# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_af523 _database_code_depnum_ccdc_archive 'CCDC 890986' #TrackingRef '[Co2TPPS(bipy)(H2O)4]3H2O.cif' _audit_creation_date 2012-06-07T09:34:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H24 Co N4 O8 S2, 1.08(O2), 3.84(O)' _chemical_formula_sum 'C32 H24 Co N4 O14 S2' _chemical_formula_weight 811.6 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/A' _space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 17.9776(2) _cell_length_b 17.9776(2) _cell_length_c 22.3567(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7225.55(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7629 _cell_measurement_theta_min 2.4557 _cell_measurement_theta_max 76.101 _cell_measurement_wavelength 1.54184 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.1198 _exptl_crystal_size_mid 0.1183 _exptl_crystal_size_min 0.021 _exptl_crystal_density_meas 1.488(4) _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method Flotation _exptl_crystal_F_000 3320 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -12 -1 0.0493 0 12 1 0.069 12 0 1 0.0545 -12 0 -1 0.0644 1 2 -14 0.0132 1 -1 -14 0.0116 -1 -1 14 0.0082 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.445 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.563 _exptl_absorpt_correction_T_max 0.908 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 5.2012 _diffrn_orient_matrix_ub_11 0.0053018 _diffrn_orient_matrix_ub_12 0.0027647 _diffrn_orient_matrix_ub_13 -0.0687225 _diffrn_orient_matrix_ub_21 -0.0850074 _diffrn_orient_matrix_ub_22 -0.0093884 _diffrn_orient_matrix_ub_23 -0.0044889 _diffrn_orient_matrix_ub_31 -0.0095252 _diffrn_orient_matrix_ub_32 0.0851435 _diffrn_orient_matrix_ub_33 0.0017681 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_number 23662 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 76.26 _diffrn_reflns_theta_full 76.26 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 3774 _reflns_number_gt 2890 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia,1997)' _computing_publication_material 'WinGX publication routines (Farrugia,1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1308P)^2^+8.3686P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3774 _refine_ls_number_parameters 274 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.204 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.004 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.117 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.8891(2) 0.1260(2) 0.13283(15) 0.0312(7) Uani 1 1 d . . . C2 C 0.8833(2) 0.0471(2) 0.12434(15) 0.0368(8) Uani 1 1 d . . . H2 H 0.8396 0.0179 0.1292 0.044 Uiso 1 1 calc R . . C3 C 0.9508(2) 0.0219(2) 0.10820(17) 0.0368(8) Uani 1 1 d . . . H3 H 0.9633 -0.0279 0.0984 0.044 Uiso 1 1 calc R . . C4 C 1.0003(2) 0.08443(19) 0.10856(14) 0.0307(7) Uani 1 1 d . . . C5 C 0.8297(2) 0.1729(2) 0.14615(14) 0.0319(7) Uani 1 1 d . . . C6 C 0.7578(2) 0.1366(2) 0.16030(16) 0.0336(7) Uani 1 1 d . . . C7 C 0.7019(2) 0.1305(2) 0.11775(17) 0.0384(8) Uani 1 1 d . . . H7 H 0.7059 0.1573 0.0812 0.046 Uiso 1 1 calc R . . C8 C 0.6406(2) 0.0864(3) 0.12773(17) 0.0403(9) Uani 1 1 d . . . H8 H 0.6032 0.0814 0.098 0.048 Uiso 1 1 calc R . . C9 C 0.6343(2) 0.0493(2) 0.18148(18) 0.0370(8) Uani 1 1 d . . . C10 C 0.6863(2) 0.0602(3) 0.22669(18) 0.0453(10) Uani 1 1 d . . . H10 H 0.6793 0.038 0.2649 0.054 Uiso 1 1 calc R . . C11 C 0.7480(2) 0.1034(3) 0.21551(18) 0.0430(9) Uani 1 1 d . . . H11 H 0.7841 0.1105 0.246 0.052 Uiso 1 1 calc R . . C12 C 1.0637(2) 0.2513(2) 0.00566(15) 0.0346(8) Uani 1 1 d . . . H12 H 1.1093 0.2542 0.0269 0.042 Uiso 1 1 calc R . . C13 C 1.0656(2) 0.2486(2) -0.05604(15) 0.0359(8) Uani 1 1 d . . . H13 H 1.112 0.2457 -0.0763 0.043 Uiso 1 1 calc R . . C14 C 1 0.25 -0.0885(2) 0.0318(11) Uani 1 2 d S . . C15 C 1 0.25 -0.1549(2) 0.0324(11) Uani 1 2 d S . . C16 C 0.9446(2) 0.2861(3) -0.18692(16) 0.0422(9) Uani 1 1 d . . . H16 H 0.9057 0.3114 -0.1667 0.051 Uiso 1 1 calc R . . C17 C 0.9469(2) 0.2847(2) -0.24838(16) 0.0416(9) Uani 1 1 d . . . H17 H 0.9088 0.3096 -0.2698 0.05 Uiso 1 1 calc R . . Co1 Co 1 0.25 0.125 0.0240(3) Uani 1 4 d S . . Co2 Co 1 0.25 -0.375 0.0278(3) Uani 1 4 d S . . N1 N 0.96121(17) 0.14807(17) 0.12221(11) 0.0275(6) Uani 1 1 d . . . N2 N 1 0.25 0.03663(18) 0.0273(8) Uani 1 2 d S . . N3 N 1 0.25 -0.2794(2) 0.0322(9) Uani 1 2 d S . . S1 S 0.56162(5) -0.01560(5) 0.19472(5) 0.0399(3) Uani 1 1 d . . . O1 O 0.59978(17) -0.08425(16) 0.21112(13) 0.0438(7) Uani 1 1 d . . . O2 O 0.51561(18) 0.01196(17) 0.24314(16) 0.0509(8) Uani 1 1 d . . . O3 O 0.5218(2) -0.0211(2) 0.13816(17) 0.0571(9) Uani 1 1 d . . . O4 O 0.94171(16) 0.35080(15) -0.37623(10) 0.0344(6) Uani 1 1 d D . . O6 O 0.3636(5) 0.9559(6) 0.2428(5) 0.075(3) Uani 0.461(7) 1 d P A 1 O8 O 0.3706(5) 1.0411(6) 0.1358(6) 0.084(3) Uani 0.461(7) 1 d P A 1 O5 O 0.5 1 0 0.122(4) Uani 0.922(13) 2 d SP A 1 O7 O 0.3566(5) 1.0000(7) 0.1959(6) 0.102(4) Uani 0.539(7) 1 d P A 2 O9 O 0.3637(5) 1.0077(5) 0.0629(5) 0.084(3) Uani 0.539(7) 1 d P A 2 O10 O 0.3540(5) 1.0119(5) 0.0127(5) 0.086(3) Uani 0.539(7) 1 d P A 2 H20 H 0.966(2) 0.3890(14) -0.3752(17) 0.029(11) Uiso 1 1 d D . . H21 H 0.910(2) 0.351(2) -0.4023(17) 0.055(15) Uiso 1 1 d 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 C1 0.0366(18) 0.0351(18) 0.0218(14) 0.0001(12) -0.0015(13) -0.0026(14) C2 0.040(2) 0.0370(19) 0.0339(19) -0.0026(13) -0.0014(14) -0.0058(16) C3 0.041(2) 0.0346(18) 0.0344(18) -0.0049(15) -0.0052(15) -0.0006(15) C4 0.0416(19) 0.0329(17) 0.0175(13) -0.0033(12) -0.0021(13) -0.0004(14) C5 0.0355(17) 0.0404(18) 0.0199(15) -0.0029(13) 0.0011(13) -0.0029(14) C6 0.0335(17) 0.0393(18) 0.0280(16) -0.0027(14) 0.0040(13) -0.0014(14) C7 0.040(2) 0.046(2) 0.0296(17) -0.0014(15) 0.0034(14) 0.0013(17) C8 0.035(2) 0.047(2) 0.038(2) -0.0050(15) 0.0002(14) -0.0024(17) C9 0.0343(18) 0.0376(19) 0.0391(19) -0.0029(15) 0.0063(15) -0.0049(15) C10 0.046(2) 0.059(3) 0.0304(18) 0.0070(17) 0.0013(16) -0.0133(19) C11 0.044(2) 0.054(2) 0.0313(19) 0.0000(17) -0.0016(16) -0.0112(18) C12 0.0302(17) 0.053(2) 0.0209(15) 0.0020(14) 0.0014(12) 0.0005(15) C13 0.0318(18) 0.056(2) 0.0202(15) 0.0036(14) 0.0018(13) -0.0016(16) C14 0.034(2) 0.043(3) 0.018(2) 0 0 -0.0015(19) C15 0.033(2) 0.046(3) 0.019(2) 0 0 -0.004(2) C16 0.040(2) 0.064(3) 0.0225(17) -0.0029(16) 0.0002(14) 0.0096(19) C17 0.043(2) 0.060(2) 0.0217(16) 0.0024(16) -0.0002(14) 0.0095(18) Co1 0.0295(4) 0.0295(4) 0.0128(5) 0 0 0 Co2 0.0341(4) 0.0341(4) 0.0153(5) 0 0 0 N1 0.0318(14) 0.0332(15) 0.0174(12) -0.0024(10) -0.0006(10) 0.0001(12) N2 0.0300(19) 0.037(2) 0.0152(18) 0 0 -0.0006(15) N3 0.035(2) 0.043(2) 0.0183(19) 0 0 -0.0004(17) S1 0.0397(5) 0.0348(5) 0.0452(5) -0.0010(4) 0.0014(4) -0.0059(4) O1 0.0489(16) 0.0385(14) 0.0441(15) -0.0074(12) -0.0001(12) -0.0029(12) O2 0.0463(16) 0.0404(15) 0.066(2) -0.0031(14) 0.0112(14) -0.0025(13) O3 0.058(2) 0.0494(18) 0.064(2) 0.0084(16) -0.0160(16) -0.0172(15) O4 0.0388(14) 0.0351(14) 0.0292(13) -0.0017(9) -0.0067(10) 0.0003(11) O6 0.043(4) 0.097(7) 0.085(7) -0.007(5) 0.007(4) -0.014(4) O8 0.057(5) 0.064(6) 0.130(10) 0.008(6) -0.014(5) 0.007(4) O5 0.110(7) 0.076(5) 0.180(10) -0.008(6) 0.055(7) -0.011(5) O7 0.060(5) 0.122(9) 0.124(9) -0.044(8) -0.016(5) 0.020(5) O9 0.079(6) 0.069(5) 0.103(7) 0.003(5) -0.020(5) 0.001(4) O10 0.073(5) 0.076(5) 0.109(8) -0.011(5) -0.009(5) -0.008(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 N1 1.376(5) . ? C1 C5 1.393(5) . ? C1 C2 1.436(5) . ? C2 C3 1.344(6) . ? C2 H2 0.95 . ? C3 C4 1.433(5) . ? C3 H3 0.95 . ? C4 N1 1.377(5) . ? C4 C5 1.388(5) 12_756 ? C5 C4 1.388(5) 15_665 ? C5 C6 1.482(5) . ? C6 C11 1.382(5) . ? C6 C7 1.389(6) . ? C7 C8 1.376(6) . ? C7 H7 0.95 . ? C8 C9 1.378(6) . ? C8 H8 0.95 . ? C9 C10 1.390(6) . ? C9 S1 1.777(4) . ? C10 C11 1.378(6) . ? C10 H10 0.95 . ? C11 H11 0.95 . ? C12 N2 1.338(4) . ? C12 C13 1.381(5) . ? C12 H12 0.95 . ? C13 C14 1.385(4) . ? C13 H13 0.95 . ? C14 C13 1.385(4) 6_654 ? C14 C15 1.483(8) . ? C15 C16 1.388(5) 6_654 ? C15 C16 1.388(5) . ? C16 C17 1.375(5) . ? C16 H16 0.95 . ? C17 N3 1.334(5) . ? C17 H17 0.95 . ? Co1 N1 1.962(3) 6_654 ? Co1 N1 1.962(3) . ? Co1 N1 1.962(3) 12_756 ? Co1 N1 1.962(3) 15_665 ? Co1 N2 1.976(4) 15_665 ? Co1 N2 1.976(4) . ? Co2 O4 2.094(3) . ? Co2 O4 2.094(3) 6_654 ? Co2 O4 2.094(3) 15_664 ? Co2 O4 2.094(3) 12_755 ? Co2 N3 2.136(4) 15_664 ? Co2 N3 2.136(4) . ? N2 C12 1.338(4) 6_654 ? N3 C17 1.334(5) 6_654 ? S1 O2 1.450(3) . ? S1 O3 1.457(4) . ? S1 O1 1.459(3) . ? O4 H20 0.811(10) . ? O4 H21 0.817(10) . ? O9 O10 1.139(13) . ? 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 N1 C1 C5 125.8(3) . . ? N1 C1 C2 109.3(3) . . ? C5 C1 C2 124.7(4) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? C2 C3 C4 107.2(3) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 125.1(3) . 12_756 ? N1 C4 C3 109.6(3) . . ? C5 C4 C3 124.7(3) 12_756 . ? C4 C5 C1 122.6(3) 15_665 . ? C4 C5 C6 120.5(3) 15_665 . ? C1 C5 C6 116.6(3) . . ? C11 C6 C7 119.0(4) . . ? C11 C6 C5 119.5(3) . . ? C7 C6 C5 121.3(3) . . ? C8 C7 C6 120.9(4) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 119.1(4) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C8 C9 C10 120.8(4) . . ? C8 C9 S1 121.5(3) . . ? C10 C9 S1 117.7(3) . . ? C11 C10 C9 119.2(4) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C6 120.6(4) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? N2 C12 C13 122.5(3) . . ? N2 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C13 116.7(5) . 6_654 ? C13 C14 C15 121.6(2) . . ? C13 C14 C15 121.6(2) 6_654 . ? C16 C15 C16 117.8(5) 6_654 . ? C16 C15 C14 121.1(2) 6_654 . ? C16 C15 C14 121.1(2) . . ? C17 C16 C15 119.1(4) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? N3 C17 C16 123.4(4) . . ? N3 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? N1 Co1 N1 176.35(14) 6_654 . ? N1 Co1 N1 90.060(5) 6_654 12_756 ? N1 Co1 N1 90.059(5) . 12_756 ? N1 Co1 N1 90.056(5) 6_654 15_665 ? N1 Co1 N1 90.059(5) . 15_665 ? N1 Co1 N1 176.35(14) 12_756 15_665 ? N1 Co1 N2 91.82(7) 6_654 15_665 ? N1 Co1 N2 91.83(7) . 15_665 ? N1 Co1 N2 88.17(7) 12_756 15_665 ? N1 Co1 N2 88.17(7) 15_665 15_665 ? N1 Co1 N2 88.18(7) 6_654 . ? N1 Co1 N2 88.17(7) . . ? N1 Co1 N2 91.83(7) 12_756 . ? N1 Co1 N2 91.83(7) 15_665 . ? N2 Co1 N2 180 15_665 . ? O4 Co2 O4 178.49(13) . 6_654 ? O4 Co2 O4 90.008(2) . 15_664 ? O4 Co2 O4 90.013(2) 6_654 15_664 ? O4 Co2 O4 90.010(2) . 12_755 ? O4 Co2 O4 90.008(2) 6_654 12_755 ? O4 Co2 O4 178.50(13) 15_664 12_755 ? O4 Co2 N3 89.25(6) . 15_664 ? O4 Co2 N3 89.25(6) 6_654 15_664 ? O4 Co2 N3 90.75(6) 15_664 15_664 ? O4 Co2 N3 90.75(6) 12_755 15_664 ? O4 Co2 N3 90.75(6) . . ? O4 Co2 N3 90.75(6) 6_654 . ? O4 Co2 N3 89.25(6) 15_664 . ? O4 Co2 N3 89.25(6) 12_755 . ? N3 Co2 N3 180 15_664 . ? C1 N1 C4 106.2(3) . . ? C1 N1 Co1 126.8(2) . . ? C4 N1 Co1 127.0(2) . . ? C12 N2 C12 117.7(4) 6_654 . ? C12 N2 Co1 121.1(2) 6_654 . ? C12 N2 Co1 121.2(2) . . ? C17 N3 C17 117.3(5) 6_654 . ? C17 N3 Co2 121.4(2) 6_654 . ? C17 N3 Co2 121.4(2) . . ? O2 S1 O3 113.0(2) . . ? O2 S1 O1 111.69(19) . . ? O3 S1 O1 113.0(2) . . ? O2 S1 C9 108.64(18) . . ? O3 S1 C9 105.2(2) . . ? O1 S1 C9 104.58(18) . . ? Co2 O4 H20 118(3) . . ? Co2 O4 H21 112(4) . . ? H20 O4 H21 113(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.6(4) . . . . ? C5 C1 C2 C3 175.8(3) . . . . ? C1 C2 C3 C4 2.1(4) . . . . ? C2 C3 C4 N1 -2.9(4) . . . . ? C2 C3 C4 C5 169.1(3) . . . 12_756 ? N1 C1 C5 C4 10.0(5) . . . 15_665 ? C2 C1 C5 C4 -165.8(3) . . . 15_665 ? N1 C1 C5 C6 -175.7(3) . . . . ? C2 C1 C5 C6 8.5(5) . . . . ? C4 C5 C6 C11 -109.9(4) 15_665 . . . ? C1 C5 C6 C11 75.7(5) . . . . ? C4 C5 C6 C7 74.7(5) 15_665 . . . ? C1 C5 C6 C7 -99.7(4) . . . . ? C11 C6 C7 C8 -6.3(6) . . . . ? C5 C6 C7 C8 169.1(4) . . . . ? C6 C7 C8 C9 1.7(6) . . . . ? C7 C8 C9 C10 4.4(6) . . . . ? C7 C8 C9 S1 -173.8(3) . . . . ? C8 C9 C10 C11 -5.7(7) . . . . ? S1 C9 C10 C11 172.6(4) . . . . ? C9 C10 C11 C6 0.9(7) . . . . ? C7 C6 C11 C10 4.9(7) . . . . ? C5 C6 C11 C10 -170.5(4) . . . . ? N2 C12 C13 C14 4.9(6) . . . . ? C12 C13 C14 C13 -2.3(3) . . . 6_654 ? C12 C13 C14 C15 177.7(3) . . . . ? C13 C14 C15 C16 31.8(3) . . . 6_654 ? C13 C14 C15 C16 -148.2(3) 6_654 . . 6_654 ? C13 C14 C15 C16 -148.2(3) . . . . ? C13 C14 C15 C16 31.8(3) 6_654 . . . ? C16 C15 C16 C17 -0.1(3) 6_654 . . . ? C14 C15 C16 C17 179.9(3) . . . . ? C15 C16 C17 N3 0.1(7) . . . . ? C5 C1 N1 C4 -177.6(3) . . . . ? C2 C1 N1 C4 -1.2(4) . . . . ? C5 C1 N1 Co1 1.7(5) . . . . ? C2 C1 N1 Co1 178.1(2) . . . . ? C5 C4 N1 C1 -169.5(3) 12_756 . . . ? C3 C4 N1 C1 2.5(4) . . . . ? C5 C4 N1 Co1 11.2(5) 12_756 . . . ? C3 C4 N1 Co1 -176.8(2) . . . . ? N1 Co1 N1 C1 164.3(3) 12_756 . . . ? N1 Co1 N1 C1 -12.0(2) 15_665 . . . ? N2 Co1 N1 C1 76.1(2) 15_665 . . . ? N2 Co1 N1 C1 -103.9(2) . . . . ? N1 Co1 N1 C4 -16.5(2) 12_756 . . . ? N1 Co1 N1 C4 167.1(3) 15_665 . . . ? N2 Co1 N1 C4 -104.7(2) 15_665 . . . ? N2 Co1 N1 C4 75.3(2) . . . . ? C13 C12 N2 C12 -2.4(3) . . . 6_654 ? C13 C12 N2 Co1 177.6(3) . . . . ? N1 Co1 N2 C12 -112.0(2) 6_654 . . 6_654 ? N1 Co1 N2 C12 68.0(2) . . . 6_654 ? N1 Co1 N2 C12 158.0(2) 12_756 . . 6_654 ? N1 Co1 N2 C12 -22.0(2) 15_665 . . 6_654 ? N1 Co1 N2 C12 68.0(2) 6_654 . . . ? N1 Co1 N2 C12 -112.0(2) . . . . ? N1 Co1 N2 C12 -22.0(2) 12_756 . . . ? N1 Co1 N2 C12 158.0(2) 15_665 . . . ? C16 C17 N3 C17 -0.1(3) . . . 6_654 ? C16 C17 N3 Co2 179.9(3) . . . . ? O4 Co2 N3 C17 -153.2(2) . . . 6_654 ? O4 Co2 N3 C17 26.8(2) 6_654 . . 6_654 ? O4 Co2 N3 C17 -63.2(2) 15_664 . . 6_654 ? O4 Co2 N3 C17 116.8(2) 12_755 . . 6_654 ? O4 Co2 N3 C17 26.8(2) . . . . ? O4 Co2 N3 C17 -153.2(2) 6_654 . . . ? O4 Co2 N3 C17 116.8(2) 15_664 . . . ? O4 Co2 N3 C17 -63.2(2) 12_755 . . . ? C8 C9 S1 O2 -116.9(4) . . . . ? C10 C9 S1 O2 64.9(4) . . . . ? C8 C9 S1 O3 4.4(4) . . . . ? C10 C9 S1 O3 -173.9(4) . . . . ? C8 C9 S1 O1 123.7(3) . . . . ? C10 C9 S1 O1 -54.5(4) . . . . ? data_af282 _database_code_depnum_ccdc_archive 'CCDC 890987' #TrackingRef '[CoTPP(bipy)][CoTPP]0.22[TPP]0.78.cif' _audit_creation_date 2011-09-13T13:04:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C54 H36 Co N6, C44 H29.56 Co0.22 N4' _chemical_formula_sum 'C98 H65.56 Co1.22 N10' _chemical_formula_weight 1455.06 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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' '-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 25.1252(4) _cell_length_b 11.7811(2) _cell_length_c 23.9790(4) _cell_angle_alpha 90 _cell_angle_beta 93.5960(10) _cell_angle_gamma 90 _cell_volume 7083.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11016 _cell_measurement_theta_min 3.5223 _cell_measurement_theta_max 76.3416 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 1.371(6) _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method Flotation _exptl_crystal_F_000 3026 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 3 -7 -3 0.0312 -3 7 3 0.0312 -8 -5 -8 0.0528 -7 -6 9 0.0397 2 -4 -13 0.0498 8 -5 -10 0.0448 16 -1 -1 0.0714 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.62452 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4023 _diffrn_orient_matrix_ub_11 0.0216777 _diffrn_orient_matrix_ub_12 -0.1174513 _diffrn_orient_matrix_ub_13 -0.0153368 _diffrn_orient_matrix_ub_21 -0.0563101 _diffrn_orient_matrix_ub_22 -0.0508145 _diffrn_orient_matrix_ub_23 0.0027039 _diffrn_orient_matrix_ub_31 -0.0117738 _diffrn_orient_matrix_ub_32 0.0266312 _diffrn_orient_matrix_ub_33 -0.0624461 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_unetI/netI 0.0346 _diffrn_reflns_number 25120 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 76.53 _diffrn_reflns_theta_full 76.53 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 7352 _reflns_number_gt 6994 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia,1997)' _computing_publication_material 'WinGX publication routines (Farrugia,1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0650P)^2^+4.2950P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7352 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.431 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.43047(6) 0.43980(13) 0.14413(6) 0.0197(3) Uani 1 1 d . . . C2 C 0.43269(7) 0.43626(14) 0.08402(7) 0.0234(3) Uani 1 1 d . . . H2 H 0.4047 0.4547 0.0571 0.028 Uiso 1 1 calc R . . C3 C 0.48256(7) 0.40145(14) 0.07355(7) 0.0230(3) Uani 1 1 d . . . H3 H 0.4957 0.3879 0.0379 0.028 Uiso 1 1 calc R . . C4 C 0.51187(6) 0.38886(13) 0.12700(6) 0.0198(3) Uani 1 1 d . . . C5 C 0.56671(6) 0.36758(13) 0.13356(7) 0.0201(3) Uani 1 1 d . . . C6 C 0.59651(6) 0.38436(13) 0.18393(7) 0.0189(3) Uani 1 1 d . . . C7 C 0.65392(6) 0.38501(14) 0.19068(7) 0.0216(3) Uani 1 1 d . . . H7 H 0.6779 0.3644 0.1633 0.026 Uiso 1 1 calc R . . C8 C 0.66735(6) 0.42039(13) 0.24337(7) 0.0210(3) Uani 1 1 d . . . H8 H 0.7024 0.4331 0.2593 0.025 Uiso 1 1 calc R . . C9 C 0.61826(6) 0.43507(13) 0.27060(7) 0.0183(3) Uani 1 1 d . . . C10 C 0.61574(6) 0.45804(13) 0.32768(7) 0.0202(3) Uani 1 1 d . . . C11 C 0.66564(6) 0.49974(14) 0.35825(6) 0.0205(3) Uani 1 1 d . . . C12 C 0.69661(7) 0.43264(15) 0.39517(8) 0.0275(3) Uani 1 1 d . . . H12 H 0.6854 0.3576 0.4031 0.033 Uiso 1 1 calc R . . C13 C 0.74400(7) 0.47453(16) 0.42074(8) 0.0304(4) Uani 1 1 d . . . H13 H 0.7649 0.4276 0.4458 0.036 Uiso 1 1 calc R . . C14 C 0.76095(7) 0.58346(15) 0.41000(8) 0.0283(4) Uani 1 1 d . . . H14 H 0.7933 0.6116 0.4275 0.034 Uiso 1 1 calc R . . C15 C 0.73029(7) 0.65081(16) 0.37360(8) 0.0322(4) Uani 1 1 d . . . H15 H 0.7416 0.7259 0.366 0.039 Uiso 1 1 calc R . . C16 C 0.68293(7) 0.60995(15) 0.34785(8) 0.0279(4) Uani 1 1 d . . . H16 H 0.6622 0.6575 0.323 0.034 Uiso 1 1 calc R . . C17 C 0.59447(6) 0.33066(14) 0.08324(6) 0.0214(3) Uani 1 1 d . . . C18 C 0.63250(7) 0.39806(15) 0.05933(8) 0.0274(4) Uani 1 1 d . . . H18 H 0.6412 0.4704 0.0748 0.033 Uiso 1 1 calc R . . C19 C 0.65786(8) 0.35957(17) 0.01267(8) 0.0333(4) Uani 1 1 d . . . H19 H 0.6837 0.406 -0.0035 0.04 Uiso 1 1 calc R . . C20 C 0.64548(8) 0.25401(18) -0.01008(7) 0.0334(4) Uani 1 1 d . . . H20 H 0.663 0.2279 -0.0416 0.04 Uiso 1 1 calc R . . C21 C 0.60754(8) 0.18643(16) 0.01312(7) 0.0310(4) Uani 1 1 d . . . H21 H 0.5989 0.1142 -0.0026 0.037 Uiso 1 1 calc R . . C22 C 0.58209(7) 0.22468(15) 0.05947(7) 0.0256(3) Uani 1 1 d . . . H22 H 0.556 0.1783 0.0752 0.031 Uiso 1 1 calc R . . C23 C 0.54315(6) 0.67313(13) 0.23822(6) 0.0205(3) Uani 1 1 d . . . H23 H 0.5743 0.6327 0.2296 0.025 Uiso 1 1 calc R . . C24 C 0.54513(6) 0.79126(13) 0.23781(7) 0.0207(3) Uani 1 1 d . . . H24 H 0.5769 0.8294 0.2293 0.025 Uiso 1 1 calc R . . C25 C 0.5 0.85304(19) 0.25 0.0191(4) Uani 1 2 d S . . C26 C 0.5 -0.02119(18) 0.25 0.0189(4) Uani 1 2 d S . . C27 C 0.45391(6) 0.04053(13) 0.23492(7) 0.0210(3) Uani 1 1 d . . . H27 H 0.4214 0.0024 0.2247 0.025 Uiso 1 1 calc R . . C28 C 0.45602(6) 0.15870(13) 0.23505(7) 0.0211(3) Uani 1 1 d . . . H28 H 0.4245 0.1994 0.2239 0.025 Uiso 1 1 calc R . . C29 C 0.73729(6) 0.34877(13) 0.61659(6) 0.0200(3) Uani 1 1 d . . . C30 C 0.69918(6) 0.35449(13) 0.65873(7) 0.0218(3) Uani 1 1 d . . . H30 H 0.7052 0.3849 0.6953 0.026 Uiso 1 1 calc R . . C31 C 0.65291(6) 0.30849(13) 0.63679(7) 0.0217(3) Uani 1 1 d . . . H31 H 0.6207 0.3012 0.6553 0.026 Uiso 1 1 calc R . . C32 C 0.66117(6) 0.27285(13) 0.58084(6) 0.0200(3) Uani 1 1 d . . . C33 C 0.62358(6) 0.21817(13) 0.54530(7) 0.0208(3) Uani 1 1 d . . . C34 C 0.63318(6) 0.17554(13) 0.49226(7) 0.0205(3) Uani 1 1 d . . . C35 C 0.59263(7) 0.12358(14) 0.45492(7) 0.0240(3) Uani 1 1 d . . . H35 H 0.5562 0.1127 0.4619 0.029 Uiso 1 1 calc R . . C36 C 0.61674(7) 0.09351(14) 0.40824(7) 0.0235(3) Uani 1 1 d . . . H36 H 0.6005 0.0575 0.376 0.028 Uiso 1 1 calc R . . C37 C 0.67210(6) 0.12703(13) 0.41694(7) 0.0206(3) Uani 1 1 d . . . C38 C 0.70974(6) 0.11390(13) 0.37687(7) 0.0206(3) Uani 1 1 d . . . C39 C 0.69413(6) 0.05965(14) 0.32174(7) 0.0204(3) Uani 1 1 d . . . C40 C 0.69312(7) -0.05839(14) 0.31622(7) 0.0235(3) Uani 1 1 d . . . H40 H 0.6981 -0.1049 0.3485 0.028 Uiso 1 1 calc R . . C41 C 0.68482(7) -0.10822(15) 0.26394(7) 0.0253(3) Uani 1 1 d . . . H41 H 0.6849 -0.1886 0.2606 0.03 Uiso 1 1 calc R . . C42 C 0.67646(7) -0.04140(15) 0.21652(7) 0.0254(3) Uani 1 1 d . . . H42 H 0.6714 -0.0757 0.1807 0.031 Uiso 1 1 calc R . . C43 C 0.67549(7) 0.07602(15) 0.22183(7) 0.0258(3) Uani 1 1 d . . . H43 H 0.6685 0.1222 0.1897 0.031 Uiso 1 1 calc R . . C44 C 0.68479(7) 0.12605(14) 0.27419(7) 0.0235(3) Uani 1 1 d . . . H44 H 0.6847 0.2064 0.2774 0.028 Uiso 1 1 calc R . . C45 C 0.56966(6) 0.20026(14) 0.56716(6) 0.0210(3) Uani 1 1 d . . . C46 C 0.53512(7) 0.29135(15) 0.57464(7) 0.0245(3) Uani 1 1 d . . . H46 H 0.5454 0.366 0.5648 0.029 Uiso 1 1 calc R . . C47 C 0.48574(7) 0.27308(16) 0.59641(7) 0.0276(3) Uani 1 1 d . . . H47 H 0.4624 0.3352 0.6012 0.033 Uiso 1 1 calc R . . C48 C 0.47060(7) 0.16459(16) 0.61112(7) 0.0273(3) Uani 1 1 d . . . H48 H 0.4368 0.1523 0.6258 0.033 Uiso 1 1 calc R . . C49 C 0.50477(7) 0.07401(15) 0.60446(7) 0.0263(3) Uani 1 1 d . . . H49 H 0.4945 -0.0003 0.6149 0.032 Uiso 1 1 calc R . . C50 C 0.55412(7) 0.09164(14) 0.58253(7) 0.0235(3) Uani 1 1 d . . . H50 H 0.5774 0.0292 0.578 0.028 Uiso 1 1 calc R . . Co1 Co 0.5 0.41292(3) 0.25 0.01647(10) Uani 1 2 d S . . Co2 Co 0.75 0.25 0.5 0.0173(3) Uani 0.22 2 d SP . . N1 N 0.47939(5) 0.41245(10) 0.16954(6) 0.0184(3) Uani 1 1 d . . . N2 N 0.57556(5) 0.41259(10) 0.23375(6) 0.0180(3) Uani 1 1 d . . . N3 N 0.5 0.61301(16) 0.25 0.0189(4) Uani 1 2 d S . . N4 N 0.5 0.21805(15) 0.25 0.0193(4) Uani 1 2 d S . . N5 N 0.68130(5) 0.17710(11) 0.46829(5) 0.0207(3) Uani 1 1 d . . . N6 N 0.71287(5) 0.29931(12) 0.57001(6) 0.0211(3) Uani 1 1 d . . . H1N H 0.7279(12) 0.286(3) 0.5401(13) 0.032(7) Uiso 0.78 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0219(7) 0.0145(7) 0.0224(7) 0.0006(6) -0.0009(6) 0.0000(6) C2 0.0241(8) 0.0225(7) 0.0233(8) 0.0006(6) -0.0013(6) 0.0009(6) C3 0.0243(8) 0.0222(8) 0.0225(8) -0.0008(6) 0.0021(6) 0.0005(6) C4 0.0221(7) 0.0163(7) 0.0209(7) -0.0005(5) 0.0016(6) -0.0002(6) C5 0.0227(7) 0.0144(7) 0.0233(7) 0.0006(5) 0.0034(6) -0.0006(5) C6 0.0198(7) 0.0128(6) 0.0244(7) 0.0014(5) 0.0038(6) 0.0002(5) C7 0.0210(7) 0.0180(7) 0.0261(8) 0.0021(6) 0.0034(6) 0.0017(6) C8 0.0195(7) 0.0166(7) 0.0268(8) 0.0027(6) 0.0014(6) 0.0002(5) C9 0.0159(7) 0.0133(6) 0.0255(7) 0.0018(5) -0.0002(6) -0.0008(5) C10 0.0210(7) 0.0140(7) 0.0253(7) 0.0013(5) -0.0001(6) 0.0010(5) C11 0.0192(7) 0.0194(7) 0.0228(7) -0.0015(6) 0.0014(6) 0.0004(6) C12 0.0285(8) 0.0207(8) 0.0324(9) 0.0002(7) -0.0042(7) 0.0011(6) C13 0.0264(8) 0.0299(9) 0.0336(9) -0.0034(7) -0.0081(7) 0.0062(7) C14 0.0196(8) 0.0304(9) 0.0344(9) -0.0087(7) -0.0015(7) -0.0016(6) C15 0.0262(8) 0.0252(9) 0.0448(10) 0.0013(7) -0.0007(7) -0.0069(7) C16 0.0239(8) 0.0231(8) 0.0363(9) 0.0060(7) -0.0026(7) -0.0029(6) C17 0.0214(7) 0.0207(7) 0.0221(7) 0.0010(6) 0.0006(6) 0.0036(6) C18 0.0286(9) 0.0251(8) 0.0290(9) 0.0027(6) 0.0060(7) 0.0010(6) C19 0.0327(9) 0.0367(10) 0.0315(9) 0.0083(7) 0.0106(7) 0.0047(7) C20 0.0359(9) 0.0421(11) 0.0228(8) 0.0009(7) 0.0065(7) 0.0145(8) C21 0.0359(9) 0.0298(9) 0.0269(8) -0.0061(7) -0.0013(7) 0.0090(7) C22 0.0260(8) 0.0245(8) 0.0261(8) -0.0012(6) 0.0007(6) 0.0021(6) C23 0.0201(7) 0.0156(7) 0.0261(7) 0.0014(6) 0.0035(6) 0.0021(5) C24 0.0205(7) 0.0156(7) 0.0261(7) 0.0007(6) 0.0020(6) -0.0017(5) C25 0.0201(10) 0.0176(10) 0.0194(10) 0 -0.0001(8) 0 C26 0.0215(10) 0.0163(10) 0.0192(10) 0 0.0029(8) 0 C27 0.0202(7) 0.0161(7) 0.0264(8) -0.0010(6) -0.0007(6) -0.0021(6) C28 0.0206(7) 0.0148(7) 0.0277(8) 0.0001(6) -0.0004(6) 0.0011(6) C29 0.0225(7) 0.0158(7) 0.0216(7) 0.0003(5) 0.0007(6) -0.0004(6) C30 0.0236(7) 0.0183(7) 0.0237(7) -0.0016(6) 0.0018(6) 0.0009(6) C31 0.0227(7) 0.0194(7) 0.0230(7) -0.0007(6) 0.0024(6) 0.0002(6) C32 0.0217(7) 0.0150(7) 0.0234(7) 0.0004(5) 0.0028(6) -0.0005(5) C33 0.0225(7) 0.0164(7) 0.0235(7) 0.0019(6) 0.0021(6) -0.0006(6) C34 0.0216(7) 0.0166(7) 0.0234(7) 0.0019(6) 0.0012(6) -0.0016(6) C35 0.0224(8) 0.0237(8) 0.0259(8) 0.0002(6) 0.0015(6) -0.0025(6) C36 0.0232(8) 0.0230(8) 0.0240(8) -0.0005(6) 0.0001(6) -0.0034(6) C37 0.0232(7) 0.0155(7) 0.0229(7) 0.0010(6) -0.0003(6) -0.0017(6) C38 0.0230(7) 0.0150(7) 0.0237(7) 0.0004(6) 0.0008(6) -0.0002(6) C39 0.0181(7) 0.0191(7) 0.0241(7) -0.0007(6) 0.0019(6) -0.0017(6) C40 0.0248(8) 0.0188(7) 0.0269(8) 0.0005(6) 0.0018(6) -0.0008(6) C41 0.0248(8) 0.0193(7) 0.0320(9) -0.0051(6) 0.0033(6) -0.0022(6) C42 0.0240(8) 0.0282(9) 0.0243(8) -0.0061(6) 0.0030(6) -0.0042(6) C43 0.0262(8) 0.0273(9) 0.0237(8) 0.0013(6) 0.0007(6) -0.0024(6) C44 0.0247(8) 0.0195(8) 0.0262(8) 0.0004(6) 0.0004(6) -0.0014(6) C45 0.0207(7) 0.0229(8) 0.0192(7) -0.0018(6) 0.0001(6) -0.0024(6) C46 0.0242(8) 0.0235(8) 0.0258(8) 0.0013(6) 0.0000(6) -0.0011(6) C47 0.0231(8) 0.0308(9) 0.0290(8) -0.0026(7) 0.0009(6) 0.0041(7) C48 0.0206(7) 0.0363(9) 0.0251(8) -0.0031(7) 0.0027(6) -0.0058(7) C49 0.0269(8) 0.0256(8) 0.0265(8) -0.0026(6) 0.0029(6) -0.0079(6) C50 0.0239(8) 0.0207(8) 0.0261(8) -0.0034(6) 0.0029(6) -0.0030(6) Co1 0.01623(17) 0.01424(18) 0.01898(18) 0 0.00139(12) 0 Co2 0.0178(7) 0.0158(7) 0.0184(7) -0.0009(6) 0.0018(6) -0.0019(6) N1 0.0188(6) 0.0143(6) 0.0222(6) -0.0001(4) 0.0007(5) 0.0001(4) N2 0.0204(6) 0.0126(6) 0.0213(6) 0.0012(4) 0.0025(5) 0.0002(4) N3 0.0230(9) 0.0133(8) 0.0203(9) 0 0.0013(7) 0 N4 0.0219(9) 0.0128(8) 0.0233(9) 0 0.0007(7) 0 N5 0.0224(6) 0.0181(6) 0.0216(6) 0.0001(5) 0.0015(5) -0.0007(5) N6 0.0207(6) 0.0201(6) 0.0225(7) 0.0003(5) 0.0013(5) -0.0023(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 N1 1.375(2) . ? C1 C10 1.396(2) 2_655 ? C1 C2 1.446(2) . ? C2 C3 1.357(2) . ? C2 H2 0.95 . ? C3 C4 1.445(2) . ? C3 H3 0.95 . ? C4 N1 1.374(2) . ? C4 C5 1.400(2) . ? C5 C6 1.395(2) . ? C5 C17 1.496(2) . ? C6 N2 1.376(2) . ? C6 C7 1.441(2) . ? C7 C8 1.353(2) . ? C7 H7 0.95 . ? C8 C9 1.442(2) . ? C8 H8 0.95 . ? C9 N2 1.372(2) . ? C9 C10 1.401(2) . ? C10 C1 1.396(2) 2_655 ? C10 C11 1.495(2) . ? C11 C12 1.388(2) . ? C11 C16 1.397(2) . ? C12 C13 1.395(2) . ? C12 H12 0.95 . ? C13 C14 1.381(3) . ? C13 H13 0.95 . ? C14 C15 1.379(3) . ? C14 H14 0.95 . ? C15 C16 1.392(2) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C17 C18 1.393(2) . ? C17 C22 1.399(2) . ? C18 C19 1.397(3) . ? C18 H18 0.95 . ? C19 C20 1.386(3) . ? C19 H19 0.95 . ? C20 C21 1.385(3) . ? C20 H20 0.95 . ? C21 C22 1.391(2) . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 N3 1.3399(18) . ? C23 C24 1.393(2) . ? C23 H23 0.95 . ? C24 C25 1.3938(19) . ? C24 H24 0.95 . ? C25 C24 1.3938(19) 2_655 ? C25 C26 1.482(3) 1_565 ? C26 C27 1.3958(19) . ? C26 C27 1.3958(19) 2_655 ? C26 C25 1.482(3) 1_545 ? C27 C28 1.393(2) . ? C27 H27 0.95 . ? C28 N4 1.3375(18) . ? C28 H28 0.95 . ? C29 N6 1.370(2) . ? C29 C38 1.401(2) 7_656 ? C29 C30 1.436(2) . ? C30 C31 1.358(2) . ? C30 H30 0.95 . ? C31 C32 1.433(2) . ? C31 H31 0.95 . ? C32 N6 1.376(2) . ? C32 C33 1.390(2) . ? C33 C34 1.402(2) . ? C33 C45 1.498(2) . ? C34 N5 1.371(2) . ? C34 C35 1.449(2) . ? C35 C36 1.353(2) . ? C35 H35 0.95 . ? C36 C37 1.448(2) . ? C36 H36 0.95 . ? C37 N5 1.372(2) . ? C37 C38 1.398(2) . ? C38 C29 1.401(2) 7_656 ? C38 C39 1.498(2) . ? C39 C44 1.390(2) . ? C39 C40 1.397(2) . ? C40 C41 1.388(2) . ? C40 H40 0.95 . ? C41 C42 1.388(3) . ? C41 H41 0.95 . ? C42 C43 1.390(2) . ? C42 H42 0.95 . ? C43 C44 1.393(2) . ? C43 H43 0.95 . ? C44 H44 0.95 . ? C45 C50 1.394(2) . ? C45 C46 1.399(2) . ? C46 C47 1.393(2) . ? C46 H46 0.95 . ? C47 C48 1.385(3) . ? C47 H47 0.95 . ? C48 C49 1.385(3) . ? C48 H48 0.95 . ? C49 C50 1.392(2) . ? C49 H49 0.95 . ? C50 H50 0.95 . ? Co1 N2 1.9619(13) . ? Co1 N2 1.9619(13) 2_655 ? Co1 N1 1.9660(13) 2_655 ? Co1 N1 1.9660(13) . ? Co1 N4 2.2958(18) . ? Co1 N3 2.3573(19) . ? Co2 N5 2.0324(13) . ? Co2 N5 2.0324(13) 7_656 ? Co2 N6 2.0549(14) . ? Co2 N6 2.0550(14) 7_656 ? Co2 H1N 1.22(3) . ? N3 C23 1.3399(18) 2_655 ? N4 C28 1.3375(18) 2_655 ? N6 H1N 0.85(3) . ? 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 N1 C1 C10 124.66(14) . 2_655 ? N1 C1 C2 110.21(14) . . ? C10 C1 C2 124.88(15) 2_655 . ? C3 C2 C1 106.67(14) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 C4 106.98(14) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 125.39(14) . . ? N1 C4 C3 110.13(14) . . ? C5 C4 C3 124.15(15) . . ? C6 C5 C4 122.90(14) . . ? C6 C5 C17 119.19(14) . . ? C4 C5 C17 117.83(14) . . ? N2 C6 C5 124.90(14) . . ? N2 C6 C7 109.63(14) . . ? C5 C6 C7 125.24(14) . . ? C8 C7 C6 107.20(14) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 106.83(14) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N2 C9 C10 125.81(14) . . ? N2 C9 C8 109.98(14) . . ? C10 C9 C8 123.93(14) . . ? C1 C10 C9 122.22(14) 2_655 . ? C1 C10 C11 120.69(14) 2_655 . ? C9 C10 C11 117.05(14) . . ? C12 C11 C16 118.37(15) . . ? C12 C11 C10 123.00(15) . . ? C16 C11 C10 118.59(14) . . ? C11 C12 C13 120.51(17) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 120.76(17) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.09(16) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 120.67(17) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 120.61(16) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C18 C17 C22 118.79(15) . . ? C18 C17 C5 122.19(15) . . ? C22 C17 C5 119.02(15) . . ? C17 C18 C19 120.23(17) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.27(17) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.06(16) . . ? C21 C20 H20 120 . . ? C19 C20 H20 120 . . ? C20 C21 C22 119.79(17) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C17 120.85(17) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? N3 C23 C24 124.02(15) . . ? N3 C23 H23 118 . . ? C24 C23 H23 118 . . ? C23 C24 C25 119.37(15) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C24 117.0(2) . 2_655 ? C24 C25 C26 121.48(10) . 1_565 ? C24 C25 C26 121.47(10) 2_655 1_565 ? C27 C26 C27 117.2(2) . 2_655 ? C27 C26 C25 121.40(10) . 1_545 ? C27 C26 C25 121.40(10) 2_655 1_545 ? C28 C27 C26 119.28(15) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? N4 C28 C27 123.62(14) . . ? N4 C28 H28 118.2 . . ? C27 C28 H28 118.2 . . ? N6 C29 C38 126.74(15) . 7_656 ? N6 C29 C30 108.01(14) . . ? C38 C29 C30 125.24(15) 7_656 . ? C31 C30 C29 107.52(14) . . ? C31 C30 H30 126.2 . . ? C29 C30 H30 126.2 . . ? C30 C31 C32 107.98(14) . . ? C30 C31 H31 126 . . ? C32 C31 H31 126 . . ? N6 C32 C33 127.04(14) . . ? N6 C32 C31 107.70(14) . . ? C33 C32 C31 125.23(15) . . ? C32 C33 C34 124.96(15) . . ? C32 C33 C45 116.45(14) . . ? C34 C33 C45 118.54(14) . . ? N5 C34 C33 125.59(15) . . ? N5 C34 C35 110.54(14) . . ? C33 C34 C35 123.87(15) . . ? C36 C35 C34 106.72(14) . . ? C36 C35 H35 126.6 . . ? C34 C35 H35 126.6 . . ? C35 C36 C37 106.57(15) . . ? C35 C36 H36 126.7 . . ? C37 C36 H36 126.7 . . ? N5 C37 C38 125.52(15) . . ? N5 C37 C36 110.67(14) . . ? C38 C37 C36 123.75(15) . . ? C37 C38 C29 124.55(15) . 7_656 ? C37 C38 C39 120.17(14) . . ? C29 C38 C39 115.26(14) 7_656 . ? C44 C39 C40 118.78(15) . . ? C44 C39 C38 120.32(15) . . ? C40 C39 C38 120.68(15) . . ? C41 C40 C39 120.48(16) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 120.43(16) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 119.48(16) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C42 C43 C44 120.05(16) . . ? C42 C43 H43 120 . . ? C44 C43 H43 120 . . ? C39 C44 C43 120.73(16) . . ? C39 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C50 C45 C46 118.94(15) . . ? C50 C45 C33 119.76(15) . . ? C46 C45 C33 121.25(15) . . ? C47 C46 C45 120.26(16) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 C46 120.22(16) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C49 C48 C47 119.95(16) . . ? C49 C48 H48 120 . . ? C47 C48 H48 120 . . ? C48 C49 C50 120.11(16) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C45 120.50(16) . . ? C49 C50 H50 119.7 . . ? C45 C50 H50 119.7 . . ? N2 Co1 N2 179.77(7) . 2_655 ? N2 Co1 N1 89.79(6) . 2_655 ? N2 Co1 N1 90.21(6) 2_655 2_655 ? N2 Co1 N1 90.21(6) . . ? N2 Co1 N1 89.79(6) 2_655 . ? N1 Co1 N1 179.68(8) 2_655 . ? N2 Co1 N4 89.89(4) . . ? N2 Co1 N4 89.89(4) 2_655 . ? N1 Co1 N4 89.84(4) 2_655 . ? N1 Co1 N4 89.84(4) . . ? N2 Co1 N3 90.11(4) . . ? N2 Co1 N3 90.11(4) 2_655 . ? N1 Co1 N3 90.16(4) 2_655 . ? N1 Co1 N3 90.16(4) . . ? N4 Co1 N3 180 . . ? N5 Co2 N5 180.00(4) . 7_656 ? N5 Co2 N6 90.38(5) . . ? N5 Co2 N6 89.62(5) 7_656 . ? N5 Co2 N6 89.62(5) . 7_656 ? N5 Co2 N6 90.38(5) 7_656 7_656 ? N6 Co2 N6 179.9990(10) . 7_656 ? N5 Co2 H1N 91.4(14) . . ? N5 Co2 H1N 88.6(14) 7_656 . ? N6 Co2 H1N 4.1(14) . . ? N6 Co2 H1N 175.9(14) 7_656 . ? C4 N1 C1 105.93(13) . . ? C4 N1 Co1 126.64(11) . . ? C1 N1 Co1 127.38(11) . . ? C9 N2 C6 106.22(13) . . ? C9 N2 Co1 126.79(11) . . ? C6 N2 Co1 126.91(11) . . ? C23 N3 C23 116.18(19) . 2_655 ? C23 N3 Co1 121.91(9) . . ? C23 N3 Co1 121.91(9) 2_655 . ? C28 N4 C28 116.96(19) . 2_655 ? C28 N4 Co1 121.52(9) . . ? C28 N4 Co1 121.52(9) 2_655 . ? C34 N5 C37 105.49(13) . . ? C34 N5 Co2 126.82(11) . . ? C37 N5 Co2 127.52(11) . . ? C29 N6 C32 108.79(13) . . ? C29 N6 Co2 125.67(11) . . ? C32 N6 Co2 124.92(11) . . ? C29 N6 H1N 125(2) . . ? C32 N6 H1N 127(2) . . ? Co2 N6 H1N 6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 2.79(19) . . . . ? C10 C1 C2 C3 -171.77(15) 2_655 . . . ? C1 C2 C3 C4 -2.73(18) . . . . ? C2 C3 C4 N1 1.89(19) . . . . ? C2 C3 C4 C5 -171.85(15) . . . . ? N1 C4 C5 C6 -9.8(3) . . . . ? C3 C4 C5 C6 163.03(15) . . . . ? N1 C4 C5 C17 173.28(14) . . . . ? C3 C4 C5 C17 -13.9(2) . . . . ? C4 C5 C6 N2 6.5(2) . . . . ? C17 C5 C6 N2 -176.54(14) . . . . ? C4 C5 C6 C7 -167.49(15) . . . . ? C17 C5 C6 C7 9.4(2) . . . . ? N2 C6 C7 C8 -3.74(18) . . . . ? C5 C6 C7 C8 171.06(15) . . . . ? C6 C7 C8 C9 3.49(17) . . . . ? C7 C8 C9 N2 -2.20(17) . . . . ? C7 C8 C9 C10 172.09(15) . . . . ? N2 C9 C10 C1 12.3(2) . . . 2_655 ? C8 C9 C10 C1 -161.12(15) . . . 2_655 ? N2 C9 C10 C11 -169.78(14) . . . . ? C8 C9 C10 C11 16.8(2) . . . . ? C1 C10 C11 C12 71.9(2) 2_655 . . . ? C9 C10 C11 C12 -106.13(19) . . . . ? C1 C10 C11 C16 -110.36(18) 2_655 . . . ? C9 C10 C11 C16 71.6(2) . . . . ? C16 C11 C12 C13 -0.5(3) . . . . ? C10 C11 C12 C13 177.28(16) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C11 -0.2(3) . . . . ? C12 C11 C16 C15 0.5(3) . . . . ? C10 C11 C16 C15 -177.35(16) . . . . ? C6 C5 C17 C18 -63.5(2) . . . . ? C4 C5 C17 C18 113.52(18) . . . . ? C6 C5 C17 C22 116.13(17) . . . . ? C4 C5 C17 C22 -66.8(2) . . . . ? C22 C17 C18 C19 -0.4(3) . . . . ? C5 C17 C18 C19 179.29(16) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? C18 C19 C20 C21 0.5(3) . . . . ? C19 C20 C21 C22 -0.3(3) . . . . ? C20 C21 C22 C17 -0.3(3) . . . . ? C18 C17 C22 C21 0.6(3) . . . . ? C5 C17 C22 C21 -179.09(15) . . . . ? N3 C23 C24 C25 -0.3(2) . . . . ? C23 C24 C25 C24 0.14(10) . . . 2_655 ? C23 C24 C25 C26 -179.86(10) . . . 1_565 ? C27 C26 C27 C28 0.61(10) 2_655 . . . ? C25 C26 C27 C28 -179.38(10) 1_545 . . . ? C26 C27 C28 N4 -1.3(2) . . . . ? N6 C29 C30 C31 0.09(18) . . . . ? C38 C29 C30 C31 -179.01(15) 7_656 . . . ? C29 C30 C31 C32 0.21(18) . . . . ? C30 C31 C32 N6 -0.44(18) . . . . ? C30 C31 C32 C33 177.69(16) . . . . ? N6 C32 C33 C34 3.1(3) . . . . ? C31 C32 C33 C34 -174.70(15) . . . . ? N6 C32 C33 C45 -179.53(15) . . . . ? C31 C32 C33 C45 2.7(2) . . . . ? C32 C33 C34 N5 2.7(3) . . . . ? C45 C33 C34 N5 -174.62(15) . . . . ? C32 C33 C34 C35 -176.98(16) . . . . ? C45 C33 C34 C35 5.7(2) . . . . ? N5 C34 C35 C36 0.16(19) . . . . ? C33 C34 C35 C36 179.91(15) . . . . ? C34 C35 C36 C37 0.00(18) . . . . ? C35 C36 C37 N5 -0.16(19) . . . . ? C35 C36 C37 C38 -177.52(16) . . . . ? N5 C37 C38 C29 -0.5(3) . . . 7_656 ? C36 C37 C38 C29 176.46(15) . . . 7_656 ? N5 C37 C38 C39 -178.69(14) . . . . ? C36 C37 C38 C39 -1.7(2) . . . . ? C37 C38 C39 C44 102.44(19) . . . . ? C29 C38 C39 C44 -75.91(19) 7_656 . . . ? C37 C38 C39 C40 -83.0(2) . . . . ? C29 C38 C39 C40 98.64(18) 7_656 . . . ? C44 C39 C40 C41 2.3(2) . . . . ? C38 C39 C40 C41 -172.36(15) . . . . ? C39 C40 C41 C42 -1.2(3) . . . . ? C40 C41 C42 C43 -1.1(3) . . . . ? C41 C42 C43 C44 2.3(3) . . . . ? C40 C39 C44 C43 -1.1(2) . . . . ? C38 C39 C44 C43 173.55(15) . . . . ? C42 C43 C44 C39 -1.2(3) . . . . ? C32 C33 C45 C50 -107.45(18) . . . . ? C34 C33 C45 C50 70.1(2) . . . . ? C32 C33 C45 C46 70.0(2) . . . . ? C34 C33 C45 C46 -112.43(18) . . . . ? C50 C45 C46 C47 -0.8(2) . . . . ? C33 C45 C46 C47 -178.30(15) . . . . ? C45 C46 C47 C48 0.4(3) . . . . ? C46 C47 C48 C49 0.3(3) . . . . ? C47 C48 C49 C50 -0.6(3) . . . . ? C48 C49 C50 C45 0.1(3) . . . . ? C46 C45 C50 C49 0.6(2) . . . . ? C33 C45 C50 C49 178.11(15) . . . . ? C5 C4 N1 C1 173.51(15) . . . . ? C3 C4 N1 C1 -0.14(17) . . . . ? C5 C4 N1 Co1 -4.2(2) . . . . ? C3 C4 N1 Co1 -177.83(10) . . . . ? C10 C1 N1 C4 172.99(15) 2_655 . . . ? C2 C1 N1 C4 -1.59(17) . . . . ? C10 C1 N1 Co1 -9.3(2) 2_655 . . . ? C2 C1 N1 Co1 176.09(11) . . . . ? N2 Co1 N1 C4 14.37(13) . . . . ? N2 Co1 N1 C4 -165.41(13) 2_655 . . . ? N4 Co1 N1 C4 -75.52(12) . . . . ? N3 Co1 N1 C4 104.48(12) . . . . ? N2 Co1 N1 C1 -162.84(13) . . . . ? N2 Co1 N1 C1 17.38(13) 2_655 . . . ? N4 Co1 N1 C1 107.27(12) . . . . ? N3 Co1 N1 C1 -72.73(12) . . . . ? C10 C9 N2 C6 -174.29(14) . . . . ? C8 C9 N2 C6 -0.14(16) . . . . ? C10 C9 N2 Co1 2.8(2) . . . . ? C8 C9 N2 Co1 176.98(10) . . . . ? C5 C6 N2 C9 -172.51(14) . . . . ? C7 C6 N2 C9 2.32(16) . . . . ? C5 C6 N2 Co1 10.4(2) . . . . ? C7 C6 N2 Co1 -174.79(10) . . . . ? N1 Co1 N2 C9 -14.19(12) 2_655 . . . ? N1 Co1 N2 C9 166.12(12) . . . . ? N4 Co1 N2 C9 -104.04(12) . . . . ? N3 Co1 N2 C9 75.96(12) . . . . ? N1 Co1 N2 C6 162.34(12) 2_655 . . . ? N1 Co1 N2 C6 -17.34(12) . . . . ? N4 Co1 N2 C6 72.50(12) . . . . ? N3 Co1 N2 C6 -107.50(12) . . . . ? C24 C23 N3 C23 0.15(11) . . . 2_655 ? C24 C23 N3 Co1 -179.85(11) . . . . ? N2 Co1 N3 C23 2.92(9) . . . . ? N2 Co1 N3 C23 -177.08(9) 2_655 . . . ? N1 Co1 N3 C23 92.71(9) 2_655 . . . ? N1 Co1 N3 C23 -87.29(9) . . . . ? N2 Co1 N3 C23 -177.08(9) . . . 2_655 ? N2 Co1 N3 C23 2.92(9) 2_655 . . 2_655 ? N1 Co1 N3 C23 -87.29(9) 2_655 . . 2_655 ? N1 Co1 N3 C23 92.71(9) . . . 2_655 ? C27 C28 N4 C28 0.67(11) . . . 2_655 ? C27 C28 N4 Co1 -179.32(11) . . . . ? N2 Co1 N4 C28 -150.28(9) . . . . ? N2 Co1 N4 C28 29.72(9) 2_655 . . . ? N1 Co1 N4 C28 119.93(9) 2_655 . . . ? N1 Co1 N4 C28 -60.07(9) . . . . ? N2 Co1 N4 C28 29.73(9) . . . 2_655 ? N2 Co1 N4 C28 -150.27(9) 2_655 . . 2_655 ? N1 Co1 N4 C28 -60.06(9) 2_655 . . 2_655 ? N1 Co1 N4 C28 119.94(9) . . . 2_655 ? C33 C34 N5 C37 180.00(15) . . . . ? C35 C34 N5 C37 -0.25(18) . . . . ? C33 C34 N5 Co2 -4.4(2) . . . . ? C35 C34 N5 Co2 175.31(11) . . . . ? C38 C37 N5 C34 177.56(15) . . . . ? C36 C37 N5 C34 0.25(17) . . . . ? C38 C37 N5 Co2 2.0(2) . . . . ? C36 C37 N5 Co2 -175.27(11) . . . . ? N6 Co2 N5 C34 1.31(13) . . . . ? N6 Co2 N5 C34 -178.69(13) 7_656 . . . ? N6 Co2 N5 C37 175.91(13) . . . . ? N6 Co2 N5 C37 -4.09(13) 7_656 . . . ? C38 C29 N6 C32 178.71(15) 7_656 . . . ? C30 C29 N6 C32 -0.37(18) . . . . ? C38 C29 N6 Co2 7.4(2) 7_656 . . . ? C30 C29 N6 Co2 -171.65(10) . . . . ? C33 C32 N6 C29 -177.59(15) . . . . ? C31 C32 N6 C29 0.50(17) . . . . ? C33 C32 N6 Co2 -6.2(2) . . . . ? C31 C32 N6 Co2 171.86(10) . . . . ? N5 Co2 N6 C29 173.50(13) . . . . ? N5 Co2 N6 C29 -6.50(13) 7_656 . . . ? N5 Co2 N6 C32 3.58(13) . . . . ? N5 Co2 N6 C32 -176.42(13) 7_656 . . . ? # END of CIF