# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ebl1@cornell.edu _publ_contact_author_name 'Emil Lobkovsky' loop_ _publ_author_name 'C. Moyses Araujo' 'Mark D. Doherty' 'Steven J. Konezny' 'Oana R. Luca' 'Alex Usyatinsky' 'Hans Grade' 'Emil Lobkovsky' 'Grigorii L. Soloveichik' 'Robert H. Crabtree' 'Victor S. Batista' # Attachment 'solo4.cif' data_solo4 _database_code_depnum_ccdc_archive 'CCDC 854625' #TrackingRef 'solo4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H46 Co N6 O4, C2 H3 N, Cl4 Co' _chemical_formula_sum 'C48 H49 Cl4 Co2 N7 O4' _chemical_formula_weight 1047.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.8237(15) _cell_length_b 15.3342(14) _cell_length_c 19.2414(16) _cell_angle_alpha 90.00 _cell_angle_beta 113.367(3) _cell_angle_gamma 90.00 _cell_volume 4827.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8647 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.62 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7617 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42880 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.10 _reflns_number_total 10559 _reflns_number_gt 7297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered solvent (water?) was SQEEZEd. ; _iucr_refine_instructions_details ; TITL solo4 in P2(1)/n CELL 0.71073 17.8237 15.3342 19.2414 90.000 113.367 90.000 ZERR 4.00 0.0015 0.0014 0.0016 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O CL CO UNIT 192 196 28 16 16 8 TEMP -100 SIZE 0.025 0.30 0.30 SHEL 100 .78 OMIT -1 0 1 L.S. 8 ACTA WPDB WGHT 0.0726 0.0000 FVAR 0.83624 CO2 6 0.329012 -0.382756 0.588739 11.00000 0.03186 0.02789 = 0.03202 -0.00264 0.01148 -0.00295 CO1 6 0.470493 0.136050 0.723626 11.00000 0.01949 0.02207 = 0.02505 0.00149 0.00960 0.00230 O1 4 0.823050 0.249937 0.671249 11.00000 0.02809 0.05685 = 0.06173 0.01476 0.02082 0.00368 O2 4 0.482168 -0.242383 0.920561 11.00000 0.05147 0.03006 = 0.03789 0.00418 0.01266 0.00067 O3 4 0.188642 0.057038 0.350825 11.00000 0.03407 0.05182 = 0.04285 -0.00918 -0.00308 0.01033 O4 4 0.395905 0.477852 0.920799 11.00000 0.05202 0.03468 = 0.06366 -0.00611 0.03382 0.00727 N1 3 0.516580 0.234902 0.685595 11.00000 0.02420 0.02183 = 0.02598 0.00285 0.00880 0.00306 N2 3 0.381050 0.210036 0.689670 11.00000 0.02019 0.02785 = 0.02196 -0.00258 0.00728 0.00333 N3 3 0.392075 0.062935 0.748107 11.00000 0.02332 0.02635 = 0.02238 -0.00062 0.00872 0.00159 N4 3 0.458808 0.051194 0.628254 11.00000 0.02320 0.02506 = 0.02765 0.00167 0.01145 0.00101 N5 3 0.565599 0.064160 0.766402 11.00000 0.02252 0.02188 = 0.02549 0.00353 0.01008 0.00227 N6 3 0.523984 0.183312 0.837232 11.00000 0.02298 0.02631 = 0.02818 -0.00007 0.00973 0.00039 C1 1 0.491195 0.386757 0.636400 11.00000 0.03929 0.02346 = 0.04779 0.00461 0.01764 0.00309 AFIX 137 H1A 2 0.550040 0.388311 0.648605 11.00000 -1.50000 H1B 2 0.476541 0.435292 0.661718 11.00000 -1.50000 H1C 2 0.461057 0.391987 0.581511 11.00000 -1.50000 AFIX 0 C2 1 0.469912 0.302973 0.662701 11.00000 0.02931 0.02311 = 0.02640 -0.00292 0.01026 0.00022 C3 1 0.389567 0.290781 0.665870 11.00000 0.02613 0.02560 = 0.02432 -0.00160 0.00648 0.00345 C4 1 0.326865 0.352063 0.648082 11.00000 0.02754 0.03056 = 0.03675 -0.00240 0.00679 0.00583 AFIX 43 H4A 2 0.332696 0.408894 0.631202 11.00000 -1.20000 AFIX 0 C5 1 0.255543 0.327270 0.655857 11.00000 0.02786 0.03603 = 0.03849 -0.00200 0.00659 0.01540 AFIX 43 H5A 2 0.211712 0.367568 0.643889 11.00000 -1.20000 AFIX 0 C6 1 0.247692 0.243482 0.681157 11.00000 0.02016 0.04571 = 0.03715 0.00116 0.00933 0.00561 AFIX 43 H6A 2 0.199126 0.226640 0.686808 11.00000 -1.20000 AFIX 0 C7 1 0.312403 0.185506 0.697818 11.00000 0.02317 0.03008 = 0.02369 -0.00323 0.00827 0.00101 C8 1 0.320143 0.097222 0.730628 11.00000 0.02139 0.03666 = 0.02184 0.00172 0.00815 0.00058 C9 1 0.251011 0.056523 0.743653 11.00000 0.02414 0.05265 = 0.04374 0.01034 0.01699 0.00102 AFIX 137 H9A 2 0.260261 -0.006434 0.750914 11.00000 -1.50000 H9B 2 0.199896 0.067168 0.699717 11.00000 -1.50000 H9C 2 0.247359 0.082038 0.788905 11.00000 -1.50000 AFIX 0 C10 1 0.595616 0.234865 0.681119 11.00000 0.02434 0.02022 = 0.03298 0.00293 0.01137 0.00202 C11 1 0.666673 0.238114 0.746838 11.00000 0.02938 0.03571 = 0.02926 0.00712 0.01062 0.00164 AFIX 43 H11A 2 0.663824 0.237681 0.795104 11.00000 -1.20000 AFIX 0 C12 1 0.741642 0.241990 0.741056 11.00000 0.02446 0.04194 = 0.03879 0.01005 0.00533 -0.00153 AFIX 43 H12A 2 0.790395 0.244262 0.785721 11.00000 -1.20000 AFIX 0 C13 1 0.746328 0.242591 0.671050 11.00000 0.02615 0.02993 = 0.05077 0.00953 0.01959 0.00488 C14 1 0.675630 0.236269 0.605507 11.00000 0.03757 0.03479 = 0.04202 0.00026 0.02484 0.00071 AFIX 43 H14A 2 0.678717 0.234766 0.557352 11.00000 -1.20000 AFIX 0 C15 1 0.600870 0.232191 0.610985 11.00000 0.02747 0.03140 = 0.03365 -0.00182 0.01236 -0.00073 AFIX 43 H15A 2 0.552373 0.227498 0.566277 11.00000 -1.20000 AFIX 0 C16 1 0.828248 0.274063 0.600690 11.00000 0.04288 0.06613 = 0.06658 0.00175 0.03645 -0.00498 AFIX 137 H16A 2 0.808834 0.225632 0.564716 11.00000 -1.50000 H16B 2 0.885164 0.287304 0.609757 11.00000 -1.50000 H16C 2 0.794270 0.325612 0.579749 11.00000 -1.50000 AFIX 0 C17 1 0.413106 -0.018319 0.789302 11.00000 0.01874 0.02624 = 0.02603 0.00288 0.00826 0.00050 C18 1 0.407347 -0.097546 0.752637 11.00000 0.02899 0.03461 = 0.02471 -0.00279 0.00911 -0.00214 AFIX 43 H18A 2 0.387636 -0.099481 0.698980 11.00000 -1.20000 AFIX 0 C19 1 0.430570 -0.174434 0.794737 11.00000 0.02859 0.02737 = 0.04012 -0.00602 0.01338 -0.00327 AFIX 43 H19A 2 0.426503 -0.228708 0.769687 11.00000 -1.20000 AFIX 0 C20 1 0.459515 -0.171584 0.872960 11.00000 0.02214 0.03180 = 0.03196 0.00660 0.00878 0.00218 C21 1 0.466868 -0.092062 0.909695 11.00000 0.03655 0.03457 = 0.02420 0.00138 0.00809 -0.00241 AFIX 43 H21A 2 0.488055 -0.089895 0.963415 11.00000 -1.20000 AFIX 0 C22 1 0.443250 -0.015925 0.867853 11.00000 0.03527 0.03202 = 0.02846 -0.00232 0.01136 -0.00498 AFIX 43 H22A 2 0.447700 0.038307 0.893055 11.00000 -1.20000 AFIX 0 C23 1 0.479457 -0.326983 0.887897 11.00000 0.04907 0.03431 = 0.05158 0.00260 0.00647 0.00249 AFIX 137 H23A 2 0.424606 -0.337539 0.849097 11.00000 -1.50000 H23B 2 0.492415 -0.371526 0.927480 11.00000 -1.50000 H23C 2 0.519498 -0.329704 0.864792 11.00000 -1.50000 AFIX 0 C24 1 0.535242 -0.065372 0.592653 11.00000 0.04515 0.05954 = 0.03255 -0.00997 0.00915 0.02063 AFIX 137 H24A 2 0.500207 -0.051587 0.539959 11.00000 -1.50000 H24B 2 0.522494 -0.124101 0.604881 11.00000 -1.50000 H24C 2 0.592687 -0.062861 0.599479 11.00000 -1.50000 AFIX 0 C25 1 0.520527 -0.000747 0.643888 11.00000 0.02788 0.02877 = 0.02942 0.00056 0.01315 0.00419 C26 1 0.583179 0.005945 0.722543 11.00000 0.02612 0.02270 = 0.03068 0.00307 0.01436 0.00326 C27 1 0.654293 -0.043512 0.751892 11.00000 0.03461 0.03443 = 0.03558 -0.00066 0.01320 0.01262 AFIX 43 H27A 2 0.667171 -0.083520 0.720552 11.00000 -1.20000 AFIX 0 C28 1 0.706212 -0.033822 0.827381 11.00000 0.02881 0.03977 = 0.04042 0.00396 0.00910 0.01290 AFIX 43 H28A 2 0.754837 -0.067479 0.848171 11.00000 -1.20000 AFIX 0 C29 1 0.687112 0.024723 0.872150 11.00000 0.02928 0.03673 = 0.03024 0.00241 0.00723 0.00806 AFIX 43 H29A 2 0.721740 0.031316 0.924154 11.00000 -1.20000 AFIX 0 C30 1 0.616016 0.074100 0.839697 11.00000 0.02415 0.02570 = 0.02769 0.00382 0.00909 -0.00060 C31 1 0.589805 0.143304 0.879458 11.00000 0.02714 0.02512 = 0.02665 0.00321 0.01129 -0.00283 C32 1 0.640074 0.161771 0.961445 11.00000 0.03706 0.04251 = 0.02736 0.00195 0.00513 0.00668 AFIX 137 H32A 2 0.612610 0.206010 0.979741 11.00000 -1.50000 H32B 2 0.694021 0.183272 0.967262 11.00000 -1.50000 H32C 2 0.646429 0.108096 0.990892 11.00000 -1.50000 AFIX 0 C33 1 0.390164 0.048610 0.557175 11.00000 0.02727 0.02986 = 0.02647 -0.00151 0.01335 0.00100 C34 1 0.358674 0.127152 0.520796 11.00000 0.02790 0.03038 = 0.02967 -0.00349 0.01134 0.00401 AFIX 43 H34A 2 0.383412 0.180679 0.543132 11.00000 -1.20000 AFIX 0 C35 1 0.291692 0.127603 0.452442 11.00000 0.03426 0.03424 = 0.03407 0.00241 0.01259 0.01123 AFIX 43 H35A 2 0.271222 0.181460 0.427819 11.00000 -1.20000 AFIX 0 C36 1 0.253626 0.049352 0.419053 11.00000 0.02475 0.04345 = 0.03227 -0.00734 0.00712 0.00790 C37 1 0.283310 -0.028538 0.455521 11.00000 0.03156 0.03477 = 0.04154 -0.00496 0.01019 -0.00134 AFIX 43 H37A 2 0.257852 -0.081931 0.433578 11.00000 -1.20000 AFIX 0 C38 1 0.351305 -0.028764 0.525219 11.00000 0.03513 0.02688 = 0.04079 0.00158 0.01338 0.00004 AFIX 43 H38A 2 0.370843 -0.082399 0.550690 11.00000 -1.20000 AFIX 0 C39 1 0.150545 -0.021527 0.315867 11.00000 0.04737 0.06542 = 0.05842 -0.02263 -0.01747 0.00217 AFIX 137 H39A 2 0.189273 -0.056594 0.303105 11.00000 -1.50000 H39B 2 0.102699 -0.008078 0.269586 11.00000 -1.50000 H39C 2 0.133279 -0.054317 0.350702 11.00000 -1.50000 AFIX 0 C40 1 0.492576 0.256112 0.863703 11.00000 0.02357 0.02788 = 0.02288 -0.00083 0.00536 0.00289 C41 1 0.425271 0.247441 0.881785 11.00000 0.02929 0.02818 = 0.03350 0.00082 0.01319 -0.00468 AFIX 43 H41A 2 0.402089 0.191400 0.880645 11.00000 -1.20000 AFIX 0 C42 1 0.390997 0.320003 0.901686 11.00000 0.02867 0.04056 = 0.03329 -0.00130 0.01586 0.00245 AFIX 43 H42A 2 0.345380 0.313400 0.915015 11.00000 -1.20000 AFIX 0 C43 1 0.423999 0.401749 0.901858 11.00000 0.03298 0.03124 = 0.03419 -0.00235 0.01179 0.00927 C44 1 0.490077 0.410978 0.882162 11.00000 0.05127 0.02643 = 0.06812 -0.00963 0.03613 -0.00747 AFIX 43 H44A 2 0.511969 0.467334 0.881605 11.00000 -1.20000 AFIX 0 C45 1 0.524792 0.338763 0.863186 11.00000 0.03459 0.03231 = 0.05516 -0.00473 0.02680 -0.00460 AFIX 43 H45A 2 0.570396 0.345615 0.849874 11.00000 -1.20000 AFIX 0 C46 1 0.330407 0.470003 0.945843 11.00000 0.07001 0.05224 = 0.06161 -0.00087 0.03841 0.01915 AFIX 137 H46A 2 0.281900 0.446673 0.904633 11.00000 -1.50000 H46B 2 0.317799 0.527521 0.960651 11.00000 -1.50000 H46C 2 0.346755 0.430449 0.989361 11.00000 -1.50000 AFIX 0 CL1 5 0.202582 -0.441700 0.558620 11.00000 0.03495 0.05147 = 0.04216 -0.00123 0.01259 -0.01140 CL2 5 0.320845 -0.234683 0.589937 11.00000 0.08098 0.02739 = 0.05099 -0.00516 0.02937 -0.00458 CL3 5 0.374949 -0.432370 0.501113 11.00000 0.03884 0.04816 = 0.03397 -0.00433 0.01238 0.00628 CL4 5 0.421033 -0.421273 0.706572 11.00000 0.03737 0.05032 = 0.03346 -0.00348 0.00928 0.00525 N1S 3 0.343879 0.326662 0.458028 11.00000 0.12330 0.07677 = 0.09481 0.01386 0.04474 -0.04414 C1S 1 0.377108 0.356335 0.425742 11.00000 0.09848 0.05777 = 0.06922 -0.00251 0.00430 -0.01707 C2S 1 0.415994 0.405786 0.381052 11.00000 0.09326 0.16167 = 0.09738 0.01864 0.02328 -0.05758 AFIX 33 H2SA 2 0.460114 0.370737 0.377104 11.00000 -1.50000 H2SB 2 0.438363 0.460870 0.406740 11.00000 -1.50000 H2SC 2 0.374813 0.417933 0.330228 11.00000 -1.50000 HKLF 4 END ; _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^)+(0.0726P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10559 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Co2 Co 0.32901(3) -0.38275(3) 0.58874(2) 0.03104(13) Uani 1 1 d . . . Co1 Co 0.47049(2) 0.13605(3) 0.72362(2) 0.02203(11) Uani 1 1 d . . . O1 O 0.82306(14) 0.24993(17) 0.67127(15) 0.0481(7) Uani 1 1 d . . . O2 O 0.48217(15) -0.24237(15) 0.92057(13) 0.0416(6) Uani 1 1 d . . . O3 O 0.18865(14) 0.05703(17) 0.35084(14) 0.0488(7) Uani 1 1 d . . . O4 O 0.39592(15) 0.47785(16) 0.92080(15) 0.0467(6) Uani 1 1 d . . . N1 N 0.51656(15) 0.23494(16) 0.68560(13) 0.0244(5) Uani 1 1 d . . . N2 N 0.38107(14) 0.21005(16) 0.68969(13) 0.0239(5) Uani 1 1 d . . . N3 N 0.39204(14) 0.06295(16) 0.74807(13) 0.0242(5) Uani 1 1 d . . . N4 N 0.45878(15) 0.05120(16) 0.62825(14) 0.0249(5) Uani 1 1 d . . . N5 N 0.56559(14) 0.06418(15) 0.76641(13) 0.0232(5) Uani 1 1 d . . . N6 N 0.52398(15) 0.18331(16) 0.83724(14) 0.0259(6) Uani 1 1 d . . . C1 C 0.4912(2) 0.3867(2) 0.6364(2) 0.0367(8) Uani 1 1 d . . . H1A H 0.5500 0.3883 0.6486 0.055 Uiso 1 1 calc R . . H1B H 0.4765 0.4353 0.6617 0.055 Uiso 1 1 calc R . . H1C H 0.4610 0.3920 0.5815 0.055 Uiso 1 1 calc R . . C2 C 0.46993(19) 0.3029(2) 0.66272(17) 0.0267(7) Uani 1 1 d . . . C3 C 0.38958(18) 0.29077(19) 0.66587(17) 0.0264(7) Uani 1 1 d . . . C4 C 0.32685(19) 0.3521(2) 0.64806(18) 0.0335(7) Uani 1 1 d . . . H4A H 0.3327 0.4089 0.6312 0.040 Uiso 1 1 calc R . . C5 C 0.2555(2) 0.3272(2) 0.65585(19) 0.0364(8) Uani 1 1 d . . . H5A H 0.2117 0.3674 0.6439 0.044 Uiso 1 1 calc R . . C6 C 0.24770(19) 0.2435(2) 0.68114(19) 0.0351(8) Uani 1 1 d . . . H6A H 0.1991 0.2266 0.6868 0.042 Uiso 1 1 calc R . . C7 C 0.31242(18) 0.1855(2) 0.69783(16) 0.0260(7) Uani 1 1 d . . . C8 C 0.32013(18) 0.0973(2) 0.73062(16) 0.0270(7) Uani 1 1 d . . . C9 C 0.25103(19) 0.0565(2) 0.7437(2) 0.0392(8) Uani 1 1 d . . . H9A H 0.2603 -0.0064 0.7509 0.059 Uiso 1 1 calc R . . H9B H 0.1999 0.0672 0.6998 0.059 Uiso 1 1 calc R . . H9C H 0.2474 0.0820 0.7889 0.059 Uiso 1 1 calc R . . C10 C 0.59564(18) 0.23489(19) 0.68114(18) 0.0260(7) Uani 1 1 d . . . C11 C 0.66666(19) 0.2381(2) 0.74685(18) 0.0318(7) Uani 1 1 d . . . H11A H 0.6638 0.2377 0.7951 0.038 Uiso 1 1 calc R . . C12 C 0.7416(2) 0.2420(2) 0.7410(2) 0.0374(8) Uani 1 1 d . . . H12A H 0.7904 0.2443 0.7857 0.045 Uiso 1 1 calc R . . C13 C 0.7463(2) 0.2426(2) 0.6711(2) 0.0346(8) Uani 1 1 d . . . C14 C 0.6756(2) 0.2363(2) 0.6055(2) 0.0352(8) Uani 1 1 d . . . H14A H 0.6787 0.2348 0.5573 0.042 Uiso 1 1 calc R . . C15 C 0.6009(2) 0.2321(2) 0.61103(18) 0.0307(7) Uani 1 1 d . . . H15A H 0.5524 0.2274 0.5663 0.037 Uiso 1 1 calc R . . C16 C 0.8283(2) 0.2741(3) 0.6007(2) 0.0540(11) Uani 1 1 d . . . H16A H 0.8088 0.2257 0.5647 0.081 Uiso 1 1 calc R . . H16B H 0.8852 0.2873 0.6098 0.081 Uiso 1 1 calc R . . H16C H 0.7943 0.3256 0.5798 0.081 Uiso 1 1 calc R . . C17 C 0.41308(17) -0.01831(19) 0.78929(16) 0.0239(6) Uani 1 1 d . . . C18 C 0.40729(19) -0.0975(2) 0.75263(18) 0.0303(7) Uani 1 1 d . . . H18A H 0.3875 -0.0995 0.6990 0.036 Uiso 1 1 calc R . . C19 C 0.43057(19) -0.1744(2) 0.79474(19) 0.0320(7) Uani 1 1 d . . . H19A H 0.4265 -0.2287 0.7697 0.038 Uiso 1 1 calc R . . C20 C 0.45954(18) -0.1715(2) 0.87295(18) 0.0294(7) Uani 1 1 d . . . C21 C 0.4669(2) -0.0921(2) 0.90970(18) 0.0331(7) Uani 1 1 d . . . H21A H 0.4880 -0.0899 0.9634 0.040 Uiso 1 1 calc R . . C22 C 0.4433(2) -0.0160(2) 0.86785(18) 0.0325(7) Uani 1 1 d . . . H22A H 0.4478 0.0383 0.8931 0.039 Uiso 1 1 calc R . . C23 C 0.4795(2) -0.3270(2) 0.8879(2) 0.0493(10) Uani 1 1 d . . . H23A H 0.4246 -0.3376 0.8492 0.074 Uiso 1 1 calc R . . H23B H 0.4925 -0.3715 0.9275 0.074 Uiso 1 1 calc R . . H23C H 0.5194 -0.3296 0.8647 0.074 Uiso 1 1 calc R . . C24 C 0.5352(2) -0.0654(3) 0.5926(2) 0.0478(10) Uani 1 1 d . . . H24A H 0.5002 -0.0515 0.5399 0.072 Uiso 1 1 calc R . . H24B H 0.5225 -0.1241 0.6048 0.072 Uiso 1 1 calc R . . H24C H 0.5927 -0.0629 0.5994 0.072 Uiso 1 1 calc R . . C25 C 0.52054(19) -0.0008(2) 0.64388(17) 0.0281(7) Uani 1 1 d . . . C26 C 0.58320(18) 0.00596(19) 0.72259(17) 0.0255(6) Uani 1 1 d . . . C27 C 0.6543(2) -0.0435(2) 0.75188(18) 0.0350(8) Uani 1 1 d . . . H27A H 0.6671 -0.0835 0.7205 0.042 Uiso 1 1 calc R . . C28 C 0.7062(2) -0.0339(2) 0.82736(19) 0.0378(8) Uani 1 1 d . . . H28A H 0.7548 -0.0675 0.8482 0.045 Uiso 1 1 calc R . . C29 C 0.68710(19) 0.0247(2) 0.87214(18) 0.0335(7) Uani 1 1 d . . . H29A H 0.7217 0.0313 0.9241 0.040 Uiso 1 1 calc R . . C30 C 0.61601(18) 0.0741(2) 0.83967(17) 0.0264(7) Uani 1 1 d . . . C31 C 0.58985(18) 0.1433(2) 0.87945(17) 0.0261(7) Uani 1 1 d . . . C32 C 0.6400(2) 0.1618(2) 0.96142(18) 0.0381(8) Uani 1 1 d . . . H32A H 0.6126 0.2060 0.9797 0.057 Uiso 1 1 calc R . . H32B H 0.6940 0.1833 0.9673 0.057 Uiso 1 1 calc R . . H32C H 0.6464 0.1081 0.9909 0.057 Uiso 1 1 calc R . . C33 C 0.39014(18) 0.0486(2) 0.55716(17) 0.0271(7) Uani 1 1 d . . . C34 C 0.35868(19) 0.1271(2) 0.52076(17) 0.0293(7) Uani 1 1 d . . . H34A H 0.3834 0.1807 0.5431 0.035 Uiso 1 1 calc R . . C35 C 0.2917(2) 0.1276(2) 0.45248(19) 0.0347(8) Uani 1 1 d . . . H35A H 0.2713 0.1815 0.4279 0.042 Uiso 1 1 calc R . . C36 C 0.25365(19) 0.0494(2) 0.41904(18) 0.0349(8) Uani 1 1 d . . . C37 C 0.2833(2) -0.0285(2) 0.45555(19) 0.0374(8) Uani 1 1 d . . . H37A H 0.2579 -0.0819 0.4336 0.045 Uiso 1 1 calc R . . C38 C 0.3513(2) -0.0287(2) 0.52524(19) 0.0349(8) Uani 1 1 d . . . H38A H 0.3708 -0.0824 0.5507 0.042 Uiso 1 1 calc R . . C39 C 0.1506(3) -0.0215(3) 0.3158(3) 0.0692(14) Uani 1 1 d . . . H39A H 0.1893 -0.0566 0.3032 0.104 Uiso 1 1 calc R . . H39B H 0.1028 -0.0081 0.2695 0.104 Uiso 1 1 calc R . . H39C H 0.1331 -0.0543 0.3506 0.104 Uiso 1 1 calc R . . C40 C 0.49259(18) 0.2561(2) 0.86366(16) 0.0260(7) Uani 1 1 d . . . C41 C 0.42531(19) 0.2475(2) 0.88180(18) 0.0302(7) Uani 1 1 d . . . H41A H 0.4022 0.1914 0.8807 0.036 Uiso 1 1 calc R . . C42 C 0.39100(19) 0.3200(2) 0.90165(18) 0.0329(7) Uani 1 1 d . . . H42A H 0.3454 0.3134 0.9149 0.039 Uiso 1 1 calc R . . C43 C 0.4240(2) 0.4017(2) 0.90185(18) 0.0334(8) Uani 1 1 d . . . C44 C 0.4901(2) 0.4109(2) 0.8822(2) 0.0449(9) Uani 1 1 d . . . H44A H 0.5120 0.4673 0.8816 0.054 Uiso 1 1 calc R . . C45 C 0.5248(2) 0.3388(2) 0.8632(2) 0.0379(8) Uani 1 1 d . . . H45A H 0.5704 0.3457 0.8500 0.045 Uiso 1 1 calc R . . C46 C 0.3304(3) 0.4700(3) 0.9458(2) 0.0574(11) Uani 1 1 d . . . H46A H 0.2819 0.4467 0.9046 0.086 Uiso 1 1 calc R . . H46B H 0.3178 0.5275 0.9607 0.086 Uiso 1 1 calc R . . H46C H 0.3467 0.4304 0.9894 0.086 Uiso 1 1 calc R . . Cl1 Cl 0.20258(5) -0.44170(6) 0.55862(5) 0.0438(2) Uani 1 1 d . . . Cl2 Cl 0.32084(7) -0.23469(6) 0.58993(6) 0.0522(3) Uani 1 1 d . . . Cl3 Cl 0.37495(5) -0.43235(6) 0.50112(5) 0.0410(2) Uani 1 1 d . . . Cl4 Cl 0.42102(5) -0.42127(6) 0.70656(5) 0.0420(2) Uani 1 1 d . . . N1S N 0.3439(3) 0.3266(3) 0.4580(3) 0.0978(17) Uani 1 1 d . . . C1S C 0.3771(4) 0.3563(3) 0.4258(3) 0.0845(17) Uani 1 1 d . . . C2S C 0.4160(4) 0.4058(5) 0.3811(4) 0.122(3) Uani 1 1 d . . . H2SA H 0.4601 0.3707 0.3771 0.183 Uiso 1 1 calc R . . H2SB H 0.4384 0.4608 0.4068 0.183 Uiso 1 1 calc R . . H2SC H 0.3748 0.4179 0.3303 0.183 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 Co2 0.0319(3) 0.0280(2) 0.0321(2) -0.00267(18) 0.0115(2) -0.00294(19) Co1 0.0195(2) 0.0222(2) 0.0252(2) 0.00149(16) 0.00969(17) 0.00235(17) O1 0.0280(13) 0.0571(17) 0.0618(17) 0.0148(13) 0.0207(12) 0.0037(12) O2 0.0518(15) 0.0302(13) 0.0379(14) 0.0042(10) 0.0126(12) 0.0008(11) O3 0.0338(14) 0.0520(17) 0.0433(15) -0.0089(12) -0.0030(11) 0.0104(12) O4 0.0522(16) 0.0344(14) 0.0638(17) -0.0062(12) 0.0338(14) 0.0073(12) N1 0.0242(13) 0.0219(13) 0.0260(13) 0.0028(10) 0.0089(11) 0.0030(11) N2 0.0202(13) 0.0285(14) 0.0219(12) -0.0027(10) 0.0072(10) 0.0034(11) N3 0.0237(13) 0.0262(14) 0.0222(13) -0.0005(10) 0.0086(10) 0.0016(11) N4 0.0229(13) 0.0252(13) 0.0279(13) 0.0018(11) 0.0115(11) 0.0011(11) N5 0.0226(13) 0.0216(13) 0.0262(13) 0.0037(10) 0.0105(11) 0.0022(11) N6 0.0233(13) 0.0263(14) 0.0279(13) -0.0001(11) 0.0098(11) 0.0001(11) C1 0.039(2) 0.0235(17) 0.048(2) 0.0047(15) 0.0178(17) 0.0028(15) C2 0.0300(17) 0.0231(16) 0.0263(16) -0.0027(12) 0.0104(13) 0.0002(13) C3 0.0265(16) 0.0250(16) 0.0248(15) -0.0014(12) 0.0071(13) 0.0033(13) C4 0.0275(17) 0.0305(18) 0.0370(18) -0.0025(14) 0.0069(14) 0.0054(15) C5 0.0282(18) 0.036(2) 0.0388(19) -0.0020(15) 0.0068(15) 0.0155(15) C6 0.0205(16) 0.046(2) 0.0370(19) 0.0012(16) 0.0094(14) 0.0057(15) C7 0.0237(16) 0.0303(17) 0.0232(15) -0.0033(13) 0.0084(13) 0.0010(13) C8 0.0213(16) 0.0376(18) 0.0219(15) 0.0013(13) 0.0082(12) 0.0003(14) C9 0.0248(17) 0.053(2) 0.044(2) 0.0105(17) 0.0173(15) 0.0009(16) C10 0.0247(16) 0.0200(15) 0.0334(17) 0.0026(13) 0.0115(13) 0.0018(13) C11 0.0298(18) 0.0352(19) 0.0296(17) 0.0072(14) 0.0107(14) 0.0016(15) C12 0.0246(17) 0.042(2) 0.0392(19) 0.0100(16) 0.0055(15) -0.0013(15) C13 0.0262(18) 0.0304(18) 0.051(2) 0.0097(15) 0.0200(16) 0.0050(14) C14 0.0374(19) 0.0346(19) 0.042(2) 0.0002(15) 0.0250(17) 0.0009(16) C15 0.0275(17) 0.0312(18) 0.0337(18) -0.0018(14) 0.0123(14) -0.0010(14) C16 0.043(2) 0.066(3) 0.067(3) 0.002(2) 0.037(2) -0.005(2) C17 0.0183(15) 0.0270(16) 0.0257(15) 0.0030(12) 0.0080(12) 0.0003(13) C18 0.0292(17) 0.0351(18) 0.0255(16) -0.0029(14) 0.0097(14) -0.0019(15) C19 0.0285(17) 0.0276(17) 0.0398(19) -0.0062(14) 0.0134(15) -0.0031(14) C20 0.0220(16) 0.0322(18) 0.0324(17) 0.0066(14) 0.0089(13) 0.0021(14) C21 0.0366(19) 0.0351(19) 0.0238(16) 0.0013(14) 0.0081(14) -0.0022(15) C22 0.0355(18) 0.0320(18) 0.0287(17) -0.0023(14) 0.0113(14) -0.0052(15) C23 0.049(2) 0.035(2) 0.051(2) 0.0026(17) 0.0064(19) 0.0026(18) C24 0.045(2) 0.060(3) 0.0328(19) -0.0096(17) 0.0091(17) 0.0204(19) C25 0.0279(17) 0.0291(17) 0.0292(16) 0.0006(13) 0.0134(14) 0.0038(14) C26 0.0261(16) 0.0226(15) 0.0313(16) 0.0033(13) 0.0149(13) 0.0032(13) C27 0.0346(19) 0.0339(19) 0.0359(19) -0.0006(15) 0.0134(15) 0.0129(15) C28 0.0294(18) 0.039(2) 0.040(2) 0.0039(16) 0.0093(15) 0.0132(16) C29 0.0290(17) 0.0367(19) 0.0304(17) 0.0022(14) 0.0071(14) 0.0077(15) C30 0.0242(16) 0.0261(16) 0.0275(16) 0.0042(13) 0.0087(13) -0.0009(13) C31 0.0269(16) 0.0252(16) 0.0269(16) 0.0034(13) 0.0114(13) -0.0027(14) C32 0.0367(19) 0.043(2) 0.0279(17) 0.0017(15) 0.0053(15) 0.0066(17) C33 0.0271(16) 0.0298(17) 0.0270(16) -0.0013(13) 0.0135(13) 0.0014(14) C34 0.0272(17) 0.0310(18) 0.0298(17) -0.0035(13) 0.0113(14) 0.0039(14) C35 0.0344(18) 0.0345(19) 0.0345(18) 0.0029(15) 0.0129(15) 0.0118(16) C36 0.0245(17) 0.043(2) 0.0328(18) -0.0080(15) 0.0072(14) 0.0077(16) C37 0.0319(19) 0.0348(19) 0.042(2) -0.0047(16) 0.0109(16) -0.0008(16) C38 0.0351(19) 0.0273(17) 0.0407(19) 0.0013(15) 0.0133(16) -0.0002(15) C39 0.047(3) 0.065(3) 0.058(3) -0.023(2) -0.018(2) 0.002(2) C40 0.0235(16) 0.0283(16) 0.0227(15) -0.0010(12) 0.0054(13) 0.0024(13) C41 0.0297(17) 0.0280(17) 0.0334(17) 0.0007(13) 0.0131(14) -0.0046(14) C42 0.0281(17) 0.040(2) 0.0334(18) -0.0016(15) 0.0156(14) 0.0023(15) C43 0.0329(18) 0.0315(18) 0.0344(18) -0.0025(14) 0.0119(15) 0.0095(15) C44 0.051(2) 0.0270(19) 0.068(3) -0.0095(17) 0.036(2) -0.0081(17) C45 0.0341(19) 0.0326(18) 0.055(2) -0.0048(16) 0.0269(17) -0.0045(16) C46 0.070(3) 0.053(3) 0.062(3) -0.001(2) 0.039(2) 0.019(2) Cl1 0.0350(5) 0.0516(6) 0.0422(5) -0.0012(4) 0.0126(4) -0.0115(4) Cl2 0.0809(7) 0.0276(5) 0.0511(6) -0.0051(4) 0.0294(5) -0.0047(5) Cl3 0.0389(5) 0.0481(5) 0.0342(4) -0.0044(4) 0.0125(4) 0.0062(4) Cl4 0.0374(5) 0.0504(5) 0.0336(5) -0.0035(4) 0.0092(4) 0.0054(4) N1S 0.123(4) 0.077(3) 0.095(4) 0.014(3) 0.045(3) -0.044(3) C1S 0.098(4) 0.058(3) 0.069(4) -0.002(3) 0.004(3) -0.017(3) C2S 0.093(5) 0.161(7) 0.098(5) 0.019(5) 0.023(4) -0.058(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co2 Cl2 2.2759(10) . ? Co2 Cl3 2.2774(9) . ? Co2 Cl1 2.2792(10) . ? Co2 Cl4 2.2867(10) . ? Co1 N2 1.852(2) . ? Co1 N5 1.913(2) . ? Co1 N3 1.989(2) . ? Co1 N1 1.996(2) . ? Co1 N6 2.135(2) . ? Co1 N4 2.191(2) . ? O1 C13 1.371(4) . ? O1 C16 1.446(4) . ? O2 C20 1.374(4) . ? O2 C23 1.434(4) . ? O3 C36 1.368(4) . ? O3 C39 1.415(5) . ? O4 C43 1.375(4) . ? O4 C46 1.434(4) . ? N1 C2 1.297(4) . ? N1 C10 1.446(4) . ? N2 C7 1.347(4) . ? N2 C3 1.349(4) . ? N3 C8 1.300(4) . ? N3 C17 1.444(4) . ? N4 C25 1.294(4) . ? N4 C33 1.429(4) . ? N5 C30 1.346(4) . ? N5 C26 1.348(4) . ? N6 C31 1.287(4) . ? N6 C40 1.429(4) . ? C1 C2 1.484(4) . ? C2 C3 1.469(4) . ? C3 C4 1.396(4) . ? C4 C5 1.391(5) . ? C5 C6 1.399(5) . ? C6 C7 1.389(4) . ? C7 C8 1.476(4) . ? C8 C9 1.489(4) . ? C10 C15 1.389(4) . ? C10 C11 1.391(4) . ? C11 C12 1.386(5) . ? C12 C13 1.382(5) . ? C13 C14 1.389(5) . ? C14 C15 1.380(4) . ? C17 C18 1.388(4) . ? C17 C22 1.389(4) . ? C18 C19 1.397(5) . ? C19 C20 1.385(4) . ? C20 C21 1.389(5) . ? C21 C22 1.385(5) . ? C24 C25 1.492(4) . ? C25 C26 1.487(4) . ? C26 C27 1.390(4) . ? C27 C28 1.386(5) . ? C28 C29 1.378(5) . ? C29 C30 1.393(4) . ? C30 C31 1.487(4) . ? C31 C32 1.500(4) . ? C33 C38 1.387(4) . ? C33 C34 1.394(4) . ? C34 C35 1.381(4) . ? C35 C36 1.403(5) . ? C36 C37 1.380(5) . ? C37 C38 1.406(5) . ? C40 C41 1.382(4) . ? C40 C45 1.393(4) . ? C41 C42 1.393(4) . ? C42 C43 1.384(5) . ? C43 C44 1.380(5) . ? C44 C45 1.385(5) . ? N1S C1S 1.111(7) . ? C1S C2S 1.506(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 Cl2 Co2 Cl3 112.57(4) . . ? Cl2 Co2 Cl1 109.72(4) . . ? Cl3 Co2 Cl1 106.79(4) . . ? Cl2 Co2 Cl4 105.74(4) . . ? Cl3 Co2 Cl4 108.70(4) . . ? Cl1 Co2 Cl4 113.43(4) . . ? N2 Co1 N5 175.39(10) . . ? N2 Co1 N3 80.86(10) . . ? N5 Co1 N3 99.18(10) . . ? N2 Co1 N1 80.04(10) . . ? N5 Co1 N1 99.92(10) . . ? N3 Co1 N1 160.88(10) . . ? N2 Co1 N6 97.20(10) . . ? N5 Co1 N6 78.19(10) . . ? N3 Co1 N6 91.11(9) . . ? N1 Co1 N6 92.06(10) . . ? N2 Co1 N4 106.61(10) . . ? N5 Co1 N4 78.00(10) . . ? N3 Co1 N4 91.21(9) . . ? N1 Co1 N4 93.47(9) . . ? N6 Co1 N4 156.14(9) . . ? C13 O1 C16 117.0(3) . . ? C20 O2 C23 118.2(3) . . ? C36 O3 C39 116.5(3) . . ? C43 O4 C46 116.6(3) . . ? C2 N1 C10 119.3(2) . . ? C2 N1 Co1 115.7(2) . . ? C10 N1 Co1 125.01(18) . . ? C7 N2 C3 121.7(3) . . ? C7 N2 Co1 118.8(2) . . ? C3 N2 Co1 119.0(2) . . ? C8 N3 C17 120.4(2) . . ? C8 N3 Co1 115.1(2) . . ? C17 N3 Co1 124.22(18) . . ? C25 N4 C33 122.1(3) . . ? C25 N4 Co1 112.4(2) . . ? C33 N4 Co1 125.41(18) . . ? C30 N5 C26 120.4(3) . . ? C30 N5 Co1 119.67(19) . . ? C26 N5 Co1 119.9(2) . . ? C31 N6 C40 122.4(3) . . ? C31 N6 Co1 114.2(2) . . ? C40 N6 Co1 123.39(19) . . ? N1 C2 C3 112.8(3) . . ? N1 C2 C1 126.6(3) . . ? C3 C2 C1 120.6(3) . . ? N2 C3 C4 121.0(3) . . ? N2 C3 C2 111.9(2) . . ? C4 C3 C2 127.1(3) . . ? C5 C4 C3 117.8(3) . . ? C4 C5 C6 120.7(3) . . ? C7 C6 C5 118.7(3) . . ? N2 C7 C6 120.2(3) . . ? N2 C7 C8 111.8(3) . . ? C6 C7 C8 127.8(3) . . ? N3 C8 C7 113.4(3) . . ? N3 C8 C9 125.7(3) . . ? C7 C8 C9 120.9(3) . . ? C15 C10 C11 119.8(3) . . ? C15 C10 N1 120.0(3) . . ? C11 C10 N1 120.2(3) . . ? C12 C11 C10 119.2(3) . . ? C13 C12 C11 120.8(3) . . ? O1 C13 C12 116.3(3) . . ? O1 C13 C14 123.6(3) . . ? C12 C13 C14 120.1(3) . . ? C15 C14 C13 119.3(3) . . ? C14 C15 C10 120.8(3) . . ? C18 C17 C22 119.6(3) . . ? C18 C17 N3 121.7(3) . . ? C22 C17 N3 118.6(3) . . ? C17 C18 C19 119.9(3) . . ? C20 C19 C18 120.1(3) . . ? O2 C20 C19 125.7(3) . . ? O2 C20 C21 114.2(3) . . ? C19 C20 C21 120.0(3) . . ? C22 C21 C20 119.9(3) . . ? C21 C22 C17 120.5(3) . . ? N4 C25 C26 114.8(3) . . ? N4 C25 C24 127.7(3) . . ? C26 C25 C24 117.5(3) . . ? N5 C26 C27 120.6(3) . . ? N5 C26 C25 114.6(3) . . ? C27 C26 C25 124.8(3) . . ? C28 C27 C26 119.3(3) . . ? C29 C28 C27 119.8(3) . . ? C28 C29 C30 118.7(3) . . ? N5 C30 C29 121.2(3) . . ? N5 C30 C31 113.8(3) . . ? C29 C30 C31 124.9(3) . . ? N6 C31 C30 114.1(3) . . ? N6 C31 C32 126.0(3) . . ? C30 C31 C32 119.9(3) . . ? C38 C33 C34 119.0(3) . . ? C38 C33 N4 122.4(3) . . ? C34 C33 N4 118.5(3) . . ? C35 C34 C33 120.4(3) . . ? C34 C35 C36 120.7(3) . . ? O3 C36 C37 124.8(3) . . ? O3 C36 C35 116.0(3) . . ? C37 C36 C35 119.2(3) . . ? C36 C37 C38 119.9(3) . . ? C33 C38 C37 120.7(3) . . ? C41 C40 C45 119.3(3) . . ? C41 C40 N6 121.1(3) . . ? C45 C40 N6 119.2(3) . . ? C40 C41 C42 120.8(3) . . ? C43 C42 C41 119.4(3) . . ? O4 C43 C44 115.2(3) . . ? O4 C43 C42 124.8(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 120.6(3) . . ? C44 C45 C40 119.8(3) . . ? N1S C1S C2S 173.3(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.643 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.077 data_solo2 _database_code_depnum_ccdc_archive 'CCDC 854626' #TrackingRef 'solo2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 Cl2 Co N5' _chemical_formula_sum 'C25 H29 Cl2 Co N5' _chemical_formula_weight 529.36 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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3191(4) _cell_length_b 15.1565(5) _cell_length_c 14.1316(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.0280(10) _cell_angle_gamma 90.00 _cell_volume 2522.90(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6318 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 27.43 _exptl_crystal_description 'flat needle' _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6577 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24507 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6267 _reflns_number_gt 4670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _iucr_refine_instructions_details ; TITL solo2 in P2(1)/n CELL 0.71073 12.3191 15.1565 14.1316 90.000 107.028 90.000 ZERR 4.00 0.0004 0.0005 0.0005 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N CL CO UNIT 100 116 20 8 4 TEMP -100 SIZE 0.05 0.20 0.50 SHEL 100 .75 L.S. 8 ACTA WPDB WGHT 0.057400 0.980700 FVAR 0.10352 CO1 5 0.656221 0.167206 0.362323 11.00000 0.02137 0.02042 = 0.01598 -0.00094 -0.00046 -0.00159 CL1 4 0.835749 0.186767 0.352972 11.00000 0.02538 0.03925 = 0.03038 -0.00810 0.00739 -0.00506 CL2 4 0.633363 0.177220 0.514641 11.00000 0.04139 0.02789 = 0.02237 -0.00314 0.01026 -0.00470 N1 3 0.648004 0.021601 0.357745 11.00000 0.02374 0.01921 = 0.01870 0.00154 0.00066 0.00080 N2 3 0.543136 0.137883 0.229289 11.00000 0.02127 0.02045 = 0.01822 0.00048 0.00049 -0.00056 N3 3 0.589000 0.297820 0.299193 11.00000 0.02392 0.01918 = 0.02116 -0.00061 0.00323 -0.00070 N4 3 0.827228 -0.162207 0.716061 11.00000 0.02789 0.02888 = 0.02262 0.00645 0.00399 0.00239 N5 3 0.731647 0.621083 0.493705 11.00000 0.07071 0.02356 = 0.04338 -0.00932 0.01800 -0.00930 C1 1 0.552512 -0.107858 0.259845 11.00000 0.05290 0.02019 = 0.03302 -0.00384 -0.00343 -0.00254 H1C 2 0.551839 -0.122996 0.202521 11.00000 0.05636 H1B 2 0.469304 -0.120947 0.255261 11.00000 0.05668 H1A 2 0.600369 -0.141696 0.308491 11.00000 0.06143 C2 1 0.579691 -0.011912 0.278799 11.00000 0.02660 0.01910 = 0.02409 -0.00145 0.00413 0.00023 C3 1 0.524506 0.053214 0.200710 11.00000 0.02359 0.02102 = 0.02131 -0.00247 0.00373 -0.00127 C4 1 0.456582 0.032505 0.105931 11.00000 0.02764 0.02512 = 0.02268 -0.00645 0.00228 -0.00390 H4 2 0.443240 -0.023505 0.088759 11.00000 0.02835 C5 1 0.409844 0.100064 0.041305 11.00000 0.02576 0.03678 = 0.01801 -0.00249 -0.00040 -0.00462 H5 2 0.367512 0.086035 -0.021954 11.00000 0.02982 C6 1 0.428305 0.186792 0.071644 11.00000 0.02571 0.02986 = 0.01869 0.00411 -0.00108 -0.00138 H6 2 0.396063 0.232863 0.028727 11.00000 0.02897 C7 1 0.495549 0.203763 0.168059 11.00000 0.02041 0.02394 = 0.02035 0.00157 0.00129 -0.00137 C8 1 0.520563 0.293902 0.210757 11.00000 0.02280 0.02134 = 0.02280 0.00416 0.00098 0.00115 C9 1 0.460019 0.369493 0.149028 11.00000 0.03784 0.02604 = 0.03513 0.00582 -0.00743 0.00148 H9C 2 0.467720 0.422564 0.196505 11.00000 0.04613 H9B 2 0.487587 0.373070 0.088798 11.00000 0.05950 H9A 2 0.378778 0.356006 0.121876 11.00000 0.04733 C10 1 0.694978 -0.030921 0.444055 11.00000 0.02786 0.01520 = 0.02298 -0.00017 0.00332 0.00046 C11 1 0.810905 -0.034026 0.488480 11.00000 0.02543 0.02160 = 0.02302 0.00098 0.00485 -0.00302 H11 2 0.858800 -0.003759 0.459227 11.00000 0.02324 C12 1 0.855975 -0.078362 0.577452 11.00000 0.02202 0.02166 = 0.02507 -0.00221 0.00114 0.00023 H12 2 0.936463 -0.083086 0.604548 11.00000 0.02013 C13 1 0.784391 -0.118111 0.626414 11.00000 0.02915 0.01683 = 0.02038 -0.00051 0.00378 0.00014 C14 1 0.667170 -0.113721 0.580094 11.00000 0.02534 0.02890 = 0.03124 0.00637 0.00986 -0.00073 H14 2 0.620392 -0.137392 0.607007 11.00000 0.03045 C15 1 0.623725 -0.071800 0.490368 11.00000 0.02326 0.02698 = 0.02991 0.00386 0.00305 0.00175 H15 2 0.546274 -0.069864 0.456989 11.00000 0.03590 C16 1 0.748416 -0.178986 0.773131 11.00000 0.03747 0.04173 = 0.02699 0.01011 0.00958 0.00387 H16C 2 0.787953 -0.200788 0.833957 11.00000 0.07711 H16B 2 0.688465 -0.221806 0.736362 11.00000 0.04924 H16A 2 0.707769 -0.121569 0.787125 11.00000 0.04515 C17 1 0.942565 -0.143199 0.775374 11.00000 0.02866 0.06066 = 0.02505 0.00930 0.00150 0.00456 H17C 2 0.999549 -0.156124 0.740565 11.00000 0.03902 H17B 2 0.959754 -0.180018 0.828504 11.00000 0.04263 H17A 2 0.953492 -0.076878 0.794588 11.00000 0.06962 C18 1 0.623160 0.381073 0.346269 11.00000 0.02210 0.01687 = 0.02476 0.00046 0.00161 0.00125 C19 1 0.672307 0.446573 0.302911 11.00000 0.02678 0.02338 = 0.02143 0.00029 0.00093 0.00035 H19 2 0.680063 0.435623 0.241181 11.00000 0.02509 C20 1 0.706211 0.525724 0.350813 11.00000 0.02753 0.02078 = 0.02898 0.00450 0.00203 -0.00106 H20 2 0.736008 0.566990 0.318825 11.00000 0.02073 C21 1 0.692578 0.542862 0.443795 11.00000 0.03111 0.01891 = 0.03064 -0.00192 0.00393 0.00259 C22 1 0.642632 0.476884 0.486620 11.00000 0.03357 0.02440 = 0.02840 -0.00168 0.00776 0.00212 H22 2 0.630547 0.484233 0.547697 11.00000 0.04165 C23 1 0.610419 0.396859 0.439005 11.00000 0.02774 0.02100 = 0.02886 0.00157 0.00616 -0.00088 H23 2 0.575335 0.354787 0.466095 11.00000 0.03759 C24 1 0.760479 0.695109 0.442195 11.00000 0.06470 0.02661 = 0.05889 -0.01030 0.01956 -0.01350 AFIX 137 H24A 2 0.829594 0.681696 0.424014 11.00000 -1.50000 H24B 2 0.773453 0.747137 0.485236 11.00000 -1.50000 H24C 2 0.698047 0.706961 0.382217 11.00000 -1.50000 AFIX 0 C25 1 0.717146 0.636070 0.590334 11.00000 0.06028 0.03769 = 0.04727 -0.01932 0.01510 -0.00993 H25C 2 0.639295 0.649666 0.581499 11.00000 0.08690 H25B 2 0.759240 0.691084 0.615321 11.00000 0.06179 H25A 2 0.743829 0.585941 0.638114 11.00000 0.05979 HKLF 4 REM solo2 in P2(1)/n REM R1 = 0.0375 for 4670 Fo > 4sig(Fo) and 0.0588 for all 6267 data REM 403 parameters refined using 0 restraints END ; _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^)+(0.0574P)^2^+0.9807P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6267 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.65622(2) 0.167206(19) 0.36232(2) 0.02052(10) Uani 1 1 d . . . Cl1 Cl 0.83575(5) 0.18677(4) 0.35297(4) 0.03184(15) Uani 1 1 d . . . Cl2 Cl 0.63336(5) 0.17722(4) 0.51464(4) 0.03035(14) Uani 1 1 d . . . N1 N 0.64800(15) 0.02160(12) 0.35774(13) 0.0217(4) Uani 1 1 d . . . N2 N 0.54314(15) 0.13788(12) 0.22929(13) 0.0211(4) Uani 1 1 d . . . N3 N 0.58900(16) 0.29782(12) 0.29919(13) 0.0221(4) Uani 1 1 d . . . N4 N 0.82723(17) -0.16221(12) 0.71606(14) 0.0272(4) Uani 1 1 d . . . N5 N 0.7316(2) 0.62108(14) 0.49371(18) 0.0456(6) Uani 1 1 d . . . C1 C 0.5525(3) -0.10786(17) 0.2598(2) 0.0388(7) Uani 1 1 d . . . H1C H 0.552(3) -0.123(2) 0.203(3) 0.056(10) Uiso 1 1 d . . . H1B H 0.469(3) -0.121(2) 0.255(2) 0.057(9) Uiso 1 1 d . . . H1A H 0.600(3) -0.142(2) 0.308(3) 0.061(10) Uiso 1 1 d . . . C2 C 0.57969(19) -0.01191(14) 0.27880(16) 0.0240(5) Uani 1 1 d . . . C3 C 0.52451(19) 0.05321(14) 0.20071(16) 0.0226(4) Uani 1 1 d . . . C4 C 0.4566(2) 0.03251(16) 0.10593(17) 0.0262(5) Uani 1 1 d . . . H4 H 0.443(2) -0.0235(17) 0.0888(18) 0.028(7) Uiso 1 1 d . . . C5 C 0.4098(2) 0.10006(16) 0.04130(18) 0.0283(5) Uani 1 1 d . . . H5 H 0.368(2) 0.0860(16) -0.0220(19) 0.030(7) Uiso 1 1 d . . . C6 C 0.4283(2) 0.18679(16) 0.07164(17) 0.0264(5) Uani 1 1 d . . . H6 H 0.396(2) 0.2329(17) 0.0287(19) 0.029(7) Uiso 1 1 d . . . C7 C 0.49555(18) 0.20376(15) 0.16806(16) 0.0226(4) Uani 1 1 d . . . C8 C 0.52056(19) 0.29390(14) 0.21076(16) 0.0235(5) Uani 1 1 d . . . C9 C 0.4600(3) 0.36949(17) 0.1490(2) 0.0369(6) Uani 1 1 d . . . H9C H 0.468(2) 0.423(2) 0.197(2) 0.046(8) Uiso 1 1 d . . . H9B H 0.488(3) 0.373(2) 0.089(2) 0.059(10) Uiso 1 1 d . . . H9A H 0.379(3) 0.356(2) 0.122(2) 0.047(8) Uiso 1 1 d . . . C10 C 0.69498(19) -0.03092(13) 0.44406(16) 0.0229(5) Uani 1 1 d . . . C11 C 0.8109(2) -0.03403(14) 0.48848(17) 0.0238(5) Uani 1 1 d . . . H11 H 0.859(2) -0.0038(16) 0.4592(17) 0.023(6) Uiso 1 1 d . . . C12 C 0.8560(2) -0.07836(15) 0.57745(17) 0.0241(5) Uani 1 1 d . . . H12 H 0.936(2) -0.0831(15) 0.6045(17) 0.020(6) Uiso 1 1 d . . . C13 C 0.7844(2) -0.11811(14) 0.62641(16) 0.0229(5) Uani 1 1 d . . . C14 C 0.6672(2) -0.11372(16) 0.58009(19) 0.0282(5) Uani 1 1 d . . . H14 H 0.620(2) -0.1374(17) 0.6070(19) 0.030(7) Uiso 1 1 d . . . C15 C 0.6237(2) -0.07180(16) 0.49037(18) 0.0277(5) Uani 1 1 d . . . H15 H 0.546(2) -0.0699(17) 0.457(2) 0.036(7) Uiso 1 1 d . . . C16 C 0.7484(3) -0.17899(19) 0.7731(2) 0.0354(6) Uani 1 1 d . . . H16C H 0.788(3) -0.201(3) 0.834(3) 0.077(12) Uiso 1 1 d . . . H16B H 0.688(3) -0.222(2) 0.736(2) 0.049(9) Uiso 1 1 d . . . H16A H 0.708(3) -0.122(2) 0.787(2) 0.045(8) Uiso 1 1 d . . . C17 C 0.9426(2) -0.1432(2) 0.7754(2) 0.0395(6) Uani 1 1 d . . . H17C H 1.000(3) -0.1561(17) 0.741(2) 0.039(8) Uiso 1 1 d . . . H17B H 0.960(3) -0.1800(19) 0.829(2) 0.043(8) Uiso 1 1 d . . . H17A H 0.953(3) -0.077(2) 0.795(2) 0.070(11) Uiso 1 1 d . . . C18 C 0.62316(19) 0.38107(14) 0.34627(16) 0.0224(5) Uani 1 1 d . . . C19 C 0.6723(2) 0.44657(15) 0.30291(17) 0.0252(5) Uani 1 1 d . . . H19 H 0.680(2) 0.4356(16) 0.2412(19) 0.025(6) Uiso 1 1 d . . . C20 C 0.7062(2) 0.52572(15) 0.35081(18) 0.0271(5) Uani 1 1 d . . . H20 H 0.736(2) 0.5670(15) 0.3188(17) 0.021(6) Uiso 1 1 d . . . C21 C 0.6926(2) 0.54286(14) 0.44379(18) 0.0280(5) Uani 1 1 d . . . C22 C 0.6426(2) 0.47688(15) 0.48662(19) 0.0291(5) Uani 1 1 d . . . H22 H 0.631(2) 0.4842(18) 0.548(2) 0.042(8) Uiso 1 1 d . . . C23 C 0.6104(2) 0.39686(15) 0.43900(18) 0.0263(5) Uani 1 1 d . . . H23 H 0.575(2) 0.3548(19) 0.466(2) 0.038(7) Uiso 1 1 d . . . C24 C 0.7605(3) 0.69511(18) 0.4422(2) 0.0498(8) Uani 1 1 d . . . H24A H 0.8296 0.6817 0.4240 0.075 Uiso 1 1 calc R . . H24B H 0.7735 0.7471 0.4852 0.075 Uiso 1 1 calc R . . H24C H 0.6980 0.7070 0.3822 0.075 Uiso 1 1 calc R . . C25 C 0.7171(3) 0.6361(2) 0.5903(3) 0.0486(8) Uani 1 1 d . . . H25C H 0.639(4) 0.650(3) 0.581(3) 0.087(14) Uiso 1 1 d . . . H25B H 0.759(3) 0.691(2) 0.615(3) 0.062(10) Uiso 1 1 d . . . H25A H 0.744(3) 0.586(2) 0.638(2) 0.060(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02137(17) 0.02042(16) 0.01598(16) -0.00094(11) -0.00046(12) -0.00159(12) Cl1 0.0254(3) 0.0393(3) 0.0304(3) -0.0081(2) 0.0074(2) -0.0051(2) Cl2 0.0414(3) 0.0279(3) 0.0224(3) -0.0031(2) 0.0103(2) -0.0047(2) N1 0.0237(9) 0.0192(9) 0.0187(9) 0.0015(7) 0.0007(8) 0.0008(7) N2 0.0213(9) 0.0205(9) 0.0182(9) 0.0005(7) 0.0005(7) -0.0006(7) N3 0.0239(9) 0.0192(8) 0.0212(9) -0.0006(7) 0.0032(8) -0.0007(8) N4 0.0279(10) 0.0289(10) 0.0226(10) 0.0064(8) 0.0040(8) 0.0024(8) N5 0.0707(18) 0.0236(11) 0.0434(14) -0.0093(10) 0.0180(13) -0.0093(11) C1 0.0529(19) 0.0202(12) 0.0330(15) -0.0038(11) -0.0034(14) -0.0025(12) C2 0.0266(12) 0.0191(10) 0.0241(11) -0.0014(9) 0.0041(9) 0.0002(9) C3 0.0236(11) 0.0210(10) 0.0213(11) -0.0025(9) 0.0037(9) -0.0013(9) C4 0.0276(12) 0.0251(12) 0.0227(11) -0.0065(9) 0.0023(9) -0.0039(10) C5 0.0258(12) 0.0368(13) 0.0180(11) -0.0025(10) -0.0004(9) -0.0046(10) C6 0.0257(12) 0.0299(12) 0.0187(11) 0.0041(9) -0.0011(9) -0.0014(10) C7 0.0204(11) 0.0239(10) 0.0203(11) 0.0016(9) 0.0013(9) -0.0014(9) C8 0.0228(11) 0.0213(10) 0.0228(11) 0.0042(9) 0.0010(9) 0.0012(9) C9 0.0378(16) 0.0260(13) 0.0351(15) 0.0058(11) -0.0074(12) 0.0015(12) C10 0.0279(12) 0.0152(9) 0.0230(11) -0.0002(8) 0.0033(9) 0.0005(9) C11 0.0254(12) 0.0216(10) 0.0230(11) 0.0010(9) 0.0048(9) -0.0030(9) C12 0.0220(11) 0.0217(11) 0.0251(12) -0.0022(9) 0.0011(9) 0.0002(9) C13 0.0292(12) 0.0168(10) 0.0204(11) -0.0005(8) 0.0038(9) 0.0001(9) C14 0.0253(12) 0.0289(12) 0.0312(13) 0.0064(10) 0.0099(10) -0.0007(10) C15 0.0233(12) 0.0270(12) 0.0299(13) 0.0039(10) 0.0031(10) 0.0018(10) C16 0.0375(15) 0.0417(15) 0.0270(13) 0.0101(12) 0.0096(12) 0.0039(13) C17 0.0287(14) 0.0607(19) 0.0250(13) 0.0093(13) 0.0015(11) 0.0046(14) C18 0.0221(11) 0.0169(10) 0.0248(11) 0.0005(8) 0.0016(9) 0.0012(8) C19 0.0268(12) 0.0234(11) 0.0214(11) 0.0003(9) 0.0009(9) 0.0004(9) C20 0.0275(12) 0.0208(11) 0.0290(12) 0.0045(9) 0.0020(10) -0.0011(10) C21 0.0311(13) 0.0189(10) 0.0306(13) -0.0019(9) 0.0039(10) 0.0026(10) C22 0.0336(13) 0.0244(11) 0.0284(13) -0.0017(10) 0.0078(11) 0.0021(10) C23 0.0277(12) 0.0210(11) 0.0289(12) 0.0016(9) 0.0062(10) -0.0009(9) C24 0.065(2) 0.0266(13) 0.059(2) -0.0103(13) 0.0196(17) -0.0135(14) C25 0.060(2) 0.0377(16) 0.0473(18) -0.0193(15) 0.0151(16) -0.0099(16) _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 N2 2.0344(18) . ? Co1 N1 2.2093(18) . ? Co1 N3 2.2289(18) . ? Co1 Cl2 2.2562(6) . ? Co1 Cl1 2.2733(6) . ? N1 C2 1.289(3) . ? N1 C10 1.429(3) . ? N2 C7 1.339(3) . ? N2 C3 1.345(3) . ? N3 C8 1.288(3) . ? N3 C18 1.431(3) . ? N4 C13 1.392(3) . ? N4 C17 1.452(3) . ? N4 C16 1.455(3) . ? N5 C21 1.391(3) . ? N5 C24 1.437(4) . ? N5 C25 1.446(4) . ? C1 C2 1.499(3) . ? C2 C3 1.488(3) . ? C3 C4 1.391(3) . ? C4 C5 1.381(3) . ? C5 C6 1.381(3) . ? C6 C7 1.396(3) . ? C7 C8 1.489(3) . ? C8 C9 1.500(3) . ? C10 C11 1.382(3) . ? C10 C15 1.385(3) . ? C11 C12 1.390(3) . ? C12 C13 1.406(3) . ? C13 C14 1.402(3) . ? C14 C15 1.379(3) . ? C18 C23 1.386(3) . ? C18 C19 1.395(3) . ? C19 C20 1.381(3) . ? C20 C21 1.397(3) . ? C21 C22 1.401(3) . ? C22 C23 1.387(3) . ? 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 N2 Co1 N1 75.03(7) . . ? N2 Co1 N3 75.55(7) . . ? N1 Co1 N3 150.11(7) . . ? N2 Co1 Cl2 130.79(5) . . ? N1 Co1 Cl2 94.46(5) . . ? N3 Co1 Cl2 100.75(5) . . ? N2 Co1 Cl1 112.91(5) . . ? N1 Co1 Cl1 99.53(5) . . ? N3 Co1 Cl1 96.58(5) . . ? Cl2 Co1 Cl1 116.23(3) . . ? C2 N1 C10 121.18(18) . . ? C2 N1 Co1 115.58(14) . . ? C10 N1 Co1 121.85(13) . . ? C7 N2 C3 120.91(19) . . ? C7 N2 Co1 119.08(15) . . ? C3 N2 Co1 119.77(15) . . ? C8 N3 C18 120.76(19) . . ? C8 N3 Co1 114.10(15) . . ? C18 N3 Co1 124.95(14) . . ? C13 N4 C17 118.4(2) . . ? C13 N4 C16 116.9(2) . . ? C17 N4 C16 114.5(2) . . ? C21 N5 C24 120.6(2) . . ? C21 N5 C25 119.5(2) . . ? C24 N5 C25 118.2(2) . . ? N1 C2 C3 114.91(19) . . ? N1 C2 C1 126.3(2) . . ? C3 C2 C1 118.8(2) . . ? N2 C3 C4 120.4(2) . . ? N2 C3 C2 114.17(19) . . ? C4 C3 C2 125.4(2) . . ? C5 C4 C3 119.1(2) . . ? C4 C5 C6 120.1(2) . . ? C5 C6 C7 118.4(2) . . ? N2 C7 C6 121.1(2) . . ? N2 C7 C8 115.02(19) . . ? C6 C7 C8 123.9(2) . . ? N3 C8 C7 115.75(19) . . ? N3 C8 C9 127.0(2) . . ? C7 C8 C9 117.2(2) . . ? C11 C10 C15 118.9(2) . . ? C11 C10 N1 120.8(2) . . ? C15 C10 N1 119.9(2) . . ? C10 C11 C12 120.9(2) . . ? C11 C12 C13 120.7(2) . . ? N4 C13 C14 120.8(2) . . ? N4 C13 C12 121.9(2) . . ? C14 C13 C12 117.3(2) . . ? C15 C14 C13 121.4(2) . . ? C14 C15 C10 120.8(2) . . ? C23 C18 C19 118.5(2) . . ? C23 C18 N3 119.51(19) . . ? C19 C18 N3 122.0(2) . . ? C20 C19 C18 120.7(2) . . ? C19 C20 C21 121.4(2) . . ? N5 C21 C20 121.1(2) . . ? N5 C21 C22 121.3(2) . . ? C20 C21 C22 117.6(2) . . ? C23 C22 C21 120.9(2) . . ? C18 C23 C22 120.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.252 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.069