data_General _audit_creation_date '2006-12-26' _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Satoru Karasawa' _publ_contact_author_email 'ENTER EMAIL ADDRESS' _publ_contact_author_fax 'ENTER FAX NUMBER' _publ_contact_author_phone 'ENTER PHONE NUMBER' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'ENTER JOURNAL NAME HERE' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER 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. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data__061020tBuPhNOpyCoNCS #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; tert-butylphenyl)-N-oxylamino}pyridine]di(thiocyanato-N)cobalt(II) ; _chemical_formula_sum 'C62 H68 Co N10 O4 S2 ' _chemical_formula_moiety 'C62 H68 Co N10 O4 S2 ' _chemical_formula_weight 1140.34 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '-X,1/2+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '+X,1/2-Y,1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 17.0307(11) _cell_length_b 21.0325(13) _cell_length_c 10.8981(8) _cell_angle_alpha 90.0000 _cell_angle_beta 129.7325(18) _cell_angle_gamma 90.0000 _cell_volume 3002.1(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 12452 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.6 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1202.00 _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.960 #============================================================================== # 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 24397 _diffrn_reflns_av_R_equivalents 0.107 _diffrn_reflns_theta_max 25.65 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 #============================================================================== # 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 5586 _reflns_number_gt 3149 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1720 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5586 _refine_ls_number_parameters 360 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0617P)^2^+2.5488P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.55 _refine_diff_density_min -0.83 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(7) 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) ; 'S' 'S' 0.125 0.123 ; 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 Co1 Co 0.0000 0.0000 0.5000 0.0329(3) Uani 1 2 d S . . S1 S -0.34326(9) 0.02677(8) -0.00220(16) 0.0697(5) Uani 1 1 d . . . O1 O 0.0819(3) 0.30117(14) 0.3015(4) 0.0539(9) Uani 1 1 d . . . O2 O 0.0971(3) -0.1231(2) 0.0074(4) 0.0758(12) Uani 1 1 d . . . N1 N 0.0456(2) 0.09273(16) 0.4705(4) 0.0367(8) Uani 1 1 d . . . N2 N 0.1127(3) 0.28146(17) 0.4393(4) 0.0413(9) Uani 1 1 d . . . N3 N 0.0425(2) -0.05426(16) 0.3766(4) 0.0369(8) Uani 1 1 d . . . N4 N 0.1364(3) -0.1457(2) 0.1458(4) 0.0489(10) Uani 1 1 d . . . N5 N -0.1447(2) 0.01396(16) 0.2857(4) 0.0379(9) Uani 1 1 d . . . C1 C -0.0103(3) 0.1252(2) 0.3321(5) 0.0381(10) Uani 1 1 d . . . H1 H -0.0658 0.1047 0.2412 0.046 Uiso 1 1 calc R . . C2 C 0.0092(3) 0.1869(2) 0.3161(5) 0.0385(10) Uani 1 1 d . . . H2 H -0.0310 0.2069 0.2171 0.046 Uiso 1 1 calc R . . C3 C 0.0907(3) 0.2183(2) 0.4518(5) 0.0370(10) Uani 1 1 d . . . C4 C 0.1516(3) 0.1855(2) 0.5968(5) 0.0377(10) Uani 1 1 d . . . H4 H 0.2081 0.2048 0.6890 0.045 Uiso 1 1 calc R . . C5 C 0.1257(3) 0.1241(2) 0.5992(5) 0.0379(10) Uani 1 1 d . . . H5 H 0.1661 0.1026 0.6962 0.045 Uiso 1 1 calc R . . C6 C 0.1675(3) 0.3248(2) 0.5708(5) 0.0378(10) Uani 1 1 d . . . C7 C 0.2297(3) 0.3703(2) 0.5792(6) 0.0458(12) Uani 1 1 d . . . H7 H 0.2364 0.3721 0.5011 0.055 Uiso 1 1 calc R . . C8 C 0.2813(3) 0.4129(2) 0.7041(6) 0.0437(11) Uani 1 1 d . . . H8 H 0.3240 0.4427 0.7102 0.052 Uiso 1 1 calc R . . C9 C 0.2714(3) 0.4127(2) 0.8218(5) 0.0361(10) Uani 1 1 d . . . C10 C 0.2061(3) 0.3676(2) 0.8070(5) 0.0400(11) Uani 1 1 d . . . H10 H 0.1970 0.3669 0.8825 0.048 Uiso 1 1 calc R . . C11 C 0.1541(3) 0.3237(2) 0.6838(5) 0.0400(10) Uani 1 1 d . . . H11 H 0.1110 0.2940 0.6770 0.048 Uiso 1 1 calc R . . C12 C 0.3326(3) 0.4586(2) 0.9619(5) 0.0432(11) Uani 1 1 d . . . C13 C 0.2922(4) 0.4633(3) 1.0527(6) 0.0624(15) Uani 1 1 d . . . H13A H 0.2208 0.4736 0.9796 0.094 Uiso 1 1 calc R . . H13B H 0.3287 0.4960 1.1323 0.094 Uiso 1 1 calc R . . H13C H 0.3018 0.4234 1.1032 0.094 Uiso 1 1 calc R . . C14 C 0.4433(4) 0.4358(3) 1.0753(7) 0.083(2) Uani 1 1 d . . . H14A H 0.4471 0.3959 1.1215 0.124 Uiso 1 1 calc R . . H14B H 0.4847 0.4667 1.1583 0.124 Uiso 1 1 calc R . . H14C H 0.4677 0.4306 1.0172 0.124 Uiso 1 1 calc R . . C15 C 0.3279(5) 0.5254(2) 0.8990(7) 0.0675(16) Uani 1 1 d . . . H15A H 0.2580 0.5383 0.8210 0.101 Uiso 1 1 calc R . . H15B H 0.3594 0.5243 0.8509 0.101 Uiso 1 1 calc R . . H15C H 0.3635 0.5551 0.9860 0.101 Uiso 1 1 calc R . . C16 C 0.1160(3) -0.0996(2) 0.4519(5) 0.0379(10) Uani 1 1 d . . . H16 H 0.1463 -0.1090 0.5571 0.045 Uiso 1 1 calc R . . C17 C 0.1489(3) -0.1326(2) 0.3835(5) 0.0392(10) Uani 1 1 d . . . H17 H 0.1997 -0.1633 0.4406 0.047 Uiso 1 1 calc R . . C18 C 0.1037(3) -0.1185(2) 0.2254(5) 0.0401(11) Uani 1 1 d . . . C19 C 0.0254(3) -0.0737(2) 0.1434(5) 0.0421(11) Uani 1 1 d . . . H19 H -0.0080 -0.0648 0.0367 0.051 Uiso 1 1 calc R . . C20 C -0.0019(3) -0.0427(2) 0.2227(5) 0.0385(10) Uani 1 1 d . . . H20 H -0.0534 -0.0124 0.1674 0.046 Uiso 1 1 calc R . . C21 C 0.2222(3) -0.1877(2) 0.2152(5) 0.0429(11) Uani 1 1 d . . . C22 C 0.2345(4) -0.2435(2) 0.2925(6) 0.0502(12) Uani 1 1 d . . . H22 H 0.1874 -0.2547 0.3055 0.060 Uiso 1 1 calc R . . C23 C 0.3176(4) -0.2834(2) 0.3513(6) 0.0513(12) Uani 1 1 d . . . H23 H 0.3247 -0.3210 0.4023 0.062 Uiso 1 1 calc R . . C24 C 0.3900(3) -0.2677(2) 0.3349(5) 0.0434(11) Uani 1 1 d . A . C25 C 0.3741(3) -0.2111(2) 0.2531(5) 0.0458(12) Uani 1 1 d . . . H25 H 0.4204 -0.1999 0.2384 0.055 Uiso 1 1 calc R . . C26 C 0.2920(3) -0.1716(2) 0.1937(6) 0.0469(12) Uani 1 1 d . . . H26 H 0.2834 -0.1345 0.1397 0.056 Uiso 1 1 calc R . . C27 C 0.4809(4) -0.3110(2) 0.3987(6) 0.0532(13) Uani 1 1 d . . . C28 C 0.5337(10) -0.3308(7) 0.5724(16) 0.062(4) Uiso 0.569(17) 1 d P A 2 H28A H 0.4831 -0.3367 0.5846 0.093 Uiso 0.569(17) 1 calc PR A 2 H28B H 0.5806 -0.2982 0.6440 0.093 Uiso 0.569(17) 1 calc PR A 2 H28C H 0.5701 -0.3699 0.5963 0.093 Uiso 0.569(17) 1 calc PR A 2 C29 C 0.5560(9) -0.2853(6) 0.3905(17) 0.075(4) Uiso 0.569(17) 1 d P A 2 H29A H 0.5254 -0.2524 0.3113 0.112 Uiso 0.569(17) 1 calc PR A 2 H29B H 0.5806 -0.3185 0.3623 0.112 Uiso 0.569(17) 1 calc PR A 2 H29C H 0.6119 -0.2680 0.4925 0.112 Uiso 0.569(17) 1 calc PR A 2 C30 C 0.4347(7) -0.3754(5) 0.2954(11) 0.054(3) Uiso 0.569(17) 1 d P A 2 H30A H 0.3664 -0.3816 0.2567 0.081 Uiso 0.569(17) 1 calc PR A 2 H30B H 0.4763 -0.4108 0.3612 0.081 Uiso 0.569(17) 1 calc PR A 2 H30C H 0.4338 -0.3723 0.2066 0.081 Uiso 0.569(17) 1 calc PR A 2 C31 C 0.5199(13) -0.3481(9) 0.548(2) 0.066(6) Uiso 0.431(17) 1 d P A 1 H31A H 0.4654 -0.3539 0.5511 0.099 Uiso 0.431(17) 1 calc PR A 1 H31B H 0.5745 -0.3250 0.6405 0.099 Uiso 0.431(17) 1 calc PR A 1 H31C H 0.5444 -0.3889 0.5457 0.099 Uiso 0.431(17) 1 calc PR A 1 C32 C 0.5795(10) -0.2645(7) 0.4587(18) 0.055(4) Uiso 0.431(17) 1 d P A 1 H32A H 0.5663 -0.2218 0.4719 0.083 Uiso 0.431(17) 1 calc PR A 1 H32B H 0.5884 -0.2653 0.3802 0.083 Uiso 0.431(17) 1 calc PR A 1 H32C H 0.6404 -0.2799 0.5585 0.083 Uiso 0.431(17) 1 calc PR A 1 C33 C 0.4600(12) -0.3471(9) 0.2674(18) 0.081(6) Uiso 0.431(17) 1 d P A 1 H33A H 0.3881 -0.3558 0.1904 0.122 Uiso 0.431(17) 1 calc PR A 1 H33B H 0.4970 -0.3865 0.3069 0.122 Uiso 0.431(17) 1 calc PR A 1 H33C H 0.4809 -0.3231 0.2179 0.122 Uiso 0.431(17) 1 calc PR A 1 C34 C -0.2273(3) 0.0191(2) 0.1655(5) 0.0370(10) 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 Co1 0.0332(4) 0.0397(5) 0.0239(4) -0.0010(4) 0.0175(3) 0.0028(4) S1 0.0401(7) 0.0969(12) 0.0405(8) -0.0140(7) 0.0112(6) 0.0147(7) O1 0.089(2) 0.0440(19) 0.045(2) 0.0041(15) 0.0500(19) 0.0025(17) O2 0.069(2) 0.125(3) 0.034(2) 0.007(2) 0.0330(18) 0.032(2) N1 0.0412(19) 0.042(2) 0.0270(19) 0.0001(16) 0.0218(16) 0.0062(17) N2 0.055(2) 0.041(2) 0.038(2) 0.0009(17) 0.0343(19) 0.0014(18) N3 0.0376(18) 0.042(2) 0.031(2) -0.0021(17) 0.0219(16) -0.0005(17) N4 0.046(2) 0.072(3) 0.029(2) -0.006(2) 0.0239(18) 0.010(2) N5 0.0386(19) 0.041(2) 0.031(2) -0.0007(16) 0.0208(17) 0.0028(16) C1 0.037(2) 0.047(3) 0.030(2) -0.003(2) 0.0215(19) 0.001(2) C2 0.047(2) 0.043(3) 0.033(2) 0.007(2) 0.028(2) 0.008(2) C3 0.047(2) 0.034(2) 0.037(2) 0.002(2) 0.030(2) 0.004(2) C4 0.041(2) 0.037(2) 0.031(2) -0.0051(19) 0.021(2) -0.004(2) C5 0.042(2) 0.044(3) 0.025(2) -0.0041(19) 0.0202(19) 0.001(2) C6 0.048(2) 0.036(2) 0.035(2) 0.001(2) 0.029(2) 0.003(2) C7 0.056(3) 0.045(3) 0.054(3) 0.002(2) 0.043(3) 0.000(2) C8 0.044(2) 0.048(3) 0.051(3) 0.002(2) 0.036(2) -0.001(2) C9 0.035(2) 0.040(2) 0.037(2) 0.001(2) 0.025(2) 0.0019(19) C10 0.049(2) 0.043(3) 0.036(3) -0.001(2) 0.031(2) -0.004(2) C11 0.050(2) 0.042(3) 0.036(3) -0.003(2) 0.032(2) -0.004(2) C12 0.040(2) 0.046(3) 0.044(3) -0.004(2) 0.027(2) -0.007(2) C13 0.085(4) 0.061(3) 0.059(3) -0.023(3) 0.054(3) -0.024(3) C14 0.045(3) 0.108(5) 0.058(4) -0.015(3) 0.016(3) 0.001(3) C15 0.101(4) 0.049(3) 0.079(4) -0.014(3) 0.070(4) -0.018(3) C16 0.040(2) 0.045(3) 0.029(2) -0.003(2) 0.0224(19) 0.004(2) C17 0.040(2) 0.045(3) 0.032(2) -0.001(2) 0.023(2) 0.006(2) C18 0.040(2) 0.051(3) 0.029(2) -0.010(2) 0.022(2) -0.002(2) C19 0.040(2) 0.061(3) 0.022(2) -0.004(2) 0.0175(19) 0.001(2) C20 0.041(2) 0.046(3) 0.028(2) -0.002(2) 0.0217(19) 0.002(2) C21 0.038(2) 0.055(3) 0.038(3) -0.010(2) 0.025(2) 0.004(2) C22 0.056(3) 0.059(3) 0.054(3) -0.013(3) 0.043(3) -0.008(2) C23 0.063(3) 0.047(3) 0.063(3) 0.001(3) 0.049(3) -0.001(2) C24 0.048(2) 0.044(3) 0.049(3) -0.006(2) 0.036(2) -0.002(2) C25 0.047(3) 0.052(3) 0.051(3) -0.003(2) 0.038(2) -0.001(2) C26 0.053(3) 0.054(3) 0.047(3) -0.004(2) 0.038(2) 0.002(2) C27 0.058(3) 0.057(3) 0.057(3) 0.003(3) 0.043(3) 0.011(2) C34 0.044(2) 0.040(2) 0.030(2) -0.0018(19) 0.025(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 2.063(3) . ? Co1 N5 2.063(3) 3_556 ? Co1 N1 2.197(4) 3_556 ? Co1 N1 2.197(4) . ? Co1 N3 2.209(3) . ? Co1 N3 2.209(3) 3_556 ? S1 C34 1.628(4) . ? O1 N2 1.302(4) . ? O2 N4 1.288(5) . ? N1 C1 1.346(5) . ? N1 C5 1.348(5) . ? N2 C3 1.411(5) . ? N2 C6 1.430(5) . ? N3 C20 1.350(5) . ? N3 C16 1.356(5) . ? N4 C18 1.416(5) . ? N4 C21 1.440(5) . ? N5 C34 1.163(5) . ? C1 C2 1.377(6) . ? C1 H1 0.9300 . ? C2 C3 1.387(6) . ? C2 H2 0.9300 . ? C3 C4 1.397(6) . ? C4 C5 1.370(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.387(6) . ? C6 C11 1.389(6) . ? C7 C8 1.377(6) . ? C7 H7 0.9300 . ? C8 C9 1.397(6) . ? C8 H8 0.9300 . ? C9 C10 1.390(6) . ? C9 C12 1.522(6) . ? C10 C11 1.386(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.527(7) . ? C12 C14 1.528(6) . ? C12 C15 1.542(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.372(6) . ? C16 H16 0.9300 . ? C17 C18 1.398(6) . ? C17 H17 0.9300 . ? C18 C19 1.395(6) . ? C19 C20 1.378(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.381(7) . ? C21 C26 1.393(6) . ? C22 C23 1.399(6) . ? C22 H22 0.9300 . ? C23 C24 1.393(6) . ? C23 H23 0.9300 . ? C24 C25 1.406(6) . ? C24 C27 1.527(6) . ? C25 C26 1.381(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C29 1.443(12) . ? C27 C33 1.450(16) . ? C27 C31 1.519(18) . ? C27 C28 1.545(14) . ? C27 C30 1.610(10) . ? C27 C32 1.673(14) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 N5 Co1 N5 180.0 . 3_556 ? N5 Co1 N1 90.81(13) . 3_556 ? N5 Co1 N1 89.19(13) 3_556 3_556 ? N5 Co1 N1 89.19(13) . . ? N5 Co1 N1 90.81(13) 3_556 . ? N1 Co1 N1 180.0 3_556 . ? N5 Co1 N3 90.17(13) . . ? N5 Co1 N3 89.83(13) 3_556 . ? N1 Co1 N3 85.07(12) 3_556 . ? N1 Co1 N3 94.93(12) . . ? N5 Co1 N3 89.83(13) . 3_556 ? N5 Co1 N3 90.17(13) 3_556 3_556 ? N1 Co1 N3 94.93(12) 3_556 3_556 ? N1 Co1 N3 85.07(12) . 3_556 ? N3 Co1 N3 180.00(15) . 3_556 ? C1 N1 C5 116.0(4) . . ? C1 N1 Co1 123.5(3) . . ? C5 N1 Co1 119.9(3) . . ? O1 N2 C3 118.4(3) . . ? O1 N2 C6 118.5(3) . . ? C3 N2 C6 123.2(4) . . ? C20 N3 C16 116.4(4) . . ? C20 N3 Co1 121.5(3) . . ? C16 N3 Co1 122.1(3) . . ? O2 N4 C18 117.0(4) . . ? O2 N4 C21 115.8(4) . . ? C18 N4 C21 126.1(4) . . ? C34 N5 Co1 177.0(4) . . ? N1 C1 C2 124.4(4) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 118.1(4) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C2 C3 C4 119.0(4) . . ? C2 C3 N2 119.4(4) . . ? C4 C3 N2 121.5(4) . . ? C5 C4 C3 118.1(4) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 124.4(4) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? C7 C6 C11 120.3(4) . . ? C7 C6 N2 119.2(4) . . ? C11 C6 N2 120.4(4) . . ? C8 C7 C6 119.5(4) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 122.0(4) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 116.9(4) . . ? C10 C9 C12 122.2(4) . . ? C8 C9 C12 120.8(4) . . ? C11 C10 C9 122.4(4) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C6 118.9(4) . . ? C10 C11 H11 120.6 . . ? C6 C11 H11 120.6 . . ? C9 C12 C13 112.8(4) . . ? C9 C12 C14 108.2(4) . . ? C13 C12 C14 109.3(4) . . ? C9 C12 C15 108.9(4) . . ? C13 C12 C15 108.2(4) . . ? C14 C12 C15 109.3(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 124.5(4) . . ? N3 C16 H16 117.7 . . ? C17 C16 H16 117.7 . . ? C16 C17 C18 117.9(4) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C19 C18 C17 118.7(4) . . ? C19 C18 N4 118.1(4) . . ? C17 C18 N4 123.2(4) . . ? C20 C19 C18 119.1(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? N3 C20 C19 123.3(4) . . ? N3 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? C22 C21 C26 119.7(4) . . ? C22 C21 N4 123.4(4) . . ? C26 C21 N4 116.8(4) . . ? C21 C22 C23 120.2(4) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 121.2(5) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 117.0(4) . . ? C23 C24 C27 121.5(4) . . ? C25 C24 C27 121.5(4) . . ? C26 C25 C24 122.2(4) . . ? C26 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C25 C26 C21 119.5(5) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C33 C27 C31 116.7(10) . . ? C29 C27 C24 115.4(6) . . ? C33 C27 C24 109.0(7) . . ? C31 C27 C24 114.6(8) . . ? C29 C27 C28 109.4(8) . . ? C24 C27 C28 110.2(6) . . ? C29 C27 C30 109.1(7) . . ? C24 C27 C30 106.5(5) . . ? C28 C27 C30 105.7(7) . . ? C33 C27 C32 104.1(9) . . ? C31 C27 C32 103.8(9) . . ? C24 C27 C32 107.5(6) . . ? C30 C27 C32 133.2(7) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N5 C34 S1 179.6(4) . . ? #============================================================================== _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR2004' _computing_structure_refinement 'SHELXL' _computing_publication_material 'CrystalStructure 3.8' #============================================================================== # 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 #==============================================================================