Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_1 _database_code_CSD 166257 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Abrahams, Brendan F.' 'Che, Chi-Ming' 'Chen, Zhen-Feng' 'Xiong, Ren-Gen' 'You, Xiao-Zeng' _publ_contact_author_name 'Prof Ren-Gen Xiong' _publ_contact_author_address ; Coordination Chemistry Inst. State Key Lab of Coordination Chemistry Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email 'xyz@netra.nju.edu.cn' _publ_contact_author_fax '86-25-3317761' _publ_contact_author_phone '86-25-3594724' _publ_requested_journal 'J. Chem.Soc. Dalton Trans.' _publ_section_title ; An unprecedented 6-fold anion-type chiral diamondoid-like 8-coordinate Cd(II) coordination polymer with a strong second-order nonlinear optical effect ; _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G. & Taylor, R. (1987). Chem. Soc. Perkin Trans. II, S1-S19. Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Orpen, A.G., Brammer, L., Allen, F.H., Kennard, O., Watson, D.G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans., S1-S83. Siemens (1996). SMART and SAINT. Area Detector Control and Integration Software. Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXTL V5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_exptl_refinement ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. ; #============================================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 Cd N6 O8' _chemical_formula_weight 712.98 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M C2221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.1187(10) _cell_length_b 23.3448(16) _cell_length_c 22.9554(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7030.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.82794 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _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 18399 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.1445 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6149 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(6) _refine_ls_number_reflns 6149 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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 0.48966(5) 0.17018(3) 0.06478(3) 0.0510(2) Uani 1 1 d . . . O8 O 0.4925(6) 0.1812(3) -0.0375(2) 0.0622(18) Uani 1 1 d . . . N3 N 0.4526(6) 0.2238(4) -0.2535(6) 0.073(3) Uani 1 1 d . . . O7 O 0.3431(6) 0.2027(3) 0.0009(3) 0.069(2) Uani 1 1 d . . . C28 C 0.4025(9) 0.1989(5) -0.0430(5) 0.055(3) Uani 1 1 d . . . C27 C 0.3637(8) 0.2095(5) -0.1021(5) 0.051(3) Uani 1 1 d . . . C26 C 0.2620(9) 0.2218(5) -0.1128(5) 0.063(4) Uani 1 1 d . . . H26A H 0.2175 0.2241 -0.0814 0.075 Uiso 1 1 calc R . . C25 C 0.9963(11) 0.1009(5) 0.1411(6) 0.086(3) Uani 1 1 d . . . H25A H 1.0626 0.0910 0.1513 0.103 Uiso 1 1 calc R . . C24 C 0.4263(8) 0.2106(5) -0.1491(5) 0.065(3) Uani 1 1 d . . . H24A H 0.4954 0.2030 -0.1443 0.077 Uiso 1 1 calc R . . C23 C 0.2911(9) 0.2316(5) -0.2131(5) 0.065(3) Uani 1 1 d . . . H23A H 0.2677 0.2384 -0.2508 0.078 Uiso 1 1 calc R . . N2 N 0.1470(8) -0.0835(4) 0.2562(6) 0.081(3) Uani 1 1 d . . . C22 C 0.9281(10) 0.1135(5) 0.1826(7) 0.073(4) Uani 1 1 d . . . O6 O 0.4374(7) 0.0722(3) 0.0548(4) 0.085(3) Uani 1 1 d . . . O5 O 0.3678(7) 0.1178(4) 0.1245(4) 0.082(3) Uani 1 1 d . . . C21 C 0.3893(8) 0.2228(5) -0.2039(4) 0.050(3) Uani 1 1 d . . . C20 C 0.6900(11) 0.1387(6) 0.0970(8) 0.071(4) Uani 1 1 d . . . O4 O 0.6253(8) 0.1420(4) 0.1331(5) 0.098(4) Uani 1 1 d . . . N1 N 0.1778(9) -0.0349(5) 0.2441(7) 0.107(4) Uani 1 1 d . . . C19 C 0.3791(11) 0.0742(6) 0.0995(6) 0.067(4) Uani 1 1 d . . . C18 C 0.2241(9) 0.2308(5) -0.1678(6) 0.071(4) Uani 1 1 d . . . H18A H 0.1546 0.2361 -0.1740 0.085 Uiso 1 1 calc R . . O3 O 0.6666(7) 0.1456(4) 0.0457(5) 0.102(3) Uani 1 1 d . . . C17 C 0.2713(10) 0.0172(5) 0.1689(6) 0.076(4) Uani 1 1 d . . . H17A H 0.2710 0.0471 0.1955 0.091 Uiso 1 1 calc R . . C16 C 0.7960(11) 0.1258(6) 0.1126(7) 0.074(4) Uani 1 1 d . . . C15 C 0.2221(11) -0.0330(5) 0.1838(6) 0.075(4) Uani 1 1 d . . . C14 C 0.2154(12) -0.0796(6) 0.1474(7) 0.101(5) Uani 1 1 d . . . H14A H 0.1836 -0.1133 0.1592 0.122 Uiso 1 1 calc R . . C13 C 0.3215(12) 0.0253(6) 0.1157(7) 0.082(5) Uani 1 1 d . . . C12 C 0.8262(9) 0.1242(5) 0.1684(6) 0.070(4) Uani 1 1 d . . . H12A H 0.7788 0.1302 0.1979 0.085 Uiso 1 1 calc R . . C11 C 0.3168(12) -0.0223(7) 0.0773(8) 0.121(6) Uani 1 1 d . . . H11A H 0.3513 -0.0209 0.0419 0.145 Uiso 1 1 calc R . . C10 C 0.8658(10) 0.1136(6) 0.0689(8) 0.091(4) Uani 1 1 d . . . H10A H 0.8446 0.1128 0.0303 0.109 Uiso 1 1 calc R . . C9 C 0.1047(10) -0.0885(6) 0.3123(7) 0.075(4) Uani 1 1 d . . . C8 C 0.0883(15) -0.0449(6) 0.3501(8) 0.126(7) Uani 1 1 d . . . H8A H 0.1074 -0.0077 0.3404 0.152 Uiso 1 1 calc R . . C7 C 0.2578(13) -0.0743(7) 0.0925(7) 0.112(5) Uani 1 1 d . . . H7A H 0.2493 -0.1033 0.0652 0.134 Uiso 1 1 calc R . . C6 C 0.9680(13) 0.1025(6) 0.0828(7) 0.111(5) Uani 1 1 d . . . H6A H 1.0159 0.0963 0.0536 0.133 Uiso 1 1 calc R . . N4 N 0.9525(6) 0.1155(4) 0.2431(7) 0.075(3) Uani 1 1 d . . . C5 C 0.0768(9) -0.1434(5) 0.3311(5) 0.062(3) Uani 1 1 d . . . H5A H 0.0874 -0.1740 0.3059 0.075 Uiso 1 1 calc R . . C4 C 0.0361(10) -0.1539(6) 0.3827(6) 0.074(4) Uani 1 1 d . . . C3 C 0.0164(10) -0.2159(7) 0.3989(7) 0.081(5) Uani 1 1 d . . . C2 C 0.0175(13) -0.1099(7) 0.4191(6) 0.107(5) Uani 1 1 d . . . H2B H -0.0128 -0.1169 0.4550 0.129 Uiso 1 1 calc R . . C1 C 0.0423(16) -0.0564(7) 0.4041(8) 0.149(9) Uani 1 1 d . . . H1B H 0.0289 -0.0265 0.4296 0.179 Uiso 1 1 calc R . . O2 O -0.0320(7) -0.2207(4) 0.4471(5) 0.104(3) Uani 1 1 d . . . O1 O 0.0472(8) -0.2545(4) 0.3734(5) 0.085(3) Uani 1 1 d . . . N5 N 0.1828(7) 0.2530(5) 0.0513(4) 0.071(3) Uani 1 1 d . . . H5B H 0.2319 0.2429 0.0259 0.085 Uiso 1 1 calc R . . H5C H 0.1293 0.2659 0.0306 0.085 Uiso 1 1 calc R . . C31 C 0.1526(12) 0.2043(6) 0.0825(8) 0.128(7) Uani 1 1 d . . . H31A H 0.1265 0.1761 0.0559 0.192 Uiso 1 1 calc R . . H31B H 0.1004 0.2145 0.1099 0.192 Uiso 1 1 calc R . . H31C H 0.2101 0.1888 0.1030 0.192 Uiso 1 1 calc R . . N7 N 0.5000 0.1531(13) 0.2500 0.262(15) Uani 1 2 d S . . N6 N 0.5000 0.041(2) 0.2500 0.38(3) Uani 1 2 d S . . C37 C 0.2192(11) 0.2974(7) 0.0864(6) 0.097(5) Uani 1 1 d . . . H37A H 0.2354 0.3299 0.0625 0.145 Uiso 1 1 calc R . . H37B H 0.2792 0.2848 0.1066 0.145 Uiso 1 1 calc R . . H37C H 0.1678 0.3079 0.1142 0.145 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0485(4) 0.0589(4) 0.0456(4) 0.0009(4) -0.0036(4) 0.0033(4) O8 0.049(4) 0.088(5) 0.049(4) -0.003(3) -0.003(4) -0.004(5) N3 0.060(6) 0.114(7) 0.045(5) -0.003(8) -0.014(6) 0.015(5) O7 0.061(5) 0.101(6) 0.046(5) -0.011(4) 0.009(4) 0.006(4) C28 0.055(8) 0.070(8) 0.039(7) -0.003(5) -0.005(6) -0.011(6) C27 0.035(6) 0.063(8) 0.056(8) 0.006(6) 0.003(6) -0.001(5) C26 0.052(8) 0.099(11) 0.036(7) -0.002(6) 0.015(6) -0.006(7) C25 0.050(8) 0.112(10) 0.096(10) -0.002(8) -0.007(10) -0.003(9) C24 0.041(6) 0.108(10) 0.044(7) -0.006(7) 0.019(6) -0.005(6) C23 0.060(8) 0.096(10) 0.038(7) 0.016(6) 0.011(6) 0.000(7) N2 0.108(8) 0.057(6) 0.077(8) 0.016(8) 0.009(8) -0.019(6) C22 0.067(9) 0.059(9) 0.092(11) 0.004(7) -0.022(8) -0.007(7) O6 0.102(7) 0.071(6) 0.083(7) 0.014(5) -0.007(6) -0.001(5) O5 0.098(7) 0.054(7) 0.094(8) 0.008(6) -0.006(5) -0.022(6) C21 0.043(7) 0.079(8) 0.027(6) 0.002(5) 0.007(5) -0.009(6) C20 0.065(10) 0.060(9) 0.089(12) -0.006(8) -0.018(9) 0.017(7) O4 0.064(6) 0.096(8) 0.133(10) -0.032(7) -0.035(6) 0.020(5) N1 0.100(9) 0.090(8) 0.131(11) 0.035(10) 0.014(10) -0.010(7) C19 0.097(11) 0.034(8) 0.068(10) 0.002(7) -0.005(8) -0.008(7) C18 0.059(8) 0.082(9) 0.072(10) 0.018(7) -0.018(7) 0.020(7) O3 0.084(7) 0.109(8) 0.113(8) 0.005(6) -0.040(6) 0.011(5) C17 0.107(11) 0.059(9) 0.062(9) -0.005(7) 0.013(8) -0.011(8) C16 0.059(9) 0.065(10) 0.099(12) -0.005(8) -0.028(8) -0.003(7) C15 0.119(11) 0.050(9) 0.056(8) 0.003(6) 0.025(8) -0.012(8) C14 0.134(14) 0.068(10) 0.103(13) 0.001(10) 0.047(11) -0.021(9) C13 0.103(12) 0.026(8) 0.117(13) -0.010(8) -0.027(10) 0.009(7) C12 0.042(7) 0.071(9) 0.098(11) -0.008(7) -0.020(7) 0.001(6) C11 0.140(14) 0.100(13) 0.122(15) 0.066(12) 0.017(12) -0.031(10) C10 0.062(8) 0.124(12) 0.088(10) 0.000(11) -0.022(10) 0.023(8) C9 0.092(10) 0.049(9) 0.083(10) 0.018(8) 0.000(8) 0.001(7) C8 0.198(19) 0.049(10) 0.132(16) 0.002(10) 0.043(14) -0.006(10) C7 0.151(16) 0.094(12) 0.091(13) -0.009(10) -0.009(11) 0.014(11) C6 0.110(14) 0.137(13) 0.085(12) 0.006(9) 0.010(10) 0.001(10) N4 0.058(6) 0.072(6) 0.094(8) 0.004(8) -0.014(7) 0.012(4) C5 0.071(8) 0.052(8) 0.064(9) -0.002(6) 0.001(7) 0.016(6) C4 0.080(10) 0.070(10) 0.070(9) 0.005(7) 0.012(7) 0.021(7) C3 0.029(7) 0.124(14) 0.090(11) 0.059(10) -0.007(8) -0.025(9) C2 0.123(13) 0.111(12) 0.088(11) 0.048(9) 0.044(11) -0.007(12) C1 0.25(3) 0.083(13) 0.113(14) -0.007(10) 0.056(16) -0.018(14) O2 0.070(6) 0.100(7) 0.143(9) 0.047(6) -0.030(6) 0.004(5) O1 0.086(8) 0.046(6) 0.123(9) 0.014(5) -0.015(6) 0.005(5) N5 0.058(6) 0.100(9) 0.056(7) 0.005(6) -0.005(5) 0.012(6) C31 0.137(14) 0.083(11) 0.163(17) 0.016(11) 0.091(13) 0.007(10) N7 0.41(5) 0.27(3) 0.111(17) 0.000 0.06(3) 0.000 N6 0.23(4) 0.62(8) 0.30(4) 0.000 -0.23(4) 0.000 C37 0.082(10) 0.135(14) 0.074(11) -0.022(10) -0.005(8) -0.023(9) _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 O1 2.310(9) 7 ? Cd1 O8 2.362(6) . ? Cd1 O6 2.400(8) . ? Cd1 O3 2.431(10) . ? Cd1 O5 2.435(9) . ? Cd1 O4 2.461(10) . ? Cd1 O7 2.534(8) . ? Cd1 O2 2.622(9) 7 ? O8 C28 1.257(13) . ? N3 N3 1.254(16) 3_654 ? N3 C21 1.409(14) . ? O7 C28 1.277(12) . ? C28 C27 1.471(13) . ? C27 C24 1.357(13) . ? C27 C26 1.387(14) . ? C26 C18 1.373(14) . ? C26 H26A 0.9300 . ? C25 C22 1.340(17) . ? C25 C6 1.389(16) . ? C25 H25A 0.9300 . ? C24 C21 1.378(13) . ? C24 H24A 0.9300 . ? C23 C21 1.321(15) . ? C23 C18 1.362(15) . ? C23 H23A 0.9300 . ? N2 N1 1.237(12) . ? N2 C9 1.406(17) . ? C22 C12 1.399(15) . ? C22 N4 1.424(18) . ? O6 C19 1.282(14) . ? O5 C19 1.177(14) . ? C20 O4 1.188(17) . ? C20 O3 1.227(15) . ? C20 C16 1.468(18) . ? N1 C15 1.501(18) . ? C19 C13 1.418(18) . ? C18 H18A 0.9300 . ? C17 C15 1.380(16) . ? C17 C13 1.399(17) . ? C17 H17A 0.9300 . ? C16 C12 1.341(16) . ? C16 C10 1.386(18) . ? C15 C14 1.375(17) . ? C14 C7 1.38(2) . ? C14 H14A 0.9300 . ? C13 C11 1.42(2) . ? C12 H12A 0.9300 . ? C11 C7 1.481(19) . ? C11 H11A 0.9300 . ? C10 C6 1.403(18) . ? C10 H10A 0.9300 . ? C9 C8 1.356(18) . ? C9 C5 1.400(15) . ? C8 C1 1.40(2) . ? C8 H8A 0.9300 . ? C7 H7A 0.9300 . ? C6 H6A 0.9300 . ? N4 N4 1.287(16) 3_755 ? C5 C4 1.322(15) . ? C5 H5A 0.9300 . ? C4 C2 1.347(17) . ? C4 C3 1.52(2) . ? C3 O1 1.147(17) . ? C3 O2 1.282(15) . ? C2 C1 1.336(18) . ? C2 H2B 0.9300 . ? C1 H1B 0.9300 . ? O2 Cd1 2.622(9) 7_545 ? O1 Cd1 2.310(9) 7_545 ? N5 C37 1.397(14) . ? N5 C31 1.400(15) . ? N5 H5B 0.9000 . ? N5 H5C 0.9000 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O8 122.1(3) 7 . ? O1 Cd1 O6 136.4(4) 7 . ? O8 Cd1 O6 90.7(3) . . ? O1 Cd1 O3 119.4(3) 7 . ? O8 Cd1 O3 80.3(3) . . ? O6 Cd1 O3 91.7(3) . . ? O1 Cd1 O5 84.2(4) 7 . ? O8 Cd1 O5 128.6(3) . . ? O6 Cd1 O5 52.2(3) . . ? O3 Cd1 O5 127.6(4) . . ? O1 Cd1 O4 87.9(3) 7 . ? O8 Cd1 O4 130.6(4) . . ? O6 Cd1 O4 90.7(3) . . ? O3 Cd1 O4 50.3(4) . . ? O5 Cd1 O4 89.0(3) . . ? O1 Cd1 O7 88.2(3) 7 . ? O8 Cd1 O7 53.4(2) . . ? O6 Cd1 O7 90.7(3) . . ? O3 Cd1 O7 133.7(3) . . ? O5 Cd1 O7 88.7(3) . . ? O4 Cd1 O7 175.7(3) . . ? O1 Cd1 O2 50.9(3) 7 7 ? O8 Cd1 O2 77.7(3) . 7 ? O6 Cd1 O2 167.7(3) . 7 ? O3 Cd1 O2 90.5(3) . 7 ? O5 Cd1 O2 133.3(4) . 7 ? O4 Cd1 O2 99.9(3) . 7 ? O7 Cd1 O2 79.0(3) . 7 ? C28 O8 Cd1 96.9(6) . . ? N3 N3 C21 118.6(16) 3_654 . ? C28 O7 Cd1 88.4(6) . . ? O8 C28 O7 121.1(10) . . ? O8 C28 C27 118.2(9) . . ? O7 C28 C27 120.3(10) . . ? C24 C27 C26 115.9(10) . . ? C24 C27 C28 121.9(10) . . ? C26 C27 C28 122.1(10) . . ? C18 C26 C27 122.9(11) . . ? C18 C26 H26A 118.6 . . ? C27 C26 H26A 118.6 . . ? C22 C25 C6 120.1(14) . . ? C22 C25 H25A 120.0 . . ? C6 C25 H25A 120.0 . . ? C27 C24 C21 121.2(10) . . ? C27 C24 H24A 119.4 . . ? C21 C24 H24A 119.4 . . ? C21 C23 C18 120.4(11) . . ? C21 C23 H23A 119.8 . . ? C18 C23 H23A 119.8 . . ? N1 N2 C9 114.3(13) . . ? C25 C22 C12 120.7(13) . . ? C25 C22 N4 123.4(12) . . ? C12 C22 N4 115.9(13) . . ? C19 O6 Cd1 93.3(7) . . ? C19 O5 Cd1 94.4(9) . . ? C23 C21 C24 121.4(10) . . ? C23 C21 N3 116.3(10) . . ? C24 C21 N3 122.2(10) . . ? O4 C20 O3 118.8(15) . . ? O4 C20 C16 121.3(17) . . ? O3 C20 C16 119.9(16) . . ? C20 O4 Cd1 95.1(11) . . ? N2 N1 C15 111.2(13) . . ? O5 C19 O6 119.8(12) . . ? O5 C19 C13 120.1(14) . . ? O6 C19 C13 119.8(13) . . ? C23 C18 C26 118.1(11) . . ? C23 C18 H18A 121.0 . . ? C26 C18 H18A 121.0 . . ? C20 O3 Cd1 95.5(9) . . ? C15 C17 C13 123.5(12) . . ? C15 C17 H17A 118.2 . . ? C13 C17 H17A 118.2 . . ? C12 C16 C10 119.3(13) . . ? C12 C16 C20 121.2(15) . . ? C10 C16 C20 119.4(14) . . ? C14 C15 C17 123.4(13) . . ? C14 C15 N1 120.8(12) . . ? C17 C15 N1 115.8(12) . . ? C15 C14 C7 117.1(13) . . ? C15 C14 H14A 121.4 . . ? C7 C14 H14A 121.4 . . ? C17 C13 C19 126.1(13) . . ? C17 C13 C11 114.4(13) . . ? C19 C13 C11 119.4(15) . . ? C16 C12 C22 120.7(13) . . ? C16 C12 H12A 119.6 . . ? C22 C12 H12A 119.6 . . ? C13 C11 C7 121.2(15) . . ? C13 C11 H11A 119.4 . . ? C7 C11 H11A 119.4 . . ? C16 C10 C6 120.3(15) . . ? C16 C10 H10A 119.8 . . ? C6 C10 H10A 119.8 . . ? C8 C9 C5 116.7(14) . . ? C8 C9 N2 125.9(13) . . ? C5 C9 N2 117.5(13) . . ? C9 C8 C1 119.2(14) . . ? C9 C8 H8A 120.4 . . ? C1 C8 H8A 120.4 . . ? C14 C7 C11 119.9(15) . . ? C14 C7 H7A 120.0 . . ? C11 C7 H7A 120.0 . . ? C25 C6 C10 118.6(15) . . ? C25 C6 H6A 120.7 . . ? C10 C6 H6A 120.7 . . ? N4 N4 C22 117.2(16) 3_755 . ? C4 C5 C9 123.5(12) . . ? C4 C5 H5A 118.2 . . ? C9 C5 H5A 118.2 . . ? C5 C4 C2 119.2(13) . . ? C5 C4 C3 117.8(13) . . ? C2 C4 C3 123.0(13) . . ? O1 C3 O2 123.1(15) . . ? O1 C3 C4 124.4(14) . . ? O2 C3 C4 112.3(16) . . ? C1 C2 C4 120.5(15) . . ? C1 C2 H2B 119.7 . . ? C4 C2 H2B 119.7 . . ? C2 C1 C8 120.8(15) . . ? C2 C1 H1B 119.6 . . ? C8 C1 H1B 119.6 . . ? C3 O2 Cd1 83.7(9) . 7_545 ? C3 O1 Cd1 102.2(10) . 7_545 ? C37 N5 C31 113.9(12) . . ? C37 N5 H5B 108.8 . . ? C31 N5 H5B 108.8 . . ? C37 N5 H5C 108.8 . . ? C31 N5 H5C 108.8 . . ? H5B N5 H5C 107.7 . . ? N5 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C37 H37A 109.5 . . ? N5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.837 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.098