0.0036(15) -0.0024(15) OW1 0.031 0.021 0.016 0.005 0.003 -0.004 O2 0.037(2) 0.0222(19) 0.0154(18) 0.0034(15) 0.0018(16) -0.0049(17) O4 0.0205(19) 0.0180(18) 0.035(2) 0.0018(16) 0.0065(17) 0.0053(15) N1 0.018(2) 0.018(2) 0.018(2) 0.0039(17) 0.0042(17) 0.0040(17) O5 0.043(3) 0.0200(19) 0.021(2) 0.0037(16) 0.0033(18) -0.0022(18) O6 0.040(2) 0.029(2) 0.019(2) 0.0113(17) 0.0100(17) 0.0011(18) C5 0.018(2) 0.026(3) 0.019(2) 0.012(2) 0.0059(19) 0.003(2) OW2 0.031 0.025 0.046 -0.001 0.009 0.006 C8 0.017(2) 0.021(2) 0.021(3) 0.004(2) 0.007(2) 0.0057(19) C1 0.015(2) 0.024(3) 0.021(3) 0.011(2) 0.0044(19) 0.006(2) C3 0.011(2) 0.017(2) 0.021(2) 0.0057(19) -0.0018(18) 0.0037(18) C4 0.019(2) 0.019(2) 0.019(2) 0.011(2) 0.0074(19) 0.0046(19) C6 0.023(3) 0.031(3) 0.017(2) 0.012(2) 0.009(2) 0.004(2) C7 0.017(2) 0.020(2) 0.017(2) 0.007(2) 0.0006(19) 0.0012(19) C2 0.019(3) 0.023(3) 0.019(3) 0.006(2) 0.006(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 Ca2 O3 2.322(4) 2_566 ? Ca2 O4 2.352(4) 2_466 ? Ca2 OW1 2.382(4) . ? Ca2 O5 2.415(4) . ? Ca2 O1 2.430(4) 2_456 ? Ca2 N1 2.500(5) . ? Ca2 O1 2.551(4) . ? Ca2 Ca2 3.993(3) 2_456 ? Ca2 H1W1 2.77(5) . ? Ca1 O6 2.266(4) . ? Ca1 O6 2.266(4) 2_567 ? Ca1 OW2 2.340(5) . ? Ca1 OW2 2.340(5) 2_567 ? Ca1 O2 2.372(4) 2_567 ? Ca1 O2 2.372(4) . ? Ca1 H1W2 2.77(6) . ? O3 C7 1.249(6) . ? O3 Ca2 2.322(4) 2_566 ? O1 C8 1.262(6) . ? O1 Ca2 2.430(4) 2_456 ? OW1 H1W1 0.82(2) . ? OW1 H2W1 0.83(5) . ? O2 C8 1.242(6) . ? O4 C7 1.260(7) . ? O4 Ca2 2.352(4) 2_466 ? N1 C1 1.326(7) . ? N1 C5 1.333(7) . ? O5 C6 1.252(7) . ? O6 C6 1.260(6) 1_556 ? C5 C4 1.392(7) . ? C5 C6 1.509(7) . ? OW2 H1W2 0.82(6) . ? OW2 H2W2 0.83(5) . ? C8 C1 1.507(7) . ? C1 C2 1.404(7) . ? C3 C2 1.379(7) . ? C3 C4 1.383(7) . ? C3 C7 1.517(7) . ? C4 H4 0.94(6) . ? C6 O6 1.260(6) 1_554 ? C2 H2 1.03(6) . ? 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 Ca2 O4 172.30(15) 2_566 2_466 ? O3 Ca2 OW1 81.91(15) 2_566 . ? O4 Ca2 OW1 91.88(15) 2_466 . ? O3 Ca2 O5 89.55(16) 2_566 . ? O4 Ca2 O5 93.57(16) 2_466 . ? OW1 Ca2 O5 77.57(15) . . ? O3 Ca2 O1 94.51(15) 2_566 2_456 ? O4 Ca2 O1 80.02(14) 2_466 2_456 ? OW1 Ca2 O1 81.54(14) . 2_456 ? O5 Ca2 O1 157.94(13) . 2_456 ? O3 Ca2 N1 86.43(15) 2_566 . ? O4 Ca2 N1 101.26(14) 2_466 . ? OW1 Ca2 N1 140.83(15) . . ? O5 Ca2 N1 65.02(14) . . ? O1 Ca2 N1 136.81(14) 2_456 . ? O3 Ca2 O1 94.96(15) 2_566 . ? O4 Ca2 O1 88.69(14) 2_466 . ? OW1 Ca2 O1 154.51(14) . . ? O5 Ca2 O1 127.84(14) . . ? O1 Ca2 O1 73.46(14) 2_456 . ? N1 Ca2 O1 63.47(13) . . ? O3 Ca2 Ca2 95.91(12) 2_566 2_456 ? O4 Ca2 Ca2 83.10(11) 2_466 2_456 ? OW1 Ca2 Ca2 119.16(12) . 2_456 ? O5 Ca2 Ca2 162.94(11) . 2_456 ? O1 Ca2 Ca2 37.77(9) 2_456 2_456 ? N1 Ca2 Ca2 99.11(11) . 2_456 ? O1 Ca2 Ca2 35.69(9) . 2_456 ? O3 Ca2 H1W1 87.9(12) 2_566 . ? O4 Ca2 H1W1 84.9(12) 2_466 . ? OW1 Ca2 H1W1 16.3(8) . . ? O5 Ca2 H1W1 92.7(9) . . ? O1 Ca2 H1W1 65.9(8) 2_456 . ? N1 Ca2 H1W1 157.0(8) . . ? O1 Ca2 H1W1 139.3(8) . . ? Ca2 Ca2 H1W1 103.6(8) 2_456 . ? O6 Ca1 O6 180.000(1) . 2_567 ? O6 Ca1 OW2 87.92(17) . . ? O6 Ca1 OW2 92.08(17) 2_567 . ? O6 Ca1 OW2 92.08(17) . 2_567 ? O6 Ca1 OW2 87.92(17) 2_567 2_567 ? OW2 Ca1 OW2 180.000(1) . 2_567 ? O6 Ca1 O2 93.16(15) . 2_567 ? O6 Ca1 O2 86.84(15) 2_567 2_567 ? OW2 Ca1 O2 87.75(17) . 2_567 ? OW2 Ca1 O2 92.25(17) 2_567 2_567 ? O6 Ca1 O2 86.84(15) . . ? O6 Ca1 O2 93.16(15) 2_567 . ? OW2 Ca1 O2 92.25(17) . . ? OW2 Ca1 O2 87.75(17) 2_567 . ? O2 Ca1 O2 180.000(1) 2_567 . ? O6 Ca1 H1W2 92.3(16) . . ? O6 Ca1 H1W2 87.7(16) 2_567 . ? OW2 Ca1 H1W2 15.9(11) . . ? OW2 Ca1 H1W2 164.1(11) 2_567 . ? O2 Ca1 H1W2 72.3(11) 2_567 . ? O2 Ca1 H1W2 107.7(11) . . ? C7 O3 Ca2 144.9(4) . 2_566 ? C8 O1 Ca2 130.4(3) . 2_456 ? C8 O1 Ca2 120.5(3) . . ? Ca2 O1 Ca2 106.54(14) 2_456 . ? Ca2 OW1 H1W1 109(4) . . ? Ca2 OW1 H2W1 127(6) . . ? H1W1 OW1 H2W1 106(7) . . ? C8 O2 Ca1 143.9(4) . . ? C7 O4 Ca2 133.3(3) . 2_466 ? C1 N1 C5 119.8(5) . . ? C1 N1 Ca2 121.5(4) . . ? C5 N1 Ca2 118.6(3) . . ? C6 O5 Ca2 122.9(3) . . ? C6 O6 Ca1 157.5(4) 1_556 . ? N1 C5 C4 122.5(5) . . ? N1 C5 C6 114.7(5) . . ? C4 C5 C6 122.7(5) . . ? Ca1 OW2 H1W2 113(6) . . ? Ca1 OW2 H2W2 123(5) . . ? H1W2 OW2 H2W2 114(7) . . ? O2 C8 O1 125.6(5) . . ? O2 C8 C1 117.7(5) . . ? O1 C8 C1 116.7(5) . . ? N1 C1 C2 121.5(5) . . ? N1 C1 C8 115.6(5) . . ? C2 C1 C8 122.9(5) . . ? C2 C3 C4 120.4(5) . . ? C2 C3 C7 119.3(5) . . ? C4 C3 C7 120.3(5) . . ? C3 C4 C5 117.5(5) . . ? C3 C4 H4 127(4) . . ? C5 C4 H4 116(4) . . ? O5 C6 O6 125.8(5) . 1_554 ? O5 C6 C5 117.1(5) . . ? O6 C6 C5 117.0(5) 1_554 . ? O3 C7 O4 125.7(5) . . ? O3 C7 C3 118.1(5) . . ? O4 C7 C3 116.2(4) . . ? C3 C2 C1 118.1(5) . . ? C3 C2 H2 122(4) . . ? C1 C2 H2 120(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 O3 Ca2 O1 C8 70.4(4) 2_566 . . . ? O4 Ca2 O1 C8 -116.4(4) 2_466 . . . ? OW1 Ca2 O1 C8 152.0(4) . . . . ? O5 Ca2 O1 C8 -22.9(5) . . . . ? O1 Ca2 O1 C8 163.6(5) 2_456 . . . ? N1 Ca2 O1 C8 -13.2(4) . . . . ? Ca2 Ca2 O1 C8 163.6(5) 2_456 . . . ? O3 Ca2 O1 Ca2 -93.24(16) 2_566 . . 2_456 ? O4 Ca2 O1 Ca2 79.98(16) 2_466 . . 2_456 ? OW1 Ca2 O1 Ca2 -11.6(4) . . . 2_456 ? O5 Ca2 O1 Ca2 173.47(17) . . . 2_456 ? O1 Ca2 O1 Ca2 0.0 2_456 . . 2_456 ? N1 Ca2 O1 Ca2 -176.7(2) . . . 2_456 ? O6 Ca1 O2 C8 -161.2(6) . . . . ? O6 Ca1 O2 C8 18.8(6) 2_567 . . . ? OW2 Ca1 O2 C8 111.1(6) . . . . ? OW2 Ca1 O2 C8 -68.9(6) 2_567 . . . ? O3 Ca2 N1 C1 -91.3(4) 2_566 . . . ? O4 Ca2 N1 C1 88.8(4) 2_466 . . . ? OW1 Ca2 N1 C1 -163.9(4) . . . . ? O5 Ca2 N1 C1 177.5(4) . . . . ? O1 Ca2 N1 C1 1.4(5) 2_456 . . . ? O1 Ca2 N1 C1 6.0(4) . . . . ? Ca2 Ca2 N1 C1 4.1(4) 2_456 . . . ? O3 Ca2 N1 C5 83.8(4) 2_566 . . . ? O4 Ca2 N1 C5 -96.1(4) 2_466 . . . ? OW1 Ca2 N1 C5 11.2(5) . . . . ? O5 Ca2 N1 C5 -7.4(4) . . . . ? O1 Ca2 N1 C5 176.5(3) 2_456 . . . ? O1 Ca2 N1 C5 -178.9(4) . . . . ? Ca2 Ca2 N1 C5 179.2(4) 2_456 . . . ? O3 Ca2 O5 C6 -74.3(5) 2_566 . . . ? O4 Ca2 O5 C6 112.8(5) 2_466 . . . ? OW1 Ca2 O5 C6 -156.1(5) . . . . ? O1 Ca2 O5 C6 -175.2(4) 2_456 . . . ? N1 Ca2 O5 C6 12.0(4) . . . . ? O1 Ca2 O5 C6 21.7(5) . . . . ? Ca2 Ca2 O5 C6 34.7(8) 2_456 . . . ? OW2 Ca1 O6 C6 -156.4(10) . . . 1_556 ? OW2 Ca1 O6 C6 23.6(10) 2_567 . . 1_556 ? O2 Ca1 O6 C6 -68.8(10) 2_567 . . 1_556 ? O2 Ca1 O6 C6 111.2(10) . . . 1_556 ? C1 N1 C5 C4 -2.6(8) . . . . ? Ca2 N1 C5 C4 -177.8(4) . . . . ? C1 N1 C5 C6 178.9(5) . . . . ? Ca2 N1 C5 C6 3.7(6) . . . . ? Ca1 O2 C8 O1 117.1(6) . . . . ? Ca1 O2 C8 C1 -62.9(8) . . . . ? Ca2 O1 C8 O2 -2.6(8) 2_456 . . . ? Ca2 O1 C8 O2 -161.7(4) . . . . ? Ca2 O1 C8 C1 177.4(3) 2_456 . . . ? Ca2 O1 C8 C1 18.2(6) . . . . ? C5 N1 C1 C2 5.1(8) . . . . ? Ca2 N1 C1 C2 -179.9(4) . . . . ? C5 N1 C1 C8 -175.2(5) . . . . ? Ca2 N1 C1 C8 -0.1(6) . . . . ? O2 C8 C1 N1 168.0(5) . . . . ? O1 C8 C1 N1 -11.9(7) . . . . ? O2 C8 C1 C2 -12.3(8) . . . . ? O1 C8 C1 C2 167.8(5) . . . . ? C2 C3 C4 C5 1.5(7) . . . . ? C7 C3 C4 C5 -178.5(5) . . . . ? N1 C5 C4 C3 -0.7(8) . . . . ? C6 C5 C4 C3 177.7(5) . . . . ? Ca2 O5 C6 O6 164.0(5) . . . 1_554 ? Ca2 O5 C6 C5 -14.8(7) . . . . ? N1 C5 C6 O5 6.7(7) . . . . ? C4 C5 C6 O5 -171.7(5) . . . . ? N1 C5 C6 O6 -172.2(5) . . . 1_554 ? C4 C5 C6 O6 9.4(8) . . . 1_554 ? Ca2 O3 C7 O4 127.5(6) 2_566 . . . ? Ca2 O3 C7 C3 -52.0(8) 2_566 . . . ? Ca2 O4 C7 O3 141.8(5) 2_466 . . . ? Ca2 O4 C7 C3 -38.7(7) 2_466 . . . ? C2 C3 C7 O3 122.0(6) . . . . ? C4 C3 C7 O3 -58.0(7) . . . . ? C2 C3 C7 O4 -57.6(7) . . . . ? C4 C3 C7 O4 122.4(5) . . . . ? C4 C3 C2 C1 0.7(8) . . . . ? C7 C3 C2 C1 -179.2(5) . . . . ? N1 C1 C2 C3 -4.1(8) . . . . ? C8 C1 C2 C3 176.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.507 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.230 #===END of CIF for Complex 7 ===================== data_complex8 _database_code_depnum_ccdc_archive 'CCDC 697866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 N2 O21 Sr3' _chemical_formula_weight 841.22 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 16.493(5) _cell_length_b 6.820(6) _cell_length_c 22.220(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2499(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description 'rectangular parallelopipeds' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 6.485 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4638 _exptl_absorpt_correction_T_max 0.5632 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15344 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3087 _reflns_number_gt 2302 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0128P)^2^+5.2780P] 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 3087 _refine_ls_number_parameters 223 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.134 _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 Sr1 Sr 0.5000 0.25833(10) 0.2500 0.01703(16) Uani 1 2 d S . . Sr2 Sr 0.55797(3) 0.45597(8) 0.08694(2) 0.02184(14) Uani 1 1 d D . . O6 O 0.4784(2) 0.1365(6) 0.13488(15) 0.0232(8) Uani 1 1 d . . . O1 O 0.3771(2) 0.3321(6) 0.31654(16) 0.0264(9) Uani 1 1 d . . . O4 O 0.1000(2) 0.0185(6) 0.08977(17) 0.0282(9) Uani 1 1 d . . . C5 C 0.3364(3) 0.1122(7) 0.1524(2) 0.0166(11) Uani 1 1 d D . . N1 N 0.3493(3) 0.1762(6) 0.20877(19) 0.0184(9) Uani 1 1 d . . . OW2 O 0.5925(3) 0.7987(8) 0.1282(3) 0.0471(13) Uani 1 1 d D . . OW1 O 0.4987(3) 0.2713(6) -0.00723(18) 0.029 Uani 1 1 d D . . O3 O 0.0508(2) 0.0558(5) 0.18172(17) 0.0249(8) Uani 1 1 d . . . C4 C 0.2596(3) 0.0767(7) 0.1299(2) 0.0194(11) Uani 1 1 d . . . H4 H 0.2529 0.0334 0.0906 0.023 Uiso 1 1 calc R . . O5 O 0.4004(2) 0.0174(7) 0.06154(18) 0.0339(10) Uani 1 1 d . . . O2 O 0.2479(2) 0.3177(7) 0.34167(17) 0.0404(12) Uani 1 1 d . . . C1 C 0.2847(3) 0.2092(7) 0.2441(2) 0.0174(11) Uani 1 1 d . . . C6 C 0.3037(3) 0.2919(8) 0.3060(2) 0.0227(12) Uani 1 1 d . . . OW3 O 0.6740(4) 0.5896(13) 0.0160(3) 0.038(2) Uani 1 1 d D . . C3 C 0.1929(3) 0.1063(7) 0.1665(2) 0.0156(11) Uani 1 1 d . . . C7 C 0.1084(3) 0.0586(8) 0.1448(2) 0.0202(11) Uani 1 1 d . . . C8 C 0.4109(3) 0.0838(7) 0.1128(2) 0.0185(11) Uani 1 1 d D . . OW5 O 0.5000 -0.1146(9) 0.2500 0.039(6) Uani 1 2 d SD . . C2 C 0.2059(3) 0.1763(7) 0.2248(2) 0.0172(11) Uani 1 1 d . . . H2 H 0.1623 0.2005 0.2503 0.021 Uiso 1 1 calc R . . OW4 O 0.6576(4) 0.1542(12) 0.0558(3) 0.0373(19) Uani 1 1 d D . . H2W2 H 0.6402(17) 0.817(11) 0.136(3) 0.06(2) Uiso 1 1 d D . . H1W2 H 0.567(6) 0.896(11) 0.137(5) 0.04(5) Uiso 1 1 d D . . H1W1 H 0.531(3) 0.205(9) -0.026(3) 0.06(2) Uiso 1 1 d D . . H2W1 H 0.467(2) 0.195(5) 0.0076(18) 0.05(4) Uiso 1 1 d D . . H1W3 H 0.668(12) 0.59(3) -0.0208(14) 0.06(7) Uiso 1 1 d D . . H2W3 H 0.703(5) 0.492(14) 0.022(7) 0.06(5) Uiso 1 1 d D . . H2W4 H 0.704(5) 0.18(4) 0.066(10) 0.07(6) Uiso 1 1 d D . . H1W4 H 0.663(13) 0.09(3) 0.026(6) 0.06(4) Uiso 1 1 d D . . H2W5 H 0.527(10) -0.16(3) 0.277(6) 0.07(6) Uiso 0.50 1 d PD . . H1W5 H 0.5000 -0.235(3) 0.2500 0.06(5) Uiso 1 2 d SD . . 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 Sr1 0.0104(3) 0.0237(3) 0.0170(3) 0.000 -0.0005(3) 0.000 Sr2 0.0167(2) 0.0309(3) 0.0180(2) 0.0010(2) -0.0015(2) 0.0015(2) O6 0.0160(19) 0.039(2) 0.0145(18) -0.0092(16) 0.0031(15) 0.0003(16) O1 0.0122(18) 0.046(2) 0.021(2) -0.0053(18) 0.0006(16) -0.0044(17) O4 0.020(2) 0.045(3) 0.0195(19) -0.0030(18) -0.0023(17) -0.0034(18) C5 0.010(2) 0.020(3) 0.020(3) -0.005(2) -0.002(2) -0.002(2) N1 0.015(2) 0.020(2) 0.020(2) -0.0022(18) 0.0001(18) -0.0006(18) OW2 0.025(3) 0.050(3) 0.067(4) -0.014(3) -0.003(3) 0.000(2) OW1 0.027(3) 0.031(3) 0.029(3) 0.001(2) 0.007(2) -0.005(2) O3 0.0132(18) 0.030(2) 0.032(2) -0.0030(18) 0.0005(16) -0.0019(16) C4 0.019(3) 0.020(3) 0.019(3) 0.004(2) -0.002(2) -0.002(2) O5 0.024(2) 0.053(3) 0.024(2) -0.014(2) 0.0058(18) -0.002(2) O2 0.020(2) 0.077(3) 0.024(2) -0.016(2) 0.0087(19) -0.005(2) C1 0.013(2) 0.020(3) 0.020(3) 0.002(2) 0.000(2) -0.0003(19) C6 0.017(3) 0.028(3) 0.023(3) -0.007(2) -0.002(2) 0.000(2) OW3 0.057(3) 0.028(7) 0.030(4) 0.002(4) 0.014(3) -0.004(4) C3 0.014(2) 0.012(2) 0.022(3) 0.004(2) -0.001(2) 0.000(2) C7 0.011(2) 0.025(3) 0.024(3) 0.007(2) -0.003(2) -0.002(2) C8 0.016(3) 0.019(3) 0.021(3) -0.002(2) 0.000(2) -0.003(2) OW5 0.053(5) 0.029(3) 0.038(4) 0.004(2) -0.011(2) 0.002(2) C2 0.016(3) 0.020(3) 0.016(2) 0.002(2) 0.001(2) -0.004(2) OW4 0.051(4) 0.025(5) 0.040(4) -0.008(4) 0.003(3) 0.004(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 Sr1 OW5 2.544(7) . ? Sr1 O1 2.559(4) 4_655 ? Sr1 O1 2.559(4) . ? Sr1 O3 2.668(4) 6_666 ? Sr1 O3 2.668(4) 7_665 ? Sr1 N1 2.708(4) 4_655 ? Sr1 N1 2.708(4) . ? Sr1 O6 2.713(3) . ? Sr1 O6 2.713(3) 4_655 ? Sr1 Sr2 3.982(3) 4_655 ? Sr1 H2W5 2.96(16) . ? Sr2 O1 2.542(4) 4_655 ? Sr2 OW2 2.575(5) . ? Sr2 OW1 2.630(4) . ? Sr2 OW3 2.641(6) . ? Sr2 O4 2.641(4) 7_665 ? Sr2 OW4 2.723(7) . ? Sr2 OW1 2.733(4) 5_665 ? Sr2 O6 2.757(4) . ? Sr2 O3 2.849(4) 7_665 ? Sr2 C7 3.110(5) 7_665 ? Sr2 Sr2 4.353(3) 5_665 ? Sr2 H2W1 2.92(4) . ? Sr2 H2W3 2.80(10) . ? O6 C8 1.269(6) . ? O1 C6 1.263(6) . ? O1 Sr2 2.542(4) 4_655 ? O4 C7 1.260(6) . ? O4 Sr2 2.641(4) 7_655 ? C5 N1 1.342(6) . ? C5 C4 1.383(7) . ? C5 C8 1.524(6) . ? N1 C1 1.341(6) . ? OW2 H2W2 0.82(2) . ? OW2 H1W2 0.81(9) . ? OW1 Sr2 2.733(4) 5_665 ? OW1 H1W1 0.81(6) . ? OW1 H2W1 0.805(19) . ? O3 C7 1.256(6) . ? O3 Sr1 2.668(4) 6_556 ? O3 Sr2 2.849(4) 7_655 ? C4 C3 1.383(7) . ? C4 H4 0.9300 . ? O5 C8 1.238(6) . ? O2 C6 1.228(6) . ? C1 C2 1.387(7) . ? C1 C6 1.520(7) . ? OW3 H1W3 0.82(2) . ? OW3 H2W3 0.83(10) . ? C3 C2 1.396(7) . ? C3 C7 1.510(7) . ? C7 Sr2 3.110(5) 7_655 ? OW5 H2W5 0.82(2) . ? OW5 H1W5 0.82(2) . ? C2 H2 0.9300 . ? OW4 H2W4 0.82(15) . ? OW4 H1W4 0.80(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 OW5 Sr1 O1 101.34(9) . 4_655 ? OW5 Sr1 O1 101.34(9) . . ? O1 Sr1 O1 157.32(18) 4_655 . ? OW5 Sr1 O3 139.49(8) . 6_666 ? O1 Sr1 O3 86.00(12) 4_655 6_666 ? O1 Sr1 O3 76.75(12) . 6_666 ? OW5 Sr1 O3 139.49(8) . 7_665 ? O1 Sr1 O3 76.75(12) 4_655 7_665 ? O1 Sr1 O3 86.00(12) . 7_665 ? O3 Sr1 O3 81.03(17) 6_666 7_665 ? OW5 Sr1 N1 78.07(9) . 4_655 ? O1 Sr1 N1 60.59(12) 4_655 4_655 ? O1 Sr1 N1 124.92(12) . 4_655 ? O3 Sr1 N1 71.12(12) 6_666 4_655 ? O3 Sr1 N1 129.64(12) 7_665 4_655 ? OW5 Sr1 N1 78.07(9) . . ? O1 Sr1 N1 124.92(12) 4_655 . ? O1 Sr1 N1 60.59(12) . . ? O3 Sr1 N1 129.64(12) 6_666 . ? O3 Sr1 N1 71.12(12) 7_665 . ? N1 Sr1 N1 156.14(18) 4_655 . ? OW5 Sr1 O6 72.17(9) . . ? O1 Sr1 O6 67.62(11) 4_655 . ? O1 Sr1 O6 120.08(11) . . ? O3 Sr1 O6 144.11(12) 6_666 . ? O3 Sr1 O6 69.85(12) 7_665 . ? N1 Sr1 O6 112.09(12) 4_655 . ? N1 Sr1 O6 59.83(12) . . ? OW5 Sr1 O6 72.17(9) . 4_655 ? O1 Sr1 O6 120.08(11) 4_655 4_655 ? O1 Sr1 O6 67.62(11) . 4_655 ? O3 Sr1 O6 69.85(12) 6_666 4_655 ? O3 Sr1 O6 144.11(12) 7_665 4_655 ? N1 Sr1 O6 59.83(12) 4_655 4_655 ? N1 Sr1 O6 112.09(12) . 4_655 ? O6 Sr1 O6 144.34(17) . 4_655 ? OW5 Sr1 Sr2 109.784(19) . 4_655 ? O1 Sr1 Sr2 130.49(9) 4_655 4_655 ? O1 Sr1 Sr2 38.52(8) . 4_655 ? O3 Sr1 Sr2 45.64(8) 6_666 4_655 ? O3 Sr1 Sr2 100.64(9) 7_665 4_655 ? N1 Sr1 Sr2 89.00(9) 4_655 4_655 ? N1 Sr1 Sr2 99.05(9) . 4_655 ? O6 Sr1 Sr2 158.44(7) . 4_655 ? O6 Sr1 Sr2 43.72(9) 4_655 4_655 ? OW5 Sr1 Sr2 109.784(19) . . ? O1 Sr1 Sr2 38.52(8) 4_655 . ? O1 Sr1 Sr2 130.49(9) . . ? O3 Sr1 Sr2 100.64(9) 6_666 . ? O3 Sr1 Sr2 45.64(8) 7_665 . ? N1 Sr1 Sr2 99.05(9) 4_655 . ? N1 Sr1 Sr2 89.00(9) . . ? O6 Sr1 Sr2 43.72(9) . . ? O6 Sr1 Sr2 158.44(7) 4_655 . ? Sr2 Sr1 Sr2 140.43(4) 4_655 . ? OW5 Sr1 H2W5 15(2) . . ? O1 Sr1 H2W5 101(4) 4_655 . ? O1 Sr1 H2W5 101(4) . . ? O3 Sr1 H2W5 125(2) 6_666 . ? O3 Sr1 H2W5 154(3) 7_665 . ? N1 Sr1 H2W5 66(3) 4_655 . ? N1 Sr1 H2W5 90(3) . . ? O6 Sr1 H2W5 85(3) . . ? O6 Sr1 H2W5 59(3) 4_655 . ? Sr2 Sr1 H2W5 100(3) 4_655 . ? Sr2 Sr1 H2W5 119(3) . . ? O1 Sr2 OW2 84.73(16) 4_655 . ? O1 Sr2 OW1 131.96(14) 4_655 . ? OW2 Sr2 OW1 143.14(16) . . ? O1 Sr2 OW3 108.24(18) 4_655 . ? OW2 Sr2 OW3 74.9(2) . . ? OW1 Sr2 OW3 87.69(18) . . ? O1 Sr2 O4 116.69(11) 4_655 7_665 ? OW2 Sr2 O4 93.61(15) . 7_665 ? OW1 Sr2 O4 74.32(13) . 7_665 ? OW3 Sr2 O4 132.3(2) . 7_665 ? O1 Sr2 OW4 73.10(18) 4_655 . ? OW2 Sr2 OW4 130.0(2) . . ? OW1 Sr2 OW4 70.1(2) . . ? OW3 Sr2 OW4 70.8(3) . . ? O4 Sr2 OW4 136.3(2) 7_665 . ? O1 Sr2 OW1 156.50(13) 4_655 5_665 ? OW2 Sr2 OW1 71.85(16) . 5_665 ? OW1 Sr2 OW1 71.53(15) . 5_665 ? OW3 Sr2 OW1 68.1(2) . 5_665 ? O4 Sr2 OW1 64.41(13) 7_665 5_665 ? OW4 Sr2 OW1 123.77(18) . 5_665 ? O1 Sr2 O6 67.16(12) 4_655 . ? OW2 Sr2 O6 133.23(15) . . ? OW1 Sr2 O6 75.66(12) . . ? OW3 Sr2 O6 148.0(2) . . ? O4 Sr2 O6 69.45(12) 7_665 . ? OW4 Sr2 O6 77.77(19) . . ? OW1 Sr2 O6 128.71(12) 5_665 . ? O1 Sr2 O3 73.80(11) 4_655 7_665 ? OW2 Sr2 O3 70.06(15) . 7_665 ? OW1 Sr2 O3 117.93(13) . 7_665 ? OW3 Sr2 O3 144.6(2) . 7_665 ? O4 Sr2 O3 47.35(11) 7_665 7_665 ? OW4 Sr2 O3 138.47(17) . 7_665 ? OW1 Sr2 O3 95.80(12) 5_665 7_665 ? O6 Sr2 O3 66.64(11) . 7_665 ? O1 Sr2 C7 95.62(13) 4_655 7_665 ? OW2 Sr2 C7 80.99(16) . 7_665 ? OW1 Sr2 C7 96.23(14) . 7_665 ? OW3 Sr2 C7 143.9(2) . 7_665 ? O4 Sr2 C7 23.54(12) 7_665 7_665 ? OW4 Sr2 C7 143.9(2) . 7_665 ? OW1 Sr2 C7 79.20(13) 5_665 7_665 ? O6 Sr2 C7 66.32(13) . 7_665 ? O3 Sr2 C7 23.82(12) 7_665 7_665 ? O1 Sr2 Sr1 38.82(8) 4_655 . ? OW2 Sr2 Sr1 92.08(14) . . ? OW1 Sr2 Sr1 118.20(9) . . ? OW3 Sr2 Sr1 146.48(16) . . ? O4 Sr2 Sr1 78.23(8) 7_665 . ? OW4 Sr2 Sr1 96.92(15) . . ? OW1 Sr2 Sr1 137.54(9) 5_665 . ? O6 Sr2 Sr1 42.84(7) . . ? O3 Sr2 Sr1 42.02(8) 7_665 . ? C7 Sr2 Sr1 59.23(10) 7_665 . ? O1 Sr2 Sr2 168.52(10) 4_655 5_665 ? OW2 Sr2 Sr2 106.74(13) . 5_665 ? OW1 Sr2 Sr2 36.56(9) . 5_665 ? OW3 Sr2 Sr2 74.99(16) . 5_665 ? O4 Sr2 Sr2 64.24(8) 7_665 5_665 ? OW4 Sr2 Sr2 98.26(16) . 5_665 ? OW1 Sr2 Sr2 34.98(9) 5_665 5_665 ? O6 Sr2 Sr2 104.06(8) . 5_665 ? O3 Sr2 Sr2 110.27(8) 7_665 5_665 ? C7 Sr2 Sr2 87.02(10) 7_665 5_665 ? Sr1 Sr2 Sr2 138.49(2) . 5_665 ? O1 Sr2 H2W1 121.5(7) 4_655 . ? OW2 Sr2 H2W1 151.9(8) . . ? OW1 Sr2 H2W1 15.6(5) . . ? OW3 Sr2 H2W1 102.8(6) . . ? O4 Sr2 H2W1 66.9(8) 7_665 . ? OW4 Sr2 H2W1 72.2(9) . . ? OW1 Sr2 H2W1 81.3(8) 5_665 . ? O6 Sr2 H2W1 60.5(6) . . ? O3 Sr2 H2W1 105.6(7) 7_665 . ? C7 Sr2 H2W1 86.3(8) 7_665 . ? Sr1 Sr2 H2W1 102.7(5) . . ? Sr2 Sr2 H2W1 47.4(7) 5_665 . ? O1 Sr2 H2W3 96(3) 4_655 . ? OW2 Sr2 H2W3 85(3) . . ? OW1 Sr2 H2W3 87(4) . . ? OW3 Sr2 H2W3 17(2) . . ? O4 Sr2 H2W3 147(3) 7_665 . ? OW4 Sr2 H2W3 54.6(16) . . ? OW1 Sr2 H2W3 84.2(15) 5_665 . ? O6 Sr2 H2W3 132.4(16) . . ? O3 Sr2 H2W3 154(4) 7_665 . ? C7 Sr2 H2W3 161.0(8) 7_665 . ? Sr1 Sr2 H2W3 135(3) . . ? Sr2 Sr2 H2W3 85(3) 5_665 . ? H2W1 Sr2 H2W3 100(4) . . ? C8 O6 Sr1 124.5(3) . . ? C8 O6 Sr2 119.5(3) . . ? Sr1 O6 Sr2 93.44(12) . . ? C6 O1 Sr2 129.2(3) . 4_655 ? C6 O1 Sr1 127.5(3) . . ? Sr2 O1 Sr1 102.66(13) 4_655 . ? C7 O4 Sr2 99.6(3) . 7_655 ? N1 C5 C4 122.6(5) . . ? N1 C5 C8 116.9(4) . . ? C4 C5 C8 120.5(4) . . ? C5 N1 C1 118.3(4) . . ? C5 N1 Sr1 121.8(3) . . ? C1 N1 Sr1 119.8(3) . . ? Sr2 OW2 H2W2 115(5) . . ? Sr2 OW2 H1W2 135(9) . . ? H2W2 OW2 H1W2 109(9) . . ? Sr2 OW1 Sr2 108.47(15) . 5_665 ? Sr2 OW1 H1W1 116(5) . . ? Sr2 OW1 H1W1 105(5) 5_665 . ? Sr2 OW1 H2W1 103(3) . . ? Sr2 OW1 H2W1 119(3) 5_665 . ? H1W1 OW1 H2W1 106(6) . . ? C7 O3 Sr1 128.4(3) . 6_556 ? C7 O3 Sr2 89.8(3) . 7_655 ? Sr1 O3 Sr2 92.34(11) 6_556 7_655 ? C3 C4 C5 119.4(5) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C1 C2 122.4(5) . . ? N1 C1 C6 115.3(4) . . ? C2 C1 C6 122.2(5) . . ? O2 C6 O1 124.6(5) . . ? O2 C6 C1 118.9(5) . . ? O1 C6 C1 116.5(5) . . ? Sr2 OW3 H1W3 120(10) . . ? Sr2 OW3 H2W3 93(8) . . ? H1W3 OW3 H2W3 102(10) . . ? C4 C3 C2 118.2(5) . . ? C4 C3 C7 121.0(5) . . ? C2 C3 C7 120.8(5) . . ? O3 C7 O4 123.2(5) . . ? O3 C7 C3 119.5(5) . . ? O4 C7 C3 117.3(5) . . ? O3 C7 Sr2 66.4(3) . 7_655 ? O4 C7 Sr2 56.8(3) . 7_655 ? C3 C7 Sr2 174.2(4) . 7_655 ? O5 C8 O6 125.5(5) . . ? O5 C8 C5 117.8(5) . . ? O6 C8 C5 116.6(4) . . ? Sr1 OW5 H2W5 113(10) . . ? Sr1 OW5 H1W5 180.000(5) . . ? H2W5 OW5 H1W5 67(10) . . ? C1 C2 C3 119.0(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? Sr2 OW4 H2W4 109(10) . . ? Sr2 OW4 H1W4 134(10) . . ? H2W4 OW4 H1W4 104.00 . . ? 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 OW5 Sr1 Sr2 O1 -83.32(15) . . . 4_655 ? O1 Sr1 Sr2 O1 151.1(2) . . . 4_655 ? O3 Sr1 Sr2 O1 69.51(17) 6_666 . . 4_655 ? O3 Sr1 Sr2 O1 135.57(18) 7_665 . . 4_655 ? N1 Sr1 Sr2 O1 -2.82(17) 4_655 . . 4_655 ? N1 Sr1 Sr2 O1 -160.26(17) . . . 4_655 ? O6 Sr1 Sr2 O1 -115.42(19) . . . 4_655 ? O6 Sr1 Sr2 O1 8.1(3) 4_655 . . 4_655 ? Sr2 Sr1 Sr2 O1 96.68(15) 4_655 . . 4_655 ? OW5 Sr1 Sr2 OW2 -162.26(12) . . . . ? O1 Sr1 Sr2 OW2 -78.94(19) 4_655 . . . ? O1 Sr1 Sr2 OW2 72.16(16) . . . . ? O3 Sr1 Sr2 OW2 -9.43(14) 6_666 . . . ? O3 Sr1 Sr2 OW2 56.63(16) 7_665 . . . ? N1 Sr1 Sr2 OW2 -81.76(15) 4_655 . . . ? N1 Sr1 Sr2 OW2 120.80(15) . . . . ? O6 Sr1 Sr2 OW2 165.63(16) . . . . ? O6 Sr1 Sr2 OW2 -70.8(3) 4_655 . . . ? Sr2 Sr1 Sr2 OW2 17.74(12) 4_655 . . . ? OW5 Sr1 Sr2 OW1 39.64(12) . . . . ? O1 Sr1 Sr2 OW1 122.95(19) 4_655 . . . ? O1 Sr1 Sr2 OW1 -85.95(16) . . . . ? O3 Sr1 Sr2 OW1 -167.54(14) 6_666 . . . ? O3 Sr1 Sr2 OW1 -101.47(16) 7_665 . . . ? N1 Sr1 Sr2 OW1 120.13(15) 4_655 . . . ? N1 Sr1 Sr2 OW1 -37.30(14) . . . . ? O6 Sr1 Sr2 OW1 7.53(16) . . . . ? O6 Sr1 Sr2 OW1 131.1(3) 4_655 . . . ? Sr2 Sr1 Sr2 OW1 -140.36(12) 4_655 . . . ? OW5 Sr1 Sr2 OW3 -97.0(4) . . . . ? O1 Sr1 Sr2 OW3 -13.6(4) 4_655 . . . ? O1 Sr1 Sr2 OW3 137.5(4) . . . . ? O3 Sr1 Sr2 OW3 55.9(4) 6_666 . . . ? O3 Sr1 Sr2 OW3 121.9(4) 7_665 . . . ? N1 Sr1 Sr2 OW3 -16.5(4) 4_655 . . . ? N1 Sr1 Sr2 OW3 -173.9(4) . . . . ? O6 Sr1 Sr2 OW3 -129.1(4) . . . . ? O6 Sr1 Sr2 OW3 -5.5(4) 4_655 . . . ? Sr2 Sr1 Sr2 OW3 83.0(4) 4_655 . . . ? OW5 Sr1 Sr2 O4 104.49(9) . . . 7_665 ? O1 Sr1 Sr2 O4 -172.20(17) 4_655 . . 7_665 ? O1 Sr1 Sr2 O4 -21.10(15) . . . 7_665 ? O3 Sr1 Sr2 O4 -102.69(12) 6_666 . . 7_665 ? O3 Sr1 Sr2 O4 -36.62(14) 7_665 . . 7_665 ? N1 Sr1 Sr2 O4 -175.02(13) 4_655 . . 7_665 ? N1 Sr1 Sr2 O4 27.55(13) . . . 7_665 ? O6 Sr1 Sr2 O4 72.38(15) . . . 7_665 ? O6 Sr1 Sr2 O4 -164.1(3) 4_655 . . 7_665 ? Sr2 Sr1 Sr2 O4 -75.51(9) 4_655 . . 7_665 ? OW5 Sr1 Sr2 OW4 -31.49(19) . . . . ? O1 Sr1 Sr2 OW4 51.8(2) 4_655 . . . ? O1 Sr1 Sr2 OW4 -157.1(2) . . . . ? O3 Sr1 Sr2 OW4 121.3(2) 6_666 . . . ? O3 Sr1 Sr2 OW4 -172.6(2) 7_665 . . . ? N1 Sr1 Sr2 OW4 49.0(2) 4_655 . . . ? N1 Sr1 Sr2 OW4 -108.4(2) . . . . ? O6 Sr1 Sr2 OW4 -63.6(2) . . . . ? O6 Sr1 Sr2 OW4 59.9(3) 4_655 . . . ? Sr2 Sr1 Sr2 OW4 148.51(19) 4_655 . . . ? OW5 Sr1 Sr2 OW1 132.70(13) . . . 5_665 ? O1 Sr1 Sr2 OW1 -144.0(2) 4_655 . . 5_665 ? O1 Sr1 Sr2 OW1 7.12(18) . . . 5_665 ? O3 Sr1 Sr2 OW1 -74.47(16) 6_666 . . 5_665 ? O3 Sr1 Sr2 OW1 -8.41(17) 7_665 . . 5_665 ? N1 Sr1 Sr2 OW1 -146.80(16) 4_655 . . 5_665 ? N1 Sr1 Sr2 OW1 55.76(16) . . . 5_665 ? O6 Sr1 Sr2 OW1 100.60(18) . . . 5_665 ? O6 Sr1 Sr2 OW1 -135.9(3) 4_655 . . 5_665 ? Sr2 Sr1 Sr2 OW1 -47.30(13) 4_655 . . 5_665 ? OW5 Sr1 Sr2 O6 32.11(11) . . . . ? O1 Sr1 Sr2 O6 115.42(19) 4_655 . . . ? O1 Sr1 Sr2 O6 -93.48(16) . . . . ? O3 Sr1 Sr2 O6 -175.07(14) 6_666 . . . ? O3 Sr1 Sr2 O6 -109.00(16) 7_665 . . . ? N1 Sr1 Sr2 O6 112.60(15) 4_655 . . . ? N1 Sr1 Sr2 O6 -44.83(14) . . . . ? O6 Sr1 Sr2 O6 123.5(3) 4_655 . . . ? Sr2 Sr1 Sr2 O6 -147.89(11) 4_655 . . . ? OW5 Sr1 Sr2 O3 141.11(11) . . . 7_665 ? O1 Sr1 Sr2 O3 -135.57(18) 4_655 . . 7_665 ? O1 Sr1 Sr2 O3 15.53(16) . . . 7_665 ? O3 Sr1 Sr2 O3 -66.06(19) 6_666 . . 7_665 ? N1 Sr1 Sr2 O3 -138.40(15) 4_655 . . 7_665 ? N1 Sr1 Sr2 O3 64.17(14) . . . 7_665 ? O6 Sr1 Sr2 O3 109.00(16) . . . 7_665 ? O6 Sr1 Sr2 O3 -127.5(3) 4_655 . . 7_665 ? Sr2 Sr1 Sr2 O3 -38.89(11) 4_655 . . 7_665 ? OW5 Sr1 Sr2 C7 119.51(12) . . . 7_665 ? O1 Sr1 Sr2 C7 -157.17(19) 4_655 . . 7_665 ? O1 Sr1 Sr2 C7 -6.07(16) . . . 7_665 ? O3 Sr1 Sr2 C7 -87.66(15) 6_666 . . 7_665 ? O3 Sr1 Sr2 C7 -21.60(16) 7_665 . . 7_665 ? N1 Sr1 Sr2 C7 -160.00(15) 4_655 . . 7_665 ? N1 Sr1 Sr2 C7 42.57(15) . . . 7_665 ? O6 Sr1 Sr2 C7 87.40(17) . . . 7_665 ? O6 Sr1 Sr2 C7 -149.1(3) 4_655 . . 7_665 ? Sr2 Sr1 Sr2 C7 -60.49(12) 4_655 . . 7_665 ? OW5 Sr1 Sr2 Sr2 79.33(3) . . . 5_665 ? O1 Sr1 Sr2 Sr2 162.65(15) 4_655 . . 5_665 ? O1 Sr1 Sr2 Sr2 -46.25(12) . . . 5_665 ? O3 Sr1 Sr2 Sr2 -127.84(8) 6_666 . . 5_665 ? O3 Sr1 Sr2 Sr2 -61.78(12) 7_665 . . 5_665 ? N1 Sr1 Sr2 Sr2 159.82(10) 4_655 . . 5_665 ? N1 Sr1 Sr2 Sr2 2.39(10) . . . 5_665 ? O6 Sr1 Sr2 Sr2 47.22(12) . . . 5_665 ? O6 Sr1 Sr2 Sr2 170.8(2) 4_655 . . 5_665 ? Sr2 Sr1 Sr2 Sr2 -100.67(3) 4_655 . . 5_665 ? OW5 Sr1 O6 C8 81.9(4) . . . . ? O1 Sr1 O6 C8 -167.2(4) 4_655 . . . ? O1 Sr1 O6 C8 -11.1(4) . . . . ? O3 Sr1 O6 C8 -121.5(4) 6_666 . . . ? O3 Sr1 O6 C8 -83.7(4) 7_665 . . . ? N1 Sr1 O6 C8 150.5(4) 4_655 . . . ? N1 Sr1 O6 C8 -4.4(4) . . . . ? O6 Sr1 O6 C8 81.9(4) 4_655 . . . ? Sr2 Sr1 O6 C8 -16.9(6) 4_655 . . . ? Sr2 Sr1 O6 C8 -129.8(4) . . . . ? OW5 Sr1 O6 Sr2 -148.31(10) . . . . ? O1 Sr1 O6 Sr2 -37.46(11) 4_655 . . . ? O1 Sr1 O6 Sr2 118.69(13) . . . . ? O3 Sr1 O6 Sr2 8.3(2) 6_666 . . . ? O3 Sr1 O6 Sr2 46.06(11) 7_665 . . . ? N1 Sr1 O6 Sr2 -79.71(14) 4_655 . . . ? N1 Sr1 O6 Sr2 125.37(16) . . . . ? O6 Sr1 O6 Sr2 -148.31(10) 4_655 . . . ? Sr2 Sr1 O6 Sr2 112.9(2) 4_655 . . . ? O1 Sr2 O6 C8 171.2(4) 4_655 . . . ? OW2 Sr2 O6 C8 113.4(4) . . . . ? OW1 Sr2 O6 C8 -39.9(3) . . . . ? OW3 Sr2 O6 C8 -100.7(5) . . . . ? O4 Sr2 O6 C8 38.5(3) 7_665 . . . ? OW4 Sr2 O6 C8 -112.2(4) . . . . ? OW1 Sr2 O6 C8 11.5(4) 5_665 . . . ? O3 Sr2 O6 C8 89.7(4) 7_665 . . . ? C7 Sr2 O6 C8 63.7(3) 7_665 . . . ? Sr1 Sr2 O6 C8 133.3(4) . . . . ? Sr2 Sr2 O6 C8 -16.6(4) 5_665 . . . ? O1 Sr2 O6 Sr1 37.91(11) 4_655 . . . ? OW2 Sr2 O6 Sr1 -19.9(2) . . . . ? OW1 Sr2 O6 Sr1 -173.15(14) . . . . ? OW3 Sr2 O6 Sr1 126.0(3) . . . . ? O4 Sr2 O6 Sr1 -94.81(12) 7_665 . . . ? OW4 Sr2 O6 Sr1 114.52(19) . . . . ? OW1 Sr2 O6 Sr1 -121.75(14) 5_665 . . . ? O3 Sr2 O6 Sr1 -43.59(10) 7_665 . . . ? C7 Sr2 O6 Sr1 -69.59(13) 7_665 . . . ? Sr2 Sr2 O6 Sr1 -149.90(7) 5_665 . . . ? OW5 Sr1 O1 C6 -64.3(5) . . . . ? O1 Sr1 O1 C6 115.7(5) 4_655 . . . ? O3 Sr1 O1 C6 157.1(5) 6_666 . . . ? O3 Sr1 O1 C6 75.4(5) 7_665 . . . ? N1 Sr1 O1 C6 -147.6(4) 4_655 . . . ? N1 Sr1 O1 C6 4.9(4) . . . . ? O6 Sr1 O1 C6 11.5(5) . . . . ? O6 Sr1 O1 C6 -129.5(5) 4_655 . . . ? Sr2 Sr1 O1 C6 -171.9(5) 4_655 . . . ? Sr2 Sr1 O1 C6 64.4(5) . . . . ? OW5 Sr1 O1 Sr2 107.60(11) . . . 4_655 ? O1 Sr1 O1 Sr2 -72.40(11) 4_655 . . 4_655 ? O3 Sr1 O1 Sr2 -30.94(13) 6_666 . . 4_655 ? O3 Sr1 O1 Sr2 -112.65(15) 7_665 . . 4_655 ? N1 Sr1 O1 Sr2 24.3(2) 4_655 . . 4_655 ? N1 Sr1 O1 Sr2 176.8(2) . . . 4_655 ? O6 Sr1 O1 Sr2 -176.57(12) . . . 4_655 ? O6 Sr1 O1 Sr2 42.46(13) 4_655 . . 4_655 ? Sr2 Sr1 O1 Sr2 -123.71(10) . . . 4_655 ? C4 C5 N1 C1 -0.9(7) . . . . ? C8 C5 N1 C1 177.7(4) . . . . ? C4 C5 N1 Sr1 -177.5(4) . . . . ? C8 C5 N1 Sr1 1.1(6) . . . . ? OW5 Sr1 N1 C5 -74.9(4) . . . . ? O1 Sr1 N1 C5 20.7(4) 4_655 . . . ? O1 Sr1 N1 C5 174.6(4) . . . . ? O3 Sr1 N1 C5 138.6(4) 6_666 . . . ? O3 Sr1 N1 C5 78.4(4) 7_665 . . . ? N1 Sr1 N1 C5 -74.9(4) 4_655 . . . ? O6 Sr1 N1 C5 1.2(4) . . . . ? O6 Sr1 N1 C5 -139.9(4) 4_655 . . . ? Sr2 Sr1 N1 C5 176.6(4) 4_655 . . . ? Sr2 Sr1 N1 C5 35.5(4) . . . . ? OW5 Sr1 N1 C1 108.6(4) . . . . ? O1 Sr1 N1 C1 -155.8(3) 4_655 . . . ? O1 Sr1 N1 C1 -1.9(3) . . . . ? O3 Sr1 N1 C1 -38.0(4) 6_666 . . . ? O3 Sr1 N1 C1 -98.1(4) 7_665 . . . ? N1 Sr1 N1 C1 108.6(4) 4_655 . . . ? O6 Sr1 N1 C1 -175.3(4) . . . . ? O6 Sr1 N1 C1 43.6(4) 4_655 . . . ? Sr2 Sr1 N1 C1 0.1(4) 4_655 . . . ? Sr2 Sr1 N1 C1 -141.0(4) . . . . ? O1 Sr2 OW1 Sr2 179.74(12) 4_655 . . 5_665 ? OW2 Sr2 OW1 Sr2 -6.9(3) . . . 5_665 ? OW3 Sr2 OW1 Sr2 -67.6(2) . . . 5_665 ? O4 Sr2 OW1 Sr2 67.72(15) 7_665 . . 5_665 ? OW4 Sr2 OW1 Sr2 -138.1(2) . . . 5_665 ? OW1 Sr2 OW1 Sr2 0.0 5_665 . . 5_665 ? O6 Sr2 OW1 Sr2 139.99(17) . . . 5_665 ? O3 Sr2 OW1 Sr2 86.76(16) 7_665 . . 5_665 ? C7 Sr2 OW1 Sr2 76.40(16) 7_665 . . 5_665 ? Sr1 Sr2 OW1 Sr2 134.71(10) . . . 5_665 ? N1 C5 C4 C3 -0.5(8) . . . . ? C8 C5 C4 C3 -179.1(4) . . . . ? C5 N1 C1 C2 1.2(7) . . . . ? Sr1 N1 C1 C2 177.8(4) . . . . ? C5 N1 C1 C6 -176.8(4) . . . . ? Sr1 N1 C1 C6 -0.2(6) . . . . ? Sr2 O1 C6 O2 4.4(9) 4_655 . . . ? Sr1 O1 C6 O2 174.2(4) . . . . ? Sr2 O1 C6 C1 -176.7(3) 4_655 . . . ? Sr1 O1 C6 C1 -6.8(7) . . . . ? N1 C1 C6 O2 -176.8(5) . . . . ? C2 C1 C6 O2 5.2(8) . . . . ? N1 C1 C6 O1 4.2(7) . . . . ? C2 C1 C6 O1 -173.8(5) . . . . ? C5 C4 C3 C2 1.6(7) . . . . ? C5 C4 C3 C7 -176.6(5) . . . . ? Sr1 O3 C7 O4 91.0(6) 6_556 . . . ? Sr2 O3 C7 O4 -1.8(5) 7_655 . . . ? Sr1 O3 C7 C3 -87.1(5) 6_556 . . . ? Sr2 O3 C7 C3 -180.0(4) 7_655 . . . ? Sr1 O3 C7 Sr2 92.8(3) 6_556 . . 7_655 ? Sr2 O4 C7 O3 2.0(6) 7_655 . . . ? Sr2 O4 C7 C3 -179.8(4) 7_655 . . . ? C4 C3 C7 O3 168.3(5) . . . . ? C2 C3 C7 O3 -9.9(7) . . . . ? C4 C3 C7 O4 -10.0(7) . . . . ? C2 C3 C7 O4 171.8(5) . . . . ? Sr1 O6 C8 O5 -175.7(4) . . . . ? Sr2 O6 C8 O5 66.1(6) . . . . ? Sr1 O6 C8 C5 6.6(6) . . . . ? Sr2 O6 C8 C5 -111.5(4) . . . . ? N1 C5 C8 O5 177.2(5) . . . . ? C4 C5 C8 O5 -4.2(7) . . . . ? N1 C5 C8 O6 -5.0(7) . . . . ? C4 C5 C8 O6 173.7(5) . . . . ? N1 C1 C2 C3 0.0(7) . . . . ? C6 C1 C2 C3 177.8(5) . . . . ? C4 C3 C2 C1 -1.4(7) . . . . ? C7 C3 C2 C1 176.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.656 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.213 #===END of CIF for Complex 8 ===================== data_complex9 _database_code_depnum_ccdc_archive 'CCDC 697867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Ba2 N2 O14' _chemical_formula_weight 728.94 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.310(3) _cell_length_b 7.851(4) _cell_length_c 17.242(4) _cell_angle_alpha 101.448(5) _cell_angle_beta 92.926(4) _cell_angle_gamma 90.140(4) _cell_volume 968.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.4 _exptl_crystal_description 'rectangular parallelopipeds' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 4.127 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4924 _exptl_absorpt_correction_T_max 0.5765 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6407 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.34 _reflns_number_total 4630 _reflns_number_gt 4023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0904P)^2^+4.1709P] 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 4630 _refine_ls_number_parameters 285 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.2091 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.167 _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 Ba1 Ba 0.24294(9) 0.00421(9) 0.73835(4) 0.0176(2) Uani 1 1 d D . . Ba2 Ba -0.24094(10) -0.22407(11) 0.82944(4) 0.0259(2) Uani 1 1 d . . . C11 C 0.2619(14) -0.3613(14) 0.9290(6) 0.0133(19) Uani 1 1 d . . . OW1 O -0.1407(15) -0.4297(14) 0.6830(5) 0.030(2) Uani 1 1 d D . . O5 O 0.0566(15) -0.3656(13) 0.4823(6) 0.033(2) Uani 1 1 d . . . H5 H 0.0183 -0.4469 0.5005 0.039 Uiso 1 1 calc R . . O3 O 0.5738(12) -0.1358(12) 0.6953(5) 0.0236(18) Uani 1 1 d . . . O8 O 0.0512(15) 0.1275(12) 0.8866(5) 0.029(2) Uani 1 1 d . . . O7 O -0.1070(13) -0.1219(12) 0.9857(5) 0.027 Uani 1 1 d . . . O10 O 0.4060(12) -0.1643(12) 0.8622(6) 0.0265(19) Uani 1 1 d . . . O9 O 0.1273(12) -0.2646(13) 0.8183(5) 0.0252(19) Uani 1 1 d . . . O6 O 0.1207(15) -0.2534(12) 0.6109(5) 0.022(2) Uani 1 1 d . . . O4 O -0.1472(13) -0.0192(12) 0.7201(6) 0.028(2) Uani 1 1 d . . . C10 C 0.1890(14) -0.5262(14) 0.9129(6) 0.0130(19) Uani 1 1 d . . . H10 H 0.1396 -0.5729 0.8624 0.016 Uiso 1 1 calc R . . O1 O 0.4425(15) 0.2663(13) 0.6831(6) 0.035(2) Uani 1 1 d . . . C4 C 0.1953(18) -0.0803(16) 0.4330(7) 0.023(2) Uani 1 1 d . . . H4 H 0.1397 -0.1682 0.3949 0.027 Uiso 1 1 calc R . . N1 N 0.2744(13) 0.0350(13) 0.5720(6) 0.0177(19) Uani 1 1 d . . . C5 C 0.197(2) -0.0891(18) 0.5138(8) 0.029 Uani 1 1 d . . . O12 O -0.3914(15) -0.5644(13) 0.8047(6) 0.033(2) Uani 1 1 d . . . O2 O 0.5290(16) 0.4262(13) 0.5980(6) 0.035(2) Uani 1 1 d . . . H6 H 0.5733 0.4869 0.6389 0.052 Uiso 1 1 calc R . . OW2 O 0.032(2) 0.3004(16) 0.7371(8) 0.049(3) Uani 1 1 d D . . O11 O 0.5202(15) 0.1901(14) 0.8389(5) 0.033 Uani 1 1 d . . . C3 C 0.2783(15) 0.0615(15) 0.4107(6) 0.017(2) Uani 1 1 d . . . C12 C -0.3395(17) -0.7025(15) 0.9959(8) 0.022(2) Uani 1 1 d . . . H12 H -0.3972 -0.8109 0.9838 0.027 Uiso 1 1 calc R . . C1 C 0.3490(16) 0.1704(15) 0.5505(6) 0.017 Uani 1 1 d . . . C8 C 0.1206(16) -0.2486(15) 0.5379(7) 0.021(2) Uani 1 1 d . . . C16 C -0.4067(19) -0.6661(17) 0.8536(7) 0.026(3) Uani 1 1 d D . . C9 C -0.1884(15) -0.3767(14) 1.0288(7) 0.016(2) Uani 1 1 d . . . C6 C 0.4452(16) 0.3045(16) 0.6139(7) 0.020(2) Uani 1 1 d . . . N2 N -0.2549(13) -0.4397(12) 0.9539(5) 0.015 Uani 1 1 d . . . C14 C 0.1095(17) 0.1947(15) 0.9538(7) 0.019(2) Uani 1 1 d . . . C13 C -0.3284(16) -0.5973(15) 0.9372(6) 0.019(2) Uani 1 1 d D . . C2 C 0.358(2) 0.1883(18) 0.4702(9) 0.021 Uani 1 1 d . . . H2 H 0.4169 0.2840 0.4579 0.037 Uiso 1 1 calc R . . C15 C 0.2635(18) -0.2528(14) 0.8653(7) 0.021(2) Uani 1 1 d . . . C7 C -0.2841(15) -0.0703(14) 0.6757(7) 0.016(2) Uani 1 1 d . . . H1W1 H -0.07(2) -0.40(3) 0.651(9) 0.034(4) Uiso 1 1 d D . . H2W1 H -0.235(15) -0.46(3) 0.655(10) 0.032(4) Uiso 1 1 d D . . H1W2 H 0.141(5) 0.319(8) 0.733(13) 0.041(7) Uiso 1 1 d D . . H2W2 H -0.017(15) 0.386(9) 0.725(7) 0.042(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0176(4) 0.0195(3) 0.0167(3) 0.0061(2) 0.0002(2) -0.0041(2) Ba2 0.0209(4) 0.0379(5) 0.0207(4) 0.0109(3) 0.0001(3) -0.0046(3) C11 0.012(5) 0.017(5) 0.013(5) 0.010(4) -0.002(4) -0.001(4) OW1 0.038(6) 0.038(5) 0.016(4) 0.012(4) -0.003(4) -0.001(4) O5 0.044(6) 0.030(5) 0.022(5) 0.003(4) 0.001(4) -0.018(4) O3 0.017(4) 0.037(5) 0.020(4) 0.017(4) -0.006(3) -0.005(3) O8 0.043(6) 0.025(5) 0.018(4) -0.001(4) -0.001(4) -0.006(4) O7 0.031(6) 0.025(6) 0.023(6) 0.005(4) -0.003(4) 0.004(4) O10 0.022(4) 0.030(5) 0.034(5) 0.020(4) 0.005(4) -0.001(4) O9 0.031(4) 0.022(5) 0.017(4) 0.011(4) -0.004(3) 0.002(4) O6 0.032(6) 0.024(5) 0.011(4) 0.004(3) 0.008(4) -0.001(4) O4 0.031(5) 0.028(5) 0.024(4) 0.004(4) -0.001(4) -0.006(4) C10 0.015(5) 0.019(5) 0.005(4) 0.002(4) 0.000(3) -0.007(4) O1 0.049(6) 0.032(5) 0.025(5) 0.006(4) -0.002(4) -0.028(5) C4 0.029(6) 0.023(6) 0.019(5) 0.008(5) 0.013(5) 0.001(5) N1 0.017(5) 0.019(5) 0.020(5) 0.009(4) 0.005(4) -0.007(4) C5 0.039(6) 0.023(6) 0.023(6) 0.000(5) -0.001(5) 0.002(5) O12 0.047(6) 0.032(5) 0.019(4) 0.006(4) -0.003(4) -0.013(4) O2 0.054(7) 0.025(5) 0.024(5) 0.006(4) -0.009(4) -0.017(4) OW2 0.052(8) 0.040(7) 0.055(8) 0.011(6) -0.006(6) 0.018(6) O11 0.046(6) 0.035(6) 0.016(6) 0.000(5) -0.001(5) -0.003(5) C3 0.013(5) 0.022(5) 0.014(5) 0.000(4) -0.002(4) -0.004(4) C12 0.025(6) 0.016(5) 0.028(6) 0.008(5) 0.003(5) -0.003(4) C1 0.025(4) 0.019(5) 0.009(4) 0.006(3) 0.004(3) 0.004(3) C8 0.019(6) 0.019(5) 0.026(6) 0.007(5) 0.001(4) -0.002(4) C16 0.032(7) 0.024(6) 0.017(5) -0.003(5) -0.001(5) -0.008(5) C9 0.023(5) 0.012(5) 0.013(5) 0.003(4) -0.006(4) -0.011(4) C6 0.021(6) 0.026(6) 0.015(5) 0.004(4) 0.008(4) -0.010(4) N2 0.022(5) 0.019(5) 0.011(5) 0.009(4) 0.005(4) -0.003(4) C14 0.023(6) 0.018(5) 0.015(5) 0.009(4) -0.006(4) -0.005(4) C13 0.021(6) 0.024(6) 0.011(5) -0.002(4) 0.007(4) 0.009(4) C2 0.026(6) 0.023(7) 0.013(6) 0.002(5) -0.002(5) -0.003(5) C15 0.023(6) 0.016(4) 0.021(6) 0.006(4) 0.004(5) -0.002(4) C7 0.014(5) 0.012(5) 0.020(5) 0.000(4) 0.002(4) -0.003(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 Ba1 O3 2.735(9) . ? Ba1 O6 2.783(9) . ? Ba1 OW2 2.797(12) . ? Ba1 O11 2.805(10) . ? Ba1 O4 2.854(10) . ? Ba1 O1 2.859(9) . ? Ba1 O9 2.887(9) . ? Ba1 O10 2.932(9) . ? Ba1 N1 2.947(10) . ? Ba1 O8 2.971(10) . ? Ba1 C15 3.257(11) . ? Ba1 Ba2 4.455(2) . ? Ba1 H1W2 2.60(7) . ? Ba2 O10 2.692(9) 1_455 ? Ba2 O9 2.724(9) . ? Ba2 O7 2.780(8) . ? Ba2 O4 2.818(10) . ? Ba2 O3 2.826(8) 1_455 ? Ba2 O12 2.831(10) . ? Ba2 OW1 2.845(10) . ? Ba2 N2 2.991(9) . ? Ba2 C7 3.126(12) . ? Ba2 Ba1 4.523(2) 1_455 ? C11 C10 1.370(14) . ? C11 C12 1.385(16) 2_547 ? C11 C15 1.517(15) . ? OW1 H1W1 0.84(18) . ? OW1 H2W1 0.83(12) . ? O5 C8 1.259(15) . ? O5 H5 0.8200 . ? O3 C7 1.250(14) 1_655 ? O3 Ba2 2.826(8) 1_655 ? O8 C14 1.228(14) . ? O7 C14 1.286(14) 2_557 ? O10 C15 1.260(15) . ? O10 Ba2 2.692(9) 1_655 ? O9 C15 1.243(15) . ? O6 C8 1.267(15) . ? O4 C7 1.244(14) . ? C10 C9 1.376(15) 2_547 ? C10 H10 0.9300 . ? O1 C6 1.288(15) . ? C4 C3 1.395(16) . ? C4 C5 1.409(18) . ? C4 H4 0.9300 . ? N1 C1 1.318(15) . ? N1 C5 1.352(16) . ? C5 C8 1.509(18) . ? O12 C16 1.280(16) . ? O2 C6 1.218(15) . ? O2 H6 0.8200 . ? OW2 H1W2 0.82(5) . ? OW2 H2W2 0.82(8) . ? O11 C16 1.222(16) 1_665 ? C3 C2 1.384(17) . ? C3 C7 1.507(15) 2_556 ? C12 C11 1.385(16) 2_547 ? C12 C13 1.433(16) . ? C12 H12 0.9300 . ? C1 C2 1.423(18) . ? C1 C6 1.503(16) . ? C16 O11 1.222(16) 1_445 ? C16 C13 1.517(13) . ? C9 N2 1.354(13) . ? C9 C10 1.376(15) 2_547 ? C9 C14 1.507(15) 2_557 ? N2 C13 1.320(15) . ? C14 O7 1.286(14) 2_557 ? C14 C9 1.507(15) 2_557 ? C2 H2 0.9300 . ? C7 O3 1.250(14) 1_455 ? C7 C3 1.507(15) 2_556 ? 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 Ba1 O6 81.2(3) . . ? O3 Ba1 OW2 141.8(4) . . ? O6 Ba1 OW2 108.3(4) . . ? O3 Ba1 O11 71.3(3) . . ? O6 Ba1 O11 152.5(3) . . ? OW2 Ba1 O11 93.1(4) . . ? O3 Ba1 O4 148.2(3) . . ? O6 Ba1 O4 67.4(3) . . ? OW2 Ba1 O4 59.0(4) . . ? O11 Ba1 O4 140.1(3) . . ? O3 Ba1 O1 73.4(3) . . ? O6 Ba1 O1 110.0(3) . . ? OW2 Ba1 O1 68.5(4) . . ? O11 Ba1 O1 61.5(3) . . ? O4 Ba1 O1 121.3(3) . . ? O3 Ba1 O9 96.9(3) . . ? O6 Ba1 O9 78.6(3) . . ? OW2 Ba1 O9 121.1(4) . . ? O11 Ba1 O9 105.3(3) . . ? O4 Ba1 O9 72.7(3) . . ? O1 Ba1 O9 165.3(3) . . ? O3 Ba1 O10 69.4(3) . . ? O6 Ba1 O10 108.3(3) . . ? OW2 Ba1 O10 135.0(3) . . ? O11 Ba1 O10 63.3(3) . . ? O4 Ba1 O10 114.8(3) . . ? O1 Ba1 O10 120.4(3) . . ? O9 Ba1 O10 44.9(2) . . ? O3 Ba1 N1 74.2(3) . . ? O6 Ba1 N1 57.1(3) . . ? OW2 Ba1 N1 80.5(4) . . ? O11 Ba1 N1 112.3(3) . . ? O4 Ba1 N1 92.0(3) . . ? O1 Ba1 N1 53.5(3) . . ? O9 Ba1 N1 135.5(3) . . ? O10 Ba1 N1 142.7(3) . . ? O3 Ba1 O8 137.9(3) . . ? O6 Ba1 O8 126.5(3) . . ? OW2 Ba1 O8 65.9(4) . . ? O11 Ba1 O8 77.6(3) . . ? O4 Ba1 O8 65.4(3) . . ? O1 Ba1 O8 115.1(3) . . ? O9 Ba1 O8 64.6(3) . . ? O10 Ba1 O8 71.5(3) . . ? N1 Ba1 O8 145.7(3) . . ? O3 Ba1 C15 84.3(3) . . ? O6 Ba1 C15 94.8(3) . . ? OW2 Ba1 C15 129.8(4) . . ? O11 Ba1 C15 83.8(3) . . ? O4 Ba1 C15 93.0(3) . . ? O1 Ba1 C15 143.1(3) . . ? O9 Ba1 C15 22.3(3) . . ? O10 Ba1 C15 22.7(3) . . ? N1 Ba1 C15 146.4(3) . . ? O8 Ba1 C15 64.5(3) . . ? O3 Ba1 Ba2 131.03(19) . . ? O6 Ba1 Ba2 76.77(19) . . ? OW2 Ba1 Ba2 87.0(3) . . ? O11 Ba1 Ba2 122.6(2) . . ? O4 Ba1 Ba2 37.97(19) . . ? O1 Ba1 Ba2 155.5(3) . . ? O9 Ba1 Ba2 36.18(18) . . ? O10 Ba1 Ba2 76.88(18) . . ? N1 Ba1 Ba2 124.22(19) . . ? O8 Ba1 Ba2 50.47(19) . . ? C15 Ba1 Ba2 55.1(2) . . ? O3 Ba1 H1W2 125.7(15) . . ? O6 Ba1 H1W2 116(5) . . ? OW2 Ba1 H1W2 16.9(5) . . ? O11 Ba1 H1W2 81(3) . . ? O4 Ba1 H1W2 75.6(11) . . ? O1 Ba1 H1W2 52.3(17) . . ? O9 Ba1 H1W2 136(3) . . ? O10 Ba1 H1W2 134(5) . . ? N1 Ba1 H1W2 75(5) . . ? O8 Ba1 H1W2 74(4) . . ? C15 Ba1 H1W2 138(5) . . ? Ba2 Ba1 H1W2 103.3(14) . . ? O10 Ba2 O9 171.9(3) 1_455 . ? O10 Ba2 O7 94.9(3) 1_455 . ? O9 Ba2 O7 77.0(3) . . ? O10 Ba2 O4 108.0(3) 1_455 . ? O9 Ba2 O4 75.7(3) . . ? O7 Ba2 O4 118.0(3) . . ? O10 Ba2 O3 71.7(3) 1_455 1_455 ? O9 Ba2 O3 114.9(2) . 1_455 ? O7 Ba2 O3 148.5(3) . 1_455 ? O4 Ba2 O3 46.3(3) . 1_455 ? O10 Ba2 O12 77.5(3) 1_455 . ? O9 Ba2 O12 105.8(3) . . ? O7 Ba2 O12 110.0(3) . . ? O4 Ba2 O12 130.6(3) . . ? O3 Ba2 O12 95.1(3) 1_455 . ? O10 Ba2 OW1 121.7(3) 1_455 . ? O9 Ba2 OW1 66.3(3) . . ? O7 Ba2 OW1 140.3(3) . . ? O4 Ba2 OW1 67.8(3) . . ? O3 Ba2 OW1 66.2(3) 1_455 . ? O12 Ba2 OW1 68.3(3) . . ? O10 Ba2 N2 83.3(3) 1_455 . ? O9 Ba2 N2 92.6(3) . . ? O7 Ba2 N2 54.8(3) . . ? O4 Ba2 N2 167.8(3) . . ? O3 Ba2 N2 145.2(3) 1_455 . ? O12 Ba2 N2 55.2(3) . . ? OW1 Ba2 N2 110.7(3) . . ? O10 Ba2 C7 92.3(3) 1_455 . ? O9 Ba2 C7 93.3(3) . . ? O7 Ba2 C7 138.7(3) . . ? O4 Ba2 C7 23.4(3) . . ? O3 Ba2 C7 23.5(3) 1_455 . ? O12 Ba2 C7 111.2(3) . . ? OW1 Ba2 C7 60.9(3) . . ? N2 Ba2 C7 166.4(3) . . ? O10 Ba2 Ba1 142.62(19) 1_455 . ? O9 Ba2 Ba1 38.73(19) . . ? O7 Ba2 Ba1 92.1(2) . . ? O4 Ba2 Ba1 38.5(2) . . ? O3 Ba2 Ba1 83.47(18) 1_455 . ? O12 Ba2 Ba1 133.5(2) . . ? OW1 Ba2 Ba1 68.8(2) . . ? N2 Ba2 Ba1 129.30(19) . . ? C7 Ba2 Ba1 59.9(2) . . ? O10 Ba2 Ba1 38.32(19) 1_455 1_455 ? O9 Ba2 Ba1 146.66(18) . 1_455 ? O7 Ba2 Ba1 121.6(2) . 1_455 ? O4 Ba2 Ba1 71.1(2) . 1_455 ? O3 Ba2 Ba1 34.90(19) 1_455 1_455 ? O12 Ba2 Ba1 93.8(2) . 1_455 ? OW1 Ba2 Ba1 97.8(2) . 1_455 ? N2 Ba2 Ba1 120.77(19) . 1_455 ? C7 Ba2 Ba1 54.0(2) . 1_455 ? Ba1 Ba2 Ba1 109.02(5) . 1_455 ? C10 C11 C12 118.4(9) . 2_547 ? C10 C11 C15 121.0(9) . . ? C12 C11 C15 120.6(10) 2_547 . ? Ba2 OW1 H1W1 127(10) . . ? Ba2 OW1 H2W1 107(10) . . ? H1W1 OW1 H2W1 102(10) . . ? C8 O5 H5 109.5 . . ? C7 O3 Ba1 131.9(8) 1_655 . ? C7 O3 Ba2 91.8(7) 1_655 1_655 ? Ba1 O3 Ba2 108.9(3) . 1_655 ? C14 O8 Ba1 131.4(9) . . ? C14 O7 Ba2 132.7(7) 2_557 . ? C15 O10 Ba2 137.5(8) . 1_655 ? C15 O10 Ba1 93.3(7) . . ? Ba2 O10 Ba1 107.0(3) 1_655 . ? C15 O9 Ba2 136.3(8) . . ? C15 O9 Ba1 95.8(7) . . ? Ba2 O9 Ba1 105.1(3) . . ? C8 O6 Ba1 127.4(8) . . ? C7 O4 Ba2 92.3(7) . . ? C7 O4 Ba1 147.2(8) . . ? Ba2 O4 Ba1 103.5(3) . . ? C11 C10 C9 120.4(9) . 2_547 ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 2_547 . ? C6 O1 Ba1 131.0(8) . . ? C3 C4 C5 119.3(12) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C1 N1 C5 117.2(11) . . ? C1 N1 Ba1 123.6(7) . . ? C5 N1 Ba1 119.0(8) . . ? N1 C5 C4 123.0(13) . . ? N1 C5 C8 117.2(12) . . ? C4 C5 C8 119.6(12) . . ? C16 O12 Ba2 129.8(8) . . ? C6 O2 H6 109.5 . . ? Ba1 OW2 H1W2 68(5) . . ? Ba1 OW2 H2W2 164(8) . . ? H1W2 OW2 H2W2 103(10) . . ? C16 O11 Ba1 140.1(9) 1_665 . ? C2 C3 C4 117.6(12) . . ? C2 C3 C7 122.3(11) . 2_556 ? C4 C3 C7 120.1(10) . 2_556 ? C11 C12 C13 118.3(10) 2_547 . ? C11 C12 H12 120.8 2_547 . ? C13 C12 H12 120.8 . . ? N1 C1 C2 123.6(11) . . ? N1 C1 C6 117.8(10) . . ? C2 C1 C6 118.3(10) . . ? O5 C8 O6 125.3(12) . . ? O5 C8 C5 115.9(11) . . ? O6 C8 C5 118.8(11) . . ? O11 C16 O12 125.8(11) 1_445 . ? O11 C16 C13 118.4(12) 1_445 . ? O12 C16 C13 115.7(11) . . ? N2 C9 C10 122.2(9) . 2_547 ? N2 C9 C14 117.1(10) . 2_557 ? C10 C9 C14 120.7(10) 2_547 2_557 ? O2 C6 O1 125.3(11) . . ? O2 C6 C1 121.6(11) . . ? O1 C6 C1 112.8(10) . . ? C13 N2 C9 118.6(9) . . ? C13 N2 Ba2 120.7(7) . . ? C9 N2 Ba2 120.7(7) . . ? O8 C14 O7 124.7(11) . 2_557 ? O8 C14 C9 120.7(10) . 2_557 ? O7 C14 C9 114.6(10) 2_557 2_557 ? N2 C13 C12 122.0(10) . . ? N2 C13 C16 118.5(10) . . ? C12 C13 C16 119.5(11) . . ? C3 C2 C1 119.2(12) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? O9 C15 O10 125.3(11) . . ? O9 C15 C11 117.2(10) . . ? O10 C15 C11 117.4(10) . . ? O9 C15 Ba1 61.9(6) . . ? O10 C15 Ba1 64.0(6) . . ? C11 C15 Ba1 174.9(8) . . ? O4 C7 O3 125.9(11) . 1_455 ? O4 C7 C3 118.3(10) . 2_556 ? O3 C7 C3 115.8(10) 1_455 2_556 ? O4 C7 Ba2 64.3(6) . . ? O3 C7 Ba2 64.6(6) 1_455 . ? C3 C7 Ba2 158.8(7) 2_556 . ? 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 O3 Ba1 Ba2 O10 -169.9(4) . . . 1_455 ? O6 Ba1 Ba2 O10 -104.3(4) . . . 1_455 ? OW2 Ba1 Ba2 O10 5.4(5) . . . 1_455 ? O11 Ba1 Ba2 O10 97.2(4) . . . 1_455 ? O4 Ba1 Ba2 O10 -34.2(5) . . . 1_455 ? O1 Ba1 Ba2 O10 5.2(6) . . . 1_455 ? O9 Ba1 Ba2 O10 167.0(5) . . . 1_455 ? O10 Ba1 Ba2 O10 143.0(5) . . . 1_455 ? N1 Ba1 Ba2 O10 -70.9(4) . . . 1_455 ? O8 Ba1 Ba2 O10 66.3(4) . . . 1_455 ? C15 Ba1 Ba2 O10 150.2(4) . . . 1_455 ? O3 Ba1 Ba2 O9 23.1(4) . . . . ? O6 Ba1 Ba2 O9 88.7(4) . . . . ? OW2 Ba1 Ba2 O9 -161.6(4) . . . . ? O11 Ba1 Ba2 O9 -69.8(4) . . . . ? O4 Ba1 Ba2 O9 158.8(4) . . . . ? O1 Ba1 Ba2 O9 -161.8(6) . . . . ? O10 Ba1 Ba2 O9 -24.0(4) . . . . ? N1 Ba1 Ba2 O9 122.1(4) . . . . ? O8 Ba1 Ba2 O9 -100.8(4) . . . . ? C15 Ba1 Ba2 O9 -16.8(4) . . . . ? O3 Ba1 Ba2 O7 89.2(3) . . . . ? O6 Ba1 Ba2 O7 154.8(3) . . . . ? OW2 Ba1 Ba2 O7 -95.5(4) . . . . ? O11 Ba1 Ba2 O7 -3.7(3) . . . . ? O4 Ba1 Ba2 O7 -135.1(4) . . . . ? O1 Ba1 Ba2 O7 -95.7(5) . . . . ? O9 Ba1 Ba2 O7 66.1(4) . . . . ? O10 Ba1 Ba2 O7 42.1(3) . . . . ? N1 Ba1 Ba2 O7 -171.8(3) . . . . ? O8 Ba1 Ba2 O7 -34.7(3) . . . . ? C15 Ba1 Ba2 O7 49.3(3) . . . . ? O3 Ba1 Ba2 O4 -135.7(4) . . . . ? O6 Ba1 Ba2 O4 -70.1(4) . . . . ? OW2 Ba1 Ba2 O4 39.6(4) . . . . ? O11 Ba1 Ba2 O4 131.4(4) . . . . ? O1 Ba1 Ba2 O4 39.4(6) . . . . ? O9 Ba1 Ba2 O4 -158.8(4) . . . . ? O10 Ba1 Ba2 O4 177.2(4) . . . . ? N1 Ba1 Ba2 O4 -36.7(4) . . . . ? O8 Ba1 Ba2 O4 100.5(4) . . . . ? C15 Ba1 Ba2 O4 -175.6(4) . . . . ? O3 Ba1 Ba2 O3 -122.1(4) . . . 1_455 ? O6 Ba1 Ba2 O3 -56.4(3) . . . 1_455 ? OW2 Ba1 Ba2 O3 53.2(3) . . . 1_455 ? O11 Ba1 Ba2 O3 145.0(3) . . . 1_455 ? O4 Ba1 Ba2 O3 13.6(4) . . . 1_455 ? O1 Ba1 Ba2 O3 53.0(5) . . . 1_455 ? O9 Ba1 Ba2 O3 -145.2(4) . . . 1_455 ? O10 Ba1 Ba2 O3 -169.2(3) . . . 1_455 ? N1 Ba1 Ba2 O3 -23.1(3) . . . 1_455 ? O8 Ba1 Ba2 O3 114.1(3) . . . 1_455 ? C15 Ba1 Ba2 O3 -162.0(3) . . . 1_455 ? O3 Ba1 Ba2 O12 -31.2(4) . . . . ? O6 Ba1 Ba2 O12 34.4(4) . . . . ? OW2 Ba1 Ba2 O12 144.1(4) . . . . ? O11 Ba1 Ba2 O12 -124.1(4) . . . . ? O4 Ba1 Ba2 O12 104.5(4) . . . . ? O1 Ba1 Ba2 O12 143.8(5) . . . . ? O9 Ba1 Ba2 O12 -54.3(4) . . . . ? O10 Ba1 Ba2 O12 -78.3(3) . . . . ? N1 Ba1 Ba2 O12 67.8(4) . . . . ? O8 Ba1 Ba2 O12 -155.1(4) . . . . ? C15 Ba1 Ba2 O12 -71.1(4) . . . . ? O3 Ba1 Ba2 OW1 -55.1(3) . . . . ? O6 Ba1 Ba2 OW1 10.6(3) . . . . ? OW2 Ba1 Ba2 OW1 120.2(4) . . . . ? O11 Ba1 Ba2 OW1 -148.0(3) . . . . ? O4 Ba1 Ba2 OW1 80.6(4) . . . . ? O1 Ba1 Ba2 OW1 120.0(5) . . . . ? O9 Ba1 Ba2 OW1 -78.1(4) . . . . ? O10 Ba1 Ba2 OW1 -102.2(3) . . . . ? N1 Ba1 Ba2 OW1 43.9(3) . . . . ? O8 Ba1 Ba2 OW1 -178.9(3) . . . . ? C15 Ba1 Ba2 OW1 -95.0(3) . . . . ? O3 Ba1 Ba2 N2 44.9(3) . . . . ? O6 Ba1 Ba2 N2 110.5(3) . . . . ? OW2 Ba1 Ba2 N2 -139.8(4) . . . . ? O11 Ba1 Ba2 N2 -48.0(4) . . . . ? O4 Ba1 Ba2 N2 -179.4(4) . . . . ? O1 Ba1 Ba2 N2 -140.0(5) . . . . ? O9 Ba1 Ba2 N2 21.8(4) . . . . ? O10 Ba1 Ba2 N2 -2.2(3) . . . . ? N1 Ba1 Ba2 N2 143.9(3) . . . . ? O8 Ba1 Ba2 N2 -78.9(4) . . . . ? C15 Ba1 Ba2 N2 5.0(3) . . . . ? O3 Ba1 Ba2 C7 -122.8(3) . . . . ? O6 Ba1 Ba2 C7 -57.2(3) . . . . ? OW2 Ba1 Ba2 C7 52.4(4) . . . . ? O11 Ba1 Ba2 C7 144.2(3) . . . . ? O4 Ba1 Ba2 C7 12.8(4) . . . . ? O1 Ba1 Ba2 C7 52.2(5) . . . . ? O9 Ba1 Ba2 C7 -145.9(4) . . . . ? O10 Ba1 Ba2 C7 -169.9(3) . . . . ? N1 Ba1 Ba2 C7 -23.9(3) . . . . ? O8 Ba1 Ba2 C7 113.3(3) . . . . ? C15 Ba1 Ba2 C7 -162.7(3) . . . . ? O3 Ba1 Ba2 Ba1 -146.2(2) . . . 1_455 ? O6 Ba1 Ba2 Ba1 -80.6(2) . . . 1_455 ? OW2 Ba1 Ba2 Ba1 29.1(3) . . . 1_455 ? O11 Ba1 Ba2 Ba1 120.9(3) . . . 1_455 ? O4 Ba1 Ba2 Ba1 -10.5(3) . . . 1_455 ? O1 Ba1 Ba2 Ba1 28.9(5) . . . 1_455 ? O9 Ba1 Ba2 Ba1 -169.3(3) . . . 1_455 ? O10 Ba1 Ba2 Ba1 166.7(2) . . . 1_455 ? N1 Ba1 Ba2 Ba1 -47.2(2) . . . 1_455 ? O8 Ba1 Ba2 Ba1 90.0(3) . . . 1_455 ? C15 Ba1 Ba2 Ba1 173.9(2) . . . 1_455 ? O6 Ba1 O3 C7 122.8(10) . . . 1_655 ? OW2 Ba1 O3 C7 14.2(12) . . . 1_655 ? O11 Ba1 O3 C7 -56.1(10) . . . 1_655 ? O4 Ba1 O3 C7 132.0(10) . . . 1_655 ? O1 Ba1 O3 C7 8.7(10) . . . 1_655 ? O9 Ba1 O3 C7 -160.0(10) . . . 1_655 ? O10 Ba1 O3 C7 -123.8(10) . . . 1_655 ? N1 Ba1 O3 C7 64.6(10) . . . 1_655 ? O8 Ba1 O3 C7 -100.6(10) . . . 1_655 ? C15 Ba1 O3 C7 -141.5(10) . . . 1_655 ? Ba2 Ba1 O3 C7 -173.4(9) . . . 1_655 ? O6 Ba1 O3 Ba2 -126.6(3) . . . 1_655 ? OW2 Ba1 O3 Ba2 124.8(5) . . . 1_655 ? O11 Ba1 O3 Ba2 54.5(3) . . . 1_655 ? O4 Ba1 O3 Ba2 -117.4(5) . . . 1_655 ? O1 Ba1 O3 Ba2 119.3(4) . . . 1_655 ? O9 Ba1 O3 Ba2 -49.4(3) . . . 1_655 ? O10 Ba1 O3 Ba2 -13.2(3) . . . 1_655 ? N1 Ba1 O3 Ba2 175.2(4) . . . 1_655 ? O8 Ba1 O3 Ba2 10.0(6) . . . 1_655 ? C15 Ba1 O3 Ba2 -30.9(3) . . . 1_655 ? Ba2 Ba1 O3 Ba2 -62.8(4) . . . 1_655 ? O3 Ba1 O8 C14 31.5(12) . . . . ? O6 Ba1 O8 C14 153.9(10) . . . . ? OW2 Ba1 O8 C14 -110.5(11) . . . . ? O11 Ba1 O8 C14 -11.3(10) . . . . ? O4 Ba1 O8 C14 -175.9(11) . . . . ? O1 Ba1 O8 C14 -61.2(11) . . . . ? O9 Ba1 O8 C14 102.5(11) . . . . ? O10 Ba1 O8 C14 54.4(10) . . . . ? N1 Ba1 O8 C14 -122.7(10) . . . . ? C15 Ba1 O8 C14 77.7(11) . . . . ? Ba2 Ba1 O8 C14 142.4(11) . . . . ? O10 Ba2 O7 C14 74.7(12) 1_455 . . 2_557 ? O9 Ba2 O7 C14 -106.1(12) . . . 2_557 ? O4 Ba2 O7 C14 -171.9(11) . . . 2_557 ? O3 Ba2 O7 C14 137.0(11) 1_455 . . 2_557 ? O12 Ba2 O7 C14 -3.8(12) . . . 2_557 ? OW1 Ba2 O7 C14 -83.5(12) . . . 2_557 ? N2 Ba2 O7 C14 -3.5(11) . . . 2_557 ? C7 Ba2 O7 C14 173.8(10) . . . 2_557 ? Ba1 Ba2 O7 C14 -142.0(11) . . . 2_557 ? Ba1 Ba2 O7 C14 104.0(11) 1_455 . . 2_557 ? O3 Ba1 O10 C15 -128.4(8) . . . . ? O6 Ba1 O10 C15 -55.6(8) . . . . ? OW2 Ba1 O10 C15 87.4(9) . . . . ? O11 Ba1 O10 C15 152.9(8) . . . . ? O4 Ba1 O10 C15 17.3(8) . . . . ? O1 Ba1 O10 C15 176.6(7) . . . . ? O9 Ba1 O10 C15 -4.5(7) . . . . ? N1 Ba1 O10 C15 -114.9(8) . . . . ? O8 Ba1 O10 C15 67.8(7) . . . . ? Ba2 Ba1 O10 C15 15.4(7) . . . . ? O3 Ba1 O10 Ba2 13.7(3) . . . 1_655 ? O6 Ba1 O10 Ba2 86.5(4) . . . 1_655 ? OW2 Ba1 O10 Ba2 -130.5(5) . . . 1_655 ? O11 Ba1 O10 Ba2 -65.0(3) . . . 1_655 ? O4 Ba1 O10 Ba2 159.4(3) . . . 1_655 ? O1 Ba1 O10 Ba2 -41.3(5) . . . 1_655 ? O9 Ba1 O10 Ba2 137.7(5) . . . 1_655 ? N1 Ba1 O10 Ba2 27.2(6) . . . 1_655 ? O8 Ba1 O10 Ba2 -150.1(4) . . . 1_655 ? C15 Ba1 O10 Ba2 142.1(9) . . . 1_655 ? Ba2 Ba1 O10 Ba2 157.6(3) . . . 1_655 ? O7 Ba2 O9 C15 5.4(11) . . . . ? O4 Ba2 O9 C15 129.3(12) . . . . ? O3 Ba2 O9 C15 154.6(11) 1_455 . . . ? O12 Ba2 O9 C15 -102.0(11) . . . . ? OW1 Ba2 O9 C15 -159.0(12) . . . . ? N2 Ba2 O9 C15 -47.5(11) . . . . ? C7 Ba2 O9 C15 144.8(11) . . . . ? Ba1 Ba2 O9 C15 115.8(13) . . . . ? Ba1 Ba2 O9 C15 134.4(10) 1_455 . . . ? O7 Ba2 O9 Ba1 -110.3(3) . . . . ? O4 Ba2 O9 Ba1 13.5(3) . . . . ? O3 Ba2 O9 Ba1 38.8(4) 1_455 . . . ? O12 Ba2 O9 Ba1 142.2(3) . . . . ? OW1 Ba2 O9 Ba1 85.2(3) . . . . ? N2 Ba2 O9 Ba1 -163.3(3) . . . . ? C7 Ba2 O9 Ba1 29.0(3) . . . . ? Ba1 Ba2 O9 Ba1 18.6(6) 1_455 . . . ? O3 Ba1 O9 C15 56.0(8) . . . . ? O6 Ba1 O9 C15 135.6(8) . . . . ? OW2 Ba1 O9 C15 -119.8(8) . . . . ? O11 Ba1 O9 C15 -16.4(8) . . . . ? O4 Ba1 O9 C15 -154.8(8) . . . . ? O1 Ba1 O9 C15 8.1(16) . . . . ? O10 Ba1 O9 C15 4.5(7) . . . . ? N1 Ba1 O9 C15 130.5(7) . . . . ? O8 Ba1 O9 C15 -84.3(8) . . . . ? Ba2 Ba1 O9 C15 -141.3(9) . . . . ? O3 Ba1 O9 Ba2 -162.7(3) . . . . ? O6 Ba1 O9 Ba2 -83.1(3) . . . . ? OW2 Ba1 O9 Ba2 21.6(5) . . . . ? O11 Ba1 O9 Ba2 124.9(3) . . . . ? O4 Ba1 O9 Ba2 -13.5(3) . . . . ? O1 Ba1 O9 Ba2 149.5(10) . . . . ? O10 Ba1 O9 Ba2 145.9(5) . . . . ? N1 Ba1 O9 Ba2 -88.2(4) . . . . ? O8 Ba1 O9 Ba2 57.0(3) . . . . ? C15 Ba1 O9 Ba2 141.3(9) . . . . ? O3 Ba1 O6 C8 -80.4(11) . . . . ? OW2 Ba1 O6 C8 61.4(11) . . . . ? O11 Ba1 O6 C8 -78.1(13) . . . . ? O4 Ba1 O6 C8 104.9(11) . . . . ? O1 Ba1 O6 C8 -11.7(11) . . . . ? O9 Ba1 O6 C8 -179.3(11) . . . . ? O10 Ba1 O6 C8 -145.2(10) . . . . ? N1 Ba1 O6 C8 -3.5(10) . . . . ? O8 Ba1 O6 C8 134.6(10) . . . . ? C15 Ba1 O6 C8 -163.9(11) . . . . ? Ba2 Ba1 O6 C8 143.7(11) . . . . ? O10 Ba2 O4 C7 -50.0(7) 1_455 . . . ? O9 Ba2 O4 C7 137.6(7) . . . . ? O7 Ba2 O4 C7 -155.9(7) . . . . ? O3 Ba2 O4 C7 -10.1(6) 1_455 . . . ? O12 Ba2 O4 C7 38.9(8) . . . . ? OW1 Ba2 O4 C7 67.7(7) . . . . ? N2 Ba2 O4 C7 153.2(11) . . . . ? Ba1 Ba2 O4 C7 151.1(8) . . . . ? Ba1 Ba2 O4 C7 -39.4(6) 1_455 . . . ? O10 Ba2 O4 Ba1 159.0(3) 1_455 . . . ? O9 Ba2 O4 Ba1 -13.5(3) . . . . ? O7 Ba2 O4 Ba1 53.0(4) . . . . ? O3 Ba2 O4 Ba1 -161.1(5) 1_455 . . . ? O12 Ba2 O4 Ba1 -112.2(4) . . . . ? OW1 Ba2 O4 Ba1 -83.4(3) . . . . ? N2 Ba2 O4 Ba1 2.2(14) . . . . ? C7 Ba2 O4 Ba1 -151.1(8) . . . . ? Ba1 Ba2 O4 Ba1 169.5(3) 1_455 . . . ? O3 Ba1 O4 C7 -29.1(17) . . . . ? O6 Ba1 O4 C7 -19.2(14) . . . . ? OW2 Ba1 O4 C7 111.2(15) . . . . ? O11 Ba1 O4 C7 163.0(13) . . . . ? O1 Ba1 O4 C7 81.2(15) . . . . ? O9 Ba1 O4 C7 -103.8(15) . . . . ? O10 Ba1 O4 C7 -119.7(14) . . . . ? N1 Ba1 O4 C7 33.6(15) . . . . ? O8 Ba1 O4 C7 -173.2(15) . . . . ? C15 Ba1 O4 C7 -113.1(15) . . . . ? Ba2 Ba1 O4 C7 -116.7(16) . . . . ? O3 Ba1 O4 Ba2 87.7(5) . . . . ? O6 Ba1 O4 Ba2 97.5(3) . . . . ? OW2 Ba1 O4 Ba2 -132.1(5) . . . . ? O11 Ba1 O4 Ba2 -80.3(5) . . . . ? O1 Ba1 O4 Ba2 -162.1(3) . . . . ? O9 Ba1 O4 Ba2 12.9(3) . . . . ? O10 Ba1 O4 Ba2 -3.0(4) . . . . ? N1 Ba1 O4 Ba2 150.4(3) . . . . ? O8 Ba1 O4 Ba2 -56.5(3) . . . . ? C15 Ba1 O4 Ba2 3.6(3) . . . . ? C12 C11 C10 C9 2.0(17) 2_547 . . 2_547 ? C15 C11 C10 C9 180.0(11) . . . 2_547 ? O3 Ba1 O1 C6 92.9(12) . . . . ? O6 Ba1 O1 C6 19.0(13) . . . . ? OW2 Ba1 O1 C6 -83.5(12) . . . . ? O11 Ba1 O1 C6 170.2(13) . . . . ? O4 Ba1 O1 C6 -56.1(13) . . . . ? O9 Ba1 O1 C6 143.1(12) . . . . ? O10 Ba1 O1 C6 146.0(11) . . . . ? N1 Ba1 O1 C6 10.5(11) . . . . ? O8 Ba1 O1 C6 -131.5(12) . . . . ? C15 Ba1 O1 C6 148.2(11) . . . . ? Ba2 Ba1 O1 C6 -83.3(13) . . . . ? O3 Ba1 N1 C1 -89.6(9) . . . . ? O6 Ba1 N1 C1 -179.3(10) . . . . ? OW2 Ba1 N1 C1 61.4(9) . . . . ? O11 Ba1 N1 C1 -28.1(10) . . . . ? O4 Ba1 N1 C1 119.5(9) . . . . ? O1 Ba1 N1 C1 -8.9(9) . . . . ? O9 Ba1 N1 C1 -173.4(8) . . . . ? O10 Ba1 N1 C1 -102.8(10) . . . . ? O8 Ba1 N1 C1 72.8(10) . . . . ? C15 Ba1 N1 C1 -142.0(9) . . . . ? Ba2 Ba1 N1 C1 141.1(8) . . . . ? O3 Ba1 N1 C5 95.6(10) . . . . ? O6 Ba1 N1 C5 6.0(9) . . . . ? OW2 Ba1 N1 C5 -113.3(10) . . . . ? O11 Ba1 N1 C5 157.2(9) . . . . ? O4 Ba1 N1 C5 -55.2(9) . . . . ? O1 Ba1 N1 C5 176.4(11) . . . . ? O9 Ba1 N1 C5 11.9(11) . . . . ? O10 Ba1 N1 C5 82.5(10) . . . . ? O8 Ba1 N1 C5 -102.0(10) . . . . ? C15 Ba1 N1 C5 43.3(12) . . . . ? Ba2 Ba1 N1 C5 -33.7(10) . . . . ? C1 N1 C5 C4 1.1(19) . . . . ? Ba1 N1 C5 C4 176.2(10) . . . . ? C1 N1 C5 C8 176.7(11) . . . . ? Ba1 N1 C5 C8 -8.2(15) . . . . ? C3 C4 C5 N1 0(2) . . . . ? C3 C4 C5 C8 -175.2(11) . . . . ? O10 Ba2 O12 C16 -89.3(12) 1_455 . . . ? O9 Ba2 O12 C16 83.1(12) . . . . ? O7 Ba2 O12 C16 1.5(13) . . . . ? O4 Ba2 O12 C16 167.6(11) . . . . ? O3 Ba2 O12 C16 -159.2(12) 1_455 . . . ? OW1 Ba2 O12 C16 138.9(13) . . . . ? N2 Ba2 O12 C16 1.1(11) . . . . ? C7 Ba2 O12 C16 -176.9(12) . . . . ? Ba1 Ba2 O12 C16 115.0(11) . . . . ? Ba1 Ba2 O12 C16 -124.2(12) 1_455 . . . ? O3 Ba1 O11 C16 111.7(14) . . . 1_665 ? O6 Ba1 O11 C16 109.4(14) . . . 1_665 ? OW2 Ba1 O11 C16 -32.6(15) . . . 1_665 ? O4 Ba1 O11 C16 -74.9(15) . . . 1_665 ? O1 Ba1 O11 C16 30.9(14) . . . 1_665 ? O9 Ba1 O11 C16 -156.0(14) . . . 1_665 ? O10 Ba1 O11 C16 -172.4(15) . . . 1_665 ? N1 Ba1 O11 C16 48.4(15) . . . 1_665 ? O8 Ba1 O11 C16 -97.0(14) . . . 1_665 ? C15 Ba1 O11 C16 -162.2(14) . . . 1_665 ? Ba2 Ba1 O11 C16 -121.0(14) . . . 1_665 ? C5 C4 C3 C2 -0.2(18) . . . . ? C5 C4 C3 C7 177.9(11) . . . 2_556 ? C5 N1 C1 C2 -2.7(18) . . . . ? Ba1 N1 C1 C2 -177.5(9) . . . . ? C5 N1 C1 C6 -176.6(11) . . . . ? Ba1 N1 C1 C6 8.5(14) . . . . ? Ba1 O6 C8 O5 -176.8(10) . . . . ? Ba1 O6 C8 C5 1.1(17) . . . . ? N1 C5 C8 O5 -176.8(12) . . . . ? C4 C5 C8 O5 -1.1(19) . . . . ? N1 C5 C8 O6 5.1(19) . . . . ? C4 C5 C8 O6 -179.1(12) . . . . ? Ba2 O12 C16 O11 177.2(10) . . . 1_445 ? Ba2 O12 C16 C13 -1.7(18) . . . . ? Ba1 O1 C6 O2 175.8(10) . . . . ? Ba1 O1 C6 C1 -10.6(17) . . . . ? N1 C1 C6 O2 174.4(12) . . . . ? C2 C1 C6 O2 0.1(19) . . . . ? N1 C1 C6 O1 0.5(17) . . . . ? C2 C1 C6 O1 -173.8(12) . . . . ? C10 C9 N2 C13 2.4(17) 2_547 . . . ? C14 C9 N2 C13 -178.6(10) 2_557 . . . ? C10 C9 N2 Ba2 -178.5(8) 2_547 . . . ? C14 C9 N2 Ba2 0.4(14) 2_557 . . . ? O10 Ba2 N2 C13 79.3(9) 1_455 . . . ? O9 Ba2 N2 C13 -107.7(9) . . . . ? O7 Ba2 N2 C13 -179.9(10) . . . . ? O4 Ba2 N2 C13 -122.9(13) . . . . ? O3 Ba2 N2 C13 35.7(11) 1_455 . . . ? O12 Ba2 N2 C13 -0.2(8) . . . . ? OW1 Ba2 N2 C13 -42.1(9) . . . . ? C7 Ba2 N2 C13 7.7(18) . . . . ? Ba1 Ba2 N2 C13 -121.2(8) . . . . ? Ba1 Ba2 N2 C13 71.1(9) 1_455 . . . ? O10 Ba2 N2 C9 -99.8(9) 1_455 . . . ? O9 Ba2 N2 C9 73.2(9) . . . . ? O7 Ba2 N2 C9 1.1(8) . . . . ? O4 Ba2 N2 C9 58.0(17) . . . . ? O3 Ba2 N2 C9 -143.3(8) 1_455 . . . ? O12 Ba2 N2 C9 -179.3(10) . . . . ? OW1 Ba2 N2 C9 138.8(8) . . . . ? C7 Ba2 N2 C9 -171.3(10) . . . . ? Ba1 Ba2 N2 C9 59.8(9) . . . . ? Ba1 Ba2 N2 C9 -108.0(8) 1_455 . . . ? Ba1 O8 C14 O7 -111.5(13) . . . 2_557 ? Ba1 O8 C14 C9 69.7(15) . . . 2_557 ? C9 N2 C13 C12 0.0(17) . . . . ? Ba2 N2 C13 C12 -179.1(8) . . . . ? C9 N2 C13 C16 178.7(11) . . . . ? Ba2 N2 C13 C16 -0.4(14) . . . . ? C11 C12 C13 N2 -3.3(17) 2_547 . . . ? C11 C12 C13 C16 178.0(11) 2_547 . . . ? O11 C16 C13 N2 -177.7(12) 1_445 . . . ? O12 C16 C13 N2 1.3(18) . . . . ? O11 C16 C13 C12 1.0(19) 1_445 . . . ? O12 C16 C13 C12 180.0(12) . . . . ? C4 C3 C2 C1 -1.2(19) . . . . ? C7 C3 C2 C1 -179.3(11) 2_556 . . . ? N1 C1 C2 C3 3(2) . . . . ? C6 C1 C2 C3 176.8(12) . . . . ? Ba2 O9 C15 O10 -128.2(12) . . . . ? Ba1 O9 C15 O10 -9.1(14) . . . . ? Ba2 O9 C15 C11 55.2(16) . . . . ? Ba1 O9 C15 C11 174.3(9) . . . . ? Ba2 O9 C15 Ba1 -119.1(11) . . . . ? Ba2 O10 C15 O9 -110.7(13) 1_655 . . . ? Ba1 O10 C15 O9 9.0(14) . . . . ? Ba2 O10 C15 C11 65.8(16) 1_655 . . . ? Ba1 O10 C15 C11 -174.5(9) . . . . ? Ba2 O10 C15 Ba1 -119.7(11) 1_655 . . . ? C10 C11 C15 O9 38.0(17) . . . . ? C12 C11 C15 O9 -144.0(12) 2_547 . . . ? C10 C11 C15 O10 -138.8(12) . . . . ? C12 C11 C15 O10 39.2(17) 2_547 . . . ? O3 Ba1 C15 O9 -124.2(8) . . . . ? O6 Ba1 C15 O9 -43.5(8) . . . . ? OW2 Ba1 C15 O9 75.2(9) . . . . ? O11 Ba1 C15 O9 164.1(8) . . . . ? O4 Ba1 C15 O9 24.0(8) . . . . ? O1 Ba1 C15 O9 -176.6(7) . . . . ? O10 Ba1 C15 O9 -171.7(13) . . . . ? N1 Ba1 C15 O9 -74.2(10) . . . . ? O8 Ba1 C15 O9 84.9(8) . . . . ? Ba2 Ba1 C15 O9 26.7(7) . . . . ? O3 Ba1 C15 O10 47.5(7) . . . . ? O6 Ba1 C15 O10 128.2(7) . . . . ? OW2 Ba1 C15 O10 -113.1(8) . . . . ? O11 Ba1 C15 O10 -24.2(7) . . . . ? O4 Ba1 C15 O10 -164.3(7) . . . . ? O1 Ba1 C15 O10 -4.9(10) . . . . ? O9 Ba1 C15 O10 171.7(13) . . . . ? N1 Ba1 C15 O10 97.5(8) . . . . ? O8 Ba1 C15 O10 -103.4(8) . . . . ? Ba2 Ba1 C15 O10 -161.6(8) . . . . ? Ba2 O4 C7 O3 20.6(12) . . . 1_455 ? Ba1 O4 C7 O3 140.2(12) . . . 1_455 ? Ba2 O4 C7 C3 -156.3(9) . . . 2_556 ? Ba1 O4 C7 C3 -37(2) . . . 2_556 ? Ba1 O4 C7 Ba2 119.6(14) . . . . ? O10 Ba2 C7 O4 133.2(7) 1_455 . . . ? O9 Ba2 C7 O4 -40.9(7) . . . . ? O7 Ba2 C7 O4 33.1(9) . . . . ? O3 Ba2 C7 O4 161.6(11) 1_455 . . . ? O12 Ba2 C7 O4 -149.3(7) . . . . ? OW1 Ba2 C7 O4 -101.4(7) . . . . ? N2 Ba2 C7 O4 -156.3(11) . . . . ? Ba1 Ba2 C7 O4 -20.4(6) . . . . ? Ba1 Ba2 C7 O4 132.0(8) 1_455 . . . ? O10 Ba2 C7 O3 -28.4(7) 1_455 . . 1_455 ? O9 Ba2 C7 O3 157.5(7) . . . 1_455 ? O7 Ba2 C7 O3 -128.4(7) . . . 1_455 ? O4 Ba2 C7 O3 -161.6(11) . . . 1_455 ? O12 Ba2 C7 O3 49.2(8) . . . 1_455 ? OW1 Ba2 C7 O3 97.0(7) . . . 1_455 ? N2 Ba2 C7 O3 42.2(15) . . . 1_455 ? Ba1 Ba2 C7 O3 178.0(7) . . . 1_455 ? Ba1 Ba2 C7 O3 -29.6(6) 1_455 . . 1_455 ? O10 Ba2 C7 C3 -125(2) 1_455 . . 2_556 ? O9 Ba2 C7 C3 61(2) . . . 2_556 ? O7 Ba2 C7 C3 135.3(19) . . . 2_556 ? O4 Ba2 C7 C3 102(2) . . . 2_556 ? O3 Ba2 C7 C3 -96(2) 1_455 . . 2_556 ? O12 Ba2 C7 C3 -47(2) . . . 2_556 ? OW1 Ba2 C7 C3 0.8(19) . . . 2_556 ? N2 Ba2 C7 C3 -54(3) . . . 2_556 ? Ba1 Ba2 C7 C3 82(2) . . . 2_556 ? Ba1 Ba2 C7 C3 -126(2) 1_455 . . 2_556 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.730 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.554 #===END of CIF for Complex 9 ===================== data_complex10 _database_code_depnum_ccdc_archive 'CCDC 697868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 Dy N O10' _chemical_formula_weight 442.67 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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.822(6) _cell_length_b 7.240(5) _cell_length_c 13.466(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.142(7) _cell_angle_gamma 90.00 _cell_volume 1146.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description 'rectangular parallelopipeds' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 6.577 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4387 _exptl_absorpt_correction_T_max 0.5058 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7154 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2788 _reflns_number_gt 2319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0489P)^2^+4.3966P] 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 2788 _refine_ls_number_parameters 177 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.119 _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 0.78394(4) 0.21528(7) 0.70526(4) 0.01278(18) Uani 1 1 d . . . OW1 O 0.8764(8) 0.3706(14) 0.8524(7) 0.0182(18) Uani 1 1 d D . . O3 O 0.9686(9) 0.0724(14) 0.7471(7) 0.018(4) Uani 1 1 d . . . O5 O 0.7504(7) -0.3882(13) 1.1512(6) 0.0156(17) Uani 1 1 d . . . O2 O 0.5059(7) 0.0303(13) 0.8818(6) 0.0194(17) Uani 1 1 d . . . C6 C 0.5973(12) 0.060(2) 0.8472(10) 0.023(4) Uani 1 1 d D . . OW2 O 0.6955(7) 0.5186(14) 0.7224(7) 0.0139(18) Uani 1 1 d D . . O4 O 1.0906(7) -0.0853(11) 0.8560(5) 0.0162(15) Uani 1 1 d . . . O1 O 0.6111(8) 0.1668(13) 0.7727(6) 0.018 Uani 1 1 d . . . C8 C 0.9919(9) -0.0222(17) 0.8258(8) 0.019(2) Uani 1 1 d . . . N1 N 0.7973(13) 0.007(2) 0.8514(10) 0.022(6) Uani 1 1 d . . . OW4 O 0.6367(8) 0.2441(14) 0.5678(7) 0.0195(19) Uani 1 1 d D . . C7 C 0.7997(13) -0.406(2) 1.0737(10) 0.021(4) Uani 1 1 d . . . C2 C 0.7032(10) -0.1562(19) 0.9718(8) 0.015(2) Uani 1 1 d . . . H2 H 0.6378 -0.1754 1.0031 0.018 Uiso 1 1 calc R . . OW3 O 0.5789(9) 0.4847(14) 0.9113(7) 0.022(2) Uani 1 1 d D . . C1 C 0.7042(10) -0.0318(16) 0.8943(9) 0.015(2) Uani 1 1 d D . . C5 C 0.8935(16) -0.078(2) 0.8818(12) 0.035(6) Uani 1 1 d . . . C4 C 0.9017(10) -0.2091(17) 0.9565(8) 0.014(2) Uani 1 1 d . . . H4 H 0.9705 -0.2675 0.9762 0.017 Uiso 1 1 calc R . . C3 C 0.8036(10) -0.2524(17) 1.0019(9) 0.013(2) Uani 1 1 d . . . O6 O 0.8457(7) -0.5599(11) 1.0527(6) 0.0189(16) Uani 1 1 d . . . H2W1 H 0.866(16) 0.39(3) 0.910(5) 0.04(5) Uiso 1 1 d D . . H1W1 H 0.924(8) 0.450(13) 0.845(9) 0.00(3) Uiso 1 1 d D . . H1W4 H 0.586(9) 0.321(16) 0.567(12) 0.03(5) Uiso 1 1 d D . . H2W4 H 0.614(12) 0.168(17) 0.525(10) 0.03(5) Uiso 1 1 d D . . H2W2 H 0.634(8) 0.53(3) 0.689(13) 0.05(6) Uiso 1 1 d D . . H1W2 H 0.722(16) 0.610(17) 0.697(14) 0.04(6) Uiso 1 1 d D . . H2W3 H 0.517(5) 0.49(2) 0.878(8) 0.00(3) Uiso 1 1 d D . . H1W3 H 0.615(10) 0.49(2) 0.863(6) 0.04(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0184(3) 0.0109(3) 0.0097(3) 0.00026(19) 0.00240(18) 0.0001(2) OW1 0.016(4) 0.022(5) 0.017(4) 0.001(4) 0.005(3) -0.006(4) O3 0.021(4) 0.015(4) 0.021(4) 0.006(3) 0.004(3) 0.003(3) O5 0.018(4) 0.018(5) 0.011(4) -0.005(3) 0.004(3) -0.007(3) O2 0.028(4) 0.018(5) 0.012(4) 0.004(3) 0.002(3) -0.004(3) C6 0.034(5) 0.021(5) 0.015(5) 0.006(4) 0.003(4) 0.002(4) OW2 0.010(4) 0.013(5) 0.018(4) 0.005(4) 0.002(3) -0.004(4) O4 0.023(4) 0.015(4) 0.011(3) 0.003(3) 0.002(3) -0.004(3) O1 0.022(6) 0.019(6) 0.015(6) 0.008(5) 0.006(5) -0.001(5) C8 0.031(5) 0.014(5) 0.011(5) 0.008(4) -0.002(4) -0.001(4) N1 0.032(4) 0.022(4) 0.011(4) 0.006(3) 0.004(3) 0.003(3) OW4 0.012(4) 0.023(5) 0.022(5) -0.006(4) -0.001(3) 0.002(4) C7 0.031(5) 0.022(5) 0.011(5) 0.004(4) 0.003(4) 0.002(4) C2 0.012(5) 0.025(6) 0.008(5) -0.006(5) 0.001(4) 0.000(5) OW3 0.027(5) 0.023(5) 0.017(4) -0.003(4) 0.002(4) 0.004(4) C1 0.013(5) 0.011(5) 0.021(6) 0.000(5) -0.004(4) -0.006(4) C5 0.047(6) 0.035(6) 0.023(6) 0.006(5) 0.005(5) 0.003(5) C4 0.016(5) 0.016(6) 0.010(5) -0.009(4) 0.005(4) -0.002(5) C3 0.009(5) 0.017(6) 0.015(5) -0.002(4) 0.006(4) 0.000(4) O6 0.027(4) 0.019(4) 0.012(4) -0.002(3) 0.005(3) 0.002(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 O4 2.286(8) 2_756 ? Dy1 O1 2.349(9) . ? Dy1 OW4 2.410(9) . ? Dy1 O3 2.427(10) . ? Dy1 OW1 2.434(9) . ? Dy1 OW2 2.453(10) . ? Dy1 N1 2.472(14) . ? Dy1 O5 2.496(9) 4 ? Dy1 O6 2.518(8) 4 ? Dy1 C7 2.872(14) 4 ? OW1 H2W1 0.81(9) . ? OW1 H1W1 0.82(10) . ? O3 C8 1.267(15) . ? O5 C7 1.256(16) . ? O5 Dy1 2.496(9) 4_556 ? O2 C6 1.241(16) . ? C6 O1 1.288(15) . ? C6 C1 1.508(14) . ? OW2 H2W2 0.82(15) . ? OW2 H1W2 0.82(11) . ? O4 C8 1.277(14) . ? O4 Dy1 2.286(8) 2_746 ? C8 C5 1.51(2) . ? N1 C5 1.32(2) . ? N1 C1 1.326(19) . ? OW4 H1W4 0.82(11) . ? OW4 H2W4 0.82(12) . ? C7 O6 1.283(17) . ? C7 C3 1.479(18) . ? C7 Dy1 2.872(14) 4_556 ? C2 C1 1.379(17) . ? C2 C3 1.398(17) . ? C2 H2 0.9300 . ? OW3 H2W3 0.82(8) . ? OW3 H1W3 0.82(10) . ? C5 C4 1.38(2) . ? C4 C3 1.403(16) . ? C4 H4 0.9300 . ? O6 Dy1 2.518(8) 4_556 ? 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 O1 149.2(3) 2_756 . ? O4 Dy1 OW4 96.4(3) 2_756 . ? O1 Dy1 OW4 73.9(3) . . ? O4 Dy1 O3 75.6(3) 2_756 . ? O1 Dy1 O3 130.1(3) . . ? OW4 Dy1 O3 140.6(3) . . ? O4 Dy1 OW1 75.5(3) 2_756 . ? O1 Dy1 OW1 95.0(3) . . ? OW4 Dy1 OW1 144.1(3) . . ? O3 Dy1 OW1 72.1(3) . . ? O4 Dy1 OW2 76.6(3) 2_756 . ? O1 Dy1 OW2 72.6(3) . . ? OW4 Dy1 OW2 73.4(3) . . ? O3 Dy1 OW2 137.8(3) . . ? OW1 Dy1 OW2 70.7(3) . . ? O4 Dy1 N1 133.2(4) 2_756 . ? O1 Dy1 N1 65.5(4) . . ? OW4 Dy1 N1 130.1(4) . . ? O3 Dy1 N1 64.9(4) . . ? OW1 Dy1 N1 69.5(4) . . ? OW2 Dy1 N1 117.6(4) . . ? O4 Dy1 O5 125.7(3) 2_756 4 ? O1 Dy1 O5 81.6(3) . 4 ? OW4 Dy1 O5 77.2(3) . 4 ? O3 Dy1 O5 77.0(3) . 4 ? OW1 Dy1 O5 136.0(3) . 4 ? OW2 Dy1 O5 145.1(3) . 4 ? N1 Dy1 O5 69.3(4) . 4 ? O4 Dy1 O6 74.5(3) 2_756 4 ? O1 Dy1 O6 126.0(3) . 4 ? OW4 Dy1 O6 70.2(3) . 4 ? O3 Dy1 O6 70.6(3) . 4 ? OW1 Dy1 O6 136.6(3) . 4 ? OW2 Dy1 O6 129.8(3) . 4 ? N1 Dy1 O6 112.2(4) . 4 ? O5 Dy1 O6 52.4(3) 4 4 ? O4 Dy1 C7 100.5(4) 2_756 4 ? O1 Dy1 C7 103.8(4) . 4 ? OW4 Dy1 C7 71.5(4) . 4 ? O3 Dy1 C7 72.3(4) . 4 ? OW1 Dy1 C7 144.0(4) . 4 ? OW2 Dy1 C7 144.2(4) . 4 ? N1 Dy1 C7 90.7(5) . 4 ? O5 Dy1 C7 25.9(3) 4 4 ? O6 Dy1 C7 26.5(3) 4 4 ? Dy1 OW1 H2W1 140(10) . . ? Dy1 OW1 H1W1 118(9) . . ? H2W1 OW1 H1W1 99(10) . . ? C8 O3 Dy1 122.3(8) . . ? C7 O5 Dy1 94.0(8) . 4_556 ? O2 C6 O1 125.9(12) . . ? O2 C6 C1 119.2(11) . . ? O1 C6 C1 114.9(12) . . ? Dy1 OW2 H2W2 113(10) . . ? Dy1 OW2 H1W2 120(10) . . ? H2W2 OW2 H1W2 93(10) . . ? C8 O4 Dy1 135.8(7) . 2_746 ? C6 O1 Dy1 125.3(8) . . ? O3 C8 O4 124.7(11) . . ? O3 C8 C5 116.9(11) . . ? O4 C8 C5 118.2(11) . . ? C5 N1 C1 119.8(14) . . ? C5 N1 Dy1 120.7(11) . . ? C1 N1 Dy1 119.3(10) . . ? Dy1 OW4 H1W4 123(10) . . ? Dy1 OW4 H2W4 129(10) . . ? H1W4 OW4 H2W4 105(14) . . ? O5 C7 O6 121.3(12) . . ? O5 C7 C3 121.0(13) . . ? O6 C7 C3 117.7(12) . . ? O5 C7 Dy1 60.1(7) . 4_556 ? O6 C7 Dy1 61.2(7) . 4_556 ? C3 C7 Dy1 176.9(10) . 4_556 ? C1 C2 C3 118.0(11) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? H2W3 OW3 H1W3 94(10) . . ? N1 C1 C2 122.8(11) . . ? N1 C1 C6 114.9(12) . . ? C2 C1 C6 122.2(11) . . ? N1 C5 C4 122.5(16) . . ? N1 C5 C8 114.1(13) . . ? C4 C5 C8 123.4(14) . . ? C5 C4 C3 118.3(13) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C2 C3 C4 118.5(11) . . ? C2 C3 C7 118.7(11) . . ? C4 C3 C7 122.6(12) . . ? C7 O6 Dy1 92.3(8) . 4_556 ? 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 O4 Dy1 O3 C8 146.8(10) 2_756 . . . ? O1 Dy1 O3 C8 -13.6(11) . . . . ? OW4 Dy1 O3 C8 -130.8(9) . . . . ? OW1 Dy1 O3 C8 67.7(9) . . . . ? OW2 Dy1 O3 C8 96.7(10) . . . . ? N1 Dy1 O3 C8 -7.5(9) . . . . ? O5 Dy1 O3 C8 -80.5(10) 4 . . . ? O6 Dy1 O3 C8 -134.9(10) 4 . . . ? C7 Dy1 O3 C8 -106.9(10) 4 . . . ? O2 C6 O1 Dy1 -178.1(10) . . . . ? C1 C6 O1 Dy1 2.2(17) . . . . ? O4 Dy1 O1 C6 -136.4(10) 2_756 . . . ? OW4 Dy1 O1 C6 148.4(11) . . . . ? O3 Dy1 O1 C6 4.4(13) . . . . ? OW1 Dy1 O1 C6 -66.4(11) . . . . ? OW2 Dy1 O1 C6 -134.3(11) . . . . ? N1 Dy1 O1 C6 -1.7(11) . . . . ? O5 Dy1 O1 C6 69.4(11) 4 . . . ? O6 Dy1 O1 C6 98.7(11) 4 . . . ? C7 Dy1 O1 C6 82.7(11) 4 . . . ? Dy1 O3 C8 O4 -173.0(8) . . . . ? Dy1 O3 C8 C5 12.7(16) . . . . ? Dy1 O4 C8 O3 -61.3(17) 2_746 . . . ? Dy1 O4 C8 C5 112.9(12) 2_746 . . . ? O4 Dy1 N1 C5 -34.6(16) 2_756 . . . ? O1 Dy1 N1 C5 175.5(15) . . . . ? OW4 Dy1 N1 C5 136.8(12) . . . . ? O3 Dy1 N1 C5 0.6(13) . . . . ? OW1 Dy1 N1 C5 -78.7(13) . . . . ? OW2 Dy1 N1 C5 -132.1(13) . . . . ? O5 Dy1 N1 C5 85.5(14) 4 . . . ? O6 Dy1 N1 C5 54.6(14) 4 . . . ? C7 Dy1 N1 C5 70.6(14) 4 . . . ? O4 Dy1 N1 C1 150.9(10) 2_756 . . . ? O1 Dy1 N1 C1 0.9(10) . . . . ? OW4 Dy1 N1 C1 -37.8(14) . . . . ? O3 Dy1 N1 C1 -174.0(13) . . . . ? OW1 Dy1 N1 C1 106.8(12) . . . . ? OW2 Dy1 N1 C1 53.3(13) . . . . ? O5 Dy1 N1 C1 -89.1(12) 4 . . . ? O6 Dy1 N1 C1 -120.0(11) 4 . . . ? C7 Dy1 N1 C1 -104.0(12) 4 . . . ? Dy1 O5 C7 O6 -1.4(14) 4_556 . . . ? Dy1 O5 C7 C3 176.7(12) 4_556 . . . ? C5 N1 C1 C2 1(2) . . . . ? Dy1 N1 C1 C2 175.6(9) . . . . ? C5 N1 C1 C6 -174.8(14) . . . . ? Dy1 N1 C1 C6 -0.2(16) . . . . ? C3 C2 C1 N1 -3.7(19) . . . . ? C3 C2 C1 C6 171.8(12) . . . . ? O2 C6 C1 N1 179.1(13) . . . . ? O1 C6 C1 N1 -1.1(18) . . . . ? O2 C6 C1 C2 3(2) . . . . ? O1 C6 C1 C2 -177.0(12) . . . . ? C1 N1 C5 C4 1(3) . . . . ? Dy1 N1 C5 C4 -173.3(11) . . . . ? C1 N1 C5 C8 179.3(13) . . . . ? Dy1 N1 C5 C8 5(2) . . . . ? O3 C8 C5 N1 -11(2) . . . . ? O4 C8 C5 N1 174.1(13) . . . . ? O3 C8 C5 C4 166.9(14) . . . . ? O4 C8 C5 C4 -8(2) . . . . ? N1 C5 C4 C3 -1(2) . . . . ? C8 C5 C4 C3 -178.5(13) . . . . ? C1 C2 C3 C4 4.1(17) . . . . ? C1 C2 C3 C7 -170.7(12) . . . . ? C5 C4 C3 C2 -2.1(18) . . . . ? C5 C4 C3 C7 172.5(13) . . . . ? O5 C7 C3 C2 -47.0(19) . . . . ? O6 C7 C3 C2 131.2(13) . . . . ? O5 C7 C3 C4 138.4(13) . . . . ? O6 C7 C3 C4 -43.4(19) . . . . ? O5 C7 O6 Dy1 1.4(14) . . . 4_556 ? C3 C7 O6 Dy1 -176.7(11) . . . 4_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.701 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.593 #===END of CIF for Complex 10 =====================