# 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 _publ_contact_author ; Botoshansky Mark Schulich Faculty of Chemistry, Technion-Israel Institute of Technology, 32000 Haifa, Israel ; _publ_contact_author_letter ; Please exchange previously deposited CIF file - deposition number 877907- with that new one. A new refinement was done according the journal referees' reports With regards M.Botoshansky ; _publ_contact_author_name 'Botoshansky Mark' _publ_contact_author_email botoshan@techunix.technion.ac.il loop_ _publ_author_name A.Mahammed M.Botoshansky Z.Gross data_Gross-36SecondReviced _database_code_depnum_ccdc_archive 'CCDC 877907' #TrackingRef '- Gross-36SecondRevise.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Gross-36 (Atif)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H10 Cl8 Co F15 N6 O0.50' _chemical_formula_weight 1342.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _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 11.610(2) _cell_length_b 12.280(2) _cell_length_c 19.439(4) _cell_angle_alpha 88.83(2) _cell_angle_beta 82.82(2) _cell_angle_gamma 87.01(2) _cell_volume 2745.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23711 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 24.75 _exptl_crystal_description cubic _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_process_details 'PLATON (Spek, A.L. 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius KappaCCD' _diffrn_measurement_method '\p- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 23553 _diffrn_reflns_av_R_equivalents 0.0942 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 24.75 _reflns_number_total 9260 _reflns_number_gt 5204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2006)' _computing_cell_refinement 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.4' _computing_publication_material Word-2003 _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^)+(0.1636P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0122(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9260 _refine_ls_number_parameters 781 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.2261 _refine_ls_wR_factor_gt 0.1930 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _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 0.40335(6) 0.25158(6) 0.22818(3) 0.0568(3) Uani 1 1 d . A . Cl1 Cl 0.18395(15) 0.31176(15) -0.00973(7) 0.0872(5) Uani 1 1 d . . . Cl2 Cl 0.00015(14) 0.42967(16) 0.11336(8) 0.0933(5) Uani 1 1 d . . . Cl3 Cl 0.04900(17) 0.4586(2) 0.42237(9) 0.1232(8) Uani 1 1 d . . . Cl4 Cl 0.25249(16) 0.37750(18) 0.50910(8) 0.1048(6) Uani 1 1 d . . . Cl5 Cl 0.71539(16) 0.14684(17) 0.42856(8) 0.1020(6) Uani 1 1 d . . . Cl6 Cl 0.83481(15) 0.04143(16) 0.28771(9) 0.0984(6) Uani 1 1 d . . . Cl7 Cl 0.68784(14) 0.06099(13) -0.00511(7) 0.0816(5) Uani 1 1 d . . . Cl8 Cl 0.45060(14) 0.17894(13) -0.05620(7) 0.0806(4) Uani 1 1 d . . . F1 F 0.1308(4) 0.6161(3) 0.2501(2) 0.1115(13) Uani 1 1 d . . . F2 F -0.0637(6) 0.7403(4) 0.2798(3) 0.164(2) Uani 1 1 d . . . F3 F -0.2690(5) 0.6429(6) 0.3197(3) 0.187(3) Uani 1 1 d . . . F4 F -0.2746(4) 0.4265(6) 0.3242(3) 0.166(3) Uani 1 1 d . . . F5 F -0.0775(4) 0.3023(4) 0.2917(3) 0.1244(16) Uani 1 1 d . . . F6 F 0.3884(5) 0.0868(4) 0.4824(2) 0.1254(17) Uani 1 1 d . . . F7 F 0.4252(6) 0.0801(4) 0.6174(2) 0.164(2) Uani 1 1 d . . . F8 F 0.5351(5) 0.2416(4) 0.6691(2) 0.146(2) Uani 1 1 d . . . F9 F 0.6080(5) 0.4115(4) 0.5876(2) 0.1233(15) Uani 1 1 d . . . F10 F 0.5720(4) 0.4187(3) 0.45274(18) 0.1011(12) Uani 1 1 d . . . F11 F 0.6672(3) -0.1206(3) 0.18493(18) 0.0905(10) Uani 1 1 d . . . F12 F 0.8646(5) -0.2419(3) 0.1459(2) 0.1208(16) Uani 1 1 d . . . F13 F 1.0571(4) -0.1424(5) 0.0876(3) 0.157(2) Uani 1 1 d . . . F14 F 1.0532(4) 0.0749(5) 0.0697(3) 0.164(2) Uani 1 1 d . . . F15 F 0.8580(4) 0.1962(4) 0.1090(2) 0.1148(14) Uani 1 1 d . . . N21 N 0.2883(4) 0.3039(4) 0.1741(2) 0.0614(10) Uani 1 1 d . . . N22 N 0.3141(4) 0.3090(3) 0.30996(19) 0.0600(10) Uani 1 1 d . . . N23 N 0.5305(3) 0.1922(3) 0.27281(19) 0.0572(10) Uani 1 1 d . . . N24 N 0.4752(4) 0.2026(3) 0.1420(2) 0.0613(10) Uani 1 1 d . . . N1 N 0.4832(4) 0.3905(4) 0.2129(2) 0.0606(10) Uani 1 1 d . . . C1 C 0.3069(5) 0.2798(4) 0.1047(2) 0.0613(13) Uani 1 1 d . . . C2 C 0.2083(5) 0.3212(5) 0.0747(3) 0.0640(13) Uani 1 1 d . . . C3 C 0.1327(5) 0.3679(5) 0.1261(3) 0.0684(14) Uani 1 1 d . . . C4 C 0.1838(5) 0.3563(4) 0.1892(3) 0.0648(13) Uani 1 1 d . . . C5 C 0.1432(5) 0.3880(5) 0.2576(3) 0.0646(13) Uani 1 1 d . . . C6 C 0.2064(5) 0.3634(5) 0.3134(3) 0.0664(14) Uani 1 1 d . . . C7 C 0.1736(5) 0.3919(5) 0.3849(3) 0.0758(16) Uani 1 1 d . . . C8 C 0.2596(5) 0.3573(5) 0.4218(3) 0.0738(15) Uani 1 1 d . . . C9 C 0.3499(5) 0.3038(5) 0.3746(2) 0.0645(13) Uani 1 1 d . . . C10 C 0.4563(5) 0.2568(4) 0.3898(3) 0.0622(13) Uani 1 1 d . . . C11 C 0.5409(5) 0.2053(4) 0.3422(2) 0.0608(12) Uani 1 1 d . . . C12 C 0.6506(5) 0.1556(5) 0.3547(3) 0.0691(14) Uani 1 1 d . . . C13 C 0.7023(5) 0.1113(4) 0.2938(3) 0.0669(14) Uani 1 1 d . . . C14 C 0.6278(4) 0.1343(4) 0.2411(2) 0.0600(12) Uani 1 1 d . . . C15 C 0.6494(4) 0.1077(4) 0.1705(3) 0.0596(12) Uani 1 1 d . . . C16 C 0.5765(4) 0.1412(4) 0.1218(3) 0.0605(12) Uani 1 1 d . . . C17 C 0.5803(5) 0.1262(4) 0.0488(2) 0.0638(13) Uani 1 1 d . . . C18 C 0.4814(5) 0.1756(4) 0.0273(2) 0.0636(13) Uani 1 1 d . . . C19 C 0.4137(4) 0.2228(4) 0.0852(2) 0.0595(12) Uani 1 1 d . . . C20 C 0.0319(5) 0.4559(5) 0.2703(3) 0.0720(15) Uani 1 1 d . . . C21 C 0.0321(6) 0.5678(6) 0.2675(3) 0.0819(17) Uani 1 1 d . . . C22 C -0.0691(10) 0.6310(7) 0.2842(4) 0.116(3) Uani 1 1 d . . . C23 C -0.1732(8) 0.5778(12) 0.3030(4) 0.122(4) Uani 1 1 d . . . C24 C -0.1747(7) 0.4698(10) 0.3059(4) 0.111(3) Uani 1 1 d . . . C25 C -0.0728(6) 0.4102(7) 0.2885(3) 0.0875(18) Uani 1 1 d . . . C26 C 0.4770(5) 0.2533(4) 0.4639(2) 0.0652(13) Uani 1 1 d . . . C27 C 0.4409(6) 0.1685(5) 0.5071(3) 0.0848(18) Uani 1 1 d . . . C28 C 0.4608(8) 0.1637(6) 0.5760(3) 0.102(2) Uani 1 1 d . . . C29 C 0.5155(8) 0.2457(6) 0.6019(3) 0.099(2) Uani 1 1 d . . . C30 C 0.5532(6) 0.3303(6) 0.5608(3) 0.0876(19) Uani 1 1 d . . . C31 C 0.5334(5) 0.3333(5) 0.4924(3) 0.0765(16) Uani 1 1 d . . . C32 C 0.7563(5) 0.0411(4) 0.1467(3) 0.0658(13) Uani 1 1 d . . . C33 C 0.7614(6) -0.0708(5) 0.1547(3) 0.0742(15) Uani 1 1 d . . . C34 C 0.8621(7) -0.1334(6) 0.1361(3) 0.090(2) Uani 1 1 d . . . C35 C 0.9592(7) -0.0855(8) 0.1073(4) 0.105(2) Uani 1 1 d . . . C37 C 0.8568(5) 0.0889(5) 0.1170(3) 0.0807(16) Uani 1 1 d . . . C36 C 0.9568(6) 0.0266(8) 0.0979(4) 0.101(2) Uani 1 1 d . . . C38 C 0.5966(5) 0.3943(5) 0.1883(3) 0.0750(15) Uani 1 1 d . . . H38 H 0.6388 0.3286 0.1793 0.090 Uiso 1 1 calc R . . C39 C 0.6543(6) 0.4893(6) 0.1756(3) 0.0869(19) Uani 1 1 d . . . H39 H 0.7329 0.4873 0.1588 0.104 Uiso 1 1 calc R . . C40 C 0.5931(7) 0.5870(6) 0.1883(4) 0.092(2) Uani 1 1 d . . . H40 H 0.6294 0.6527 0.1806 0.110 Uiso 1 1 calc R . . C41 C 0.4795(7) 0.5853(5) 0.2122(3) 0.0856(18) Uani 1 1 d . . . H41 H 0.4362 0.6506 0.2207 0.103 Uiso 1 1 calc R . . C42 C 0.4268(6) 0.4880(5) 0.2240(3) 0.0751(15) Uani 1 1 d . . . H42 H 0.3480 0.4897 0.2406 0.090 Uiso 1 1 calc R . . N2 N 0.3237(4) 0.1105(4) 0.2417(2) 0.0656(11) Uani 1 1 d . . . C43 C 0.3124(15) 0.0646(13) 0.3095(7) 0.073(5) Uani 0.362(9) 1 d P A 1 H43 H 0.3375 0.1026 0.3453 0.088 Uiso 0.362(9) 1 calc PR A 1 C44 C 0.2643(19) -0.0367(16) 0.3238(9) 0.096(7) Uani 0.362(9) 1 d P A 1 H44 H 0.2569 -0.0652 0.3687 0.115 Uiso 0.362(9) 1 calc PR A 1 C45 C 0.230(3) -0.091(2) 0.2733(14) 0.097(8) Uani 0.362(9) 1 d P A 1 H45 H 0.1971 -0.1587 0.2825 0.116 Uiso 0.362(9) 1 calc PR A 1 C46 C 0.242(5) -0.046(2) 0.2028(14) 0.098(12) Uani 0.362(9) 1 d P A 1 H46 H 0.2181 -0.0817 0.1657 0.118 Uiso 0.362(9) 1 calc PR A 1 C47 C 0.2920(18) 0.0501(14) 0.1960(8) 0.074(6) Uani 0.362(9) 1 d P A 1 H47 H 0.3052 0.0770 0.1508 0.089 Uiso 0.362(9) 1 calc PR A 1 C43A C 0.2084(10) 0.1056(11) 0.2506(9) 0.125(6) Uani 0.638(9) 1 d P A 2 H43A H 0.1632 0.1697 0.2597 0.150 Uiso 0.638(9) 1 calc PR A 2 C44A C 0.1535(13) 0.0099(13) 0.2470(12) 0.150(7) Uani 0.638(9) 1 d P A 2 H44A H 0.0729 0.0097 0.2549 0.179 Uiso 0.638(9) 1 calc PR A 2 C45A C 0.217(2) -0.0839(18) 0.2319(16) 0.121(9) Uani 0.638(9) 1 d P A 2 H45A H 0.1808 -0.1495 0.2305 0.145 Uiso 0.638(9) 1 calc PR A 2 C46A C 0.3227(15) -0.0808(12) 0.2202(11) 0.117(5) Uani 0.638(9) 1 d P A 2 H46A H 0.3673 -0.1445 0.2091 0.140 Uiso 0.638(9) 1 calc PR A 2 C47A C 0.3771(12) 0.0175(11) 0.2233(7) 0.105(4) Uani 0.638(9) 1 d P A 2 H47A H 0.4572 0.0166 0.2115 0.126 Uiso 0.638(9) 1 calc PR A 2 C48 C 0.1981(16) 0.6478(11) 0.0595(12) 0.276(12) Uani 1 1 d . . . C49 C 0.3014(17) 0.6057(11) 0.0467(14) 0.271(12) Uani 1 1 d . . . C50 C 0.3884(14) 0.5575(12) 0.0156(11) 0.162(5) Uani 1 1 d . . . C51 C 0.496(4) 0.514(2) 0.0279(10) 0.246(12) Uani 1 1 d . . . O1 O 0.033(2) -0.208(2) 0.4429(13) 0.267(10) Uiso 0.50 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 0.0612(4) 0.0639(4) 0.0448(4) -0.0042(3) -0.0036(3) -0.0031(3) Cl1 0.0964(11) 0.1107(12) 0.0581(8) -0.0098(8) -0.0244(7) 0.0000(9) Cl2 0.0723(10) 0.1311(15) 0.0776(9) -0.0063(9) -0.0205(7) 0.0128(9) Cl3 0.1014(13) 0.196(2) 0.0638(9) -0.0273(11) -0.0001(8) 0.0592(14) Cl4 0.0988(12) 0.1617(18) 0.0500(8) -0.0218(9) -0.0020(7) 0.0219(12) Cl5 0.1029(12) 0.1364(15) 0.0692(9) -0.0210(9) -0.0334(9) 0.0327(11) Cl6 0.0864(11) 0.1261(14) 0.0833(10) -0.0282(10) -0.0251(8) 0.0337(10) Cl7 0.0883(10) 0.0921(10) 0.0594(8) -0.0155(7) 0.0100(7) 0.0029(8) Cl8 0.1028(11) 0.0928(10) 0.0463(7) -0.0071(7) -0.0082(7) -0.0061(9) F1 0.127(4) 0.086(3) 0.123(3) -0.007(2) -0.021(3) -0.006(2) F2 0.221(6) 0.125(4) 0.152(5) -0.046(3) -0.078(4) 0.077(4) F3 0.134(4) 0.313(8) 0.106(3) -0.068(4) -0.036(3) 0.129(5) F4 0.066(3) 0.303(8) 0.122(4) 0.024(4) 0.009(2) -0.002(4) F5 0.096(3) 0.140(4) 0.134(4) 0.024(3) 0.002(3) -0.028(3) F6 0.202(5) 0.104(3) 0.076(2) 0.002(2) -0.017(3) -0.067(3) F7 0.298(8) 0.125(4) 0.072(3) 0.031(3) -0.025(3) -0.061(4) F8 0.253(6) 0.134(4) 0.060(2) -0.014(2) -0.061(3) 0.021(4) F9 0.163(4) 0.123(3) 0.095(3) -0.025(3) -0.048(3) -0.020(3) F10 0.136(3) 0.097(3) 0.073(2) 0.000(2) -0.011(2) -0.034(2) F11 0.113(3) 0.080(2) 0.080(2) 0.0035(18) -0.017(2) -0.018(2) F12 0.187(4) 0.082(3) 0.098(3) -0.028(2) -0.052(3) 0.044(3) F13 0.114(4) 0.189(5) 0.155(5) -0.037(4) 0.001(3) 0.073(4) F14 0.080(3) 0.232(6) 0.167(5) 0.001(5) 0.036(3) -0.012(3) F15 0.101(3) 0.102(3) 0.138(4) 0.017(3) 0.005(2) -0.022(2) N21 0.065(3) 0.072(3) 0.046(2) -0.0101(19) -0.0050(18) -0.002(2) N22 0.064(3) 0.070(3) 0.044(2) -0.0033(19) -0.0030(18) 0.004(2) N23 0.059(2) 0.064(2) 0.048(2) -0.0064(19) -0.0043(18) -0.002(2) N24 0.065(3) 0.067(3) 0.052(2) -0.007(2) -0.0045(19) -0.005(2) N1 0.068(3) 0.068(3) 0.045(2) -0.0024(19) -0.0040(19) 0.000(2) C1 0.070(3) 0.068(3) 0.045(2) -0.003(2) -0.005(2) -0.009(3) C2 0.067(3) 0.076(3) 0.051(3) -0.002(3) -0.015(2) -0.007(3) C3 0.064(3) 0.080(4) 0.063(3) 0.000(3) -0.016(3) -0.005(3) C4 0.062(3) 0.074(3) 0.058(3) -0.004(3) -0.008(2) 0.004(3) C5 0.063(3) 0.075(3) 0.054(3) -0.002(3) -0.001(2) -0.001(3) C6 0.068(3) 0.081(4) 0.049(3) -0.009(3) -0.001(2) -0.001(3) C7 0.071(4) 0.103(4) 0.050(3) -0.005(3) -0.001(3) 0.009(3) C8 0.072(4) 0.096(4) 0.050(3) -0.009(3) 0.006(2) 0.002(3) C9 0.068(3) 0.076(3) 0.048(3) -0.005(2) -0.003(2) -0.003(3) C10 0.070(3) 0.067(3) 0.049(3) -0.004(2) -0.009(2) -0.002(3) C11 0.067(3) 0.068(3) 0.049(3) -0.002(2) -0.010(2) -0.004(3) C12 0.080(4) 0.076(4) 0.054(3) -0.008(3) -0.021(3) 0.004(3) C13 0.067(3) 0.068(3) 0.065(3) -0.008(3) -0.008(3) 0.006(3) C14 0.060(3) 0.068(3) 0.051(3) -0.004(2) -0.003(2) 0.000(2) C15 0.057(3) 0.063(3) 0.058(3) -0.008(2) -0.001(2) 0.001(2) C16 0.060(3) 0.065(3) 0.054(3) -0.007(2) 0.004(2) -0.006(2) C17 0.086(4) 0.058(3) 0.045(3) -0.006(2) 0.003(2) -0.006(3) C18 0.076(3) 0.069(3) 0.046(3) -0.003(2) -0.004(2) -0.010(3) C19 0.067(3) 0.067(3) 0.044(2) -0.003(2) -0.006(2) -0.008(3) C20 0.058(3) 0.098(4) 0.058(3) -0.006(3) -0.005(2) 0.012(3) C21 0.081(4) 0.089(5) 0.078(4) -0.012(3) -0.022(3) 0.013(4) C22 0.161(9) 0.108(6) 0.080(5) -0.032(4) -0.042(5) 0.056(6) C23 0.086(6) 0.201(11) 0.075(5) -0.030(6) -0.018(4) 0.063(7) C24 0.068(5) 0.187(9) 0.074(4) 0.000(6) -0.002(3) 0.018(6) C25 0.080(5) 0.108(5) 0.073(4) -0.002(4) -0.005(3) -0.004(4) C26 0.079(4) 0.070(3) 0.047(3) -0.009(2) -0.009(2) -0.001(3) C27 0.121(5) 0.079(4) 0.056(3) -0.005(3) -0.012(3) -0.012(4) C28 0.167(7) 0.084(4) 0.056(3) 0.011(3) -0.017(4) -0.011(5) C29 0.162(7) 0.092(5) 0.046(3) -0.007(3) -0.030(4) 0.008(5) C30 0.111(5) 0.089(4) 0.069(4) -0.024(3) -0.033(4) -0.004(4) C31 0.090(4) 0.078(4) 0.060(3) 0.003(3) -0.006(3) 0.001(3) C32 0.071(3) 0.069(3) 0.055(3) -0.012(2) 0.001(2) 0.002(3) C33 0.088(4) 0.077(4) 0.058(3) -0.011(3) -0.010(3) 0.002(3) C34 0.122(6) 0.086(5) 0.067(4) -0.022(3) -0.032(4) 0.026(4) C35 0.096(5) 0.127(7) 0.085(5) -0.029(5) -0.001(4) 0.040(5) C37 0.073(4) 0.082(4) 0.084(4) -0.009(3) 0.005(3) -0.005(3) C36 0.067(4) 0.143(7) 0.089(5) -0.014(5) 0.013(3) -0.003(4) C38 0.074(4) 0.083(4) 0.068(3) 0.002(3) -0.006(3) -0.011(3) C39 0.079(4) 0.098(5) 0.088(4) 0.015(4) -0.017(3) -0.029(4) C40 0.115(6) 0.070(4) 0.093(5) 0.007(4) -0.021(4) -0.016(4) C41 0.106(5) 0.063(4) 0.087(4) -0.003(3) -0.009(4) -0.007(3) C42 0.084(4) 0.072(4) 0.068(3) -0.011(3) -0.007(3) -0.003(3) N2 0.069(3) 0.065(3) 0.061(3) -0.002(2) -0.003(2) 0.001(2) C43 0.104(13) 0.072(10) 0.044(7) -0.012(7) 0.002(7) -0.030(9) C44 0.134(17) 0.090(12) 0.062(10) -0.004(9) 0.006(10) -0.042(12) C45 0.13(2) 0.078(14) 0.084(17) 0.015(14) -0.009(14) -0.053(15) C46 0.17(4) 0.08(2) 0.057(13) 0.004(12) -0.037(15) -0.02(2) C47 0.111(15) 0.072(11) 0.049(8) 0.004(8) -0.029(9) -0.041(11) C43A 0.061(7) 0.105(9) 0.205(16) 0.009(10) 0.003(8) -0.016(6) C44A 0.089(9) 0.103(11) 0.26(2) 0.040(13) -0.014(12) -0.028(9) C45A 0.125(17) 0.090(13) 0.16(3) 0.016(17) -0.064(19) -0.014(10) C46A 0.121(13) 0.076(8) 0.150(14) -0.012(9) 0.006(11) -0.018(9) C47A 0.098(9) 0.103(10) 0.107(9) -0.004(7) 0.016(7) -0.024(8) C48 0.208(15) 0.119(10) 0.46(3) 0.047(13) 0.104(18) 0.046(10) C49 0.178(16) 0.094(9) 0.52(4) 0.049(14) 0.031(19) -0.020(9) C50 0.182(16) 0.121(11) 0.182(13) -0.024(11) 0.006(14) -0.060(11) C51 0.45(3) 0.192(18) 0.134(11) 0.041(12) -0.133(18) -0.16(2) _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 N24 1.872(4) . ? Co1 N21 1.880(4) . ? Co1 N23 1.909(4) . ? Co1 N22 1.912(4) . ? Co1 N1 1.984(4) . ? Co1 N2 2.004(5) . ? Cl1 C2 1.708(5) . ? Cl2 C3 1.724(6) . ? Cl3 C7 1.712(6) . ? Cl4 C8 1.712(6) . ? Cl5 C12 1.701(5) . ? Cl6 C13 1.714(6) . ? Cl7 C17 1.703(5) . ? Cl8 C18 1.704(5) . ? F1 C21 1.321(8) . ? F2 C22 1.348(10) . ? F3 C23 1.345(9) . ? F4 C24 1.307(9) . ? F5 C25 1.329(8) . ? F6 C27 1.328(7) . ? F7 C28 1.342(7) . ? F8 C29 1.353(6) . ? F9 C30 1.358(7) . ? F10 C31 1.351(6) . ? F11 C33 1.345(7) . ? F12 C34 1.341(8) . ? F13 C35 1.321(8) . ? F14 C36 1.344(8) . ? F15 C37 1.324(7) . ? N21 C4 1.345(6) . ? N21 C1 1.375(6) . ? N22 C9 1.372(6) . ? N22 C6 1.380(7) . ? N23 C11 1.383(6) . ? N23 C14 1.386(6) . ? N24 C16 1.381(7) . ? N24 C19 1.399(6) . ? N1 C42 1.343(7) . ? N1 C38 1.346(7) . ? C1 C19 1.405(7) . ? C1 C2 1.415(7) . ? C2 C3 1.359(8) . ? C3 C4 1.431(7) . ? C4 C5 1.409(7) . ? C5 C6 1.403(7) . ? C5 C20 1.498(8) . ? C6 C7 1.440(7) . ? C7 C8 1.347(8) . ? C8 C9 1.443(8) . ? C9 C10 1.399(7) . ? C10 C11 1.398(7) . ? C10 C26 1.490(7) . ? C11 C12 1.430(7) . ? C12 C13 1.369(8) . ? C13 C14 1.436(7) . ? C14 C15 1.405(7) . ? C15 C16 1.389(7) . ? C15 C32 1.480(7) . ? C16 C17 1.430(7) . ? C17 C18 1.379(7) . ? C18 C19 1.407(7) . ? C20 C21 1.373(9) . ? C20 C25 1.369(9) . ? C21 C22 1.382(10) . ? C22 C23 1.408(13) . ? C23 C24 1.327(13) . ? C24 C25 1.368(11) . ? C26 C31 1.371(8) . ? C26 C27 1.373(7) . ? C27 C28 1.387(8) . ? C28 C29 1.355(10) . ? C29 C30 1.354(9) . ? C30 C31 1.376(8) . ? C32 C37 1.388(8) . ? C32 C33 1.379(8) . ? C33 C34 1.378(9) . ? C34 C35 1.352(11) . ? C35 C36 1.384(11) . ? C37 C36 1.373(9) . ? C38 C39 1.377(8) . ? C38 H38 0.9300 . ? C39 C40 1.373(10) . ? C39 H39 0.9300 . ? C40 C41 1.344(9) . ? C40 H40 0.9300 . ? C41 C42 1.373(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? N2 C47 1.269(15) . ? N2 C47A 1.304(14) . ? N2 C43A 1.332(12) . ? N2 C43 1.416(14) . ? C43 C44 1.40(2) . ? C43 H43 0.9300 . ? C44 C45 1.32(3) . ? C44 H44 0.9300 . ? C45 C46 1.46(3) . ? C45 H45 0.9300 . ? C46 C47 1.34(4) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C43A C44A 1.373(18) . ? C43A H43A 0.9300 . ? C44A C45A 1.35(3) . ? C44A H44A 0.9300 . ? C45A C46A 1.22(3) . ? C45A H45A 0.9300 . ? C46A C47A 1.397(17) . ? C46A H46A 0.9300 . ? C47A H47A 0.9300 . ? C48 C49 1.278(19) . ? C49 C50 1.24(2) . ? C50 C51 1.38(4) . ? C50 C51 1.71(5) 2_665 ? C51 C51 1.13(4) 2_665 ? C51 C50 1.71(5) 2_665 ? 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 N24 Co1 N21 81.98(18) . . ? N24 Co1 N23 91.07(18) . . ? N21 Co1 N23 173.06(18) . . ? N24 Co1 N22 172.62(18) . . ? N21 Co1 N22 90.63(18) . . ? N23 Co1 N22 96.31(17) . . ? N24 Co1 N1 89.83(18) . . ? N21 Co1 N1 90.46(18) . . ? N23 Co1 N1 89.34(17) . . ? N22 Co1 N1 90.24(18) . . ? N24 Co1 N2 89.06(18) . . ? N21 Co1 N2 89.18(19) . . ? N23 Co1 N2 90.89(18) . . ? N22 Co1 N2 90.84(19) . . ? N1 Co1 N2 178.87(18) . . ? C4 N21 C1 109.9(4) . . ? C4 N21 Co1 133.5(3) . . ? C1 N21 Co1 116.5(4) . . ? C9 N22 C6 109.6(4) . . ? C9 N22 Co1 124.3(3) . . ? C6 N22 Co1 126.1(3) . . ? C11 N23 C14 109.7(4) . . ? C11 N23 Co1 124.2(3) . . ? C14 N23 Co1 126.1(3) . . ? C16 N24 C19 110.1(4) . . ? C16 N24 Co1 133.0(3) . . ? C19 N24 Co1 116.7(3) . . ? C42 N1 C38 115.1(5) . . ? C42 N1 Co1 122.2(4) . . ? C38 N1 Co1 122.7(4) . . ? N21 C1 C19 113.2(4) . . ? N21 C1 C2 107.3(5) . . ? C19 C1 C2 139.4(5) . . ? C3 C2 C1 107.6(4) . . ? C3 C2 Cl1 125.2(4) . . ? C1 C2 Cl1 127.2(4) . . ? C2 C3 C4 107.9(5) . . ? C2 C3 Cl2 123.9(4) . . ? C4 C3 Cl2 128.2(5) . . ? N21 C4 C5 120.9(5) . . ? N21 C4 C3 107.3(5) . . ? C5 C4 C3 131.8(5) . . ? C6 C5 C4 122.4(5) . . ? C6 C5 C20 118.9(5) . . ? C4 C5 C20 118.6(5) . . ? C5 C6 N22 126.4(5) . . ? C5 C6 C7 127.0(5) . . ? N22 C6 C7 106.6(4) . . ? C8 C7 C6 108.8(5) . . ? C8 C7 Cl3 122.2(4) . . ? C6 C7 Cl3 129.0(4) . . ? C7 C8 C9 107.7(5) . . ? C7 C8 Cl4 122.5(5) . . ? C9 C8 Cl4 129.9(4) . . ? N22 C9 C10 124.9(5) . . ? N22 C9 C8 107.4(5) . . ? C10 C9 C8 127.7(5) . . ? C11 C10 C9 125.5(5) . . ? C11 C10 C26 117.1(5) . . ? C9 C10 C26 117.2(5) . . ? N23 C11 C10 124.5(4) . . ? N23 C11 C12 107.5(5) . . ? C10 C11 C12 128.0(5) . . ? C13 C12 C11 107.7(4) . . ? C13 C12 Cl5 122.0(4) . . ? C11 C12 Cl5 130.4(4) . . ? C12 C13 C14 108.7(5) . . ? C12 C13 Cl6 122.0(4) . . ? C14 C13 Cl6 129.3(4) . . ? N23 C14 C15 126.0(4) . . ? N23 C14 C13 106.5(4) . . ? C15 C14 C13 127.5(5) . . ? C16 C15 C14 123.6(5) . . ? C16 C15 C32 118.2(5) . . ? C14 C15 C32 118.1(5) . . ? C15 C16 N24 120.1(5) . . ? C15 C16 C17 133.8(5) . . ? N24 C16 C17 106.1(4) . . ? C18 C17 C16 108.6(5) . . ? C18 C17 Cl7 124.0(4) . . ? C16 C17 Cl7 127.4(4) . . ? C17 C18 C19 108.4(4) . . ? C17 C18 Cl8 124.6(4) . . ? C19 C18 Cl8 127.0(4) . . ? N24 C19 C1 111.5(4) . . ? N24 C19 C18 106.8(4) . . ? C1 C19 C18 141.7(5) . . ? C21 C20 C25 117.3(6) . . ? C21 C20 C5 120.7(6) . . ? C25 C20 C5 121.9(6) . . ? F1 C21 C20 119.8(6) . . ? F1 C21 C22 119.2(8) . . ? C20 C21 C22 121.0(8) . . ? F2 C22 C21 118.3(10) . . ? F2 C22 C23 123.3(9) . . ? C21 C22 C23 118.3(8) . . ? F3 C23 C24 122.6(11) . . ? F3 C23 C22 116.0(12) . . ? C24 C23 C22 121.3(8) . . ? F4 C24 C23 117.8(9) . . ? F4 C24 C25 123.7(10) . . ? C23 C24 C25 118.5(8) . . ? F5 C25 C20 119.5(6) . . ? F5 C25 C24 117.0(8) . . ? C20 C25 C24 123.5(8) . . ? C31 C26 C27 116.7(5) . . ? C31 C26 C10 122.1(5) . . ? C27 C26 C10 121.1(5) . . ? F6 C27 C26 119.8(5) . . ? F6 C27 C28 118.5(6) . . ? C26 C27 C28 121.7(6) . . ? C29 C28 F7 119.8(6) . . ? C29 C28 C27 119.3(6) . . ? F7 C28 C27 120.9(7) . . ? C28 C29 C30 120.7(5) . . ? C28 C29 F8 119.6(6) . . ? C30 C29 F8 119.7(7) . . ? F9 C30 C29 119.9(6) . . ? F9 C30 C31 120.9(6) . . ? C29 C30 C31 119.2(6) . . ? F10 C31 C30 117.8(6) . . ? F10 C31 C26 119.8(5) . . ? C30 C31 C26 122.4(5) . . ? C37 C32 C33 117.1(5) . . ? C37 C32 C15 121.4(5) . . ? C33 C32 C15 121.4(5) . . ? F11 C33 C34 118.5(6) . . ? F11 C33 C32 119.3(5) . . ? C34 C33 C32 122.1(6) . . ? F12 C34 C33 120.6(8) . . ? F12 C34 C35 119.5(7) . . ? C33 C34 C35 119.9(7) . . ? F13 C35 C36 118.5(9) . . ? F13 C35 C34 122.0(9) . . ? C36 C35 C34 119.5(7) . . ? F15 C37 C36 119.2(6) . . ? F15 C37 C32 120.0(6) . . ? C36 C37 C32 120.8(6) . . ? F14 C36 C35 119.8(7) . . ? F14 C36 C37 119.6(8) . . ? C35 C36 C37 120.5(7) . . ? N1 C38 C39 124.2(6) . . ? N1 C38 H38 117.9 . . ? C39 C38 H38 117.9 . . ? C40 C39 C38 118.6(7) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? C41 C40 C39 118.3(6) . . ? C41 C40 H40 120.9 . . ? C39 C40 H40 120.9 . . ? C40 C41 C42 120.5(7) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? N1 C42 C41 123.3(6) . . ? N1 C42 H42 118.4 . . ? C41 C42 H42 118.4 . . ? C47 N2 C47A 56.8(10) . . ? C47 N2 C43A 70.2(12) . . ? C47A N2 C43A 112.9(10) . . ? C47 N2 C43 114.5(10) . . ? C47A N2 C43 85.0(9) . . ? C43A N2 C43 82.3(10) . . ? C47 N2 Co1 128.4(7) . . ? C47A N2 Co1 121.8(6) . . ? C43A N2 Co1 122.6(7) . . ? C43 N2 Co1 116.7(7) . . ? C44 C43 N2 121.4(14) . . ? C44 C43 H43 119.3 . . ? N2 C43 H43 119.3 . . ? C45 C44 C43 119.6(17) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 120(2) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 114(2) . . ? C45 C46 H46 122.8 . . ? C47 C46 H46 122.8 . . ? N2 C47 C46 130.0(16) . . ? N2 C47 H47 115.0 . . ? C46 C47 H47 115.0 . . ? N2 C43A C44A 122.7(13) . . ? N2 C43A H43A 118.7 . . ? C44A C43A H43A 118.7 . . ? C43A C44A C45A 119.9(16) . . ? C43A C44A H44A 120.0 . . ? C45A C44A H44A 120.0 . . ? C46A C45A C44A 119(2) . . ? C46A C45A H45A 120.7 . . ? C44A C45A H45A 120.7 . . ? C45A C46A C47A 120.7(17) . . ? C45A C46A H46A 119.7 . . ? C47A C46A H46A 119.7 . . ? N2 C47A C46A 124.8(12) . . ? N2 C47A H47A 117.6 . . ? C46A C47A H47A 117.6 . . ? C50 C49 C48 160(3) . . ? C49 C50 C51 140(3) . . ? C49 C50 C51 177.3(16) . 2_665 ? C51 C50 C51 41.5(12) . 2_665 ? C51 C51 C50 85(3) 2_665 . ? C51 C51 C50 53(4) 2_665 2_665 ? C50 C51 C50 138.5(12) . 2_665 ? loop_ # start Validation Reply Form _vrf_PLAT366_I ; PROBLEM: Short? C(sp?)-C(sp?) Bond C51 - C51_a ...1.14 Ang. RESPONSE: Disordered n-heptane molecule ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.75 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.686 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.095