# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Kilner, Colin' 'Halcrow, Malcolm A.' _publ_contact_author_name M.A.Halcrow _publ_contact_author_email M.A.Halcrow@leeds.ac.uk _publ_section_title ; An Unusual Discontinuity in the Thermal Spin Transition in [Co(terpy)2][BF4]2 ; # Attachment '- Co Dalton revised.cif' #================================================================= data_mh325ht _database_code_depnum_ccdc_archive 'CCDC 781735' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.6393(13) _cell_length_b 12.5032(13) _cell_length_c 19.570(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.254(5) _cell_angle_gamma 90.00 _cell_volume 3074.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 375(2) _cell_measurement_reflns_used 26955 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.67 _exptl_crystal_description fragment _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 1.106 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 375(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26955 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.67 _reflns_number_total 7522 _reflns_number_gt 6131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over three equally occupied sites labelled 'A', 'B' and 'C', sharing a common wholly occupied B atom B38. Anion B43--F47 was refined over three equally occupied orientations 'A', 'B' and 'C', with orientations A and B sharing the same B atom B43A which therefore has occupancy 0.67. The refined restraints B---F = 1.38(2) and F...F = 2.25(2)\%A were applied to these groups. All non-H atoms with occupancy >0.5 were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0897P)^2^+0.1364P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.255(14) _refine_ls_number_reflns 7522 _refine_ls_number_parameters 454 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _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 0.25063(2) 0.27214(3) 0.25004(2) 0.05325(12) Uani 1 1 d . . . N2 N 0.2592(3) 0.2665(2) 0.3549(2) 0.0608(9) Uani 1 1 d . . . C3 C 0.3498(3) 0.2984(3) 0.39304(19) 0.0664(8) Uani 1 1 d . . . C4 C 0.3579(5) 0.2956(5) 0.4644(3) 0.0934(13) Uani 1 1 d . . . H4 H 0.4202 0.3160 0.4909 0.112 Uiso 1 1 calc R . . C5 C 0.2710(6) 0.2616(5) 0.4942(3) 0.1002(18) Uani 1 1 d . . . H5 H 0.2743 0.2609 0.5419 0.120 Uiso 1 1 calc R . . C6 C 0.1792(5) 0.2285(5) 0.4563(3) 0.0974(16) Uani 1 1 d . . . H6 H 0.1212 0.2046 0.4775 0.117 Uiso 1 1 calc R . . C7 C 0.1761(3) 0.2320(3) 0.3849(2) 0.0676(8) Uani 1 1 d . . . C8 C 0.4357(3) 0.3342(3) 0.35163(19) 0.0634(8) Uani 1 1 d . . . N9 N 0.4079(2) 0.3334(2) 0.28242(15) 0.0595(6) Uani 1 1 d . . . C10 C 0.4799(3) 0.3657(3) 0.2408(2) 0.0690(8) Uani 1 1 d . . . H10 H 0.4615 0.3650 0.1934 0.083 Uiso 1 1 calc R . . C11 C 0.5804(3) 0.3996(4) 0.2666(3) 0.0826(12) Uani 1 1 d . . . H11 H 0.6287 0.4226 0.2371 0.099 Uiso 1 1 calc R . . C12 C 0.6082(3) 0.3990(4) 0.3364(3) 0.0915(14) Uani 1 1 d . . . H12 H 0.6758 0.4209 0.3545 0.110 Uiso 1 1 calc R . . C13 C 0.5353(3) 0.3657(4) 0.3797(2) 0.0850(12) Uani 1 1 d . . . H13 H 0.5533 0.3646 0.4270 0.102 Uiso 1 1 calc R . . C14 C 0.0833(3) 0.1996(3) 0.3352(2) 0.0698(9) Uani 1 1 d . . . N15 N 0.0994(2) 0.2061(2) 0.26898(18) 0.0652(7) Uani 1 1 d . . . C16 C 0.0210(3) 0.1751(3) 0.2204(3) 0.0812(11) Uani 1 1 d . . . H16 H 0.0326 0.1780 0.1743 0.097 Uiso 1 1 calc R . . C17 C -0.0762(4) 0.1393(4) 0.2379(4) 0.1001(17) Uani 1 1 d . . . H17 H -0.1294 0.1174 0.2043 0.120 Uiso 1 1 calc R . . C18 C -0.0926(4) 0.1369(5) 0.3074(4) 0.107(2) Uani 1 1 d . . . H18 H -0.1582 0.1156 0.3202 0.128 Uiso 1 1 calc R . . C19 C -0.0127(4) 0.1656(4) 0.3564(3) 0.0948(14) Uani 1 1 d . . . H19 H -0.0221 0.1626 0.4028 0.114 Uiso 1 1 calc R . . N20 N 0.2429(3) 0.2823(2) 0.1461(2) 0.0608(9) Uani 1 1 d . . . C21 C 0.2760(3) 0.1994(3) 0.1097(2) 0.0638(8) Uani 1 1 d . . . C22 C 0.2753(5) 0.2055(4) 0.0384(3) 0.0857(12) Uani 1 1 d . . . H22 H 0.2980 0.1478 0.0138 0.103 Uiso 1 1 calc R . . C23 C 0.2411(5) 0.2969(5) 0.0054(3) 0.0968(16) Uani 1 1 d . . . H23 H 0.2399 0.3019 -0.0421 0.116 Uiso 1 1 calc R . . C24 C 0.2077(4) 0.3832(4) 0.0428(2) 0.0843(11) Uani 1 1 d . . . H24 H 0.1846 0.4464 0.0209 0.101 Uiso 1 1 calc R . . C25 C 0.2099(3) 0.3727(3) 0.11283(18) 0.0646(8) Uani 1 1 d . . . C26 C 0.3109(3) 0.1043(3) 0.15315(19) 0.0639(8) Uani 1 1 d . . . N27 N 0.3084(2) 0.1189(2) 0.22083(15) 0.0604(6) Uani 1 1 d . . . C28 C 0.3402(3) 0.0386(3) 0.2631(2) 0.0739(9) Uani 1 1 d . . . H28 H 0.3401 0.0490 0.3101 0.089 Uiso 1 1 calc R . . C29 C 0.3732(4) -0.0591(4) 0.2403(3) 0.0899(13) Uani 1 1 d . . . H29 H 0.3944 -0.1137 0.2711 0.108 Uiso 1 1 calc R . . C30 C 0.3738(4) -0.0733(4) 0.1698(3) 0.0980(16) Uani 1 1 d . . . H30 H 0.3953 -0.1381 0.1525 0.118 Uiso 1 1 calc R . . C31 C 0.3424(3) 0.0090(4) 0.1260(3) 0.0850(11) Uani 1 1 d . . . H31 H 0.3424 0.0008 0.0788 0.102 Uiso 1 1 calc R . . C32 C 0.1751(3) 0.4563(3) 0.16025(19) 0.0631(7) Uani 1 1 d . . . N33 N 0.1822(2) 0.4279(2) 0.22752(15) 0.0614(6) Uani 1 1 d . . . C34 C 0.1476(3) 0.4987(3) 0.2721(2) 0.0736(9) Uani 1 1 d . . . H34 H 0.1488 0.4787 0.3180 0.088 Uiso 1 1 calc R . . C35 C 0.1107(3) 0.5990(3) 0.2531(3) 0.0849(12) Uani 1 1 d . . . H35 H 0.0885 0.6461 0.2855 0.102 Uiso 1 1 calc R . . C36 C 0.1074(4) 0.6277(4) 0.1860(3) 0.0960(16) Uani 1 1 d . . . H36 H 0.0841 0.6956 0.1721 0.115 Uiso 1 1 calc R . . C37 C 0.1387(3) 0.5561(3) 0.1387(3) 0.0799(10) Uani 1 1 d . . . H37 H 0.1353 0.5749 0.0926 0.096 Uiso 1 1 calc R . . B38 B 0.0122(6) -0.0250(6) 0.0618(3) 0.115(2) Uani 1 1 d D . . F39A F -0.0190(10) -0.0556(10) -0.0016(5) 0.101(3) Uiso 0.34 1 d PD A 1 F40A F 0.0859(10) -0.0876(11) 0.1014(6) 0.118(4) Uiso 0.34 1 d PD A 1 F41A F -0.0766(7) -0.0101(9) 0.0990(5) 0.091(3) Uiso 0.34 1 d PD A 1 F42A F 0.0549(8) 0.0821(8) 0.0625(5) 0.102(3) Uiso 0.34 1 d PD A 1 F39B F -0.0517(10) -0.0340(10) -0.0046(5) 0.110(4) Uiso 0.33 1 d PD A 2 F40B F 0.0535(11) -0.1240(9) 0.0862(6) 0.104(3) Uiso 0.33 1 d PD A 2 F41B F -0.0458(16) 0.014(2) 0.1094(10) 0.235(14) Uiso 0.33 1 d PD A 2 F42B F 0.0885(9) 0.0454(10) 0.0519(7) 0.123(4) Uiso 0.33 1 d PD A 2 F39C F 0.0711(13) 0.0029(15) 0.0150(8) 0.186(7) Uiso 0.33 1 d PD A 3 F40C F 0.0001(14) -0.1355(10) 0.0685(8) 0.159(5) Uiso 0.33 1 d PD A 3 F41C F -0.0706(9) 0.0279(11) 0.0885(7) 0.111(4) Uiso 0.33 1 d PD A 3 F42C F 0.0922(14) -0.0069(19) 0.1237(9) 0.244(10) Uiso 0.33 1 d PD A 3 B43A B -0.0319(8) 0.5085(10) -0.0607(5) 0.099(3) Uani 0.67 1 d PD . . F44A F -0.0066(8) 0.5372(10) 0.0034(4) 0.098(3) Uiso 0.34 1 d PD B 1 F45A F 0.0144(10) 0.4291(10) -0.0915(6) 0.108(3) Uiso 0.34 1 d PD B 1 F46A F -0.1449(6) 0.4934(9) -0.0676(5) 0.095(2) Uiso 0.34 1 d PD B 1 F47A F -0.0174(14) 0.5968(12) -0.1073(8) 0.180(6) Uiso 0.34 1 d PD B 1 F44B F -0.0257(9) 0.4567(9) 0.0061(5) 0.120(3) Uiso 0.33 1 d PD B 2 F45B F 0.0604(10) 0.5631(12) -0.0628(8) 0.158(5) Uiso 0.33 1 d PD B 2 F46B F -0.1304(8) 0.5456(11) -0.0836(6) 0.107(3) Uiso 0.33 1 d PD B 2 F47B F -0.0187(13) 0.4142(11) -0.0996(7) 0.145(6) Uiso 0.33 1 d PD B 2 B43C B -0.0405(14) 0.5387(14) -0.0589(10) 0.085(7) Uiso 0.33 1 d PD B 3 F44C F 0.0358(11) 0.4961(13) -0.0970(7) 0.147(4) Uiso 0.33 1 d PD B 3 F45C F 0.0088(8) 0.5979(10) -0.0079(5) 0.113(3) Uiso 0.33 1 d PD B 3 F46C F -0.1063(10) 0.6052(11) -0.0991(6) 0.125(3) Uiso 0.33 1 d PD B 3 F47C F -0.1029(19) 0.4558(16) -0.0387(13) 0.258(12) Uiso 0.33 1 d PD B 3 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 0.04755(17) 0.05143(18) 0.0608(2) -0.0016(2) 0.00597(13) -0.0002(2) N2 0.0610(19) 0.0568(17) 0.064(2) -0.0019(13) 0.0050(17) 0.0027(12) C3 0.0687(19) 0.0657(18) 0.0643(19) -0.0045(15) 0.0047(15) 0.0064(15) C4 0.098(3) 0.113(4) 0.068(2) -0.005(2) 0.000(2) 0.001(3) C5 0.119(5) 0.118(4) 0.066(3) 0.008(2) 0.020(3) 0.013(3) C6 0.097(4) 0.120(4) 0.080(3) 0.020(3) 0.034(3) 0.014(3) C7 0.067(2) 0.0651(19) 0.074(2) 0.0005(16) 0.0226(17) 0.0064(15) C8 0.0621(17) 0.0572(16) 0.0691(19) -0.0080(14) -0.0009(14) 0.0012(13) N9 0.0534(13) 0.0528(13) 0.0716(16) -0.0001(12) 0.0039(11) -0.0016(10) C10 0.0603(17) 0.0609(17) 0.086(2) 0.0015(17) 0.0086(16) -0.0006(14) C11 0.0549(18) 0.077(3) 0.118(4) 0.003(2) 0.0153(19) -0.0070(16) C12 0.0582(19) 0.092(3) 0.121(4) -0.017(3) -0.006(2) -0.011(2) C13 0.068(2) 0.093(3) 0.089(3) -0.007(2) -0.016(2) -0.0009(19) C14 0.0625(18) 0.0531(15) 0.098(3) 0.0010(17) 0.0258(18) -0.0004(14) N15 0.0553(14) 0.0522(13) 0.088(2) -0.0061(13) 0.0096(14) -0.0004(11) C16 0.0641(19) 0.064(2) 0.112(3) -0.015(2) -0.003(2) -0.0029(16) C17 0.062(2) 0.080(3) 0.156(5) -0.023(3) 0.002(3) -0.008(2) C18 0.060(2) 0.092(3) 0.173(6) 0.003(4) 0.033(3) -0.013(2) C19 0.076(3) 0.082(3) 0.133(4) 0.010(3) 0.041(3) -0.008(2) N20 0.0490(16) 0.0607(19) 0.073(3) -0.0042(14) 0.0083(17) -0.0027(11) C21 0.0559(17) 0.0653(18) 0.070(2) -0.0089(16) 0.0085(15) -0.0036(15) C22 0.095(3) 0.089(3) 0.074(3) -0.015(2) 0.013(2) 0.000(2) C23 0.119(4) 0.107(4) 0.064(3) 0.007(3) 0.010(3) -0.008(3) C24 0.093(3) 0.087(3) 0.070(2) 0.011(2) -0.001(2) 0.001(2) C25 0.0549(15) 0.0668(18) 0.070(2) 0.0043(15) -0.0015(14) -0.0028(14) C26 0.0556(15) 0.0629(18) 0.073(2) -0.0097(15) 0.0080(14) 0.0031(13) N27 0.0507(12) 0.0542(14) 0.0758(17) -0.0038(12) 0.0041(11) -0.0004(10) C28 0.0676(19) 0.065(2) 0.087(2) 0.0060(17) -0.0002(17) 0.0038(15) C29 0.080(2) 0.066(2) 0.122(4) 0.009(2) 0.004(2) 0.0088(19) C30 0.095(3) 0.066(2) 0.130(4) -0.022(3) 0.002(3) 0.018(2) C31 0.084(2) 0.075(2) 0.097(3) -0.021(2) 0.014(2) 0.008(2) C32 0.0537(15) 0.0600(17) 0.075(2) 0.0073(15) 0.0029(14) -0.0027(13) N33 0.0523(12) 0.0555(14) 0.0768(18) -0.0006(13) 0.0092(11) -0.0001(11) C34 0.0679(18) 0.067(2) 0.088(2) -0.0111(18) 0.0184(17) 0.0000(16) C35 0.073(2) 0.067(2) 0.115(4) -0.012(2) 0.013(2) 0.0085(19) C36 0.092(3) 0.058(2) 0.135(5) 0.008(3) -0.003(3) 0.018(2) C37 0.075(2) 0.063(2) 0.099(3) 0.013(2) -0.004(2) 0.0067(16) B38 0.134(6) 0.126(6) 0.091(4) 0.010(4) 0.038(4) -0.012(5) B43A 0.097(7) 0.118(9) 0.080(6) -0.024(6) 0.006(4) 0.006(6) _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 N20 2.030(4) . ? Co1 N2 2.045(4) . ? Co1 N27 2.149(3) . ? Co1 N15 2.151(3) . ? Co1 N33 2.156(3) . ? Co1 N9 2.160(3) . ? N2 C7 1.329(6) . ? N2 C3 1.357(6) . ? C3 C4 1.390(6) . ? C3 C8 1.492(6) . ? C4 C5 1.366(9) . ? C5 C6 1.371(10) . ? C6 C7 1.396(7) . ? C7 C14 1.495(6) . ? C8 N9 1.362(5) . ? C8 C13 1.375(5) . ? N9 C10 1.348(5) . ? C10 C11 1.382(5) . ? C11 C12 1.373(7) . ? C12 C13 1.382(7) . ? C14 N15 1.337(5) . ? C14 C19 1.390(6) . ? N15 C16 1.353(5) . ? C16 C17 1.386(7) . ? C17 C18 1.398(9) . ? C18 C19 1.363(8) . ? N20 C25 1.347(5) . ? N20 C21 1.350(5) . ? C21 C22 1.395(7) . ? C21 C26 1.500(5) . ? C22 C23 1.360(8) . ? C23 C24 1.395(8) . ? C24 C25 1.373(6) . ? C25 C32 1.495(5) . ? C26 N27 1.341(5) . ? C26 C31 1.382(5) . ? N27 C28 1.334(5) . ? C28 C29 1.381(7) . ? C29 C30 1.392(8) . ? C30 C31 1.370(8) . ? C32 N33 1.357(5) . ? C32 C37 1.380(5) . ? N33 C34 1.350(5) . ? C34 C35 1.375(6) . ? C35 C36 1.357(8) . ? C36 C37 1.376(7) . ? B38 F39A 1.317(11) . ? B38 F40A 1.386(11) . ? B38 F41A 1.415(10) . ? B38 F42A 1.443(11) . ? B38 F42B 1.334(11) . ? B38 F41B 1.339(14) . ? B38 F40B 1.407(11) . ? B38 F39B 1.458(11) . ? B38 F39C 1.290(13) . ? B38 F41C 1.387(11) . ? B38 F40C 1.398(13) . ? B38 F42C 1.508(14) . ? B43A F44A 1.310(11) . ? B43A F45A 1.330(13) . ? B43A F46A 1.432(11) . ? B43A F47A 1.456(14) . ? B43A F45B 1.357(13) . ? B43A F46B 1.358(12) . ? B43A F47B 1.423(14) . ? B43A F44B 1.453(12) . ? B43C F45C 1.341(16) . ? B43C F46C 1.363(17) . ? B43C F47C 1.387(17) . ? B43C F44C 1.387(17) . ? 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 N20 Co1 N2 178.36(12) . . ? N20 Co1 N27 76.70(12) . . ? N2 Co1 N27 104.70(12) . . ? N20 Co1 N15 104.49(14) . . ? N2 Co1 N15 76.39(15) . . ? N27 Co1 N15 92.16(10) . . ? N20 Co1 N33 76.35(12) . . ? N2 Co1 N33 102.28(12) . . ? N27 Co1 N33 152.94(12) . . ? N15 Co1 N33 92.18(11) . . ? N20 Co1 N9 102.35(13) . . ? N2 Co1 N9 76.78(14) . . ? N27 Co1 N9 93.78(10) . . ? N15 Co1 N9 153.16(13) . . ? N33 Co1 N9 94.30(10) . . ? C7 N2 C3 120.9(4) . . ? C7 N2 Co1 119.7(3) . . ? C3 N2 Co1 119.4(3) . . ? N2 C3 C4 120.7(4) . . ? N2 C3 C8 114.2(3) . . ? C4 C3 C8 125.1(4) . . ? C5 C4 C3 117.5(5) . . ? C4 C5 C6 122.4(6) . . ? C5 C6 C7 117.5(5) . . ? N2 C7 C6 120.9(5) . . ? N2 C7 C14 113.8(4) . . ? C6 C7 C14 125.3(4) . . ? N9 C8 C13 121.7(4) . . ? N9 C8 C3 114.5(3) . . ? C13 C8 C3 123.9(3) . . ? C10 N9 C8 118.8(3) . . ? C10 N9 Co1 126.1(2) . . ? C8 N9 Co1 115.1(2) . . ? N9 C10 C11 121.7(4) . . ? C12 C11 C10 119.2(4) . . ? C11 C12 C13 119.7(4) . . ? C8 C13 C12 119.0(4) . . ? N15 C14 C19 122.5(4) . . ? N15 C14 C7 115.0(3) . . ? C19 C14 C7 122.5(4) . . ? C14 N15 C16 119.2(4) . . ? C14 N15 Co1 115.0(2) . . ? C16 N15 Co1 125.8(3) . . ? N15 C16 C17 121.3(5) . . ? C16 C17 C18 118.5(5) . . ? C19 C18 C17 120.1(5) . . ? C18 C19 C14 118.4(5) . . ? C25 N20 C21 119.1(4) . . ? C25 N20 Co1 121.0(3) . . ? C21 N20 Co1 119.8(3) . . ? N20 C21 C22 121.2(4) . . ? N20 C21 C26 113.4(4) . . ? C22 C21 C26 125.4(4) . . ? C23 C22 C21 119.2(5) . . ? C22 C23 C24 120.0(5) . . ? C25 C24 C23 118.4(4) . . ? N20 C25 C24 122.3(4) . . ? N20 C25 C32 112.5(3) . . ? C24 C25 C32 125.2(4) . . ? N27 C26 C31 122.4(4) . . ? N27 C26 C21 114.5(3) . . ? C31 C26 C21 123.0(4) . . ? C28 N27 C26 118.1(3) . . ? C28 N27 Co1 126.4(3) . . ? C26 N27 Co1 115.4(2) . . ? N27 C28 C29 123.2(4) . . ? C28 C29 C30 117.8(4) . . ? C31 C30 C29 119.5(4) . . ? C30 C31 C26 118.9(4) . . ? N33 C32 C37 121.2(4) . . ? N33 C32 C25 115.2(3) . . ? C37 C32 C25 123.6(3) . . ? C34 N33 C32 117.6(3) . . ? C34 N33 Co1 127.7(3) . . ? C32 N33 Co1 114.7(2) . . ? N33 C34 C35 123.2(4) . . ? C36 C35 C34 118.5(4) . . ? C35 C36 C37 119.8(4) . . ? C36 C37 C32 119.6(4) . . ? F39A B38 F40A 118.4(9) . . ? F39A B38 F41A 110.5(8) . . ? F40A B38 F41A 108.0(8) . . ? F39A B38 F42A 110.6(8) . . ? F40A B38 F42A 106.9(9) . . ? F41A B38 F42A 101.0(8) . . ? F42B B38 F41B 108.6(13) . . ? F42B B38 F40B 112.5(9) . . ? F41B B38 F40B 107.3(12) . . ? F42B B38 F39B 105.0(8) . . ? F41B B38 F39B 110.9(11) . . ? F40B B38 F39B 112.5(9) . . ? F39C B38 F41C 131.0(11) . . ? F39C B38 F40C 114.2(11) . . ? F41C B38 F40C 109.9(9) . . ? F39C B38 F42C 98.2(11) . . ? F41C B38 F42C 95.4(10) . . ? F40C B38 F42C 98.3(10) . . ? F44A B43A F45A 124.4(10) . . ? F44A B43A F46A 105.3(8) . . ? F45A B43A F46A 110.0(10) . . ? F44A B43A F47A 110.9(11) . . ? F45A B43A F47A 100.9(10) . . ? F46A B43A F47A 103.5(10) . . ? F45B B43A F46B 125.4(12) . . ? F45B B43A F47B 104.5(10) . . ? F46B B43A F47B 105.2(9) . . ? F45B B43A F44B 106.8(9) . . ? F46B B43A F44B 114.0(9) . . ? F47B B43A F44B 96.5(10) . . ? F45C B43C F46C 107.3(13) . . ? F45C B43C F47C 115.6(16) . . ? F46C B43C F47C 106.9(15) . . ? F45C B43C F44C 108.6(14) . . ? F46C B43C F44C 109.9(14) . . ? F47C B43C F44C 108.5(15) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.67 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.381 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.048 #=END data_mh325350 _database_code_depnum_ccdc_archive 'CCDC 781736' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.6512(10) _cell_length_b 12.5056(10) _cell_length_c 19.5416(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.416(4) _cell_angle_gamma 90.00 _cell_volume 3072.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 350(2) _cell_measurement_reflns_used 27070 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.56 _exptl_crystal_description fragment _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 1.068 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 350(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27070 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.56 _reflns_number_total 7529 _reflns_number_gt 6492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over three equally occupied sites labelled 'A', 'B' and 'C', sharing a common wholly occupied B atom B38. Anion B43--F47 was refined over three equally occupied orientations 'A', 'B' and 'C', with orientations A and B sharing the same B atom B43A which therefore has occupancy 0.67. The refined restraints B---F = 1.38(2) and F...F = 2.25(2)\%A were applied to these groups. All non-H atoms with occupancy >0.5 were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0809P)^2^+0.2923P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.230(12) _refine_ls_number_reflns 7529 _refine_ls_number_parameters 454 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.069 _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 0.25061(2) 0.27287(2) 0.250040(17) 0.04642(10) Uani 1 1 d . . . N2 N 0.2599(3) 0.2668(2) 0.35487(19) 0.0529(8) Uani 1 1 d . . . C3 C 0.3503(3) 0.2986(3) 0.39300(17) 0.0604(7) Uani 1 1 d . . . C4 C 0.3584(4) 0.2959(4) 0.4643(2) 0.0837(11) Uani 1 1 d . . . H4 H 0.4206 0.3166 0.4909 0.100 Uiso 1 1 calc R . . C5 C 0.2714(5) 0.2615(5) 0.4943(3) 0.0908(15) Uani 1 1 d . . . H5 H 0.2748 0.2611 0.5421 0.109 Uiso 1 1 calc R . . C6 C 0.1797(4) 0.2279(4) 0.4564(3) 0.0857(13) Uani 1 1 d . . . H6 H 0.1220 0.2033 0.4776 0.103 Uiso 1 1 calc R . . C7 C 0.1762(3) 0.2319(2) 0.38493(19) 0.0596(7) Uani 1 1 d . . . C8 C 0.4356(2) 0.3345(2) 0.35172(16) 0.0552(6) Uani 1 1 d . . . N9 N 0.40792(18) 0.33432(18) 0.28228(13) 0.0518(5) Uani 1 1 d . . . C10 C 0.4794(2) 0.3666(3) 0.24075(19) 0.0613(7) Uani 1 1 d . . . H10 H 0.4607 0.3663 0.1934 0.074 Uiso 1 1 calc R . . C11 C 0.5806(3) 0.4005(3) 0.2666(2) 0.0740(10) Uani 1 1 d . . . H11 H 0.6287 0.4232 0.2369 0.089 Uiso 1 1 calc R . . C12 C 0.6089(3) 0.4000(4) 0.3366(3) 0.0821(12) Uani 1 1 d . . . H12 H 0.6766 0.4220 0.3547 0.099 Uiso 1 1 calc R . . C13 C 0.5359(3) 0.3667(3) 0.3798(2) 0.0762(10) Uani 1 1 d . . . H13 H 0.5540 0.3659 0.4272 0.091 Uiso 1 1 calc R . . C14 C 0.0833(3) 0.2002(3) 0.3348(2) 0.0619(8) Uani 1 1 d . . . N15 N 0.0990(2) 0.2065(2) 0.26857(16) 0.0590(6) Uani 1 1 d . . . C16 C 0.0204(3) 0.1755(3) 0.2200(2) 0.0736(9) Uani 1 1 d . . . H16 H 0.0320 0.1780 0.1738 0.088 Uiso 1 1 calc R . . C17 C -0.0770(3) 0.1400(4) 0.2373(3) 0.0924(15) Uani 1 1 d . . . H17 H -0.1303 0.1186 0.2034 0.111 Uiso 1 1 calc R . . C18 C -0.0934(3) 0.1371(4) 0.3066(4) 0.0992(17) Uani 1 1 d . . . H18 H -0.1589 0.1156 0.3193 0.119 Uiso 1 1 calc R . . C19 C -0.0126(3) 0.1661(3) 0.3562(3) 0.0864(12) Uani 1 1 d . . . H19 H -0.0217 0.1630 0.4027 0.104 Uiso 1 1 calc R . . N20 N 0.2435(3) 0.2835(2) 0.14583(19) 0.0529(8) Uani 1 1 d . . . C21 C 0.2761(3) 0.2002(3) 0.10941(18) 0.0573(7) Uani 1 1 d . . . C22 C 0.2760(4) 0.2062(4) 0.0381(2) 0.0769(11) Uani 1 1 d . . . H22 H 0.2990 0.1486 0.0135 0.092 Uiso 1 1 calc R . . C23 C 0.2417(5) 0.2979(5) 0.0049(3) 0.0878(13) Uani 1 1 d . . . H23 H 0.2408 0.3031 -0.0426 0.105 Uiso 1 1 calc R . . C24 C 0.2077(3) 0.3845(3) 0.04271(19) 0.0759(10) Uani 1 1 d . . . H24 H 0.1842 0.4475 0.0208 0.091 Uiso 1 1 calc R . . C25 C 0.2100(2) 0.3738(3) 0.11296(16) 0.0561(6) Uani 1 1 d . . . C26 C 0.3108(2) 0.1052(3) 0.15312(17) 0.0570(7) Uani 1 1 d . . . N27 N 0.30851(18) 0.11970(19) 0.22089(14) 0.0543(5) Uani 1 1 d . . . C28 C 0.3399(3) 0.0387(3) 0.2633(2) 0.0664(8) Uani 1 1 d . . . H28 H 0.3393 0.0488 0.3104 0.080 Uiso 1 1 calc R . . C29 C 0.3733(3) -0.0589(3) 0.2405(3) 0.0792(11) Uani 1 1 d . . . H29 H 0.3949 -0.1133 0.2713 0.095 Uiso 1 1 calc R . . C30 C 0.3736(4) -0.0730(3) 0.1703(3) 0.0898(14) Uani 1 1 d . . . H30 H 0.3949 -0.1379 0.1531 0.108 Uiso 1 1 calc R . . C31 C 0.3424(3) 0.0094(3) 0.1260(2) 0.0759(9) Uani 1 1 d . . . H31 H 0.3424 0.0010 0.0787 0.091 Uiso 1 1 calc R . . C32 C 0.1750(2) 0.4578(2) 0.16017(17) 0.0562(6) Uani 1 1 d . . . N33 N 0.18225(19) 0.42854(19) 0.22775(14) 0.0542(5) Uani 1 1 d . . . C34 C 0.1475(3) 0.4995(3) 0.2725(2) 0.0661(8) Uani 1 1 d . . . H34 H 0.1489 0.4794 0.3185 0.079 Uiso 1 1 calc R . . C35 C 0.1102(3) 0.5997(3) 0.2536(3) 0.0791(11) Uani 1 1 d . . . H35 H 0.0879 0.6464 0.2861 0.095 Uiso 1 1 calc R . . C36 C 0.1066(4) 0.6293(3) 0.1864(3) 0.0847(13) Uani 1 1 d . . . H36 H 0.0827 0.6970 0.1725 0.102 Uiso 1 1 calc R . . C37 C 0.1387(3) 0.5575(3) 0.1388(2) 0.0732(9) Uani 1 1 d . . . H37 H 0.1357 0.5765 0.0927 0.088 Uiso 1 1 calc R . . B38 B 0.0126(5) -0.0254(5) 0.0615(3) 0.1031(19) Uani 1 1 d D . . F39A F -0.0189(8) -0.0580(8) -0.0013(4) 0.085(3) Uiso 0.34 1 d PD A 1 F40A F 0.0858(9) -0.0872(10) 0.1022(6) 0.110(3) Uiso 0.34 1 d PD A 1 F41A F -0.0768(7) -0.0106(9) 0.0985(5) 0.084(3) Uiso 0.34 1 d PD A 1 F42A F 0.0570(7) 0.0819(7) 0.0625(4) 0.090(2) Uiso 0.34 1 d PD A 1 F39B F -0.0512(8) -0.0332(8) -0.0065(4) 0.092(3) Uiso 0.33 1 d PD A 2 F40B F 0.0565(9) -0.1226(8) 0.0872(5) 0.088(2) Uiso 0.33 1 d PD A 2 F41B F -0.0467(14) 0.0164(18) 0.1069(9) 0.205(11) Uiso 0.33 1 d PD A 2 F42B F 0.0888(8) 0.0456(9) 0.0517(6) 0.108(3) Uiso 0.33 1 d PD A 2 F39C F 0.0689(13) 0.0029(15) 0.0147(8) 0.190(7) Uiso 0.33 1 d PD A 3 F40C F 0.0039(12) -0.1361(9) 0.0707(7) 0.142(4) Uiso 0.33 1 d PD A 3 F41C F -0.0726(8) 0.0254(10) 0.0902(6) 0.094(3) Uiso 0.33 1 d PD A 3 F42C F 0.0923(14) -0.0020(19) 0.1228(9) 0.256(10) Uiso 0.33 1 d PD A 3 B43A B -0.0326(7) 0.5093(10) -0.0603(4) 0.090(3) Uani 0.67 1 d PD . . F44A F -0.0069(7) 0.5363(8) 0.0040(4) 0.089(2) Uiso 0.34 1 d PD B 1 F45A F 0.0161(10) 0.4308(10) -0.0916(6) 0.103(3) Uiso 0.34 1 d PD B 1 F46A F -0.1448(6) 0.4931(8) -0.0667(4) 0.0846(18) Uiso 0.34 1 d PD B 1 F47A F -0.0173(13) 0.5966(11) -0.1075(7) 0.168(5) Uiso 0.34 1 d PD B 1 F44B F -0.0258(8) 0.4531(8) 0.0064(4) 0.106(2) Uiso 0.33 1 d PD B 2 F45B F 0.0590(9) 0.5655(11) -0.0597(7) 0.150(4) Uiso 0.33 1 d PD B 2 F46B F -0.1320(7) 0.5450(10) -0.0825(5) 0.097(2) Uiso 0.33 1 d PD B 2 F47B F -0.0158(11) 0.4153(9) -0.0997(6) 0.119(4) Uiso 0.33 1 d PD B 2 B43C B -0.0402(15) 0.5382(15) -0.0587(10) 0.092(8) Uiso 0.33 1 d PD B 3 F44C F 0.0367(10) 0.4987(12) -0.0967(7) 0.136(4) Uiso 0.33 1 d PD B 3 F45C F 0.0083(8) 0.5971(9) -0.0073(5) 0.107(3) Uiso 0.33 1 d PD B 3 F46C F -0.1082(8) 0.6033(10) -0.0986(5) 0.112(3) Uiso 0.33 1 d PD B 3 F47C F -0.1024(18) 0.4540(15) -0.0397(12) 0.247(11) Uiso 0.33 1 d PD B 3 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 0.04253(15) 0.04626(16) 0.05055(17) -0.00149(19) 0.00559(11) -0.00005(17) N2 0.0531(16) 0.0501(15) 0.055(2) -0.0005(11) 0.0063(15) 0.0029(10) C3 0.0625(17) 0.0589(16) 0.0588(17) -0.0051(13) 0.0024(13) 0.0053(13) C4 0.089(3) 0.101(3) 0.059(2) -0.0027(19) -0.0004(18) 0.002(2) C5 0.106(4) 0.111(4) 0.058(3) 0.009(2) 0.020(3) 0.011(3) C6 0.089(3) 0.103(3) 0.071(3) 0.019(2) 0.033(2) 0.010(2) C7 0.0624(18) 0.0558(16) 0.0634(18) 0.0026(13) 0.0190(15) 0.0052(13) C8 0.0528(14) 0.0518(14) 0.0600(16) -0.0070(12) 0.0015(12) 0.0003(11) N9 0.0469(11) 0.0493(12) 0.0589(13) 0.0000(10) 0.0047(9) -0.0008(9) C10 0.0535(15) 0.0561(15) 0.075(2) 0.0030(14) 0.0095(14) -0.0010(12) C11 0.0493(16) 0.068(2) 0.106(3) 0.0021(19) 0.0147(17) -0.0082(14) C12 0.0517(17) 0.082(3) 0.110(3) -0.013(2) -0.0043(18) -0.0090(17) C13 0.0631(19) 0.084(2) 0.077(2) -0.0095(18) -0.0130(17) -0.0023(17) C14 0.0562(16) 0.0482(14) 0.085(2) 0.0017(14) 0.0235(15) 0.0009(12) N15 0.0489(12) 0.0474(12) 0.0812(18) -0.0064(11) 0.0094(12) -0.0004(9) C16 0.0589(17) 0.0585(18) 0.101(3) -0.0132(18) -0.0006(17) -0.0040(14) C17 0.0551(19) 0.072(2) 0.147(5) -0.024(3) -0.001(2) -0.0059(17) C18 0.055(2) 0.085(3) 0.161(6) 0.007(3) 0.029(3) -0.013(2) C19 0.070(2) 0.077(2) 0.118(3) 0.010(2) 0.038(2) -0.0085(18) N20 0.0461(15) 0.0559(16) 0.057(2) -0.0040(11) 0.0074(14) -0.0031(10) C21 0.0529(15) 0.0584(15) 0.0609(17) -0.0089(14) 0.0085(13) -0.0037(13) C22 0.082(3) 0.083(2) 0.067(2) -0.0147(19) 0.009(2) 0.002(2) C23 0.108(4) 0.101(3) 0.054(2) 0.009(2) 0.009(2) -0.008(3) C24 0.084(2) 0.077(2) 0.065(2) 0.0107(17) -0.0003(18) -0.0020(18) C25 0.0490(13) 0.0578(15) 0.0599(16) 0.0014(13) -0.0007(12) -0.0038(12) C26 0.0469(13) 0.0563(15) 0.0676(18) -0.0101(13) 0.0055(12) 0.0027(11) N27 0.0451(11) 0.0507(12) 0.0668(15) -0.0028(11) 0.0046(10) 0.0002(9) C28 0.0587(16) 0.0625(18) 0.077(2) 0.0056(15) 0.0022(15) 0.0029(14) C29 0.071(2) 0.0560(18) 0.109(3) 0.008(2) 0.003(2) 0.0085(16) C30 0.091(3) 0.058(2) 0.117(4) -0.020(2) 0.000(3) 0.017(2) C31 0.079(2) 0.068(2) 0.082(2) -0.0195(18) 0.0147(18) 0.0069(17) C32 0.0490(13) 0.0521(14) 0.0663(17) 0.0049(13) 0.0013(12) -0.0013(11) N33 0.0468(11) 0.0497(12) 0.0670(15) -0.0010(11) 0.0097(10) -0.0006(10) C34 0.0594(16) 0.0617(17) 0.079(2) -0.0091(16) 0.0176(15) -0.0003(14) C35 0.068(2) 0.062(2) 0.107(3) -0.013(2) 0.011(2) 0.0056(17) C36 0.083(3) 0.0522(19) 0.117(4) 0.008(2) -0.001(2) 0.0165(18) C37 0.069(2) 0.0557(17) 0.091(2) 0.0126(17) -0.0070(18) 0.0065(14) B38 0.126(5) 0.108(4) 0.081(3) 0.005(3) 0.036(3) -0.013(4) B43A 0.079(5) 0.130(9) 0.060(4) -0.023(5) 0.008(3) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N20 2.033(4) . ? Co1 N2 2.040(4) . ? Co1 N27 2.150(2) . ? Co1 N33 2.155(2) . ? Co1 N15 2.158(3) . ? Co1 N9 2.161(2) . ? N2 C7 1.340(5) . ? N2 C3 1.354(5) . ? C3 C4 1.386(6) . ? C3 C8 1.486(5) . ? C4 C5 1.373(8) . ? C5 C6 1.372(9) . ? C6 C7 1.393(6) . ? C7 C14 1.497(5) . ? C8 N9 1.363(4) . ? C8 C13 1.386(5) . ? N9 C10 1.343(4) . ? C10 C11 1.389(5) . ? C11 C12 1.374(7) . ? C12 C13 1.383(6) . ? C14 N15 1.333(5) . ? C14 C19 1.394(5) . ? N15 C16 1.352(5) . ? C16 C17 1.388(6) . ? C17 C18 1.392(8) . ? C18 C19 1.377(7) . ? N20 C25 1.344(4) . ? N20 C21 1.353(5) . ? C21 C22 1.396(6) . ? C21 C26 1.500(5) . ? C22 C23 1.364(7) . ? C23 C24 1.404(7) . ? C24 C25 1.376(5) . ? C25 C32 1.498(5) . ? C26 N27 1.340(4) . ? C26 C31 1.387(5) . ? N27 C28 1.340(4) . ? C28 C29 1.382(6) . ? C29 C30 1.384(7) . ? C30 C31 1.375(7) . ? C32 N33 1.364(4) . ? C32 C37 1.376(4) . ? N33 C34 1.354(4) . ? C34 C35 1.376(6) . ? C35 C36 1.359(7) . ? C36 C37 1.386(6) . ? B38 F39A 1.312(9) . ? B38 F40A 1.387(10) . ? B38 F41A 1.421(9) . ? B38 F42A 1.454(10) . ? B38 F41B 1.331(13) . ? B38 F42B 1.341(10) . ? B38 F40B 1.406(10) . ? B38 F39B 1.478(10) . ? B38 F39C 1.271(12) . ? B38 F40C 1.401(12) . ? B38 F41C 1.420(10) . ? B38 F42C 1.507(14) . ? B43A F44A 1.305(10) . ? B43A F45A 1.342(13) . ? B43A F46A 1.425(10) . ? B43A F47A 1.457(13) . ? B43A F45B 1.354(12) . ? B43A F46B 1.360(11) . ? B43A F47B 1.434(13) . ? B43A F44B 1.474(12) . ? B43C F45C 1.338(17) . ? B43C F46C 1.365(17) . ? B43C F44C 1.379(17) . ? B43C F47C 1.389(17) . ? 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 N20 Co1 N2 178.21(12) . . ? N20 Co1 N27 76.78(11) . . ? N2 Co1 N27 104.48(10) . . ? N20 Co1 N33 76.49(11) . . ? N2 Co1 N33 102.30(10) . . ? N27 Co1 N33 153.15(10) . . ? N20 Co1 N15 104.62(12) . . ? N2 Co1 N15 76.68(13) . . ? N27 Co1 N15 92.13(9) . . ? N33 Co1 N15 92.14(10) . . ? N20 Co1 N9 101.85(11) . . ? N2 Co1 N9 76.86(12) . . ? N27 Co1 N9 93.68(9) . . ? N33 Co1 N9 94.21(9) . . ? N15 Co1 N9 153.53(11) . . ? C7 N2 C3 121.0(4) . . ? C7 N2 Co1 119.5(3) . . ? C3 N2 Co1 119.5(3) . . ? N2 C3 C4 120.6(4) . . ? N2 C3 C8 114.2(3) . . ? C4 C3 C8 125.2(3) . . ? C5 C4 C3 117.7(5) . . ? C6 C5 C4 122.3(5) . . ? C5 C6 C7 117.5(4) . . ? N2 C7 C6 120.9(4) . . ? N2 C7 C14 113.6(3) . . ? C6 C7 C14 125.6(4) . . ? N9 C8 C13 121.1(3) . . ? N9 C8 C3 114.8(2) . . ? C13 C8 C3 124.1(3) . . ? C10 N9 C8 119.1(3) . . ? C10 N9 Co1 126.3(2) . . ? C8 N9 Co1 114.59(19) . . ? N9 C10 C11 121.8(3) . . ? C12 C11 C10 119.2(4) . . ? C11 C12 C13 119.4(3) . . ? C12 C13 C8 119.4(4) . . ? N15 C14 C19 122.6(4) . . ? N15 C14 C7 115.4(3) . . ? C19 C14 C7 122.0(4) . . ? C14 N15 C16 119.2(3) . . ? C14 N15 Co1 114.6(2) . . ? C16 N15 Co1 126.1(3) . . ? N15 C16 C17 121.5(4) . . ? C16 C17 C18 118.6(4) . . ? C19 C18 C17 119.8(4) . . ? C18 C19 C14 118.2(5) . . ? C25 N20 C21 119.6(4) . . ? C25 N20 Co1 120.7(2) . . ? C21 N20 Co1 119.7(3) . . ? N20 C21 C22 121.2(4) . . ? N20 C21 C26 113.4(3) . . ? C22 C21 C26 125.4(3) . . ? C23 C22 C21 119.0(4) . . ? C22 C23 C24 119.9(4) . . ? C25 C24 C23 118.4(4) . . ? N20 C25 C24 121.9(3) . . ? N20 C25 C32 113.2(3) . . ? C24 C25 C32 124.9(3) . . ? N27 C26 C31 122.3(3) . . ? N27 C26 C21 114.7(3) . . ? C31 C26 C21 123.0(3) . . ? C26 N27 C28 118.1(3) . . ? C26 N27 Co1 115.4(2) . . ? C28 N27 Co1 126.5(2) . . ? N27 C28 C29 123.2(4) . . ? C28 C29 C30 117.9(4) . . ? C31 C30 C29 119.8(4) . . ? C30 C31 C26 118.7(4) . . ? N33 C32 C37 121.4(3) . . ? N33 C32 C25 114.5(2) . . ? C37 C32 C25 124.1(3) . . ? C34 N33 C32 117.3(3) . . ? C34 N33 Co1 127.8(2) . . ? C32 N33 Co1 114.9(2) . . ? N33 C34 C35 123.3(4) . . ? C36 C35 C34 118.8(4) . . ? C35 C36 C37 119.4(4) . . ? C32 C37 C36 119.7(4) . . ? F39A B38 F40A 118.4(8) . . ? F39A B38 F41A 110.0(7) . . ? F40A B38 F41A 107.4(7) . . ? F39A B38 F42A 112.1(7) . . ? F40A B38 F42A 105.9(8) . . ? F41A B38 F42A 101.6(7) . . ? F41B B38 F42B 107.6(12) . . ? F41B B38 F40B 109.4(11) . . ? F42B B38 F40B 111.2(8) . . ? F41B B38 F39B 109.4(10) . . ? F42B B38 F39B 104.1(7) . . ? F40B B38 F39B 114.7(7) . . ? F39C B38 F40C 115.2(11) . . ? F39C B38 F41C 132.1(10) . . ? F40C B38 F41C 108.6(8) . . ? F39C B38 F42C 97.9(11) . . ? F40C B38 F42C 98.3(10) . . ? F41C B38 F42C 93.9(9) . . ? F44A B43A F45A 123.4(10) . . ? F44A B43A F46A 105.1(7) . . ? F45A B43A F46A 111.1(9) . . ? F44A B43A F47A 112.3(11) . . ? F45A B43A F47A 99.1(9) . . ? F46A B43A F47A 104.6(9) . . ? F45B B43A F46B 126.3(12) . . ? F45B B43A F47B 104.6(10) . . ? F46B B43A F47B 106.5(8) . . ? F45B B43A F44B 106.0(8) . . ? F46B B43A F44B 113.6(8) . . ? F47B B43A F44B 95.0(9) . . ? F45C B43C F46C 108.0(14) . . ? F45C B43C F44C 108.0(14) . . ? F46C B43C F44C 110.1(15) . . ? F45C B43C F47C 116.3(17) . . ? F46C B43C F47C 105.4(15) . . ? F44C B43C F47C 109.1(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.412 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.047 #=END data_mh325325 _database_code_depnum_ccdc_archive 'CCDC 781737' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.6234(12) _cell_length_b 12.4686(12) _cell_length_c 19.5075(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.558(5) _cell_angle_gamma 90.00 _cell_volume 3050.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 325(2) _cell_measurement_reflns_used 26460 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.39 _exptl_crystal_description fragment _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 1.198 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 325(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26460 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.39 _reflns_number_total 7333 _reflns_number_gt 6522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over two equally occupied sites labelled 'A' and 'B', sharing a common wholly occupied B atom B38. Anion B43--F47 was refined over three equally occupied orientations 'A', 'B' and 'C', with orientations A and B sharing the same B atom B43A which therefore has occupancy 0.67. The refined restraints B---F = 1.37(2) and F...F = 2.24(2)\%A were applied to these groups. All non-H atoms with occupancy >0.5 were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0919P)^2^+0.1259P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.231(12) _refine_ls_number_reflns 7333 _refine_ls_number_parameters 438 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.062 _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 0.250680(19) 0.27362(2) 0.250100(17) 0.04290(10) Uani 1 1 d . . . N2 N 0.2603(3) 0.2675(2) 0.35519(19) 0.0496(8) Uani 1 1 d . . . C3 C 0.3509(3) 0.2991(3) 0.39340(17) 0.0554(7) Uani 1 1 d . . . C4 C 0.3604(4) 0.2955(4) 0.4650(2) 0.0775(10) Uani 1 1 d . . . H4 H 0.4226 0.3164 0.4918 0.093 Uiso 1 1 calc R . . C5 C 0.2700(5) 0.2584(5) 0.4949(3) 0.0859(14) Uani 1 1 d . . . H5 H 0.2730 0.2550 0.5427 0.103 Uiso 1 1 calc R . . C6 C 0.1808(4) 0.2281(4) 0.4565(3) 0.0784(12) Uani 1 1 d . . . H6 H 0.1224 0.2043 0.4773 0.094 Uiso 1 1 calc R . . C7 C 0.1760(3) 0.2326(2) 0.3850(2) 0.0553(7) Uani 1 1 d . . . C8 C 0.4360(2) 0.3349(2) 0.35189(17) 0.0511(6) Uani 1 1 d . . . N9 N 0.40747(19) 0.33521(18) 0.28227(13) 0.0480(5) Uani 1 1 d . . . C10 C 0.4791(2) 0.3677(3) 0.24063(18) 0.0564(7) Uani 1 1 d . . . H10 H 0.4601 0.3677 0.1931 0.068 Uiso 1 1 calc R . . C11 C 0.5814(3) 0.4015(3) 0.2670(2) 0.0693(9) Uani 1 1 d . . . H11 H 0.6296 0.4241 0.2373 0.083 Uiso 1 1 calc R . . C12 C 0.6098(3) 0.4011(4) 0.3363(3) 0.0749(11) Uani 1 1 d . . . H12 H 0.6776 0.4235 0.3543 0.090 Uiso 1 1 calc R . . C13 C 0.5367(3) 0.3669(3) 0.3805(2) 0.0698(9) Uani 1 1 d . . . H13 H 0.5553 0.3655 0.4280 0.084 Uiso 1 1 calc R . . C14 C 0.0834(3) 0.2007(3) 0.3345(2) 0.0588(8) Uani 1 1 d . . . N15 N 0.0996(2) 0.2070(2) 0.26774(17) 0.0553(6) Uani 1 1 d . . . C16 C 0.0202(3) 0.1767(3) 0.2196(2) 0.0681(9) Uani 1 1 d . . . H16 H 0.0311 0.1803 0.1733 0.082 Uiso 1 1 calc R . . C17 C -0.0773(3) 0.1403(3) 0.2366(3) 0.0851(14) Uani 1 1 d . . . H17 H -0.1304 0.1184 0.2025 0.102 Uiso 1 1 calc R . . C18 C -0.0934(3) 0.1375(4) 0.3047(3) 0.0871(15) Uani 1 1 d . . . H18 H -0.1592 0.1158 0.3169 0.104 Uiso 1 1 calc R . . C19 C -0.0126(3) 0.1668(3) 0.3560(3) 0.0807(12) Uani 1 1 d . . . H19 H -0.0224 0.1638 0.4025 0.097 Uiso 1 1 calc R . . N20 N 0.2440(3) 0.2840(2) 0.14611(19) 0.0494(7) Uani 1 1 d . . . C21 C 0.2766(3) 0.2010(3) 0.10966(18) 0.0528(6) Uani 1 1 d . . . C22 C 0.2767(4) 0.2066(4) 0.0381(2) 0.0700(10) Uani 1 1 d . . . H22 H 0.3009 0.1492 0.0136 0.084 Uiso 1 1 calc R . . C23 C 0.2402(5) 0.2994(5) 0.0046(3) 0.0816(12) Uani 1 1 d . . . H23 H 0.2373 0.3040 -0.0432 0.098 Uiso 1 1 calc R . . C24 C 0.2078(3) 0.3859(3) 0.04206(19) 0.0715(9) Uani 1 1 d . . . H24 H 0.1854 0.4495 0.0200 0.086 Uiso 1 1 calc R . . C25 C 0.2095(2) 0.3754(2) 0.11321(16) 0.0527(6) Uani 1 1 d . . . C26 C 0.3108(2) 0.1061(2) 0.15300(17) 0.0524(6) Uani 1 1 d . . . N27 N 0.30851(18) 0.12026(19) 0.22118(14) 0.0506(5) Uani 1 1 d . . . C28 C 0.3402(3) 0.0389(3) 0.2640(2) 0.0616(8) Uani 1 1 d . . . H28 H 0.3392 0.0486 0.3112 0.074 Uiso 1 1 calc R . . C29 C 0.3740(3) -0.0583(3) 0.2408(3) 0.0751(10) Uani 1 1 d . . . H29 H 0.3966 -0.1127 0.2717 0.090 Uiso 1 1 calc R . . C30 C 0.3735(4) -0.0727(3) 0.1708(3) 0.0831(13) Uani 1 1 d . . . H30 H 0.3940 -0.1382 0.1538 0.100 Uiso 1 1 calc R . . C31 C 0.3425(3) 0.0099(3) 0.1258(2) 0.0738(10) Uani 1 1 d . . . H31 H 0.3429 0.0013 0.0785 0.089 Uiso 1 1 calc R . . C32 C 0.1754(2) 0.4589(2) 0.16051(17) 0.0513(6) Uani 1 1 d . . . N33 N 0.18197(19) 0.42910(19) 0.22745(14) 0.0514(5) Uani 1 1 d . . . C34 C 0.1473(3) 0.4997(3) 0.27381(19) 0.0596(7) Uani 1 1 d . . . H34 H 0.1490 0.4791 0.3197 0.072 Uiso 1 1 calc R . . C35 C 0.1098(3) 0.6010(3) 0.2545(3) 0.0751(11) Uani 1 1 d . . . H35 H 0.0876 0.6481 0.2870 0.090 Uiso 1 1 calc R . . C36 C 0.1062(4) 0.6308(3) 0.1859(3) 0.0771(12) Uani 1 1 d . . . H36 H 0.0817 0.6986 0.1718 0.092 Uiso 1 1 calc R . . C37 C 0.1390(3) 0.5595(3) 0.1384(2) 0.0680(9) Uani 1 1 d . . . H37 H 0.1367 0.5786 0.0922 0.082 Uiso 1 1 calc R . . B38 B 0.0110(5) -0.0255(5) 0.0608(3) 0.0898(16) Uani 1 1 d D . . F39A F -0.0184(7) -0.0587(8) -0.0019(4) 0.108(2) Uiso 0.50 1 d PD A 1 F40A F 0.0777(6) -0.0987(6) 0.0983(4) 0.1082(19) Uiso 0.50 1 d PD A 1 F41A F -0.0756(6) -0.0035(7) 0.0981(4) 0.092(2) Uiso 0.50 1 d PD A 1 F42A F 0.0648(5) 0.0743(6) 0.0609(4) 0.1009(17) Uiso 0.50 1 d PD A 1 F39B F -0.0512(8) -0.0324(9) -0.0099(4) 0.129(3) Uiso 0.50 1 d PD A 2 F40B F 0.0281(7) -0.1295(7) 0.0784(4) 0.129(3) Uiso 0.50 1 d PD A 2 F41B F -0.0633(8) 0.0272(9) 0.0940(5) 0.126(4) Uiso 0.50 1 d PD A 2 F42B F 0.0941(9) 0.0296(10) 0.0475(7) 0.173(4) Uiso 0.50 1 d PD A 2 B43A B -0.0326(6) 0.5068(8) -0.0604(4) 0.080(2) Uani 0.67 1 d PD . . F44A F -0.0102(7) 0.5321(9) 0.0044(4) 0.089(2) Uiso 0.34 1 d PD B 1 F45A F 0.0161(9) 0.4379(10) -0.0945(6) 0.097(3) Uiso 0.34 1 d PD B 1 F46A F -0.1454(6) 0.4938(7) -0.0675(4) 0.0756(17) Uiso 0.34 1 d PD B 1 F47A F -0.0246(17) 0.6024(13) -0.1029(9) 0.223(10) Uiso 0.34 1 d PD B 1 F44B F -0.0263(7) 0.4539(7) 0.0073(4) 0.090(2) Uiso 0.33 1 d PD B 2 F45B F 0.0567(9) 0.5673(11) -0.0589(7) 0.140(4) Uiso 0.33 1 d PD B 2 F46B F -0.1308(6) 0.5451(9) -0.0818(5) 0.087(2) Uiso 0.33 1 d PD B 2 F47B F -0.0114(10) 0.4130(9) -0.0967(6) 0.104(4) Uiso 0.33 1 d PD B 2 B43C B -0.0398(13) 0.5410(12) -0.0587(8) 0.066(5) Uiso 0.33 1 d PD B 3 F44C F 0.0371(10) 0.5060(13) -0.0981(7) 0.136(4) Uiso 0.33 1 d PD B 3 F45C F 0.0055(8) 0.5948(8) -0.0063(5) 0.098(3) Uiso 0.33 1 d PD B 3 F46C F -0.1103(9) 0.6008(10) -0.0984(6) 0.112(3) Uiso 0.33 1 d PD B 3 F47C F -0.0931(18) 0.4517(14) -0.0402(11) 0.233(10) Uiso 0.33 1 d PD B 3 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 0.03913(15) 0.04233(16) 0.04719(17) -0.00127(18) 0.00475(11) 0.00011(16) N2 0.0499(16) 0.0482(15) 0.0509(19) 0.0007(11) 0.0064(14) 0.0037(10) C3 0.0579(16) 0.0558(15) 0.0513(16) -0.0045(13) 0.0015(13) 0.0041(13) C4 0.080(2) 0.096(3) 0.0550(19) -0.0025(19) 0.0022(17) 0.004(2) C5 0.105(4) 0.103(3) 0.053(2) 0.007(2) 0.021(2) 0.005(3) C6 0.075(3) 0.097(3) 0.068(3) 0.016(2) 0.028(2) 0.008(2) C7 0.0578(18) 0.0506(15) 0.0604(18) 0.0035(13) 0.0199(15) 0.0052(13) C8 0.0493(14) 0.0480(13) 0.0548(16) -0.0069(12) 0.0006(12) 0.0008(11) N9 0.0456(11) 0.0442(11) 0.0541(13) 0.0002(10) 0.0051(9) 0.0005(9) C10 0.0493(14) 0.0515(14) 0.0683(19) 0.0012(14) 0.0061(13) -0.0018(12) C11 0.0455(15) 0.064(2) 0.100(3) 0.0040(19) 0.0127(16) -0.0068(14) C12 0.0474(16) 0.078(2) 0.097(3) -0.013(2) -0.0044(17) -0.0074(16) C13 0.0573(18) 0.077(2) 0.072(2) -0.0080(18) -0.0091(16) -0.0029(16) C14 0.0506(15) 0.0458(13) 0.084(2) 0.0027(15) 0.0245(15) -0.0003(12) N15 0.0468(12) 0.0428(11) 0.0762(18) -0.0057(11) 0.0071(12) -0.0001(9) C16 0.0567(17) 0.0516(16) 0.093(3) -0.0130(17) -0.0058(17) -0.0014(14) C17 0.0515(18) 0.062(2) 0.138(4) -0.024(2) -0.004(2) -0.0047(16) C18 0.050(2) 0.083(3) 0.131(5) 0.000(3) 0.025(2) -0.0145(18) C19 0.062(2) 0.073(2) 0.113(3) 0.011(2) 0.037(2) -0.0065(17) N20 0.0435(14) 0.0493(14) 0.056(2) -0.0035(11) 0.0067(14) -0.0024(10) C21 0.0479(15) 0.0546(15) 0.0566(17) -0.0073(13) 0.0089(13) -0.0034(13) C22 0.071(2) 0.079(2) 0.060(2) -0.0122(18) 0.0077(19) 0.0026(19) C23 0.103(3) 0.090(3) 0.052(2) 0.008(2) 0.009(2) 0.002(3) C24 0.081(2) 0.074(2) 0.0574(19) 0.0110(17) -0.0017(17) -0.0008(18) C25 0.0485(13) 0.0526(14) 0.0555(16) 0.0031(12) -0.0008(12) -0.0034(11) C26 0.0449(13) 0.0514(15) 0.0611(17) -0.0078(12) 0.0066(12) 0.0017(11) N27 0.0412(10) 0.0459(12) 0.0643(15) -0.0018(10) 0.0040(10) -0.0010(9) C28 0.0531(16) 0.0594(17) 0.071(2) 0.0086(15) 0.0012(14) 0.0012(13) C29 0.067(2) 0.0554(18) 0.100(3) 0.0061(19) -0.0024(19) 0.0103(16) C30 0.086(3) 0.0540(19) 0.107(3) -0.015(2) 0.003(2) 0.0174(19) C31 0.076(2) 0.0627(19) 0.083(2) -0.0202(18) 0.0099(19) 0.0105(17) C32 0.0439(13) 0.0475(13) 0.0617(16) 0.0027(12) 0.0018(11) -0.0008(11) N33 0.0433(10) 0.0460(11) 0.0652(15) 0.0003(11) 0.0083(10) 0.0007(9) C34 0.0563(16) 0.0562(16) 0.0679(19) -0.0072(14) 0.0142(14) 0.0012(13) C35 0.063(2) 0.0560(19) 0.107(3) -0.010(2) 0.014(2) 0.0042(16) C36 0.077(3) 0.0459(17) 0.106(3) 0.0042(19) 0.000(2) 0.0118(16) C37 0.0623(18) 0.0509(16) 0.088(2) 0.0144(16) -0.0018(17) 0.0026(13) B38 0.101(4) 0.096(4) 0.076(3) 0.003(3) 0.025(3) -0.011(3) B43A 0.073(5) 0.091(7) 0.075(5) -0.018(5) 0.008(3) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N20 2.025(4) . ? Co1 N2 2.041(4) . ? Co1 N15 2.144(3) . ? Co1 N27 2.145(2) . ? Co1 N9 2.149(2) . ? Co1 N33 2.149(2) . ? N2 C7 1.342(5) . ? N2 C3 1.351(5) . ? C3 C4 1.389(5) . ? C3 C8 1.486(5) . ? C4 C5 1.418(8) . ? C5 C6 1.334(8) . ? C6 C7 1.390(6) . ? C7 C14 1.493(6) . ? C8 N9 1.365(4) . ? C8 C13 1.387(5) . ? N9 C10 1.345(4) . ? C10 C11 1.400(5) . ? C11 C12 1.359(7) . ? C12 C13 1.399(6) . ? C14 N15 1.344(5) . ? C14 C19 1.392(5) . ? N15 C16 1.347(4) . ? C16 C17 1.387(6) . ? C17 C18 1.366(8) . ? C18 C19 1.394(7) . ? N20 C21 1.346(5) . ? N20 C25 1.356(4) . ? C21 C22 1.398(6) . ? C21 C26 1.489(5) . ? C22 C23 1.382(7) . ? C23 C24 1.392(7) . ? C24 C25 1.392(5) . ? C25 C32 1.487(5) . ? C26 N27 1.345(4) . ? C26 C31 1.389(5) . ? N27 C28 1.346(4) . ? C28 C29 1.378(6) . ? C29 C30 1.377(7) . ? C30 C31 1.380(7) . ? C32 N33 1.351(4) . ? C32 C37 1.387(4) . ? N33 C34 1.369(4) . ? C34 C35 1.386(5) . ? C35 C36 1.384(7) . ? C36 C37 1.381(6) . ? B38 F39A 1.304(9) . ? B38 F40A 1.392(9) . ? B38 F41A 1.408(9) . ? B38 F42A 1.417(9) . ? B38 F42B 1.305(10) . ? B38 F40B 1.353(9) . ? B38 F41B 1.368(10) . ? B38 F39B 1.509(10) . ? B43A F45A 1.286(12) . ? B43A F44A 1.301(10) . ? B43A F46A 1.425(10) . ? B43A F47A 1.463(14) . ? B43A F46B 1.349(11) . ? B43A F45B 1.354(12) . ? B43A F47B 1.408(13) . ? B43A F44B 1.469(11) . ? B43C F45C 1.300(15) . ? B43C F46C 1.337(15) . ? B43C F47C 1.371(16) . ? B43C F44C 1.377(15) . ? 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 N20 Co1 N2 178.20(13) . . ? N20 Co1 N15 104.44(12) . . ? N2 Co1 N15 77.07(13) . . ? N20 Co1 N27 76.69(11) . . ? N2 Co1 N27 104.34(11) . . ? N15 Co1 N27 91.85(9) . . ? N20 Co1 N9 101.63(11) . . ? N2 Co1 N9 76.88(12) . . ? N15 Co1 N9 153.93(11) . . ? N27 Co1 N9 93.76(9) . . ? N20 Co1 N33 76.52(11) . . ? N2 Co1 N33 102.52(11) . . ? N15 Co1 N33 92.13(10) . . ? N27 Co1 N33 153.07(11) . . ? N9 Co1 N33 94.26(9) . . ? C7 N2 C3 121.3(4) . . ? C7 N2 Co1 119.2(3) . . ? C3 N2 Co1 119.5(3) . . ? N2 C3 C4 121.0(4) . . ? N2 C3 C8 114.0(3) . . ? C4 C3 C8 125.0(3) . . ? C3 C4 C5 116.3(4) . . ? C6 C5 C4 122.0(5) . . ? C5 C6 C7 119.3(4) . . ? N2 C7 C6 120.1(4) . . ? N2 C7 C14 113.6(3) . . ? C6 C7 C14 126.3(4) . . ? N9 C8 C13 121.7(3) . . ? N9 C8 C3 114.7(2) . . ? C13 C8 C3 123.6(3) . . ? C10 N9 C8 118.8(3) . . ? C10 N9 Co1 126.3(2) . . ? C8 N9 Co1 114.80(19) . . ? N9 C10 C11 121.7(3) . . ? C12 C11 C10 119.4(4) . . ? C11 C12 C13 119.8(3) . . ? C8 C13 C12 118.6(4) . . ? N15 C14 C19 122.9(4) . . ? N15 C14 C7 115.4(3) . . ? C19 C14 C7 121.7(4) . . ? C14 N15 C16 118.5(3) . . ? C14 N15 Co1 114.5(2) . . ? C16 N15 Co1 127.0(3) . . ? N15 C16 C17 122.3(5) . . ? C18 C17 C16 118.5(4) . . ? C17 C18 C19 120.8(4) . . ? C14 C19 C18 117.1(5) . . ? C21 N20 C25 119.8(4) . . ? C21 N20 Co1 120.0(3) . . ? C25 N20 Co1 120.1(2) . . ? N20 C21 C22 121.6(4) . . ? N20 C21 C26 113.4(3) . . ? C22 C21 C26 125.0(3) . . ? C23 C22 C21 118.5(4) . . ? C22 C23 C24 120.2(4) . . ? C25 C24 C23 118.6(4) . . ? N20 C25 C24 121.3(3) . . ? N20 C25 C32 113.3(3) . . ? C24 C25 C32 125.5(3) . . ? N27 C26 C31 122.1(3) . . ? N27 C26 C21 114.8(3) . . ? C31 C26 C21 123.1(3) . . ? C26 N27 C28 118.4(3) . . ? C26 N27 Co1 115.1(2) . . ? C28 N27 Co1 126.5(2) . . ? N27 C28 C29 122.7(4) . . ? C30 C29 C28 118.3(4) . . ? C29 C30 C31 120.2(4) . . ? C30 C31 C26 118.3(4) . . ? N33 C32 C37 122.0(3) . . ? N33 C32 C25 114.6(2) . . ? C37 C32 C25 123.3(3) . . ? C32 N33 C34 118.2(3) . . ? C32 N33 Co1 115.2(2) . . ? C34 N33 Co1 126.6(2) . . ? N33 C34 C35 122.1(4) . . ? C36 C35 C34 118.7(4) . . ? C37 C36 C35 119.7(3) . . ? C36 C37 C32 119.2(4) . . ? F39A B38 F40A 112.0(7) . . ? F39A B38 F41A 113.1(7) . . ? F40A B38 F41A 108.3(6) . . ? F39A B38 F42A 111.5(7) . . ? F40A B38 F42A 108.3(6) . . ? F41A B38 F42A 103.2(6) . . ? F42B B38 F40B 116.5(8) . . ? F42B B38 F41B 116.9(9) . . ? F40B B38 F41B 116.0(7) . . ? F42B B38 F39B 101.2(7) . . ? F40B B38 F39B 103.1(7) . . ? F41B B38 F39B 98.5(7) . . ? F45A B43A F44A 127.0(10) . . ? F45A B43A F46A 113.9(9) . . ? F44A B43A F46A 103.1(7) . . ? F45A B43A F47A 100.5(10) . . ? F44A B43A F47A 109.3(11) . . ? F46A B43A F47A 99.8(10) . . ? F46B B43A F45B 122.8(11) . . ? F46B B43A F47B 111.0(8) . . ? F45B B43A F47B 105.6(9) . . ? F46B B43A F44B 113.0(8) . . ? F45B B43A F44B 105.7(8) . . ? F47B B43A F44B 94.9(8) . . ? F45C B43C F46C 111.8(12) . . ? F45C B43C F47C 113.4(15) . . ? F46C B43C F47C 106.9(14) . . ? F45C B43C F44C 109.2(13) . . ? F46C B43C F44C 108.6(12) . . ? F47C B43C F44C 106.7(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.414 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.055 #=END data_mh325rt _database_code_depnum_ccdc_archive 'CCDC 781738' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.6392(11) _cell_length_b 12.4722(11) _cell_length_c 19.4609(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.711(4) _cell_angle_gamma 90.00 _cell_volume 3046.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 26027 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 28.26 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26027 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.26 _reflns_number_total 7040 _reflns_number_gt 6470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over two equally occupied sites labelled 'A' and 'B', sharing a common wholly occupied B atom B38. Anion B43--F47 was refined over three equally occupied orientations 'A', 'B' and 'C', with orientations A and B sharing the same B atom B43A which therefore has occupancy 0.67. The refined restraints B---F = 1.38(2) and F...F = 2.25(2)\%A were applied to these groups. All non-H atoms with occupancy >0.5 were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0887P)^2^+2.1009P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.055(15) _refine_ls_number_reflns 7040 _refine_ls_number_parameters 437 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.057 _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 0.74942(3) 0.72541(3) 0.74987(2) 0.03873(11) Uani 1 1 d . . . N2 N 0.7400(3) 0.7316(2) 0.6460(2) 0.0483(9) Uani 1 1 d . . . C3 C 0.6489(3) 0.7000(3) 0.60648(19) 0.0495(7) Uani 1 1 d . . . C4 C 0.6399(4) 0.7032(5) 0.5344(2) 0.0702(12) Uani 1 1 d . . . H4 H 0.5781 0.6812 0.5074 0.084 Uiso 1 1 calc R . . C5 C 0.7290(6) 0.7414(5) 0.5043(3) 0.0775(15) Uani 1 1 d . . . H5 H 0.7256 0.7457 0.4564 0.093 Uiso 1 1 calc R . . C6 C 0.8193(5) 0.7720(4) 0.5438(3) 0.0706(14) Uani 1 1 d . . . H6 H 0.8777 0.7961 0.5232 0.085 Uiso 1 1 calc R . . C7 C 0.8242(3) 0.7671(3) 0.6158(2) 0.0524(8) Uani 1 1 d . . . C8 C 0.5635(3) 0.6641(3) 0.64814(19) 0.0473(7) Uani 1 1 d . . . N9 N 0.5924(2) 0.6640(2) 0.71770(16) 0.0449(6) Uani 1 1 d . . . C10 C 0.5208(3) 0.6310(3) 0.7592(2) 0.0502(7) Uani 1 1 d . . . H10 H 0.5404 0.6302 0.8067 0.060 Uiso 1 1 calc R . . C11 C 0.4183(3) 0.5981(4) 0.7334(3) 0.0617(10) Uani 1 1 d . . . H11 H 0.3701 0.5760 0.7632 0.074 Uiso 1 1 calc R . . C12 C 0.3902(4) 0.5991(4) 0.6630(3) 0.0662(11) Uani 1 1 d . . . H12 H 0.3223 0.5776 0.6447 0.079 Uiso 1 1 calc R . . C13 C 0.4631(3) 0.6321(4) 0.6191(2) 0.0621(10) Uani 1 1 d . . . H13 H 0.4449 0.6328 0.5714 0.075 Uiso 1 1 calc R . . C14 C 0.9162(3) 0.7983(3) 0.6654(2) 0.0510(8) Uani 1 1 d . . . N15 N 0.9006(3) 0.7924(2) 0.73275(19) 0.0502(7) Uani 1 1 d . . . C16 C 0.9790(3) 0.8229(3) 0.7812(3) 0.0621(10) Uani 1 1 d . . . H16 H 0.9672 0.8198 0.8274 0.075 Uiso 1 1 calc R . . C17 C 1.0774(4) 0.8593(4) 0.7652(4) 0.0788(16) Uani 1 1 d . . . H17 H 1.1305 0.8808 0.7995 0.095 Uiso 1 1 calc R . . C18 C 1.0929(4) 0.8621(5) 0.6952(4) 0.0776(16) Uani 1 1 d . . . H18 H 1.1582 0.8841 0.6824 0.093 Uiso 1 1 calc R . . C19 C 1.0123(4) 0.8326(4) 0.6451(3) 0.0749(13) Uani 1 1 d . . . H19 H 1.0220 0.8355 0.5985 0.090 Uiso 1 1 calc R . . N20 N 0.7559(3) 0.7158(2) 0.8530(2) 0.0433(8) Uani 1 1 d . . . C21 C 0.7225(3) 0.7967(3) 0.8897(2) 0.0498(8) Uani 1 1 d . . . C22 C 0.7222(4) 0.7917(4) 0.9619(3) 0.0636(11) Uani 1 1 d . . . H22 H 0.6987 0.8494 0.9864 0.076 Uiso 1 1 calc R . . C23 C 0.7578(5) 0.6987(5) 0.9951(3) 0.0730(13) Uani 1 1 d . . . H23 H 0.7591 0.6936 1.0429 0.088 Uiso 1 1 calc R . . C24 C 0.7915(4) 0.6129(4) 0.9582(2) 0.0643(10) Uani 1 1 d . . . H24 H 0.8144 0.5498 0.9806 0.077 Uiso 1 1 calc R . . C25 C 0.7905(3) 0.6230(3) 0.88677(19) 0.0471(7) Uani 1 1 d . . . C26 C 0.6892(3) 0.8924(3) 0.8472(2) 0.0488(8) Uani 1 1 d . . . N27 N 0.6917(2) 0.8784(2) 0.77870(16) 0.0456(6) Uani 1 1 d . . . C28 C 0.6593(3) 0.9606(3) 0.7350(2) 0.0546(8) Uani 1 1 d . . . H28 H 0.6592 0.9504 0.6877 0.065 Uiso 1 1 calc R . . C29 C 0.6269(4) 1.0582(3) 0.7583(3) 0.0695(12) Uani 1 1 d . . . H29 H 0.6061 1.1133 0.7274 0.083 Uiso 1 1 calc R . . C30 C 0.6259(4) 1.0724(4) 0.8284(3) 0.0758(14) Uani 1 1 d . . . H30 H 0.6044 1.1377 0.8451 0.091 Uiso 1 1 calc R . . C31 C 0.6571(4) 0.9894(3) 0.8746(3) 0.0684(11) Uani 1 1 d . . . H31 H 0.6566 0.9982 0.9220 0.082 Uiso 1 1 calc R . . C32 C 0.8244(3) 0.5396(3) 0.8399(2) 0.0479(7) Uani 1 1 d . . . N33 N 0.8181(2) 0.5695(2) 0.77222(17) 0.0478(6) Uani 1 1 d . . . C34 C 0.8534(3) 0.4991(3) 0.7258(2) 0.0579(9) Uani 1 1 d . . . H34 H 0.8517 0.5198 0.6798 0.070 Uiso 1 1 calc R . . C35 C 0.8916(4) 0.3978(4) 0.7454(3) 0.0690(12) Uani 1 1 d . . . H35 H 0.9147 0.3509 0.7131 0.083 Uiso 1 1 calc R . . C36 C 0.8942(4) 0.3686(4) 0.8142(3) 0.0756(14) Uani 1 1 d . . . H36 H 0.9187 0.3010 0.8286 0.091 Uiso 1 1 calc R . . C37 C 0.8607(3) 0.4393(3) 0.8611(3) 0.0632(10) Uani 1 1 d . . . H37 H 0.8625 0.4196 0.9073 0.076 Uiso 1 1 calc R . . B38 B 0.9890(6) 1.0256(6) 0.9383(3) 0.0867(19) Uani 1 1 d D . . F39A F 1.0163(7) 1.0590(8) 1.0031(4) 0.092(2) Uiso 0.50 1 d PD A 1 F40A F 0.9218(6) 1.1018(6) 0.9021(4) 0.094(2) Uiso 0.50 1 d PD A 1 F41A F 1.0759(6) 1.0071(7) 0.9024(4) 0.083(2) Uiso 0.50 1 d PD A 1 F42A F 0.9334(6) 0.9260(6) 0.9376(4) 0.0893(18) Uiso 0.50 1 d PD A 1 F39B F 1.0524(8) 1.0323(8) 1.0099(4) 0.110(3) Uiso 0.50 1 d PD A 2 F40B F 0.9712(7) 1.1287(7) 0.9198(4) 0.108(2) Uiso 0.50 1 d PD A 2 F41B F 1.0644(7) 0.9721(8) 0.9054(5) 0.103(3) Uiso 0.50 1 d PD A 2 F42B F 0.9059(10) 0.9687(11) 0.9514(8) 0.173(6) Uiso 0.50 1 d PD A 2 B43A B 1.0314(7) 0.4935(10) 1.0591(5) 0.076(3) Uani 0.67 1 d PD . . F44A F 1.0106(9) 0.4669(11) 0.9951(5) 0.093(3) Uiso 0.34 1 d PD B 1 F45A F 0.9979(13) 0.5887(11) 1.0852(9) 0.124(7) Uiso 0.34 1 d PD B 1 F46A F 1.1465(6) 0.5048(8) 1.0680(4) 0.0646(18) Uiso 0.34 1 d PD B 1 F47A F 1.0087(16) 0.4160(15) 1.1089(9) 0.179(8) Uiso 0.34 1 d PD B 1 F44B F 1.0257(8) 0.5478(8) 0.9921(4) 0.084(2) Uiso 0.33 1 d PD B 2 F45B F 0.9462(10) 0.4241(11) 1.0524(8) 0.126(4) Uiso 0.33 1 d PD B 2 F46B F 1.1296(7) 0.4541(10) 1.0801(5) 0.079(2) Uiso 0.33 1 d PD B 2 F47B F 0.9984(9) 0.5701(10) 1.1018(6) 0.081(3) Uiso 0.33 1 d PD B 2 B43C B 1.0398(15) 0.4613(15) 1.0590(10) 0.073(7) Uiso 0.33 1 d PD B 3 F44C F 0.9655(10) 0.5052(12) 1.0972(7) 0.114(4) Uiso 0.33 1 d PD B 3 F45C F 0.9934(9) 0.4045(10) 1.0063(6) 0.096(3) Uiso 0.33 1 d PD B 3 F46C F 1.1089(10) 0.3965(11) 1.0986(7) 0.113(4) Uiso 0.33 1 d PD B 3 F47C F 1.0991(18) 0.5468(15) 1.0388(12) 0.205(10) Uiso 0.33 1 d PD B 3 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 0.03555(17) 0.03891(18) 0.04153(19) -0.0016(2) 0.00371(12) -0.00004(19) N2 0.0449(19) 0.0428(17) 0.058(3) 0.0003(13) 0.0105(18) 0.0001(12) C3 0.0524(18) 0.0518(18) 0.0432(17) -0.0039(14) 0.0006(14) 0.0049(15) C4 0.077(3) 0.087(3) 0.044(2) -0.003(2) -0.0017(19) 0.000(2) C5 0.095(4) 0.092(4) 0.047(3) 0.000(2) 0.017(3) 0.006(3) C6 0.068(3) 0.086(3) 0.062(3) 0.018(2) 0.026(2) 0.015(2) C7 0.0486(19) 0.0490(19) 0.062(2) 0.0032(16) 0.0162(17) 0.0091(15) C8 0.0463(16) 0.0434(16) 0.0504(18) -0.0068(14) -0.0021(14) 0.0000(14) N9 0.0433(13) 0.0393(13) 0.0515(15) -0.0026(12) 0.0034(11) 0.0009(11) C10 0.0466(17) 0.0475(17) 0.056(2) 0.0005(15) 0.0057(14) 0.0001(14) C11 0.0423(18) 0.055(2) 0.088(3) 0.000(2) 0.0115(18) -0.0054(16) C12 0.0458(19) 0.070(3) 0.081(3) -0.009(2) -0.0030(19) -0.0064(19) C13 0.050(2) 0.066(2) 0.067(2) -0.0088(19) -0.0076(17) -0.0048(17) C14 0.0464(17) 0.0370(14) 0.072(2) 0.0045(15) 0.0176(16) 0.0007(13) N15 0.0449(15) 0.0381(13) 0.0672(19) -0.0053(13) 0.0054(14) 0.0004(11) C16 0.0514(19) 0.0482(19) 0.084(3) -0.0101(19) -0.0023(19) -0.0046(16) C17 0.044(2) 0.063(3) 0.126(5) -0.017(3) -0.004(2) -0.0027(19) C18 0.043(2) 0.073(3) 0.119(5) 0.002(3) 0.018(3) -0.015(2) C19 0.060(2) 0.066(3) 0.105(4) 0.012(3) 0.035(2) -0.003(2) N20 0.0355(16) 0.0399(15) 0.055(2) -0.0029(12) 0.0058(15) -0.0017(11) C21 0.0422(17) 0.0535(19) 0.054(2) -0.0093(16) 0.0085(15) -0.0016(15) C22 0.064(3) 0.073(3) 0.054(2) -0.013(2) 0.009(2) -0.002(2) C23 0.095(4) 0.080(3) 0.045(2) 0.004(2) 0.012(2) -0.003(3) C24 0.074(3) 0.064(2) 0.053(2) 0.0106(18) -0.0036(19) -0.004(2) C25 0.0422(15) 0.0461(16) 0.0511(18) 0.0024(14) -0.0021(13) -0.0010(13) C26 0.0387(15) 0.0472(17) 0.060(2) -0.0114(15) 0.0051(14) 0.0033(13) N27 0.0390(12) 0.0416(14) 0.0555(16) -0.0023(12) 0.0028(11) -0.0003(11) C28 0.0493(18) 0.0516(19) 0.061(2) 0.0079(16) -0.0001(16) 0.0020(15) C29 0.056(2) 0.046(2) 0.103(4) 0.006(2) -0.003(2) 0.0112(18) C30 0.074(3) 0.049(2) 0.103(4) -0.017(2) 0.007(3) 0.015(2) C31 0.074(3) 0.051(2) 0.080(3) -0.018(2) 0.010(2) 0.012(2) C32 0.0403(15) 0.0457(16) 0.0557(19) 0.0032(15) -0.0024(13) 0.0007(13) N33 0.0411(13) 0.0439(14) 0.0588(17) -0.0004(13) 0.0075(12) -0.0010(12) C34 0.0518(19) 0.0537(19) 0.070(2) -0.0095(18) 0.0142(17) -0.0028(17) C35 0.057(2) 0.054(2) 0.096(4) -0.015(2) 0.012(2) 0.0049(19) C36 0.075(3) 0.048(2) 0.102(4) 0.004(2) 0.000(3) 0.016(2) C37 0.059(2) 0.052(2) 0.076(3) 0.0115(19) -0.0019(19) 0.0034(17) B38 0.105(5) 0.097(5) 0.063(3) 0.011(3) 0.025(3) -0.010(4) B43A 0.061(5) 0.106(9) 0.062(5) -0.020(5) 0.011(4) -0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N20 2.003(4) . ? Co1 N2 2.013(5) . ? Co1 N27 2.141(3) . ? Co1 N15 2.147(3) . ? Co1 N9 2.151(3) . ? Co1 N33 2.153(3) . ? N2 C7 1.349(6) . ? N2 C3 1.365(6) . ? C3 C4 1.395(6) . ? C3 C8 1.493(5) . ? C4 C5 1.412(9) . ? C5 C6 1.355(9) . ? C6 C7 1.396(7) . ? C7 C14 1.474(6) . ? C8 N9 1.360(5) . ? C8 C13 1.387(5) . ? N9 C10 1.345(5) . ? C10 C11 1.395(5) . ? C11 C12 1.376(7) . ? C12 C13 1.390(7) . ? C14 N15 1.350(5) . ? C14 C19 1.388(6) . ? N15 C16 1.341(5) . ? C16 C17 1.392(7) . ? C17 C18 1.399(9) . ? C18 C19 1.376(8) . ? N20 C21 1.333(5) . ? N20 C25 1.377(5) . ? C21 C22 1.407(7) . ? C21 C26 1.486(6) . ? C22 C23 1.377(8) . ? C23 C24 1.384(8) . ? C24 C25 1.395(6) . ? C25 C32 1.479(5) . ? C26 N27 1.347(5) . ? C26 C31 1.401(5) . ? N27 C28 1.363(5) . ? C28 C29 1.379(6) . ? C29 C30 1.376(8) . ? C30 C31 1.398(8) . ? C32 N33 1.362(5) . ? C32 C37 1.378(5) . ? N33 C34 1.371(5) . ? C34 C35 1.390(7) . ? C35 C36 1.385(8) . ? C36 C37 1.371(8) . ? B38 F42B 1.317(11) . ? B38 F39A 1.335(9) . ? B38 F40B 1.347(10) . ? B38 F41B 1.380(10) . ? B38 F41A 1.387(9) . ? B38 F40A 1.407(9) . ? B38 F42A 1.427(9) . ? B38 F39B 1.526(10) . ? B43A F47C 1.187(19) . ? B43A F44C 1.186(16) . ? B43A F44A 1.286(11) . ? B43A F46B 1.353(12) . ? B43A F47B 1.363(13) . ? B43A F45B 1.376(12) . ? B43A F45A 1.377(14) . ? B43A F47A 1.421(14) . ? B43A F46A 1.452(10) . ? B43A F44B 1.463(12) . ? B43A F45C 1.550(15) . ? B43A F46C 1.685(17) . ? B43C F45C 1.325(17) . ? B43C F46C 1.362(17) . ? B43C F44C 1.378(17) . ? B43C F47C 1.386(17) . ? 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 N20 Co1 N2 178.38(16) . . ? N20 Co1 N27 76.46(12) . . ? N2 Co1 N27 104.29(12) . . ? N20 Co1 N15 104.25(14) . . ? N2 Co1 N15 77.21(15) . . ? N27 Co1 N15 91.78(11) . . ? N20 Co1 N9 101.45(13) . . ? N2 Co1 N9 77.11(14) . . ? N27 Co1 N9 93.55(11) . . ? N15 Co1 N9 154.30(13) . . ? N20 Co1 N33 77.01(12) . . ? N2 Co1 N33 102.30(13) . . ? N27 Co1 N33 153.34(12) . . ? N15 Co1 N33 92.15(11) . . ? N9 Co1 N33 94.24(11) . . ? C7 N2 C3 120.4(4) . . ? C7 N2 Co1 119.5(3) . . ? C3 N2 Co1 120.1(3) . . ? N2 C3 C4 121.5(4) . . ? N2 C3 C8 113.4(3) . . ? C4 C3 C8 125.1(4) . . ? C3 C4 C5 116.8(5) . . ? C6 C5 C4 121.3(5) . . ? C5 C6 C7 119.5(5) . . ? N2 C7 C6 120.4(5) . . ? N2 C7 C14 113.8(4) . . ? C6 C7 C14 125.7(4) . . ? N9 C8 C13 122.1(4) . . ? N9 C8 C3 114.4(3) . . ? C13 C8 C3 123.4(4) . . ? C10 N9 C8 118.4(3) . . ? C10 N9 Co1 126.6(2) . . ? C8 N9 Co1 114.9(2) . . ? N9 C10 C11 122.4(4) . . ? C12 C11 C10 118.4(4) . . ? C11 C12 C13 120.2(4) . . ? C8 C13 C12 118.4(4) . . ? N15 C14 C19 121.7(4) . . ? N15 C14 C7 115.3(3) . . ? C19 C14 C7 123.0(4) . . ? C16 N15 C14 119.2(4) . . ? C16 N15 Co1 126.9(3) . . ? C14 N15 Co1 113.9(2) . . ? N15 C16 C17 122.8(5) . . ? C16 C17 C18 117.2(5) . . ? C19 C18 C17 120.4(4) . . ? C18 C19 C14 118.8(5) . . ? C21 N20 C25 118.9(4) . . ? C21 N20 Co1 120.9(3) . . ? C25 N20 Co1 120.1(3) . . ? N20 C21 C22 122.7(4) . . ? N20 C21 C26 113.3(4) . . ? C22 C21 C26 124.0(4) . . ? C23 C22 C21 117.8(4) . . ? C22 C23 C24 120.8(5) . . ? C23 C24 C25 118.7(4) . . ? N20 C25 C24 121.1(4) . . ? N20 C25 C32 113.3(3) . . ? C24 C25 C32 125.6(3) . . ? N27 C26 C31 122.0(4) . . ? N27 C26 C21 114.2(3) . . ? C31 C26 C21 123.8(4) . . ? C26 N27 C28 118.6(3) . . ? C26 N27 Co1 115.0(2) . . ? C28 N27 Co1 126.4(3) . . ? N27 C28 C29 122.6(4) . . ? C30 C29 C28 118.5(4) . . ? C29 C30 C31 120.5(4) . . ? C30 C31 C26 117.8(5) . . ? N33 C32 C37 121.1(4) . . ? N33 C32 C25 114.5(3) . . ? C37 C32 C25 124.3(4) . . ? C32 N33 C34 118.4(3) . . ? C32 N33 Co1 114.8(2) . . ? C34 N33 Co1 126.9(3) . . ? N33 C34 C35 122.1(4) . . ? C36 C35 C34 118.2(4) . . ? C37 C36 C35 120.0(4) . . ? C36 C37 C32 120.2(5) . . ? F39A B38 F41A 113.3(7) . . ? F39A B38 F40A 109.7(7) . . ? F41A B38 F40A 109.1(6) . . ? F39A B38 F42A 110.6(7) . . ? F41A B38 F42A 105.6(7) . . ? F40A B38 F42A 108.4(7) . . ? F42B B38 F40B 117.0(9) . . ? F42B B38 F41B 116.0(9) . . ? F40B B38 F41B 116.1(7) . . ? F42B B38 F39B 101.5(8) . . ? F40B B38 F39B 104.2(7) . . ? F41B B38 F39B 97.6(7) . . ? F44A B43A F45A 122.9(12) . . ? F44A B43A F47A 116.7(12) . . ? F45A B43A F47A 103.9(11) . . ? F44A B43A F46A 103.2(8) . . ? F45A B43A F46A 102.7(10) . . ? F47A B43A F46A 105.3(11) . . ? F46B B43A F47B 113.9(9) . . ? F46B B43A F44B 112.6(8) . . ? F47B B43A F44B 103.4(10) . . ? F45B B43A F44B 104.5(9) . . ? F45C B43C F46C 108.6(14) . . ? F45C B43C F44C 111.2(14) . . ? F46C B43C F44C 111.3(14) . . ? F45C B43C F47C 113.4(16) . . ? F46C B43C F47C 106.5(15) . . ? F44C B43C F47C 105.8(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.436 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.067 #=END data_mh325250 _database_code_depnum_ccdc_archive 'CCDC 781739' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.5930(12) _cell_length_b 12.4003(12) _cell_length_c 19.3600(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.109(5) _cell_angle_gamma 90.00 _cell_volume 3000.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 26108 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 28.51 _exptl_crystal_description fragment _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26108 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.51 _reflns_number_total 7284 _reflns_number_gt 6804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over two equally occupied sites labelled 'A' and 'B', sharing a common wholly occupied B atom B38. Anion B43--F47 was refined over three equally occupied orientations 'A', 'B' and 'C', with orientations A and B sharing the same B atom B43A which therefore has occupancy 0.67. The refined restraints B---F = 1.38(2) and F...F = 2.25(2)\%A were applied to these groups. All non-H atoms with occupancy >0.5 were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0732P)^2^+1.1803P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.246(12) _refine_ls_number_reflns 7284 _refine_ls_number_parameters 438 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.063 _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 0.25056(2) 0.27733(2) 0.250111(18) 0.03369(9) Uani 1 1 d . . . N2 N 0.2608(2) 0.27046(19) 0.35463(17) 0.0401(6) Uani 1 1 d . . . C3 C 0.3519(2) 0.3005(2) 0.39361(15) 0.0424(6) Uani 1 1 d . . . C4 C 0.3613(3) 0.2954(3) 0.46621(19) 0.0592(8) Uani 1 1 d . . . H4 H 0.4241 0.3160 0.4934 0.071 Uiso 1 1 calc R . . C5 C 0.2736(4) 0.2587(4) 0.4962(2) 0.0673(10) Uani 1 1 d . . . H5 H 0.2777 0.2553 0.5445 0.081 Uiso 1 1 calc R . . C6 C 0.1816(4) 0.2276(3) 0.4566(2) 0.0616(10) Uani 1 1 d . . . H6 H 0.1234 0.2027 0.4773 0.074 Uiso 1 1 calc R . . C7 C 0.1764(3) 0.2339(2) 0.38418(18) 0.0445(6) Uani 1 1 d . . . C8 C 0.4368(2) 0.3379(2) 0.35199(15) 0.0403(5) Uani 1 1 d . . . N9 N 0.40741(17) 0.33845(17) 0.28213(12) 0.0385(4) Uani 1 1 d . . . C10 C 0.4778(2) 0.3724(2) 0.24056(16) 0.0435(6) Uani 1 1 d . . . H10 H 0.4573 0.3739 0.1927 0.052 Uiso 1 1 calc R . . C11 C 0.5813(2) 0.4057(3) 0.26644(19) 0.0517(7) Uani 1 1 d . . . H11 H 0.6288 0.4287 0.2364 0.062 Uiso 1 1 calc R . . C12 C 0.6112(3) 0.4037(3) 0.3373(2) 0.0564(8) Uani 1 1 d . . . H12 H 0.6798 0.4250 0.3557 0.068 Uiso 1 1 calc R . . C13 C 0.5387(2) 0.3698(3) 0.38112(18) 0.0535(7) Uani 1 1 d . . . H13 H 0.5577 0.3684 0.4291 0.064 Uiso 1 1 calc R . . C14 C 0.0831(2) 0.2032(2) 0.33302(19) 0.0462(6) Uani 1 1 d . . . N15 N 0.09969(19) 0.21019(18) 0.26582(15) 0.0446(5) Uani 1 1 d . . . C16 C 0.0205(2) 0.1793(2) 0.2166(2) 0.0557(8) Uani 1 1 d . . . H16 H 0.0324 0.1821 0.1702 0.067 Uiso 1 1 calc R . . C17 C -0.0777(3) 0.1436(3) 0.2322(3) 0.0716(12) Uani 1 1 d . . . H17 H -0.1309 0.1222 0.1973 0.086 Uiso 1 1 calc R . . C18 C -0.0947(3) 0.1407(4) 0.3021(3) 0.0740(13) Uani 1 1 d . . . H18 H -0.1607 0.1195 0.3143 0.089 Uiso 1 1 calc R . . C19 C -0.0133(3) 0.1694(3) 0.3528(3) 0.0656(10) Uani 1 1 d . . . H19 H -0.0229 0.1661 0.3996 0.079 Uiso 1 1 calc R . . N20 N 0.2441(2) 0.28802(19) 0.14618(17) 0.0390(6) Uani 1 1 d . . . C21 C 0.2772(2) 0.2054(2) 0.10999(17) 0.0429(6) Uani 1 1 d . . . C22 C 0.2783(3) 0.2117(3) 0.0377(2) 0.0571(9) Uani 1 1 d . . . H22 H 0.3017 0.1539 0.0129 0.069 Uiso 1 1 calc R . . C23 C 0.2435(4) 0.3067(4) 0.0043(2) 0.0657(9) Uani 1 1 d . . . H23 H 0.2431 0.3129 -0.0436 0.079 Uiso 1 1 calc R . . C24 C 0.2095(3) 0.3917(3) 0.04165(18) 0.0568(8) Uani 1 1 d . . . H24 H 0.1866 0.4556 0.0194 0.068 Uiso 1 1 calc R . . C25 C 0.2099(2) 0.3807(2) 0.11332(15) 0.0419(6) Uani 1 1 d . . . C26 C 0.3111(2) 0.1097(2) 0.15363(16) 0.0415(6) Uani 1 1 d . . . N27 N 0.30854(17) 0.12422(18) 0.22217(13) 0.0420(5) Uani 1 1 d . . . C28 C 0.3392(2) 0.0423(2) 0.26624(19) 0.0502(7) Uani 1 1 d . . . H28 H 0.3376 0.0518 0.3137 0.060 Uiso 1 1 calc R . . C29 C 0.3733(3) -0.0561(3) 0.2420(2) 0.0613(9) Uani 1 1 d . . . H29 H 0.3954 -0.1113 0.2731 0.074 Uiso 1 1 calc R . . C30 C 0.3736(3) -0.0706(3) 0.1715(3) 0.0684(11) Uani 1 1 d . . . H30 H 0.3949 -0.1362 0.1544 0.082 Uiso 1 1 calc R . . C31 C 0.3423(3) 0.0126(3) 0.1263(2) 0.0580(8) Uani 1 1 d . . . H31 H 0.3420 0.0040 0.0786 0.070 Uiso 1 1 calc R . . C32 C 0.1748(2) 0.4638(2) 0.16092(16) 0.0418(5) Uani 1 1 d . . . N33 N 0.18105(18) 0.43290(17) 0.22869(13) 0.0411(5) Uani 1 1 d . . . C34 C 0.1460(2) 0.5029(2) 0.27490(19) 0.0500(7) Uani 1 1 d . . . H34 H 0.1482 0.4819 0.3212 0.060 Uiso 1 1 calc R . . C35 C 0.1071(3) 0.6046(3) 0.2556(2) 0.0592(9) Uani 1 1 d . . . H35 H 0.0837 0.6510 0.2883 0.071 Uiso 1 1 calc R . . C36 C 0.1039(3) 0.6356(3) 0.1868(3) 0.0653(10) Uani 1 1 d . . . H36 H 0.0790 0.7038 0.1728 0.078 Uiso 1 1 calc R . . C37 C 0.1380(3) 0.5646(2) 0.1388(2) 0.0544(7) Uani 1 1 d . . . H37 H 0.1361 0.5845 0.0924 0.065 Uiso 1 1 calc R . . B38 B 0.0114(4) -0.0246(4) 0.0598(3) 0.0701(12) Uani 1 1 d D . . F39A F -0.0160(5) -0.0606(6) -0.0039(3) 0.0748(15) Uiso 0.50 1 d PD A 1 F40A F 0.0794(5) -0.1022(5) 0.0982(3) 0.0775(14) Uiso 0.50 1 d PD A 1 F41A F -0.0734(5) -0.0055(6) 0.0975(4) 0.075(2) Uiso 0.50 1 d PD A 1 F42A F 0.0694(4) 0.0749(4) 0.0612(3) 0.0692(12) Uiso 0.50 1 d PD A 1 F39B F -0.0486(6) -0.0364(6) -0.0117(3) 0.089(2) Uiso 0.50 1 d PD A 2 F40B F 0.0374(5) -0.1259(5) 0.0824(3) 0.0943(18) Uiso 0.50 1 d PD A 2 F41B F -0.0696(6) 0.0228(6) 0.0938(4) 0.081(2) Uiso 0.50 1 d PD A 2 F42B F 0.0915(6) 0.0405(7) 0.0479(5) 0.115(3) Uiso 0.50 1 d PD A 2 B43A B -0.0306(6) 0.5026(8) -0.0571(4) 0.068(2) Uani 0.67 1 d PD . . F44A F -0.0107(8) 0.5288(9) 0.0061(4) 0.094(3) Uiso 0.34 1 d PD B 1 F45A F -0.0067(9) 0.4084(8) -0.0915(6) 0.084(4) Uiso 0.34 1 d PD B 1 F46A F -0.1470(5) 0.4950(6) -0.0656(3) 0.0559(13) Uiso 0.34 1 d PD B 1 F47A F -0.0035(16) 0.5857(14) -0.1035(9) 0.211(8) Uiso 0.34 1 d PD B 1 F44B F -0.0253(5) 0.4442(5) 0.0099(3) 0.0632(14) Uiso 0.33 1 d PD B 2 F45B F 0.0506(7) 0.5748(7) -0.0496(5) 0.096(2) Uiso 0.33 1 d PD B 2 F46B F -0.1316(5) 0.5411(7) -0.0786(4) 0.0620(15) Uiso 0.33 1 d PD B 2 F47B F 0.0088(8) 0.4315(9) -0.0991(5) 0.072(3) Uiso 0.33 1 d PD B 2 B43C B -0.0420(13) 0.5382(12) -0.0580(8) 0.067(6) Uiso 0.33 1 d PD B 3 F44C F 0.0319(8) 0.4941(9) -0.0965(5) 0.099(3) Uiso 0.33 1 d PD B 3 F45C F 0.0044(7) 0.5964(7) -0.0062(4) 0.080(2) Uiso 0.33 1 d PD B 3 F46C F -0.1113(8) 0.5991(9) -0.0991(5) 0.101(3) Uiso 0.33 1 d PD B 3 F47C F -0.0960(18) 0.4524(15) -0.0324(11) 0.245(11) Uiso 0.33 1 d PD B 3 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 0.02923(13) 0.03228(14) 0.03933(15) -0.00103(15) 0.00329(10) -0.00002(14) N2 0.0372(13) 0.0380(12) 0.0454(17) 0.0019(9) 0.0071(12) 0.0021(8) C3 0.0429(13) 0.0426(13) 0.0410(14) -0.0028(11) 0.0031(11) 0.0039(10) C4 0.063(2) 0.072(2) 0.0413(16) -0.0013(14) 0.0028(14) 0.0037(16) C5 0.080(3) 0.078(2) 0.046(2) 0.0054(19) 0.0163(19) 0.005(2) C6 0.061(2) 0.071(2) 0.058(2) 0.0141(16) 0.0245(18) 0.0075(16) C7 0.0436(15) 0.0385(13) 0.0541(17) 0.0044(12) 0.0167(13) 0.0046(11) C8 0.0369(12) 0.0381(12) 0.0444(13) -0.0049(10) -0.0005(10) 0.0011(9) N9 0.0353(10) 0.0343(10) 0.0455(12) -0.0019(9) 0.0029(8) 0.0009(8) C10 0.0393(12) 0.0388(12) 0.0525(16) 0.0002(11) 0.0065(11) -0.0006(10) C11 0.0380(13) 0.0451(15) 0.073(2) -0.0008(14) 0.0108(13) -0.0057(11) C12 0.0344(13) 0.0593(19) 0.074(2) -0.0118(17) 0.0001(13) -0.0054(13) C13 0.0431(15) 0.0583(17) 0.0561(18) -0.0058(14) -0.0054(13) -0.0028(12) C14 0.0376(13) 0.0357(12) 0.0679(19) 0.0039(12) 0.0174(13) 0.0012(10) N15 0.0354(11) 0.0344(10) 0.0635(16) -0.0044(10) 0.0048(10) 0.0009(8) C16 0.0431(14) 0.0392(13) 0.082(2) -0.0131(14) -0.0052(15) -0.0004(11) C17 0.0419(16) 0.0455(17) 0.123(4) -0.016(2) -0.0069(19) -0.0033(13) C18 0.0378(17) 0.063(2) 0.123(4) -0.001(2) 0.019(2) -0.0119(15) C19 0.0474(17) 0.0549(18) 0.099(3) 0.0118(18) 0.0283(18) -0.0047(14) N20 0.0313(12) 0.0386(11) 0.0466(17) -0.0022(10) 0.0026(11) -0.0015(8) C21 0.0372(13) 0.0438(13) 0.0479(15) -0.0058(12) 0.0062(12) -0.0029(11) C22 0.060(2) 0.061(2) 0.0514(19) -0.0086(15) 0.0093(17) -0.0012(15) C23 0.082(3) 0.070(2) 0.0457(19) 0.0025(18) 0.0085(17) -0.003(2) C24 0.0638(19) 0.0538(17) 0.0504(17) 0.0071(13) -0.0027(14) -0.0022(14) C25 0.0366(12) 0.0385(12) 0.0488(15) 0.0020(11) -0.0018(11) -0.0025(10) C26 0.0339(11) 0.0374(12) 0.0532(16) -0.0065(11) 0.0050(10) 0.0019(9) N27 0.0322(10) 0.0391(11) 0.0538(13) -0.0010(10) 0.0017(9) -0.0013(8) C28 0.0431(14) 0.0449(14) 0.0607(18) 0.0069(13) -0.0009(13) 0.0003(11) C29 0.0506(16) 0.0397(15) 0.090(3) 0.0062(16) -0.0054(16) 0.0082(13) C30 0.065(2) 0.0433(16) 0.094(3) -0.0144(18) 0.000(2) 0.0135(15) C31 0.0580(18) 0.0480(16) 0.068(2) -0.0167(15) 0.0086(15) 0.0079(13) C32 0.0332(11) 0.0367(12) 0.0538(15) 0.0042(11) -0.0015(10) -0.0010(9) N33 0.0327(9) 0.0351(10) 0.0558(14) -0.0008(9) 0.0060(9) -0.0012(8) C34 0.0409(14) 0.0462(14) 0.0642(19) -0.0098(13) 0.0116(13) -0.0002(11) C35 0.0494(16) 0.0451(16) 0.084(3) -0.0128(16) 0.0111(16) 0.0027(13) C36 0.062(2) 0.0374(16) 0.094(3) 0.0004(17) -0.002(2) 0.0110(14) C37 0.0505(16) 0.0417(14) 0.069(2) 0.0075(13) -0.0030(14) 0.0000(12) B38 0.080(3) 0.075(3) 0.057(2) 0.006(2) 0.016(2) -0.009(2) B43A 0.049(3) 0.093(7) 0.061(4) -0.025(4) 0.006(3) -0.013(4) _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 N20 2.008(3) . ? Co1 N2 2.013(3) . ? Co1 N27 2.128(2) . ? Co1 N15 2.130(3) . ? Co1 N9 2.135(2) . ? Co1 N33 2.138(2) . ? N2 C3 1.345(4) . ? N2 C7 1.346(4) . ? C3 C4 1.397(5) . ? C3 C8 1.491(4) . ? C4 C5 1.387(6) . ? C5 C6 1.364(7) . ? C6 C7 1.398(6) . ? C7 C14 1.490(5) . ? C8 N9 1.357(4) . ? C8 C13 1.393(4) . ? N9 C10 1.337(4) . ? C10 C11 1.399(4) . ? C11 C12 1.377(5) . ? C12 C13 1.387(5) . ? C14 N15 1.346(4) . ? C14 C19 1.382(4) . ? N15 C16 1.347(4) . ? C16 C17 1.382(6) . ? C17 C18 1.395(7) . ? C18 C19 1.376(6) . ? N20 C21 1.336(4) . ? N20 C25 1.358(4) . ? C21 C22 1.404(5) . ? C21 C26 1.489(4) . ? C22 C23 1.388(6) . ? C23 C24 1.376(6) . ? C24 C25 1.394(4) . ? C25 C32 1.485(4) . ? C26 N27 1.343(4) . ? C26 C31 1.391(4) . ? N27 C28 1.352(4) . ? C28 C29 1.394(5) . ? C29 C30 1.378(7) . ? C30 C31 1.377(6) . ? C32 N33 1.360(4) . ? C32 C37 1.382(4) . ? N33 C34 1.359(4) . ? C34 C35 1.387(5) . ? C35 C36 1.381(6) . ? C36 C37 1.387(6) . ? B38 F39A 1.316(7) . ? B38 F41A 1.388(8) . ? B38 F42A 1.432(7) . ? B38 F40A 1.433(7) . ? B38 F42B 1.334(8) . ? B38 F40B 1.356(8) . ? B38 F41B 1.410(8) . ? B38 F39B 1.500(8) . ? B43A F44A 1.261(10) . ? B43A F45A 1.396(12) . ? B43A F47A 1.436(13) . ? B43A F46A 1.457(8) . ? B43A F47B 1.336(11) . ? B43A F45B 1.353(10) . ? B43A F46B 1.373(10) . ? B43A F44B 1.480(10) . ? B43C F45C 1.313(15) . ? B43C F46C 1.339(15) . ? B43C F44C 1.375(15) . ? B43C F47C 1.387(16) . ? 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 N20 Co1 N2 178.08(13) . . ? N20 Co1 N27 77.10(10) . . ? N2 Co1 N27 103.67(10) . . ? N20 Co1 N15 104.05(11) . . ? N2 Co1 N15 77.73(12) . . ? N27 Co1 N15 91.59(9) . . ? N20 Co1 N9 100.87(10) . . ? N2 Co1 N9 77.36(11) . . ? N27 Co1 N9 93.23(8) . . ? N15 Co1 N9 155.07(10) . . ? N20 Co1 N33 77.37(10) . . ? N2 Co1 N33 101.94(10) . . ? N27 Co1 N33 154.29(10) . . ? N15 Co1 N33 91.68(9) . . ? N9 Co1 N33 94.47(8) . . ? C3 N2 C7 121.2(3) . . ? C3 N2 Co1 119.8(2) . . ? C7 N2 Co1 119.0(3) . . ? N2 C3 C4 120.8(3) . . ? N2 C3 C8 113.7(3) . . ? C4 C3 C8 125.5(3) . . ? C5 C4 C3 117.6(4) . . ? C6 C5 C4 121.5(4) . . ? C5 C6 C7 118.6(4) . . ? N2 C7 C6 120.3(3) . . ? N2 C7 C14 113.8(3) . . ? C6 C7 C14 126.0(3) . . ? N9 C8 C13 121.7(3) . . ? N9 C8 C3 114.5(2) . . ? C13 C8 C3 123.8(3) . . ? C10 N9 C8 118.8(2) . . ? C10 N9 Co1 126.57(19) . . ? C8 N9 Co1 114.59(18) . . ? N9 C10 C11 122.3(3) . . ? C12 C11 C10 118.7(3) . . ? C11 C12 C13 119.6(3) . . ? C12 C13 C8 118.8(3) . . ? N15 C14 C19 122.3(3) . . ? N15 C14 C7 115.0(2) . . ? C19 C14 C7 122.7(3) . . ? C14 N15 C16 118.4(3) . . ? C14 N15 Co1 114.3(2) . . ? C16 N15 Co1 127.2(3) . . ? N15 C16 C17 122.7(4) . . ? C16 C17 C18 118.0(4) . . ? C19 C18 C17 119.7(4) . . ? C18 C19 C14 118.9(4) . . ? C21 N20 C25 120.3(3) . . ? C21 N20 Co1 119.9(2) . . ? C25 N20 Co1 119.7(2) . . ? N20 C21 C22 121.5(3) . . ? N20 C21 C26 113.6(3) . . ? C22 C21 C26 124.9(3) . . ? C23 C22 C21 118.0(3) . . ? C24 C23 C22 120.5(4) . . ? C23 C24 C25 119.0(3) . . ? N20 C25 C24 120.7(3) . . ? N20 C25 C32 113.5(3) . . ? C24 C25 C32 125.8(3) . . ? N27 C26 C31 122.3(3) . . ? N27 C26 C21 114.4(2) . . ? C31 C26 C21 123.3(3) . . ? C26 N27 C28 118.8(3) . . ? C26 N27 Co1 114.96(18) . . ? C28 N27 Co1 126.2(2) . . ? N27 C28 C29 121.4(3) . . ? C30 C29 C28 119.1(3) . . ? C31 C30 C29 119.7(3) . . ? C30 C31 C26 118.6(4) . . ? N33 C32 C37 122.0(3) . . ? N33 C32 C25 114.7(2) . . ? C37 C32 C25 123.3(3) . . ? C34 N33 C32 118.1(2) . . ? C34 N33 Co1 127.4(2) . . ? C32 N33 Co1 114.50(18) . . ? N33 C34 C35 122.4(3) . . ? C36 C35 C34 118.7(3) . . ? C35 C36 C37 119.6(3) . . ? C32 C37 C36 119.2(4) . . ? F39A B38 F41A 114.9(5) . . ? F39A B38 F42A 112.6(5) . . ? F41A B38 F42A 105.5(5) . . ? F39A B38 F40A 109.2(5) . . ? F41A B38 F40A 106.9(5) . . ? F42A B38 F40A 107.3(5) . . ? F42B B38 F40B 117.3(6) . . ? F42B B38 F41B 115.7(6) . . ? F40B B38 F41B 113.3(5) . . ? F42B B38 F39B 101.9(5) . . ? F40B B38 F39B 106.4(5) . . ? F41B B38 F39B 99.2(5) . . ? F44A B43A F45A 130.5(10) . . ? F44A B43A F47A 112.9(11) . . ? F45A B43A F47A 102.7(10) . . ? F44A B43A F46A 101.7(7) . . ? F45A B43A F46A 99.5(7) . . ? F47A B43A F46A 106.8(10) . . ? F47B B43A F45B 99.7(8) . . ? F47B B43A F46B 116.4(7) . . ? F45B B43A F46B 117.5(9) . . ? F47B B43A F44B 103.3(8) . . ? F45B B43A F44B 106.1(7) . . ? F46B B43A F44B 112.0(6) . . ? F45C B43C F46C 109.8(12) . . ? F45C B43C F44C 111.5(13) . . ? F46C B43C F44C 109.7(12) . . ? F45C B43C F47C 109.9(15) . . ? F46C B43C F47C 109.4(15) . . ? F44C B43C F47C 106.5(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.428 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.074 #=END data_mh325200 _database_code_depnum_ccdc_archive 'CCDC 781740' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.5995(10) _cell_length_b 12.3791(10) _cell_length_c 19.2204(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.552(4) _cell_angle_gamma 90.00 _cell_volume 2971.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 25802 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.35 _exptl_crystal_description fragment _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25802 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.35 _reflns_number_total 7147 _reflns_number_gt 6888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over two equally occupied sites labelled 'A' and 'B', sharing a common wholly occupied B atom B38. Anion B43--F47 was also refined over two occupied orientations 'A' and 'B', with occupancies of 0.67 and 0.33 respectively. The refined restraints B---F = 1.38(2) and F...F = 2.25(2)\%A were applied to these groups. All non-H atoms with occupancy >0.5 were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0569P)^2^+1.2776P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.239(10) _refine_ls_number_reflns 7147 _refine_ls_number_parameters 442 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.069 _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 0.250540(16) 0.281302(18) 0.250070(15) 0.02680(7) Uani 1 1 d . . . N2 N 0.26102(19) 0.27353(15) 0.35330(14) 0.0317(5) Uani 1 1 d . . . C3 C 0.35273(19) 0.30218(19) 0.39315(13) 0.0340(4) Uani 1 1 d . . . C4 C 0.3633(2) 0.2953(2) 0.46630(15) 0.0469(6) Uani 1 1 d . . . H4 H 0.4263 0.3157 0.4939 0.056 Uiso 1 1 calc R . . C5 C 0.2753(3) 0.2566(3) 0.49643(17) 0.0555(7) Uani 1 1 d . . . H5 H 0.2802 0.2507 0.5450 0.067 Uiso 1 1 calc R . . C6 C 0.1820(3) 0.2270(2) 0.45563(18) 0.0492(7) Uani 1 1 d . . . H6 H 0.1240 0.2013 0.4760 0.059 Uiso 1 1 calc R . . C7 C 0.1764(2) 0.23641(19) 0.38288(14) 0.0362(5) Uani 1 1 d . . . C8 C 0.43709(17) 0.34003(17) 0.35207(12) 0.0319(4) Uani 1 1 d . . . N9 N 0.40649(14) 0.34235(14) 0.28137(10) 0.0308(4) Uani 1 1 d . . . C10 C 0.47630(18) 0.37668(17) 0.23943(13) 0.0349(5) Uani 1 1 d . . . H10 H 0.4554 0.3786 0.1912 0.042 Uiso 1 1 calc R . . C11 C 0.58012(19) 0.4098(2) 0.26617(15) 0.0407(5) Uani 1 1 d . . . H11 H 0.6272 0.4337 0.2361 0.049 Uiso 1 1 calc R . . C12 C 0.6115(2) 0.4065(2) 0.33762(16) 0.0440(6) Uani 1 1 d . . . H12 H 0.6803 0.4275 0.3561 0.053 Uiso 1 1 calc R . . C13 C 0.53945(19) 0.3714(2) 0.38190(14) 0.0426(5) Uani 1 1 d . . . H13 H 0.5591 0.3690 0.4302 0.051 Uiso 1 1 calc R . . C14 C 0.0830(2) 0.20635(18) 0.33086(16) 0.0390(5) Uani 1 1 d . . . N15 N 0.10046(16) 0.21427(14) 0.26296(13) 0.0364(4) Uani 1 1 d . . . C16 C 0.0217(2) 0.1845(2) 0.21224(18) 0.0480(6) Uani 1 1 d . . . H16 H 0.0340 0.1883 0.1656 0.058 Uiso 1 1 calc R . . C17 C -0.0770(2) 0.1485(2) 0.2272(2) 0.0615(10) Uani 1 1 d . . . H17 H -0.1299 0.1281 0.1912 0.074 Uiso 1 1 calc R . . C18 C -0.0952(2) 0.1436(3) 0.2963(3) 0.0673(12) Uani 1 1 d . . . H18 H -0.1612 0.1206 0.3074 0.081 Uiso 1 1 calc R . . C19 C -0.0145(2) 0.1729(2) 0.3494(2) 0.0559(8) Uani 1 1 d . . . H19 H -0.0257 0.1701 0.3963 0.067 Uiso 1 1 calc R . . N20 N 0.24472(18) 0.29322(17) 0.14713(14) 0.0319(5) Uani 1 1 d . . . C21 C 0.2777(2) 0.20947(19) 0.11022(14) 0.0350(5) Uani 1 1 d . . . C22 C 0.2796(3) 0.2165(2) 0.03806(18) 0.0468(7) Uani 1 1 d . . . H22 H 0.3030 0.1588 0.0131 0.056 Uiso 1 1 calc R . . C23 C 0.2455(3) 0.3121(3) 0.00446(17) 0.0545(7) Uani 1 1 d . . . H23 H 0.2457 0.3186 -0.0437 0.065 Uiso 1 1 calc R . . C24 C 0.2113(2) 0.3973(2) 0.04175(15) 0.0467(6) Uani 1 1 d . . . H24 H 0.1890 0.4614 0.0192 0.056 Uiso 1 1 calc R . . C25 C 0.21055(17) 0.38590(18) 0.11373(13) 0.0346(5) Uani 1 1 d . . . C26 C 0.31142(17) 0.11362(18) 0.15414(13) 0.0347(5) Uani 1 1 d . . . N27 N 0.30852(14) 0.12822(15) 0.22368(11) 0.0333(4) Uani 1 1 d . . . C28 C 0.33857(19) 0.0462(2) 0.26784(15) 0.0414(5) Uani 1 1 d . . . H28 H 0.3369 0.0556 0.3157 0.050 Uiso 1 1 calc R . . C29 C 0.3722(2) -0.0527(2) 0.24362(19) 0.0530(7) Uani 1 1 d . . . H29 H 0.3936 -0.1082 0.2750 0.064 Uiso 1 1 calc R . . C30 C 0.3732(3) -0.0672(2) 0.1728(2) 0.0572(8) Uani 1 1 d . . . H30 H 0.3952 -0.1327 0.1558 0.069 Uiso 1 1 calc R . . C31 C 0.3413(2) 0.0163(2) 0.12712(17) 0.0491(6) Uani 1 1 d . . . H31 H 0.3400 0.0073 0.0790 0.059 Uiso 1 1 calc R . . C32 C 0.17470(17) 0.46818(18) 0.16216(14) 0.0351(5) Uani 1 1 d . . . N33 N 0.18096(15) 0.43696(15) 0.22993(11) 0.0344(4) Uani 1 1 d . . . C34 C 0.14559(19) 0.5056(2) 0.27664(15) 0.0411(5) Uani 1 1 d . . . H34 H 0.1477 0.4840 0.3231 0.049 Uiso 1 1 calc R . . C35 C 0.1060(2) 0.6080(2) 0.25696(18) 0.0484(7) Uani 1 1 d . . . H35 H 0.0826 0.6539 0.2900 0.058 Uiso 1 1 calc R . . C36 C 0.1021(3) 0.6403(2) 0.1881(2) 0.0521(7) Uani 1 1 d . . . H36 H 0.0768 0.7086 0.1742 0.062 Uiso 1 1 calc R . . C37 C 0.1365(2) 0.5692(2) 0.13923(16) 0.0445(6) Uani 1 1 d . . . H37 H 0.1339 0.5890 0.0924 0.053 Uiso 1 1 calc R . . B38 B 0.0135(3) -0.0244(3) 0.05811(19) 0.0552(8) Uani 1 1 d D . . F39A F -0.0142(4) -0.0603(4) -0.0069(3) 0.0614(13) Uiso 0.50 1 d PD A 1 F40A F 0.0813(4) -0.1029(3) 0.0971(2) 0.0588(10) Uiso 0.50 1 d PD A 1 F41A F -0.0707(5) -0.0010(5) 0.0954(3) 0.0576(17) Uiso 0.50 1 d PD A 1 F42A F 0.0731(3) 0.0751(3) 0.0600(2) 0.0509(10) Uiso 0.50 1 d PD A 1 F39B F -0.0435(4) -0.0391(5) -0.0123(3) 0.0695(14) Uiso 0.50 1 d PD A 2 F40B F 0.0430(4) -0.1232(4) 0.0839(3) 0.0766(13) Uiso 0.50 1 d PD A 2 F41B F -0.0687(5) 0.0213(5) 0.0938(4) 0.067(2) Uiso 0.50 1 d PD A 2 F42B F 0.0917(5) 0.0480(5) 0.0493(3) 0.0767(16) Uiso 0.50 1 d PD A 2 B43A B -0.0293(4) 0.4960(7) -0.0505(4) 0.0575(17) Uani 0.67 1 d PD B 1 F44A F -0.0245(3) 0.4460(4) 0.01332(18) 0.0943(13) Uani 0.67 1 d PD B 1 F45A F 0.0393(5) 0.5808(5) -0.0440(5) 0.195(4) Uani 0.67 1 d PD B 1 F46A F -0.1382(2) 0.5216(5) -0.0712(2) 0.0936(16) Uani 0.67 1 d PD B 1 F47A F 0.0019(3) 0.4197(3) -0.09543(16) 0.0706(9) Uani 0.67 1 d PD B 1 B43B B -0.0456(11) 0.5349(11) -0.0599(7) 0.058(4) Uiso 0.33 1 d PD C 2 F44B F 0.0272(8) 0.4937(8) -0.0964(5) 0.100(3) Uiso 0.33 1 d PD C 2 F45B F -0.0025(8) 0.5710(9) 0.0024(4) 0.091(3) Uiso 0.33 1 d PD C 2 F46B F -0.1048(10) 0.6069(10) -0.0996(6) 0.131(4) Uiso 0.33 1 d PD C 2 F47B F -0.1215(15) 0.4590(16) -0.0482(11) 0.252(13) Uiso 0.33 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02285(11) 0.02535(11) 0.03218(13) -0.00086(12) 0.00357(8) 0.00005(11) N2 0.0296(10) 0.0288(10) 0.0369(13) 0.0003(8) 0.0057(9) 0.0028(7) C3 0.0329(10) 0.0340(10) 0.0350(12) -0.0025(9) 0.0043(9) 0.0035(8) C4 0.0514(15) 0.0542(15) 0.0342(13) -0.0031(11) 0.0030(11) 0.0045(12) C5 0.068(2) 0.0657(17) 0.0346(14) 0.0063(14) 0.0131(14) 0.0042(16) C6 0.0486(17) 0.0538(16) 0.0492(17) 0.0083(12) 0.0218(14) 0.0047(12) C7 0.0358(12) 0.0305(10) 0.0447(14) 0.0016(9) 0.0137(10) 0.0030(9) C8 0.0291(9) 0.0307(10) 0.0352(11) -0.0039(8) 0.0019(8) 0.0015(8) N9 0.0293(8) 0.0278(8) 0.0348(9) -0.0011(7) 0.0022(7) 0.0014(7) C10 0.0344(10) 0.0299(10) 0.0408(12) -0.0011(9) 0.0061(9) 0.0018(8) C11 0.0322(11) 0.0358(11) 0.0552(15) -0.0037(11) 0.0101(10) -0.0031(9) C12 0.0305(11) 0.0428(14) 0.0575(16) -0.0096(12) 0.0011(10) -0.0055(10) C13 0.0341(11) 0.0477(13) 0.0439(14) -0.0066(11) -0.0030(10) -0.0009(9) C14 0.0331(11) 0.0280(10) 0.0574(16) 0.0032(10) 0.0121(10) 0.0012(8) N15 0.0303(9) 0.0273(8) 0.0514(12) -0.0031(8) 0.0049(8) 0.0018(7) C16 0.0375(12) 0.0346(11) 0.0687(18) -0.0120(12) -0.0051(12) 0.0034(9) C17 0.0362(14) 0.0383(14) 0.105(3) -0.0144(16) -0.0094(16) -0.0017(11) C18 0.0293(14) 0.0452(17) 0.129(4) 0.0027(19) 0.0151(17) -0.0083(11) C19 0.0384(13) 0.0454(14) 0.088(2) 0.0125(14) 0.0232(14) -0.0007(11) N20 0.0243(10) 0.0325(10) 0.0388(13) -0.0005(8) 0.0034(9) -0.0011(7) C21 0.0297(11) 0.0351(11) 0.0401(13) -0.0046(9) 0.0048(10) -0.0019(8) C22 0.0494(17) 0.0517(16) 0.0400(15) -0.0074(11) 0.0088(13) -0.0023(11) C23 0.0668(19) 0.0590(16) 0.0379(14) -0.0003(14) 0.0076(13) -0.0029(15) C24 0.0526(14) 0.0461(13) 0.0397(13) 0.0073(11) -0.0004(11) -0.0023(11) C25 0.0289(10) 0.0312(10) 0.0429(13) 0.0031(9) 0.0016(9) -0.0014(8) C26 0.0264(9) 0.0327(10) 0.0448(13) -0.0071(9) 0.0039(9) 0.0009(8) N27 0.0259(8) 0.0310(9) 0.0426(11) -0.0008(8) 0.0026(7) -0.0009(7) C28 0.0345(11) 0.0388(12) 0.0493(14) 0.0060(10) -0.0007(10) -0.0019(9) C29 0.0427(14) 0.0322(12) 0.080(2) 0.0075(13) -0.0056(13) 0.0043(10) C30 0.0519(16) 0.0339(13) 0.084(2) -0.0098(14) 0.0002(16) 0.0094(11) C31 0.0464(14) 0.0427(14) 0.0577(17) -0.0145(12) 0.0054(12) 0.0091(11) C32 0.0270(9) 0.0297(10) 0.0471(12) 0.0015(9) -0.0011(9) -0.0016(8) N33 0.0252(7) 0.0290(8) 0.0492(12) -0.0008(8) 0.0056(7) -0.0009(7) C34 0.0318(11) 0.0377(12) 0.0544(15) -0.0068(10) 0.0084(10) -0.0041(9) C35 0.0383(13) 0.0373(13) 0.071(2) -0.0130(13) 0.0106(12) 0.0020(10) C36 0.0467(16) 0.0311(13) 0.076(2) 0.0023(13) 0.0002(14) 0.0069(10) C37 0.0398(12) 0.0328(11) 0.0581(16) 0.0047(11) -0.0035(11) 0.0020(9) B38 0.063(2) 0.063(2) 0.0420(17) 0.0054(15) 0.0146(15) -0.0054(17) B43A 0.029(2) 0.081(5) 0.062(4) -0.027(4) 0.003(2) -0.005(3) F44A 0.070(2) 0.157(4) 0.060(2) -0.015(2) 0.0207(16) -0.014(2) F45A 0.150(5) 0.108(4) 0.287(9) 0.106(5) -0.121(6) -0.083(4) F46A 0.0460(15) 0.158(4) 0.071(2) -0.061(3) -0.0144(14) 0.037(2) F47A 0.0644(18) 0.093(2) 0.0547(17) -0.0062(16) 0.0102(14) 0.0256(17) _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 1.973(3) . ? Co1 N20 1.976(3) . ? Co1 N15 2.109(2) . ? Co1 N27 2.1165(19) . ? Co1 N9 2.1174(18) . ? Co1 N33 2.1313(19) . ? N2 C3 1.347(3) . ? N2 C7 1.353(3) . ? C3 C4 1.397(4) . ? C3 C8 1.481(3) . ? C4 C5 1.401(5) . ? C5 C6 1.374(5) . ? C6 C7 1.396(4) . ? C7 C14 1.488(4) . ? C8 N9 1.363(3) . ? C8 C13 1.396(3) . ? N9 C10 1.338(3) . ? C10 C11 1.402(3) . ? C11 C12 1.379(4) . ? C12 C13 1.392(4) . ? C14 N15 1.355(4) . ? C14 C19 1.386(4) . ? N15 C16 1.348(3) . ? C16 C17 1.385(5) . ? C17 C18 1.379(6) . ? C18 C19 1.391(5) . ? N20 C21 1.352(3) . ? N20 C25 1.357(3) . ? C21 C22 1.393(4) . ? C21 C26 1.485(3) . ? C22 C23 1.390(5) . ? C23 C24 1.375(5) . ? C24 C25 1.392(4) . ? C25 C32 1.489(3) . ? C26 N27 1.354(3) . ? C26 C31 1.384(3) . ? N27 C28 1.346(3) . ? C28 C29 1.395(4) . ? C29 C30 1.375(5) . ? C30 C31 1.381(5) . ? C32 N33 1.351(3) . ? C32 C37 1.390(3) . ? N33 C34 1.354(3) . ? C34 C35 1.395(4) . ? C35 C36 1.378(5) . ? C36 C37 1.397(4) . ? B38 F39A 1.330(6) . ? B38 F41A 1.386(7) . ? B38 F40A 1.439(6) . ? B38 F42A 1.440(5) . ? B38 F40B 1.355(6) . ? B38 F42B 1.359(6) . ? B38 F41B 1.431(7) . ? B38 F39B 1.457(6) . ? B43A F45A 1.355(7) . ? B43A F44A 1.368(9) . ? B43A F47A 1.373(7) . ? B43A F46A 1.414(6) . ? B43B F44B 1.327(14) . ? B43B F45B 1.327(14) . ? B43B F46B 1.336(13) . ? B43B F47B 1.380(15) . ? 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 N20 177.75(11) . . ? N2 Co1 N15 78.77(10) . . ? N20 Co1 N15 103.37(9) . . ? N2 Co1 N27 102.57(8) . . ? N20 Co1 N27 78.20(8) . . ? N15 Co1 N27 91.08(7) . . ? N2 Co1 N9 78.16(9) . . ? N20 Co1 N9 99.72(8) . . ? N15 Co1 N9 156.91(9) . . ? N27 Co1 N9 92.92(7) . . ? N2 Co1 N33 101.44(8) . . ? N20 Co1 N33 77.90(9) . . ? N15 Co1 N33 91.34(7) . . ? N27 Co1 N33 155.88(8) . . ? N9 Co1 N33 94.19(7) . . ? C3 N2 C7 121.0(3) . . ? C3 N2 Co1 119.85(19) . . ? C7 N2 Co1 119.1(2) . . ? N2 C3 C4 121.2(2) . . ? N2 C3 C8 113.7(2) . . ? C4 C3 C8 125.1(2) . . ? C3 C4 C5 117.4(3) . . ? C6 C5 C4 121.3(3) . . ? C5 C6 C7 118.5(3) . . ? N2 C7 C6 120.7(3) . . ? N2 C7 C14 113.6(2) . . ? C6 C7 C14 125.7(2) . . ? N9 C8 C13 121.9(2) . . ? N9 C8 C3 114.17(18) . . ? C13 C8 C3 123.9(2) . . ? C10 N9 C8 119.01(19) . . ? C10 N9 Co1 126.96(16) . . ? C8 N9 Co1 113.95(14) . . ? N9 C10 C11 121.8(2) . . ? C12 C11 C10 119.2(2) . . ? C11 C12 C13 119.6(2) . . ? C12 C13 C8 118.5(2) . . ? N15 C14 C19 122.1(3) . . ? N15 C14 C7 114.5(2) . . ? C19 C14 C7 123.4(3) . . ? C16 N15 C14 118.6(2) . . ? C16 N15 Co1 127.5(2) . . ? C14 N15 Co1 113.79(16) . . ? N15 C16 C17 122.2(3) . . ? C18 C17 C16 118.8(3) . . ? C17 C18 C19 119.8(3) . . ? C14 C19 C18 118.4(3) . . ? C21 N20 C25 120.0(3) . . ? C21 N20 Co1 119.64(18) . . ? C25 N20 Co1 120.31(18) . . ? N20 C21 C22 121.4(2) . . ? N20 C21 C26 113.5(2) . . ? C22 C21 C26 125.1(2) . . ? C23 C22 C21 118.1(3) . . ? C24 C23 C22 120.6(3) . . ? C23 C24 C25 119.0(3) . . ? N20 C25 C24 120.8(2) . . ? N20 C25 C32 112.7(2) . . ? C24 C25 C32 126.5(2) . . ? N27 C26 C31 122.1(2) . . ? N27 C26 C21 114.31(19) . . ? C31 C26 C21 123.6(2) . . ? C28 N27 C26 118.7(2) . . ? C28 N27 Co1 127.02(18) . . ? C26 N27 Co1 114.26(15) . . ? N27 C28 C29 121.6(3) . . ? C30 C29 C28 119.2(3) . . ? C29 C30 C31 119.5(3) . . ? C30 C31 C26 118.9(3) . . ? N33 C32 C37 122.5(2) . . ? N33 C32 C25 115.01(19) . . ? C37 C32 C25 122.5(2) . . ? C32 N33 C34 118.5(2) . . ? C32 N33 Co1 113.84(15) . . ? C34 N33 Co1 127.64(18) . . ? N33 C34 C35 121.8(3) . . ? C36 C35 C34 119.4(3) . . ? C35 C36 C37 119.2(3) . . ? C32 C37 C36 118.6(3) . . ? F39A B38 F41A 115.6(4) . . ? F39A B38 F40A 109.1(4) . . ? F41A B38 F40A 108.3(4) . . ? F39A B38 F42A 112.4(4) . . ? F41A B38 F42A 103.9(4) . . ? F40A B38 F42A 107.0(4) . . ? F40B B38 F42B 118.2(5) . . ? F40B B38 F41B 111.2(4) . . ? F42B B38 F41B 112.5(5) . . ? F40B B38 F39B 107.8(4) . . ? F42B B38 F39B 104.0(4) . . ? F41B B38 F39B 101.3(4) . . ? F45A B43A F44A 108.5(5) . . ? F45A B43A F47A 111.0(6) . . ? F44A B43A F47A 105.7(6) . . ? F45A B43A F46A 115.8(7) . . ? F44A B43A F46A 106.3(5) . . ? F47A B43A F46A 108.9(4) . . ? F44B B43B F45B 112.2(11) . . ? F44B B43B F46B 109.2(11) . . ? F45B B43B F46B 115.0(11) . . ? F44B B43B F47B 111.5(13) . . ? F45B B43B F47B 107.0(13) . . ? F46B B43B F47B 101.6(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.486 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.050 #=END data_mh325150 _database_code_depnum_ccdc_archive 'CCDC 781741' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.6087(9) _cell_length_b 12.3683(9) _cell_length_c 19.0895(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.888(3) _cell_angle_gamma 90.00 _cell_volume 2948.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25597 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.31 _exptl_crystal_description fragment _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25597 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7084 _reflns_number_gt 6895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The crystal was refined as a racemic twin. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over two equally occupied sites labelled 'A' and 'B', sharing a common wholly occupied B atom B38. Anion B43--F47 was also refined over two occupied orientations 'A' and 'B', with occupancies of 0.80 and 0.20 respectively. The refined restraints B---F = 1.39(2) and F...F = 2.27(2)\%A were applied to these groups. All non-H atoms with occupancy >0.5 were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0419P)^2^+1.5431P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.231(8) _refine_ls_number_reflns 7084 _refine_ls_number_parameters 442 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.043 _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 0.250410(15) 0.285452(16) 0.250059(13) 0.02160(6) Uani 1 1 d . . . N2 N 0.26052(15) 0.27565(12) 0.35208(11) 0.0245(4) Uani 1 1 d . . . C3 C 0.35281(15) 0.30377(15) 0.39315(11) 0.0268(4) Uani 1 1 d . . . C4 C 0.36350(19) 0.29469(17) 0.46657(12) 0.0355(5) Uani 1 1 d . . . H4 H 0.4268 0.3143 0.4946 0.043 Uiso 1 1 calc R . . C5 C 0.2762(2) 0.2552(2) 0.49685(13) 0.0408(5) Uani 1 1 d . . . H5 H 0.2816 0.2477 0.5457 0.049 Uiso 1 1 calc R . . C6 C 0.1818(2) 0.22725(19) 0.45477(14) 0.0377(5) Uani 1 1 d . . . H6 H 0.1235 0.2017 0.4748 0.045 Uiso 1 1 calc R . . C7 C 0.17616(16) 0.23832(16) 0.38161(11) 0.0280(4) Uani 1 1 d . . . C8 C 0.43693(14) 0.34241(15) 0.35192(10) 0.0251(3) Uani 1 1 d . . . N9 N 0.40519(12) 0.34611(12) 0.28066(9) 0.0251(3) Uani 1 1 d . . . C10 C 0.47481(15) 0.38132(15) 0.23851(11) 0.0275(4) Uani 1 1 d . . . H10 H 0.4531 0.3847 0.1900 0.033 Uiso 1 1 calc R . . C11 C 0.57914(16) 0.41308(17) 0.26530(12) 0.0317(4) Uani 1 1 d . . . H11 H 0.6260 0.4368 0.2350 0.038 Uiso 1 1 calc R . . C12 C 0.61160(17) 0.40862(18) 0.33758(13) 0.0341(5) Uani 1 1 d . . . H12 H 0.6806 0.4294 0.3563 0.041 Uiso 1 1 calc R . . C13 C 0.54000(15) 0.37268(17) 0.38193(11) 0.0321(4) Uani 1 1 d . . . H13 H 0.5604 0.3689 0.4306 0.039 Uiso 1 1 calc R . . C14 C 0.08279(16) 0.20952(14) 0.32843(12) 0.0297(4) Uani 1 1 d . . . N15 N 0.10059(14) 0.21887(12) 0.26027(10) 0.0295(4) Uani 1 1 d . . . C16 C 0.02247(18) 0.18942(17) 0.20836(14) 0.0377(5) Uani 1 1 d . . . H16 H 0.0354 0.1937 0.1617 0.045 Uiso 1 1 calc R . . C17 C -0.07632(19) 0.15300(19) 0.22213(17) 0.0470(7) Uani 1 1 d . . . H17 H -0.1287 0.1327 0.1853 0.056 Uiso 1 1 calc R . . C18 C -0.09590(19) 0.1473(2) 0.29163(19) 0.0519(8) Uani 1 1 d . . . H18 H -0.1624 0.1245 0.3018 0.062 Uiso 1 1 calc R . . C19 C -0.01566(17) 0.17572(19) 0.34639(15) 0.0424(5) Uani 1 1 d . . . H19 H -0.0274 0.1723 0.3934 0.051 Uiso 1 1 calc R . . N20 N 0.24482(15) 0.29723(14) 0.14799(11) 0.0247(4) Uani 1 1 d . . . C21 C 0.27847(17) 0.21371(15) 0.11094(12) 0.0285(4) Uani 1 1 d . . . C22 C 0.2814(2) 0.22163(19) 0.03828(14) 0.0372(5) Uani 1 1 d . . . H22 H 0.3050 0.1639 0.0132 0.045 Uiso 1 1 calc R . . C23 C 0.2486(2) 0.3171(2) 0.00431(13) 0.0429(5) Uani 1 1 d . . . H23 H 0.2502 0.3241 -0.0440 0.051 Uiso 1 1 calc R . . C24 C 0.21317(18) 0.40276(19) 0.04224(12) 0.0371(5) Uani 1 1 d . . . H24 H 0.1910 0.4671 0.0197 0.044 Uiso 1 1 calc R . . C25 C 0.21139(14) 0.39052(15) 0.11462(11) 0.0274(4) Uani 1 1 d . . . C26 C 0.31127(14) 0.11761(15) 0.15524(11) 0.0274(4) Uani 1 1 d . . . N27 N 0.30848(12) 0.13273(13) 0.22542(9) 0.0273(3) Uani 1 1 d . . . C28 C 0.33809(16) 0.05014(18) 0.27013(13) 0.0348(4) Uani 1 1 d . . . H28 H 0.3365 0.0598 0.3183 0.042 Uiso 1 1 calc R . . C29 C 0.3710(2) -0.04902(19) 0.24623(16) 0.0448(6) Uani 1 1 d . . . H29 H 0.3919 -0.1045 0.2780 0.054 Uiso 1 1 calc R . . C30 C 0.3721(2) -0.0640(2) 0.17472(17) 0.0480(7) Uani 1 1 d . . . H30 H 0.3936 -0.1298 0.1579 0.058 Uiso 1 1 calc R . . C31 C 0.34073(18) 0.02008(18) 0.12789(14) 0.0394(5) Uani 1 1 d . . . H31 H 0.3396 0.0110 0.0794 0.047 Uiso 1 1 calc R . . C32 C 0.17475(14) 0.47251(15) 0.16278(11) 0.0272(4) Uani 1 1 d . . . N33 N 0.18133(12) 0.44079(12) 0.23142(9) 0.0273(3) Uani 1 1 d . . . C34 C 0.14514(15) 0.50861(16) 0.27829(12) 0.0320(4) Uani 1 1 d . . . H34 H 0.1474 0.4868 0.3251 0.038 Uiso 1 1 calc R . . C35 C 0.10425(17) 0.61106(18) 0.25820(14) 0.0386(5) Uani 1 1 d . . . H35 H 0.0799 0.6566 0.2913 0.046 Uiso 1 1 calc R . . C36 C 0.1005(2) 0.64381(19) 0.18882(16) 0.0408(6) Uani 1 1 d . . . H36 H 0.0749 0.7121 0.1750 0.049 Uiso 1 1 calc R . . C37 C 0.13549(16) 0.57356(16) 0.13971(13) 0.0347(5) Uani 1 1 d . . . H37 H 0.1327 0.5937 0.0925 0.042 Uiso 1 1 calc R . . B38 B 0.0157(2) -0.0230(3) 0.05643(15) 0.0429(6) Uani 1 1 d D . . F39A F -0.0120(3) -0.0600(3) -0.00989(19) 0.0416(8) Uiso 0.50 1 d PD A 1 F40A F 0.0830(3) -0.1028(3) 0.09639(18) 0.0422(8) Uiso 0.50 1 d PD A 1 F41A F -0.0690(4) 0.0002(4) 0.0928(3) 0.0444(14) Uiso 0.50 1 d PD A 1 F42A F 0.0779(3) 0.0749(3) 0.05806(17) 0.0349(7) Uiso 0.50 1 d PD A 1 F39B F -0.0390(3) -0.0421(3) -0.0144(2) 0.0501(10) Uiso 0.50 1 d PD A 2 F40B F 0.0512(3) -0.1203(3) 0.0853(2) 0.0576(10) Uiso 0.50 1 d PD A 2 F41B F -0.0666(4) 0.0201(4) 0.0930(3) 0.0483(16) Uiso 0.50 1 d PD A 2 F42B F 0.0944(3) 0.0504(3) 0.0504(2) 0.0531(11) Uiso 0.50 1 d PD A 2 B43A B -0.0301(3) 0.4926(4) -0.0466(2) 0.0493(10) Uani 0.80 1 d PD B 1 F44A F -0.02298(18) 0.4384(2) 0.01754(12) 0.0677(6) Uani 0.80 1 d PD B 1 F45A F 0.0355(3) 0.5809(3) -0.0395(3) 0.138(2) Uani 0.80 1 d PD B 1 F46A F -0.13793(17) 0.5188(3) -0.06875(13) 0.0754(9) Uani 0.80 1 d PD B 1 F47A F 0.00347(17) 0.4192(2) -0.09423(11) 0.0621(6) Uani 0.80 1 d PD B 1 B43B B -0.0476(11) 0.5371(12) -0.0601(7) 0.043(4) Uiso 0.20 1 d PD C 2 F44B F 0.0277(7) 0.4943(8) -0.0967(5) 0.058(2) Uiso 0.20 1 d PD C 2 F45B F -0.0025(10) 0.5748(12) 0.0041(6) 0.085(4) Uiso 0.20 1 d PD C 2 F46B F -0.1111(10) 0.6066(10) -0.0983(6) 0.093(4) Uiso 0.20 1 d PD C 2 F47B F -0.1161(18) 0.4546(17) -0.0423(13) 0.228(14) Uiso 0.20 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01788(9) 0.01978(9) 0.02713(11) -0.00104(10) 0.00306(7) -0.00013(9) N2 0.0228(8) 0.0209(8) 0.0302(10) -0.0011(6) 0.0054(7) 0.0018(6) C3 0.0259(8) 0.0258(8) 0.0285(10) -0.0009(7) 0.0031(7) 0.0020(7) C4 0.0376(11) 0.0396(11) 0.0284(10) -0.0015(8) 0.0013(8) 0.0016(8) C5 0.0488(13) 0.0471(12) 0.0275(11) 0.0038(10) 0.0087(10) 0.0039(11) C6 0.0381(12) 0.0407(12) 0.0373(13) 0.0058(9) 0.0158(10) 0.0031(9) C7 0.0283(9) 0.0229(8) 0.0343(11) 0.0007(8) 0.0098(8) 0.0015(7) C8 0.0240(8) 0.0234(8) 0.0273(9) -0.0021(7) 0.0012(7) 0.0020(6) N9 0.0243(7) 0.0221(7) 0.0284(8) -0.0009(6) 0.0017(6) 0.0017(6) C10 0.0275(8) 0.0254(8) 0.0297(10) 0.0005(7) 0.0043(7) 0.0027(7) C11 0.0276(9) 0.0279(9) 0.0408(11) -0.0011(8) 0.0093(8) -0.0017(7) C12 0.0244(9) 0.0337(11) 0.0427(12) -0.0077(9) -0.0004(8) -0.0045(8) C13 0.0265(9) 0.0368(10) 0.0312(10) -0.0050(8) -0.0023(8) -0.0015(7) C14 0.0241(9) 0.0217(8) 0.0445(12) 0.0028(8) 0.0083(8) 0.0008(6) N15 0.0258(8) 0.0223(7) 0.0400(10) -0.0016(6) 0.0035(7) 0.0031(6) C16 0.0342(10) 0.0250(9) 0.0506(13) -0.0077(9) -0.0058(9) 0.0054(8) C17 0.0311(11) 0.0292(11) 0.076(2) -0.0106(11) -0.0089(11) 0.0001(8) C18 0.0229(10) 0.0351(12) 0.097(3) 0.0070(13) 0.0079(12) -0.0059(9) C19 0.0292(10) 0.0353(11) 0.0653(16) 0.0118(11) 0.0157(10) -0.0008(8) N20 0.0189(8) 0.0248(8) 0.0298(10) -0.0011(6) 0.0017(7) -0.0007(6) C21 0.0243(9) 0.0284(9) 0.0326(11) -0.0048(7) 0.0030(8) -0.0015(7) C22 0.0394(13) 0.0402(12) 0.0324(12) -0.0068(9) 0.0072(10) -0.0017(9) C23 0.0520(14) 0.0486(13) 0.0281(11) -0.0003(10) 0.0054(10) -0.0055(11) C24 0.0407(11) 0.0362(11) 0.0326(11) 0.0061(9) -0.0007(9) -0.0022(8) C25 0.0220(8) 0.0248(8) 0.0342(10) 0.0021(7) 0.0001(7) -0.0021(6) C26 0.0200(7) 0.0265(9) 0.0353(10) -0.0056(7) 0.0022(7) 0.0006(6) N27 0.0213(7) 0.0257(7) 0.0342(9) -0.0005(6) 0.0014(6) -0.0017(6) C28 0.0277(9) 0.0347(10) 0.0406(12) 0.0072(8) -0.0007(8) -0.0044(8) C29 0.0346(11) 0.0297(11) 0.0659(17) 0.0105(11) -0.0080(11) 0.0011(9) C30 0.0400(12) 0.0284(11) 0.0729(19) -0.0081(11) -0.0022(12) 0.0090(9) C31 0.0363(10) 0.0340(11) 0.0472(13) -0.0133(10) 0.0031(9) 0.0063(8) C32 0.0210(8) 0.0229(8) 0.0364(10) 0.0014(7) -0.0007(7) -0.0019(6) N33 0.0192(6) 0.0251(7) 0.0372(9) 0.0000(6) 0.0027(6) -0.0018(6) C34 0.0247(9) 0.0313(10) 0.0404(11) -0.0044(8) 0.0056(8) -0.0049(7) C35 0.0301(10) 0.0284(10) 0.0581(15) -0.0125(10) 0.0093(9) 0.0004(8) C36 0.0356(11) 0.0223(10) 0.0634(16) 0.0025(9) 0.0026(10) 0.0045(8) C37 0.0309(9) 0.0260(9) 0.0451(12) 0.0043(8) -0.0025(9) 0.0007(7) B38 0.0484(15) 0.0478(15) 0.0337(14) 0.0044(11) 0.0101(11) -0.0029(12) B43A 0.0273(15) 0.068(3) 0.050(2) -0.019(2) -0.0021(15) -0.0017(17) F44A 0.0544(12) 0.1019(19) 0.0490(13) -0.0097(12) 0.0147(10) -0.0110(12) F45A 0.110(3) 0.078(2) 0.194(4) 0.067(2) -0.086(3) -0.0538(19) F46A 0.0412(10) 0.122(2) 0.0583(13) -0.0474(15) -0.0107(9) 0.0311(12) F47A 0.0530(12) 0.0885(17) 0.0453(11) -0.0040(11) 0.0086(9) 0.0248(12) _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 1.938(2) . ? Co1 N20 1.945(2) . ? Co1 N15 2.0943(17) . ? Co1 N9 2.0975(15) . ? Co1 N27 2.1023(17) . ? Co1 N33 2.1193(16) . ? N2 C7 1.352(3) . ? N2 C3 1.356(3) . ? C3 C4 1.394(3) . ? C3 C8 1.484(3) . ? C4 C5 1.399(3) . ? C5 C6 1.386(4) . ? C6 C7 1.395(3) . ? C7 C14 1.488(3) . ? C8 N9 1.365(2) . ? C8 C13 1.398(3) . ? N9 C10 1.342(3) . ? C10 C11 1.401(3) . ? C11 C12 1.385(3) . ? C12 C13 1.393(3) . ? C14 N15 1.355(3) . ? C14 C19 1.396(3) . ? N15 C16 1.348(3) . ? C16 C17 1.383(4) . ? C17 C18 1.384(5) . ? C18 C19 1.396(4) . ? N20 C21 1.353(3) . ? N20 C25 1.357(3) . ? C21 C22 1.396(4) . ? C21 C26 1.484(3) . ? C22 C23 1.383(4) . ? C23 C24 1.391(4) . ? C24 C25 1.393(3) . ? C25 C32 1.485(3) . ? C26 N27 1.358(3) . ? C26 C31 1.385(3) . ? N27 C28 1.351(3) . ? C28 C29 1.392(3) . ? C29 C30 1.379(4) . ? C30 C31 1.392(4) . ? C32 N33 1.359(3) . ? C32 C37 1.393(3) . ? N33 C34 1.351(3) . ? C34 C35 1.402(3) . ? C35 C36 1.380(4) . ? C36 C37 1.393(4) . ? B38 F39A 1.346(5) . ? B38 F41A 1.382(6) . ? B38 F42A 1.440(4) . ? B38 F40A 1.448(4) . ? B38 F42B 1.361(5) . ? B38 F40B 1.372(5) . ? B38 F41B 1.431(6) . ? B38 F39B 1.450(5) . ? B43A F45A 1.366(5) . ? B43A F44A 1.388(6) . ? B43A F47A 1.391(5) . ? B43A F46A 1.405(4) . ? B43B F46B 1.323(14) . ? B43B F44B 1.360(14) . ? B43B F45B 1.361(14) . ? B43B F47B 1.409(15) . ? 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 N20 178.18(9) . . ? N2 Co1 N15 79.49(8) . . ? N20 Co1 N15 102.33(7) . . ? N2 Co1 N9 79.17(7) . . ? N20 Co1 N9 99.01(7) . . ? N15 Co1 N9 158.65(7) . . ? N2 Co1 N27 101.06(7) . . ? N20 Co1 N27 78.99(7) . . ? N15 Co1 N27 90.79(6) . . ? N9 Co1 N27 92.55(6) . . ? N2 Co1 N33 101.20(7) . . ? N20 Co1 N33 78.84(7) . . ? N15 Co1 N33 90.97(6) . . ? N9 Co1 N33 93.88(6) . . ? N27 Co1 N33 157.62(7) . . ? C7 N2 C3 120.6(2) . . ? C7 N2 Co1 119.57(16) . . ? C3 N2 Co1 119.85(15) . . ? N2 C3 C4 121.16(19) . . ? N2 C3 C8 113.27(18) . . ? C4 C3 C8 125.57(18) . . ? C3 C4 C5 118.1(2) . . ? C6 C5 C4 120.6(2) . . ? C5 C6 C7 118.5(2) . . ? N2 C7 C6 121.1(2) . . ? N2 C7 C14 113.04(19) . . ? C6 C7 C14 125.87(19) . . ? N9 C8 C13 121.90(18) . . ? N9 C8 C3 113.97(16) . . ? C13 C8 C3 124.13(18) . . ? C10 N9 C8 118.81(16) . . ? C10 N9 Co1 127.53(13) . . ? C8 N9 Co1 113.57(12) . . ? N9 C10 C11 122.06(19) . . ? C12 C11 C10 119.1(2) . . ? C11 C12 C13 119.39(18) . . ? C12 C13 C8 118.70(19) . . ? N15 C14 C19 122.1(2) . . ? N15 C14 C7 114.50(17) . . ? C19 C14 C7 123.4(2) . . ? C16 N15 C14 118.8(2) . . ? C16 N15 Co1 127.98(17) . . ? C14 N15 Co1 113.16(13) . . ? N15 C16 C17 122.3(3) . . ? C16 C17 C18 118.8(2) . . ? C17 C18 C19 119.9(2) . . ? C14 C19 C18 118.0(3) . . ? C21 N20 C25 120.2(2) . . ? C21 N20 Co1 119.71(15) . . ? C25 N20 Co1 120.01(15) . . ? N20 C21 C22 121.3(2) . . ? N20 C21 C26 113.35(19) . . ? C22 C21 C26 125.38(19) . . ? C23 C22 C21 118.6(2) . . ? C22 C23 C24 120.2(2) . . ? C23 C24 C25 118.9(2) . . ? N20 C25 C24 120.8(2) . . ? N20 C25 C32 113.15(18) . . ? C24 C25 C32 126.07(18) . . ? N27 C26 C31 122.44(19) . . ? N27 C26 C21 114.14(16) . . ? C31 C26 C21 123.4(2) . . ? C28 N27 C26 118.49(18) . . ? C28 N27 Co1 127.78(16) . . ? C26 N27 Co1 113.67(12) . . ? N27 C28 C29 121.9(2) . . ? C30 C29 C28 119.1(2) . . ? C29 C30 C31 119.7(2) . . ? C26 C31 C30 118.4(2) . . ? N33 C32 C37 122.39(19) . . ? N33 C32 C25 114.64(16) . . ? C37 C32 C25 123.0(2) . . ? C34 N33 C32 118.54(17) . . ? C34 N33 Co1 128.33(14) . . ? C32 N33 Co1 113.13(13) . . ? N33 C34 C35 121.7(2) . . ? C36 C35 C34 119.4(2) . . ? C35 C36 C37 119.4(2) . . ? C32 C37 C36 118.6(2) . . ? F39A B38 F41A 115.1(3) . . ? F39A B38 F42A 112.1(3) . . ? F41A B38 F42A 105.7(3) . . ? F39A B38 F40A 108.8(3) . . ? F41A B38 F40A 108.3(3) . . ? F42A B38 F40A 106.5(3) . . ? F42B B38 F40B 114.7(3) . . ? F42B B38 F41B 112.2(4) . . ? F40B B38 F41B 110.4(3) . . ? F42B B38 F39B 106.8(3) . . ? F40B B38 F39B 108.6(3) . . ? F41B B38 F39B 103.4(3) . . ? F45A B43A F44A 109.5(3) . . ? F45A B43A F47A 110.6(4) . . ? F44A B43A F47A 105.8(4) . . ? F45A B43A F46A 113.1(4) . . ? F44A B43A F46A 108.7(3) . . ? F47A B43A F46A 108.8(3) . . ? F46B B43B F44B 112.5(12) . . ? F46B B43B F45B 114.8(12) . . ? F44B B43B F45B 111.2(11) . . ? F46B B43B F47B 105.0(13) . . ? F44B B43B F47B 109.6(14) . . ? F45B B43B F47B 103.0(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.448 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.047 #=END data_mh325 _database_code_depnum_ccdc_archive 'CCDC 781742' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.6088(11) _cell_length_b 12.3489(11) _cell_length_c 18.9484(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.937(4) _cell_angle_gamma 90.00 _cell_volume 2922.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25068 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.20 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.657 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25068 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.20 _reflns_number_total 6739 _reflns_number_gt 6491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0424P)^2^+3.9105P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(11) _refine_ls_number_reflns 6739 _refine_ls_number_parameters 426 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.073 _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 0.75004(2) 0.71154(2) 0.749749(19) 0.01688(8) Uani 1 1 d . . . N2 N 0.7412(2) 0.72220(17) 0.64878(14) 0.0171(5) Uani 1 1 d . . . C3 C 0.6473(2) 0.6952(2) 0.60660(15) 0.0205(5) Uani 1 1 d . . . C4 C 0.6367(2) 0.7068(2) 0.53226(15) 0.0260(6) Uani 1 1 d . . . H4 H 0.5717 0.6881 0.5033 0.031 Uiso 1 1 calc R . . C5 C 0.7237(3) 0.7464(3) 0.50192(16) 0.0297(6) Uani 1 1 d . . . H5 H 0.7178 0.7553 0.4517 0.036 Uiso 1 1 calc R . . C6 C 0.8195(2) 0.7730(3) 0.54488(17) 0.0265(6) Uani 1 1 d . . . H6 H 0.8792 0.7990 0.5244 0.032 Uiso 1 1 calc R . . C7 C 0.8254(2) 0.7604(2) 0.61892(14) 0.0182(5) Uani 1 1 d . . . C8 C 0.5635(2) 0.6564(2) 0.64763(14) 0.0190(5) Uani 1 1 d . . . N9 N 0.59581(17) 0.65110(17) 0.71945(12) 0.0196(4) Uani 1 1 d . . . C10 C 0.5261(2) 0.6154(2) 0.76184(15) 0.0214(5) Uani 1 1 d . . . H10 H 0.5484 0.6110 0.8117 0.026 Uiso 1 1 calc R . . C11 C 0.4215(2) 0.5843(2) 0.73475(15) 0.0234(5) Uani 1 1 d . . . H11 H 0.3736 0.5597 0.7659 0.028 Uiso 1 1 calc R . . C12 C 0.3888(2) 0.5901(2) 0.66211(16) 0.0254(6) Uani 1 1 d . . . H12 H 0.3183 0.5688 0.6428 0.030 Uiso 1 1 calc R . . C13 C 0.4598(2) 0.6271(2) 0.61741(15) 0.0229(5) Uani 1 1 d . . . H13 H 0.4384 0.6325 0.5675 0.027 Uiso 1 1 calc R . . C14 C 0.9178(2) 0.7875(2) 0.67181(15) 0.0214(5) Uani 1 1 d . . . N15 N 0.89964(18) 0.77752(17) 0.74052(13) 0.0217(5) Uani 1 1 d . . . C16 C 0.9771(2) 0.8078(2) 0.79324(17) 0.0271(6) Uani 1 1 d . . . H16 H 0.9628 0.8046 0.8411 0.033 Uiso 1 1 calc R . . C17 C 1.0771(3) 0.8434(3) 0.7799(2) 0.0351(7) Uani 1 1 d . . . H17 H 1.1307 0.8631 0.8180 0.042 Uiso 1 1 calc R . . C18 C 1.0968(2) 0.8494(3) 0.7102(2) 0.0355(8) Uani 1 1 d . . . H18 H 1.1650 0.8724 0.7000 0.043 Uiso 1 1 calc R . . C19 C 1.0164(2) 0.8218(2) 0.65404(17) 0.0286(6) Uani 1 1 d . . . H19 H 1.0287 0.8263 0.6058 0.034 Uiso 1 1 calc R . . N20 N 0.75449(18) 0.70049(18) 0.85078(13) 0.0156(5) Uani 1 1 d . . . C21 C 0.7195(2) 0.7843(2) 0.88830(15) 0.0205(5) Uani 1 1 d . . . C22 C 0.7156(3) 0.7757(3) 0.96168(17) 0.0264(6) Uani 1 1 d . . . H22 H 0.6915 0.8348 0.9874 0.032 Uiso 1 1 calc R . . C23 C 0.7475(2) 0.6795(3) 0.99625(16) 0.0301(6) Uani 1 1 d . . . H23 H 0.7449 0.6723 1.0459 0.036 Uiso 1 1 calc R . . C24 C 0.7835(2) 0.5935(2) 0.95794(15) 0.0257(6) Uani 1 1 d . . . H24 H 0.8053 0.5273 0.9811 0.031 Uiso 1 1 calc R . . C25 C 0.78700(19) 0.6063(2) 0.88504(14) 0.0199(5) Uani 1 1 d . . . C26 C 0.68884(19) 0.8803(2) 0.84348(14) 0.0196(5) Uani 1 1 d . . . N27 N 0.69212(17) 0.86415(19) 0.77251(12) 0.0214(4) Uani 1 1 d . . . C28 C 0.6637(2) 0.9464(3) 0.72766(17) 0.0296(6) Uani 1 1 d . . . H28 H 0.6661 0.9362 0.6782 0.036 Uiso 1 1 calc R . . C29 C 0.6307(2) 1.0466(3) 0.7511(2) 0.0339(7) Uani 1 1 d . . . H29 H 0.6100 1.1032 0.7181 0.041 Uiso 1 1 calc R . . C30 C 0.6288(2) 1.0618(3) 0.8232(2) 0.0356(8) Uani 1 1 d . . . H30 H 0.6068 1.1294 0.8402 0.043 Uiso 1 1 calc R . . C31 C 0.6593(2) 0.9779(2) 0.87106(17) 0.0287(6) Uani 1 1 d . . . H31 H 0.6598 0.9874 0.9209 0.034 Uiso 1 1 calc R . . C32 C 0.82479(19) 0.5247(2) 0.83705(14) 0.0192(5) Uani 1 1 d . . . N33 N 0.81875(17) 0.55673(18) 0.76778(12) 0.0205(4) Uani 1 1 d . . . C34 C 0.8562(2) 0.4891(2) 0.72138(15) 0.0227(5) Uani 1 1 d . . . H34 H 0.8543 0.5117 0.6733 0.027 Uiso 1 1 calc R . . C35 C 0.8977(2) 0.3868(2) 0.74114(17) 0.0273(6) Uani 1 1 d . . . H35 H 0.9234 0.3409 0.7070 0.033 Uiso 1 1 calc R . . C36 C 0.9009(2) 0.3534(2) 0.81110(18) 0.0290(7) Uani 1 1 d . . . H36 H 0.9267 0.2833 0.8252 0.035 Uiso 1 1 calc R . . C37 C 0.8658(2) 0.4237(2) 0.86076(16) 0.0258(6) Uani 1 1 d . . . H37 H 0.8697 0.4036 0.9094 0.031 Uiso 1 1 calc R . . B38 B 0.9820(3) 1.0214(3) 0.94344(19) 0.0292(7) Uani 1 1 d . . . F39 F 1.02195(17) 1.05135(17) 1.01311(10) 0.0410(5) Uani 1 1 d . . . F40 F 0.9272(2) 1.10899(17) 0.90779(11) 0.0478(5) Uani 1 1 d . . . F41 F 1.06603(15) 0.98830(15) 0.90777(9) 0.0342(4) Uani 1 1 d . . . F42 F 0.91185(15) 0.93343(16) 0.94509(10) 0.0393(5) Uani 1 1 d . . . B43 B 1.0302(3) 0.5118(4) 1.0444(2) 0.0390(9) Uani 1 1 d . A 1 F44 F 1.02135(17) 0.5661(2) 0.97909(11) 0.0500(5) Uani 1 1 d . . . F45 F 0.99452(17) 0.5811(2) 1.09364(11) 0.0535(6) Uani 1 1 d . A 1 F46 F 1.13739(17) 0.4844(2) 1.06600(12) 0.0584(7) Uani 1 1 d . A 1 F47 F 0.9670(3) 0.4204(2) 1.03656(19) 0.0879(11) Uani 1 1 d . A 1 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 0.01428(13) 0.01631(14) 0.01992(15) -0.00101(15) 0.00193(10) -0.00052(14) N2 0.0185(11) 0.0132(10) 0.0208(12) -0.0023(8) 0.0074(10) -0.0033(8) C3 0.0210(12) 0.0185(12) 0.0222(13) -0.0025(10) 0.0033(10) 0.0026(10) C4 0.0265(13) 0.0306(14) 0.0198(13) -0.0022(11) -0.0012(11) 0.0003(11) C5 0.0342(15) 0.0362(15) 0.0176(14) 0.0023(12) -0.0006(12) 0.0030(13) C6 0.0273(15) 0.0301(14) 0.0225(15) 0.0052(11) 0.0048(12) -0.0009(11) C7 0.0179(12) 0.0176(11) 0.0198(13) -0.0001(10) 0.0053(10) 0.0043(10) C8 0.0196(11) 0.0182(11) 0.0182(12) -0.0021(9) -0.0013(9) 0.0030(9) N9 0.0213(10) 0.0170(10) 0.0199(11) -0.0012(8) 0.0004(9) 0.0024(8) C10 0.0244(12) 0.0199(11) 0.0198(13) 0.0026(10) 0.0022(10) 0.0027(10) C11 0.0244(13) 0.0220(13) 0.0246(14) -0.0021(10) 0.0056(11) 0.0002(11) C12 0.0203(12) 0.0253(14) 0.0290(15) -0.0057(12) -0.0020(11) -0.0024(11) C13 0.0206(12) 0.0254(13) 0.0210(13) -0.0040(10) -0.0028(10) -0.0012(10) C14 0.0190(11) 0.0180(11) 0.0271(14) 0.0038(10) 0.0028(10) 0.0034(9) N15 0.0248(11) 0.0150(10) 0.0249(12) 0.0009(9) 0.0013(9) 0.0055(9) C16 0.0283(13) 0.0185(12) 0.0320(15) -0.0028(11) -0.0052(12) 0.0053(11) C17 0.0277(15) 0.0212(14) 0.052(2) -0.0069(13) -0.0089(14) 0.0017(11) C18 0.0188(13) 0.0266(15) 0.060(2) 0.0060(15) 0.0005(14) -0.0027(12) C19 0.0217(12) 0.0278(14) 0.0370(17) 0.0085(12) 0.0067(12) 0.0003(11) N20 0.0115(10) 0.0171(10) 0.0178(12) -0.0030(8) 0.0009(9) -0.0020(8) C21 0.0163(12) 0.0211(13) 0.0233(14) -0.0012(10) -0.0004(10) -0.0004(9) C22 0.0270(14) 0.0303(15) 0.0221(15) -0.0063(11) 0.0037(12) -0.0005(12) C23 0.0340(15) 0.0341(15) 0.0211(14) 0.0001(12) 0.0002(12) -0.0039(13) C24 0.0259(13) 0.0279(14) 0.0221(14) 0.0036(11) -0.0015(11) -0.0029(11) C25 0.0160(11) 0.0193(11) 0.0230(13) 0.0015(10) -0.0026(10) -0.0023(9) C26 0.0146(10) 0.0203(12) 0.0232(13) -0.0023(10) 0.0007(9) 0.0027(9) N27 0.0176(9) 0.0231(11) 0.0221(11) -0.0014(9) -0.0020(8) -0.0035(9) C28 0.0229(13) 0.0329(15) 0.0313(16) 0.0068(12) -0.0025(12) -0.0050(11) C29 0.0266(14) 0.0248(14) 0.0459(19) 0.0103(14) -0.0107(13) 0.0004(12) C30 0.0274(15) 0.0227(14) 0.054(2) -0.0051(14) -0.0028(14) 0.0097(12) C31 0.0255(13) 0.0253(14) 0.0344(16) -0.0090(12) 0.0011(12) 0.0039(11) C32 0.0160(10) 0.0182(11) 0.0215(13) 0.0025(10) -0.0037(9) -0.0011(9) N33 0.0167(9) 0.0201(10) 0.0238(12) 0.0015(9) -0.0006(8) -0.0025(8) C34 0.0180(12) 0.0267(13) 0.0227(13) -0.0005(10) 0.0004(10) -0.0046(10) C35 0.0227(13) 0.0237(14) 0.0357(17) -0.0079(12) 0.0050(11) 0.0006(11) C36 0.0264(14) 0.0191(13) 0.0408(18) 0.0021(12) 0.0020(13) 0.0020(11) C37 0.0225(12) 0.0223(13) 0.0313(15) 0.0060(11) -0.0012(11) -0.0004(10) B38 0.0343(17) 0.0289(16) 0.0243(17) 0.0000(13) 0.0040(13) -0.0036(14) F39 0.0571(12) 0.0447(11) 0.0217(9) -0.0093(8) 0.0069(8) -0.0123(10) F40 0.0689(14) 0.0429(11) 0.0348(11) 0.0119(9) 0.0188(10) 0.0195(10) F41 0.0389(10) 0.0403(10) 0.0244(9) -0.0002(7) 0.0086(7) -0.0025(8) F42 0.0359(10) 0.0487(12) 0.0315(10) 0.0050(9) -0.0018(8) -0.0156(9) B43 0.0286(17) 0.056(2) 0.0302(19) -0.0093(18) -0.0040(15) -0.0012(17) F44 0.0420(11) 0.0725(15) 0.0359(12) -0.0045(10) 0.0069(9) -0.0075(11) F45 0.0401(11) 0.0881(17) 0.0323(11) -0.0074(11) 0.0053(9) 0.0232(12) F46 0.0367(10) 0.0906(18) 0.0444(13) -0.0326(12) -0.0072(9) 0.0215(11) F47 0.085(2) 0.0521(15) 0.107(2) 0.0309(15) -0.0557(18) -0.0255(14) _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 1.906(3) . ? Co1 N20 1.912(2) . ? Co1 N15 2.084(2) . ? Co1 N27 2.088(2) . ? Co1 N9 2.088(2) . ? Co1 N33 2.107(2) . ? N2 C7 1.355(3) . ? N2 C3 1.375(4) . ? C3 C4 1.404(4) . ? C3 C8 1.476(4) . ? C4 C5 1.395(4) . ? C5 C6 1.400(4) . ? C6 C7 1.403(4) . ? C7 C14 1.467(4) . ? C8 N9 1.367(3) . ? C8 C13 1.400(3) . ? N9 C10 1.345(3) . ? C10 C11 1.401(4) . ? C11 C12 1.383(4) . ? C12 C13 1.393(4) . ? C14 N15 1.358(4) . ? C14 C19 1.398(4) . ? N15 C16 1.350(4) . ? C16 C17 1.392(5) . ? C17 C18 1.379(5) . ? C18 C19 1.406(5) . ? N20 C21 1.363(3) . ? N20 C25 1.367(3) . ? C21 C22 1.402(4) . ? C21 C26 1.478(4) . ? C22 C23 1.389(5) . ? C23 C24 1.398(4) . ? C24 C25 1.397(4) . ? C25 C32 1.479(4) . ? C26 N27 1.366(3) . ? C26 C31 1.385(4) . ? N27 C28 1.341(4) . ? C28 C29 1.396(5) . ? C29 C30 1.383(5) . ? C30 C31 1.395(5) . ? C32 N33 1.363(3) . ? C32 C37 1.400(4) . ? N33 C34 1.344(4) . ? C34 C35 1.399(4) . ? C35 C36 1.384(5) . ? C36 C37 1.397(4) . ? B38 F41 1.395(4) . ? B38 F39 1.396(4) . ? B38 F42 1.404(4) . ? B38 F40 1.405(4) . ? F44 B43 1.398(5) . ? B43 F47 1.377(5) . ? B43 F45 1.387(5) . ? B43 F46 1.399(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N20 178.35(12) . . ? N2 Co1 N15 79.44(10) . . ? N20 Co1 N15 102.13(9) . . ? N2 Co1 N27 99.87(9) . . ? N20 Co1 N27 79.65(9) . . ? N15 Co1 N27 90.63(8) . . ? N2 Co1 N9 79.95(10) . . ? N20 Co1 N9 98.47(9) . . ? N15 Co1 N9 159.39(9) . . ? N27 Co1 N9 92.31(8) . . ? N2 Co1 N33 101.03(9) . . ? N20 Co1 N33 79.53(9) . . ? N15 Co1 N33 90.67(8) . . ? N27 Co1 N33 158.94(9) . . ? N9 Co1 N33 93.83(8) . . ? C7 N2 C3 120.2(3) . . ? C7 N2 Co1 120.2(2) . . ? C3 N2 Co1 119.55(19) . . ? N2 C3 C4 120.9(2) . . ? N2 C3 C8 113.2(2) . . ? C4 C3 C8 125.9(2) . . ? C5 C4 C3 118.5(3) . . ? C4 C5 C6 120.5(3) . . ? C5 C6 C7 118.6(3) . . ? N2 C7 C6 121.3(3) . . ? N2 C7 C14 112.9(2) . . ? C6 C7 C14 125.8(2) . . ? N9 C8 C13 121.9(2) . . ? N9 C8 C3 113.8(2) . . ? C13 C8 C3 124.4(2) . . ? C10 N9 C8 118.7(2) . . ? C10 N9 Co1 127.88(18) . . ? C8 N9 Co1 113.26(17) . . ? N9 C10 C11 122.1(3) . . ? C12 C11 C10 119.1(3) . . ? C11 C12 C13 119.6(3) . . ? C12 C13 C8 118.6(3) . . ? N15 C14 C19 122.1(3) . . ? N15 C14 C7 114.3(2) . . ? C19 C14 C7 123.6(3) . . ? C16 N15 C14 118.9(3) . . ? C16 N15 Co1 128.1(2) . . ? C14 N15 Co1 112.98(18) . . ? N15 C16 C17 122.3(3) . . ? C18 C17 C16 118.6(3) . . ? C17 C18 C19 120.3(3) . . ? C14 C19 C18 117.6(3) . . ? C21 N20 C25 119.7(3) . . ? C21 N20 Co1 120.07(19) . . ? C25 N20 Co1 120.10(19) . . ? N20 C21 C22 121.2(3) . . ? N20 C21 C26 112.8(2) . . ? C22 C21 C26 126.1(2) . . ? C23 C22 C21 119.0(3) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 118.9(3) . . ? N20 C25 C24 121.2(3) . . ? N20 C25 C32 112.8(2) . . ? C24 C25 C32 126.0(2) . . ? N27 C26 C31 123.0(3) . . ? N27 C26 C21 114.1(2) . . ? C31 C26 C21 122.9(3) . . ? C28 N27 C26 118.2(2) . . ? C28 N27 Co1 128.6(2) . . ? C26 N27 Co1 113.21(17) . . ? N27 C28 C29 122.3(3) . . ? C30 C29 C28 118.7(3) . . ? C29 C30 C31 120.0(3) . . ? C26 C31 C30 117.7(3) . . ? N33 C32 C37 122.4(3) . . ? N33 C32 C25 114.5(2) . . ? C37 C32 C25 123.0(2) . . ? C34 N33 C32 118.2(2) . . ? C34 N33 Co1 129.12(18) . . ? C32 N33 Co1 112.73(17) . . ? N33 C34 C35 122.6(3) . . ? C36 C35 C34 119.1(3) . . ? C35 C36 C37 119.3(3) . . ? C36 C37 C32 118.4(3) . . ? F41 B38 F39 109.7(3) . . ? F41 B38 F42 107.9(3) . . ? F39 B38 F42 109.3(3) . . ? F41 B38 F40 110.4(3) . . ? F39 B38 F40 109.9(3) . . ? F42 B38 F40 109.7(3) . . ? F47 B43 F45 110.0(4) . . ? F47 B43 F44 108.9(3) . . ? F45 B43 F44 107.8(3) . . ? F47 B43 F46 110.7(4) . . ? F45 B43 F46 110.0(3) . . ? F44 B43 F46 109.3(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.627 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.066 #=END data_mh32530 _database_code_depnum_ccdc_archive 'CCDC 781743' #TrackingRef '- Co Dalton revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)cobalt(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Co N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Co F8 N6' _chemical_formula_weight 699.09 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.580(3) _cell_length_b 12.365(3) _cell_length_c 18.801(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.988(7) _cell_angle_gamma 90.00 _cell_volume 2896.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 15884 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.67 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.082 _exptl_absorpt_correction_T_max 1.195 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 30(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15884 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.67 _reflns_number_total 5543 _reflns_number_gt 5047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0195P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(10) _refine_ls_number_reflns 5543 _refine_ls_number_parameters 425 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24981(2) 0.29018(3) 0.25055(2) 0.01380(8) Uani 1 1 d . . . N2 N 0.25897(19) 0.27883(17) 0.35238(13) 0.0132(5) Uani 1 1 d . . . C3 C 0.3523(2) 0.3045(2) 0.39411(15) 0.0141(5) Uani 1 1 d . . . C4 C 0.3624(2) 0.2922(2) 0.46846(14) 0.0152(6) Uani 1 1 d . . . H4 H 0.4275 0.3106 0.4979 0.018 Uiso 1 1 calc R . . C5 C 0.2755(2) 0.2524(2) 0.49866(15) 0.0171(6) Uani 1 1 d . . . H5 H 0.2814 0.2434 0.5492 0.021 Uiso 1 1 calc R . . C6 C 0.1801(2) 0.2258(2) 0.45577(15) 0.0158(6) Uani 1 1 d . . . H6 H 0.1205 0.1986 0.4763 0.019 Uiso 1 1 calc R . . C7 C 0.1742(2) 0.2402(2) 0.38139(15) 0.0141(5) Uani 1 1 d . . . C8 C 0.4366(2) 0.3441(2) 0.35261(14) 0.0130(5) Uani 1 1 d . . . N9 N 0.40290(17) 0.34981(17) 0.28038(12) 0.0144(5) Uani 1 1 d . . . C10 C 0.4724(2) 0.3866(2) 0.23751(15) 0.0162(6) Uani 1 1 d . . . H10 H 0.4492 0.3920 0.1874 0.019 Uiso 1 1 calc R . . C11 C 0.5775(2) 0.4172(2) 0.26421(15) 0.0165(6) Uani 1 1 d . . . H11 H 0.6249 0.4426 0.2327 0.020 Uiso 1 1 calc R . . C12 C 0.6113(2) 0.4100(2) 0.33738(15) 0.0163(6) Uani 1 1 d . . . H12 H 0.6823 0.4304 0.3567 0.020 Uiso 1 1 calc R . . C13 C 0.5402(2) 0.3725(2) 0.38245(15) 0.0158(6) Uani 1 1 d . . . H13 H 0.5621 0.3666 0.4327 0.019 Uiso 1 1 calc R . . C14 C 0.0808(2) 0.2137(2) 0.32725(14) 0.0132(5) Uani 1 1 d . . . N15 N 0.10067(18) 0.22495(17) 0.25826(12) 0.0164(5) Uani 1 1 d . . . C16 C 0.0232(2) 0.1957(2) 0.20507(16) 0.0194(6) Uani 1 1 d . . . H16 H 0.0377 0.2006 0.1569 0.023 Uiso 1 1 calc R . . C17 C -0.0767(2) 0.1588(2) 0.21725(16) 0.0204(6) Uani 1 1 d . . . H17 H -0.1295 0.1388 0.1783 0.024 Uiso 1 1 calc R . . C18 C -0.0981(2) 0.1515(2) 0.28821(17) 0.0225(7) Uani 1 1 d . . . H18 H -0.1665 0.1285 0.2982 0.027 Uiso 1 1 calc R . . C19 C -0.0177(2) 0.1786(2) 0.34397(15) 0.0181(6) Uani 1 1 d . . . H19 H -0.0299 0.1732 0.3926 0.022 Uiso 1 1 calc R . . N20 N 0.24536(19) 0.30198(18) 0.14810(13) 0.0142(5) Uani 1 1 d . . . C21 C 0.2810(2) 0.2176(2) 0.11091(15) 0.0144(6) Uani 1 1 d . . . C22 C 0.2866(2) 0.2268(2) 0.03741(15) 0.0155(6) Uani 1 1 d . . . H22 H 0.3115 0.1681 0.0116 0.019 Uiso 1 1 calc R . . C23 C 0.2553(2) 0.3233(2) 0.00282(15) 0.0183(6) Uani 1 1 d . . . H23 H 0.2587 0.3310 -0.0471 0.022 Uiso 1 1 calc R . . C24 C 0.2189(2) 0.4086(2) 0.04134(14) 0.0156(6) Uani 1 1 d . . . H24 H 0.1977 0.4750 0.0181 0.019 Uiso 1 1 calc R . . C25 C 0.2138(2) 0.3955(2) 0.11399(14) 0.0137(5) Uani 1 1 d . . . C26 C 0.3109(2) 0.1209(2) 0.15554(14) 0.0132(5) Uani 1 1 d . . . N27 N 0.30827(17) 0.13647(18) 0.22693(12) 0.0158(5) Uani 1 1 d . . . C28 C 0.3362(2) 0.0538(2) 0.27224(15) 0.0196(6) Uani 1 1 d . . . H28 H 0.3340 0.0640 0.3221 0.024 Uiso 1 1 calc R . . C29 C 0.3684(2) -0.0470(2) 0.24818(17) 0.0233(6) Uani 1 1 d . . . H29 H 0.3887 -0.1040 0.2812 0.028 Uiso 1 1 calc R . . C30 C 0.3699(2) -0.0615(2) 0.17525(17) 0.0222(7) Uani 1 1 d . . . H30 H 0.3913 -0.1290 0.1577 0.027 Uiso 1 1 calc R . . C31 C 0.3400(2) 0.0227(2) 0.12793(15) 0.0169(6) Uani 1 1 d . . . H31 H 0.3394 0.0134 0.0777 0.020 Uiso 1 1 calc R . . C32 C 0.1749(2) 0.4772(2) 0.16191(14) 0.0149(5) Uani 1 1 d . . . N33 N 0.18005(17) 0.44650(18) 0.23177(12) 0.0147(5) Uani 1 1 d . . . C34 C 0.1413(2) 0.5139(2) 0.27819(15) 0.0171(6) Uani 1 1 d . . . H34 H 0.1426 0.4915 0.3266 0.021 Uiso 1 1 calc R . . C35 C 0.0993(2) 0.6159(2) 0.25779(16) 0.0178(6) Uani 1 1 d . . . H35 H 0.0727 0.6618 0.2918 0.021 Uiso 1 1 calc R . . C36 C 0.0973(2) 0.6487(2) 0.18712(15) 0.0177(6) Uani 1 1 d . . . H36 H 0.0716 0.7185 0.1724 0.021 Uiso 1 1 calc R . . C37 C 0.1333(2) 0.5779(2) 0.13792(15) 0.0166(6) Uani 1 1 d . . . H37 H 0.1297 0.5977 0.0888 0.020 Uiso 1 1 calc R . . B38 B 0.0201(3) -0.0190(3) 0.05603(18) 0.0185(7) Uani 1 1 d . . . F39 F -0.01912(13) -0.05035(13) -0.01444(8) 0.0207(4) Uani 1 1 d . . . F40 F 0.07488(14) -0.10632(13) 0.09253(9) 0.0230(4) Uani 1 1 d . . . F41 F -0.06605(12) 0.01265(12) 0.09146(8) 0.0190(4) Uani 1 1 d . . . F42 F 0.09001(13) 0.06935(12) 0.05451(9) 0.0198(4) Uani 1 1 d . . . B43 B -0.0297(3) 0.4825(3) -0.04321(19) 0.0180(7) Uani 1 1 d . A 1 F44 F -0.01996(12) 0.42886(13) 0.02311(8) 0.0208(4) Uani 1 1 d . . . F45 F 0.00570(13) 0.41406(13) -0.09446(9) 0.0237(4) Uani 1 1 d . A 1 F46 F -0.13818(13) 0.51032(13) -0.06389(9) 0.0240(4) Uani 1 1 d . A 1 F47 F 0.03271(14) 0.57724(14) -0.03713(10) 0.0318(4) Uani 1 1 d . A 1 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 0.01206(16) 0.01229(15) 0.01709(17) -0.00140(17) 0.00217(13) -0.00011(16) N2 0.0129(12) 0.0103(11) 0.0166(13) -0.0015(9) 0.0021(11) -0.0008(9) C3 0.0145(13) 0.0110(12) 0.0161(13) -0.0018(11) 0.0001(11) 0.0026(11) C4 0.0156(14) 0.0148(13) 0.0141(13) -0.0013(11) -0.0020(11) 0.0021(11) C5 0.0205(14) 0.0179(13) 0.0129(14) 0.0010(12) 0.0020(12) 0.0014(12) C6 0.0157(14) 0.0150(13) 0.0164(14) -0.0007(11) 0.0015(12) 0.0006(10) C7 0.0152(14) 0.0116(12) 0.0155(13) -0.0031(11) 0.0021(11) 0.0007(11) C8 0.0142(13) 0.0110(12) 0.0127(13) -0.0013(10) -0.0020(10) 0.0034(10) N9 0.0141(11) 0.0140(11) 0.0142(11) -0.0023(10) -0.0006(9) 0.0019(9) C10 0.0199(14) 0.0127(12) 0.0151(13) 0.0013(11) -0.0009(12) 0.0028(11) C11 0.0178(14) 0.0132(13) 0.0188(14) 0.0002(11) 0.0039(12) 0.0004(11) C12 0.0180(14) 0.0144(13) 0.0156(14) -0.0017(11) -0.0005(11) -0.0009(11) C13 0.0171(14) 0.0143(13) 0.0154(14) 0.0003(11) 0.0004(11) 0.0016(11) C14 0.0152(13) 0.0097(12) 0.0143(13) 0.0000(10) 0.0005(11) 0.0011(10) N15 0.0217(13) 0.0129(11) 0.0147(12) -0.0011(10) 0.0026(10) 0.0024(9) C16 0.0263(15) 0.0143(13) 0.0161(14) -0.0004(11) -0.0023(12) 0.0059(12) C17 0.0208(15) 0.0137(13) 0.0229(16) -0.0020(12) -0.0102(13) 0.0023(11) C18 0.0156(14) 0.0151(14) 0.0350(19) 0.0032(13) -0.0027(14) -0.0030(12) C19 0.0151(14) 0.0185(13) 0.0202(15) 0.0065(12) 0.0004(12) 0.0015(11) N20 0.0120(12) 0.0143(11) 0.0155(13) -0.0009(10) -0.0010(10) -0.0020(9) C21 0.0112(13) 0.0135(13) 0.0178(14) -0.0027(11) -0.0002(11) -0.0010(10) C22 0.0152(14) 0.0172(14) 0.0133(14) -0.0010(11) -0.0003(11) 0.0012(11) C23 0.0184(15) 0.0219(14) 0.0145(14) 0.0009(12) 0.0026(12) -0.0041(12) C24 0.0145(13) 0.0137(13) 0.0177(14) 0.0066(11) -0.0005(11) -0.0001(11) C25 0.0100(12) 0.0127(12) 0.0178(14) 0.0000(11) -0.0003(11) -0.0014(10) C26 0.0096(12) 0.0172(13) 0.0129(13) -0.0005(11) 0.0019(10) -0.0001(10) N27 0.0133(11) 0.0175(11) 0.0165(12) -0.0029(10) 0.0024(10) -0.0023(9) C28 0.0174(14) 0.0251(15) 0.0146(14) 0.0056(12) -0.0043(12) -0.0062(12) C29 0.0192(15) 0.0202(15) 0.0278(17) 0.0086(13) -0.0063(13) -0.0030(12) C30 0.0145(14) 0.0173(14) 0.0336(18) -0.0030(14) -0.0012(13) 0.0002(12) C31 0.0148(13) 0.0175(14) 0.0179(14) -0.0016(12) 0.0002(11) 0.0020(11) C32 0.0127(13) 0.0158(13) 0.0153(13) -0.0014(11) -0.0016(11) -0.0029(10) N33 0.0133(11) 0.0160(11) 0.0145(12) 0.0030(9) 0.0005(9) -0.0008(9) C34 0.0126(13) 0.0222(14) 0.0155(14) -0.0004(12) -0.0017(11) -0.0043(11) C35 0.0158(14) 0.0184(14) 0.0187(15) -0.0029(12) 0.0014(11) -0.0028(11) C36 0.0162(14) 0.0146(13) 0.0217(16) -0.0001(12) 0.0008(12) -0.0021(11) C37 0.0160(14) 0.0160(13) 0.0171(14) 0.0042(12) -0.0003(12) -0.0019(11) B38 0.0197(16) 0.0180(16) 0.0174(17) -0.0003(13) 0.0013(14) -0.0037(13) F39 0.0259(9) 0.0200(8) 0.0160(8) -0.0041(7) 0.0019(7) -0.0036(7) F40 0.0300(9) 0.0196(8) 0.0197(8) 0.0055(7) 0.0050(7) 0.0056(7) F41 0.0189(8) 0.0217(8) 0.0171(8) -0.0010(7) 0.0044(7) -0.0001(7) F42 0.0196(8) 0.0214(8) 0.0176(8) 0.0012(7) -0.0005(7) -0.0053(7) B43 0.0130(15) 0.0178(16) 0.0231(17) -0.0038(14) 0.0020(14) -0.0017(13) F44 0.0194(8) 0.0261(9) 0.0170(9) 0.0004(7) 0.0026(7) -0.0006(7) F45 0.0209(9) 0.0315(9) 0.0187(9) -0.0022(8) 0.0032(7) 0.0076(8) F46 0.0189(8) 0.0314(10) 0.0201(9) -0.0080(8) -0.0027(7) 0.0056(7) F47 0.0339(10) 0.0223(9) 0.0349(11) 0.0073(8) -0.0101(9) -0.0076(8) _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 1.907(3) . ? Co1 N20 1.925(2) . ? Co1 N9 2.066(2) . ? Co1 N15 2.066(2) . ? Co1 N27 2.107(2) . ? Co1 N33 2.132(2) . ? N2 C7 1.351(3) . ? N2 C3 1.356(4) . ? C3 C4 1.394(4) . ? C3 C8 1.484(4) . ? C4 C5 1.390(4) . ? C5 C6 1.390(4) . ? C6 C7 1.402(4) . ? C7 C14 1.481(4) . ? C8 N9 1.367(3) . ? C8 C13 1.390(4) . ? N9 C10 1.348(3) . ? C10 C11 1.400(4) . ? C11 C12 1.385(4) . ? C12 C13 1.394(4) . ? C14 N15 1.362(3) . ? C14 C19 1.389(4) . ? N15 C16 1.345(4) . ? C16 C17 1.386(4) . ? C17 C18 1.400(4) . ? C18 C19 1.393(4) . ? N20 C25 1.355(3) . ? N20 C21 1.366(3) . ? C21 C22 1.398(4) . ? C21 C26 1.479(4) . ? C22 C23 1.389(4) . ? C23 C24 1.393(4) . ? C24 C25 1.386(4) . ? C25 C32 1.482(4) . ? C26 N27 1.361(3) . ? C26 C31 1.390(4) . ? N27 C28 1.345(3) . ? C28 C29 1.405(4) . ? C29 C30 1.386(4) . ? C30 C31 1.387(4) . ? C32 N33 1.360(3) . ? C32 C37 1.400(4) . ? N33 C34 1.346(3) . ? C34 C35 1.400(4) . ? C35 C36 1.386(4) . ? C36 C37 1.394(4) . ? B38 F39 1.403(4) . ? B38 F41 1.404(4) . ? B38 F42 1.406(3) . ? B38 F40 1.407(4) . ? F44 B43 1.403(4) . ? B43 F45 1.401(4) . ? B43 F47 1.406(4) . ? B43 F46 1.408(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N20 178.22(12) . . ? N2 Co1 N9 80.19(9) . . ? N20 Co1 N9 98.11(9) . . ? N2 Co1 N15 80.19(10) . . ? N20 Co1 N15 101.51(9) . . ? N9 Co1 N15 160.37(9) . . ? N2 Co1 N27 99.85(9) . . ? N20 Co1 N27 79.63(9) . . ? N9 Co1 N27 92.27(9) . . ? N15 Co1 N27 90.55(9) . . ? N2 Co1 N33 101.48(9) . . ? N20 Co1 N33 79.13(9) . . ? N9 Co1 N33 93.91(9) . . ? N15 Co1 N33 90.50(9) . . ? N27 Co1 N33 158.51(9) . . ? C7 N2 C3 121.2(3) . . ? C7 N2 Co1 119.4(2) . . ? C3 N2 Co1 119.36(19) . . ? N2 C3 C4 120.4(2) . . ? N2 C3 C8 113.4(2) . . ? C4 C3 C8 126.2(2) . . ? C5 C4 C3 118.7(3) . . ? C4 C5 C6 120.8(3) . . ? C5 C6 C7 118.0(3) . . ? N2 C7 C6 120.9(3) . . ? N2 C7 C14 113.3(2) . . ? C6 C7 C14 125.8(2) . . ? N9 C8 C13 122.1(2) . . ? N9 C8 C3 113.2(2) . . ? C13 C8 C3 124.7(2) . . ? C10 N9 C8 118.3(2) . . ? C10 N9 Co1 128.00(19) . . ? C8 N9 Co1 113.58(17) . . ? N9 C10 C11 122.4(3) . . ? C12 C11 C10 118.9(3) . . ? C11 C12 C13 119.4(3) . . ? C8 C13 C12 118.9(3) . . ? N15 C14 C19 122.3(3) . . ? N15 C14 C7 113.5(2) . . ? C19 C14 C7 124.1(2) . . ? C16 N15 C14 118.1(2) . . ? C16 N15 Co1 128.58(19) . . ? C14 N15 Co1 113.29(18) . . ? N15 C16 C17 123.1(3) . . ? C16 C17 C18 118.5(3) . . ? C19 C18 C17 119.1(3) . . ? C14 C19 C18 118.8(3) . . ? C25 N20 C21 120.3(2) . . ? C25 N20 Co1 120.29(18) . . ? C21 N20 Co1 119.23(19) . . ? N20 C21 C22 120.6(3) . . ? N20 C21 C26 113.8(2) . . ? C22 C21 C26 125.6(2) . . ? C23 C22 C21 118.8(3) . . ? C22 C23 C24 120.0(3) . . ? C25 C24 C23 119.2(2) . . ? N20 C25 C24 121.1(2) . . ? N20 C25 C32 113.2(2) . . ? C24 C25 C32 125.7(2) . . ? N27 C26 C31 122.4(2) . . ? N27 C26 C21 113.9(2) . . ? C31 C26 C21 123.6(2) . . ? C28 N27 C26 118.5(2) . . ? C28 N27 Co1 128.29(19) . . ? C26 N27 Co1 113.13(17) . . ? N27 C28 C29 122.1(3) . . ? C30 C29 C28 118.5(3) . . ? C29 C30 C31 119.9(3) . . ? C30 C31 C26 118.6(3) . . ? N33 C32 C37 121.7(2) . . ? N33 C32 C25 114.9(2) . . ? C37 C32 C25 123.4(2) . . ? C34 N33 C32 118.7(2) . . ? C34 N33 Co1 129.19(18) . . ? C32 N33 Co1 112.12(17) . . ? N33 C34 C35 122.5(2) . . ? C36 C35 C34 118.8(3) . . ? C35 C36 C37 119.2(3) . . ? C36 C37 C32 119.1(3) . . ? F39 B38 F41 109.4(2) . . ? F39 B38 F42 109.5(2) . . ? F41 B38 F42 108.6(2) . . ? F39 B38 F40 109.4(2) . . ? F41 B38 F40 109.9(2) . . ? F42 B38 F40 109.9(2) . . ? F45 B43 F44 109.2(2) . . ? F45 B43 F47 109.4(2) . . ? F44 B43 F47 110.0(3) . . ? F45 B43 F46 110.3(3) . . ? F44 B43 F46 108.8(2) . . ? F47 B43 F46 109.2(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.381 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.059