# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Seth M. Cohen' _publ_contact_author_address ;U.C. San Diego Dept. of Chemistry and Biochemistry 9500 Gilman Drive La Jolla, CA 92093-0358 ; _publ_contact_author_email scohen@ucsd.edu _publ_contact_author_phone 858-822-5596 _publ_contact_author_fax 858-822-5598 loop_ _publ_author_name _publ_author_address S.M.Cohen ;U.C. San Diego Dept. of Chemistry and Biochemistry 9500 Gilman Drive La Jolla, CA 92093-0358 ; D.L.Murphy ;U.C. San Diego Dept. of Chemistry and Biochemistry 9500 Gilman Drive La Jolla, CA 92093-0358 ; M.R.Malachowski ;Department of Chemistry University of San Diego San Diego, CA 92110-2492 ; C.F.Campana ;Single Crystal X-ray Diffraction Bruker AXS Inc. Madison, Wisconsin 53711-5373 ; _publ_section_title ; A Chiral, Heterometallic Metal-Organic Framework Derived from a Tris(Chelate) Coordination Complex ; data_Co(4-cydpm)3 _database_code_depnum_ccdc_archive 'CCDC 281272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H30 Cl1.50 Co N9' _chemical_formula_weight 844.91 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' 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 14.8303(8) _cell_length_b 16.3535(8) _cell_length_c 20.0347(10) _cell_angle_alpha 72.6680(10) _cell_angle_beta 68.7730(10) _cell_angle_gamma 72.6340(10) _cell_volume 4223.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8313 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.34 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1734 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.893041 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36097 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.53 _reflns_number_total 18461 _reflns_number_gt 14110 _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^)+(0.1029P)^2^+9.2486P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18461 _refine_ls_number_parameters 1117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1982 _refine_ls_wR_factor_gt 0.1821 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.002 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 Cl2 Cl 0.25247(10) 0.59421(10) 0.87849(7) 0.0541(3) Uani 1 1 d . . . Co1 Co 0.77513(4) 0.75368(3) 0.57244(3) 0.02000(13) Uani 1 1 d . . . N6 N 0.7376(2) 0.85875(19) 0.61118(16) 0.0227(6) Uani 1 1 d . . . N1 N 0.8387(2) 0.82231(19) 0.47884(16) 0.0216(6) Uani 1 1 d . . . N4 N 0.7154(2) 0.68922(19) 0.66970(16) 0.0220(6) Uani 1 1 d . . . N5 N 0.8989(2) 0.71521(19) 0.59677(16) 0.0225(6) Uani 1 1 d . . . Co2 Co 0.71537(3) 0.74020(3) 0.08532(2) 0.01547(12) Uani 1 1 d . . . C29 C 0.7210(3) 0.5990(2) 0.69179(19) 0.0203(7) Uani 1 1 d . . . C4 C 0.7960(3) 0.8699(2) 0.4235(2) 0.0233(8) Uani 1 1 d . . . N15 N 0.6778(2) 0.83345(18) 0.00783(15) 0.0173(6) Uani 1 1 d . . . N12 N 0.7529(2) 0.64026(18) 0.15918(16) 0.0174(6) Uani 1 1 d . . . N10 N 0.8446(2) 0.71334(18) 0.01412(16) 0.0176(6) Uani 1 1 d . . . N13 N 0.5893(2) 0.77854(19) 0.15539(16) 0.0186(6) Uani 1 1 d . . . N14 N 0.7663(2) 0.81567(18) 0.11498(16) 0.0184(6) Uani 1 1 d . . . N11 N 0.6635(2) 0.66137(19) 0.06006(15) 0.0174(6) Uani 1 1 d . . . C77 C 0.5642(2) 0.7512(2) 0.23170(19) 0.0174(7) Uani 1 1 d . . . C61 C 0.7122(3) 0.6133(2) 0.00504(19) 0.0194(7) Uani 1 1 d . . . C49 C 0.9240(3) 0.7448(2) 0.00147(19) 0.0200(7) Uani 1 1 d . . . H49 H 0.9255 0.7843 0.0260 0.024 Uiso 1 1 calc R . . C62 C 0.6453(3) 0.5680(2) 0.0022(2) 0.0229(7) Uani 1 1 d . . . H62 H 0.6584 0.5318 -0.0297 0.027 Uiso 1 1 calc R . . C81 C 0.8128(3) 0.7907(2) 0.16622(19) 0.0216(7) Uani 1 1 d . . . H81 H 0.8207 0.7347 0.1958 0.026 Uiso 1 1 calc R . . C65 C 0.8291(2) 0.5724(2) 0.1470(2) 0.0205(7) Uani 1 1 d . . . H65 H 0.8740 0.5671 0.1011 0.025 Uiso 1 1 calc R . . C96 C 0.6374(3) 0.8280(2) -0.04010(19) 0.0210(7) Uani 1 1 d . . . H96 H 0.6218 0.7772 -0.0407 0.025 Uiso 1 1 calc R . . C51 C 0.9730(3) 0.6559(2) -0.0758(2) 0.0220(7) Uani 1 1 d . . . H51 H 1.0106 0.6231 -0.1113 0.026 Uiso 1 1 calc R . . C50 C 1.0049(3) 0.7109(2) -0.0535(2) 0.0224(7) Uani 1 1 d . . . H50 H 1.0677 0.7232 -0.0713 0.027 Uiso 1 1 calc R . . C63 C 0.5585(3) 0.5883(3) 0.0553(2) 0.0266(8) Uani 1 1 d . . . H63 H 0.5009 0.5687 0.0665 0.032 Uiso 1 1 calc R . . N2 N 0.6505(2) 0.78311(19) 0.55021(16) 0.0213(6) Uani 1 1 d . . . C53 C 0.8099(3) 0.6122(2) -0.03818(19) 0.0194(7) Uani 1 1 d . . . C52 C 0.8724(2) 0.6582(2) -0.03473(19) 0.0186(7) Uani 1 1 d . . . N3 N 0.8096(2) 0.65220(19) 0.53034(16) 0.0209(6) Uani 1 1 d . . . C21 C 0.7612(3) 0.5420(2) 0.64388(19) 0.0205(7) Uani 1 1 d . . . C22 C 0.7648(3) 0.4462(2) 0.67524(19) 0.0211(7) Uani 1 1 d . . . C16 C 0.5677(3) 0.7571(2) 0.5940(2) 0.0258(8) Uani 1 1 d . . . H16 H 0.5618 0.7194 0.6397 0.031 Uiso 1 1 calc R . . C28 C 0.8575(3) 0.3889(2) 0.6669(2) 0.0245(8) Uani 1 1 d . . . H28 H 0.9147 0.4108 0.6420 0.029 Uiso 1 1 calc R . . C23 C 0.6799(3) 0.4126(2) 0.7123(2) 0.0251(8) Uani 1 1 d . . . H23 H 0.6179 0.4504 0.7186 0.030 Uiso 1 1 calc R . . C94 C 0.6544(3) 0.9657(2) -0.07130(19) 0.0220(7) Uani 1 1 d . . . H94 H 0.6540 1.0241 -0.0946 0.026 Uiso 1 1 calc R . . C60 C 0.8920(3) 0.4641(2) -0.0659(2) 0.0239(8) Uani 1 1 d . . . H60 H 0.8852 0.4426 -0.0162 0.029 Uiso 1 1 calc R . . C75 C 0.6100(3) 0.6278(2) 0.4666(2) 0.0271(8) Uani 1 1 d . . . H75 H 0.6509 0.6249 0.4935 0.032 Uiso 1 1 calc R . . C76 C 0.6427(3) 0.6493(2) 0.3906(2) 0.0230(7) Uani 1 1 d . . . H76 H 0.7059 0.6602 0.3666 0.028 Uiso 1 1 calc R . . C69 C 0.6178(3) 0.6773(2) 0.26837(19) 0.0184(7) Uani 1 1 d . . . C54 C 0.8546(2) 0.5523(2) -0.09144(19) 0.0191(7) Uani 1 1 d . . . C78 C 0.4758(3) 0.8091(2) 0.2633(2) 0.0203(7) Uani 1 1 d . . . H78 H 0.4434 0.8064 0.3131 0.024 Uiso 1 1 calc R . . C55 C 0.8648(3) 0.5834(2) -0.1657(2) 0.0247(8) Uani 1 1 d . . . H55 H 0.8400 0.6423 -0.1830 0.030 Uiso 1 1 calc R . . C70 C 0.5810(3) 0.6547(2) 0.34983(19) 0.0202(7) Uani 1 1 d . . . C80 C 0.5186(3) 0.8494(2) 0.1412(2) 0.0205(7) Uani 1 1 d . . . H80 H 0.5170 0.8808 0.0944 0.025 Uiso 1 1 calc R . . C30 C 0.6764(3) 0.5777(3) 0.7691(2) 0.0241(8) Uani 1 1 d . . . H30 H 0.6713 0.5220 0.7980 0.029 Uiso 1 1 calc R . . C73 C 0.5163(3) 0.6108(2) 0.5020(2) 0.0279(8) Uani 1 1 d . . . C31 C 0.6424(3) 0.6547(3) 0.7926(2) 0.0257(8) Uani 1 1 d . . . H31 H 0.6092 0.6616 0.8405 0.031 Uiso 1 1 calc R . . C95 C 0.6216(3) 0.9085(2) -0.0894(2) 0.0223(7) Uani 1 1 d . . . H95 H 0.5939 0.9203 -0.1270 0.027 Uiso 1 1 calc R . . C64 C 0.5730(3) 0.6449(2) 0.0900(2) 0.0238(8) Uani 1 1 d . . . H64 H 0.5252 0.6677 0.1289 0.029 Uiso 1 1 calc R . . C46 C 0.7277(3) 0.9569(2) 0.6763(2) 0.0264(8) Uani 1 1 d . . . H46 H 0.7417 0.9841 0.7050 0.032 Uiso 1 1 calc R . . C18 C 0.8682(3) 0.5653(2) 0.4479(2) 0.0263(8) Uani 1 1 d . . . H18 H 0.8955 0.5479 0.4033 0.032 Uiso 1 1 calc R . . C15 C 0.4900(3) 0.7937(3) 0.5622(2) 0.0283(8) Uani 1 1 d . . . H15 H 0.4255 0.7850 0.5825 0.034 Uiso 1 1 calc R . . C34 C 1.0490(3) 0.6362(3) 0.6082(2) 0.0284(8) Uani 1 1 d . . . H34 H 1.1077 0.5939 0.6025 0.034 Uiso 1 1 calc R . . C33 C 0.9732(3) 0.6470(2) 0.5779(2) 0.0251(8) Uani 1 1 d . . . H33 H 0.9742 0.6118 0.5487 0.030 Uiso 1 1 calc R . . C20 C 0.8015(3) 0.5671(2) 0.5675(2) 0.0223(7) Uani 1 1 d . . . C14 C 0.5284(3) 0.8448(3) 0.4953(2) 0.0277(8) Uani 1 1 d . . . H14 H 0.4945 0.8779 0.4617 0.033 Uiso 1 1 calc R . . C38 C 0.9083(3) 0.8520(2) 0.7157(2) 0.0229(7) Uani 1 1 d . . . C59 C 0.9393(3) 0.4084(2) -0.1142(2) 0.0241(8) Uani 1 1 d . . . H59 H 0.9639 0.3494 -0.0969 0.029 Uiso 1 1 calc R . . C19 C 0.8377(3) 0.5127(2) 0.5162(2) 0.0239(8) Uani 1 1 d . . . H19 H 0.8404 0.4529 0.5266 0.029 Uiso 1 1 calc R . . C45 C 0.7841(3) 0.8772(2) 0.65280(19) 0.0225(7) Uani 1 1 d . . . C39 C 0.8545(3) 0.8461(2) 0.7894(2) 0.0235(8) Uani 1 1 d . . . H39 H 0.7947 0.8281 0.8072 0.028 Uiso 1 1 calc R . . C24 C 0.6866(3) 0.3237(3) 0.7399(2) 0.0276(8) Uani 1 1 d . . . H24 H 0.6295 0.3015 0.7638 0.033 Uiso 1 1 calc R . . C48 C 0.6580(3) 0.9232(2) 0.6092(2) 0.0265(8) Uani 1 1 d . . . H48 H 0.6136 0.9269 0.5849 0.032 Uiso 1 1 calc R . . C47 C 0.6493(3) 0.9854(3) 0.6484(2) 0.0307(9) Uani 1 1 d . . . H47 H 0.5999 1.0358 0.6542 0.037 Uiso 1 1 calc R . . C71 C 0.4864(3) 0.6383(2) 0.3866(2) 0.0254(8) Uani 1 1 d . . . H71 H 0.4447 0.6422 0.3600 0.031 Uiso 1 1 calc R . . C66 C 0.8330(3) 0.5099(2) 0.2121(2) 0.0229(7) Uani 1 1 d . . . H66 H 0.8796 0.4575 0.2168 0.027 Uiso 1 1 calc R . . C37 C 0.8709(3) 0.8258(2) 0.66686(19) 0.0215(7) Uani 1 1 d . . . C27 C 0.8649(3) 0.3000(2) 0.6955(2) 0.0270(8) Uani 1 1 d . . . H27 H 0.9268 0.2624 0.6904 0.032 Uiso 1 1 calc R . . C35 C 1.0194(3) 0.7005(2) 0.6485(2) 0.0252(8) Uani 1 1 d . . . H35 H 1.0535 0.7092 0.6758 0.030 Uiso 1 1 calc R . . C2 C 0.9541(3) 0.8846(3) 0.3833(2) 0.0299(9) Uani 1 1 d . . . H2 H 1.0145 0.8999 0.3553 0.036 Uiso 1 1 calc R . . C92 C 0.8227(3) 1.0772(3) -0.0306(2) 0.0289(8) Uani 1 1 d . . . H92 H 0.8827 1.0370 -0.0330 0.035 Uiso 1 1 calc R . . C6 C 0.6632(3) 0.9370(2) 0.3651(2) 0.0246(8) Uani 1 1 d . . . C93 C 0.6896(2) 0.9193(2) -0.00976(19) 0.0193(7) Uani 1 1 d . . . C86 C 0.7345(3) 1.0480(2) -0.0003(2) 0.0222(7) Uani 1 1 d . . . C25 C 0.7801(3) 0.2669(2) 0.7315(2) 0.0268(8) Uani 1 1 d . . . C41 C 0.9780(3) 0.8940(2) 0.8097(2) 0.0268(8) Uani 1 1 d . . . C79 C 0.4476(3) 0.8694(2) 0.2063(2) 0.0215(7) Uani 1 1 d . . . H79 H 0.3919 0.9150 0.2101 0.026 Uiso 1 1 calc R . . C85 C 0.7323(2) 0.9523(2) 0.0258(2) 0.0199(7) Uani 1 1 d . . . C1 C 0.9318(3) 0.8326(2) 0.4547(2) 0.0278(8) Uani 1 1 d . . . H1 H 0.9766 0.8083 0.4817 0.033 Uiso 1 1 calc R . . C87 C 0.6450(3) 1.1085(2) 0.0043(2) 0.0256(8) Uani 1 1 d . . . H87 H 0.5860 1.0890 0.0249 0.031 Uiso 1 1 calc R . . C32 C 0.6673(3) 0.7216(2) 0.7305(2) 0.0252(8) Uani 1 1 d . . . H32 H 0.6524 0.7808 0.7314 0.030 Uiso 1 1 calc R . . C3 C 0.8691(3) 0.9081(2) 0.3633(2) 0.0276(8) Uani 1 1 d . . . H3 H 0.8609 0.9424 0.3188 0.033 Uiso 1 1 calc R . . C17 C 0.8498(3) 0.6505(2) 0.4590(2) 0.0243(8) Uani 1 1 d . . . H17 H 0.8637 0.6992 0.4218 0.029 Uiso 1 1 calc R . . C74 C 0.4834(4) 0.5861(3) 0.5814(2) 0.0368(10) Uani 1 1 d . . . C36 C 0.9264(3) 0.7506(2) 0.63965(19) 0.0225(7) Uani 1 1 d . . . C68 C 0.7037(3) 0.6232(2) 0.23407(19) 0.0185(7) Uani 1 1 d . . . C67 C 0.7549(3) 0.5408(2) 0.2675(2) 0.0209(7) Uani 1 1 d . . . H67 H 0.7384 0.5136 0.3169 0.025 Uiso 1 1 calc R . . C44 C 0.9964(3) 0.8803(3) 0.6897(2) 0.0313(9) Uani 1 1 d . . . H44 H 1.0322 0.8856 0.6403 0.038 Uiso 1 1 calc R . . C12 C 0.6405(3) 0.9047(3) 0.3181(2) 0.0279(8) Uani 1 1 d . . . H12 H 0.6476 0.8445 0.3249 0.034 Uiso 1 1 calc R . . C84 C 0.7699(3) 0.9036(2) 0.0836(2) 0.0207(7) Uani 1 1 d . . . C13 C 0.6290(3) 0.8375(2) 0.4870(2) 0.0229(7) Uani 1 1 d . . . C40 C 0.8893(3) 0.8669(2) 0.8365(2) 0.0265(8) Uani 1 1 d . . . H40 H 0.8532 0.8627 0.8858 0.032 Uiso 1 1 calc R . . C82 C 0.8483(3) 0.8604(2) 0.1697(2) 0.0255(8) Uani 1 1 d . . . H82 H 0.8836 0.8583 0.2004 0.031 Uiso 1 1 calc R . . N7 N 0.5138(3) 1.1606(2) 0.15559(19) 0.0347(8) Uani 1 1 d . . . C9 C 0.5937(3) 1.0509(3) 0.2521(2) 0.0263(8) Uani 1 1 d . . . C88 C 0.6426(3) 1.1974(2) -0.0212(2) 0.0263(8) Uani 1 1 d . . . H88 H 0.5824 1.2377 -0.0173 0.032 Uiso 1 1 calc R . . C10 C 0.5507(3) 1.1115(3) 0.1967(2) 0.0294(9) Uani 1 1 d . . . C11 C 0.6073(3) 0.9614(3) 0.2608(2) 0.0279(8) Uani 1 1 d . . . H11 H 0.5941 0.9394 0.2283 0.033 Uiso 1 1 calc R . . C58 C 1.0065(3) 0.3825(3) -0.2379(2) 0.0262(8) Uani 1 1 d . . . C91 C 0.8219(3) 1.1657(3) -0.0572(2) 0.0295(9) Uani 1 1 d . . . H91 H 0.8810 1.1850 -0.0778 0.035 Uiso 1 1 calc R . . C57 C 0.9502(3) 0.4401(2) -0.1884(2) 0.0210(7) Uani 1 1 d . . . C89 C 0.7314(3) 1.2258(2) -0.0529(2) 0.0275(8) Uani 1 1 d . . . C90 C 0.7263(3) 1.3187(3) -0.0801(2) 0.0322(9) Uani 1 1 d . . . C83 C 0.8202(3) 0.9314(2) 0.1187(2) 0.0245(8) Uani 1 1 d . . . H83 H 0.8318 0.9873 0.1089 0.029 Uiso 1 1 calc R . . C8 C 0.6180(4) 1.0843(3) 0.2981(2) 0.0350(10) Uani 1 1 d . . . H8 H 0.6110 1.1444 0.2911 0.042 Uiso 1 1 calc R . . N17 N 0.4580(4) 0.5644(3) 0.6438(2) 0.0517(11) Uani 1 1 d . . . C72 C 0.4539(3) 0.6162(3) 0.4625(2) 0.0301(9) Uani 1 1 d . . . H72 H 0.3908 0.6052 0.4869 0.036 Uiso 1 1 calc R . . N16 N 1.0542(3) 0.3354(2) -0.27628(18) 0.0330(8) Uani 1 1 d . . . N18 N 0.7182(3) 1.3930(2) -0.1015(2) 0.0403(9) Uani 1 1 d . . . N8 N 0.7990(3) 0.0988(2) 0.7784(3) 0.0484(11) Uani 1 1 d . . . N9 N 1.0453(3) 0.9274(3) 0.8992(3) 0.0473(10) Uani 1 1 d . . . C26 C 0.7888(3) 0.1733(3) 0.7592(3) 0.0336(9) Uani 1 1 d . . . C7 C 0.6526(4) 1.0274(3) 0.3543(2) 0.0361(10) Uani 1 1 d . . . H7 H 0.6690 1.0493 0.3852 0.043 Uiso 1 1 calc R . . C56 C 0.9113(3) 0.5279(3) -0.2141(2) 0.0269(8) Uani 1 1 d . . . H56 H 0.9167 0.5490 -0.2636 0.032 Uiso 1 1 calc R . . C43 C 1.0317(3) 0.9009(3) 0.7362(2) 0.0324(9) Uani 1 1 d . . . H43 H 1.0912 0.9194 0.7183 0.039 Uiso 1 1 calc R . . C42 C 1.0153(3) 0.9131(3) 0.8593(3) 0.0357(10) Uani 1 1 d . . . Cl1 Cl 0.42307(10) 0.66147(11) 0.78376(8) 0.0588(4) Uani 1 1 d . . . Cl3 Cl 0.24060(14) 0.72049(10) 0.74496(11) 0.0767(5) Uani 1 1 d . . . C97 C 0.3161(3) 0.6323(3) 0.7886(3) 0.0402(10) Uani 1 1 d . . . H97 H 0.3366 0.5845 0.7627 0.048 Uiso 1 1 calc R . . C98 C 0.8047(11) 0.1586(10) 0.5153(6) 0.229(10) Uani 1 1 d . . . H98 H 0.8567 0.1899 0.4822 0.275 Uiso 1 1 calc R . . C5 C 0.6982(3) 0.8778(2) 0.4279(2) 0.0227(7) Uani 1 1 d . . . Cl4 Cl 0.88789(15) 0.06304(13) 0.51753(11) 0.1001(8) Uani 1 1 d . . . Cl6 Cl 0.78459(14) 0.21264(17) 0.57946(11) 0.0954(7) Uani 1 1 d . . . Cl5 Cl 0.7422(2) 0.1971(2) 0.45696(18) 0.1486(13) 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 Cl2 0.0451(7) 0.0686(9) 0.0410(7) -0.0055(6) -0.0030(5) -0.0198(6) Co1 0.0214(2) 0.0155(2) 0.0176(2) -0.00587(18) -0.00371(19) 0.00367(18) N6 0.0240(15) 0.0167(14) 0.0213(15) -0.0064(12) -0.0040(12) 0.0032(12) N1 0.0209(15) 0.0174(14) 0.0199(15) -0.0053(12) -0.0030(12) 0.0028(12) N4 0.0232(15) 0.0179(15) 0.0202(15) -0.0065(12) -0.0046(12) 0.0023(12) N5 0.0246(16) 0.0172(14) 0.0197(15) -0.0073(12) -0.0040(12) 0.0043(12) Co2 0.0138(2) 0.0145(2) 0.0169(2) -0.00416(17) -0.00575(17) 0.00100(17) C29 0.0196(17) 0.0185(17) 0.0197(17) -0.0030(14) -0.0072(14) 0.0010(13) C4 0.0297(19) 0.0150(16) 0.0208(18) -0.0062(14) -0.0058(15) 0.0014(14) N15 0.0135(13) 0.0187(14) 0.0179(14) -0.0041(11) -0.0053(11) 0.0000(11) N12 0.0158(13) 0.0154(14) 0.0192(14) -0.0044(11) -0.0049(11) -0.0007(11) N10 0.0157(13) 0.0163(14) 0.0201(14) -0.0034(11) -0.0072(11) -0.0005(11) N13 0.0166(14) 0.0171(14) 0.0208(15) -0.0053(12) -0.0069(12) 0.0009(11) N14 0.0182(14) 0.0149(14) 0.0214(15) -0.0053(11) -0.0085(12) 0.0019(11) N11 0.0139(13) 0.0194(14) 0.0170(14) -0.0049(11) -0.0037(11) -0.0008(11) C77 0.0159(16) 0.0156(16) 0.0198(17) -0.0061(13) -0.0045(13) -0.0006(13) C61 0.0187(16) 0.0172(16) 0.0219(17) -0.0050(14) -0.0090(14) 0.0011(13) C49 0.0205(17) 0.0184(17) 0.0206(17) -0.0025(13) -0.0085(14) -0.0023(13) C62 0.0233(18) 0.0194(17) 0.0262(19) -0.0074(15) -0.0077(15) -0.0022(14) C81 0.0219(17) 0.0212(17) 0.0202(17) -0.0035(14) -0.0094(14) 0.0005(14) C65 0.0145(16) 0.0204(17) 0.0233(18) -0.0076(14) -0.0034(14) 0.0009(13) C96 0.0172(16) 0.0225(18) 0.0226(18) -0.0070(14) -0.0062(14) -0.0008(14) C51 0.0192(17) 0.0211(17) 0.0221(18) -0.0050(14) -0.0054(14) 0.0001(14) C50 0.0165(16) 0.0249(18) 0.0223(18) -0.0026(14) -0.0047(14) -0.0036(14) C63 0.0183(17) 0.0257(19) 0.039(2) -0.0099(17) -0.0090(16) -0.0059(15) N2 0.0217(15) 0.0160(14) 0.0200(15) -0.0057(12) -0.0026(12) 0.0020(12) C53 0.0209(17) 0.0164(16) 0.0178(17) -0.0033(13) -0.0077(14) 0.0025(13) C52 0.0175(16) 0.0160(16) 0.0196(17) -0.0044(13) -0.0069(13) 0.0024(13) N3 0.0214(15) 0.0172(14) 0.0193(15) -0.0061(12) -0.0051(12) 0.0036(12) C21 0.0171(16) 0.0197(17) 0.0212(17) -0.0046(14) -0.0070(14) 0.0029(13) C22 0.0233(18) 0.0184(17) 0.0178(17) -0.0037(13) -0.0069(14) 0.0019(14) C16 0.0266(19) 0.0205(18) 0.0254(19) -0.0085(15) -0.0030(15) -0.0003(15) C28 0.0207(18) 0.0223(18) 0.0273(19) -0.0029(15) -0.0073(15) -0.0021(14) C23 0.0209(18) 0.0228(18) 0.030(2) -0.0106(15) -0.0085(15) 0.0043(14) C94 0.0198(17) 0.0219(18) 0.0190(17) 0.0004(14) -0.0064(14) -0.0011(14) C60 0.0250(18) 0.0247(19) 0.0178(17) -0.0043(14) -0.0070(15) 0.0011(15) C75 0.036(2) 0.0208(18) 0.0212(18) -0.0066(15) -0.0102(16) 0.0021(16) C76 0.0235(18) 0.0207(18) 0.0206(18) -0.0057(14) -0.0038(14) -0.0008(14) C69 0.0206(17) 0.0152(16) 0.0212(17) -0.0060(13) -0.0072(14) -0.0031(13) C54 0.0149(16) 0.0197(17) 0.0235(18) -0.0082(14) -0.0059(14) -0.0011(13) C78 0.0192(17) 0.0166(16) 0.0233(18) -0.0077(14) -0.0050(14) 0.0007(13) C55 0.0284(19) 0.0184(17) 0.0257(19) -0.0049(15) -0.0121(16) 0.0026(15) C70 0.0220(17) 0.0146(16) 0.0187(17) -0.0036(13) -0.0039(14) 0.0011(13) C80 0.0190(17) 0.0193(17) 0.0224(18) -0.0055(14) -0.0093(14) 0.0020(13) C30 0.0235(18) 0.0242(19) 0.0210(18) -0.0034(15) -0.0072(15) -0.0007(15) C73 0.036(2) 0.0195(18) 0.0222(19) -0.0065(15) -0.0029(16) -0.0018(16) C31 0.0267(19) 0.028(2) 0.0165(17) -0.0067(15) -0.0025(15) -0.0007(15) C95 0.0173(17) 0.0269(19) 0.0201(17) -0.0008(14) -0.0081(14) -0.0022(14) C64 0.0193(17) 0.0228(18) 0.0256(19) -0.0066(15) -0.0033(15) -0.0020(14) C46 0.0279(19) 0.0189(18) 0.027(2) -0.0097(15) -0.0057(16) 0.0037(15) C18 0.029(2) 0.0246(19) 0.0211(18) -0.0120(15) -0.0028(15) 0.0021(15) C15 0.0239(19) 0.0246(19) 0.033(2) -0.0112(16) -0.0043(16) 0.0000(15) C34 0.028(2) 0.0223(19) 0.028(2) -0.0089(16) -0.0078(16) 0.0063(15) C33 0.0266(19) 0.0190(18) 0.0248(19) -0.0087(15) -0.0074(15) 0.0058(14) C20 0.0209(17) 0.0196(17) 0.0231(18) -0.0082(14) -0.0070(14) 0.0046(14) C14 0.028(2) 0.0252(19) 0.029(2) -0.0106(16) -0.0107(16) 0.0030(15) C38 0.0262(18) 0.0155(16) 0.0219(18) -0.0049(14) -0.0052(15) 0.0013(14) C59 0.0251(18) 0.0182(17) 0.0258(19) -0.0048(14) -0.0100(15) 0.0029(14) C19 0.0260(19) 0.0169(17) 0.0251(19) -0.0080(14) -0.0069(15) 0.0034(14) C45 0.0257(18) 0.0183(17) 0.0184(17) -0.0066(14) -0.0034(14) 0.0013(14) C39 0.0199(17) 0.0231(18) 0.0247(19) -0.0053(15) -0.0062(15) -0.0008(14) C24 0.0223(18) 0.0252(19) 0.033(2) -0.0095(16) -0.0041(16) -0.0039(15) C48 0.028(2) 0.0184(18) 0.028(2) -0.0065(15) -0.0085(16) 0.0033(15) C47 0.031(2) 0.0207(19) 0.036(2) -0.0127(17) -0.0105(18) 0.0075(16) C71 0.0269(19) 0.0206(18) 0.0256(19) -0.0069(15) -0.0048(15) -0.0024(15) C66 0.0185(17) 0.0189(17) 0.0260(19) -0.0054(14) -0.0069(15) 0.0045(13) C37 0.0244(18) 0.0186(17) 0.0162(16) -0.0046(13) -0.0016(14) -0.0016(14) C27 0.0209(18) 0.0189(18) 0.036(2) -0.0052(16) -0.0098(16) 0.0033(14) C35 0.0240(18) 0.0226(18) 0.0250(19) -0.0071(15) -0.0069(15) 0.0023(15) C2 0.026(2) 0.0235(19) 0.030(2) -0.0023(16) -0.0008(16) -0.0036(15) C92 0.0220(19) 0.0225(19) 0.041(2) -0.0030(17) -0.0137(17) -0.0021(15) C6 0.0276(19) 0.0216(18) 0.0208(18) -0.0055(14) -0.0066(15) 0.0000(15) C93 0.0150(16) 0.0188(17) 0.0212(17) -0.0032(14) -0.0051(13) -0.0011(13) C86 0.0236(18) 0.0177(17) 0.0270(19) -0.0046(14) -0.0120(15) -0.0015(14) C25 0.0273(19) 0.0182(18) 0.030(2) -0.0027(15) -0.0082(16) -0.0011(15) C41 0.030(2) 0.0156(17) 0.036(2) -0.0074(15) -0.0131(17) -0.0011(15) C79 0.0174(16) 0.0181(17) 0.0267(19) -0.0082(14) -0.0060(14) 0.0020(13) C85 0.0149(16) 0.0157(16) 0.0249(18) -0.0046(14) -0.0058(14) 0.0026(13) C1 0.0259(19) 0.0217(19) 0.030(2) -0.0065(16) -0.0063(16) 0.0015(15) C87 0.0233(18) 0.0215(18) 0.030(2) -0.0031(15) -0.0090(16) -0.0038(15) C32 0.0289(19) 0.0210(18) 0.0215(18) -0.0088(15) -0.0050(15) 0.0018(15) C3 0.034(2) 0.0181(18) 0.0222(19) -0.0010(15) -0.0048(16) -0.0019(15) C17 0.0266(19) 0.0207(18) 0.0189(18) -0.0059(14) -0.0043(15) 0.0033(14) C74 0.051(3) 0.023(2) 0.028(2) -0.0082(17) 0.0000(19) -0.0078(19) C36 0.0232(18) 0.0195(17) 0.0190(17) -0.0039(14) -0.0057(14) 0.0024(14) C68 0.0198(17) 0.0160(16) 0.0184(17) -0.0030(13) -0.0082(14) 0.0003(13) C67 0.0218(17) 0.0158(16) 0.0214(17) -0.0023(13) -0.0072(14) 0.0006(13) C44 0.034(2) 0.025(2) 0.027(2) -0.0065(16) 0.0003(17) -0.0071(17) C12 0.033(2) 0.0198(18) 0.030(2) -0.0060(15) -0.0099(17) -0.0029(15) C84 0.0180(16) 0.0191(17) 0.0246(18) -0.0070(14) -0.0076(14) 0.0004(13) C13 0.0259(18) 0.0159(17) 0.0250(18) -0.0072(14) -0.0083(15) 0.0021(14) C40 0.0256(19) 0.0238(19) 0.0260(19) -0.0080(15) -0.0069(16) 0.0022(15) C82 0.0277(19) 0.0252(19) 0.029(2) -0.0086(16) -0.0166(16) -0.0002(15) N7 0.043(2) 0.0315(19) 0.0287(18) -0.0091(15) -0.0168(16) 0.0041(16) C9 0.0269(19) 0.0256(19) 0.0228(19) -0.0072(15) -0.0084(15) 0.0029(15) C88 0.0233(18) 0.0185(18) 0.034(2) -0.0055(15) -0.0117(16) 0.0029(14) C10 0.032(2) 0.027(2) 0.028(2) -0.0122(17) -0.0083(17) 0.0013(16) C11 0.033(2) 0.0253(19) 0.027(2) -0.0084(16) -0.0108(17) -0.0038(16) C58 0.0263(19) 0.030(2) 0.0235(19) -0.0072(16) -0.0129(16) 0.0005(16) C91 0.0248(19) 0.0225(19) 0.040(2) -0.0025(17) -0.0110(17) -0.0066(15) C57 0.0179(16) 0.0244(18) 0.0211(17) -0.0099(14) -0.0059(14) 0.0003(14) C89 0.032(2) 0.0160(17) 0.034(2) 0.0000(15) -0.0147(17) -0.0032(15) C90 0.029(2) 0.026(2) 0.042(2) -0.0012(18) -0.0152(18) -0.0062(16) C83 0.0238(18) 0.0216(18) 0.030(2) -0.0078(15) -0.0103(16) -0.0031(14) C8 0.056(3) 0.0176(19) 0.032(2) -0.0077(16) -0.021(2) 0.0040(18) N17 0.078(3) 0.040(2) 0.027(2) -0.0099(17) 0.004(2) -0.019(2) C72 0.027(2) 0.026(2) 0.028(2) -0.0077(16) 0.0030(16) -0.0039(16) N16 0.0356(19) 0.0356(19) 0.0260(17) -0.0139(15) -0.0132(15) 0.0072(15) N18 0.042(2) 0.0223(18) 0.055(2) 0.0022(17) -0.0222(19) -0.0065(16) N8 0.034(2) 0.023(2) 0.073(3) -0.0035(19) -0.008(2) -0.0020(16) N9 0.047(2) 0.043(2) 0.067(3) -0.018(2) -0.026(2) -0.0132(19) C26 0.023(2) 0.025(2) 0.044(2) -0.0067(18) -0.0038(18) -0.0023(16) C7 0.060(3) 0.0202(19) 0.032(2) -0.0084(17) -0.024(2) 0.0018(19) C56 0.032(2) 0.027(2) 0.0201(18) -0.0050(15) -0.0113(16) -0.0001(16) C43 0.028(2) 0.0227(19) 0.043(2) -0.0061(17) -0.0044(18) -0.0095(16) C42 0.031(2) 0.026(2) 0.052(3) -0.0108(19) -0.013(2) -0.0064(17) Cl1 0.0482(7) 0.0823(10) 0.0476(7) -0.0029(7) -0.0122(6) -0.0301(7) Cl3 0.0894(12) 0.0522(9) 0.0941(12) 0.0136(8) -0.0615(11) -0.0098(8) C97 0.034(2) 0.042(3) 0.041(3) -0.003(2) -0.014(2) -0.007(2) C98 0.261(16) 0.263(16) 0.132(9) -0.141(11) -0.145(11) 0.196(14) C5 0.0293(19) 0.0139(16) 0.0211(18) -0.0063(14) -0.0086(15) 0.0044(14) Cl4 0.0878(13) 0.0747(12) 0.0698(11) 0.0121(9) 0.0151(10) 0.0037(10) Cl6 0.0593(10) 0.153(2) 0.0747(12) -0.0469(13) -0.0235(9) 0.0033(11) Cl5 0.1182(19) 0.193(3) 0.188(3) -0.110(2) -0.119(2) 0.0496(19) _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 Cl2 C97 1.724(5) . ? Co1 N3 1.934(3) . ? Co1 N1 1.940(3) . ? Co1 N5 1.943(3) . ? Co1 N4 1.943(3) . ? Co1 N6 1.943(3) . ? Co1 N2 1.944(3) . ? N6 C48 1.332(5) . ? N6 C45 1.397(5) . ? N1 C1 1.332(5) . ? N1 C4 1.392(5) . ? N4 C32 1.342(5) . ? N4 C29 1.395(5) . ? N5 C33 1.348(4) . ? N5 C36 1.390(5) . ? Co2 N15 1.937(3) . ? Co2 N14 1.941(3) . ? Co2 N11 1.942(3) . ? Co2 N13 1.945(3) . ? Co2 N12 1.945(3) . ? Co2 N10 1.947(3) . ? C29 C21 1.389(5) . ? C29 C30 1.425(5) . ? C4 C5 1.389(5) . ? C4 C3 1.424(5) . ? N15 C96 1.338(4) . ? N15 C93 1.390(4) . ? N12 C65 1.335(4) . ? N12 C68 1.393(4) . ? N10 C49 1.336(5) . ? N10 C52 1.397(4) . ? N13 C80 1.348(4) . ? N13 C77 1.399(4) . ? N14 C81 1.338(4) . ? N14 C84 1.396(4) . ? N11 C64 1.331(5) . ? N11 C61 1.398(4) . ? C77 C69 1.396(5) . ? C77 C78 1.426(5) . ? C61 C53 1.390(5) . ? C61 C62 1.429(5) . ? C49 C50 1.404(5) . ? C62 C63 1.365(5) . ? C81 C82 1.420(5) . ? C65 C66 1.406(5) . ? C96 C95 1.404(5) . ? C51 C50 1.370(5) . ? C51 C52 1.415(5) . ? C63 C64 1.412(5) . ? N2 C16 1.330(5) . ? N2 C13 1.396(5) . ? C53 C52 1.387(5) . ? C53 C54 1.504(5) . ? N3 C17 1.339(5) . ? N3 C20 1.387(5) . ? C21 C20 1.405(5) . ? C21 C22 1.497(5) . ? C22 C23 1.390(5) . ? C22 C28 1.399(5) . ? C16 C15 1.409(6) . ? C28 C27 1.381(5) . ? C23 C24 1.379(5) . ? C94 C95 1.358(5) . ? C94 C93 1.429(5) . ? C60 C59 1.383(5) . ? C60 C54 1.392(5) . ? C75 C73 1.383(6) . ? C75 C76 1.387(5) . ? C76 C70 1.400(5) . ? C69 C68 1.391(5) . ? C69 C70 1.488(5) . ? C54 C55 1.388(5) . ? C78 C79 1.372(5) . ? C55 C56 1.381(5) . ? C70 C71 1.394(5) . ? C80 C79 1.405(5) . ? C30 C31 1.366(5) . ? C73 C72 1.388(6) . ? C73 C74 1.450(6) . ? C31 C32 1.408(5) . ? C46 C47 1.369(6) . ? C46 C45 1.432(5) . ? C18 C19 1.378(5) . ? C18 C17 1.407(5) . ? C15 C14 1.372(6) . ? C34 C35 1.387(5) . ? C34 C33 1.404(6) . ? C20 C19 1.412(5) . ? C14 C13 1.413(5) . ? C38 C44 1.386(6) . ? C38 C39 1.391(5) . ? C38 C37 1.494(5) . ? C59 C57 1.385(5) . ? C45 C37 1.384(5) . ? C39 C40 1.387(5) . ? C24 C25 1.403(5) . ? C48 C47 1.412(5) . ? C71 C72 1.387(5) . ? C66 C67 1.372(5) . ? C37 C36 1.399(5) . ? C27 C25 1.383(6) . ? C35 C36 1.422(5) . ? C2 C3 1.372(6) . ? C2 C1 1.407(6) . ? C92 C91 1.382(5) . ? C92 C86 1.391(5) . ? C6 C12 1.382(5) . ? C6 C7 1.397(5) . ? C6 C5 1.495(5) . ? C93 C85 1.400(5) . ? C86 C87 1.389(5) . ? C86 C85 1.502(5) . ? C25 C26 1.448(5) . ? C41 C40 1.382(6) . ? C41 C43 1.386(6) . ? C41 C42 1.440(6) . ? C85 C84 1.392(5) . ? C87 C88 1.385(5) . ? C74 N17 1.142(6) . ? C68 C67 1.436(5) . ? C44 C43 1.378(6) . ? C12 C11 1.388(6) . ? C84 C83 1.426(5) . ? C13 C5 1.396(5) . ? C82 C83 1.370(5) . ? N7 C10 1.137(5) . ? C9 C11 1.382(5) . ? C9 C8 1.391(6) . ? C9 C10 1.450(5) . ? C88 C89 1.392(6) . ? C58 N16 1.148(5) . ? C58 C57 1.435(5) . ? C91 C89 1.397(5) . ? C57 C56 1.391(5) . ? C89 C90 1.442(5) . ? C90 N18 1.146(5) . ? C8 C7 1.381(6) . ? N8 C26 1.143(5) . ? N9 C42 1.150(6) . ? Cl1 C97 1.751(5) . ? Cl3 C97 1.758(5) . ? C98 Cl5 1.619(9) . ? C98 Cl6 1.663(10) . ? C98 Cl4 1.677(9) . ? 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 N3 Co1 N1 91.29(13) . . ? N3 Co1 N5 89.80(13) . . ? N1 Co1 N5 90.26(13) . . ? N3 Co1 N4 92.08(13) . . ? N1 Co1 N4 175.65(13) . . ? N5 Co1 N4 87.00(13) . . ? N3 Co1 N6 177.33(13) . . ? N1 Co1 N6 87.14(13) . . ? N5 Co1 N6 92.37(13) . . ? N4 Co1 N6 89.59(13) . . ? N3 Co1 N2 86.92(13) . . ? N1 Co1 N2 92.52(13) . . ? N5 Co1 N2 175.74(13) . . ? N4 Co1 N2 90.41(13) . . ? N6 Co1 N2 90.98(13) . . ? C48 N6 C45 106.5(3) . . ? C48 N6 Co1 126.9(3) . . ? C45 N6 Co1 126.3(2) . . ? C1 N1 C4 106.6(3) . . ? C1 N1 Co1 126.8(3) . . ? C4 N1 Co1 126.6(3) . . ? C32 N4 C29 106.1(3) . . ? C32 N4 Co1 126.8(3) . . ? C29 N4 Co1 127.0(2) . . ? C33 N5 C36 106.4(3) . . ? C33 N5 Co1 127.0(3) . . ? C36 N5 Co1 126.6(2) . . ? N15 Co2 N14 92.55(12) . . ? N15 Co2 N11 89.81(12) . . ? N14 Co2 N11 177.41(12) . . ? N15 Co2 N13 90.33(12) . . ? N14 Co2 N13 86.11(12) . . ? N11 Co2 N13 92.84(12) . . ? N15 Co2 N12 175.62(12) . . ? N14 Co2 N12 91.54(12) . . ? N11 Co2 N12 86.12(12) . . ? N13 Co2 N12 91.48(12) . . ? N15 Co2 N10 87.13(12) . . ? N14 Co2 N10 88.71(12) . . ? N11 Co2 N10 92.45(12) . . ? N13 Co2 N10 174.13(12) . . ? N12 Co2 N10 91.43(12) . . ? C21 C29 N4 123.8(3) . . ? C21 C29 C30 127.3(3) . . ? N4 C29 C30 108.8(3) . . ? C5 C4 N1 124.7(3) . . ? C5 C4 C3 126.9(4) . . ? N1 C4 C3 108.4(3) . . ? C96 N15 C93 106.4(3) . . ? C96 N15 Co2 127.2(2) . . ? C93 N15 Co2 126.5(2) . . ? C65 N12 C68 106.6(3) . . ? C65 N12 Co2 126.1(2) . . ? C68 N12 Co2 127.2(2) . . ? C49 N10 C52 106.2(3) . . ? C49 N10 Co2 126.9(2) . . ? C52 N10 Co2 126.8(2) . . ? C80 N13 C77 106.3(3) . . ? C80 N13 Co2 125.8(2) . . ? C77 N13 Co2 126.4(2) . . ? C81 N14 C84 106.5(3) . . ? C81 N14 Co2 125.9(2) . . ? C84 N14 Co2 127.4(2) . . ? C64 N11 C61 106.3(3) . . ? C64 N11 Co2 126.7(2) . . ? C61 N11 Co2 127.0(2) . . ? C69 C77 N13 123.9(3) . . ? C69 C77 C78 127.4(3) . . ? N13 C77 C78 108.7(3) . . ? C53 C61 N11 123.6(3) . . ? C53 C61 C62 127.7(3) . . ? N11 C61 C62 108.7(3) . . ? N10 C49 C50 111.5(3) . . ? C63 C62 C61 106.7(3) . . ? N14 C81 C82 111.4(3) . . ? N12 C65 C66 111.5(3) . . ? N15 C96 C95 111.5(3) . . ? C50 C51 C52 107.2(3) . . ? C51 C50 C49 106.4(3) . . ? C62 C63 C64 106.8(3) . . ? C16 N2 C13 106.5(3) . . ? C16 N2 Co1 126.2(3) . . ? C13 N2 Co1 127.3(2) . . ? C61 C53 C52 126.2(3) . . ? C61 C53 C54 117.5(3) . . ? C52 C53 C54 116.2(3) . . ? C53 C52 N10 123.8(3) . . ? C53 C52 C51 127.6(3) . . ? N10 C52 C51 108.5(3) . . ? C17 N3 C20 106.8(3) . . ? C17 N3 Co1 126.0(3) . . ? C20 N3 Co1 127.2(2) . . ? C29 C21 C20 125.0(3) . . ? C29 C21 C22 118.3(3) . . ? C20 C21 C22 116.8(3) . . ? C23 C22 C28 119.2(3) . . ? C23 C22 C21 122.6(3) . . ? C28 C22 C21 118.2(3) . . ? N2 C16 C15 111.4(4) . . ? C27 C28 C22 120.5(4) . . ? C24 C23 C22 120.6(3) . . ? C95 C94 C93 107.2(3) . . ? C59 C60 C54 120.1(3) . . ? C73 C75 C76 119.6(4) . . ? C75 C76 C70 120.4(4) . . ? C68 C69 C77 124.6(3) . . ? C68 C69 C70 117.4(3) . . ? C77 C69 C70 118.1(3) . . ? C55 C54 C60 119.3(3) . . ? C55 C54 C53 121.9(3) . . ? C60 C54 C53 118.7(3) . . ? C79 C78 C77 106.8(3) . . ? C56 C55 C54 120.7(3) . . ? C71 C70 C76 119.1(3) . . ? C71 C70 C69 121.3(3) . . ? C76 C70 C69 119.5(3) . . ? N13 C80 C79 111.1(3) . . ? C31 C30 C29 106.9(3) . . ? C75 C73 C72 120.8(4) . . ? C75 C73 C74 119.4(4) . . ? C72 C73 C74 119.8(4) . . ? C30 C31 C32 106.8(3) . . ? C94 C95 C96 106.7(3) . . ? N11 C64 C63 111.6(3) . . ? C47 C46 C45 106.8(3) . . ? C19 C18 C17 106.4(3) . . ? C14 C15 C16 106.3(4) . . ? C35 C34 C33 106.8(3) . . ? N5 C33 C34 111.1(3) . . ? N3 C20 C21 124.1(3) . . ? N3 C20 C19 108.9(3) . . ? C21 C20 C19 127.0(3) . . ? C15 C14 C13 107.2(4) . . ? C44 C38 C39 119.0(4) . . ? C44 C38 C37 121.7(3) . . ? C39 C38 C37 119.3(3) . . ? C60 C59 C57 120.2(3) . . ? C18 C19 C20 106.9(3) . . ? C37 C45 N6 124.2(3) . . ? C37 C45 C46 127.4(4) . . ? N6 C45 C46 108.4(3) . . ? C40 C39 C38 120.5(4) . . ? C23 C24 C25 119.6(4) . . ? N6 C48 C47 111.6(4) . . ? C46 C47 C48 106.6(3) . . ? C72 C71 C70 120.5(4) . . ? C67 C66 C65 106.9(3) . . ? C45 C37 C36 125.4(3) . . ? C45 C37 C38 117.6(3) . . ? C36 C37 C38 116.9(3) . . ? C28 C27 C25 120.0(3) . . ? C34 C35 C36 106.3(3) . . ? C3 C2 C1 106.3(4) . . ? C91 C92 C86 120.4(4) . . ? C12 C6 C7 119.4(4) . . ? C12 C6 C5 121.8(3) . . ? C7 C6 C5 118.8(3) . . ? N15 C93 C85 125.0(3) . . ? N15 C93 C94 108.3(3) . . ? C85 C93 C94 126.7(3) . . ? C87 C86 C92 119.6(3) . . ? C87 C86 C85 118.2(3) . . ? C92 C86 C85 122.2(3) . . ? C27 C25 C24 120.1(3) . . ? C27 C25 C26 119.4(3) . . ? C24 C25 C26 120.6(4) . . ? C40 C41 C43 120.3(4) . . ? C40 C41 C42 119.4(4) . . ? C43 C41 C42 120.3(4) . . ? C78 C79 C80 107.2(3) . . ? C84 C85 C93 124.8(3) . . ? C84 C85 C86 118.9(3) . . ? C93 C85 C86 116.3(3) . . ? N1 C1 C2 111.6(4) . . ? C88 C87 C86 120.8(4) . . ? N4 C32 C31 111.4(3) . . ? C2 C3 C4 107.1(3) . . ? N3 C17 C18 111.0(3) . . ? N17 C74 C73 178.1(4) . . ? N5 C36 C37 124.0(3) . . ? N5 C36 C35 109.3(3) . . ? C37 C36 C35 126.7(4) . . ? C69 C68 N12 124.3(3) . . ? C69 C68 C67 127.2(3) . . ? N12 C68 C67 108.5(3) . . ? C66 C67 C68 106.5(3) . . ? C43 C44 C38 120.8(4) . . ? C6 C12 C11 120.4(4) . . ? C85 C84 N14 123.7(3) . . ? C85 C84 C83 127.6(3) . . ? N14 C84 C83 108.7(3) . . ? N2 C13 C5 123.4(3) . . ? N2 C13 C14 108.5(3) . . ? C5 C13 C14 128.0(4) . . ? C41 C40 C39 119.6(4) . . ? C83 C82 C81 106.3(3) . . ? C11 C9 C8 120.4(4) . . ? C11 C9 C10 120.6(4) . . ? C8 C9 C10 119.0(4) . . ? C87 C88 C89 119.1(3) . . ? N7 C10 C9 177.0(4) . . ? C9 C11 C12 119.8(4) . . ? N16 C58 C57 177.4(4) . . ? C92 C91 C89 119.4(4) . . ? C59 C57 C56 120.0(3) . . ? C59 C57 C58 118.9(3) . . ? C56 C57 C58 121.1(3) . . ? C88 C89 C91 120.6(3) . . ? C88 C89 C90 117.7(3) . . ? C91 C89 C90 121.7(4) . . ? N18 C90 C89 177.2(4) . . ? C82 C83 C84 107.2(3) . . ? C7 C8 C9 119.5(4) . . ? C71 C72 C73 119.6(4) . . ? N8 C26 C25 177.1(5) . . ? C8 C7 C6 120.5(4) . . ? C55 C56 C57 119.7(3) . . ? C44 C43 C41 119.7(4) . . ? N9 C42 C41 179.3(5) . . ? Cl2 C97 Cl1 110.5(3) . . ? Cl2 C97 Cl3 111.5(3) . . ? Cl1 C97 Cl3 111.1(3) . . ? Cl5 C98 Cl6 119.9(6) . . ? Cl5 C98 Cl4 123.6(7) . . ? Cl6 C98 Cl4 116.5(5) . . ? C4 C5 C13 125.5(3) . . ? C4 C5 C6 117.2(3) . . ? C13 C5 C6 117.2(3) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 2.354 _refine_diff_density_min -1.568 _refine_diff_density_rms 0.109 data_MOF-Co/Ag-2 _database_code_depnum_ccdc_archive 'CCDC 281273' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63.44 H44.44 Ag Co F3 N9 O3 S' _chemical_formula_weight 1236.63 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M F432 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -y, -z' 'y, x, -z' '-x, y, -z' '-y, -x, -z' 'z, x, y' '-x, z, y' '-z, -x, y' 'x, -z, y' 'z, -x, -y' 'x, z, -y' '-z, x, -y' '-x, -z, -y' 'y, z, x' '-z, -y, -x' '-z, y, x' 'z, y, -x' 'z, -y, x' 'y, -z, -x' '-y, -z, x' '-y, z, -x' 'x, y+1/2, z+1/2' '-y, x+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'y, -x+1/2, z+1/2' 'x, -y+1/2, -z+1/2' 'y, x+1/2, -z+1/2' '-x, y+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'z, x+1/2, y+1/2' '-x, z+1/2, y+1/2' '-z, -x+1/2, y+1/2' 'x, -z+1/2, y+1/2' 'z, -x+1/2, -y+1/2' 'x, z+1/2, -y+1/2' '-z, x+1/2, -y+1/2' '-x, -z+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-z, -y+1/2, -x+1/2' '-z, y+1/2, x+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-y+1/2, x, z+1/2' '-x+1/2, -y, z+1/2' 'y+1/2, -x, z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x, -z+1/2' '-x+1/2, y, -z+1/2' '-y+1/2, -x, -z+1/2' 'z+1/2, x, y+1/2' '-x+1/2, z, y+1/2' '-z+1/2, -x, y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, -x, -y+1/2' 'x+1/2, z, -y+1/2' '-z+1/2, x, -y+1/2' '-x+1/2, -z, -y+1/2' 'y+1/2, z, x+1/2' '-z+1/2, -y, -x+1/2' '-z+1/2, y, x+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' '-y+1/2, z, -x+1/2' 'x+1/2, y+1/2, z' '-y+1/2, x+1/2, z' '-x+1/2, -y+1/2, z' 'y+1/2, -x+1/2, z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z' '-x+1/2, y+1/2, -z' '-y+1/2, -x+1/2, -z' 'z+1/2, x+1/2, y' '-x+1/2, z+1/2, y' '-z+1/2, -x+1/2, y' 'x+1/2, -z+1/2, y' 'z+1/2, -x+1/2, -y' 'x+1/2, z+1/2, -y' '-z+1/2, x+1/2, -y' '-x+1/2, -z+1/2, -y' 'y+1/2, z+1/2, x' '-z+1/2, -y+1/2, -x' '-z+1/2, y+1/2, x' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' '-y+1/2, z+1/2, -x' _cell_length_a 34.7494(14) _cell_length_b 34.7494(14) _cell_length_c 34.7494(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 41961(3) _cell_formula_units_Z 32 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 20130 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7403 _exptl_absorpt_correction_T_max 0.8694 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60529 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4039 _reflns_number_gt 3601 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+265.4330P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(5) _refine_ls_number_reflns 4039 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2320 _refine_ls_wR_factor_gt 0.2272 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 Ag1 Ag 0.10308(4) -0.10308(4) 0.10308(4) 0.1467(9) Uani 1 3 d S . . Co1 Co 0.135390(16) 0.135390(16) 0.364610(16) 0.0377(3) Uani 1 3 d S . . N1 N 0.17260(15) 0.11623(12) 0.32770(15) 0.0460(9) Uani 1 1 d . . . N2 N 0.09496(13) 0.10225(11) 0.34622(11) 0.0398(9) Uani 1 1 d . . . N3 N 0.1093(2) -0.0593(2) 0.1471(2) 0.095(3) Uani 1 1 d . . . C1 C 0.21072(19) 0.1248(2) 0.32688(17) 0.0628(17) Uani 1 1 d . . . H1 H 0.2231 0.1426 0.3436 0.075 Uiso 1 1 calc R . . C2 C 0.2296(2) 0.1033(2) 0.29754(19) 0.0679(19) Uani 1 1 d . . . H2 H 0.2559 0.1051 0.2903 0.081 Uiso 1 1 calc R . . C3 C 0.20161(17) 0.07915(19) 0.28147(17) 0.0554(15) Uani 1 1 d . . . H3 H 0.2055 0.0609 0.2615 0.066 Uiso 1 1 calc R . . C4 C 0.16620(18) 0.08703(18) 0.30063(14) 0.0503(13) Uani 1 1 d . . . C5 C 0.13095(16) 0.07044(13) 0.29349(14) 0.0393(10) Uani 1 1 d . . . C6 C 0.09678(15) 0.07790(13) 0.31356(12) 0.0352(9) Uani 1 1 d . . . C7 C 0.0602(2) 0.06060(16) 0.30813(14) 0.0504(12) Uani 1 1 d . . . H7 H 0.0535 0.0430 0.2883 0.061 Uiso 1 1 calc R . . C8 C 0.03578(16) 0.07395(15) 0.33707(17) 0.0469(12) Uani 1 1 d . . . H8 H 0.0096 0.0673 0.3413 0.056 Uiso 1 1 calc R . . C9 C 0.05868(13) 0.09951(16) 0.35850(15) 0.0408(10) Uani 1 1 d . . . H9 H 0.0491 0.1136 0.3799 0.049 Uiso 1 1 calc R . . C10 C 0.12866(18) 0.04199(15) 0.26102(16) 0.0487(13) Uani 1 1 d . . . C11 C 0.1148(3) 0.05271(18) 0.22576(18) 0.073(2) Uani 1 1 d . . . H11 H 0.1084 0.0790 0.2220 0.088 Uiso 1 1 calc R . . C12 C 0.1098(3) 0.0294(2) 0.19724(19) 0.073(2) Uani 1 1 d . . . H12 H 0.0990 0.0381 0.1737 0.087 Uiso 1 1 calc R . . C13 C 0.1210(2) -0.01031(17) 0.2019(2) 0.068(2) Uani 1 1 d . . . C14 C 0.1347(2) -0.02248(17) 0.2365(2) 0.0637(17) Uani 1 1 d . . . H14 H 0.1413 -0.0487 0.2403 0.076 Uiso 1 1 calc R . . C15 C 0.1390(2) 0.00453(19) 0.2666(2) 0.0626(16) Uani 1 1 d . . . H15 H 0.1491 -0.0034 0.2907 0.075 Uiso 1 1 calc R . . C16 C 0.1158(2) -0.0374(2) 0.1721(2) 0.075(2) 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 Ag1 0.1467(9) 0.1467(9) 0.1467(9) -0.1024(9) 0.1024(9) -0.1024(9) Co1 0.0377(3) 0.0377(3) 0.0377(3) 0.0032(2) 0.0032(2) -0.0032(2) N1 0.043(3) 0.052(2) 0.044(3) 0.000(2) 0.0124(16) -0.006(2) N2 0.045(2) 0.037(2) 0.0377(18) 0.0042(15) -0.0021(17) 0.0077(17) N3 0.091(5) 0.075(4) 0.119(6) -0.055(4) 0.062(4) -0.033(3) C1 0.058(4) 0.093(5) 0.037(3) 0.010(3) 0.017(3) -0.001(3) C2 0.057(4) 0.097(5) 0.049(3) -0.009(3) 0.024(3) 0.000(4) C3 0.052(3) 0.067(4) 0.046(3) 0.005(3) 0.022(3) 0.008(3) C4 0.058(3) 0.065(3) 0.028(2) 0.006(2) 0.011(2) 0.013(3) C5 0.055(3) 0.030(2) 0.032(2) 0.0085(17) 0.005(2) 0.000(2) C6 0.047(2) 0.0278(19) 0.031(2) 0.0011(16) 0.0020(18) 0.0026(17) C7 0.080(4) 0.027(2) 0.044(2) 0.001(2) -0.006(3) -0.003(2) C8 0.045(3) 0.041(3) 0.054(3) 0.002(2) -0.003(2) -0.005(2) C9 0.029(2) 0.051(3) 0.042(3) -0.006(2) 0.0002(18) -0.003(2) C10 0.062(3) 0.042(3) 0.042(3) -0.001(2) 0.022(2) -0.008(2) C11 0.135(7) 0.039(3) 0.046(3) 0.008(2) 0.020(4) -0.007(4) C12 0.117(7) 0.063(4) 0.038(3) 0.004(3) 0.013(4) 0.001(4) C13 0.079(4) 0.044(3) 0.081(5) -0.019(3) 0.031(4) -0.011(3) C14 0.070(4) 0.034(3) 0.087(5) 0.003(3) 0.005(4) 0.006(3) C15 0.084(4) 0.037(3) 0.067(3) 0.000(3) -0.005(3) -0.002(3) C16 0.076(5) 0.074(5) 0.074(5) -0.019(4) 0.035(4) -0.007(4) _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 Ag1 N3 2.170(6) 23 ? Ag1 N3 2.170(6) . ? Ag1 N3 2.170(6) 13 ? Co1 N2 1.926(4) 63 ? Co1 N2 1.926(4) . ? Co1 N2 1.926(4) 46 ? Co1 N1 1.939(4) 63 ? Co1 N1 1.939(4) . ? Co1 N1 1.939(4) 46 ? N1 C1 1.358(8) . ? N1 C4 1.401(8) . ? N2 C9 1.334(6) . ? N2 C6 1.417(6) . ? N3 C16 1.176(10) . ? C1 C2 1.423(9) . ? C1 H1 0.9500 . ? C2 C3 1.401(10) . ? C2 H2 0.9500 . ? C3 C4 1.426(8) . ? C3 H3 0.9500 . ? C4 C5 1.376(8) . ? C5 C6 1.401(7) . ? C5 C10 1.502(7) . ? C6 C7 1.419(8) . ? C7 C8 1.395(9) . ? C7 H7 0.9500 . ? C8 C9 1.406(7) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.364(8) . ? C10 C11 1.369(9) . ? C11 C12 1.293(10) . ? C11 H11 0.9500 . ? C12 C13 1.442(10) . ? C12 H12 0.9500 . ? C13 C14 1.358(11) . ? C13 C16 1.411(10) . ? C14 C15 1.413(10) . ? C14 H14 0.9500 . ? C15 H15 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 N3 Ag1 N3 119.65(6) 23 . ? N3 Ag1 N3 119.65(6) 23 13 ? N3 Ag1 N3 119.65(6) . 13 ? N2 Co1 N2 90.25(16) 63 . ? N2 Co1 N2 90.25(16) 63 46 ? N2 Co1 N2 90.24(16) . 46 ? N2 Co1 N1 93.5(2) 63 63 ? N2 Co1 N1 174.4(2) . 63 ? N2 Co1 N1 85.62(19) 46 63 ? N2 Co1 N1 85.62(19) 63 . ? N2 Co1 N1 93.5(2) . . ? N2 Co1 N1 174.4(2) 46 . ? N1 Co1 N1 90.87(17) 63 . ? N2 Co1 N1 174.4(2) 63 46 ? N2 Co1 N1 85.62(19) . 46 ? N2 Co1 N1 93.5(2) 46 46 ? N1 Co1 N1 90.86(17) 63 46 ? N1 Co1 N1 90.86(17) . 46 ? C1 N1 C4 107.4(5) . . ? C1 N1 Co1 126.1(4) . . ? C4 N1 Co1 125.9(4) . . ? C9 N2 C6 104.8(4) . . ? C9 N2 Co1 128.7(3) . . ? C6 N2 Co1 126.2(3) . . ? C16 N3 Ag1 173.5(9) . . ? N1 C1 C2 110.5(6) . . ? N1 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? C3 C2 C1 106.2(6) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 C4 107.3(6) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? C5 C4 N1 124.4(5) . . ? C5 C4 C3 127.1(6) . . ? N1 C4 C3 108.4(6) . . ? C4 C5 C6 125.9(5) . . ? C4 C5 C10 117.3(5) . . ? C6 C5 C10 116.8(5) . . ? C5 C6 N2 123.2(5) . . ? C5 C6 C7 127.9(5) . . ? N2 C6 C7 108.6(4) . . ? C8 C7 C6 107.9(4) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? C7 C8 C9 104.4(5) . . ? C7 C8 H8 127.8 . . ? C9 C8 H8 127.8 . . ? N2 C9 C8 114.2(5) . . ? N2 C9 H9 122.9 . . ? C8 C9 H9 122.9 . . ? C15 C10 C11 118.6(6) . . ? C15 C10 C5 120.5(6) . . ? C11 C10 C5 120.8(5) . . ? C12 C11 C10 124.3(7) . . ? C12 C11 H11 117.9 . . ? C10 C11 H11 117.9 . . ? C11 C12 C13 118.5(7) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C14 C13 C16 119.1(7) . . ? C14 C13 C12 119.5(6) . . ? C16 C13 C12 121.3(8) . . ? C13 C14 C15 119.0(6) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C10 C15 C14 120.1(6) . . ? C10 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? N3 C16 C13 176.2(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.271 _refine_diff_density_min -1.737 _refine_diff_density_rms 0.092