# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Avinash S. Kumbhar' _publ_contact_author_email askum@chem.unipune.ernet.in loop_ _publ_author_name V.A.Kawade A.A.Kumbhar A.S.Kumbhar C.Nather A.Erxleben ; U.B.Sonawane ; R.R.Joshi data_19a _database_code_depnum_ccdc_archive 'CCDC 779557' #TrackingRef 'CPBPG.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Co N8 O9 S2' _chemical_formula_weight 771.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+3/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' _cell_length_a 13.6859(9) _cell_length_b 13.6859(9) _cell_length_c 19.184(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3593.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3238 _cell_measurement_theta_min 5.17 _cell_measurement_theta_max 25.33 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8801 _exptl_absorpt_correction_T_max 0.9081 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.1048 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7716 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 5.17 _diffrn_reflns_theta_max 25.33 _reflns_number_total 3238 _reflns_number_gt 2644 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP III (M.N. Burnett, C.K. Johnson, 1996), ORTEX, PC windows version (P. McArdle, J. Appl. Crystallogr. 1995, 28, 65) ; _computing_publication_material ? _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^)+(0.1280P)^2^+3.3800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _Check for _chemical_absolute_configuration unk _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(5) _refine_ls_number_reflns 3238 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2339 _refine_ls_wR_factor_gt 0.2283 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.71091(6) 0.28909(6) 0.2500 0.0305(4) Uani 1 2 d S . . O1 O 0.7376(4) 0.1766(3) 0.3196(3) 0.0403(12) Uani 1 1 d . . . O2 O 0.7058(5) 0.0191(4) 0.3422(3) 0.0568(16) Uani 1 1 d . . . O3 O 0.1898(5) 0.5261(7) 0.2048(5) 0.084(3) Uani 1 1 d . . . N1 N 0.5945(4) 0.3492(4) 0.3127(3) 0.0292(12) Uani 1 1 d . . . N2 N 0.6199(5) 0.1771(4) 0.2098(3) 0.0362(14) Uani 1 1 d . . . N3 N 0.3122(5) 0.5422(6) 0.2872(4) 0.059(2) Uani 1 1 d . . . H3A H 0.2734 0.5330 0.3265 0.071 Uiso 1 1 d R . . N4 N 0.4395(7) 0.6488(5) 0.3246(4) 0.058(2) Uani 1 1 d . . . H4 H 0.4406 0.6550 0.3692 0.069 Uiso 1 1 d R . . C1 C 0.5700(6) 0.3167(6) 0.3768(4) 0.0400(18) Uani 1 1 d . . . H1 H 0.6036 0.2640 0.3958 0.048 Uiso 1 1 calc R . . C2 C 0.4946(6) 0.3609(6) 0.4154(4) 0.0464(19) Uani 1 1 d . . . H2 H 0.4778 0.3370 0.4592 0.056 Uiso 1 1 calc R . . C3 C 0.4459(6) 0.4401(6) 0.3878(3) 0.0365(15) Uani 1 1 d . . . H3 H 0.3972 0.4712 0.4132 0.044 Uiso 1 1 calc R . . C4 C 0.4706(5) 0.4735(5) 0.3204(4) 0.0336(14) Uani 1 1 d . . . C5 C 0.5444(4) 0.4259(5) 0.2856(3) 0.0277(14) Uani 1 1 d . . . C6 C 0.4172(5) 0.5587(5) 0.2903(4) 0.0377(17) Uani 1 1 d . . . C7 C 0.2752(6) 0.5391(7) 0.2198(5) 0.057(2) Uani 1 1 d . . . C8 C 0.6252(5) 0.0949(5) 0.2453(4) 0.0357(15) Uani 1 1 d . . . C9 C 0.5733(6) 0.0109(5) 0.2282(5) 0.047(2) Uani 1 1 d . . . H9 H 0.5794 -0.0457 0.2546 0.057 Uiso 1 1 calc R . . C10 C 0.5121(8) 0.0139(7) 0.1707(5) 0.062(3) Uani 1 1 d . . . H10 H 0.4762 -0.0407 0.1574 0.075 Uiso 1 1 calc R . . C11 C 0.5061(8) 0.0988(8) 0.1343(6) 0.068(3) Uani 1 1 d . . . H11 H 0.4652 0.1028 0.0957 0.081 Uiso 1 1 calc R . . C12 C 0.5599(7) 0.1784(7) 0.1542(5) 0.059(2) Uani 1 1 d . . . H12 H 0.5548 0.2356 0.1283 0.071 Uiso 1 1 calc R . . C13 C 0.6949(5) 0.0971(5) 0.3082(4) 0.0376(16) Uani 1 1 d . . . S1 S 0.7084(3) 0.2463(3) 0.53353(19) 0.0978(11) Uani 1 1 d . . . O4 O 0.6817(9) 0.3533(8) 0.5425(4) 0.117(4) Uani 1 1 d . . . C14 C 0.8202(15) 0.2463(15) 0.4881(11) 0.163(9) Uani 1 1 d . . . H14A H 0.8090 0.2647 0.4404 0.244 Uiso 1 1 calc R . . H14B H 0.8484 0.1822 0.4896 0.244 Uiso 1 1 calc R . . H14C H 0.8641 0.2922 0.5093 0.244 Uiso 1 1 calc R . . C15 C 0.7406(16) 0.2038(18) 0.6134(10) 0.150(7) Uiso 1 1 d . . . H15A H 0.7385 0.1337 0.6133 0.225 Uiso 1 1 calc R . . H15B H 0.6959 0.2285 0.6477 0.225 Uiso 1 1 calc R . . H15C H 0.8056 0.2253 0.6243 0.225 Uiso 1 1 calc R . . O1W O 0.9419(13) 0.1665(15) 0.7356(6) 0.094(6) Uani 0.50 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 Co1 0.0280(4) 0.0280(4) 0.0355(6) -0.0017(4) -0.0017(4) -0.0006(5) O1 0.042(3) 0.033(3) 0.046(3) 0.003(2) -0.016(2) 0.002(2) O2 0.048(3) 0.054(3) 0.068(4) 0.030(3) -0.021(3) -0.004(3) O3 0.031(3) 0.120(7) 0.102(6) 0.044(5) -0.006(4) -0.007(3) N1 0.027(3) 0.035(3) 0.026(3) 0.010(2) 0.000(2) -0.005(2) N2 0.046(4) 0.039(3) 0.024(3) 0.000(3) -0.013(3) -0.003(3) N3 0.024(3) 0.085(5) 0.069(5) 0.029(4) 0.023(3) 0.000(3) N4 0.089(6) 0.033(3) 0.051(4) 0.000(3) 0.018(4) 0.001(4) C1 0.044(4) 0.049(4) 0.027(3) 0.015(3) 0.002(3) 0.011(3) C2 0.047(5) 0.052(5) 0.040(4) 0.013(4) 0.015(4) 0.006(4) C3 0.039(4) 0.048(4) 0.023(3) 0.002(3) 0.010(3) -0.001(3) C4 0.033(4) 0.033(4) 0.035(3) 0.006(3) 0.005(3) -0.005(3) C5 0.023(3) 0.028(3) 0.031(3) 0.002(3) 0.003(3) -0.006(3) C6 0.028(3) 0.044(4) 0.041(4) 0.009(3) 0.012(3) -0.002(3) C7 0.035(4) 0.065(5) 0.072(6) 0.028(5) 0.000(4) 0.006(4) C8 0.027(3) 0.035(3) 0.045(4) -0.009(4) 0.000(3) 0.001(2) C9 0.040(4) 0.024(4) 0.078(6) -0.007(4) -0.011(4) 0.000(3) C10 0.077(7) 0.042(5) 0.068(6) -0.018(5) -0.027(5) -0.007(4) C11 0.069(6) 0.066(6) 0.069(6) -0.001(5) -0.036(5) -0.021(5) C12 0.064(6) 0.045(5) 0.068(6) 0.001(4) -0.032(5) 0.005(4) C13 0.036(4) 0.035(4) 0.042(4) 0.004(3) 0.001(3) 0.000(3) S1 0.107(2) 0.091(2) 0.096(2) -0.0194(18) -0.007(2) 0.026(2) O4 0.151(10) 0.126(8) 0.074(5) -0.011(5) -0.012(6) 0.065(7) C14 0.146(15) 0.20(2) 0.142(15) -0.068(15) 0.005(13) 0.088(15) O1W 0.096(11) 0.146(16) 0.040(7) 0.011(8) -0.018(7) 0.051(10) _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 O1 2.070(5) . ? Co1 O1 2.070(5) 8_665 ? Co1 N2 2.120(6) . ? Co1 N2 2.120(6) 8_665 ? Co1 N1 2.159(6) . ? Co1 N1 2.159(6) 8_665 ? O1 C13 1.253(9) . ? O2 C13 1.260(9) . ? O3 C7 1.216(12) . ? N1 C1 1.350(9) . ? N1 C5 1.358(8) . ? N2 C8 1.317(10) . ? N2 C12 1.346(10) . ? N3 C7 1.390(13) . ? N3 C6 1.457(9) . ? N3 H3A 0.9300 . ? N4 C7 1.376(11) 8_665 ? N4 C6 1.430(11) . ? N4 H4 0.8600 . ? C1 C2 1.407(11) . ? C1 H1 0.9300 . ? C2 C3 1.378(12) . ? C2 H2 0.9300 . ? C3 C4 1.412(9) . ? C3 H3 0.9300 . ? C4 C5 1.375(10) . ? C4 C6 1.493(10) . ? C5 C5 1.480(13) 8_665 ? C6 C6 1.615(14) 8_665 ? C7 N4 1.376(11) 8_665 ? C8 C9 1.391(10) . ? C8 C13 1.538(10) . ? C9 C10 1.385(12) . ? C9 H9 0.9300 . ? C10 C11 1.358(14) . ? C10 H10 0.9300 . ? C11 C12 1.370(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? S1 O4 1.519(11) . ? S1 C15 1.696(19) . ? S1 C14 1.76(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 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 O1 Co1 O1 98.8(3) . 8_665 ? O1 Co1 N2 78.5(2) . . ? O1 Co1 N2 94.3(2) 8_665 . ? O1 Co1 N2 94.3(2) . 8_665 ? O1 Co1 N2 78.5(2) 8_665 8_665 ? N2 Co1 N2 169.0(3) . 8_665 ? O1 Co1 N1 93.1(2) . . ? O1 Co1 N1 167.2(2) 8_665 . ? N2 Co1 N1 92.6(2) . . ? N2 Co1 N1 96.2(2) 8_665 . ? O1 Co1 N1 167.2(2) . 8_665 ? O1 Co1 N1 93.1(2) 8_665 8_665 ? N2 Co1 N1 96.2(2) . 8_665 ? N2 Co1 N1 92.6(2) 8_665 8_665 ? N1 Co1 N1 75.4(3) . 8_665 ? C13 O1 Co1 116.8(5) . . ? C1 N1 C5 118.6(6) . . ? C1 N1 Co1 124.5(5) . . ? C5 N1 Co1 117.0(4) . . ? C8 N2 C12 117.1(7) . . ? C8 N2 Co1 113.4(5) . . ? C12 N2 Co1 129.5(6) . . ? C7 N3 C6 113.7(7) . . ? C7 N3 H3A 122.8 . . ? C6 N3 H3A 123.4 . . ? C7 N4 C6 114.4(7) 8_665 . ? C7 N4 H4 122.4 8_665 . ? C6 N4 H4 123.2 . . ? N1 C1 C2 121.4(7) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 119.3(7) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.4(7) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 117.9(7) . . ? C5 C4 C6 122.8(6) . . ? C3 C4 C6 119.3(7) . . ? N1 C5 C4 123.4(6) . . ? N1 C5 C5 115.3(4) . 8_665 ? C4 C5 C5 121.3(4) . 8_665 ? N4 C6 N3 111.3(7) . . ? N4 C6 C4 113.0(7) . . ? N3 C6 C4 112.2(6) . . ? N4 C6 C6 102.8(6) . 8_665 ? N3 C6 C6 101.2(7) . 8_665 ? C4 C6 C6 115.5(4) . 8_665 ? O3 C7 N4 127.8(10) . 8_665 ? O3 C7 N3 125.0(9) . . ? N4 C7 N3 107.1(7) 8_665 . ? N2 C8 C9 123.7(7) . . ? N2 C8 C13 115.0(6) . . ? C9 C8 C13 121.3(7) . . ? C10 C9 C8 118.2(8) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C11 C10 C9 118.2(8) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 120.3(9) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? N2 C12 C11 122.5(9) . . ? N2 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? O1 C13 O2 126.2(7) . . ? O1 C13 C8 116.3(6) . . ? O2 C13 C8 117.5(6) . . ? O4 S1 C15 106.8(9) . . ? O4 S1 C14 105.3(9) . . ? C15 S1 C14 102.8(10) . . ? S1 C14 H14A 109.5 . . ? S1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S1 C15 H15A 109.5 . . ? S1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.044 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.111 # Attachment 'CPPZ.CIF' data_cppza _database_code_depnum_ccdc_archive 'CCDC 779558' #TrackingRef 'CPPZ.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Co N6 O4' _chemical_formula_weight 585.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 24.0172(13) _cell_length_b 17.3052(11) _cell_length_c 14.1228(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5869.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 8 _cell_measurement_theta_max 24 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36615 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 24.95 _reflns_number_total 5090 _reflns_number_gt 3925 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0352P)^2^+22.5874P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5090 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1623 _refine_ls_wR_factor_gt 0.1544 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.34367(2) 0.20008(4) 0.63100(5) 0.0292(2) Uani 1 1 d . . . N1 N 0.25568(15) 0.2061(2) 0.6105(3) 0.0286(9) Uani 1 1 d . . . C1 C 0.24203(18) 0.2038(3) 0.5179(3) 0.0267(10) Uani 1 1 d . . . C2 C 0.1869(2) 0.2061(3) 0.4890(4) 0.0385(12) Uani 1 1 d . . . H2 H 0.1778 0.2048 0.4235 0.046 Uiso 1 1 calc R . . C3 C 0.1459(2) 0.2101(4) 0.5560(4) 0.0436(14) Uani 1 1 d . . . H3 H 0.1079 0.2125 0.5377 0.052 Uiso 1 1 calc R . . C4 C 0.1606(2) 0.2106(3) 0.6518(4) 0.0387(12) Uani 1 1 d . . . H4 H 0.1328 0.2115 0.6996 0.046 Uiso 1 1 calc R . . C5 C 0.2162(2) 0.2098(3) 0.6754(4) 0.0329(11) Uani 1 1 d . . . H5 H 0.2264 0.2119 0.7403 0.040 Uiso 1 1 calc R . . C6 C 0.2903(2) 0.1955(3) 0.4487(3) 0.0305(11) Uani 1 1 d . . . O1 O 0.33894(14) 0.1967(2) 0.4859(2) 0.0370(8) Uani 1 1 d . . . O2 O 0.28009(16) 0.1892(3) 0.3646(3) 0.0513(10) Uani 1 1 d . . . N11 N 0.33564(16) 0.0777(2) 0.6488(3) 0.0309(9) Uani 1 1 d . . . C11 C 0.32854(18) 0.0580(3) 0.7403(3) 0.0296(11) Uani 1 1 d . . . C12 C 0.3191(2) -0.0173(3) 0.7692(4) 0.0329(11) Uani 1 1 d . . . H12 H 0.3146 -0.0290 0.8344 0.040 Uiso 1 1 calc R . . C13 C 0.3163(2) -0.0755(3) 0.7013(4) 0.0384(12) Uani 1 1 d . . . H13 H 0.3098 -0.1276 0.7193 0.046 Uiso 1 1 calc R . . C14 C 0.3233(2) -0.0558(3) 0.6069(4) 0.0356(12) Uani 1 1 d . . . H14 H 0.3219 -0.0941 0.5588 0.043 Uiso 1 1 calc R . . C15 C 0.33212(19) 0.0206(3) 0.5846(4) 0.0315(11) Uani 1 1 d . . . H15 H 0.3360 0.0339 0.5196 0.038 Uiso 1 1 calc R . . C16 C 0.3319(2) 0.1245(3) 0.8107(3) 0.0342(12) Uani 1 1 d . . . O11 O 0.33985(14) 0.19129(19) 0.7753(2) 0.0335(8) Uani 1 1 d . . . O12 O 0.3281(2) 0.1095(2) 0.8952(3) 0.0619(13) Uani 1 1 d . . . N21 N 0.43258(15) 0.2067(2) 0.6277(3) 0.0292(9) Uani 1 1 d . . . C21 C 0.45338(18) 0.2795(2) 0.6278(3) 0.0232(9) Uani 1 1 d . . . C22 C 0.41331(18) 0.3434(3) 0.6302(3) 0.0278(10) Uani 1 1 d . . . N22 N 0.35896(15) 0.3229(2) 0.6342(3) 0.0303(9) Uani 1 1 d . . . C23 C 0.3216(2) 0.3786(3) 0.6361(4) 0.0374(12) Uani 1 1 d . . . H23 H 0.2833 0.3648 0.6393 0.045 Uiso 1 1 calc R . . C24 C 0.3354(2) 0.4570(3) 0.6336(4) 0.0426(13) Uani 1 1 d . . . H24 H 0.3071 0.4954 0.6341 0.051 Uiso 1 1 calc R . . C25 C 0.3910(2) 0.4778(3) 0.6304(4) 0.0383(12) Uani 1 1 d . . . H25 H 0.4016 0.5307 0.6295 0.046 Uiso 1 1 calc R . . C26 C 0.4313(2) 0.4196(3) 0.6284(3) 0.0293(10) Uani 1 1 d . . . C27 C 0.49112(19) 0.4367(3) 0.6259(3) 0.0281(10) Uani 1 1 d . . . N23 N 0.50691(18) 0.5102(2) 0.6227(3) 0.0360(10) Uani 1 1 d . . . C28 C 0.5630(2) 0.5235(3) 0.6207(4) 0.0360(12) Uani 1 1 d . . . C29 C 0.5826(3) 0.6011(3) 0.6163(4) 0.0452(14) Uani 1 1 d . . . H29 H 0.5570 0.6429 0.6155 0.054 Uiso 1 1 calc R . . C30 C 0.6390(3) 0.6150(4) 0.6133(4) 0.0521(16) Uani 1 1 d . . . H30 H 0.6521 0.6667 0.6085 0.063 Uiso 1 1 calc R . . C31 C 0.6780(3) 0.5533(4) 0.6173(4) 0.0510(15) Uani 1 1 d . . . H31 H 0.7168 0.5638 0.6164 0.061 Uiso 1 1 calc R . . C32 C 0.6594(2) 0.4791(3) 0.6223(4) 0.0443(13) Uani 1 1 d . . . H32 H 0.6857 0.4381 0.6251 0.053 Uiso 1 1 calc R . . C33 C 0.6022(2) 0.4621(3) 0.6237(4) 0.0370(12) Uani 1 1 d . . . N24 N 0.58503(16) 0.3870(2) 0.6265(3) 0.0336(9) Uani 1 1 d . . . C34 C 0.53028(19) 0.3748(3) 0.6271(3) 0.0298(10) Uani 1 1 d . . . C35 C 0.51056(18) 0.2943(3) 0.6270(3) 0.0265(10) Uani 1 1 d . . . C36 C 0.54705(19) 0.2311(3) 0.6271(4) 0.0328(11) Uani 1 1 d . . . H36 H 0.5862 0.2391 0.6278 0.039 Uiso 1 1 calc R . . C37 C 0.5258(2) 0.1578(3) 0.6263(4) 0.0361(12) Uani 1 1 d . . . H37 H 0.5500 0.1144 0.6259 0.043 Uiso 1 1 calc R . . C38 C 0.4680(2) 0.1473(3) 0.6260(4) 0.0333(11) Uani 1 1 d . . . H38 H 0.4535 0.0963 0.6246 0.040 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0218(3) 0.0358(4) 0.0301(4) 0.0008(3) -0.0003(3) -0.0035(3) N1 0.0262(19) 0.032(2) 0.027(2) -0.0008(18) -0.0005(17) -0.0008(17) C1 0.028(2) 0.023(2) 0.029(2) -0.002(2) -0.004(2) 0.003(2) C2 0.037(3) 0.042(3) 0.037(3) 0.002(2) -0.011(2) 0.003(2) C3 0.023(3) 0.065(4) 0.043(3) 0.006(3) -0.004(2) 0.001(2) C4 0.028(2) 0.050(3) 0.038(3) 0.000(2) 0.003(2) 0.003(2) C5 0.032(3) 0.040(3) 0.027(3) 0.000(2) 0.000(2) 0.000(2) C6 0.036(3) 0.025(2) 0.031(3) -0.001(2) -0.001(2) 0.007(2) O1 0.0306(18) 0.048(2) 0.0320(18) 0.0026(16) 0.0052(15) 0.0019(17) O2 0.051(2) 0.076(3) 0.026(2) -0.004(2) 0.0002(18) 0.015(2) N11 0.024(2) 0.042(2) 0.026(2) -0.0044(18) -0.0001(17) -0.0047(18) C11 0.018(2) 0.041(3) 0.030(3) 0.001(2) 0.0003(19) -0.008(2) C12 0.032(3) 0.038(3) 0.029(3) 0.002(2) 0.001(2) -0.005(2) C13 0.034(3) 0.033(3) 0.048(3) 0.005(2) -0.001(2) -0.007(2) C14 0.032(3) 0.040(3) 0.035(3) -0.009(2) 0.003(2) -0.007(2) C15 0.028(3) 0.037(3) 0.030(3) -0.001(2) 0.000(2) -0.007(2) C16 0.032(3) 0.045(3) 0.026(3) -0.002(2) -0.004(2) -0.010(2) O11 0.0322(18) 0.0378(19) 0.0304(18) -0.0045(15) -0.0022(15) -0.0031(16) O12 0.102(4) 0.057(3) 0.027(2) -0.0005(18) 0.007(2) -0.030(2) N21 0.0268(19) 0.029(2) 0.032(2) 0.0032(19) -0.0012(17) 0.0014(17) C21 0.032(2) 0.019(2) 0.019(2) 0.0026(18) 0.000(2) 0.0011(17) C22 0.023(2) 0.038(3) 0.022(2) 0.000(2) 0.000(2) 0.0017(19) N22 0.027(2) 0.031(2) 0.033(2) -0.0006(18) 0.0007(18) 0.0014(16) C23 0.026(2) 0.040(3) 0.046(3) 0.001(3) -0.001(2) -0.004(2) C24 0.035(3) 0.036(3) 0.057(4) -0.002(3) -0.004(3) 0.010(2) C25 0.039(3) 0.035(3) 0.040(3) -0.003(3) -0.005(3) 0.000(2) C26 0.035(3) 0.030(2) 0.023(2) 0.004(2) -0.001(2) 0.002(2) C27 0.032(2) 0.029(2) 0.024(2) 0.002(2) -0.005(2) -0.0041(19) N23 0.044(2) 0.033(2) 0.030(2) 0.0011(19) -0.006(2) -0.0059(19) C28 0.040(3) 0.038(3) 0.030(3) 0.007(2) -0.006(2) -0.014(2) C29 0.062(4) 0.030(3) 0.043(3) 0.007(2) -0.006(3) -0.014(3) C30 0.060(4) 0.056(4) 0.041(3) 0.003(3) -0.003(3) -0.029(3) C31 0.044(3) 0.066(4) 0.042(3) 0.006(3) -0.001(3) -0.027(3) C32 0.040(3) 0.048(3) 0.045(3) 0.001(3) -0.001(3) -0.013(3) C33 0.045(3) 0.038(3) 0.029(3) 0.004(2) -0.003(2) -0.014(2) N24 0.029(2) 0.038(2) 0.034(2) 0.004(2) 0.0023(19) -0.0080(17) C34 0.029(2) 0.042(3) 0.018(2) 0.006(2) 0.003(2) -0.004(2) C35 0.028(2) 0.029(2) 0.022(2) 0.004(2) 0.0011(19) -0.0036(19) C36 0.019(2) 0.043(3) 0.036(3) 0.010(2) 0.004(2) 0.001(2) C37 0.030(2) 0.033(3) 0.045(3) 0.004(2) 0.003(2) 0.000(2) C38 0.031(2) 0.027(2) 0.041(3) 0.002(2) -0.003(2) -0.002(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 O11 2.045(3) . ? Co1 O1 2.053(3) . ? Co1 N1 2.136(4) . ? Co1 N21 2.139(4) . ? Co1 N11 2.142(4) . ? Co1 N22 2.158(4) . ? N1 C5 1.320(6) . ? N1 C1 1.350(6) . ? C1 C2 1.385(6) . ? C1 C6 1.522(6) . ? C2 C3 1.369(7) . ? C3 C4 1.398(7) . ? C4 C5 1.376(7) . ? C6 O2 1.218(6) . ? C6 O1 1.281(6) . ? N11 C15 1.344(6) . ? N11 C11 1.347(6) . ? C11 C12 1.383(7) . ? C11 C16 1.523(7) . ? C12 C13 1.392(7) . ? C13 C14 1.387(7) . ? C14 C15 1.376(7) . ? C16 O12 1.225(6) . ? C16 O11 1.274(6) . ? N21 C38 1.334(6) . ? N21 C21 1.356(6) . ? C21 C35 1.397(6) . ? C21 C22 1.465(6) . ? C22 N22 1.354(6) . ? C22 C26 1.389(6) . ? N22 C23 1.318(6) . ? C23 C24 1.397(7) . ? C24 C25 1.385(7) . ? C25 C26 1.396(7) . ? C26 C27 1.467(7) . ? C27 N23 1.328(6) . ? C27 C34 1.426(7) . ? N23 C28 1.367(6) . ? C28 C33 1.420(7) . ? C28 C29 1.425(7) . ? C29 C30 1.375(8) . ? C30 C31 1.421(9) . ? C31 C32 1.360(8) . ? C32 C33 1.407(7) . ? C33 N24 1.363(6) . ? N24 C34 1.332(6) . ? C34 C35 1.472(6) . ? C35 C36 1.401(6) . ? C36 C37 1.367(7) . ? C37 C38 1.400(7) . ? 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 O11 Co1 O1 171.75(13) . . ? O11 Co1 N1 95.39(14) . . ? O1 Co1 N1 79.14(14) . . ? O11 Co1 N21 94.04(15) . . ? O1 Co1 N21 92.01(15) . . ? N1 Co1 N21 169.25(15) . . ? O11 Co1 N11 78.76(14) . . ? O1 Co1 N11 94.82(15) . . ? N1 Co1 N11 88.55(15) . . ? N21 Co1 N11 98.36(15) . . ? O11 Co1 N22 93.43(15) . . ? O1 Co1 N22 93.37(16) . . ? N1 Co1 N22 97.10(15) . . ? N21 Co1 N22 77.17(14) . . ? N11 Co1 N22 170.80(15) . . ? C5 N1 C1 120.0(4) . . ? C5 N1 Co1 128.3(3) . . ? C1 N1 Co1 111.7(3) . . ? N1 C1 C2 121.1(4) . . ? N1 C1 C6 116.1(4) . . ? C2 C1 C6 122.7(4) . . ? C3 C2 C1 119.1(5) . . ? C2 C3 C4 119.2(5) . . ? C5 C4 C3 118.7(5) . . ? N1 C5 C4 122.0(5) . . ? O2 C6 O1 125.8(5) . . ? O2 C6 C1 118.8(4) . . ? O1 C6 C1 115.5(4) . . ? C6 O1 Co1 117.4(3) . . ? C15 N11 C11 117.0(4) . . ? C15 N11 Co1 130.8(3) . . ? C11 N11 Co1 112.0(3) . . ? N11 C11 C12 122.8(5) . . ? N11 C11 C16 115.3(4) . . ? C12 C11 C16 121.9(4) . . ? C11 C12 C13 119.1(5) . . ? C14 C13 C12 118.6(5) . . ? C15 C14 C13 118.4(5) . . ? N11 C15 C14 124.1(5) . . ? O12 C16 O11 125.9(5) . . ? O12 C16 C11 118.2(5) . . ? O11 C16 C11 115.9(4) . . ? C16 O11 Co1 117.7(3) . . ? C38 N21 C21 118.7(4) . . ? C38 N21 Co1 126.6(3) . . ? C21 N21 Co1 114.7(3) . . ? N21 C21 C35 122.1(4) . . ? N21 C21 C22 117.3(4) . . ? C35 C21 C22 120.5(4) . . ? N22 C22 C26 123.3(4) . . ? N22 C22 C21 115.9(4) . . ? C26 C22 C21 120.8(4) . . ? C23 N22 C22 117.8(4) . . ? C23 N22 Co1 127.3(3) . . ? C22 N22 Co1 114.9(3) . . ? N22 C23 C24 123.2(5) . . ? C25 C24 C23 118.8(5) . . ? C24 C25 C26 118.8(5) . . ? C22 C26 C25 118.0(4) . . ? C22 C26 C27 119.8(4) . . ? C25 C26 C27 122.2(4) . . ? N23 C27 C34 122.1(4) . . ? N23 C27 C26 118.3(4) . . ? C34 C27 C26 119.6(4) . . ? C27 N23 C28 116.3(4) . . ? N23 C28 C33 121.8(4) . . ? N23 C28 C29 119.0(5) . . ? C33 C28 C29 119.2(5) . . ? C30 C29 C28 119.5(6) . . ? C29 C30 C31 121.0(5) . . ? C32 C31 C30 119.7(5) . . ? C31 C32 C33 121.2(6) . . ? N24 C33 C32 119.7(5) . . ? N24 C33 C28 120.9(4) . . ? C32 C33 C28 119.3(5) . . ? C34 N24 C33 116.7(4) . . ? N24 C34 C27 122.1(4) . . ? N24 C34 C35 117.9(4) . . ? C27 C34 C35 119.9(4) . . ? C21 C35 C36 118.2(4) . . ? C21 C35 C34 119.3(4) . . ? C36 C35 C34 122.5(4) . . ? C37 C36 C35 119.3(4) . . ? C36 C37 C38 119.4(5) . . ? N21 C38 C37 122.2(5) . . ? # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 -0.006 526.0 39.3 2 1.000 0.500 -0.010 525.9 39.1 _platon_squeeze_details ; N: No S.U.'s (esd) on observed/calculated parameters. #------------------------------------------------------------------------------- N: Number of moved primary input atoms: .................................. 59 N: Number of Ignored Lines on INPUT ...................................... 2 of which blank in column 1 ..................................... 2 N: Total Potential Solvent Accessible Void Vol .................. 1049.8 Ang^3 N: Electron Count / Cell = 78 - To be included in D(calc), F000 & Mol.Wght. ; _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.421 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.078 # Attachment 'CPQ.CIF' data_cpq _database_code_depnum_ccdc_archive 'CCDC 779559' #TrackingRef 'CPQ.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 Co N6 O4' _chemical_formula_weight 535.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5253(5) _cell_length_b 18.4782(15) _cell_length_c 13.9892(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.898(7) _cell_angle_gamma 90.00 _cell_volume 2198.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 6 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9881 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4289 _reflns_number_gt 3143 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0843P)^2^+1.2311P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4289 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.61918(5) 0.24907(2) 0.32798(3) 0.01657(17) Uani 1 1 d . . . C1 C 0.5970(4) 0.09545(17) 0.3757(2) 0.0219(7) Uani 1 1 d . . . C2 C 0.6333(5) 0.0241(2) 0.3997(3) 0.0338(9) Uani 1 1 d . . . H2 H 0.5523 -0.0105 0.4058 0.041 Uiso 1 1 calc R . . C3 C 0.7896(6) 0.0045(2) 0.4147(4) 0.0427(11) Uani 1 1 d . . . H3 H 0.8170 -0.0440 0.4309 0.051 Uiso 1 1 calc R . . C4 C 0.9059(5) 0.0557(2) 0.4059(3) 0.0366(9) Uani 1 1 d . . . H4 H 1.0138 0.0430 0.4153 0.044 Uiso 1 1 calc R . . C5 C 0.8610(4) 0.12635(19) 0.3829(3) 0.0263(8) Uani 1 1 d . . . H5 H 0.9405 0.1619 0.3774 0.032 Uiso 1 1 calc R . . N1 N 0.7113(3) 0.14602(14) 0.3684(2) 0.0202(6) Uani 1 1 d . . . C6 C 0.4295(4) 0.12199(18) 0.3540(2) 0.0219(7) Uani 1 1 d . . . O1 O 0.4183(3) 0.18709(13) 0.32328(17) 0.0230(5) Uani 1 1 d . . . O2 O 0.3189(3) 0.08064(14) 0.3674(2) 0.0344(7) Uani 1 1 d . . . N21 N 0.6007(3) 0.28763(15) 0.4720(2) 0.0184(6) Uani 1 1 d . . . C21 C 0.5054(4) 0.34635(17) 0.4790(2) 0.0188(7) Uani 1 1 d . . . C22 C 0.4364(4) 0.37642(17) 0.3897(2) 0.0188(7) Uani 1 1 d . . . N22 N 0.4762(3) 0.34510(15) 0.3063(2) 0.0186(6) Uani 1 1 d . . . C23 C 0.4162(4) 0.37395(18) 0.2245(3) 0.0224(7) Uani 1 1 d . . . H23 H 0.4442 0.3528 0.1662 0.027 Uiso 1 1 calc R . . C24 C 0.3149(4) 0.43317(19) 0.2191(3) 0.0269(8) Uani 1 1 d . . . H24 H 0.2753 0.4516 0.1588 0.032 Uiso 1 1 calc R . . C25 C 0.2734(4) 0.46461(18) 0.3035(3) 0.0262(8) Uani 1 1 d . . . H25 H 0.2046 0.5051 0.3019 0.031 Uiso 1 1 calc R . . C26 C 0.3335(4) 0.43623(17) 0.3912(3) 0.0210(7) Uani 1 1 d . . . C27 C 0.2961(4) 0.46610(18) 0.4841(3) 0.0238(7) Uani 1 1 d . . . N23 N 0.1911(4) 0.52181(16) 0.4837(3) 0.0347(8) Uani 1 1 d . . . C28 C 0.1573(5) 0.5454(2) 0.5697(4) 0.0389(10) Uani 1 1 d . . . H28 H 0.0833 0.5835 0.5734 0.047 Uiso 1 1 calc R . . C29 C 0.2256(5) 0.5167(2) 0.6547(3) 0.0376(10) Uani 1 1 d . . . H29 H 0.1970 0.5363 0.7138 0.045 Uiso 1 1 calc R . . N24 N 0.3288(4) 0.46301(17) 0.6566(2) 0.0333(8) Uani 1 1 d . . . C30 C 0.3638(4) 0.43733(19) 0.5691(3) 0.0237(8) Uani 1 1 d . . . C31 C 0.4758(4) 0.37768(18) 0.5673(2) 0.0207(7) Uani 1 1 d . . . C32 C 0.5538(4) 0.3491(2) 0.6503(3) 0.0259(8) Uani 1 1 d . . . H32 H 0.5395 0.3702 0.7110 0.031 Uiso 1 1 calc R . . C33 C 0.6513(4) 0.2902(2) 0.6431(3) 0.0269(8) Uani 1 1 d . . . H33 H 0.7054 0.2703 0.6986 0.032 Uiso 1 1 calc R . . C34 C 0.6693(4) 0.26010(19) 0.5522(2) 0.0215(7) Uani 1 1 d . . . H34 H 0.7333 0.2183 0.5478 0.026 Uiso 1 1 calc R . . C11 C 0.7671(4) 0.28515(17) 0.1529(2) 0.0183(7) Uani 1 1 d . . . C12 C 0.7904(4) 0.30032(19) 0.0575(3) 0.0238(7) Uani 1 1 d . . . H12 H 0.8696 0.3334 0.0412 0.029 Uiso 1 1 calc R . . C13 C 0.6955(4) 0.2661(2) -0.0134(3) 0.0277(8) Uani 1 1 d . . . H13 H 0.7081 0.2758 -0.0791 0.033 Uiso 1 1 calc R . . C14 C 0.5816(4) 0.2174(2) 0.0130(3) 0.0261(8) Uani 1 1 d . . . H14 H 0.5164 0.1928 -0.0343 0.031 Uiso 1 1 calc R . . C15 C 0.5651(4) 0.20526(19) 0.1103(3) 0.0230(7) Uani 1 1 d . . . H15 H 0.4879 0.1718 0.1283 0.028 Uiso 1 1 calc R . . N11 N 0.6540(3) 0.23907(14) 0.1792(2) 0.0178(6) Uani 1 1 d . . . C16 C 0.8659(4) 0.32005(17) 0.2350(3) 0.0212(7) Uani 1 1 d . . . O11 O 0.8316(3) 0.30098(13) 0.31897(18) 0.0244(5) Uani 1 1 d . . . O12 O 0.9699(3) 0.36287(14) 0.2154(2) 0.0338(7) 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 0.0199(3) 0.0170(3) 0.0129(2) 0.00004(17) 0.00187(16) 0.00044(17) C1 0.0322(19) 0.0166(15) 0.0169(18) -0.0042(13) 0.0011(14) -0.0028(14) C2 0.044(2) 0.0214(17) 0.037(2) 0.0024(16) 0.0044(18) -0.0019(16) C3 0.057(3) 0.0177(18) 0.052(3) 0.0050(18) -0.004(2) 0.0096(18) C4 0.037(2) 0.034(2) 0.038(2) 0.0008(18) -0.0037(18) 0.0127(17) C5 0.0283(19) 0.0267(18) 0.0238(19) -0.0002(15) 0.0013(15) 0.0039(14) N1 0.0267(15) 0.0194(13) 0.0145(14) -0.0021(11) 0.0014(11) 0.0025(11) C6 0.0279(18) 0.0227(16) 0.0154(17) -0.0061(13) 0.0041(14) -0.0045(14) O1 0.0260(13) 0.0235(12) 0.0197(13) 0.0017(10) 0.0023(10) -0.0014(10) O2 0.0343(15) 0.0272(14) 0.0426(18) -0.0065(12) 0.0087(13) -0.0135(11) N21 0.0157(13) 0.0225(14) 0.0166(14) 0.0001(11) -0.0015(11) -0.0011(11) C21 0.0223(16) 0.0167(15) 0.0179(17) 0.0001(12) 0.0054(13) -0.0011(12) C22 0.0207(16) 0.0160(15) 0.0199(17) -0.0012(13) 0.0032(13) -0.0043(12) N22 0.0192(13) 0.0207(13) 0.0156(14) 0.0023(11) 0.0002(11) -0.0009(11) C23 0.0254(17) 0.0227(16) 0.0183(17) 0.0011(13) -0.0032(14) -0.0002(13) C24 0.0281(19) 0.0252(17) 0.027(2) 0.0096(15) -0.0015(15) 0.0010(14) C25 0.0248(18) 0.0203(16) 0.033(2) 0.0032(15) 0.0009(15) 0.0030(14) C26 0.0177(16) 0.0160(15) 0.030(2) 0.0016(14) 0.0061(13) -0.0021(12) C27 0.0221(16) 0.0174(15) 0.033(2) -0.0012(14) 0.0080(14) -0.0043(13) N23 0.0351(18) 0.0189(15) 0.052(2) -0.0023(14) 0.0165(16) 0.0021(13) C28 0.041(2) 0.0226(18) 0.056(3) -0.0106(18) 0.020(2) 0.0007(16) C29 0.048(2) 0.0254(19) 0.042(3) -0.0125(17) 0.022(2) -0.0037(17) N24 0.0445(19) 0.0265(16) 0.0308(19) -0.0083(14) 0.0165(15) -0.0049(14) C30 0.0260(18) 0.0217(17) 0.0242(19) -0.0068(14) 0.0078(14) -0.0047(13) C31 0.0214(16) 0.0219(16) 0.0194(17) -0.0026(13) 0.0060(13) -0.0072(13) C32 0.0276(18) 0.0343(19) 0.0162(18) -0.0047(15) 0.0045(14) -0.0061(15) C33 0.0259(19) 0.038(2) 0.0161(18) 0.0026(15) 0.0004(14) -0.0030(15) C34 0.0188(16) 0.0316(18) 0.0137(16) 0.0030(14) -0.0007(12) 0.0025(13) C11 0.0200(16) 0.0163(15) 0.0190(17) 0.0008(12) 0.0048(13) 0.0021(12) C12 0.0275(18) 0.0242(17) 0.0203(18) 0.0031(14) 0.0064(14) 0.0044(14) C13 0.032(2) 0.036(2) 0.0158(17) 0.0025(14) 0.0057(15) 0.0073(15) C14 0.0236(18) 0.0334(19) 0.0208(19) -0.0049(15) -0.0019(14) -0.0006(15) C15 0.0217(17) 0.0268(17) 0.0209(18) -0.0040(14) 0.0042(14) -0.0022(13) N11 0.0186(14) 0.0169(13) 0.0186(14) -0.0017(11) 0.0055(11) 0.0021(10) C16 0.0220(17) 0.0168(15) 0.0249(18) -0.0031(13) 0.0029(14) 0.0019(13) O11 0.0264(13) 0.0269(12) 0.0196(13) -0.0024(10) -0.0010(10) -0.0057(10) O12 0.0326(15) 0.0317(14) 0.0379(16) -0.0046(12) 0.0092(12) -0.0153(11) _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 O1 2.058(2) . ? Co1 O11 2.061(2) . ? Co1 N1 2.122(3) . ? Co1 N11 2.130(3) . ? Co1 N21 2.153(3) . ? Co1 N22 2.162(3) . ? C1 N1 1.358(4) . ? C1 C2 1.390(5) . ? C1 C6 1.521(5) . ? C2 C3 1.383(6) . ? C3 C4 1.382(6) . ? C4 C5 1.391(5) . ? C5 N1 1.330(5) . ? C6 O2 1.238(4) . ? C6 O1 1.279(4) . ? N21 C34 1.331(4) . ? N21 C21 1.363(4) . ? C21 C31 1.402(5) . ? C21 C22 1.455(5) . ? C22 N22 1.365(4) . ? C22 C26 1.412(5) . ? N22 C23 1.333(4) . ? C23 C24 1.392(5) . ? C24 C25 1.383(5) . ? C25 C26 1.399(5) . ? C26 C27 1.467(5) . ? C27 N23 1.364(5) . ? C27 C30 1.392(5) . ? N23 C28 1.330(6) . ? C28 C29 1.393(7) . ? C29 N24 1.325(5) . ? N24 C30 1.364(4) . ? C30 C31 1.459(5) . ? C31 C32 1.401(5) . ? C32 C33 1.377(5) . ? C33 C34 1.407(5) . ? C11 N11 1.356(4) . ? C11 C12 1.391(5) . ? C11 C16 1.520(5) . ? C12 C13 1.390(5) . ? C13 C14 1.392(5) . ? C14 C15 1.396(5) . ? C15 N11 1.339(4) . ? C16 O12 1.233(4) . ? C16 O11 1.279(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O11 171.94(9) . . ? O1 Co1 N1 78.52(10) . . ? O11 Co1 N1 97.07(10) . . ? O1 Co1 N11 95.24(10) . . ? O11 Co1 N11 78.42(10) . . ? N1 Co1 N11 96.25(10) . . ? O1 Co1 N21 95.76(10) . . ? O11 Co1 N21 91.37(10) . . ? N1 Co1 N21 95.57(11) . . ? N11 Co1 N21 165.23(10) . . ? O1 Co1 N22 89.56(10) . . ? O11 Co1 N22 95.68(10) . . ? N1 Co1 N22 165.61(11) . . ? N11 Co1 N22 92.81(10) . . ? N21 Co1 N22 77.46(11) . . ? N1 C1 C2 121.4(3) . . ? N1 C1 C6 115.6(3) . . ? C2 C1 C6 123.0(3) . . ? C3 C2 C1 118.8(4) . . ? C4 C3 C2 119.8(4) . . ? C3 C4 C5 118.4(4) . . ? N1 C5 C4 122.5(4) . . ? C5 N1 C1 119.1(3) . . ? C5 N1 Co1 128.3(2) . . ? C1 N1 Co1 112.5(2) . . ? O2 C6 O1 126.3(3) . . ? O2 C6 C1 119.0(3) . . ? O1 C6 C1 114.7(3) . . ? C6 O1 Co1 118.0(2) . . ? C34 N21 C21 118.3(3) . . ? C34 N21 Co1 127.3(2) . . ? C21 N21 Co1 114.4(2) . . ? N21 C21 C31 122.4(3) . . ? N21 C21 C22 116.8(3) . . ? C31 C21 C22 120.8(3) . . ? N22 C22 C26 122.4(3) . . ? N22 C22 C21 117.5(3) . . ? C26 C22 C21 120.1(3) . . ? C23 N22 C22 117.4(3) . . ? C23 N22 Co1 128.9(2) . . ? C22 N22 Co1 113.5(2) . . ? N22 C23 C24 124.2(3) . . ? C25 C24 C23 118.5(3) . . ? C24 C25 C26 119.4(3) . . ? C25 C26 C22 118.1(3) . . ? C25 C26 C27 123.2(3) . . ? C22 C26 C27 118.7(3) . . ? N23 C27 C30 121.7(3) . . ? N23 C27 C26 117.6(3) . . ? C30 C27 C26 120.7(3) . . ? C28 N23 C27 115.3(4) . . ? N23 C28 C29 122.9(4) . . ? N24 C29 C28 122.7(4) . . ? C29 N24 C30 115.3(4) . . ? N24 C30 C27 122.0(3) . . ? N24 C30 C31 117.5(3) . . ? C27 C30 C31 120.5(3) . . ? C32 C31 C21 118.0(3) . . ? C32 C31 C30 123.0(3) . . ? C21 C31 C30 119.0(3) . . ? C33 C32 C31 119.5(3) . . ? C32 C33 C34 118.8(3) . . ? N21 C34 C33 122.9(3) . . ? N11 C11 C12 122.5(3) . . ? N11 C11 C16 115.4(3) . . ? C12 C11 C16 122.1(3) . . ? C13 C12 C11 118.6(3) . . ? C12 C13 C14 119.2(3) . . ? C13 C14 C15 118.7(3) . . ? N11 C15 C14 122.5(3) . . ? C15 N11 C11 118.4(3) . . ? C15 N11 Co1 129.4(2) . . ? C11 N11 Co1 111.0(2) . . ? O12 C16 O11 126.4(3) . . ? O12 C16 C11 118.3(3) . . ? O11 C16 C11 115.3(3) . . ? C16 O11 Co1 116.2(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.739 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.095