#Supplementary Material (ESI) for Chemical Communications #This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 _publ_requested_journal CrystEngComm loop_ _publ_author_name 'Curtis Berlinguette' _publ_contact_author_name 'Curtis Berlinguette' _publ_contact_author_address ; ; _publ_contact_author_email cberling@ucalgary.ca # Attachment '- shelxl.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 804604' #TrackingRef '- shelxl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; aqua(2,6-(bis(bis-2-pyridyl0methoxymethane)pyridine)cobalt(II) percloro ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H27 Co N5 O3, 2(Cl O4)' _chemical_formula_sum 'C29 H27 Cl2 Co N5 O11' _chemical_formula_weight 751.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5935(3) _cell_length_b 12.7118(6) _cell_length_c 19.2504(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.663(2) _cell_angle_gamma 90.00 _cell_volume 3075.43(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 27.49 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9386 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details 'SORTAV: (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9892 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6977 _reflns_number_gt 5940 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0105P)^2^+6.5741P] 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 6977 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _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 0.24969(3) 0.21928(3) 0.981030(17) 0.01993(9) Uani 1 1 d . . . Cl1 Cl 0.13410(6) 0.57484(5) 0.87192(3) 0.03014(15) Uani 1 1 d . . . Cl2 Cl 0.37052(6) 0.55185(5) 1.12602(4) 0.03293(16) Uani 1 1 d . . . O2 O 0.11691(15) 0.01836(14) 0.79995(9) 0.0273(4) Uani 1 1 d . . . N4 N 0.40260(17) 0.20825(17) 1.03387(11) 0.0229(4) Uani 1 1 d . . . O1 O 0.24812(17) 0.37813(15) 0.99032(11) 0.0304(4) Uani 1 1 d . . . O3 O 0.37100(15) -0.02516(14) 1.14135(9) 0.0278(4) Uani 1 1 d . . . N5 N 0.19893(16) 0.18959(16) 1.08711(10) 0.0211(4) Uani 1 1 d . . . N3 N 0.25195(16) 0.05547(16) 0.97175(10) 0.0207(4) Uani 1 1 d . . . N2 N 0.29590(16) 0.22090(16) 0.87632(10) 0.0219(4) Uani 1 1 d . . . N1 N 0.09409(17) 0.22354(17) 0.92602(10) 0.0225(4) Uani 1 1 d . . . C14 C 0.25112(19) 0.15138(19) 0.83010(12) 0.0208(5) Uani 1 1 d . . . C13 C 0.2785(2) 0.1485(2) 0.76161(13) 0.0244(5) Uani 1 1 d . . . H13 H 0.2448 0.1003 0.7296 0.029 Uiso 1 1 calc R . . C16 C -0.0245(2) 0.1596(2) 0.83248(13) 0.0256(5) Uani 1 1 d . . . H16 H -0.0389 0.1104 0.7959 0.031 Uiso 1 1 calc R . . C20 C 0.1203(2) 0.2438(2) 1.11404(13) 0.0249(5) Uani 1 1 d . . . H20 H 0.0914 0.3024 1.0888 0.030 Uiso 1 1 calc R . . O10 O 0.27877(17) 0.48322(18) 1.11310(10) 0.0392(5) Uani 1 1 d . . . C25 C 0.4211(2) 0.13276(19) 1.08186(13) 0.0224(5) Uani 1 1 d . . . C23 C 0.2044(2) 0.0777(2) 1.18806(13) 0.0263(5) Uani 1 1 d . . . H23 H 0.2352 0.0195 1.2129 0.032 Uiso 1 1 calc R . . C19 C 0.0218(2) 0.2983(2) 0.93805(13) 0.0259(5) Uani 1 1 d . . . H19 H 0.0377 0.3471 0.9747 0.031 Uiso 1 1 calc R . . C4 C 0.2488(2) -0.1076(2) 1.03249(14) 0.0283(6) Uani 1 1 d . . . H4 H 0.2714 -0.1489 1.0718 0.034 Uiso 1 1 calc R . . C22 C 0.1207(2) 0.1340(2) 1.21399(14) 0.0287(6) Uani 1 1 d . . . H22 H 0.0927 0.1142 1.2568 0.034 Uiso 1 1 calc R . . C18 C -0.0744(2) 0.3076(2) 0.89963(14) 0.0301(6) Uani 1 1 d . . . H18 H -0.1229 0.3622 0.9092 0.036 Uiso 1 1 calc R . . C5 C 0.2802(2) -0.00320(19) 1.02786(13) 0.0222(5) Uani 1 1 d . . . C1 C 0.19186(19) 0.01253(19) 0.91854(12) 0.0215(5) Uani 1 1 d . . . C3 C 0.1843(2) -0.1503(2) 0.97926(14) 0.0320(6) Uani 1 1 d . . . H3 H 0.1610 -0.2212 0.9819 0.038 Uiso 1 1 calc R . . C15 C 0.0711(2) 0.1566(2) 0.87252(12) 0.0224(5) Uani 1 1 d . . . C21 C 0.0790(2) 0.2186(2) 1.17685(13) 0.0272(5) Uani 1 1 d . . . H21 H 0.0229 0.2590 1.1940 0.033 Uiso 1 1 calc R . . C29 C 0.4746(2) 0.2855(2) 1.02895(14) 0.0284(6) Uani 1 1 d . . . H29 H 0.4611 0.3386 0.9948 0.034 Uiso 1 1 calc R . . C17 C -0.0982(2) 0.2358(2) 0.84707(14) 0.0285(6) Uani 1 1 d . . . H17 H -0.1648 0.2388 0.8211 0.034 Uiso 1 1 calc R . . C6 C 0.1609(2) 0.0814(2) 0.85492(12) 0.0219(5) Uani 1 1 d . . . C2 C 0.1539(2) -0.0896(2) 0.92216(14) 0.0290(6) Uani 1 1 d . . . H2 H 0.1075 -0.1173 0.8858 0.035 Uiso 1 1 calc R . . C7 C 0.3335(2) 0.05130(19) 1.09236(13) 0.0220(5) Uani 1 1 d . . . C12 C 0.3556(2) 0.2168(2) 0.74030(13) 0.0271(5) Uani 1 1 d . . . H12 H 0.3776 0.2136 0.6941 0.033 Uiso 1 1 calc R . . C24 C 0.24149(19) 0.10875(19) 1.12501(12) 0.0213(5) Uani 1 1 d . . . C11 C 0.4001(2) 0.2892(2) 0.78655(14) 0.0277(5) Uani 1 1 d . . . H11 H 0.4522 0.3376 0.7727 0.033 Uiso 1 1 calc R . . C10 C 0.3671(2) 0.2897(2) 0.85393(13) 0.0245(5) Uani 1 1 d . . . H10 H 0.3961 0.3410 0.8856 0.029 Uiso 1 1 calc R . . O5 O 0.0378(2) 0.5420(2) 0.83551(14) 0.0560(7) Uani 1 1 d . . . O6 O 0.2113(2) 0.49125(19) 0.86978(12) 0.0522(6) Uani 1 1 d . . . C9 C 0.4549(3) -0.0935(2) 1.12021(19) 0.0375(7) Uani 1 1 d . . . O9 O 0.4431(2) 0.5359(2) 1.07413(16) 0.0708(9) Uani 1 1 d . . . O4 O 0.1730(2) 0.6669(2) 0.83927(15) 0.0566(7) Uani 1 1 d . . . C26 C 0.5127(2) 0.1352(2) 1.12725(14) 0.0278(6) Uani 1 1 d . . . H26 H 0.5243 0.0822 1.1617 0.033 Uiso 1 1 calc R . . C28 C 0.5675(2) 0.2912(2) 1.07132(16) 0.0345(6) Uani 1 1 d . . . H28 H 0.6173 0.3462 1.0658 0.041 Uiso 1 1 calc R . . C8 C 0.1808(3) -0.0628(2) 0.77202(15) 0.0327(6) Uani 1 1 d . . . O7 O 0.1152(2) 0.5969(2) 0.94261(12) 0.0599(7) Uani 1 1 d . . . C27 C 0.5860(2) 0.2153(2) 1.12151(15) 0.0332(6) Uani 1 1 d . . . H27 H 0.6484 0.2178 1.1519 0.040 Uiso 1 1 calc R . . O11 O 0.4212(2) 0.5237(3) 1.19186(15) 0.0756(10) Uani 1 1 d . . . O8 O 0.3372(2) 0.6568(2) 1.1274(2) 0.0831(11) Uani 1 1 d . . . H1B H 0.231(3) 0.416(3) 0.956(2) 0.061(12) Uiso 1 1 d . . . H1A H 0.262(3) 0.408(3) 1.026(2) 0.050(11) Uiso 1 1 d . . . H8A H 0.172(2) -0.055(2) 0.7215(15) 0.023(7) Uiso 1 1 d . . . H8B H 0.154(2) -0.129(2) 0.7866(15) 0.027(8) Uiso 1 1 d . . . H8C H 0.258(3) -0.057(3) 0.7884(16) 0.035(8) Uiso 1 1 d . . . H9C H 0.512(3) -0.085(3) 1.1558(19) 0.052(10) Uiso 1 1 d . . . H9A H 0.477(3) -0.072(3) 1.074(2) 0.069(13) Uiso 1 1 d . . . H9B H 0.429(3) -0.160(3) 1.120(2) 0.059(12) 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 0.02155(17) 0.01827(16) 0.01979(16) -0.00028(12) -0.00008(12) 0.00030(13) Cl1 0.0351(4) 0.0243(3) 0.0304(3) -0.0003(2) -0.0026(3) 0.0051(3) Cl2 0.0310(3) 0.0307(3) 0.0376(4) -0.0026(3) 0.0064(3) -0.0089(3) O2 0.0304(10) 0.0262(9) 0.0247(9) -0.0068(7) -0.0019(7) -0.0029(8) N4 0.0226(11) 0.0222(10) 0.0239(10) 0.0004(8) 0.0009(8) 0.0003(8) O1 0.0441(12) 0.0206(9) 0.0254(10) 0.0005(8) -0.0068(9) 0.0013(8) O3 0.0295(10) 0.0254(9) 0.0282(9) 0.0060(7) -0.0002(8) 0.0075(8) N5 0.0214(10) 0.0221(10) 0.0197(10) 0.0002(8) 0.0005(8) 0.0003(8) N3 0.0210(10) 0.0201(10) 0.0211(10) -0.0013(8) 0.0016(8) 0.0009(8) N2 0.0218(10) 0.0229(10) 0.0210(10) 0.0001(8) 0.0010(8) 0.0006(8) N1 0.0217(10) 0.0248(11) 0.0210(10) 0.0016(8) 0.0016(8) 0.0009(8) C14 0.0200(12) 0.0194(11) 0.0230(12) 0.0013(9) 0.0019(9) 0.0029(9) C13 0.0290(13) 0.0212(12) 0.0229(12) 0.0000(9) -0.0004(10) 0.0023(10) C16 0.0237(13) 0.0292(13) 0.0238(12) 0.0029(10) -0.0005(10) -0.0047(10) C20 0.0249(13) 0.0273(13) 0.0222(12) -0.0010(10) -0.0001(10) 0.0043(10) O10 0.0408(12) 0.0461(13) 0.0313(10) -0.0063(9) 0.0065(9) -0.0207(10) C25 0.0215(12) 0.0219(12) 0.0238(12) -0.0011(9) 0.0027(9) 0.0050(10) C23 0.0280(13) 0.0248(13) 0.0261(13) 0.0020(10) 0.0007(10) -0.0027(10) C19 0.0279(13) 0.0272(13) 0.0229(12) 0.0000(10) 0.0034(10) 0.0009(11) C4 0.0367(15) 0.0210(12) 0.0272(13) 0.0014(10) 0.0029(11) -0.0023(11) C22 0.0293(14) 0.0323(14) 0.0249(13) 0.0008(11) 0.0042(10) -0.0040(11) C18 0.0271(14) 0.0340(15) 0.0294(13) 0.0040(11) 0.0045(11) 0.0044(11) C5 0.0218(12) 0.0214(12) 0.0238(12) 0.0005(9) 0.0036(9) 0.0011(9) C1 0.0209(12) 0.0226(12) 0.0213(11) -0.0006(9) 0.0036(9) -0.0001(9) C3 0.0445(17) 0.0210(13) 0.0311(14) -0.0028(10) 0.0066(12) -0.0088(12) C15 0.0215(12) 0.0262(12) 0.0199(11) 0.0007(9) 0.0029(9) -0.0019(10) C21 0.0236(13) 0.0315(14) 0.0267(13) -0.0045(11) 0.0028(10) 0.0018(11) C29 0.0272(13) 0.0284(13) 0.0296(13) 0.0025(11) 0.0008(10) -0.0045(11) C17 0.0206(12) 0.0367(15) 0.0280(13) 0.0089(11) -0.0003(10) 0.0001(11) C6 0.0230(12) 0.0218(12) 0.0206(11) -0.0019(9) -0.0009(9) -0.0032(10) C2 0.0366(15) 0.0263(13) 0.0241(12) -0.0027(10) 0.0032(11) -0.0081(11) C7 0.0236(12) 0.0199(11) 0.0224(12) 0.0035(9) -0.0001(9) 0.0029(10) C12 0.0295(14) 0.0283(13) 0.0237(12) 0.0050(10) 0.0037(10) 0.0032(11) C24 0.0211(12) 0.0207(12) 0.0217(11) -0.0025(9) -0.0015(9) -0.0010(9) C11 0.0253(13) 0.0284(13) 0.0296(13) 0.0071(11) 0.0032(10) -0.0011(11) C10 0.0244(12) 0.0238(12) 0.0249(12) 0.0030(10) -0.0010(10) -0.0008(10) O5 0.0535(15) 0.0447(14) 0.0664(16) -0.0003(12) -0.0225(13) -0.0073(12) O6 0.0668(17) 0.0477(14) 0.0430(13) 0.0109(11) 0.0110(12) 0.0304(13) C9 0.0335(16) 0.0252(15) 0.053(2) 0.0032(13) -0.0029(14) 0.0122(12) O9 0.0689(19) 0.0635(18) 0.086(2) -0.0150(15) 0.0496(16) -0.0217(15) O4 0.0471(15) 0.0410(14) 0.0810(19) 0.0246(13) -0.0020(13) -0.0022(11) C26 0.0258(13) 0.0269(13) 0.0304(13) 0.0000(11) -0.0014(10) 0.0073(11) C28 0.0259(14) 0.0353(15) 0.0418(16) 0.0008(13) -0.0007(12) -0.0066(12) C8 0.0480(19) 0.0246(14) 0.0259(14) -0.0056(11) 0.0058(12) -0.0013(13) O7 0.086(2) 0.0563(16) 0.0377(13) -0.0145(11) 0.0059(13) 0.0137(15) C27 0.0228(13) 0.0359(15) 0.0398(15) -0.0003(12) -0.0068(11) -0.0003(12) O11 0.0705(19) 0.093(2) 0.0598(17) 0.0223(16) -0.0210(14) -0.0429(18) O8 0.0500(17) 0.0315(14) 0.167(3) -0.0141(17) -0.0010(19) 0.0025(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.027(2) . ? Co1 N3 2.090(2) . ? Co1 N4 2.124(2) . ? Co1 N2 2.134(2) . ? Co1 N1 2.168(2) . ? Co1 N5 2.211(2) . ? Cl1 O5 1.423(2) . ? Cl1 O7 1.424(2) . ? Cl1 O4 1.429(2) . ? Cl1 O6 1.442(2) . ? Cl2 O8 1.399(3) . ? Cl2 O9 1.411(3) . ? Cl2 O11 1.428(3) . ? Cl2 O10 1.456(2) . ? O2 C6 1.412(3) . ? O2 C8 1.435(3) . ? N4 C25 1.342(3) . ? N4 C29 1.344(3) . ? O1 H1B 0.84(4) . ? O1 H1A 0.79(4) . ? O3 C7 1.414(3) . ? O3 C9 1.446(3) . ? N5 C20 1.337(3) . ? N5 C24 1.351(3) . ? N3 C5 1.342(3) . ? N3 C1 1.349(3) . ? N2 C10 1.343(3) . ? N2 C14 1.352(3) . ? N1 C19 1.346(3) . ? N1 C15 1.353(3) . ? C14 C13 1.385(3) . ? C14 C6 1.543(3) . ? C13 C12 1.383(4) . ? C13 H13 0.9500 . ? C16 C17 1.383(4) . ? C16 C15 1.387(3) . ? C16 H16 0.9500 . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C25 C26 1.402(3) . ? C25 C7 1.536(3) . ? C23 C24 1.386(3) . ? C23 C22 1.393(4) . ? C23 H23 0.9500 . ? C19 C18 1.384(4) . ? C19 H19 0.9500 . ? C4 C3 1.378(4) . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C22 C21 1.377(4) . ? C22 H22 0.9500 . ? C18 C17 1.382(4) . ? C18 H18 0.9500 . ? C5 C7 1.538(3) . ? C1 C2 1.387(4) . ? C1 C6 1.536(3) . ? C3 C2 1.377(4) . ? C3 H3 0.9500 . ? C15 C6 1.535(3) . ? C21 H21 0.9500 . ? C29 C28 1.385(4) . ? C29 H29 0.9500 . ? C17 H17 0.9500 . ? C2 H2 0.9500 . ? C7 C24 1.538(3) . ? C12 C11 1.375(4) . ? C12 H12 0.9500 . ? C11 C10 1.388(4) . ? C11 H11 0.9500 . ? C10 H10 0.9500 . ? C9 H9C 0.97(4) . ? C9 H9A 0.99(4) . ? C9 H9B 0.91(4) . ? C26 C27 1.383(4) . ? C26 H26 0.9500 . ? C28 C27 1.375(4) . ? C28 H28 0.9500 . ? C8 H8A 0.98(3) . ? C8 H8B 0.95(3) . ? C8 H8C 1.00(3) . ? C27 H27 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N3 179.73(9) . . ? O1 Co1 N4 92.13(8) . . ? N3 Co1 N4 87.61(8) . . ? O1 Co1 N2 94.50(9) . . ? N3 Co1 N2 85.58(8) . . ? N4 Co1 N2 99.17(8) . . ? O1 Co1 N1 90.26(8) . . ? N3 Co1 N1 90.00(8) . . ? N4 Co1 N1 177.58(8) . . ? N2 Co1 N1 80.26(8) . . ? O1 Co1 N5 94.79(8) . . ? N3 Co1 N5 85.14(8) . . ? N4 Co1 N5 81.56(8) . . ? N2 Co1 N5 170.65(8) . . ? N1 Co1 N5 98.62(8) . . ? O5 Cl1 O7 109.83(18) . . ? O5 Cl1 O4 109.18(15) . . ? O7 Cl1 O4 110.00(17) . . ? O5 Cl1 O6 108.93(16) . . ? O7 Cl1 O6 109.03(15) . . ? O4 Cl1 O6 109.85(16) . . ? O8 Cl2 O9 111.1(2) . . ? O8 Cl2 O11 109.9(2) . . ? O9 Cl2 O11 108.6(2) . . ? O8 Cl2 O10 109.79(16) . . ? O9 Cl2 O10 109.59(15) . . ? O11 Cl2 O10 107.84(15) . . ? C6 O2 C8 119.1(2) . . ? C25 N4 C29 118.9(2) . . ? C25 N4 Co1 119.28(17) . . ? C29 N4 Co1 120.86(17) . . ? Co1 O1 H1B 120(3) . . ? Co1 O1 H1A 123(3) . . ? H1B O1 H1A 116(4) . . ? C7 O3 C9 116.3(2) . . ? C20 N5 C24 117.4(2) . . ? C20 N5 Co1 122.34(16) . . ? C24 N5 Co1 120.03(16) . . ? C5 N3 C1 119.5(2) . . ? C5 N3 Co1 119.30(16) . . ? C1 N3 Co1 117.24(16) . . ? C10 N2 C14 118.3(2) . . ? C10 N2 Co1 122.51(17) . . ? C14 N2 Co1 119.22(17) . . ? C19 N1 C15 117.4(2) . . ? C19 N1 Co1 122.24(17) . . ? C15 N1 Co1 119.95(17) . . ? N2 C14 C13 121.7(2) . . ? N2 C14 C6 117.2(2) . . ? C13 C14 C6 120.9(2) . . ? C12 C13 C14 119.2(2) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C17 C16 C15 118.4(2) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? N5 C20 C21 123.2(2) . . ? N5 C20 H20 118.4 . . ? C21 C20 H20 118.4 . . ? N4 C25 C26 120.9(2) . . ? N4 C25 C7 118.6(2) . . ? C26 C25 C7 120.1(2) . . ? C24 C23 C22 118.2(2) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? N1 C19 C18 123.1(2) . . ? N1 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C3 C4 C5 119.0(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C21 C22 C23 119.2(2) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C17 C18 C19 118.5(3) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? N3 C5 C4 121.4(2) . . ? N3 C5 C7 118.6(2) . . ? C4 C5 C7 119.3(2) . . ? N3 C1 C2 121.3(2) . . ? N3 C1 C6 118.4(2) . . ? C2 C1 C6 120.2(2) . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? N1 C15 C16 122.8(2) . . ? N1 C15 C6 115.7(2) . . ? C16 C15 C6 121.3(2) . . ? C22 C21 C20 118.8(2) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N4 C29 C28 123.0(3) . . ? N4 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C18 C17 C16 119.7(2) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? O2 C6 C15 105.04(19) . . ? O2 C6 C1 109.9(2) . . ? C15 C6 C1 109.4(2) . . ? O2 C6 C14 110.9(2) . . ? C15 C6 C14 106.1(2) . . ? C1 C6 C14 114.9(2) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? O3 C7 C25 109.8(2) . . ? O3 C7 C24 106.38(19) . . ? C25 C7 C24 107.5(2) . . ? O3 C7 C5 109.8(2) . . ? C25 C7 C5 118.5(2) . . ? C24 C7 C5 104.02(19) . . ? C11 C12 C13 119.5(2) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? N5 C24 C23 123.1(2) . . ? N5 C24 C7 115.1(2) . . ? C23 C24 C7 121.8(2) . . ? C12 C11 C10 118.3(2) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? N2 C10 C11 122.9(2) . . ? N2 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? O3 C9 H9C 105(2) . . ? O3 C9 H9A 110(2) . . ? H9C C9 H9A 112(3) . . ? O3 C9 H9B 107(3) . . ? H9C C9 H9B 111(3) . . ? H9A C9 H9B 111(3) . . ? C27 C26 C25 119.5(3) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C27 C28 C29 118.4(3) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? O2 C8 H8A 105.8(17) . . ? O2 C8 H8B 107.9(18) . . ? H8A C8 H8B 112(2) . . ? O2 C8 H8C 112.8(19) . . ? H8A C8 H8C 110(2) . . ? H8B C8 H8C 109(3) . . ? C28 C27 C26 119.3(3) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O6 0.84(4) 1.92(4) 2.744(3) 170(4) . O1 H1A O10 0.79(4) 1.93(4) 2.721(3) 174(4) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.553 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.071