# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Peter Comba' _publ_contact_author_address ; Peter Comba Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone +49-6221-548529 _publ_contact_author_fax +49-6221-546617 _publ_contact_author_email peter.comba@aci.uni-heidelberg.de _publ_section_title ; Oxidative N-dealkylation in cobalt-bispidine-H2O2 systems ; loop_ _publ_author_name 'P. Comba' 'Shigemasa Kuwata' 'Gerald Linti' 'Hans Pritzkow' 'Mate Tarnai' 'Hubert Wadepohl' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 600455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C22H25Cl2CoN4_ClO4_0.25CH3CN _chemical_formula_sum 'C22.50 H25.75 Cl3 Co N4.25 O10' _chemical_formula_weight 681.00 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3160(17) _cell_length_b 12.937(3) _cell_length_c 13.434(3) _cell_angle_alpha 77.85(3) _cell_angle_beta 76.36(3) _cell_angle_gamma 82.11(3) _cell_volume 1367.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.513 _exptl_crystal_size_mid 0.427 _exptl_crystal_size_min 0.162 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 697 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 8697 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 24.01 _reflns_number_total 4001 _reflns_number_gt 3095 _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^)+(0.1065P)^2^+1.0350P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4001 _refine_ls_number_parameters 437 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1681 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.003 _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 0.22341(8) 0.88703(5) 0.18141(5) 0.0235(2) Uani 1 1 d . . . Cl2 Cl -0.04904(16) 0.94117(10) 0.21168(10) 0.0308(3) Uani 1 1 d . . . Cl1 Cl 0.26958(17) 1.03566(10) 0.06042(11) 0.0411(4) Uani 1 1 d . . . N1 N 0.2139(5) 0.7537(3) 0.2838(3) 0.0205(9) Uani 1 1 d . . . N2 N 0.4723(5) 0.8514(3) 0.1447(3) 0.0241(9) Uani 1 1 d . . . N3 N 0.2327(5) 0.9495(3) 0.2999(3) 0.0272(10) Uani 1 1 d . . . N4 N 0.1818(5) 0.8007(3) 0.0920(3) 0.0271(10) Uani 1 1 d . . . C1 C 0.3110(6) 0.7668(4) 0.3597(4) 0.0217(11) Uani 1 1 d . . . H1A H 0.2818 0.7132 0.4250 0.026 Uiso 1 1 calc R . . C2 C 0.5018(6) 0.7560(4) 0.3181(4) 0.0221(11) Uani 1 1 d . . . C3 C 0.5541(6) 0.6508(4) 0.2777(4) 0.0245(11) Uani 1 1 d . . . C4 C 0.4709(6) 0.6576(4) 0.1834(4) 0.0234(11) Uani 1 1 d . . . C5 C 0.2793(6) 0.6664(4) 0.2207(4) 0.0210(11) Uani 1 1 d . . . H5A H 0.2438 0.5969 0.2634 0.025 Uiso 1 1 calc R . . C6 C 0.5596(6) 0.8487(4) 0.2294(4) 0.0250(11) Uani 1 1 d . . . H6A H 0.5331 0.9166 0.2553 0.030 Uiso 1 1 calc R . . H6B H 0.6812 0.8384 0.2032 0.030 Uiso 1 1 calc R . . C7 C 0.5307(6) 0.7539(4) 0.1007(4) 0.0242(11) Uani 1 1 d . . . H7A H 0.6536 0.7469 0.0804 0.029 Uiso 1 1 calc R . . H7B H 0.4860 0.7575 0.0379 0.029 Uiso 1 1 calc R . . C8 C 0.2578(6) 0.8759(4) 0.3833(4) 0.0271(12) Uani 1 1 d . . . C9 C 0.2471(7) 0.9037(4) 0.4789(4) 0.0311(12) Uani 1 1 d . . . H9A H 0.2640 0.8512 0.5376 0.037 Uiso 1 1 calc R . . C10 C 0.2116(8) 1.0087(5) 0.4871(5) 0.0410(15) Uani 1 1 d . . . H10A H 0.2050 1.0296 0.5517 0.049 Uiso 1 1 calc R . . C11 C 0.1857(7) 1.0832(4) 0.4022(5) 0.0411(15) Uani 1 1 d . . . H11A H 0.1619 1.1561 0.4071 0.049 Uiso 1 1 calc R . . C12 C 0.1946(7) 1.0509(4) 0.3088(5) 0.0342(13) Uani 1 1 d . . . H12A H 0.1732 1.1020 0.2503 0.041 Uiso 1 1 calc R . . C13 C 0.1977(6) 0.6952(4) 0.1292(4) 0.0225(11) Uani 1 1 d . . . C14 C 0.1465(7) 0.6222(4) 0.0852(4) 0.0327(13) Uani 1 1 d . . . H14A H 0.1570 0.5486 0.1141 0.039 Uiso 1 1 calc R . . C15 C 0.0786(8) 0.6586(5) -0.0031(5) 0.0440(16) Uani 1 1 d . . . H15A H 0.0418 0.6100 -0.0352 0.053 Uiso 1 1 calc R . . C16 C 0.0659(8) 0.7656(5) -0.0427(4) 0.0452(17) Uani 1 1 d . . . H16A H 0.0227 0.7918 -0.1036 0.054 Uiso 1 1 calc R . . C17 C 0.1167(7) 0.8349(5) 0.0073(4) 0.0361(14) Uani 1 1 d . . . H17A H 0.1050 0.9090 -0.0194 0.043 Uiso 1 1 calc R . . C18 C 0.5860(7) 0.7595(4) 0.4065(4) 0.0280(12) Uani 1 1 d . . . C19 C 0.6418(11) 0.6691(6) 0.5686(5) 0.063(2) Uani 1 1 d . . . H19A H 0.6398 0.5977 0.6113 0.094 Uiso 1 1 calc R . . H19B H 0.5811 0.7208 0.6111 0.094 Uiso 1 1 calc R . . H19C H 0.7572 0.6862 0.5419 0.094 Uiso 1 1 calc R . . C20 C 0.5335(7) 0.5577(4) 0.1372(4) 0.0255(12) Uani 1 1 d . . . C21 C 0.4958(9) 0.3770(4) 0.1517(5) 0.0420(15) Uani 1 1 d . . . H21A H 0.4114 0.3271 0.1840 0.063 Uiso 1 1 calc R . . H21B H 0.5999 0.3489 0.1739 0.063 Uiso 1 1 calc R . . H21C H 0.5145 0.3862 0.0757 0.063 Uiso 1 1 calc R . . C22 C 0.0437(6) 0.7274(4) 0.3454(4) 0.0250(11) Uani 1 1 d . . . H22A H 0.0533 0.6609 0.3953 0.038 Uiso 1 1 calc R . . H22B H -0.0250 0.7195 0.2979 0.038 Uiso 1 1 calc R . . H22C H -0.0080 0.7848 0.3832 0.038 Uiso 1 1 calc R . . O1 O 0.6591(5) 0.8301(3) 0.4112(3) 0.0374(10) Uani 1 1 d . . . O2 O 0.5641(6) 0.6731(3) 0.4820(3) 0.0466(11) Uani 1 1 d . . . O3 O 0.7267(4) 0.6420(3) 0.2505(3) 0.0300(9) Uani 1 1 d . . . H3A H 0.7587 0.6163 0.1959 0.045 Uiso 1 1 calc R . . O4 O 0.4938(5) 0.5626(2) 0.3509(3) 0.0283(8) Uani 1 1 d . . . H4A H 0.4974 0.5702 0.4109 0.042 Uiso 1 1 calc R . . O5 O 0.6550(5) 0.5520(3) 0.0688(3) 0.0370(10) Uani 1 1 d . . . O6 O 0.4393(5) 0.4783(3) 0.1833(3) 0.0322(9) Uani 1 1 d . . . Cl3 Cl 0.9449(12) 0.3768(7) 0.3058(5) 0.0396(15) Uani 0.50 1 d P A 1 O9 O 0.882(5) 0.4405(19) 0.231(2) 0.070(9) Uani 0.50 1 d P A 1 O10 O 0.870(5) 0.2757(15) 0.307(2) 0.228(16) Uani 0.50 1 d P A 1 O11 O 0.807(2) 0.415(2) 0.4141(12) 0.188(12) Uani 0.50 1 d P A 1 O12 O 1.060(5) 0.371(4) 0.308(2) 0.27(3) Uani 0.50 1 d P A 1 Cl3A Cl 0.9119(18) 0.3873(13) 0.3317(10) 0.127(6) Uani 0.50 1 d P B 2 O13 O 1.0901(19) 0.3197(13) 0.2495(13) 0.110(6) Uani 0.50 1 d P B 2 O14 O 0.910(2) 0.3093(13) 0.3964(12) 0.127(7) Uani 0.50 1 d P B 2 O15 O 1.038(2) 0.4602(10) 0.3310(12) 0.094(5) Uani 0.50 1 d P B 2 O16 O 0.842(4) 0.433(2) 0.240(2) 0.073(10) Uani 0.50 1 d P B 2 N31 N 0.460(4) 0.865(2) -0.139(2) 0.079(9) Uani 0.25 1 d PD . . C31 C 0.344(5) 0.878(3) -0.297(2) 0.102(17) Uani 0.25 1 d PD . . H31A H 0.4082 0.8254 -0.3381 0.153 Uiso 0.25 1 calc PR . . H31B H 0.3457 0.9484 -0.3409 0.153 Uiso 0.25 1 calc PR . . H31C H 0.2290 0.8593 -0.2721 0.153 Uiso 0.25 1 calc PR . . C32 C 0.412(4) 0.877(3) -0.215(3) 0.097(15) Uani 0.25 1 d PD . . 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 0.0178(4) 0.0238(4) 0.0238(4) 0.0023(3) -0.0005(3) -0.0015(3) Cl2 0.0183(7) 0.0351(7) 0.0348(7) -0.0020(5) -0.0029(5) -0.0001(5) Cl1 0.0281(8) 0.0333(7) 0.0433(8) 0.0162(6) 0.0051(6) 0.0030(6) N1 0.021(2) 0.027(2) 0.0127(19) -0.0027(15) -0.0026(16) -0.0022(17) N2 0.018(2) 0.024(2) 0.025(2) 0.0012(16) 0.0013(17) -0.0026(17) N3 0.014(2) 0.024(2) 0.041(3) -0.0039(18) 0.0005(19) -0.0044(17) N4 0.016(2) 0.036(2) 0.023(2) -0.0003(18) 0.0012(17) 0.0020(18) C1 0.019(3) 0.027(2) 0.019(2) -0.0038(19) 0.0002(19) -0.007(2) C2 0.022(3) 0.023(2) 0.021(2) -0.0008(19) -0.003(2) -0.006(2) C3 0.022(3) 0.021(2) 0.026(3) 0.003(2) -0.005(2) -0.003(2) C4 0.021(3) 0.023(2) 0.023(3) 0.0014(19) -0.003(2) -0.002(2) C5 0.020(3) 0.022(2) 0.019(2) -0.0026(18) 0.0000(19) -0.005(2) C6 0.018(3) 0.026(3) 0.028(3) 0.000(2) -0.002(2) -0.005(2) C7 0.021(3) 0.024(2) 0.021(2) 0.0012(19) 0.001(2) 0.001(2) C8 0.014(3) 0.025(3) 0.038(3) -0.003(2) 0.003(2) -0.007(2) C9 0.023(3) 0.043(3) 0.030(3) -0.013(2) -0.001(2) -0.009(2) C10 0.032(4) 0.045(3) 0.051(4) -0.025(3) -0.001(3) -0.010(3) C11 0.028(4) 0.033(3) 0.065(4) -0.019(3) -0.004(3) -0.006(2) C12 0.024(3) 0.029(3) 0.049(3) -0.007(2) -0.006(3) -0.005(2) C13 0.013(3) 0.032(3) 0.020(2) -0.004(2) -0.0020(19) -0.001(2) C14 0.023(3) 0.039(3) 0.037(3) -0.010(2) -0.007(2) 0.000(2) C15 0.038(4) 0.056(4) 0.044(4) -0.020(3) -0.018(3) 0.007(3) C16 0.048(4) 0.066(4) 0.026(3) -0.018(3) -0.024(3) 0.021(3) C17 0.025(3) 0.053(3) 0.023(3) -0.002(2) -0.004(2) 0.011(3) C18 0.029(3) 0.026(3) 0.025(3) -0.004(2) 0.001(2) -0.002(2) C19 0.099(7) 0.064(4) 0.040(4) 0.011(3) -0.044(4) -0.040(4) C20 0.030(3) 0.029(3) 0.019(3) -0.002(2) -0.013(2) -0.001(2) C21 0.061(5) 0.030(3) 0.037(3) -0.011(2) -0.011(3) 0.001(3) C22 0.014(3) 0.029(3) 0.029(3) -0.002(2) 0.002(2) -0.008(2) O1 0.044(3) 0.037(2) 0.035(2) -0.0045(16) -0.0061(18) -0.0210(19) O2 0.073(3) 0.042(2) 0.033(2) 0.0087(17) -0.029(2) -0.028(2) O3 0.019(2) 0.0346(19) 0.035(2) -0.0082(15) -0.0042(15) 0.0024(15) O4 0.041(2) 0.0226(17) 0.0219(17) 0.0029(13) -0.0105(16) -0.0086(16) O5 0.037(2) 0.041(2) 0.027(2) -0.0091(16) 0.0057(18) 0.0009(18) O6 0.040(2) 0.0270(19) 0.031(2) -0.0077(15) -0.0064(17) -0.0033(17) Cl3 0.040(4) 0.043(2) 0.0273(19) 0.0132(19) -0.013(2) 0.009(2) O9 0.072(17) 0.054(10) 0.057(10) 0.014(8) -0.003(8) 0.031(8) O10 0.46(5) 0.088(13) 0.14(2) 0.050(12) -0.10(3) -0.09(2) O11 0.074(10) 0.33(3) 0.072(10) 0.128(14) 0.012(8) -0.007(14) O12 0.23(4) 0.46(7) 0.11(2) -0.09(3) -0.09(2) 0.18(4) Cl3A 0.063(6) 0.123(9) 0.137(11) 0.076(7) -0.006(7) 0.011(5) O13 0.075(10) 0.116(11) 0.103(12) -0.018(9) 0.015(9) 0.046(9) O14 0.146(15) 0.111(11) 0.070(9) 0.079(9) 0.000(9) -0.015(10) O15 0.107(13) 0.071(8) 0.111(12) -0.008(7) -0.015(9) -0.057(8) O16 0.062(16) 0.077(13) 0.107(19) -0.065(13) -0.051(14) 0.028(9) N31 0.08(2) 0.10(2) 0.057(17) 0.001(15) -0.017(16) -0.055(18) C31 0.16(4) 0.12(3) 0.038(16) -0.056(18) -0.07(2) 0.10(3) C32 0.08(3) 0.07(2) 0.11(4) -0.02(2) 0.04(3) 0.00(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 N4 1.917(5) . ? Co1 N3 1.952(5) . ? Co1 N1 1.965(4) . ? Co1 N2 2.023(4) . ? Co1 Cl2 2.2447(15) . ? Co1 Cl1 2.2538(16) . ? N1 C1 1.489(6) . ? N1 C22 1.505(6) . ? N1 C5 1.519(6) . ? N2 C6 1.479(7) . ? N2 C7 1.479(6) . ? N3 C12 1.330(6) . ? N3 C8 1.346(7) . ? N4 C17 1.341(7) . ? N4 C13 1.351(6) . ? C1 C8 1.497(7) . ? C1 C2 1.550(7) . ? C2 C18 1.526(7) . ? C2 C3 1.541(7) . ? C2 C6 1.542(7) . ? C3 O3 1.390(6) . ? C3 O4 1.404(6) . ? C3 C4 1.562(7) . ? C4 C20 1.526(7) . ? C4 C7 1.536(6) . ? C4 C5 1.549(7) . ? C5 C13 1.498(7) . ? C8 C9 1.386(8) . ? C9 C10 1.371(8) . ? C10 C11 1.369(9) . ? C11 C12 1.386(8) . ? C13 C14 1.373(8) . ? C14 C15 1.399(8) . ? C15 C16 1.374(9) . ? C16 C17 1.387(9) . ? C18 O1 1.185(6) . ? C18 O2 1.343(6) . ? C19 O2 1.447(7) . ? C20 O5 1.201(6) . ? C20 O6 1.333(6) . ? C21 O6 1.446(6) . ? Cl3 O12 0.95(4) . ? Cl3 O9 1.32(2) . ? Cl3 O10 1.52(3) . ? Cl3 O11 1.74(2) . ? Cl3A O14 1.184(17) . ? Cl3A O16 1.46(3) . ? Cl3A O15 1.50(2) . ? Cl3A O13 1.859(18) . ? N31 C32 1.16(3) . ? C31 C32 1.35(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 N4 Co1 N3 165.40(17) . . ? N4 Co1 N1 83.64(16) . . ? N3 Co1 N1 83.79(16) . . ? N4 Co1 N2 93.22(17) . . ? N3 Co1 N2 93.54(18) . . ? N1 Co1 N2 87.20(16) . . ? N4 Co1 Cl2 87.83(13) . . ? N3 Co1 Cl2 86.66(13) . . ? N1 Co1 Cl2 98.20(13) . . ? N2 Co1 Cl2 174.58(11) . . ? N4 Co1 Cl1 97.43(13) . . ? N3 Co1 Cl1 95.98(13) . . ? N1 Co1 Cl1 172.73(13) . . ? N2 Co1 Cl1 85.56(12) . . ? Cl2 Co1 Cl1 89.03(6) . . ? C1 N1 C22 107.0(4) . . ? C1 N1 C5 117.1(4) . . ? C22 N1 C5 106.3(4) . . ? C1 N1 Co1 105.4(3) . . ? C22 N1 Co1 116.1(3) . . ? C5 N1 Co1 105.5(3) . . ? C6 N2 C7 107.9(4) . . ? C6 N2 Co1 115.0(3) . . ? C7 N2 Co1 116.5(3) . . ? C12 N3 C8 120.0(5) . . ? C12 N3 Co1 126.6(4) . . ? C8 N3 Co1 112.7(3) . . ? C17 N4 C13 118.3(5) . . ? C17 N4 Co1 126.4(4) . . ? C13 N4 Co1 114.5(3) . . ? N1 C1 C8 106.1(4) . . ? N1 C1 C2 113.9(4) . . ? C8 C1 C2 109.1(4) . . ? C18 C2 C3 111.0(4) . . ? C18 C2 C6 106.8(4) . . ? C3 C2 C6 109.1(4) . . ? C18 C2 C1 108.5(4) . . ? C3 C2 C1 109.4(4) . . ? C6 C2 C1 112.1(4) . . ? O3 C3 O4 111.8(4) . . ? O3 C3 C2 106.2(4) . . ? O4 C3 C2 112.8(4) . . ? O3 C3 C4 113.3(4) . . ? O4 C3 C4 105.5(4) . . ? C2 C3 C4 107.2(4) . . ? C20 C4 C7 108.1(4) . . ? C20 C4 C5 111.2(4) . . ? C7 C4 C5 112.0(4) . . ? C20 C4 C3 107.6(4) . . ? C7 C4 C3 108.0(4) . . ? C5 C4 C3 109.8(4) . . ? C13 C5 N1 105.0(4) . . ? C13 C5 C4 110.4(4) . . ? N1 C5 C4 113.0(4) . . ? N2 C6 C2 108.2(4) . . ? N2 C7 C4 108.8(4) . . ? N3 C8 C9 121.2(5) . . ? N3 C8 C1 113.9(4) . . ? C9 C8 C1 124.7(5) . . ? C10 C9 C8 118.6(5) . . ? C11 C10 C9 120.0(6) . . ? C10 C11 C12 119.1(5) . . ? N3 C12 C11 121.1(5) . . ? N4 C13 C14 122.7(5) . . ? N4 C13 C5 113.4(4) . . ? C14 C13 C5 123.9(4) . . ? C13 C14 C15 118.6(5) . . ? C16 C15 C14 118.9(6) . . ? C15 C16 C17 119.3(5) . . ? N4 C17 C16 122.1(5) . . ? O1 C18 O2 122.7(5) . . ? O1 C18 C2 125.3(5) . . ? O2 C18 C2 111.9(4) . . ? O5 C20 O6 124.7(5) . . ? O5 C20 C4 123.4(5) . . ? O6 C20 C4 111.9(4) . . ? C18 O2 C19 115.7(5) . . ? C20 O6 C21 116.4(4) . . ? O12 Cl3 O9 123(3) . . ? O12 Cl3 O10 117(3) . . ? O9 Cl3 O10 99.1(18) . . ? O12 Cl3 O11 115.7(19) . . ? O9 Cl3 O11 99.2(15) . . ? O10 Cl3 O11 98.1(16) . . ? O14 Cl3A O16 140(2) . . ? O14 Cl3A O15 114.4(17) . . ? O16 Cl3A O15 105.4(16) . . ? O14 Cl3A O13 88.0(14) . . ? O16 Cl3A O13 90.3(15) . . ? O15 Cl3A O13 83.6(11) . . ? N31 C32 C31 172(4) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 24.01 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.067 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.125 #eof # Attachment 'CoIIIL2aqua-chloro.cif' data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 600456' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 Cl3 Co N4 O16' _chemical_formula_weight 767.75 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3500(15) _cell_length_b 13.2623(18) _cell_length_c 13.9803(18) _cell_angle_alpha 113.766(2) _cell_angle_beta 91.005(3) _cell_angle_gamma 109.556(2) _cell_volume 1786.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7734 _exptl_absorpt_correction_T_max 0.9923 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19634 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6310 _reflns_number_gt 4694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR2002 (Giacovazzo, 2002)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1306P)^2^+1.4972P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6310 _refine_ls_number_parameters 424 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2127 _refine_ls_wR_factor_gt 0.2001 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.214 _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 C1 C 0.7007(5) 0.2141(4) 0.1644(4) 0.0255(11) Uani 1 1 d . . . C2 C 0.8124(5) 0.1751(5) 0.1762(4) 0.0250(11) Uani 1 1 d . . . H2 H 0.8897 0.2237 0.1588 0.030 Uiso 1 1 calc R . . C4 C 0.8413(4) 0.2945(4) 0.3791(4) 0.0215(10) Uani 1 1 d . . . H4 H 0.9243 0.3618 0.3956 0.026 Uiso 1 1 calc R . . C5 C 0.7306(5) 0.3318(4) 0.3596(4) 0.0257(11) Uani 1 1 d . . . C6 C 0.6019(5) 0.2429(4) 0.3575(4) 0.0280(11) Uani 1 1 d . . . H6A H 0.5987 0.2406 0.4273 0.034 Uiso 1 1 calc R . . H6B H 0.5327 0.2669 0.3422 0.034 Uiso 1 1 calc R . . C8 C 0.5743(4) 0.1300(4) 0.1706(4) 0.0260(11) Uani 1 1 d . . . H8A H 0.5061 0.1591 0.1645 0.031 Uiso 1 1 calc R . . H8B H 0.5523 0.0499 0.1116 0.031 Uiso 1 1 calc R . . C9 C 0.7325(5) 0.3415(4) 0.2525(4) 0.0277(12) Uani 1 1 d . . . C10 C 0.6838(5) 0.2122(4) 0.0533(4) 0.0305(12) Uani 1 1 d . . . C11 C 0.7810(7) 0.2971(6) -0.0588(5) 0.0455(16) Uani 1 1 d . . . H11A H 0.7652 0.2189 -0.1171 0.068 Uiso 1 1 calc R . . H11B H 0.8617 0.3544 -0.0599 0.068 Uiso 1 1 calc R . . H11C H 0.7119 0.3231 -0.0673 0.068 Uiso 1 1 calc R . . C12 C 0.7599(5) 0.4560(5) 0.4494(4) 0.0301(12) Uani 1 1 d . . . C13 C 0.6752(7) 0.5924(6) 0.5567(7) 0.077(3) Uani 1 1 d . . . H13A H 0.5933 0.6006 0.5682 0.115 Uiso 1 1 calc R . . H13B H 0.7261 0.6521 0.5342 0.115 Uiso 1 1 calc R . . H13C H 0.7206 0.6042 0.6229 0.115 Uiso 1 1 calc R . . C14 C 0.7767(5) 0.0463(4) 0.1033(4) 0.0255(11) Uani 1 1 d . . . C15 C 0.8072(6) 0.0039(5) 0.0031(4) 0.0352(13) Uani 1 1 d . . . H15 H 0.8579 0.0570 -0.0229 0.042 Uiso 1 1 calc R . . C16 C 0.7618(6) -0.1186(6) -0.0590(5) 0.0401(14) Uani 1 1 d . . . H16 H 0.7828 -0.1502 -0.1275 0.048 Uiso 1 1 calc R . . C17 C 0.6862(6) -0.1935(5) -0.0201(4) 0.0360(13) Uani 1 1 d . . . H17 H 0.6518 -0.2770 -0.0626 0.043 Uiso 1 1 calc R . . C18 C 0.6612(5) -0.1459(4) 0.0813(4) 0.0302(12) Uani 1 1 d . . . H18 H 0.6113 -0.1975 0.1091 0.036 Uiso 1 1 calc R . . C19 C 0.8250(5) 0.2628(4) 0.4714(4) 0.0254(11) Uani 1 1 d . . . C20 C 0.8755(5) 0.3414(5) 0.5760(4) 0.0322(12) Uani 1 1 d . . . H20 H 0.9343 0.4196 0.5946 0.039 Uiso 1 1 calc R . . C21 C 0.8383(6) 0.3032(5) 0.6537(5) 0.0428(15) Uani 1 1 d . . . H21 H 0.8709 0.3560 0.7266 0.051 Uiso 1 1 calc R . . C22 C 0.7549(6) 0.1899(6) 0.6258(5) 0.0449(15) Uani 1 1 d . . . H22 H 0.7273 0.1641 0.6786 0.054 Uiso 1 1 calc R . . C23 C 0.7113(6) 0.1134(5) 0.5188(5) 0.0369(13) Uani 1 1 d . . . H23 H 0.6562 0.0335 0.4987 0.044 Uiso 1 1 calc R . . C30 C 0.9720(4) 0.1833(5) 0.2990(4) 0.0262(11) Uani 1 1 d . . . H30A H 0.9747 0.1113 0.2415 0.039 Uiso 1 1 calc R . . H30B H 0.9922 0.1834 0.3675 0.039 Uiso 1 1 calc R . . H30C H 1.0343 0.2534 0.2960 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.25358(12) 0.06709(12) 0.31964(11) 0.0345(4) Uani 1 1 d D . . Cl2 Cl 0.12661(14) 0.39431(13) 0.11080(14) 0.0481(4) Uani 1 1 d D . . Co1 Co 0.70600(6) 0.05197(6) 0.29286(5) 0.0226(2) Uani 1 1 d . . . N1 N 0.7450(4) 0.1496(4) 0.4438(3) 0.0267(10) Uani 1 1 d . . . N2 N 0.7062(4) -0.0276(4) 0.1417(3) 0.0255(9) Uani 1 1 d . . . N3 N 0.8419(3) 0.1859(3) 0.2870(3) 0.0193(8) Uani 1 1 d . . . N7 N 0.5859(4) 0.1242(4) 0.2736(4) 0.0257(10) Uani 1 1 d . . . O1 O 0.5911(4) 0.1494(3) -0.0127(3) 0.0387(10) Uani 1 1 d . . . O2 O 0.7874(4) 0.2893(3) 0.0423(3) 0.0361(9) Uani 1 1 d . . . O3 O 0.8630(3) 0.5284(3) 0.4923(3) 0.0304(8) Uani 1 1 d . . . O4 O 0.6539(4) 0.4736(4) 0.4742(4) 0.0595(15) Uani 1 1 d . . . O5 O 0.8549(3) 0.4194(3) 0.2597(3) 0.0285(8) Uani 1 1 d . . . H5 H 0.8666 0.4144 0.1990 0.043 Uiso 1 1 calc R . . O6 O 0.6370(4) 0.3775(3) 0.2304(3) 0.0385(10) Uani 1 1 d . . . H6 H 0.6638 0.4520 0.2580 0.058 Uiso 1 1 calc R . . Cl3 Cl 0.54191(15) -0.09500(13) 0.29615(13) 0.0452(4) Uani 1 1 d . . . O8 O 0.8192(4) -0.0236(3) 0.3148(3) 0.0324(9) Uani 1 1 d . . . O9 O 0.3497(4) 0.1007(5) 0.4044(4) 0.0672(16) Uani 1 1 d D . . O10 O 0.2876(8) -0.0047(5) 0.2271(4) 0.117(3) Uani 1 1 d D . . O11 O 0.2520(8) 0.1640(4) 0.3061(4) 0.110(3) Uani 1 1 d D . . O12 O 0.1403(5) 0.0029(9) 0.3355(7) 0.218(8) Uani 1 1 d D . . O13 O 0.1446(7) 0.4012(8) 0.2180(6) 0.141(4) Uani 1 1 d D . . O14 O 0.0499(4) 0.4608(3) 0.1167(3) 0.0442(10) Uani 1 1 d D . . O15 O 0.0582(6) 0.2729(4) 0.0493(7) 0.123(3) Uani 1 1 d D . . O16 O 0.2420(6) 0.4405(6) 0.0894(8) 0.167(5) Uani 1 1 d D . . O17 O 0.9442(5) 0.8939(5) 0.1604(5) 0.0693(15) Uani 1 1 d . . . H7 H 0.523(6) 0.079(6) 0.279(5) 0.034(17) Uiso 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 C1 0.020(2) 0.021(3) 0.031(3) 0.012(2) -0.002(2) 0.002(2) C2 0.021(2) 0.029(3) 0.027(3) 0.016(2) 0.004(2) 0.006(2) C4 0.015(2) 0.015(2) 0.028(3) 0.008(2) -0.002(2) -0.0002(19) C5 0.018(2) 0.017(2) 0.034(3) 0.006(2) -0.003(2) 0.004(2) C6 0.021(3) 0.022(3) 0.037(3) 0.009(2) 0.003(2) 0.007(2) C8 0.017(2) 0.019(2) 0.035(3) 0.008(2) -0.006(2) 0.003(2) C9 0.019(2) 0.020(3) 0.040(3) 0.013(2) -0.005(2) 0.003(2) C10 0.034(3) 0.018(3) 0.036(3) 0.010(2) -0.004(3) 0.007(2) C11 0.058(4) 0.038(3) 0.038(4) 0.024(3) -0.001(3) 0.007(3) C12 0.027(3) 0.024(3) 0.035(3) 0.010(2) 0.000(2) 0.008(2) C13 0.039(4) 0.041(4) 0.096(6) -0.026(4) -0.012(4) 0.021(3) C14 0.021(2) 0.024(3) 0.028(3) 0.009(2) -0.001(2) 0.007(2) C15 0.043(3) 0.037(3) 0.025(3) 0.010(2) 0.005(2) 0.018(3) C16 0.048(4) 0.045(4) 0.027(3) 0.010(3) 0.004(3) 0.025(3) C17 0.045(3) 0.027(3) 0.028(3) 0.002(2) -0.001(3) 0.018(3) C18 0.031(3) 0.019(3) 0.033(3) 0.006(2) -0.003(2) 0.007(2) C19 0.021(2) 0.026(3) 0.031(3) 0.015(2) 0.006(2) 0.006(2) C20 0.036(3) 0.025(3) 0.027(3) 0.008(2) 0.002(2) 0.007(2) C21 0.061(4) 0.034(3) 0.026(3) 0.012(3) 0.006(3) 0.010(3) C22 0.055(4) 0.038(3) 0.037(4) 0.020(3) 0.011(3) 0.007(3) C23 0.049(4) 0.026(3) 0.031(3) 0.014(2) 0.014(3) 0.006(3) C30 0.017(2) 0.028(3) 0.031(3) 0.012(2) -0.002(2) 0.005(2) Cl1 0.0245(7) 0.0340(7) 0.0435(8) 0.0166(6) 0.0065(6) 0.0096(6) Cl2 0.0364(8) 0.0354(8) 0.0659(11) 0.0154(8) 0.0094(7) 0.0137(7) Co1 0.0218(4) 0.0150(4) 0.0269(4) 0.0088(3) 0.0027(3) 0.0025(3) N1 0.027(2) 0.019(2) 0.026(2) 0.0081(18) 0.0029(18) 0.0013(18) N2 0.023(2) 0.020(2) 0.027(2) 0.0065(18) -0.0061(18) 0.0057(18) N3 0.0144(19) 0.018(2) 0.024(2) 0.0099(17) -0.0004(16) 0.0033(16) N7 0.015(2) 0.019(2) 0.036(3) 0.010(2) 0.0047(19) 0.0002(18) O1 0.036(2) 0.028(2) 0.038(2) 0.0092(18) -0.0152(19) 0.0027(18) O2 0.036(2) 0.030(2) 0.035(2) 0.0190(18) -0.0054(17) -0.0015(17) O3 0.026(2) 0.0151(17) 0.037(2) 0.0058(16) -0.0042(16) -0.0008(16) O4 0.023(2) 0.031(2) 0.078(3) -0.019(2) -0.008(2) 0.0101(18) O5 0.0263(19) 0.0223(18) 0.031(2) 0.0147(16) -0.0027(16) -0.0013(15) O6 0.037(2) 0.0185(18) 0.054(3) 0.0121(19) -0.0105(19) 0.0093(17) Cl3 0.0402(8) 0.0352(8) 0.0534(10) 0.0192(7) 0.0074(7) 0.0062(7) O8 0.038(2) 0.026(2) 0.032(2) 0.0105(17) 0.0016(17) 0.0128(17) O9 0.042(3) 0.074(4) 0.075(4) 0.049(3) -0.013(2) -0.010(3) O10 0.235(10) 0.085(5) 0.049(4) 0.005(3) 0.004(5) 0.110(6) O11 0.224(9) 0.041(3) 0.053(3) -0.003(3) -0.039(4) 0.066(4) O12 0.036(4) 0.47(2) 0.253(12) 0.301(15) 0.030(5) 0.043(7) O13 0.115(6) 0.194(10) 0.188(9) 0.157(9) 0.034(6) 0.053(6) O14 0.043(2) 0.032(2) 0.055(3) 0.016(2) 0.006(2) 0.016(2) O15 0.078(4) 0.048(4) 0.228(10) 0.039(5) 0.056(5) 0.030(3) O16 0.097(6) 0.156(8) 0.379(16) 0.204(10) 0.156(8) 0.087(6) O17 0.061(3) 0.065(3) 0.068(4) 0.011(3) 0.000(3) 0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C8 1.523(7) . ? C1 C9 1.550(7) . ? C1 C10 1.550(8) . ? C1 C2 1.550(7) . ? C2 C14 1.497(7) . ? C2 N3 1.518(6) . ? C2 H2 1.0000 . ? C4 N3 1.498(6) . ? C4 C19 1.507(7) . ? C4 C5 1.552(6) . ? C4 H4 1.0000 . ? C5 C6 1.530(7) . ? C5 C12 1.533(7) . ? C5 C9 1.554(8) . ? C6 N7 1.484(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 N7 1.478(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O6 1.397(6) . ? C9 O5 1.399(6) . ? C10 O1 1.188(6) . ? C10 O2 1.334(7) . ? C11 O2 1.459(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O3 1.187(6) . ? C12 O4 1.326(7) . ? C13 O4 1.464(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N2 1.342(7) . ? C14 C15 1.383(8) . ? C15 C16 1.395(8) . ? C15 H15 0.9500 . ? C16 C17 1.379(9) . ? C16 H16 0.9500 . ? C17 C18 1.378(8) . ? C17 H17 0.9500 . ? C18 N2 1.348(7) . ? C18 H18 0.9500 . ? C19 N1 1.355(7) . ? C19 C20 1.377(8) . ? C20 C21 1.390(8) . ? C20 H20 0.9500 . ? C21 C22 1.366(9) . ? C21 H21 0.9500 . ? C22 C23 1.387(9) . ? C22 H22 0.9500 . ? C23 N1 1.332(7) . ? C23 H23 0.9500 . ? C30 N3 1.496(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? Cl1 O12 1.362(5) . ? Cl1 O11 1.378(4) . ? Cl1 O9 1.413(4) . ? Cl1 O10 1.414(5) . ? Cl2 O16 1.344(5) . ? Cl2 O15 1.399(5) . ? Cl2 O14 1.415(4) . ? Cl2 O13 1.470(6) . ? Co1 N1 1.925(4) . ? Co1 N2 1.945(4) . ? Co1 N3 1.956(4) . ? Co1 O8 1.961(4) . ? Co1 N7 1.979(4) . ? Co1 Cl3 2.2169(17) . ? N7 H7 0.79(7) . ? O5 H5 0.8400 . ? O6 H6 0.8400 . ? 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 C8 C1 C9 110.4(4) . . ? C8 C1 C10 106.0(4) . . ? C9 C1 C10 110.2(4) . . ? C8 C1 C2 112.6(4) . . ? C9 C1 C2 108.2(4) . . ? C10 C1 C2 109.3(4) . . ? C14 C2 N3 105.4(4) . . ? C14 C2 C1 109.7(4) . . ? N3 C2 C1 112.0(4) . . ? C14 C2 H2 109.9 . . ? N3 C2 H2 109.9 . . ? C1 C2 H2 109.9 . . ? N3 C4 C19 105.8(4) . . ? N3 C4 C5 113.0(4) . . ? C19 C4 C5 108.7(4) . . ? N3 C4 H4 109.7 . . ? C19 C4 H4 109.7 . . ? C5 C4 H4 109.7 . . ? C6 C5 C12 112.0(4) . . ? C6 C5 C4 111.6(4) . . ? C12 C5 C4 105.9(4) . . ? C6 C5 C9 110.1(4) . . ? C12 C5 C9 108.3(4) . . ? C4 C5 C9 108.7(4) . . ? N7 C6 C5 108.2(4) . . ? N7 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? N7 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? N7 C8 C1 108.7(4) . . ? N7 C8 H8A 110.0 . . ? C1 C8 H8A 110.0 . . ? N7 C8 H8B 110.0 . . ? C1 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? O6 C9 O5 113.2(4) . . ? O6 C9 C1 105.8(4) . . ? O5 C9 C1 113.0(4) . . ? O6 C9 C5 112.2(4) . . ? O5 C9 C5 106.0(4) . . ? C1 C9 C5 106.5(4) . . ? O1 C10 O2 125.2(5) . . ? O1 C10 C1 124.0(5) . . ? O2 C10 C1 110.8(4) . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C12 O4 123.3(5) . . ? O3 C12 C5 125.6(5) . . ? O4 C12 C5 111.1(4) . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C15 121.5(5) . . ? N2 C14 C2 114.0(4) . . ? C15 C14 C2 124.4(5) . . ? C14 C15 C16 118.5(6) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 119.5(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C18 C17 C16 119.2(5) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N2 C18 C17 121.3(5) . . ? N2 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? N1 C19 C20 121.3(5) . . ? N1 C19 C4 113.6(4) . . ? C20 C19 C4 124.8(5) . . ? C19 C20 C21 118.2(5) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C22 C21 C20 120.2(6) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 118.9(6) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? N1 C23 C22 121.3(5) . . ? N1 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? N3 C30 H30A 109.5 . . ? N3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O12 Cl1 O11 113.5(4) . . ? O12 Cl1 O9 109.0(3) . . ? O11 Cl1 O9 111.5(3) . . ? O12 Cl1 O10 110.1(5) . . ? O11 Cl1 O10 106.7(3) . . ? O9 Cl1 O10 105.8(3) . . ? O16 Cl2 O15 116.8(4) . . ? O16 Cl2 O14 113.3(3) . . ? O15 Cl2 O14 111.0(3) . . ? O16 Cl2 O13 107.6(4) . . ? O15 Cl2 O13 102.1(4) . . ? O14 Cl2 O13 104.5(3) . . ? N1 Co1 N2 167.26(18) . . ? N1 Co1 N3 84.59(17) . . ? N2 Co1 N3 84.27(17) . . ? N1 Co1 O8 87.67(17) . . ? N2 Co1 O8 87.13(16) . . ? N3 Co1 O8 94.90(16) . . ? N1 Co1 N7 91.59(18) . . ? N2 Co1 N7 94.10(18) . . ? N3 Co1 N7 87.55(17) . . ? O8 Co1 N7 177.37(18) . . ? N1 Co1 Cl3 96.10(13) . . ? N2 Co1 Cl3 95.46(13) . . ? N3 Co1 Cl3 175.81(12) . . ? O8 Co1 Cl3 89.26(12) . . ? N7 Co1 Cl3 88.30(14) . . ? C23 N1 C19 119.9(5) . . ? C23 N1 Co1 126.5(4) . . ? C19 N1 Co1 113.2(3) . . ? C14 N2 C18 119.9(5) . . ? C14 N2 Co1 113.0(3) . . ? C18 N2 Co1 126.2(4) . . ? C30 N3 C4 107.4(4) . . ? C30 N3 C2 106.7(4) . . ? C4 N3 C2 117.6(4) . . ? C30 N3 Co1 114.6(3) . . ? C4 N3 Co1 105.8(3) . . ? C2 N3 Co1 105.1(3) . . ? C8 N7 C6 107.0(4) . . ? C8 N7 Co1 115.2(3) . . ? C6 N7 Co1 117.4(3) . . ? C8 N7 H7 112(5) . . ? C6 N7 H7 105(5) . . ? Co1 N7 H7 99(4) . . ? C10 O2 C11 115.6(4) . . ? C12 O4 C13 113.9(4) . . ? C9 O5 H5 109.5 . . ? C9 O6 H6 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.943 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.116 # 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 -0.006 -0.006 0.494 408.0 101.2 #_platon_squeeze_details #; ? #; _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' # Attachment 'CoIIIL3CO3.CIF' data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 600457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2( C22 H22 Co N4 O9), P F6, K3, 9.4( H2 O)' _chemical_formula_sum 'C44 H63 Co2 F6 K3 N8 O27.5 P1' _chemical_formula_weight 1524.16 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8467(8) _cell_length_b 14.6159(9) _cell_length_c 16.919(1) _cell_angle_alpha 101.279(1) _cell_angle_beta 111.414(1) _cell_angle_gamma 107.638(1) _cell_volume 2851.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1566 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 'CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51481 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 32.02 _reflns_number_total 19451 _reflns_number_gt 13002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The PF6-ion is disordered. At one position there is a water molecule (O278) partly displaced by two water moleculkes (o27 and O28). Some of the hydrogen atoms of water molecules could not be located. 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^)+(0.0514P)^2^+5.7100P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19451 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.008 _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 0.73412(3) 0.61427(3) 0.90347(2) 0.01557(8) Uani 1 1 d . . . Co2 Co 0.72600(3) 0.12253(3) 0.18529(2) 0.01299(7) Uani 1 1 d . . . K1 K 0.68882(5) 0.07200(5) 0.65370(4) 0.02184(12) Uani 1 1 d . . . K2 K 0.30783(5) 0.20283(5) 0.52427(4) 0.02785(14) Uani 1 1 d . . . K3 K 0.09804(6) 0.22670(5) 0.63297(4) 0.02847(14) Uani 1 1 d . . . O1 O 0.52358(17) 0.28950(15) 0.66106(13) 0.0174(4) Uani 1 1 d . B . O2 O 0.56055(17) 0.22809(15) 0.78095(14) 0.0196(4) Uani 1 1 d . B . O3 O 0.32675(17) 0.28643(17) 0.68645(14) 0.0265(4) Uani 1 1 d . B . O4 O 0.37028(18) 0.30826(17) 0.83137(14) 0.0250(4) Uani 1 1 d . B . O5 O 0.71431(18) 0.27300(16) 0.67690(14) 0.0243(4) Uani 1 1 d . B . O6 O 0.8444(2) 0.3125(2) 0.81798(17) 0.0398(6) Uani 1 1 d . B . O7 O 0.80142(16) -0.02419(14) 0.43909(13) 0.0160(3) Uani 1 1 d . . . O8 O 0.88025(16) 0.15291(15) 0.49747(12) 0.0171(4) Uani 1 1 d . . . O9 O 1.08506(16) 0.15439(15) 0.47190(13) 0.0205(4) Uani 1 1 d . . . O10 O 1.00589(16) -0.01514(15) 0.40463(13) 0.0198(4) Uani 1 1 d . . . O11 O 0.53939(16) -0.04271(15) 0.37269(13) 0.0195(4) Uani 1 1 d . . . O12 O 0.66476(16) 0.10526(15) 0.48541(12) 0.0199(4) Uani 1 1 d . . . O13 O 0.81990(19) 0.71911(16) 1.02009(13) 0.0260(4) Uani 1 1 d . . . O14 O 0.76884(17) 0.74732(14) 0.89335(13) 0.0203(4) Uani 1 1 d . . . O15 O 0.8695(3) 0.88336(19) 1.02296(18) 0.0572(9) Uani 1 1 d . . . O16 O 0.73016(16) 0.22901(14) 0.13462(13) 0.0179(4) Uani 1 1 d . . . O17 O 0.65279(17) 0.06814(15) 0.05657(12) 0.0183(4) Uani 1 1 d . . . O18 O 0.65256(18) 0.18147(17) -0.01809(14) 0.0244(4) Uani 1 1 d . . . O19 O 0.7257(4) 0.1155(3) 0.8461(3) 0.0774(13) Uani 1 1 d . . . O20 O 0.9255(3) 0.2096(3) 0.7235(3) 0.0816(15) Uani 1 1 d . . . O21 O 0.53069(19) -0.11938(17) 0.51118(15) 0.0237(4) Uani 1 1 d . . . O22 O 0.4087(4) 0.2734(4) 0.4238(3) 0.0920(14) Uani 1 1 d . B . O23 O 0.1881(2) 0.04182(19) 0.35492(19) 0.0319(5) Uani 1 1 d . . . O24 O 0.1003(4) 0.4238(3) 0.6531(5) 0.131(3) Uani 1 1 d . B . O25 O 0.1553(2) 0.2432(3) 0.80629(17) 0.0514(9) Uani 1 1 d . B . O26 O 0.8682(3) 0.3440(3) 0.6012(3) 0.0759(12) Uani 1 1 d . . . O27 O 0.9594(5) 0.0552(4) 0.8213(4) 0.0317(16) Uani 0.399(6) 1 d P A 1 O28 O 0.8522(5) 0.0275(5) 0.9283(4) 0.0344(16) Uani 0.399(6) 1 d P A 1 O278 O 0.8802(4) 0.0267(3) 0.8377(3) 0.0396(13) Uani 0.601(6) 1 d P A 2 N1 N 0.65122(18) 0.53113(16) 0.77670(14) 0.0141(4) Uani 1 1 d . . . N2 N 0.71047(19) 0.48442(17) 0.93512(14) 0.0167(4) Uani 1 1 d . . . N3 N 0.5889(2) 0.61030(17) 0.89169(15) 0.0173(4) Uani 1 1 d . . . N4 N 0.86744(19) 0.61382(17) 0.89232(15) 0.0184(4) Uani 1 1 d . . . N5 N 0.80569(18) 0.20130(16) 0.31369(14) 0.0140(4) Uani 1 1 d . . . N6 N 0.71065(17) -0.00681(16) 0.21594(14) 0.0124(4) Uani 1 1 d . . . N7 N 0.87279(19) 0.14021(17) 0.19447(16) 0.0172(4) Uani 1 1 d . . . N8 N 0.59227(18) 0.12637(16) 0.19470(14) 0.0138(4) Uani 1 1 d . . . C1 C 0.5316(2) 0.46952(19) 0.76056(16) 0.0140(4) Uani 1 1 d . . . C2 C 0.5237(2) 0.37957(19) 0.79701(17) 0.0147(4) Uani 1 1 d . B . C3 C 0.5878(2) 0.4162(2) 0.90008(17) 0.0170(5) Uani 1 1 d . . . C4 C 0.7596(2) 0.4182(2) 0.89927(18) 0.0170(5) Uani 1 1 d . . . C5 C 0.7045(2) 0.38250(19) 0.79602(17) 0.0153(4) Uani 1 1 d . B . C6 C 0.7193(2) 0.47319(19) 0.76040(17) 0.0153(4) Uani 1 1 d . . . C7 C 0.5749(2) 0.31533(19) 0.75527(17) 0.0155(5) Uani 1 1 d . . . C8 C 0.6425(2) 0.5939(2) 0.71648(18) 0.0172(5) Uani 1 1 d . . . C9 C 0.5010(2) 0.5431(2) 0.81174(17) 0.0168(5) Uani 1 1 d . . . C10 C 0.5697(3) 0.6734(2) 0.94818(19) 0.0218(5) Uani 1 1 d . . . C11 C 0.4625(3) 0.6712(2) 0.9259(2) 0.0235(6) Uani 1 1 d . . . C12 C 0.3722(3) 0.6031(2) 0.8429(2) 0.0228(6) Uani 1 1 d . . . C13 C 0.3914(2) 0.5371(2) 0.78519(19) 0.0198(5) Uani 1 1 d . . . C14 C 0.3946(2) 0.3178(2) 0.76813(19) 0.0188(5) Uani 1 1 d . . . C15 C 0.7665(3) 0.5157(2) 1.03560(18) 0.0229(6) Uani 1 1 d . . . C16 C 0.7606(2) 0.3177(2) 0.76145(19) 0.0196(5) Uani 1 1 d . . . C17 C 0.8424(2) 0.5480(2) 0.81205(18) 0.0173(5) Uani 1 1 d . . . C18 C 0.9774(2) 0.6745(2) 0.9508(2) 0.0231(6) Uani 1 1 d . . . C19 C 1.0643(3) 0.6715(2) 0.9306(2) 0.0270(6) Uani 1 1 d . . . C20 C 1.0387(3) 0.6065(2) 0.8474(2) 0.0263(6) Uani 1 1 d . . . C21 C 0.9257(2) 0.5432(2) 0.7869(2) 0.0217(5) Uani 1 1 d . . . C22 C 0.8233(3) 0.7910(2) 0.9815(2) 0.0301(7) Uani 1 1 d . . . C23 C 0.9116(2) 0.18184(19) 0.35078(18) 0.0147(4) Uani 1 1 d . . . C24 C 0.8880(2) 0.07654(19) 0.36328(16) 0.0133(4) Uani 1 1 d . . . C25 C 0.8204(2) -0.01185(19) 0.27239(16) 0.0131(4) Uani 1 1 d . . . C26 C 0.6434(2) -0.02462(19) 0.26739(16) 0.0126(4) Uani 1 1 d . . . C27 C 0.7014(2) 0.06131(19) 0.35878(16) 0.0129(4) Uani 1 1 d . . . C28 C 0.7208(2) 0.16805(19) 0.34960(17) 0.0141(4) Uani 1 1 d . . . C29 C 0.8193(2) 0.06574(19) 0.41846(16) 0.0135(4) Uani 1 1 d . . . C30 C 0.8423(2) 0.3136(2) 0.3314(2) 0.0184(5) Uani 1 1 d . . . C31 C 0.9560(2) 0.1822(2) 0.28098(19) 0.0177(5) Uani 1 1 d . . . C32 C 0.8992(3) 0.1201(2) 0.1261(2) 0.0235(6) Uani 1 1 d . . . C33 C 1.0102(3) 0.1398(3) 0.1418(2) 0.0288(7) Uani 1 1 d . . . C34 C 1.0956(3) 0.1851(2) 0.2296(3) 0.0292(7) Uani 1 1 d . . . C35 C 1.0691(2) 0.2078(2) 0.3007(2) 0.0235(6) Uani 1 1 d . . . C36 C 1.0033(2) 0.0722(2) 0.41797(17) 0.0164(5) Uani 1 1 d . . . C37 C 0.6493(2) -0.0939(2) 0.12807(17) 0.0160(5) Uani 1 1 d . . . C38 C 0.6280(2) 0.0391(2) 0.40930(17) 0.0156(5) Uani 1 1 d . . . C39 C 0.6105(2) 0.16280(19) 0.28145(17) 0.0146(4) Uani 1 1 d . . . C40 C 0.4920(2) 0.1073(2) 0.12708(18) 0.0172(5) Uani 1 1 d . . . C41 C 0.4069(2) 0.1243(2) 0.1433(2) 0.0212(5) Uani 1 1 d . . . C42 C 0.4258(2) 0.1633(2) 0.2318(2) 0.0238(6) Uani 1 1 d . . . C43 C 0.5303(2) 0.1832(2) 0.30238(19) 0.0202(5) Uani 1 1 d . . . C44 C 0.6763(2) 0.1609(2) 0.05213(18) 0.0186(5) Uani 1 1 d . . . P1 P 0.2890(4) 0.5092(2) 0.5085(3) 0.0382(7) Uani 0.532(5) 1 d P B 1 F1 F 0.3667(6) 0.5688(4) 0.6134(3) 0.0573(17) Uani 0.532(5) 1 d P B 1 F2 F 0.2725(5) 0.4016(3) 0.5255(4) 0.0535(15) Uani 0.532(5) 1 d P B 1 F3 F 0.2240(5) 0.4483(4) 0.4019(3) 0.0527(15) Uani 0.532(5) 1 d P B 1 F4 F 0.1829(7) 0.5079(6) 0.5129(5) 0.075(2) Uani 0.532(5) 1 d P B 1 F5 F 0.3125(6) 0.6132(4) 0.4893(4) 0.077(2) Uani 0.532(5) 1 d P B 1 F6 F 0.4085(5) 0.5135(5) 0.5046(4) 0.079(2) Uani 0.532(5) 1 d P B 1 P1A P 0.2675(4) 0.4735(4) 0.5057(3) 0.0409(9) Uani 0.468(5) 1 d P B 2 F1A F 0.2966(5) 0.3819(5) 0.4696(5) 0.0641(19) Uani 0.468(5) 1 d P B 2 F2A F 0.3857(5) 0.5248(6) 0.5902(5) 0.061(2) Uani 0.468(5) 1 d P B 2 F3A F 0.3189(6) 0.5348(5) 0.4534(4) 0.061(2) Uani 0.468(5) 1 d P B 2 F4A F 0.2401(7) 0.5700(9) 0.5430(7) 0.143(6) Uani 0.468(5) 1 d P B 2 F5A F 0.1440(5) 0.4236(6) 0.4209(4) 0.071(2) Uani 0.468(5) 1 d P B 2 F6A F 0.2134(7) 0.4106(8) 0.5567(5) 0.121(4) Uani 0.468(5) 1 d P B 2 H1 H 0.482(3) 0.442(2) 0.699(2) 0.011(7) Uiso 1 1 d . . . H1O H 0.568(4) 0.280(3) 0.652(3) 0.032(11) Uiso 1 1 d . . . H2O H 0.536(3) 0.184(3) 0.739(3) 0.034(11) Uiso 1 1 d . . . H3A H 0.554(3) 0.451(3) 0.926(2) 0.020 Uiso 1 1 d . . . H3B H 0.584(3) 0.363(3) 0.917(2) 0.018(8) Uiso 1 1 d . . . H4A H 0.839(3) 0.453(3) 0.922(2) 0.017(8) Uiso 1 1 d . . . H4B H 0.745(3) 0.361(3) 0.916(2) 0.015(8) Uiso 1 1 d . . . H6 H 0.699(3) 0.449(2) 0.699(2) 0.013(7) Uiso 1 1 d . . . H7O H 0.856(4) -0.017(3) 0.481(3) 0.036(11) Uiso 1 1 d . . . H8O H 0.837(3) 0.156(3) 0.518(2) 0.022(9) Uiso 1 1 d . . . H8A H 0.599(3) 0.548(2) 0.654(2) 0.015(8) Uiso 1 1 d . . . H8B H 0.717(3) 0.634(3) 0.725(2) 0.023(9) Uiso 1 1 d . . . H8C H 0.606(3) 0.634(3) 0.729(2) 0.024(9) Uiso 1 1 d . . . H10 H 0.633(3) 0.721(3) 1.006(3) 0.034(10) Uiso 1 1 d . . . H11 H 0.451(3) 0.714(3) 0.964(3) 0.030(10) Uiso 1 1 d . . . H12 H 0.302(3) 0.603(3) 0.829(2) 0.023(9) Uiso 1 1 d . . . H13 H 0.334(3) 0.492(3) 0.728(2) 0.019(8) Uiso 1 1 d . . . H15A H 0.757(3) 0.454(3) 1.052(2) 0.023(9) Uiso 1 1 d . . . H15B H 0.726(3) 0.551(3) 1.058(2) 0.021(9) Uiso 1 1 d . . . H15C H 0.845(3) 0.557(3) 1.056(2) 0.027(9) Uiso 1 1 d . . . H18 H 0.989(3) 0.715(3) 0.997(2) 0.020(9) Uiso 1 1 d . . . H19 H 1.139(3) 0.715(3) 0.975(3) 0.030(10) Uiso 1 1 d . . . H20 H 1.093(3) 0.603(3) 0.830(3) 0.031(10) Uiso 1 1 d . . . H21 H 0.907(3) 0.501(3) 0.732(3) 0.033(10) Uiso 1 1 d . . . H23 H 0.963(3) 0.231(3) 0.404(2) 0.018(8) Uiso 1 1 d . . . H25A H 0.860(3) -0.013(3) 0.237(2) 0.019(8) Uiso 1 1 d . . . H25B H 0.803(3) -0.073(3) 0.283(2) 0.025(9) Uiso 1 1 d . . . H26A H 0.570(3) -0.030(2) 0.235(2) 0.015(8) Uiso 1 1 d . . . H26B H 0.642(3) -0.083(2) 0.278(2) 0.013(7) Uiso 1 1 d . . . H28 H 0.747(3) 0.215(3) 0.407(2) 0.018(8) Uiso 1 1 d . . . H30A H 0.892(3) 0.333(2) 0.309(2) 0.013(8) Uiso 1 1 d . . . H30B H 0.781(3) 0.328(3) 0.309(2) 0.025(9) Uiso 1 1 d . . . H30C H 0.881(3) 0.350(3) 0.398(3) 0.026(9) Uiso 1 1 d . . . H32 H 0.836(4) 0.089(3) 0.065(3) 0.045(12) Uiso 1 1 d . . . H33 H 1.027(3) 0.124(3) 0.092(3) 0.030(10) Uiso 1 1 d . . . H34 H 1.169(3) 0.197(3) 0.242(2) 0.028(9) Uiso 1 1 d . . . H35 H 1.127(3) 0.240(3) 0.362(3) 0.031(10) Uiso 1 1 d . . . H37A H 0.694(3) -0.085(2) 0.094(2) 0.014(8) Uiso 1 1 d . . . H37B H 0.580(3) -0.088(3) 0.098(2) 0.025(9) Uiso 1 1 d . . . H37C H 0.641(3) -0.157(2) 0.140(2) 0.014(8) Uiso 1 1 d . . . H40 H 0.479(3) 0.079(3) 0.067(2) 0.024(9) Uiso 1 1 d . . . H41 H 0.345(3) 0.112(3) 0.101(2) 0.021(9) Uiso 1 1 d . . . H42 H 0.367(3) 0.175(3) 0.246(3) 0.030(10) Uiso 1 1 d . . . H43 H 0.546(3) 0.209(3) 0.360(3) 0.029(10) Uiso 1 1 d . . . H20O H 0.989(4) 0.218(3) 0.755(3) 0.039(12) Uiso 1 1 d . . . H20Q H 0.909(6) 0.247(6) 0.755(5) 0.11(3) Uiso 1 1 d . . . H21O H 0.472(4) -0.121(3) 0.510(3) 0.036(11) Uiso 1 1 d . . . H21Q H 0.532(4) -0.098(3) 0.467(3) 0.040(11) Uiso 1 1 d . . . H23O H 0.125(4) 0.011(4) 0.365(3) 0.052(13) Uiso 1 1 d . . . H23Q H 0.156(5) 0.021(4) 0.296(4) 0.074(18) Uiso 1 1 d . . . H25O H 0.232(6) 0.265(5) 0.816(5) 0.11(2) Uiso 1 1 d . . . H25Q H 0.162(4) 0.253(4) 0.867(4) 0.070(16) Uiso 1 1 d . . . H24O H 0.0132 0.4084 0.6378 0.117(13) Uiso 1 1 d . . . H19O H 0.6967 0.1310 0.8835 0.117(13) Uiso 1 1 d . . . H19Q H 0.7625 0.1824 0.8446 0.117(13) Uiso 1 1 d . . . H22O H 0.3993 0.3357 0.4527 0.117(13) Uiso 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 0.01656(17) 0.01094(16) 0.01222(15) 0.00113(12) 0.00253(13) 0.00363(13) Co2 0.01235(15) 0.01302(15) 0.01262(15) 0.00434(12) 0.00466(12) 0.00527(12) K1 0.0188(3) 0.0181(3) 0.0242(3) 0.0028(2) 0.0074(2) 0.0077(2) K2 0.0168(3) 0.0312(3) 0.0194(3) 0.0053(3) 0.0011(2) 0.0005(2) K3 0.0194(3) 0.0249(3) 0.0226(3) -0.0018(2) -0.0019(2) 0.0063(2) O1 0.0154(9) 0.0167(9) 0.0141(8) 0.0014(7) 0.0042(7) 0.0046(7) O2 0.0209(10) 0.0113(9) 0.0204(10) 0.0045(8) 0.0059(8) 0.0037(8) O3 0.0163(9) 0.0286(11) 0.0193(10) 0.0017(8) 0.0023(8) 0.0015(8) O4 0.0200(10) 0.0293(11) 0.0259(10) 0.0139(9) 0.0105(9) 0.0077(9) O5 0.0212(10) 0.0200(10) 0.0241(10) -0.0010(8) 0.0080(8) 0.0072(8) O6 0.0460(15) 0.0582(17) 0.0299(12) 0.0169(12) 0.0142(11) 0.0421(14) O7 0.0142(9) 0.0165(9) 0.0131(8) 0.0061(7) 0.0023(7) 0.0053(7) O8 0.0136(8) 0.0181(9) 0.0121(8) -0.0007(7) 0.0023(7) 0.0053(7) O9 0.0126(9) 0.0186(9) 0.0201(9) 0.0039(8) 0.0008(7) 0.0036(7) O10 0.0160(9) 0.0180(9) 0.0211(9) 0.0063(8) 0.0030(8) 0.0083(7) O11 0.0169(9) 0.0189(9) 0.0179(9) 0.0028(7) 0.0088(8) 0.0026(7) O12 0.0179(9) 0.0231(10) 0.0136(8) 0.0005(7) 0.0068(7) 0.0061(8) O13 0.0315(12) 0.0170(10) 0.0142(9) -0.0010(7) 0.0025(8) 0.0045(9) O14 0.0241(10) 0.0110(8) 0.0182(9) 0.0026(7) 0.0056(8) 0.0043(7) O15 0.094(3) 0.0158(11) 0.0267(13) -0.0017(10) 0.0074(15) 0.0088(14) O16 0.0182(9) 0.0168(9) 0.0183(9) 0.0078(7) 0.0069(7) 0.0072(7) O17 0.0208(9) 0.0193(9) 0.0132(8) 0.0051(7) 0.0059(7) 0.0090(8) O18 0.0233(10) 0.0336(12) 0.0207(10) 0.0155(9) 0.0094(8) 0.0142(9) O19 0.162(4) 0.087(3) 0.096(3) 0.076(2) 0.108(3) 0.104(3) O20 0.0250(16) 0.058(2) 0.122(4) -0.019(2) 0.025(2) 0.0091(15) O21 0.0198(10) 0.0292(11) 0.0227(10) 0.0079(9) 0.0105(9) 0.0102(9) O22 0.115(4) 0.095(3) 0.092(3) 0.047(3) 0.067(3) 0.043(3) O23 0.0220(11) 0.0294(12) 0.0398(14) 0.0051(11) 0.0125(11) 0.0111(10) O24 0.050(2) 0.050(2) 0.220(6) 0.039(3) -0.005(3) 0.0129(19) O25 0.0288(14) 0.095(3) 0.0170(11) -0.0018(13) 0.0055(10) 0.0273(15) O26 0.090(3) 0.0469(19) 0.100(3) -0.0009(19) 0.076(3) 0.0150(18) O27 0.031(3) 0.025(3) 0.023(3) 0.004(2) 0.001(2) 0.006(2) O28 0.036(3) 0.034(3) 0.036(3) 0.016(3) 0.019(3) 0.013(3) O278 0.041(3) 0.044(3) 0.028(2) 0.0018(18) 0.0090(19) 0.026(2) N1 0.0139(10) 0.0121(9) 0.0138(9) 0.0040(8) 0.0045(8) 0.0046(8) N2 0.0161(10) 0.0146(10) 0.0128(9) 0.0033(8) 0.0023(8) 0.0044(8) N3 0.0212(11) 0.0147(10) 0.0141(10) 0.0038(8) 0.0067(9) 0.0075(9) N4 0.0169(10) 0.0125(10) 0.0182(10) 0.0052(8) 0.0024(9) 0.0034(8) N5 0.0116(9) 0.0108(9) 0.0155(9) 0.0025(8) 0.0037(8) 0.0039(8) N6 0.0104(9) 0.0120(9) 0.0112(9) 0.0015(7) 0.0030(7) 0.0039(7) N7 0.0175(10) 0.0170(10) 0.0225(11) 0.0110(9) 0.0112(9) 0.0085(9) N8 0.0117(9) 0.0120(9) 0.0147(9) 0.0033(8) 0.0038(8) 0.0044(8) C1 0.0127(11) 0.0130(11) 0.0118(10) 0.0021(9) 0.0034(9) 0.0036(9) C2 0.0146(11) 0.0106(10) 0.0136(11) 0.0026(9) 0.0039(9) 0.0026(9) C3 0.0172(12) 0.0156(12) 0.0144(11) 0.0057(9) 0.0051(10) 0.0043(10) C4 0.0155(12) 0.0146(11) 0.0166(11) 0.0056(9) 0.0036(10) 0.0054(10) C5 0.0145(11) 0.0115(11) 0.0164(11) 0.0039(9) 0.0044(9) 0.0046(9) C6 0.0147(11) 0.0126(11) 0.0158(11) 0.0037(9) 0.0050(9) 0.0054(9) C7 0.0150(11) 0.0115(11) 0.0142(11) 0.0024(9) 0.0031(9) 0.0040(9) C8 0.0195(12) 0.0144(11) 0.0161(12) 0.0070(10) 0.0060(10) 0.0064(10) C9 0.0204(12) 0.0155(11) 0.0166(11) 0.0064(9) 0.0084(10) 0.0093(10) C10 0.0328(15) 0.0172(12) 0.0165(12) 0.0051(10) 0.0111(12) 0.0121(12) C11 0.0374(17) 0.0236(14) 0.0237(13) 0.0128(11) 0.0199(13) 0.0200(13) C12 0.0284(15) 0.0244(14) 0.0272(14) 0.0152(12) 0.0162(12) 0.0172(12) C13 0.0226(13) 0.0208(13) 0.0179(12) 0.0087(10) 0.0078(11) 0.0120(11) C14 0.0160(12) 0.0137(11) 0.0223(13) 0.0053(10) 0.0062(10) 0.0043(10) C15 0.0237(14) 0.0252(14) 0.0111(11) 0.0055(10) 0.0018(10) 0.0069(12) C16 0.0204(13) 0.0134(11) 0.0258(13) 0.0070(10) 0.0107(11) 0.0074(10) C17 0.0141(11) 0.0139(11) 0.0193(12) 0.0066(10) 0.0040(10) 0.0038(9) C18 0.0198(13) 0.0138(12) 0.0203(13) 0.0048(11) -0.0013(11) 0.0010(10) C19 0.0153(13) 0.0186(13) 0.0356(16) 0.0146(12) 0.0009(12) 0.0026(11) C20 0.0168(13) 0.0226(14) 0.0390(17) 0.0167(13) 0.0099(13) 0.0072(11) C21 0.0189(13) 0.0193(13) 0.0278(14) 0.0110(11) 0.0099(11) 0.0079(11) C22 0.0394(18) 0.0179(14) 0.0189(13) 0.0023(11) 0.0055(13) 0.0062(13) C23 0.0096(10) 0.0136(11) 0.0172(11) 0.0043(9) 0.0033(9) 0.0041(9) C24 0.0106(10) 0.0121(10) 0.0137(10) 0.0035(9) 0.0035(9) 0.0033(9) C25 0.0113(10) 0.0140(11) 0.0136(10) 0.0051(9) 0.0041(9) 0.0064(9) C26 0.0104(10) 0.0133(11) 0.0115(10) 0.0034(9) 0.0036(9) 0.0039(9) C27 0.0099(10) 0.0149(11) 0.0094(10) 0.0019(8) 0.0016(8) 0.0043(9) C28 0.0108(10) 0.0154(11) 0.0132(11) 0.0017(9) 0.0042(9) 0.0050(9) C29 0.0116(10) 0.0137(11) 0.0108(10) 0.0020(8) 0.0028(9) 0.0041(9) C30 0.0155(12) 0.0121(11) 0.0228(13) 0.0049(10) 0.0054(10) 0.0044(10) C31 0.0162(12) 0.0143(11) 0.0249(13) 0.0096(10) 0.0102(10) 0.0064(10) C32 0.0296(15) 0.0275(15) 0.0296(15) 0.0188(12) 0.0204(13) 0.0179(13) C33 0.0346(17) 0.0341(17) 0.0461(19) 0.0291(15) 0.0324(16) 0.0229(14) C34 0.0241(15) 0.0276(15) 0.057(2) 0.0284(15) 0.0289(15) 0.0165(13) C35 0.0157(12) 0.0217(13) 0.0389(17) 0.0188(13) 0.0138(12) 0.0080(11) C36 0.0131(11) 0.0188(12) 0.0145(11) 0.0057(9) 0.0041(9) 0.0058(9) C37 0.0174(12) 0.0132(11) 0.0117(10) 0.0004(9) 0.0041(9) 0.0045(9) C38 0.0142(11) 0.0183(12) 0.0136(11) 0.0051(9) 0.0055(9) 0.0069(9) C39 0.0144(11) 0.0118(11) 0.0130(10) 0.0022(9) 0.0034(9) 0.0044(9) C40 0.0159(12) 0.0143(11) 0.0160(11) 0.0040(9) 0.0027(10) 0.0057(9) C41 0.0149(12) 0.0196(13) 0.0221(13) 0.0054(11) 0.0014(11) 0.0080(10) C42 0.0180(13) 0.0255(14) 0.0278(14) 0.0057(12) 0.0085(11) 0.0135(11) C43 0.0178(12) 0.0199(13) 0.0205(13) 0.0023(10) 0.0069(11) 0.0098(10) C44 0.0157(12) 0.0234(13) 0.0198(12) 0.0092(10) 0.0085(10) 0.0100(10) P1 0.0571(19) 0.0192(12) 0.0171(9) 0.0023(10) 0.0067(10) 0.0040(12) F1 0.085(4) 0.038(3) 0.017(2) 0.0007(19) 0.009(2) 0.009(3) F2 0.079(4) 0.027(2) 0.052(3) 0.022(2) 0.023(3) 0.022(2) F3 0.059(3) 0.043(3) 0.0194(19) -0.0020(18) 0.006(2) -0.002(2) F4 0.092(5) 0.102(6) 0.075(5) 0.044(4) 0.056(4) 0.064(5) F5 0.099(5) 0.034(3) 0.045(3) 0.018(2) 0.001(3) -0.003(3) F6 0.048(3) 0.109(5) 0.051(3) 0.007(3) 0.021(3) 0.011(3) P1A 0.0376(17) 0.056(3) 0.0154(10) 0.0031(18) 0.0036(11) 0.0189(19) F1A 0.052(4) 0.065(4) 0.078(5) 0.037(4) 0.021(3) 0.029(3) F2A 0.032(3) 0.073(5) 0.039(4) 0.015(3) -0.002(3) -0.004(3) F3A 0.111(6) 0.065(4) 0.046(3) 0.037(3) 0.053(4) 0.052(4) F4A 0.054(5) 0.157(10) 0.108(7) -0.096(7) -0.008(5) 0.050(6) F5A 0.045(3) 0.092(5) 0.034(3) -0.008(3) -0.013(3) 0.030(3) F6A 0.064(5) 0.156(9) 0.058(4) 0.010(5) 0.028(4) -0.046(5) _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 O13 1.912(2) . ? Co1 O14 1.9146(19) . ? Co1 N4 1.925(2) . ? Co1 N3 1.928(2) . ? Co1 N1 1.932(2) . ? Co1 N2 2.036(2) . ? Co2 O17 1.9039(18) . ? Co2 N7 1.913(2) . ? Co2 O16 1.9141(19) . ? Co2 N8 1.932(2) . ? Co2 N5 1.940(2) . ? Co2 N6 2.027(2) . ? K1 O23 2.738(2) 2_656 ? K1 O5 2.780(2) . ? K1 O21 2.868(2) . ? K1 O12 2.899(2) . ? K1 O20 2.904(4) . ? K1 O11 2.906(2) 2_656 ? K1 O19 3.006(3) . ? K1 K2 4.5484(10) 2_656 ? K2 O3 2.657(2) . ? K2 O9 2.690(2) 1_455 ? K2 O1 2.720(2) . ? K2 O22 2.729(4) . ? K2 O23 2.833(3) . ? K2 O7 2.901(2) 2_656 ? K2 F1A 2.969(6) . ? K2 O21 3.032(2) 2_656 ? K2 F2 3.087(5) . ? K2 K1 4.5484(10) 2_656 ? K3 O9 2.641(2) 1_455 ? K3 O25 2.682(3) . ? K3 O8 2.743(2) 1_455 ? K3 O3 2.745(2) . ? K3 O10 2.811(2) 2_656 ? K3 O24 2.823(4) . ? K3 O20 3.251(4) 1_455 ? K3 C36 3.400(3) 1_455 ? O1 C7 1.401(3) . ? O1 H1O 0.73(4) . ? O2 C7 1.407(3) . ? O2 H2O 0.74(4) . ? O3 C14 1.243(3) . ? O4 C14 1.253(3) . ? O5 C16 1.263(3) . ? O6 C16 1.240(4) . ? O7 C29 1.399(3) . ? O7 K2 2.901(2) 2_656 ? O7 H7O 0.78(4) . ? O8 C29 1.408(3) . ? O8 K3 2.7434(19) 1_655 ? O8 H8O 0.80(4) . ? O9 C36 1.245(3) . ? O9 K3 2.641(2) 1_655 ? O9 K2 2.690(2) 1_655 ? O10 C36 1.265(3) . ? O10 K3 2.811(2) 2_656 ? O11 C38 1.259(3) . ? O11 K1 2.906(2) 2_656 ? O12 C38 1.260(3) . ? O13 C22 1.340(4) . ? O14 C22 1.310(4) . ? O15 C22 1.225(4) . ? O16 C44 1.320(3) . ? O17 C44 1.319(3) . ? O18 C44 1.235(3) . ? O19 H19O 0.89 . ? O19 H19Q 0.97 . ? O20 K3 3.251(4) 1_655 ? O20 H20O 0.80(5) . ? O20 H20Q 0.83(7) . ? O21 K2 3.032(2) 2_656 ? O21 H21O 0.81(4) . ? O21 H21Q 0.87(4) . ? O22 H22O 1.02 . ? O23 K1 2.738(2) 2_656 ? O23 H23O 0.95(5) . ? O23 H23Q 0.88(6) . ? O24 H24O 1.08 . ? O25 H25O 0.95(7) . ? O25 H25Q 0.98(6) . ? N1 C8 1.495(3) . ? N1 C6 1.505(3) . ? N1 C1 1.516(3) . ? N2 C15 1.489(3) . ? N2 C4 1.496(3) . ? N2 C3 1.496(4) . ? N3 C10 1.350(3) . ? N3 C9 1.353(3) . ? N4 C18 1.350(4) . ? N4 C17 1.354(3) . ? N5 C30 1.494(3) . ? N5 C23 1.509(3) . ? N5 C28 1.510(3) . ? N6 C26 1.492(3) . ? N6 C37 1.495(3) . ? N6 C25 1.504(3) . ? N7 C32 1.342(4) . ? N7 C31 1.355(4) . ? N8 C40 1.339(3) . ? N8 C39 1.358(3) . ? C1 C9 1.505(4) . ? C1 C2 1.549(3) . ? C1 H1 0.93(3) . ? C2 C3 1.527(3) . ? C2 C7 1.547(4) . ? C2 C14 1.568(4) . ? C3 H3A 0.94(3) . ? C3 H3B 0.86(3) . ? C4 C5 1.528(4) . ? C4 H4A 0.95(3) . ? C4 H4B 0.91(3) . ? C5 C6 1.549(4) . ? C5 C16 1.551(4) . ? C5 C7 1.557(4) . ? C6 C17 1.508(4) . ? C6 H6 0.94(3) . ? C8 H8A 0.97(3) . ? C8 H8B 0.96(4) . ? C8 H8C 0.92(4) . ? C9 C13 1.385(4) . ? C10 C11 1.380(4) . ? C10 H10 0.97(4) . ? C11 C12 1.395(5) . ? C11 H11 0.91(4) . ? C12 C13 1.389(4) . ? C12 H12 0.91(4) . ? C13 H13 0.93(3) . ? C15 H15A 0.98(4) . ? C15 H15B 0.98(4) . ? C15 H15C 0.96(4) . ? C17 C21 1.382(4) . ? C18 C19 1.376(5) . ? C18 H18 0.81(4) . ? C19 C20 1.384(5) . ? C19 H19 0.94(4) . ? C20 C21 1.391(4) . ? C20 H20 0.91(4) . ? C21 H21 0.91(4) . ? C23 C31 1.517(4) . ? C23 C24 1.547(3) . ? C23 H23 0.90(3) . ? C24 C25 1.533(3) . ? C24 C36 1.554(3) . ? C24 C29 1.554(3) . ? C25 H25A 0.95(3) . ? C25 H25B 0.92(4) . ? C26 C27 1.528(3) . ? C26 H26A 0.94(3) . ? C26 H26B 0.89(3) . ? C27 C29 1.548(3) . ? C27 C28 1.550(4) . ? C27 C38 1.553(3) . ? C28 C39 1.508(3) . ? C28 H28 0.94(3) . ? C30 H30A 0.89(3) . ? C30 H30B 0.91(4) . ? C30 H30C 1.00(4) . ? C31 C35 1.385(4) . ? C32 C33 1.385(4) . ? C32 H32 0.97(4) . ? C33 C34 1.379(5) . ? C33 H33 0.96(4) . ? C34 C35 1.389(5) . ? C34 H34 0.92(4) . ? C35 H35 0.95(4) . ? C36 K3 3.400(3) 1_655 ? C37 H37A 0.99(3) . ? C37 H37B 0.95(4) . ? C37 H37C 0.96(3) . ? C39 C43 1.377(4) . ? C40 C41 1.384(4) . ? C40 H40 0.94(4) . ? C41 C42 1.387(4) . ? C41 H41 0.83(4) . ? C42 C43 1.396(4) . ? C42 H42 0.98(4) . ? C43 H43 0.90(4) . ? P1 F4 1.492(8) . ? P1 F5 1.579(6) . ? P1 F1 1.580(6) . ? P1 F3 1.599(5) . ? P1 F2 1.616(5) . ? P1 F6 1.664(8) . ? P1A F2A 1.553(7) . ? P1A F3A 1.574(7) . ? P1A F1A 1.585(8) . ? P1A F6A 1.587(9) . ? P1A F5A 1.600(7) . ? P1A F4A 1.638(10) . ? 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 O13 Co1 O14 68.89(9) . . ? O13 Co1 N4 93.64(10) . . ? O14 Co1 N4 89.37(9) . . ? O13 Co1 N3 94.65(10) . . ? O14 Co1 N3 87.97(9) . . ? N4 Co1 N3 169.74(10) . . ? O13 Co1 N1 168.44(9) . . ? O14 Co1 N1 99.56(9) . . ? N4 Co1 N1 85.53(9) . . ? N3 Co1 N1 85.14(9) . . ? O13 Co1 N2 102.30(9) . . ? O14 Co1 N2 171.19(9) . . ? N4 Co1 N2 91.24(9) . . ? N3 Co1 N2 92.90(9) . . ? N1 Co1 N2 89.25(9) . . ? O17 Co2 N7 93.58(9) . . ? O17 Co2 O16 68.74(8) . . ? N7 Co2 O16 89.18(9) . . ? O17 Co2 N8 94.81(9) . . ? N7 Co2 N8 169.86(10) . . ? O16 Co2 N8 88.54(9) . . ? O17 Co2 N5 169.86(9) . . ? N7 Co2 N5 85.94(9) . . ? O16 Co2 N5 101.12(9) . . ? N8 Co2 N5 84.80(9) . . ? O17 Co2 N6 101.12(8) . . ? N7 Co2 N6 90.01(9) . . ? O16 Co2 N6 169.76(8) . . ? N8 Co2 N6 93.97(9) . . ? N5 Co2 N6 89.01(8) . . ? O23 K1 O5 138.45(7) 2_656 . ? O23 K1 O21 74.23(7) 2_656 . ? O5 K1 O21 133.25(7) . . ? O23 K1 O12 93.90(8) 2_656 . ? O5 K1 O12 72.30(6) . . ? O21 K1 O12 73.38(6) . . ? O23 K1 O20 71.22(10) 2_656 . ? O5 K1 O20 68.62(10) . . ? O21 K1 O20 137.22(10) . . ? O12 K1 O20 84.51(12) . . ? O23 K1 O11 139.24(7) 2_656 2_656 ? O5 K1 O11 82.10(6) . 2_656 ? O21 K1 O11 71.49(6) . 2_656 ? O12 K1 O11 96.80(6) . 2_656 ? O20 K1 O11 148.87(9) . 2_656 ? O23 K1 O19 101.59(9) 2_656 . ? O5 K1 O19 87.31(8) . . ? O21 K1 O19 123.49(10) . . ? O12 K1 O19 159.61(7) . . ? O20 K1 O19 87.97(14) . . ? O11 K1 O19 80.10(9) 2_656 . ? O3 K2 O9 83.09(7) . 1_455 ? O3 K2 O1 65.24(6) . . ? O9 K2 O1 148.30(7) 1_455 . ? O3 K2 O22 133.81(12) . . ? O9 K2 O22 121.07(12) 1_455 . ? O1 K2 O22 84.56(12) . . ? O3 K2 O23 149.55(8) . . ? O9 K2 O23 73.26(7) 1_455 . ? O1 K2 O23 135.51(7) . . ? O22 K2 O23 76.00(12) . . ? O3 K2 O7 78.09(6) . 2_656 ? O9 K2 O7 67.05(6) 1_455 2_656 ? O1 K2 O7 103.32(6) . 2_656 ? O22 K2 O7 145.55(11) . 2_656 ? O23 K2 O7 75.19(7) . 2_656 ? O3 K2 F1A 93.41(17) . . ? O9 K2 F1A 82.14(13) 1_455 . ? O1 K2 F1A 100.09(13) . . ? O22 K2 F1A 56.91(18) . . ? O23 K2 F1A 101.86(16) . . ? O7 K2 F1A 148.70(14) 2_656 . ? O3 K2 O21 125.39(7) . 2_656 ? O9 K2 O21 141.79(7) 1_455 2_656 ? O1 K2 O21 65.21(6) . 2_656 ? O22 K2 O21 60.20(11) . 2_656 ? O23 K2 O21 70.40(7) . 2_656 ? O7 K2 O21 92.32(6) 2_656 2_656 ? F1A K2 O21 116.44(15) . 2_656 ? O3 K2 F2 73.33(12) . . ? O9 K2 F2 73.08(12) 1_455 . ? O1 K2 F2 97.57(11) . . ? O22 K2 F2 77.34(16) . . ? O23 K2 F2 116.02(11) . . ? O7 K2 F2 133.01(13) 2_656 . ? F1A K2 F2 21.34(16) . . ? O21 K2 F2 134.66(13) 2_656 . ? O9 K3 O25 154.72(9) 1_455 . ? O9 K3 O8 68.08(6) 1_455 1_455 ? O25 K3 O8 125.51(8) . 1_455 ? O9 K3 O3 82.33(6) 1_455 . ? O25 K3 O3 84.26(8) . . ? O8 K3 O3 149.74(7) 1_455 . ? O9 K3 O10 79.31(6) 1_455 2_656 ? O25 K3 O10 85.26(9) . 2_656 ? O8 K3 O10 71.78(6) 1_455 2_656 ? O3 K3 O10 109.84(7) . 2_656 ? O9 K3 O24 106.77(16) 1_455 . ? O25 K3 O24 95.88(17) . . ? O8 K3 O24 86.85(10) 1_455 . ? O3 K3 O24 96.09(11) . . ? O10 K3 O24 154.01(11) 2_656 . ? O9 K3 O20 137.69(9) 1_455 1_455 ? O25 K3 O20 55.37(11) . 1_455 ? O8 K3 O20 71.35(9) 1_455 1_455 ? O3 K3 O20 138.91(10) . 1_455 ? O10 K3 O20 77.15(9) 2_656 1_455 ? O24 K3 O20 82.18(16) . 1_455 ? O9 K3 C36 18.96(6) 1_455 1_455 ? O25 K3 C36 147.47(9) . 1_455 ? O8 K3 C36 54.96(6) 1_455 1_455 ? O3 K3 C36 97.65(6) . 1_455 ? O10 K3 C36 63.43(6) 2_656 1_455 ? O24 K3 C36 116.04(15) . 1_455 ? O20 K3 C36 120.12(9) 1_455 1_455 ? C7 O1 K2 136.62(16) . . ? C7 O1 H1O 99(3) . . ? K2 O1 H1O 119(3) . . ? C7 O2 H2O 106(3) . . ? C14 O3 K2 140.95(19) . . ? C14 O3 K3 120.09(18) . . ? K2 O3 K3 96.35(7) . . ? C16 O5 K1 105.15(17) . . ? C29 O7 K2 159.96(15) . 2_656 ? C29 O7 H7O 110(3) . . ? K2 O7 H7O 84(3) 2_656 . ? C29 O8 K3 130.58(15) . 1_655 ? C29 O8 H8O 106(3) . . ? K3 O8 H8O 111(3) 1_655 . ? C36 O9 K3 117.47(17) . 1_655 ? C36 O9 K2 127.87(17) . 1_655 ? K3 O9 K2 98.07(6) 1_655 1_655 ? C36 O10 K3 150.94(17) . 2_656 ? C38 O11 K1 128.74(17) . 2_656 ? C38 O12 K1 127.86(17) . . ? C22 O13 Co1 90.39(17) . . ? C22 O14 Co1 91.19(17) . . ? C44 O16 Co2 90.61(15) . . ? C44 O17 Co2 91.08(15) . . ? H19O O19 H19Q 100 . . ? H20O O20 H20Q 106(6) . . ? K1 O21 K2 100.83(7) . 2_656 ? K1 O23 K2 109.46(9) 2_656 . ? H23O O23 H23Q 101(4) . . ? H25O O25 H25Q 103(5) . . ? C8 N1 C6 107.7(2) . . ? C8 N1 C1 107.4(2) . . ? C6 N1 C1 117.61(19) . . ? C8 N1 Co1 112.50(16) . . ? C6 N1 Co1 105.83(15) . . ? C1 N1 Co1 105.93(15) . . ? C15 N2 C4 108.0(2) . . ? C15 N2 C3 108.4(2) . . ? C4 N2 C3 105.1(2) . . ? C15 N2 Co1 107.55(17) . . ? C4 N2 Co1 114.35(16) . . ? C3 N2 Co1 113.24(16) . . ? C10 N3 C9 119.3(2) . . ? C10 N3 Co1 127.3(2) . . ? C9 N3 Co1 113.01(17) . . ? C18 N4 C17 119.0(3) . . ? C18 N4 Co1 127.9(2) . . ? C17 N4 Co1 112.89(18) . . ? C30 N5 C23 107.61(19) . . ? C30 N5 C28 108.1(2) . . ? C23 N5 C28 117.5(2) . . ? C30 N5 Co2 112.03(17) . . ? C23 N5 Co2 105.88(15) . . ? C28 N5 Co2 105.71(15) . . ? C26 N6 C37 108.07(19) . . ? C26 N6 C25 104.52(18) . . ? C37 N6 C25 108.49(19) . . ? C26 N6 Co2 113.03(15) . . ? C37 N6 Co2 106.73(15) . . ? C25 N6 Co2 115.75(15) . . ? C32 N7 C31 119.8(2) . . ? C32 N7 Co2 127.0(2) . . ? C31 N7 Co2 113.09(18) . . ? C40 N8 C39 119.1(2) . . ? C40 N8 Co2 127.28(18) . . ? C39 N8 Co2 113.24(17) . . ? C9 C1 N1 105.6(2) . . ? C9 C1 C2 108.6(2) . . ? N1 C1 C2 112.8(2) . . ? C9 C1 H1 112.0(19) . . ? N1 C1 H1 110.3(19) . . ? C2 C1 H1 107.6(19) . . ? C3 C2 C7 109.7(2) . . ? C3 C2 C1 112.4(2) . . ? C7 C2 C1 107.4(2) . . ? C3 C2 C14 107.8(2) . . ? C7 C2 C14 112.8(2) . . ? C1 C2 C14 106.9(2) . . ? N2 C3 C2 112.0(2) . . ? N2 C3 H3A 109(2) . . ? C2 C3 H3A 110(2) . . ? N2 C3 H3B 108(2) . . ? C2 C3 H3B 109(2) . . ? H3A C3 H3B 108(3) . . ? N2 C4 C5 110.5(2) . . ? N2 C4 H4A 112(2) . . ? C5 C4 H4A 108(2) . . ? N2 C4 H4B 109(2) . . ? C5 C4 H4B 108(2) . . ? H4A C4 H4B 109(3) . . ? C4 C5 C6 112.3(2) . . ? C4 C5 C16 109.1(2) . . ? C6 C5 C16 108.0(2) . . ? C4 C5 C7 110.5(2) . . ? C6 C5 C7 108.2(2) . . ? C16 C5 C7 108.7(2) . . ? N1 C6 C17 106.3(2) . . ? N1 C6 C5 112.4(2) . . ? C17 C6 C5 108.3(2) . . ? N1 C6 H6 110.4(19) . . ? C17 C6 H6 110(2) . . ? C5 C6 H6 109.3(19) . . ? O1 C7 O2 111.9(2) . . ? O1 C7 C2 110.0(2) . . ? O2 C7 C2 109.0(2) . . ? O1 C7 C5 110.0(2) . . ? O2 C7 C5 108.7(2) . . ? C2 C7 C5 107.1(2) . . ? N1 C8 H8A 108.8(19) . . ? N1 C8 H8B 110(2) . . ? H8A C8 H8B 107(3) . . ? N1 C8 H8C 109(2) . . ? H8A C8 H8C 110(3) . . ? H8B C8 H8C 112(3) . . ? N3 C9 C13 122.2(2) . . ? N3 C9 C1 113.6(2) . . ? C13 C9 C1 123.9(2) . . ? N3 C10 C11 121.5(3) . . ? N3 C10 H10 119(2) . . ? C11 C10 H10 120(2) . . ? C10 C11 C12 119.3(3) . . ? C10 C11 H11 121(2) . . ? C12 C11 H11 120(2) . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 122(2) . . ? C11 C12 H12 118(2) . . ? C9 C13 C12 118.4(3) . . ? C9 C13 H13 119(2) . . ? C12 C13 H13 122(2) . . ? O3 C14 O4 126.6(3) . . ? O3 C14 C2 117.7(2) . . ? O4 C14 C2 115.6(2) . . ? N2 C15 H15A 109(2) . . ? N2 C15 H15B 108(2) . . ? H15A C15 H15B 108(3) . . ? N2 C15 H15C 107(2) . . ? H15A C15 H15C 110(3) . . ? H15B C15 H15C 115(3) . . ? O6 C16 O5 125.8(3) . . ? O6 C16 C5 118.2(3) . . ? O5 C16 C5 115.9(2) . . ? N4 C17 C21 122.0(3) . . ? N4 C17 C6 113.3(2) . . ? C21 C17 C6 124.2(2) . . ? N4 C18 C19 121.6(3) . . ? N4 C18 H18 116(3) . . ? C19 C18 H18 122(3) . . ? C18 C19 C20 119.5(3) . . ? C18 C19 H19 117(2) . . ? C20 C19 H19 123(2) . . ? C19 C20 C21 119.2(3) . . ? C19 C20 H20 123(3) . . ? C21 C20 H20 118(2) . . ? C17 C21 C20 118.5(3) . . ? C17 C21 H21 121(3) . . ? C20 C21 H21 120(3) . . ? O15 C22 O14 125.7(3) . . ? O15 C22 O13 124.8(3) . . ? O14 C22 O13 109.5(2) . . ? N5 C23 C31 106.1(2) . . ? N5 C23 C24 112.9(2) . . ? C31 C23 C24 107.7(2) . . ? N5 C23 H23 110(2) . . ? C31 C23 H23 111(2) . . ? C24 C23 H23 108(2) . . ? C25 C24 C23 111.9(2) . . ? C25 C24 C36 109.7(2) . . ? C23 C24 C36 108.9(2) . . ? C25 C24 C29 109.22(19) . . ? C23 C24 C29 108.5(2) . . ? C36 C24 C29 108.57(19) . . ? N6 C25 C24 110.94(19) . . ? N6 C25 H25A 107(2) . . ? C24 C25 H25A 114(2) . . ? N6 C25 H25B 108(2) . . ? C24 C25 H25B 109(2) . . ? H25A C25 H25B 108(3) . . ? N6 C26 C27 111.17(19) . . ? N6 C26 H26A 112(2) . . ? C27 C26 H26A 109(2) . . ? N6 C26 H26B 106(2) . . ? C27 C26 H26B 108(2) . . ? H26A C26 H26B 111(3) . . ? C26 C27 C29 110.6(2) . . ? C26 C27 C28 112.7(2) . . ? C29 C27 C28 107.16(19) . . ? C26 C27 C38 109.0(2) . . ? C29 C27 C38 107.41(19) . . ? C28 C27 C38 109.8(2) . . ? C39 C28 N5 105.9(2) . . ? C39 C28 C27 108.8(2) . . ? N5 C28 C27 112.58(19) . . ? C39 C28 H28 112(2) . . ? N5 C28 H28 110(2) . . ? C27 C28 H28 107(2) . . ? O7 C29 O8 111.3(2) . . ? O7 C29 C27 107.6(2) . . ? O8 C29 C27 111.2(2) . . ? O7 C29 C24 112.6(2) . . ? O8 C29 C24 106.9(2) . . ? C27 C29 C24 107.17(19) . . ? N5 C30 H30A 108(2) . . ? N5 C30 H30B 110(2) . . ? H30A C30 H30B 115(3) . . ? N5 C30 H30C 109(2) . . ? H30A C30 H30C 109(3) . . ? H30B C30 H30C 106(3) . . ? N7 C31 C35 121.3(3) . . ? N7 C31 C23 113.6(2) . . ? C35 C31 C23 124.4(3) . . ? N7 C32 C33 121.4(3) . . ? N7 C32 H32 116(3) . . ? C33 C32 H32 122(3) . . ? C34 C33 C32 119.0(3) . . ? C34 C33 H33 121(2) . . ? C32 C33 H33 120(2) . . ? C33 C34 C35 119.9(3) . . ? C33 C34 H34 120(2) . . ? C35 C34 H34 120(2) . . ? C31 C35 C34 118.5(3) . . ? C31 C35 H35 120(2) . . ? C34 C35 H35 122(2) . . ? O9 C36 O10 125.4(2) . . ? O9 C36 C24 117.5(2) . . ? O10 C36 C24 117.1(2) . . ? N6 C37 H37A 109.4(19) . . ? N6 C37 H37B 103(2) . . ? H37A C37 H37B 111(3) . . ? N6 C37 H37C 109.2(19) . . ? H37A C37 H37C 109(3) . . ? H37B C37 H37C 115(3) . . ? O11 C38 O12 125.6(2) . . ? O11 C38 C27 118.4(2) . . ? O12 C38 C27 115.9(2) . . ? N8 C39 C43 122.1(2) . . ? N8 C39 C28 113.0(2) . . ? C43 C39 C28 124.6(2) . . ? N8 C40 C41 121.7(2) . . ? N8 C40 H40 118(2) . . ? C41 C40 H40 120(2) . . ? C40 C41 C42 119.4(3) . . ? C40 C41 H41 121(2) . . ? C42 C41 H41 120(2) . . ? C41 C42 C43 118.9(3) . . ? C41 C42 H42 122(2) . . ? C43 C42 H42 119(2) . . ? C39 C43 C42 118.7(3) . . ? C39 C43 H43 120(2) . . ? C42 C43 H43 122(2) . . ? O18 C44 O17 125.5(3) . . ? O18 C44 O16 124.9(3) . . ? O17 C44 O16 109.5(2) . . ? F4 P1 F5 91.5(5) . . ? F4 P1 F1 93.8(5) . . ? F5 P1 F1 90.9(3) . . ? F4 P1 F3 93.2(4) . . ? F5 P1 F3 89.3(3) . . ? F1 P1 F3 173.0(5) . . ? F4 P1 F2 93.1(4) . . ? F5 P1 F2 175.3(5) . . ? F1 P1 F2 90.1(3) . . ? F3 P1 F2 89.2(3) . . ? F4 P1 F6 178.7(5) . . ? F5 P1 F6 87.4(4) . . ? F1 P1 F6 85.5(4) . . ? F3 P1 F6 87.4(4) . . ? F2 P1 F6 88.0(4) . . ? P1 F2 K2 156.8(4) . . ? F2A P1A F3A 89.9(4) . . ? F2A P1A F1A 90.6(5) . . ? F3A P1A F1A 90.7(4) . . ? F2A P1A F6A 91.2(4) . . ? F3A P1A F6A 178.9(5) . . ? F1A P1A F6A 89.3(6) . . ? F2A P1A F5A 177.6(5) . . ? F3A P1A F5A 90.8(4) . . ? F1A P1A F5A 91.7(4) . . ? F6A P1A F5A 88.1(5) . . ? F2A P1A F4A 88.7(5) . . ? F3A P1A F4A 88.2(7) . . ? F1A P1A F4A 178.6(7) . . ? F6A P1A F4A 91.9(7) . . ? F5A P1A F4A 89.1(4) . . ? P1A F1A K2 133.0(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.972 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.114 # Attachment 'CoIIL2diaqua.cif' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 600458' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H29 Cl2 Co N4 O17' _chemical_formula_weight 763.33 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7753(8) _cell_length_b 12.5214(10) _cell_length_c 15.2590(12) _cell_angle_alpha 91.266(2) _cell_angle_beta 109.016(2) _cell_angle_gamma 111.689(1) _cell_volume 1784.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _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 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 0.9018 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19613 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6313 _reflns_number_gt 4436 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2800P)^2^+0.3141P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6313 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.1045 _refine_ls_wR_factor_ref 0.3652 _refine_ls_wR_factor_gt 0.3371 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 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 0.3562(6) 0.9967(5) 0.2503(4) 0.0331(13) Uani 1 1 d . A 1 H1 H 0.3305 1.0558 0.2141 0.040 Uiso 1 1 calc R A 1 C2 C 0.5156(6) 1.0567(6) 0.3199(4) 0.0356(13) Uani 1 1 d . A 1 C3 C 0.6131(7) 1.0891(5) 0.2616(4) 0.0375(14) Uani 1 1 d . A 1 C4 C 0.5999(6) 0.9739(5) 0.2107(4) 0.0348(13) Uani 1 1 d . A 1 C5 C 0.4422(6) 0.9121(5) 0.1401(4) 0.0293(12) Uani 1 1 d . A 1 H5 H 0.4271 0.9576 0.0875 0.035 Uiso 1 1 calc R A 1 C6 C 0.5575(7) 0.9799(6) 0.3897(4) 0.0432(16) Uani 1 1 d . A 1 H6A H 0.6574 1.0226 0.4334 0.052 Uiso 1 1 calc R A 1 H6B H 0.4945 0.9603 0.4270 0.052 Uiso 1 1 calc R A 1 C7 C 0.6418(7) 0.9011(6) 0.2862(4) 0.0434(16) Uani 1 1 d . A 1 H7A H 0.6369 0.8282 0.2558 0.052 Uiso 1 1 calc R A 1 H7B H 0.7416 0.9454 0.3296 0.052 Uiso 1 1 calc R A 1 C8 C 0.4179(6) 0.7893(5) 0.1000(4) 0.0333(13) Uani 1 1 d . A 1 C9 C 0.4408(7) 0.7683(5) 0.0194(4) 0.0369(14) Uani 1 1 d . A 1 H9 H 0.4660 0.8286 -0.0163 0.044 Uiso 1 1 calc R A 1 C10 C 0.4264(8) 0.6575(6) -0.0089(5) 0.0469(16) Uani 1 1 d . A 1 H10 H 0.4416 0.6401 -0.0645 0.056 Uiso 1 1 calc R A 1 C11 C 0.3893(8) 0.5714(6) 0.0455(5) 0.0475(16) Uani 1 1 d . A 1 H11 H 0.3797 0.4947 0.0277 0.057 Uiso 1 1 calc R A 1 C12 C 0.3666(8) 0.5989(6) 0.1256(5) 0.0474(16) Uani 1 1 d . A 1 H12 H 0.3401 0.5403 0.1623 0.057 Uiso 1 1 calc R A 1 C13 C 0.2575(6) 0.9517(6) 0.3043(4) 0.0424(15) Uani 1 1 d . A 1 C14 C 0.1977(7) 1.0178(7) 0.3354(4) 0.0487(17) Uani 1 1 d . A 1 H14 H 0.2145 1.0940 0.3207 0.058 Uiso 1 1 calc R A 1 C15 C 0.1132(8) 0.9725(9) 0.3882(5) 0.063(2) Uani 1 1 d . A 1 H15 H 0.0716 1.0172 0.4103 0.076 Uiso 1 1 calc R A 1 C16 C 0.0911(8) 0.8647(12) 0.4075(5) 0.081(4) Uani 1 1 d . A 1 H16 H 0.0315 0.8319 0.4424 0.098 Uiso 1 1 calc R A 1 C17 C 0.1521(9) 0.8027(9) 0.3781(5) 0.070(3) Uani 1 1 d . A 1 H17 H 0.1357 0.7269 0.3937 0.085 Uiso 1 1 calc R A 1 C18 C 0.5362(7) 1.1669(6) 0.3786(4) 0.0431(15) Uani 1 1 d . A 1 C19 C 0.5325(10) 1.3555(7) 0.3743(5) 0.060(2) Uani 1 1 d . A 1 H19A H 0.4534 1.3445 0.3963 0.090 Uiso 1 1 calc R A 1 H19B H 0.5360 1.4124 0.3311 0.090 Uiso 1 1 calc R A 1 H19C H 0.6229 1.3842 0.4282 0.090 Uiso 1 1 calc R A 1 C20 C 0.6946(7) 1.0012(6) 0.1512(4) 0.0412(15) Uani 1 1 d . A 1 C21 C 0.9012(10) 0.9964(11) 0.1341(6) 0.083(3) Uani 1 1 d . A 1 H21A H 0.8457 0.9543 0.0697 0.125 Uiso 1 1 calc R A 1 H21B H 0.9780 0.9701 0.1632 0.125 Uiso 1 1 calc R A 1 H21C H 0.9427 1.0801 0.1328 0.125 Uiso 1 1 calc R A 1 C22 C 0.1939(6) 0.8700(6) 0.1044(4) 0.0352(13) Uani 1 1 d . A 1 H22A H 0.1162 0.8510 0.1290 0.053 Uiso 1 1 calc R A 1 H22B H 0.1748 0.8035 0.0595 0.053 Uiso 1 1 calc R A 1 H22C H 0.1999 0.9379 0.0726 0.053 Uiso 1 1 calc R A 1 Cl1 Cl 0.24035(19) 0.26077(14) 0.11734(13) 0.0597(6) Uani 1 1 d G B 1 O9 O 0.1558(3) 0.2981(3) 0.04401(16) 0.101(3) Uani 1 1 d G B 1 O10 O 0.2140(5) 0.1440(2) 0.09003(17) 0.145(4) Uani 1 1 d G B 1 O11 O 0.3856(2) 0.3309(3) 0.13750(14) 0.091(2) Uani 1 1 d G B 1 O12 O 0.20601(16) 0.27005(16) 0.19784(12) 0.133(4) Uani 1 1 d G B 1 Cl2A Cl 0.2690(3) 0.3204(3) 0.5521(3) 0.075(2) Uani 0.500(9) 1 d PG C 1 O13A O 0.1383(4) 0.3351(5) 0.5318(3) 0.168(6) Uani 0.500(9) 1 d PG C 1 O14A O 0.3558(4) 0.3997(3) 0.5093(3) 0.168(6) Uani 0.500(9) 1 d PG C 1 O16A O 0.3423(4) 0.3428(4) 0.6510(4) 0.168(6) Uani 0.500(9) 1 d PG C 1 O15A O 0.2394(5) 0.2042(3) 0.5163(3) 0.168(6) Uani 0.500(9) 1 d PG C 1 Cl2B Cl 0.2416(3) 0.2954(3) 0.5077(3) 0.0668(18) Uani 0.500(9) 1 d PG C 2 O13B O 0.1656(4) 0.3595(4) 0.5224(3) 0.100(3) Uani 0.500(9) 1 d PG C 2 O14B O 0.3889(4) 0.3645(4) 0.5463(3) 0.100(3) Uani 0.500(9) 1 d PG C 2 O15B O 0.2104(5) 0.1965(3) 0.5512(4) 0.100(3) Uani 0.500(9) 1 d PG C 2 O16B O 0.2015(2) 0.2612(2) 0.4110(2) 0.100(3) Uani 0.500(9) 1 d PG C 2 Co1 Co 0.32636(9) 0.75833(7) 0.26045(6) 0.0434(4) Uani 1 1 d . A . N1 N 0.5446(6) 0.8727(5) 0.3399(4) 0.0457(14) Uani 1 1 d . . . N2 N 0.3311(5) 0.8967(4) 0.1828(3) 0.0301(10) Uani 1 1 d . . . N3 N 0.3811(6) 0.7064(4) 0.1523(4) 0.0375(12) Uani 1 1 d . . . N4 N 0.2384(6) 0.8448(6) 0.3258(4) 0.0524(16) Uani 1 1 d . . . O1 O 0.7510(5) 1.1534(5) 0.3265(3) 0.0551(13) Uani 1 1 d . . . H1A H 0.8036 1.1918 0.2982 0.083 Uiso 1 1 calc R A 1 O2 O 0.5703(5) 1.1521(4) 0.1897(3) 0.0401(10) Uani 1 1 d . . . H2 H 0.5427 1.1988 0.2099 0.060 Uiso 1 1 calc R A 1 O3 O 0.5672(6) 1.1810(5) 0.4628(3) 0.0542(13) Uani 1 1 d . . . O4 O 0.5106(5) 1.2450(4) 0.3258(3) 0.0453(11) Uani 1 1 d . . . O5 O 0.6697(4) 1.0375(4) 0.0796(3) 0.0379(10) Uani 1 1 d . . . O6 O 0.8073(5) 0.9734(6) 0.1884(3) 0.0604(15) Uani 1 1 d . . . O7 O 0.1114(6) 0.6350(5) 0.1902(5) 0.0717(16) Uani 1 1 d . . . O8 O 0.3452(7) 0.6345(6) 0.3449(5) 0.087(2) Uani 1 1 d . . . C98 C 0.7902(14) 0.6672(16) 0.1916(11) 0.155(7) Uani 1 1 d . . . H98A H 0.7678 0.7341 0.2030 0.232 Uiso 1 1 calc R . . H98B H 0.8226 0.6395 0.2510 0.232 Uiso 1 1 calc R . . H98C H 0.7044 0.6045 0.1473 0.232 Uiso 1 1 calc R . . O99 O 0.8927(11) 0.6989(11) 0.1558(8) 0.144 Uani 1 1 d . . . H101 H 0.562(7) 0.819(6) 0.397(5) 0.047(19) Uiso 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 C1 0.037(3) 0.048(3) 0.019(2) 0.011(2) 0.011(2) 0.021(3) C2 0.034(3) 0.046(4) 0.028(3) 0.012(3) 0.012(2) 0.016(3) C3 0.040(3) 0.039(3) 0.027(3) 0.014(2) 0.015(2) 0.007(3) C4 0.029(3) 0.047(3) 0.036(3) 0.024(3) 0.015(2) 0.020(3) C5 0.030(3) 0.031(3) 0.032(3) 0.014(2) 0.013(2) 0.016(2) C6 0.034(3) 0.066(4) 0.029(3) 0.025(3) 0.010(3) 0.019(3) C7 0.038(3) 0.062(4) 0.041(3) 0.031(3) 0.017(3) 0.027(3) C8 0.032(3) 0.032(3) 0.041(3) 0.015(2) 0.013(2) 0.017(2) C9 0.042(3) 0.038(3) 0.044(3) 0.017(3) 0.022(3) 0.024(3) C10 0.061(4) 0.051(4) 0.047(4) 0.017(3) 0.030(3) 0.033(3) C11 0.056(4) 0.035(3) 0.071(4) 0.020(3) 0.037(4) 0.026(3) C12 0.054(4) 0.042(4) 0.062(4) 0.025(3) 0.030(3) 0.028(3) C13 0.029(3) 0.062(4) 0.033(3) 0.013(3) 0.011(3) 0.014(3) C14 0.033(3) 0.076(5) 0.036(3) 0.004(3) 0.011(3) 0.022(3) C15 0.036(4) 0.095(7) 0.047(4) -0.003(4) 0.016(3) 0.014(4) C16 0.035(4) 0.150(11) 0.034(4) -0.006(5) 0.018(3) 0.007(5) C17 0.044(4) 0.093(7) 0.044(4) 0.022(4) 0.009(4) 0.000(4) C18 0.043(4) 0.049(4) 0.028(3) 0.005(3) 0.011(3) 0.010(3) C19 0.077(5) 0.051(4) 0.046(4) -0.011(3) 0.021(4) 0.020(4) C20 0.030(3) 0.058(4) 0.036(3) 0.015(3) 0.007(3) 0.023(3) C21 0.059(5) 0.159(11) 0.070(5) 0.057(6) 0.039(5) 0.069(6) C22 0.032(3) 0.044(3) 0.037(3) 0.008(3) 0.014(2) 0.021(3) Cl1 0.0622(12) 0.0396(10) 0.0771(13) 0.0233(9) 0.0227(10) 0.0215(9) O9 0.076(4) 0.072(4) 0.125(6) 0.027(4) -0.010(4) 0.035(4) O10 0.229(11) 0.057(4) 0.107(6) 0.010(4) -0.016(6) 0.078(6) O11 0.060(4) 0.121(6) 0.096(5) 0.070(4) 0.030(3) 0.034(4) O12 0.095(6) 0.234(12) 0.079(5) 0.034(6) 0.054(5) 0.057(7) Cl2A 0.065(3) 0.081(3) 0.110(5) 0.054(3) 0.047(3) 0.046(3) O13A 0.258(16) 0.095(8) 0.194(12) 0.051(8) 0.093(11) 0.105(9) O14A 0.258(16) 0.095(8) 0.194(12) 0.051(8) 0.093(11) 0.105(9) O16A 0.258(16) 0.095(8) 0.194(12) 0.051(8) 0.093(11) 0.105(9) O15A 0.258(16) 0.095(8) 0.194(12) 0.051(8) 0.093(11) 0.105(9) Cl2B 0.067(3) 0.107(4) 0.059(3) 0.034(3) 0.038(2) 0.055(3) O13B 0.079(5) 0.139(8) 0.112(6) 0.066(5) 0.043(4) 0.065(5) O14B 0.079(5) 0.139(8) 0.112(6) 0.066(5) 0.043(4) 0.065(5) O15B 0.079(5) 0.139(8) 0.112(6) 0.066(5) 0.043(4) 0.065(5) O16B 0.079(5) 0.139(8) 0.112(6) 0.066(5) 0.043(4) 0.065(5) Co1 0.0412(6) 0.0402(6) 0.0558(6) 0.0221(4) 0.0215(4) 0.0195(4) N1 0.045(3) 0.060(4) 0.050(3) 0.035(3) 0.026(3) 0.031(3) N2 0.027(2) 0.035(3) 0.031(2) 0.014(2) 0.0109(19) 0.014(2) N3 0.040(3) 0.035(3) 0.049(3) 0.021(2) 0.022(2) 0.023(2) N4 0.042(3) 0.066(4) 0.043(3) 0.026(3) 0.021(3) 0.008(3) O1 0.035(3) 0.071(4) 0.037(2) 0.012(2) 0.008(2) 0.002(2) O2 0.050(3) 0.038(2) 0.034(2) 0.0136(18) 0.0164(19) 0.016(2) O3 0.069(3) 0.067(3) 0.021(2) 0.009(2) 0.016(2) 0.022(3) O4 0.062(3) 0.043(3) 0.031(2) 0.0062(19) 0.016(2) 0.022(2) O5 0.035(2) 0.048(3) 0.038(2) 0.0213(19) 0.0177(18) 0.0199(19) O6 0.040(3) 0.116(5) 0.044(3) 0.032(3) 0.020(2) 0.046(3) O7 0.051(3) 0.058(3) 0.094(4) 0.007(3) 0.012(3) 0.022(3) O8 0.082(5) 0.079(4) 0.093(4) 0.048(4) 0.026(4) 0.026(4) C98 0.083(9) 0.220(18) 0.158(13) -0.067(12) 0.035(9) 0.071(10) O99 0.111 0.168 0.153 0.010 0.035 0.069 _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 N2 1.489(8) . ? C1 C13 1.508(8) . ? C1 C2 1.570(8) . ? C1 H1 1.0000 . ? C2 C6 1.522(8) . ? C2 C18 1.531(9) . ? C2 C3 1.539(8) . ? C3 O1 1.400(8) . ? C3 O2 1.419(7) . ? C3 C4 1.559(9) . ? C4 C20 1.531(8) . ? C4 C7 1.541(7) . ? C4 C5 1.563(8) . ? C5 N2 1.496(7) . ? C5 C8 1.537(8) . ? C5 H5 1.0000 . ? C6 N1 1.465(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.480(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.345(7) . ? C8 C9 1.370(8) . ? C9 C10 1.381(9) . ? C9 H9 0.9500 . ? C10 C11 1.397(9) . ? C10 H10 0.9500 . ? C11 C12 1.382(10) . ? C11 H11 0.9500 . ? C12 N3 1.334(8) . ? C12 H12 0.9500 . ? C13 N4 1.342(9) . ? C13 C14 1.379(10) . ? C14 C15 1.384(11) . ? C14 H14 0.9500 . ? C15 C16 1.339(15) . ? C15 H15 0.9500 . ? C16 C17 1.339(15) . ? C16 H16 0.9500 . ? C17 N4 1.384(10) . ? C17 H17 0.9500 . ? C18 O3 1.208(7) . ? C18 O4 1.330(8) . ? C19 O4 1.456(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O5 1.181(7) . ? C20 O6 1.337(7) . ? C21 O6 1.461(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N2 1.481(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? Cl1 O9 1.4049(10) . ? Cl1 O11 1.4049(10) . ? Cl1 O10 1.4074(10) . ? Cl1 O12 1.4074(10) . ? Cl2A O13A 1.4213(10) . ? Cl2A O16A 1.4213(11) . ? Cl2A O15A 1.4239(10) . ? Cl2A O14A 1.4239(11) . ? Cl2B O15B 1.4002(10) . ? Cl2B O13B 1.4002(10) . ? Cl2B O14B 1.4027(11) . ? Cl2B O16B 1.4027(10) . ? Co1 O8 2.064(6) . ? Co1 N3 2.089(5) . ? Co1 N4 2.096(7) . ? Co1 N2 2.115(4) . ? Co1 O7 2.136(6) . ? Co1 N1 2.151(6) . ? N1 H101 1.12(7) . ? O1 H1A 0.8400 . ? O2 H2 0.8400 . ? C98 O99 1.325(17) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? 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 N2 C1 C13 107.6(5) . . ? N2 C1 C2 113.0(5) . . ? C13 C1 C2 110.2(4) . . ? N2 C1 H1 108.7 . . ? C13 C1 H1 108.7 . . ? C2 C1 H1 108.7 . . ? C6 C2 C18 106.1(5) . . ? C6 C2 C3 110.5(5) . . ? C18 C2 C3 109.8(5) . . ? C6 C2 C1 112.7(5) . . ? C18 C2 C1 109.6(5) . . ? C3 C2 C1 108.2(4) . . ? O1 C3 O2 112.2(5) . . ? O1 C3 C2 105.3(4) . . ? O2 C3 C2 112.6(5) . . ? O1 C3 C4 112.6(5) . . ? O2 C3 C4 106.1(4) . . ? C2 C3 C4 108.0(5) . . ? C20 C4 C7 112.0(5) . . ? C20 C4 C3 110.2(5) . . ? C7 C4 C3 107.9(5) . . ? C20 C4 C5 106.2(5) . . ? C7 C4 C5 113.3(5) . . ? C3 C4 C5 107.2(5) . . ? N2 C5 C8 106.4(4) . . ? N2 C5 C4 114.4(4) . . ? C8 C5 C4 108.8(4) . . ? N2 C5 H5 109.0 . . ? C8 C5 H5 109.0 . . ? C4 C5 H5 109.0 . . ? N1 C6 C2 110.2(5) . . ? N1 C6 H6A 109.6 . . ? C2 C6 H6A 109.6 . . ? N1 C6 H6B 109.6 . . ? C2 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N1 C7 C4 110.5(5) . . ? N1 C7 H7A 109.5 . . ? C4 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C9 122.8(5) . . ? N3 C8 C5 115.5(5) . . ? C9 C8 C5 121.7(5) . . ? C8 C9 C10 118.5(6) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C9 C10 C11 119.0(6) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 119.2(6) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N3 C12 C11 121.3(6) . . ? N3 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? N4 C13 C14 121.4(6) . . ? N4 C13 C1 115.6(6) . . ? C14 C13 C1 122.8(6) . . ? C13 C14 C15 119.7(8) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 118.8(9) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 120.6(8) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 N4 122.5(9) . . ? C16 C17 H17 118.7 . . ? N4 C17 H17 118.7 . . ? O3 C18 O4 123.1(6) . . ? O3 C18 C2 124.6(6) . . ? O4 C18 C2 112.3(5) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? O5 C20 O6 123.7(6) . . ? O5 C20 C4 125.0(5) . . ? O6 C20 C4 111.3(5) . . ? O6 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? O6 C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? O9 Cl1 O11 109.3 . . ? O9 Cl1 O10 109.5 . . ? O11 Cl1 O10 109.5 . . ? O9 Cl1 O12 109.5 . . ? O11 Cl1 O12 109.5 . . ? O10 Cl1 O12 109.5 . . ? O13A Cl2A O16A 109.3 . . ? O13A Cl2A O15A 109.5 . . ? O16A Cl2A O15A 109.5 . . ? O13A Cl2A O14A 109.5 . . ? O16A Cl2A O14A 109.5 . . ? O15A Cl2A O14A 109.5 . . ? O15B Cl2B O13B 109.3 . . ? O15B Cl2B O14B 109.5 . . ? O13B Cl2B O14B 109.5 . . ? O15B Cl2B O16B 109.5 . . ? O13B Cl2B O16B 109.5 . . ? O14B Cl2B O16B 109.5 . . ? O8 Co1 N3 100.6(3) . . ? O8 Co1 N4 101.7(3) . . ? N3 Co1 N4 156.7(2) . . ? O8 Co1 N2 173.6(2) . . ? N3 Co1 N2 79.62(18) . . ? N4 Co1 N2 79.1(2) . . ? O8 Co1 O7 85.0(3) . . ? N3 Co1 O7 89.0(2) . . ? N4 Co1 O7 85.9(2) . . ? N2 Co1 O7 101.3(2) . . ? O8 Co1 N1 90.1(2) . . ? N3 Co1 N1 92.4(2) . . ? N4 Co1 N1 94.6(2) . . ? N2 Co1 N1 83.56(19) . . ? O7 Co1 N1 175.1(2) . . ? C6 N1 C7 110.0(5) . . ? C6 N1 Co1 113.0(4) . . ? C7 N1 Co1 115.0(4) . . ? C6 N1 H101 104(4) . . ? C7 N1 H101 118(4) . . ? Co1 N1 H101 96(4) . . ? C22 N2 C1 108.3(4) . . ? C22 N2 C5 107.0(4) . . ? C1 N2 C5 117.0(4) . . ? C22 N2 Co1 112.6(4) . . ? C1 N2 Co1 105.6(3) . . ? C5 N2 Co1 106.5(3) . . ? C12 N3 C8 119.3(6) . . ? C12 N3 Co1 126.3(4) . . ? C8 N3 Co1 113.9(4) . . ? C13 N4 C17 116.9(7) . . ? C13 N4 Co1 113.5(4) . . ? C17 N4 Co1 129.2(6) . . ? C18 O4 C19 117.2(5) . . ? C20 O6 C21 113.8(5) . . ? O99 C98 H98A 109.5 . . ? O99 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? O99 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? 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 N2 C1 C2 C6 -68.9(6) . . . . ? C13 C1 C2 C6 51.4(7) . . . . ? N2 C1 C2 C18 173.2(4) . . . . ? C13 C1 C2 C18 -66.5(6) . . . . ? N2 C1 C2 C3 53.6(6) . . . . ? C13 C1 C2 C3 173.9(5) . . . . ? C6 C2 C3 O1 -62.7(7) . . . . ? C18 C2 C3 O1 54.0(6) . . . . ? C1 C2 C3 O1 173.5(5) . . . . ? C6 C2 C3 O2 174.7(5) . . . . ? C18 C2 C3 O2 -68.6(6) . . . . ? C1 C2 C3 O2 50.9(7) . . . . ? C6 C2 C3 C4 57.9(6) . . . . ? C18 C2 C3 C4 174.6(5) . . . . ? C1 C2 C3 C4 -65.9(6) . . . . ? O1 C3 C4 C20 -64.3(6) . . . . ? O2 C3 C4 C20 58.8(6) . . . . ? C2 C3 C4 C20 179.8(4) . . . . ? O1 C3 C4 C7 58.3(6) . . . . ? O2 C3 C4 C7 -178.6(5) . . . . ? C2 C3 C4 C7 -57.6(6) . . . . ? O1 C3 C4 C5 -179.4(4) . . . . ? O2 C3 C4 C5 -56.3(6) . . . . ? C2 C3 C4 C5 64.7(5) . . . . ? C20 C4 C5 N2 -169.9(5) . . . . ? C7 C4 C5 N2 66.7(6) . . . . ? C3 C4 C5 N2 -52.2(5) . . . . ? C20 C4 C5 C8 71.2(5) . . . . ? C7 C4 C5 C8 -52.1(6) . . . . ? C3 C4 C5 C8 -171.0(4) . . . . ? C18 C2 C6 N1 -178.6(5) . . . . ? C3 C2 C6 N1 -59.7(7) . . . . ? C1 C2 C6 N1 61.5(6) . . . . ? C20 C4 C7 N1 -177.9(6) . . . . ? C3 C4 C7 N1 60.7(7) . . . . ? C5 C4 C7 N1 -57.8(7) . . . . ? N2 C5 C8 N3 -38.4(6) . . . . ? C4 C5 C8 N3 85.3(6) . . . . ? N2 C5 C8 C9 145.3(5) . . . . ? C4 C5 C8 C9 -91.0(6) . . . . ? N3 C8 C9 C10 -0.5(9) . . . . ? C5 C8 C9 C10 175.5(6) . . . . ? C8 C9 C10 C11 0.0(10) . . . . ? C9 C10 C11 C12 0.6(11) . . . . ? C10 C11 C12 N3 -0.8(11) . . . . ? N2 C1 C13 N4 37.5(7) . . . . ? C2 C1 C13 N4 -86.0(7) . . . . ? N2 C1 C13 C14 -146.7(6) . . . . ? C2 C1 C13 C14 89.8(7) . . . . ? N4 C13 C14 C15 -1.6(10) . . . . ? C1 C13 C14 C15 -177.1(6) . . . . ? C13 C14 C15 C16 -0.2(10) . . . . ? C14 C15 C16 C17 1.4(12) . . . . ? C15 C16 C17 N4 -0.9(12) . . . . ? C6 C2 C18 O3 -5.9(9) . . . . ? C3 C2 C18 O3 -125.3(7) . . . . ? C1 C2 C18 O3 116.0(7) . . . . ? C6 C2 C18 O4 176.5(5) . . . . ? C3 C2 C18 O4 57.1(7) . . . . ? C1 C2 C18 O4 -61.6(7) . . . . ? C7 C4 C20 O5 166.2(7) . . . . ? C3 C4 C20 O5 -73.7(8) . . . . ? C5 C4 C20 O5 42.1(8) . . . . ? C7 C4 C20 O6 -10.8(8) . . . . ? C3 C4 C20 O6 109.3(6) . . . . ? C5 C4 C20 O6 -135.0(6) . . . . ? C2 C6 N1 C7 61.0(6) . . . . ? C2 C6 N1 Co1 -69.0(5) . . . . ? C4 C7 N1 C6 -62.5(7) . . . . ? C4 C7 N1 Co1 66.4(6) . . . . ? O8 Co1 N1 C6 -115.9(4) . . . . ? N3 Co1 N1 C6 143.5(4) . . . . ? N4 Co1 N1 C6 -14.2(4) . . . . ? N2 Co1 N1 C6 64.3(4) . . . . ? O7 Co1 N1 C6 -109(3) . . . . ? O8 Co1 N1 C7 116.7(5) . . . . ? N3 Co1 N1 C7 16.1(4) . . . . ? N4 Co1 N1 C7 -141.6(4) . . . . ? N2 Co1 N1 C7 -63.1(4) . . . . ? O7 Co1 N1 C7 123(3) . . . . ? C13 C1 N2 C22 75.1(5) . . . . ? C2 C1 N2 C22 -163.1(5) . . . . ? C13 C1 N2 C5 -164.0(4) . . . . ? C2 C1 N2 C5 -42.2(6) . . . . ? C13 C1 N2 Co1 -45.7(5) . . . . ? C2 C1 N2 Co1 76.1(5) . . . . ? C8 C5 N2 C22 -76.0(5) . . . . ? C4 C5 N2 C22 163.8(5) . . . . ? C8 C5 N2 C1 162.5(4) . . . . ? C4 C5 N2 C1 42.3(6) . . . . ? C8 C5 N2 Co1 44.7(4) . . . . ? C4 C5 N2 Co1 -75.5(5) . . . . ? O8 Co1 N2 C22 178(2) . . . . ? N3 Co1 N2 C22 85.3(4) . . . . ? N4 Co1 N2 C22 -85.1(4) . . . . ? O7 Co1 N2 C22 -1.6(4) . . . . ? N1 Co1 N2 C22 179.0(4) . . . . ? O8 Co1 N2 C1 -64(2) . . . . ? N3 Co1 N2 C1 -156.7(4) . . . . ? N4 Co1 N2 C1 32.9(3) . . . . ? O7 Co1 N2 C1 116.4(4) . . . . ? N1 Co1 N2 C1 -63.1(4) . . . . ? O8 Co1 N2 C5 61(2) . . . . ? N3 Co1 N2 C5 -31.7(3) . . . . ? N4 Co1 N2 C5 157.9(4) . . . . ? O7 Co1 N2 C5 -118.6(4) . . . . ? N1 Co1 N2 C5 62.0(3) . . . . ? C11 C12 N3 C8 0.3(10) . . . . ? C11 C12 N3 Co1 171.7(5) . . . . ? C9 C8 N3 C12 0.4(9) . . . . ? C5 C8 N3 C12 -175.9(5) . . . . ? C9 C8 N3 Co1 -172.1(5) . . . . ? C5 C8 N3 Co1 11.7(6) . . . . ? O8 Co1 N3 C12 26.2(6) . . . . ? N4 Co1 N3 C12 -135.8(6) . . . . ? N2 Co1 N3 C12 -160.2(6) . . . . ? O7 Co1 N3 C12 -58.5(6) . . . . ? N1 Co1 N3 C12 116.8(6) . . . . ? O8 Co1 N3 C8 -162.0(4) . . . . ? N4 Co1 N3 C8 36.0(8) . . . . ? N2 Co1 N3 C8 11.6(4) . . . . ? O7 Co1 N3 C8 113.3(4) . . . . ? N1 Co1 N3 C8 -71.4(4) . . . . ? C14 C13 N4 C17 2.0(9) . . . . ? C1 C13 N4 C17 177.9(5) . . . . ? C14 C13 N4 Co1 175.2(5) . . . . ? C1 C13 N4 Co1 -8.9(7) . . . . ? C16 C17 N4 C13 -0.8(10) . . . . ? C16 C17 N4 Co1 -172.7(6) . . . . ? O8 Co1 N4 C13 159.5(5) . . . . ? N3 Co1 N4 C13 -38.5(8) . . . . ? N2 Co1 N4 C13 -14.0(4) . . . . ? O7 Co1 N4 C13 -116.4(5) . . . . ? N1 Co1 N4 C13 68.5(5) . . . . ? O8 Co1 N4 C17 -28.3(6) . . . . ? N3 Co1 N4 C17 133.6(6) . . . . ? N2 Co1 N4 C17 158.1(6) . . . . ? O7 Co1 N4 C17 55.7(6) . . . . ? N1 Co1 N4 C17 -119.4(6) . . . . ? O3 C18 O4 C19 4.9(10) . . . . ? C2 C18 O4 C19 -177.5(6) . . . . ? O5 C20 O6 C21 2.3(11) . . . . ? C4 C20 O6 C21 179.4(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.843 _refine_diff_density_min -1.450 _refine_diff_density_rms 0.147 # 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 0.000 0.500 0.288 262.1 58.1 _platon_squeeze_details ; ? ; _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'