# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1 _database_code_depnum_ccdc_archive 'CCDC 876730' #TrackingRef 'complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H15 N O12 Zn2' _chemical_formula_sum 'C12 H15 N O12 Zn2' _chemical_formula_weight 495.99 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' 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' Zn Zn 0.2839 1.4301 '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' _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 8.9884(9) _cell_length_b 9.3145(9) _cell_length_c 9.8343(11) _cell_angle_alpha 94.624(4) _cell_angle_beta 104.185(3) _cell_angle_gamma 98.138(5) _cell_volume 784.48(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1993 _cell_measurement_theta_min 2.1515 _cell_measurement_theta_max 27.4680 _exptl_crystal_description Plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 3.130 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6776 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5114 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2708 _reflns_number_gt 2446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0765P)^2^+2.5372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2708 _refine_ls_number_parameters 242 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1351 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.074 _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 Zn1 Zn -0.25852(7) 0.14772(6) 0.96571(6) 0.0237(2) Uani 1 1 d . . . O1 O 0.3337(4) 0.8294(4) 0.8414(4) 0.0270(8) Uani 1 1 d . . . N1 N 0.2067(5) 0.3641(5) 0.7469(5) 0.0227(9) Uani 1 1 d . . . C1 C 0.2807(6) 0.6946(6) 0.8163(5) 0.0230(11) Uani 1 1 d . . . O5 O 0.0747(5) 0.3167(5) 0.9601(4) 0.0344(10) Uani 1 1 d . . . Zn2 Zn 0.28152(7) 0.45126(6) 0.97955(6) 0.0237(2) Uani 1 1 d . . . O2 O 0.2128(4) 0.6328(4) 0.9009(4) 0.0236(8) Uani 1 1 d . . . C2 C 0.2924(6) 0.6118(6) 0.6822(5) 0.0205(10) Uani 1 1 d . . . O3 O 0.4618(4) 0.3536(4) 0.9614(4) 0.0276(9) Uani 1 1 d . . . C3 C 0.3417(7) 0.6979(6) 0.5845(6) 0.0285(12) Uani 1 1 d . . . H3 H 0.3729 0.8005 0.6087 0.034 Uiso 1 1 calc R . . O4 O 0.5323(4) 0.1744(4) 0.8389(4) 0.0287(9) Uani 1 1 d . . . C4 C 0.3446(7) 0.6328(6) 0.4528(6) 0.0272(12) Uani 1 1 d . . . H4 H 0.3790 0.6909 0.3878 0.033 Uiso 1 1 calc R . . C5 C 0.2977(6) 0.4837(6) 0.4163(5) 0.0217(11) Uani 1 1 d . . . O6 O -0.1491(4) 0.2005(4) 0.8150(4) 0.0305(9) Uani 1 1 d . . . C6 C 0.2908(6) 0.4134(6) 0.2702(6) 0.0269(12) Uani 1 1 d . . . O7 O 0.3175(5) 0.4993(4) 0.1840(4) 0.0336(10) Uani 1 1 d . . . C7 C 0.2537(6) 0.3984(6) 0.5139(5) 0.0251(11) Uani 1 1 d . . . H7 H 0.2231 0.2959 0.4888 0.030 Uiso 1 1 calc R . . O8 O 0.2567(6) 0.2768(4) 0.2462(4) 0.0394(11) Uani 1 1 d . . . C8 C 0.2532(6) 0.4601(6) 0.6481(5) 0.0215(11) Uani 1 1 d . . . O9 O -0.0477(5) 0.0977(4) 1.0969(4) 0.0342(9) Uani 1 1 d . . . C9 C 0.0362(6) 0.3287(7) 0.7135(6) 0.0274(12) Uani 1 1 d . . . H9A H -0.0018 0.2513 0.6321 0.033 Uiso 1 1 calc R . . H9B H -0.0092 0.4163 0.6864 0.033 Uiso 1 1 calc R . . O10 O -0.3399(5) -0.0710(4) 0.9147(5) 0.0329(9) Uani 1 1 d . . . C10 C -0.0166(6) 0.2770(6) 0.8393(6) 0.0265(12) Uani 1 1 d . . . C11 C 0.2807(6) 0.2294(6) 0.7524(6) 0.0247(11) Uani 1 1 d . . . H11A H 0.2918 0.1977 0.6574 0.030 Uiso 1 1 calc R . . H11B H 0.2122 0.1498 0.7793 0.030 Uiso 1 1 calc R . . C12 C 0.4397(5) 0.2556(5) 0.8577(5) 0.0239(11) Uani 1 1 d . . . H9D H 0.0243 0.1709 1.1002 0.029 Uiso 1 1 d R . . H9C H 0.0007 0.0270 1.1232 0.029 Uiso 1 1 d R . . H10C H -0.3655 -0.1305 0.9692 0.029 Uiso 1 1 d R . . H10D H -0.3532 -0.1218 0.8336 0.029 Uiso 1 1 d R . . O11 O 0.3189(5) 0.0224(5) 0.4300(5) 0.144(4) Uani 1 1 d RU . . O12 O -0.0246(5) 0.0772(5) 1.3826(5) 0.178(5) Uani 1 1 d RU . . 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 Zn1 0.0255(4) 0.0245(4) 0.0228(4) -0.0009(2) 0.0101(3) 0.0048(3) O1 0.030(2) 0.023(2) 0.027(2) -0.0004(15) 0.0102(16) 0.0000(16) N1 0.024(2) 0.024(2) 0.021(2) 0.0031(18) 0.0085(18) 0.0038(19) C1 0.019(2) 0.029(3) 0.020(3) -0.002(2) 0.001(2) 0.007(2) O5 0.032(2) 0.046(2) 0.023(2) 0.0025(18) 0.0093(17) -0.0048(19) Zn2 0.0293(4) 0.0267(4) 0.0166(4) 0.0021(2) 0.0080(3) 0.0072(3) O2 0.030(2) 0.0263(19) 0.0167(18) 0.0010(15) 0.0110(15) 0.0036(16) C2 0.022(2) 0.026(3) 0.014(2) -0.001(2) 0.007(2) 0.002(2) O3 0.0263(19) 0.029(2) 0.027(2) -0.0029(16) 0.0066(16) 0.0079(16) C3 0.033(3) 0.025(3) 0.026(3) -0.003(2) 0.010(2) 0.001(2) O4 0.028(2) 0.029(2) 0.030(2) -0.0001(16) 0.0080(17) 0.0101(17) C4 0.037(3) 0.023(3) 0.022(3) 0.004(2) 0.009(2) 0.002(2) C5 0.022(2) 0.030(3) 0.015(3) -0.001(2) 0.007(2) 0.009(2) O6 0.024(2) 0.037(2) 0.030(2) 0.0023(17) 0.0087(16) -0.0011(18) C6 0.026(3) 0.032(3) 0.023(3) 0.002(2) 0.006(2) 0.007(2) O7 0.045(2) 0.035(2) 0.020(2) 0.0015(17) 0.0127(18) -0.0009(19) C7 0.030(3) 0.023(3) 0.019(3) -0.003(2) 0.003(2) 0.002(2) O8 0.063(3) 0.029(2) 0.027(2) -0.0034(17) 0.014(2) 0.010(2) C8 0.019(2) 0.026(3) 0.018(3) 0.001(2) 0.005(2) 0.001(2) O9 0.031(2) 0.034(2) 0.038(2) 0.0081(18) 0.0093(18) 0.0065(18) C9 0.022(3) 0.038(3) 0.023(3) 0.004(2) 0.008(2) 0.004(2) O10 0.038(2) 0.0204(19) 0.042(2) -0.0016(17) 0.0158(19) 0.0032(17) C10 0.029(3) 0.026(3) 0.026(3) 0.003(2) 0.009(2) 0.008(2) C11 0.027(3) 0.028(3) 0.021(3) 0.003(2) 0.008(2) 0.008(2) C12 0.025(3) 0.023(3) 0.024(3) 0.004(2) 0.010(2) 0.000(2) O11 0.171(6) 0.126(5) 0.128(5) 0.015(4) 0.032(4) 0.015(4) O12 0.193(6) 0.169(6) 0.162(6) 0.029(5) 0.037(5) 0.005(5) _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 Zn1 O6 2.025(4) . ? Zn1 O10 2.042(4) . ? Zn1 O4 2.046(4) 1_455 ? Zn1 O9 2.150(4) . ? Zn1 O1 2.169(4) 2_567 ? Zn1 O2 2.266(4) 2_567 ? Zn1 C1 2.565(5) 2_567 ? O1 C1 1.260(6) . ? O1 Zn1 2.169(4) 2_567 ? N1 C8 1.467(7) . ? N1 C9 1.469(7) . ? N1 C11 1.500(7) . ? N1 Zn2 2.267(4) . ? C1 O2 1.274(7) . ? C1 C2 1.507(7) . ? C1 Zn1 2.565(5) 2_567 ? O5 C10 1.260(7) . ? O5 Zn2 2.047(4) . ? Zn2 O7 1.960(4) 1_556 ? Zn2 O3 2.004(4) . ? Zn2 O2 2.028(4) . ? O2 Zn1 2.266(4) 2_567 ? C2 C8 1.399(7) . ? C2 C3 1.413(8) . ? O3 C12 1.270(6) . ? C3 C4 1.393(8) . ? C3 H3 0.9500 . ? O4 C12 1.237(6) . ? O4 Zn1 2.046(4) 1_655 ? C4 C5 1.384(8) . ? C4 H4 0.9500 . ? C5 C7 1.388(8) . ? C5 C6 1.513(7) . ? O6 C10 1.255(7) . ? C6 O7 1.253(7) . ? C6 O8 1.255(7) . ? O7 Zn2 1.960(4) 1_554 ? C7 C8 1.398(7) . ? C7 H7 0.9500 . ? O9 H9D 0.8635 . ? O9 H9C 0.8619 . ? C9 C10 1.519(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O10 H10C 0.8483 . ? O10 H10D 0.8664 . ? C11 C12 1.519(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zn1 O10 104.16(17) . . ? O6 Zn1 O4 91.19(16) . 1_455 ? O10 Zn1 O4 85.49(16) . 1_455 ? O6 Zn1 O9 90.97(16) . . ? O10 Zn1 O9 89.06(16) . . ? O4 Zn1 O9 174.49(15) 1_455 . ? O6 Zn1 O1 159.23(15) . 2_567 ? O10 Zn1 O1 96.30(16) . 2_567 ? O4 Zn1 O1 94.01(15) 1_455 2_567 ? O9 Zn1 O1 85.73(16) . 2_567 ? O6 Zn1 O2 100.34(15) . 2_567 ? O10 Zn1 O2 155.45(15) . 2_567 ? O4 Zn1 O2 95.71(14) 1_455 2_567 ? O9 Zn1 O2 88.89(15) . 2_567 ? O1 Zn1 O2 59.15(13) 2_567 2_567 ? O6 Zn1 C1 130.05(17) . 2_567 ? O10 Zn1 C1 125.67(17) . 2_567 ? O4 Zn1 C1 95.50(15) 1_455 2_567 ? O9 Zn1 C1 86.98(16) . 2_567 ? O1 Zn1 C1 29.38(16) 2_567 2_567 ? O2 Zn1 C1 29.78(15) 2_567 2_567 ? C1 O1 Zn1 93.0(3) . 2_567 ? C8 N1 C9 110.0(4) . . ? C8 N1 C11 112.9(4) . . ? C9 N1 C11 111.9(4) . . ? C8 N1 Zn2 117.3(3) . . ? C9 N1 Zn2 104.7(3) . . ? C11 N1 Zn2 99.5(3) . . ? O1 C1 O2 119.6(5) . . ? O1 C1 C2 118.8(5) . . ? O2 C1 C2 121.5(5) . . ? O1 C1 Zn1 57.6(3) . 2_567 ? O2 C1 Zn1 62.0(3) . 2_567 ? C2 C1 Zn1 175.7(4) . 2_567 ? C10 O5 Zn2 119.5(4) . . ? O7 Zn2 O3 103.74(17) 1_556 . ? O7 Zn2 O2 103.34(16) 1_556 . ? O3 Zn2 O2 130.16(16) . . ? O7 Zn2 O5 93.29(17) 1_556 . ? O3 Zn2 O5 116.44(17) . . ? O2 Zn2 O5 102.81(16) . . ? O7 Zn2 N1 169.88(17) 1_556 . ? O3 Zn2 N1 79.14(15) . . ? O2 Zn2 N1 81.37(15) . . ? O5 Zn2 N1 76.85(16) . . ? C1 O2 Zn2 119.8(3) . . ? C1 O2 Zn1 88.2(3) . 2_567 ? Zn2 O2 Zn1 122.86(17) . 2_567 ? C8 C2 C3 119.5(5) . . ? C8 C2 C1 124.7(5) . . ? C3 C2 C1 115.7(5) . . ? C12 O3 Zn2 117.7(3) . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C12 O4 Zn1 130.9(3) . 1_655 ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C7 119.6(5) . . ? C4 C5 C6 120.6(5) . . ? C7 C5 C6 119.8(5) . . ? C10 O6 Zn1 124.4(4) . . ? O7 C6 O8 126.5(5) . . ? O7 C6 C5 115.9(5) . . ? O8 C6 C5 117.6(5) . . ? C6 O7 Zn2 126.8(4) . 1_554 ? C5 C7 C8 121.5(5) . . ? C5 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C2 118.9(5) . . ? C7 C8 N1 118.9(5) . . ? C2 C8 N1 122.2(5) . . ? Zn1 O9 H9D 106.3 . . ? Zn1 O9 H9C 143.6 . . ? H9D O9 H9C 105.4 . . ? N1 C9 C10 111.0(4) . . ? N1 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N1 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? Zn1 O10 H10C 126.8 . . ? Zn1 O10 H10D 126.8 . . ? H10C O10 H10D 106.3 . . ? O6 C10 O5 125.1(5) . . ? O6 C10 C9 117.5(5) . . ? O5 C10 C9 117.4(5) . . ? N1 C11 C12 111.8(4) . . ? N1 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? O4 C12 O3 126.0(4) . . ? O4 C12 C11 117.2(4) . . ? O3 C12 C11 116.7(4) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.363 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.130 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 876731' #TrackingRef 'complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H19 N4 O10 Zn3' _chemical_formula_sum 'C27 H19 N4 O10 Zn3' _chemical_formula_weight 755.57 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 15.7991(12) _cell_length_b 11.4257(6) _cell_length_c 18.7582(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.367(4) _cell_angle_gamma 90.00 _cell_volume 3294.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8805 _cell_measurement_theta_min 2.2216 _cell_measurement_theta_max 27.5087 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 2.223 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8401 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25232 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7508 _reflns_number_gt 6504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.227 0.500 0.227 850.4 6.6 _platon_squeeze_details ; ; _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^)+(0.0917P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7508 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Zn1 Zn 0.578982(19) 0.68356(3) 0.193965(16) 0.01949(10) Uani 1 1 d . . . Zn2 Zn 0.773749(19) 0.80838(3) 0.170126(16) 0.01894(10) Uani 1 1 d . . . Zn3 Zn 0.582956(18) 1.09088(3) -0.000345(15) 0.01840(10) Uani 1 1 d . . . O2 O 0.4350(2) 1.0683(3) 0.15127(14) 0.0582(8) Uani 1 1 d . . . O3 O 0.51453(13) 1.20479(16) -0.07389(10) 0.0240(4) Uani 1 1 d . . . O4 O 0.45451(13) 1.38014(17) -0.09296(10) 0.0265(4) Uani 1 1 d . . . O5 O 0.64041(12) 1.01903(16) 0.09969(10) 0.0233(4) Uani 1 1 d . . . O6 O 0.77018(12) 0.99103(17) 0.17200(10) 0.0232(4) Uani 1 1 d . . . O7 O 0.87804(13) 1.55106(18) 0.24218(11) 0.0286(4) Uani 1 1 d . . . O8 O 0.76215(13) 1.62597(17) 0.16366(11) 0.0279(4) Uani 1 1 d . . . O10 O 0.69669(15) 0.79786(19) 0.06180(11) 0.0313(5) Uani 1 1 d . . . N1 N 0.58381(14) 1.25067(19) 0.07509(11) 0.0181(4) Uani 1 1 d . . . N2 N 1.29582(16) 0.8878(2) 0.03091(13) 0.0271(5) Uani 1 1 d . . . N3 N 0.89142(15) 0.8248(2) 0.13143(14) 0.0265(5) Uani 1 1 d . . . N4 N 0.46241(16) 0.7020(2) 0.22267(14) 0.0279(5) Uani 1 1 d . . . C1 C 0.71241(16) 1.0564(2) 0.13721(12) 0.0167(5) Uani 1 1 d . . . C2 C 0.73172(17) 1.1861(2) 0.14186(14) 0.0174(5) Uani 1 1 d . . . C3 C 0.81675(18) 1.2161(2) 0.17775(15) 0.0244(6) Uani 1 1 d . . . H3 H 0.8579 1.1553 0.1932 0.029 Uiso 1 1 calc R . . C4 C 0.84304(18) 1.3309(2) 0.19149(16) 0.0251(6) Uani 1 1 d . . . H4 H 0.9012 1.3488 0.2161 0.030 Uiso 1 1 calc R . . C5 C 0.78297(17) 1.4194(2) 0.16865(13) 0.0192(5) Uani 1 1 d . . . C6 C 0.69947(17) 1.3932(2) 0.12995(13) 0.0181(5) Uani 1 1 d . . . H6 H 0.6596 1.4550 0.1133 0.022 Uiso 1 1 calc R . . C7 C 0.67270(16) 1.2778(2) 0.11497(12) 0.0164(5) Uani 1 1 d . . . C8 C 0.80908(16) 1.5427(2) 0.19198(13) 0.0181(5) Uani 1 1 d . . . C9 C 0.53107(18) 1.2132(3) 0.12761(15) 0.0254(6) Uani 1 1 d . . . H9A H 0.4952 1.2806 0.1361 0.031 Uiso 1 1 calc R . . H9B H 0.5715 1.1946 0.1750 0.031 Uiso 1 1 calc R . . C10 C 0.47107(18) 1.1088(2) 0.10530(15) 0.0244(6) Uani 1 1 d . . . C11 C 0.54125(19) 1.3457(2) 0.02571(15) 0.0274(6) Uani 1 1 d . . . C12 C 0.50007(17) 1.3052(2) -0.05164(15) 0.0204(5) Uani 1 1 d . . . C13 C 1.2611(2) 0.7831(3) 0.03943(18) 0.0337(7) Uani 1 1 d . . . H13 H 1.2941 0.7154 0.0343 0.040 Uiso 1 1 calc R . . C14 C 1.1818(2) 0.7674(3) 0.05493(18) 0.0366(7) Uani 1 1 d . . . H14 H 1.1603 0.6908 0.0597 0.044 Uiso 1 1 calc R . . C15 C 1.1322(2) 0.8662(3) 0.06372(17) 0.0342(7) Uani 1 1 d . . . C16 C 1.1674(2) 0.9737(3) 0.0553(2) 0.0456(9) Uani 1 1 d . . . H16 H 1.1362 1.0429 0.0609 0.055 Uiso 1 1 calc R . . C17 C 1.2476(2) 0.9815(3) 0.03882(19) 0.0388(8) Uani 1 1 d . . . H17 H 1.2700 1.0571 0.0327 0.047 Uiso 1 1 calc R . . C18 C 1.04709(19) 0.8531(3) 0.08440(18) 0.0334(7) Uani 1 1 d . . . C19 C 0.9946(2) 0.7559(4) 0.0651(2) 0.0526(10) Uani 1 1 d . . . H19 H 1.0105 0.6966 0.0352 0.063 Uiso 1 1 calc R . . C20 C 0.9182(2) 0.7454(3) 0.0899(2) 0.0459(9) Uani 1 1 d . . . H20 H 0.8835 0.6775 0.0764 0.055 Uiso 1 1 calc R . . C21 C 0.9421(2) 0.9202(3) 0.1479(2) 0.0426(8) Uani 1 1 d . . . H21 H 0.9242 0.9793 0.1769 0.051 Uiso 1 1 calc R . . C22 C 1.0180(2) 0.9376(3) 0.1255(2) 0.0436(8) Uani 1 1 d . . . H22 H 1.0504 1.0076 0.1383 0.052 Uiso 1 1 calc R . . C23 C 0.4144(2) 0.8002(3) 0.21059(17) 0.0300(6) Uani 1 1 d . . . H23 H 0.4387 0.8678 0.1937 0.036 Uiso 1 1 calc R . . C24 C 0.3320(2) 0.8065(3) 0.22169(18) 0.0324(7) Uani 1 1 d . . . H24 H 0.3003 0.8778 0.2132 0.039 Uiso 1 1 calc R . . C25 C 0.29515(19) 0.7085(3) 0.24533(18) 0.0343(7) Uani 1 1 d . . . C26 C 0.3453(2) 0.6075(4) 0.2594(3) 0.0575(12) Uani 1 1 d . . . H26 H 0.3212 0.5383 0.2746 0.069 Uiso 1 1 calc R . . C27 C 0.42860(8) 0.60713(10) 0.25147(7) 0.0496(10) Uani 1 1 d . . . H27 H 0.4640 0.5402 0.2661 0.060 Uiso 1 1 calc R . . H11A H 0.4993 1.3794 0.0519 0.060 Uiso 1 1 d R . . H11B H 0.5819 1.4016 0.0243 0.060 Uiso 1 1 d R . . O9 O 0.66100(8) 0.81008(10) 0.21680(7) 0.0185(4) Uani 1 1 d R . . O1 O 0.46111(8) 1.07168(10) 0.03900(7) 0.0206(4) Uani 1 1 d 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 Zn1 0.01595(18) 0.01610(18) 0.02382(17) 0.00335(11) -0.00073(12) -0.00144(11) Zn2 0.01776(18) 0.01288(17) 0.02612(18) 0.00193(11) 0.00495(13) -0.00015(10) Zn3 0.01643(17) 0.01396(17) 0.02348(17) -0.00070(11) 0.00186(12) -0.00140(11) O2 0.083(2) 0.0572(17) 0.0440(14) -0.0135(13) 0.0352(14) -0.0360(16) O3 0.0307(11) 0.0154(9) 0.0234(9) -0.0013(7) 0.0012(8) 0.0006(8) O4 0.0269(10) 0.0195(10) 0.0270(9) 0.0018(8) -0.0066(8) 0.0049(8) O5 0.0217(9) 0.0124(9) 0.0310(9) 0.0009(7) -0.0037(7) -0.0017(7) O6 0.0201(9) 0.0129(9) 0.0326(10) 0.0047(7) -0.0020(8) 0.0001(7) O7 0.0226(10) 0.0191(10) 0.0383(11) -0.0109(8) -0.0049(8) -0.0003(8) O8 0.0298(11) 0.0130(9) 0.0353(10) -0.0018(8) -0.0038(8) -0.0008(8) O10 0.0343(12) 0.0254(11) 0.0310(10) 0.0025(8) 0.0007(9) 0.0038(9) N1 0.0169(10) 0.0137(10) 0.0207(10) -0.0015(8) -0.0020(8) -0.0015(8) N2 0.0214(12) 0.0288(13) 0.0323(12) 0.0030(10) 0.0084(10) -0.0040(10) N3 0.0192(12) 0.0259(13) 0.0358(13) 0.0019(10) 0.0093(10) -0.0011(9) N4 0.0166(11) 0.0324(14) 0.0353(13) 0.0091(10) 0.0070(10) 0.0017(10) C1 0.0211(12) 0.0122(11) 0.0163(10) 0.0000(9) 0.0031(9) -0.0028(9) C2 0.0185(12) 0.0114(12) 0.0204(12) -0.0007(9) 0.0005(9) 0.0006(9) C3 0.0202(13) 0.0125(12) 0.0349(14) 0.0007(10) -0.0047(11) 0.0005(10) C4 0.0199(13) 0.0160(13) 0.0345(14) -0.0024(11) -0.0034(11) -0.0023(10) C5 0.0181(12) 0.0139(12) 0.0234(12) -0.0010(9) 0.0005(10) -0.0030(9) C6 0.0213(13) 0.0113(12) 0.0189(11) 0.0004(9) -0.0011(9) 0.0005(9) C7 0.0170(12) 0.0136(12) 0.0156(10) -0.0010(9) -0.0024(9) -0.0004(9) C8 0.0178(12) 0.0116(12) 0.0244(12) -0.0024(9) 0.0041(9) -0.0023(9) C9 0.0212(13) 0.0253(14) 0.0296(13) -0.0110(11) 0.0057(11) -0.0051(11) C10 0.0253(14) 0.0206(14) 0.0278(13) -0.0047(11) 0.0072(11) -0.0059(11) C11 0.0299(15) 0.0154(13) 0.0281(13) -0.0010(11) -0.0113(11) 0.0057(11) C12 0.0160(12) 0.0154(13) 0.0274(13) -0.0009(10) 0.0000(10) -0.0020(9) C13 0.0303(16) 0.0313(17) 0.0415(17) -0.0030(13) 0.0123(13) -0.0018(13) C14 0.0328(17) 0.0336(18) 0.0464(18) -0.0028(15) 0.0153(14) -0.0073(14) C15 0.0245(15) 0.0417(19) 0.0359(15) 0.0018(14) 0.0064(12) -0.0014(13) C16 0.0323(18) 0.038(2) 0.073(2) 0.0143(18) 0.0266(17) 0.0057(15) C17 0.0304(16) 0.0329(18) 0.058(2) 0.0084(15) 0.0206(15) 0.0025(14) C18 0.0226(14) 0.0390(18) 0.0403(16) 0.0046(14) 0.0106(12) -0.0029(13) C19 0.041(2) 0.055(2) 0.071(3) -0.027(2) 0.0328(19) -0.0131(18) C20 0.0368(19) 0.043(2) 0.066(2) -0.0191(18) 0.0280(17) -0.0157(16) C21 0.0296(17) 0.0324(18) 0.071(2) -0.0069(17) 0.0222(17) -0.0008(14) C22 0.0328(18) 0.0296(17) 0.073(2) -0.0060(17) 0.0208(17) -0.0105(14) C23 0.0273(15) 0.0293(16) 0.0333(15) 0.0043(12) 0.0068(12) 0.0008(12) C24 0.0249(15) 0.0348(18) 0.0381(16) 0.0033(13) 0.0087(12) 0.0063(12) C25 0.0185(15) 0.0420(19) 0.0432(17) 0.0029(15) 0.0089(13) 0.0023(13) C26 0.0289(19) 0.045(2) 0.103(3) 0.026(2) 0.025(2) 0.0018(16) C27 0.0284(18) 0.039(2) 0.086(3) 0.024(2) 0.0229(18) 0.0047(15) O9 0.0150(9) 0.0131(9) 0.0267(9) 0.0005(7) 0.0031(7) -0.0008(6) O1 0.0179(9) 0.0172(9) 0.0255(9) -0.0053(7) 0.0029(7) -0.0049(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 Zn1 O9 1.9224(12) . ? Zn1 O7 1.9523(19) 2_645 ? Zn1 O4 1.9839(19) 3_675 ? Zn1 N4 2.046(2) . ? Zn2 O6 2.0881(19) . ? Zn2 O8 2.093(2) 1_545 ? Zn2 O10 2.117(2) . ? Zn2 O9 2.1333(13) 2_655 ? Zn2 N3 2.155(2) . ? Zn2 O9 2.1590(13) . ? Zn3 O3 2.0189(19) . ? Zn3 O1 2.0560(12) 3_675 ? Zn3 O5 2.0571(18) . ? Zn3 N2 2.136(2) 3_775 ? Zn3 O1 2.2261(13) . ? Zn3 N1 2.308(2) . ? O2 C10 1.229(4) . ? O3 C12 1.260(3) . ? O4 C12 1.262(3) . ? O4 Zn1 1.9839(19) 3_675 ? O5 C1 1.266(3) . ? O6 C1 1.242(3) . ? O7 C8 1.268(3) . ? O7 Zn1 1.9523(19) 2_665 ? O8 C8 1.247(3) . ? O8 Zn2 2.093(2) 1_565 ? N1 C7 1.464(3) . ? N1 C11 1.484(3) . ? N1 C9 1.493(4) . ? N2 C13 1.341(4) . ? N2 C17 1.342(4) . ? N2 Zn3 2.136(2) 3_775 ? N3 C20 1.327(4) . ? N3 C21 1.345(4) . ? N4 C23 1.343(4) . ? N4 C27 1.373(3) . ? C1 C2 1.511(3) . ? C2 C3 1.399(4) . ? C2 C7 1.416(3) . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.384(4) . ? C5 C8 1.504(3) . ? C6 C7 1.392(3) . ? C6 H6 0.9500 . ? C9 C10 1.521(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O1 1.289(3) . ? C11 C12 1.518(4) . ? C11 H11A 0.9890 . ? C11 H11B 0.9106 . ? C13 C14 1.363(4) . ? C13 H13 0.9500 . ? C14 C15 1.406(5) . ? C14 H14 0.9500 . ? C15 C16 1.372(5) . ? C15 C18 1.491(4) . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C22 1.378(5) . ? C18 C19 1.384(5) . ? C19 C20 1.396(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.375(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.368(4) . ? C23 H23 0.9500 . ? C24 C25 1.382(5) . ? C24 H24 0.9500 . ? C25 C26 1.390(5) . ? C25 C25 1.477(6) 2 ? C26 C27 1.358(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? O9 Zn2 2.1333(13) 2_655 ? O1 Zn3 2.0560(12) 3_675 ? 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 O9 Zn1 O7 108.99(7) . 2_645 ? O9 Zn1 O4 120.39(8) . 3_675 ? O7 Zn1 O4 106.24(8) 2_645 3_675 ? O9 Zn1 N4 117.73(8) . . ? O7 Zn1 N4 97.18(9) 2_645 . ? O4 Zn1 N4 103.39(10) 3_675 . ? O6 Zn2 O8 173.55(8) . 1_545 ? O6 Zn2 O10 93.51(8) . . ? O8 Zn2 O10 82.22(8) 1_545 . ? O6 Zn2 O9 89.02(6) . 2_655 ? O8 Zn2 O9 94.72(6) 1_545 2_655 ? O10 Zn2 O9 173.37(7) . 2_655 ? O6 Zn2 N3 86.99(9) . . ? O8 Zn2 N3 97.92(9) 1_545 . ? O10 Zn2 N3 91.78(9) . . ? O9 Zn2 N3 94.47(8) 2_655 . ? O6 Zn2 O9 87.49(6) . . ? O8 Zn2 O9 87.88(7) 1_545 . ? O10 Zn2 O9 92.55(7) . . ? O9 Zn2 O9 81.44(5) 2_655 . ? N3 Zn2 O9 173.18(7) . . ? O3 Zn3 O1 104.91(6) . 3_675 ? O3 Zn3 O5 159.11(8) . . ? O1 Zn3 O5 90.18(6) 3_675 . ? O3 Zn3 N2 96.60(9) . 3_775 ? O1 Zn3 N2 105.05(8) 3_675 3_775 ? O5 Zn3 N2 93.23(9) . 3_775 ? O3 Zn3 O1 85.56(7) . . ? O1 Zn3 O1 77.27(5) 3_675 . ? O5 Zn3 O1 83.76(6) . . ? N2 Zn3 O1 176.24(7) 3_775 . ? O3 Zn3 N1 80.52(7) . . ? O1 Zn3 N1 152.18(7) 3_675 . ? O5 Zn3 N1 79.49(7) . . ? N2 Zn3 N1 101.30(9) 3_775 . ? O1 Zn3 N1 75.98(6) . . ? C12 O3 Zn3 118.05(17) . . ? C12 O4 Zn1 109.03(17) . 3_675 ? C1 O5 Zn3 121.52(16) . . ? C1 O6 Zn2 127.74(16) . . ? C8 O7 Zn1 129.13(18) . 2_665 ? C8 O8 Zn2 134.38(18) . 1_565 ? C7 N1 C11 114.0(2) . . ? C7 N1 C9 109.85(19) . . ? C11 N1 C9 112.4(2) . . ? C7 N1 Zn3 110.49(15) . . ? C11 N1 Zn3 104.99(15) . . ? C9 N1 Zn3 104.64(15) . . ? C13 N2 C17 116.1(3) . . ? C13 N2 Zn3 123.4(2) . 3_775 ? C17 N2 Zn3 120.4(2) . 3_775 ? C20 N3 C21 115.8(3) . . ? C20 N3 Zn2 123.7(2) . . ? C21 N3 Zn2 120.4(2) . . ? C23 N4 C27 118.0(2) . . ? C23 N4 Zn1 123.3(2) . . ? C27 N4 Zn1 118.55(16) . . ? O6 C1 O5 123.1(2) . . ? O6 C1 C2 116.5(2) . . ? O5 C1 C2 120.5(2) . . ? C3 C2 C7 118.0(2) . . ? C3 C2 C1 115.3(2) . . ? C7 C2 C1 126.7(2) . . ? C4 C3 C2 122.4(3) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 C8 121.3(2) . . ? C4 C5 C8 118.1(2) . . ? C5 C6 C7 121.3(2) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 119.0(2) . . ? C6 C7 N1 121.0(2) . . ? C2 C7 N1 120.0(2) . . ? O8 C8 O7 125.7(2) . . ? O8 C8 C5 119.6(2) . . ? O7 C8 C5 114.7(2) . . ? N1 C9 C10 116.8(2) . . ? N1 C9 H9A 108.1 . . ? C10 C9 H9A 108.1 . . ? N1 C9 H9B 108.1 . . ? C10 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? O2 C10 O1 125.5(3) . . ? O2 C10 C9 117.6(3) . . ? O1 C10 C9 116.9(2) . . ? N1 C11 C12 113.9(2) . . ? N1 C11 H11A 103.5 . . ? C12 C11 H11A 113.9 . . ? N1 C11 H11B 108.1 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 107.4 . . ? O3 C12 O4 122.4(2) . . ? O3 C12 C11 121.6(2) . . ? O4 C12 C11 116.0(2) . . ? N2 C13 C14 124.4(3) . . ? N2 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C13 C14 C15 118.9(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 117.0(3) . . ? C16 C15 C18 122.2(3) . . ? C14 C15 C18 120.7(3) . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? N2 C17 C16 123.4(3) . . ? N2 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? C22 C18 C19 116.8(3) . . ? C22 C18 C15 120.8(3) . . ? C19 C18 C15 122.3(3) . . ? C18 C19 C20 119.6(3) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N3 C20 C19 123.7(3) . . ? N3 C20 H20 118.2 . . ? C19 C20 H20 118.2 . . ? N3 C21 C22 124.2(3) . . ? N3 C21 H21 117.9 . . ? C22 C21 H21 117.9 . . ? C21 C22 C18 119.8(3) . . ? C21 C22 H22 120.1 . . ? C18 C22 H22 120.1 . . ? N4 C23 C24 122.6(3) . . ? N4 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 118.0(3) . . ? C24 C25 C25 121.9(2) . 2 ? C26 C25 C25 120.1(2) . 2 ? C27 C26 C25 120.4(3) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 N4 121.0(2) . . ? C26 C27 H27 119.5 . . ? N4 C27 H27 119.5 . . ? Zn1 O9 Zn2 111.14(6) . 2_655 ? Zn1 O9 Zn2 118.67(6) . . ? Zn2 O9 Zn2 98.55(5) 2_655 . ? C10 O1 Zn3 126.39(15) . 3_675 ? C10 O1 Zn3 111.44(14) . . ? Zn3 O1 Zn3 102.73(5) 3_675 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.709 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.195 data_3 _database_code_depnum_ccdc_archive 'CCDC 876732' #TrackingRef 'complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H15 Cd2 N O12' _chemical_formula_sum 'C12 H15 Cd2 N O12' _chemical_formula_weight 590.05 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.761(2) _cell_length_b 10.374(3) _cell_length_c 11.889(3) _cell_angle_alpha 92.286(4) _cell_angle_beta 95.457(2) _cell_angle_gamma 98.643(4) _cell_volume 819.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2122 _cell_measurement_theta_min 2.7027 _cell_measurement_theta_max 27.4778 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 2.664 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9033 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5322 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2783 _reflns_number_gt 2399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0565P)^2^+0.4262P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2783 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 0.97041(5) 0.80956(3) 0.96117(3) 0.01668(14) Uani 1 1 d . . . O1 O 0.6011(5) 0.7048(3) 0.6338(3) 0.0213(8) Uani 1 1 d . . . N1 N 1.1499(6) 0.8562(4) 0.7858(3) 0.0130(8) Uani 1 1 d . . . C1 C 0.7161(7) 0.7717(5) 0.7107(4) 0.0141(10) Uani 1 1 d . . . Cd2 Cd 0.48207(5) 0.49860(3) 0.66251(3) 0.01683(14) Uani 1 1 d . . . O2 O 0.7309(5) 0.7419(3) 0.8123(3) 0.0238(8) Uani 1 1 d . . . C2 C 0.8345(7) 0.8961(5) 0.6767(4) 0.0147(10) Uani 1 1 d . . . O8 O 1.3164(5) 1.2980(3) 0.6321(3) 0.0204(8) Uani 1 1 d . . . O11 O 0.7369(6) 0.6469(4) 1.0318(4) 0.0342(10) Uani 1 1 d . . . O12 O 1.1645(6) 0.7976(4) 1.1376(3) 0.0268(9) Uani 1 1 d . . . O3 O 1.2601(6) 0.5261(3) 0.7900(3) 0.0242(8) Uani 1 1 d . . . C3 C 0.7333(7) 0.9743(5) 0.6070(4) 0.0181(11) Uani 1 1 d . . . H3 H 0.5978 0.9440 0.5779 0.022 Uiso 1 1 calc R . . O4 O 1.1438(6) 0.6451(4) 0.9203(3) 0.0270(9) Uani 1 1 d . . . C4 C 0.8249(7) 1.0955(5) 0.5789(4) 0.0185(11) Uani 1 1 d . . . H4 H 0.7514 1.1496 0.5342 0.022 Uiso 1 1 calc R . . O5 O 1.1827(5) 1.0274(4) 0.9684(3) 0.0216(8) Uani 1 1 d . . . C5 C 1.0272(7) 1.1371(5) 0.6172(4) 0.0156(10) Uani 1 1 d . . . O6 O 1.4664(5) 1.1370(3) 0.9177(3) 0.0227(8) Uani 1 1 d . . . C6 C 1.1320(7) 1.0566(5) 0.6830(4) 0.0144(10) Uani 1 1 d . . . H6 H 1.2704 1.0846 0.7070 0.017 Uiso 1 1 calc R . . O7 O 1.0398(5) 1.3385(3) 0.5288(3) 0.0232(8) Uani 1 1 d . . . C7 C 1.0402(7) 0.9368(5) 0.7144(4) 0.0139(10) Uani 1 1 d . . . C8 C 1.1643(7) 0.7270(5) 0.7350(4) 0.0149(10) Uani 1 1 d . . . H8A H 1.2791 0.7352 0.6886 0.018 Uiso 1 1 calc R . . H8B H 1.0404 0.6958 0.6839 0.018 Uiso 1 1 calc R . . O9 O 0.7083(5) 0.4639(3) 0.5283(3) 0.0206(8) Uani 1 1 d . . . C9 C 1.1921(7) 0.6257(5) 0.8225(4) 0.0178(11) Uani 1 1 d . . . O10 O 0.6922(8) 0.4538(4) 0.8150(4) 0.0485(13) Uani 1 1 d . . . C10 C 1.3505(7) 0.9226(5) 0.8338(4) 0.0164(10) Uani 1 1 d . . . H10A H 1.4305 0.9525 0.7715 0.020 Uiso 1 1 calc R . . H10B H 1.4215 0.8602 0.8763 0.020 Uiso 1 1 calc R . . C11 C 1.3346(7) 1.0394(5) 0.9124(4) 0.0160(10) Uani 1 1 d . . . C12 C 1.1358(7) 1.2684(5) 0.5908(4) 0.0156(10) Uani 1 1 d . . . H12C H 1.1300 0.8366 1.2007 0.019 Uiso 1 1 d R . . H11C H 0.7221 0.5850 1.0814 0.019 Uiso 1 1 d R . . H10C H 0.7587 0.3898 0.8321 0.019 Uiso 1 1 d R . . H10D H 0.7166 0.5071 0.8757 0.019 Uiso 1 1 d R . . H12D H 1.2934 0.8339 1.1354 0.019 Uiso 1 1 d R . . H11D H 0.6548 0.7012 1.0529 0.019 Uiso 1 1 d 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 0.0205(2) 0.0141(2) 0.0163(2) 0.00056(15) 0.00416(15) 0.00415(15) O1 0.0229(19) 0.0144(19) 0.0230(19) 0.0019(15) 0.0011(15) -0.0082(15) N1 0.0123(19) 0.010(2) 0.017(2) 0.0010(16) -0.0016(16) 0.0057(16) C1 0.015(2) 0.013(3) 0.015(2) 0.001(2) 0.0035(19) 0.003(2) Cd2 0.0173(2) 0.0113(2) 0.0214(2) 0.00111(15) 0.00512(15) -0.00130(15) O2 0.027(2) 0.021(2) 0.0216(19) 0.0062(15) 0.0012(16) -0.0057(16) C2 0.016(2) 0.014(3) 0.013(2) -0.0016(19) 0.0013(19) 0.000(2) O8 0.0187(19) 0.0139(18) 0.027(2) 0.0051(15) -0.0011(15) -0.0023(14) O11 0.035(2) 0.030(2) 0.044(2) 0.0235(19) 0.0150(19) 0.0125(19) O12 0.024(2) 0.034(2) 0.0223(19) -0.0020(17) 0.0048(16) 0.0039(17) O3 0.037(2) 0.0113(19) 0.029(2) 0.0058(16) 0.0164(17) 0.0102(16) C3 0.013(2) 0.017(3) 0.022(3) 0.003(2) -0.003(2) 0.001(2) O4 0.044(2) 0.023(2) 0.0203(19) 0.0073(16) 0.0141(17) 0.0167(18) C4 0.018(3) 0.017(3) 0.021(3) 0.007(2) -0.004(2) 0.003(2) O5 0.0224(19) 0.0193(19) 0.0241(19) -0.0023(15) 0.0077(15) 0.0041(15) C5 0.020(3) 0.011(2) 0.015(2) 0.0002(19) 0.004(2) 0.000(2) O6 0.0179(18) 0.022(2) 0.0255(19) -0.0009(16) -0.0006(15) -0.0032(15) C6 0.012(2) 0.016(3) 0.014(2) 0.0010(19) -0.0027(19) -0.0002(19) O7 0.0222(19) 0.019(2) 0.030(2) 0.0140(16) 0.0024(16) 0.0043(16) C7 0.014(2) 0.014(3) 0.013(2) -0.0013(19) 0.0013(19) 0.0018(19) C8 0.021(2) 0.013(3) 0.013(2) 0.0006(19) 0.0036(19) 0.005(2) O9 0.0176(18) 0.0180(19) 0.0268(19) 0.0015(15) 0.0066(15) 0.0017(15) C9 0.016(2) 0.013(3) 0.023(3) 0.002(2) 0.003(2) 0.000(2) O10 0.060(3) 0.031(3) 0.051(3) -0.005(2) -0.027(2) 0.019(2) C10 0.011(2) 0.014(3) 0.025(3) 0.003(2) 0.000(2) 0.0034(19) C11 0.015(2) 0.021(3) 0.012(2) 0.002(2) -0.0019(19) 0.005(2) C12 0.020(3) 0.014(3) 0.013(2) 0.000(2) 0.005(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 Cd1 O4 2.273(4) . ? Cd1 O5 2.283(4) 2_777 ? Cd1 O2 2.294(4) . ? Cd1 O11 2.368(4) . ? Cd1 O12 2.384(4) . ? Cd1 O5 2.482(4) . ? Cd1 N1 2.537(4) . ? O1 C1 1.254(6) . ? O1 Cd2 2.221(3) . ? N1 C7 1.447(6) . ? N1 C8 1.469(6) . ? N1 C10 1.477(6) . ? C1 O2 1.257(6) . ? C1 C2 1.504(7) . ? Cd2 O8 2.209(3) 1_445 ? Cd2 O3 2.271(4) 1_455 ? Cd2 O10 2.302(4) . ? Cd2 O9 2.366(3) . ? Cd2 O9 2.572(4) 2_666 ? C2 C3 1.387(7) . ? C2 C7 1.415(7) . ? O8 C12 1.260(6) . ? O8 Cd2 2.209(3) 1_665 ? O3 C9 1.254(6) . ? O3 Cd2 2.271(4) 1_655 ? C3 C4 1.383(7) . ? O4 C9 1.254(6) . ? C4 C5 1.398(7) . ? O5 C11 1.270(6) . ? O5 Cd1 2.283(4) 2_777 ? C5 C6 1.390(7) . ? C5 C12 1.507(7) . ? O6 C11 1.240(6) . ? C6 C7 1.385(7) . ? O7 C12 1.260(6) . ? C8 C9 1.527(7) . ? O9 Cd2 2.572(4) 2_666 ? C10 C11 1.523(7) . ? 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 Cd1 O5 170.76(13) . 2_777 ? O4 Cd1 O2 91.60(14) . . ? O5 Cd1 O2 96.50(13) 2_777 . ? O4 Cd1 O11 86.05(14) . . ? O5 Cd1 O11 91.80(14) 2_777 . ? O2 Cd1 O11 74.58(14) . . ? O4 Cd1 O12 78.76(13) . . ? O5 Cd1 O12 92.10(13) 2_777 . ? O2 Cd1 O12 157.41(13) . . ? O11 Cd1 O12 84.33(14) . . ? O4 Cd1 O5 112.27(13) . . ? O5 Cd1 O5 67.06(14) 2_777 . ? O2 Cd1 O5 121.13(12) . . ? O11 Cd1 O5 153.89(13) . . ? O12 Cd1 O5 81.45(13) . . ? O4 Cd1 N1 69.80(13) . . ? O5 Cd1 N1 116.60(13) 2_777 . ? O2 Cd1 N1 75.17(12) . . ? O11 Cd1 N1 140.36(14) . . ? O12 Cd1 N1 119.14(13) . . ? O5 Cd1 N1 65.60(12) . . ? C1 O1 Cd2 119.0(3) . . ? C7 N1 C8 115.1(4) . . ? C7 N1 C10 113.5(4) . . ? C8 N1 C10 110.3(4) . . ? C7 N1 Cd1 109.3(3) . . ? C8 N1 Cd1 104.9(3) . . ? C10 N1 Cd1 102.6(3) . . ? O1 C1 O2 123.6(4) . . ? O1 C1 C2 116.4(4) . . ? O2 C1 C2 119.9(4) . . ? O8 Cd2 O1 160.49(13) 1_445 . ? O8 Cd2 O3 85.92(13) 1_445 1_455 ? O1 Cd2 O3 100.93(13) . 1_455 ? O8 Cd2 O10 95.97(15) 1_445 . ? O1 Cd2 O10 102.68(15) . . ? O3 Cd2 O10 85.84(17) 1_455 . ? O8 Cd2 O9 92.46(13) 1_445 . ? O1 Cd2 O9 80.58(13) . . ? O3 Cd2 O9 178.37(12) 1_455 . ? O10 Cd2 O9 94.44(17) . . ? O8 Cd2 O9 83.46(12) 1_445 2_666 ? O1 Cd2 O9 77.19(12) . 2_666 ? O3 Cd2 O9 103.75(13) 1_455 2_666 ? O10 Cd2 O9 170.30(16) . 2_666 ? O9 Cd2 O9 75.93(13) . 2_666 ? C1 O2 Cd1 132.1(3) . . ? C3 C2 C7 119.5(4) . . ? C3 C2 C1 117.4(4) . . ? C7 C2 C1 123.0(4) . . ? C12 O8 Cd2 125.4(3) . 1_665 ? C9 O3 Cd2 131.3(3) . 1_655 ? C4 C3 C2 121.6(5) . . ? C9 O4 Cd1 121.1(3) . . ? C3 C4 C5 119.0(5) . . ? C11 O5 Cd1 127.3(3) . 2_777 ? C11 O5 Cd1 117.7(3) . . ? Cd1 O5 Cd1 112.94(14) 2_777 . ? C6 C5 C4 119.6(4) . . ? C6 C5 C12 118.6(4) . . ? C4 C5 C12 121.8(4) . . ? C7 C6 C5 121.9(4) . . ? C6 C7 C2 118.3(4) . . ? C6 C7 N1 121.1(4) . . ? C2 C7 N1 120.6(4) . . ? N1 C8 C9 113.1(4) . . ? Cd2 O9 Cd2 104.07(13) . 2_666 ? O3 C9 O4 124.2(5) . . ? O3 C9 C8 116.6(4) . . ? O4 C9 C8 119.2(4) . . ? N1 C10 C11 111.3(4) . . ? O6 C11 O5 125.0(5) . . ? O6 C11 C10 119.3(4) . . ? O5 C11 C10 115.7(4) . . ? O7 C12 O8 125.6(4) . . ? O7 C12 C5 117.6(4) . . ? O8 C12 C5 116.8(4) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.657 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.254 data_complex4 _database_code_depnum_ccdc_archive 'CCDC 876733' #TrackingRef 'complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H35 Cd4 N4 O22.50' _chemical_formula_sum 'C34 H35 Cd4 N4 O22.50' _chemical_formula_weight 1309.26 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 P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.0861(6) _cell_length_b 14.2083(3) _cell_length_c 19.2980(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.836(2) _cell_angle_gamma 90.00 _cell_volume 4912.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11961 _cell_measurement_theta_min 2.0370 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2556 _exptl_absorpt_coefficient_mu 1.787 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7164 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30817 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8538 _reflns_number_gt 8106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0636P)^2^+14.0267P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8538 _refine_ls_number_parameters 582 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.16340(2) 0.79502(3) 0.437160(19) 0.03106(11) Uani 1 1 d . . . O1 O 0.2333(2) 0.8484(3) 0.54851(19) 0.0430(9) Uani 1 1 d . . . N1 N 0.3234(2) 0.9709(3) 0.6520(2) 0.0276(8) Uani 1 1 d . . . C1 C 0.1905(3) 0.9191(4) 0.5528(3) 0.0327(11) Uani 1 1 d . . . Cd2 Cd 0.32912(2) 0.79813(3) 0.624455(19) 0.03377(12) Uani 1 1 d . . . O2 O 0.1485(2) 0.9485(3) 0.50154(19) 0.0461(9) Uani 1 1 d . . . N2 N 0.4376(2) 0.5740(3) 0.8929(2) 0.0306(9) Uani 1 1 d . . . C2 C 0.1867(3) 0.9650(3) 0.6227(2) 0.0319(10) Uani 1 1 d . . . Cd3 Cd 0.51193(2) 0.86648(3) 1.02204(2) 0.03668(12) Uani 1 1 d . . . O3 O 0.0954(3) 1.1080(6) 0.8337(3) 0.100(2) Uani 1 1 d . . . N3 N 0.2815(2) 0.7578(3) 0.8673(3) 0.0393(10) Uani 1 1 d . . . C3 C 0.1159(3) 0.9828(4) 0.6395(3) 0.0444(13) Uani 1 1 d . . . H3 H 0.0736 0.9667 0.6069 0.053 Uiso 1 1 calc R . . Cd4 Cd 0.400257(19) 0.72986(2) 0.835553(18) 0.02938(11) Uani 1 1 d . . . O4 O 0.2156(3) 1.1218(4) 0.8559(3) 0.0718(15) Uani 1 1 d . . . N4 N -0.0531(3) 0.7809(3) 1.0188(3) 0.0470(12) Uani 1 1 d . . . C4 C 0.1053(4) 1.0231(5) 0.7024(3) 0.0529(16) Uani 1 1 d . . . H4A H 0.0565 1.0361 0.7128 0.063 Uiso 1 1 calc R . . O5 O 0.4098(2) 0.8908(3) 0.5632(2) 0.0402(9) Uani 1 1 d . . . C5 C 0.1677(4) 1.0442(4) 0.7502(3) 0.0461(14) Uani 1 1 d . . . O6 O 0.4179(2) 1.0187(3) 0.50077(18) 0.0399(8) Uani 1 1 d . . . C6 C 0.1582(5) 1.0945(5) 0.8185(3) 0.0575(18) Uani 1 1 d . . . O7 O 0.3652(2) 0.8214(2) 0.73912(18) 0.0361(8) Uani 1 1 d . . . C7 C 0.2390(3) 1.0267(4) 0.7345(3) 0.0369(12) Uani 1 1 d . . . H7 H 0.2810 1.0413 0.7680 0.044 Uiso 1 1 calc R . . O8 O 0.4185(2) 0.9114(3) 0.82254(19) 0.0451(9) Uani 1 1 d . . . C8 C 0.2499(3) 0.9885(3) 0.6710(2) 0.0296(10) Uani 1 1 d . . . O9 O 0.4235(3) 0.7526(3) 1.0634(2) 0.0595(13) Uani 1 1 d . . . C9 C 0.3396(3) 1.0261(3) 0.5905(2) 0.0304(10) Uani 1 1 d . . . H9A H 0.3616 1.0874 0.6065 0.036 Uiso 1 1 calc R . . H9B H 0.2924 1.0386 0.5595 0.036 Uiso 1 1 calc R . . O10 O 0.4402(2) 0.7585(2) 0.95331(18) 0.0338(8) Uani 1 1 d . . . C10 C 0.3931(3) 0.9747(3) 0.5493(2) 0.0308(10) Uani 1 1 d . . . O11 O 0.1923(3) 0.3654(4) 1.0135(3) 0.0736(15) Uani 1 1 d . . . C11 C 0.3852(3) 0.9814(3) 0.7098(3) 0.0315(10) Uani 1 1 d . . . H11A H 0.3787 1.0411 0.7348 0.038 Uiso 1 1 calc R . . H11B H 0.4329 0.9852 0.6903 0.038 Uiso 1 1 calc R . . O12 O 0.2510(3) 0.3170(3) 0.9294(3) 0.0718(15) Uani 1 1 d . . . C12 C 0.3890(3) 0.9011(4) 0.7612(3) 0.0314(10) Uani 1 1 d . . . O13 O 0.5277(2) 0.7077(3) 0.8424(2) 0.0384(8) Uani 1 1 d . . . C13 C 0.4145(3) 0.7174(4) 1.0039(3) 0.0383(12) Uani 1 1 d . . . O14 O 0.6208(2) 0.6807(3) 0.9261(2) 0.0454(10) Uani 1 1 d . . . C14 C 0.3724(3) 0.6264(3) 0.9913(3) 0.0359(11) Uani 1 1 d . . . O15 O 0.3457(2) 0.6104(3) 0.7678(2) 0.0423(9) Uani 1 1 d . . . C15 C 0.3192(4) 0.6099(4) 1.0357(3) 0.0479(14) Uani 1 1 d . . . H15 H 0.3134 0.6540 1.0716 0.057 Uiso 1 1 calc R . . O16 O 0.3509(4) 0.4624(4) 0.7357(4) 0.121(3) Uani 1 1 d . . . C16 C 0.2748(4) 0.5308(4) 1.0285(3) 0.0515(15) Uani 1 1 d . . . H16 H 0.2384 0.5209 1.0589 0.062 Uiso 1 1 calc R . . O17 O 0.2487(3) 0.6864(3) 0.6608(2) 0.0577(11) Uani 1 1 d . . . C17 C 0.2834(3) 0.4664(4) 0.9775(3) 0.0393(12) Uani 1 1 d . . . O18 O 0.1007(6) 0.6782(8) 0.3483(6) 0.166(4) Uani 1 1 d . . . C18 C 0.2379(3) 0.3769(4) 0.9720(3) 0.0437(13) Uani 1 1 d . . . O19 O 0.5921(3) 0.7501(4) 1.0649(3) 0.0770(15) Uani 1 1 d . . . C19 C 0.3360(3) 0.4815(3) 0.9326(3) 0.0334(11) Uani 1 1 d . . . H19 H 0.3406 0.4371 0.8966 0.040 Uiso 1 1 calc R . . O20 O 0.5237(3) 0.9213(3) 1.1323(2) 0.0500(10) Uani 1 1 d . . . C20 C 0.3824(3) 0.5602(3) 0.9391(3) 0.0299(10) Uani 1 1 d . . . C21 C 0.5145(3) 0.5874(4) 0.9278(3) 0.0348(11) Uani 1 1 d . . . H21A H 0.5423 0.5277 0.9258 0.042 Uiso 1 1 calc R . . H21B H 0.5131 0.6024 0.9777 0.042 Uiso 1 1 calc R . . C22 C 0.5559(3) 0.6650(3) 0.8953(3) 0.0330(11) Uani 1 1 d . . . C23 C 0.4361(3) 0.5094(4) 0.8329(3) 0.0391(12) Uani 1 1 d . . . H23A H 0.4325 0.4439 0.8497 0.047 Uiso 1 1 calc R . . H23B H 0.4837 0.5153 0.8133 0.047 Uiso 1 1 calc R . . C24 C 0.3719(4) 0.5272(4) 0.7749(3) 0.0488(14) Uani 1 1 d . . . C25 C 0.2637(3) 0.8365(4) 0.8995(3) 0.0489(15) Uani 1 1 d . . . H25 H 0.2986 0.8868 0.9040 0.059 Uiso 1 1 calc R . . C26 C 0.1976(4) 0.8484(5) 0.9264(4) 0.0568(17) Uani 1 1 d . . . H26 H 0.1863 0.9068 0.9466 0.068 Uiso 1 1 calc R . . C27 C 0.1474(3) 0.7733(4) 0.9236(4) 0.0478(15) Uani 1 1 d . . . C28 C 0.1663(3) 0.6917(5) 0.8914(4) 0.0553(17) Uani 1 1 d . . . H28 H 0.1337 0.6390 0.8881 0.066 Uiso 1 1 calc R . . C29 C 0.2327(3) 0.6871(4) 0.8639(4) 0.0493(15) Uani 1 1 d . . . H29 H 0.2443 0.6305 0.8415 0.059 Uiso 1 1 calc R . . C30 C 0.0680(4) 0.8394(6) 1.0082(4) 0.077(3) Uani 1 1 d . . . H30 H 0.1061 0.8833 1.0242 0.092 Uiso 1 1 calc R . . C31 C 0.0023(4) 0.8379(7) 1.0380(5) 0.079(3) Uani 1 1 d . . . H31 H -0.0026 0.8811 1.0747 0.095 Uiso 1 1 calc R . . C32 C -0.0466(5) 0.7282(7) 0.9632(6) 0.100(4) Uani 1 1 d . . . H32 H -0.0878 0.6899 0.9452 0.120 Uiso 1 1 calc R . . C33 C 0.0156(5) 0.7257(8) 0.9304(6) 0.109(4) Uani 1 1 d . . . H33 H 0.0162 0.6879 0.8898 0.131 Uiso 1 1 calc R . . C34 C 0.0777(3) 0.7780(4) 0.9561(4) 0.0516(16) Uani 1 1 d . . . O21 O 0.5000 0.8192(5) 1.2500 0.083(2) Uani 1 2 d S . . O22 O 0.3913(8) 0.2935(7) 0.6951(4) 0.173(5) Uani 1 1 d . . . O23 O 0.3356(5) 1.2087(9) 0.8078(5) 0.161(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0307(2) 0.0320(2) 0.0331(2) 0.00617(14) 0.01400(15) 0.00618(14) O1 0.054(2) 0.044(2) 0.0305(18) -0.0080(16) 0.0019(17) 0.0137(19) N1 0.032(2) 0.0275(19) 0.0243(19) 0.0030(16) 0.0084(16) 0.0033(16) C1 0.035(3) 0.032(2) 0.033(3) 0.001(2) 0.011(2) 0.000(2) Cd2 0.0429(2) 0.0280(2) 0.0318(2) -0.00142(14) 0.01000(16) 0.00625(15) O2 0.051(2) 0.051(2) 0.0344(19) -0.0026(18) -0.0011(17) 0.0120(19) N2 0.030(2) 0.028(2) 0.035(2) 0.0033(17) 0.0099(17) -0.0015(17) C2 0.036(3) 0.033(2) 0.028(2) 0.001(2) 0.010(2) 0.005(2) Cd3 0.0438(2) 0.0317(2) 0.0366(2) -0.00291(15) 0.01297(17) -0.00589(16) O3 0.091(4) 0.167(7) 0.045(3) -0.016(3) 0.025(3) 0.066(4) N3 0.030(2) 0.044(3) 0.047(3) 0.001(2) 0.0139(19) 0.001(2) C3 0.040(3) 0.057(3) 0.038(3) -0.004(3) 0.009(2) 0.008(3) Cd4 0.0292(2) 0.02792(19) 0.0321(2) 0.00530(14) 0.00780(15) 0.00174(14) O4 0.094(4) 0.075(3) 0.055(3) -0.035(3) 0.042(3) -0.022(3) N4 0.037(3) 0.047(3) 0.062(3) -0.016(2) 0.026(2) -0.008(2) C4 0.048(3) 0.067(4) 0.048(3) -0.001(3) 0.022(3) 0.013(3) O5 0.049(2) 0.0343(19) 0.042(2) 0.0020(16) 0.0217(17) 0.0094(17) C5 0.062(4) 0.048(3) 0.032(3) -0.001(2) 0.019(3) 0.013(3) O6 0.047(2) 0.045(2) 0.0303(18) 0.0018(16) 0.0133(16) -0.0061(17) C6 0.088(5) 0.056(4) 0.035(3) 0.002(3) 0.031(3) 0.021(4) O7 0.053(2) 0.0252(17) 0.0300(18) 0.0036(14) 0.0059(16) 0.0004(16) C7 0.049(3) 0.037(3) 0.026(2) 0.000(2) 0.011(2) 0.010(2) O8 0.055(2) 0.044(2) 0.033(2) 0.0075(17) -0.0042(18) -0.0080(19) C8 0.036(3) 0.027(2) 0.027(2) 0.0015(19) 0.0098(19) 0.007(2) O9 0.098(4) 0.048(2) 0.036(2) -0.0085(19) 0.021(2) -0.030(2) C9 0.038(3) 0.025(2) 0.030(2) 0.0050(19) 0.011(2) 0.005(2) O10 0.042(2) 0.0267(17) 0.0344(19) 0.0014(14) 0.0096(15) -0.0077(15) C10 0.032(2) 0.031(2) 0.030(2) -0.002(2) 0.006(2) -0.001(2) O11 0.057(3) 0.066(3) 0.104(4) 0.005(3) 0.033(3) -0.026(2) C11 0.035(3) 0.029(2) 0.031(2) 0.003(2) 0.007(2) -0.003(2) O12 0.076(3) 0.044(3) 0.103(4) -0.015(3) 0.039(3) -0.030(2) C12 0.029(2) 0.036(3) 0.030(3) 0.002(2) 0.008(2) 0.005(2) O13 0.0313(19) 0.040(2) 0.046(2) 0.0135(17) 0.0140(16) 0.0005(15) C13 0.048(3) 0.030(3) 0.039(3) -0.002(2) 0.010(2) -0.007(2) O14 0.031(2) 0.038(2) 0.066(3) 0.0150(19) 0.0036(18) -0.0055(16) C14 0.044(3) 0.028(2) 0.038(3) 0.003(2) 0.013(2) -0.006(2) O15 0.049(2) 0.037(2) 0.041(2) -0.0041(16) 0.0069(17) 0.0003(18) C15 0.061(4) 0.038(3) 0.050(3) -0.003(3) 0.027(3) -0.010(3) O16 0.144(6) 0.074(4) 0.122(5) -0.062(4) -0.063(5) 0.039(4) C16 0.056(4) 0.044(3) 0.062(4) 0.003(3) 0.036(3) -0.008(3) O17 0.051(3) 0.060(3) 0.062(3) 0.008(2) 0.009(2) -0.006(2) C17 0.037(3) 0.031(3) 0.051(3) 0.010(2) 0.012(2) -0.004(2) O18 0.152(9) 0.154(9) 0.173(9) -0.038(7) -0.038(7) 0.002(7) C18 0.034(3) 0.036(3) 0.063(4) 0.010(3) 0.014(3) -0.007(2) O19 0.088(4) 0.076(3) 0.068(3) 0.010(3) 0.012(3) 0.027(3) C19 0.035(3) 0.022(2) 0.045(3) 0.004(2) 0.009(2) -0.001(2) O20 0.068(3) 0.048(2) 0.034(2) -0.0043(18) 0.0079(19) -0.010(2) C20 0.029(2) 0.028(2) 0.035(2) 0.008(2) 0.0103(19) -0.0037(19) C21 0.028(2) 0.030(2) 0.047(3) 0.010(2) 0.009(2) -0.001(2) C22 0.029(3) 0.025(2) 0.047(3) 0.005(2) 0.013(2) 0.000(2) C23 0.043(3) 0.030(3) 0.047(3) -0.003(2) 0.017(2) 0.005(2) C24 0.053(4) 0.043(3) 0.049(3) -0.013(3) 0.006(3) 0.007(3) C25 0.038(3) 0.048(3) 0.066(4) -0.012(3) 0.026(3) -0.008(3) C26 0.044(3) 0.053(4) 0.080(5) -0.026(3) 0.031(3) -0.013(3) C27 0.033(3) 0.050(3) 0.066(4) -0.017(3) 0.026(3) -0.006(3) C28 0.036(3) 0.051(4) 0.083(5) -0.016(3) 0.025(3) -0.011(3) C29 0.040(3) 0.046(3) 0.065(4) -0.013(3) 0.020(3) -0.002(3) C30 0.046(4) 0.095(6) 0.097(6) -0.056(5) 0.036(4) -0.037(4) C31 0.044(4) 0.107(6) 0.096(6) -0.064(5) 0.040(4) -0.036(4) C32 0.060(5) 0.103(7) 0.149(9) -0.081(7) 0.060(6) -0.043(5) C33 0.064(5) 0.131(8) 0.145(9) -0.099(8) 0.064(6) -0.048(5) C34 0.036(3) 0.051(3) 0.074(4) -0.017(3) 0.028(3) -0.012(3) O21 0.121(7) 0.058(4) 0.074(5) 0.000 0.025(5) 0.000 O22 0.302(15) 0.137(7) 0.076(5) -0.001(5) 0.018(7) 0.120(9) O23 0.107(6) 0.277(14) 0.098(6) -0.045(7) 0.017(5) -0.035(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 Cd1 O12 2.265(4) 4_565 ? Cd1 O4 2.269(4) 4_575 ? Cd1 N4 2.282(5) 2_556 ? Cd1 O1 2.460(4) . ? Cd1 O18 2.540(9) . ? Cd1 O2 2.542(4) . ? Cd1 O3 2.594(7) 4_575 ? O1 C1 1.277(6) . ? O1 Cd2 2.229(4) . ? N1 C8 1.449(6) . ? N1 C11 1.475(6) . ? N1 C9 1.484(6) . ? N1 Cd2 2.517(4) . ? C1 O2 1.235(6) . ? C1 C2 1.509(7) . ? Cd2 O14 2.191(4) 2_656 ? Cd2 O7 2.245(3) . ? Cd2 O17 2.325(5) . ? Cd2 O5 2.395(4) . ? N2 C20 1.440(6) . ? N2 C21 1.472(6) . ? N2 C23 1.476(7) . ? N2 Cd4 2.527(4) . ? C2 C3 1.386(8) . ? C2 C8 1.413(7) . ? Cd3 O20 2.248(4) . ? Cd3 O19 2.278(5) . ? Cd3 O10 2.308(3) . ? Cd3 O5 2.337(4) 2_656 ? Cd3 O6 2.352(4) 4_576 ? Cd3 O9 2.482(4) . ? Cd3 O6 2.577(4) 2_656 ? Cd3 C13 2.748(5) . ? O3 C6 1.227(9) . ? O3 Cd1 2.594(7) 4_576 ? N3 C29 1.332(8) . ? N3 C25 1.339(8) . ? N3 Cd4 2.347(4) . ? C3 C4 1.380(8) . ? Cd4 O15 2.283(4) . ? Cd4 O7 2.288(3) . ? Cd4 O13 2.312(4) . ? Cd4 O10 2.325(3) . ? Cd4 O8 2.617(4) . ? O4 C6 1.242(9) . ? O4 Cd1 2.269(4) 4_576 ? N4 C31 1.301(8) . ? N4 C32 1.325(9) . ? N4 Cd1 2.282(5) 2_556 ? C4 C5 1.389(9) . ? O5 C10 1.250(6) . ? O5 Cd3 2.337(4) 2_656 ? C5 C7 1.388(8) . ? C5 C6 1.529(8) . ? O6 C10 1.258(6) . ? O6 Cd3 2.352(4) 4_575 ? O6 Cd3 2.577(4) 2_656 ? O7 C12 1.264(6) . ? C7 C8 1.379(7) . ? O8 C12 1.238(6) . ? O9 C13 1.243(7) . ? C9 C10 1.521(7) . ? O10 C13 1.279(7) . ? O11 C18 1.234(8) . ? C11 C12 1.507(7) . ? O12 C18 1.229(8) . ? O12 Cd1 2.265(4) 4_566 ? O13 C22 1.236(6) . ? C13 C14 1.503(7) . ? O14 C22 1.261(6) . ? O14 Cd2 2.191(4) 2_656 ? C14 C15 1.392(8) . ? C14 C20 1.409(7) . ? O15 C24 1.275(7) . ? C15 C16 1.378(8) . ? O16 C24 1.219(8) . ? C16 C17 1.368(9) . ? C17 C19 1.389(8) . ? C17 C18 1.511(7) . ? C19 C20 1.393(7) . ? C21 C22 1.516(7) . ? C23 C24 1.518(8) . ? C25 C26 1.378(8) . ? C26 C27 1.397(9) . ? C27 C28 1.381(9) . ? C27 C34 1.483(8) . ? C28 C29 1.378(9) . ? C30 C34 1.361(9) . ? C30 C31 1.390(9) . ? C32 C33 1.365(11) . ? C33 C34 1.382(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Cd1 O4 87.70(19) 4_565 4_575 ? O12 Cd1 N4 128.14(18) 4_565 2_556 ? O4 Cd1 N4 140.40(19) 4_575 2_556 ? O12 Cd1 O1 89.63(18) 4_565 . ? O4 Cd1 O1 103.33(19) 4_575 . ? N4 Cd1 O1 94.18(18) 2_556 . ? O12 Cd1 O18 75.4(3) 4_565 . ? O4 Cd1 O18 93.6(3) 4_575 . ? N4 Cd1 O18 82.0(3) 2_556 . ? O1 Cd1 O18 157.0(3) . . ? O12 Cd1 O2 139.18(18) 4_565 . ? O4 Cd1 O2 88.45(17) 4_575 . ? N4 Cd1 O2 74.76(17) 2_556 . ? O1 Cd1 O2 52.02(12) . . ? O18 Cd1 O2 145.4(3) . . ? O12 Cd1 O3 125.8(2) 4_565 4_575 ? O4 Cd1 O3 52.39(19) 4_575 4_575 ? N4 Cd1 O3 89.23(18) 2_556 4_575 ? O1 Cd1 O3 129.92(18) . 4_575 ? O18 Cd1 O3 72.9(3) . 4_575 ? O2 Cd1 O3 81.35(19) . 4_575 ? C1 O1 Cd2 129.2(3) . . ? C1 O1 Cd1 93.2(3) . . ? Cd2 O1 Cd1 137.42(17) . . ? C8 N1 C11 114.6(4) . . ? C8 N1 C9 113.5(4) . . ? C11 N1 C9 109.9(4) . . ? C8 N1 Cd2 106.7(3) . . ? C11 N1 Cd2 102.1(3) . . ? C9 N1 Cd2 109.2(3) . . ? O2 C1 O1 121.7(5) . . ? O2 C1 C2 118.2(4) . . ? O1 C1 C2 120.0(4) . . ? O14 Cd2 O1 106.43(14) 2_656 . ? O14 Cd2 O7 117.96(14) 2_656 . ? O1 Cd2 O7 134.15(14) . . ? O14 Cd2 O17 85.87(17) 2_656 . ? O1 Cd2 O17 87.42(16) . . ? O7 Cd2 O17 85.01(15) . . ? O14 Cd2 O5 83.21(14) 2_656 . ? O1 Cd2 O5 88.34(15) . . ? O7 Cd2 O5 106.90(14) . . ? O17 Cd2 O5 166.65(15) . . ? O14 Cd2 N1 150.25(15) 2_656 . ? O1 Cd2 N1 77.04(13) . . ? O7 Cd2 N1 70.32(12) . . ? O17 Cd2 N1 123.87(15) . . ? O5 Cd2 N1 67.23(12) . . ? C1 O2 Cd1 90.4(3) . . ? C20 N2 C21 115.3(4) . . ? C20 N2 C23 117.4(4) . . ? C21 N2 C23 110.8(4) . . ? C20 N2 Cd4 102.9(3) . . ? C21 N2 Cd4 105.5(3) . . ? C23 N2 Cd4 103.0(3) . . ? C3 C2 C8 119.5(5) . . ? C3 C2 C1 116.4(5) . . ? C8 C2 C1 124.1(4) . . ? O20 Cd3 O19 86.25(19) . . ? O20 Cd3 O10 138.35(14) . . ? O19 Cd3 O10 90.35(19) . . ? O20 Cd3 O5 128.81(15) . 2_656 ? O19 Cd3 O5 86.91(18) . 2_656 ? O10 Cd3 O5 92.32(13) . 2_656 ? O20 Cd3 O6 84.13(14) . 4_576 ? O19 Cd3 O6 167.36(17) . 4_576 ? O10 Cd3 O6 91.39(13) . 4_576 ? O5 Cd3 O6 105.53(13) 2_656 4_576 ? O20 Cd3 O9 84.45(14) . . ? O19 Cd3 O9 79.4(2) . . ? O10 Cd3 O9 54.21(13) . . ? O5 Cd3 O9 143.24(13) 2_656 . ? O6 Cd3 O9 91.47(16) 4_576 . ? O20 Cd3 O6 83.45(13) . 2_656 ? O19 Cd3 O6 111.53(19) . 2_656 ? O10 Cd3 O6 135.35(12) . 2_656 ? O5 Cd3 O6 52.83(12) 2_656 2_656 ? O6 Cd3 O6 75.50(14) 4_576 2_656 ? O9 Cd3 O6 163.03(14) . 2_656 ? O20 Cd3 C13 111.33(16) . . ? O19 Cd3 C13 81.5(2) . . ? O10 Cd3 C13 27.59(14) . . ? O5 Cd3 C13 117.63(15) 2_656 . ? O6 Cd3 C13 94.37(16) 4_576 . ? O9 Cd3 C13 26.88(15) . . ? O6 Cd3 C13 161.47(14) 2_656 . ? C6 O3 Cd1 84.8(5) . 4_576 ? C29 N3 C25 116.9(5) . . ? C29 N3 Cd4 118.9(4) . . ? C25 N3 Cd4 123.2(4) . . ? C4 C3 C2 121.7(6) . . ? O15 Cd4 O7 84.64(13) . . ? O15 Cd4 O13 106.33(14) . . ? O7 Cd4 O13 106.68(13) . . ? O15 Cd4 O10 137.96(13) . . ? O7 Cd4 O10 135.25(12) . . ? O13 Cd4 O10 78.07(13) . . ? O15 Cd4 N3 86.30(16) . . ? O7 Cd4 N3 87.39(15) . . ? O13 Cd4 N3 161.64(15) . . ? O10 Cd4 N3 83.63(15) . . ? O15 Cd4 N2 70.64(13) . . ? O7 Cd4 N2 151.97(13) . . ? O13 Cd4 N2 69.55(13) . . ? O10 Cd4 N2 72.30(13) . . ? N3 Cd4 N2 103.51(15) . . ? O15 Cd4 O8 136.72(12) . . ? O7 Cd4 O8 52.12(12) . . ? O13 Cd4 O8 90.13(13) . . ? O10 Cd4 O8 83.96(11) . . ? N3 Cd4 O8 89.42(15) . . ? N2 Cd4 O8 151.22(12) . . ? C6 O4 Cd1 99.9(4) . 4_576 ? C31 N4 C32 115.6(6) . . ? C31 N4 Cd1 121.1(4) . 2_556 ? C32 N4 Cd1 121.9(4) . 2_556 ? C3 C4 C5 118.5(6) . . ? C10 O5 Cd3 98.1(3) . 2_656 ? C10 O5 Cd2 119.0(3) . . ? Cd3 O5 Cd2 137.28(16) 2_656 . ? C7 C5 C4 120.7(5) . . ? C7 C5 C6 119.2(6) . . ? C4 C5 C6 119.9(6) . . ? C10 O6 Cd3 122.5(3) . 4_575 ? C10 O6 Cd3 86.7(3) . 2_656 ? Cd3 O6 Cd3 104.50(14) 4_575 2_656 ? O3 C6 O4 122.7(6) . . ? O3 C6 C5 119.6(7) . . ? O4 C6 C5 117.7(6) . . ? C12 O7 Cd2 120.3(3) . . ? C12 O7 Cd4 101.0(3) . . ? Cd2 O7 Cd4 136.82(16) . . ? C8 C7 C5 121.0(5) . . ? C12 O8 Cd4 86.1(3) . . ? C7 C8 C2 118.6(5) . . ? C7 C8 N1 122.7(4) . . ? C2 C8 N1 118.7(4) . . ? C13 O9 Cd3 88.6(3) . . ? N1 C9 C10 111.9(4) . . ? C13 O10 Cd3 95.7(3) . . ? C13 O10 Cd4 124.7(3) . . ? Cd3 O10 Cd4 138.92(15) . . ? O5 C10 O6 122.3(5) . . ? O5 C10 C9 119.9(4) . . ? O6 C10 C9 117.8(4) . . ? N1 C11 C12 112.6(4) . . ? C18 O12 Cd1 104.0(4) . 4_566 ? O8 C12 O7 120.7(5) . . ? O8 C12 C11 120.9(5) . . ? O7 C12 C11 118.2(4) . . ? C22 O13 Cd4 114.2(3) . . ? O9 C13 O10 120.4(5) . . ? O9 C13 C14 119.7(5) . . ? O10 C13 C14 120.0(5) . . ? O9 C13 Cd3 64.6(3) . . ? O10 C13 Cd3 56.7(2) . . ? C14 C13 Cd3 170.3(4) . . ? C22 O14 Cd2 109.8(3) . 2_656 ? C15 C14 C20 119.7(5) . . ? C15 C14 C13 115.0(5) . . ? C20 C14 C13 125.3(5) . . ? C24 O15 Cd4 120.1(4) . . ? C16 C15 C14 121.2(6) . . ? C17 C16 C15 119.8(5) . . ? C16 C17 C19 120.0(5) . . ? C16 C17 C18 119.9(5) . . ? C19 C17 C18 120.0(5) . . ? O12 C18 O11 123.2(6) . . ? O12 C18 C17 118.5(5) . . ? O11 C18 C17 118.2(6) . . ? C17 C19 C20 121.5(5) . . ? C19 C20 C14 117.8(5) . . ? C19 C20 N2 120.9(5) . . ? C14 C20 N2 121.3(4) . . ? N2 C21 C22 113.2(4) . . ? O13 C22 O14 123.7(5) . . ? O13 C22 C21 121.9(4) . . ? O14 C22 C21 114.4(4) . . ? N2 C23 C24 113.9(4) . . ? O16 C24 O15 123.6(6) . . ? O16 C24 C23 118.2(6) . . ? O15 C24 C23 118.0(5) . . ? N3 C25 C26 123.5(6) . . ? C25 C26 C27 119.0(6) . . ? C28 C27 C26 117.3(5) . . ? C28 C27 C34 120.3(5) . . ? C26 C27 C34 122.3(5) . . ? C29 C28 C27 119.7(6) . . ? N3 C29 C28 123.4(6) . . ? C34 C30 C31 120.0(6) . . ? N4 C31 C30 124.0(6) . . ? N4 C32 C33 124.1(7) . . ? C32 C33 C34 120.0(7) . . ? C30 C34 C33 115.4(6) . . ? C30 C34 C27 123.0(6) . . ? C33 C34 C27 121.3(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.307 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.132