# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Hans-Conrad zur Loye' _publ_contact_author_address ; Chemistry and Biochemistry University of South Carolina 631 Sumter Street Columbia South Carolina 29208 UNITED STATES OF AMERICA ; _publ_contact_author_email ZURLOYE@SC.EDU _publ_section_title ; Assembly of Large Simple 1D and Rare Polycatenated 3D Molecular Ladders from T-shaped Building Blocks Containing a New, Long N,N'-Bidentate Ligand ; loop_ _publ_author_name 'Hans-Conrad zur Loye' 'Andrea Goforth' 'Mark D. Smith' 'Cheng-Yong Su' data_cy0117s _database_code_depnum_ccdc_archive 'CCDC 235891' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71.40 H61.20 Cl8.40 Co2 N16 O13.20' _chemical_formula_weight 1770.20 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1474(6) _cell_length_b 13.4825(7) _cell_length_c 15.8374(9) _cell_angle_alpha 85.4010(10) _cell_angle_beta 88.9770(10) _cell_angle_gamma 68.0390(10) _cell_volume 2002.89(19) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 6887 _cell_measurement_theta_min 2.473 _cell_measurement_theta_max 24.997 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7765 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(SADABS, Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 16065 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7058 _reflns_number_gt 5636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0774P)^2^+2.0975P] 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 7058 _refine_ls_number_parameters 559 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1446 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.061 _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 Co Co 0.10617(5) 0.50394(4) 0.25842(3) 0.02831(16) Uani 1 1 d . . . C1 C 0.2019(4) 0.3171(3) 0.3922(2) 0.0392(9) Uani 1 1 d . . . H1 H 0.2021 0.2793 0.3441 0.047 Uiso 1 1 calc R . . C2 C 0.2501(4) 0.2589(3) 0.4686(2) 0.0446(10) Uani 1 1 d . . . H2 H 0.2822 0.1828 0.4726 0.053 Uiso 1 1 calc R . . C3 C 0.2512(4) 0.3127(3) 0.5396(2) 0.0374(9) Uani 1 1 d . . . C4 C 0.2013(4) 0.4236(3) 0.5300(2) 0.0390(9) Uani 1 1 d . . . H4 H 0.1984 0.4634 0.5773 0.047 Uiso 1 1 calc R . . C5 C 0.1556(4) 0.4758(3) 0.4513(2) 0.0366(9) Uani 1 1 d . . . H5 H 0.1233 0.5519 0.4457 0.044 Uiso 1 1 calc R . . C6 C 0.3058(4) 0.2547(3) 0.6220(2) 0.0398(9) Uani 1 1 d . . . H6 H 0.2949 0.2943 0.6704 0.048 Uiso 1 1 calc R . . C7 C 0.4152(4) 0.1028(3) 0.7122(2) 0.0410(9) Uani 1 1 d . . . C8 C 0.3250(4) 0.1186(3) 0.7797(2) 0.0434(10) Uani 1 1 d . . . H8 H 0.2286 0.1661 0.7729 0.052 Uiso 1 1 calc R . . C9 C 0.3759(4) 0.0640(3) 0.8590(2) 0.0389(9) Uani 1 1 d . . . H9 H 0.3136 0.0755 0.9059 0.047 Uiso 1 1 calc R . . C10 C 0.5131(4) -0.0051(3) 0.8695(2) 0.0346(8) Uani 1 1 d . . . H10 H 0.5456 -0.0406 0.9237 0.042 Uiso 1 1 calc R . . C11 C 0.6079(4) -0.0249(3) 0.8011(2) 0.0320(8) Uani 1 1 d . . . C12 C 0.5596(4) 0.0299(3) 0.7205(2) 0.0348(8) Uani 1 1 d . . . C13 C 0.6532(4) 0.0125(3) 0.6515(2) 0.0409(9) Uani 1 1 d . . . H13 H 0.6209 0.0503 0.5980 0.049 Uiso 1 1 calc R . . C14 C 0.7904(4) -0.0587(3) 0.6616(2) 0.0393(9) Uani 1 1 d . . . H14 H 0.8533 -0.0690 0.6151 0.047 Uiso 1 1 calc R . . C15 C 0.8393(4) -0.1169(3) 0.7399(2) 0.0358(8) Uani 1 1 d . . . H15 H 0.9340 -0.1678 0.7454 0.043 Uiso 1 1 calc R . . C16 C 0.7511(4) -0.1006(3) 0.8086(2) 0.0302(8) Uani 1 1 d . . . C17 C 0.9209(4) -0.2076(3) 0.9083(2) 0.0323(8) Uani 1 1 d . . . H17 H 0.9915 -0.1973 0.8724 0.039 Uiso 1 1 calc R . . C18 C 1.1441(4) -0.3941(3) 1.0836(2) 0.0348(8) Uani 1 1 d . . . H18 H 1.2422 -0.4288 1.0978 0.042 Uiso 1 1 calc R . . C19 C 1.1065(4) -0.3291(3) 1.0090(2) 0.0350(8) Uani 1 1 d . . . H19 H 1.1776 -0.3198 0.9730 0.042 Uiso 1 1 calc R . . C20 C 0.9635(4) -0.2776(3) 0.9869(2) 0.0290(7) Uani 1 1 d . . . C21 C 0.8649(4) -0.2962(3) 1.0411(2) 0.0348(8) Uani 1 1 d . . . H21 H 0.7663 -0.2640 1.0278 0.042 Uiso 1 1 calc R . . C22 C 0.9115(4) -0.3618(3) 1.1144(2) 0.0376(9) Uani 1 1 d . . . H22 H 0.8424 -0.3731 1.1510 0.045 Uiso 1 1 calc R . . N1 N 0.1546(3) 0.4248(2) 0.38252(17) 0.0310(7) Uani 1 1 d . . . N2 N 0.3667(3) 0.1540(3) 0.63028(19) 0.0454(9) Uani 1 1 d . . . N3 N 0.7903(3) -0.1605(2) 0.88782(17) 0.0317(7) Uani 1 1 d . . . N4 N 1.0484(3) -0.4106(2) 1.13702(17) 0.0307(6) Uani 1 1 d . . . C23 C 0.3363(4) 0.3436(3) 0.1562(2) 0.0326(8) Uani 1 1 d . . . H23 H 0.2580 0.3535 0.1199 0.039 Uiso 1 1 calc R . . C24 C 0.4670(4) 0.2695(3) 0.1375(2) 0.0336(8) Uani 1 1 d . . . H24 H 0.4785 0.2298 0.0891 0.040 Uiso 1 1 calc R . . C25 C 0.5821(4) 0.2534(3) 0.1905(2) 0.0332(8) Uani 1 1 d . . . C26 C 0.5605(4) 0.3135(3) 0.2596(2) 0.0352(8) Uani 1 1 d . . . H26 H 0.6370 0.3046 0.2969 0.042 Uiso 1 1 calc R . . C27 C 0.4262(4) 0.3867(3) 0.2736(2) 0.0341(8) Uani 1 1 d . . . H27 H 0.4123 0.4278 0.3213 0.041 Uiso 1 1 calc R . . C28 C 0.7255(4) 0.1747(3) 0.1735(3) 0.0380(9) Uani 1 1 d . . . H28 H 0.8011 0.1625 0.2124 0.046 Uiso 1 1 calc R . . C29 C 0.8857(4) 0.0469(3) 0.0945(2) 0.0355(8) Uani 1 1 d . . . C30 C 0.9726(4) -0.0182(3) 0.1587(2) 0.0386(9) Uani 1 1 d . . . H30 H 0.9400 -0.0139 0.2154 0.046 Uiso 1 1 calc R . . C31 C 1.1087(4) -0.0908(3) 0.1412(2) 0.0396(9) Uani 1 1 d . . . H31 H 1.1680 -0.1348 0.1862 0.047 Uiso 1 1 calc R . . C32 C 1.1571(4) -0.0990(3) 0.0601(2) 0.0369(9) Uani 1 1 d . . . H32 H 1.2508 -0.1470 0.0495 0.044 Uiso 1 1 calc R . . C33 C 1.0695(4) -0.0368(3) -0.0081(2) 0.0310(8) Uani 1 1 d . . . N5 N 0.3140(3) 0.4026(2) 0.22303(17) 0.0301(6) Uani 1 1 d . . . N6 N 0.7487(3) 0.1234(2) 0.1078(2) 0.0362(7) Uani 1 1 d . . . N11 N 0.0919(4) 0.6895(3) 0.30583(19) 0.0417(8) Uani 1 1 d . . . O11 O 0.2102(3) 0.6196(2) 0.28633(17) 0.0440(7) Uani 1 1 d . . . O12 O -0.0123(3) 0.6599(2) 0.30648(16) 0.0432(7) Uani 1 1 d . . . O13 O 0.0802(4) 0.7786(2) 0.3226(2) 0.0673(10) Uani 1 1 d . . . N12 N -0.0877(3) 0.4147(3) 0.23940(19) 0.0385(7) Uani 1 1 d . . . O14 O -0.1259(3) 0.5003(2) 0.27609(17) 0.0472(7) Uani 1 1 d . . . O15 O 0.0401(2) 0.3802(2) 0.21477(16) 0.0379(6) Uani 1 1 d . . . O16 O -0.1653(3) 0.3672(3) 0.2272(2) 0.0607(9) Uani 1 1 d . . . C1SA C 0.4795(6) 0.4085(4) 0.8170(4) 0.0610(14) Uani 0.894(2) 1 d PD A 1 H1S1 H 0.5690 0.4091 0.7915 0.073 Uiso 0.894(2) 1 calc PR A 1 H1S2 H 0.4006 0.4517 0.7776 0.073 Uiso 0.894(2) 1 calc PR A 1 Cl1A Cl 0.48680(19) 0.27781(13) 0.82791(14) 0.0947(7) Uani 0.894(2) 1 d PD A 1 Cl2A Cl 0.45495(19) 0.46733(16) 0.91163(11) 0.0872(6) Uani 0.894(2) 1 d PD A 1 C1SB C 0.562(4) 0.331(5) 0.8328(16) 0.100 Uiso 0.106(2) 1 d PD A 2 H1S3 H 0.6481 0.3477 0.8226 0.120 Uiso 0.106(2) 1 calc PR A 2 H1S4 H 0.5871 0.2529 0.8290 0.120 Uiso 0.106(2) 1 calc PR A 2 Cl1B Cl 0.4907(19) 0.3691(15) 0.9318(10) 0.100 Uiso 0.106(2) 1 d PD A 2 Cl2B Cl 0.429(2) 0.4042(14) 0.7612(11) 0.100 Uiso 0.106(2) 1 d PD A 2 C2S C 0.2685(9) -0.2466(7) 0.4901(6) 0.100(3) Uani 0.70 1 d PD B 3 H2S1 H 0.2331 -0.2232 0.4312 0.119 Uiso 0.70 1 calc PR B 3 H2S2 H 0.2944 -0.1894 0.5118 0.119 Uiso 0.70 1 calc PR B 3 Cl3 Cl 0.4192(3) -0.3635(4) 0.4900(2) 0.1497(14) Uani 0.70 1 d PD B 3 Cl4 Cl 0.1316(3) -0.2631(3) 0.5525(3) 0.0938(13) Uani 0.70 1 d PD B 3 C3S C 0.343(6) -0.298(3) 0.444(3) 0.09(2) Uiso 0.10 1 d PD C 4 H3S1 H 0.2798 -0.2725 0.3935 0.114 Uiso 0.10 1 calc PR C 4 H3S2 H 0.3824 -0.2427 0.4535 0.114 Uiso 0.10 1 calc PR C 4 Cl5 Cl 0.481(3) -0.416(2) 0.4244(17) 0.149(9) Uiso 0.10 1 d PD C 4 Cl6 Cl 0.245(3) -0.313(2) 0.5313(15) 0.118(8) Uiso 0.10 1 d PD C 4 C4S C 0.182(4) -0.1670(19) 0.5017(12) 0.074(10) Uiso 0.15 1 d PD D 5 H4S1 H 0.0960 -0.1318 0.4653 0.089 Uiso 0.15 1 calc PR D 5 H4S2 H 0.2651 -0.1864 0.4640 0.089 Uiso 0.15 1 calc PR D 5 Cl7 Cl 0.1739(18) -0.2841(11) 0.5502(11) 0.060(4) Uiso 0.15 1 d PD D 5 Cl8 Cl 0.1936(13) -0.0743(9) 0.5676(7) 0.091(3) Uiso 0.15 1 d PD D 5 C5S C 0.2271(16) 0.0200(16) 0.604(3) 0.060(10) Uiso 0.15 1 d PD E 6 H5S1 H 0.2197 0.0471 0.6608 0.072 Uiso 0.15 1 calc PR E 6 H5S2 H 0.2194 0.0799 0.5613 0.072 Uiso 0.15 1 calc PR E 6 Cl9 Cl 0.3909(11) -0.0824(8) 0.5952(7) 0.076(3) Uiso 0.15 1 d PD E 6 Cl10 Cl 0.0887(13) -0.0219(10) 0.5889(8) 0.094(3) Uiso 0.15 1 d PD E 6 O1S O 0.2970(11) -0.0262(7) 0.5580(5) 0.100(3) Uani 0.50 1 d PD F 7 H1S H 0.3491 -0.0724 0.5923 0.149 Uiso 0.50 1 d PR F 7 C6S C 0.1527(12) 0.0180(10) 0.5914(7) 0.083(4) Uani 0.50 1 d PD F 7 H6S1 H 0.1476 -0.0226 0.6447 0.125 Uiso 0.50 1 calc PR F 7 H6S2 H 0.0852 0.0127 0.5502 0.125 Uiso 0.50 1 calc PR F 7 H6S3 H 0.1289 0.0935 0.6015 0.125 Uiso 0.50 1 calc PR F 7 O2S O 0.3962(12) -0.0288(10) 0.5547(7) 0.14(3) Uiso 0.10 1 d PRD F 8 H2S H 0.4153 -0.0652 0.5138 0.217 Uiso 0.10 1 d PR F 8 C7S C 0.3253(12) -0.0787(10) 0.6225(7) 0.048(10) Uiso 0.10 1 d PRD F 8 H7S1 H 0.3663 -0.0794 0.6782 0.072 Uiso 0.10 1 calc PR F 8 H7S2 H 0.3412 -0.1524 0.6102 0.072 Uiso 0.10 1 calc PR F 8 H7S3 H 0.2230 -0.0364 0.6225 0.072 Uiso 0.10 1 calc PR F 8 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 Co 0.0228(3) 0.0298(3) 0.0213(2) 0.00608(18) -0.00090(17) 0.00120(19) C1 0.043(2) 0.037(2) 0.0288(19) 0.0076(16) -0.0063(16) -0.0069(17) C2 0.048(2) 0.038(2) 0.033(2) 0.0104(17) -0.0042(18) -0.0023(18) C3 0.0254(18) 0.043(2) 0.0291(19) 0.0094(16) -0.0008(15) 0.0018(16) C4 0.0306(19) 0.048(2) 0.0251(18) 0.0027(16) -0.0013(15) 0.0001(17) C5 0.0283(19) 0.038(2) 0.0303(19) 0.0059(16) 0.0014(15) 0.0011(16) C6 0.031(2) 0.045(2) 0.0285(19) 0.0062(17) 0.0006(15) 0.0014(17) C7 0.043(2) 0.038(2) 0.0262(19) 0.0087(16) -0.0070(16) 0.0016(17) C8 0.037(2) 0.039(2) 0.037(2) 0.0079(17) -0.0028(17) 0.0051(17) C9 0.036(2) 0.040(2) 0.0302(19) 0.0052(16) 0.0020(16) -0.0029(17) C10 0.040(2) 0.0329(19) 0.0234(17) 0.0083(15) -0.0035(15) -0.0069(16) C11 0.036(2) 0.0283(18) 0.0247(18) 0.0054(14) -0.0059(15) -0.0056(15) C12 0.035(2) 0.0316(19) 0.0269(18) 0.0063(15) -0.0053(15) -0.0017(16) C13 0.043(2) 0.039(2) 0.0260(19) 0.0111(16) -0.0024(16) -0.0005(18) C14 0.039(2) 0.041(2) 0.0268(19) 0.0081(16) 0.0011(16) -0.0043(17) C15 0.034(2) 0.033(2) 0.0308(19) 0.0057(15) -0.0034(15) -0.0033(16) C16 0.0357(19) 0.0252(17) 0.0248(17) 0.0078(14) -0.0058(15) -0.0074(15) C17 0.035(2) 0.0334(19) 0.0266(18) 0.0041(15) -0.0029(15) -0.0114(16) C18 0.0262(18) 0.039(2) 0.0307(19) 0.0093(16) -0.0056(15) -0.0045(16) C19 0.0315(19) 0.038(2) 0.0293(18) 0.0096(15) 0.0007(15) -0.0085(16) C20 0.0295(18) 0.0246(17) 0.0267(17) 0.0017(14) -0.0038(14) -0.0036(14) C21 0.0250(18) 0.039(2) 0.0294(19) 0.0069(16) -0.0043(14) -0.0011(15) C22 0.031(2) 0.045(2) 0.0281(19) 0.0089(16) 0.0019(15) -0.0058(17) N1 0.0243(15) 0.0336(16) 0.0244(15) 0.0046(12) -0.0008(12) 0.0000(12) N2 0.0390(18) 0.047(2) 0.0282(17) 0.0104(14) -0.0053(14) 0.0068(16) N3 0.0340(17) 0.0266(15) 0.0237(15) 0.0053(12) -0.0042(12) -0.0004(13) N4 0.0258(15) 0.0334(16) 0.0250(15) 0.0046(12) -0.0017(12) -0.0033(12) C23 0.0256(18) 0.036(2) 0.0305(19) 0.0028(15) -0.0020(14) -0.0066(15) C24 0.0332(19) 0.0321(19) 0.0304(19) -0.0033(15) 0.0043(15) -0.0065(16) C25 0.0252(18) 0.0323(19) 0.037(2) 0.0024(16) 0.0045(15) -0.0063(15) C26 0.0250(18) 0.042(2) 0.0334(19) 0.0008(16) -0.0012(15) -0.0071(16) C27 0.0271(18) 0.042(2) 0.0266(18) -0.0033(15) 0.0025(14) -0.0053(16) C28 0.0240(18) 0.037(2) 0.047(2) -0.0004(18) 0.0034(16) -0.0054(16) C29 0.0273(18) 0.0301(19) 0.045(2) -0.0030(16) 0.0053(16) -0.0063(15) C30 0.036(2) 0.035(2) 0.039(2) 0.0015(17) 0.0045(17) -0.0075(17) C31 0.035(2) 0.033(2) 0.039(2) 0.0022(16) -0.0010(17) -0.0012(16) C32 0.0228(18) 0.0301(19) 0.049(2) -0.0033(17) 0.0026(16) 0.0001(15) C33 0.0248(17) 0.0243(17) 0.042(2) -0.0018(15) 0.0042(15) -0.0072(14) N5 0.0247(15) 0.0330(16) 0.0241(14) 0.0060(12) -0.0009(12) -0.0024(12) N6 0.0267(16) 0.0330(16) 0.0416(18) -0.0007(14) 0.0081(13) -0.0035(13) N11 0.055(2) 0.0305(18) 0.0301(17) 0.0070(13) -0.0030(15) -0.0076(16) O11 0.0394(15) 0.0406(15) 0.0456(16) 0.0017(12) -0.0033(12) -0.0084(13) O12 0.0385(15) 0.0409(15) 0.0363(15) 0.0049(12) 0.0028(12) -0.0007(13) O13 0.105(3) 0.0352(17) 0.056(2) -0.0027(14) 0.0062(18) -0.0204(17) N12 0.0342(18) 0.0406(19) 0.0345(17) 0.0063(15) -0.0031(14) -0.0086(15) O14 0.0543(18) 0.0423(16) 0.0332(14) -0.0009(12) 0.0037(13) -0.0052(13) O15 0.0246(13) 0.0429(15) 0.0387(14) 0.0049(12) -0.0009(11) -0.0059(11) O16 0.0410(17) 0.065(2) 0.082(2) -0.0096(18) 0.0052(16) -0.0262(16) C1SA 0.044(3) 0.068(4) 0.066(4) -0.004(3) -0.011(3) -0.014(3) Cl1A 0.0749(11) 0.0566(9) 0.1498(18) -0.0023(10) -0.0231(11) -0.0214(8) Cl2A 0.0749(11) 0.0980(14) 0.0829(11) -0.0247(10) 0.0100(9) -0.0225(9) C2S 0.118(9) 0.105(8) 0.081(6) 0.005(6) -0.006(6) -0.050(7) Cl3 0.0674(17) 0.205(4) 0.162(3) -0.037(3) -0.0061(18) -0.029(2) Cl4 0.068(2) 0.086(2) 0.113(2) 0.0000(16) 0.0155(18) -0.0138(16) O1S 0.146(10) 0.096(7) 0.062(5) -0.026(5) -0.007(6) -0.047(7) C6S 0.079(9) 0.116(10) 0.069(8) -0.028(7) 0.034(7) -0.051(8) _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 Co N4 2.133(3) 1_464 ? Co N1 2.133(3) . ? Co N5 2.134(3) . ? Co O15 2.179(3) . ? Co O12 2.186(3) . ? Co O11 2.258(3) . ? Co O14 2.384(3) . ? C1 N1 1.344(5) . ? C1 C2 1.379(5) . ? C2 C3 1.387(6) . ? C3 C4 1.384(5) . ? C3 C6 1.470(5) . ? C4 C5 1.378(5) . ? C5 N1 1.337(5) . ? C6 N2 1.261(5) . ? C7 C8 1.372(5) . ? C7 N2 1.424(4) . ? C7 C12 1.429(5) . ? C8 C9 1.406(5) . ? C9 C10 1.359(5) . ? C10 C11 1.409(5) . ? C11 C12 1.420(5) . ? C11 C16 1.430(5) . ? C12 C13 1.410(5) . ? C13 C14 1.367(5) . ? C14 C15 1.406(5) . ? C15 C16 1.375(5) . ? C16 N3 1.413(4) . ? C17 N3 1.272(4) . ? C17 C20 1.467(5) . ? C18 N4 1.346(4) . ? C18 C19 1.382(5) . ? C19 C20 1.390(5) . ? C20 C21 1.386(5) . ? C21 C22 1.377(5) . ? C22 N4 1.336(4) . ? N4 Co 2.133(3) 1_646 ? C23 N5 1.341(5) . ? C23 C24 1.374(5) . ? C24 C25 1.390(5) . ? C25 C26 1.379(5) . ? C25 C28 1.480(5) . ? C26 C27 1.378(5) . ? C27 N5 1.344(4) . ? C28 N6 1.265(5) . ? C29 C30 1.375(5) . ? C29 N6 1.411(4) . ? C29 C33 1.435(5) 2_755 ? C30 C31 1.401(5) . ? C31 C32 1.365(5) . ? C32 C33 1.411(5) . ? C33 C33 1.423(6) 2_755 ? C33 C29 1.435(5) 2_755 ? N11 O13 1.214(4) . ? N11 O12 1.262(4) . ? N11 O11 1.270(4) . ? N12 O16 1.212(4) . ? N12 O14 1.259(4) . ? N12 O15 1.269(4) . ? C1SA Cl2A 1.722(6) . ? C1SA Cl1A 1.730(6) . ? C1SB Cl2B 1.72(2) . ? C1SB Cl1B 1.75(2) . ? C2S Cl3 1.738(9) . ? C2S Cl4 1.761(9) . ? C3S Cl5 1.732(12) . ? C3S Cl6 1.734(12) . ? C4S Cl7 1.728(12) . ? C4S Cl8 1.729(12) . ? C5S Cl10 1.725(12) . ? C5S Cl9 1.731(12) . ? O1S C6S 1.466(9) . ? O2S C7S 1.5303 . ? 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 N4 Co N1 176.99(11) 1_464 . ? N4 Co N5 95.46(10) 1_464 . ? N1 Co N5 87.46(10) . . ? N4 Co O15 88.75(10) 1_464 . ? N1 Co O15 92.22(11) . . ? N5 Co O15 84.93(10) . . ? N4 Co O12 84.28(10) 1_464 . ? N1 Co O12 92.98(10) . . ? N5 Co O12 142.46(12) . . ? O15 Co O12 132.49(10) . . ? N4 Co O11 87.62(11) 1_464 . ? N1 Co O11 91.94(11) . . ? N5 Co O11 84.92(11) . . ? O15 Co O11 168.85(10) . . ? O12 Co O11 57.55(10) . . ? N4 Co O14 91.19(10) 1_464 . ? N1 Co O14 87.02(10) . . ? N5 Co O14 139.80(11) . . ? O15 Co O14 55.56(9) . . ? O12 Co O14 77.61(10) . . ? O11 Co O14 135.04(10) . . ? N1 C1 C2 123.2(4) . . ? C1 C2 C3 119.3(4) . . ? C4 C3 C2 117.7(3) . . ? C4 C3 C6 120.6(4) . . ? C2 C3 C6 121.7(3) . . ? C5 C4 C3 119.5(4) . . ? N1 C5 C4 123.3(4) . . ? N2 C6 C3 121.9(4) . . ? C8 C7 N2 121.4(3) . . ? C8 C7 C12 121.2(3) . . ? N2 C7 C12 117.4(3) . . ? C7 C8 C9 119.6(3) . . ? C10 C9 C8 120.8(3) . . ? C9 C10 C11 121.1(3) . . ? C10 C11 C12 119.3(3) . . ? C10 C11 C16 122.7(3) . . ? C12 C11 C16 118.0(3) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 C7 121.8(3) . . ? C11 C12 C7 118.0(3) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 120.7(3) . . ? C16 C15 C14 120.5(3) . . ? C15 C16 N3 123.6(3) . . ? C15 C16 C11 120.4(3) . . ? N3 C16 C11 115.9(3) . . ? N3 C17 C20 120.6(3) . . ? N4 C18 C19 123.1(3) . . ? C18 C19 C20 119.4(3) . . ? C21 C20 C19 117.6(3) . . ? C21 C20 C17 122.0(3) . . ? C19 C20 C17 120.4(3) . . ? C22 C21 C20 119.3(3) . . ? N4 C22 C21 123.8(3) . . ? C5 N1 C1 117.1(3) . . ? C5 N1 Co 123.2(2) . . ? C1 N1 Co 119.3(2) . . ? C6 N2 C7 118.9(3) . . ? C17 N3 C16 120.0(3) . . ? C22 N4 C18 116.8(3) . . ? C22 N4 Co 120.2(2) . 1_646 ? C18 N4 Co 122.6(2) . 1_646 ? N5 C23 C24 123.1(3) . . ? C23 C24 C25 119.0(3) . . ? C26 C25 C24 118.4(3) . . ? C26 C25 C28 120.2(3) . . ? C24 C25 C28 121.4(3) . . ? C27 C26 C25 119.0(3) . . ? N5 C27 C26 123.1(3) . . ? N6 C28 C25 120.9(3) . . ? C30 C29 N6 123.6(3) . . ? C30 C29 C33 120.2(3) . 2_755 ? N6 C29 C33 116.2(3) . 2_755 ? C29 C30 C31 120.6(4) . . ? C32 C31 C30 120.6(3) . . ? C31 C32 C33 120.7(3) . . ? C32 C33 C33 119.5(4) . 2_755 ? C32 C33 C29 122.3(3) . 2_755 ? C33 C33 C29 118.2(4) 2_755 2_755 ? C23 N5 C27 117.4(3) . . ? C23 N5 Co 122.2(2) . . ? C27 N5 Co 120.0(2) . . ? C28 N6 C29 119.6(3) . . ? O13 N11 O12 122.4(4) . . ? O13 N11 O11 122.1(4) . . ? O12 N11 O11 115.5(3) . . ? N11 O11 Co 91.6(2) . . ? N11 O12 Co 95.2(2) . . ? O16 N12 O14 123.8(3) . . ? O16 N12 O15 121.0(3) . . ? O14 N12 O15 115.2(3) . . ? N12 O14 Co 89.9(2) . . ? N12 O15 Co 99.4(2) . . ? Cl2A C1SA Cl1A 113.1(3) . . ? Cl2B C1SB Cl1B 104.8(17) . . ? Cl3 C2S Cl4 112.7(5) . . ? Cl5 C3S Cl6 112.6(14) . . ? Cl7 C4S Cl8 116.7(12) . . ? Cl10 C5S Cl9 112.0(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 C3 -0.3(6) . . . . ? C1 C2 C3 C4 0.9(6) . . . . ? C1 C2 C3 C6 -178.0(4) . . . . ? C2 C3 C4 C5 -1.3(6) . . . . ? C6 C3 C4 C5 177.6(3) . . . . ? C3 C4 C5 N1 1.1(6) . . . . ? C4 C3 C6 N2 -171.7(4) . . . . ? C2 C3 C6 N2 7.1(6) . . . . ? N2 C7 C8 C9 178.0(4) . . . . ? C12 C7 C8 C9 1.4(6) . . . . ? C7 C8 C9 C10 -0.7(6) . . . . ? C8 C9 C10 C11 -0.6(6) . . . . ? C9 C10 C11 C12 1.2(6) . . . . ? C9 C10 C11 C16 -177.1(4) . . . . ? C10 C11 C12 C13 179.1(4) . . . . ? C16 C11 C12 C13 -2.6(6) . . . . ? C10 C11 C12 C7 -0.4(6) . . . . ? C16 C11 C12 C7 177.9(3) . . . . ? C8 C7 C12 C13 179.7(4) . . . . ? N2 C7 C12 C13 3.0(6) . . . . ? C8 C7 C12 C11 -0.9(6) . . . . ? N2 C7 C12 C11 -177.6(4) . . . . ? C11 C12 C13 C14 1.2(6) . . . . ? C7 C12 C13 C14 -179.4(4) . . . . ? C12 C13 C14 C15 1.2(6) . . . . ? C13 C14 C15 C16 -2.0(6) . . . . ? C14 C15 C16 N3 176.2(3) . . . . ? C14 C15 C16 C11 0.5(6) . . . . ? C10 C11 C16 C15 -180.0(4) . . . . ? C12 C11 C16 C15 1.8(5) . . . . ? C10 C11 C16 N3 4.0(5) . . . . ? C12 C11 C16 N3 -174.2(3) . . . . ? N4 C18 C19 C20 0.1(6) . . . . ? C18 C19 C20 C21 -1.3(5) . . . . ? C18 C19 C20 C17 179.6(3) . . . . ? N3 C17 C20 C21 0.8(5) . . . . ? N3 C17 C20 C19 179.8(3) . . . . ? C19 C20 C21 C22 1.6(5) . . . . ? C17 C20 C21 C22 -179.3(3) . . . . ? C20 C21 C22 N4 -0.6(6) . . . . ? C4 C5 N1 C1 -0.5(5) . . . . ? C4 C5 N1 Co -172.9(3) . . . . ? C2 C1 N1 C5 0.0(6) . . . . ? C2 C1 N1 Co 172.8(3) . . . . ? N4 Co N1 C5 -47(2) 1_464 . . . ? N5 Co N1 C5 119.4(3) . . . . ? O15 Co N1 C5 -155.8(3) . . . . ? O12 Co N1 C5 -23.1(3) . . . . ? O11 Co N1 C5 34.5(3) . . . . ? O14 Co N1 C5 -100.5(3) . . . . ? N4 Co N1 C1 141(2) 1_464 . . . ? N5 Co N1 C1 -52.9(3) . . . . ? O15 Co N1 C1 31.9(3) . . . . ? O12 Co N1 C1 164.7(3) . . . . ? O11 Co N1 C1 -137.7(3) . . . . ? O14 Co N1 C1 87.2(3) . . . . ? C3 C6 N2 C7 -179.0(4) . . . . ? C8 C7 N2 C6 55.1(6) . . . . ? C12 C7 N2 C6 -128.2(4) . . . . ? C20 C17 N3 C16 -174.6(3) . . . . ? C15 C16 N3 C17 22.7(5) . . . . ? C11 C16 N3 C17 -161.4(3) . . . . ? C21 C22 N4 C18 -0.7(6) . . . . ? C21 C22 N4 Co 173.1(3) . . . 1_646 ? C19 C18 N4 C22 0.9(6) . . . . ? C19 C18 N4 Co -172.7(3) . . . 1_646 ? N5 C23 C24 C25 0.7(5) . . . . ? C23 C24 C25 C26 -0.5(5) . . . . ? C23 C24 C25 C28 -179.9(3) . . . . ? C24 C25 C26 C27 0.2(5) . . . . ? C28 C25 C26 C27 179.6(3) . . . . ? C25 C26 C27 N5 0.1(6) . . . . ? C26 C25 C28 N6 -175.9(3) . . . . ? C24 C25 C28 N6 3.4(6) . . . . ? N6 C29 C30 C31 -178.5(4) . . . . ? C33 C29 C30 C31 3.5(6) 2_755 . . . ? C29 C30 C31 C32 -0.6(6) . . . . ? C30 C31 C32 C33 -2.0(6) . . . . ? C31 C32 C33 C33 1.4(6) . . . 2_755 ? C31 C32 C33 C29 -177.0(4) . . . 2_755 ? C24 C23 N5 C27 -0.4(5) . . . . ? C24 C23 N5 Co -172.9(3) . . . . ? C26 C27 N5 C23 0.0(5) . . . . ? C26 C27 N5 Co 172.7(3) . . . . ? N4 Co N5 C23 -53.5(3) 1_464 . . . ? N1 Co N5 C23 127.2(3) . . . . ? O15 Co N5 C23 34.7(3) . . . . ? O12 Co N5 C23 -141.2(3) . . . . ? O11 Co N5 C23 -140.6(3) . . . . ? O14 Co N5 C23 44.8(3) . . . . ? N4 Co N5 C27 134.2(3) 1_464 . . . ? N1 Co N5 C27 -45.1(3) . . . . ? O15 Co N5 C27 -137.6(3) . . . . ? O12 Co N5 C27 46.5(3) . . . . ? O11 Co N5 C27 47.1(3) . . . . ? O14 Co N5 C27 -127.5(3) . . . . ? C25 C28 N6 C29 -178.3(3) . . . . ? C30 C29 N6 C28 36.1(5) . . . . ? C33 C29 N6 C28 -145.9(3) 2_755 . . . ? O13 N11 O11 Co -175.0(3) . . . . ? O12 N11 O11 Co 4.9(3) . . . . ? N4 Co O11 N11 81.7(2) 1_464 . . . ? N1 Co O11 N11 -95.3(2) . . . . ? N5 Co O11 N11 177.4(2) . . . . ? O15 Co O11 N11 152.8(4) . . . . ? O12 Co O11 N11 -3.03(18) . . . . ? O14 Co O11 N11 -7.6(2) . . . . ? O13 N11 O12 Co 174.8(3) . . . . ? O11 N11 O12 Co -5.1(3) . . . . ? N4 Co O12 N11 -87.8(2) 1_464 . . . ? N1 Co O12 N11 93.5(2) . . . . ? N5 Co O12 N11 3.8(3) . . . . ? O15 Co O12 N11 -170.78(17) . . . . ? O11 Co O12 N11 3.06(18) . . . . ? O14 Co O12 N11 179.8(2) . . . . ? O16 N12 O14 Co 180.0(3) . . . . ? O15 N12 O14 Co -0.4(3) . . . . ? N4 Co O14 N12 87.9(2) 1_464 . . . ? N1 Co O14 N12 -94.5(2) . . . . ? N5 Co O14 N12 -12.0(3) . . . . ? O15 Co O14 N12 0.25(17) . . . . ? O12 Co O14 N12 171.8(2) . . . . ? O11 Co O14 N12 175.75(17) . . . . ? O16 N12 O15 Co -179.9(3) . . . . ? O14 N12 O15 Co 0.4(3) . . . . ? N4 Co O15 N12 -92.5(2) 1_464 . . . ? N1 Co O15 N12 84.6(2) . . . . ? N5 Co O15 N12 171.9(2) . . . . ? O12 Co O15 N12 -11.5(2) . . . . ? O11 Co O15 N12 -163.6(4) . . . . ? O14 Co O15 N12 -0.26(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.945 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.080 #cy21231s_Cd.cif data_cy21231s _database_code_depnum_ccdc_archive 'CCDC 235892' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H48 Cd2 N16 O12' _chemical_formula_weight 1482.00 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.6034(9) _cell_length_b 13.5413(8) _cell_length_c 15.8953(10) _cell_angle_alpha 90.00 _cell_angle_beta 116.0690(10) _cell_angle_gamma 90.00 _cell_volume 3016.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 5853 _cell_measurement_theta_min 2.906 _cell_measurement_theta_max 24.984 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7761 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 21894 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5315 _reflns_number_gt 4837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0458P)^2^+8.0327P] 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 5315 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Cd Cd 0.16258(2) 0.01671(2) 0.71555(2) 0.03597(12) Uani 1 1 d . . . C1 C 0.1363(4) 0.2406(3) 0.6406(4) 0.0438(11) Uani 1 1 d . . . H1 H 0.1346 0.2492 0.6991 0.053 Uiso 1 1 calc R . . C2 C 0.1230(4) 0.3211(4) 0.5855(4) 0.0497(12) Uani 1 1 d . . . H2 H 0.1131 0.3840 0.6063 0.060 Uiso 1 1 calc R . . C3 C 0.1236(3) 0.3119(3) 0.4985(3) 0.0396(10) Uani 1 1 d . . . C4 C 0.1392(3) 0.2180(3) 0.4727(3) 0.0420(11) Uani 1 1 d . . . H4 H 0.1401 0.2072 0.4141 0.050 Uiso 1 1 calc R . . C5 C 0.1534(3) 0.1413(3) 0.5338(3) 0.0427(11) Uani 1 1 d . . . H5 H 0.1651 0.0777 0.5158 0.051 Uiso 1 1 calc R . . C6 C 0.1137(4) 0.3999(3) 0.4410(4) 0.0467(12) Uani 1 1 d . . . H6 H 0.1149 0.4627 0.4682 0.056 Uiso 1 1 calc R . . C7 C 0.0944(3) 0.4864(3) 0.3083(3) 0.0386(10) Uani 1 1 d . . . C8 C 0.0639(3) 0.5746(3) 0.3280(3) 0.0452(11) Uani 1 1 d . . . H8 H 0.0440 0.5770 0.3765 0.054 Uiso 1 1 calc R . . C9 C 0.0613(4) 0.6607(3) 0.2789(4) 0.0468(12) Uani 1 1 d . . . H9 H 0.0424 0.7211 0.2961 0.056 Uiso 1 1 calc R . . C10 C 0.0856(3) 0.6593(3) 0.2063(3) 0.0411(10) Uani 1 1 d . . . H10 H 0.0847 0.7188 0.1742 0.049 Uiso 1 1 calc R . . C11 C 0.1120(3) 0.5700(3) 0.1788(3) 0.0370(10) Uani 1 1 d . . . C12 C 0.1171(3) 0.4817(3) 0.2302(3) 0.0380(10) Uani 1 1 d . . . C13 C 0.1456(4) 0.3929(3) 0.2041(4) 0.0486(12) Uani 1 1 d . . . H13 H 0.1497 0.3340 0.2381 0.058 Uiso 1 1 calc R . . C14 C 0.1675(5) 0.3914(4) 0.1299(4) 0.0633(16) Uani 1 1 d . . . H14 H 0.1873 0.3313 0.1130 0.076 Uiso 1 1 calc R . . C15 C 0.1613(4) 0.4775(4) 0.0782(4) 0.0565(14) Uani 1 1 d . . . H15 H 0.1766 0.4745 0.0266 0.068 Uiso 1 1 calc R . . C16 C 0.1339(3) 0.5654(3) 0.1005(3) 0.0410(10) Uani 1 1 d . . . C17 C 0.0999(4) 0.6528(4) -0.0350(4) 0.0489(12) Uani 1 1 d . . . H17 H 0.0682 0.5950 -0.0677 0.059 Uiso 1 1 calc R . . C18 C 0.1473(3) 0.9043(3) -0.1066(3) 0.0410(11) Uani 1 1 d . . . H18 H 0.1659 0.9682 -0.0801 0.049 Uiso 1 1 calc R . . C19 C 0.1364(3) 0.8314(3) -0.0512(3) 0.0403(10) Uani 1 1 d . . . H19 H 0.1485 0.8450 0.0117 0.048 Uiso 1 1 calc R . . C20 C 0.1075(3) 0.7382(3) -0.0889(3) 0.0422(11) Uani 1 1 d . . . C21 C 0.0893(4) 0.7239(4) -0.1817(4) 0.0572(14) Uani 1 1 d . . . H21 H 0.0678 0.6616 -0.2109 0.069 Uiso 1 1 calc R . . C22 C 0.1029(4) 0.8014(4) -0.2309(4) 0.0511(13) Uani 1 1 d . . . H22 H 0.0895 0.7903 -0.2944 0.061 Uiso 1 1 calc R . . C23 C 0.1423(3) -0.1473(3) 0.5644(3) 0.0385(10) Uani 1 1 d . . . H23 H 0.0768 -0.1369 0.5488 0.046 Uiso 1 1 calc R . . C24 C 0.1661(3) -0.2207(3) 0.5178(3) 0.0395(10) Uani 1 1 d . . . H24 H 0.1177 -0.2595 0.4712 0.047 Uiso 1 1 calc R . . C25 C 0.2614(3) -0.2370(3) 0.5400(3) 0.0370(10) Uani 1 1 d . . . C26 C 0.3280(3) -0.1759(3) 0.6049(3) 0.0423(11) Uani 1 1 d . . . H26 H 0.3937 -0.1826 0.6197 0.051 Uiso 1 1 calc R . . C27 C 0.2983(3) -0.1047(3) 0.6483(3) 0.0423(11) Uani 1 1 d . . . H27 H 0.3451 -0.0634 0.6937 0.051 Uiso 1 1 calc R . . C28 C 0.2912(3) -0.3171(3) 0.4963(3) 0.0400(10) Uani 1 1 d . . . H28 H 0.2445 -0.3596 0.4524 0.048 Uiso 1 1 calc R . . C29 C 0.4032(3) -0.4054(3) 0.4689(3) 0.0350(10) Uani 1 1 d . . . C30 C 0.3533(3) -0.4203(4) 0.3752(3) 0.0469(12) Uani 1 1 d . . . H30 H 0.2989 -0.3807 0.3398 0.056 Uiso 1 1 calc R . . C31 C 0.4867(3) -0.4621(3) 0.5236(3) 0.0303(9) Uani 1 1 d . . . C32 C 0.5411(3) -0.4482(3) 0.6206(3) 0.0390(10) Uani 1 1 d . . . H32 H 0.5238 -0.3981 0.6521 0.047 Uiso 1 1 calc R . . C33 C 0.6185(4) -0.5064(4) 0.6695(4) 0.0492(12) Uani 1 1 d . . . H33 H 0.6540 -0.4970 0.7351 0.059 Uiso 1 1 calc R . . N1 N 0.1518(3) 0.1499(3) 0.6171(3) 0.0359(8) Uani 1 1 d . . . N2 N 0.1038(3) 0.3978(3) 0.3588(3) 0.0414(9) Uani 1 1 d . . . N3 N 0.1345(3) 0.6542(3) 0.0541(3) 0.0409(9) Uani 1 1 d . . . N4 N 0.1334(3) 0.8908(3) -0.1952(3) 0.0369(8) Uani 1 1 d . . . N5 N 0.2064(3) -0.0909(3) 0.6296(3) 0.0367(8) Uani 1 1 d . . . N6 N 0.3785(3) -0.3300(3) 0.5167(3) 0.0365(8) Uani 1 1 d . . . N11 N -0.0313(3) 0.0511(3) 0.6550(3) 0.0509(11) Uani 1 1 d . . . O11 O -0.0020(2) -0.0113(3) 0.6137(3) 0.0533(9) Uani 1 1 d . . . O12 O 0.0305(3) 0.1003(2) 0.7210(3) 0.0526(9) Uani 1 1 d . . . O13 O -0.1166(3) 0.0622(4) 0.6311(3) 0.0819(14) Uani 1 1 d . . . N12 N 0.3408(3) 0.0788(3) 0.8633(3) 0.0467(10) Uani 1 1 d . . . O14 O 0.3423(3) 0.0537(4) 0.7914(3) 0.0833(14) Uani 1 1 d . . . O15 O 0.2608(3) 0.0814(3) 0.8632(3) 0.0715(12) Uani 1 1 d . . . O16 O 0.4145(3) 0.0974(3) 0.9338(3) 0.0719(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 Cd 0.0482(2) 0.02748(18) 0.0406(2) 0.00194(13) 0.02721(16) 0.00706(13) C1 0.062(3) 0.033(2) 0.047(3) -0.002(2) 0.034(2) -0.005(2) C2 0.072(3) 0.033(3) 0.058(3) -0.002(2) 0.041(3) -0.001(2) C3 0.044(2) 0.034(2) 0.044(3) -0.001(2) 0.022(2) -0.0051(19) C4 0.051(3) 0.042(3) 0.040(3) 0.003(2) 0.026(2) 0.001(2) C5 0.055(3) 0.033(2) 0.046(3) 0.001(2) 0.028(2) 0.005(2) C6 0.061(3) 0.033(2) 0.054(3) 0.002(2) 0.033(3) -0.001(2) C7 0.043(2) 0.038(2) 0.038(2) 0.004(2) 0.020(2) 0.0003(19) C8 0.058(3) 0.044(3) 0.037(3) 0.001(2) 0.024(2) 0.011(2) C9 0.056(3) 0.036(3) 0.050(3) 0.001(2) 0.025(2) 0.014(2) C10 0.047(3) 0.034(2) 0.043(3) 0.009(2) 0.021(2) 0.0109(19) C11 0.036(2) 0.038(2) 0.037(2) 0.0017(19) 0.0156(19) 0.0010(18) C12 0.039(2) 0.035(2) 0.041(3) 0.002(2) 0.019(2) -0.0001(18) C13 0.072(3) 0.032(3) 0.055(3) 0.001(2) 0.040(3) 0.000(2) C14 0.107(5) 0.035(3) 0.071(4) -0.003(3) 0.059(4) 0.008(3) C15 0.090(4) 0.045(3) 0.054(3) 0.003(2) 0.049(3) 0.002(3) C16 0.047(3) 0.038(3) 0.042(3) 0.004(2) 0.024(2) 0.001(2) C17 0.052(3) 0.045(3) 0.049(3) 0.002(2) 0.021(2) -0.009(2) C18 0.053(3) 0.030(2) 0.050(3) -0.002(2) 0.033(2) 0.0068(19) C19 0.049(3) 0.040(3) 0.039(3) 0.003(2) 0.026(2) 0.006(2) C20 0.041(2) 0.044(3) 0.043(3) 0.006(2) 0.020(2) 0.000(2) C21 0.073(4) 0.044(3) 0.049(3) -0.001(2) 0.022(3) -0.020(3) C22 0.069(3) 0.046(3) 0.035(3) 0.000(2) 0.019(2) -0.011(2) C23 0.038(2) 0.042(3) 0.040(3) 0.004(2) 0.022(2) 0.0103(19) C24 0.045(3) 0.040(2) 0.036(3) 0.0015(19) 0.020(2) 0.0049(19) C25 0.046(3) 0.034(2) 0.039(3) 0.0073(19) 0.025(2) 0.0058(19) C26 0.039(2) 0.047(3) 0.045(3) 0.002(2) 0.023(2) 0.009(2) C27 0.049(3) 0.040(3) 0.044(3) -0.004(2) 0.026(2) 0.001(2) C28 0.051(3) 0.036(2) 0.038(3) 0.0008(19) 0.024(2) 0.007(2) C29 0.044(2) 0.029(2) 0.044(3) 0.0014(18) 0.031(2) 0.0051(18) C30 0.048(3) 0.048(3) 0.045(3) 0.004(2) 0.021(2) 0.014(2) C31 0.038(2) 0.023(2) 0.038(2) -0.0019(17) 0.0245(19) -0.0023(16) C32 0.043(2) 0.037(2) 0.046(3) -0.008(2) 0.027(2) 0.0023(19) C33 0.054(3) 0.056(3) 0.038(3) -0.009(2) 0.020(2) 0.006(2) N1 0.044(2) 0.0340(19) 0.036(2) 0.0002(15) 0.0236(17) 0.0013(15) N2 0.055(2) 0.036(2) 0.040(2) 0.0037(17) 0.0272(19) 0.0025(17) N3 0.048(2) 0.037(2) 0.043(2) 0.0071(17) 0.0242(19) 0.0045(16) N4 0.042(2) 0.033(2) 0.040(2) 0.0040(16) 0.0217(17) 0.0049(15) N5 0.047(2) 0.0329(19) 0.040(2) 0.0073(16) 0.0278(18) 0.0091(16) N6 0.045(2) 0.0304(19) 0.043(2) 0.0017(16) 0.0279(18) 0.0082(15) N11 0.049(2) 0.058(3) 0.059(3) 0.032(2) 0.036(2) 0.020(2) O11 0.052(2) 0.056(2) 0.057(2) 0.0015(17) 0.0286(18) 0.0072(16) O12 0.077(3) 0.0387(19) 0.064(2) 0.0110(17) 0.051(2) 0.0131(17) O13 0.059(2) 0.117(4) 0.084(3) 0.051(3) 0.045(2) 0.038(2) N12 0.067(3) 0.035(2) 0.041(2) -0.0032(18) 0.026(2) 0.0004(19) O14 0.077(3) 0.116(4) 0.052(3) -0.026(2) 0.023(2) 0.016(3) O15 0.078(3) 0.087(3) 0.070(3) -0.035(2) 0.051(2) -0.037(2) O16 0.077(3) 0.080(3) 0.050(2) -0.018(2) 0.021(2) -0.014(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 Cd N5 2.296(3) . ? Cd O15 2.338(4) . ? Cd N1 2.345(4) . ? Cd O12 2.386(3) . ? Cd N4 2.386(4) 1_546 ? Cd O11 2.389(4) . ? Cd O14 2.568(5) . ? C1 N1 1.338(6) . ? C1 C2 1.355(7) . ? C1 H1 0.9500 . ? C2 C3 1.393(7) . ? C2 H2 0.9500 . ? C3 C4 1.389(6) . ? C3 C6 1.469(6) . ? C4 C5 1.373(6) . ? C4 H4 0.9500 . ? C5 N1 1.339(6) . ? C5 H5 0.9500 . ? C6 N2 1.247(6) . ? C6 H6 0.9500 . ? C7 C8 1.372(6) . ? C7 N2 1.415(6) . ? C7 C12 1.434(6) . ? C8 C9 1.395(7) . ? C8 H8 0.9500 . ? C9 C10 1.364(6) . ? C9 H9 0.9500 . ? C10 C11 1.407(6) . ? C10 H10 0.9500 . ? C11 C16 1.428(6) . ? C11 C12 1.431(6) . ? C12 C13 1.406(6) . ? C13 C14 1.364(7) . ? C13 H13 0.9500 . ? C14 C15 1.406(7) . ? C14 H14 0.9500 . ? C15 C16 1.362(7) . ? C15 H15 0.9500 . ? C16 N3 1.413(6) . ? C17 N3 1.276(6) . ? C17 C20 1.474(7) . ? C17 H17 0.9500 . ? C18 N4 1.340(6) . ? C18 C19 1.382(6) . ? C18 H18 0.9500 . ? C19 C20 1.385(7) . ? C19 H19 0.9500 . ? C20 C21 1.387(7) . ? C21 C22 1.380(7) . ? C21 H21 0.9500 . ? C22 N4 1.332(6) . ? C22 H22 0.9500 . ? C23 N5 1.322(6) . ? C23 C24 1.385(6) . ? C23 H23 0.9500 . ? C24 C25 1.387(6) . ? C24 H24 0.9500 . ? C25 C26 1.374(7) . ? C25 C28 1.469(6) . ? C26 C27 1.379(6) . ? C26 H26 0.9500 . ? C27 N5 1.344(6) . ? C27 H27 0.9500 . ? C28 N6 1.266(6) . ? C28 H28 0.9500 . ? C29 C30 1.359(6) . ? C29 N6 1.423(5) . ? C29 C31 1.431(6) . ? C30 C33 1.400(6) 3_646 ? C30 H30 0.9500 . ? C31 C32 1.408(6) . ? C31 C31 1.436(8) 3_646 ? C32 C33 1.364(7) . ? C32 H32 0.9500 . ? C33 C30 1.400(6) 3_646 ? C33 H33 0.9500 . ? N4 Cd 2.386(4) 1_564 ? N11 O13 1.223(5) . ? N11 O12 1.260(6) . ? N11 O11 1.270(6) . ? N12 O14 1.202(5) . ? N12 O16 1.229(5) . ? N12 O15 1.248(5) . ? 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 N5 Cd O15 126.84(14) . . ? N5 Cd N1 92.49(12) . . ? O15 Cd N1 101.85(14) . . ? N5 Cd O12 144.11(14) . . ? O15 Cd O12 88.92(15) . . ? N1 Cd O12 81.38(11) . . ? N5 Cd N4 94.84(12) . 1_546 ? O15 Cd N4 83.27(14) . 1_546 ? N1 Cd N4 165.91(12) . 1_546 ? O12 Cd N4 85.64(11) . 1_546 ? N5 Cd O11 90.51(13) . . ? O15 Cd O11 140.81(13) . . ? N1 Cd O11 85.96(12) . . ? O12 Cd O11 53.93(13) . . ? N4 Cd O11 81.97(12) 1_546 . ? N5 Cd O14 81.62(14) . . ? O15 Cd O14 49.95(13) . . ? N1 Cd O14 84.64(15) . . ? O12 Cd O14 132.26(15) . . ? N4 Cd O14 108.31(15) 1_546 . ? O11 Cd O14 167.45(13) . . ? N1 C1 C2 123.6(4) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 120.2(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 117.0(4) . . ? C4 C3 C6 122.9(4) . . ? C2 C3 C6 120.0(4) . . ? C5 C4 C3 118.6(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 124.5(4) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? N2 C6 C3 124.4(4) . . ? N2 C6 H6 117.8 . . ? C3 C6 H6 117.8 . . ? C8 C7 N2 124.6(4) . . ? C8 C7 C12 118.7(4) . . ? N2 C7 C12 116.7(4) . . ? C7 C8 C9 121.8(4) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.2(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C16 121.5(4) . . ? C10 C11 C12 119.4(4) . . ? C16 C11 C12 119.0(4) . . ? C13 C12 C11 119.5(4) . . ? C13 C12 C7 121.6(4) . . ? C11 C12 C7 118.9(4) . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.9(5) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 121.4(5) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 N3 122.2(4) . . ? C15 C16 C11 119.2(4) . . ? N3 C16 C11 118.4(4) . . ? N3 C17 C20 122.1(5) . . ? N3 C17 H17 118.9 . . ? C20 C17 H17 118.9 . . ? N4 C18 C19 124.3(4) . . ? N4 C18 H18 117.9 . . ? C19 C18 H18 117.9 . . ? C18 C19 C20 118.9(4) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C21 117.6(4) . . ? C19 C20 C17 123.9(4) . . ? C21 C20 C17 118.5(4) . . ? C22 C21 C20 119.1(5) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? N4 C22 C21 124.4(5) . . ? N4 C22 H22 117.8 . . ? C21 C22 H22 117.8 . . ? N5 C23 C24 123.1(4) . . ? N5 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 117.9(4) . . ? C26 C25 C28 120.5(4) . . ? C24 C25 C28 121.6(4) . . ? C25 C26 C27 119.2(4) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N5 C27 C26 123.2(4) . . ? N5 C27 H27 118.4 . . ? C26 C27 H27 118.4 . . ? N6 C28 C25 120.6(4) . . ? N6 C28 H28 119.7 . . ? C25 C28 H28 119.7 . . ? C30 C29 N6 122.2(4) . . ? C30 C29 C31 121.1(4) . . ? N6 C29 C31 116.6(4) . . ? C29 C30 C33 120.3(4) . 3_646 ? C29 C30 H30 119.8 . . ? C33 C30 H30 119.8 3_646 . ? C32 C31 C29 122.9(4) . . ? C32 C31 C31 119.6(5) . 3_646 ? C29 C31 C31 117.4(5) . 3_646 ? C33 C32 C31 120.3(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C30 121.2(5) . 3_646 ? C32 C33 H33 119.4 . . ? C30 C33 H33 119.4 3_646 . ? C1 N1 C5 116.1(4) . . ? C1 N1 Cd 119.3(3) . . ? C5 N1 Cd 124.4(3) . . ? C6 N2 C7 120.6(4) . . ? C17 N3 C16 118.1(4) . . ? C22 N4 C18 115.7(4) . . ? C22 N4 Cd 121.5(3) . 1_564 ? C18 N4 Cd 122.8(3) . 1_564 ? C23 N5 C27 117.3(4) . . ? C23 N5 Cd 120.9(3) . . ? C27 N5 Cd 121.6(3) . . ? C28 N6 C29 118.5(4) . . ? O13 N11 O12 121.5(5) . . ? O13 N11 O11 120.7(5) . . ? O12 N11 O11 117.7(4) . . ? N11 O11 Cd 93.9(3) . . ? N11 O12 Cd 94.3(3) . . ? O14 N12 O16 121.6(5) . . ? O14 N12 O15 116.3(4) . . ? O16 N12 O15 122.0(4) . . ? N12 O14 Cd 91.6(3) . . ? N12 O15 Cd 101.8(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 N1 C1 C2 C3 0.9(8) . . . . ? C1 C2 C3 C4 -0.6(7) . . . . ? C1 C2 C3 C6 -177.1(5) . . . . ? C2 C3 C4 C5 -0.4(7) . . . . ? C6 C3 C4 C5 176.1(5) . . . . ? C3 C4 C5 N1 1.1(7) . . . . ? C4 C3 C6 N2 11.3(8) . . . . ? C2 C3 C6 N2 -172.4(5) . . . . ? N2 C7 C8 C9 176.3(5) . . . . ? C12 C7 C8 C9 -4.9(7) . . . . ? C7 C8 C9 C10 2.7(8) . . . . ? C8 C9 C10 C11 1.2(7) . . . . ? C9 C10 C11 C16 177.3(5) . . . . ? C9 C10 C11 C12 -2.8(7) . . . . ? C10 C11 C12 C13 -178.5(4) . . . . ? C16 C11 C12 C13 1.4(7) . . . . ? C10 C11 C12 C7 0.5(6) . . . . ? C16 C11 C12 C7 -179.5(4) . . . . ? C8 C7 C12 C13 -177.8(5) . . . . ? N2 C7 C12 C13 1.1(7) . . . . ? C8 C7 C12 C11 3.2(7) . . . . ? N2 C7 C12 C11 -177.9(4) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C7 C12 C13 C14 -179.4(5) . . . . ? C12 C13 C14 C15 -0.5(9) . . . . ? C13 C14 C15 C16 0.4(10) . . . . ? C14 C15 C16 N3 174.9(5) . . . . ? C14 C15 C16 C11 0.7(8) . . . . ? C10 C11 C16 C15 178.4(5) . . . . ? C12 C11 C16 C15 -1.6(7) . . . . ? C10 C11 C16 N3 3.9(7) . . . . ? C12 C11 C16 N3 -176.0(4) . . . . ? N4 C18 C19 C20 -1.3(7) . . . . ? C18 C19 C20 C21 -1.2(7) . . . . ? C18 C19 C20 C17 175.5(4) . . . . ? N3 C17 C20 C19 -11.9(8) . . . . ? N3 C17 C20 C21 164.7(5) . . . . ? C19 C20 C21 C22 1.5(8) . . . . ? C17 C20 C21 C22 -175.3(5) . . . . ? C20 C21 C22 N4 0.5(9) . . . . ? N5 C23 C24 C25 0.2(7) . . . . ? C23 C24 C25 C26 -2.8(6) . . . . ? C23 C24 C25 C28 176.9(4) . . . . ? C24 C25 C26 C27 3.1(7) . . . . ? C28 C25 C26 C27 -176.6(4) . . . . ? C25 C26 C27 N5 -0.8(7) . . . . ? C26 C25 C28 N6 -1.2(7) . . . . ? C24 C25 C28 N6 179.1(4) . . . . ? N6 C29 C30 C33 178.4(4) . . . 3_646 ? C31 C29 C30 C33 1.5(7) . . . 3_646 ? C30 C29 C31 C32 179.3(4) . . . . ? N6 C29 C31 C32 2.3(6) . . . . ? C30 C29 C31 C31 -2.5(7) . . . 3_646 ? N6 C29 C31 C31 -179.5(4) . . . 3_646 ? C29 C31 C32 C33 178.2(4) . . . . ? C31 C31 C32 C33 0.0(7) 3_646 . . . ? C31 C32 C33 C30 1.1(8) . . . 3_646 ? C2 C1 N1 C5 -0.2(7) . . . . ? C2 C1 N1 Cd -175.6(4) . . . . ? C4 C5 N1 C1 -0.8(7) . . . . ? C4 C5 N1 Cd 174.4(4) . . . . ? N5 Cd N1 C1 -173.3(3) . . . . ? O15 Cd N1 C1 -44.8(4) . . . . ? O12 Cd N1 C1 42.3(3) . . . . ? N4 Cd N1 C1 65.3(7) 1_546 . . . ? O11 Cd N1 C1 96.4(3) . . . . ? O14 Cd N1 C1 -91.9(3) . . . . ? N5 Cd N1 C5 11.7(4) . . . . ? O15 Cd N1 C5 140.2(4) . . . . ? O12 Cd N1 C5 -132.7(4) . . . . ? N4 Cd N1 C5 -109.6(6) 1_546 . . . ? O11 Cd N1 C5 -78.6(4) . . . . ? O14 Cd N1 C5 93.1(4) . . . . ? C3 C6 N2 C7 179.8(4) . . . . ? C8 C7 N2 C6 -22.7(7) . . . . ? C12 C7 N2 C6 158.5(5) . . . . ? C20 C17 N3 C16 -172.6(4) . . . . ? C15 C16 N3 C17 45.4(7) . . . . ? C11 C16 N3 C17 -140.3(5) . . . . ? C21 C22 N4 C18 -2.8(8) . . . . ? C21 C22 N4 Cd 176.6(4) . . . 1_564 ? C19 C18 N4 C22 3.2(7) . . . . ? C19 C18 N4 Cd -176.1(3) . . . 1_564 ? C24 C23 N5 C27 2.2(6) . . . . ? C24 C23 N5 Cd -172.8(3) . . . . ? C26 C27 N5 C23 -1.9(7) . . . . ? C26 C27 N5 Cd 173.0(3) . . . . ? O15 Cd N5 C23 157.1(3) . . . . ? N1 Cd N5 C23 -96.1(3) . . . . ? O12 Cd N5 C23 -17.4(4) . . . . ? N4 Cd N5 C23 71.9(3) 1_546 . . . ? O11 Cd N5 C23 -10.1(3) . . . . ? O14 Cd N5 C23 179.7(3) . . . . ? O15 Cd N5 C27 -17.6(4) . . . . ? N1 Cd N5 C27 89.2(3) . . . . ? O12 Cd N5 C27 167.9(3) . . . . ? N4 Cd N5 C27 -102.8(3) 1_546 . . . ? O11 Cd N5 C27 175.2(3) . . . . ? O14 Cd N5 C27 5.0(3) . . . . ? C25 C28 N6 C29 -176.8(4) . . . . ? C30 C29 N6 C28 42.6(6) . . . . ? C31 C29 N6 C28 -140.4(4) . . . . ? O13 N11 O11 Cd -176.2(4) . . . . ? O12 N11 O11 Cd 3.6(4) . . . . ? N5 Cd O11 N11 -176.8(3) . . . . ? O15 Cd O11 N11 19.5(4) . . . . ? N1 Cd O11 N11 -84.3(3) . . . . ? O12 Cd O11 N11 -2.1(2) . . . . ? N4 Cd O11 N11 88.4(3) 1_546 . . . ? O14 Cd O11 N11 -125.9(6) . . . . ? O13 N11 O12 Cd 176.2(4) . . . . ? O11 N11 O12 Cd -3.6(4) . . . . ? N5 Cd O12 N11 11.1(4) . . . . ? O15 Cd O12 N11 -164.5(3) . . . . ? N1 Cd O12 N11 93.3(3) . . . . ? N4 Cd O12 N11 -81.2(3) 1_546 . . . ? O11 Cd O12 N11 2.1(2) . . . . ? O14 Cd O12 N11 168.0(2) . . . . ? O16 N12 O14 Cd 172.8(4) . . . . ? O15 N12 O14 Cd -4.7(5) . . . . ? N5 Cd O14 N12 -153.3(4) . . . . ? O15 Cd O14 N12 3.0(3) . . . . ? N1 Cd O14 N12 113.3(3) . . . . ? O12 Cd O14 N12 40.1(4) . . . . ? N4 Cd O14 N12 -61.0(4) 1_546 . . . ? O11 Cd O14 N12 155.0(5) . . . . ? O14 N12 O15 Cd 5.3(5) . . . . ? O16 N12 O15 Cd -172.2(4) . . . . ? N5 Cd O15 N12 26.9(4) . . . . ? N1 Cd O15 N12 -75.4(3) . . . . ? O12 Cd O15 N12 -156.3(3) . . . . ? N4 Cd O15 N12 117.9(3) 1_546 . . . ? O11 Cd O15 N12 -173.6(3) . . . . ? O14 Cd O15 N12 -2.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.215 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.085