# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Jonathan Steed' 'Lucas Applegarth' 'Nigel Clark' 'Andres E. Goeta' 'Judith A.K. Howard' 'Andrew D.M. Parker' 'Ivana Radosavljevic-Evans' 'Christine Richardson' _publ_contact_author_name 'Jonathan Steed' _publ_contact_author_address ; Department of Chemistry University of Durham University Science Laboratories South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email JON.STEED@DUR.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Modular Nanometer-Scale Structuring of Gel Fibres by Sequential Self-Organization ; data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 281274' _audit_creation_date 05-15-02 _audit_creation_method CRYSTALS_ver_12-03-99 _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 43.826(4) _cell_angle_alpha 90 _cell_length_b 5.2608(5) _cell_angle_beta 90 _cell_length_c 14.0960(14) _cell_angle_gamma 90 _cell_volume 3250.0(5) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P m n 21 ' _space_group_name_Hall 'P 2ac -2' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,z x+1/2,-y,z+1/2 -x+1/2,-y,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Ag ' -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C28 H26 Ag1 Cl3 N8 O5.74 ' _chemical_formula_moiety ' C28 H26 Ag1 Cl3 N8 O5.74 ' _chemical_compound_source ; ? ; _chemical_formula_weight 780.66 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 120 _exptl_crystal_description ' plates ' _exptl_crystal_colour ' pale pink ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1575.730 _exptl_absorpt_coefficient_mu 0.920 _diffrn_measurement_device_type ; Bruker SMART ; _diffrn_radiation_monochromator graphite _computing_data_collection ; SMART (Siemens, 1993) ; _computing_data_reduction ; SAINT (Siemens ,1995) ; _computing_cell_refinement ; SAINT (Siemens ,1995) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Siemens, 1996) ; _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.96 # Sheldrick geometric definitions 0.83 0.96 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 120 _diffrn_reflns_number 27657 _reflns_number_total 7287 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 25989 # Number of reflections without Friedels Law is 7287 # Theoretical number of reflections is about 3826 _diffrn_reflns_theta_min 3.719 _diffrn_reflns_theta_max 27.823 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.432 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min 0 _reflns_limit_h_max 55 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _refine_diff_density_min -1.33 _refine_diff_density_max 2.76 _refine_ls_number_reflns 6271 _refine_ls_number_restraints 7 _refine_ls_number_parameters 419 #_refine_ls_R_factor_ref 0.0473 _refine_ls_wR_factor_ref 0.1110 _refine_ls_goodness_of_fit_ref 0.8655 #_reflns_number_all 7282 _refine_ls_R_factor_all 0.0539 _refine_ls_wR_factor_all 0.1125 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6271 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_gt 0.1110 _refine_ls_shift/su_max 0.001573 _refine_ls_abs_structure_Flack 0.55(3) _refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs' _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 9.62 13.9 7.22 1.78 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993) SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.170564(9) 0.53259(6) -0.18598(6) 0.0316 1.0000 Uani . . . . . . N1 N 0.17482(9) 0.2710(8) -0.0666(3) 0.0237 1.0000 Uani . . . . . . C5 C 0.15637(11) 0.3137(9) 0.0075(3) 0.0227 1.0000 Uani . . . . . . C4 C 0.15575(10) 0.1540(9) 0.0869(3) 0.0209 1.0000 Uani . . . . . . N2 N 0.13790(9) 0.1966(8) 0.1669(3) 0.0272 1.0000 Uani . . . . . . C6 C 0.11498(11) 0.3769(10) 0.1749(3) 0.0275 1.0000 Uani . . . . . . N3 N 0.10342(10) 0.3864(9) 0.2653(3) 0.0285 1.0000 Uani . . . . . . C7 C 0.07842(10) 0.5378(9) 0.2948(3) 0.0246 1.0000 Uani . . . . . . C12 C 0.06846(12) 0.7506(11) 0.2473(4) 0.0358 1.0000 Uani . . . . . . C11 C 0.04352(13) 0.8867(11) 0.2815(4) 0.0363 1.0000 Uani . . . . . . C10 C 0.02852(11) 0.8181(10) 0.3624(4) 0.0294 1.0000 Uani . . . . . . C13 C 0.000000(6) 0.9594(15) 0.3940(7) 0.0371 1.0000 Uani S T . . . . C9 C 0.03967(13) 0.6105(12) 0.4128(4) 0.0370 1.0000 Uani . . . . . . C8 C 0.06450(13) 0.4687(11) 0.3790(4) 0.0358 1.0000 Uani . . . . . . O1 O 0.10614(12) 0.5058(9) 0.1101(3) 0.0564 1.0000 Uani . . . . . . C3 C 0.17524(10) -0.0574(9) 0.0876(3) 0.0242 1.0000 Uani . . . . . . C2 C 0.19430(12) -0.0955(9) 0.0114(3) 0.0265 1.0000 Uani . . . . . . C1 C 0.19329(11) 0.0707(9) -0.0655(3) 0.0253 1.0000 Uani . . . . . . N7 N 0.12645(12) 0.7873(10) -0.1152(3) 0.0375 1.0000 Uani . . . . . . C27 C 0.10851(14) 0.9339(11) -0.0978(4) 0.0377 1.0000 Uani . . . . . . C28 C 0.08607(17) 1.1365(17) -0.0809(5) 0.0602 1.0000 Uani . . . . . . N4 N 0.18065(9) 0.7846(8) -0.3056(3) 0.0241 1.0000 Uani . . . . . . C18 C 0.16073(11) 0.9753(9) -0.3224(4) 0.0251 1.0000 Uani . . . . . . C17 C 0.16352(10) 1.1395(9) -0.3995(3) 0.0205 1.0000 Uani . . . . . . N5 N 0.14326(9) 1.3313(8) -0.4217(3) 0.0252 1.0000 Uani . . . . . . C19 C 0.12151(11) 1.4306(9) -0.3614(3) 0.0231 1.0000 Uani . . . . . . O2 O 0.11853(7) 1.3634(7) -0.2789(2) 0.0266 1.0000 Uani . . . . . . N6 N 0.10458(9) 1.6182(8) -0.4042(3) 0.0252 1.0000 Uani . . . . . . C20 C 0.07991(10) 1.7533(10) -0.3626(3) 0.0246 1.0000 Uani . . . . . . C21 C 0.06443(11) 1.6763(11) -0.2816(4) 0.0332 1.0000 Uani . . . . . . C22 C 0.03930(12) 1.8135(12) -0.2505(4) 0.0368 1.0000 Uani . . . . . . C23 C 0.02862(11) 2.0246(10) -0.2991(4) 0.0333 1.0000 Uani . . . . . . C26 C 0.000000(6) 2.1591(17) -0.2652(6) 0.0409 1.0000 Uani S T . . . . C24 C 0.04433(13) 2.0995(10) -0.3799(4) 0.0353 1.0000 Uani . . . . . . C25 C 0.06997(13) 1.9677(10) -0.4101(4) 0.0330 1.0000 Uani . . . . . . C16 C 0.18833(11) 1.1000(10) -0.4612(3) 0.0257 1.0000 Uani . . . . . . C15 C 0.20854(13) 0.9056(10) -0.4431(3) 0.0304 1.0000 Uani . . . . . . C14 C 0.20401(12) 0.7502(10) -0.3645(3) 0.0297 1.0000 Uani . . . . . . N8 N 0.35060(10) 0.2021(8) -0.1203(3) 0.0280 1.0000 Uani . . . . . . O5 O 0.37384(8) 0.1069(8) -0.0877(3) 0.0358 1.0000 Uani . . . . . . O4 O 0.33568(8) 0.0902(8) -0.1835(4) 0.0410 1.0000 Uani . . . . . . Cl3 Cl 0.21113(3) 0.3854(3) 0.20801(12) 0.0424 1.0000 Uani . . . . . . Cl2 Cl 0.24554(3) 0.4278(3) 0.38281(11) 0.0430 1.0000 Uani . . . . . . Cl1 Cl 0.25122(3) 0.8082(3) 0.23557(12) 0.0411 1.0000 Uani . . . . . . C29 C 0.22589(12) 0.5962(10) 0.2927(4) 0.0344 1.0000 Uani . . . . . . O3 O 0.34074(11) 0.4099(8) -0.0904(3) 0.0394 1.0000 Uani . . . . . . H4 H 0.14277(11) 0.4663(9) 0.0062(3) 0.0364 1.0000 Uiso R . . . . . H10 H 0.07863(12) 0.8045(11) 0.1870(4) 0.0392 1.0000 Uiso R . . . . . H9 H 0.03655(13) 1.0405(11) 0.2459(4) 0.0487 1.0000 Uiso R . . . . . H12 H 0.000000(6) 0.9795(15) 0.4646(7) 0.0403 1.0000 Uiso RS . . . . . H11 H 0.000000(6) 1.1308(15) 0.3634(7) 0.0403 1.0000 Uiso RS . . . . . H8 H 0.02962(13) 0.5598(12) 0.4736(4) 0.0479 1.0000 Uiso R . . . . . H7 H 0.07219(13) 0.3227(11) 0.4176(4) 0.0423 1.0000 Uiso R . . . . . H3 H 0.17524(10) -0.1791(9) 0.1421(3) 0.0336 1.0000 Uiso R . . . . . H2 H 0.20853(12) -0.2440(9) 0.0108(3) 0.0321 1.0000 Uiso R . . . . . H1 H 0.20712(11) 0.0411(9) -0.1209(3) 0.0339 1.0000 Uiso R . . . . . H16 H 0.14397(11) 1.0050(9) -0.2755(4) 0.0390 1.0000 Uiso R . . . . . H19 H 0.07197(11) 1.5280(11) -0.2439(4) 0.0484 1.0000 Uiso R . . . . . H20 H 0.02806(12) 1.7533(12) -0.1930(4) 0.0451 1.0000 Uiso R . . . . . H23 H 0.000000(6) 2.3273(17) -0.2983(6) 0.0558 1.0000 Uiso RS . . . . . H24 H 0.000000(6) 2.1865(17) -0.1950(6) 0.0558 1.0000 Uiso RS . . . . . H21 H 0.03717(13) 2.2510(10) -0.4165(4) 0.0477 1.0000 Uiso R . . . . . H22 H 0.08143(13) 2.0296(10) -0.4670(4) 0.0422 1.0000 Uiso R . . . . . H15 H 0.19154(11) 1.2131(10) -0.5174(3) 0.0358 1.0000 Uiso R . . . . . H14 H 0.22580(13) 0.8744(10) -0.4880(3) 0.0360 1.0000 Uiso R . . . . . H13 H 0.21915(12) 0.6120(10) -0.3520(3) 0.0378 1.0000 Uiso R . . . . . H18 H 0.11051(9) 1.6655(8) -0.4704(3) 0.0354 1.0000 Uiso R . . . . . H17 H 0.14397(9) 1.3998(8) -0.4879(3) 0.0358 1.0000 Uiso R . . . . . H6 H 0.11414(10) 0.2837(9) 0.3148(3) 0.0357 1.0000 Uiso R . . . . . H5 H 0.14223(9) 0.0908(8) 0.2243(3) 0.0387 1.0000 Uiso R . . . . . H25 H 0.06777(10) 1.0609(10) -0.0493(3) 0.0823 1.0000 Uiso R . . . . . H27 H 0.0958 1.2604 -0.0355 0.0823 1.0000 Uiso . . . . . . H26 H 0.0800 1.2139 -0.1390 0.0823 1.0000 Uiso . . . . . . H28 H 0.20847(12) 0.6906(10) 0.3221(4) 0.0465 1.0000 Uiso R . . . . . O6 O 0.0000 0.482(2) 0.1465(9) 0.0500 0.562(18) Uiso S . . . . . O7 O 0.4696(2) 0.405(2) 0.4923(8) 0.0500 0.461(12) Uiso . . . . . . 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 0.04592(19) 0.02444(15) 0.02449(15) 0.0083(2) -0.0067(2) -0.00201(15) N1 0.029(2) 0.0217(18) 0.0199(18) 0.0013(14) -0.0045(15) -0.0024(16) C5 0.022(2) 0.021(2) 0.026(2) -0.0038(18) -0.0112(17) 0.0036(17) C4 0.022(2) 0.020(2) 0.021(2) 0.0001(17) -0.0074(17) 0.0001(17) N2 0.027(2) 0.028(2) 0.0260(19) 0.0056(16) -0.0037(16) 0.0075(16) C6 0.028(2) 0.030(2) 0.025(2) -0.0066(19) -0.0062(18) 0.008(2) N3 0.027(2) 0.032(2) 0.026(2) 0.0000(17) 0.0024(16) 0.0074(18) C7 0.023(2) 0.028(2) 0.022(3) -0.0037(18) -0.0029(15) -0.0004(18) C12 0.031(3) 0.031(3) 0.046(3) 0.002(2) 0.007(2) 0.006(2) C11 0.035(3) 0.028(3) 0.046(3) -0.004(2) 0.006(2) 0.007(2) C10 0.022(2) 0.028(3) 0.038(3) -0.013(2) -0.0021(19) -0.002(2) C13 0.026(3) 0.030(4) 0.055(5) -0.021(4) 0.0000 0.0000 C9 0.030(3) 0.045(3) 0.036(3) -0.007(2) 0.000(2) 0.002(2) C8 0.037(3) 0.036(3) 0.034(2) -0.001(2) -0.003(2) 0.008(2) O1 0.070(3) 0.063(3) 0.036(2) 0.002(2) -0.001(2) 0.048(3) C3 0.024(2) 0.021(2) 0.027(2) 0.0063(17) -0.0039(17) -0.0005(18) C2 0.031(2) 0.018(2) 0.030(3) -0.0003(18) 0.000(2) 0.0017(19) C1 0.028(2) 0.024(2) 0.023(2) -0.0002(17) 0.0018(18) 0.0003(19) N7 0.049(3) 0.034(2) 0.030(2) 0.0037(19) -0.007(2) -0.002(2) C27 0.044(3) 0.036(3) 0.034(3) -0.006(2) -0.006(2) -0.006(3) C28 0.050(4) 0.076(5) 0.054(4) -0.023(4) -0.009(3) 0.016(4) N4 0.0271(19) 0.0197(18) 0.0254(19) 0.0004(15) -0.0108(16) -0.0034(15) C18 0.027(2) 0.022(2) 0.027(2) -0.0025(19) -0.0021(17) -0.0049(18) C17 0.023(2) 0.024(2) 0.015(2) -0.0017(16) -0.0024(15) -0.0003(17) N5 0.029(2) 0.024(2) 0.0223(18) 0.0023(15) 0.0000(16) 0.0001(17) C19 0.024(2) 0.021(2) 0.025(2) -0.0011(17) -0.0043(17) -0.0031(18) O2 0.0267(17) 0.0319(18) 0.0213(16) 0.0029(14) 0.0018(13) 0.0016(14) N6 0.0247(19) 0.0255(19) 0.0253(19) 0.0004(15) -0.0015(15) 0.0001(16) C20 0.017(2) 0.027(2) 0.029(2) -0.0062(18) -0.0066(17) -0.0012(18) C21 0.024(2) 0.038(3) 0.037(3) -0.004(2) -0.0015(19) -0.002(2) C22 0.026(2) 0.046(3) 0.039(3) -0.004(2) 0.007(2) -0.008(2) C23 0.019(2) 0.032(3) 0.049(3) -0.021(2) -0.004(2) -0.0037(19) C26 0.032(4) 0.041(4) 0.050(5) -0.024(4) 0.0000 0.0000 C24 0.033(3) 0.028(3) 0.044(3) -0.006(2) -0.006(2) 0.005(2) C25 0.032(3) 0.028(2) 0.040(3) 0.001(2) 0.003(2) 0.002(2) C16 0.026(2) 0.025(2) 0.027(2) 0.0061(18) 0.0027(18) -0.0004(19) C15 0.036(3) 0.030(3) 0.025(2) -0.0017(19) 0.005(2) 0.002(2) C14 0.035(3) 0.025(2) 0.029(2) -0.0008(19) -0.006(2) -0.003(2) N8 0.033(2) 0.032(2) 0.0194(17) -0.0031(17) 0.0003(16) 0.0019(18) O5 0.0263(18) 0.046(2) 0.035(2) 0.0026(17) -0.0047(14) 0.0011(16) O4 0.0377(19) 0.048(2) 0.0376(18) -0.020(3) -0.006(2) 0.0139(15) Cl3 0.0419(7) 0.0310(6) 0.0544(8) -0.0025(6) -0.0196(6) -0.0013(5) Cl2 0.0384(7) 0.0533(9) 0.0373(6) 0.0096(6) -0.0044(6) 0.0063(6) Cl1 0.0428(7) 0.0293(6) 0.0512(8) 0.0026(6) -0.0071(6) -0.0026(5) C29 0.030(2) 0.031(2) 0.042(3) -0.004(2) -0.005(2) 0.0054(19) O3 0.054(2) 0.033(2) 0.0311(19) -0.0147(16) 0.0034(17) 0.0054(17) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 . N4 . 2.190(4) yes Ag1 . N7 . 2.556(5) yes Ag1 . N1 . 2.181(4) yes N1 . C1 . 1.329(6) yes N1 . C5 . 1.340(7) yes C5 . H4 . 1.000 no C5 . C4 . 1.400(7) yes C4 . C3 . 1.402(6) yes C4 . N2 . 1.390(6) yes N2 . H5 . 1.000 no N2 . C6 . 1.387(6) yes C6 . O1 . 1.202(7) yes C6 . N3 . 1.373(6) yes N3 . H6 . 1.000 no N3 . C7 . 1.417(6) yes C7 . C8 . 1.383(7) yes C7 . C12 . 1.376(7) yes C12 . H10 . 1.000 no C12 . C11 . 1.393(8) yes C11 . H9 . 1.000 no C11 . C10 . 1.365(8) yes C10 . C9 . 1.392(8) yes C10 . C13 . 1.521(6) yes C13 . H11 . 1.000 no C13 . H12 . 1.000 no C9 . H8 . 1.000 no C9 . C8 . 1.403(8) yes C8 . H7 . 1.000 no C3 . H3 . 1.000 no C3 . C2 . 1.376(7) yes C2 . H2 . 1.000 no C2 . C1 . 1.393(7) yes C1 . H1 . 1.000 no N7 . C27 . 1.128(8) yes C27 . C28 . 1.470(10) yes C28 . H26 . 0.952 no C28 . H27 . 1.008 no C28 . H25 . 1.000 no N4 . C14 . 1.331(7) yes N4 . C18 . 1.351(7) yes C18 . H16 . 1.000 no C18 . C17 . 1.395(7) yes C17 . C16 . 1.408(6) yes C17 . N5 . 1.380(6) yes N5 . H17 . 1.000 no N5 . C19 . 1.380(6) yes C19 . N6 . 1.374(6) yes C19 . O2 . 1.223(6) yes N6 . H18 . 1.000 no N6 . C20 . 1.421(6) yes C20 . C25 . 1.382(7) yes C20 . C21 . 1.389(7) yes C21 . H19 . 1.000 no C21 . C22 . 1.388(8) yes C22 . H20 . 1.000 no C22 . C23 . 1.386(9) yes C23 . C24 . 1.388(9) yes C23 . C26 . 1.517(6) yes C26 . H24 . 1.000 no C26 . H23 . 1.000 no C24 . H21 . 1.000 no C24 . C25 . 1.388(8) yes C25 . H22 . 1.000 no C16 . H15 . 1.000 no C16 . C15 . 1.377(8) yes C15 . H14 . 1.000 no C15 . C14 . 1.391(7) yes C14 . H13 . 1.000 no N8 . O3 . 1.249(6) yes N8 . O4 . 1.253(6) yes N8 . O5 . 1.224(6) yes Cl3 . C29 . 1.753(5) yes Cl2 . C29 . 1.772(5) yes Cl1 . C29 . 1.768(6) yes C29 . H28 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N4 . Ag1 . N7 . 97.82(15) yes N4 . Ag1 . N1 . 163.41(14) yes N7 . Ag1 . N1 . 95.41(15) yes C1 . N1 . C5 . 119.4(4) yes C1 . N1 . Ag1 . 124.2(3) yes C5 . N1 . Ag1 . 116.4(3) yes H4 . C5 . C4 . 118.981 no H4 . C5 . N1 . 118.715 no C4 . C5 . N1 . 122.3(4) yes C3 . C4 . N2 . 117.7(4) yes C3 . C4 . C5 . 118.1(4) yes N2 . C4 . C5 . 124.2(4) yes H5 . N2 . C6 . 116.886 no H5 . N2 . C4 . 117.370 no C6 . N2 . C4 . 125.7(4) yes O1 . C6 . N3 . 124.5(5) yes O1 . C6 . N2 . 123.9(5) yes N3 . C6 . N2 . 111.6(4) yes H6 . N3 . C7 . 117.567 no H6 . N3 . C6 . 117.044 no C7 . N3 . C6 . 125.3(4) yes C8 . C7 . C12 . 119.5(5) yes C8 . C7 . N3 . 116.4(4) yes C12 . C7 . N3 . 124.1(4) yes H10 . C12 . C11 . 119.869 no H10 . C12 . C7 . 120.193 no C11 . C12 . C7 . 119.9(5) yes H9 . C11 . C10 . 119.049 no H9 . C11 . C12 . 118.835 no C10 . C11 . C12 . 122.1(5) yes C9 . C10 . C13 . 121.5(6) yes C9 . C10 . C11 . 117.7(5) yes C13 . C10 . C11 . 120.8(6) yes H11 . C13 . H12 . 109.467 no H11 . C13 . C10 2_555 108.310 no H12 . C13 . C10 2_555 110.081 no H11 . C13 . C10 . 108.310 no H12 . C13 . C10 . 110.081 no C10 2_555 C13 . C10 . 110.5(6) yes H8 . C9 . C8 . 119.430 no H8 . C9 . C10 . 119.498 no C8 . C9 . C10 . 121.1(5) yes H7 . C8 . C7 . 121.371 no H7 . C8 . C9 . 118.974 no C7 . C8 . C9 . 119.6(5) yes H3 . C3 . C2 . 120.427 no H3 . C3 . C4 . 120.918 no C2 . C3 . C4 . 118.7(4) yes H2 . C2 . C1 . 120.272 no H2 . C2 . C3 . 119.904 no C1 . C2 . C3 . 119.8(4) yes H1 . C1 . N1 . 118.895 no H1 . C1 . C2 . 119.351 no N1 . C1 . C2 . 121.7(4) yes C27 . N7 . Ag1 . 166.0(5) yes C28 . C27 . N7 . 175.8(7) yes H26 . C28 . H27 . 112.790 no H26 . C28 . H25 . 109.266 no H27 . C28 . H25 . 108.197 no H26 . C28 . C27 . 110.953 no H27 . C28 . C27 . 106.814 no H25 . C28 . C27 . 108.695 no C14 . N4 . C18 . 119.3(4) yes C14 . N4 . Ag1 . 123.6(3) yes C18 . N4 . Ag1 . 117.0(3) yes H16 . C18 . C17 . 118.853 no H16 . C18 . N4 . 118.369 no C17 . C18 . N4 . 122.7(5) yes C16 . C17 . N5 . 117.7(4) yes C16 . C17 . C18 . 117.3(4) yes N5 . C17 . C18 . 125.0(4) yes H17 . N5 . C19 . 117.343 no H17 . N5 . C17 . 117.050 no C19 . N5 . C17 . 125.6(4) yes N6 . C19 . O2 . 124.6(4) yes N6 . C19 . N5 . 112.0(4) yes O2 . C19 . N5 . 123.4(4) yes H18 . N6 . C20 . 117.293 no H18 . N6 . C19 . 116.615 no C20 . N6 . C19 . 126.1(4) yes C25 . C20 . C21 . 118.9(5) yes C25 . C20 . N6 . 116.6(4) yes C21 . C20 . N6 . 124.4(5) yes H19 . C21 . C22 . 120.021 no H19 . C21 . C20 . 120.216 no C22 . C21 . C20 . 119.7(5) yes H20 . C22 . C23 . 119.221 no H20 . C22 . C21 . 118.809 no C23 . C22 . C21 . 121.9(5) yes C24 . C23 . C26 . 122.4(6) yes C24 . C23 . C22 . 117.8(5) yes C26 . C23 . C22 . 119.8(6) yes H24 . C26 . H23 . 109.466 no H24 . C26 . C23 2_555 112.265 no H23 . C26 . C23 2_555 105.428 no H24 . C26 . C23 . 112.265 no H23 . C26 . C23 . 105.428 no C23 2_555 C26 . C23 . 111.5(6) yes H21 . C24 . C25 . 119.596 no H21 . C24 . C23 . 119.619 no C25 . C24 . C23 . 120.8(5) yes H22 . C25 . C20 . 119.715 no H22 . C25 . C24 . 119.347 no C20 . C25 . C24 . 120.9(5) yes H15 . C16 . C15 . 119.896 no H15 . C16 . C17 . 120.641 no C15 . C16 . C17 . 119.5(4) yes H14 . C15 . C14 . 121.075 no H14 . C15 . C16 . 119.380 no C14 . C15 . C16 . 119.5(5) yes H13 . C14 . N4 . 119.939 no H13 . C14 . C15 . 118.222 no N4 . C14 . C15 . 121.8(5) yes O3 . N8 . O4 . 118.1(4) yes O3 . N8 . O5 . 121.3(4) yes O4 . N8 . O5 . 120.6(4) yes H28 . C29 . Cl3 . 108.289 no H28 . C29 . Cl1 . 110.750 no Cl3 . C29 . Cl1 . 108.7(3) yes H28 . C29 . Cl2 . 108.865 no Cl3 . C29 . Cl2 . 110.6(3) yes Cl1 . C29 . Cl2 . 109.7(3) yes data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 281275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 05srv052 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56 Co N14 O16' _chemical_formula_weight 999.88 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' _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 9.3380(6) _cell_length_b 11.3324(7) _cell_length_c 11.4099(7) _cell_angle_alpha 74.1670(10) _cell_angle_beta 71.2920(10) _cell_angle_gamma 80.3580(10) _cell_volume 1095.99(12) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5772 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 30.50 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 525 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details 'XPREP 6.14 in SHELXTL (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Microfocus X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD Diffractometer with Bede Microsource' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14659 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 30.52 _reflns_number_total 6590 _reflns_number_gt 5923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.5238P] 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 6590 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.0000 0.0000 0.01190(7) Uani 1 2 d S . . O1 O -0.68800(12) 0.33540(10) 0.22651(10) 0.0176(2) Uani 1 1 d . . . N1 N -0.21420(13) 0.11517(11) -0.00445(11) 0.0147(2) Uani 1 1 d . . . C1 C -0.30929(16) 0.08600(14) -0.05701(14) 0.0170(3) Uani 1 1 d . . . H1 H -0.2788 0.0189 -0.0972 0.020 Uiso 1 1 calc R . . O2 O -1.07569(13) 0.96151(11) 0.40768(10) 0.0217(2) Uani 1 1 d . . . N2 N -0.43818(13) 0.37210(12) 0.12565(12) 0.0166(2) Uani 1 1 d . . . C2 C -0.45034(17) 0.14990(14) -0.05500(14) 0.0178(3) Uani 1 1 d . . . H2 H -0.5136 0.1274 -0.0945 0.021 Uiso 1 1 calc R . . O3 O 0.00542(13) 0.06820(11) 0.15427(11) 0.0187(2) Uani 1 1 d . . . N3 N -0.58398(14) 0.48029(12) 0.27097(12) 0.0163(2) Uani 1 1 d . . . C3 C -0.49832(16) 0.24689(14) 0.00511(14) 0.0163(3) Uani 1 1 d . . . H3 H -0.5941 0.2920 0.0071 0.020 Uiso 1 1 calc R . . O4 O 0.12783(13) 0.13728(11) -0.12136(11) 0.0190(2) Uani 1 1 d . . . N4 N -1.04929(15) 0.77857(12) 0.54605(13) 0.0195(3) Uani 1 1 d . . . C4 C -0.40195(16) 0.27610(13) 0.06233(13) 0.0145(3) Uani 1 1 d . . . O5 O -0.17803(14) 0.45566(11) 0.14381(14) 0.0286(3) Uani 1 1 d . . . N5 N -1.25462(14) 0.91423(12) 0.60203(12) 0.0174(2) Uani 1 1 d . . . C5 C -0.26099(16) 0.20903(13) 0.05381(14) 0.0151(3) Uani 1 1 d . . . H5 H -0.1946 0.2307 0.0911 0.018 Uiso 1 1 calc R . . O6 O -0.31330(13) 0.61806(12) 0.19797(13) 0.0273(3) Uani 1 1 d . . . N6 N -1.60633(15) 1.10502(13) 0.69422(13) 0.0209(3) Uani 1 1 d . . . C6 C -0.57835(16) 0.39410(13) 0.20857(13) 0.0143(3) Uani 1 1 d . . . O7 O -0.06813(13) 0.60608(11) 0.15148(13) 0.0254(3) Uani 1 1 d . . . N7 N -0.18651(15) 0.56106(12) 0.16437(13) 0.0189(3) Uani 1 1 d . . . C7 C -0.72547(15) 0.52518(13) 0.35422(13) 0.0148(3) Uani 1 1 d . . . H7 H -0.7909 0.4553 0.3981 0.018 Uiso 1 1 calc R . . O8 O 0.08810(17) 0.29559(13) 0.13071(16) 0.0350(3) Uani 1 1 d . . . C8 C -0.81059(16) 0.62712(14) 0.27728(14) 0.0169(3) Uani 1 1 d . . . H8A H -0.8406 0.5931 0.2183 0.020 Uiso 1 1 calc R . . H8B H -0.7421 0.6923 0.2256 0.020 Uiso 1 1 calc R . . C9 C -0.95189(16) 0.68372(14) 0.36203(14) 0.0172(3) Uani 1 1 d . . . H9A H -1.0259 0.6211 0.4063 0.021 Uiso 1 1 calc R . . H9B H -0.9997 0.7528 0.3087 0.021 Uiso 1 1 calc R . . C10 C -0.91284(16) 0.73084(14) 0.46046(13) 0.0160(3) Uani 1 1 d . . . H10 H -0.8447 0.7987 0.4149 0.019 Uiso 1 1 calc R . . C11 C -0.83068(17) 0.62829(14) 0.53901(14) 0.0185(3) Uani 1 1 d . . . H11A H -0.9003 0.5638 0.5900 0.022 Uiso 1 1 calc R . . H11B H -0.8012 0.6619 0.5986 0.022 Uiso 1 1 calc R . . C12 C -0.68894(17) 0.57101(15) 0.45447(15) 0.0192(3) Uani 1 1 d . . . H12A H -0.6141 0.6330 0.4116 0.023 Uiso 1 1 calc R . . H12B H -0.6425 0.5013 0.5082 0.023 Uiso 1 1 calc R . . C13 C -1.12195(16) 0.88919(14) 0.51042(13) 0.0155(3) Uani 1 1 d . . . C14 C -1.36262(16) 1.01388(14) 0.58877(14) 0.0155(3) Uani 1 1 d . . . C15 C -1.35371(17) 1.10936(15) 0.48060(15) 0.0195(3) Uani 1 1 d . . . H15 H -1.2681 1.1119 0.4075 0.023 Uiso 1 1 calc R . . C16 C -1.47325(18) 1.20101(15) 0.48228(15) 0.0217(3) Uani 1 1 d . . . H16 H -1.4698 1.2673 0.4097 0.026 Uiso 1 1 calc R . . C17 C -1.59698(18) 1.19574(15) 0.58929(16) 0.0217(3) Uani 1 1 d . . . H17 H -1.6781 1.2586 0.5883 0.026 Uiso 1 1 calc R . . C18 C -1.49194(17) 1.01703(14) 0.69293(14) 0.0188(3) Uani 1 1 d . . . H18 H -1.4986 0.9524 0.7673 0.023 Uiso 1 1 calc R . . H3N H -0.5132 0.5199 0.2537 0.019(5) Uiso 1 1 d R . . H2N H -0.3668 0.4023 0.1311 0.022(5) Uiso 1 1 d R . . H5N H -1.2821 0.8522 0.6687 0.026(5) Uiso 1 1 d R . . H31 H -0.018(3) 0.033(2) 0.225(2) 0.030(6) Uiso 1 1 d . . . H32 H 0.039(3) 0.143(2) 0.151(2) 0.032(6) Uiso 1 1 d . . . H41 H 0.108(3) 0.206(2) -0.122(2) 0.037(7) Uiso 1 1 d . . . H42 H 0.209(3) 0.128(2) -0.176(3) 0.045(7) Uiso 1 1 d . . . H81 H 0.022(4) 0.360(3) 0.123(3) 0.064(9) Uiso 1 1 d . . . H82 H 0.158(3) 0.318(3) 0.149(3) 0.051(8) Uiso 1 1 d . . . H4N H -1.088(3) 0.735(2) 0.611(2) 0.038(7) Uiso 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 Co1 0.01236(12) 0.01021(13) 0.01241(12) -0.00329(9) -0.00221(9) -0.00073(9) O1 0.0161(5) 0.0163(5) 0.0211(5) -0.0050(4) -0.0048(4) -0.0034(4) N1 0.0151(5) 0.0125(5) 0.0159(5) -0.0034(4) -0.0037(4) -0.0010(4) C1 0.0175(6) 0.0151(7) 0.0189(6) -0.0062(5) -0.0039(5) -0.0017(5) O2 0.0222(5) 0.0211(6) 0.0152(5) -0.0006(4) -0.0004(4) 0.0001(4) N2 0.0123(5) 0.0163(6) 0.0233(6) -0.0098(5) -0.0039(5) -0.0004(4) C2 0.0176(6) 0.0186(7) 0.0194(7) -0.0055(5) -0.0065(5) -0.0033(5) O3 0.0256(5) 0.0164(5) 0.0137(5) -0.0035(4) -0.0044(4) -0.0033(4) N3 0.0130(5) 0.0150(6) 0.0216(6) -0.0082(5) -0.0026(4) -0.0013(4) C3 0.0142(6) 0.0170(7) 0.0174(6) -0.0036(5) -0.0050(5) -0.0007(5) O4 0.0173(5) 0.0134(5) 0.0208(5) -0.0036(4) 0.0014(4) -0.0013(4) N4 0.0206(6) 0.0154(6) 0.0155(6) -0.0024(5) 0.0019(5) 0.0010(5) C4 0.0148(6) 0.0120(6) 0.0163(6) -0.0040(5) -0.0034(5) -0.0009(5) O5 0.0242(6) 0.0217(6) 0.0477(8) -0.0160(6) -0.0152(5) -0.0003(5) N5 0.0170(6) 0.0150(6) 0.0150(5) -0.0010(4) -0.0003(4) 0.0000(4) C5 0.0147(6) 0.0140(6) 0.0178(6) -0.0049(5) -0.0056(5) -0.0007(5) O6 0.0186(5) 0.0240(6) 0.0396(7) -0.0118(5) -0.0063(5) 0.0005(4) N6 0.0179(6) 0.0201(6) 0.0235(6) -0.0078(5) -0.0028(5) -0.0002(5) C6 0.0143(6) 0.0120(6) 0.0157(6) -0.0018(5) -0.0058(5) 0.0014(5) O7 0.0202(5) 0.0228(6) 0.0392(7) -0.0092(5) -0.0142(5) -0.0035(4) N7 0.0208(6) 0.0177(6) 0.0209(6) -0.0037(5) -0.0104(5) -0.0019(5) C7 0.0128(6) 0.0144(6) 0.0158(6) -0.0055(5) -0.0015(5) 0.0000(5) O8 0.0319(7) 0.0217(7) 0.0607(10) -0.0102(6) -0.0270(7) 0.0000(5) C8 0.0149(6) 0.0205(7) 0.0148(6) -0.0063(5) -0.0037(5) 0.0021(5) C9 0.0143(6) 0.0200(7) 0.0173(6) -0.0064(5) -0.0042(5) 0.0017(5) C10 0.0154(6) 0.0157(7) 0.0147(6) -0.0041(5) -0.0013(5) 0.0000(5) C11 0.0213(7) 0.0188(7) 0.0158(6) -0.0058(5) -0.0060(5) 0.0017(5) C12 0.0182(6) 0.0216(7) 0.0201(7) -0.0093(6) -0.0082(5) 0.0043(5) C13 0.0154(6) 0.0165(7) 0.0155(6) -0.0060(5) -0.0039(5) -0.0013(5) C14 0.0154(6) 0.0155(7) 0.0172(6) -0.0064(5) -0.0047(5) -0.0017(5) C15 0.0197(7) 0.0197(7) 0.0181(7) -0.0042(6) -0.0045(5) -0.0014(5) C16 0.0235(7) 0.0206(7) 0.0203(7) -0.0026(6) -0.0087(6) 0.0005(6) C17 0.0187(7) 0.0205(7) 0.0277(8) -0.0088(6) -0.0082(6) 0.0016(5) C18 0.0200(7) 0.0164(7) 0.0177(6) -0.0046(5) -0.0024(5) -0.0010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.0369(11) 2 ? Co1 O4 2.0369(11) . ? Co1 O3 2.1238(11) . ? Co1 O3 2.1238(11) 2 ? Co1 N1 2.2048(12) . ? Co1 N1 2.2048(12) 2 ? O1 C6 1.2459(17) . ? N1 C1 1.3437(19) . ? N1 C5 1.3445(18) . ? C1 C2 1.389(2) . ? O2 C13 1.2255(18) . ? N2 C6 1.3767(17) . ? N2 C4 1.4032(18) . ? C2 C3 1.389(2) . ? N3 C6 1.3424(18) . ? N3 C7 1.4629(17) . ? C3 C4 1.393(2) . ? N4 C13 1.3458(19) . ? N4 C10 1.4591(18) . ? C4 C5 1.3939(19) . ? O5 N7 1.2638(17) . ? N5 C13 1.3860(18) . ? N5 C14 1.3923(19) . ? O6 N7 1.2464(17) . ? N6 C18 1.333(2) . ? N6 C17 1.338(2) . ? O7 N7 1.2440(17) . ? C7 C8 1.524(2) . ? C7 C12 1.526(2) . ? C8 C9 1.5245(19) . ? C9 C10 1.528(2) . ? C10 C11 1.522(2) . ? C11 C12 1.529(2) . ? C14 C15 1.392(2) . ? C14 C18 1.4000(19) . ? C15 C16 1.391(2) . ? C16 C17 1.381(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co1 O4 180.00(9) 2 . ? O4 Co1 O3 91.32(5) 2 . ? O4 Co1 O3 88.68(5) . . ? O4 Co1 O3 88.68(5) 2 2 ? O4 Co1 O3 91.32(5) . 2 ? O3 Co1 O3 180.00(5) . 2 ? O4 Co1 N1 87.54(5) 2 . ? O4 Co1 N1 92.46(5) . . ? O3 Co1 N1 89.31(4) . . ? O3 Co1 N1 90.69(4) 2 . ? O4 Co1 N1 92.46(5) 2 2 ? O4 Co1 N1 87.54(5) . 2 ? O3 Co1 N1 90.69(4) . 2 ? O3 Co1 N1 89.31(4) 2 2 ? N1 Co1 N1 180.00(7) . 2 ? C1 N1 C5 117.54(12) . . ? C1 N1 Co1 120.02(10) . . ? C5 N1 Co1 122.19(10) . . ? N1 C1 C2 122.68(13) . . ? C6 N2 C4 123.60(12) . . ? C3 C2 C1 119.65(14) . . ? C6 N3 C7 122.53(12) . . ? C2 C3 C4 118.10(13) . . ? C13 N4 C10 122.12(13) . . ? C3 C4 C5 118.66(13) . . ? C3 C4 N2 123.17(13) . . ? C5 C4 N2 118.15(13) . . ? C13 N5 C14 127.02(13) . . ? N1 C5 C4 123.34(13) . . ? C18 N6 C17 117.88(13) . . ? O1 C6 N3 123.53(13) . . ? O1 C6 N2 122.30(13) . . ? N3 C6 N2 114.12(13) . . ? O7 N7 O6 120.97(13) . . ? O7 N7 O5 119.46(13) . . ? O6 N7 O5 119.56(13) . . ? N3 C7 C8 110.70(12) . . ? N3 C7 C12 108.99(11) . . ? C8 C7 C12 110.90(12) . . ? C7 C8 C9 112.15(12) . . ? C8 C9 C10 111.24(12) . . ? N4 C10 C11 108.82(12) . . ? N4 C10 C9 111.12(12) . . ? C11 C10 C9 110.62(12) . . ? C10 C11 C12 111.54(12) . . ? C7 C12 C11 111.89(12) . . ? O2 C13 N4 123.71(13) . . ? O2 C13 N5 122.95(14) . . ? N4 C13 N5 113.34(13) . . ? C15 C14 N5 125.60(13) . . ? C15 C14 C18 117.46(14) . . ? N5 C14 C18 116.93(13) . . ? C16 C15 C14 118.31(14) . . ? C17 C16 C15 120.08(15) . . ? N6 C17 C16 122.19(15) . . ? N6 C18 C14 124.08(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N O6 0.80 2.16 2.9634(17) 175.8 . N2 H2N O5 0.82 2.02 2.8359(17) 172.9 . N5 H5N O1 0.88 2.15 2.9887(17) 157.9 2_366 O3 H32 O8 0.94(2) 1.80(2) 2.7320(18) 173(2) . O4 H41 O7 0.76(3) 2.06(3) 2.8145(17) 172(3) 2_565 O4 H41 N7 0.76(3) 2.74(3) 3.4302(18) 152(2) 2_565 O8 H82 O1 0.84(3) 1.97(3) 2.7966(18) 166(3) 1_655 N4 H4N O1 0.78(3) 2.39(2) 3.0934(17) 150(2) 2_366 O4 H42 N6 0.83(3) 1.91(3) 2.7365(17) 178(3) 1_744 O3 H31 O2 0.77(2) 1.95(3) 2.7185(16) 174(2) 1_645 O8 H81 O5 0.87(3) 1.98(3) 2.8086(19) 158(3) . _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.552 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.071