data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(PY5Me2)Co(NCCH3)](OTf)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H34 Co F6 N8 O6 S2' _chemical_formula_weight 923.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 P_21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5624(12) _cell_length_b 15.9060(15) _cell_length_c 20.257(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.067(2) _cell_angle_gamma 90.00 _cell_volume 4047.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9315 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6351 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52504 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.34 _reflns_number_total 7392 _reflns_number_gt 6250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0811P)^2^+9.8913P] 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_number_reflns 7392 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.83143(3) 0.09851(3) 0.33955(2) 0.02125(15) Uani 1 1 d . . . S1 S 0.75247(7) 0.08748(6) 0.05108(4) 0.0308(2) Uani 1 1 d . . . S003 S 0.29533(9) 0.07670(8) 0.31724(6) 0.0486(3) Uani 1 1 d . . . C1 C 0.9920(3) 0.0795(3) 0.21593(19) 0.0375(9) Uani 1 1 d . . . O6 O 0.2417(3) 0.0975(5) 0.3757(3) 0.129(2) Uani 1 1 d . . . C3 C 0.7139(3) -0.0094(2) 0.23880(17) 0.0329(8) Uani 1 1 d . . . H006 H 0.7464 0.0274 0.2097 0.039 Uiso 1 1 calc R . . O2 O 0.7049(3) 0.16868(18) 0.05886(16) 0.0511(8) Uani 1 1 d . . . F1 F 0.9221(3) 0.1654(4) 0.0125(3) 0.153(2) Uani 1 1 d . . . N6 N 0.7283(2) 0.10221(16) 0.41961(13) 0.0216(6) Uani 1 1 d . . . O1 O 0.8149(3) 0.0563(2) 0.10592(14) 0.0539(8) Uani 1 1 d . . . N2 N 0.7381(2) 0.19739(17) 0.29600(13) 0.0261(6) Uani 1 1 d . . . N4 N 0.9131(2) -0.00020(17) 0.39160(13) 0.0242(6) Uani 1 1 d . . . O3 O 0.6836(3) 0.0270(2) 0.0211(2) 0.0755(12) Uani 1 1 d . . . C30 C 0.7337(3) -0.0544(2) 0.41844(16) 0.0243(7) Uani 1 1 d . . . N3 N 0.9119(2) 0.20425(17) 0.38069(13) 0.0251(6) Uani 1 1 d . . . C22 C 0.8570(3) -0.0615(2) 0.42124(15) 0.0236(7) Uani 1 1 d . . . C2 C 1.0614(4) 0.0633(4) 0.1609(2) 0.0598(13) Uani 1 1 d . . . H01A H 1.1343 0.0680 0.1754 0.090 Uiso 1 1 calc R . . H01B H 1.0473 0.1036 0.1265 0.090 Uiso 1 1 calc R . . H01C H 1.0485 0.0076 0.1443 0.090 Uiso 1 1 calc R . . C11 C 0.6250(3) 0.3154(2) 0.30986(19) 0.0342(8) Uani 1 1 d . . . H18 H 0.5952 0.3553 0.3376 0.041 Uiso 1 1 calc R . . C23 C 0.6999(2) 0.0298(2) 0.44979(16) 0.0229(7) Uani 1 1 d . . . N1 N 0.7395(2) -0.00350(17) 0.30340(13) 0.0255(6) Uani 1 1 d . . . C7 C 0.6962(3) -0.0589(2) 0.34550(17) 0.0257(7) Uani 1 1 d . . . N5 N 0.9372(3) 0.09043(19) 0.25930(15) 0.0314(7) Uani 1 1 d . . . C33 C 0.8527(5) 0.1060(5) -0.0107(3) 0.083(2) Uani 1 1 d . . . C16 C 0.9085(3) 0.3326(2) 0.44080(17) 0.0307(8) Uani 1 1 d . . . H025 H 0.8695 0.3743 0.4617 0.037 Uiso 1 1 calc R . . C18 C 1.0193(3) -0.0062(2) 0.39230(18) 0.0312(8) Uani 1 1 d . . . H026 H 1.0579 0.0363 0.3722 0.037 Uiso 1 1 calc R . . C17 C 0.8566(3) 0.2652(2) 0.41072(15) 0.0254(7) Uani 1 1 d . . . C28 C 0.7337(3) 0.2579(2) 0.40903(16) 0.0266(7) Uani 1 1 d . . . C31 C 0.6858(3) -0.1282(2) 0.45694(19) 0.0341(8) Uani 1 1 d . . . H02A H 0.6098 -0.1225 0.4575 0.051 Uiso 1 1 calc R . . H02B H 0.7136 -0.1279 0.5014 0.051 Uiso 1 1 calc R . . H02C H 0.7042 -0.1802 0.4360 0.051 Uiso 1 1 calc R . . C26 C 0.6465(3) 0.1810(2) 0.50501(17) 0.0307(8) Uani 1 1 d . . . H030 H 0.6285 0.2327 0.5230 0.037 Uiso 1 1 calc R . . C21 C 0.9083(3) -0.1289(2) 0.45181(17) 0.0306(8) Uani 1 1 d . . . H031 H 0.8687 -0.1704 0.4725 0.037 Uiso 1 1 calc R . . F5 F 0.4718(3) 0.1043(4) 0.3846(2) 0.143(2) Uani 1 1 d . . . C6 C 0.6232(3) -0.1184(2) 0.3228(2) 0.0356(8) Uani 1 1 d . . . H033 H 0.5930 -0.1559 0.3522 0.043 Uiso 1 1 calc R . . C14 C 1.0743(3) 0.2766(2) 0.40669(19) 0.0369(9) Uani 1 1 d . . . H034 H 1.1481 0.2791 0.4042 0.044 Uiso 1 1 calc R . . C27 C 0.7007(3) 0.1769(2) 0.44574(16) 0.0240(7) Uani 1 1 d . . . C9 C 0.6457(3) 0.2572(2) 0.20266(19) 0.0360(8) Uani 1 1 d . . . H036 H 0.6310 0.2564 0.1575 0.043 Uiso 1 1 calc R . . C25 C 0.6199(3) 0.1074(2) 0.53673(17) 0.0318(8) Uani 1 1 d . . . H037 H 0.5855 0.1093 0.5770 0.038 Uiso 1 1 calc R . . C20 C 1.0179(3) -0.1343(2) 0.45150(18) 0.0352(8) Uani 1 1 d . . . H038 H 1.0526 -0.1796 0.4715 0.042 Uiso 1 1 calc R . . F2 F 0.9072(4) 0.0389(4) -0.02239(17) 0.150(3) Uani 1 1 d . . . O4 O 0.3213(6) -0.0080(3) 0.3247(4) 0.160(3) Uani 1 1 d . . . F3 F 0.8079(4) 0.1301(4) -0.06665(19) 0.162(3) Uani 1 1 d . . . C15 C 1.0188(3) 0.3374(2) 0.43946(19) 0.0367(9) Uani 1 1 d . . . H042 H 1.0545 0.3814 0.4605 0.044 Uiso 1 1 calc R . . C4 C 0.6426(3) -0.0667(3) 0.21347(19) 0.0391(9) Uani 1 1 d . . . H043 H 0.6266 -0.0685 0.1685 0.047 Uiso 1 1 calc R . . C24 C 0.6446(3) 0.0310(2) 0.50842(17) 0.0285(7) Uani 1 1 d . . . H044 H 0.6243 -0.0190 0.5284 0.034 Uiso 1 1 calc R . . C13 C 1.0183(3) 0.2117(2) 0.37758(18) 0.0317(8) Uani 1 1 d . . . H045 H 1.0559 0.1710 0.3546 0.038 Uiso 1 1 calc R . . F4 F 0.4835(4) 0.1250(4) 0.2826(2) 0.150(2) Uani 1 1 d . . . C5 C 0.5955(3) -0.1217(3) 0.2565(2) 0.0437(10) Uani 1 1 d . . . H047 H 0.5456 -0.1606 0.2411 0.052 Uiso 1 1 calc R . . C10 C 0.5991(3) 0.3155(2) 0.2430(2) 0.0382(9) Uani 1 1 d . . . H048 H 0.5508 0.3544 0.2258 0.046 Uiso 1 1 calc R . . C19 C 1.0750(3) -0.0720(2) 0.42125(19) 0.0359(8) Uani 1 1 d . . . H049 H 1.1489 -0.0740 0.4203 0.043 Uiso 1 1 calc R . . C29 C 0.6853(3) 0.3349(2) 0.44322(19) 0.0349(8) Uani 1 1 d . . . H05A H 0.6091 0.3297 0.4431 0.052 Uiso 1 1 calc R . . H05B H 0.7047 0.3850 0.4199 0.052 Uiso 1 1 calc R . . H05C H 0.7117 0.3380 0.4879 0.052 Uiso 1 1 calc R . . C8 C 0.7147(3) 0.1998(2) 0.23109(17) 0.0317(8) Uani 1 1 d . . . H051 H 0.7469 0.1606 0.2038 0.038 Uiso 1 1 calc R . . C12 C 0.6954(3) 0.2562(2) 0.33550(17) 0.0259(7) Uani 1 1 d . . . C32 C 0.4243(4) 0.1219(4) 0.3308(3) 0.0595(13) Uani 1 1 d . . . F6 F 0.4134(5) 0.2075(4) 0.3410(4) 0.173(3) Uani 1 1 d . . . C35 C 0.1630(6) 0.2869(4) 0.1971(3) 0.0757(19) Uani 1 1 d . . . C37 C 0.8794(5) 0.3607(4) 0.6135(2) 0.0605(13) Uani 1 1 d . . . N01 N 0.8391(5) 0.2990(4) 0.6023(3) 0.0909(17) Uani 1 1 d . . . O5 O 0.2577(5) 0.1059(5) 0.2613(3) 0.182(4) Uani 1 1 d . . . C36 C 0.9318(7) 0.4394(5) 0.6246(3) 0.101(3) Uani 1 1 d . . . H02D H 0.9391 0.4682 0.5833 0.151 Uiso 1 1 calc R . . H02E H 1.0010 0.4296 0.6440 0.151 Uiso 1 1 calc R . . H02F H 0.8905 0.4731 0.6539 0.151 Uiso 1 1 calc R . . C34 C 0.2581(7) 0.3184(5) 0.2316(4) 0.099(2) Uani 1 1 d . . . H05D H 0.3185 0.3125 0.2037 0.149 Uiso 1 1 calc R . . H05E H 0.2698 0.2867 0.2714 0.149 Uiso 1 1 calc R . . H05F H 0.2484 0.3766 0.2424 0.149 Uiso 1 1 calc R . . N04 N 0.0888(5) 0.2645(4) 0.1710(3) 0.095(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0210(2) 0.0212(2) 0.0214(2) 0.00060(16) -0.00125(17) -0.00067(16) S1 0.0329(5) 0.0302(5) 0.0292(4) 0.0010(3) -0.0019(4) 0.0009(4) S003 0.0357(6) 0.0561(7) 0.0541(6) 0.0154(5) 0.0009(5) -0.0092(5) C1 0.034(2) 0.047(2) 0.0305(19) 0.0002(16) -0.0050(17) 0.0010(17) O6 0.038(2) 0.247(8) 0.101(4) -0.025(4) 0.009(2) -0.023(3) C3 0.038(2) 0.0343(19) 0.0263(17) -0.0047(14) -0.0071(15) 0.0052(16) O2 0.0498(18) 0.0369(16) 0.067(2) -0.0130(14) 0.0027(15) 0.0059(14) F1 0.060(3) 0.169(5) 0.233(6) 0.084(5) 0.050(3) -0.010(3) N6 0.0191(13) 0.0219(13) 0.0236(13) 0.0002(10) -0.0033(11) 0.0000(10) O1 0.0515(18) 0.079(2) 0.0312(15) 0.0105(15) -0.0077(13) 0.0059(17) N2 0.0269(15) 0.0253(14) 0.0259(14) 0.0039(11) -0.0039(11) -0.0021(12) N4 0.0210(14) 0.0242(14) 0.0272(14) -0.0021(11) -0.0029(11) -0.0013(11) O3 0.073(2) 0.0314(16) 0.120(3) -0.0015(18) -0.054(2) -0.0016(16) C30 0.0233(17) 0.0211(16) 0.0284(17) 0.0011(13) -0.0003(13) -0.0019(13) N3 0.0238(14) 0.0243(14) 0.0272(14) 0.0026(11) -0.0037(11) -0.0029(11) C22 0.0266(17) 0.0224(16) 0.0217(15) -0.0036(12) -0.0035(13) 0.0007(13) C2 0.045(3) 0.097(4) 0.038(2) -0.014(2) 0.0058(19) 0.010(3) C11 0.0299(19) 0.0295(18) 0.043(2) 0.0055(16) -0.0036(16) 0.0018(15) C23 0.0191(15) 0.0236(16) 0.0259(16) 0.0008(13) -0.0038(12) -0.0020(12) N1 0.0269(15) 0.0233(14) 0.0260(14) -0.0029(11) -0.0035(11) 0.0029(11) C7 0.0215(16) 0.0241(16) 0.0315(17) -0.0039(13) -0.0023(13) 0.0021(13) N5 0.0315(16) 0.0350(17) 0.0279(15) 0.0011(12) 0.0030(13) -0.0012(13) C33 0.071(4) 0.120(6) 0.057(3) 0.039(3) 0.021(3) 0.054(4) C16 0.038(2) 0.0248(17) 0.0294(17) 0.0023(14) -0.0080(15) -0.0024(15) C18 0.0226(17) 0.0310(18) 0.0399(19) 0.0002(15) -0.0018(15) -0.0027(14) C17 0.0304(18) 0.0224(16) 0.0232(15) 0.0045(13) -0.0047(13) -0.0027(13) C28 0.0298(18) 0.0205(16) 0.0294(17) -0.0003(13) -0.0027(14) 0.0012(13) C31 0.034(2) 0.0266(18) 0.042(2) 0.0041(15) 0.0053(16) -0.0040(15) C26 0.0308(19) 0.0303(18) 0.0309(17) -0.0046(14) 0.0035(14) 0.0045(15) C21 0.034(2) 0.0279(17) 0.0294(17) 0.0020(14) -0.0046(14) 0.0029(15) F5 0.060(2) 0.258(7) 0.108(3) 0.086(4) -0.031(2) -0.066(3) C6 0.0290(19) 0.0353(19) 0.042(2) -0.0070(16) -0.0005(16) -0.0074(16) C14 0.0263(18) 0.038(2) 0.046(2) 0.0105(17) -0.0086(16) -0.0081(16) C27 0.0210(16) 0.0250(16) 0.0258(16) -0.0009(13) -0.0024(12) 0.0012(13) C9 0.037(2) 0.037(2) 0.0330(19) 0.0113(16) -0.0104(16) -0.0057(17) C25 0.0271(18) 0.042(2) 0.0264(17) -0.0004(15) 0.0049(14) 0.0017(15) C20 0.039(2) 0.0318(19) 0.0348(19) 0.0011(15) -0.0090(16) 0.0080(16) F2 0.139(4) 0.259(6) 0.053(2) 0.004(3) 0.021(2) 0.150(4) O4 0.185(7) 0.053(3) 0.239(8) 0.017(4) -0.094(6) -0.029(3) F3 0.128(4) 0.290(7) 0.070(2) 0.098(3) 0.050(2) 0.128(4) C15 0.042(2) 0.0276(18) 0.040(2) 0.0052(15) -0.0156(17) -0.0108(16) C4 0.038(2) 0.045(2) 0.0341(19) -0.0149(17) -0.0105(16) 0.0070(18) C24 0.0268(17) 0.0309(18) 0.0277(17) 0.0045(14) 0.0009(14) -0.0008(14) C13 0.0253(18) 0.0320(18) 0.0377(19) 0.0044(15) -0.0024(14) -0.0026(15) F4 0.101(3) 0.275(7) 0.076(3) -0.027(3) 0.043(2) -0.110(4) C5 0.033(2) 0.047(2) 0.051(2) -0.021(2) -0.0086(18) -0.0068(18) C10 0.033(2) 0.035(2) 0.047(2) 0.0145(17) -0.0095(17) 0.0007(16) C19 0.0232(18) 0.041(2) 0.043(2) -0.0012(17) -0.0079(15) 0.0074(16) C29 0.039(2) 0.0249(18) 0.041(2) -0.0044(15) -0.0009(16) 0.0036(15) C8 0.037(2) 0.0294(18) 0.0286(17) 0.0036(14) -0.0037(15) -0.0030(15) C12 0.0228(16) 0.0225(16) 0.0323(17) 0.0038(13) -0.0034(13) -0.0041(13) C32 0.041(3) 0.083(4) 0.054(3) 0.024(3) -0.002(2) -0.019(3) F6 0.115(4) 0.118(4) 0.284(8) -0.040(5) -0.035(5) -0.042(3) C35 0.073(4) 0.078(4) 0.077(4) 0.030(3) 0.022(3) 0.040(4) C37 0.064(3) 0.075(4) 0.043(3) 0.006(2) 0.004(2) -0.011(3) N01 0.108(5) 0.098(4) 0.068(3) -0.015(3) 0.025(3) -0.025(4) O5 0.127(5) 0.276(9) 0.138(5) 0.133(6) -0.098(4) -0.118(5) C36 0.137(7) 0.093(5) 0.072(4) 0.014(4) -0.013(4) -0.052(5) C34 0.120(6) 0.083(5) 0.094(5) 0.012(4) -0.002(5) 0.029(4) N04 0.071(4) 0.098(4) 0.116(5) 0.045(4) 0.024(3) 0.042(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N6 2.095(3) . ? Co N1 2.115(3) . ? Co N5 2.122(3) . ? Co N3 2.125(3) . ? Co N2 2.142(3) . ? Co N4 2.142(3) . ? S1 O3 1.423(3) . ? S1 O2 1.433(3) . ? S1 O1 1.436(3) . ? S1 C33 1.816(6) . ? S003 O5 1.305(5) . ? S003 O4 1.394(6) . ? S003 O6 1.413(5) . ? S003 C32 1.789(5) . ? C1 N5 1.140(5) . ? C1 C2 1.452(6) . ? C3 N1 1.345(4) . ? C3 C4 1.371(5) . ? F1 C33 1.365(10) . ? N6 C27 1.349(4) . ? N6 C23 1.355(4) . ? N2 C8 1.342(4) . ? N2 C12 1.349(4) . ? N4 C18 1.338(4) . ? N4 C22 1.350(4) . ? C30 C31 1.538(5) . ? C30 C7 1.544(4) . ? C30 C23 1.545(4) . ? C30 C22 1.553(5) . ? N3 C13 1.344(5) . ? N3 C17 1.345(4) . ? C22 C21 1.391(5) . ? C11 C12 1.386(5) . ? C11 C10 1.387(5) . ? C23 C24 1.387(5) . ? N1 C7 1.348(4) . ? C7 C6 1.389(5) . ? C33 F2 1.291(7) . ? C33 F3 1.313(7) . ? C16 C15 1.388(6) . ? C16 C17 1.390(5) . ? C18 C19 1.383(5) . ? C17 C28 1.548(5) . ? C28 C29 1.538(5) . ? C28 C27 1.547(4) . ? C28 C12 1.557(5) . ? C26 C25 1.379(5) . ? C26 C27 1.393(5) . ? C21 C20 1.379(5) . ? F5 C32 1.265(6) . ? C6 C5 1.383(6) . ? C14 C15 1.372(6) . ? C14 C13 1.375(5) . ? C9 C10 1.375(6) . ? C9 C8 1.377(5) . ? C25 C24 1.382(5) . ? C20 C19 1.375(6) . ? C4 C5 1.376(6) . ? F4 C32 1.240(6) . ? C32 F6 1.383(8) . ? C35 N04 1.121(9) . ? C35 C34 1.461(11) . ? C37 N01 1.125(7) . ? C37 C36 1.429(9) . ? 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 N6 Co N1 87.02(10) . . ? N6 Co N5 178.03(11) . . ? N1 Co N5 91.95(11) . . ? N6 Co N3 88.33(10) . . ? N1 Co N3 174.95(11) . . ? N5 Co N3 92.76(11) . . ? N6 Co N2 87.52(10) . . ? N1 Co N2 97.44(11) . . ? N5 Co N2 94.28(11) . . ? N3 Co N2 80.40(11) . . ? N6 Co N4 86.38(10) . . ? N1 Co N4 82.05(11) . . ? N5 Co N4 91.82(11) . . ? N3 Co N4 99.61(10) . . ? N2 Co N4 173.90(11) . . ? O3 S1 O2 113.9(2) . . ? O3 S1 O1 114.5(2) . . ? O2 S1 O1 116.7(2) . . ? O3 S1 C33 103.8(3) . . ? O2 S1 C33 103.0(3) . . ? O1 S1 C33 102.3(2) . . ? O5 S003 O4 121.3(5) . . ? O5 S003 O6 118.3(5) . . ? O4 S003 O6 104.4(5) . . ? O5 S003 C32 107.6(3) . . ? O4 S003 C32 99.4(3) . . ? O6 S003 C32 102.8(3) . . ? N5 C1 C2 178.5(5) . . ? N1 C3 C4 123.5(4) . . ? C27 N6 C23 120.0(3) . . ? C27 N6 Co 119.7(2) . . ? C23 N6 Co 119.8(2) . . ? C8 N2 C12 118.6(3) . . ? C8 N2 Co 122.2(2) . . ? C12 N2 Co 119.1(2) . . ? C18 N4 C22 118.2(3) . . ? C18 N4 Co 121.7(2) . . ? C22 N4 Co 119.9(2) . . ? C31 C30 C7 109.5(3) . . ? C31 C30 C23 109.9(3) . . ? C7 C30 C23 110.6(3) . . ? C31 C30 C22 109.0(3) . . ? C7 C30 C22 108.6(3) . . ? C23 C30 C22 109.2(3) . . ? C13 N3 C17 118.7(3) . . ? C13 N3 Co 121.2(2) . . ? C17 N3 Co 120.1(2) . . ? N4 C22 C21 120.9(3) . . ? N4 C22 C30 117.4(3) . . ? C21 C22 C30 121.7(3) . . ? C12 C11 C10 120.2(4) . . ? N6 C23 C24 120.9(3) . . ? N6 C23 C30 118.3(3) . . ? C24 C23 C30 120.7(3) . . ? C3 N1 C7 118.6(3) . . ? C3 N1 Co 120.6(2) . . ? C7 N1 Co 120.4(2) . . ? N1 C7 C6 120.5(3) . . ? N1 C7 C30 117.1(3) . . ? C6 C7 C30 122.4(3) . . ? C1 N5 Co 174.6(3) . . ? F2 C33 F3 107.7(6) . . ? F2 C33 F1 107.3(6) . . ? F3 C33 F1 110.9(7) . . ? F2 C33 S1 111.6(5) . . ? F3 C33 S1 110.5(5) . . ? F1 C33 S1 108.7(5) . . ? C15 C16 C17 119.6(3) . . ? N4 C18 C19 123.7(3) . . ? N3 C17 C16 120.8(3) . . ? N3 C17 C28 117.4(3) . . ? C16 C17 C28 121.8(3) . . ? C29 C28 C27 109.6(3) . . ? C29 C28 C17 109.4(3) . . ? C27 C28 C17 109.1(3) . . ? C29 C28 C12 109.1(3) . . ? C27 C28 C12 111.4(3) . . ? C17 C28 C12 108.2(3) . . ? C25 C26 C27 119.3(3) . . ? C20 C21 C22 120.0(3) . . ? C5 C6 C7 120.0(4) . . ? C15 C14 C13 118.4(4) . . ? N6 C27 C26 120.8(3) . . ? N6 C27 C28 118.1(3) . . ? C26 C27 C28 121.0(3) . . ? C10 C9 C8 118.1(3) . . ? C26 C25 C24 119.6(3) . . ? C19 C20 C21 119.1(3) . . ? C14 C15 C16 119.2(3) . . ? C3 C4 C5 118.1(4) . . ? C25 C24 C23 119.2(3) . . ? N3 C13 C14 123.2(4) . . ? C4 C5 C6 119.1(4) . . ? C9 C10 C11 119.0(3) . . ? C20 C19 C18 118.1(3) . . ? N2 C8 C9 123.6(4) . . ? N2 C12 C11 120.5(3) . . ? N2 C12 C28 117.4(3) . . ? C11 C12 C28 122.0(3) . . ? F4 C32 F5 114.0(5) . . ? F4 C32 F6 98.1(5) . . ? F5 C32 F6 97.9(6) . . ? F4 C32 S003 116.7(4) . . ? F5 C32 S003 117.0(4) . . ? F6 C32 S003 109.1(4) . . ? N04 C35 C34 178.4(8) . . ? N01 C37 C36 177.3(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.504 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.089