# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jon Zubieta' _publ_contact_author_email JAZUBIET@SYR.EDU _publ_section_title ; Chemically and Thermally Stable Microporous Metal Organic Frameworks of the Cadmium(II)/ 4-Pyridyltetrazolate Family and the Structural Influences of Chloride Incorporation. ; loop_ _publ_author_name 'Jon Zubieta' 'Wayne Ouellette' # Attachment 'AllCIFsB907149K.cif' data_pa-3[Cd4(OH)2(4-pt)6(DMF)4]12DMF(112DMF) _database_code_depnum_ccdc_archive 'CCDC 725328' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 CD4 N34 O6, C36 H84 O12 N12' _chemical_formula_sum 'C84 H138 Cd4 N46 O18' _chemical_formula_weight 2530.00 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 Cubic _symmetry_space_group_name_H-M Pa-3 _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 41.5947(4) _cell_length_b 41.5947(4) _cell_length_c 41.5947(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 71963.8(12) _cell_formula_units_Z 24 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6392 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 16.51 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 31200 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8006 _exptl_absorpt_correction_T_max 0.8006 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _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 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 1158528 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.01 _reflns_number_total 21144 _reflns_number_gt 17369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2002)' _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^)+(0.0924P)^2^+526.2036P] 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 21144 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.1152 _refine_ls_wR_factor_ref 0.2548 _refine_ls_wR_factor_gt 0.2379 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.55136(2) 0.674305(17) 0.820911(18) 0.0436(2) Uani 1 1 d . . . Cd2 Cd 0.593877(16) 0.756902(15) 0.787293(15) 0.03047(18) Uani 1 1 d . . . Cd3 Cd 0.480161(17) 0.829697(17) 1.006466(17) 0.0377(2) Uani 1 1 d . . . Cd4 Cd 0.443263(16) 0.783988(17) 1.087021(16) 0.03395(19) Uani 1 1 d . . . O1 O 0.5683(3) 0.6507(3) 0.8695(3) 0.113(4) Uani 1 1 d . . . O2 O 0.4961(3) 0.6689(3) 0.8321(4) 0.138(5) Uani 1 1 d . . . O3 O 0.6349(3) 0.7856(3) 0.8144(3) 0.108(4) Uani 1 1 d . . . O4 O 0.4591(3) 0.8730(2) 0.9794(2) 0.089(3) Uani 1 1 d . . . O5 O 0.4314(3) 0.7281(3) 1.0889(3) 0.099(3) Uani 1 1 d . . . O6 O 0.3950(2) 0.7966(3) 1.1143(3) 0.110(4) Uani 1 1 d . . . N1 N 0.5386(2) 0.7004(2) 0.7709(2) 0.047(2) Uani 1 1 d . . . N2 N 0.5174(2) 0.6912(2) 0.7484(2) 0.050(2) Uani 1 1 d . . . N3 N 0.5540(2) 0.7269(2) 0.7615(2) 0.041(2) Uani 1 1 d . . . N4 N 0.5425(2) 0.7358(2) 0.73291(19) 0.040(2) Uani 1 1 d . . . N5 N 0.4678(2) 0.7174(2) 0.6374(2) 0.051(2) Uani 1 1 d . . . N6 N 0.6058(2) 0.6813(2) 0.8068(2) 0.057(3) Uani 1 1 d . . . N7 N 0.6263(2) 0.6565(2) 0.8041(2) 0.057(3) Uani 1 1 d . . . N8 N 0.6190(2) 0.7086(2) 0.7975(2) 0.053(2) Uani 1 1 d . . . N9 N 0.6494(3) 0.7028(2) 0.7872(3) 0.066(3) Uani 1 1 d . . . N10 N 0.7387(2) 0.6201(2) 0.7655(2) 0.052(2) Uani 1 1 d . . . N11 N 0.5623(2) 0.7510(2) 0.8352(2) 0.048(2) Uani 1 1 d . . . N12 N 0.5533(2) 0.7740(2) 0.8556(2) 0.054(2) Uani 1 1 d . . . N13 N 0.5499(2) 0.7224(2) 0.8456(2) 0.051(2) Uani 1 1 d . . . N14 N 0.5330(2) 0.7277(2) 0.8722(2) 0.051(2) Uani 1 1 d . . . N15 N 0.4913(2) 0.8054(2) 0.9571(2) 0.060(3) Uani 1 1 d . . . N16 N 0.5011(2) 0.7862(2) 1.0347(2) 0.052(2) Uani 1 1 d . . . N17 N 0.4906(2) 0.7713(2) 1.0603(2) 0.049(2) Uani 1 1 d . . . N18 N 0.5122(2) 0.7492(2) 1.0692(2) 0.056(2) Uani 1 1 d . . . N19 N 0.5303(2) 0.7740(2) 1.0266(2) 0.054(2) Uani 1 1 d . . . N20 N 0.6246(2) 0.7017(3) 1.0504(3) 0.063(3) Uani 1 1 d . . . N21 N 0.4696(2) 0.8529(2) 1.0556(2) 0.046(2) Uani 1 1 d . . . N22 N 0.45806(18) 0.8391(2) 1.0822(2) 0.042(2) Uani 1 1 d . . . N23 N 0.4800(2) 0.8824(2) 1.0622(2) 0.047(2) Uani 1 1 d . . . N24 N 0.4616(2) 0.8595(2) 1.10663(19) 0.042(2) Uani 1 1 d . . . N25 N 0.5016(2) 0.9705(2) 1.1453(2) 0.060(3) Uani 1 1 d . . . N26 N 0.43245(19) 0.8016(2) 1.0111(2) 0.041(2) Uani 1 1 d . . . N27 N 0.4183(2) 0.7879(2) 1.0357(2) 0.045(2) Uani 1 1 d . . . N28 N 0.4127(2) 0.8016(2) 0.98548(19) 0.048(2) Uani 1 1 d . . . N29 N 0.38842(17) 0.7790(2) 1.0277(2) 0.040(2) Uani 1 1 d . . . N30 N 0.3030(2) 0.7807(2) 0.9365(2) 0.043(2) Uani 1 1 d . . . C1 C 0.5204(3) 0.7136(2) 0.7256(3) 0.045(3) Uani 1 1 d . . . C2 C 0.5018(3) 0.7148(3) 0.6959(3) 0.052(3) Uani 1 1 d . . . C3 C 0.5076(3) 0.7388(3) 0.6730(3) 0.071(4) Uani 1 1 d . . . H3 H 0.5236 0.7546 0.6768 0.085 Uiso 1 1 calc R . . C4 C 0.4788(3) 0.6920(3) 0.6888(3) 0.054(3) Uani 1 1 d . . . H4 H 0.4736 0.6753 0.7035 0.065 Uiso 1 1 calc R . . C5 C 0.4900(3) 0.7392(3) 0.6449(3) 0.066(4) Uani 1 1 d . . . H5 H 0.4940 0.7561 0.6300 0.079 Uiso 1 1 calc R . . C6 C 0.4631(3) 0.6945(3) 0.6588(3) 0.055(3) Uani 1 1 d . . . H6 H 0.4479 0.6783 0.6536 0.066 Uiso 1 1 calc R . . C7 C 0.6526(3) 0.6712(3) 0.7915(3) 0.053(3) Uani 1 1 d . . . C8 C 0.6817(3) 0.6530(3) 0.7822(3) 0.058(3) Uani 1 1 d . . . C9 C 0.6849(3) 0.6210(3) 0.7883(3) 0.068(4) Uani 1 1 d . . . H9 H 0.6680 0.6092 0.7982 0.081 Uiso 1 1 calc R . . C10 C 0.7076(4) 0.6685(4) 0.7687(4) 0.081(4) Uani 1 1 d . . . H10 H 0.7069 0.6911 0.7655 0.098 Uiso 1 1 calc R . . C11 C 0.7135(3) 0.6059(3) 0.7797(3) 0.061(3) Uani 1 1 d . . . H11 H 0.7154 0.5836 0.7843 0.074 Uiso 1 1 calc R . . C12 C 0.7347(3) 0.6511(3) 0.7597(3) 0.070(4) Uani 1 1 d . . . H12 H 0.7514 0.6622 0.7487 0.084 Uiso 1 1 calc R . . C13 C 0.5353(3) 0.7596(3) 0.8773(2) 0.047(3) Uani 1 1 d . . . C14 C 0.5192(3) 0.7756(3) 0.9048(3) 0.055(3) Uani 1 1 d . . . C15 C 0.5161(3) 0.8084(3) 0.9057(3) 0.068(4) Uani 1 1 d . . . H15 H 0.5223 0.8214 0.8880 0.082 Uiso 1 1 calc R . . C16 C 0.5063(3) 0.7577(3) 0.9293(3) 0.073(4) Uani 1 1 d . . . H16 H 0.5076 0.7349 0.9293 0.088 Uiso 1 1 calc R . . C17 C 0.4912(4) 0.7743(3) 0.9539(3) 0.075(4) Uani 1 1 d . . . H17 H 0.4799 0.7620 0.9695 0.091 Uiso 1 1 calc R . . C18 C 0.5033(3) 0.8219(3) 0.9336(3) 0.062(3) Uani 1 1 d . . . H18 H 0.5034 0.8447 0.9354 0.074 Uiso 1 1 calc R . . C19 C 0.5362(2) 0.7528(3) 1.0476(3) 0.050(3) Uani 1 1 d . . . C20 C 0.5664(3) 0.7341(3) 1.0490(3) 0.062(3) Uani 1 1 d . . . C21 C 0.5727(3) 0.7105(3) 1.0713(4) 0.074(4) Uani 1 1 d . . . H21 H 0.5565 0.7042 1.0861 0.089 Uiso 1 1 calc R . . C22 C 0.5895(3) 0.7402(3) 1.0250(3) 0.070(4) Uani 1 1 d . . . H22 H 0.5856 0.7551 1.0082 0.084 Uiso 1 1 calc R . . C23 C 0.6187(3) 0.7231(3) 1.0272(4) 0.076(4) Uani 1 1 d . . . H23 H 0.6348 0.7270 1.0115 0.091 Uiso 1 1 calc R . . C24 C 0.6023(3) 0.6960(3) 1.0723(4) 0.075(4) Uani 1 1 d . . . H24 H 0.6070 0.6815 1.0893 0.090 Uiso 1 1 calc R . . C25 C 0.3858(2) 0.7873(2) 0.9968(2) 0.038(2) Uani 1 1 d . . . C26 C 0.3574(2) 0.7835(3) 0.9766(3) 0.044(2) Uani 1 1 d . . . C27 C 0.3576(4) 0.7944(7) 0.9457(4) 0.173(13) Uani 1 1 d . . . H27 H 0.3762 0.8044 0.9371 0.208 Uiso 1 1 calc R . . C28 C 0.3302(4) 0.7746(6) 0.9874(4) 0.135(9) Uani 1 1 d . . . H28 H 0.3273 0.7699 1.0095 0.163 Uiso 1 1 calc R . . C29 C 0.3303(4) 0.7909(8) 0.9270(4) 0.179(14) Uani 1 1 d . . . H29 H 0.3321 0.7967 0.9050 0.215 Uiso 1 1 calc R . . C30 C 0.3033(4) 0.7719(5) 0.9647(4) 0.120(8) Uani 1 1 d . . . H30 H 0.2841 0.7623 0.9727 0.144 Uiso 1 1 calc R . . C31 C 0.4756(3) 0.8853(3) 1.0938(3) 0.051(3) Uani 1 1 d . . . C32 C 0.4851(3) 0.9136(3) 1.1117(3) 0.059(3) Uani 1 1 d . . . C33 C 0.4975(4) 0.9404(3) 1.0970(3) 0.079(4) Uani 1 1 d . . . H33 H 0.5007 0.9401 1.0744 0.094 Uiso 1 1 calc R . . C34 C 0.4823(3) 0.9160(3) 1.1446(3) 0.058(3) Uani 1 1 d . . . H34 H 0.4747 0.8981 1.1566 0.069 Uiso 1 1 calc R . . C35 C 0.5053(4) 0.9675(3) 1.1138(3) 0.072(4) Uani 1 1 d . . . H35 H 0.5140 0.9852 1.1022 0.087 Uiso 1 1 calc R . . C36 C 0.4903(3) 0.9434(3) 1.1602(3) 0.063(3) Uani 1 1 d . . . H36 H 0.4879 0.9439 1.1829 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0575(5) 0.0329(4) 0.0405(4) -0.0093(3) 0.0025(4) 0.0061(3) Cd2 0.0335(4) 0.0297(4) 0.0282(3) -0.0076(3) 0.0017(3) 0.0076(3) Cd3 0.0338(4) 0.0418(4) 0.0374(4) -0.0154(3) 0.0065(3) -0.0107(3) Cd4 0.0257(3) 0.0421(4) 0.0340(4) -0.0096(3) -0.0033(3) 0.0011(3) O1 0.173(12) 0.074(7) 0.092(8) -0.002(6) -0.004(8) 0.021(8) O2 0.092(9) 0.125(11) 0.196(15) -0.067(10) 0.022(9) -0.009(8) O3 0.099(8) 0.126(10) 0.099(8) 0.007(7) -0.006(7) 0.002(7) O4 0.144(10) 0.066(6) 0.057(6) 0.008(5) 0.003(6) -0.033(6) O5 0.098(8) 0.097(8) 0.100(8) 0.001(6) 0.010(7) 0.000(6) O6 0.054(6) 0.171(12) 0.104(8) 0.047(8) -0.017(6) -0.023(7) N1 0.056(6) 0.039(5) 0.046(5) -0.014(4) -0.001(4) 0.016(4) N2 0.067(6) 0.040(5) 0.044(5) -0.007(4) -0.018(5) -0.001(4) N3 0.045(5) 0.036(5) 0.043(5) -0.006(4) 0.000(4) 0.011(4) N4 0.045(5) 0.040(5) 0.037(5) -0.003(4) -0.002(4) 0.008(4) N5 0.055(6) 0.044(5) 0.054(6) 0.015(5) -0.004(5) 0.000(4) N6 0.058(6) 0.061(6) 0.050(6) -0.006(5) 0.000(5) 0.021(5) N7 0.060(6) 0.045(5) 0.066(6) 0.003(5) 0.003(5) 0.019(5) N8 0.052(6) 0.050(6) 0.059(6) -0.001(5) 0.005(5) 0.007(5) N9 0.067(7) 0.051(6) 0.078(7) 0.013(5) 0.010(6) 0.020(5) N10 0.053(6) 0.038(5) 0.065(6) 0.011(4) -0.015(5) 0.004(4) N11 0.057(6) 0.037(5) 0.049(5) -0.010(4) -0.004(4) 0.005(4) N12 0.077(7) 0.039(5) 0.047(5) -0.022(4) 0.006(5) 0.010(5) N13 0.058(6) 0.064(6) 0.033(5) -0.016(4) 0.007(4) 0.011(5) N14 0.071(6) 0.038(5) 0.044(5) -0.001(4) 0.014(5) -0.005(4) N15 0.058(6) 0.059(7) 0.063(7) -0.010(5) 0.015(5) -0.020(5) N16 0.027(5) 0.060(6) 0.069(7) -0.019(5) 0.003(4) 0.002(4) N17 0.031(5) 0.054(6) 0.062(6) -0.011(5) -0.012(4) 0.003(4) N18 0.051(6) 0.063(6) 0.053(6) -0.007(5) -0.002(5) 0.003(5) N19 0.031(5) 0.059(6) 0.071(7) 0.006(5) 0.005(5) -0.001(4) N20 0.059(6) 0.063(7) 0.068(7) 0.003(6) 0.020(5) 0.009(5) N21 0.039(5) 0.040(5) 0.058(6) -0.012(4) 0.002(4) 0.004(4) N22 0.027(4) 0.055(5) 0.044(5) -0.013(4) 0.000(4) -0.001(4) N23 0.052(5) 0.042(5) 0.048(5) -0.012(4) 0.013(4) -0.006(4) N24 0.049(5) 0.043(5) 0.035(5) -0.021(4) 0.003(4) -0.004(4) N25 0.071(7) 0.063(6) 0.045(6) -0.010(5) 0.030(5) -0.019(5) N26 0.032(4) 0.047(5) 0.043(5) -0.015(4) -0.002(4) 0.001(4) N27 0.042(5) 0.056(6) 0.036(5) -0.015(4) 0.000(4) -0.004(4) N28 0.040(5) 0.074(6) 0.029(4) 0.000(4) -0.008(4) -0.007(5) N29 0.020(4) 0.058(5) 0.043(5) -0.003(4) -0.007(3) -0.012(4) N30 0.047(5) 0.048(5) 0.033(5) -0.006(4) 0.006(4) -0.008(4) C1 0.047(6) 0.039(6) 0.049(6) -0.005(5) -0.009(5) 0.003(5) C2 0.052(7) 0.051(7) 0.053(7) 0.005(6) -0.003(5) 0.004(6) C3 0.081(9) 0.081(9) 0.051(7) 0.012(7) -0.034(7) -0.034(8) C4 0.054(7) 0.057(7) 0.052(7) 0.017(6) -0.010(6) -0.005(6) C5 0.078(9) 0.054(7) 0.065(8) 0.010(6) -0.009(7) -0.025(7) C6 0.054(7) 0.057(7) 0.054(7) -0.004(6) -0.015(6) -0.004(6) C7 0.041(6) 0.055(7) 0.063(7) 0.008(6) 0.000(5) 0.013(5) C8 0.056(7) 0.052(7) 0.066(8) 0.013(6) -0.004(6) 0.018(6) C9 0.042(7) 0.067(8) 0.093(10) 0.010(7) 0.008(7) 0.019(6) C10 0.076(10) 0.066(9) 0.102(12) 0.026(8) 0.017(9) 0.028(8) C11 0.060(8) 0.048(7) 0.076(9) 0.001(6) 0.001(7) 0.007(6) C12 0.053(7) 0.071(9) 0.088(10) 0.028(7) 0.022(7) 0.013(6) C13 0.058(7) 0.052(7) 0.030(5) -0.007(5) 0.022(5) 0.004(5) C14 0.056(7) 0.048(7) 0.060(7) -0.016(6) 0.010(6) -0.010(6) C15 0.092(10) 0.070(9) 0.043(7) -0.027(6) 0.028(7) -0.006(7) C16 0.099(11) 0.063(8) 0.057(8) -0.036(7) 0.028(7) -0.028(8) C17 0.095(11) 0.064(9) 0.067(9) -0.020(7) 0.037(8) -0.042(8) C18 0.079(9) 0.047(7) 0.060(8) -0.016(6) 0.017(7) 0.006(6) C19 0.028(5) 0.070(8) 0.054(7) -0.021(6) -0.003(5) 0.006(5) C20 0.054(7) 0.067(8) 0.067(8) -0.008(7) 0.004(6) 0.008(6) C21 0.045(7) 0.078(9) 0.100(11) 0.016(8) 0.024(7) 0.018(7) C22 0.058(8) 0.069(9) 0.083(10) 0.016(7) 0.011(7) 0.019(7) C23 0.045(7) 0.081(10) 0.101(11) 0.024(9) 0.013(7) 0.006(7) C24 0.053(8) 0.077(9) 0.096(11) 0.025(8) 0.018(7) 0.015(7) C25 0.031(5) 0.047(6) 0.037(6) -0.013(5) 0.001(4) -0.001(4) C26 0.033(5) 0.051(6) 0.047(6) -0.012(5) 0.003(5) -0.003(5) C27 0.051(10) 0.38(4) 0.090(13) 0.098(19) -0.020(9) -0.060(16) C28 0.077(11) 0.25(3) 0.075(11) 0.074(14) -0.042(9) -0.068(14) C29 0.064(11) 0.40(4) 0.075(12) 0.068(18) -0.020(9) -0.063(18) C30 0.065(10) 0.20(2) 0.100(13) 0.070(14) -0.018(9) -0.058(12) C31 0.059(7) 0.038(6) 0.056(7) -0.019(5) 0.005(6) -0.006(5) C32 0.071(8) 0.049(7) 0.057(7) -0.011(6) 0.015(6) -0.009(6) C33 0.112(12) 0.065(9) 0.058(8) -0.028(7) 0.030(8) -0.029(8) C34 0.084(9) 0.033(6) 0.055(7) -0.015(5) 0.003(6) -0.014(6) C35 0.104(11) 0.047(7) 0.065(9) -0.008(6) 0.031(8) -0.023(7) C36 0.075(9) 0.069(8) 0.044(7) -0.019(6) 0.013(6) -0.016(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 N13 2.249(9) . ? Cd1 N20 2.272(10) 19_557 ? Cd1 O1 2.355(12) . ? Cd1 O2 2.356(13) . ? Cd1 N6 2.358(10) . ? Cd1 N1 2.404(9) . ? Cd2 N8 2.302(9) . ? Cd2 N30 2.311(9) 18_765 ? Cd2 N10 2.323(9) 9 ? Cd2 N3 2.336(9) . ? Cd2 O3 2.368(12) . ? Cd2 N11 2.398(9) . ? Cd3 O4 2.298(10) . ? Cd3 N21 2.303(9) . ? Cd3 N25 2.309(10) 12_675 ? Cd3 N26 2.311(8) . ? Cd3 N16 2.326(10) . ? Cd3 N15 2.335(10) . ? Cd4 N17 2.322(9) . ? Cd4 N5 2.331(9) 15_576 ? Cd4 O6 2.365(12) . ? Cd4 O5 2.378(11) . ? Cd4 N27 2.379(8) . ? Cd4 N22 2.382(9) . ? N1 N3 1.335(12) . ? N1 N2 1.343(12) . ? N2 C1 1.335(14) . ? N3 N4 1.332(11) . ? N4 C1 1.340(13) . ? N5 C6 1.321(14) . ? N5 C5 1.333(14) . ? N5 Cd4 2.331(9) 15_575 ? N6 N8 1.319(13) . ? N6 N7 1.343(12) . ? N7 C7 1.358(15) . ? N8 N9 1.355(13) . ? N9 C7 1.335(14) . ? N10 C12 1.321(15) . ? N10 C11 1.341(15) . ? N10 Cd2 2.323(9) 5 ? N11 N12 1.334(11) . ? N11 N13 1.369(13) . ? N12 C13 1.315(13) . ? N13 N14 1.329(12) . ? N14 C13 1.349(13) . ? N15 C18 1.298(15) . ? N15 C17 1.300(16) . ? N16 N17 1.305(13) . ? N16 N19 1.359(12) . ? N17 N18 1.338(13) . ? N18 C19 1.353(14) . ? N19 C19 1.266(15) . ? N20 C24 1.322(16) . ? N20 C23 1.337(16) . ? N20 Cd1 2.272(10) 22_576 ? N21 N23 1.327(11) . ? N21 N22 1.335(12) . ? N22 N24 1.334(11) . ? N23 C31 1.334(14) . ? N24 C31 1.330(14) . ? N25 C35 1.326(15) . ? N25 C36 1.370(15) . ? N25 Cd3 2.309(10) 6_467 ? N26 N27 1.312(12) . ? N26 N28 1.344(11) . ? N27 N29 1.340(11) . ? N28 C25 1.353(13) . ? N29 C25 1.336(13) . ? N30 C30 1.231(17) . ? N30 C29 1.276(19) . ? N30 Cd2 2.311(9) 24_557 ? C1 C2 1.460(15) . ? C2 C4 1.379(16) . ? C2 C3 1.402(16) . ? C3 C5 1.379(16) . ? C3 H3 0.9500 . ? C4 C6 1.409(15) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.478(15) . ? C8 C9 1.363(17) . ? C8 C10 1.375(18) . ? C9 C11 1.393(16) . ? C9 H9 0.9500 . ? C10 C12 1.392(17) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.481(14) . ? C14 C15 1.370(17) . ? C14 C16 1.372(17) . ? C15 C18 1.393(15) . ? C15 H15 0.9500 . ? C16 C17 1.383(16) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.481(16) . ? C20 C21 1.376(18) . ? C20 C22 1.408(18) . ? C21 C24 1.370(17) . ? C21 H21 0.9500 . ? C22 C23 1.409(17) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.457(14) . ? C26 C28 1.271(18) . ? C26 C27 1.363(19) . ? C27 C29 1.38(2) . ? C27 H27 0.9500 . ? C28 C30 1.47(2) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.449(15) . ? C32 C33 1.372(17) . ? C32 C34 1.377(16) . ? C33 C35 1.366(17) . ? C33 H33 0.9500 . ? C34 C36 1.353(15) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 N13 Cd1 N20 176.3(4) . 19_557 ? N13 Cd1 O1 89.3(4) . . ? N20 Cd1 O1 88.9(4) 19_557 . ? N13 Cd1 O2 88.2(4) . . ? N20 Cd1 O2 88.7(4) 19_557 . ? O1 Cd1 O2 94.7(6) . . ? N13 Cd1 N6 91.7(3) . . ? N20 Cd1 N6 91.6(4) 19_557 . ? O1 Cd1 N6 88.8(4) . . ? O2 Cd1 N6 176.6(5) . . ? N13 Cd1 N1 89.3(3) . . ? N20 Cd1 N1 92.8(3) 19_557 . ? O1 Cd1 N1 175.1(4) . . ? O2 Cd1 N1 89.9(5) . . ? N6 Cd1 N1 86.6(3) . . ? N8 Cd2 N30 173.1(3) . 18_765 ? N8 Cd2 N10 94.6(3) . 9 ? N30 Cd2 N10 91.5(3) 18_765 9 ? N8 Cd2 N3 86.6(3) . . ? N30 Cd2 N3 90.0(3) 18_765 . ? N10 Cd2 N3 90.9(3) 9 . ? N8 Cd2 O3 91.4(4) . . ? N30 Cd2 O3 91.9(4) 18_765 . ? N10 Cd2 O3 90.0(4) 9 . ? N3 Cd2 O3 178.0(4) . . ? N8 Cd2 N11 90.4(3) . . ? N30 Cd2 N11 83.4(3) 18_765 . ? N10 Cd2 N11 174.2(3) 9 . ? N3 Cd2 N11 86.5(3) . . ? O3 Cd2 N11 92.8(4) . . ? O4 Cd3 N21 91.9(3) . . ? O4 Cd3 N25 86.7(4) . 12_675 ? N21 Cd3 N25 93.4(3) . 12_675 ? O4 Cd3 N26 96.4(3) . . ? N21 Cd3 N26 88.6(3) . . ? N25 Cd3 N26 176.3(3) 12_675 . ? O4 Cd3 N16 179.0(4) . . ? N21 Cd3 N16 87.1(3) . . ? N25 Cd3 N16 93.6(4) 12_675 . ? N26 Cd3 N16 83.4(3) . . ? O4 Cd3 N15 89.2(4) . . ? N21 Cd3 N15 178.9(4) . . ? N25 Cd3 N15 86.6(3) 12_675 . ? N26 Cd3 N15 91.4(3) . . ? N16 Cd3 N15 91.8(4) . . ? N17 Cd4 N5 93.1(3) . 15_576 ? N17 Cd4 O6 179.6(4) . . ? N5 Cd4 O6 86.9(3) 15_576 . ? N17 Cd4 O5 88.2(4) . . ? N5 Cd4 O5 92.1(4) 15_576 . ? O6 Cd4 O5 91.4(4) . . ? N17 Cd4 N27 87.5(3) . . ? N5 Cd4 N27 177.5(3) 15_576 . ? O6 Cd4 N27 92.6(3) . . ? O5 Cd4 N27 90.4(4) . . ? N17 Cd4 N22 87.6(3) . . ? N5 Cd4 N22 89.2(3) 15_576 . ? O6 Cd4 N22 92.7(4) . . ? O5 Cd4 N22 175.7(3) . . ? N27 Cd4 N22 88.3(3) . . ? N3 N1 N2 110.2(8) . . ? N3 N1 Cd1 121.5(6) . . ? N2 N1 Cd1 128.3(7) . . ? C1 N2 N1 103.6(9) . . ? N4 N3 N1 108.6(8) . . ? N4 N3 Cd2 121.1(6) . . ? N1 N3 Cd2 130.2(6) . . ? N3 N4 C1 105.0(8) . . ? C6 N5 C5 115.9(10) . . ? C6 N5 Cd4 121.6(8) . 15_575 ? C5 N5 Cd4 122.1(8) . 15_575 ? N8 N6 N7 111.9(9) . . ? N8 N6 Cd1 125.3(7) . . ? N7 N6 Cd1 122.4(8) . . ? N6 N7 C7 101.5(9) . . ? N6 N8 N9 109.1(9) . . ? N6 N8 Cd2 128.1(7) . . ? N9 N8 Cd2 121.4(7) . . ? C7 N9 N8 103.2(10) . . ? C12 N10 C11 114.2(10) . . ? C12 N10 Cd2 122.7(8) . 5 ? C11 N10 Cd2 122.7(7) . 5 ? N12 N11 N13 108.3(9) . . ? N12 N11 Cd2 127.8(7) . . ? N13 N11 Cd2 123.9(6) . . ? C13 N12 N11 105.8(9) . . ? N14 N13 N11 108.6(8) . . ? N14 N13 Cd1 122.8(7) . . ? N11 N13 Cd1 128.3(6) . . ? N13 N14 C13 104.9(8) . . ? C18 N15 C17 116.7(11) . . ? C18 N15 Cd3 120.7(8) . . ? C17 N15 Cd3 121.5(9) . . ? N17 N16 N19 108.9(9) . . ? N17 N16 Cd3 131.0(7) . . ? N19 N16 Cd3 119.9(8) . . ? N16 N17 N18 109.2(9) . . ? N16 N17 Cd4 124.5(7) . . ? N18 N17 Cd4 126.2(8) . . ? N17 N18 C19 103.5(10) . . ? C19 N19 N16 105.1(9) . . ? C24 N20 C23 119.2(11) . . ? C24 N20 Cd1 123.5(9) . 22_576 ? C23 N20 Cd1 117.2(8) . 22_576 ? N23 N21 N22 110.0(8) . . ? N23 N21 Cd3 120.6(7) . . ? N22 N21 Cd3 128.5(6) . . ? N24 N22 N21 108.5(8) . . ? N24 N22 Cd4 125.2(7) . . ? N21 N22 Cd4 125.3(6) . . ? N21 N23 C31 104.1(9) . . ? C31 N24 N22 104.8(8) . . ? C35 N25 C36 114.2(10) . . ? C35 N25 Cd3 121.3(8) . 6_467 ? C36 N25 Cd3 123.9(7) . 6_467 ? N27 N26 N28 110.2(8) . . ? N27 N26 Cd3 132.0(6) . . ? N28 N26 Cd3 117.3(7) . . ? N26 N27 N29 110.0(8) . . ? N26 N27 Cd4 122.4(6) . . ? N29 N27 Cd4 127.6(7) . . ? N26 N28 C25 103.3(8) . . ? C25 N29 N27 104.2(8) . . ? C30 N30 C29 112.6(13) . . ? C30 N30 Cd2 124.4(9) . 24_557 ? C29 N30 Cd2 122.1(10) . 24_557 ? N2 C1 N4 112.5(9) . . ? N2 C1 C2 125.2(10) . . ? N4 C1 C2 122.3(10) . . ? C4 C2 C3 117.8(10) . . ? C4 C2 C1 121.8(10) . . ? C3 C2 C1 120.5(11) . . ? C5 C3 C2 119.5(11) . . ? C5 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C2 C4 C6 117.3(11) . . ? C2 C4 H4 121.3 . . ? C6 C4 H4 121.3 . . ? N5 C5 C3 123.9(12) . . ? N5 C5 H5 118.1 . . ? C3 C5 H5 118.1 . . ? N5 C6 C4 125.6(11) . . ? N5 C6 H6 117.2 . . ? C4 C6 H6 117.2 . . ? N9 C7 N7 114.4(10) . . ? N9 C7 C8 123.6(11) . . ? N7 C7 C8 122.0(10) . . ? C9 C8 C10 117.3(12) . . ? C9 C8 C7 122.2(12) . . ? C10 C8 C7 120.5(11) . . ? C8 C9 C11 118.4(12) . . ? C8 C9 H9 120.8 . . ? C11 C9 H9 120.8 . . ? C8 C10 C12 119.9(13) . . ? C8 C10 H10 120.0 . . ? C12 C10 H10 120.0 . . ? N10 C11 C9 125.7(12) . . ? N10 C11 H11 117.2 . . ? C9 C11 H11 117.2 . . ? N10 C12 C10 124.2(12) . . ? N10 C12 H12 117.9 . . ? C10 C12 H12 117.9 . . ? N12 C13 N14 112.3(8) . . ? N12 C13 C14 125.5(10) . . ? N14 C13 C14 122.2(9) . . ? C15 C14 C16 118.8(11) . . ? C15 C14 C13 120.8(11) . . ? C16 C14 C13 120.4(11) . . ? C14 C15 C18 117.4(12) . . ? C14 C15 H15 121.3 . . ? C18 C15 H15 121.3 . . ? C14 C16 C17 117.3(12) . . ? C14 C16 H16 121.4 . . ? C17 C16 H16 121.4 . . ? N15 C17 C16 124.7(12) . . ? N15 C17 H17 117.6 . . ? C16 C17 H17 117.6 . . ? N15 C18 C15 124.2(12) . . ? N15 C18 H18 117.9 . . ? C15 C18 H18 117.9 . . ? N19 C19 N18 113.2(10) . . ? N19 C19 C20 123.9(11) . . ? N18 C19 C20 122.9(12) . . ? C21 C20 C22 118.5(12) . . ? C21 C20 C19 124.4(12) . . ? C22 C20 C19 117.1(12) . . ? C24 C21 C20 120.3(13) . . ? C24 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C20 C22 C23 116.9(12) . . ? C20 C22 H22 121.6 . . ? C23 C22 H22 121.6 . . ? N20 C23 C22 122.7(13) . . ? N20 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? N20 C24 C21 122.1(13) . . ? N20 C24 H24 119.0 . . ? C21 C24 H24 119.0 . . ? N29 C25 N28 112.3(8) . . ? N29 C25 C26 126.3(9) . . ? N28 C25 C26 121.3(9) . . ? C28 C26 C27 115.6(12) . . ? C28 C26 C25 123.4(11) . . ? C27 C26 C25 120.1(11) . . ? C26 C27 C29 119.4(16) . . ? C26 C27 H27 120.3 . . ? C29 C27 H27 120.3 . . ? C26 C28 C30 118.5(14) . . ? C26 C28 H28 120.8 . . ? C30 C28 H28 120.8 . . ? N30 C29 C27 126.4(16) . . ? N30 C29 H29 116.8 . . ? C27 C29 H29 116.8 . . ? N30 C30 C28 126.6(14) . . ? N30 C30 H30 116.7 . . ? C28 C30 H30 116.7 . . ? N24 C31 N23 112.4(9) . . ? N24 C31 C32 124.7(10) . . ? N23 C31 C32 122.9(11) . . ? C33 C32 C34 114.6(11) . . ? C33 C32 C31 122.2(11) . . ? C34 C32 C31 123.2(11) . . ? C35 C33 C32 122.0(12) . . ? C35 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C36 C34 C32 121.2(12) . . ? C36 C34 H34 119.4 . . ? C32 C34 H34 119.4 . . ? N25 C35 C33 123.9(12) . . ? N25 C35 H35 118.1 . . ? C33 C35 H35 118.1 . . ? C34 C36 N25 124.0(11) . . ? C34 C36 H36 118.0 . . ? N25 C36 H36 118.0 . . ? 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 N13 Cd1 N1 N3 47.0(7) . . . . ? N20 Cd1 N1 N3 -136.1(7) 19_557 . . . ? O1 Cd1 N1 N3 -25(4) . . . . ? O2 Cd1 N1 N3 135.2(7) . . . . ? N6 Cd1 N1 N3 -44.7(7) . . . . ? N13 Cd1 N1 N2 -135.9(8) . . . . ? N20 Cd1 N1 N2 41.0(8) 19_557 . . . ? O1 Cd1 N1 N2 152(4) . . . . ? O2 Cd1 N1 N2 -47.8(8) . . . . ? N6 Cd1 N1 N2 132.4(8) . . . . ? N3 N1 N2 C1 -1.3(11) . . . . ? Cd1 N1 N2 C1 -178.6(7) . . . . ? N2 N1 N3 N4 1.4(10) . . . . ? Cd1 N1 N3 N4 178.9(6) . . . . ? N2 N1 N3 Cd2 -179.8(6) . . . . ? Cd1 N1 N3 Cd2 -2.3(11) . . . . ? N8 Cd2 N3 N4 -134.3(7) . . . . ? N30 Cd2 N3 N4 51.7(7) 18_765 . . . ? N10 Cd2 N3 N4 -39.7(7) 9 . . . ? O3 Cd2 N3 N4 -155(10) . . . . ? N11 Cd2 N3 N4 135.1(7) . . . . ? N8 Cd2 N3 N1 47.0(8) . . . . ? N30 Cd2 N3 N1 -127.0(8) 18_765 . . . ? N10 Cd2 N3 N1 141.6(8) 9 . . . ? O3 Cd2 N3 N1 27(11) . . . . ? N11 Cd2 N3 N1 -43.6(8) . . . . ? N1 N3 N4 C1 -0.8(10) . . . . ? Cd2 N3 N4 C1 -179.8(6) . . . . ? N13 Cd1 N6 N8 -38.7(9) . . . . ? N20 Cd1 N6 N8 143.2(9) 19_557 . . . ? O1 Cd1 N6 N8 -127.9(9) . . . . ? O2 Cd1 N6 N8 48(7) . . . . ? N1 Cd1 N6 N8 50.5(9) . . . . ? N13 Cd1 N6 N7 149.0(8) . . . . ? N20 Cd1 N6 N7 -29.1(9) 19_557 . . . ? O1 Cd1 N6 N7 59.8(8) . . . . ? O2 Cd1 N6 N7 -124(7) . . . . ? N1 Cd1 N6 N7 -121.8(8) . . . . ? N8 N6 N7 C7 -1.5(12) . . . . ? Cd1 N6 N7 C7 171.7(7) . . . . ? N7 N6 N8 N9 1.2(13) . . . . ? Cd1 N6 N8 N9 -171.8(7) . . . . ? N7 N6 N8 Cd2 167.2(7) . . . . ? Cd1 N6 N8 Cd2 -5.8(13) . . . . ? N30 Cd2 N8 N6 18(3) 18_765 . . . ? N10 Cd2 N8 N6 -132.9(9) 9 . . . ? N3 Cd2 N8 N6 -42.2(9) . . . . ? O3 Cd2 N8 N6 137.0(9) . . . . ? N11 Cd2 N8 N6 44.2(9) . . . . ? N30 Cd2 N8 N9 -177(23) 18_765 . . . ? N10 Cd2 N8 N9 31.6(9) 9 . . . ? N3 Cd2 N8 N9 122.2(9) . . . . ? O3 Cd2 N8 N9 -58.5(9) . . . . ? N11 Cd2 N8 N9 -151.3(9) . . . . ? N6 N8 N9 C7 -0.3(13) . . . . ? Cd2 N8 N9 C7 -167.4(8) . . . . ? N8 Cd2 N11 N12 143.1(9) . . . . ? N30 Cd2 N11 N12 -40.0(9) 18_765 . . . ? N10 Cd2 N11 N12 -67(3) 9 . . . ? N3 Cd2 N11 N12 -130.3(9) . . . . ? O3 Cd2 N11 N12 51.6(9) . . . . ? N8 Cd2 N11 N13 -38.5(8) . . . . ? N30 Cd2 N11 N13 138.5(8) 18_765 . . . ? N10 Cd2 N11 N13 112(3) 9 . . . ? N3 Cd2 N11 N13 48.1(8) . . . . ? O3 Cd2 N11 N13 -130.0(8) . . . . ? N13 N11 N12 C13 -1.2(12) . . . . ? Cd2 N11 N12 C13 177.4(7) . . . . ? N12 N11 N13 N14 0.6(12) . . . . ? Cd2 N11 N13 N14 -178.1(7) . . . . ? N12 N11 N13 Cd1 173.8(7) . . . . ? Cd2 N11 N13 Cd1 -4.9(12) . . . . ? N20 Cd1 N13 N14 6(6) 19_557 . . . ? O1 Cd1 N13 N14 -55.2(9) . . . . ? O2 Cd1 N13 N14 39.5(9) . . . . ? N6 Cd1 N13 N14 -144.0(9) . . . . ? N1 Cd1 N13 N14 129.4(9) . . . . ? N20 Cd1 N13 N11 -166(5) 19_557 . . . ? O1 Cd1 N13 N11 132.4(9) . . . . ? O2 Cd1 N13 N11 -132.9(10) . . . . ? N6 Cd1 N13 N11 43.7(9) . . . . ? N1 Cd1 N13 N11 -42.9(9) . . . . ? N11 N13 N14 C13 0.3(12) . . . . ? Cd1 N13 N14 C13 -173.4(7) . . . . ? O4 Cd3 N15 C18 42.6(10) . . . . ? N21 Cd3 N15 C18 -133(19) . . . . ? N25 Cd3 N15 C18 -44.1(10) 12_675 . . . ? N26 Cd3 N15 C18 139.0(10) . . . . ? N16 Cd3 N15 C18 -137.6(10) . . . . ? O4 Cd3 N15 C17 -149.5(11) . . . . ? N21 Cd3 N15 C17 35(19) . . . . ? N25 Cd3 N15 C17 123.8(11) 12_675 . . . ? N26 Cd3 N15 C17 -53.1(11) . . . . ? N16 Cd3 N15 C17 30.3(11) . . . . ? O4 Cd3 N16 N17 30(22) . . . . ? N21 Cd3 N16 N17 42.5(9) . . . . ? N25 Cd3 N16 N17 135.8(9) 12_675 . . . ? N26 Cd3 N16 N17 -46.3(9) . . . . ? N15 Cd3 N16 N17 -137.5(9) . . . . ? O4 Cd3 N16 N19 -144(22) . . . . ? N21 Cd3 N16 N19 -131.4(8) . . . . ? N25 Cd3 N16 N19 -38.2(8) 12_675 . . . ? N26 Cd3 N16 N19 139.7(8) . . . . ? N15 Cd3 N16 N19 48.5(8) . . . . ? N19 N16 N17 N18 -0.6(11) . . . . ? Cd3 N16 N17 N18 -175.1(7) . . . . ? N19 N16 N17 Cd4 176.2(6) . . . . ? Cd3 N16 N17 Cd4 1.7(13) . . . . ? N5 Cd4 N17 N16 -133.6(8) 15_576 . . . ? O6 Cd4 N17 N16 145(68) . . . . ? O5 Cd4 N17 N16 134.4(8) . . . . ? N27 Cd4 N17 N16 43.9(8) . . . . ? N22 Cd4 N17 N16 -44.5(8) . . . . ? N5 Cd4 N17 N18 42.6(8) 15_576 . . . ? O6 Cd4 N17 N18 -39(62) . . . . ? O5 Cd4 N17 N18 -49.3(8) . . . . ? N27 Cd4 N17 N18 -139.8(8) . . . . ? N22 Cd4 N17 N18 131.8(8) . . . . ? N16 N17 N18 C19 1.4(11) . . . . ? Cd4 N17 N18 C19 -175.3(7) . . . . ? N17 N16 N19 C19 -0.6(12) . . . . ? Cd3 N16 N19 C19 174.6(7) . . . . ? O4 Cd3 N21 N23 -53.2(8) . . . . ? N25 Cd3 N21 N23 33.6(8) 12_675 . . . ? N26 Cd3 N21 N23 -149.5(8) . . . . ? N16 Cd3 N21 N23 127.0(8) . . . . ? N15 Cd3 N21 N23 123(19) . . . . ? O4 Cd3 N21 N22 138.5(8) . . . . ? N25 Cd3 N21 N22 -134.7(8) 12_675 . . . ? N26 Cd3 N21 N22 42.2(8) . . . . ? N16 Cd3 N21 N22 -41.2(8) . . . . ? N15 Cd3 N21 N22 -46(19) . . . . ? N23 N21 N22 N24 -1.5(11) . . . . ? Cd3 N21 N22 N24 167.8(6) . . . . ? N23 N21 N22 Cd4 -170.5(6) . . . . ? Cd3 N21 N22 Cd4 -1.2(11) . . . . ? N17 Cd4 N22 N24 -122.6(7) . . . . ? N5 Cd4 N22 N24 -29.5(7) 15_576 . . . ? O6 Cd4 N22 N24 57.4(8) . . . . ? O5 Cd4 N22 N24 -138(5) . . . . ? N27 Cd4 N22 N24 149.9(7) . . . . ? N17 Cd4 N22 N21 44.7(7) . . . . ? N5 Cd4 N22 N21 137.8(8) 15_576 . . . ? O6 Cd4 N22 N21 -135.4(8) . . . . ? O5 Cd4 N22 N21 30(5) . . . . ? N27 Cd4 N22 N21 -42.8(7) . . . . ? N22 N21 N23 C31 2.6(11) . . . . ? Cd3 N21 N23 C31 -167.6(7) . . . . ? N21 N22 N24 C31 -0.4(11) . . . . ? Cd4 N22 N24 C31 168.7(7) . . . . ? O4 Cd3 N26 N27 -130.3(9) . . . . ? N21 Cd3 N26 N27 -38.5(9) . . . . ? N25 Cd3 N26 N27 84(5) 12_675 . . . ? N16 Cd3 N26 N27 48.8(9) . . . . ? N15 Cd3 N26 N27 140.4(9) . . . . ? O4 Cd3 N26 N28 40.4(7) . . . . ? N21 Cd3 N26 N28 132.2(7) . . . . ? N25 Cd3 N26 N28 -105(5) 12_675 . . . ? N16 Cd3 N26 N28 -140.5(7) . . . . ? N15 Cd3 N26 N28 -48.9(7) . . . . ? N28 N26 N27 N29 -1.3(11) . . . . ? Cd3 N26 N27 N29 169.9(6) . . . . ? N28 N26 N27 Cd4 -177.7(6) . . . . ? Cd3 N26 N27 Cd4 -6.5(12) . . . . ? N17 Cd4 N27 N26 -41.4(8) . . . . ? N5 Cd4 N27 N26 61(7) 15_576 . . . ? O6 Cd4 N27 N26 139.0(8) . . . . ? O5 Cd4 N27 N26 -129.6(8) . . . . ? N22 Cd4 N27 N26 46.4(7) . . . . ? N17 Cd4 N27 N29 142.9(8) . . . . ? N5 Cd4 N27 N29 -115(7) 15_576 . . . ? O6 Cd4 N27 N29 -36.8(9) . . . . ? O5 Cd4 N27 N29 54.6(8) . . . . ? N22 Cd4 N27 N29 -129.4(8) . . . . ? N27 N26 N28 C25 0.6(11) . . . . ? Cd3 N26 N28 C25 -172.1(6) . . . . ? N26 N27 N29 C25 1.4(11) . . . . ? Cd4 N27 N29 C25 177.6(7) . . . . ? N1 N2 C1 N4 0.7(12) . . . . ? N1 N2 C1 C2 -178.6(10) . . . . ? N3 N4 C1 N2 0.0(12) . . . . ? N3 N4 C1 C2 179.4(9) . . . . ? N2 C1 C2 C4 0.0(18) . . . . ? N4 C1 C2 C4 -179.2(11) . . . . ? N2 C1 C2 C3 -177.7(12) . . . . ? N4 C1 C2 C3 3.1(18) . . . . ? C4 C2 C3 C5 1(2) . . . . ? C1 C2 C3 C5 179.2(12) . . . . ? C3 C2 C4 C6 0.6(18) . . . . ? C1 C2 C4 C6 -177.2(11) . . . . ? C6 N5 C5 C3 0(2) . . . . ? Cd4 N5 C5 C3 -172.6(11) 15_575 . . . ? C2 C3 C5 N5 -2(2) . . . . ? C5 N5 C6 C4 2.0(18) . . . . ? Cd4 N5 C6 C4 174.9(9) 15_575 . . . ? C2 C4 C6 N5 -2.4(19) . . . . ? N8 N9 C7 N7 -0.7(14) . . . . ? N8 N9 C7 C8 177.0(11) . . . . ? N6 N7 C7 N9 1.3(14) . . . . ? N6 N7 C7 C8 -176.4(11) . . . . ? N9 C7 C8 C9 176.6(13) . . . . ? N7 C7 C8 C9 -6(2) . . . . ? N9 C7 C8 C10 1(2) . . . . ? N7 C7 C8 C10 178.2(13) . . . . ? C10 C8 C9 C11 -2(2) . . . . ? C7 C8 C9 C11 -178.0(12) . . . . ? C9 C8 C10 C12 5(2) . . . . ? C7 C8 C10 C12 -179.2(13) . . . . ? C12 N10 C11 C9 0.0(19) . . . . ? Cd2 N10 C11 C9 173.5(10) 5 . . . ? C8 C9 C11 N10 0(2) . . . . ? C11 N10 C12 C10 3(2) . . . . ? Cd2 N10 C12 C10 -170.6(12) 5 . . . ? C8 C10 C12 N10 -5(2) . . . . ? N11 N12 C13 N14 1.5(13) . . . . ? N11 N12 C13 C14 -178.8(11) . . . . ? N13 N14 C13 N12 -1.1(14) . . . . ? N13 N14 C13 C14 179.2(11) . . . . ? N12 C13 C14 C15 15(2) . . . . ? N14 C13 C14 C15 -165.7(12) . . . . ? N12 C13 C14 C16 -167.5(13) . . . . ? N14 C13 C14 C16 12.2(19) . . . . ? C16 C14 C15 C18 8(2) . . . . ? C13 C14 C15 C18 -174.2(12) . . . . ? C15 C14 C16 C17 -1(2) . . . . ? C13 C14 C16 C17 -179.1(12) . . . . ? C18 N15 C17 C16 8(2) . . . . ? Cd3 N15 C17 C16 -160.0(12) . . . . ? C14 C16 C17 N15 -7(2) . . . . ? C17 N15 C18 C15 -1(2) . . . . ? Cd3 N15 C18 C15 167.8(11) . . . . ? C14 C15 C18 N15 -7(2) . . . . ? N16 N19 C19 N18 1.6(13) . . . . ? N16 N19 C19 C20 -177.2(10) . . . . ? N17 N18 C19 N19 -1.9(13) . . . . ? N17 N18 C19 C20 176.8(10) . . . . ? N19 C19 C20 C21 -178.5(13) . . . . ? N18 C19 C20 C21 3(2) . . . . ? N19 C19 C20 C22 -1.3(19) . . . . ? N18 C19 C20 C22 -179.9(12) . . . . ? C22 C20 C21 C24 8(2) . . . . ? C19 C20 C21 C24 -175.3(13) . . . . ? C21 C20 C22 C23 -5(2) . . . . ? C19 C20 C22 C23 177.9(12) . . . . ? C24 N20 C23 C22 0(2) . . . . ? Cd1 N20 C23 C22 -176.3(11) 22_576 . . . ? C20 C22 C23 N20 1(2) . . . . ? C23 N20 C24 C21 3(2) . . . . ? Cd1 N20 C24 C21 178.9(11) 22_576 . . . ? C20 C21 C24 N20 -7(2) . . . . ? N27 N29 C25 N28 -1.1(11) . . . . ? N27 N29 C25 C26 -178.6(10) . . . . ? N26 N28 C25 N29 0.3(11) . . . . ? N26 N28 C25 C26 178.0(9) . . . . ? N29 C25 C26 C28 8(2) . . . . ? N28 C25 C26 C28 -169.3(17) . . . . ? N29 C25 C26 C27 177.0(18) . . . . ? N28 C25 C26 C27 0(2) . . . . ? C28 C26 C27 C29 -9(4) . . . . ? C25 C26 C27 C29 -179(2) . . . . ? C27 C26 C28 C30 10(3) . . . . ? C25 C26 C28 C30 179.4(16) . . . . ? C30 N30 C29 C27 -4(4) . . . . ? Cd2 N30 C29 C27 165(3) 24_557 . . . ? C26 C27 C29 N30 7(5) . . . . ? C29 N30 C30 C28 5(3) . . . . ? Cd2 N30 C30 C28 -164.1(18) 24_557 . . . ? C26 C28 C30 N30 -9(4) . . . . ? N22 N24 C31 N23 2.1(13) . . . . ? N22 N24 C31 C32 -178.1(11) . . . . ? N21 N23 C31 N24 -2.9(13) . . . . ? N21 N23 C31 C32 177.2(11) . . . . ? N24 C31 C32 C33 -175.6(13) . . . . ? N23 C31 C32 C33 4(2) . . . . ? N24 C31 C32 C34 4(2) . . . . ? N23 C31 C32 C34 -176.2(12) . . . . ? C34 C32 C33 C35 -2(2) . . . . ? C31 C32 C33 C35 177.6(14) . . . . ? C33 C32 C34 C36 2(2) . . . . ? C31 C32 C34 C36 -177.2(13) . . . . ? C36 N25 C35 C33 3(2) . . . . ? Cd3 N25 C35 C33 -168.5(12) 6_467 . . . ? C32 C33 C35 N25 -1(3) . . . . ? C32 C34 C36 N25 0(2) . . . . ? C35 N25 C36 C34 -2(2) . . . . ? Cd3 N25 C36 C34 168.5(10) 6_467 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.468 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.127 #### data_pbcn[Cd4Cl3(4-pt)4(OH)(DMF)3]8DMF14MeOH(28DMF14MeOH) _database_code_depnum_ccdc_archive 'CCDC 725329' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H38 Cd4 Cl3 N23 O4, C24 H56 O8 N8, C12 O12 H48' _chemical_formula_sum 'C69 H142 Cd4 Cl3 N31 O24' _chemical_formula_weight 2346.09 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall -P2n2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 35.5933(10) _cell_length_b 20.8616(6) _cell_length_c 22.2038(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16487.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7919 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 20.93 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9664 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8111 _exptl_absorpt_correction_T_max 0.9307 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _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 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 160645 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14416 _reflns_number_gt 10125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2006)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2002)' _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^)+(0.1640P)^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 14416 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.2463 _refine_ls_wR_factor_gt 0.2352 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.08200(2) 0.59534(4) 0.36581(5) 0.0472(3) Uani 1 1 d . . . Cd2 Cd 0.156497(17) 0.73077(3) 0.38184(3) 0.02083(19) Uani 1 1 d . . . Cd3 Cd 0.165250(17) 0.85614(3) 0.25714(3) 0.02021(19) Uani 1 1 d . . . Cd4 Cd 0.091943(18) 0.84850(3) 0.13343(3) 0.02090(19) Uani 1 1 d . . . Cl1 Cl 0.09860(7) 0.68755(13) 0.44055(11) 0.0332(6) Uani 1 1 d . . . Cl2 Cl 0.20803(6) 0.76926(12) 0.30445(11) 0.0305(5) Uani 1 1 d . . . Cl3 Cl 0.11483(6) 0.93276(11) 0.21244(10) 0.0260(5) Uani 1 1 d . . . O90 O 0.0740(4) 0.5168(6) 0.4420(7) 0.102(4) Uani 1 1 d . . . O91 O 0.0699(3) 0.5145(5) 0.2971(5) 0.072(3) Uani 1 1 d . . . O92 O 0.03053(18) 0.8730(3) 0.1565(3) 0.0322(16) Uani 1 1 d . . . O93 O 0.0711(2) 0.7730(4) 0.0600(4) 0.049(2) Uani 1 1 d . . . N1 N 0.1426(3) 0.5814(4) 0.3455(5) 0.048(3) Uani 1 1 d . . . N2 N 0.1688(2) 0.6254(4) 0.3562(4) 0.034(2) Uani 1 1 d . . . N3 N 0.1608(3) 0.5271(5) 0.3203(5) 0.044(2) Uani 1 1 d . . . N4 N 0.2031(2) 0.6045(4) 0.3404(4) 0.036(2) Uani 1 1 d . . . N5 N 0.2876(3) 0.4284(5) 0.2622(4) 0.042(2) Uani 1 1 d . . . N6 N 0.1413(2) 0.8359(4) 0.3964(3) 0.0242(17) Uani 1 1 d . . . N7 N 0.1455(2) 0.8803(4) 0.3544(4) 0.0323(19) Uani 1 1 d . . . N8 N 0.1363(2) 0.9375(5) 0.3770(4) 0.033(2) Uani 1 1 d . . . N9 N 0.1280(2) 0.8638(5) 0.4482(4) 0.037(2) Uani 1 1 d . . . N10 N 0.0959(2) 1.0697(5) 0.5598(4) 0.038(2) Uani 1 1 d . . . N11 N 0.1165(2) 0.7288(4) 0.2923(3) 0.0251(17) Uani 1 1 d . . . N12 N 0.1167(2) 0.7763(3) 0.2540(3) 0.0207(16) Uani 1 1 d . . . N13 N 0.09035(19) 0.7663(4) 0.2136(3) 0.0205(16) Uani 1 1 d . . . N14 N 0.08907(19) 0.6867(4) 0.2772(4) 0.0240(17) Uani 1 1 d . . . N15 N -0.0215(2) 0.6286(4) 0.1463(4) 0.0265(18) Uani 1 1 d . . . N16 N 0.1792(2) 0.8237(4) 0.1608(4) 0.0278(18) Uani 1 1 d . . . N17 N 0.1553(2) 0.8187(4) 0.1171(4) 0.033(2) Uani 1 1 d . . . N18 N 0.1726(2) 0.8083(4) 0.0634(4) 0.0271(18) Uani 1 1 d . . . N19 N 0.2143(2) 0.8117(4) 0.1386(4) 0.0314(19) Uani 1 1 d . . . N20 N 0.2968(2) 0.7744(4) -0.0447(4) 0.034(2) Uani 1 1 d . . . C1 C 0.1966(3) 0.5455(5) 0.3196(5) 0.037(3) Uani 1 1 d . . . C2 C 0.2271(3) 0.5071(4) 0.2985(5) 0.031(2) Uani 1 1 d . . . C3 C 0.2209(3) 0.4484(6) 0.2694(5) 0.042(3) Uani 1 1 d . . . H3 H 0.1960 0.4340 0.2621 0.050 Uiso 1 1 calc R . . C4 C 0.2642(3) 0.5257(5) 0.3073(6) 0.041(3) Uani 1 1 d . . . H4 H 0.2700 0.5659 0.3251 0.049 Uiso 1 1 calc R . . C5 C 0.2933(3) 0.4828(6) 0.2889(6) 0.051(3) Uani 1 1 d . . . H5 H 0.3185 0.4949 0.2968 0.061 Uiso 1 1 calc R . . C6 C 0.2512(3) 0.4115(5) 0.2513(5) 0.040(3) Uani 1 1 d . . . H6 H 0.2464 0.3726 0.2303 0.047 Uiso 1 1 calc R . . C7 C 0.1258(3) 0.9260(5) 0.4334(5) 0.031(2) Uani 1 1 d . . . C8 C 0.1146(2) 0.9770(4) 0.4775(4) 0.023(2) Uani 1 1 d . . . C9 C 0.1172(4) 1.0401(6) 0.4597(5) 0.049(3) Uani 1 1 d . . . H9 H 0.1257 1.0521 0.4207 0.059 Uiso 1 1 calc R . . C10 C 0.1026(3) 0.9595(5) 0.5341(4) 0.028(2) Uani 1 1 d . . . H10 H 0.0998 0.9158 0.5452 0.034 Uiso 1 1 calc R . . C11 C 0.0947(3) 1.0086(6) 0.5743(5) 0.042(3) Uani 1 1 d . . . H11 H 0.0880 0.9976 0.6144 0.050 Uiso 1 1 calc R . . C12 C 0.1064(4) 1.0855(6) 0.5031(5) 0.044(3) Uani 1 1 d . . . H12 H 0.1064 1.1295 0.4921 0.053 Uiso 1 1 calc R . . C13 C 0.0736(2) 0.7101(4) 0.2292(3) 0.0123(16) Uani 1 1 d . . . C14 C 0.0427(2) 0.6813(4) 0.1972(4) 0.0202(18) Uani 1 1 d . . . C15 C 0.0156(2) 0.7201(4) 0.1686(4) 0.0158(17) Uani 1 1 d . . . H15 H 0.0191 0.7652 0.1666 0.019 Uiso 1 1 calc R . . C16 C 0.0365(2) 0.6155(4) 0.1965(4) 0.0214(19) Uani 1 1 d . . . H16 H 0.0542 0.5870 0.2140 0.026 Uiso 1 1 calc R . . C17 C 0.0047(3) 0.5925(5) 0.1703(5) 0.033(2) Uani 1 1 d . . . H17 H 0.0012 0.5473 0.1694 0.039 Uiso 1 1 calc R . . C18 C -0.0155(3) 0.6927(5) 0.1441(4) 0.028(2) Uani 1 1 d . . . H18 H -0.0336 0.7193 0.1250 0.034 Uiso 1 1 calc R . . C19 C 0.2079(3) 0.8020(5) 0.0797(4) 0.031(2) Uani 1 1 d . . . C20 C 0.2387(3) 0.7922(5) 0.0377(4) 0.027(2) Uani 1 1 d . . . C21 C 0.2327(3) 0.8057(7) -0.0256(5) 0.050(3) Uani 1 1 d . . . H21 H 0.2096 0.8221 -0.0406 0.060 Uiso 1 1 calc R . . C22 C 0.2747(3) 0.7739(7) 0.0565(5) 0.053(4) Uani 1 1 d . . . H22 H 0.2801 0.7673 0.0980 0.064 Uiso 1 1 calc R . . C23 C 0.3023(3) 0.7659(7) 0.0131(6) 0.055(3) Uani 1 1 d . . . H23 H 0.3267 0.7534 0.0260 0.066 Uiso 1 1 calc R . . C24 C 0.2636(3) 0.7926(6) -0.0631(5) 0.047(3) Uani 1 1 d . . . H24 H 0.2600 0.7975 -0.1052 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0271(5) 0.0417(5) 0.0728(7) -0.0015(4) -0.0039(4) 0.0089(4) Cd2 0.0127(3) 0.0312(4) 0.0186(3) -0.0036(3) -0.0039(2) 0.0059(3) Cd3 0.0126(3) 0.0276(4) 0.0205(4) -0.0053(3) 0.0016(2) -0.0035(3) Cd4 0.0149(3) 0.0272(4) 0.0207(4) 0.0046(3) 0.0033(2) -0.0017(3) Cl1 0.0233(12) 0.0487(15) 0.0275(12) 0.0044(11) -0.0014(10) 0.0044(11) Cl2 0.0165(11) 0.0445(14) 0.0304(12) -0.0051(11) 0.0003(9) 0.0023(10) Cl3 0.0226(11) 0.0278(12) 0.0277(12) -0.0022(9) 0.0040(9) -0.0017(9) O90 0.092(9) 0.074(8) 0.139(12) 0.002(8) -0.014(8) 0.020(7) O91 0.039(5) 0.083(7) 0.094(8) -0.014(6) -0.015(5) 0.007(5) O92 0.021(4) 0.039(4) 0.036(4) 0.004(3) 0.005(3) -0.004(3) O93 0.035(4) 0.073(6) 0.040(5) 0.011(4) 0.004(4) -0.011(4) N1 0.028(5) 0.032(5) 0.085(8) 0.009(5) 0.007(5) 0.011(4) N2 0.018(4) 0.044(5) 0.040(5) 0.008(4) -0.004(4) 0.011(4) N3 0.032(5) 0.043(6) 0.056(6) -0.009(5) 0.000(4) 0.013(4) N4 0.021(4) 0.035(5) 0.050(6) 0.002(4) -0.004(4) 0.003(4) N5 0.030(5) 0.049(6) 0.048(6) 0.000(5) 0.008(4) -0.005(4) N6 0.015(4) 0.035(4) 0.023(4) -0.011(3) -0.001(3) 0.013(3) N7 0.025(4) 0.032(5) 0.040(5) -0.007(4) 0.000(4) 0.001(4) N8 0.027(5) 0.055(6) 0.018(4) -0.009(4) -0.002(3) -0.002(4) N9 0.031(5) 0.054(6) 0.027(5) -0.013(4) 0.003(4) 0.005(4) N10 0.031(5) 0.046(6) 0.037(5) -0.003(4) 0.001(4) 0.006(4) N11 0.021(4) 0.030(4) 0.024(4) 0.001(3) 0.005(3) 0.010(3) N12 0.019(4) 0.029(4) 0.014(4) -0.003(3) 0.002(3) 0.010(3) N13 0.012(4) 0.032(4) 0.017(4) 0.001(3) 0.004(3) 0.006(3) N14 0.011(4) 0.031(4) 0.030(4) 0.003(3) 0.001(3) -0.005(3) N15 0.016(4) 0.030(4) 0.033(4) -0.003(3) 0.005(3) -0.009(3) N16 0.021(4) 0.040(5) 0.022(4) 0.000(4) 0.003(3) -0.006(4) N17 0.025(4) 0.039(5) 0.035(5) 0.002(4) 0.013(4) 0.000(4) N18 0.024(4) 0.029(4) 0.028(4) -0.002(3) 0.007(3) 0.000(3) N19 0.012(4) 0.037(5) 0.045(5) -0.001(4) 0.006(3) -0.004(3) N20 0.026(5) 0.049(5) 0.027(5) 0.005(4) 0.003(4) 0.005(4) C1 0.024(5) 0.028(5) 0.058(7) -0.004(5) -0.008(5) 0.006(4) C2 0.034(6) 0.022(5) 0.037(6) -0.006(4) -0.003(5) 0.007(4) C3 0.033(6) 0.047(7) 0.045(7) -0.012(5) -0.010(5) 0.008(5) C4 0.024(5) 0.032(6) 0.066(8) -0.007(5) -0.006(5) 0.001(4) C5 0.027(6) 0.049(7) 0.076(9) -0.014(6) -0.008(6) 0.013(5) C6 0.032(6) 0.038(6) 0.049(7) -0.006(5) -0.013(5) 0.004(5) C7 0.027(5) 0.037(6) 0.031(6) -0.023(5) 0.001(4) 0.006(4) C8 0.020(5) 0.028(5) 0.022(5) -0.012(4) 0.005(4) 0.003(4) C9 0.055(8) 0.059(8) 0.034(6) -0.021(6) 0.002(6) 0.017(6) C10 0.034(5) 0.023(5) 0.028(5) -0.009(4) 0.014(4) -0.001(4) C11 0.042(7) 0.043(7) 0.040(6) -0.004(5) 0.009(5) -0.008(5) C12 0.057(8) 0.041(6) 0.034(6) -0.002(5) -0.002(6) 0.007(6) C13 0.006(4) 0.018(4) 0.012(4) 0.001(3) -0.001(3) -0.009(3) C14 0.021(5) 0.021(4) 0.018(4) -0.001(3) 0.008(4) 0.008(4) C15 0.016(4) 0.017(4) 0.014(4) 0.005(3) 0.000(3) -0.005(3) C16 0.013(4) 0.021(4) 0.031(5) 0.011(4) 0.002(4) 0.002(3) C17 0.024(5) 0.027(5) 0.047(6) 0.002(4) 0.000(5) -0.005(4) C18 0.018(5) 0.052(6) 0.015(4) -0.002(4) 0.001(4) 0.006(4) C19 0.023(5) 0.043(6) 0.026(5) 0.008(4) -0.002(4) 0.008(4) C20 0.025(5) 0.033(5) 0.023(5) -0.008(4) 0.002(4) 0.006(4) C21 0.032(6) 0.076(9) 0.041(7) -0.007(6) 0.008(5) 0.020(6) C22 0.024(6) 0.108(11) 0.027(6) 0.005(6) 0.008(5) -0.002(6) C23 0.020(6) 0.072(9) 0.073(9) 0.004(7) -0.001(6) 0.008(6) C24 0.039(7) 0.069(8) 0.034(6) -0.003(6) 0.003(5) 0.019(6) _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 N1 2.224(9) . ? Cd1 N15 2.280(7) 3 ? Cd1 O91 2.314(11) . ? Cd1 O90 2.372(14) . ? Cd1 Cl1 2.608(3) . ? Cd2 N6 2.282(8) . ? Cd2 N2 2.312(9) . ? Cd2 N20 2.333(8) 2_565 ? Cd2 N11 2.445(8) . ? Cd2 Cl1 2.600(3) . ? Cd2 Cl2 2.639(2) . ? Cd3 N5 2.260(10) 8_665 ? Cd3 N16 2.299(8) . ? Cd3 N7 2.326(9) . ? Cd3 N12 2.401(8) . ? Cd3 Cl2 2.590(3) . ? Cd3 Cl3 2.600(2) . ? Cd4 O92 2.302(7) . ? Cd4 N10 2.368(9) 7_575 ? Cd4 N17 2.368(8) . ? Cd4 O93 2.385(9) . ? Cd4 N13 2.472(7) . ? Cd4 Cl3 2.614(2) . ? N1 N2 1.330(13) . ? N1 N3 1.420(13) . ? N2 N4 1.342(12) . ? N3 C1 1.330(14) . ? N4 C1 1.334(13) . ? N5 C5 1.295(15) . ? N5 C6 1.365(14) . ? N5 Cd3 2.260(10) 8_655 ? N6 N7 1.323(12) . ? N6 N9 1.374(11) . ? N7 N8 1.335(12) . ? N8 C7 1.330(13) . ? N9 C7 1.342(14) . ? N10 C11 1.315(15) . ? N10 C12 1.353(15) . ? N10 Cd4 2.368(9) 7_576 ? N11 N12 1.306(10) . ? N11 N14 1.355(11) . ? N12 N13 1.314(10) . ? N13 C13 1.360(11) . ? N14 C13 1.296(11) . ? N15 C17 1.310(13) . ? N15 C18 1.356(13) . ? N15 Cd1 2.280(7) 3 ? N16 N17 1.294(12) . ? N16 N19 1.365(11) . ? N17 N18 1.359(11) . ? N18 C19 1.312(12) . ? N19 C19 1.342(13) . ? N20 C24 1.307(14) . ? N20 C23 1.311(16) . ? N20 Cd2 2.333(8) 2_564 ? C1 C2 1.427(14) . ? C2 C4 1.390(15) . ? C2 C3 1.402(14) . ? C3 C6 1.383(15) . ? C3 H3 0.9500 . ? C4 C5 1.430(15) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.498(12) . ? C8 C10 1.378(13) . ? C8 C9 1.378(16) . ? C9 C12 1.405(15) . ? C9 H9 0.9500 . ? C10 C11 1.387(14) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.442(12) . ? C14 C16 1.391(13) . ? C14 C15 1.409(12) . ? C15 C18 1.360(12) . ? C15 H15 0.9500 . ? C16 C17 1.361(13) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.456(13) . ? C20 C22 1.401(15) . ? C20 C21 1.449(15) . ? C21 C24 1.404(15) . ? C21 H21 0.9500 . ? C22 C23 1.385(17) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? 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 Cd1 N15 158.9(4) . 3 ? N1 Cd1 O91 87.2(4) . . ? N15 Cd1 O91 88.2(3) 3 . ? N1 Cd1 O90 99.9(4) . . ? N15 Cd1 O90 100.4(4) 3 . ? O91 Cd1 O90 86.8(5) . . ? N1 Cd1 Cl1 90.3(3) . . ? N15 Cd1 Cl1 93.7(2) 3 . ? O91 Cd1 Cl1 177.3(3) . . ? O90 Cd1 Cl1 94.8(3) . . ? N6 Cd2 N2 173.4(3) . . ? N6 Cd2 N20 96.6(3) . 2_565 ? N2 Cd2 N20 89.6(3) . 2_565 ? N6 Cd2 N11 89.6(3) . . ? N2 Cd2 N11 83.9(3) . . ? N20 Cd2 N11 169.4(3) 2_565 . ? N6 Cd2 Cl1 94.3(2) . . ? N2 Cd2 Cl1 86.8(2) . . ? N20 Cd2 Cl1 101.5(2) 2_565 . ? N11 Cd2 Cl1 86.59(19) . . ? N6 Cd2 Cl2 88.0(2) . . ? N2 Cd2 Cl2 89.8(2) . . ? N20 Cd2 Cl2 88.5(2) 2_565 . ? N11 Cd2 Cl2 83.12(19) . . ? Cl1 Cd2 Cl2 169.46(8) . . ? N5 Cd3 N16 94.7(3) 8_665 . ? N5 Cd3 N7 91.9(3) 8_665 . ? N16 Cd3 N7 173.4(3) . . ? N5 Cd3 N12 177.7(3) 8_665 . ? N16 Cd3 N12 85.7(3) . . ? N7 Cd3 N12 87.7(3) . . ? N5 Cd3 Cl2 90.6(2) 8_665 . ? N16 Cd3 Cl2 92.5(2) . . ? N7 Cd3 Cl2 87.3(2) . . ? N12 Cd3 Cl2 87.11(18) . . ? N5 Cd3 Cl3 97.0(2) 8_665 . ? N16 Cd3 Cl3 88.6(2) . . ? N7 Cd3 Cl3 90.7(2) . . ? N12 Cd3 Cl3 85.32(18) . . ? Cl2 Cd3 Cl3 172.25(8) . . ? O92 Cd4 N10 92.9(3) . 7_575 ? O92 Cd4 N17 175.4(3) . . ? N10 Cd4 N17 91.5(3) 7_575 . ? O92 Cd4 O93 90.2(3) . . ? N10 Cd4 O93 91.3(3) 7_575 . ? N17 Cd4 O93 91.1(3) . . ? O92 Cd4 N13 88.4(2) . . ? N10 Cd4 N13 176.9(3) 7_575 . ? N17 Cd4 N13 87.2(3) . . ? O93 Cd4 N13 91.6(3) . . ? O92 Cd4 Cl3 89.85(19) . . ? N10 Cd4 Cl3 87.7(2) 7_575 . ? N17 Cd4 Cl3 89.0(2) . . ? O93 Cd4 Cl3 179.0(2) . . ? N13 Cd4 Cl3 89.44(18) . . ? Cd2 Cl1 Cd1 96.68(8) . . ? Cd3 Cl2 Cd2 93.92(7) . . ? Cd3 Cl3 Cd4 93.32(7) . . ? N2 N1 N3 107.5(8) . . ? N2 N1 Cd1 123.6(7) . . ? N3 N1 Cd1 128.8(7) . . ? N1 N2 N4 111.4(9) . . ? N1 N2 Cd2 124.6(6) . . ? N4 N2 Cd2 123.1(7) . . ? C1 N3 N1 102.2(9) . . ? C1 N4 N2 103.5(8) . . ? C5 N5 C6 117.3(10) . . ? C5 N5 Cd3 119.4(8) . 8_655 ? C6 N5 Cd3 121.5(7) . 8_655 ? N7 N6 N9 109.4(8) . . ? N7 N6 Cd2 123.1(6) . . ? N9 N6 Cd2 127.4(7) . . ? N6 N7 N8 109.5(8) . . ? N6 N7 Cd3 122.4(6) . . ? N8 N7 Cd3 128.0(7) . . ? C7 N8 N7 105.2(9) . . ? C7 N9 N6 103.0(8) . . ? C11 N10 C12 118.3(10) . . ? C11 N10 Cd4 121.7(8) . 7_576 ? C12 N10 Cd4 118.9(8) . 7_576 ? N12 N11 N14 109.5(7) . . ? N12 N11 Cd2 120.9(6) . . ? N14 N11 Cd2 129.1(6) . . ? N11 N12 N13 108.7(7) . . ? N11 N12 Cd3 120.7(6) . . ? N13 N12 Cd3 130.1(6) . . ? N12 N13 C13 106.0(7) . . ? N12 N13 Cd4 111.4(5) . . ? C13 N13 Cd4 142.3(6) . . ? C13 N14 N11 105.4(7) . . ? C17 N15 C18 118.1(8) . . ? C17 N15 Cd1 122.9(6) . 3 ? C18 N15 Cd1 116.3(6) . 3 ? N17 N16 N19 108.4(8) . . ? N17 N16 Cd3 125.4(6) . . ? N19 N16 Cd3 126.0(6) . . ? N16 N17 N18 111.9(8) . . ? N16 N17 Cd4 119.4(6) . . ? N18 N17 Cd4 127.4(6) . . ? C19 N18 N17 101.9(8) . . ? C19 N19 N16 102.9(8) . . ? C24 N20 C23 118.7(10) . . ? C24 N20 Cd2 116.1(7) . 2_564 ? C23 N20 Cd2 124.9(7) . 2_564 ? N3 C1 N4 115.3(9) . . ? N3 C1 C2 124.7(10) . . ? N4 C1 C2 120.0(9) . . ? C4 C2 C3 117.1(10) . . ? C4 C2 C1 121.3(9) . . ? C3 C2 C1 121.6(10) . . ? C6 C3 C2 120.0(10) . . ? C6 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C2 C4 C5 118.2(10) . . ? C2 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N5 C5 C4 124.4(11) . . ? N5 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? N5 C6 C3 122.8(10) . . ? N5 C6 H6 118.6 . . ? C3 C6 H6 118.6 . . ? N8 C7 N9 112.9(8) . . ? N8 C7 C8 124.2(10) . . ? N9 C7 C8 122.8(9) . . ? C10 C8 C9 122.3(9) . . ? C10 C8 C7 119.5(9) . . ? C9 C8 C7 118.2(9) . . ? C8 C9 C12 115.4(11) . . ? C8 C9 H9 122.3 . . ? C12 C9 H9 122.3 . . ? C8 C10 C11 117.1(9) . . ? C8 C10 H10 121.5 . . ? C11 C10 H10 121.5 . . ? N10 C11 C10 123.4(11) . . ? N10 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? N10 C12 C9 123.3(11) . . ? N10 C12 H12 118.3 . . ? C9 C12 H12 118.3 . . ? N14 C13 N13 110.4(7) . . ? N14 C13 C14 125.0(7) . . ? N13 C13 C14 124.6(7) . . ? C16 C14 C15 116.9(8) . . ? C16 C14 C13 122.6(8) . . ? C15 C14 C13 120.3(8) . . ? C18 C15 C14 119.8(8) . . ? C18 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C14 119.0(8) . . ? C17 C16 H16 120.5 . . ? C14 C16 H16 120.5 . . ? N15 C17 C16 124.2(9) . . ? N15 C17 H17 117.9 . . ? C16 C17 H17 117.9 . . ? N15 C18 C15 121.8(9) . . ? N15 C18 H18 119.1 . . ? C15 C18 H18 119.1 . . ? N18 C19 N19 114.6(9) . . ? N18 C19 C20 124.0(9) . . ? N19 C19 C20 121.1(8) . . ? C22 C20 C21 118.6(9) . . ? C22 C20 C19 122.5(9) . . ? C21 C20 C19 118.8(9) . . ? C24 C21 C20 114.9(10) . . ? C24 C21 H21 122.6 . . ? C20 C21 H21 122.6 . . ? C23 C22 C20 118.2(11) . . ? C23 C22 H22 120.9 . . ? C20 C22 H22 120.9 . . ? N20 C23 C22 124.0(11) . . ? N20 C23 H23 118.0 . . ? C22 C23 H23 118.0 . . ? N20 C24 C21 125.4(11) . . ? N20 C24 H24 117.3 . . ? C21 C24 H24 117.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Cd2 Cl1 Cd1 138.1(2) . . . . ? N2 Cd2 Cl1 Cd1 -35.4(2) . . . . ? N20 Cd2 Cl1 Cd1 -124.4(2) 2_565 . . . ? N11 Cd2 Cl1 Cd1 48.68(19) . . . . ? Cl2 Cd2 Cl1 Cd1 36.1(5) . . . . ? N1 Cd1 Cl1 Cd2 33.7(3) . . . . ? N15 Cd1 Cl1 Cd2 -125.6(2) 3 . . . ? O91 Cd1 Cl1 Cd2 8(6) . . . . ? O90 Cd1 Cl1 Cd2 133.6(3) . . . . ? N5 Cd3 Cl2 Cd2 133.5(3) 8_665 . . . ? N16 Cd3 Cl2 Cd2 -131.8(2) . . . . ? N7 Cd3 Cl2 Cd2 41.6(2) . . . . ? N12 Cd3 Cl2 Cd2 -46.27(17) . . . . ? Cl3 Cd3 Cl2 Cd2 -33.7(6) . . . . ? N6 Cd2 Cl2 Cd3 -41.0(2) . . . . ? N2 Cd2 Cl2 Cd3 132.7(2) . . . . ? N20 Cd2 Cl2 Cd3 -137.7(2) 2_565 . . . ? N11 Cd2 Cl2 Cd3 48.84(19) . . . . ? Cl1 Cd2 Cl2 Cd3 61.5(5) . . . . ? N5 Cd3 Cl3 Cd4 135.5(3) 8_665 . . . ? N16 Cd3 Cl3 Cd4 40.9(2) . . . . ? N7 Cd3 Cl3 Cd4 -132.5(2) . . . . ? N12 Cd3 Cl3 Cd4 -44.82(17) . . . . ? Cl2 Cd3 Cl3 Cd4 -57.4(6) . . . . ? O92 Cd4 Cl3 Cd3 135.07(18) . . . . ? N10 Cd4 Cl3 Cd3 -132.0(2) 7_575 . . . ? N17 Cd4 Cl3 Cd3 -40.5(2) . . . . ? O93 Cd4 Cl3 Cd3 -134(12) . . . . ? N13 Cd4 Cl3 Cd3 46.69(17) . . . . ? N15 Cd1 N1 N2 81.8(14) 3 . . . ? O91 Cd1 N1 N2 159.4(10) . . . . ? O90 Cd1 N1 N2 -114.4(9) . . . . ? Cl1 Cd1 N1 N2 -19.5(9) . . . . ? N15 Cd1 N1 N3 -98.8(12) 3 . . . ? O91 Cd1 N1 N3 -21.2(10) . . . . ? O90 Cd1 N1 N3 65.1(11) . . . . ? Cl1 Cd1 N1 N3 160.0(10) . . . . ? N3 N1 N2 N4 -0.3(12) . . . . ? Cd1 N1 N2 N4 179.2(7) . . . . ? N3 N1 N2 Cd2 169.1(7) . . . . ? Cd1 N1 N2 Cd2 -11.4(13) . . . . ? N6 Cd2 N2 N1 -65(3) . . . . ? N20 Cd2 N2 N1 136.5(9) 2_565 . . . ? N11 Cd2 N2 N1 -51.9(9) . . . . ? Cl1 Cd2 N2 N1 35.0(9) . . . . ? Cl2 Cd2 N2 N1 -135.0(9) . . . . ? N6 Cd2 N2 N4 104(3) . . . . ? N20 Cd2 N2 N4 -55.3(8) 2_565 . . . ? N11 Cd2 N2 N4 116.3(8) . . . . ? Cl1 Cd2 N2 N4 -156.8(8) . . . . ? Cl2 Cd2 N2 N4 33.2(8) . . . . ? N2 N1 N3 C1 0.5(12) . . . . ? Cd1 N1 N3 C1 -179.0(8) . . . . ? N1 N2 N4 C1 0.0(12) . . . . ? Cd2 N2 N4 C1 -169.6(7) . . . . ? N2 Cd2 N6 N7 -41(3) . . . . ? N20 Cd2 N6 N7 117.4(7) 2_565 . . . ? N11 Cd2 N6 N7 -54.0(7) . . . . ? Cl1 Cd2 N6 N7 -140.5(7) . . . . ? Cl2 Cd2 N6 N7 29.1(7) . . . . ? N2 Cd2 N6 N9 141(2) . . . . ? N20 Cd2 N6 N9 -60.5(8) 2_565 . . . ? N11 Cd2 N6 N9 128.2(7) . . . . ? Cl1 Cd2 N6 N9 41.6(7) . . . . ? Cl2 Cd2 N6 N9 -148.7(7) . . . . ? N9 N6 N7 N8 1.6(10) . . . . ? Cd2 N6 N7 N8 -176.6(6) . . . . ? N9 N6 N7 Cd3 -177.6(6) . . . . ? Cd2 N6 N7 Cd3 4.2(10) . . . . ? N5 Cd3 N7 N6 -126.2(7) 8_665 . . . ? N16 Cd3 N7 N6 53(3) . . . . ? N12 Cd3 N7 N6 51.5(7) . . . . ? Cl2 Cd3 N7 N6 -35.7(7) . . . . ? Cl3 Cd3 N7 N6 136.8(7) . . . . ? N5 Cd3 N7 N8 54.8(8) 8_665 . . . ? N16 Cd3 N7 N8 -126(2) . . . . ? N12 Cd3 N7 N8 -127.5(8) . . . . ? Cl2 Cd3 N7 N8 145.3(8) . . . . ? Cl3 Cd3 N7 N8 -42.2(8) . . . . ? N6 N7 N8 C7 -1.1(10) . . . . ? Cd3 N7 N8 C7 178.1(7) . . . . ? N7 N6 N9 C7 -1.5(10) . . . . ? Cd2 N6 N9 C7 176.6(6) . . . . ? N6 Cd2 N11 N12 42.5(6) . . . . ? N2 Cd2 N11 N12 -136.1(6) . . . . ? N20 Cd2 N11 N12 -83.5(17) 2_565 . . . ? Cl1 Cd2 N11 N12 136.8(6) . . . . ? Cl2 Cd2 N11 N12 -45.5(6) . . . . ? N6 Cd2 N11 N14 -129.2(7) . . . . ? N2 Cd2 N11 N14 52.2(7) . . . . ? N20 Cd2 N11 N14 104.8(17) 2_565 . . . ? Cl1 Cd2 N11 N14 -34.9(7) . . . . ? Cl2 Cd2 N11 N14 142.8(7) . . . . ? N14 N11 N12 N13 -0.7(9) . . . . ? Cd2 N11 N12 N13 -173.9(5) . . . . ? N14 N11 N12 Cd3 -173.2(5) . . . . ? Cd2 N11 N12 Cd3 13.6(8) . . . . ? N5 Cd3 N12 N11 20(8) 8_665 . . . ? N16 Cd3 N12 N11 119.6(6) . . . . ? N7 Cd3 N12 N11 -60.6(6) . . . . ? Cl2 Cd3 N12 N11 26.8(6) . . . . ? Cl3 Cd3 N12 N11 -151.5(6) . . . . ? N5 Cd3 N12 N13 -150(7) 8_665 . . . ? N16 Cd3 N12 N13 -51.2(7) . . . . ? N7 Cd3 N12 N13 128.6(7) . . . . ? Cl2 Cd3 N12 N13 -144.0(7) . . . . ? Cl3 Cd3 N12 N13 37.7(7) . . . . ? N11 N12 N13 C13 0.4(9) . . . . ? Cd3 N12 N13 C13 172.0(5) . . . . ? N11 N12 N13 Cd4 -174.9(5) . . . . ? Cd3 N12 N13 Cd4 -3.3(8) . . . . ? O92 Cd4 N13 N12 -122.6(5) . . . . ? N10 Cd4 N13 N12 -8(6) 7_575 . . . ? N17 Cd4 N13 N12 56.3(6) . . . . ? O93 Cd4 N13 N12 147.3(5) . . . . ? Cl3 Cd4 N13 N12 -32.7(5) . . . . ? O92 Cd4 N13 C13 64.9(9) . . . . ? N10 Cd4 N13 C13 180(100) 7_575 . . . ? N17 Cd4 N13 C13 -116.2(9) . . . . ? O93 Cd4 N13 C13 -25.2(9) . . . . ? Cl3 Cd4 N13 C13 154.8(9) . . . . ? N12 N11 N14 C13 0.7(9) . . . . ? Cd2 N11 N14 C13 173.2(6) . . . . ? N5 Cd3 N16 N17 -130.9(8) 8_665 . . . ? N7 Cd3 N16 N17 50(3) . . . . ? N12 Cd3 N16 N17 51.4(8) . . . . ? Cl2 Cd3 N16 N17 138.3(8) . . . . ? Cl3 Cd3 N16 N17 -34.0(8) . . . . ? N5 Cd3 N16 N19 43.3(8) 8_665 . . . ? N7 Cd3 N16 N19 -136(2) . . . . ? N12 Cd3 N16 N19 -134.4(8) . . . . ? Cl2 Cd3 N16 N19 -47.5(7) . . . . ? Cl3 Cd3 N16 N19 140.2(7) . . . . ? N19 N16 N17 N18 -4.7(11) . . . . ? Cd3 N16 N17 N18 170.3(6) . . . . ? N19 N16 N17 Cd4 -172.4(6) . . . . ? Cd3 N16 N17 Cd4 2.6(10) . . . . ? O92 Cd4 N17 N16 -45(4) . . . . ? N10 Cd4 N17 N16 117.9(7) 7_575 . . . ? O93 Cd4 N17 N16 -150.8(7) . . . . ? N13 Cd4 N17 N16 -59.3(7) . . . . ? Cl3 Cd4 N17 N16 30.2(7) . . . . ? O92 Cd4 N17 N18 149(3) . . . . ? N10 Cd4 N17 N18 -47.7(8) 7_575 . . . ? O93 Cd4 N17 N18 43.6(8) . . . . ? N13 Cd4 N17 N18 135.1(8) . . . . ? Cl3 Cd4 N17 N18 -135.4(8) . . . . ? N16 N17 N18 C19 5.3(11) . . . . ? Cd4 N17 N18 C19 171.9(7) . . . . ? N17 N16 N19 C19 1.9(10) . . . . ? Cd3 N16 N19 C19 -173.0(7) . . . . ? N1 N3 C1 N4 -0.6(14) . . . . ? N1 N3 C1 C2 179.4(11) . . . . ? N2 N4 C1 N3 0.4(13) . . . . ? N2 N4 C1 C2 -179.6(10) . . . . ? N3 C1 C2 C4 -170.3(12) . . . . ? N4 C1 C2 C4 9.7(17) . . . . ? N3 C1 C2 C3 8.1(18) . . . . ? N4 C1 C2 C3 -171.9(11) . . . . ? C4 C2 C3 C6 0.6(17) . . . . ? C1 C2 C3 C6 -177.9(11) . . . . ? C3 C2 C4 C5 -2.9(17) . . . . ? C1 C2 C4 C5 175.5(11) . . . . ? C6 N5 C5 C4 0(2) . . . . ? Cd3 N5 C5 C4 -164.9(10) 8_655 . . . ? C2 C4 C5 N5 3(2) . . . . ? C5 N5 C6 C3 -2.5(18) . . . . ? Cd3 N5 C6 C3 161.9(9) 8_655 . . . ? C2 C3 C6 N5 2.3(18) . . . . ? N7 N8 C7 N9 0.1(11) . . . . ? N7 N8 C7 C8 177.2(9) . . . . ? N6 N9 C7 N8 0.8(11) . . . . ? N6 N9 C7 C8 -176.3(8) . . . . ? N8 C7 C8 C10 177.1(10) . . . . ? N9 C7 C8 C10 -6.2(15) . . . . ? N8 C7 C8 C9 -3.7(15) . . . . ? N9 C7 C8 C9 173.1(10) . . . . ? C10 C8 C9 C12 -0.6(17) . . . . ? C7 C8 C9 C12 -179.8(10) . . . . ? C9 C8 C10 C11 -2.9(16) . . . . ? C7 C8 C10 C11 176.3(9) . . . . ? C12 N10 C11 C10 -1.7(17) . . . . ? Cd4 N10 C11 C10 -169.9(8) 7_576 . . . ? C8 C10 C11 N10 4.2(17) . . . . ? C11 N10 C12 C9 -2.3(18) . . . . ? Cd4 N10 C12 C9 166.2(10) 7_576 . . . ? C8 C9 C12 N10 3.3(18) . . . . ? N11 N14 C13 N13 -0.5(9) . . . . ? N11 N14 C13 C14 -179.7(8) . . . . ? N12 N13 C13 N14 0.1(9) . . . . ? Cd4 N13 C13 N14 172.8(7) . . . . ? N12 N13 C13 C14 179.3(8) . . . . ? Cd4 N13 C13 C14 -7.9(14) . . . . ? N14 C13 C14 C16 -29.0(13) . . . . ? N13 C13 C14 C16 151.9(8) . . . . ? N14 C13 C14 C15 146.2(9) . . . . ? N13 C13 C14 C15 -32.9(12) . . . . ? C16 C14 C15 C18 2.4(12) . . . . ? C13 C14 C15 C18 -173.0(8) . . . . ? C15 C14 C16 C17 -1.8(13) . . . . ? C13 C14 C16 C17 173.5(9) . . . . ? C18 N15 C17 C16 3.9(15) . . . . ? Cd1 N15 C17 C16 -157.0(8) 3 . . . ? C14 C16 C17 N15 -1.4(15) . . . . ? C17 N15 C18 C15 -3.2(13) . . . . ? Cd1 N15 C18 C15 159.0(7) 3 . . . ? C14 C15 C18 N15 0.0(13) . . . . ? N17 N18 C19 N19 -4.1(11) . . . . ? N17 N18 C19 C20 -177.7(10) . . . . ? N16 N19 C19 N18 1.5(12) . . . . ? N16 N19 C19 C20 175.3(9) . . . . ? N18 C19 C20 C22 -168.0(11) . . . . ? N19 C19 C20 C22 18.9(17) . . . . ? N18 C19 C20 C21 16.1(16) . . . . ? N19 C19 C20 C21 -157.1(11) . . . . ? C22 C20 C21 C24 6.1(17) . . . . ? C19 C20 C21 C24 -177.8(11) . . . . ? C21 C20 C22 C23 -3.9(19) . . . . ? C19 C20 C22 C23 -179.9(12) . . . . ? C24 N20 C23 C22 1(2) . . . . ? Cd2 N20 C23 C22 174.9(11) 2_564 . . . ? C20 C22 C23 N20 0(2) . . . . ? C23 N20 C24 C21 2(2) . . . . ? Cd2 N20 C24 C21 -172.7(11) 2_564 . . . ? C20 C21 C24 N20 -5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.040 _refine_diff_density_min -1.239 _refine_diff_density_rms 0.216 data_c2c[Cd5Cl6(4-pt)4(DMF)2(H2O)2]10DMF(310DMF) _database_code_depnum_ccdc_archive 'CCDC 725330' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 Cd5 Cl6 N22 O4, C30 H70 O10 N10' _chemical_formula_sum 'C60 H104 Cd5 Cl6 N32 O14' _chemical_formula_weight 2272.45 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc 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 29.728(5) _cell_length_b 12.530(2) _cell_length_c 20.920(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.847(4) _cell_angle_gamma 90.00 _cell_volume 7071(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3684 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.17 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4568 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6930 _exptl_absorpt_correction_T_max 0.9315 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _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 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 33877 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5064 _reflns_number_gt 3605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1410P)^2^+81.9517P] 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 5064 _refine_ls_number_parameters 306 _refine_ls_number_restraints 315 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2339 _refine_ls_wR_factor_gt 0.2225 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.24975(4) 1.11708(7) 0.23966(5) 0.0171(3) Uani 1 1 d U . . Cd2 Cd 0.25487(4) 0.89305(7) 0.34534(5) 0.0156(3) Uani 1 1 d U . . Cd3 Cd 0.0000 0.5000 0.5000 0.0395(5) Uani 1 2 d SU . . Cl1 Cl 0.18546(13) 1.2280(2) 0.13232(17) 0.0215(8) Uani 1 1 d U . . Cl2 Cl 0.32301(14) 1.0275(3) 0.34932(18) 0.0274(8) Uani 1 1 d U . . Cl3 Cl 0.18653(13) 1.0422(3) 0.28246(18) 0.0250(8) Uani 1 1 d U . . O1 O -0.0324(5) 0.3765(10) 0.4130(8) 0.055(3) Uani 1 1 d U . . O2 O -0.0502(6) 0.6385(13) 0.4289(10) 0.085(5) Uani 1 1 d U . . N1 N 0.2437(4) 0.9466(7) 0.1819(5) 0.0113(19) Uani 1 1 d U . . N2 N 0.2411(4) 0.8688(8) 0.2233(6) 0.021(2) Uani 1 1 d U . . N3 N 0.2416(4) 0.7740(8) 0.1949(5) 0.016(2) Uani 1 1 d U . . N4 N 0.2443(4) 0.7876(8) 0.1334(5) 0.013(2) Uani 1 1 d U . . N5 N 0.2603(4) 1.0440(8) -0.0476(5) 0.018(2) Uani 1 1 d U . . N6 N 0.1672(4) 0.7588(8) 0.3716(6) 0.022(2) Uani 1 1 d U . . N7 N 0.1961(4) 0.7620(8) 0.3352(5) 0.016(2) Uani 1 1 d U . . N8 N 0.1922(4) 0.6689(8) 0.3024(5) 0.017(2) Uani 1 1 d U . . N9 N 0.1613(5) 0.6045(8) 0.3152(6) 0.026(3) Uani 1 1 d U . . N10 N 0.0575(5) 0.5430(11) 0.4584(8) 0.043(3) Uani 1 1 d U . . N11 N -0.0897(5) 0.3144(11) 0.3098(8) 0.048(3) Uani 1 1 d U . . C1 C 0.2467(6) 0.8983(10) 0.1255(8) 0.027(3) Uani 1 1 d U . . C2 C 0.2514(5) 0.9462(10) 0.0678(6) 0.014(2) Uani 1 1 d U . . C3 C 0.2368(5) 1.0504(10) 0.0484(6) 0.015(2) Uani 1 1 d U . . H3 H 0.2230 1.0910 0.0740 0.017 Uiso 1 1 calc R . . C4 C 0.2423(4) 1.0957(9) -0.0079(6) 0.008(2) Uani 1 1 d U . . H4 H 0.2327 1.1681 -0.0190 0.010 Uiso 1 1 calc R . . C5 C 0.2740(6) 0.9419(10) -0.0312(7) 0.023(3) Uani 1 1 d U . . H5 H 0.2862 0.9021 -0.0593 0.028 Uiso 1 1 calc R . . C6 C 0.2706(6) 0.8934(11) 0.0268(7) 0.029(3) Uani 1 1 d U . . H6 H 0.2818 0.8220 0.0384 0.035 Uiso 1 1 calc R . . C7 C 0.1474(5) 0.6607(11) 0.3574(7) 0.020(3) Uani 1 1 d U . . C8 C 0.1160(6) 0.6212(12) 0.3917(9) 0.033(3) Uani 1 1 d U . . C9 C 0.0935(7) 0.5231(13) 0.3763(10) 0.048(4) Uani 1 1 d U . . H9 H 0.0980 0.4775 0.3432 0.058 Uiso 1 1 calc R . . C10 C 0.1119(7) 0.6774(14) 0.4439(9) 0.047(4) Uani 1 1 d U . . H10 H 0.1288 0.7434 0.4586 0.057 Uiso 1 1 calc R . . C11 C 0.0821(7) 0.6375(15) 0.4767(10) 0.053(5) Uani 1 1 d U . . H11 H 0.0792 0.6785 0.5130 0.063 Uiso 1 1 calc R . . C12 C 0.0642(7) 0.4918(14) 0.4096(11) 0.054(5) Uani 1 1 d U . . H12 H 0.0472 0.4258 0.3951 0.065 Uiso 1 1 calc R . . C13 C -0.0697(7) 0.3879(15) 0.3554(11) 0.047(4) Uani 1 1 d U . . H13 H -0.0843 0.4568 0.3449 0.057 Uiso 1 1 calc R . . C14 C -0.1318(6) 0.3282(13) 0.2411(9) 0.045(4) Uani 1 1 d U . . H14A H -0.1428 0.4027 0.2355 0.067 Uiso 1 1 calc R . . H14B H -0.1591 0.2818 0.2384 0.067 Uiso 1 1 calc R . . H14C H -0.1218 0.3091 0.2036 0.067 Uiso 1 1 calc R . . C15 C -0.0724(8) 0.2031(16) 0.3264(14) 0.083(7) Uani 1 1 d U . . H15A H -0.0362 0.2010 0.3446 0.125 Uiso 1 1 calc R . . H15B H -0.0870 0.1596 0.2837 0.125 Uiso 1 1 calc R . . H15C H -0.0825 0.1749 0.3621 0.125 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0419(7) 0.0026(5) 0.0175(6) -0.0008(4) 0.0229(5) 0.0007(4) Cd2 0.0398(7) 0.0024(5) 0.0139(5) -0.0029(4) 0.0203(5) -0.0034(4) Cd3 0.0416(11) 0.0402(10) 0.0539(12) 0.0011(8) 0.0369(9) -0.0088(8) Cl1 0.038(2) 0.0102(16) 0.0230(18) 0.0011(13) 0.0188(16) 0.0016(14) Cl2 0.052(2) 0.0161(17) 0.0239(18) 0.0038(14) 0.0259(17) 0.0010(15) Cl3 0.041(2) 0.0171(17) 0.0293(19) 0.0021(14) 0.0272(17) 0.0009(15) O1 0.036(7) 0.072(8) 0.072(8) -0.018(6) 0.036(5) -0.019(5) O2 0.072(10) 0.082(9) 0.121(14) 0.032(9) 0.058(10) 0.014(7) N1 0.016(4) 0.005(3) 0.016(3) 0.002(3) 0.009(3) 0.000(3) N2 0.034(7) 0.012(5) 0.028(5) -0.005(4) 0.024(5) -0.001(4) N3 0.026(4) 0.010(3) 0.015(4) 0.000(3) 0.013(3) -0.003(3) N4 0.016(3) 0.012(3) 0.012(3) -0.0024(17) 0.0075(18) -0.0003(18) N5 0.029(4) 0.015(4) 0.012(4) -0.004(3) 0.012(3) -0.001(3) N6 0.036(7) 0.017(5) 0.011(6) -0.004(4) 0.011(6) -0.004(5) N7 0.026(4) 0.014(3) 0.014(4) -0.003(3) 0.015(3) 0.004(3) N8 0.038(7) 0.005(5) 0.016(6) -0.005(4) 0.019(5) 0.001(4) N9 0.043(7) 0.010(5) 0.034(7) -0.009(5) 0.027(6) -0.003(5) N10 0.046(7) 0.043(7) 0.057(9) -0.002(6) 0.040(7) -0.011(5) N11 0.042(8) 0.036(7) 0.068(8) 0.002(6) 0.024(6) 0.004(6) C1 0.051(9) 0.013(5) 0.027(7) -0.001(4) 0.026(7) 0.000(6) C2 0.020(5) 0.015(4) 0.009(4) 0.003(3) 0.008(3) 0.001(3) C3 0.021(4) 0.013(4) 0.012(4) -0.005(3) 0.010(3) 0.002(3) C4 0.011(3) 0.008(3) 0.007(3) -0.0017(18) 0.0037(19) 0.0009(18) C5 0.056(9) 0.005(5) 0.020(7) 0.000(5) 0.027(7) 0.008(6) C6 0.062(10) 0.015(6) 0.019(7) -0.002(5) 0.026(7) 0.010(6) C7 0.020(7) 0.020(6) 0.020(7) -0.006(5) 0.010(5) -0.002(5) C8 0.043(9) 0.027(7) 0.041(8) -0.001(6) 0.027(7) -0.004(6) C9 0.066(11) 0.029(8) 0.079(12) -0.009(7) 0.059(9) -0.006(7) C10 0.067(11) 0.048(9) 0.047(10) -0.015(7) 0.043(9) -0.032(8) C11 0.062(11) 0.061(10) 0.059(11) -0.019(8) 0.049(9) -0.028(8) C12 0.063(11) 0.035(9) 0.094(13) -0.016(8) 0.062(10) -0.015(8) C13 0.053(10) 0.044(8) 0.060(9) -0.003(7) 0.038(6) -0.008(8) C14 0.056(11) 0.025(9) 0.061(9) 0.001(7) 0.033(6) 0.008(7) C15 0.070(15) 0.043(9) 0.112(19) 0.003(10) 0.014(13) 0.012(10) _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 N8 2.336(10) 4 ? Cd1 N3 2.348(10) 4 ? Cd1 N1 2.424(10) . ? Cd1 Cl3 2.575(3) . ? Cd1 Cl1 2.649(3) . ? Cd1 Cl2 2.658(4) . ? Cd2 N5 2.315(10) 6_576 ? Cd2 N7 2.341(11) . ? Cd2 N2 2.428(11) . ? Cd2 Cl2 2.609(4) . ? Cd2 Cl1 2.636(3) 4_545 ? Cd2 Cl3 2.665(4) . ? Cd3 O1 2.271(13) . ? Cd3 O1 2.271(13) 5_566 ? Cd3 N10 2.286(12) 5_566 ? Cd3 N10 2.286(12) . ? Cd3 O2 2.363(15) 5_566 ? Cd3 O2 2.363(15) . ? Cl1 Cd2 2.636(3) 4 ? O1 C13 1.26(2) . ? N1 N2 1.328(14) . ? N1 C1 1.361(17) . ? N2 N3 1.332(14) . ? N3 N4 1.333(14) . ? N3 Cd1 2.348(10) 4_545 ? N4 C1 1.402(16) . ? N5 C4 1.331(15) . ? N5 C5 1.343(16) . ? N5 Cd2 2.315(10) 6_575 ? N6 C7 1.341(17) . ? N6 N7 1.366(14) . ? N7 N8 1.333(14) . ? N8 N9 1.330(15) . ? N8 Cd1 2.336(10) 4_545 ? N9 C7 1.323(17) . ? N10 C12 1.29(2) . ? N10 C11 1.36(2) . ? N11 C13 1.28(2) . ? N11 C14 1.47(2) . ? N11 C15 1.48(2) . ? C1 C2 1.408(18) . ? C2 C3 1.381(18) . ? C2 C6 1.382(18) . ? C3 C4 1.377(17) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.400(19) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.48(2) . ? C8 C10 1.35(2) . ? C8 C9 1.37(2) . ? C9 C12 1.38(2) . ? C9 H9 0.9500 . ? C10 C11 1.42(2) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 N8 Cd1 N3 94.0(4) 4 4 ? N8 Cd1 N1 88.2(3) 4 . ? N3 Cd1 N1 174.9(3) 4 . ? N8 Cd1 Cl3 174.7(3) 4 . ? N3 Cd1 Cl3 91.1(3) 4 . ? N1 Cd1 Cl3 86.6(2) . . ? N8 Cd1 Cl1 85.4(3) 4 . ? N3 Cd1 Cl1 85.3(3) 4 . ? N1 Cd1 Cl1 99.4(2) . . ? Cl3 Cd1 Cl1 96.55(11) . . ? N8 Cd1 Cl2 88.6(3) 4 . ? N3 Cd1 Cl2 90.1(3) 4 . ? N1 Cd1 Cl2 85.4(2) . . ? Cl3 Cd1 Cl2 89.95(11) . . ? Cl1 Cd1 Cl2 172.09(11) . . ? N5 Cd2 N7 94.2(4) 6_576 . ? N5 Cd2 N2 166.4(4) 6_576 . ? N7 Cd2 N2 91.5(4) . . ? N5 Cd2 Cl2 90.6(3) 6_576 . ? N7 Cd2 Cl2 174.6(2) . . ? N2 Cd2 Cl2 84.3(3) . . ? N5 Cd2 Cl1 109.1(3) 6_576 4_545 ? N7 Cd2 Cl1 83.5(3) . 4_545 ? N2 Cd2 Cl1 83.8(3) . 4_545 ? Cl2 Cd2 Cl1 92.61(11) . 4_545 ? N5 Cd2 Cl3 88.1(3) 6_576 . ? N7 Cd2 Cl3 93.5(3) . . ? N2 Cd2 Cl3 79.2(3) . . ? Cl2 Cd2 Cl3 89.06(11) . . ? Cl1 Cd2 Cl3 162.63(11) 4_545 . ? O1 Cd3 O1 179.997(2) . 5_566 ? O1 Cd3 N10 90.6(5) . 5_566 ? O1 Cd3 N10 89.4(5) 5_566 5_566 ? O1 Cd3 N10 89.4(5) . . ? O1 Cd3 N10 90.6(5) 5_566 . ? N10 Cd3 N10 179.999(2) 5_566 . ? O1 Cd3 O2 87.0(6) . 5_566 ? O1 Cd3 O2 93.0(6) 5_566 5_566 ? N10 Cd3 O2 87.9(5) 5_566 5_566 ? N10 Cd3 O2 92.1(5) . 5_566 ? O1 Cd3 O2 93.0(6) . . ? O1 Cd3 O2 87.0(6) 5_566 . ? N10 Cd3 O2 92.1(5) 5_566 . ? N10 Cd3 O2 87.9(5) . . ? O2 Cd3 O2 179.998(3) 5_566 . ? Cd2 Cl1 Cd1 93.97(11) 4 . ? Cd2 Cl2 Cd1 84.35(12) . . ? Cd1 Cl3 Cd2 84.88(11) . . ? C13 O1 Cd3 126.7(12) . . ? N2 N1 C1 106.4(10) . . ? N2 N1 Cd1 109.5(7) . . ? C1 N1 Cd1 143.7(8) . . ? N1 N2 N3 110.4(10) . . ? N1 N2 Cd2 124.4(8) . . ? N3 N2 Cd2 123.5(8) . . ? N2 N3 N4 109.5(9) . . ? N2 N3 Cd1 120.4(8) . 4_545 ? N4 N3 Cd1 129.3(7) . 4_545 ? N3 N4 C1 105.4(10) . . ? C4 N5 C5 117.6(11) . . ? C4 N5 Cd2 123.7(8) . 6_575 ? C5 N5 Cd2 117.5(8) . 6_575 ? C7 N6 N7 103.0(10) . . ? N8 N7 N6 108.7(10) . . ? N8 N7 Cd2 124.1(8) . . ? N6 N7 Cd2 126.1(7) . . ? N9 N8 N7 110.2(10) . . ? N9 N8 Cd1 126.1(8) . 4_545 ? N7 N8 Cd1 121.2(8) . 4_545 ? C7 N9 N8 104.2(10) . . ? C12 N10 C11 114.4(14) . . ? C12 N10 Cd3 124.9(11) . . ? C11 N10 Cd3 119.8(11) . . ? C13 N11 C14 125.7(16) . . ? C13 N11 C15 119.9(18) . . ? C14 N11 C15 114.3(15) . . ? N1 C1 N4 108.3(11) . . ? N1 C1 C2 128.3(12) . . ? N4 C1 C2 123.5(12) . . ? C3 C2 C6 115.5(12) . . ? C3 C2 C1 121.6(12) . . ? C6 C2 C1 122.9(12) . . ? C4 C3 C2 120.4(12) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? N5 C4 C3 123.8(11) . . ? N5 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? N5 C5 C6 120.7(12) . . ? N5 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C2 C6 C5 122.0(12) . . ? C2 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? N9 C7 N6 113.8(12) . . ? N9 C7 C8 125.6(13) . . ? N6 C7 C8 120.4(12) . . ? C10 C8 C9 117.3(15) . . ? C10 C8 C7 120.5(14) . . ? C9 C8 C7 121.9(14) . . ? C8 C9 C12 118.9(16) . . ? C8 C9 H9 120.5 . . ? C12 C9 H9 120.5 . . ? C8 C10 C11 119.6(16) . . ? C8 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N10 C11 C10 122.7(16) . . ? N10 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N10 C12 C9 126.7(17) . . ? N10 C12 H12 116.7 . . ? C9 C12 H12 116.7 . . ? O1 C13 N11 125.5(18) . . ? O1 C13 H13 117.3 . . ? N11 C13 H13 117.3 . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N11 C15 H15A 109.5 . . ? N11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Cd1 Cl1 Cd2 -45.7(3) 4 . . 4 ? N3 Cd1 Cl1 Cd2 48.7(3) 4 . . 4 ? N1 Cd1 Cl1 Cd2 -133.1(2) . . . 4 ? Cl3 Cd1 Cl1 Cd2 139.33(11) . . . 4 ? Cl2 Cd1 Cl1 Cd2 -5.7(8) . . . 4 ? N5 Cd2 Cl2 Cd1 -113.1(3) 6_576 . . . ? N7 Cd2 Cl2 Cd1 94(3) . . . . ? N2 Cd2 Cl2 Cd1 54.2(3) . . . . ? Cl1 Cd2 Cl2 Cd1 137.69(10) 4_545 . . . ? Cl3 Cd2 Cl2 Cd1 -25.01(10) . . . . ? N8 Cd1 Cl2 Cd2 -148.9(3) 4 . . . ? N3 Cd1 Cl2 Cd2 117.1(3) 4 . . . ? N1 Cd1 Cl2 Cd2 -60.6(2) . . . . ? Cl3 Cd1 Cl2 Cd2 25.95(10) . . . . ? Cl1 Cd1 Cl2 Cd2 171.2(7) . . . . ? N8 Cd1 Cl3 Cd2 49(3) 4 . . . ? N3 Cd1 Cl3 Cd2 -115.4(3) 4 . . . ? N1 Cd1 Cl3 Cd2 60.1(2) . . . . ? Cl1 Cd1 Cl3 Cd2 159.19(10) . . . . ? Cl2 Cd1 Cl3 Cd2 -25.34(10) . . . . ? N5 Cd2 Cl3 Cd1 116.5(3) 6_576 . . . ? N7 Cd2 Cl3 Cd1 -149.4(2) . . . . ? N2 Cd2 Cl3 Cd1 -58.5(3) . . . . ? Cl2 Cd2 Cl3 Cd1 25.86(11) . . . . ? Cl1 Cd2 Cl3 Cd1 -69.9(4) 4_545 . . . ? O1 Cd3 O1 C13 95(4) 5_566 . . . ? N10 Cd3 O1 C13 81.8(14) 5_566 . . . ? N10 Cd3 O1 C13 -98.2(14) . . . . ? O2 Cd3 O1 C13 169.6(14) 5_566 . . . ? O2 Cd3 O1 C13 -10.4(14) . . . . ? N8 Cd1 N1 N2 139.4(8) 4 . . . ? N3 Cd1 N1 N2 23(4) 4 . . . ? Cl3 Cd1 N1 N2 -39.5(7) . . . . ? Cl1 Cd1 N1 N2 -135.6(7) . . . . ? Cl2 Cd1 N1 N2 50.7(7) . . . . ? N8 Cd1 N1 C1 -31.3(16) 4 . . . ? N3 Cd1 N1 C1 -147(4) 4 . . . ? Cl3 Cd1 N1 C1 149.7(15) . . . . ? Cl1 Cd1 N1 C1 53.6(16) . . . . ? Cl2 Cd1 N1 C1 -120.1(15) . . . . ? C1 N1 N2 N3 -0.9(14) . . . . ? Cd1 N1 N2 N3 -175.2(8) . . . . ? C1 N1 N2 Cd2 164.5(9) . . . . ? Cd1 N1 N2 Cd2 -9.8(11) . . . . ? N5 Cd2 N2 N1 31(2) 6_576 . . . ? N7 Cd2 N2 N1 146.2(10) . . . . ? Cl2 Cd2 N2 N1 -37.3(9) . . . . ? Cl1 Cd2 N2 N1 -130.5(9) 4_545 . . . ? Cl3 Cd2 N2 N1 52.9(9) . . . . ? N5 Cd2 N2 N3 -165.2(13) 6_576 . . . ? N7 Cd2 N2 N3 -50.2(10) . . . . ? Cl2 Cd2 N2 N3 126.3(10) . . . . ? Cl1 Cd2 N2 N3 33.1(9) 4_545 . . . ? Cl3 Cd2 N2 N3 -143.5(10) . . . . ? N1 N2 N3 N4 -0.3(14) . . . . ? Cd2 N2 N3 N4 -165.9(8) . . . . ? N1 N2 N3 Cd1 170.3(7) . . . 4_545 ? Cd2 N2 N3 Cd1 4.7(13) . . . 4_545 ? N2 N3 N4 C1 1.3(13) . . . . ? Cd1 N3 N4 C1 -168.1(9) 4_545 . . . ? C7 N6 N7 N8 -0.1(13) . . . . ? C7 N6 N7 Cd2 -168.8(8) . . . . ? N5 Cd2 N7 N8 -149.3(9) 6_576 . . . ? N2 Cd2 N7 N8 43.1(9) . . . . ? Cl2 Cd2 N7 N8 4(4) . . . . ? Cl1 Cd2 N7 N8 -40.5(9) 4_545 . . . ? Cl3 Cd2 N7 N8 122.3(9) . . . . ? N5 Cd2 N7 N6 17.8(10) 6_576 . . . ? N2 Cd2 N7 N6 -149.9(10) . . . . ? Cl2 Cd2 N7 N6 171(2) . . . . ? Cl1 Cd2 N7 N6 126.5(10) 4_545 . . . ? Cl3 Cd2 N7 N6 -70.6(10) . . . . ? N6 N7 N8 N9 0.7(14) . . . . ? Cd2 N7 N8 N9 169.7(8) . . . . ? N6 N7 N8 Cd1 -162.5(8) . . . 4_545 ? Cd2 N7 N8 Cd1 6.5(12) . . . 4_545 ? N7 N8 N9 C7 -1.0(15) . . . . ? Cd1 N8 N9 C7 161.2(9) 4_545 . . . ? O1 Cd3 N10 C12 -7.8(16) . . . . ? O1 Cd3 N10 C12 172.2(16) 5_566 . . . ? N10 Cd3 N10 C12 55(22) 5_566 . . . ? O2 Cd3 N10 C12 79.1(17) 5_566 . . . ? O2 Cd3 N10 C12 -100.9(17) . . . . ? O1 Cd3 N10 C11 161.3(15) . . . . ? O1 Cd3 N10 C11 -18.7(15) 5_566 . . . ? N10 Cd3 N10 C11 -136(22) 5_566 . . . ? O2 Cd3 N10 C11 -111.8(15) 5_566 . . . ? O2 Cd3 N10 C11 68.2(15) . . . . ? N2 N1 C1 N4 1.7(15) . . . . ? Cd1 N1 C1 N4 172.6(9) . . . . ? N2 N1 C1 C2 -178.3(14) . . . . ? Cd1 N1 C1 C2 -7(3) . . . . ? N3 N4 C1 N1 -1.9(15) . . . . ? N3 N4 C1 C2 178.1(13) . . . . ? N1 C1 C2 C3 -23(2) . . . . ? N4 C1 C2 C3 157.3(13) . . . . ? N1 C1 C2 C6 157.3(15) . . . . ? N4 C1 C2 C6 -23(2) . . . . ? C6 C2 C3 C4 -0.7(19) . . . . ? C1 C2 C3 C4 179.3(13) . . . . ? C5 N5 C4 C3 -0.3(19) . . . . ? Cd2 N5 C4 C3 167.0(9) 6_575 . . . ? C2 C3 C4 N5 1.5(19) . . . . ? C4 N5 C5 C6 -2(2) . . . . ? Cd2 N5 C5 C6 -169.8(11) 6_575 . . . ? C3 C2 C6 C5 -1(2) . . . . ? C1 C2 C6 C5 178.7(14) . . . . ? N5 C5 C6 C2 3(2) . . . . ? N8 N9 C7 N6 1.0(16) . . . . ? N8 N9 C7 C8 -174.7(13) . . . . ? N7 N6 C7 N9 -0.6(15) . . . . ? N7 N6 C7 C8 175.4(12) . . . . ? N9 C7 C8 C10 167.1(16) . . . . ? N6 C7 C8 C10 -8(2) . . . . ? N9 C7 C8 C9 -7(3) . . . . ? N6 C7 C8 C9 177.2(16) . . . . ? C10 C8 C9 C12 6(3) . . . . ? C7 C8 C9 C12 -179.2(17) . . . . ? C9 C8 C10 C11 -4(3) . . . . ? C7 C8 C10 C11 -179.2(17) . . . . ? C12 N10 C11 C10 1(3) . . . . ? Cd3 N10 C11 C10 -169.1(15) . . . . ? C8 C10 C11 N10 1(3) . . . . ? C11 N10 C12 C9 1(3) . . . . ? Cd3 N10 C12 C9 170.4(16) . . . . ? C8 C9 C12 N10 -5(3) . . . . ? Cd3 O1 C13 N11 -173.9(13) . . . . ? C14 N11 C13 O1 -177.1(16) . . . . ? C15 N11 C13 O1 7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.493 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.265