Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Floriana Tuna' 'Guy Clarkson' 'Nathaniel W. Alcock' 'Michael J. Hannon' _publ_contact_author_name 'Dr Michael Hannon' _publ_contact_author_address ; Department of Chemistry University of Warwick Gibbet Hill Road Coventry CV4 7AL UNITED KINGDOM ; _publ_contact_author_email M.J.HANNON@WARWICK.AC.UK _publ_section_title ; The effect of phenyl substituents on supramolecular assemblies containing directly linked bis-pyridylimine ligands: synthesis and structural characterisation of mononuclear nickel(II) and dinuclear silver(I) and cobalt(III) complexes of (2-pyridyl)phenylketazine ; data_ft13 _database_code_CSD 189697 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H50.50 Co2 F18 N8 O8.25 P3' _chemical_formula_weight 1484.28 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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 12.2068(18) _cell_length_b 13.2943(19) _cell_length_c 21.456(3) _cell_angle_alpha 80.385(3) _cell_angle_beta 82.541(3) _cell_angle_gamma 73.978(3) _cell_volume 3286.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4636 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description plathe _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1503 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 15747 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.1666 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10201 _reflns_number_gt 4967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0970P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10201 _refine_ls_number_parameters 815 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1671 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2066 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 Co1 Co 0.19969(8) -0.09331(7) 0.25836(4) 0.0259(3) Uani 1 1 d . . . O1 O 0.2585(4) 0.0198(4) 0.2721(2) 0.0266(12) Uani 1 1 d . . . H01 H 0.176(6) 0.107(5) 0.286(3) 0.040 Uiso 1 1 d . . . Co2 Co 0.36926(8) -0.06505(8) 0.32692(4) 0.0262(3) Uani 1 1 d . . . O2 O 0.3384(4) -0.1766(4) 0.2912(2) 0.0266(12) Uani 1 1 d . . . H02A H 0.338(5) -0.248(5) 0.324(3) 0.040 Uiso 1 1 d . . . N11 N 0.1643(5) -0.2188(5) 0.2436(3) 0.0300(15) Uani 1 1 d . . . C12 C 0.0683(7) -0.2424(7) 0.2669(3) 0.038(2) Uani 1 1 d . . . H12A H 0.0122 -0.1926 0.2891 0.046 Uiso 1 1 calc R . . C13 C 0.0440(8) -0.3379(7) 0.2607(4) 0.049(2) Uani 1 1 d . . . H13A H -0.0268 -0.3523 0.2775 0.059 Uiso 1 1 calc R . . C14 C 0.1276(8) -0.4093(7) 0.2291(4) 0.051(2) Uani 1 1 d . . . H14A H 0.1157 -0.4754 0.2249 0.061 Uiso 1 1 calc R . . C15 C 0.2291(7) -0.3851(6) 0.2035(3) 0.041(2) Uani 1 1 d . . . H15A H 0.2864 -0.4337 0.1812 0.050 Uiso 1 1 calc R . . C16 C 0.2457(7) -0.2886(6) 0.2110(3) 0.0297(19) Uani 1 1 d . . . C17 C 0.3534(6) -0.2604(6) 0.1792(3) 0.0313(19) Uani 1 1 d . . . C18 C 0.4565(7) -0.3473(6) 0.1681(4) 0.035(2) Uani 1 1 d . . . C19 C 0.4956(8) -0.4294(7) 0.2179(4) 0.055(3) Uani 1 1 d . . . H19A H 0.4529 -0.4305 0.2582 0.066 Uiso 1 1 calc R . . N21 N 0.3918(5) 0.0594(5) 0.3504(3) 0.0286(15) Uani 1 1 d . . . C22 C 0.3721(6) 0.0768(6) 0.4113(4) 0.038(2) Uani 1 1 d . . . H22A H 0.3557 0.0226 0.4430 0.046 Uiso 1 1 calc R . . C23 C 0.3750(7) 0.1724(7) 0.4294(4) 0.044(2) Uani 1 1 d . . . H23A H 0.3628 0.1823 0.4729 0.053 Uiso 1 1 calc R . . C24 C 0.3956(7) 0.2512(7) 0.3837(4) 0.051(2) Uani 1 1 d . . . H24A H 0.3952 0.3175 0.3949 0.061 Uiso 1 1 calc R . . C25 C 0.4172(7) 0.2338(6) 0.3204(4) 0.044(2) Uani 1 1 d . . . H25A H 0.4346 0.2871 0.2883 0.053 Uiso 1 1 calc R . . C26 C 0.4130(6) 0.1382(6) 0.3048(3) 0.0296(19) Uani 1 1 d . . . C27 C 0.4438(6) 0.1159(6) 0.2375(3) 0.0311(19) Uani 1 1 d . . . C28 C 0.4308(7) 0.2089(6) 0.1857(4) 0.036(2) Uani 1 1 d . . . C29 C 0.3239(7) 0.2830(6) 0.1821(4) 0.041(2) Uani 1 1 d . . . H29A H 0.2618 0.2755 0.2125 0.050 Uiso 1 1 calc R . . O31 O 0.1193(4) -0.0995(4) 0.3410(2) 0.0287(12) Uani 1 1 d . . . C31 C 0.1592(7) -0.0938(6) 0.3924(3) 0.032(2) Uani 1 1 d . . . O32 O 0.2555(4) -0.0755(4) 0.3956(2) 0.0304(13) Uani 1 1 d . . . C32 C 0.0873(6) -0.1127(6) 0.4533(3) 0.039(2) Uani 1 1 d . . . H32A H 0.0161 -0.1252 0.4440 0.058 Uiso 1 1 calc R . . H32B H 0.0694 -0.0506 0.4755 0.058 Uiso 1 1 calc R . . H32C H 0.1295 -0.1746 0.4802 0.058 Uiso 1 1 calc R . . C110 C 0.5952(9) -0.5080(7) 0.2083(4) 0.066(3) Uani 1 1 d . . . H11A H 0.6214 -0.5627 0.2417 0.079 Uiso 1 1 calc R . . C111 C 0.6555(8) -0.5055(7) 0.1495(5) 0.069(3) Uani 1 1 d . . . H11B H 0.7234 -0.5597 0.1425 0.083 Uiso 1 1 calc R . . C112 C 0.6202(8) -0.4269(7) 0.1005(4) 0.060(3) Uani 1 1 d . . . H11C H 0.6629 -0.4277 0.0602 0.072 Uiso 1 1 calc R . . C113 C 0.5224(7) -0.3465(6) 0.1098(4) 0.044(2) Uani 1 1 d . . . H11D H 0.4999 -0.2905 0.0764 0.053 Uiso 1 1 calc R . . N114 N 0.3612(5) -0.1647(5) 0.1565(3) 0.0278(15) Uani 1 1 d . . . N115 N 0.2637(5) -0.0882(5) 0.1734(3) 0.0272(15) Uani 1 1 d . . . C116 C 0.2173(6) -0.0055(6) 0.1341(3) 0.0301(19) Uani 1 1 d . . . C117 C 0.1041(6) 0.0529(6) 0.1605(3) 0.0314(19) Uani 1 1 d . . . N118 N 0.0737(5) 0.0100(5) 0.2203(3) 0.0311(16) Uani 1 1 d . . . C119 C -0.0287(6) 0.0506(6) 0.2494(4) 0.037(2) Uani 1 1 d . . . H11F H -0.0478 0.0223 0.2918 0.044 Uiso 1 1 calc R . . C120 C -0.1082(7) 0.1341(7) 0.2182(4) 0.045(2) Uani 1 1 d . . . H12B H -0.1815 0.1618 0.2388 0.054 Uiso 1 1 calc R . . C121 C -0.0792(7) 0.1759(7) 0.1572(4) 0.046(2) Uani 1 1 d . . . H12C H -0.1329 0.2325 0.1355 0.055 Uiso 1 1 calc R . . C122 C 0.0270(7) 0.1360(6) 0.1278(4) 0.043(2) Uani 1 1 d . . . H12D H 0.0476 0.1646 0.0857 0.051 Uiso 1 1 calc R . . C123 C 0.2710(6) 0.0255(6) 0.0698(3) 0.0308(19) Uani 1 1 d . . . C124 C 0.3147(7) -0.0456(6) 0.0266(4) 0.045(2) Uani 1 1 d . . . H12E H 0.3077 -0.1161 0.0365 0.054 Uiso 1 1 calc R . . C125 C 0.3685(8) -0.0132(7) -0.0312(4) 0.054(3) Uani 1 1 d . . . H12F H 0.3992 -0.0620 -0.0607 0.065 Uiso 1 1 calc R . . C126 C 0.3775(8) 0.0871(9) -0.0461(4) 0.063(3) Uani 1 1 d . . . H12G H 0.4148 0.1082 -0.0858 0.076 Uiso 1 1 calc R . . C127 C 0.3325(8) 0.1597(7) -0.0035(4) 0.057(3) Uani 1 1 d . . . H12H H 0.3388 0.2303 -0.0144 0.068 Uiso 1 1 calc R . . C128 C 0.2787(7) 0.1295(6) 0.0543(4) 0.040(2) Uani 1 1 d . . . H12I H 0.2471 0.1790 0.0832 0.048 Uiso 1 1 calc R . . C210 C 0.3104(9) 0.3662(7) 0.1340(4) 0.060(3) Uani 1 1 d . . . H21A H 0.2373 0.4148 0.1302 0.072 Uiso 1 1 calc R . . C211 C 0.4010(11) 0.3806(7) 0.0910(5) 0.071(3) Uani 1 1 d . . . H21B H 0.3908 0.4399 0.0588 0.085 Uiso 1 1 calc R . . C212 C 0.5069(10) 0.3083(8) 0.0951(4) 0.067(3) Uani 1 1 d . . . H21C H 0.5696 0.3178 0.0656 0.081 Uiso 1 1 calc R . . N214 N 0.4918(5) 0.0248(5) 0.2182(3) 0.0283(15) Uani 1 1 d . . . N215 N 0.4959(5) -0.0582(5) 0.2678(3) 0.0265(15) Uani 1 1 d . . . C216 C 0.5880(6) -0.1380(6) 0.2724(3) 0.0304(19) Uani 1 1 d . . . C217 C 0.5803(6) -0.2075(6) 0.3334(3) 0.0316(19) Uani 1 1 d . . . N218 N 0.4831(5) -0.1708(5) 0.3717(3) 0.0307(16) Uani 1 1 d . . . C219 C 0.4716(7) -0.2208(6) 0.4307(3) 0.034(2) Uani 1 1 d . . . H21E H 0.4047 -0.1949 0.4573 0.041 Uiso 1 1 calc R . . C220 C 0.5538(8) -0.3090(7) 0.4546(4) 0.049(2) Uani 1 1 d . . . H22B H 0.5436 -0.3428 0.4967 0.059 Uiso 1 1 calc R . . C221 C 0.6520(8) -0.3467(7) 0.4150(4) 0.054(3) Uani 1 1 d . . . H22C H 0.7095 -0.4070 0.4301 0.065 Uiso 1 1 calc R . . C222 C 0.6652(7) -0.2958(6) 0.3537(4) 0.047(2) Uani 1 1 d . . . H22D H 0.7311 -0.3209 0.3262 0.056 Uiso 1 1 calc R . . C223 C 0.6862(6) -0.1546(6) 0.2247(3) 0.035(2) Uani 1 1 d . . . C224 C 0.7444(7) -0.0782(7) 0.2041(4) 0.046(2) Uani 1 1 d . . . H22E H 0.7220 -0.0132 0.2210 0.055 Uiso 1 1 calc R . . C225 C 0.8374(7) -0.0979(8) 0.1577(4) 0.059(3) Uani 1 1 d . . . H22F H 0.8784 -0.0461 0.1429 0.071 Uiso 1 1 calc R . . C226 C 0.8692(8) -0.1941(9) 0.1336(4) 0.064(3) Uani 1 1 d . . . H22G H 0.9326 -0.2076 0.1027 0.076 Uiso 1 1 calc R . . C227 C 0.8116(8) -0.2678(8) 0.1535(4) 0.052(3) Uani 1 1 d . . . H22H H 0.8332 -0.3319 0.1355 0.063 Uiso 1 1 calc R . . C228 C 0.7215(7) -0.2513(6) 0.1995(4) 0.044(2) Uani 1 1 d . . . H22I H 0.6830 -0.3050 0.2145 0.053 Uiso 1 1 calc R . . C323 C 0.5212(8) 0.2215(6) 0.1427(4) 0.048(2) Uani 1 1 d . . . H32D H 0.5934 0.1712 0.1453 0.058 Uiso 1 1 calc R . . P10 P -0.26614(19) 0.0047(2) 0.39920(11) 0.0479(7) Uani 1 1 d . . . F11 F -0.3616(4) -0.0589(4) 0.4136(2) 0.0743(16) Uani 1 1 d . . . F12 F -0.1707(4) 0.0705(4) 0.3850(2) 0.0740(17) Uani 1 1 d . . . F13 F -0.1877(4) -0.0816(4) 0.3572(2) 0.0693(16) Uani 1 1 d . . . F14 F -0.3437(4) 0.0918(4) 0.4408(2) 0.0740(17) Uani 1 1 d . . . F15 F -0.2063(4) -0.0596(4) 0.4610(2) 0.0720(17) Uani 1 1 d . . . F16 F -0.3245(4) 0.0692(4) 0.3367(2) 0.0790(17) Uani 1 1 d . . . P20 P -0.8259(2) -0.3048(3) 0.02241(13) 0.0749(10) Uani 1 1 d . . . F21 F -0.8518(5) -0.2208(5) 0.0725(3) 0.099(2) Uani 1 1 d . . . F22 F -0.8663(5) -0.3861(5) 0.0771(3) 0.095(2) Uani 1 1 d . . . F23 F -0.7856(5) -0.2215(5) -0.0320(3) 0.108(2) Uani 1 1 d . . . F24 F -0.7981(7) -0.3829(6) -0.0266(3) 0.142(3) Uani 1 1 d . . . F25 F -0.9525(4) -0.2622(5) 0.0037(2) 0.0865(19) Uani 1 1 d . . . F26 F -0.6993(5) -0.3462(7) 0.0439(3) 0.142(3) Uani 1 1 d . . . P30 P 0.2901(4) -0.4357(3) 0.41584(16) 0.1032(14) Uani 1 1 d . . . F31 F 0.2438(6) -0.5311(5) 0.4497(3) 0.119(2) Uani 1 1 d . . . F32 F 0.3444(14) -0.3432(7) 0.3802(5) 0.275(8) Uani 1 1 d . . . F33 F 0.1676(12) -0.3647(8) 0.4009(6) 0.263(7) Uani 1 1 d . . . F34 F 0.2902(13) -0.3926(8) 0.4769(4) 0.255(7) Uani 1 1 d . . . F35 F 0.4171(7) -0.5071(6) 0.4243(4) 0.146(3) Uani 1 1 d . . . F36 F 0.2944(9) -0.4790(7) 0.3511(3) 0.171(4) Uani 1 1 d . . . O01 O 0.1107(6) 0.1813(5) 0.3184(4) 0.091(2) Uani 1 1 d . . . C01 C 0.0640(8) 0.1870(5) 0.3838(3) 0.123(5) Uani 1 1 d . . . H01A H 0.1175 0.1375 0.4120 0.185 Uiso 1 1 calc R . . H01B H -0.0093 0.1684 0.3901 0.185 Uiso 1 1 calc R . . H01C H 0.0522 0.2590 0.3933 0.185 Uiso 1 1 calc R . . O02A O -0.1153(6) -0.5147(6) 0.3340(3) 0.114(5) Uiso 0.654(12) 1 d PR A 1 C02A C -0.0470(6) -0.5148(6) 0.3878(3) 0.129(8) Uiso 0.654(12) 1 d PR A 1 O02B O -0.0559(6) -0.4394(6) 0.4192(3) 0.176(15) Uiso 0.346(12) 1 d PR A 2 C02B C -0.0814(6) -0.3317(6) 0.4466(3) 0.122(15) Uiso 0.346(12) 1 d PR A 2 O03A O 0.6759(6) -0.6570(7) 0.3856(3) 0.158(7) Uiso 0.629(14) 1 d PR B 1 C03A C 0.6828(5) -0.5693(7) 0.3661(3) 0.089(7) Uiso 0.629(14) 1 d PR B 1 O03B O 0.7552(5) -0.6816(7) 0.3620(3) 0.132(11) Uiso 0.371(14) 1 d PR B 2 C03B C 0.7011(6) -0.7055(6) 0.3314(3) 0.099(12) Uiso 0.371(14) 1 d PR B 2 O04A O 0.0208(10) -0.6304(9) 0.2519(9) 0.072(6) Uiso 0.61(4) 1 d P C 1 O04B O -0.001(2) -0.6219(19) 0.212(2) 0.120(12) Uiso 0.39(4) 1 d P C 2 O05 O -0.001(2) -0.572(2) 0.1029(14) 0.091(9) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0284(6) 0.0312(6) 0.0151(6) -0.0017(5) -0.0013(4) -0.0040(5) O1 0.022(3) 0.033(3) 0.023(3) 0.000(2) 0.001(2) -0.007(2) Co2 0.0255(6) 0.0324(6) 0.0177(6) -0.0050(5) -0.0013(4) -0.0022(5) O2 0.032(3) 0.025(3) 0.021(3) -0.003(2) -0.005(2) -0.003(2) N11 0.029(4) 0.044(4) 0.020(4) -0.004(3) -0.005(3) -0.014(3) C12 0.035(5) 0.055(6) 0.024(5) 0.000(4) -0.008(4) -0.013(4) C13 0.059(6) 0.052(6) 0.038(5) 0.004(5) -0.009(5) -0.022(5) C14 0.080(7) 0.043(5) 0.040(6) -0.006(5) -0.005(5) -0.032(5) C15 0.062(6) 0.042(5) 0.021(5) -0.011(4) 0.006(4) -0.017(5) C16 0.044(5) 0.037(5) 0.009(4) 0.004(4) -0.010(4) -0.013(4) C17 0.037(5) 0.039(5) 0.014(4) -0.007(4) -0.004(3) 0.000(4) C18 0.047(5) 0.032(5) 0.025(5) -0.003(4) -0.003(4) -0.007(4) C19 0.071(7) 0.047(6) 0.034(5) -0.005(5) 0.000(5) 0.003(5) N21 0.023(4) 0.040(4) 0.022(4) -0.007(3) 0.001(3) -0.007(3) C22 0.046(5) 0.046(5) 0.023(5) -0.006(4) 0.001(4) -0.012(4) C23 0.057(6) 0.052(6) 0.026(5) -0.016(5) -0.007(4) -0.010(5) C24 0.066(7) 0.039(5) 0.052(6) -0.028(5) -0.005(5) -0.008(5) C25 0.060(6) 0.034(5) 0.043(6) -0.014(4) -0.002(5) -0.016(4) C26 0.032(5) 0.029(4) 0.027(5) -0.010(4) -0.002(4) -0.003(4) C27 0.030(5) 0.034(5) 0.028(5) 0.000(4) -0.006(4) -0.007(4) C28 0.052(6) 0.031(5) 0.026(5) -0.009(4) -0.002(4) -0.008(4) C29 0.047(6) 0.029(5) 0.041(5) -0.005(4) -0.007(4) 0.003(4) O31 0.026(3) 0.040(3) 0.018(3) -0.006(2) 0.001(2) -0.006(2) C31 0.036(5) 0.032(5) 0.015(4) 0.000(4) 0.006(4) 0.007(4) O32 0.029(3) 0.041(3) 0.018(3) -0.005(2) 0.002(2) -0.005(3) C32 0.037(5) 0.060(6) 0.014(4) 0.001(4) 0.004(4) -0.010(4) C110 0.079(7) 0.051(6) 0.044(6) -0.003(5) 0.001(6) 0.016(6) C111 0.064(7) 0.045(6) 0.076(8) -0.011(6) 0.000(6) 0.018(5) C112 0.071(7) 0.046(6) 0.047(6) -0.018(5) 0.012(5) 0.009(5) C113 0.053(6) 0.042(5) 0.029(5) -0.003(4) 0.005(4) -0.004(5) N114 0.036(4) 0.030(4) 0.013(3) -0.006(3) -0.001(3) -0.001(3) N115 0.031(4) 0.029(4) 0.021(4) -0.006(3) 0.003(3) -0.006(3) C116 0.032(5) 0.036(5) 0.019(4) -0.001(4) 0.000(4) -0.007(4) C117 0.036(5) 0.039(5) 0.021(5) -0.005(4) -0.002(4) -0.012(4) N118 0.033(4) 0.040(4) 0.018(4) 0.001(3) -0.007(3) -0.007(3) C119 0.024(5) 0.052(5) 0.030(5) -0.007(4) 0.003(4) -0.004(4) C120 0.024(5) 0.058(6) 0.045(6) -0.010(5) -0.005(4) 0.004(4) C121 0.043(6) 0.050(6) 0.036(6) -0.004(5) -0.011(4) 0.004(5) C122 0.045(6) 0.037(5) 0.034(5) 0.005(4) -0.014(4) 0.007(4) C123 0.035(5) 0.038(5) 0.015(4) 0.002(4) -0.002(3) -0.004(4) C124 0.061(6) 0.042(5) 0.024(5) 0.001(4) -0.004(4) -0.004(5) C125 0.071(7) 0.054(6) 0.027(5) -0.006(5) 0.000(5) 0.000(5) C126 0.068(7) 0.089(8) 0.017(5) 0.000(6) 0.002(5) -0.001(6) C127 0.062(6) 0.064(6) 0.041(6) 0.015(5) 0.005(5) -0.028(5) C128 0.053(6) 0.037(5) 0.024(5) 0.004(4) 0.005(4) -0.009(4) C210 0.086(8) 0.042(6) 0.040(6) -0.010(5) -0.009(6) 0.006(5) C211 0.126(10) 0.035(6) 0.041(6) -0.004(5) -0.006(7) -0.005(7) C212 0.095(9) 0.066(7) 0.037(6) -0.006(6) 0.022(6) -0.029(7) N214 0.028(4) 0.026(4) 0.027(4) -0.002(3) -0.002(3) -0.001(3) N215 0.029(4) 0.031(4) 0.017(3) -0.003(3) -0.005(3) -0.004(3) C216 0.029(5) 0.039(5) 0.023(4) -0.013(4) -0.002(4) -0.003(4) C217 0.031(5) 0.036(5) 0.025(5) -0.005(4) -0.006(4) -0.002(4) N218 0.029(4) 0.038(4) 0.019(4) -0.001(3) -0.005(3) 0.001(3) C219 0.039(5) 0.045(5) 0.016(4) -0.001(4) -0.009(4) -0.004(4) C220 0.058(6) 0.052(6) 0.028(5) 0.005(4) -0.010(5) -0.005(5) C221 0.066(7) 0.047(6) 0.038(6) 0.006(5) -0.017(5) 0.004(5) C222 0.044(5) 0.047(5) 0.036(5) -0.003(5) -0.012(4) 0.013(5) C223 0.025(5) 0.052(5) 0.022(4) -0.011(4) -0.004(4) 0.005(4) C224 0.028(5) 0.064(6) 0.043(6) -0.016(5) 0.000(4) -0.003(5) C225 0.037(6) 0.099(8) 0.041(6) -0.008(6) 0.005(5) -0.023(6) C226 0.038(6) 0.109(9) 0.031(6) -0.028(6) 0.007(4) 0.009(6) C227 0.042(6) 0.066(7) 0.042(6) -0.029(5) 0.004(5) 0.007(5) C228 0.038(5) 0.048(5) 0.041(5) -0.012(5) -0.003(4) 0.002(4) C323 0.061(6) 0.042(5) 0.037(5) -0.009(5) 0.015(5) -0.012(5) P10 0.0346(14) 0.0820(18) 0.0301(14) -0.0196(14) 0.0037(11) -0.0163(13) F11 0.051(3) 0.109(4) 0.074(4) -0.016(3) -0.003(3) -0.039(3) F12 0.060(4) 0.113(4) 0.066(4) -0.037(3) 0.019(3) -0.047(3) F13 0.066(4) 0.088(4) 0.052(3) -0.030(3) 0.006(3) -0.010(3) F14 0.055(3) 0.109(4) 0.057(3) -0.041(3) 0.019(3) -0.012(3) F15 0.045(3) 0.128(5) 0.037(3) -0.005(3) -0.005(2) -0.017(3) F16 0.071(4) 0.110(5) 0.041(3) -0.002(3) -0.016(3) 0.000(3) P20 0.0584(19) 0.101(2) 0.0347(16) 0.0059(17) 0.0008(14) 0.0180(17) F21 0.111(5) 0.125(5) 0.056(4) -0.019(4) -0.003(4) -0.021(4) F22 0.115(5) 0.098(5) 0.059(4) 0.021(4) -0.016(4) -0.019(4) F23 0.107(5) 0.157(6) 0.045(4) 0.029(4) -0.007(3) -0.036(5) F24 0.165(7) 0.135(6) 0.108(6) -0.075(5) 0.038(5) 0.001(5) F25 0.063(4) 0.125(5) 0.046(3) -0.005(3) -0.016(3) 0.021(3) F26 0.065(4) 0.214(8) 0.094(5) 0.033(5) -0.023(4) 0.024(5) P30 0.197(4) 0.052(2) 0.058(2) 0.0110(17) -0.058(2) -0.019(3) F31 0.148(7) 0.125(6) 0.080(5) 0.013(4) -0.010(4) -0.045(5) F32 0.56(2) 0.153(8) 0.201(10) 0.137(8) -0.254(13) -0.227(12) F33 0.339(16) 0.138(8) 0.278(14) -0.064(9) -0.206(13) 0.099(10) F34 0.48(2) 0.172(9) 0.109(7) -0.086(7) -0.108(10) 0.003(11) F35 0.155(8) 0.110(6) 0.173(8) 0.021(6) -0.029(6) -0.050(6) F36 0.318(12) 0.165(8) 0.052(5) -0.006(5) -0.039(6) -0.092(8) O01 0.081(5) 0.084(5) 0.093(6) -0.026(5) 0.004(5) 0.005(4) C01 0.089(10) 0.140(12) 0.122(12) -0.052(10) 0.011(9) 0.012(9) _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 N115 1.886(5) . ? Co1 O2 1.898(5) . ? Co1 O31 1.913(4) . ? Co1 O1 1.913(5) . ? Co1 N11 1.919(6) . ? Co1 N118 1.924(6) . ? Co1 Co2 2.8273(15) . ? O1 Co2 1.901(5) . ? Co2 N215 1.881(5) . ? Co2 O32 1.904(4) . ? Co2 N21 1.906(6) . ? Co2 N218 1.909(6) . ? Co2 O2 1.922(5) . ? N11 C12 1.312(9) . ? N11 C16 1.365(9) . ? C12 C13 1.412(10) . ? C13 C14 1.379(11) . ? C14 C15 1.388(11) . ? C15 C16 1.389(10) . ? C16 C17 1.513(10) . ? C17 N114 1.307(8) . ? C17 C18 1.479(10) . ? C18 C113 1.398(10) . ? C18 C19 1.419(10) . ? C19 C110 1.385(11) . ? N21 C22 1.345(9) . ? N21 C26 1.364(8) . ? C22 C23 1.401(10) . ? C23 C24 1.364(10) . ? C24 C25 1.395(10) . ? C25 C26 1.383(10) . ? C26 C27 1.502(10) . ? C27 N214 1.302(8) . ? C27 C28 1.505(10) . ? C28 C323 1.372(10) . ? C28 C29 1.404(10) . ? C29 C210 1.370(10) . ? O31 C31 1.284(9) . ? C31 O32 1.277(9) . ? C31 C32 1.502(9) . ? C110 C111 1.377(11) . ? C111 C112 1.373(11) . ? C112 C113 1.382(10) . ? N114 N115 1.387(7) . ? N115 C116 1.308(8) . ? C116 C117 1.478(10) . ? C116 C123 1.493(9) . ? C117 N118 1.363(8) . ? C117 C122 1.392(10) . ? N118 C119 1.334(8) . ? C119 C120 1.396(10) . ? C120 C121 1.375(10) . ? C121 C122 1.372(10) . ? C123 C124 1.387(10) . ? C123 C128 1.393(9) . ? C124 C125 1.386(10) . ? C125 C126 1.349(11) . ? C126 C127 1.393(12) . ? C127 C128 1.378(10) . ? C210 C211 1.380(12) . ? C211 C212 1.384(13) . ? C212 C323 1.395(11) . ? N214 N215 1.394(7) . ? N215 C216 1.316(8) . ? C216 C223 1.465(9) . ? C216 C217 1.480(10) . ? C217 N218 1.372(8) . ? C217 C222 1.383(10) . ? N218 C219 1.338(8) . ? C219 C220 1.388(10) . ? C220 C221 1.398(11) . ? C221 C222 1.386(10) . ? C223 C224 1.377(10) . ? C223 C228 1.413(10) . ? C224 C225 1.406(10) . ? C225 C226 1.396(12) . ? C226 C227 1.340(12) . ? C227 C228 1.376(10) . ? P10 F11 1.591(5) . ? P10 F15 1.597(5) . ? P10 F14 1.598(5) . ? P10 F13 1.601(5) . ? P10 F16 1.602(5) . ? P10 F12 1.612(5) . ? P20 F24 1.541(7) . ? P20 F25 1.572(6) . ? P20 F22 1.584(6) . ? P20 F26 1.592(7) . ? P20 F23 1.597(6) . ? P20 F21 1.618(7) . ? P30 F34 1.515(8) . ? P30 F31 1.561(7) . ? P30 F33 1.573(11) . ? P30 F36 1.580(8) . ? P30 F35 1.593(9) . ? P30 F32 1.594(9) . ? O01 C01 1.450(9) . ? O02A C02A 1.5095 . ? O02B C02B 1.5738 . ? O03A C03A 1.1927 . ? O03B C03B 1.1249 . ? 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 N115 Co1 O2 93.6(2) . . ? N115 Co1 O31 173.5(2) . . ? O2 Co1 O31 91.6(2) . . ? N115 Co1 O1 92.1(2) . . ? O2 Co1 O1 82.2(2) . . ? O31 Co1 O1 92.53(19) . . ? N115 Co1 N11 84.7(2) . . ? O2 Co1 N11 90.0(2) . . ? O31 Co1 N11 91.4(2) . . ? O1 Co1 N11 171.4(2) . . ? N115 Co1 N118 82.1(3) . . ? O2 Co1 N118 169.8(2) . . ? O31 Co1 N118 93.4(2) . . ? O1 Co1 N118 88.7(2) . . ? N11 Co1 N118 98.7(3) . . ? N115 Co1 Co2 104.74(18) . . ? O2 Co1 Co2 42.58(14) . . ? O31 Co1 Co2 81.74(15) . . ? O1 Co1 Co2 42.00(14) . . ? N11 Co1 Co2 131.33(18) . . ? N118 Co1 Co2 129.64(18) . . ? Co2 O1 Co1 95.7(2) . . ? N215 Co2 O1 95.1(2) . . ? N215 Co2 O32 172.0(2) . . ? O1 Co2 O32 92.1(2) . . ? N215 Co2 N21 84.2(2) . . ? O1 Co2 N21 89.9(2) . . ? O32 Co2 N21 92.5(2) . . ? N215 Co2 N218 81.8(3) . . ? O1 Co2 N218 168.8(2) . . ? O32 Co2 N218 91.7(2) . . ? N21 Co2 N218 100.5(3) . . ? N215 Co2 O2 92.8(2) . . ? O1 Co2 O2 81.9(2) . . ? O32 Co2 O2 91.6(2) . . ? N21 Co2 O2 171.0(2) . . ? N218 Co2 O2 87.5(2) . . ? N215 Co2 Co1 106.12(18) . . ? O1 Co2 Co1 42.32(14) . . ? O32 Co2 Co1 81.52(16) . . ? N21 Co2 Co1 130.96(18) . . ? N218 Co2 Co1 128.19(19) . . ? O2 Co2 Co1 41.93(14) . . ? Co1 O2 Co2 95.5(2) . . ? C12 N11 C16 119.4(7) . . ? C12 N11 Co1 122.3(5) . . ? C16 N11 Co1 118.2(5) . . ? N11 C12 C13 123.3(8) . . ? C14 C13 C12 117.1(8) . . ? C13 C14 C15 120.3(8) . . ? C14 C15 C16 119.0(8) . . ? N11 C16 C15 120.9(7) . . ? N11 C16 C17 120.7(6) . . ? C15 C16 C17 118.4(7) . . ? N114 C17 C18 116.5(7) . . ? N114 C17 C16 125.1(6) . . ? C18 C17 C16 118.2(6) . . ? C113 C18 C19 118.4(7) . . ? C113 C18 C17 120.7(7) . . ? C19 C18 C17 120.8(7) . . ? C110 C19 C18 120.7(8) . . ? C22 N21 C26 118.9(6) . . ? C22 N21 Co2 120.3(5) . . ? C26 N21 Co2 120.2(5) . . ? N21 C22 C23 121.9(7) . . ? C24 C23 C22 119.0(7) . . ? C23 C24 C25 119.6(8) . . ? C26 C25 C24 119.3(7) . . ? N21 C26 C25 121.2(7) . . ? N21 C26 C27 118.8(6) . . ? C25 C26 C27 119.7(7) . . ? N214 C27 C26 127.4(7) . . ? N214 C27 C28 114.5(6) . . ? C26 C27 C28 117.7(6) . . ? C323 C28 C29 120.3(7) . . ? C323 C28 C27 121.0(7) . . ? C29 C28 C27 118.7(7) . . ? C210 C29 C28 119.0(8) . . ? C31 O31 Co1 125.3(5) . . ? O32 C31 O31 125.1(6) . . ? O32 C31 C32 118.1(7) . . ? O31 C31 C32 116.8(7) . . ? C31 O32 Co2 126.1(5) . . ? C111 C110 C19 118.9(9) . . ? C112 C111 C110 121.8(8) . . ? C111 C112 C113 120.0(8) . . ? C112 C113 C18 120.2(8) . . ? C17 N114 N115 112.3(6) . . ? C116 N115 N114 123.3(6) . . ? C116 N115 Co1 116.4(5) . . ? N114 N115 Co1 120.0(4) . . ? N115 C116 C117 112.0(6) . . ? N115 C116 C123 124.1(6) . . ? C117 C116 C123 123.9(7) . . ? N118 C117 C122 120.6(7) . . ? N118 C117 C116 113.1(6) . . ? C122 C117 C116 125.9(7) . . ? C119 N118 C117 120.2(6) . . ? C119 N118 Co1 126.6(5) . . ? C117 N118 Co1 112.5(5) . . ? N118 C119 C120 120.8(7) . . ? C121 C120 C119 119.3(8) . . ? C122 C121 C120 120.1(8) . . ? C121 C122 C117 119.0(7) . . ? C124 C123 C128 120.0(7) . . ? C124 C123 C116 122.4(7) . . ? C128 C123 C116 117.6(7) . . ? C125 C124 C123 119.5(8) . . ? C126 C125 C124 120.6(8) . . ? C125 C126 C127 120.4(8) . . ? C128 C127 C126 120.1(8) . . ? C127 C128 C123 119.3(8) . . ? C29 C210 C211 121.1(9) . . ? C210 C211 C212 119.8(9) . . ? C211 C212 C323 119.7(9) . . ? C27 N214 N215 111.6(6) . . ? C216 N215 N214 120.3(6) . . ? C216 N215 Co2 117.7(5) . . ? N214 N215 Co2 121.9(4) . . ? N215 C216 C223 124.9(7) . . ? N215 C216 C217 110.7(6) . . ? C223 C216 C217 124.3(7) . . ? N218 C217 C222 121.9(7) . . ? N218 C217 C216 113.0(6) . . ? C222 C217 C216 124.9(7) . . ? C219 N218 C217 118.7(6) . . ? C219 N218 Co2 127.7(5) . . ? C217 N218 Co2 112.8(5) . . ? N218 C219 C220 122.6(7) . . ? C219 C220 C221 118.4(7) . . ? C222 C221 C220 119.8(8) . . ? C217 C222 C221 118.7(8) . . ? C224 C223 C228 119.7(7) . . ? C224 C223 C216 121.5(7) . . ? C228 C223 C216 118.8(7) . . ? C223 C224 C225 119.1(8) . . ? C226 C225 C224 119.6(9) . . ? C227 C226 C225 121.1(8) . . ? C226 C227 C228 120.5(8) . . ? C227 C228 C223 120.0(8) . . ? C28 C323 C212 119.9(8) . . ? F11 P10 F15 90.4(3) . . ? F11 P10 F14 89.8(3) . . ? F15 P10 F14 89.8(3) . . ? F11 P10 F13 90.8(3) . . ? F15 P10 F13 90.4(3) . . ? F14 P10 F13 179.3(3) . . ? F11 P10 F16 90.2(3) . . ? F15 P10 F16 179.2(3) . . ? F14 P10 F16 90.7(3) . . ? F13 P10 F16 89.1(3) . . ? F11 P10 F12 179.2(3) . . ? F15 P10 F12 89.8(3) . . ? F14 P10 F12 89.4(3) . . ? F13 P10 F12 90.0(3) . . ? F16 P10 F12 89.6(3) . . ? F24 P20 F25 90.8(4) . . ? F24 P20 F22 93.1(4) . . ? F25 P20 F22 89.1(4) . . ? F24 P20 F26 91.4(5) . . ? F25 P20 F26 177.7(4) . . ? F22 P20 F26 90.0(4) . . ? F24 P20 F23 87.8(4) . . ? F25 P20 F23 90.8(3) . . ? F22 P20 F23 179.1(4) . . ? F26 P20 F23 90.0(4) . . ? F24 P20 F21 178.0(4) . . ? F25 P20 F21 90.1(3) . . ? F22 P20 F21 88.6(3) . . ? F26 P20 F21 87.7(4) . . ? F23 P20 F21 90.5(4) . . ? F34 P30 F31 94.1(6) . . ? F34 P30 F33 94.8(7) . . ? F31 P30 F33 93.3(7) . . ? F34 P30 F36 177.7(8) . . ? F31 P30 F36 87.8(4) . . ? F33 P30 F36 86.4(6) . . ? F34 P30 F35 89.7(6) . . ? F31 P30 F35 89.0(4) . . ? F33 P30 F35 174.8(6) . . ? F36 P30 F35 89.1(5) . . ? F34 P30 F32 87.2(7) . . ? F31 P30 F32 176.6(8) . . ? F33 P30 F32 89.7(7) . . ? F36 P30 F32 90.8(5) . . ? F35 P30 F32 87.9(7) . . ? 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 O01 H01 O1 1.32(7) 1.36(7) 2.638(8) 161(6) . O2 H02A F32 1.09(7) 1.58(7) 2.663(8) 171(6) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.682 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.096 data_ft14 _database_code_CSD 189698 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H44 Ag2 B2 F8 N8 O2' _chemical_formula_weight 1178.29 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.4450(16) _cell_length_b 15.3350(11) _cell_length_c 32.547(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.053(2) _cell_angle_gamma 90.00 _cell_volume 9854.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4736 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 39427 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.1395 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.36 _reflns_number_total 22036 _reflns_number_gt 10162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22036 _refine_ls_number_parameters 1320 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1802 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.1758 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.043 _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 0.21934(3) 0.59385(4) 0.854682(17) 0.04053(16) Uani 1 1 d . . . Ag2 Ag -0.00633(3) 0.51903(3) 0.866317(18) 0.03975(16) Uani 1 1 d . . . Ag3 Ag 0.28621(3) 0.39700(4) 0.642873(17) 0.03975(16) Uani 1 1 d . . . Ag4 Ag 0.51033(3) 0.47032(4) 0.625700(19) 0.04331(17) Uani 1 1 d . . . N101 N 0.1848(3) 0.7002(4) 0.80889(17) 0.0349(14) Uani 1 1 d . . . C102 C 0.2237(4) 0.7667(5) 0.8035(2) 0.0418(19) Uani 1 1 d . . . H10B H 0.2696 0.7669 0.8197 0.050 Uiso 1 1 calc R . . C103 C 0.2019(4) 0.8351(5) 0.7761(2) 0.0431(19) Uani 1 1 d . . . H10E H 0.2320 0.8808 0.7736 0.052 Uiso 1 1 calc R . . C104 C 0.1361(4) 0.8360(4) 0.7524(2) 0.0409(19) Uani 1 1 d . . . H10C H 0.1192 0.8824 0.7333 0.049 Uiso 1 1 calc R . . C105 C 0.0948(4) 0.7675(4) 0.7572(2) 0.0385(18) Uani 1 1 d . . . H10D H 0.0489 0.7663 0.7409 0.046 Uiso 1 1 calc R . . C106 C 0.1202(3) 0.6997(4) 0.78573(19) 0.0281(15) Uani 1 1 d . . . C107 C 0.0764(3) 0.6248(4) 0.79110(18) 0.0239(14) Uani 1 1 d . . . C108 C 0.0023(3) 0.6330(4) 0.7759(2) 0.0289(15) Uani 1 1 d . . . C109 C -0.0305(3) 0.7059(4) 0.7881(2) 0.0341(17) Uani 1 1 d . . . H10A H -0.0046 0.7496 0.8058 0.041 Uiso 1 1 calc R . . C110 C -0.1013(4) 0.7143(5) 0.7742(2) 0.0408(19) Uani 1 1 d . . . H11D H -0.1233 0.7631 0.7826 0.049 Uiso 1 1 calc R . . C111 C -0.1383(4) 0.6517(5) 0.7483(2) 0.045(2) Uani 1 1 d . . . H11C H -0.1861 0.6577 0.7389 0.054 Uiso 1 1 calc R . . C112 C -0.1076(4) 0.5798(5) 0.7356(2) 0.046(2) Uani 1 1 d . . . H11B H -0.1340 0.5371 0.7175 0.055 Uiso 1 1 calc R . . C113 C -0.0378(3) 0.5709(4) 0.7498(2) 0.0346(17) Uani 1 1 d . . . H11A H -0.0168 0.5212 0.7414 0.041 Uiso 1 1 calc R . . N114 N 0.1079(3) 0.5571(3) 0.80861(16) 0.0277(13) Uani 1 1 d . . . N115 N 0.0678(2) 0.4913(3) 0.81813(16) 0.0284(13) Uani 1 1 d . . . C116 C 0.0928(3) 0.4132(4) 0.82245(18) 0.0237(14) Uani 1 1 d . . . C117 C 0.0513(3) 0.3446(4) 0.8370(2) 0.0298(16) Uani 1 1 d . . . N118 N 0.0041(3) 0.3751(3) 0.85629(17) 0.0294(13) Uani 1 1 d . . . C119 C -0.0353(3) 0.3153(5) 0.8686(2) 0.0390(18) Uani 1 1 d . . . H11E H -0.0690 0.3352 0.8818 0.047 Uiso 1 1 calc R . . C120 C -0.0293(4) 0.2274(5) 0.8632(2) 0.0407(18) Uani 1 1 d . . . H12E H -0.0575 0.1876 0.8730 0.049 Uiso 1 1 calc R . . C121 C 0.0176(4) 0.1979(5) 0.8435(2) 0.045(2) Uani 1 1 d . . . H12C H 0.0220 0.1372 0.8389 0.054 Uiso 1 1 calc R . . C122 C 0.0586(4) 0.2573(4) 0.8304(2) 0.0367(17) Uani 1 1 d . . . H12A H 0.0918 0.2378 0.8167 0.044 Uiso 1 1 calc R . . C123 C 0.1576(3) 0.3867(4) 0.8132(2) 0.0313(16) Uani 1 1 d . . . C124 C 0.2031(3) 0.3316(4) 0.8412(2) 0.0352(17) Uani 1 1 d . . . H12B H 0.1920 0.3107 0.8660 0.042 Uiso 1 1 calc R . . C125 C 0.2628(4) 0.3073(5) 0.8334(3) 0.051(2) Uani 1 1 d . . . H12G H 0.2941 0.2721 0.8533 0.061 Uiso 1 1 calc R . . C126 C 0.2773(4) 0.3347(5) 0.7965(3) 0.058(2) Uani 1 1 d . . . H12H H 0.3190 0.3182 0.7910 0.069 Uiso 1 1 calc R . . C127 C 0.2329(4) 0.3850(5) 0.7675(3) 0.057(2) Uani 1 1 d . . . H12F H 0.2429 0.4007 0.7416 0.069 Uiso 1 1 calc R . . C128 C 0.1729(4) 0.4134(4) 0.7759(2) 0.0424(19) Uani 1 1 d . . . H12D H 0.1428 0.4505 0.7564 0.051 Uiso 1 1 calc R . . N201 N 0.2791(3) 0.5031(3) 0.90157(16) 0.0307(13) Uani 1 1 d . . . C202 C 0.3416(3) 0.4768(4) 0.9005(2) 0.0328(16) Uani 1 1 d . . . H20B H 0.3610 0.5007 0.8794 0.039 Uiso 1 1 calc R . . C203 C 0.3785(3) 0.4164(5) 0.9287(2) 0.0447(19) Uani 1 1 d . . . H20C H 0.4229 0.4004 0.9276 0.054 Uiso 1 1 calc R . . C204 C 0.3494(4) 0.3801(5) 0.9584(2) 0.048(2) Uani 1 1 d . . . H20E H 0.3735 0.3376 0.9778 0.058 Uiso 1 1 calc R . . C205 C 0.2851(3) 0.4054(4) 0.9601(2) 0.0387(18) Uani 1 1 d . . . H20A H 0.2642 0.3801 0.9802 0.046 Uiso 1 1 calc R . . C206 C 0.2518(3) 0.4686(4) 0.9318(2) 0.0274(15) Uani 1 1 d . . . C207 C 0.1836(3) 0.5003(4) 0.93348(19) 0.0294(16) Uani 1 1 d . . . C208 C 0.1443(3) 0.4525(5) 0.9585(2) 0.0332(17) Uani 1 1 d . . . C209 C 0.1254(4) 0.3676(5) 0.9497(2) 0.047(2) Uani 1 1 d . . . H20D H 0.1416 0.3366 0.9291 0.056 Uiso 1 1 calc R . . C210 C 0.0822(4) 0.3252(6) 0.9708(3) 0.060(2) Uani 1 1 d . . . H21B H 0.0682 0.2668 0.9640 0.072 Uiso 1 1 calc R . . C211 C 0.0604(4) 0.3709(7) 1.0021(3) 0.068(3) Uani 1 1 d . . . H21D H 0.0302 0.3439 1.0160 0.081 Uiso 1 1 calc R . . C212 C 0.0826(4) 0.4546(6) 1.0128(3) 0.064(3) Uani 1 1 d . . . H21E H 0.0697 0.4842 1.0351 0.076 Uiso 1 1 calc R . . C213 C 0.1237(4) 0.4957(5) 0.9909(2) 0.049(2) Uani 1 1 d . . . H21C H 0.1381 0.5539 0.9980 0.058 Uiso 1 1 calc R . . N214 N 0.1631(3) 0.5712(3) 0.91296(16) 0.0290(13) Uani 1 1 d . . . N215 N 0.0980(3) 0.5965(4) 0.91235(16) 0.0308(13) Uani 1 1 d . . . C216 C 0.0867(3) 0.6802(4) 0.91059(18) 0.0270(15) Uani 1 1 d . . . C217 C 0.0153(3) 0.7057(4) 0.9064(2) 0.0280(15) Uani 1 1 d . . . N218 N -0.0341(2) 0.6481(3) 0.88825(16) 0.0296(13) Uani 1 1 d . . . C219 C -0.0987(3) 0.6700(4) 0.8851(2) 0.0335(17) Uani 1 1 d . . . H21A H -0.1335 0.6302 0.8721 0.040 Uiso 1 1 calc R . . C220 C -0.1163(3) 0.7485(5) 0.9000(2) 0.0392(18) Uani 1 1 d . . . H22B H -0.1627 0.7622 0.8967 0.047 Uiso 1 1 calc R . . C221 C -0.0677(4) 0.8061(4) 0.9194(2) 0.0380(18) Uani 1 1 d . . . H22E H -0.0794 0.8592 0.9308 0.046 Uiso 1 1 calc R . . C222 C -0.0008(3) 0.7857(4) 0.9224(2) 0.0363(17) Uani 1 1 d . . . H22D H 0.0342 0.8256 0.9351 0.044 Uiso 1 1 calc R . . C223 C 0.1378(3) 0.7491(4) 0.9137(2) 0.0302(16) Uani 1 1 d . . . C224 C 0.1249(4) 0.8199(4) 0.8861(2) 0.0407(18) Uani 1 1 d . . . H22A H 0.0823 0.8247 0.8658 0.049 Uiso 1 1 calc R . . C225 C 0.1734(5) 0.8829(5) 0.8879(3) 0.053(2) Uani 1 1 d . . . H22H H 0.1641 0.9303 0.8685 0.064 Uiso 1 1 calc R . . C226 C 0.2339(4) 0.8785(6) 0.9169(3) 0.057(2) Uani 1 1 d . . . H22F H 0.2666 0.9229 0.9179 0.068 Uiso 1 1 calc R . . C227 C 0.2485(4) 0.8104(6) 0.9449(3) 0.052(2) Uani 1 1 d . . . H22G H 0.2910 0.8073 0.9654 0.062 Uiso 1 1 calc R . . C228 C 0.2002(3) 0.7458(5) 0.9429(2) 0.0395(18) Uani 1 1 d . . . H22C H 0.2103 0.6981 0.9622 0.047 Uiso 1 1 calc R . . N301 N 0.5040(3) 0.6115(3) 0.64099(17) 0.0338(14) Uani 1 1 d . . . C302 C 0.5430(3) 0.6721(5) 0.6291(2) 0.0427(19) Uani 1 1 d . . . H30B H 0.5742 0.6537 0.6138 0.051 Uiso 1 1 calc R . . C303 C 0.5400(4) 0.7597(5) 0.6382(2) 0.045(2) Uani 1 1 d . . . H30E H 0.5694 0.8003 0.6300 0.054 Uiso 1 1 calc R . . C304 C 0.4932(4) 0.7871(5) 0.6596(2) 0.045(2) Uani 1 1 d . . . H30D H 0.4894 0.8470 0.6660 0.054 Uiso 1 1 calc R . . C305 C 0.4523(4) 0.7254(4) 0.6712(2) 0.0377(18) Uani 1 1 d . . . H30A H 0.4197 0.7428 0.6857 0.045 Uiso 1 1 calc R . . C306 C 0.4585(3) 0.6384(4) 0.66186(19) 0.0273(15) Uani 1 1 d . . . C307 C 0.4167(3) 0.5686(4) 0.67603(19) 0.0260(15) Uani 1 1 d . . . C308 C 0.3544(3) 0.5956(4) 0.6868(2) 0.0315(16) Uani 1 1 d . . . C309 C 0.3091(4) 0.6504(4) 0.6608(3) 0.046(2) Uani 1 1 d . . . H30C H 0.3196 0.6742 0.6363 0.055 Uiso 1 1 calc R . . C310 C 0.2486(4) 0.6715(5) 0.6695(3) 0.059(2) Uani 1 1 d . . . H31D H 0.2175 0.7086 0.6506 0.071 Uiso 1 1 calc R . . C311 C 0.2329(5) 0.6397(6) 0.7051(4) 0.078(3) Uani 1 1 d . . . H31E H 0.1910 0.6544 0.7109 0.094 Uiso 1 1 calc R . . C312 C 0.2778(5) 0.5867(6) 0.7321(3) 0.072(3) Uani 1 1 d . . . H31B H 0.2675 0.5658 0.7572 0.087 Uiso 1 1 calc R . . C313 C 0.3390(4) 0.5625(4) 0.7234(2) 0.046(2) Uani 1 1 d . . . H31C H 0.3695 0.5244 0.7421 0.055 Uiso 1 1 calc R . . N314 N 0.4420(3) 0.4915(4) 0.67775(15) 0.0295(13) Uani 1 1 d . . . N315 N 0.4001(3) 0.4250(3) 0.68558(17) 0.0296(13) Uani 1 1 d . . . C316 C 0.4308(3) 0.3568(4) 0.70444(19) 0.0233(14) Uani 1 1 d . . . C317 C 0.3865(3) 0.2826(4) 0.7087(2) 0.0257(15) Uani 1 1 d . . . N318 N 0.3196(3) 0.2879(3) 0.68839(17) 0.0329(13) Uani 1 1 d . . . C319 C 0.2794(3) 0.2212(4) 0.6929(2) 0.0368(17) Uani 1 1 d . . . H31A H 0.2327 0.2247 0.6784 0.044 Uiso 1 1 calc R . . C320 C 0.3013(4) 0.1486(5) 0.7169(2) 0.0426(19) Uani 1 1 d . . . H32E H 0.2709 0.1030 0.7190 0.051 Uiso 1 1 calc R . . C321 C 0.3690(4) 0.1441(5) 0.7379(2) 0.045(2) Uani 1 1 d . . . H32H H 0.3859 0.0949 0.7551 0.054 Uiso 1 1 calc R . . C322 C 0.4125(3) 0.2107(4) 0.7340(2) 0.0345(17) Uani 1 1 d . . . H32C H 0.4593 0.2076 0.7483 0.041 Uiso 1 1 calc R . . C323 C 0.5053(3) 0.3505(4) 0.7232(2) 0.0272(15) Uani 1 1 d . . . C324 C 0.5418(3) 0.2828(4) 0.7110(2) 0.0353(17) Uani 1 1 d . . . H32B H 0.5193 0.2410 0.6906 0.042 Uiso 1 1 calc R . . C325 C 0.6108(4) 0.2772(5) 0.7287(2) 0.0424(19) Uani 1 1 d . . . H32F H 0.6360 0.2317 0.7201 0.051 Uiso 1 1 calc R . . C326 C 0.6434(4) 0.3371(5) 0.7587(3) 0.047(2) Uani 1 1 d . . . H32G H 0.6906 0.3318 0.7714 0.056 Uiso 1 1 calc R . . C327 C 0.6074(3) 0.4044(4) 0.7701(2) 0.0337(16) Uani 1 1 d . . . H32D H 0.6299 0.4463 0.7904 0.040 Uiso 1 1 calc R . . C328 C 0.5385(3) 0.4110(4) 0.7522(2) 0.0323(16) Uani 1 1 d . . . H32A H 0.5138 0.4579 0.7600 0.039 Uiso 1 1 calc R . . N401 N 0.5376(3) 0.3393(3) 0.60568(17) 0.0348(14) Uani 1 1 d . . . C402 C 0.6012(3) 0.3141(5) 0.6086(2) 0.0385(18) Uani 1 1 d . . . H40A H 0.6369 0.3527 0.6216 0.046 Uiso 1 1 calc R . . C403 C 0.6180(4) 0.2352(5) 0.5938(2) 0.0380(18) Uani 1 1 d . . . H40C H 0.6642 0.2209 0.5965 0.046 Uiso 1 1 calc R . . C404 C 0.5681(4) 0.1776(5) 0.5752(2) 0.0442(19) Uani 1 1 d . . . H40E H 0.5787 0.1228 0.5649 0.053 Uiso 1 1 calc R . . C405 C 0.5004(4) 0.2022(4) 0.5717(2) 0.0397(18) Uani 1 1 d . . . H40D H 0.4641 0.1644 0.5586 0.048 Uiso 1 1 calc R . . C406 C 0.4875(3) 0.2832(4) 0.5878(2) 0.0290(16) Uani 1 1 d . . . C407 C 0.4154(3) 0.3104(4) 0.58380(19) 0.0284(15) Uani 1 1 d . . . C408 C 0.3638(3) 0.2414(4) 0.5828(2) 0.0293(16) Uani 1 1 d . . . C409 C 0.3790(3) 0.1722(4) 0.6119(2) 0.0324(16) Uani 1 1 d . . . H40B H 0.4229 0.1682 0.6309 0.039 Uiso 1 1 calc R . . C410 C 0.3312(4) 0.1103(4) 0.6131(2) 0.0385(18) Uani 1 1 d . . . H41C H 0.3418 0.0639 0.6330 0.046 Uiso 1 1 calc R . . C411 C 0.2678(4) 0.1154(5) 0.5853(3) 0.043(2) Uani 1 1 d . . . H41D H 0.2346 0.0726 0.5863 0.052 Uiso 1 1 calc R . . C412 C 0.2522(3) 0.1826(5) 0.5560(2) 0.0401(19) Uani 1 1 d . . . H41B H 0.2086 0.1848 0.5367 0.048 Uiso 1 1 calc R . . C413 C 0.2990(3) 0.2467(4) 0.5544(2) 0.0332(17) Uani 1 1 d . . . H41A H 0.2876 0.2934 0.5347 0.040 Uiso 1 1 calc R . . N414 N 0.4062(2) 0.3931(3) 0.58253(16) 0.0273(13) Uani 1 1 d . . . N415 N 0.3404(3) 0.4191(3) 0.58179(16) 0.0314(13) Uani 1 1 d . . . C416 C 0.3209(3) 0.4929(4) 0.5637(2) 0.0303(16) Uani 1 1 d . . . C417 C 0.2521(3) 0.5222(4) 0.5660(2) 0.0289(15) Uani 1 1 d . . . N418 N 0.2259(3) 0.4882(3) 0.59646(16) 0.0315(13) Uani 1 1 d . . . C419 C 0.1636(3) 0.5122(4) 0.5976(2) 0.0380(18) Uani 1 1 d . . . H41E H 0.1449 0.4884 0.6190 0.046 Uiso 1 1 calc R . . C420 C 0.1261(4) 0.5698(5) 0.5690(2) 0.047(2) Uani 1 1 d . . . H42A H 0.0822 0.5860 0.5710 0.056 Uiso 1 1 calc R . . C421 C 0.1515(4) 0.6044(5) 0.5374(3) 0.060(2) Uani 1 1 d . . . H42E H 0.1257 0.6438 0.5170 0.072 Uiso 1 1 calc R . . C422 C 0.2163(4) 0.5796(5) 0.5365(2) 0.049(2) Uani 1 1 d . . . H42C H 0.2358 0.6026 0.5154 0.058 Uiso 1 1 calc R . . C423 C 0.3599(3) 0.5474(5) 0.5413(2) 0.0350(17) Uani 1 1 d . . . C424 C 0.3709(4) 0.6327(5) 0.5525(2) 0.053(2) Uani 1 1 d . . . H42D H 0.3492 0.6578 0.5722 0.063 Uiso 1 1 calc R . . C425 C 0.4141(5) 0.6840(7) 0.5352(3) 0.084(3) Uani 1 1 d . . . H42H H 0.4237 0.7426 0.5442 0.100 Uiso 1 1 calc R . . C426 C 0.4421(5) 0.6485(9) 0.5051(4) 0.099(5) Uani 1 1 d . . . H42F H 0.4704 0.6831 0.4927 0.118 Uiso 1 1 calc R . . C427 C 0.4298(5) 0.5648(8) 0.4931(4) 0.096(4) Uani 1 1 d . . . H42G H 0.4494 0.5415 0.4720 0.116 Uiso 1 1 calc R . . C428 C 0.3894(4) 0.5119(6) 0.5108(3) 0.062(3) Uani 1 1 d . . . H42B H 0.3819 0.4526 0.5024 0.075 Uiso 1 1 calc R . . B10 B -0.0540(6) 0.9607(7) 0.8297(3) 0.058(3) Uani 1 1 d . . . F11 F -0.0232(3) 0.9898(3) 0.87077(15) 0.0818(16) Uani 1 1 d . . . F12 F -0.0063(3) 0.9187(3) 0.81361(17) 0.0819(16) Uani 1 1 d . . . F13 F -0.1065(3) 0.9060(3) 0.83005(14) 0.0769(16) Uani 1 1 d . . . F14 F -0.0762(2) 1.0327(3) 0.80470(15) 0.0607(12) Uani 1 1 d . . . B20 B 0.4544(5) 0.5341(6) 0.8331(3) 0.050(3) Uani 1 1 d . . . F21 F 0.4855(3) 0.5092(3) 0.87501(16) 0.0852(16) Uani 1 1 d . . . F22 F 0.4059(3) 0.5957(3) 0.83326(15) 0.0853(18) Uani 1 1 d . . . F23 F 0.4239(2) 0.4616(3) 0.81124(15) 0.0605(13) Uani 1 1 d . . . F24 F 0.5001(3) 0.5678(3) 0.81325(17) 0.0884(18) Uani 1 1 d . . . B30 B 0.1940(6) 0.5510(7) 0.1605(4) 0.063(3) Uani 1 1 d . . . F31 F 0.1888(2) 0.6393(3) 0.16910(16) 0.0777(15) Uani 1 1 d . . . F32 F 0.2571(3) 0.5376(4) 0.15484(19) 0.119(2) Uani 1 1 d . . . F33 F 0.1485(3) 0.5325(4) 0.1238(3) 0.132(3) Uani 1 1 d . . . F34 F 0.1871(6) 0.5106(5) 0.1939(3) 0.219(6) Uani 1 1 d . . . B40A B 0.6747(13) 0.6623(17) 0.5612(7) 0.039(9) Uiso 0.275(10) 1 d PD A 1 F43A F 0.6763(19) 0.588(2) 0.5730(11) 0.184(16) Uiso 0.275(10) 1 d PD A 1 F41A F 0.729(2) 0.682(3) 0.5529(14) 0.24(3) Uiso 0.275(10) 1 d PD A 1 F42A F 0.6307(19) 0.672(2) 0.5282(10) 0.205(19) Uiso 0.275(10) 1 d PD A 1 F44A F 0.6668(12) 0.7113(15) 0.5882(7) 0.114(10) Uiso 0.275(10) 1 d PD A 1 B40B B 0.7340(11) 0.6448(11) 0.5655(5) 0.145(10) Uani 0.725(10) 1 d PDU A 2 F41B F 0.6710(9) 0.6717(10) 0.5612(9) 0.51(3) Uani 0.725(10) 1 d PDU A 2 F42B F 0.7522(8) 0.5926(7) 0.5977(4) 0.210(9) Uani 0.725(10) 1 d PD A 2 F43B F 0.7379(6) 0.6012(6) 0.5306(3) 0.157(5) Uani 0.725(10) 1 d PD A 2 F44B F 0.7712(6) 0.7162(6) 0.5701(3) 0.152(5) Uani 0.725(10) 1 d PD A 2 O11 O 0.6561(4) 0.5098(4) 0.6350(3) 0.102(3) Uani 1 1 d . . . H11 H 0.6593 0.5467 0.6165 0.153 Uiso 1 1 calc R . . C11 C 0.6915(6) 0.5397(8) 0.6753(3) 0.111(4) Uani 1 1 d . . . H11I H 0.7386 0.5518 0.6754 0.166 Uiso 1 1 calc R . . H11J H 0.6905 0.4950 0.6966 0.166 Uiso 1 1 calc R . . H11K H 0.6703 0.5932 0.6821 0.166 Uiso 1 1 calc R . . O22 O 0.5736(7) 0.4088(6) 0.9306(4) 0.193(5) Uani 1 1 d . . . H22 H 0.5399 0.4315 0.9136 0.289 Uiso 1 1 calc R . . C22 C 0.5944(9) 0.4604(8) 0.9650(4) 0.188(9) Uani 1 1 d . . . H11F H 0.6249 0.5053 0.9593 0.283 Uiso 1 1 calc R . . H11G H 0.6183 0.4251 0.9894 0.283 Uiso 1 1 calc R . . H11H H 0.5550 0.4882 0.9714 0.283 Uiso 1 1 calc R . . O33A O 0.0600(9) 0.0171(15) 0.9493(6) 0.183(9) Uiso 0.66(2) 1 d P B 1 C33A C 0.1177(12) 0.0690(16) 0.9483(8) 0.139(10) Uiso 0.66(2) 1 d P B 1 O33B O 0.061(2) 0.087(3) 0.9465(12) 0.188(16) Uiso 0.34(2) 1 d P B 2 C33B C 0.1302(19) 0.102(2) 0.9932(13) 0.116(17) Uiso 0.34(2) 1 d P B 2 O44A O 0.3074(6) 0.6655(7) 1.0994(4) 0.089(5) Uiso 0.562(11) 1 d P C 1 C44A C 0.254(2) 0.6626(18) 1.0631(12) 0.169(12) Uiso 0.562(11) 1 d P C 1 O44B O 0.1925(10) 0.6860(10) 1.0385(5) 0.095(6) Uiso 0.438(11) 1 d P C 2 C44B C 0.1437(11) 0.6814(13) 1.0563(6) 0.067(7) Uiso 0.438(11) 1 d P C 2 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 0.0261(3) 0.0505(4) 0.0431(3) 0.0169(3) 0.0057(3) -0.0012(3) Ag2 0.0310(3) 0.0305(4) 0.0607(4) -0.0054(3) 0.0172(3) -0.0012(3) Ag3 0.0264(3) 0.0479(4) 0.0428(3) 0.0146(3) 0.0050(3) -0.0025(3) Ag4 0.0337(3) 0.0325(4) 0.0675(4) -0.0078(3) 0.0200(3) -0.0057(3) N101 0.026(3) 0.040(4) 0.041(4) 0.005(3) 0.012(3) -0.010(3) C102 0.028(4) 0.052(5) 0.047(5) 0.009(4) 0.012(4) 0.000(4) C103 0.037(5) 0.037(5) 0.055(5) 0.002(4) 0.010(4) -0.014(4) C104 0.049(5) 0.028(5) 0.048(5) 0.013(3) 0.018(4) 0.000(4) C105 0.037(4) 0.035(5) 0.041(4) 0.009(3) 0.006(3) -0.003(4) C106 0.032(4) 0.027(4) 0.025(4) -0.006(3) 0.008(3) -0.002(3) C107 0.027(4) 0.021(4) 0.024(3) -0.002(3) 0.009(3) -0.003(3) C108 0.024(4) 0.031(4) 0.032(4) 0.000(3) 0.007(3) -0.001(3) C109 0.033(4) 0.037(5) 0.030(4) 0.001(3) 0.004(3) 0.003(3) C110 0.041(5) 0.038(5) 0.051(5) 0.012(4) 0.024(4) 0.015(4) C111 0.026(4) 0.049(6) 0.062(5) 0.014(4) 0.015(4) 0.000(4) C112 0.031(4) 0.035(5) 0.066(5) 0.002(4) 0.005(4) -0.013(4) C113 0.027(4) 0.031(4) 0.043(4) 0.005(3) 0.004(3) -0.007(3) N114 0.026(3) 0.026(3) 0.029(3) -0.001(2) 0.005(2) -0.004(3) N115 0.021(3) 0.024(3) 0.042(3) -0.003(2) 0.010(2) -0.005(3) C116 0.020(3) 0.021(4) 0.026(3) -0.005(3) -0.002(3) -0.002(3) C117 0.029(4) 0.027(4) 0.034(4) 0.000(3) 0.009(3) -0.005(3) N118 0.024(3) 0.017(3) 0.044(3) 0.002(2) 0.004(3) -0.002(2) C119 0.027(4) 0.041(5) 0.046(5) 0.002(3) 0.003(3) -0.003(4) C120 0.041(5) 0.029(5) 0.055(5) 0.012(3) 0.017(4) -0.006(4) C121 0.054(5) 0.023(5) 0.061(5) -0.007(3) 0.022(4) -0.014(4) C122 0.045(5) 0.020(4) 0.048(5) -0.003(3) 0.015(4) -0.005(3) C123 0.025(4) 0.024(4) 0.046(4) -0.014(3) 0.011(3) -0.003(3) C124 0.028(4) 0.036(5) 0.037(4) -0.004(3) 0.002(3) 0.009(3) C125 0.026(4) 0.053(6) 0.066(6) -0.021(4) -0.001(4) 0.002(4) C126 0.037(5) 0.047(6) 0.093(7) -0.012(5) 0.023(5) 0.004(4) C127 0.056(6) 0.042(6) 0.091(7) -0.018(5) 0.051(5) -0.018(4) C128 0.050(5) 0.026(4) 0.056(5) -0.002(3) 0.021(4) -0.007(4) N201 0.025(3) 0.031(3) 0.037(3) 0.003(2) 0.010(3) 0.004(3) C202 0.019(4) 0.031(4) 0.046(4) -0.010(3) 0.005(3) -0.003(3) C203 0.023(4) 0.057(6) 0.048(5) -0.007(4) -0.001(4) 0.011(4) C204 0.047(5) 0.041(5) 0.052(5) 0.005(4) 0.006(4) 0.016(4) C205 0.033(4) 0.040(5) 0.043(4) 0.006(3) 0.009(3) 0.005(4) C206 0.023(4) 0.023(4) 0.035(4) 0.002(3) 0.004(3) 0.002(3) C207 0.020(4) 0.038(5) 0.029(4) -0.001(3) 0.005(3) 0.002(3) C208 0.029(4) 0.036(5) 0.033(4) 0.010(3) 0.006(3) 0.007(3) C209 0.046(5) 0.046(5) 0.042(5) 0.011(4) 0.001(4) -0.011(4) C210 0.045(5) 0.065(6) 0.053(6) 0.023(4) -0.015(4) -0.023(5) C211 0.039(5) 0.101(8) 0.063(6) 0.040(6) 0.013(5) 0.001(5) C212 0.057(6) 0.077(7) 0.066(6) 0.028(5) 0.031(5) 0.024(5) C213 0.059(5) 0.044(5) 0.049(5) 0.013(4) 0.025(4) 0.016(4) N214 0.022(3) 0.028(3) 0.037(3) -0.001(2) 0.007(3) 0.003(3) N215 0.020(3) 0.038(4) 0.033(3) 0.009(3) 0.005(2) 0.000(3) C216 0.023(4) 0.035(5) 0.022(3) 0.005(3) 0.004(3) 0.004(3) C217 0.028(4) 0.019(4) 0.038(4) 0.009(3) 0.011(3) 0.006(3) N218 0.012(3) 0.037(4) 0.038(3) 0.004(3) 0.002(2) 0.000(3) C219 0.026(4) 0.026(4) 0.050(5) 0.004(3) 0.013(3) 0.002(3) C220 0.023(4) 0.044(5) 0.054(5) 0.011(4) 0.016(4) 0.006(4) C221 0.039(5) 0.027(5) 0.050(5) 0.003(3) 0.016(4) 0.007(4) C222 0.025(4) 0.034(5) 0.050(5) 0.005(3) 0.010(3) 0.003(3) C223 0.020(4) 0.032(4) 0.040(4) -0.003(3) 0.011(3) 0.003(3) C224 0.036(5) 0.036(5) 0.052(5) -0.001(4) 0.013(4) 0.001(4) C225 0.064(6) 0.042(5) 0.067(6) -0.004(4) 0.038(5) -0.007(5) C226 0.044(6) 0.055(6) 0.080(7) -0.027(5) 0.032(5) -0.028(5) C227 0.033(5) 0.064(7) 0.060(6) -0.031(5) 0.015(4) -0.009(4) C228 0.032(4) 0.046(5) 0.041(4) -0.008(3) 0.011(4) 0.004(4) N301 0.020(3) 0.038(4) 0.040(3) 0.007(3) 0.001(3) -0.003(3) C302 0.027(4) 0.046(5) 0.052(5) 0.017(4) 0.005(4) -0.004(4) C303 0.050(5) 0.036(5) 0.045(5) 0.011(3) 0.006(4) -0.021(4) C304 0.062(5) 0.024(5) 0.049(5) -0.004(3) 0.016(4) -0.016(4) C305 0.047(5) 0.029(5) 0.039(4) 0.003(3) 0.014(4) -0.012(4) C306 0.027(4) 0.024(4) 0.025(4) -0.001(3) -0.002(3) -0.003(3) C307 0.026(4) 0.022(4) 0.028(4) -0.005(3) 0.004(3) -0.010(3) C308 0.025(4) 0.019(4) 0.049(4) -0.003(3) 0.005(3) -0.004(3) C309 0.040(5) 0.028(5) 0.064(5) -0.010(4) 0.006(4) 0.002(4) C310 0.037(5) 0.053(6) 0.087(7) -0.019(5) 0.014(5) 0.008(4) C311 0.053(6) 0.050(7) 0.145(11) -0.037(6) 0.050(7) -0.018(5) C312 0.087(8) 0.042(6) 0.111(9) -0.017(5) 0.068(7) -0.021(5) C313 0.052(5) 0.037(5) 0.055(5) 0.004(4) 0.025(4) -0.008(4) N314 0.030(3) 0.026(4) 0.027(3) 0.002(2) -0.001(2) -0.006(3) N315 0.023(3) 0.023(4) 0.042(3) -0.001(2) 0.008(3) -0.008(3) C316 0.022(4) 0.018(4) 0.030(4) -0.001(3) 0.008(3) -0.002(3) C317 0.029(4) 0.016(4) 0.035(4) 0.000(3) 0.011(3) -0.001(3) N318 0.027(3) 0.035(4) 0.036(3) -0.001(3) 0.008(3) -0.003(3) C319 0.029(4) 0.040(5) 0.040(4) -0.003(3) 0.007(3) -0.018(4) C320 0.050(5) 0.033(5) 0.051(5) 0.003(4) 0.024(4) -0.010(4) C321 0.045(5) 0.035(5) 0.058(5) 0.009(4) 0.019(4) -0.001(4) C322 0.029(4) 0.028(4) 0.047(4) 0.003(3) 0.010(3) -0.002(3) C323 0.022(4) 0.025(4) 0.034(4) 0.002(3) 0.005(3) -0.002(3) C324 0.032(4) 0.029(4) 0.044(4) -0.002(3) 0.009(3) -0.001(3) C325 0.040(5) 0.037(5) 0.058(5) 0.012(4) 0.026(4) 0.014(4) C326 0.027(4) 0.051(6) 0.063(6) 0.026(4) 0.012(4) 0.002(4) C327 0.028(4) 0.027(4) 0.042(4) 0.004(3) 0.002(3) -0.003(3) C328 0.033(4) 0.027(4) 0.041(4) 0.003(3) 0.017(3) 0.000(3) N401 0.027(3) 0.034(4) 0.045(4) 0.001(3) 0.013(3) -0.001(3) C402 0.022(4) 0.041(5) 0.054(5) 0.010(4) 0.013(4) -0.001(3) C403 0.028(4) 0.035(5) 0.055(5) 0.013(3) 0.017(4) 0.012(4) C404 0.041(5) 0.037(5) 0.058(5) 0.005(4) 0.019(4) 0.006(4) C405 0.039(5) 0.029(5) 0.053(5) 0.003(3) 0.015(4) -0.002(4) C406 0.026(4) 0.027(4) 0.034(4) 0.005(3) 0.007(3) 0.000(3) C407 0.030(4) 0.025(4) 0.031(4) 0.000(3) 0.009(3) -0.002(3) C408 0.034(4) 0.027(4) 0.029(4) -0.010(3) 0.011(3) -0.004(3) C409 0.034(4) 0.030(4) 0.034(4) -0.010(3) 0.011(3) -0.007(3) C410 0.040(5) 0.036(5) 0.042(4) -0.005(3) 0.015(4) -0.010(4) C411 0.036(5) 0.033(5) 0.066(6) -0.021(4) 0.022(4) -0.016(4) C412 0.024(4) 0.050(5) 0.046(5) -0.022(4) 0.008(3) -0.006(4) C413 0.030(4) 0.037(5) 0.032(4) -0.011(3) 0.006(3) -0.002(3) N414 0.020(3) 0.027(4) 0.034(3) 0.004(2) 0.007(2) 0.004(3) N415 0.026(3) 0.029(4) 0.036(3) 0.001(3) 0.002(3) 0.003(3) C416 0.022(4) 0.035(5) 0.031(4) -0.003(3) 0.001(3) -0.001(3) C417 0.029(4) 0.020(4) 0.037(4) 0.003(3) 0.007(3) 0.000(3) N418 0.022(3) 0.033(4) 0.037(3) -0.002(2) 0.005(3) -0.006(3) C419 0.032(4) 0.031(5) 0.055(5) -0.003(3) 0.018(4) 0.000(3) C420 0.029(4) 0.048(5) 0.061(6) -0.009(4) 0.009(4) 0.013(4) C421 0.037(5) 0.081(7) 0.060(6) 0.026(5) 0.006(4) 0.029(5) C422 0.038(5) 0.058(6) 0.050(5) 0.013(4) 0.012(4) 0.007(4) C423 0.026(4) 0.034(5) 0.040(4) 0.017(3) -0.001(3) -0.007(3) C424 0.048(5) 0.062(6) 0.040(5) 0.027(4) -0.004(4) -0.016(4) C425 0.074(8) 0.077(8) 0.078(8) 0.044(6) -0.021(6) -0.029(6) C426 0.044(6) 0.134(11) 0.115(10) 0.096(9) 0.016(6) 0.014(7) C427 0.073(8) 0.123(10) 0.115(9) 0.081(8) 0.063(7) 0.051(8) C428 0.053(5) 0.079(7) 0.062(6) 0.037(5) 0.027(5) 0.025(5) B10 0.076(8) 0.061(8) 0.043(6) -0.004(5) 0.028(6) -0.011(6) F11 0.093(4) 0.089(4) 0.060(3) -0.005(3) 0.014(3) -0.033(3) F12 0.100(4) 0.057(3) 0.102(4) 0.019(3) 0.050(3) 0.036(3) F13 0.115(4) 0.064(3) 0.062(3) -0.018(2) 0.042(3) -0.049(3) F14 0.054(3) 0.041(3) 0.087(4) 0.004(2) 0.018(3) 0.001(2) B20 0.064(7) 0.025(6) 0.071(7) -0.003(5) 0.035(6) 0.012(5) F21 0.098(4) 0.081(4) 0.078(4) 0.007(3) 0.024(3) 0.024(3) F22 0.149(5) 0.050(3) 0.076(4) 0.017(2) 0.062(4) 0.046(3) F23 0.048(3) 0.033(3) 0.098(4) 0.001(2) 0.014(3) -0.006(2) F24 0.102(4) 0.086(4) 0.099(4) -0.030(3) 0.065(4) -0.042(3) B30 0.050(7) 0.041(7) 0.099(9) -0.009(6) 0.023(7) 0.019(6) F31 0.081(4) 0.061(4) 0.090(4) -0.021(3) 0.018(3) 0.000(3) F32 0.065(4) 0.183(7) 0.101(5) -0.055(4) 0.006(3) 0.042(4) F33 0.051(4) 0.109(5) 0.211(8) -0.092(5) -0.012(4) -0.003(3) F34 0.365(14) 0.117(6) 0.269(12) 0.083(7) 0.252(11) 0.082(7) B40B 0.26(2) 0.10(2) 0.088(18) -0.024(16) 0.07(2) 0.02(2) F41B 0.30(3) 0.078(13) 1.23(10) -0.11(3) 0.32(4) -0.023(14) F42B 0.35(2) 0.139(10) 0.197(14) 0.088(9) 0.177(16) 0.091(12) F43B 0.227(13) 0.161(10) 0.087(7) -0.059(6) 0.050(8) -0.052(8) F44B 0.216(13) 0.068(7) 0.189(11) -0.060(6) 0.084(9) -0.079(8) O11 0.094(6) 0.075(5) 0.158(8) -0.049(5) 0.070(6) -0.020(4) C11 0.095(9) 0.132(11) 0.080(8) -0.015(7) -0.022(7) 0.003(8) O22 0.274(16) 0.108(8) 0.147(10) -0.011(7) -0.032(9) 0.021(8) C22 0.39(3) 0.102(11) 0.058(8) -0.032(7) 0.022(11) -0.083(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N201 2.189(5) . ? Ag1 N101 2.199(5) . ? Ag1 N114 2.446(5) . ? Ag1 N214 2.485(5) . ? Ag2 N218 2.227(5) . ? Ag2 N118 2.249(5) . ? Ag2 N115 2.484(5) . ? Ag2 N215 2.559(5) . ? Ag3 N418 2.189(5) . ? Ag3 N318 2.222(5) . ? Ag3 N315 2.420(5) . ? Ag3 N415 2.538(5) . ? Ag4 N401 2.227(5) . ? Ag4 N301 2.233(5) . ? Ag4 N314 2.481(5) . ? Ag4 N414 2.521(5) . ? N101 C102 1.332(8) . ? N101 C106 1.340(8) . ? C102 C103 1.374(9) . ? C103 C104 1.365(9) . ? C104 C105 1.381(9) . ? C105 C106 1.401(8) . ? C106 C107 1.494(8) . ? C107 N114 1.276(7) . ? C107 C108 1.471(8) . ? C108 C113 1.393(9) . ? C108 C109 1.413(8) . ? C109 C110 1.406(9) . ? C110 C111 1.367(10) . ? C111 C112 1.383(9) . ? C112 C113 1.388(9) . ? N114 N115 1.384(6) . ? N115 C116 1.297(7) . ? C116 C123 1.490(8) . ? C116 C117 1.503(8) . ? C117 N118 1.362(7) . ? C117 C122 1.371(8) . ? N118 C119 1.350(8) . ? C119 C120 1.369(9) . ? C120 C121 1.361(9) . ? C121 C122 1.380(9) . ? C123 C128 1.389(9) . ? C123 C124 1.404(9) . ? C124 C125 1.360(9) . ? C125 C126 1.376(11) . ? C126 C127 1.366(11) . ? C127 C128 1.393(9) . ? N201 C202 1.349(7) . ? N201 C206 1.358(7) . ? C202 C203 1.381(9) . ? C203 C204 1.378(10) . ? C204 C205 1.387(9) . ? C205 C206 1.389(8) . ? C206 C207 1.491(8) . ? C207 N214 1.288(8) . ? C207 C208 1.479(8) . ? C208 C209 1.367(9) . ? C208 C213 1.399(9) . ? C209 C210 1.409(10) . ? C210 C211 1.400(12) . ? C211 C212 1.375(11) . ? C212 C213 1.388(10) . ? N214 N215 1.381(6) . ? N215 C216 1.302(7) . ? C216 C223 1.471(9) . ? C216 C217 1.485(8) . ? C217 N218 1.356(8) . ? C217 C222 1.403(8) . ? N218 C219 1.340(7) . ? C219 C220 1.379(9) . ? C220 C221 1.357(9) . ? C221 C222 1.384(8) . ? C223 C228 1.379(9) . ? C223 C224 1.391(9) . ? C224 C225 1.374(9) . ? C225 C226 1.349(11) . ? C226 C227 1.367(11) . ? C227 C228 1.389(9) . ? N301 C302 1.345(8) . ? N301 C306 1.351(8) . ? C302 C303 1.380(9) . ? C303 C304 1.386(10) . ? C304 C305 1.380(8) . ? C305 C306 1.380(8) . ? C306 C307 1.515(8) . ? C307 N314 1.287(7) . ? C307 C308 1.465(8) . ? C308 C309 1.369(9) . ? C308 C313 1.405(9) . ? C309 C310 1.377(10) . ? C310 C311 1.371(12) . ? C311 C312 1.363(13) . ? C312 C313 1.402(11) . ? N314 N315 1.398(6) . ? N315 C316 1.290(7) . ? C316 C317 1.484(8) . ? C316 C323 1.490(8) . ? C317 N318 1.358(7) . ? C317 C322 1.396(8) . ? N318 C319 1.343(7) . ? C319 C320 1.367(9) . ? C320 C321 1.378(9) . ? C321 C322 1.380(9) . ? C323 C328 1.372(8) . ? C323 C324 1.394(8) . ? C324 C325 1.383(9) . ? C325 C326 1.379(10) . ? C326 C327 1.375(9) . ? C327 C328 1.382(8) . ? N401 C402 1.337(8) . ? N401 C406 1.348(8) . ? C402 C403 1.378(9) . ? C403 C404 1.366(9) . ? C404 C405 1.411(9) . ? C405 C406 1.400(9) . ? C406 C407 1.504(8) . ? C407 N414 1.281(7) . ? C407 C408 1.489(8) . ? C408 C409 1.402(9) . ? C408 C413 1.407(8) . ? C409 C410 1.371(8) . ? C410 C411 1.376(9) . ? C411 C412 1.384(10) . ? C412 C413 1.381(9) . ? N414 N415 1.396(7) . ? N415 C416 1.291(8) . ? C416 C423 1.472(8) . ? C416 C417 1.498(8) . ? C417 N418 1.349(7) . ? C417 C422 1.365(9) . ? N418 C419 1.335(7) . ? C419 C420 1.366(9) . ? C420 C421 1.374(10) . ? C421 C422 1.385(9) . ? C423 C424 1.361(10) . ? C423 C428 1.399(10) . ? C424 C425 1.405(11) . ? C425 C426 1.370(14) . ? C426 C427 1.345(15) . ? C427 C428 1.386(11) . ? B10 F13 1.365(10) . ? B10 F14 1.376(11) . ? B10 F12 1.380(10) . ? B10 F11 1.395(10) . ? B20 F24 1.368(10) . ? B20 F22 1.370(9) . ? B20 F23 1.379(10) . ? B20 F21 1.400(11) . ? B30 F34 1.290(13) . ? B30 F33 1.341(13) . ? B30 F32 1.367(11) . ? B30 F31 1.391(10) . ? B40A F44A 1.20(3) . ? B40A F43A 1.20(3) . ? B40A F42A 1.22(3) . ? B40A F41A 1.24(3) . ? B40B F42B 1.296(16) . ? B40B F44B 1.318(17) . ? B40B F41B 1.325(18) . ? B40B F43B 1.338(15) . ? O11 C11 1.402(10) . ? O22 C22 1.346(12) . ? O33A C33A 1.43(3) . ? O33B C33B 1.80(5) . ? O44A C44A 1.38(4) . ? O44B C44B 1.28(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 N201 Ag1 N101 165.32(19) . . ? N201 Ag1 N114 122.89(19) . . ? N101 Ag1 N114 70.82(19) . . ? N201 Ag1 N214 70.39(18) . . ? N101 Ag1 N214 119.34(18) . . ? N114 Ag1 N214 83.88(17) . . ? N218 Ag2 N118 163.78(18) . . ? N218 Ag2 N115 127.06(18) . . ? N118 Ag2 N115 69.15(18) . . ? N218 Ag2 N215 69.10(18) . . ? N118 Ag2 N215 116.38(18) . . ? N115 Ag2 N215 84.07(16) . . ? N418 Ag3 N318 164.16(19) . . ? N418 Ag3 N315 124.63(18) . . ? N318 Ag3 N315 70.58(19) . . ? N418 Ag3 N415 69.89(18) . . ? N318 Ag3 N415 120.12(18) . . ? N315 Ag3 N415 82.84(17) . . ? N401 Ag4 N301 166.75(19) . . ? N401 Ag4 N314 123.08(18) . . ? N301 Ag4 N314 69.22(18) . . ? N401 Ag4 N414 69.67(19) . . ? N301 Ag4 N414 119.34(18) . . ? N314 Ag4 N414 84.16(16) . . ? C102 N101 C106 117.7(6) . . ? C102 N101 Ag1 124.0(5) . . ? C106 N101 Ag1 118.2(4) . . ? N101 C102 C103 124.4(7) . . ? C104 C103 C102 118.7(7) . . ? C103 C104 C105 118.0(7) . . ? C104 C105 C106 120.5(7) . . ? N101 C106 C105 120.6(6) . . ? N101 C106 C107 118.1(6) . . ? C105 C106 C107 121.2(6) . . ? N114 C107 C108 125.1(6) . . ? N114 C107 C106 115.5(6) . . ? C108 C107 C106 119.4(6) . . ? C113 C108 C109 117.7(6) . . ? C113 C108 C107 122.5(6) . . ? C109 C108 C107 119.8(6) . . ? C110 C109 C108 120.4(6) . . ? C111 C110 C109 119.5(7) . . ? C110 C111 C112 121.4(7) . . ? C111 C112 C113 119.2(7) . . ? C112 C113 C108 121.8(7) . . ? C107 N114 N115 115.7(5) . . ? C107 N114 Ag1 111.6(4) . . ? N115 N114 Ag1 122.8(4) . . ? C116 N115 N114 117.2(5) . . ? C116 N115 Ag2 112.2(4) . . ? N114 N115 Ag2 120.7(4) . . ? N115 C116 C123 125.2(6) . . ? N115 C116 C117 116.2(5) . . ? C123 C116 C117 118.6(5) . . ? N118 C117 C122 121.8(6) . . ? N118 C117 C116 115.5(5) . . ? C122 C117 C116 122.6(6) . . ? C119 N118 C117 116.9(6) . . ? C119 N118 Ag2 122.5(4) . . ? C117 N118 Ag2 120.6(4) . . ? N118 C119 C120 123.3(7) . . ? C121 C120 C119 119.1(6) . . ? C120 C121 C122 119.0(7) . . ? C117 C122 C121 119.7(7) . . ? C128 C123 C124 118.8(6) . . ? C128 C123 C116 120.7(6) . . ? C124 C123 C116 120.4(6) . . ? C125 C124 C123 121.3(7) . . ? C124 C125 C126 119.0(8) . . ? C127 C126 C125 121.3(7) . . ? C126 C127 C128 120.2(8) . . ? C123 C128 C127 119.2(7) . . ? C202 N201 C206 118.3(5) . . ? C202 N201 Ag1 122.2(4) . . ? C206 N201 Ag1 119.5(4) . . ? N201 C202 C203 122.7(6) . . ? C204 C203 C202 118.5(6) . . ? C203 C204 C205 120.1(7) . . ? C204 C205 C206 118.3(6) . . ? N201 C206 C205 122.0(6) . . ? N201 C206 C207 117.7(5) . . ? C205 C206 C207 120.3(6) . . ? N214 C207 C208 123.7(6) . . ? N214 C207 C206 116.0(5) . . ? C208 C207 C206 120.3(6) . . ? C209 C208 C213 118.9(7) . . ? C209 C208 C207 121.5(6) . . ? C213 C208 C207 119.5(7) . . ? C208 C209 C210 121.1(8) . . ? C211 C210 C209 118.8(8) . . ? C212 C211 C210 120.3(8) . . ? C211 C212 C213 119.8(8) . . ? C212 C213 C208 120.9(8) . . ? C207 N214 N215 115.3(5) . . ? C207 N214 Ag1 111.2(4) . . ? N215 N214 Ag1 125.8(4) . . ? C216 N215 N214 115.9(5) . . ? C216 N215 Ag2 108.7(4) . . ? N214 N215 Ag2 122.1(4) . . ? N215 C216 C223 126.2(6) . . ? N215 C216 C217 115.0(6) . . ? C223 C216 C217 118.8(6) . . ? N218 C217 C222 120.8(6) . . ? N218 C217 C216 118.2(6) . . ? C222 C217 C216 121.0(6) . . ? C219 N218 C217 118.5(6) . . ? C219 N218 Ag2 121.8(4) . . ? C217 N218 Ag2 119.7(4) . . ? N218 C219 C220 122.2(6) . . ? C221 C220 C219 120.4(6) . . ? C220 C221 C222 118.4(7) . . ? C221 C222 C217 119.6(7) . . ? C228 C223 C224 117.5(7) . . ? C228 C223 C216 122.2(6) . . ? C224 C223 C216 120.3(6) . . ? C225 C224 C223 120.4(8) . . ? C226 C225 C224 121.0(8) . . ? C225 C226 C227 120.4(8) . . ? C226 C227 C228 119.0(8) . . ? C223 C228 C227 121.6(7) . . ? C302 N301 C306 118.0(6) . . ? C302 N301 Ag4 122.2(5) . . ? C306 N301 Ag4 119.7(4) . . ? N301 C302 C303 123.3(7) . . ? C302 C303 C304 118.5(7) . . ? C305 C304 C303 118.4(7) . . ? C304 C305 C306 120.4(7) . . ? N301 C306 C305 121.4(6) . . ? N301 C306 C307 117.0(6) . . ? C305 C306 C307 121.6(6) . . ? N314 C307 C308 127.9(6) . . ? N314 C307 C306 114.2(5) . . ? C308 C307 C306 117.9(6) . . ? C309 C308 C313 118.8(7) . . ? C309 C308 C307 121.0(6) . . ? C313 C308 C307 120.1(6) . . ? C308 C309 C310 121.1(8) . . ? C311 C310 C309 120.7(9) . . ? C312 C311 C310 119.4(9) . . ? C311 C312 C313 121.0(9) . . ? C312 C313 C308 118.9(8) . . ? C307 N314 N315 114.8(5) . . ? C307 N314 Ag4 112.5(4) . . ? N315 N314 Ag4 120.7(4) . . ? C316 N315 N314 115.6(5) . . ? C316 N315 Ag3 114.0(4) . . ? N314 N315 Ag3 124.7(4) . . ? N315 C316 C317 115.7(6) . . ? N315 C316 C323 124.5(5) . . ? C317 C316 C323 119.7(5) . . ? N318 C317 C322 121.0(6) . . ? N318 C317 C316 118.0(5) . . ? C322 C317 C316 120.9(6) . . ? C319 N318 C317 118.0(6) . . ? C319 N318 Ag3 123.7(5) . . ? C317 N318 Ag3 117.8(4) . . ? N318 C319 C320 124.3(7) . . ? C319 C320 C321 117.5(7) . . ? C320 C321 C322 120.4(7) . . ? C321 C322 C317 118.8(6) . . ? C328 C323 C324 119.7(6) . . ? C328 C323 C316 120.5(6) . . ? C324 C323 C316 119.9(6) . . ? C325 C324 C323 119.5(7) . . ? C326 C325 C324 120.4(7) . . ? C327 C326 C325 119.9(7) . . ? C326 C327 C328 120.0(7) . . ? C323 C328 C327 120.6(6) . . ? C402 N401 C406 117.5(6) . . ? C402 N401 Ag4 123.6(5) . . ? C406 N401 Ag4 118.9(4) . . ? N401 C402 C403 123.8(7) . . ? C404 C403 C402 119.8(6) . . ? C403 C404 C405 117.9(7) . . ? C406 C405 C404 118.8(7) . . ? N401 C406 C405 122.2(6) . . ? N401 C406 C407 118.5(6) . . ? C405 C406 C407 119.2(6) . . ? N414 C407 C408 127.2(6) . . ? N414 C407 C406 114.3(6) . . ? C408 C407 C406 118.5(6) . . ? C409 C408 C413 119.5(6) . . ? C409 C408 C407 119.4(6) . . ? C413 C408 C407 121.0(6) . . ? C410 C409 C408 120.6(7) . . ? C409 C410 C411 120.0(7) . . ? C410 C411 C412 120.2(7) . . ? C413 C412 C411 121.2(7) . . ? C412 C413 C408 118.5(7) . . ? C407 N414 N415 114.7(5) . . ? C407 N414 Ag4 110.5(4) . . ? N415 N414 Ag4 123.1(4) . . ? C416 N415 N414 116.1(5) . . ? C416 N415 Ag3 109.2(4) . . ? N414 N415 Ag3 124.2(4) . . ? N415 C416 C423 125.6(6) . . ? N415 C416 C417 115.0(6) . . ? C423 C416 C417 119.4(6) . . ? N418 C417 C422 121.5(6) . . ? N418 C417 C416 118.6(6) . . ? C422 C417 C416 119.9(6) . . ? C419 N418 C417 118.5(6) . . ? C419 N418 Ag3 121.8(4) . . ? C417 N418 Ag3 119.7(4) . . ? N418 C419 C420 122.1(6) . . ? C419 C420 C421 120.3(7) . . ? C420 C421 C422 117.2(7) . . ? C417 C422 C421 120.3(7) . . ? C424 C423 C428 119.6(7) . . ? C424 C423 C416 119.0(7) . . ? C428 C423 C416 121.2(7) . . ? C423 C424 C425 120.5(9) . . ? C426 C425 C424 119.1(10) . . ? C427 C426 C425 120.4(10) . . ? C426 C427 C428 121.7(10) . . ? C427 C428 C423 118.6(9) . . ? F13 B10 F14 111.0(9) . . ? F13 B10 F12 110.6(8) . . ? F14 B10 F12 107.9(7) . . ? F13 B10 F11 110.4(7) . . ? F14 B10 F11 107.9(8) . . ? F12 B10 F11 109.0(9) . . ? F24 B20 F22 109.0(7) . . ? F24 B20 F23 109.5(7) . . ? F22 B20 F23 109.1(8) . . ? F24 B20 F21 111.7(8) . . ? F22 B20 F21 109.3(7) . . ? F23 B20 F21 108.3(7) . . ? F34 B30 F33 116.6(11) . . ? F34 B30 F32 110.8(10) . . ? F33 B30 F32 107.9(9) . . ? F34 B30 F31 105.6(9) . . ? F33 B30 F31 108.3(8) . . ? F32 B30 F31 107.3(9) . . ? F44A B40A F43A 111.0(18) . . ? F44A B40A F42A 111.3(19) . . ? F43A B40A F42A 110.4(19) . . ? F44A B40A F41A 107.9(19) . . ? F43A B40A F41A 110.2(19) . . ? F42A B40A F41A 105.9(18) . . ? F42B B40B F44B 112.6(15) . . ? F42B B40B F41B 110.2(16) . . ? F44B B40B F41B 105.6(14) . . ? F42B B40B F43B 108.1(14) . . ? F44B B40B F43B 110.6(14) . . ? F41B B40B F43B 109.7(16) . . ? 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 O11 H11 F43A 0.84 1.67 2.47(3) 159.3 . O11 H11 F42B 0.84 2.25 2.860(14) 129.2 . O11 H11 F44A 0.84 2.71 3.48(2) 153.4 . O11 H11 F41B 0.84 2.68 3.52(3) 176.6 . O22 H22 F21 0.84 1.87 2.683(11) 161.6 . _diffrn_measured_fraction_theta_max 0.813 _diffrn_reflns_theta_full 29.36 _diffrn_measured_fraction_theta_full 0.813 _refine_diff_density_max 0.877 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.105 data_ft15 _database_code_CSD 189699 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 F12 N8 Ni P2' _chemical_formula_weight 1073.50 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.787(2) _cell_length_b 15.172(2) _cell_length_c 19.527(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.6600(10) _cell_angle_gamma 90.00 _cell_volume 4563.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6428 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour topaz _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 20867 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_sigmaI/netI 0.1531 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.00 _reflns_number_total 7133 _reflns_number_gt 3881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7133 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1556 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.004 _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 Ni1 Ni -0.74269(4) -0.13989(4) 0.04001(4) 0.0244(2) Uani 1 1 d . . . N101 N -0.8571(3) -0.1890(3) 0.0615(2) 0.0256(12) Uani 1 1 d . . . C102 C -0.9300(3) -0.1436(4) 0.0613(3) 0.0367(16) Uani 1 1 d . . . H10A H -0.9383 -0.0889 0.0371 0.044 Uiso 1 1 calc R . . C103 C -0.9937(4) -0.1728(4) 0.0946(4) 0.0475(19) Uani 1 1 d . . . H10C H -1.0449 -0.1392 0.0929 0.057 Uiso 1 1 calc R . . C104 C -0.9809(4) -0.2513(4) 0.1300(3) 0.0428(17) Uani 1 1 d . . . H10E H -1.0232 -0.2722 0.1541 0.051 Uiso 1 1 calc R . . C105 C -0.9072(3) -0.3000(4) 0.1310(3) 0.0390(17) Uani 1 1 d . . . H10D H -0.8984 -0.3550 0.1549 0.047 Uiso 1 1 calc R . . C106 C -0.8457(3) -0.2673(4) 0.0962(3) 0.0275(14) Uani 1 1 d . . . C107 C -0.7632(3) -0.3133(4) 0.0961(3) 0.0270(14) Uani 1 1 d . . . C108 C -0.7514(4) -0.4075(4) 0.1160(3) 0.0289(15) Uani 1 1 d . . . C109 C -0.8146(4) -0.4691(4) 0.0879(4) 0.0472(19) Uani 1 1 d . . . H10B H -0.8656 -0.4512 0.0552 0.057 Uiso 1 1 calc R . . C110 C -0.8032(4) -0.5566(4) 0.1075(4) 0.063(2) Uani 1 1 d . . . H11G H -0.8458 -0.5991 0.0877 0.076 Uiso 1 1 calc R . . C111 C -0.7286(5) -0.5826(5) 0.1567(4) 0.063(2) Uani 1 1 d . . . H11E H -0.7215 -0.6424 0.1713 0.076 Uiso 1 1 calc R . . C112 C -0.6656(5) -0.5214(5) 0.1840(4) 0.0527(19) Uani 1 1 d . . . H11F H -0.6148 -0.5393 0.2168 0.063 Uiso 1 1 calc R . . C113 C -0.6763(4) -0.4345(4) 0.1638(3) 0.0375(16) Uani 1 1 d . . . H11A H -0.6325 -0.3927 0.1823 0.045 Uiso 1 1 calc R . . N114 N -0.7044(3) -0.2627(3) 0.0761(2) 0.0239(11) Uani 1 1 d . . . N115 N -0.6345(3) -0.3103(3) 0.0632(2) 0.0287(12) Uani 1 1 d . . . C116 C -0.5652(3) -0.2659(4) 0.0590(3) 0.0269(14) Uani 1 1 d . . . C117 C -0.5453(3) -0.1696(4) 0.0716(3) 0.0294(15) Uani 1 1 d . . . N118 N -0.6090(3) -0.1086(3) 0.0484(2) 0.0262(12) Uani 1 1 d . . . C119 C -0.5850(4) -0.0233(4) 0.0578(3) 0.0327(15) Uani 1 1 d . . . H11B H -0.6272 0.0202 0.0397 0.039 Uiso 1 1 calc R . . C120 C -0.5037(4) 0.0053(4) 0.0916(3) 0.0343(16) Uani 1 1 d . . . H12C H -0.4905 0.0663 0.0966 0.041 Uiso 1 1 calc R . . C121 C -0.4422(4) -0.0574(4) 0.1180(3) 0.0362(16) Uani 1 1 d . . . H12B H -0.3861 -0.0397 0.1429 0.043 Uiso 1 1 calc R . . C122 C -0.4617(3) -0.1461(4) 0.1083(3) 0.0369(16) Uani 1 1 d . . . H12A H -0.4196 -0.1899 0.1260 0.044 Uiso 1 1 calc R . . C123 C -0.4934(3) -0.3213(4) 0.0441(3) 0.0294(15) Uani 1 1 d . . . C124 C -0.4421(4) -0.2915(4) -0.0010(3) 0.0448(18) Uani 1 1 d . . . H12D H -0.4522 -0.2344 -0.0210 0.054 Uiso 1 1 calc R . . C125 C -0.3769(4) -0.3431(5) -0.0174(3) 0.055(2) Uani 1 1 d . . . H12I H -0.3432 -0.3218 -0.0487 0.067 Uiso 1 1 calc R . . C126 C -0.3614(4) -0.4248(5) 0.0117(4) 0.053(2) Uani 1 1 d . . . H12G H -0.3156 -0.4597 0.0017 0.064 Uiso 1 1 calc R . . C127 C -0.4120(4) -0.4576(4) 0.0557(3) 0.0458(18) Uani 1 1 d . . . H12H H -0.4019 -0.5153 0.0746 0.055 Uiso 1 1 calc R . . C128 C -0.4773(4) -0.4060(4) 0.0721(3) 0.0374(16) Uani 1 1 d . . . H12F H -0.5114 -0.4284 0.1027 0.045 Uiso 1 1 calc R . . N201 N -0.7263(3) -0.0707(3) 0.1345(2) 0.0254(11) Uani 1 1 d . . . C202 C -0.6710(3) -0.1037(4) 0.1911(3) 0.0326(15) Uani 1 1 d . . . H20C H -0.6488 -0.1613 0.1875 0.039 Uiso 1 1 calc R . . C203 C -0.6441(3) -0.0592(4) 0.2545(3) 0.0349(16) Uani 1 1 d . . . H20B H -0.6041 -0.0853 0.2926 0.042 Uiso 1 1 calc R . . C204 C -0.6772(3) 0.0237(4) 0.2602(3) 0.0381(16) Uani 1 1 d . . . H20E H -0.6603 0.0566 0.3024 0.046 Uiso 1 1 calc R . . C205 C -0.7360(3) 0.0581(4) 0.2030(3) 0.0364(16) Uani 1 1 d . . . H20A H -0.7603 0.1148 0.2066 0.044 Uiso 1 1 calc R . . C206 C -0.7597(3) 0.0114(4) 0.1408(3) 0.0259(14) Uani 1 1 d . . . C207 C -0.8222(3) 0.0529(3) 0.0802(3) 0.0281(15) Uani 1 1 d . . . C208 C -0.8846(3) 0.1187(4) 0.0982(3) 0.0316(15) Uani 1 1 d . . . C209 C -0.9331(4) 0.0984(4) 0.1471(3) 0.0396(17) Uani 1 1 d . . . H20D H -0.9234 0.0443 0.1720 0.048 Uiso 1 1 calc R . . C210 C -0.9962(4) 0.1567(5) 0.1601(4) 0.0482(19) Uani 1 1 d . . . H21E H -1.0302 0.1418 0.1930 0.058 Uiso 1 1 calc R . . C211 C -1.0087(4) 0.2351(5) 0.1254(4) 0.055(2) Uani 1 1 d . . . H21G H -1.0515 0.2749 0.1343 0.066 Uiso 1 1 calc R . . C212 C -0.9592(4) 0.2577(4) 0.0767(4) 0.0484(19) Uani 1 1 d . . . H21C H -0.9687 0.3123 0.0524 0.058 Uiso 1 1 calc R . . C213 C -0.8967(3) 0.2003(4) 0.0642(3) 0.0415(18) Uani 1 1 d . . . H21B H -0.8616 0.2162 0.0323 0.050 Uiso 1 1 calc R . . N214 N -0.8314(3) 0.0419(3) 0.0129(3) 0.0302(12) Uani 1 1 d . . . N215 N -0.7875(3) -0.0266(3) -0.0107(2) 0.0243(11) Uani 1 1 d . . . C216 C -0.7851(3) -0.0230(3) -0.0780(3) 0.0264(14) Uani 1 1 d . . . C217 C -0.7629(3) -0.1081(3) -0.1076(3) 0.0257(14) Uani 1 1 d . . . N218 N -0.7584(3) -0.1784(3) -0.0638(2) 0.0236(11) Uani 1 1 d . . . C219 C -0.7509(3) -0.2585(4) -0.0900(3) 0.0313(15) Uani 1 1 d . . . H21F H -0.7479 -0.3078 -0.0595 0.038 Uiso 1 1 calc R . . C220 C -0.7470(3) -0.2737(4) -0.1592(3) 0.0344(16) Uani 1 1 d . . . H22G H -0.7465 -0.3321 -0.1767 0.041 Uiso 1 1 calc R . . C221 C -0.7441(3) -0.2021(4) -0.2021(3) 0.0358(16) Uani 1 1 d . . . H22J H -0.7368 -0.2102 -0.2487 0.043 Uiso 1 1 calc R . . C222 C -0.7519(3) -0.1170(4) -0.1759(3) 0.0331(16) Uani 1 1 d . . . H22C H -0.7498 -0.0666 -0.2043 0.040 Uiso 1 1 calc R . . C223 C -0.8042(3) 0.0581(3) -0.1216(3) 0.0253(14) Uani 1 1 d . . . C224 C -0.8616(3) 0.0565(4) -0.1879(3) 0.0328(15) Uani 1 1 d . . . H22E H -0.8902 0.0033 -0.2053 0.039 Uiso 1 1 calc R . . C225 C -0.8761(4) 0.1326(4) -0.2275(3) 0.0414(16) Uani 1 1 d . . . H22B H -0.9147 0.1311 -0.2722 0.050 Uiso 1 1 calc R . . C226 C -0.8355(4) 0.2110(4) -0.2032(4) 0.0415(18) Uani 1 1 d . . . H22F H -0.8461 0.2628 -0.2312 0.050 Uiso 1 1 calc R . . C227 C -0.7793(4) 0.2136(4) -0.1380(4) 0.0434(18) Uani 1 1 d . . . H22D H -0.7508 0.2671 -0.1215 0.052 Uiso 1 1 calc R . . C228 C -0.7645(3) 0.1382(4) -0.0965(3) 0.0337(15) Uani 1 1 d . . . H22A H -0.7275 0.1409 -0.0511 0.040 Uiso 1 1 calc R . . P10 P -0.46860(10) -0.28770(11) 0.29087(10) 0.0393(5) Uani 1 1 d . . . F11 F -0.4601(2) -0.1853(2) 0.3113(2) 0.0628(12) Uani 1 1 d . . . F12 F -0.4794(2) -0.39011(19) 0.27093(18) 0.0509(10) Uani 1 1 d . . . F13 F -0.3949(2) -0.2780(2) 0.2468(2) 0.0694(12) Uani 1 1 d . . . F14 F -0.5415(2) -0.2634(2) 0.22189(19) 0.0618(11) Uani 1 1 d . . . F15 F -0.5424(2) -0.2971(2) 0.3351(2) 0.0575(11) Uani 1 1 d . . . F16 F -0.39663(19) -0.3127(2) 0.35998(18) 0.0527(10) Uani 1 1 d . . . P20 P -0.10126(12) -0.00597(11) 0.63970(11) 0.0474(5) Uani 1 1 d . . . F21 F -0.1041(3) -0.0750(2) 0.5781(2) 0.0764(13) Uani 1 1 d . A . F22 F -0.0980(2) 0.0631(3) 0.7014(2) 0.0871(15) Uani 1 1 d . A . F23A F -0.0142(4) -0.0493(4) 0.6845(3) 0.093(3) Uani 0.903(10) 1 d P A 1 F24A F -0.0451(6) 0.0583(5) 0.6053(4) 0.142(4) Uani 0.903(10) 1 d P A 1 F25A F -0.1872(4) 0.0384(4) 0.5960(4) 0.107(3) Uani 0.903(10) 1 d P A 1 F26A F -0.1562(4) -0.0718(3) 0.6745(3) 0.089(2) Uani 0.903(10) 1 d P A 1 F23B F -0.005(3) 0.005(3) 0.634(3) 0.055(16) Uiso 0.097(10) 1 d P A 2 F24B F -0.113(3) 0.078(2) 0.5856(19) 0.030(12) Uiso 0.097(10) 1 d P A 2 F25B F -0.195(3) -0.001(3) 0.636(2) 0.045(15) Uiso 0.097(10) 1 d P A 2 F26B F -0.076(4) -0.077(3) 0.688(2) 0.052(16) Uiso 0.097(10) 1 d P A 2 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 Ni1 0.0280(4) 0.0229(4) 0.0226(5) 0.0008(4) 0.0062(3) 0.0025(4) N101 0.021(3) 0.030(3) 0.027(3) -0.003(2) 0.007(2) 0.001(2) C102 0.029(3) 0.035(4) 0.044(5) -0.001(3) 0.006(3) -0.001(3) C103 0.041(4) 0.037(4) 0.071(6) 0.006(4) 0.027(4) 0.012(3) C104 0.028(4) 0.055(5) 0.052(5) 0.005(4) 0.024(3) 0.001(3) C105 0.031(4) 0.046(4) 0.041(5) 0.013(3) 0.008(3) 0.000(3) C106 0.026(3) 0.030(4) 0.026(4) 0.003(3) 0.005(3) 0.000(3) C107 0.025(3) 0.032(4) 0.023(4) -0.001(3) 0.002(3) 0.001(3) C108 0.033(4) 0.022(4) 0.036(4) 0.000(3) 0.016(3) 0.005(3) C109 0.039(4) 0.030(4) 0.076(6) 0.009(4) 0.020(4) -0.001(3) C110 0.049(5) 0.033(4) 0.117(8) -0.004(4) 0.037(5) -0.012(4) C111 0.071(6) 0.035(5) 0.101(7) 0.029(5) 0.055(5) 0.019(4) C112 0.072(5) 0.049(5) 0.043(5) 0.012(4) 0.026(4) 0.020(4) C113 0.041(4) 0.034(4) 0.042(5) -0.001(3) 0.019(3) 0.005(3) N114 0.023(3) 0.029(3) 0.020(3) -0.005(2) 0.006(2) 0.008(2) N115 0.025(3) 0.036(3) 0.023(3) 0.003(2) -0.001(2) 0.005(2) C116 0.025(3) 0.033(4) 0.021(4) 0.005(3) 0.001(3) 0.001(3) C117 0.027(3) 0.038(4) 0.025(4) -0.003(3) 0.008(3) 0.001(3) N118 0.030(3) 0.030(3) 0.023(3) 0.000(2) 0.013(2) 0.001(2) C119 0.038(4) 0.031(4) 0.035(4) 0.004(3) 0.020(3) 0.004(3) C120 0.038(4) 0.034(4) 0.036(4) -0.011(3) 0.018(3) -0.007(3) C121 0.025(3) 0.053(4) 0.031(4) -0.003(3) 0.007(3) -0.008(3) C122 0.027(3) 0.040(4) 0.044(5) 0.000(3) 0.009(3) -0.007(3) C123 0.024(3) 0.036(4) 0.024(4) 0.005(3) -0.002(3) 0.005(3) C124 0.043(4) 0.050(4) 0.043(5) -0.003(4) 0.013(4) 0.013(4) C125 0.058(5) 0.075(6) 0.038(5) 0.012(4) 0.021(4) 0.017(4) C126 0.037(4) 0.081(6) 0.043(5) -0.006(4) 0.012(4) 0.019(4) C127 0.056(4) 0.035(4) 0.043(5) -0.002(3) 0.003(4) 0.021(4) C128 0.047(4) 0.037(4) 0.028(4) -0.002(3) 0.007(3) 0.002(3) N201 0.026(3) 0.029(3) 0.023(3) -0.003(2) 0.008(2) 0.004(2) C202 0.036(4) 0.031(4) 0.032(4) 0.002(3) 0.009(3) 0.007(3) C203 0.036(4) 0.038(4) 0.030(4) 0.004(3) 0.007(3) 0.005(3) C204 0.038(4) 0.046(4) 0.027(4) -0.003(3) 0.001(3) 0.001(3) C205 0.035(4) 0.036(4) 0.036(5) -0.009(3) 0.003(3) 0.000(3) C206 0.023(3) 0.031(4) 0.026(4) 0.001(3) 0.009(3) -0.003(3) C207 0.029(3) 0.027(4) 0.031(4) -0.004(3) 0.012(3) -0.007(3) C208 0.026(3) 0.034(4) 0.032(4) -0.010(3) 0.000(3) 0.004(3) C209 0.038(4) 0.038(4) 0.045(5) -0.012(3) 0.011(3) 0.000(3) C210 0.033(4) 0.061(5) 0.054(5) -0.023(4) 0.018(3) -0.004(4) C211 0.031(4) 0.047(5) 0.079(7) -0.032(4) -0.003(4) 0.002(4) C212 0.046(4) 0.029(4) 0.065(6) -0.008(4) -0.001(4) 0.005(3) C213 0.033(4) 0.032(4) 0.058(5) -0.013(3) 0.006(3) 0.009(3) N214 0.032(3) 0.029(3) 0.031(4) -0.001(2) 0.010(2) 0.004(2) N215 0.028(3) 0.021(3) 0.024(3) -0.001(2) 0.007(2) 0.006(2) C216 0.019(3) 0.031(4) 0.028(4) -0.003(3) 0.003(3) -0.004(3) C217 0.026(3) 0.027(4) 0.025(4) -0.009(3) 0.006(3) -0.003(3) N218 0.029(3) 0.019(3) 0.025(3) 0.001(2) 0.010(2) 0.004(2) C219 0.027(3) 0.036(4) 0.028(4) 0.006(3) 0.001(3) 0.002(3) C220 0.040(4) 0.030(4) 0.032(5) -0.008(3) 0.005(3) 0.003(3) C221 0.040(4) 0.040(4) 0.029(4) -0.005(3) 0.012(3) 0.008(3) C222 0.036(4) 0.034(4) 0.029(4) 0.002(3) 0.006(3) 0.002(3) C223 0.022(3) 0.024(3) 0.030(4) 0.002(3) 0.006(3) 0.008(3) C224 0.034(4) 0.034(4) 0.030(4) 0.002(3) 0.007(3) 0.003(3) C225 0.047(4) 0.041(4) 0.037(5) 0.008(4) 0.010(3) 0.006(4) C226 0.040(4) 0.031(4) 0.056(5) 0.021(4) 0.016(4) 0.011(3) C227 0.034(4) 0.028(4) 0.069(6) 0.017(4) 0.013(4) 0.006(3) C228 0.022(3) 0.039(4) 0.039(4) -0.003(4) 0.003(3) -0.002(3) P10 0.0396(10) 0.0367(11) 0.0382(12) 0.0038(9) 0.0012(9) -0.0021(8) F11 0.056(2) 0.036(2) 0.089(3) -0.006(2) 0.002(2) -0.0066(18) F12 0.058(2) 0.035(2) 0.054(3) -0.0028(18) 0.0017(19) -0.0012(17) F13 0.067(3) 0.077(3) 0.074(3) 0.021(2) 0.037(2) -0.002(2) F14 0.066(2) 0.054(2) 0.052(3) 0.012(2) -0.019(2) 0.0089(19) F15 0.045(2) 0.057(2) 0.077(3) 0.007(2) 0.026(2) 0.0065(19) F16 0.043(2) 0.068(2) 0.040(3) 0.001(2) -0.0059(18) 0.0021(19) P20 0.0496(13) 0.0365(11) 0.0560(15) -0.0006(10) 0.0113(10) -0.0046(9) F21 0.118(3) 0.062(3) 0.048(3) -0.017(2) 0.015(2) 0.010(3) F22 0.093(3) 0.064(3) 0.096(4) -0.036(3) 0.001(3) 0.014(2) F23A 0.061(4) 0.115(5) 0.090(5) -0.035(4) -0.014(3) 0.039(4) F24A 0.169(9) 0.112(6) 0.168(8) 0.002(6) 0.086(7) -0.081(6) F25A 0.121(5) 0.068(4) 0.103(6) -0.008(4) -0.041(4) 0.046(4) F26A 0.107(5) 0.079(4) 0.097(5) -0.006(3) 0.055(4) -0.038(3) _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 Ni1 N215 2.032(4) . ? Ni1 N114 2.037(4) . ? Ni1 N218 2.072(4) . ? Ni1 N101 2.080(4) . ? Ni1 N201 2.090(4) . ? Ni1 N118 2.134(4) . ? N101 C102 1.340(6) . ? N101 C106 1.359(6) . ? C102 C103 1.384(7) . ? C103 C104 1.371(8) . ? C104 C105 1.376(7) . ? C105 C106 1.393(7) . ? C106 C107 1.478(7) . ? C107 N114 1.327(6) . ? C107 C108 1.482(7) . ? C108 C109 1.390(7) . ? C108 C113 1.400(7) . ? C109 C110 1.382(8) . ? C110 C111 1.404(9) . ? C111 C112 1.380(8) . ? C112 C113 1.376(8) . ? N114 N115 1.388(5) . ? N115 C116 1.302(6) . ? C116 C123 1.490(7) . ? C116 C117 1.504(7) . ? C117 N118 1.370(6) . ? C117 C122 1.402(7) . ? N118 C119 1.349(6) . ? C119 C120 1.379(7) . ? C120 C121 1.375(7) . ? C121 C122 1.385(7) . ? C123 C124 1.395(8) . ? C123 C128 1.399(7) . ? C124 C125 1.387(7) . ? C125 C126 1.363(8) . ? C126 C127 1.387(8) . ? C127 C128 1.387(7) . ? N201 C202 1.345(6) . ? N201 C206 1.368(6) . ? C202 C203 1.392(7) . ? C203 C204 1.377(7) . ? C204 C205 1.388(7) . ? C205 C206 1.385(7) . ? C206 C207 1.503(7) . ? C207 N214 1.301(7) . ? C207 C208 1.498(7) . ? C208 C209 1.382(8) . ? C208 C213 1.398(7) . ? C209 C210 1.398(7) . ? C210 C211 1.362(9) . ? C211 C212 1.399(9) . ? C212 C213 1.379(7) . ? N214 N215 1.383(5) . ? N215 C216 1.325(6) . ? C216 C217 1.487(7) . ? C216 C223 1.489(7) . ? C217 N218 1.358(6) . ? C217 C222 1.389(7) . ? N218 C219 1.333(6) . ? C219 C220 1.387(7) . ? C220 C221 1.378(7) . ? C221 C222 1.404(7) . ? C223 C228 1.404(7) . ? C223 C224 1.409(7) . ? C224 C225 1.380(7) . ? C225 C226 1.385(7) . ? C226 C227 1.383(8) . ? C227 C228 1.392(7) . ? P10 F13 1.597(4) . ? P10 F12 1.602(3) . ? P10 F15 1.601(4) . ? P10 F11 1.602(4) . ? P10 F16 1.608(3) . ? P10 F14 1.611(3) . ? P20 F26B 1.43(4) . ? P20 F25B 1.47(4) . ? P20 F23B 1.55(5) . ? P20 F24A 1.565(5) . ? P20 F26A 1.572(5) . ? P20 F25A 1.586(5) . ? P20 F21 1.589(4) . ? P20 F22 1.590(4) . ? P20 F23A 1.600(5) . ? P20 F24B 1.64(4) . ? 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 N215 Ni1 N114 171.10(17) . . ? N215 Ni1 N218 78.92(17) . . ? N114 Ni1 N218 92.49(17) . . ? N215 Ni1 N101 100.15(17) . . ? N114 Ni1 N101 78.86(17) . . ? N218 Ni1 N101 99.99(16) . . ? N215 Ni1 N201 88.15(18) . . ? N114 Ni1 N201 100.59(17) . . ? N218 Ni1 N201 166.20(17) . . ? N101 Ni1 N201 86.94(16) . . ? N215 Ni1 N118 94.70(17) . . ? N114 Ni1 N118 87.95(17) . . ? N218 Ni1 N118 92.40(16) . . ? N101 Ni1 N118 162.21(17) . . ? N201 Ni1 N118 83.78(16) . . ? C102 N101 C106 118.0(5) . . ? C102 N101 Ni1 126.7(4) . . ? C106 N101 Ni1 112.8(3) . . ? N101 C102 C103 123.1(6) . . ? C104 C103 C102 118.3(6) . . ? C103 C104 C105 120.2(6) . . ? C104 C105 C106 118.7(6) . . ? N101 C106 C105 121.6(5) . . ? N101 C106 C107 115.6(5) . . ? C105 C106 C107 122.7(5) . . ? N114 C107 C106 113.6(5) . . ? N114 C107 C108 125.4(5) . . ? C106 C107 C108 121.1(5) . . ? C109 C108 C113 119.8(5) . . ? C109 C108 C107 120.4(5) . . ? C113 C108 C107 119.8(5) . . ? C110 C109 C108 119.8(6) . . ? C109 C110 C111 119.9(6) . . ? C112 C111 C110 120.1(6) . . ? C113 C112 C111 120.1(6) . . ? C112 C113 C108 120.3(6) . . ? C107 N114 N115 112.8(4) . . ? C107 N114 Ni1 117.2(3) . . ? N115 N114 Ni1 126.9(3) . . ? C116 N115 N114 117.1(5) . . ? N115 C116 C123 114.0(5) . . ? N115 C116 C117 129.8(5) . . ? C123 C116 C117 116.1(5) . . ? N118 C117 C122 122.6(5) . . ? N118 C117 C116 119.3(5) . . ? C122 C117 C116 118.1(5) . . ? C119 N118 C117 116.0(5) . . ? C119 N118 Ni1 117.9(4) . . ? C117 N118 Ni1 121.2(4) . . ? N118 C119 C120 124.9(5) . . ? C121 C120 C119 118.0(5) . . ? C120 C121 C122 120.1(5) . . ? C121 C122 C117 118.3(5) . . ? C124 C123 C128 117.7(5) . . ? C124 C123 C116 120.8(5) . . ? C128 C123 C116 121.5(5) . . ? C125 C124 C123 121.8(6) . . ? C126 C125 C124 119.4(6) . . ? C125 C126 C127 120.6(6) . . ? C126 C127 C128 120.0(6) . . ? C127 C128 C123 120.5(6) . . ? C202 N201 C206 117.3(5) . . ? C202 N201 Ni1 118.0(4) . . ? C206 N201 Ni1 124.1(4) . . ? N201 C202 C203 124.4(5) . . ? C204 C203 C202 117.9(6) . . ? C203 C204 C205 118.5(6) . . ? C206 C205 C204 121.1(5) . . ? N201 C206 C205 120.6(5) . . ? N201 C206 C207 120.6(5) . . ? C205 C206 C207 118.7(5) . . ? N214 C207 C208 112.9(5) . . ? N214 C207 C206 130.6(5) . . ? C208 C207 C206 116.5(5) . . ? C209 C208 C213 119.1(5) . . ? C209 C208 C207 120.4(5) . . ? C213 C208 C207 120.5(6) . . ? C208 C209 C210 120.7(6) . . ? C211 C210 C209 119.5(7) . . ? C210 C211 C212 120.8(6) . . ? C213 C212 C211 119.6(6) . . ? C212 C213 C208 120.3(6) . . ? C207 N214 N215 118.6(5) . . ? C216 N215 N214 115.1(4) . . ? C216 N215 Ni1 115.8(4) . . ? N214 N215 Ni1 128.3(4) . . ? N215 C216 C217 114.2(5) . . ? N215 C216 C223 123.7(5) . . ? C217 C216 C223 122.1(5) . . ? N218 C217 C222 121.8(5) . . ? N218 C217 C216 115.0(5) . . ? C222 C217 C216 123.1(5) . . ? C219 N218 C217 118.2(5) . . ? C219 N218 Ni1 129.0(4) . . ? C217 N218 Ni1 111.8(3) . . ? N218 C219 C220 123.5(5) . . ? C221 C220 C219 118.4(5) . . ? C220 C221 C222 119.0(6) . . ? C217 C222 C221 118.7(5) . . ? C228 C223 C224 118.9(5) . . ? C228 C223 C216 119.8(5) . . ? C224 C223 C216 121.3(5) . . ? C225 C224 C223 119.6(5) . . ? C224 C225 C226 121.4(6) . . ? C227 C226 C225 119.6(6) . . ? C226 C227 C228 120.4(6) . . ? C227 C228 C223 120.2(5) . . ? F13 P10 F12 90.6(2) . . ? F13 P10 F15 179.8(2) . . ? F12 P10 F15 89.58(19) . . ? F13 P10 F11 90.8(2) . . ? F12 P10 F11 178.6(2) . . ? F15 P10 F11 89.1(2) . . ? F13 P10 F16 90.6(2) . . ? F12 P10 F16 89.59(18) . . ? F15 P10 F16 89.5(2) . . ? F11 P10 F16 90.9(2) . . ? F13 P10 F14 90.0(2) . . ? F12 P10 F14 90.01(19) . . ? F15 P10 F14 90.0(2) . . ? F11 P10 F14 89.52(19) . . ? F16 P10 F14 179.3(2) . . ? F26B P20 F25B 102(3) . . ? F26B P20 F23B 89(2) . . ? F25B P20 F23B 169(3) . . ? F26B P20 F24A 130(2) . . ? F25B P20 F24A 127(2) . . ? F23B P20 F24A 41.4(19) . . ? F26B P20 F26A 49(2) . . ? F25B P20 F26A 53.6(19) . . ? F23B P20 F26A 138(2) . . ? F24A P20 F26A 178.9(4) . . ? F26B P20 F25A 139(2) . . ? F25B P20 F25A 38.5(18) . . ? F23B P20 F25A 130(2) . . ? F24A P20 F25A 90.2(4) . . ? F26A P20 F25A 90.8(3) . . ? F26B P20 F21 87.4(16) . . ? F25B P20 F21 97.5(16) . . ? F23B P20 F21 82.9(17) . . ? F24A P20 F21 90.6(3) . . ? F26A P20 F21 89.0(2) . . ? F25A P20 F21 89.6(3) . . ? F26B P20 F22 92.6(16) . . ? F25B P20 F22 82.7(16) . . ? F23B P20 F22 96.9(17) . . ? F24A P20 F22 89.3(3) . . ? F26A P20 F22 91.2(3) . . ? F25A P20 F22 90.5(3) . . ? F21 P20 F22 179.8(2) . . ? F26B P20 F23A 41(2) . . ? F25B P20 F23A 142(2) . . ? F23B P20 F23A 49(2) . . ? F24A P20 F23A 89.5(4) . . ? F26A P20 F23A 89.5(3) . . ? F25A P20 F23A 179.1(3) . . ? F21 P20 F23A 91.2(2) . . ? F22 P20 F23A 88.6(2) . . ? F26B P20 F24B 170(3) . . ? F25B P20 F24B 88(2) . . ? F23B P20 F24B 81(2) . . ? F24A P20 F24B 40.0(13) . . ? F26A P20 F24B 141.0(15) . . ? F25A P20 F24B 50.3(14) . . ? F21 P20 F24B 92.5(13) . . ? F22 P20 F24B 87.5(13) . . ? F23A P20 F24B 129.3(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.293 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.077