# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Zhong Zhang' _publ_contact_author_email zhangzhong@mailbox.gxnu.edu.cn _publ_section_title ; Structural diversity of transition-metal complexes derived from N-propionic acid functionalized 1,4,7-triazacyclononane: From enchanting cluster motifs to unprecedented homometallic polymeric networks ; loop_ _publ_author_name 'Zhong Zhang' 'Jian Lu' 'Di Wu' 'Zi Chen' 'Fu Liang' 'Zhi Wang' # Attachment '- zzcomplexes CIF.txt' data_1 #TrackingRef '- zzcomplexes CIF.txt' _database_code_depnum_ccdc_archive 'CCDC 831022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H60 Cu5 N6 O18, 4(Cl O4)' _chemical_formula_sum 'C30 H60 Cl4 Cu5 N6 O34' _chemical_formula_weight 1508.34 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 _symmetry_space_group_name_Hall '-P 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' _cell_length_a 10.3966(11) _cell_length_b 10.3966(11) _cell_length_c 27.848(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2606.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 18233 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1534 _exptl_absorpt_coefficient_mu 2.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4326 _exptl_absorpt_correction_T_max 0.5271 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21499 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1699 _reflns_number_gt 1303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+1.9500P] 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 1699 _refine_ls_number_parameters 133 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.171 _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 Cu1 Cu 0.6667 0.3333 0.13364(3) 0.0289(4) Uani 1 3 d S . . Cu2 Cu 0.50599(9) 0.50599(9) 0.2500 0.0422(4) Uani 1 2 d S . . C1 C 0.5148(7) 0.1042(7) 0.0652(2) 0.0500(16) Uani 1 1 d . . . H1A H 0.4491 0.0578 0.0381 0.060 Uiso 1 1 calc R . . H1B H 0.4921 0.0281 0.0892 0.060 Uiso 1 1 calc R . . C2 C 0.4928(7) 0.3256(7) 0.04884(19) 0.0476(15) Uani 1 1 d . . . H2A H 0.3931 0.3069 0.0426 0.057 Uiso 1 1 calc R . . H2B H 0.5322 0.3106 0.0191 0.057 Uiso 1 1 calc R . . C3 C 0.3393(6) 0.1402(7) 0.1108(3) 0.0484(16) Uani 1 1 d . . . H3A H 0.3423 0.0749 0.1351 0.058 Uiso 1 1 calc R . . H3B H 0.2631 0.0790 0.0877 0.058 Uiso 1 1 calc R . . C4 C 0.2966(6) 0.2456(7) 0.1345(2) 0.0416(14) Uani 1 1 d . . . H4A H 0.2951 0.3111 0.1100 0.050 Uiso 1 1 calc R . . H4B H 0.1964 0.1873 0.1468 0.050 Uiso 1 1 calc R . . C5 C 0.3960(6) 0.3405(6) 0.17506(19) 0.0376(13) Uani 1 1 d . . . Cl1 Cl 0.3333 0.6667 0.09318(11) 0.0565(8) Uani 1 3 d SD . . Cl2 Cl 1.0000 1.0000 0.2500 0.0495(10) Uani 1 6 d SD . . Cl3 Cl 0.0000 1.0000 0.0000 0.0783(15) Uani 1 6 d S . . N1 N 0.4864(6) 0.2181(5) 0.08560(16) 0.0414(12) Uani 1 1 d . . . O1 O 0.5252(4) 0.3633(4) 0.18031(13) 0.0370(9) Uani 1 1 d . . . O2 O 0.3462(4) 0.3993(5) 0.20331(15) 0.0475(10) Uani 1 1 d . . . O3 O 0.5866(8) 0.6833(5) 0.2108(3) 0.116(3) Uani 1 1 d . . . H3C H 0.5680 0.7380 0.1926 0.175 Uiso 1 1 d R . . H3D H 0.6672 0.6891 0.2015 0.175 Uiso 1 1 d R . . O11 O 0.2789(8) 0.5231(8) 0.0728(3) 0.118(3) Uani 1 1 d D . . O12 O 0.3333 0.6667 0.1434(3) 0.180(8) Uani 1 3 d SD . . O21 O 1.0000 1.0000 0.1991(4) 0.124(10) Uani 0.50 3 d SPD . . O22 O 0.8788(12) 0.8712(13) 0.2250(4) 0.090(4) Uani 0.50 1 d P . . O31 O 0.0000 1.0000 0.0520(10) 0.115(9) Uani 0.50 3 d SP . . O32 O 0.068(3) 0.913(2) 0.0134(7) 0.142(7) Uani 0.50 1 d P . . 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 Cu1 0.0344(5) 0.0344(5) 0.0177(5) 0.000 0.000 0.0172(2) Cu2 0.0362(5) 0.0362(5) 0.0559(7) -0.0039(2) 0.0039(2) 0.0194(5) C1 0.059(4) 0.057(4) 0.035(3) -0.018(3) -0.020(3) 0.030(3) C2 0.056(4) 0.063(4) 0.026(3) 0.003(3) -0.009(3) 0.031(3) C3 0.040(3) 0.046(4) 0.047(4) -0.001(3) -0.008(3) 0.013(3) C4 0.025(3) 0.050(4) 0.042(3) 0.004(3) -0.007(2) 0.013(3) C5 0.031(3) 0.045(3) 0.037(3) 0.013(3) 0.005(2) 0.020(3) Cl1 0.0569(11) 0.0569(11) 0.0556(17) 0.000 0.000 0.0284(5) Cl2 0.0350(12) 0.0350(12) 0.078(3) 0.000 0.000 0.0175(6) Cl3 0.085(2) 0.085(2) 0.065(3) 0.000 0.000 0.0423(12) N1 0.051(3) 0.049(3) 0.032(2) -0.004(2) -0.011(2) 0.031(2) O1 0.032(2) 0.041(2) 0.040(2) -0.0059(17) -0.0081(17) 0.0196(18) O2 0.038(2) 0.067(3) 0.046(2) 0.002(2) 0.0051(19) 0.032(2) O3 0.155(6) 0.040(3) 0.162(6) 0.034(3) 0.107(5) 0.055(4) O11 0.114(5) 0.087(5) 0.144(6) -0.026(5) -0.050(5) 0.043(4) O12 0.231(14) 0.231(14) 0.080(9) 0.000 0.000 0.115(7) O21 0.137(16) 0.137(16) 0.098(19) 0.000 0.000 0.068(8) O22 0.053(6) 0.067(7) 0.132(11) -0.026(7) -0.023(7) 0.016(6) O31 0.122(14) 0.122(14) 0.103(19) 0.000 0.000 0.061(7) O32 0.168(18) 0.119(14) 0.160(18) 0.019(12) -0.003(14) 0.086(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 Cu1 O1 2.099(4) 3_665 ? Cu1 O1 2.099(4) 2_655 ? Cu1 O1 2.099(4) . ? Cu1 N1 2.120(5) 2_655 ? Cu1 N1 2.120(5) . ? Cu1 N1 2.120(5) 3_665 ? Cu2 O3 1.936(5) 4 ? Cu2 O3 1.936(5) . ? Cu2 O2 1.959(4) . ? Cu2 O2 1.959(4) 4 ? C1 N1 1.470(8) . ? C1 C2 1.517(9) 2_655 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N1 1.492(7) . ? C2 C1 1.517(9) 3_665 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.499(8) . ? C3 C4 1.524(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.516(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O1 1.250(6) . ? C5 O2 1.257(7) . ? Cl1 O12 1.398(9) . ? Cl1 O11 1.424(6) 3_565 ? Cl1 O11 1.424(6) 2_665 ? Cl1 O11 1.424(6) . ? Cl2 O21 1.417(10) . ? Cl2 O21 1.417(10) 4 ? Cl2 O22 1.475(10) . ? Cl2 O22 1.475(10) 3_675 ? Cl2 O22 1.475(10) 6_675 ? Cl2 O22 1.475(10) 4 ? Cl2 O22 1.475(10) 5_765 ? Cl2 O22 1.475(10) 2_765 ? Cl3 O32 1.446(17) 2_675 ? Cl3 O32 1.446(17) 3_465 ? Cl3 O32 1.446(17) 8_455 ? Cl3 O32 1.446(17) 9_665 ? Cl3 O32 1.446(17) . ? Cl3 O32 1.446(17) 7_575 ? Cl3 O31 1.45(3) 7_575 ? Cl3 O31 1.45(3) . ? O3 H3C 0.8522 . ? O3 H3D 0.8504 . ? O21 O22 1.488(12) 3_675 ? O21 O22 1.488(12) 2_765 ? O22 O22 1.40(2) 4 ? O31 O32 1.76(2) 3_465 ? O31 O32 1.76(2) 2_675 ? O32 O32 1.58(2) 8_455 ? O32 O32 1.58(2) 9_665 ? 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 Cu1 O1 85.71(14) 3_665 2_655 ? O1 Cu1 O1 85.71(14) 3_665 . ? O1 Cu1 O1 85.71(14) 2_655 . ? O1 Cu1 N1 101.36(16) 3_665 2_655 ? O1 Cu1 N1 89.29(17) 2_655 2_655 ? O1 Cu1 N1 171.03(16) . 2_655 ? O1 Cu1 N1 171.03(16) 3_665 . ? O1 Cu1 N1 101.36(16) 2_655 . ? O1 Cu1 N1 89.29(17) . . ? N1 Cu1 N1 84.4(2) 2_655 . ? O1 Cu1 N1 89.29(17) 3_665 3_665 ? O1 Cu1 N1 171.03(16) 2_655 3_665 ? O1 Cu1 N1 101.36(16) . 3_665 ? N1 Cu1 N1 84.4(2) 2_655 3_665 ? N1 Cu1 N1 84.4(2) . 3_665 ? O3 Cu2 O3 92.4(5) 4 . ? O3 Cu2 O2 166.86(19) 4 . ? O3 Cu2 O2 90.3(3) . . ? O3 Cu2 O2 90.3(3) 4 4 ? O3 Cu2 O2 166.86(19) . 4 ? O2 Cu2 O2 90.0(3) . 4 ? N1 C1 C2 112.7(5) . 2_655 ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 2_655 . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 2_655 . ? H1A C1 H1B 107.8 . . ? N1 C2 C1 111.7(4) . 3_665 ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 3_665 . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 3_665 . ? H2A C2 H2B 107.9 . . ? N1 C3 C4 113.5(5) . . ? N1 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 116.3(5) . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4B 108.2 . . ? C3 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? O1 C5 O2 120.0(5) . . ? O1 C5 C4 121.9(5) . . ? O2 C5 C4 118.0(5) . . ? O12 Cl1 O11 113.5(4) . 3_565 ? O12 Cl1 O11 113.5(4) . 2_665 ? O11 Cl1 O11 105.1(4) 3_565 2_665 ? O12 Cl1 O11 113.5(4) . . ? O11 Cl1 O11 105.1(4) 3_565 . ? O11 Cl1 O11 105.1(4) 2_665 . ? O21 Cl2 O21 180.000(1) . 4 ? O21 Cl2 O22 61.9(5) . . ? O21 Cl2 O22 118.1(5) 4 . ? O21 Cl2 O22 61.9(5) . 3_675 ? O21 Cl2 O22 118.1(5) 4 3_675 ? O22 Cl2 O22 99.6(6) . 3_675 ? O21 Cl2 O22 118.1(5) . 6_675 ? O21 Cl2 O22 61.9(5) 4 6_675 ? O22 Cl2 O22 132.8(10) . 6_675 ? O22 Cl2 O22 56.5(9) 3_675 6_675 ? O21 Cl2 O22 118.1(5) . 4 ? O21 Cl2 O22 61.9(5) 4 4 ? O22 Cl2 O22 56.5(9) . 4 ? O22 Cl2 O22 122.6(11) 3_675 4 ? O22 Cl2 O22 99.6(6) 6_675 4 ? O21 Cl2 O22 118.1(5) . 5_765 ? O21 Cl2 O22 61.9(5) 4 5_765 ? O22 Cl2 O22 122.6(11) . 5_765 ? O22 Cl2 O22 132.8(10) 3_675 5_765 ? O22 Cl2 O22 99.6(6) 6_675 5_765 ? O22 Cl2 O22 99.6(6) 4 5_765 ? O21 Cl2 O22 61.9(5) . 2_765 ? O21 Cl2 O22 118.1(5) 4 2_765 ? O22 Cl2 O22 99.6(6) . 2_765 ? O22 Cl2 O22 99.6(6) 3_675 2_765 ? O22 Cl2 O22 122.6(11) 6_675 2_765 ? O22 Cl2 O22 132.8(10) 4 2_765 ? O22 Cl2 O22 56.5(9) 5_765 2_765 ? O32 Cl3 O32 113.6(7) 2_675 3_465 ? O32 Cl3 O32 180.0(15) 2_675 8_455 ? O32 Cl3 O32 66.4(7) 3_465 8_455 ? O32 Cl3 O32 66.4(7) 2_675 9_665 ? O32 Cl3 O32 180(3) 3_465 9_665 ? O32 Cl3 O32 113.6(7) 8_455 9_665 ? O32 Cl3 O32 113.6(7) 2_675 . ? O32 Cl3 O32 113.6(7) 3_465 . ? O32 Cl3 O32 66.4(7) 8_455 . ? O32 Cl3 O32 66.4(7) 9_665 . ? O32 Cl3 O32 66.4(7) 2_675 7_575 ? O32 Cl3 O32 66.4(7) 3_465 7_575 ? O32 Cl3 O32 113.6(7) 8_455 7_575 ? O32 Cl3 O32 113.6(7) 9_665 7_575 ? O32 Cl3 O32 180.0(15) . 7_575 ? O32 Cl3 O31 105.0(8) 2_675 7_575 ? O32 Cl3 O31 105.0(8) 3_465 7_575 ? O32 Cl3 O31 75.0(8) 8_455 7_575 ? O32 Cl3 O31 75.0(8) 9_665 7_575 ? O32 Cl3 O31 105.0(8) . 7_575 ? O32 Cl3 O31 75.0(8) 7_575 7_575 ? O32 Cl3 O31 75.0(8) 2_675 . ? O32 Cl3 O31 75.0(8) 3_465 . ? O32 Cl3 O31 105.0(8) 8_455 . ? O32 Cl3 O31 105.0(8) 9_665 . ? O32 Cl3 O31 75.0(8) . . ? O32 Cl3 O31 105.0(8) 7_575 . ? O31 Cl3 O31 180.000(2) 7_575 . ? C1 N1 C2 112.7(5) . . ? C1 N1 C3 107.9(5) . . ? C2 N1 C3 112.2(5) . . ? C1 N1 Cu1 102.8(3) . . ? C2 N1 Cu1 108.3(4) . . ? C3 N1 Cu1 112.7(3) . . ? C5 O1 Cu1 131.7(4) . . ? C5 O2 Cu2 104.6(3) . . ? Cu2 O3 H3C 146.7 . . ? Cu2 O3 H3D 100.4 . . ? H3C O3 H3D 108.4 . . ? Cl2 O21 O22 61.0(5) . 3_675 ? Cl2 O21 O22 61.0(5) . 2_765 ? O22 O21 O22 98.5(7) 3_675 2_765 ? O22 O22 Cl2 61.8(5) 4 . ? Cl3 O31 O32 52.4(9) . 3_465 ? Cl3 O31 O32 52.4(9) . 2_675 ? O32 O31 O32 86.7(13) 3_465 2_675 ? Cl3 O32 O32 56.8(3) . 8_455 ? Cl3 O32 O32 56.8(3) . 9_665 ? O32 O32 O32 99.5(17) 8_455 9_665 ? 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 C3 C4 C5 -64.1(7) . . . . ? C3 C4 C5 O1 19.3(8) . . . . ? C3 C4 C5 O2 -162.1(5) . . . . ? C2 C1 N1 C2 68.8(7) 2_655 . . . ? C2 C1 N1 C3 -166.8(5) 2_655 . . . ? C2 C1 N1 Cu1 -47.6(5) 2_655 . . . ? C1 C2 N1 C1 -131.1(6) 3_665 . . . ? C1 C2 N1 C3 106.9(6) 3_665 . . . ? C1 C2 N1 Cu1 -18.1(6) 3_665 . . . ? C4 C3 N1 C1 179.0(5) . . . . ? C4 C3 N1 C2 -56.3(6) . . . . ? C4 C3 N1 Cu1 66.2(5) . . . . ? O1 Cu1 N1 C1 -59.6(4) 2_655 . . . ? O1 Cu1 N1 C1 -145.1(4) . . . . ? N1 Cu1 N1 C1 28.6(4) 2_655 . . . ? N1 Cu1 N1 C1 113.5(3) 3_665 . . . ? O1 Cu1 N1 C2 -179.1(4) 2_655 . . . ? O1 Cu1 N1 C2 95.4(4) . . . . ? N1 Cu1 N1 C2 -91.0(3) 2_655 . . . ? N1 Cu1 N1 C2 -6.1(4) 3_665 . . . ? O1 Cu1 N1 C3 56.3(4) 2_655 . . . ? O1 Cu1 N1 C3 -29.2(4) . . . . ? N1 Cu1 N1 C3 144.4(5) 2_655 . . . ? N1 Cu1 N1 C3 -130.7(5) 3_665 . . . ? O2 C5 O1 Cu1 -162.7(4) . . . . ? C4 C5 O1 Cu1 15.8(8) . . . . ? O1 Cu1 O1 C5 162.6(5) 3_665 . . . ? O1 Cu1 O1 C5 -111.4(5) 2_655 . . . ? N1 Cu1 O1 C5 -9.9(5) . . . . ? N1 Cu1 O1 C5 74.2(5) 3_665 . . . ? O1 C5 O2 Cu2 -2.6(6) . . . . ? C4 C5 O2 Cu2 178.8(4) . . . . ? O3 Cu2 O2 C5 -10.5(13) 4 . . . ? O3 Cu2 O2 C5 91.3(4) . . . . ? O2 Cu2 O2 C5 -101.8(4) 4 . . . ? O22 Cl2 O21 O22 120.000(9) . . . 3_675 ? O22 Cl2 O21 O22 -6.0(12) 6_675 . . 3_675 ? O22 Cl2 O21 O22 114.0(12) 4 . . 3_675 ? O22 Cl2 O21 O22 -126.0(12) 5_765 . . 3_675 ? O22 Cl2 O21 O22 -120.000(8) 2_765 . . 3_675 ? O22 Cl2 O21 O22 -120.000(3) . . . 2_765 ? O22 Cl2 O21 O22 120.000(3) 3_675 . . 2_765 ? O22 Cl2 O21 O22 114.0(12) 6_675 . . 2_765 ? O22 Cl2 O21 O22 -126.0(12) 4 . . 2_765 ? O22 Cl2 O21 O22 -6.0(12) 5_765 . . 2_765 ? O21 Cl2 O22 O22 -173.6(13) . . . 4 ? O21 Cl2 O22 O22 6.4(13) 4 . . 4 ? O22 Cl2 O22 O22 -122.8(14) 3_675 . . 4 ? O22 Cl2 O22 O22 -70.1(9) 6_675 . . 4 ? O22 Cl2 O22 O22 79.3(10) 5_765 . . 4 ? O22 Cl2 O22 O22 135.6(13) 2_765 . . 4 ? O32 Cl3 O31 O32 120.000(1) 2_675 . . 3_465 ? O32 Cl3 O31 O32 -60.000(1) 8_455 . . 3_465 ? O32 Cl3 O31 O32 180.0 9_665 . . 3_465 ? O32 Cl3 O31 O32 -120.0 . . . 3_465 ? O32 Cl3 O31 O32 60.0 7_575 . . 3_465 ? O32 Cl3 O31 O32 -120.000(4) 3_465 . . 2_675 ? O32 Cl3 O31 O32 180.000(4) 8_455 . . 2_675 ? O32 Cl3 O31 O32 60.000(5) 9_665 . . 2_675 ? O32 Cl3 O31 O32 120.000(3) . . . 2_675 ? O32 Cl3 O31 O32 -60.000(4) 7_575 . . 2_675 ? O32 Cl3 O32 O32 180.000(4) 2_675 . . 8_455 ? O32 Cl3 O32 O32 48(2) 3_465 . . 8_455 ? O32 Cl3 O32 O32 -132(2) 9_665 . . 8_455 ? O31 Cl3 O32 O32 -65.9(11) 7_575 . . 8_455 ? O31 Cl3 O32 O32 114.1(11) . . . 8_455 ? O32 Cl3 O32 O32 -48(2) 2_675 . . 9_665 ? O32 Cl3 O32 O32 180.000(3) 3_465 . . 9_665 ? O32 Cl3 O32 O32 132(2) 8_455 . . 9_665 ? O31 Cl3 O32 O32 65.9(11) 7_575 . . 9_665 ? O31 Cl3 O32 O32 -114.1(11) . . . 9_665 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.809 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.094 data_2 #TrackingRef '- zzcomplexes CIF.txt' _database_code_depnum_ccdc_archive 'CCDC 831023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H132 N12 O42 Zn9, 9(H2 O), 6(Cl O4)' _chemical_formula_sum 'C60 H150 Cl6 N12 O75 Zn9' _chemical_formula_weight 3040.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C2/m ' _symmetry_space_group_name_Hall '-C 2y ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.8299(16) _cell_length_b 28.9620(18) _cell_length_c 15.5709(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.01(2) _cell_angle_gamma 90.00 _cell_volume 5637.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3735 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 23.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3132 _exptl_absorpt_coefficient_mu 2.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5859 _exptl_absorpt_correction_T_max 0.6506 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25925 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5655 _reflns_number_gt 4988 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.9900P] 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 5655 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 C1 C 0.6297(3) 0.18920(14) 0.8068(3) 0.0374(8) Uani 1 1 d . . . H1A H 0.6139 0.2165 0.8376 0.045 Uiso 1 1 calc R . . H1B H 0.5680 0.1689 0.7983 0.045 Uiso 1 1 calc R . . C2 C 0.6476(3) 0.20283(14) 0.7201(3) 0.0397(9) Uani 1 1 d . . . H2A H 0.6939 0.2297 0.7275 0.048 Uiso 1 1 calc R . . H2B H 0.5796 0.2116 0.6822 0.048 Uiso 1 1 calc R . . C3 C 0.7883(3) 0.18328(12) 0.6428(2) 0.0329(8) Uani 1 1 d . . . H3A H 0.7662 0.2102 0.6063 0.039 Uiso 1 1 calc R . . H3B H 0.8105 0.1598 0.6063 0.039 Uiso 1 1 calc R . . C4 C 0.8822(3) 0.19596(14) 0.7171(3) 0.0411(9) Uani 1 1 d . . . H4A H 0.9451 0.2006 0.6933 0.049 Uiso 1 1 calc R . . H4B H 0.8668 0.2248 0.7434 0.049 Uiso 1 1 calc R . . C5 C 0.9206(3) 0.17831(14) 0.8759(3) 0.0387(9) Uani 1 1 d . . . H5A H 0.9732 0.2029 0.8835 0.046 Uiso 1 1 calc R . . H5B H 0.9474 0.1544 0.9189 0.046 Uiso 1 1 calc R . . C6 C 0.8133(3) 0.19744(15) 0.8914(3) 0.0454(10) Uani 1 1 d . . . H6A H 0.8211 0.2034 0.9539 0.054 Uiso 1 1 calc R . . H6B H 0.7977 0.2266 0.8606 0.054 Uiso 1 1 calc R . . C7 C 0.6907(3) 0.14055(14) 0.9354(3) 0.0373(8) Uani 1 1 d . . . H7A H 0.6354 0.1184 0.9109 0.045 Uiso 1 1 calc R . . H7B H 0.6601 0.1626 0.9697 0.045 Uiso 1 1 calc R . . C8 C 0.7817(3) 0.11527(14) 0.9970(3) 0.0417(9) Uani 1 1 d . . . H8A H 0.8348 0.1381 1.0230 0.050 Uiso 1 1 calc R . . H8B H 0.7534 0.1023 1.0445 0.050 Uiso 1 1 calc R . . C9 C 0.8391(3) 0.07698(13) 0.9603(2) 0.0326(7) Uani 1 1 d . . . C10 C 0.6205(3) 0.14239(13) 0.6042(2) 0.0351(8) Uani 1 1 d . . . H10A H 0.6590 0.1187 0.5799 0.042 Uiso 1 1 calc R . . H10B H 0.5944 0.1647 0.5579 0.042 Uiso 1 1 calc R . . C11 C 0.5244(3) 0.12002(15) 0.6305(3) 0.0479(10) Uani 1 1 d . . . H11A H 0.4868 0.1440 0.6549 0.057 Uiso 1 1 calc R . . H11B H 0.4764 0.1091 0.5771 0.057 Uiso 1 1 calc R . . C12 C 0.5436(3) 0.08083(14) 0.6948(3) 0.0363(8) Uani 1 1 d . . . C13 C 0.9996(3) 0.12902(13) 0.7811(3) 0.0352(8) Uani 1 1 d . . . H13A H 1.0058 0.1047 0.8248 0.042 Uiso 1 1 calc R . . H13B H 1.0642 0.1475 0.7962 0.042 Uiso 1 1 calc R . . C14 C 0.9941(3) 0.10695(14) 0.6920(3) 0.0392(9) Uani 1 1 d . . . H14A H 1.0608 0.0906 0.6948 0.047 Uiso 1 1 calc R . . H14B H 0.9907 0.1316 0.6491 0.047 Uiso 1 1 calc R . . C15 C 0.9022(3) 0.07336(13) 0.6563(2) 0.0345(8) Uani 1 1 d . . . Cl1 Cl 0.5000 0.27348(5) 0.5000 0.0394(3) Uani 1 2 d S . . Cl2 Cl 0.68400(8) 0.16521(4) 0.19217(7) 0.0461(2) Uani 1 1 d . . . N1 N 0.7222(3) 0.16561(10) 0.8613(2) 0.0359(7) Uani 1 1 d . . . N2 N 0.6962(2) 0.16588(11) 0.6763(2) 0.0350(7) Uani 1 1 d . . . N3 N 0.9053(3) 0.15922(11) 0.7869(2) 0.0351(7) Uani 1 1 d . . . O1 O 0.83188(19) 0.07421(9) 0.87690(17) 0.0351(6) Uani 1 1 d . . . O2 O 0.8919(2) 0.04968(9) 1.01517(17) 0.0378(6) Uani 1 1 d . . . O3 O 0.6324(2) 0.07846(9) 0.75289(18) 0.0380(6) Uani 1 1 d . . . O4 O 0.4711(2) 0.05149(10) 0.69085(18) 0.0403(6) Uani 1 1 d . . . O5 O 0.8212(2) 0.07354(8) 0.69011(17) 0.0356(6) Uani 1 1 d . . . O6 O 0.91245(19) 0.04908(8) 0.59291(16) 0.0309(5) Uani 1 1 d . . . O7 O 1.0482(3) 0.0000 1.1388(2) 0.0327(8) Uani 1 2 d S . . H7C H 1.1048 0.0158 1.1570 0.049 Uiso 0.50 1 d PR . . H7D H 1.0634 -0.0271 1.1588 0.049 Uiso 0.50 1 d PR . . O8 O 0.6232(3) 0.0000 0.8367(2) 0.0393(8) Uani 1 2 d S . . H8C H 0.6519 0.0240 0.8205 0.059 Uiso 0.50 1 d PR . . H8D H 0.6531 -0.0238 0.8212 0.059 Uiso 0.50 1 d PR . . O9 O 0.2998(3) 0.0000 0.7280(2) 0.0377(8) Uani 1 2 d S . . H9C H 0.2742 -0.0250 0.7431 0.057 Uiso 0.50 1 d PR . . H9D H 0.2723 0.0221 0.7513 0.057 Uiso 0.50 1 d PR . . O10 O 0.4417(2) -0.04997(10) 0.87175(19) 0.0451(7) Uani 1 1 d . . . H10C H 0.3762 -0.0575 0.8635 0.068 Uiso 1 1 d R . . H10D H 0.4631 -0.0393 0.9236 0.068 Uiso 1 1 d R . . O11 O 0.7110(3) 0.0000 0.6145(2) 0.0311(7) Uani 1 2 d S . . H11C H 0.7368 0.0192 0.6550 0.047 Uiso 0.50 1 d PR . . H11D H 0.7113 -0.0262 0.6392 0.047 Uiso 0.50 1 d PR . . O12 O 0.7133(2) 0.05058(9) 0.45499(18) 0.0370(6) Uani 1 1 d . . . H12C H 0.7133 0.0735 0.4891 0.056 Uiso 1 1 d R . . H12D H 0.7425 0.0594 0.4140 0.056 Uiso 1 1 d R . . O13 O 0.8990(3) 0.0000 0.4274(2) 0.0352(8) Uani 1 2 d S . . H13C H 0.8696 -0.0160 0.3828 0.053 Uiso 0.50 1 d PR . . H13D H 0.9572 -0.0128 0.4535 0.053 Uiso 0.50 1 d PR . . O14 O 0.3373(3) 1.0000 0.9788(2) 0.0360(8) Uani 1 2 d S . . H14C H 0.3253 0.9827 1.0197 0.054 Uiso 0.50 1 d PR . . H14D H 0.2783 1.0100 0.9481 0.054 Uiso 0.50 1 d PR . . O15 O 0.7824(2) 0.13796(9) 0.43022(18) 0.0381(6) Uani 1 1 d . . . H15C H 0.7310 0.1534 0.3994 0.057 Uiso 1 1 d R . . H15D H 0.8335 0.1367 0.4038 0.057 Uiso 1 1 d R . . O16 O 0.1449(4) 0.0000 0.8220(3) 0.0514(11) Uani 1 2 d S . . H16C H 0.1427 -0.0052 0.8753 0.077 Uiso 0.50 1 d PR . . H16D H 0.0853 0.0110 0.7945 0.077 Uiso 0.50 1 d PR . . O17 O 0.5000 1.0000 0.5000 0.0438(13) Uani 1 4 d S . . H17C H 0.4546 1.0089 0.4545 0.066 Uiso 0.25 1 d PR . . H17D H 0.5564 0.9909 0.4851 0.066 Uiso 0.25 1 d PR . . O21 O 0.5485(2) 0.30119(11) 0.5604(2) 0.0510(8) Uani 1 1 d . . . O22 O 0.5675(2) 0.24635(10) 0.4624(2) 0.0432(7) Uani 1 1 d . . . O31 O 0.6555(2) 0.18739(10) 0.2631(2) 0.0442(7) Uani 1 1 d . . . O32 O 0.7590(2) 0.19039(10) 0.1600(2) 0.0454(7) Uani 1 1 d . . . O33 O 0.7300(2) 0.12038(10) 0.21753(19) 0.0431(7) Uani 1 1 d . . . O34 O 0.5956(2) 0.15739(10) 0.1248(2) 0.0492(7) Uani 1 1 d . . . Zn1 Zn 1.0000 0.0000 1.0000 0.02286(17) Uani 1 4 d S . . Zn2 Zn 0.76800(3) 0.118786(13) 0.77368(2) 0.02553(12) Uani 1 1 d . . . Zn3 Zn 0.80925(5) 0.0000 0.52525(4) 0.03357(16) Uani 1 2 d S . . Zn4 Zn 0.45967(5) 0.0000 0.78081(4) 0.03563(16) Uani 1 2 d S . . 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 0.038(2) 0.036(2) 0.040(2) 0.0078(15) 0.0138(17) 0.0128(16) C2 0.043(2) 0.0341(19) 0.040(2) 0.0115(16) 0.0050(17) 0.0055(16) C3 0.044(2) 0.0294(17) 0.0253(17) -0.0001(13) 0.0086(15) -0.0112(15) C4 0.0342(19) 0.038(2) 0.050(2) 0.0090(17) 0.0079(17) -0.0109(16) C5 0.042(2) 0.0353(19) 0.039(2) -0.0133(16) 0.0102(17) -0.0157(16) C6 0.046(2) 0.034(2) 0.052(2) -0.0140(18) 0.0030(19) -0.0090(17) C7 0.044(2) 0.037(2) 0.0330(19) 0.0065(15) 0.0143(16) 0.0155(16) C8 0.047(2) 0.042(2) 0.035(2) 0.0041(16) 0.0075(17) 0.0131(18) C9 0.0321(18) 0.0316(18) 0.0343(19) 0.0010(14) 0.0078(15) -0.0020(14) C10 0.0341(18) 0.0350(19) 0.0311(18) 0.0101(15) -0.0035(15) -0.0010(15) C11 0.034(2) 0.044(2) 0.060(3) 0.0104(19) -0.0013(19) -0.0002(17) C12 0.0214(16) 0.049(2) 0.039(2) 0.0039(16) 0.0076(14) -0.0010(15) C13 0.0332(18) 0.037(2) 0.0340(19) -0.0035(15) 0.0058(15) -0.0121(15) C14 0.040(2) 0.040(2) 0.035(2) -0.0039(16) 0.0022(16) -0.0047(17) C15 0.0285(17) 0.039(2) 0.0316(19) -0.0027(15) -0.0030(14) 0.0024(15) Cl1 0.0427(7) 0.0425(7) 0.0337(6) 0.000 0.0105(5) 0.000 Cl2 0.0365(5) 0.0487(6) 0.0554(6) -0.0127(4) 0.0152(4) -0.0036(4) N1 0.0424(17) 0.0294(15) 0.0342(16) -0.0010(13) 0.0047(14) -0.0017(13) N2 0.0318(15) 0.0381(16) 0.0321(16) 0.0046(13) 0.0012(13) -0.0013(13) N3 0.0340(15) 0.0359(16) 0.0319(16) -0.0021(13) 0.0003(13) -0.0056(13) O1 0.0287(12) 0.0395(14) 0.0363(14) 0.0068(11) 0.0056(10) 0.0062(11) O2 0.0361(13) 0.0416(14) 0.0339(14) 0.0077(11) 0.0042(11) 0.0133(12) O3 0.0309(13) 0.0400(14) 0.0413(15) 0.0032(11) 0.0046(11) -0.0032(11) O4 0.0388(14) 0.0462(16) 0.0324(14) 0.0062(11) 0.0006(11) -0.0060(12) O5 0.0436(14) 0.0304(13) 0.0324(14) -0.0067(10) 0.0075(11) 0.0000(11) O6 0.0303(12) 0.0339(13) 0.0286(12) -0.0005(10) 0.0070(10) -0.0019(10) O7 0.0398(19) 0.0340(18) 0.0195(16) 0.000 -0.0034(14) 0.000 O8 0.0359(19) 0.044(2) 0.0334(19) 0.000 -0.0013(15) 0.000 O9 0.0364(19) 0.046(2) 0.0295(19) 0.000 0.0041(15) 0.000 O10 0.0506(16) 0.0513(17) 0.0358(15) 0.0098(12) 0.0149(13) 0.0072(14) O11 0.0266(16) 0.0352(18) 0.0290(18) 0.000 0.0011(14) 0.000 O12 0.0323(13) 0.0340(13) 0.0412(15) 0.0049(11) 0.0008(11) 0.0012(10) O13 0.0378(19) 0.041(2) 0.0275(18) 0.000 0.0080(15) 0.000 O14 0.0260(17) 0.043(2) 0.037(2) 0.000 0.0042(15) 0.000 O15 0.0298(13) 0.0385(14) 0.0442(15) 0.0072(12) 0.0046(11) 0.0121(11) O16 0.061(3) 0.056(3) 0.035(2) 0.000 0.0059(19) 0.000 O17 0.048(3) 0.043(3) 0.040(3) 0.000 0.010(3) 0.000 O21 0.0466(16) 0.0543(18) 0.0575(19) -0.0132(15) 0.0232(14) -0.0207(14) O22 0.0452(15) 0.0381(15) 0.0495(17) 0.0075(12) 0.0174(13) 0.0125(12) O31 0.0482(16) 0.0441(16) 0.0426(16) -0.0129(12) 0.0152(13) -0.0092(13) O32 0.0481(16) 0.0466(16) 0.0436(16) 0.0070(13) 0.0149(13) -0.0041(13) O33 0.0440(16) 0.0434(16) 0.0447(16) 0.0085(12) 0.0161(13) -0.0025(12) O34 0.0492(17) 0.0427(16) 0.0505(18) -0.0180(13) 0.0001(14) 0.0031(13) Zn1 0.0250(4) 0.0224(4) 0.0182(3) 0.000 -0.0013(3) 0.000 Zn2 0.0247(2) 0.0247(2) 0.0251(2) 0.00018(14) 0.00114(15) -0.00002(14) Zn3 0.0274(3) 0.0425(3) 0.0293(3) 0.000 0.0032(2) 0.000 Zn4 0.0328(3) 0.0385(3) 0.0353(3) 0.000 0.0072(2) 0.000 _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 N1 1.463(5) . ? C1 C2 1.474(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.480(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.483(5) . ? C3 C4 1.516(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.502(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.464(5) . ? C5 C6 1.553(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.480(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N1 1.494(5) . ? C7 C8 1.521(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.513(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.246(5) . ? C9 O1 1.283(5) . ? C10 N2 1.474(5) . ? C10 C11 1.528(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.496(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O4 1.251(5) . ? C12 O3 1.288(4) . ? C13 N3 1.512(5) . ? C13 C14 1.515(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.534(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O6 1.243(4) . ? C15 O5 1.266(5) . ? Cl1 O21 1.286(3) . ? Cl1 O21 1.286(3) 2_656 ? Cl1 O22 1.392(3) . ? Cl1 O22 1.392(3) 2_656 ? Cl2 O34 1.379(3) . ? Cl2 O32 1.388(3) . ? Cl2 O31 1.395(3) . ? Cl2 O33 1.444(3) . ? N1 Zn2 2.099(3) . ? N2 Zn2 2.093(3) . ? N3 Zn2 2.087(3) . ? O1 Zn2 2.080(2) . ? O2 Zn1 2.049(3) . ? O3 Zn2 2.059(3) . ? O4 Zn4 2.074(3) . ? O5 Zn2 2.068(3) . ? O6 Zn3 2.063(2) . ? O7 Zn1 2.110(3) . ? O7 H7C 0.8503 . ? O7 H7D 0.8495 . ? O8 Zn4 2.082(4) . ? O8 H8C 0.8500 . ? O8 H8D 0.8506 . ? O9 Zn4 2.030(4) . ? O9 H9C 0.8501 . ? O9 H9D 0.8499 . ? O10 Zn4 2.074(3) . ? O10 H10C 0.8500 . ? O10 H10D 0.8500 . ? O11 Zn3 2.076(4) . ? O11 H11C 0.8500 . ? O11 H11D 0.8499 . ? O12 Zn3 2.062(2) . ? O12 H12C 0.8499 . ? O12 H12D 0.8500 . ? O13 Zn3 2.106(4) . ? O13 H13C 0.8500 . ? O13 H13D 0.8497 . ? O14 H14C 0.8501 . ? O14 H14D 0.8500 . ? O15 H15C 0.8500 . ? O15 H15D 0.8500 . ? O16 H16C 0.8501 . ? O16 H16D 0.8501 . ? O17 H17C 0.8499 . ? O17 H17D 0.8500 . ? Zn1 O2 2.049(3) 6 ? Zn1 O2 2.049(3) 5_757 ? Zn1 O2 2.049(3) 2_757 ? Zn1 O7 2.110(3) 5_757 ? Zn3 O12 2.062(2) 6 ? Zn3 O6 2.063(2) 6 ? Zn4 O10 2.074(3) 6 ? Zn4 O4 2.074(3) 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 N1 C1 C2 112.5(3) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C1 C2 N2 113.4(3) . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? N2 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N2 C3 C4 111.9(3) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 112.0(3) . . ? N3 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 110.3(3) . . ? N3 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N3 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N1 C6 C5 113.2(3) . . ? N1 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? N1 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? N1 C7 C8 114.7(3) . . ? N1 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 119.0(3) . . ? C9 C8 H8A 107.6 . . ? C7 C8 H8A 107.6 . . ? C9 C8 H8B 107.6 . . ? C7 C8 H8B 107.6 . . ? H8A C8 H8B 107.0 . . ? O2 C9 O1 124.0(3) . . ? O2 C9 C8 116.2(3) . . ? O1 C9 C8 119.8(3) . . ? N2 C10 C11 115.1(3) . . ? N2 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? N2 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C10 118.7(3) . . ? C12 C11 H11A 107.6 . . ? C10 C11 H11A 107.6 . . ? C12 C11 H11B 107.6 . . ? C10 C11 H11B 107.6 . . ? H11A C11 H11B 107.1 . . ? O4 C12 O3 121.9(4) . . ? O4 C12 C11 118.3(3) . . ? O3 C12 C11 119.8(3) . . ? N3 C13 C14 115.2(3) . . ? N3 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? N3 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C13 C14 C15 118.2(3) . . ? C13 C14 H14A 107.8 . . ? C15 C14 H14A 107.8 . . ? C13 C14 H14B 107.8 . . ? C15 C14 H14B 107.8 . . ? H14A C14 H14B 107.1 . . ? O6 C15 O5 125.2(3) . . ? O6 C15 C14 115.8(3) . . ? O5 C15 C14 118.9(3) . . ? O21 Cl1 O21 102.7(3) . 2_656 ? O21 Cl1 O22 114.56(19) . . ? O21 Cl1 O22 106.79(18) 2_656 . ? O21 Cl1 O22 106.79(18) . 2_656 ? O21 Cl1 O22 114.56(19) 2_656 2_656 ? O22 Cl1 O22 111.3(3) . 2_656 ? O34 Cl2 O32 109.3(2) . . ? O34 Cl2 O31 111.12(19) . . ? O32 Cl2 O31 111.73(19) . . ? O34 Cl2 O33 106.02(18) . . ? O32 Cl2 O33 107.28(18) . . ? O31 Cl2 O33 111.19(19) . . ? C1 N1 C6 111.9(3) . . ? C1 N1 C7 110.5(3) . . ? C6 N1 C7 112.9(3) . . ? C1 N1 Zn2 103.5(2) . . ? C6 N1 Zn2 107.0(2) . . ? C7 N1 Zn2 110.6(2) . . ? C10 N2 C2 114.3(3) . . ? C10 N2 C3 109.2(3) . . ? C2 N2 C3 111.6(3) . . ? C10 N2 Zn2 111.0(2) . . ? C2 N2 Zn2 107.4(2) . . ? C3 N2 Zn2 102.7(2) . . ? C5 N3 C4 112.3(3) . . ? C5 N3 C13 109.7(3) . . ? C4 N3 C13 113.4(3) . . ? C5 N3 Zn2 103.6(2) . . ? C4 N3 Zn2 107.5(2) . . ? C13 N3 Zn2 109.8(2) . . ? C9 O1 Zn2 132.0(2) . . ? C9 O2 Zn1 130.1(3) . . ? C12 O3 Zn2 131.5(3) . . ? C12 O4 Zn4 128.3(2) . . ? C15 O5 Zn2 133.0(2) . . ? C15 O6 Zn3 128.7(2) . . ? Zn1 O7 H7C 111.8 . . ? Zn1 O7 H7D 111.4 . . ? H7C O7 H7D 105.4 . . ? Zn4 O8 H8C 109.9 . . ? Zn4 O8 H8D 111.0 . . ? H8C O8 H8D 108.9 . . ? Zn4 O9 H9C 107.9 . . ? Zn4 O9 H9D 107.8 . . ? H9C O9 H9D 107.2 . . ? Zn4 O10 H10C 109.5 . . ? Zn4 O10 H10D 109.4 . . ? H10C O10 H10D 109.5 . . ? Zn3 O11 H11C 107.6 . . ? Zn3 O11 H11D 111.2 . . ? H11C O11 H11D 106.6 . . ? Zn3 O12 H12C 107.9 . . ? Zn3 O12 H12D 107.6 . . ? H12C O12 H12D 107.2 . . ? Zn3 O13 H13C 112.1 . . ? Zn3 O13 H13D 102.6 . . ? H13C O13 H13D 109.4 . . ? H14C O14 H14D 109.5 . . ? H15C O15 H15D 109.5 . . ? H16C O16 H16D 109.5 . . ? H17C O17 H17D 109.5 . . ? O2 Zn1 O2 90.78(16) 6 5_757 ? O2 Zn1 O2 180.00(11) 6 2_757 ? O2 Zn1 O2 89.22(16) 5_757 2_757 ? O2 Zn1 O2 89.22(16) 6 . ? O2 Zn1 O2 180.00(15) 5_757 . ? O2 Zn1 O2 90.78(16) 2_757 . ? O2 Zn1 O7 93.91(10) 6 5_757 ? O2 Zn1 O7 86.09(10) 5_757 5_757 ? O2 Zn1 O7 86.09(10) 2_757 5_757 ? O2 Zn1 O7 93.91(10) . 5_757 ? O2 Zn1 O7 86.09(10) 6 . ? O2 Zn1 O7 93.91(10) 5_757 . ? O2 Zn1 O7 93.91(10) 2_757 . ? O2 Zn1 O7 86.09(10) . . ? O7 Zn1 O7 180.000(1) 5_757 . ? O3 Zn2 O5 85.90(11) . . ? O3 Zn2 O1 86.65(11) . . ? O5 Zn2 O1 87.96(11) . . ? O3 Zn2 N3 176.63(12) . . ? O5 Zn2 N3 91.53(12) . . ? O1 Zn2 N3 95.46(11) . . ? O3 Zn2 N2 92.12(11) . . ? O5 Zn2 N2 96.36(12) . . ? O1 Zn2 N2 175.41(12) . . ? N3 Zn2 N2 85.98(12) . . ? O3 Zn2 N1 96.79(12) . . ? O5 Zn2 N1 177.07(12) . . ? O1 Zn2 N1 91.04(12) . . ? N3 Zn2 N1 85.82(13) . . ? N2 Zn2 N1 84.72(13) . . ? O12 Zn3 O12 90.53(15) 6 . ? O12 Zn3 O6 176.73(10) 6 . ? O12 Zn3 O6 91.11(10) . . ? O12 Zn3 O6 91.11(10) 6 6 ? O12 Zn3 O6 176.73(10) . 6 ? O6 Zn3 O6 87.11(14) . 6 ? O12 Zn3 O11 88.57(10) 6 . ? O12 Zn3 O11 88.57(10) . . ? O6 Zn3 O11 94.29(9) . . ? O6 Zn3 O11 94.29(9) 6 . ? O12 Zn3 O13 88.55(11) 6 . ? O12 Zn3 O13 88.55(11) . . ? O6 Zn3 O13 88.67(10) . . ? O6 Zn3 O13 88.67(10) 6 . ? O11 Zn3 O13 175.90(14) . . ? O9 Zn4 O10 91.12(12) . . ? O9 Zn4 O10 91.12(12) . 6 ? O10 Zn4 O10 88.53(17) . 6 ? O9 Zn4 O4 86.84(11) . 6 ? O10 Zn4 O4 89.72(12) . 6 ? O10 Zn4 O4 177.28(12) 6 6 ? O9 Zn4 O4 86.84(11) . . ? O10 Zn4 O4 177.28(12) . . ? O10 Zn4 O4 89.72(12) 6 . ? O4 Zn4 O4 91.96(16) 6 . ? O9 Zn4 O8 179.24(15) . . ? O10 Zn4 O8 88.34(12) . . ? O10 Zn4 O8 88.34(12) 6 . ? O4 Zn4 O8 93.68(11) 6 . ? O4 Zn4 O8 93.68(11) . . ? 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 C1 C2 N2 45.6(5) . . . . ? N2 C3 C4 N3 46.6(4) . . . . ? N3 C5 C6 N1 45.8(5) . . . . ? N1 C7 C8 C9 -61.6(5) . . . . ? C7 C8 C9 O2 -161.6(4) . . . . ? C7 C8 C9 O1 18.6(6) . . . . ? N2 C10 C11 C12 -64.4(5) . . . . ? C10 C11 C12 O4 -152.2(4) . . . . ? C10 C11 C12 O3 28.8(6) . . . . ? N3 C13 C14 C15 -62.1(5) . . . . ? C13 C14 C15 O6 -165.8(3) . . . . ? C13 C14 C15 O5 17.0(5) . . . . ? C2 C1 N1 C6 70.0(4) . . . . ? C2 C1 N1 C7 -163.3(3) . . . . ? C2 C1 N1 Zn2 -44.9(4) . . . . ? C5 C6 N1 C1 -131.2(4) . . . . ? C5 C6 N1 C7 103.5(4) . . . . ? C5 C6 N1 Zn2 -18.4(4) . . . . ? C8 C7 N1 C1 -179.2(3) . . . . ? C8 C7 N1 C6 -53.1(4) . . . . ? C8 C7 N1 Zn2 66.7(4) . . . . ? C11 C10 N2 C2 -57.7(4) . . . . ? C11 C10 N2 C3 176.5(3) . . . . ? C11 C10 N2 Zn2 63.9(4) . . . . ? C1 C2 N2 C10 103.8(4) . . . . ? C1 C2 N2 C3 -131.7(3) . . . . ? C1 C2 N2 Zn2 -19.8(4) . . . . ? C4 C3 N2 C10 -164.4(3) . . . . ? C4 C3 N2 C2 68.3(4) . . . . ? C4 C3 N2 Zn2 -46.6(3) . . . . ? C6 C5 N3 C4 69.1(4) . . . . ? C6 C5 N3 C13 -163.9(3) . . . . ? C6 C5 N3 Zn2 -46.7(3) . . . . ? C3 C4 N3 C5 -133.1(3) . . . . ? C3 C4 N3 C13 101.9(4) . . . . ? C3 C4 N3 Zn2 -19.7(4) . . . . ? C14 C13 N3 C5 -180.0(3) . . . . ? C14 C13 N3 C4 -53.5(4) . . . . ? C14 C13 N3 Zn2 66.8(3) . . . . ? O2 C9 O1 Zn2 -170.7(3) . . . . ? C8 C9 O1 Zn2 9.1(5) . . . . ? O1 C9 O2 Zn1 10.7(6) . . . . ? C8 C9 O2 Zn1 -169.0(3) . . . . ? O4 C12 O3 Zn2 177.1(3) . . . . ? C11 C12 O3 Zn2 -3.9(6) . . . . ? O3 C12 O4 Zn4 10.4(6) . . . . ? C11 C12 O4 Zn4 -168.7(3) . . . . ? O6 C15 O5 Zn2 -163.9(3) . . . . ? C14 C15 O5 Zn2 13.0(5) . . . . ? O5 C15 O6 Zn3 -2.9(5) . . . . ? C14 C15 O6 Zn3 -179.9(2) . . . . ? C9 O2 Zn1 O2 -109.5(3) . . . 6 ? C9 O2 Zn1 O2 70.5(3) . . . 2_757 ? C9 O2 Zn1 O7 -15.7(3) . . . 5_757 ? C9 O2 Zn1 O7 164.3(3) . . . . ? C12 O3 Zn2 O5 -90.3(3) . . . . ? C12 O3 Zn2 O1 -178.5(3) . . . . ? C12 O3 Zn2 N2 5.9(3) . . . . ? C12 O3 Zn2 N1 90.8(3) . . . . ? C15 O5 Zn2 O3 173.3(3) . . . . ? C15 O5 Zn2 O1 -99.9(3) . . . . ? C15 O5 Zn2 N3 -4.5(3) . . . . ? C15 O5 Zn2 N2 81.7(3) . . . . ? C9 O1 Zn2 O3 -97.7(3) . . . . ? C9 O1 Zn2 O5 176.3(3) . . . . ? C9 O1 Zn2 N3 84.9(3) . . . . ? C9 O1 Zn2 N1 -1.0(3) . . . . ? C5 N3 Zn2 O5 -149.4(2) . . . . ? C4 N3 Zn2 O5 91.5(3) . . . . ? C13 N3 Zn2 O5 -32.3(2) . . . . ? C5 N3 Zn2 O1 -61.3(2) . . . . ? C4 N3 Zn2 O1 179.6(3) . . . . ? C13 N3 Zn2 O1 55.8(2) . . . . ? C5 N3 Zn2 N2 114.4(3) . . . . ? C4 N3 Zn2 N2 -4.8(3) . . . . ? C13 N3 Zn2 N2 -128.6(2) . . . . ? C5 N3 Zn2 N1 29.4(2) . . . . ? C4 N3 Zn2 N1 -89.8(3) . . . . ? C13 N3 Zn2 N1 146.5(2) . . . . ? C10 N2 Zn2 O3 -33.0(3) . . . . ? C2 N2 Zn2 O3 92.6(2) . . . . ? C3 N2 Zn2 O3 -149.6(2) . . . . ? C10 N2 Zn2 O5 53.1(3) . . . . ? C2 N2 Zn2 O5 178.7(2) . . . . ? C3 N2 Zn2 O5 -63.5(2) . . . . ? C10 N2 Zn2 N3 144.2(3) . . . . ? C2 N2 Zn2 N3 -90.2(2) . . . . ? C3 N2 Zn2 N3 27.6(2) . . . . ? C10 N2 Zn2 N1 -129.6(3) . . . . ? C2 N2 Zn2 N1 -4.1(2) . . . . ? C3 N2 Zn2 N1 113.7(2) . . . . ? C1 N1 Zn2 O3 -65.5(2) . . . . ? C6 N1 Zn2 O3 176.2(3) . . . . ? C7 N1 Zn2 O3 52.9(3) . . . . ? C1 N1 Zn2 O1 -152.3(2) . . . . ? C6 N1 Zn2 O1 89.4(3) . . . . ? C7 N1 Zn2 O1 -33.9(3) . . . . ? C1 N1 Zn2 N3 112.3(2) . . . . ? C6 N1 Zn2 N3 -6.0(3) . . . . ? C7 N1 Zn2 N3 -129.3(3) . . . . ? C1 N1 Zn2 N2 26.0(2) . . . . ? C6 N1 Zn2 N2 -92.3(3) . . . . ? C7 N1 Zn2 N2 144.4(3) . . . . ? C15 O6 Zn3 O12 78.9(3) . . . . ? C15 O6 Zn3 O6 -103.8(3) . . . 6 ? C15 O6 Zn3 O11 -9.7(3) . . . . ? C15 O6 Zn3 O13 167.4(3) . . . . ? C12 O4 Zn4 O9 157.9(3) . . . . ? C12 O4 Zn4 O10 66.8(3) . . . 6 ? C12 O4 Zn4 O4 -115.4(3) . . . 6 ? C12 O4 Zn4 O8 -21.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.330 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.068 data_3 #TrackingRef '- zzcomplexes CIF.txt' _database_code_depnum_ccdc_archive 'CCDC 831024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H52 Cd2 N6 O12, 2(Cl O4)' _chemical_formula_sum 'C30 H52 Cd2 Cl2 N6 O20' _chemical_formula_weight 1112.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5334(19) _cell_length_b 10.120(2) _cell_length_c 12.316(2) _cell_angle_alpha 70.239(3) _cell_angle_beta 86.463(3) _cell_angle_gamma 70.013(3) _cell_volume 1049.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 612 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 16.92 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7099 _exptl_absorpt_correction_T_max 0.7574 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5785 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4049 _reflns_number_gt 3071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.8500P] 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 4049 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 C1 C 0.8310(8) 0.7921(9) 0.6876(7) 0.073(2) Uani 1 1 d . . . H1A H 0.8238 0.8402 0.6044 0.087 Uiso 1 1 calc R . . H1B H 0.8698 0.8481 0.7207 0.087 Uiso 1 1 calc R . . C2 C 0.6765(8) 0.8098(9) 0.7252(6) 0.068(2) Uani 1 1 d . . . H2A H 0.6123 0.8334 0.6583 0.081 Uiso 1 1 calc R . . H2B H 0.6421 0.8950 0.7517 0.081 Uiso 1 1 calc R . . C3 C 0.5586(7) 0.5966(7) 0.7781(5) 0.0483(15) Uani 1 1 d . . . H3A H 0.4785 0.5870 0.8294 0.058 Uiso 1 1 calc R . . H3B H 0.5128 0.6645 0.7026 0.058 Uiso 1 1 calc R . . C4 C 0.6418(7) 0.4481(9) 0.7681(7) 0.0617(19) Uani 1 1 d . . . H4A H 0.6280 0.3727 0.8373 0.074 Uiso 1 1 calc R . . H4B H 0.5953 0.4407 0.7035 0.074 Uiso 1 1 calc R . . C5 C 0.8799(7) 0.4541(7) 0.6462(5) 0.0489(15) Uani 1 1 d . . . H5A H 0.8038 0.5034 0.5830 0.059 Uiso 1 1 calc R . . H5B H 0.9446 0.3629 0.6348 0.059 Uiso 1 1 calc R . . C6 C 0.9716(8) 0.5516(7) 0.6309(6) 0.0517(16) Uani 1 1 d . . . H6A H 0.9523 0.6217 0.5524 0.062 Uiso 1 1 calc R . . H6B H 1.0763 0.4897 0.6397 0.062 Uiso 1 1 calc R . . C7 C 1.1063(8) 0.6534(8) 0.7243(7) 0.0633(19) Uani 1 1 d . . . H7A H 1.1089 0.7009 0.7803 0.076 Uiso 1 1 calc R . . H7B H 1.1832 0.5553 0.7475 0.076 Uiso 1 1 calc R . . C8 C 1.1302(8) 0.7509(8) 0.6006(6) 0.0564(17) Uani 1 1 d . . . H8A H 1.2143 0.6945 0.5673 0.068 Uiso 1 1 calc R . . H8B H 1.0414 0.7880 0.5496 0.068 Uiso 1 1 calc R . . C9 C 1.1608(8) 0.8754(8) 0.6215(6) 0.0572(18) Uani 1 1 d . . . C10 C 0.5819(8) 0.7156(8) 0.9260(6) 0.0562(18) Uani 1 1 d . . . H10A H 0.5872 0.6246 0.9887 0.067 Uiso 1 1 calc R . . H10B H 0.4768 0.7706 0.9030 0.067 Uiso 1 1 calc R . . C11 C 0.6425(8) 0.8142(8) 0.9791(7) 0.0619(19) Uani 1 1 d . . . H11A H 0.6334 0.9097 0.9204 0.074 Uiso 1 1 calc R . . H11B H 0.5844 0.8326 1.0432 0.074 Uiso 1 1 calc R . . C12 C 0.7991(8) 0.7299(8) 1.0184(6) 0.0532(17) Uani 1 1 d . . . C13 C 0.8354(8) 0.2479(8) 0.7867(6) 0.0553(17) Uani 1 1 d . . . H13A H 0.9408 0.1959 0.8097 0.066 Uiso 1 1 calc R . . H13B H 0.8135 0.2239 0.7213 0.066 Uiso 1 1 calc R . . C14 C 0.7422(8) 0.1935(8) 0.8876(6) 0.0556(17) Uani 1 1 d . . . H14A H 0.6387 0.2587 0.8704 0.067 Uiso 1 1 calc R . . H14B H 0.7463 0.0937 0.8948 0.067 Uiso 1 1 calc R . . C15 C 0.7974(7) 0.1906(8) 1.0023(5) 0.0495(16) Uani 1 1 d . . . Cd1 Cd 0.89469(5) 0.47712(5) 0.89075(4) 0.03939(15) Uani 1 1 d . . . Cl1 Cl 0.41854(19) 0.23218(19) 0.64561(14) 0.0512(4) Uani 1 1 d . . . N1 N 0.9446(6) 0.6409(6) 0.7145(4) 0.0492(13) Uani 1 1 d . . . N2 N 0.6545(6) 0.6701(7) 0.8246(5) 0.0595(15) Uani 1 1 d . . . N3 N 0.8035(5) 0.4092(6) 0.7520(4) 0.0436(12) Uani 1 1 d . . . O1 O 1.2816(5) 0.9101(5) 0.5834(4) 0.0480(10) Uani 1 1 d . . . H1C H 1.3231 0.8588 0.5406 0.072 Uiso 1 1 d R . . O2 O 1.0789(5) 0.9504(4) 0.6715(3) 0.0432(10) Uani 1 1 d . . . O3 O 0.8678(5) 0.5981(5) 1.0279(3) 0.0460(10) Uani 1 1 d . . . O4 O 0.8793(5) 0.7748(5) 1.0663(4) 0.0578(12) Uani 1 1 d . . . O5 O 0.8001(5) 0.3045(5) 1.0155(4) 0.0481(10) Uani 1 1 d . . . O6 O 0.8326(5) 0.0661(5) 1.0897(4) 0.0530(11) Uani 1 1 d . . . H6C H 0.7925 0.0098 1.0758 0.079 Uiso 1 1 d R . . O7 O 0.3274(5) 0.3780(5) 0.6144(4) 0.0551(12) Uani 1 1 d . . . O8 O 0.4891(5) 0.1751(6) 0.7449(4) 0.0610(13) Uani 1 1 d . . . O9 O 0.3394(6) 0.1689(6) 0.6318(5) 0.0682(14) Uani 1 1 d . . . O10 O 0.5055(5) 0.2207(5) 0.5623(4) 0.0529(11) 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 C1 0.043(4) 0.071(5) 0.064(5) -0.015(4) 0.000(3) 0.021(4) C2 0.051(4) 0.072(5) 0.057(4) -0.008(4) -0.017(3) -0.003(4) C3 0.047(4) 0.042(4) 0.043(3) -0.007(3) -0.006(3) -0.004(3) C4 0.043(4) 0.073(5) 0.064(4) -0.026(4) -0.013(3) -0.009(3) C5 0.053(4) 0.039(3) 0.038(3) -0.004(3) -0.008(3) -0.003(3) C6 0.053(4) 0.045(4) 0.050(4) -0.014(3) -0.010(3) -0.007(3) C7 0.053(4) 0.055(4) 0.069(5) -0.004(4) -0.020(3) -0.015(3) C8 0.051(4) 0.055(4) 0.059(4) -0.013(3) -0.015(3) -0.016(3) C9 0.048(4) 0.059(4) 0.055(4) -0.013(3) 0.013(3) -0.015(3) C10 0.059(4) 0.050(4) 0.045(4) -0.006(3) 0.012(3) -0.011(3) C11 0.052(4) 0.054(4) 0.060(4) 0.004(3) -0.020(3) -0.013(3) C12 0.058(4) 0.056(4) 0.047(4) -0.023(3) 0.019(3) -0.019(3) C13 0.072(5) 0.056(4) 0.041(3) -0.019(3) 0.018(3) -0.025(4) C14 0.056(4) 0.051(4) 0.056(4) -0.021(3) 0.004(3) -0.012(3) C15 0.041(3) 0.055(4) 0.045(4) -0.008(3) 0.012(3) -0.016(3) Cd1 0.0413(2) 0.0395(2) 0.0385(2) -0.01688(17) 0.00697(16) -0.01231(17) Cl1 0.0534(10) 0.0520(10) 0.0497(9) -0.0198(7) 0.0154(8) -0.0195(8) N1 0.055(3) 0.048(3) 0.037(3) -0.006(2) -0.009(2) -0.014(3) N2 0.051(3) 0.054(3) 0.059(3) -0.015(3) -0.006(3) -0.002(3) N3 0.039(3) 0.054(3) 0.037(3) -0.016(2) -0.009(2) -0.013(2) O1 0.050(3) 0.039(2) 0.055(3) -0.013(2) -0.004(2) -0.0173(19) O2 0.054(3) 0.037(2) 0.032(2) -0.0036(17) -0.0062(18) -0.0140(19) O3 0.050(2) 0.044(2) 0.044(2) -0.0183(19) 0.0059(19) -0.013(2) O4 0.063(3) 0.049(3) 0.053(3) -0.013(2) 0.009(2) -0.015(2) O5 0.045(2) 0.047(3) 0.050(2) -0.011(2) -0.0090(19) -0.015(2) O6 0.061(3) 0.042(2) 0.045(2) -0.0044(19) 0.001(2) -0.014(2) O7 0.049(3) 0.052(3) 0.060(3) -0.005(2) -0.014(2) -0.022(2) O8 0.054(3) 0.064(3) 0.053(3) -0.014(2) 0.009(2) -0.013(2) O9 0.059(3) 0.061(3) 0.075(3) -0.018(3) 0.018(3) -0.016(3) O10 0.045(2) 0.060(3) 0.037(2) -0.008(2) -0.0043(19) -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 N1 1.481(9) . ? C1 C2 1.486(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.594(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.484(9) . ? C3 N2 1.592(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.474(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.464(8) . ? C5 C6 1.489(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.542(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.562(10) . ? C7 N1 1.605(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.490(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.190(8) . ? C9 O1 1.330(8) . ? C10 N2 1.522(9) . ? C10 C11 1.625(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.459(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.236(8) . ? C12 O4 1.271(8) . ? C13 N3 1.464(8) . ? C13 C14 1.540(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.525(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O5 1.227(8) . ? C15 O6 1.303(7) . ? Cd1 O3 2.301(4) 2_767 ? Cd1 O5 2.306(4) . ? Cd1 N3 2.353(5) . ? Cd1 O3 2.356(4) . ? Cd1 N1 2.380(5) . ? Cd1 N2 2.412(6) . ? Cd1 O4 2.626(5) 2_767 ? Cl1 O9 1.196(6) . ? Cl1 O8 1.280(5) . ? Cl1 O10 1.290(4) . ? Cl1 O7 1.364(5) . ? O1 H1C 0.8500 . ? O3 Cd1 2.301(4) 2_767 ? O4 Cd1 2.626(5) 2_767 ? O6 H6C 0.8499 . ? 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 N1 C1 C2 119.9(7) . . ? N1 C1 H1A 107.3 . . ? C2 C1 H1A 107.3 . . ? N1 C1 H1B 107.3 . . ? C2 C1 H1B 107.3 . . ? H1A C1 H1B 106.9 . . ? C1 C2 N2 116.5(6) . . ? C1 C2 H2A 108.2 . . ? N2 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? N2 C2 H2B 108.2 . . ? H2A C2 H2B 107.3 . . ? C4 C3 N2 115.9(5) . . ? C4 C3 H3A 108.3 . . ? N2 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? N2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N3 C4 C3 118.3(6) . . ? N3 C4 H4A 107.7 . . ? C3 C4 H4A 107.7 . . ? N3 C4 H4B 107.7 . . ? C3 C4 H4B 107.7 . . ? H4A C4 H4B 107.1 . . ? N3 C5 C6 122.5(6) . . ? N3 C5 H5A 106.7 . . ? C6 C5 H5A 106.7 . . ? N3 C5 H5B 106.7 . . ? C6 C5 H5B 106.7 . . ? H5A C5 H5B 106.6 . . ? C5 C6 N1 115.8(6) . . ? C5 C6 H6A 108.3 . . ? N1 C6 H6A 108.3 . . ? C5 C6 H6B 108.3 . . ? N1 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C8 C7 N1 105.1(5) . . ? C8 C7 H7A 110.7 . . ? N1 C7 H7A 110.7 . . ? C8 C7 H7B 110.7 . . ? N1 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C9 C8 C7 103.0(6) . . ? C9 C8 H8A 111.2 . . ? C7 C8 H8A 111.2 . . ? C9 C8 H8B 111.2 . . ? C7 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? O2 C9 O1 116.2(7) . . ? O2 C9 C8 122.6(6) . . ? O1 C9 C8 121.3(6) . . ? N2 C10 C11 120.9(6) . . ? N2 C10 H10A 107.1 . . ? C11 C10 H10A 107.1 . . ? N2 C10 H10B 107.1 . . ? C11 C10 H10B 107.1 . . ? H10A C10 H10B 106.8 . . ? C12 C11 C10 107.7(6) . . ? C12 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? C12 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? O3 C12 O4 108.6(6) . . ? O3 C12 C11 126.8(7) . . ? O4 C12 C11 123.7(7) . . ? N3 C13 C14 111.7(5) . . ? N3 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N3 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 112.6(6) . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? O5 C15 O6 119.7(6) . . ? O5 C15 C14 121.4(6) . . ? O6 C15 C14 118.8(6) . . ? O3 Cd1 O5 102.17(15) 2_767 . ? O3 Cd1 N3 130.95(16) 2_767 . ? O5 Cd1 N3 82.01(17) . . ? O3 Cd1 O3 75.10(16) 2_767 . ? O5 Cd1 O3 90.17(15) . . ? N3 Cd1 O3 153.81(16) . . ? O3 Cd1 N1 93.72(17) 2_767 . ? O5 Cd1 N1 159.66(17) . . ? N3 Cd1 N1 77.97(18) . . ? O3 Cd1 N1 106.31(17) . . ? O3 Cd1 N2 149.14(19) 2_767 . ? O5 Cd1 N2 95.25(19) . . ? N3 Cd1 N2 76.3(2) . . ? O3 Cd1 N2 79.62(18) . . ? N1 Cd1 N2 76.6(2) . . ? O3 Cd1 O4 48.26(16) 2_767 2_767 ? O5 Cd1 O4 77.02(15) . 2_767 ? N3 Cd1 O4 87.02(17) . 2_767 ? O3 Cd1 O4 115.64(16) . 2_767 ? N1 Cd1 O4 105.29(17) . 2_767 ? N2 Cd1 O4 162.51(19) . 2_767 ? O9 Cl1 O8 114.7(4) . . ? O9 Cl1 O10 99.7(3) . . ? O8 Cl1 O10 113.1(3) . . ? O9 Cl1 O7 103.8(3) . . ? O8 Cl1 O7 117.0(3) . . ? O10 Cl1 O7 106.7(3) . . ? C1 N1 C6 122.3(5) . . ? C1 N1 C7 108.3(6) . . ? C6 N1 C7 101.3(5) . . ? C1 N1 Cd1 109.9(4) . . ? C6 N1 Cd1 103.9(4) . . ? C7 N1 Cd1 110.6(4) . . ? C10 N2 C3 110.3(5) . . ? C10 N2 C2 110.5(6) . . ? C3 N2 C2 111.8(5) . . ? C10 N2 Cd1 109.1(4) . . ? C3 N2 Cd1 105.6(4) . . ? C2 N2 Cd1 109.4(4) . . ? C5 N3 C13 107.9(5) . . ? C5 N3 C4 128.8(5) . . ? C13 N3 C4 95.7(5) . . ? C5 N3 Cd1 107.0(4) . . ? C13 N3 Cd1 112.7(4) . . ? C4 N3 Cd1 104.3(4) . . ? C9 O1 H1C 107.2 . . ? C12 O3 Cd1 110.4(4) . 2_767 ? C12 O3 Cd1 129.6(4) . . ? Cd1 O3 Cd1 104.90(16) 2_767 . ? C12 O4 Cd1 92.5(4) . 2_767 ? C15 O5 Cd1 126.0(4) . . ? C15 O6 H6C 107.9 . . ? 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 C1 C2 N2 18.2(11) . . . . ? N2 C3 C4 N3 -25.6(9) . . . . ? N3 C5 C6 N1 -17.8(8) . . . . ? N1 C7 C8 C9 124.3(6) . . . . ? C7 C8 C9 O2 -53.8(8) . . . . ? C7 C8 C9 O1 127.1(7) . . . . ? N2 C10 C11 C12 -59.4(8) . . . . ? C10 C11 C12 O3 -10.9(9) . . . . ? C10 C11 C12 O4 -178.8(6) . . . . ? N3 C13 C14 C15 -73.4(7) . . . . ? C13 C14 C15 O5 60.1(8) . . . . ? C13 C14 C15 O6 -124.5(6) . . . . ? C2 C1 N1 C6 91.3(9) . . . . ? C2 C1 N1 C7 -151.7(7) . . . . ? C2 C1 N1 Cd1 -30.7(9) . . . . ? C5 C6 N1 C1 -89.7(8) . . . . ? C5 C6 N1 C7 149.9(5) . . . . ? C5 C6 N1 Cd1 35.1(6) . . . . ? C8 C7 N1 C1 -64.6(7) . . . . ? C8 C7 N1 C6 65.1(6) . . . . ? C8 C7 N1 Cd1 174.8(4) . . . . ? O3 Cd1 N1 C1 -126.8(5) 2_767 . . . ? O5 Cd1 N1 C1 91.7(7) . . . . ? N3 Cd1 N1 C1 102.0(5) . . . . ? O3 Cd1 N1 C1 -51.3(5) . . . . ? N2 Cd1 N1 C1 23.5(5) . . . . ? O4 Cd1 N1 C1 -174.5(5) 2_767 . . . ? O3 Cd1 N1 C6 100.7(4) 2_767 . . . ? O5 Cd1 N1 C6 -40.8(7) . . . . ? N3 Cd1 N1 C6 -30.4(4) . . . . ? O3 Cd1 N1 C6 176.3(3) . . . . ? N2 Cd1 N1 C6 -108.9(4) . . . . ? O4 Cd1 N1 C6 53.1(4) 2_767 . . . ? O3 Cd1 N1 C7 -7.2(4) 2_767 . . . ? O5 Cd1 N1 C7 -148.7(5) . . . . ? N3 Cd1 N1 C7 -138.4(5) . . . . ? O3 Cd1 N1 C7 68.3(4) . . . . ? N2 Cd1 N1 C7 143.1(5) . . . . ? O4 Cd1 N1 C7 -54.9(5) 2_767 . . . ? C11 C10 N2 C3 -171.4(5) . . . . ? C11 C10 N2 C2 -47.3(8) . . . . ? C11 C10 N2 Cd1 73.0(6) . . . . ? C4 C3 N2 C10 -127.5(6) . . . . ? C4 C3 N2 C2 109.1(6) . . . . ? C4 C3 N2 Cd1 -9.8(7) . . . . ? C1 C2 N2 C10 124.3(8) . . . . ? C1 C2 N2 C3 -112.4(7) . . . . ? C1 C2 N2 Cd1 4.2(8) . . . . ? O3 Cd1 N2 C10 -61.1(6) 2_767 . . . ? O5 Cd1 N2 C10 63.3(5) . . . . ? N3 Cd1 N2 C10 143.8(5) . . . . ? O3 Cd1 N2 C10 -25.9(4) . . . . ? N1 Cd1 N2 C10 -135.6(5) . . . . ? O4 Cd1 N2 C10 126.0(6) 2_767 . . . ? O3 Cd1 N2 C3 -179.7(3) 2_767 . . . ? O5 Cd1 N2 C3 -55.2(4) . . . . ? N3 Cd1 N2 C3 25.2(4) . . . . ? O3 Cd1 N2 C3 -144.4(4) . . . . ? N1 Cd1 N2 C3 105.8(4) . . . . ? O4 Cd1 N2 C3 7.4(8) 2_767 . . . ? O3 Cd1 N2 C2 59.8(6) 2_767 . . . ? O5 Cd1 N2 C2 -175.7(5) . . . . ? N3 Cd1 N2 C2 -95.3(5) . . . . ? O3 Cd1 N2 C2 95.1(5) . . . . ? N1 Cd1 N2 C2 -14.6(4) . . . . ? O4 Cd1 N2 C2 -113.0(7) 2_767 . . . ? C6 C5 N3 C13 -132.6(6) . . . . ? C6 C5 N3 C4 114.2(7) . . . . ? C6 C5 N3 Cd1 -11.1(7) . . . . ? C14 C13 N3 C5 -172.0(5) . . . . ? C14 C13 N3 C4 -38.1(7) . . . . ? C14 C13 N3 Cd1 70.0(6) . . . . ? C3 C4 N3 C5 -79.7(9) . . . . ? C3 C4 N3 C13 161.9(6) . . . . ? C3 C4 N3 Cd1 46.7(7) . . . . ? O3 Cd1 N3 C5 -61.6(4) 2_767 . . . ? O5 Cd1 N3 C5 -160.8(4) . . . . ? O3 Cd1 N3 C5 125.4(4) . . . . ? N1 Cd1 N3 C5 22.9(4) . . . . ? N2 Cd1 N3 C5 101.8(4) . . . . ? O4 Cd1 N3 C5 -83.5(4) 2_767 . . . ? O3 Cd1 N3 C13 56.8(5) 2_767 . . . ? O5 Cd1 N3 C13 -42.4(4) . . . . ? O3 Cd1 N3 C13 -116.2(5) . . . . ? N1 Cd1 N3 C13 141.3(4) . . . . ? N2 Cd1 N3 C13 -139.8(4) . . . . ? O4 Cd1 N3 C13 34.9(4) 2_767 . . . ? O3 Cd1 N3 C4 159.4(4) 2_767 . . . ? O5 Cd1 N3 C4 60.2(4) . . . . ? O3 Cd1 N3 C4 -13.6(6) . . . . ? N1 Cd1 N3 C4 -116.2(4) . . . . ? N2 Cd1 N3 C4 -37.2(4) . . . . ? O4 Cd1 N3 C4 137.5(4) 2_767 . . . ? O4 C12 O3 Cd1 -5.6(6) . . . 2_767 ? C11 C12 O3 Cd1 -175.0(6) . . . 2_767 ? O4 C12 O3 Cd1 -137.2(4) . . . . ? C11 C12 O3 Cd1 53.4(9) . . . . ? O3 Cd1 O3 C12 133.5(6) 2_767 . . . ? O5 Cd1 O3 C12 -124.0(5) . . . . ? N3 Cd1 O3 C12 -52.0(7) . . . . ? N1 Cd1 O3 C12 43.9(6) . . . . ? N2 Cd1 O3 C12 -28.7(5) . . . . ? O4 Cd1 O3 C12 160.4(5) 2_767 . . . ? O3 Cd1 O3 Cd1 0.0 2_767 . . 2_767 ? O5 Cd1 O3 Cd1 102.55(17) . . . 2_767 ? N3 Cd1 O3 Cd1 174.6(3) . . . 2_767 ? N1 Cd1 O3 Cd1 -89.54(19) . . . 2_767 ? N2 Cd1 O3 Cd1 -162.1(2) . . . 2_767 ? O4 Cd1 O3 Cd1 26.9(2) 2_767 . . 2_767 ? O3 C12 O4 Cd1 4.6(5) . . . 2_767 ? C11 C12 O4 Cd1 174.4(6) . . . 2_767 ? O6 C15 O5 Cd1 137.1(4) . . . . ? C14 C15 O5 Cd1 -47.5(8) . . . . ? O3 Cd1 O5 C15 -96.5(5) 2_767 . . . ? N3 Cd1 O5 C15 33.8(5) . . . . ? O3 Cd1 O5 C15 -171.3(5) . . . . ? N1 Cd1 O5 C15 44.0(8) . . . . ? N2 Cd1 O5 C15 109.1(5) . . . . ? O4 Cd1 O5 C15 -55.0(5) 2_767 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1C O10 0.85 2.11 2.900(6) 154.1 2_766 O6 H6C O4 0.85 2.28 2.938(7) 134.8 1_545 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.798 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.103 data_4 #TrackingRef '- zzcomplexes CIF.txt' _database_code_depnum_ccdc_archive 'CCDC 831025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H20 Cd N3 O3, C H4 O, Cl O4' _chemical_formula_sum 'C10 H24 Cd Cl N3 O8' _chemical_formula_weight 462.17 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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' '-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 24.083(3) _cell_length_b 8.6672(17) _cell_length_c 18.565(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.03(3) _cell_angle_gamma 90.00 _cell_volume 3388.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 12790 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6238 _exptl_absorpt_correction_T_max 0.6806 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13825 _diffrn_reflns_av_R_equivalents 0.1439 _diffrn_reflns_av_sigmaI/netI 0.1105 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2965 _reflns_number_gt 1991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+2.0000P] 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 2965 _refine_ls_number_parameters 209 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1484 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.2127 _refine_ls_wR_factor_gt 0.1923 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.185 _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 C1 C 0.0658(5) 0.5459(13) 0.2019(7) 0.032(3) Uani 1 1 d . . . H1A H 0.0622 0.5292 0.1481 0.038 Uiso 1 1 calc R . . H1B H 0.0232 0.5614 0.1937 0.038 Uiso 1 1 calc R . . C2 C 0.0937(6) 0.3983(15) 0.2541(8) 0.048(3) Uani 1 1 d . . . H2A H 0.0882 0.4029 0.3025 0.058 Uiso 1 1 calc R . . H2B H 0.0709 0.3087 0.2221 0.058 Uiso 1 1 calc R . . C3 C 0.2039(6) 0.3534(15) 0.3689(9) 0.056(4) Uani 1 1 d . . . H3A H 0.2463 0.3286 0.3787 0.067 Uiso 1 1 calc R . . H3B H 0.1879 0.2645 0.3849 0.067 Uiso 1 1 calc R . . C4 C 0.2080(7) 0.490(2) 0.4230(8) 0.068(5) Uani 1 1 d . . . H4A H 0.1690 0.4954 0.4261 0.081 Uiso 1 1 calc R . . H4B H 0.2426 0.4722 0.4783 0.081 Uiso 1 1 calc R . . C5 C 0.1737(6) 0.7619(16) 0.3838(8) 0.049(3) Uani 1 1 d . . . H5A H 0.1876 0.8591 0.3719 0.059 Uiso 1 1 calc R . . H5B H 0.1737 0.7733 0.4358 0.059 Uiso 1 1 calc R . . C6 C 0.1056(6) 0.7284(14) 0.3156(8) 0.048(3) Uani 1 1 d . . . H6A H 0.0882 0.6451 0.3334 0.057 Uiso 1 1 calc R . . H6B H 0.0796 0.8192 0.3074 0.057 Uiso 1 1 calc R . . C7 C 0.0743(5) 0.8068(15) 0.1761(8) 0.049(4) Uani 1 1 d . . . H7A H 0.0307 0.8209 0.1641 0.059 Uiso 1 1 calc R . . H7B H 0.0732 0.7720 0.1258 0.059 Uiso 1 1 calc R . . C8 C 0.1068(5) 0.9633(15) 0.1983(9) 0.050(4) Uani 1 1 d . . . H8A H 0.0798 1.0345 0.1551 0.060 Uiso 1 1 calc R . . H8B H 0.1072 0.9972 0.2483 0.060 Uiso 1 1 calc R . . C9 C 0.1733(6) 0.9832(15) 0.2114(8) 0.040(3) Uani 1 1 d . . . C10 C 0.0791(8) 0.284(2) 0.0077(11) 0.093(6) Uani 1 1 d . . . H10A H 0.0613 0.2016 0.0246 0.139 Uiso 1 1 calc R . . H10B H 0.0723 0.2633 -0.0468 0.139 Uiso 1 1 calc R . . H10C H 0.0590 0.3794 0.0079 0.139 Uiso 1 1 calc R . . Cd1 Cd 0.20507(4) 0.60831(10) 0.25775(5) 0.0353(4) Uani 1 1 d . . . Cl1 Cl 0.08357(19) 0.8392(5) 0.9448(2) 0.0611(10) Uani 1 1 d D . . N1 N 0.1019(4) 0.6854(12) 0.2364(6) 0.036(2) Uani 1 1 d . . . N2 N 0.1627(5) 0.3820(11) 0.2803(6) 0.044(3) Uani 1 1 d . . . H2C H 0.1678 0.3037 0.2514 0.053 Uiso 1 1 calc R . . N3 N 0.2185(5) 0.6431(12) 0.3924(6) 0.047(3) Uani 1 1 d . . . H3C H 0.2587 0.6767 0.4267 0.056 Uiso 1 1 calc R . . O1 O 0.2102(4) 0.8687(9) 0.2325(5) 0.043(2) Uani 1 1 d . . . O2 O 0.1895(4) 1.1106(9) 0.2004(5) 0.043(2) Uani 1 1 d . . . O3 O 0.1785(5) 0.5762(10) 0.1216(5) 0.065(3) Uani 1 1 d . . . H3D H 0.1826 0.4797 0.1176 0.098 Uiso 1 1 d R . . H3E H 0.1387 0.5934 0.0969 0.098 Uiso 1 1 d R . . O4 O 0.1435(5) 0.2938(11) 0.0616(6) 0.073(3) Uani 1 1 d . . . H4C H 0.1534 0.2116 0.0901 0.110 Uiso 1 1 d R . . O11 O 0.1350(8) 0.852(3) 1.0184(9) 0.209(11) Uani 1 1 d D . . O12 O 0.0767(10) 0.6843(11) 0.9325(11) 0.164(8) Uani 1 1 d D . . O13 O 0.0887(13) 0.9090(17) 0.8843(11) 0.209(11) Uani 1 1 d D . . O14 O 0.0345(8) 0.894(2) 0.9526(14) 0.190(9) Uani 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 0.028(6) 0.036(6) 0.028(7) -0.007(6) 0.011(5) -0.014(6) C2 0.044(7) 0.045(8) 0.057(8) -0.003(7) 0.026(7) -0.008(7) C3 0.048(8) 0.047(9) 0.077(11) 0.030(8) 0.034(8) 0.008(7) C4 0.044(9) 0.109(14) 0.038(9) 0.005(9) 0.010(7) -0.009(9) C5 0.053(8) 0.055(9) 0.047(8) -0.014(7) 0.030(7) -0.006(7) C6 0.056(9) 0.034(7) 0.066(10) 0.000(7) 0.040(8) 0.006(7) C7 0.027(7) 0.046(8) 0.066(10) 0.008(7) 0.017(7) 0.000(6) C8 0.029(7) 0.034(7) 0.091(11) 0.002(8) 0.032(7) -0.004(6) C9 0.043(8) 0.032(8) 0.043(8) 0.006(6) 0.020(7) 0.014(7) C10 0.069(12) 0.068(12) 0.104(15) -0.006(11) 0.013(11) -0.010(10) Cd1 0.0311(5) 0.0333(5) 0.0433(6) -0.0006(5) 0.0194(4) 0.0003(4) Cl1 0.064(2) 0.067(3) 0.057(2) 0.017(2) 0.032(2) 0.019(2) N1 0.025(5) 0.040(6) 0.036(6) 0.006(5) 0.010(5) 0.004(5) N2 0.040(6) 0.037(6) 0.056(7) 0.006(6) 0.024(5) 0.001(5) N3 0.038(6) 0.050(7) 0.044(7) -0.005(5) 0.013(5) -0.009(5) O1 0.029(4) 0.032(5) 0.063(6) -0.002(4) 0.018(4) -0.001(4) O2 0.038(5) 0.021(4) 0.065(6) -0.016(5) 0.022(4) -0.011(4) O3 0.091(8) 0.045(6) 0.049(6) 0.006(5) 0.026(6) 0.008(5) O4 0.075(7) 0.053(7) 0.065(7) 0.000(5) 0.013(6) -0.014(6) O11 0.123(14) 0.24(2) 0.149(17) 0.036(15) -0.027(13) -0.037(14) O12 0.29(2) 0.070(10) 0.205(18) 0.020(11) 0.184(18) 0.012(12) O13 0.43(3) 0.106(13) 0.180(18) 0.064(12) 0.21(2) 0.054(16) O14 0.156(15) 0.180(18) 0.28(2) 0.061(16) 0.140(17) 0.079(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 C1 N1 1.445(14) . ? C1 C2 1.548(16) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.495(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.472(16) . ? C3 C4 1.52(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.513(19) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.443(16) . ? C5 C6 1.538(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.476(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N1 1.442(15) . ? C7 C8 1.519(17) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.508(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.221(14) . ? C9 O1 1.261(13) . ? C10 O4 1.380(17) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? Cd1 O2 2.267(8) 4_545 ? Cd1 O3 2.304(9) . ? Cd1 O1 2.320(8) . ? Cd1 N2 2.340(10) . ? Cd1 N3 2.379(10) . ? Cd1 N1 2.414(9) . ? Cl1 O11 1.331(9) . ? Cl1 O13 1.332(9) . ? Cl1 O14 1.346(9) . ? Cl1 O12 1.359(9) . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? O2 Cd1 2.267(8) 4 ? O3 H3D 0.8502 . ? O3 H3E 0.8502 . ? O4 H4C 0.8496 . ? 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 N1 C1 C2 115.4(9) . . ? N1 C1 H1A 108.4 . . ? C2 C1 H1A 108.4 . . ? N1 C1 H1B 108.4 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? N2 C2 C1 111.0(10) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C4 113.5(11) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 113.7(11) . . ? N3 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? N3 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N3 C5 C6 113.4(10) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N1 C6 C5 113.1(10) . . ? N1 C6 H6A 108.9 . . ? C5 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? N1 C7 C8 117.3(10) . . ? N1 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? N1 C7 H7B 108.0 . . ? C8 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C9 C8 C7 120.9(11) . . ? C9 C8 H8A 107.1 . . ? C7 C8 H8A 107.1 . . ? C9 C8 H8B 107.1 . . ? C7 C8 H8B 107.1 . . ? H8A C8 H8B 106.8 . . ? O2 C9 O1 122.1(12) . . ? O2 C9 C8 118.4(11) . . ? O1 C9 C8 119.5(11) . . ? O4 C10 H10A 109.5 . . ? O4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 Cd1 O3 92.6(3) 4_545 . ? O2 Cd1 O1 84.3(3) 4_545 . ? O3 Cd1 O1 84.8(3) . . ? O2 Cd1 N2 117.3(3) 4_545 . ? O3 Cd1 N2 100.5(3) . . ? O1 Cd1 N2 157.2(3) . . ? O2 Cd1 N3 94.6(3) 4_545 . ? O3 Cd1 N3 172.8(3) . . ? O1 Cd1 N3 95.5(3) . . ? N2 Cd1 N3 76.5(4) . . ? O2 Cd1 N1 161.2(3) 4_545 . ? O3 Cd1 N1 97.9(3) . . ? O1 Cd1 N1 81.3(3) . . ? N2 Cd1 N1 76.0(3) . . ? N3 Cd1 N1 75.0(3) . . ? O11 Cl1 O13 114.1(16) . . ? O11 Cl1 O14 106.8(16) . . ? O13 Cl1 O14 112.0(12) . . ? O11 Cl1 O12 103.3(13) . . ? O13 Cl1 O12 111.2(11) . . ? O14 Cl1 O12 109.0(12) . . ? C7 N1 C1 108.4(9) . . ? C7 N1 C6 111.9(10) . . ? C1 N1 C6 112.7(9) . . ? C7 N1 Cd1 112.2(7) . . ? C1 N1 Cd1 101.0(7) . . ? C6 N1 Cd1 110.3(7) . . ? C3 N2 C2 114.8(10) . . ? C3 N2 Cd1 103.0(7) . . ? C2 N2 Cd1 112.0(7) . . ? C3 N2 H2C 108.9 . . ? C2 N2 H2C 108.9 . . ? Cd1 N2 H2C 108.9 . . ? C5 N3 C4 114.5(11) . . ? C5 N3 Cd1 105.1(7) . . ? C4 N3 Cd1 108.7(8) . . ? C5 N3 H3C 109.4 . . ? C4 N3 H3C 109.4 . . ? Cd1 N3 H3C 109.4 . . ? C9 O1 Cd1 136.9(8) . . ? C9 O2 Cd1 109.2(8) . 4 ? Cd1 O3 H3D 103.4 . . ? Cd1 O3 H3E 102.2 . . ? H3D O3 H3E 105.9 . . ? C10 O4 H4C 106.1 . . ? 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 C1 C2 N2 -49.0(14) . . . . ? N2 C3 C4 N3 -46.0(15) . . . . ? N3 C5 C6 N1 -49.7(15) . . . . ? N1 C7 C8 C9 64.4(17) . . . . ? C7 C8 C9 O2 154.6(13) . . . . ? C7 C8 C9 O1 -24.7(19) . . . . ? C8 C7 N1 C1 -177.4(10) . . . . ? C8 C7 N1 C6 57.8(14) . . . . ? C8 C7 N1 Cd1 -66.8(13) . . . . ? C2 C1 N1 C7 172.7(10) . . . . ? C2 C1 N1 C6 -62.9(13) . . . . ? C2 C1 N1 Cd1 54.7(10) . . . . ? C5 C6 N1 C7 -107.7(12) . . . . ? C5 C6 N1 C1 129.9(11) . . . . ? C5 C6 N1 Cd1 17.9(12) . . . . ? O2 Cd1 N1 C7 74.1(13) 4_545 . . . ? O3 Cd1 N1 C7 -49.6(8) . . . . ? O1 Cd1 N1 C7 33.9(8) . . . . ? N2 Cd1 N1 C7 -148.5(9) . . . . ? N3 Cd1 N1 C7 132.0(9) . . . . ? O2 Cd1 N1 C1 -170.7(8) 4_545 . . . ? O3 Cd1 N1 C1 65.6(7) . . . . ? O1 Cd1 N1 C1 149.1(7) . . . . ? N2 Cd1 N1 C1 -33.3(6) . . . . ? N3 Cd1 N1 C1 -112.8(7) . . . . ? O2 Cd1 N1 C6 -51.3(14) 4_545 . . . ? O3 Cd1 N1 C6 -175.0(8) . . . . ? O1 Cd1 N1 C6 -91.5(8) . . . . ? N2 Cd1 N1 C6 86.1(8) . . . . ? N3 Cd1 N1 C6 6.6(8) . . . . ? C4 C3 N2 C2 -67.4(14) . . . . ? C4 C3 N2 Cd1 54.7(11) . . . . ? C1 C2 N2 C3 129.7(11) . . . . ? C1 C2 N2 Cd1 12.6(12) . . . . ? O2 Cd1 N2 C3 53.0(9) 4_545 . . . ? O3 Cd1 N2 C3 151.6(8) . . . . ? O1 Cd1 N2 C3 -106.7(10) . . . . ? N3 Cd1 N2 C3 -35.2(8) . . . . ? N1 Cd1 N2 C3 -112.8(8) . . . . ? O2 Cd1 N2 C2 176.9(7) 4_545 . . . ? O3 Cd1 N2 C2 -84.5(8) . . . . ? O1 Cd1 N2 C2 17.3(14) . . . . ? N3 Cd1 N2 C2 88.7(8) . . . . ? N1 Cd1 N2 C2 11.1(8) . . . . ? C6 C5 N3 C4 -66.9(14) . . . . ? C6 C5 N3 Cd1 52.4(12) . . . . ? C3 C4 N3 C5 127.6(12) . . . . ? C3 C4 N3 Cd1 10.3(13) . . . . ? O2 Cd1 N3 C5 133.6(8) 4_545 . . . ? O1 Cd1 N3 C5 49.0(8) . . . . ? N2 Cd1 N3 C5 -109.4(8) . . . . ? N1 Cd1 N3 C5 -30.5(7) . . . . ? O2 Cd1 N3 C4 -103.3(8) 4_545 . . . ? O1 Cd1 N3 C4 172.1(8) . . . . ? N2 Cd1 N3 C4 13.7(8) . . . . ? N1 Cd1 N3 C4 92.6(8) . . . . ? O2 C9 O1 Cd1 -177.9(8) . . . . ? C8 C9 O1 Cd1 1.4(18) . . . . ? O2 Cd1 O1 C9 -173.4(12) 4_545 . . . ? O3 Cd1 O1 C9 93.5(12) . . . . ? N2 Cd1 O1 C9 -11.4(17) . . . . ? N3 Cd1 O1 C9 -79.3(12) . . . . ? N1 Cd1 O1 C9 -5.4(11) . . . . ? O1 C9 O2 Cd1 -8.6(15) . . . 4 ? C8 C9 O2 Cd1 172.2(9) . . . 4 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.324 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.155