Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Dalton.Trans. _journal_coden_Cambridge 0182 _audit_creation_date 2007-8-23 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record 2007-06-21 # SUBMISSION DETAILS _publ_contact_author_name 'Noboru Koga' _publ_contact_author_address ; Graduate School of Pharmaceutical Sciences Kyushu University Fukuoka 812-8582 JAPAN ; _publ_contact_author_email koga@fc.phar.kyushu-u.ac.jp _publ_contact_author_fax +81-92-642-6590 _publ_contact_author_phone +81-92-642-6593 _publ_requested_category FA _publ_section_title ; Formation of Monometallic SMM with S value of 3/2 in Diluted Frozen Solution ; _publ_section_abstract ; SMM in diluted frozen solutions ; #============================================================================== # TITLE AND AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Satoru Karasawa' ; Graduate School of Pharmaceutical Sciences Kyushu University Fukuoka 812-8582 JAPAN ; 'Natsuki Watanabe' ; Graduate School of Pharmaceutical Sciences Kyushu University Fukuoka 812-8582 JAPAN ; 'Daisuke Yoshihara' ; Graduate School of Pharmaceutical Sciences Kyushu University Fukuoka 812-8582 JAPAN ; 'Motohiro Nakano' ; Department of Applied Chemistry, Graduate School of Engineering Osaka University Osaka 565-0871 JAPAN ; 'Noboru Koga' ; Graduate School of Pharmaceutical Sciences Kyushu University Fukuoka 812-8582 JAPAN ; #============================================================================== # TEXT _publ_section_references ; Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; #============================================================================== data__[Co(hfpip)2(4NOpy)2] _database_code_depnum_ccdc_archive 'CCDC 658520' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C40 H38 Co F12 N6 O4 ' _chemical_formula_moiety 'C40 H38 Co F12 N6 O4 ' _chemical_formula_weight 953.69 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 11.1742(7) _cell_length_b 21.3708(15) _cell_length_c 18.4941(11) _cell_angle_alpha 90.0000 _cell_angle_beta 101.7170(17) _cell_angle_gamma 90.0000 _cell_volume 4324.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14480 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948.00 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 14589 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_max 27.86 _diffrn_measured_fraction_theta_max 0.812 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8038 _reflns_number_gt 4700 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.1820 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 8038 _refine_ls_number_parameters 570 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0589P)^2^+9.1773P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.37 _refine_diff_density_min -0.44 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Co Co 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Co 0.99653(6) 0.01203(3) 0.26207(4) 0.0367(2) Uani 1.00 1 d . . . F(1) F 1.1726(3) -0.08884(19) 0.4816(2) 0.0887(12) Uani 1.00 1 d . . . F(2) F 1.2536(4) -0.0095(2) 0.5386(2) 0.1121(17) Uani 1.00 1 d . . . F(3) F 1.3259(3) -0.0486(2) 0.4520(2) 0.0860(12) Uani 1.00 1 d . . . F(4) F 1.0810(4) 0.17478(19) 0.4952(2) 0.1124(18) Uani 1.00 1 d . . . F(5) F 0.9027(3) 0.18543(16) 0.43220(18) 0.0669(9) Uani 1.00 1 d . . . F(6) F 1.0531(3) 0.21625(16) 0.3872(2) 0.0806(11) Uani 1.00 1 d . . . F(7) F 0.7204(3) 0.0059(2) 0.0462(2) 0.0935(13) Uani 1.00 1 d . . . F(8) F 0.8191(3) 0.0588(2) -0.02166(19) 0.0883(12) Uani 1.00 1 d . . . F(9) F 0.7285(4) 0.1051(2) 0.0558(2) 0.1049(16) Uani 1.00 1 d . . . F(10) F 1.2171(3) 0.0920(2) 0.0416(2) 0.0903(13) Uani 1.00 1 d . . . F(11) F 1.2725(5) 0.1476(2) 0.1373(2) 0.133(2) Uani 1.00 1 d . . . F(12) F 1.3368(3) 0.0544(2) 0.1348(2) 0.0986(14) Uani 1.00 1 d . . . O(1) O 0.4275(3) -0.12077(19) 0.2784(2) 0.0595(11) Uani 1.00 1 d . . . O(2) O 1.1921(3) -0.28121(18) 0.1642(2) 0.0589(10) Uani 1.00 1 d . . . O(3) O 1.1065(2) -0.02176(15) 0.35362(18) 0.0396(8) Uani 1.00 1 d . . . O(4) O 0.8809(3) 0.03969(16) 0.17014(19) 0.0438(8) Uani 1.00 1 d . . . N(1) N 0.8370(3) -0.03465(19) 0.2885(2) 0.0385(9) Uani 1.00 1 d . . . N(2) N 0.5290(3) -0.1371(2) 0.3202(2) 0.0418(10) Uani 1.00 1 d . . . N(3) N 1.0287(3) -0.07547(19) 0.2085(2) 0.0373(9) Uani 1.00 1 d . . . N(4) N 1.0923(3) -0.2556(2) 0.1294(2) 0.0431(10) Uani 1.00 1 d . . . N(5) N 0.9684(3) 0.09432(19) 0.3247(2) 0.0393(10) Uani 1.00 1 d . . . N(6) N 1.1407(3) 0.05665(19) 0.2168(2) 0.0430(10) Uani 1.00 1 d . . . C(1) C 0.7207(4) -0.0199(2) 0.2555(2) 0.0433(12) Uani 1.00 1 d . . . C(2) C 0.6202(4) -0.0530(2) 0.2645(2) 0.0448(13) Uani 1.00 1 d . . . C(3) C 0.6344(4) -0.1051(2) 0.3103(2) 0.0362(11) Uani 1.00 1 d . . . C(4) C 0.7533(4) -0.1219(2) 0.3440(2) 0.0450(13) Uani 1.00 1 d . . . C(5) C 0.8495(4) -0.0854(2) 0.3314(2) 0.0447(13) Uani 1.00 1 d . . . C(6) C 0.5234(4) -0.1884(2) 0.3756(2) 0.0415(12) Uani 1.00 1 d . . . C(7) C 0.3898(5) -0.1991(3) 0.3771(3) 0.0669(18) Uani 1.00 1 d . . . C(8) C 0.5873(6) -0.1669(3) 0.4525(3) 0.081(2) Uani 1.00 1 d . . . C(9) C 0.5769(6) -0.2474(2) 0.3504(4) 0.0744(19) Uani 1.00 1 d . . . C(10) C 0.9408(4) -0.1062(2) 0.1612(3) 0.0475(13) Uani 1.00 1 d . . . C(11) C 0.9553(4) -0.1639(2) 0.1319(2) 0.0447(12) Uani 1.00 1 d . . . C(12) C 1.0672(4) -0.1944(2) 0.1521(2) 0.0376(11) Uani 1.00 1 d . . . C(13) C 1.1599(4) -0.1629(2) 0.1998(2) 0.0426(12) Uani 1.00 1 d . . . C(14) C 1.1367(4) -0.1050(2) 0.2264(2) 0.0414(12) Uani 1.00 1 d . . . C(15) C 1.0110(5) -0.2937(2) 0.0706(3) 0.0518(14) Uani 1.00 1 d . . . C(16) C 0.8994(5) -0.3139(3) 0.1006(3) 0.0680(18) Uani 1.00 1 d . . . C(17) C 1.0828(5) -0.3516(3) 0.0577(3) 0.080(2) Uani 1.00 1 d . . . C(18) C 0.9785(6) -0.2566(3) -0.0001(3) 0.077(2) Uani 1.00 1 d . . . C(19) C 1.2221(5) -0.0341(2) 0.4721(3) 0.0532(14) Uani 1.00 1 d . . . C(20) C 1.1398(4) 0.0059(2) 0.4153(2) 0.0427(12) Uani 1.00 1 d . . . C(21) C 1.1095(5) 0.0639(2) 0.4370(3) 0.0508(14) Uani 1.00 1 d . . . C(22) C 1.0278(4) 0.1060(2) 0.3916(3) 0.0446(12) Uani 1.00 1 d . . . C(23) C 1.0157(6) 0.1706(2) 0.4271(3) 0.0602(16) Uani 1.00 1 d . . . C(25) C 0.7597(4) 0.1355(2) 0.2982(3) 0.0499(13) Uani 1.00 1 d . . . C(26) C 0.6706(5) 0.1722(3) 0.2564(3) 0.0610(16) Uani 1.00 1 d . . . C(27) C 0.6975(5) 0.2108(2) 0.2023(3) 0.0595(16) Uani 1.00 1 d . . . C(28) C 0.8130(6) 0.2116(2) 0.1893(3) 0.0598(16) Uani 1.00 1 d . . . C(29) C 0.9034(5) 0.1745(2) 0.2304(3) 0.0531(14) Uani 1.00 1 d . . . C(30) C 0.8784(4) 0.1369(2) 0.2859(2) 0.0397(11) Uani 1.00 1 d . . . C(31) C 0.7955(6) 0.0550(3) 0.0463(3) 0.0665(18) Uani 1.00 1 d . . . C(32) C 0.9082(5) 0.0513(2) 0.1080(3) 0.0498(14) Uani 1.00 1 d . . . C(33) C 1.0214(5) 0.0609(2) 0.0922(3) 0.0542(15) Uani 1.00 1 d . . . C(34) C 1.1312(5) 0.0674(2) 0.1461(3) 0.0505(14) Uani 1.00 1 d . . . C(35) C 1.2406(7) 0.0902(3) 0.1157(3) 0.0679(18) Uani 1.00 1 d . . . C(36) C 1.2493(4) 0.0759(2) 0.2691(3) 0.0463(13) Uani 1.00 1 d . . . C(37) C 1.3409(4) 0.0340(2) 0.2970(3) 0.0541(15) Uani 1.00 1 d . . . C(38) C 1.4413(5) 0.0532(3) 0.3484(3) 0.0633(16) Uani 1.00 1 d . . . C(39) C 1.4511(5) 0.1144(3) 0.3738(3) 0.0645(17) Uani 1.00 1 d . . . C(40) C 1.3595(5) 0.1559(3) 0.3463(3) 0.0644(17) Uani 1.00 1 d . . . C(41) C 1.2576(5) 0.1368(2) 0.2948(3) 0.0578(15) Uani 1.00 1 d . . . H(1) H 0.7084 0.0158 0.2242 0.052 Uiso 1.00 1 c R . . H(2) H 0.5410 -0.0405 0.2396 0.054 Uiso 1.00 1 c R . . H(3) H 0.7681 -0.1576 0.3751 0.054 Uiso 1.00 1 c R . . H(4) H 0.9299 -0.0973 0.3550 0.054 Uiso 1.00 1 c R . . H(5) H 0.3397 -0.1897 0.3284 0.080 Uiso 1.00 1 c R . . H(6) H 0.3657 -0.1718 0.4142 0.080 Uiso 1.00 1 c R . . H(7) H 0.3777 -0.2429 0.3896 0.080 Uiso 1.00 1 c R . . H(8) H 0.6737 -0.1789 0.4612 0.097 Uiso 1.00 1 c R . . H(9) H 0.5484 -0.1866 0.4896 0.097 Uiso 1.00 1 c R . . H(10) H 0.5809 -0.1213 0.4559 0.097 Uiso 1.00 1 c R . . H(11) H 0.6404 -0.2364 0.3230 0.089 Uiso 1.00 1 c R . . H(12) H 0.5123 -0.2713 0.3184 0.089 Uiso 1.00 1 c R . . H(13) H 0.6129 -0.2727 0.3936 0.089 Uiso 1.00 1 c R . . H(14) H 0.8634 -0.0865 0.1472 0.057 Uiso 1.00 1 c R . . H(15) H 0.8898 -0.1829 0.0983 0.054 Uiso 1.00 1 c R . . H(16) H 1.2386 -0.1812 0.2140 0.051 Uiso 1.00 1 c R . . H(17) H 1.2012 -0.0847 0.2594 0.050 Uiso 1.00 1 c R . . H(18) H 0.8289 -0.3180 0.0596 0.082 Uiso 1.00 1 c R . . H(19) H 0.8818 -0.2823 0.1355 0.082 Uiso 1.00 1 c R . . H(20) H 0.9159 -0.3542 0.1259 0.082 Uiso 1.00 1 c R . . H(21) H 1.1289 -0.3429 0.0191 0.095 Uiso 1.00 1 c R . . H(22) H 1.0262 -0.3863 0.0422 0.095 Uiso 1.00 1 c R . . H(23) H 1.1396 -0.3628 0.1036 0.095 Uiso 1.00 1 c R . . H(24) H 0.9653 -0.2853 -0.0423 0.093 Uiso 1.00 1 c R . . H(25) H 1.0455 -0.2279 -0.0036 0.093 Uiso 1.00 1 c R . . H(26) H 0.9037 -0.2326 -0.0003 0.093 Uiso 1.00 1 c R . . H(27) H 1.1454 0.0772 0.4856 0.061 Uiso 1.00 1 c R . . H(28) H 0.7401 0.1093 0.3356 0.060 Uiso 1.00 1 c R . . H(29) H 0.5896 0.1708 0.2649 0.073 Uiso 1.00 1 c R . . H(30) H 0.6360 0.2367 0.1742 0.071 Uiso 1.00 1 c R . . H(31) H 0.8318 0.2379 0.1517 0.072 Uiso 1.00 1 c R . . H(32) H 0.9833 0.1749 0.2202 0.064 Uiso 1.00 1 c R . . H(33) H 1.0269 0.0634 0.0417 0.065 Uiso 1.00 1 c R . . H(34) H 1.3348 -0.0082 0.2807 0.065 Uiso 1.00 1 c R . . H(35) H 1.5046 0.0241 0.3668 0.076 Uiso 1.00 1 c R . . H(36) H 1.5201 0.1273 0.4095 0.077 Uiso 1.00 1 c R . . H(37) H 1.3658 0.1981 0.3628 0.077 Uiso 1.00 1 c R . . H(38) H 1.1937 0.1657 0.2771 0.069 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0313(3) 0.0324(3) 0.0465(4) 0.0001(3) 0.0081(2) 0.0016(3) F(1) 0.078(2) 0.070(2) 0.111(3) 0.000(2) 0.001(2) 0.045(2) F(2) 0.156(4) 0.093(3) 0.063(2) 0.069(3) -0.036(2) -0.022(2) F(3) 0.050(2) 0.108(3) 0.099(2) 0.032(2) 0.0119(19) 0.030(2) F(4) 0.139(3) 0.070(2) 0.094(2) 0.046(2) -0.058(2) -0.042(2) F(5) 0.075(2) 0.057(2) 0.072(2) 0.0111(19) 0.0219(19) -0.0105(17) F(6) 0.085(2) 0.041(2) 0.122(3) -0.0124(19) 0.036(2) -0.019(2) F(7) 0.080(2) 0.119(3) 0.071(2) -0.011(2) -0.009(2) -0.007(2) F(8) 0.105(3) 0.109(3) 0.048(2) 0.023(2) 0.0088(19) 0.008(2) F(9) 0.120(3) 0.110(3) 0.071(2) 0.069(3) -0.014(2) -0.007(2) F(10) 0.110(3) 0.103(3) 0.071(2) -0.023(2) 0.050(2) 0.004(2) F(11) 0.203(5) 0.084(3) 0.151(4) -0.088(3) 0.126(4) -0.051(3) F(12) 0.061(2) 0.142(4) 0.105(3) -0.005(2) 0.045(2) 0.009(2) O(1) 0.0282(19) 0.060(2) 0.084(2) -0.0036(18) -0.0034(19) 0.019(2) O(2) 0.041(2) 0.047(2) 0.085(2) 0.0074(19) 0.003(2) -0.011(2) O(3) 0.0357(18) 0.035(2) 0.049(2) -0.0011(15) 0.0110(15) -0.0006(16) O(4) 0.045(2) 0.041(2) 0.046(2) 0.0046(17) 0.0101(16) 0.0064(17) N(1) 0.033(2) 0.035(2) 0.046(2) 0.0045(19) 0.0043(18) 0.0020(19) N(2) 0.030(2) 0.037(2) 0.058(2) -0.0038(19) 0.0081(19) 0.001(2) N(3) 0.029(2) 0.038(2) 0.046(2) -0.0018(19) 0.0097(18) 0.0054(19) N(4) 0.036(2) 0.037(2) 0.055(2) -0.005(2) 0.009(2) -0.012(2) N(5) 0.035(2) 0.037(2) 0.046(2) 0.0039(19) 0.0096(19) 0.008(2) N(6) 0.039(2) 0.033(2) 0.059(2) 0.0053(19) 0.014(2) -0.000(2) C(1) 0.037(2) 0.038(3) 0.054(3) 0.002(2) 0.007(2) 0.009(2) C(2) 0.027(2) 0.047(3) 0.059(3) 0.002(2) 0.004(2) 0.006(2) C(3) 0.029(2) 0.036(2) 0.044(2) -0.003(2) 0.008(2) -0.005(2) C(4) 0.034(2) 0.039(3) 0.062(3) -0.001(2) 0.009(2) 0.008(2) C(5) 0.029(2) 0.050(3) 0.052(3) -0.002(2) 0.002(2) 0.004(2) C(6) 0.032(2) 0.038(3) 0.054(3) -0.001(2) 0.009(2) 0.004(2) C(7) 0.045(3) 0.067(4) 0.095(4) -0.004(3) 0.027(3) 0.017(3) C(8) 0.098(5) 0.093(5) 0.049(3) -0.037(4) 0.008(3) 0.013(3) C(9) 0.078(4) 0.047(3) 0.110(5) 0.011(3) 0.046(4) 0.009(3) C(10) 0.036(2) 0.041(3) 0.063(3) 0.002(2) 0.004(2) -0.002(2) C(11) 0.034(2) 0.044(3) 0.053(3) 0.001(2) 0.001(2) -0.007(2) C(12) 0.036(2) 0.036(2) 0.043(2) -0.002(2) 0.016(2) -0.000(2) C(13) 0.031(2) 0.041(3) 0.057(3) 0.001(2) 0.011(2) -0.004(2) C(14) 0.032(2) 0.033(3) 0.059(3) -0.005(2) 0.010(2) -0.005(2) C(15) 0.048(3) 0.051(3) 0.056(3) -0.003(2) 0.011(2) -0.017(2) C(16) 0.055(3) 0.060(4) 0.091(4) -0.018(3) 0.022(3) -0.026(3) C(17) 0.057(4) 0.073(4) 0.103(5) 0.010(3) 0.004(3) -0.049(4) C(18) 0.094(5) 0.093(5) 0.046(3) 0.002(4) 0.014(3) -0.007(3) C(19) 0.049(3) 0.051(3) 0.056(3) 0.010(2) 0.002(2) -0.001(2) C(20) 0.033(2) 0.043(3) 0.052(3) -0.001(2) 0.008(2) 0.002(2) C(21) 0.055(3) 0.044(3) 0.051(3) 0.007(2) 0.005(2) -0.009(2) C(22) 0.043(3) 0.037(3) 0.055(3) 0.000(2) 0.012(2) 0.002(2) C(23) 0.062(4) 0.045(3) 0.065(4) 0.007(3) -0.007(3) -0.006(3) C(25) 0.044(3) 0.048(3) 0.058(3) 0.008(2) 0.011(2) 0.004(2) C(26) 0.046(3) 0.064(4) 0.071(4) 0.014(3) 0.008(3) 0.004(3) C(27) 0.061(4) 0.054(3) 0.059(3) 0.023(3) 0.001(3) 0.002(3) C(28) 0.082(4) 0.039(3) 0.061(3) 0.020(3) 0.020(3) 0.012(2) C(29) 0.054(3) 0.040(3) 0.070(3) 0.012(2) 0.023(2) 0.010(2) C(30) 0.045(3) 0.031(2) 0.041(2) 0.003(2) 0.003(2) -0.002(2) C(31) 0.081(4) 0.067(4) 0.049(3) 0.021(4) 0.008(3) 0.003(3) C(32) 0.061(3) 0.030(3) 0.057(3) 0.009(2) 0.010(3) 0.002(2) C(33) 0.075(4) 0.039(3) 0.051(3) 0.004(3) 0.019(3) 0.002(2) C(34) 0.064(3) 0.031(3) 0.063(3) -0.006(2) 0.028(3) -0.001(2) C(35) 0.085(5) 0.055(4) 0.072(4) -0.018(3) 0.037(3) -0.009(3) C(36) 0.038(3) 0.040(3) 0.065(3) -0.005(2) 0.022(2) -0.003(2) C(37) 0.036(3) 0.050(3) 0.077(4) -0.011(2) 0.014(2) -0.010(3) C(38) 0.041(3) 0.069(4) 0.080(4) -0.006(3) 0.013(3) -0.003(3) C(39) 0.041(3) 0.079(5) 0.074(4) -0.021(3) 0.015(3) -0.023(3) C(40) 0.059(4) 0.056(4) 0.083(4) -0.016(3) 0.025(3) -0.021(3) C(41) 0.052(3) 0.039(3) 0.086(4) -0.005(2) 0.024(3) -0.008(3) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co(1) O(3) 2.013(3) yes . . Co(1) O(4) 2.004(3) yes . . Co(1) N(1) 2.183(4) yes . . Co(1) N(3) 2.180(4) yes . . Co(1) N(5) 2.164(4) yes . . Co(1) N(6) 2.181(4) yes . . F(1) C(19) 1.322(7) yes . . F(2) C(19) 1.318(6) yes . . F(3) C(19) 1.324(7) yes . . F(4) C(23) 1.323(7) yes . . F(5) C(23) 1.324(7) yes . . F(6) C(23) 1.339(7) yes . . F(7) C(31) 1.343(8) yes . . F(8) C(31) 1.338(7) yes . . F(9) C(31) 1.338(8) yes . . F(10) C(35) 1.343(8) yes . . F(11) C(35) 1.316(8) yes . . F(12) C(35) 1.309(8) yes . . O(1) N(2) 1.285(4) yes . . O(2) N(4) 1.291(5) yes . . O(3) C(20) 1.271(6) yes . . O(4) C(32) 1.273(7) yes . . N(1) C(1) 1.356(5) yes . . N(1) C(5) 1.334(6) yes . . N(2) C(3) 1.406(6) yes . . N(2) C(6) 1.510(6) yes . . N(3) C(10) 1.346(6) yes . . N(3) C(14) 1.343(6) yes . . N(4) C(12) 1.418(6) yes . . N(4) C(15) 1.506(6) yes . . N(5) C(22) 1.303(6) yes . . N(5) C(30) 1.436(6) yes . . N(6) C(34) 1.309(7) yes . . N(6) C(36) 1.449(6) yes . . C(1) C(2) 1.366(7) yes . . C(2) C(3) 1.388(7) yes . . C(3) C(4) 1.396(6) yes . . C(4) C(5) 1.385(7) yes . . C(6) C(7) 1.516(7) yes . . C(6) C(8) 1.526(7) yes . . C(6) C(9) 1.510(8) yes . . C(10) C(11) 1.370(7) yes . . C(11) C(12) 1.393(6) yes . . C(12) C(13) 1.391(6) yes . . C(13) C(14) 1.374(7) yes . . C(15) C(16) 1.525(9) yes . . C(15) C(17) 1.520(9) yes . . C(15) C(18) 1.509(8) yes . . C(19) C(20) 1.511(7) yes . . C(20) C(21) 1.368(7) yes . . C(21) C(22) 1.426(7) yes . . C(22) C(23) 1.548(8) yes . . C(25) C(26) 1.374(7) yes . . C(25) C(30) 1.392(7) yes . . C(26) C(27) 1.377(9) yes . . C(27) C(28) 1.359(9) yes . . C(28) C(29) 1.384(7) yes . . C(29) C(30) 1.375(7) yes . . C(31) C(32) 1.519(8) yes . . C(32) C(33) 1.370(9) yes . . C(33) C(34) 1.422(7) yes . . C(34) C(35) 1.527(10) yes . . C(36) C(37) 1.378(7) yes . . C(36) C(41) 1.383(8) yes . . C(37) C(38) 1.378(7) yes . . C(38) C(39) 1.386(9) yes . . C(39) C(40) 1.372(8) yes . . C(40) C(41) 1.390(8) yes . . C(1) H(1) 0.950 no . . C(2) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(5) H(4) 0.950 no . . C(7) H(5) 0.980 no . . C(7) H(6) 0.980 no . . C(7) H(7) 0.980 no . . C(8) H(8) 0.980 no . . C(8) H(9) 0.980 no . . C(8) H(10) 0.980 no . . C(9) H(11) 0.980 no . . C(9) H(12) 0.980 no . . C(9) H(13) 0.980 no . . C(10) H(14) 0.950 no . . C(11) H(15) 0.950 no . . C(13) H(16) 0.950 no . . C(14) H(17) 0.950 no . . C(16) H(18) 0.980 no . . C(16) H(19) 0.980 no . . C(16) H(20) 0.980 no . . C(17) H(21) 0.980 no . . C(17) H(22) 0.980 no . . C(17) H(23) 0.980 no . . C(18) H(24) 0.980 no . . C(18) H(25) 0.980 no . . C(18) H(26) 0.980 no . . C(21) H(27) 0.950 no . . C(25) H(28) 0.950 no . . C(26) H(29) 0.950 no . . C(27) H(30) 0.950 no . . C(28) H(31) 0.950 no . . C(29) H(32) 0.950 no . . C(33) H(33) 0.950 no . . C(37) H(34) 0.950 no . . C(38) H(35) 0.950 no . . C(39) H(36) 0.950 no . . C(40) H(37) 0.950 no . . C(41) H(38) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(3) Co(1) O(4) 175.86(13) yes . . . O(3) Co(1) N(1) 91.96(14) yes . . . O(3) Co(1) N(3) 86.89(13) yes . . . O(3) Co(1) N(5) 88.35(13) yes . . . O(3) Co(1) N(6) 96.17(14) yes . . . O(4) Co(1) N(1) 84.81(14) yes . . . O(4) Co(1) N(3) 90.28(14) yes . . . O(4) Co(1) N(5) 94.35(14) yes . . . O(4) Co(1) N(6) 86.83(15) yes . . . N(1) Co(1) N(3) 85.82(15) yes . . . N(1) Co(1) N(5) 92.14(15) yes . . . N(1) Co(1) N(6) 170.58(15) yes . . . N(3) Co(1) N(5) 174.75(15) yes . . . N(3) Co(1) N(6) 89.87(15) yes . . . N(5) Co(1) N(6) 92.84(16) yes . . . Co(1) O(3) C(20) 127.3(3) yes . . . Co(1) O(4) C(32) 126.3(3) yes . . . Co(1) N(1) C(1) 123.0(3) yes . . . Co(1) N(1) C(5) 120.9(3) yes . . . C(1) N(1) C(5) 115.6(4) yes . . . O(1) N(2) C(3) 116.7(4) yes . . . O(1) N(2) C(6) 116.9(3) yes . . . C(3) N(2) C(6) 126.4(3) yes . . . Co(1) N(3) C(10) 123.2(3) yes . . . Co(1) N(3) C(14) 121.0(3) yes . . . C(10) N(3) C(14) 115.5(4) yes . . . O(2) N(4) C(12) 116.5(3) yes . . . O(2) N(4) C(15) 117.6(4) yes . . . C(12) N(4) C(15) 125.9(3) yes . . . Co(1) N(5) C(22) 124.2(3) yes . . . Co(1) N(5) C(30) 114.2(2) yes . . . C(22) N(5) C(30) 121.6(4) yes . . . Co(1) N(6) C(34) 122.9(3) yes . . . Co(1) N(6) C(36) 116.8(3) yes . . . C(34) N(6) C(36) 120.3(4) yes . . . N(1) C(1) C(2) 124.1(4) yes . . . C(1) C(2) C(3) 119.7(4) yes . . . N(2) C(3) C(2) 118.4(4) yes . . . N(2) C(3) C(4) 124.3(4) yes . . . C(2) C(3) C(4) 117.3(4) yes . . . C(3) C(4) C(5) 118.8(4) yes . . . N(1) C(5) C(4) 124.5(4) yes . . . N(2) C(6) C(7) 107.4(4) yes . . . N(2) C(6) C(8) 109.7(4) yes . . . N(2) C(6) C(9) 108.9(4) yes . . . C(7) C(6) C(8) 107.8(5) yes . . . C(7) C(6) C(9) 109.4(4) yes . . . C(8) C(6) C(9) 113.5(4) yes . . . N(3) C(10) C(11) 124.6(4) yes . . . C(10) C(11) C(12) 119.1(4) yes . . . N(4) C(12) C(11) 124.9(4) yes . . . N(4) C(12) C(13) 117.9(4) yes . . . C(11) C(12) C(13) 117.1(4) yes . . . C(12) C(13) C(14) 119.6(4) yes . . . N(3) C(14) C(13) 124.1(4) yes . . . N(4) C(15) C(16) 108.0(4) yes . . . N(4) C(15) C(17) 107.1(4) yes . . . N(4) C(15) C(18) 110.2(4) yes . . . C(16) C(15) C(17) 108.9(5) yes . . . C(16) C(15) C(18) 113.1(4) yes . . . C(17) C(15) C(18) 109.4(5) yes . . . F(1) C(19) F(2) 105.6(5) yes . . . F(1) C(19) F(3) 104.1(4) yes . . . F(1) C(19) C(20) 112.3(4) yes . . . F(2) C(19) F(3) 105.8(4) yes . . . F(2) C(19) C(20) 115.7(5) yes . . . F(3) C(19) C(20) 112.4(5) yes . . . O(3) C(20) C(19) 112.8(4) yes . . . O(3) C(20) C(21) 129.8(4) yes . . . C(19) C(20) C(21) 117.4(4) yes . . . C(20) C(21) C(22) 124.5(4) yes . . . N(5) C(22) C(21) 125.5(4) yes . . . N(5) C(22) C(23) 120.1(4) yes . . . C(21) C(22) C(23) 114.4(4) yes . . . F(4) C(23) F(5) 105.4(5) yes . . . F(4) C(23) F(6) 107.6(5) yes . . . F(4) C(23) C(22) 112.6(4) yes . . . F(5) C(23) F(6) 105.9(4) yes . . . F(5) C(23) C(22) 114.2(4) yes . . . F(6) C(23) C(22) 110.6(5) yes . . . C(26) C(25) C(30) 120.1(5) yes . . . C(25) C(26) C(27) 120.7(5) yes . . . C(26) C(27) C(28) 119.4(5) yes . . . C(27) C(28) C(29) 120.6(5) yes . . . C(28) C(29) C(30) 120.6(5) yes . . . N(5) C(30) C(25) 119.9(4) yes . . . N(5) C(30) C(29) 121.1(4) yes . . . C(25) C(30) C(29) 118.6(4) yes . . . F(7) C(31) F(8) 106.8(5) yes . . . F(7) C(31) F(9) 104.9(5) yes . . . F(7) C(31) C(32) 112.5(5) yes . . . F(8) C(31) F(9) 107.3(5) yes . . . F(8) C(31) C(32) 114.6(6) yes . . . F(9) C(31) C(32) 110.1(5) yes . . . O(4) C(32) C(31) 112.0(5) yes . . . O(4) C(32) C(33) 128.5(4) yes . . . C(31) C(32) C(33) 119.5(5) yes . . . C(32) C(33) C(34) 124.6(5) yes . . . N(6) C(34) C(33) 124.5(5) yes . . . N(6) C(34) C(35) 121.0(4) yes . . . C(33) C(34) C(35) 114.5(5) yes . . . F(10) C(35) F(11) 105.5(5) yes . . . F(10) C(35) F(12) 105.8(6) yes . . . F(10) C(35) C(34) 112.3(5) yes . . . F(11) C(35) F(12) 107.9(5) yes . . . F(11) C(35) C(34) 112.0(6) yes . . . F(12) C(35) C(34) 112.9(5) yes . . . N(6) C(36) C(37) 121.6(4) yes . . . N(6) C(36) C(41) 119.0(4) yes . . . C(37) C(36) C(41) 119.3(4) yes . . . C(36) C(37) C(38) 120.4(5) yes . . . C(37) C(38) C(39) 120.7(5) yes . . . C(38) C(39) C(40) 119.0(5) yes . . . C(39) C(40) C(41) 120.6(6) yes . . . C(36) C(41) C(40) 120.1(5) yes . . . N(1) C(1) H(1) 117.9 no . . . C(2) C(1) H(1) 118.0 no . . . C(1) C(2) H(2) 120.1 no . . . C(3) C(2) H(2) 120.1 no . . . C(3) C(4) H(3) 120.6 no . . . C(5) C(4) H(3) 120.6 no . . . N(1) C(5) H(4) 117.7 no . . . C(4) C(5) H(4) 117.7 no . . . C(6) C(7) H(5) 109.5 no . . . C(6) C(7) H(6) 109.5 no . . . C(6) C(7) H(7) 109.5 no . . . H(5) C(7) H(6) 109.5 no . . . H(5) C(7) H(7) 109.5 no . . . H(6) C(7) H(7) 109.5 no . . . C(6) C(8) H(8) 109.5 no . . . C(6) C(8) H(9) 109.5 no . . . C(6) C(8) H(10) 109.5 no . . . H(8) C(8) H(9) 109.5 no . . . H(8) C(8) H(10) 109.5 no . . . H(9) C(8) H(10) 109.5 no . . . C(6) C(9) H(11) 109.5 no . . . C(6) C(9) H(12) 109.5 no . . . C(6) C(9) H(13) 109.5 no . . . H(11) C(9) H(12) 109.5 no . . . H(11) C(9) H(13) 109.5 no . . . H(12) C(9) H(13) 109.5 no . . . N(3) C(10) H(14) 117.7 no . . . C(11) C(10) H(14) 117.7 no . . . C(10) C(11) H(15) 120.4 no . . . C(12) C(11) H(15) 120.4 no . . . C(12) C(13) H(16) 120.2 no . . . C(14) C(13) H(16) 120.2 no . . . N(3) C(14) H(17) 118.0 no . . . C(13) C(14) H(17) 118.0 no . . . C(15) C(16) H(18) 109.5 no . . . C(15) C(16) H(19) 109.5 no . . . C(15) C(16) H(20) 109.5 no . . . H(18) C(16) H(19) 109.5 no . . . H(18) C(16) H(20) 109.5 no . . . H(19) C(16) H(20) 109.5 no . . . C(15) C(17) H(21) 109.5 no . . . C(15) C(17) H(22) 109.5 no . . . C(15) C(17) H(23) 109.5 no . . . H(21) C(17) H(22) 109.5 no . . . H(21) C(17) H(23) 109.5 no . . . H(22) C(17) H(23) 109.5 no . . . C(15) C(18) H(24) 109.5 no . . . C(15) C(18) H(25) 109.5 no . . . C(15) C(18) H(26) 109.5 no . . . H(24) C(18) H(25) 109.5 no . . . H(24) C(18) H(26) 109.5 no . . . H(25) C(18) H(26) 109.5 no . . . C(20) C(21) H(27) 117.8 no . . . C(22) C(21) H(27) 117.8 no . . . C(26) C(25) H(28) 120.0 no . . . C(30) C(25) H(28) 120.0 no . . . C(25) C(26) H(29) 119.6 no . . . C(27) C(26) H(29) 119.6 no . . . C(26) C(27) H(30) 120.3 no . . . C(28) C(27) H(30) 120.3 no . . . C(27) C(28) H(31) 119.7 no . . . C(29) C(28) H(31) 119.7 no . . . C(28) C(29) H(32) 119.7 no . . . C(30) C(29) H(32) 119.7 no . . . C(32) C(33) H(33) 117.7 no . . . C(34) C(33) H(33) 117.7 no . . . C(36) C(37) H(34) 119.8 no . . . C(38) C(37) H(34) 119.8 no . . . C(37) C(38) H(35) 119.7 no . . . C(39) C(38) H(35) 119.6 no . . . C(38) C(39) H(36) 120.5 no . . . C(40) C(39) H(36) 120.5 no . . . C(39) C(40) H(37) 119.7 no . . . C(41) C(40) H(37) 119.7 no . . . C(36) C(41) H(38) 120.0 no . . . C(40) C(41) H(38) 120.0 no . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data__[CoBAMP(NCS)2D1py] _database_code_depnum_ccdc_archive 'CCDC 658521' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H32 Co N8 O S2 ' _chemical_formula_moiety 'C27 H32 Co N8 O S2 ' _chemical_formula_weight 607.66 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.8634(7) _cell_length_b 12.1032(9) _cell_length_c 12.5051(8) _cell_angle_alpha 115.1366(17) _cell_angle_beta 90.7389(17) _cell_angle_gamma 113.5048(18) _cell_volume 1454.24(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8341 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634.00 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 9059 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_theta_max 27.70 _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5388 _reflns_number_gt 3724 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.2128 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5388 _refine_ls_number_parameters 353 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0613P)^2^+7.3420P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.99 _refine_diff_density_min -1.22 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Co Co 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Co 0.39611(7) 0.07032(8) 0.78003(7) 0.0293(2) Uani 1.00 1 d . . . S(1) S 0.59627(18) 0.43056(18) 0.67824(17) 0.0491(4) Uani 1.00 1 d . . . S(2) S 0.12189(16) -0.26922(17) 0.88902(15) 0.0445(4) Uani 1.00 1 d . . . O(1) O 0.0505(4) 0.3560(4) 0.8771(3) 0.0404(10) Uani 1.00 1 d . . . N(1) N 0.2748(4) 0.1593(4) 0.8090(4) 0.0293(10) Uani 1.00 1 d . . . N(2) N 0.4590(4) 0.2241(4) 0.9861(4) 0.0290(10) Uani 1.00 1 d . . . N(3) N 0.2636(4) -0.0349(4) 0.5904(4) 0.0267(9) Uani 1.00 1 d . . . N(4) N 0.5167(4) 0.2143(5) 0.7339(4) 0.0349(11) Uani 1.00 1 d . . . N(5) N 0.2843(4) -0.0781(5) 0.8234(4) 0.0329(10) Uani 1.00 1 d . . . N(6) N 0.5254(4) -0.0163(4) 0.7469(4) 0.0303(10) Uani 1.00 1 d . . . N(7) N 0.9053(4) -0.0905(5) 0.7913(5) 0.0375(11) Uani 1.00 1 d . . . N(8) N 0.9923(5) -0.0273(6) 0.8626(5) 0.0535(15) Uani 1.00 1 d . . . C(1) C 0.2100(5) 0.1527(5) 0.7158(5) 0.0300(12) Uani 1.00 1 d . . . C(2) C 0.1321(5) 0.2149(6) 0.7311(5) 0.0340(12) Uani 1.00 1 d . . . C(3) C 0.1238(5) 0.2910(6) 0.8492(5) 0.0344(13) Uani 1.00 1 d . . . C(4) C 0.1936(5) 0.3009(6) 0.9466(5) 0.0353(13) Uani 1.00 1 d . . . C(5) C 0.2668(5) 0.2324(5) 0.9220(5) 0.0316(12) Uani 1.00 1 d . . . C(6) C 0.3402(5) 0.2271(6) 1.0179(5) 0.0323(12) Uani 1.00 1 d . . . C(7) C 0.5494(6) 0.3636(6) 1.0120(5) 0.0376(13) Uani 1.00 1 d . . . C(8) C 0.5113(6) 0.1838(6) 1.0630(5) 0.0386(14) Uani 1.00 1 d . . . C(9) C 0.2338(5) 0.0741(6) 0.5938(5) 0.0344(13) Uani 1.00 1 d . . . C(10) C 0.3237(5) -0.0774(6) 0.4863(5) 0.0349(13) Uani 1.00 1 d . . . C(11) C 0.1471(5) -0.1515(6) 0.5761(5) 0.0382(14) Uani 1.00 1 d . . . C(12) C -0.0277(5) 0.3444(6) 0.7797(5) 0.0379(13) Uani 1.00 1 d . . . C(13) C -0.1124(5) 0.4066(6) 0.8332(6) 0.0410(14) Uani 1.00 1 d . . . C(14) C 0.6476(5) 0.0650(5) 0.8074(5) 0.0309(12) Uani 1.00 1 d . . . C(15) C 0.7375(5) 0.0188(5) 0.7942(5) 0.0333(12) Uani 1.00 1 d . . . C(16) C 0.7073(5) -0.1175(5) 0.7161(5) 0.0307(12) Uani 1.00 1 d . . . C(17) C 0.5810(5) -0.2019(6) 0.6530(5) 0.0335(12) Uani 1.00 1 d . . . C(18) C 0.4965(5) -0.1480(5) 0.6711(5) 0.0308(12) Uani 1.00 1 d . . . C(19) C 0.8014(5) -0.1694(6) 0.7042(5) 0.0336(12) Uani 1.00 1 d . . . C(20) C 0.7984(5) -0.2965(5) 0.6061(5) 0.0319(12) Uani 1.00 1 d . . . C(21) C 0.8670(5) -0.3554(6) 0.6344(5) 0.0344(13) Uani 1.00 1 d . . . C(22) C 0.8706(6) -0.4685(6) 0.5430(6) 0.0447(16) Uani 1.00 1 d . . . C(23) C 0.8073(6) -0.5253(6) 0.4250(6) 0.0475(16) Uani 1.00 1 d . . . C(24) C 0.7378(6) -0.4687(6) 0.3987(6) 0.0436(15) Uani 1.00 1 d . . . C(25) C 0.7336(6) -0.3535(6) 0.4889(5) 0.0408(14) Uani 1.00 1 d . . . C(26) C 0.5500(5) 0.3043(6) 0.7109(5) 0.0310(12) Uani 1.00 1 d . . . C(27) C 0.2174(5) -0.1578(6) 0.8511(5) 0.0320(12) Uani 1.00 1 d . . . H(1) H 0.0863 0.2067 0.6649 0.041 Uiso 1.00 1 c R . . H(2) H 0.1908 0.3523 1.0258 0.042 Uiso 1.00 1 c R . . H(3) H 0.3591 0.3064 1.0953 0.039 Uiso 1.00 1 c R . . H(4) H 0.2894 0.1463 1.0257 0.039 Uiso 1.00 1 c R . . H(5) H 0.5326 0.4289 1.0781 0.045 Uiso 1.00 1 c R . . H(6) H 0.5404 0.3750 0.9415 0.045 Uiso 1.00 1 c R . . H(7) H 0.6337 0.3773 1.0332 0.045 Uiso 1.00 1 c R . . H(8) H 0.4437 0.1222 1.0812 0.046 Uiso 1.00 1 c R . . H(9) H 0.5639 0.2634 1.1369 0.046 Uiso 1.00 1 c R . . H(10) H 0.5604 0.1394 1.0209 0.046 Uiso 1.00 1 c R . . H(11) H 0.1596 0.0338 0.5311 0.041 Uiso 1.00 1 c R . . H(12) H 0.3034 0.1367 0.5769 0.041 Uiso 1.00 1 c R . . H(13) H 0.2599 -0.1508 0.4157 0.042 Uiso 1.00 1 c R . . H(14) H 0.3815 -0.1073 0.5049 0.042 Uiso 1.00 1 c R . . H(15) H 0.3684 -0.0016 0.4712 0.042 Uiso 1.00 1 c R . . H(16) H -0.0771 0.2492 0.7210 0.045 Uiso 1.00 1 c R . . H(17) H 0.0243 0.3916 0.7390 0.045 Uiso 1.00 1 c R . . H(18) H -0.1309 0.4449 0.7860 0.049 Uiso 1.00 1 c R . . H(19) H -0.0717 0.4772 0.9148 0.049 Uiso 1.00 1 c R . . H(20) H -0.1894 0.3378 0.8333 0.049 Uiso 1.00 1 c R . . H(21) H 0.6714 0.1564 0.8603 0.037 Uiso 1.00 1 c R . . H(22) H 0.8198 0.0791 0.8379 0.040 Uiso 1.00 1 c R . . H(23) H 0.5548 -0.2936 0.5994 0.040 Uiso 1.00 1 c R . . H(24) H 0.4136 -0.2061 0.6283 0.037 Uiso 1.00 1 c R . . H(25) H 0.9093 -0.3188 0.7135 0.041 Uiso 1.00 1 c R . . H(26) H 0.9166 -0.5075 0.5612 0.054 Uiso 1.00 1 c R . . H(27) H 0.8117 -0.6009 0.3642 0.057 Uiso 1.00 1 c R . . H(28) H 0.6933 -0.5078 0.3199 0.052 Uiso 1.00 1 c R . . H(29) H 0.6873 -0.3151 0.4701 0.049 Uiso 1.00 1 c R . . H(30) H 0.1317 -0.1400 0.6545 0.046 Uiso 1.00 1 c R . . H(31) H 0.1555 -0.2341 0.5339 0.046 Uiso 1.00 1 c R . . H(32) H 0.0778 -0.1565 0.5306 0.046 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0346(4) 0.0297(4) 0.0333(4) 0.0183(3) 0.0104(3) 0.0191(3) S(1) 0.0625(11) 0.0378(9) 0.0499(10) 0.0159(8) 0.0088(8) 0.0291(7) S(2) 0.0447(9) 0.0410(9) 0.0442(9) 0.0089(7) 0.0061(7) 0.0264(7) O(1) 0.050(2) 0.045(2) 0.041(2) 0.037(2) 0.0111(19) 0.019(2) N(1) 0.034(2) 0.029(2) 0.025(2) 0.015(2) 0.0087(19) 0.0114(19) N(2) 0.039(2) 0.029(2) 0.030(2) 0.021(2) 0.011(2) 0.018(2) N(3) 0.022(2) 0.029(2) 0.030(2) 0.0134(19) 0.0023(18) 0.0127(19) N(4) 0.039(2) 0.039(2) 0.041(2) 0.024(2) 0.014(2) 0.024(2) N(5) 0.034(2) 0.036(2) 0.036(2) 0.019(2) 0.009(2) 0.021(2) N(6) 0.036(2) 0.029(2) 0.032(2) 0.017(2) 0.013(2) 0.018(2) N(7) 0.034(2) 0.038(2) 0.045(3) 0.022(2) 0.012(2) 0.018(2) N(8) 0.049(3) 0.047(3) 0.055(3) 0.025(3) 0.004(3) 0.012(2) C(1) 0.032(2) 0.031(3) 0.032(2) 0.016(2) 0.007(2) 0.018(2) C(2) 0.040(3) 0.037(3) 0.031(2) 0.020(2) 0.003(2) 0.017(2) C(3) 0.036(3) 0.031(3) 0.037(3) 0.018(2) 0.007(2) 0.014(2) C(4) 0.045(3) 0.037(3) 0.032(3) 0.023(2) 0.008(2) 0.018(2) C(5) 0.035(3) 0.030(3) 0.038(3) 0.020(2) 0.008(2) 0.018(2) C(6) 0.039(3) 0.037(3) 0.029(2) 0.023(2) 0.009(2) 0.016(2) C(7) 0.047(3) 0.037(3) 0.035(3) 0.024(2) 0.011(2) 0.018(2) C(8) 0.045(3) 0.044(3) 0.038(3) 0.025(3) 0.006(2) 0.024(2) C(9) 0.043(3) 0.042(3) 0.028(2) 0.026(2) 0.012(2) 0.017(2) C(10) 0.040(3) 0.049(3) 0.025(2) 0.027(2) 0.013(2) 0.019(2) C(11) 0.035(3) 0.039(3) 0.032(3) 0.014(2) -0.003(2) 0.012(2) C(12) 0.033(3) 0.041(3) 0.044(3) 0.021(2) 0.003(2) 0.019(2) C(13) 0.034(3) 0.039(3) 0.052(3) 0.022(2) 0.008(2) 0.018(2) C(14) 0.033(2) 0.026(2) 0.035(3) 0.014(2) 0.010(2) 0.014(2) C(15) 0.035(3) 0.031(3) 0.035(3) 0.014(2) 0.007(2) 0.017(2) C(16) 0.039(3) 0.033(3) 0.031(2) 0.021(2) 0.015(2) 0.019(2) C(17) 0.037(3) 0.028(3) 0.037(3) 0.015(2) 0.009(2) 0.016(2) C(18) 0.036(3) 0.031(3) 0.030(2) 0.017(2) 0.005(2) 0.016(2) C(19) 0.032(2) 0.032(3) 0.038(3) 0.014(2) 0.003(2) 0.018(2) C(20) 0.031(2) 0.031(3) 0.035(3) 0.015(2) 0.007(2) 0.016(2) C(21) 0.032(2) 0.038(3) 0.045(3) 0.021(2) 0.012(2) 0.025(2) C(22) 0.037(3) 0.036(3) 0.065(4) 0.019(2) 0.018(3) 0.025(3) C(23) 0.054(4) 0.038(3) 0.052(4) 0.028(3) 0.022(3) 0.015(3) C(24) 0.051(3) 0.036(3) 0.039(3) 0.017(3) 0.011(2) 0.016(2) C(25) 0.045(3) 0.038(3) 0.046(3) 0.023(3) 0.013(2) 0.021(2) C(26) 0.033(2) 0.033(3) 0.033(3) 0.016(2) 0.010(2) 0.019(2) C(27) 0.031(2) 0.033(3) 0.027(2) 0.014(2) -0.005(2) 0.011(2) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co(1) N(1) 2.069(6) yes . . Co(1) N(2) 2.331(4) yes . . Co(1) N(3) 2.336(4) yes . . Co(1) N(4) 2.075(6) yes . . Co(1) N(5) 2.055(6) yes . . Co(1) N(6) 2.134(6) yes . . S(1) C(26) 1.634(8) yes . . S(2) C(27) 1.632(7) yes . . O(1) C(3) 1.349(9) yes . . O(1) C(12) 1.444(9) yes . . N(1) C(1) 1.343(9) yes . . N(1) C(5) 1.341(7) yes . . N(2) C(6) 1.480(8) yes . . N(2) C(7) 1.479(7) yes . . N(2) C(8) 1.473(11) yes . . N(3) C(9) 1.481(10) yes . . N(3) C(10) 1.489(8) yes . . N(3) C(11) 1.469(7) yes . . N(4) C(26) 1.162(10) yes . . N(5) C(27) 1.167(8) yes . . N(6) C(14) 1.358(6) yes . . N(6) C(18) 1.352(7) yes . . N(7) N(8) 1.101(7) yes . . N(7) C(19) 1.327(7) yes . . C(1) C(2) 1.377(11) yes . . C(1) C(9) 1.518(8) yes . . C(2) C(3) 1.400(8) yes . . C(3) C(4) 1.397(10) yes . . C(4) C(5) 1.378(11) yes . . C(5) C(6) 1.511(11) yes . . C(12) C(13) 1.489(11) yes . . C(14) C(15) 1.370(10) yes . . C(15) C(16) 1.398(8) yes . . C(16) C(17) 1.406(7) yes . . C(16) C(19) 1.465(10) yes . . C(17) C(18) 1.372(11) yes . . C(19) C(20) 1.492(8) yes . . C(20) C(21) 1.402(12) yes . . C(20) C(25) 1.380(9) yes . . C(21) C(22) 1.378(9) yes . . C(22) C(23) 1.383(10) yes . . C(23) C(24) 1.376(13) yes . . C(24) C(25) 1.393(9) yes . . C(2) H(1) 0.930 no . . C(4) H(2) 0.930 no . . C(6) H(3) 0.970 no . . C(6) H(4) 0.970 no . . C(7) H(5) 0.960 no . . C(7) H(6) 0.960 no . . C(7) H(7) 0.960 no . . C(8) H(8) 0.960 no . . C(8) H(9) 0.960 no . . C(8) H(10) 0.960 no . . C(9) H(11) 0.970 no . . C(9) H(12) 0.970 no . . C(10) H(13) 0.960 no . . C(10) H(14) 0.960 no . . C(10) H(15) 0.960 no . . C(11) H(30) 0.960 no . . C(11) H(31) 0.960 no . . C(11) H(32) 0.960 no . . C(12) H(16) 0.970 no . . C(12) H(17) 0.970 no . . C(13) H(18) 0.960 no . . C(13) H(19) 0.960 no . . C(13) H(20) 0.960 no . . C(14) H(21) 0.930 no . . C(15) H(22) 0.930 no . . C(17) H(23) 0.930 no . . C(18) H(24) 0.930 no . . C(21) H(25) 0.930 no . . C(22) H(26) 0.930 no . . C(23) H(27) 0.930 no . . C(24) H(28) 0.930 no . . C(25) H(29) 0.930 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Co(1) N(2) 75.73(19) yes . . . N(1) Co(1) N(3) 75.36(18) yes . . . N(1) Co(1) N(4) 90.4(2) yes . . . N(1) Co(1) N(5) 93.3(2) yes . . . N(1) Co(1) N(6) 177.6(2) yes . . . N(2) Co(1) N(3) 151.1(2) yes . . . N(2) Co(1) N(4) 92.98(18) yes . . . N(2) Co(1) N(5) 88.08(18) yes . . . N(2) Co(1) N(6) 104.82(19) yes . . . N(3) Co(1) N(4) 87.70(19) yes . . . N(3) Co(1) N(5) 93.08(18) yes . . . N(3) Co(1) N(6) 104.09(18) yes . . . N(4) Co(1) N(5) 176.3(2) yes . . . N(4) Co(1) N(6) 87.3(2) yes . . . N(5) Co(1) N(6) 89.0(2) yes . . . C(3) O(1) C(12) 118.7(4) yes . . . Co(1) N(1) C(1) 120.5(3) yes . . . Co(1) N(1) C(5) 120.2(4) yes . . . C(1) N(1) C(5) 119.2(6) yes . . . Co(1) N(2) C(6) 102.8(2) yes . . . Co(1) N(2) C(7) 112.8(3) yes . . . Co(1) N(2) C(8) 115.2(3) yes . . . C(6) N(2) C(7) 108.0(5) yes . . . C(6) N(2) C(8) 109.1(5) yes . . . C(7) N(2) C(8) 108.6(4) yes . . . Co(1) N(3) C(9) 102.8(2) yes . . . Co(1) N(3) C(10) 114.3(3) yes . . . Co(1) N(3) C(11) 111.2(4) yes . . . C(9) N(3) C(10) 108.6(5) yes . . . C(9) N(3) C(11) 109.5(5) yes . . . C(10) N(3) C(11) 110.1(4) yes . . . Co(1) N(4) C(26) 157.1(5) yes . . . Co(1) N(5) C(27) 176.1(5) yes . . . Co(1) N(6) C(14) 118.6(4) yes . . . Co(1) N(6) C(18) 125.7(3) yes . . . C(14) N(6) C(18) 115.7(6) yes . . . N(8) N(7) C(19) 178.4(8) yes . . . N(1) C(1) C(2) 122.6(5) yes . . . N(1) C(1) C(9) 113.7(6) yes . . . C(2) C(1) C(9) 123.6(6) yes . . . C(1) C(2) C(3) 118.0(6) yes . . . O(1) C(3) C(2) 124.2(6) yes . . . O(1) C(3) C(4) 116.3(5) yes . . . C(2) C(3) C(4) 119.5(7) yes . . . C(3) C(4) C(5) 118.3(5) yes . . . N(1) C(5) C(4) 122.4(6) yes . . . N(1) C(5) C(6) 113.8(6) yes . . . C(4) C(5) C(6) 123.7(5) yes . . . N(2) C(6) C(5) 110.8(5) yes . . . N(3) C(9) C(1) 111.8(6) yes . . . O(1) C(12) C(13) 107.8(5) yes . . . N(6) C(14) C(15) 123.1(5) yes . . . C(14) C(15) C(16) 121.0(4) yes . . . C(15) C(16) C(17) 116.0(6) yes . . . C(15) C(16) C(19) 121.7(4) yes . . . C(17) C(16) C(19) 122.3(5) yes . . . C(16) C(17) C(18) 119.4(5) yes . . . N(6) C(18) C(17) 124.7(4) yes . . . N(7) C(19) C(16) 115.5(5) yes . . . N(7) C(19) C(20) 115.4(6) yes . . . C(16) C(19) C(20) 129.1(4) yes . . . C(19) C(20) C(21) 118.4(5) yes . . . C(19) C(20) C(25) 121.5(7) yes . . . C(21) C(20) C(25) 120.0(6) yes . . . C(20) C(21) C(22) 118.9(6) yes . . . C(21) C(22) C(23) 121.5(8) yes . . . C(22) C(23) C(24) 119.1(6) yes . . . C(23) C(24) C(25) 120.6(6) yes . . . C(20) C(25) C(24) 119.7(8) yes . . . S(1) C(26) N(4) 179.8(6) yes . . . S(2) C(27) N(5) 179.1(7) yes . . . C(1) C(2) H(1) 121.0 no . . . C(3) C(2) H(1) 121.0 no . . . C(3) C(4) H(2) 120.9 no . . . C(5) C(4) H(2) 120.9 no . . . N(2) C(6) H(3) 109.5 no . . . N(2) C(6) H(4) 109.5 no . . . C(5) C(6) H(3) 109.5 no . . . C(5) C(6) H(4) 109.5 no . . . H(3) C(6) H(4) 108.1 no . . . N(2) C(7) H(5) 109.5 no . . . N(2) C(7) H(6) 109.5 no . . . N(2) C(7) H(7) 109.5 no . . . H(5) C(7) H(6) 109.5 no . . . H(5) C(7) H(7) 109.5 no . . . H(6) C(7) H(7) 109.5 no . . . N(2) C(8) H(8) 109.5 no . . . N(2) C(8) H(9) 109.5 no . . . N(2) C(8) H(10) 109.5 no . . . H(8) C(8) H(9) 109.5 no . . . H(8) C(8) H(10) 109.5 no . . . H(9) C(8) H(10) 109.5 no . . . N(3) C(9) H(11) 109.3 no . . . N(3) C(9) H(12) 109.2 no . . . C(1) C(9) H(11) 109.3 no . . . C(1) C(9) H(12) 109.2 no . . . H(11) C(9) H(12) 107.9 no . . . N(3) C(10) H(13) 109.5 no . . . N(3) C(10) H(14) 109.5 no . . . N(3) C(10) H(15) 109.5 no . . . H(13) C(10) H(14) 109.5 no . . . H(13) C(10) H(15) 109.5 no . . . H(14) C(10) H(15) 109.5 no . . . N(3) C(11) H(30) 109.5 no . . . N(3) C(11) H(31) 109.5 no . . . N(3) C(11) H(32) 109.5 no . . . H(30) C(11) H(31) 109.5 no . . . H(30) C(11) H(32) 109.5 no . . . H(31) C(11) H(32) 109.5 no . . . O(1) C(12) H(16) 110.2 no . . . O(1) C(12) H(17) 110.1 no . . . C(13) C(12) H(16) 110.2 no . . . C(13) C(12) H(17) 110.2 no . . . H(16) C(12) H(17) 108.5 no . . . C(12) C(13) H(18) 109.5 no . . . C(12) C(13) H(19) 109.5 no . . . C(12) C(13) H(20) 109.5 no . . . H(18) C(13) H(19) 109.5 no . . . H(18) C(13) H(20) 109.5 no . . . H(19) C(13) H(20) 109.5 no . . . N(6) C(14) H(21) 118.4 no . . . C(15) C(14) H(21) 118.4 no . . . C(14) C(15) H(22) 119.5 no . . . C(16) C(15) H(22) 119.5 no . . . C(16) C(17) H(23) 120.3 no . . . C(18) C(17) H(23) 120.3 no . . . N(6) C(18) H(24) 117.7 no . . . C(17) C(18) H(24) 117.7 no . . . C(20) C(21) H(25) 120.5 no . . . C(22) C(21) H(25) 120.6 no . . . C(21) C(22) H(26) 119.2 no . . . C(23) C(22) H(26) 119.3 no . . . C(22) C(23) H(27) 120.4 no . . . C(24) C(23) H(27) 120.4 no . . . C(23) C(24) H(28) 119.7 no . . . C(25) C(24) H(28) 119.7 no . . . C(20) C(25) H(29) 120.1 no . . . C(24) C(25) H(29) 120.1 no . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '[Co_hfpip_2_4NOpy_2].CIF' # TEXT _publ_section_references ; Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ;