# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Gerhard Erker' 'Tobias Blomker' 'Roland Frohlich' 'Gerald Kehr' 'Nina Kleigrewe' 'Winfried Steffen' _publ_contact_author_name 'Prof Gerhard Erker' _publ_contact_author_address ; Prof Gerhard Erker Organisch-Chemisches Institut der Universitat Munster Corrensstrasse 40 Muenster 48149 GERMANY ; _publ_contact_author_email ' ERKER@UNI-MUENSTER.DE' _publ_section_title ; Generation of bis(imino)pyridine cobalt(I) cations under metal alkyl free conditions that polymerize ethene ; data_erk2208 _database_code_depnum_ccdc_archive 'CCDC 230096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H53 B Br Co F20 N4' _chemical_formula_weight 1455.79 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 20.027(1) _cell_length_b 12.241(1) _cell_length_c 25.895(1) _cell_angle_alpha 90.00 _cell_angle_beta 93.75(1) _cell_angle_gamma 90.00 _cell_volume 6334.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6601 _exptl_absorpt_correction_T_max 0.9704 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20215 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11147 _reflns_number_gt 6954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (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^)+(0.0466P)^2^+5.8689P] 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 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11147 _refine_ls_number_parameters 866 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.23100(3) 0.77781(4) 0.27338(2) 0.02853(14) Uani 1 1 d . . . N1 N 0.21600(16) 0.7555(3) 0.19913(12) 0.0334(8) Uani 1 1 d . . . C2 C 0.1607(2) 0.6998(4) 0.18405(18) 0.0518(12) Uani 1 1 d . . . H2 H 0.1337 0.6721 0.2099 0.062 Uiso 1 1 calc R . . C3 C 0.1412(3) 0.6808(5) 0.1333(2) 0.0799(19) Uani 1 1 d . . . H3 H 0.1019 0.6399 0.1242 0.096 Uiso 1 1 calc R . . C4 C 0.1794(3) 0.7219(5) 0.0954(2) 0.0779(18) Uani 1 1 d . . . H4 H 0.1659 0.7124 0.0598 0.093 Uiso 1 1 calc R . . C5 C 0.2373(3) 0.7768(4) 0.11022(18) 0.0612(14) Uani 1 1 d . . . H5 H 0.2655 0.8040 0.0851 0.073 Uiso 1 1 calc R . . C6 C 0.2537(2) 0.7915(3) 0.16185(16) 0.0423(11) Uani 1 1 d . . . H6 H 0.2939 0.8294 0.1718 0.051 Uiso 1 1 calc R . . N11 N 0.15288(14) 0.8680(2) 0.28334(11) 0.0240(7) Uani 1 1 d . . . C12 C 0.14157(18) 0.8881(3) 0.33179(14) 0.0252(8) Uani 1 1 d . . . C13 C 0.08831(19) 0.9602(3) 0.35045(15) 0.0343(10) Uani 1 1 d . . . H13A H 0.0655 0.9979 0.3209 0.051 Uiso 1 1 calc R . . H13B H 0.1085 1.0141 0.3747 0.051 Uiso 1 1 calc R . . H13C H 0.0559 0.9159 0.3680 0.051 Uiso 1 1 calc R . . C14 C 0.18937(18) 0.8348(3) 0.36880(14) 0.0262(9) Uani 1 1 d . . . N15 N 0.23658(14) 0.7807(2) 0.34298(11) 0.0245(7) Uani 1 1 d . . . C16 C 0.19196(19) 0.8345(3) 0.42194(14) 0.0321(9) Uani 1 1 d . . . H16 H 0.1589 0.8720 0.4398 0.039 Uiso 1 1 calc R . . C17 C 0.2433(2) 0.7787(3) 0.44952(15) 0.0374(10) Uani 1 1 d . . . H17 H 0.2454 0.7781 0.4863 0.045 Uiso 1 1 calc R . . C18 C 0.2913(2) 0.7241(3) 0.42327(15) 0.0355(9) Uani 1 1 d . . . H18 H 0.3264 0.6857 0.4419 0.043 Uiso 1 1 calc R . . C19 C 0.28780(18) 0.7261(3) 0.36962(14) 0.0274(8) Uani 1 1 d . . . C20 C 0.33274(18) 0.6806(3) 0.33377(14) 0.0269(9) Uani 1 1 d . . . C21 C 0.39580(19) 0.6235(3) 0.35270(16) 0.0381(10) Uani 1 1 d . . . H21A H 0.4189 0.5963 0.3231 0.057 Uiso 1 1 calc R . . H21B H 0.3848 0.5620 0.3749 0.057 Uiso 1 1 calc R . . H21C H 0.4249 0.6748 0.3726 0.057 Uiso 1 1 calc R . . N22 N 0.31293(14) 0.6979(2) 0.28529(11) 0.0251(7) Uani 1 1 d . . . C111 C 0.11231(18) 0.9139(3) 0.24040(14) 0.0253(8) Uani 1 1 d . . . C112 C 0.04794(18) 0.8742(3) 0.22705(15) 0.0299(9) Uani 1 1 d . . . C113 C 0.0170(2) 0.9093(3) 0.18019(16) 0.0389(10) Uani 1 1 d . . . H113 H -0.0263 0.8825 0.1698 0.047 Uiso 1 1 calc R . . C114 C 0.0474(2) 0.9815(3) 0.14870(17) 0.0431(11) Uani 1 1 d . . . H114 H 0.0257 1.0025 0.1165 0.052 Uiso 1 1 calc R . . C115 C 0.1096(2) 1.0236(3) 0.16387(16) 0.0384(10) Uani 1 1 d . . . H115 H 0.1297 1.0753 0.1423 0.046 Uiso 1 1 calc R . . C116 C 0.14326(18) 0.9919(3) 0.21005(15) 0.0300(9) Uani 1 1 d . . . C117 C 0.01032(19) 0.7942(3) 0.25973(16) 0.0352(10) Uani 1 1 d . . . H117 H 0.0395 0.7767 0.2915 0.042 Uiso 1 1 calc R . . C118 C -0.0076(2) 0.6868(3) 0.23172(19) 0.0497(12) Uani 1 1 d . . . H11A H -0.0363 0.7021 0.2004 0.075 Uiso 1 1 calc R . . H11B H -0.0313 0.6389 0.2547 0.075 Uiso 1 1 calc R . . H11C H 0.0335 0.6507 0.2221 0.075 Uiso 1 1 calc R . . C119 C -0.0544(2) 0.8471(4) 0.27685(18) 0.0508(12) Uani 1 1 d . . . H11D H -0.0435 0.9158 0.2949 0.076 Uiso 1 1 calc R . . H11E H -0.0762 0.7974 0.3002 0.076 Uiso 1 1 calc R . . H11F H -0.0846 0.8619 0.2464 0.076 Uiso 1 1 calc R . . C120 C 0.21094(19) 1.0407(3) 0.22794(15) 0.0344(10) Uani 1 1 d . . . H120 H 0.2390 0.9804 0.2439 0.041 Uiso 1 1 calc R . . C121 C 0.2030(2) 1.1270(3) 0.26947(17) 0.0480(12) Uani 1 1 d . . . H12A H 0.1744 1.1861 0.2553 0.072 Uiso 1 1 calc R . . H12B H 0.2470 1.1564 0.2808 0.072 Uiso 1 1 calc R . . H12C H 0.1825 1.0939 0.2990 0.072 Uiso 1 1 calc R . . C122 C 0.2490(2) 1.0895(4) 0.18411(18) 0.0508(12) Uani 1 1 d . . . H12D H 0.2515 1.0357 0.1563 0.076 Uiso 1 1 calc R . . H12E H 0.2944 1.1094 0.1973 0.076 Uiso 1 1 calc R . . H12F H 0.2256 1.1549 0.1706 0.076 Uiso 1 1 calc R . . C221 C 0.35488(18) 0.6669(3) 0.24463(14) 0.0282(9) Uani 1 1 d . . . C222 C 0.33769(19) 0.5733(3) 0.21508(15) 0.0305(9) Uani 1 1 d . . . C223 C 0.3763(2) 0.5499(3) 0.17392(17) 0.0447(11) Uani 1 1 d . . . H223 H 0.3660 0.4874 0.1532 0.054 Uiso 1 1 calc R . . C224 C 0.4295(2) 0.6157(4) 0.16236(17) 0.0477(12) Uani 1 1 d . . . H224 H 0.4553 0.5978 0.1340 0.057 Uiso 1 1 calc R . . C225 C 0.4451(2) 0.7065(4) 0.19164(17) 0.0431(11) Uani 1 1 d . . . H225 H 0.4816 0.7511 0.1831 0.052 Uiso 1 1 calc R . . C226 C 0.40860(18) 0.7347(3) 0.23372(15) 0.0324(9) Uani 1 1 d . . . C227 C 0.2807(2) 0.4993(3) 0.22837(17) 0.0392(10) Uani 1 1 d . . . H227 H 0.2470 0.5454 0.2450 0.047 Uiso 1 1 calc R . . C228 C 0.3056(3) 0.4131(4) 0.2678(2) 0.0620(14) Uani 1 1 d . . . H22A H 0.3384 0.3659 0.2523 0.093 Uiso 1 1 calc R . . H22B H 0.2677 0.3689 0.2778 0.093 Uiso 1 1 calc R . . H22C H 0.3266 0.4493 0.2985 0.093 Uiso 1 1 calc R . . C229 C 0.2451(2) 0.4442(4) 0.1812(2) 0.0644(15) Uani 1 1 d . . . H22D H 0.2328 0.4995 0.1549 0.097 Uiso 1 1 calc R . . H22E H 0.2047 0.4073 0.1916 0.097 Uiso 1 1 calc R . . H22F H 0.2751 0.3905 0.1668 0.097 Uiso 1 1 calc R . . C230 C 0.4274(2) 0.8373(3) 0.26453(17) 0.0438(11) Uani 1 1 d . . . H230 H 0.3983 0.8405 0.2945 0.053 Uiso 1 1 calc R . . C231 C 0.4154(3) 0.9399(4) 0.2334(2) 0.0822(19) Uani 1 1 d . . . H23A H 0.4391 0.9351 0.2015 0.123 Uiso 1 1 calc R . . H23B H 0.4319 1.0030 0.2537 0.123 Uiso 1 1 calc R . . H23C H 0.3673 0.9484 0.2246 0.123 Uiso 1 1 calc R . . C232 C 0.5000(3) 0.8333(5) 0.2863(3) 0.095(2) Uani 1 1 d . . . H23D H 0.5298 0.8462 0.2584 0.142 Uiso 1 1 calc R . . H23E H 0.5095 0.7613 0.3017 0.142 Uiso 1 1 calc R . . H23F H 0.5074 0.8898 0.3129 0.142 Uiso 1 1 calc R . . B1 B 0.2167(2) 0.3296(3) 0.47316(17) 0.0292(10) Uani 1 1 d . . . C31 C 0.26388(18) 0.2700(3) 0.43144(14) 0.0277(9) Uani 1 1 d . . . C32 C 0.26177(19) 0.1617(3) 0.41569(15) 0.0306(9) Uani 1 1 d . . . F32 F 0.21457(11) 0.09226(17) 0.43159(9) 0.0417(6) Uani 1 1 d . . . C33 C 0.3066(2) 0.1154(3) 0.38336(16) 0.0368(10) Uani 1 1 d . . . F33 F 0.30020(12) 0.01012(18) 0.36831(10) 0.0529(7) Uani 1 1 d . . . C34 C 0.3577(2) 0.1764(3) 0.36670(16) 0.0393(10) Uani 1 1 d . . . F34 F 0.40202(12) 0.1323(2) 0.33535(10) 0.0592(7) Uani 1 1 d . . . C35 C 0.36415(19) 0.2835(3) 0.38216(15) 0.0345(10) Uani 1 1 d . . . F35 F 0.41487(11) 0.34442(19) 0.36618(9) 0.0489(6) Uani 1 1 d . . . C36 C 0.31758(19) 0.3269(3) 0.41306(15) 0.0308(9) Uani 1 1 d . . . F36 F 0.32587(11) 0.43343(17) 0.42616(9) 0.0423(6) Uani 1 1 d . . . C41 C 0.15234(19) 0.2553(3) 0.48933(15) 0.0297(9) Uani 1 1 d . . . C42 C 0.1342(2) 0.2301(3) 0.53848(15) 0.0339(9) Uani 1 1 d . . . F42 F 0.17368(11) 0.25812(19) 0.58105(9) 0.0460(6) Uani 1 1 d . . . C43 C 0.0752(2) 0.1763(3) 0.54891(17) 0.0399(10) Uani 1 1 d . . . F43 F 0.06243(13) 0.1541(2) 0.59846(10) 0.0609(7) Uani 1 1 d . . . C44 C 0.0310(2) 0.1474(3) 0.50958(19) 0.0426(11) Uani 1 1 d . . . F44 F -0.02737(12) 0.0986(2) 0.51928(11) 0.0621(8) Uani 1 1 d . . . C45 C 0.0456(2) 0.1697(3) 0.45952(18) 0.0404(11) Uani 1 1 d . . . F45 F 0.00272(12) 0.1406(2) 0.42002(11) 0.0601(7) Uani 1 1 d . . . C46 C 0.1044(2) 0.2227(3) 0.45067(16) 0.0353(10) Uani 1 1 d . . . F46 F 0.11526(11) 0.24351(18) 0.40045(9) 0.0443(6) Uani 1 1 d . . . C51 C 0.17820(18) 0.4412(3) 0.44950(15) 0.0312(9) Uani 1 1 d . . . C52 C 0.1698(2) 0.4729(3) 0.39878(16) 0.0370(10) Uani 1 1 d . . . F52 F 0.20065(12) 0.4187(2) 0.36141(9) 0.0514(7) Uani 1 1 d . . . C53 C 0.1298(2) 0.5590(3) 0.38090(17) 0.0412(11) Uani 1 1 d . . . F53 F 0.12398(13) 0.5844(2) 0.33006(11) 0.0609(8) Uani 1 1 d . . . C54 C 0.0948(2) 0.6175(3) 0.4153(2) 0.0455(12) Uani 1 1 d . . . F54 F 0.05438(12) 0.70066(19) 0.39871(12) 0.0650(8) Uani 1 1 d . . . C55 C 0.1009(2) 0.5900(3) 0.46642(19) 0.0448(11) Uani 1 1 d . . . F55 F 0.06688(14) 0.6473(2) 0.50108(12) 0.0691(8) Uani 1 1 d . . . C56 C 0.1417(2) 0.5045(3) 0.48268(16) 0.0363(10) Uani 1 1 d . . . F56 F 0.14455(12) 0.48127(19) 0.53386(9) 0.0487(6) Uani 1 1 d . . . C61 C 0.27220(18) 0.3537(3) 0.52205(14) 0.0279(9) Uani 1 1 d . . . C62 C 0.30302(19) 0.2657(3) 0.54800(15) 0.0311(9) Uani 1 1 d . . . F62 F 0.28259(11) 0.16286(16) 0.53612(9) 0.0401(6) Uani 1 1 d . . . C63 C 0.35523(19) 0.2750(3) 0.58542(16) 0.0355(10) Uani 1 1 d . . . F63 F 0.38251(12) 0.18486(19) 0.60845(10) 0.0520(7) Uani 1 1 d . . . C64 C 0.37966(19) 0.3759(3) 0.59928(16) 0.0355(10) Uani 1 1 d . . . F64 F 0.43012(12) 0.3857(2) 0.63567(10) 0.0566(7) Uani 1 1 d . . . C65 C 0.35153(19) 0.4658(3) 0.57523(16) 0.0344(10) Uani 1 1 d . . . F65 F 0.37445(12) 0.56619(19) 0.58874(10) 0.0542(7) Uani 1 1 d . . . C66 C 0.30001(19) 0.4535(3) 0.53770(15) 0.0313(9) Uani 1 1 d . . . F66 F 0.27754(11) 0.54750(16) 0.51520(9) 0.0409(6) Uani 1 1 d . . . Br Br 0.50173(4) 0.64984(6) 0.49994(3) 0.0993(3) Uani 1 1 d . . . C71 C 0.4565(3) 0.7858(4) 0.4935(2) 0.0606(13) Uani 1 1 d . . . C72 C 0.4134(3) 0.8151(5) 0.5301(2) 0.0669(15) Uani 1 1 d . . . H72 H 0.4058 0.7678 0.5582 0.080 Uiso 1 1 calc R . . C73 C 0.3807(3) 0.9166(5) 0.5253(2) 0.0747(16) Uani 1 1 d . . . H73 H 0.3500 0.9378 0.5499 0.090 Uiso 1 1 calc R . . C74 C 0.3931(3) 0.9841(5) 0.4857(3) 0.0833(18) Uani 1 1 d . . . H74 H 0.3717 1.0533 0.4831 0.100 Uiso 1 1 calc R . . C75 C 0.4369(3) 0.9533(5) 0.4488(2) 0.0832(18) Uani 1 1 d . . . H75 H 0.4450 1.0008 0.4208 0.100 Uiso 1 1 calc R . . C76 C 0.4685(3) 0.8526(5) 0.4531(2) 0.0728(16) Uani 1 1 d . . . H76 H 0.4984 0.8304 0.4281 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0268(3) 0.0321(3) 0.0270(3) 0.0015(2) 0.0044(2) 0.0049(2) N1 0.030(2) 0.041(2) 0.0293(19) 0.0016(15) 0.0027(15) 0.0123(16) C2 0.033(3) 0.078(3) 0.044(3) -0.014(2) 0.004(2) -0.002(2) C3 0.041(3) 0.139(6) 0.059(4) -0.027(4) -0.003(3) -0.006(3) C4 0.070(4) 0.131(5) 0.031(3) -0.014(3) -0.013(3) 0.014(4) C5 0.075(4) 0.071(3) 0.038(3) 0.005(3) 0.009(3) 0.011(3) C6 0.052(3) 0.041(3) 0.035(3) 0.004(2) 0.005(2) 0.004(2) N11 0.0218(17) 0.0241(16) 0.0266(18) 0.0010(13) 0.0050(14) -0.0013(13) C12 0.024(2) 0.0191(18) 0.033(2) 0.0005(16) 0.0060(17) -0.0033(16) C13 0.033(2) 0.032(2) 0.039(2) -0.0010(18) 0.0100(19) 0.0011(18) C14 0.030(2) 0.0178(18) 0.032(2) 0.0010(16) 0.0101(18) -0.0045(17) N15 0.0248(17) 0.0213(15) 0.0275(17) 0.0027(14) 0.0037(14) -0.0026(14) C16 0.031(2) 0.038(2) 0.029(2) -0.0007(18) 0.0101(18) -0.0017(19) C17 0.043(3) 0.048(2) 0.022(2) 0.0032(19) 0.0052(19) -0.002(2) C18 0.035(2) 0.041(2) 0.031(2) 0.0069(19) 0.0002(18) 0.001(2) C19 0.027(2) 0.0248(19) 0.031(2) 0.0031(17) 0.0032(17) -0.0036(18) C20 0.023(2) 0.0254(19) 0.032(2) 0.0055(16) 0.0011(17) -0.0024(16) C21 0.029(2) 0.047(3) 0.038(2) 0.008(2) 0.0002(19) 0.005(2) N22 0.0227(17) 0.0253(17) 0.0276(18) 0.0009(13) 0.0051(14) -0.0001(13) C111 0.027(2) 0.0232(19) 0.026(2) 0.0041(16) 0.0057(17) 0.0050(17) C112 0.022(2) 0.032(2) 0.036(2) 0.0003(17) 0.0036(18) 0.0021(17) C113 0.021(2) 0.050(3) 0.045(3) 0.002(2) -0.0022(19) 0.000(2) C114 0.040(3) 0.050(3) 0.039(3) 0.013(2) -0.004(2) 0.004(2) C115 0.037(3) 0.042(2) 0.037(2) 0.0141(19) 0.009(2) 0.003(2) C116 0.026(2) 0.030(2) 0.035(2) 0.0012(17) 0.0079(18) 0.0047(18) C117 0.028(2) 0.039(2) 0.039(2) 0.0039(19) 0.0011(18) -0.0071(19) C118 0.037(3) 0.043(3) 0.071(3) -0.002(2) 0.012(2) -0.013(2) C119 0.038(3) 0.060(3) 0.056(3) -0.006(2) 0.017(2) -0.005(2) C120 0.026(2) 0.036(2) 0.042(2) 0.0123(19) 0.0049(19) 0.0041(18) C121 0.042(3) 0.048(3) 0.054(3) 0.002(2) 0.002(2) -0.014(2) C122 0.038(3) 0.055(3) 0.060(3) 0.016(2) 0.013(2) -0.007(2) C221 0.022(2) 0.030(2) 0.032(2) 0.0035(17) 0.0021(17) 0.0063(17) C222 0.030(2) 0.029(2) 0.033(2) 0.0023(17) 0.0037(18) 0.0064(18) C223 0.051(3) 0.038(2) 0.046(3) -0.006(2) 0.014(2) 0.006(2) C224 0.047(3) 0.051(3) 0.048(3) 0.003(2) 0.022(2) 0.016(2) C225 0.033(2) 0.048(3) 0.050(3) 0.008(2) 0.014(2) -0.001(2) C226 0.026(2) 0.036(2) 0.035(2) 0.0066(18) 0.0005(18) 0.0015(18) C227 0.032(2) 0.035(2) 0.051(3) -0.006(2) 0.010(2) -0.0009(19) C228 0.065(3) 0.045(3) 0.077(4) 0.011(3) 0.008(3) -0.016(3) C229 0.055(3) 0.068(3) 0.070(4) -0.021(3) 0.003(3) -0.014(3) C230 0.038(3) 0.049(3) 0.045(3) 0.000(2) 0.011(2) -0.015(2) C231 0.109(5) 0.038(3) 0.094(5) -0.009(3) -0.030(4) 0.009(3) C232 0.071(4) 0.073(4) 0.132(6) 0.012(4) -0.056(4) -0.025(3) B1 0.026(3) 0.030(2) 0.033(3) 0.001(2) 0.007(2) 0.000(2) C31 0.026(2) 0.027(2) 0.030(2) 0.0022(17) 0.0019(17) -0.0007(17) C32 0.028(2) 0.030(2) 0.033(2) 0.0000(18) 0.0018(18) -0.0042(18) F32 0.0357(14) 0.0292(12) 0.0619(17) -0.0068(11) 0.0166(12) -0.0059(11) C33 0.037(3) 0.028(2) 0.045(3) -0.0075(19) 0.003(2) -0.0019(19) F33 0.0513(16) 0.0347(14) 0.0746(19) -0.0219(12) 0.0178(14) -0.0043(12) C34 0.035(3) 0.041(2) 0.043(3) -0.005(2) 0.012(2) 0.004(2) F34 0.0501(16) 0.0605(17) 0.0709(19) -0.0157(14) 0.0329(14) 0.0030(13) C35 0.026(2) 0.040(2) 0.038(2) 0.005(2) 0.0088(19) -0.006(2) F35 0.0374(14) 0.0512(15) 0.0605(17) 0.0027(12) 0.0227(12) -0.0072(12) C36 0.034(2) 0.025(2) 0.034(2) -0.0017(17) 0.0044(19) -0.0008(18) F36 0.0468(15) 0.0306(12) 0.0514(15) -0.0004(11) 0.0181(12) -0.0078(11) C41 0.027(2) 0.024(2) 0.038(2) -0.0036(17) 0.0067(18) 0.0032(17) C42 0.034(2) 0.033(2) 0.036(2) -0.0068(19) 0.0068(19) 0.0002(19) F42 0.0466(15) 0.0603(16) 0.0322(13) -0.0027(11) 0.0103(11) -0.0080(12) C43 0.040(3) 0.037(2) 0.045(3) -0.003(2) 0.019(2) 0.001(2) F43 0.0595(17) 0.0721(18) 0.0544(17) 0.0080(14) 0.0291(14) -0.0087(14) C44 0.029(2) 0.032(2) 0.069(3) -0.003(2) 0.015(2) -0.002(2) F44 0.0330(15) 0.0553(16) 0.101(2) -0.0100(15) 0.0273(14) -0.0126(13) C45 0.024(2) 0.036(2) 0.061(3) -0.009(2) -0.003(2) 0.000(2) F45 0.0330(15) 0.0682(18) 0.078(2) -0.0150(15) -0.0063(14) -0.0088(13) C46 0.033(2) 0.033(2) 0.040(3) -0.002(2) 0.0074(19) 0.004(2) F46 0.0390(14) 0.0538(15) 0.0397(14) 0.0013(11) -0.0010(11) -0.0021(11) C51 0.027(2) 0.027(2) 0.039(2) -0.0011(18) 0.0002(18) -0.0044(18) C52 0.037(3) 0.035(2) 0.040(3) 0.0025(19) 0.006(2) -0.003(2) F52 0.0607(17) 0.0572(16) 0.0370(15) 0.0085(12) 0.0076(13) 0.0104(13) C53 0.034(3) 0.039(2) 0.049(3) 0.015(2) -0.004(2) -0.007(2) F53 0.0606(18) 0.0565(17) 0.0635(19) 0.0242(14) -0.0123(14) -0.0035(14) C54 0.028(2) 0.028(2) 0.079(4) 0.009(2) -0.006(2) 0.005(2) F54 0.0478(16) 0.0377(15) 0.107(2) 0.0148(14) -0.0136(16) 0.0098(13) C55 0.036(3) 0.033(2) 0.066(3) -0.005(2) 0.006(2) 0.005(2) F55 0.0624(18) 0.0537(17) 0.092(2) -0.0129(15) 0.0122(16) 0.0271(14) C56 0.035(2) 0.033(2) 0.041(3) -0.0007(19) 0.002(2) 0.002(2) F56 0.0532(16) 0.0488(15) 0.0449(16) -0.0055(12) 0.0106(12) 0.0122(12) C61 0.029(2) 0.026(2) 0.030(2) 0.0025(16) 0.0103(17) 0.0033(17) C62 0.031(2) 0.029(2) 0.034(2) -0.0004(18) 0.0142(18) -0.0015(18) F62 0.0426(14) 0.0255(12) 0.0521(15) 0.0053(11) 0.0026(11) -0.0004(10) C63 0.027(2) 0.035(2) 0.045(3) 0.013(2) 0.0078(19) 0.007(2) F63 0.0480(16) 0.0440(14) 0.0630(17) 0.0186(12) -0.0052(13) 0.0074(12) C64 0.026(2) 0.042(3) 0.038(2) -0.001(2) -0.0013(19) -0.004(2) F64 0.0447(16) 0.0614(17) 0.0609(18) -0.0011(13) -0.0183(14) 0.0003(13) C65 0.029(2) 0.033(2) 0.041(3) -0.0062(19) 0.006(2) -0.0065(19) F65 0.0547(17) 0.0392(14) 0.0668(18) -0.0078(12) -0.0101(14) -0.0112(12) C66 0.029(2) 0.027(2) 0.039(2) 0.0048(18) 0.0102(19) 0.0036(18) F66 0.0497(15) 0.0241(12) 0.0478(15) 0.0014(10) -0.0049(12) 0.0018(11) Br 0.1146(6) 0.0840(5) 0.1023(6) 0.0044(4) 0.0297(4) 0.0292(4) C71 0.056(3) 0.066(3) 0.060(3) 0.000(3) 0.006(3) -0.002(3) C72 0.072(4) 0.072(4) 0.058(4) -0.006(3) 0.009(3) -0.005(3) C73 0.076(4) 0.095(5) 0.053(4) -0.012(3) 0.000(3) -0.005(4) C74 0.078(4) 0.084(4) 0.087(5) 0.000(4) -0.007(4) 0.023(4) C75 0.073(4) 0.096(5) 0.082(5) 0.026(4) 0.013(4) 0.017(4) C76 0.054(3) 0.099(5) 0.066(4) 0.005(3) 0.010(3) 0.008(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 Co N15 1.799(3) . ? Co N22 1.918(3) . ? Co N11 1.946(3) . ? Co N1 1.946(3) . ? N1 C2 1.337(5) . ? N1 C6 1.338(5) . ? C2 C3 1.367(6) . ? C3 C4 1.377(8) . ? C4 C5 1.374(7) . ? C5 C6 1.367(6) . ? N11 C12 1.313(4) . ? N11 C111 1.447(4) . ? C12 C14 1.463(5) . ? C12 C13 1.489(5) . ? C14 N15 1.365(4) . ? C14 C16 1.374(5) . ? N15 C19 1.372(4) . ? C16 C17 1.391(5) . ? C17 C18 1.386(5) . ? C18 C19 1.387(5) . ? C19 C20 1.446(5) . ? C20 N22 1.309(4) . ? C20 C21 1.498(5) . ? N22 C221 1.440(5) . ? C111 C112 1.400(5) . ? C111 C116 1.405(5) . ? C112 C113 1.394(5) . ? C112 C117 1.525(5) . ? C113 C114 1.372(6) . ? C114 C115 1.381(6) . ? C115 C116 1.390(5) . ? C116 C120 1.525(5) . ? C117 C118 1.533(5) . ? C117 C119 1.539(5) . ? C120 C121 1.523(6) . ? C120 C122 1.530(5) . ? C221 C226 1.402(5) . ? C221 C222 1.408(5) . ? C222 C223 1.387(5) . ? C222 C227 1.514(5) . ? C223 C224 1.383(6) . ? C224 C225 1.370(6) . ? C225 C226 1.395(5) . ? C226 C230 1.522(6) . ? C227 C228 1.528(6) . ? C227 C229 1.530(6) . ? C230 C231 1.504(6) . ? C230 C232 1.527(6) . ? B1 C31 1.651(6) . ? B1 C41 1.654(6) . ? B1 C61 1.655(6) . ? B1 C51 1.666(6) . ? C31 C32 1.387(5) . ? C31 C36 1.391(5) . ? C32 F32 1.355(4) . ? C32 C33 1.388(5) . ? C33 F33 1.350(4) . ? C33 C34 1.360(6) . ? C34 F34 1.353(4) . ? C34 C35 1.375(5) . ? C35 F35 1.347(4) . ? C35 C36 1.375(5) . ? C36 F36 1.354(4) . ? C41 C42 1.381(5) . ? C41 C46 1.399(5) . ? C42 F42 1.358(4) . ? C42 C43 1.394(6) . ? C43 F43 1.352(5) . ? C43 C44 1.353(6) . ? C44 F44 1.351(5) . ? C44 C45 1.375(6) . ? C45 F45 1.340(5) . ? C45 C46 1.376(6) . ? C46 F46 1.357(4) . ? C51 C52 1.369(5) . ? C51 C56 1.398(5) . ? C52 F52 1.354(5) . ? C52 C53 1.386(6) . ? C53 F53 1.350(5) . ? C53 C54 1.371(6) . ? C54 F54 1.353(4) . ? C54 C55 1.364(6) . ? C55 F55 1.357(5) . ? C55 C56 1.377(6) . ? C56 F56 1.353(5) . ? C61 C66 1.392(5) . ? C61 C62 1.393(5) . ? C62 F62 1.352(4) . ? C62 C63 1.383(5) . ? C63 F63 1.352(4) . ? C63 C64 1.369(5) . ? C64 F64 1.341(4) . ? C64 C65 1.368(5) . ? C65 F65 1.349(4) . ? C65 C66 1.379(5) . ? C66 F66 1.353(4) . ? Br C71 1.898(5) . ? C71 C76 1.362(7) . ? C71 C72 1.370(7) . ? C72 C73 1.406(7) . ? C73 C74 1.352(8) . ? C74 C75 1.390(8) . ? C75 C76 1.388(8) . ? 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 N15 Co N22 81.52(13) . . ? N15 Co N11 81.59(13) . . ? N22 Co N11 162.74(12) . . ? N15 Co N1 171.24(13) . . ? N22 Co N1 99.36(13) . . ? N11 Co N1 97.88(12) . . ? C2 N1 C6 116.9(4) . . ? C2 N1 Co 115.6(3) . . ? C6 N1 Co 127.5(3) . . ? N1 C2 C3 123.1(5) . . ? C2 C3 C4 119.1(5) . . ? C5 C4 C3 118.6(5) . . ? C6 C5 C4 118.7(5) . . ? N1 C6 C5 123.5(4) . . ? C12 N11 C111 122.6(3) . . ? C12 N11 Co 115.1(2) . . ? C111 N11 Co 122.3(2) . . ? N11 C12 C14 113.3(3) . . ? N11 C12 C13 126.4(3) . . ? C14 C12 C13 120.2(3) . . ? N15 C14 C16 120.5(3) . . ? N15 C14 C12 109.9(3) . . ? C16 C14 C12 129.6(3) . . ? C14 N15 C19 120.6(3) . . ? C14 N15 Co 120.1(2) . . ? C19 N15 Co 119.3(2) . . ? C14 C16 C17 119.6(4) . . ? C18 C17 C16 119.9(4) . . ? C17 C18 C19 119.4(4) . . ? N15 C19 C18 120.0(3) . . ? N15 C19 C20 109.9(3) . . ? C18 C19 C20 130.0(4) . . ? N22 C20 C19 113.0(3) . . ? N22 C20 C21 125.9(3) . . ? C19 C20 C21 121.1(3) . . ? C20 N22 C221 120.2(3) . . ? C20 N22 Co 116.1(2) . . ? C221 N22 Co 123.4(2) . . ? C112 C111 C116 122.0(3) . . ? C112 C111 N11 121.1(3) . . ? C116 C111 N11 116.6(3) . . ? C113 C112 C111 117.2(3) . . ? C113 C112 C117 118.2(3) . . ? C111 C112 C117 124.5(3) . . ? C114 C113 C112 121.8(4) . . ? C113 C114 C115 119.9(4) . . ? C114 C115 C116 121.2(4) . . ? C115 C116 C111 117.6(4) . . ? C115 C116 C120 121.6(3) . . ? C111 C116 C120 120.8(3) . . ? C112 C117 C118 113.4(3) . . ? C112 C117 C119 110.2(3) . . ? C118 C117 C119 108.8(3) . . ? C121 C120 C116 110.8(3) . . ? C121 C120 C122 109.4(3) . . ? C116 C120 C122 113.8(3) . . ? C226 C221 C222 122.4(3) . . ? C226 C221 N22 118.9(3) . . ? C222 C221 N22 118.6(3) . . ? C223 C222 C221 117.1(4) . . ? C223 C222 C227 121.2(4) . . ? C221 C222 C227 121.6(3) . . ? C224 C223 C222 121.5(4) . . ? C225 C224 C223 120.2(4) . . ? C224 C225 C226 121.3(4) . . ? C225 C226 C221 117.4(4) . . ? C225 C226 C230 119.3(4) . . ? C221 C226 C230 123.3(4) . . ? C222 C227 C228 110.3(3) . . ? C222 C227 C229 113.6(4) . . ? C228 C227 C229 110.1(4) . . ? C231 C230 C226 112.5(4) . . ? C231 C230 C232 109.9(4) . . ? C226 C230 C232 111.3(4) . . ? C31 B1 C41 114.3(3) . . ? C31 B1 C61 101.3(3) . . ? C41 B1 C61 113.6(3) . . ? C31 B1 C51 113.1(3) . . ? C41 B1 C51 101.2(3) . . ? C61 B1 C51 114.0(3) . . ? C32 C31 C36 112.8(3) . . ? C32 C31 B1 127.4(3) . . ? C36 C31 B1 119.4(3) . . ? F32 C32 C31 121.2(3) . . ? F32 C32 C33 114.8(3) . . ? C31 C32 C33 124.0(4) . . ? F33 C33 C34 119.5(4) . . ? F33 C33 C32 120.7(3) . . ? C34 C33 C32 119.8(4) . . ? F34 C34 C33 120.5(4) . . ? F34 C34 C35 120.2(4) . . ? C33 C34 C35 119.3(4) . . ? F35 C35 C36 121.3(3) . . ? F35 C35 C34 119.8(3) . . ? C36 C35 C34 119.0(4) . . ? F36 C36 C35 116.2(3) . . ? F36 C36 C31 118.8(3) . . ? C35 C36 C31 125.0(3) . . ? C42 C41 C46 112.7(3) . . ? C42 C41 B1 127.8(3) . . ? C46 C41 B1 119.1(3) . . ? F42 C42 C41 121.1(3) . . ? F42 C42 C43 114.7(4) . . ? C41 C42 C43 124.2(4) . . ? F43 C43 C44 120.4(4) . . ? F43 C43 C42 119.6(4) . . ? C44 C43 C42 119.9(4) . . ? F44 C44 C43 120.5(4) . . ? F44 C44 C45 120.2(4) . . ? C43 C44 C45 119.2(4) . . ? F45 C45 C44 120.1(4) . . ? F45 C45 C46 120.7(4) . . ? C44 C45 C46 119.2(4) . . ? F46 C46 C45 116.2(4) . . ? F46 C46 C41 119.1(3) . . ? C45 C46 C41 124.7(4) . . ? C52 C51 C56 113.4(4) . . ? C52 C51 B1 127.6(4) . . ? C56 C51 B1 118.5(4) . . ? F52 C52 C51 120.9(4) . . ? F52 C52 C53 114.5(4) . . ? C51 C52 C53 124.6(4) . . ? F53 C53 C54 119.9(4) . . ? F53 C53 C52 120.8(4) . . ? C54 C53 C52 119.3(4) . . ? F54 C54 C55 120.5(4) . . ? F54 C54 C53 120.5(4) . . ? C55 C54 C53 119.0(4) . . ? F55 C55 C54 119.9(4) . . ? F55 C55 C56 120.3(4) . . ? C54 C55 C56 119.8(4) . . ? F56 C56 C55 116.4(4) . . ? F56 C56 C51 119.7(3) . . ? C55 C56 C51 123.9(4) . . ? C66 C61 C62 112.5(3) . . ? C66 C61 B1 127.9(3) . . ? C62 C61 B1 119.0(3) . . ? F62 C62 C63 116.1(3) . . ? F62 C62 C61 119.5(3) . . ? C63 C62 C61 124.4(4) . . ? F63 C63 C64 119.6(4) . . ? F63 C63 C62 120.5(4) . . ? C64 C63 C62 119.9(4) . . ? F64 C64 C65 121.2(4) . . ? F64 C64 C63 120.3(4) . . ? C65 C64 C63 118.5(4) . . ? F65 C65 C64 119.4(4) . . ? F65 C65 C66 120.6(4) . . ? C64 C65 C66 120.0(4) . . ? F66 C66 C65 115.0(3) . . ? F66 C66 C61 120.4(3) . . ? C65 C66 C61 124.6(4) . . ? C76 C71 C72 121.7(5) . . ? C76 C71 Br 119.1(4) . . ? C72 C71 Br 119.2(4) . . ? C71 C72 C73 118.7(5) . . ? C74 C73 C72 119.9(6) . . ? C73 C74 C75 120.8(6) . . ? C76 C75 C74 119.3(6) . . ? C71 C76 C75 119.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N15 Co N1 C2 21.7(10) . . . . ? N22 Co N1 C2 116.7(3) . . . . ? N11 Co N1 C2 -64.2(3) . . . . ? N15 Co N1 C6 -160.0(8) . . . . ? N22 Co N1 C6 -64.9(3) . . . . ? N11 Co N1 C6 114.1(3) . . . . ? C6 N1 C2 C3 -1.3(7) . . . . ? Co N1 C2 C3 177.2(4) . . . . ? N1 C2 C3 C4 -0.9(9) . . . . ? C2 C3 C4 C5 2.6(9) . . . . ? C3 C4 C5 C6 -2.1(8) . . . . ? C2 N1 C6 C5 1.9(6) . . . . ? Co N1 C6 C5 -176.4(3) . . . . ? C4 C5 C6 N1 -0.2(7) . . . . ? N15 Co N11 C12 0.3(2) . . . . ? N22 Co N11 C12 -11.6(5) . . . . ? N1 Co N11 C12 171.5(2) . . . . ? N15 Co N11 C111 177.4(3) . . . . ? N22 Co N11 C111 165.4(3) . . . . ? N1 Co N11 C111 -11.4(3) . . . . ? C111 N11 C12 C14 -179.0(3) . . . . ? Co N11 C12 C14 -1.9(4) . . . . ? C111 N11 C12 C13 -1.3(5) . . . . ? Co N11 C12 C13 175.8(3) . . . . ? N11 C12 C14 N15 2.9(4) . . . . ? C13 C12 C14 N15 -174.9(3) . . . . ? N11 C12 C14 C16 -177.8(4) . . . . ? C13 C12 C14 C16 4.4(6) . . . . ? C16 C14 N15 C19 -0.7(5) . . . . ? C12 C14 N15 C19 178.7(3) . . . . ? C16 C14 N15 Co 177.8(3) . . . . ? C12 C14 N15 Co -2.8(4) . . . . ? N22 Co N15 C14 177.9(3) . . . . ? N11 Co N15 C14 1.5(2) . . . . ? N1 Co N15 C14 -85.7(9) . . . . ? N22 Co N15 C19 -3.5(3) . . . . ? N11 Co N15 C19 -180.0(3) . . . . ? N1 Co N15 C19 92.9(9) . . . . ? N15 C14 C16 C17 0.2(5) . . . . ? C12 C14 C16 C17 -179.0(4) . . . . ? C14 C16 C17 C18 0.0(6) . . . . ? C16 C17 C18 C19 0.3(6) . . . . ? C14 N15 C19 C18 1.0(5) . . . . ? Co N15 C19 C18 -177.6(3) . . . . ? C14 N15 C19 C20 -177.1(3) . . . . ? Co N15 C19 C20 4.4(4) . . . . ? C17 C18 C19 N15 -0.7(6) . . . . ? C17 C18 C19 C20 176.8(4) . . . . ? N15 C19 C20 N22 -2.7(4) . . . . ? C18 C19 C20 N22 179.6(4) . . . . ? N15 C19 C20 C21 175.6(3) . . . . ? C18 C19 C20 C21 -2.2(6) . . . . ? C19 C20 N22 C221 174.3(3) . . . . ? C21 C20 N22 C221 -3.8(5) . . . . ? C19 C20 N22 Co 0.1(4) . . . . ? C21 C20 N22 Co -178.0(3) . . . . ? N15 Co N22 C20 1.8(3) . . . . ? N11 Co N22 C20 13.8(6) . . . . ? N1 Co N22 C20 -169.4(3) . . . . ? N15 Co N22 C221 -172.2(3) . . . . ? N11 Co N22 C221 -160.2(4) . . . . ? N1 Co N22 C221 16.6(3) . . . . ? C12 N11 C111 C112 -74.7(4) . . . . ? Co N11 C111 C112 108.5(3) . . . . ? C12 N11 C111 C116 111.6(4) . . . . ? Co N11 C111 C116 -65.3(4) . . . . ? C116 C111 C112 C113 4.3(5) . . . . ? N11 C111 C112 C113 -169.1(3) . . . . ? C116 C111 C112 C117 -176.7(4) . . . . ? N11 C111 C112 C117 9.9(5) . . . . ? C111 C112 C113 C114 -1.3(6) . . . . ? C117 C112 C113 C114 179.7(4) . . . . ? C112 C113 C114 C115 -1.8(7) . . . . ? C113 C114 C115 C116 1.9(6) . . . . ? C114 C115 C116 C111 1.0(6) . . . . ? C114 C115 C116 C120 -178.0(4) . . . . ? C112 C111 C116 C115 -4.2(5) . . . . ? N11 C111 C116 C115 169.5(3) . . . . ? C112 C111 C116 C120 174.8(3) . . . . ? N11 C111 C116 C120 -11.5(5) . . . . ? C113 C112 C117 C118 59.4(5) . . . . ? C111 C112 C117 C118 -119.6(4) . . . . ? C113 C112 C117 C119 -62.9(5) . . . . ? C111 C112 C117 C119 118.2(4) . . . . ? C115 C116 C120 C121 101.6(4) . . . . ? C111 C116 C120 C121 -77.4(4) . . . . ? C115 C116 C120 C122 -22.2(5) . . . . ? C111 C116 C120 C122 158.8(4) . . . . ? C20 N22 C221 C226 -79.1(4) . . . . ? Co N22 C221 C226 94.7(4) . . . . ? C20 N22 C221 C222 105.0(4) . . . . ? Co N22 C221 C222 -81.2(4) . . . . ? C226 C221 C222 C223 -0.2(6) . . . . ? N22 C221 C222 C223 175.6(3) . . . . ? C226 C221 C222 C227 178.3(3) . . . . ? N22 C221 C222 C227 -6.0(5) . . . . ? C221 C222 C223 C224 0.1(6) . . . . ? C227 C222 C223 C224 -178.4(4) . . . . ? C222 C223 C224 C225 -0.2(7) . . . . ? C223 C224 C225 C226 0.4(7) . . . . ? C224 C225 C226 C221 -0.5(6) . . . . ? C224 C225 C226 C230 -179.1(4) . . . . ? C222 C221 C226 C225 0.4(6) . . . . ? N22 C221 C226 C225 -175.4(3) . . . . ? C222 C221 C226 C230 178.9(4) . . . . ? N22 C221 C226 C230 3.2(5) . . . . ? C223 C222 C227 C228 91.3(5) . . . . ? C221 C222 C227 C228 -87.1(5) . . . . ? C223 C222 C227 C229 -32.9(5) . . . . ? C221 C222 C227 C229 148.7(4) . . . . ? C225 C226 C230 C231 66.1(5) . . . . ? C221 C226 C230 C231 -112.4(5) . . . . ? C225 C226 C230 C232 -57.8(5) . . . . ? C221 C226 C230 C232 123.7(4) . . . . ? C41 B1 C31 C32 -11.2(6) . . . . ? C61 B1 C31 C32 111.3(4) . . . . ? C51 B1 C31 C32 -126.3(4) . . . . ? C41 B1 C31 C36 176.8(3) . . . . ? C61 B1 C31 C36 -60.7(4) . . . . ? C51 B1 C31 C36 61.7(5) . . . . ? C36 C31 C32 F32 177.2(3) . . . . ? B1 C31 C32 F32 4.9(6) . . . . ? C36 C31 C32 C33 -2.4(6) . . . . ? B1 C31 C32 C33 -174.8(4) . . . . ? F32 C32 C33 F33 2.4(6) . . . . ? C31 C32 C33 F33 -177.9(4) . . . . ? F32 C32 C33 C34 -177.4(4) . . . . ? C31 C32 C33 C34 2.3(6) . . . . ? F33 C33 C34 F34 -0.1(6) . . . . ? C32 C33 C34 F34 179.7(4) . . . . ? F33 C33 C34 C35 -179.9(4) . . . . ? C32 C33 C34 C35 -0.1(6) . . . . ? F34 C34 C35 F35 -0.3(6) . . . . ? C33 C34 C35 F35 179.5(4) . . . . ? F34 C34 C35 C36 178.5(4) . . . . ? C33 C34 C35 C36 -1.6(6) . . . . ? F35 C35 C36 F36 0.1(6) . . . . ? C34 C35 C36 F36 -178.8(3) . . . . ? F35 C35 C36 C31 -179.8(3) . . . . ? C34 C35 C36 C31 1.4(6) . . . . ? C32 C31 C36 F36 -179.2(3) . . . . ? B1 C31 C36 F36 -6.2(5) . . . . ? C32 C31 C36 C35 0.6(6) . . . . ? B1 C31 C36 C35 173.6(4) . . . . ? C31 B1 C41 C42 128.5(4) . . . . ? C61 B1 C41 C42 13.0(5) . . . . ? C51 B1 C41 C42 -109.6(4) . . . . ? C31 B1 C41 C46 -60.0(4) . . . . ? C61 B1 C41 C46 -175.5(3) . . . . ? C51 B1 C41 C46 61.9(4) . . . . ? C46 C41 C42 F42 -178.2(3) . . . . ? B1 C41 C42 F42 -6.2(6) . . . . ? C46 C41 C42 C43 1.1(5) . . . . ? B1 C41 C42 C43 173.1(4) . . . . ? F42 C42 C43 F43 -1.5(5) . . . . ? C41 C42 C43 F43 179.2(3) . . . . ? F42 C42 C43 C44 177.9(4) . . . . ? C41 C42 C43 C44 -1.4(6) . . . . ? F43 C43 C44 F44 1.7(6) . . . . ? C42 C43 C44 F44 -177.7(3) . . . . ? F43 C43 C44 C45 -179.2(4) . . . . ? C42 C43 C44 C45 1.4(6) . . . . ? F44 C44 C45 F45 -1.6(6) . . . . ? C43 C44 C45 F45 179.3(4) . . . . ? F44 C44 C45 C46 177.9(3) . . . . ? C43 C44 C45 C46 -1.2(6) . . . . ? F45 C45 C46 F46 0.4(5) . . . . ? C44 C45 C46 F46 -179.1(3) . . . . ? F45 C45 C46 C41 -179.4(3) . . . . ? C44 C45 C46 C41 1.1(6) . . . . ? C42 C41 C46 F46 179.2(3) . . . . ? B1 C41 C46 F46 6.5(5) . . . . ? C42 C41 C46 C45 -0.9(5) . . . . ? B1 C41 C46 C45 -173.7(4) . . . . ? C31 B1 C51 C52 15.3(5) . . . . ? C41 B1 C51 C52 -107.4(4) . . . . ? C61 B1 C51 C52 130.4(4) . . . . ? C31 B1 C51 C56 -174.2(3) . . . . ? C41 B1 C51 C56 63.1(4) . . . . ? C61 B1 C51 C56 -59.2(5) . . . . ? C56 C51 C52 F52 -178.7(3) . . . . ? B1 C51 C52 F52 -7.9(6) . . . . ? C56 C51 C52 C53 0.2(6) . . . . ? B1 C51 C52 C53 171.1(4) . . . . ? F52 C52 C53 F53 -0.5(5) . . . . ? C51 C52 C53 F53 -179.5(4) . . . . ? F52 C52 C53 C54 178.2(4) . . . . ? C51 C52 C53 C54 -0.9(6) . . . . ? F53 C53 C54 F54 -0.1(6) . . . . ? C52 C53 C54 F54 -178.8(3) . . . . ? F53 C53 C54 C55 179.5(4) . . . . ? C52 C53 C54 C55 0.8(6) . . . . ? F54 C54 C55 F55 -0.8(6) . . . . ? C53 C54 C55 F55 179.7(4) . . . . ? F54 C54 C55 C56 179.4(4) . . . . ? C53 C54 C55 C56 -0.2(6) . . . . ? F55 C55 C56 F56 1.0(6) . . . . ? C54 C55 C56 F56 -179.2(4) . . . . ? F55 C55 C56 C51 179.7(4) . . . . ? C54 C55 C56 C51 -0.5(7) . . . . ? C52 C51 C56 F56 179.1(3) . . . . ? B1 C51 C56 F56 7.3(5) . . . . ? C52 C51 C56 C55 0.4(6) . . . . ? B1 C51 C56 C55 -171.3(4) . . . . ? C31 B1 C61 C66 106.8(4) . . . . ? C41 B1 C61 C66 -130.2(4) . . . . ? C51 B1 C61 C66 -15.0(5) . . . . ? C31 B1 C61 C62 -64.0(4) . . . . ? C41 B1 C61 C62 58.9(4) . . . . ? C51 B1 C61 C62 174.2(3) . . . . ? C66 C61 C62 F62 -178.4(3) . . . . ? B1 C61 C62 F62 -6.2(5) . . . . ? C66 C61 C62 C63 0.3(5) . . . . ? B1 C61 C62 C63 172.5(4) . . . . ? F62 C62 C63 F63 -0.8(5) . . . . ? C61 C62 C63 F63 -179.6(3) . . . . ? F62 C62 C63 C64 179.1(3) . . . . ? C61 C62 C63 C64 0.3(6) . . . . ? F63 C63 C64 F64 -0.3(6) . . . . ? C62 C63 C64 F64 179.8(4) . . . . ? F63 C63 C64 C65 179.6(4) . . . . ? C62 C63 C64 C65 -0.3(6) . . . . ? F64 C64 C65 F65 -0.7(6) . . . . ? C63 C64 C65 F65 179.3(3) . . . . ? F64 C64 C65 C66 179.6(3) . . . . ? C63 C64 C65 C66 -0.4(6) . . . . ? F65 C65 C66 F66 2.5(5) . . . . ? C64 C65 C66 F66 -177.8(3) . . . . ? F65 C65 C66 C61 -178.6(3) . . . . ? C64 C65 C66 C61 1.1(6) . . . . ? C62 C61 C66 F66 177.8(3) . . . . ? B1 C61 C66 F66 6.5(6) . . . . ? C62 C61 C66 C65 -1.1(5) . . . . ? B1 C61 C66 C65 -172.4(4) . . . . ? C76 C71 C72 C73 0.5(8) . . . . ? Br C71 C72 C73 179.2(4) . . . . ? C71 C72 C73 C74 -1.3(8) . . . . ? C72 C73 C74 C75 1.4(9) . . . . ? C73 C74 C75 C76 -0.7(9) . . . . ? C72 C71 C76 C75 0.3(9) . . . . ? Br C71 C76 C75 -178.5(4) . . . . ? C74 C75 C76 C71 -0.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.551 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.063