# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Liya Wang' _publ_contact_author_address ; ; _publ_contact_author_email gzliu@yahoo.com.cn loop_ _publ_author_name 'Xiaoling Li' 'Guangzhen Liu' 'Lingyun Xin' 'Liya Wang' data_a _database_code_depnum_ccdc_archive 'CCDC 880568' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Co2 N4 O10' _chemical_formula_weight 724.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.771(2) _cell_length_b 14.711(2) _cell_length_c 8.3852(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.485(2) _cell_angle_gamma 90.00 _cell_volume 1899.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4175 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.73 _exptl_crystal_description block _exptl_crystal_colour amaranth _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8016 _exptl_absorpt_correction_T_max 0.8438 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14211 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3533 _reflns_number_gt 2915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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 'Bruker SHELXTL' _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^)+(0.0556P)^2^+0.2170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3533 _refine_ls_number_parameters 209 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.285 _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 0.38970(2) 0.08276(2) 0.83167(4) 0.02357(14) Uani 1 1 d . . . O1 O 0.35476(12) 0.21783(12) 0.8574(2) 0.0328(5) Uani 1 1 d . . . O2 O 0.40607(12) 0.35944(12) 0.8657(2) 0.0337(5) Uani 1 1 d . . . O3 O 0.45189(11) 0.43016(11) 0.5726(2) 0.0262(4) Uani 1 1 d . . . O4 O 0.58261(11) 0.45303(11) 0.7320(2) 0.0300(4) Uani 1 1 d . . . O5 O 0.31367(13) 0.08868(13) 0.5833(2) 0.0391(5) Uani 1 1 d . . . H1W H 0.2718 0.1263 0.5700 0.059 Uiso 1 1 d R . . H2W H 0.3441 0.1114 0.5211 0.059 Uiso 1 1 d R . . N1 N 0.49320(13) 0.15422(13) 0.7610(2) 0.0247(5) Uani 1 1 d . . . N2 N 0.27541(14) 0.03362(15) 0.9033(3) 0.0307(5) Uani 1 1 d . . . C1 C 0.48099(15) 0.24476(16) 0.7542(3) 0.0221(5) Uani 1 1 d . . . C2 C 0.53517(16) 0.30221(16) 0.6900(3) 0.0231(5) Uani 1 1 d . . . C3 C 0.60546(16) 0.26388(18) 0.6416(3) 0.0269(6) Uani 1 1 d . . . H3 H 0.6437 0.3012 0.6017 0.032 Uiso 1 1 calc R . . C4 C 0.62042(17) 0.17111(18) 0.6513(3) 0.0282(6) Uani 1 1 d . . . C5 C 0.56109(17) 0.11853(17) 0.7108(3) 0.0279(6) Uani 1 1 d . . . H5A H 0.5688 0.0558 0.7161 0.033 Uiso 1 1 calc R . . C6 C 0.40834(16) 0.27797(17) 0.8312(3) 0.0240(6) Uani 1 1 d . . . C7 C 0.52047(16) 0.40319(16) 0.6638(3) 0.0230(5) Uani 1 1 d . . . C8 C 0.69617(19) 0.1265(2) 0.5991(5) 0.0504(8) Uani 1 1 d U . . H8A H 0.7063 0.0678 0.6528 0.060 Uiso 1 1 calc R . . H8B H 0.6800 0.1153 0.4825 0.060 Uiso 1 1 calc R . . C9 C 0.7779(2) 0.1773(3) 0.6335(7) 0.0840(10) Uani 1 1 d U . . H9A H 0.7721 0.2307 0.5663 0.126 Uiso 1 1 calc R . . H9B H 0.8236 0.1397 0.6102 0.126 Uiso 1 1 calc R . . H9C H 0.7918 0.1947 0.7465 0.126 Uiso 1 1 calc R . . C10 C 0.2558(2) 0.0640(2) 1.0405(4) 0.0427(7) Uani 1 1 d . . . H10 H 0.2952 0.1019 1.1080 0.051 Uiso 1 1 calc R . . C11 C 0.1798(2) 0.0420(3) 1.0870(4) 0.0536(9) Uani 1 1 d . . . H11 H 0.1689 0.0653 1.1839 0.064 Uiso 1 1 calc R . . C12 C 0.12006(19) -0.0137(2) 0.9920(4) 0.0477(8) Uani 1 1 d . . . C13 C 0.1426(2) -0.0484(3) 0.8545(5) 0.0622(10) Uani 1 1 d . . . H13 H 0.1058 -0.0893 0.7885 0.075 Uiso 1 1 calc R . . C14 C 0.2194(2) -0.0228(2) 0.8140(4) 0.0484(8) Uani 1 1 d . . . H14 H 0.2324 -0.0464 0.7192 0.058 Uiso 1 1 calc R . . C15 C 0.0343(2) -0.0344(3) 1.0351(5) 0.0654(11) Uani 1 1 d . . . H15A H 0.0419 -0.0354 1.1530 0.079 Uiso 1 1 calc R . . H15B H 0.0150 -0.0943 0.9941 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0225(2) 0.0175(2) 0.0335(2) 0.00210(13) 0.01202(15) 0.00023(13) O1 0.0307(10) 0.0224(9) 0.0515(12) 0.0032(8) 0.0230(9) 0.0018(8) O2 0.0477(12) 0.0203(10) 0.0393(11) -0.0015(8) 0.0228(9) 0.0019(8) O3 0.0257(10) 0.0236(9) 0.0314(10) 0.0025(7) 0.0105(8) 0.0020(7) O4 0.0296(10) 0.0191(9) 0.0403(11) 0.0017(8) 0.0052(8) -0.0040(8) O5 0.0368(11) 0.0467(13) 0.0370(11) 0.0084(9) 0.0152(9) -0.0006(9) N1 0.0271(11) 0.0183(10) 0.0310(12) 0.0002(9) 0.0115(9) 0.0009(9) N2 0.0246(11) 0.0320(12) 0.0379(13) 0.0016(10) 0.0118(10) -0.0003(10) C1 0.0235(13) 0.0184(12) 0.0253(13) 0.0009(10) 0.0069(10) -0.0013(10) C2 0.0262(13) 0.0201(12) 0.0236(12) -0.0007(10) 0.0068(10) -0.0012(10) C3 0.0233(13) 0.0231(14) 0.0372(15) 0.0025(11) 0.0132(11) -0.0037(10) C4 0.0271(14) 0.0258(14) 0.0337(15) -0.0023(11) 0.0111(11) 0.0010(11) C5 0.0293(14) 0.0174(12) 0.0392(16) 0.0019(11) 0.0123(12) 0.0033(11) C6 0.0294(14) 0.0214(14) 0.0235(13) 0.0030(10) 0.0105(10) 0.0036(10) C7 0.0263(13) 0.0209(12) 0.0256(13) -0.0003(10) 0.0141(11) -0.0015(10) C8 0.0345(15) 0.0454(17) 0.080(2) -0.0063(16) 0.0323(15) 0.0062(13) C9 0.0448(17) 0.063(2) 0.151(3) -0.013(2) 0.0364(19) 0.0043(16) C10 0.0317(16) 0.056(2) 0.0424(18) -0.0051(15) 0.0129(13) -0.0101(14) C11 0.0426(19) 0.077(3) 0.048(2) -0.0015(18) 0.0255(16) -0.0025(18) C12 0.0282(16) 0.053(2) 0.067(2) 0.0123(17) 0.0199(15) -0.0013(14) C13 0.0398(19) 0.066(2) 0.084(3) -0.018(2) 0.0208(19) -0.0263(18) C14 0.0386(17) 0.050(2) 0.062(2) -0.0140(16) 0.0237(15) -0.0146(15) C15 0.0380(19) 0.075(3) 0.092(3) 0.021(2) 0.0338(19) -0.0062(17) _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 O4 2.0539(17) 2_646 ? Co1 O3 2.0548(18) 4_566 ? Co1 O1 2.0855(18) . ? Co1 N1 2.130(2) . ? Co1 N2 2.145(2) . ? Co1 O5 2.168(2) . ? O1 C6 1.275(3) . ? O2 C6 1.235(3) . ? O3 C7 1.247(3) . ? O3 Co1 2.0548(18) 4_565 ? O4 C7 1.258(3) . ? O4 Co1 2.0539(17) 2_656 ? O5 H1W 0.8499 . ? O5 H2W 0.8500 . ? N1 C5 1.339(3) . ? N1 C1 1.345(3) . ? N2 C14 1.320(4) . ? N2 C10 1.332(4) . ? C1 C2 1.390(3) . ? C1 C6 1.513(3) . ? C2 C3 1.380(3) . ? C2 C7 1.512(3) . ? C3 C4 1.384(4) . ? C3 H3 0.9300 . ? C4 C5 1.388(4) . ? C4 C8 1.508(4) . ? C5 H5A 0.9300 . ? C8 C9 1.464(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.377(4) . ? C10 H10 0.9300 . ? C11 C12 1.367(5) . ? C11 H11 0.9300 . ? C12 C13 1.376(5) . ? C12 C15 1.505(4) . ? C13 C14 1.380(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C15 1.505(7) 3_557 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? 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 O4 Co1 O3 94.95(7) 2_646 4_566 ? O4 Co1 O1 171.08(7) 2_646 . ? O3 Co1 O1 93.85(7) 4_566 . ? O4 Co1 N1 99.64(7) 2_646 . ? O3 Co1 N1 95.02(7) 4_566 . ? O1 Co1 N1 78.12(7) . . ? O4 Co1 N2 89.90(8) 2_646 . ? O3 Co1 N2 86.85(8) 4_566 . ? O1 Co1 N2 92.03(8) . . ? N1 Co1 N2 170.06(8) . . ? O4 Co1 O5 83.82(7) 2_646 . ? O3 Co1 O5 174.35(7) 4_566 . ? O1 Co1 O5 87.56(7) . . ? N1 Co1 O5 90.63(8) . . ? N2 Co1 O5 87.63(8) . . ? C6 O1 Co1 116.34(16) . . ? C7 O3 Co1 137.75(16) . 4_565 ? C7 O4 Co1 127.75(16) . 2_656 ? Co1 O5 H1W 113.9 . . ? Co1 O5 H2W 109.7 . . ? H1W O5 H2W 101.0 . . ? C5 N1 C1 119.4(2) . . ? C5 N1 Co1 127.34(16) . . ? C1 N1 Co1 112.91(15) . . ? C14 N2 C10 116.7(3) . . ? C14 N2 Co1 123.5(2) . . ? C10 N2 Co1 119.67(19) . . ? N1 C1 C2 121.6(2) . . ? N1 C1 C6 114.6(2) . . ? C2 C1 C6 123.7(2) . . ? C3 C2 C1 117.7(2) . . ? C3 C2 C7 117.8(2) . . ? C1 C2 C7 124.4(2) . . ? C2 C3 C4 121.6(2) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C3 C4 C5 116.8(2) . . ? C3 C4 C8 123.2(2) . . ? C5 C4 C8 120.0(3) . . ? N1 C5 C4 122.8(2) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O2 C6 O1 125.4(2) . . ? O2 C6 C1 118.4(2) . . ? O1 C6 C1 116.1(2) . . ? O3 C7 O4 125.5(2) . . ? O3 C7 C2 119.1(2) . . ? O4 C7 C2 115.3(2) . . ? C9 C8 C4 116.1(3) . . ? C9 C8 H8A 108.3 . . ? C4 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? C4 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 123.0(3) . . ? N2 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 116.2(3) . . ? C11 C12 C15 121.5(3) . . ? C13 C12 C15 122.3(3) . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? N2 C14 C13 123.2(3) . . ? N2 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? C12 C15 C15 112.2(4) . 3_557 ? C12 C15 H15A 109.2 . . ? C15 C15 H15A 109.2 3_557 . ? C12 C15 H15B 109.2 . . ? C15 C15 H15B 109.2 3_557 . ? H15A C15 H15B 107.9 . . ? 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 O4 Co1 O1 C6 -80.0(5) 2_646 . . . ? O3 Co1 O1 C6 90.66(18) 4_566 . . . ? N1 Co1 O1 C6 -3.66(18) . . . . ? N2 Co1 O1 C6 177.64(19) . . . . ? O5 Co1 O1 C6 -94.82(19) . . . . ? O4 Co1 N1 C5 -7.7(2) 2_646 . . . ? O3 Co1 N1 C5 88.2(2) 4_566 . . . ? O1 Co1 N1 C5 -178.9(2) . . . . ? N2 Co1 N1 C5 -171.3(4) . . . . ? O5 Co1 N1 C5 -91.5(2) . . . . ? O4 Co1 N1 C1 165.77(17) 2_646 . . . ? O3 Co1 N1 C1 -98.34(17) 4_566 . . . ? O1 Co1 N1 C1 -5.45(17) . . . . ? N2 Co1 N1 C1 2.1(6) . . . . ? O5 Co1 N1 C1 81.93(17) . . . . ? O4 Co1 N2 C14 -46.2(2) 2_646 . . . ? O3 Co1 N2 C14 -141.2(2) 4_566 . . . ? O1 Co1 N2 C14 125.1(2) . . . . ? N1 Co1 N2 C14 117.7(5) . . . . ? O5 Co1 N2 C14 37.6(2) . . . . ? O4 Co1 N2 C10 137.4(2) 2_646 . . . ? O3 Co1 N2 C10 42.4(2) 4_566 . . . ? O1 Co1 N2 C10 -51.3(2) . . . . ? N1 Co1 N2 C10 -58.7(6) . . . . ? O5 Co1 N2 C10 -138.8(2) . . . . ? C5 N1 C1 C2 2.7(4) . . . . ? Co1 N1 C1 C2 -171.36(18) . . . . ? C5 N1 C1 C6 -173.5(2) . . . . ? Co1 N1 C1 C6 12.5(3) . . . . ? N1 C1 C2 C3 -3.7(4) . . . . ? C6 C1 C2 C3 172.2(2) . . . . ? N1 C1 C2 C7 174.0(2) . . . . ? C6 C1 C2 C7 -10.2(4) . . . . ? C1 C2 C3 C4 2.1(4) . . . . ? C7 C2 C3 C4 -175.7(2) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C2 C3 C4 C8 179.7(3) . . . . ? C1 N1 C5 C4 0.0(4) . . . . ? Co1 N1 C5 C4 173.10(19) . . . . ? C3 C4 C5 N1 -1.5(4) . . . . ? C8 C4 C5 N1 179.1(3) . . . . ? Co1 O1 C6 O2 -167.5(2) . . . . ? Co1 O1 C6 C1 11.3(3) . . . . ? N1 C1 C6 O2 162.8(2) . . . . ? C2 C1 C6 O2 -13.3(4) . . . . ? N1 C1 C6 O1 -16.2(3) . . . . ? C2 C1 C6 O1 167.7(2) . . . . ? Co1 O3 C7 O4 114.9(3) 4_565 . . . ? Co1 O3 C7 C2 -61.1(3) 4_565 . . . ? Co1 O4 C7 O3 -19.9(4) 2_656 . . . ? Co1 O4 C7 C2 156.27(17) 2_656 . . . ? C3 C2 C7 O3 118.4(3) . . . . ? C1 C2 C7 O3 -59.2(3) . . . . ? C3 C2 C7 O4 -58.0(3) . . . . ? C1 C2 C7 O4 124.3(3) . . . . ? C3 C4 C8 C9 36.9(5) . . . . ? C5 C4 C8 C9 -143.8(4) . . . . ? C14 N2 C10 C11 -2.6(5) . . . . ? Co1 N2 C10 C11 174.0(3) . . . . ? N2 C10 C11 C12 0.3(6) . . . . ? C10 C11 C12 C13 2.8(5) . . . . ? C10 C11 C12 C15 -176.4(3) . . . . ? C11 C12 C13 C14 -3.5(6) . . . . ? C15 C12 C13 C14 175.7(3) . . . . ? C10 N2 C14 C13 1.9(5) . . . . ? Co1 N2 C14 C13 -174.6(3) . . . . ? C12 C13 C14 N2 1.2(6) . . . . ? C11 C12 C15 C15 88.0(6) . . . 3_557 ? C13 C12 C15 C15 -91.1(6) . . . 3_557 ? 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 O5 H2W O2 0.85 1.84 2.681(3) 169.4 4_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.526 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.062 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 0.288 -0.130 472.4 55.2 _platon_squeeze_details ; ? ; # Attachment '- 2.cif' data_a_2 _database_code_depnum_ccdc_archive 'CCDC 880569' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Co2 N4 O10' _chemical_formula_weight 724.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.36(2) _cell_length_b 14.75(2) _cell_length_c 8.276(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.746(19) _cell_angle_gamma 90.00 _cell_volume 1728(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 911 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 21.39 _exptl_crystal_description block _exptl_crystal_colour amaranth _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7924 _exptl_absorpt_correction_T_max 0.8963 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3151 _diffrn_reflns_av_R_equivalents 0.1270 _diffrn_reflns_av_sigmaI/netI 0.1296 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3151 _reflns_number_gt 1704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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 'Bruker SHELXTL' _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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3151 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.1915 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.87991(7) 0.91761(6) 0.09275(11) 0.0329(3) Uani 1 1 d . . . N1 N 0.9936(4) 0.8468(3) 0.2377(6) 0.0315(14) Uani 1 1 d . . . N2 N 0.7560(4) 0.9631(4) -0.0698(7) 0.0365(15) Uani 1 1 d . . . O1 O 0.8424(3) 0.7829(3) 0.0410(5) 0.0414(13) Uani 1 1 d . . . O2 O 0.9002(4) 0.6422(3) 0.0651(5) 0.0433(14) Uani 1 1 d . . . O3 O 0.9499(3) 0.5706(3) 0.3934(5) 0.0332(12) Uani 1 1 d . . . O4 O 1.0910(4) 0.5476(3) 0.3265(5) 0.0369(12) Uani 1 1 d . . . O5 O 0.7953(3) 0.9124(3) 0.2849(5) 0.0440(13) Uani 1 1 d . . . H1W H 0.7388 0.8927 0.2659 0.066 Uiso 1 1 d R . . H2W H 0.8422 0.8889 0.3470 0.066 Uiso 1 1 d R . . C1 C 0.9808(5) 0.7551(4) 0.2356(7) 0.0288(17) Uani 1 1 d . . . C2 C 1.0405(5) 0.6974(4) 0.3366(7) 0.0297(17) Uani 1 1 d . . . C3 C 1.1186(5) 0.7356(5) 0.4389(8) 0.0404(19) Uani 1 1 d . . . H3 H 1.1605 0.6982 0.5066 0.048 Uiso 1 1 calc R . . C4 C 1.1339(5) 0.8269(4) 0.4401(8) 0.0350(19) Uani 1 1 d . . . C5 C 1.0678(5) 0.8809(5) 0.3415(8) 0.0360(18) Uani 1 1 d . . . H5 H 1.0751 0.9435 0.3475 0.043 Uiso 1 1 calc R . . C6 C 0.9015(5) 0.7228(4) 0.1028(8) 0.0332(18) Uani 1 1 d . . . C7 C 1.0241(6) 0.5958(4) 0.3516(8) 0.0304(17) Uani 1 1 d . . . C8 C 1.2179(5) 0.8697(5) 0.5494(10) 0.052(2) Uani 1 1 d . . . H8A H 1.2351 0.9243 0.4961 0.062 Uiso 1 1 calc R . . H8B H 1.1982 0.8879 0.6511 0.062 Uiso 1 1 calc R . . C9 C 1.3003(7) 0.8146(8) 0.5886(18) 0.140(6) Uani 1 1 d . . . H9A H 1.2857 0.7619 0.6478 0.210 Uiso 1 1 calc R . . H9B H 1.3495 0.8486 0.6551 0.210 Uiso 1 1 calc R . . H9C H 1.3211 0.7961 0.4894 0.210 Uiso 1 1 calc R . . C10 C 0.7430(6) 0.9303(5) -0.2218(9) 0.057(2) Uani 1 1 d . . . H10 H 0.7899 0.8937 -0.2523 0.068 Uiso 1 1 calc R . . C11 C 0.6639(6) 0.9477(6) -0.3358(9) 0.057(2) Uani 1 1 d . . . H11 H 0.6591 0.9233 -0.4405 0.068 Uiso 1 1 calc R . . C12 C 0.5934(6) 0.9990(5) -0.2996(10) 0.056(2) Uani 1 1 d . . . C13 C 0.6076(6) 1.0354(6) -0.1409(10) 0.071(3) Uani 1 1 d . . . H13 H 0.5624 1.0739 -0.1098 0.086 Uiso 1 1 calc R . . C14 C 0.6870(6) 1.0148(6) -0.0319(10) 0.063(3) Uani 1 1 d . . . H14 H 0.6932 1.0381 0.0739 0.076 Uiso 1 1 calc R . . C15 C 0.5019(6) 1.0214(6) -0.4165(9) 0.067(3) Uani 1 1 d . . . H15A H 0.4485 1.0004 -0.3690 0.081 Uiso 1 1 calc R . . H15B H 0.4965 1.0867 -0.4291 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0465(7) 0.0196(5) 0.0262(5) 0.0024(4) -0.0119(4) 0.0001(5) N1 0.046(4) 0.016(3) 0.027(3) 0.000(2) -0.008(3) -0.004(3) N2 0.038(4) 0.038(3) 0.028(3) 0.001(3) -0.009(3) 0.007(3) O1 0.055(3) 0.025(3) 0.036(3) 0.002(2) -0.017(2) 0.003(2) O2 0.077(4) 0.022(3) 0.023(3) -0.003(2) -0.014(2) 0.003(2) O3 0.041(3) 0.026(3) 0.028(3) -0.003(2) -0.008(2) 0.001(2) O4 0.055(3) 0.016(2) 0.036(3) 0.001(2) -0.003(2) 0.010(2) O5 0.040(3) 0.050(3) 0.036(3) 0.010(2) -0.011(2) -0.002(3) C1 0.042(5) 0.024(4) 0.015(3) -0.007(3) -0.011(3) -0.001(3) C2 0.051(5) 0.019(3) 0.015(3) -0.001(3) -0.007(3) 0.003(3) C3 0.050(5) 0.031(4) 0.033(4) 0.000(3) -0.013(4) 0.004(3) C4 0.046(5) 0.020(4) 0.030(4) 0.001(3) -0.018(3) -0.005(3) C5 0.043(5) 0.023(3) 0.039(4) -0.001(3) -0.003(4) -0.004(3) C6 0.050(5) 0.018(4) 0.026(4) 0.008(3) -0.011(3) 0.001(3) C7 0.040(5) 0.022(4) 0.024(4) 0.002(3) -0.011(3) 0.004(3) C8 0.052(5) 0.047(5) 0.048(5) 0.000(4) -0.016(4) -0.016(4) C9 0.054(7) 0.093(9) 0.238(17) -0.037(9) -0.078(9) 0.015(6) C10 0.073(6) 0.051(5) 0.039(5) -0.005(4) -0.016(4) 0.026(4) C11 0.063(6) 0.075(6) 0.026(4) -0.012(4) -0.013(4) 0.029(5) C12 0.059(6) 0.056(5) 0.044(5) 0.002(4) -0.015(4) 0.010(5) C13 0.067(7) 0.095(7) 0.043(5) -0.029(5) -0.021(4) 0.038(5) C14 0.067(6) 0.069(6) 0.042(5) -0.017(4) -0.027(4) 0.022(5) C15 0.064(6) 0.087(7) 0.040(5) -0.001(5) -0.022(4) 0.008(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 O4 2.050(5) 2_755 ? Co1 O3 2.079(6) 4_575 ? Co1 O1 2.085(5) . ? Co1 N1 2.129(5) . ? Co1 N2 2.148(6) . ? Co1 O5 2.160(5) . ? N1 C5 1.347(8) . ? N1 C1 1.364(7) . ? N2 C14 1.330(10) . ? N2 C10 1.331(9) . ? O1 C6 1.273(7) . ? O2 C6 1.228(7) . ? O3 C7 1.232(8) . ? O3 Co1 2.079(6) 4_576 ? O4 C7 1.242(8) . ? O4 Co1 2.050(5) 2_745 ? O5 H1W 0.8500 . ? O5 H2W 0.8500 . ? C1 C2 1.385(8) . ? C1 C6 1.519(8) . ? C2 C3 1.404(9) . ? C2 C7 1.525(9) . ? C3 C4 1.366(9) . ? C3 H3 0.9300 . ? C4 C5 1.393(9) . ? C4 C8 1.517(9) . ? C5 H5 0.9300 . ? C8 C9 1.427(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.373(10) . ? C10 H10 0.9300 . ? C11 C12 1.337(11) . ? C11 H11 0.9300 . ? C12 C13 1.401(10) . ? C12 C15 1.530(10) . ? C13 C14 1.364(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C15 1.512(15) 3_674 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? 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 O4 Co1 O3 94.66(19) 2_755 4_575 ? O4 Co1 O1 171.9(2) 2_755 . ? O3 Co1 O1 93.41(19) 4_575 . ? O4 Co1 N1 100.4(2) 2_755 . ? O3 Co1 N1 93.5(2) 4_575 . ? O1 Co1 N1 78.12(19) . . ? O4 Co1 N2 90.8(2) 2_755 . ? O3 Co1 N2 86.4(2) 4_575 . ? O1 Co1 N2 90.7(2) . . ? N1 Co1 N2 168.8(2) . . ? O4 Co1 O5 84.4(2) 2_755 . ? O3 Co1 O5 174.16(17) 4_575 . ? O1 Co1 O5 87.69(19) . . ? N1 Co1 O5 92.3(2) . . ? N2 Co1 O5 87.9(2) . . ? C5 N1 C1 118.0(5) . . ? C5 N1 Co1 128.6(4) . . ? C1 N1 Co1 113.0(4) . . ? C14 N2 C10 116.2(6) . . ? C14 N2 Co1 127.0(5) . . ? C10 N2 Co1 116.6(5) . . ? C6 O1 Co1 116.8(4) . . ? C7 O3 Co1 139.0(4) . 4_576 ? C7 O4 Co1 127.0(5) . 2_745 ? Co1 O5 H1W 120.9 . . ? Co1 O5 H2W 88.4 . . ? H1W O5 H2W 127.3 . . ? N1 C1 C2 122.3(5) . . ? N1 C1 C6 113.8(5) . . ? C2 C1 C6 123.7(5) . . ? C1 C2 C3 117.8(6) . . ? C1 C2 C7 124.4(6) . . ? C3 C2 C7 117.6(5) . . ? C4 C3 C2 120.8(6) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 117.9(6) . . ? C3 C4 C8 121.7(6) . . ? C5 C4 C8 120.4(6) . . ? N1 C5 C4 123.2(6) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? O2 C6 O1 126.3(6) . . ? O2 C6 C1 117.7(5) . . ? O1 C6 C1 116.0(6) . . ? O3 C7 O4 127.2(6) . . ? O3 C7 C2 118.2(6) . . ? O4 C7 C2 114.5(7) . . ? C9 C8 C4 116.3(7) . . ? C9 C8 H8A 108.2 . . ? C4 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? C4 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 123.3(8) . . ? N2 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C12 C11 C10 121.4(8) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 115.6(7) . . ? C11 C12 C15 125.5(7) . . ? C13 C12 C15 118.9(8) . . ? C14 C13 C12 120.5(8) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? N2 C14 C13 123.0(8) . . ? N2 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C15 C15 C12 112.5(9) 3_674 . ? C15 C15 H15A 109.1 3_674 . ? C12 C15 H15A 109.1 . . ? C15 C15 H15B 109.1 3_674 . ? C12 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? 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 O5 H2W O2 0.85 1.91 2.667(7) 147.5 4_576 O5 H2W N1 0.85 2.57 3.094(9) 121.2 . _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.105 _refine_diff_density_min -0.976 _refine_diff_density_rms 0.115 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 0.455 0.250 -0.025 167.8 14.0 2 0.545 0.750 0.017 167.8 14.1 _platon_squeeze_details ; ? ;