# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'FengFeng Jiao' _publ_contact_author_email jiao@udel.edu loop_ _publ_author_name 'Bryan Yonemoto' 'Zhuo-jia Lin' 'Feng Jiao' data_fengs1 _database_code_depnum_ccdc_archive 'CCDC 885307' #TrackingRef '- DEL-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H32 Co4 N5 O20 P5' _chemical_formula_weight 872.93 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 26.631(5) _cell_length_b 7.6331(15) _cell_length_c 6.8120(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1384.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 2.732 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker P4' _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 3054 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.99 _reflns_number_total 741 _reflns_number_gt 575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0682P)^2^+1.2562P] 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 741 _refine_ls_number_parameters 65 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.073 _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 0.25826(3) 0.0000 1.0000 0.0243(3) Uani 1 2 d S . . P1 P 0.18372(5) 0.2044(2) 0.7500 0.0226(4) Uani 1 2 d S . . O1 O 0.19533(11) 0.3095(4) 0.9359(4) 0.0373(8) Uani 1 1 d . . . O2 O 0.22150(14) 0.0437(5) 0.7500 0.0235(9) Uani 1 2 d S . . O3 O 0.13091(15) 0.1375(6) 0.7500 0.0417(12) Uani 1 2 d S . . N1 N 0.1273(3) -0.2275(9) 0.7500 0.0600(19) Uani 1 2 d S . . H1A H 0.1250 -0.1107 0.7500 0.072 Uiso 1 2 d SR . . H1B H 0.1457 -0.2565 0.6441 0.072 Uiso 1 1 d R . . C1 C 0.0862(3) -0.3387(15) 0.7500 0.081(3) Uani 1 2 d S . . H1C H 0.0933 -0.4621 0.7500 0.097 Uiso 1 2 d SR . . H1D H 0.0683 -0.2930 0.6389 0.097 Uiso 1 1 d R . . P2 P 0.0000 -0.1267(8) 0.2500 0.0658(14) Uani 0.50 4 d SPU . 1 O1Q O 0.0000 -0.027(5) 0.075(4) 0.232(17) Uani 0.50 2 d SP . 1 O2Q O -0.0422(4) -0.2554(18) 0.2500 0.100(5) Uani 0.50 2 d SPU A 1 H2 H -0.0713 -0.2151 0.2500 0.150 Uiso 0.50 2 d SPR A 1 N2 N 0.0000 -0.1267(8) 0.2500 0.0658(14) Uani 0.50 4 d SPU B 2 H2A H -0.0279 -0.0859 0.3132 0.099 Uiso 0.13 1 d PR B 2 H2B H 0.0000 -0.0859 0.1268 0.099 Uiso 0.25 2 d SPR B 2 C2 C 0.0000 -0.298(3) 0.2500 0.059(6) Uani 0.50 4 d SPU B 2 H2D H 0.0340 -0.3400 0.2500 0.088 Uiso 0.25 2 d SPR B 2 H2E H -0.0167 -0.3400 0.1342 0.088 Uiso 0.13 1 d PR B 2 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 0.0315(5) 0.0245(5) 0.0169(4) -0.0025(3) 0.000 0.000 P1 0.0271(7) 0.0150(7) 0.0258(7) 0.000 0.000 -0.0011(6) O1 0.0454(17) 0.0326(18) 0.0340(16) -0.0136(14) 0.0129(13) -0.0115(15) O2 0.031(2) 0.019(2) 0.0204(17) 0.000 0.000 0.0072(15) O3 0.026(2) 0.030(3) 0.069(3) 0.000 0.000 -0.0014(19) N1 0.084(5) 0.046(5) 0.050(4) 0.000 0.000 -0.021(4) C1 0.075(6) 0.091(9) 0.077(6) 0.000 0.000 -0.033(6) P2 0.086(4) 0.054(3) 0.058(3) 0.000 0.000 0.000 O1Q 0.32(4) 0.21(4) 0.17(3) 0.15(2) 0.000 0.000 O2Q 0.040(7) 0.054(9) 0.207(15) 0.000 0.000 0.000(6) N2 0.086(4) 0.054(3) 0.058(3) 0.000 0.000 0.000 C2 0.040(11) 0.033(12) 0.102(16) 0.000 0.000 0.000 _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 1.958(3) 13_557 ? Co1 O1 1.958(3) 16_545 ? Co1 O2 1.992(2) . ? Co1 O2 1.992(2) 11_556 ? P1 O3 1.496(4) . ? P1 O1 1.531(3) . ? P1 O1 1.531(3) 10_557 ? P1 O2 1.586(4) . ? O1 Co1 1.958(3) 13_557 ? O2 Co1 1.992(2) 10_557 ? N1 C1 1.385(10) . ? P2 O1Q 1.413(19) 10_556 ? P2 O1Q 1.413(19) . ? P2 O2Q 1.493(13) 3 ? P2 O2Q 1.493(13) . ? O1Q O1Q 1.10(4) 9 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 101.72(19) 13_557 16_545 ? O1 Co1 O2 112.11(15) 13_557 . ? O1 Co1 O2 104.12(12) 16_545 . ? O1 Co1 O2 104.12(12) 13_557 11_556 ? O1 Co1 O2 112.11(15) 16_545 11_556 ? O2 Co1 O2 121.1(2) . 11_556 ? O3 P1 O1 111.63(14) . . ? O3 P1 O1 111.63(14) . 10_557 ? O1 P1 O1 111.7(3) . 10_557 ? O3 P1 O2 109.4(2) . . ? O1 P1 O2 106.08(16) . . ? O1 P1 O2 106.08(16) 10_557 . ? P1 O1 Co1 134.53(18) . 13_557 ? P1 O2 Co1 116.17(12) . . ? P1 O2 Co1 116.17(12) . 10_557 ? Co1 O2 Co1 117.46(19) . 10_557 ? O1Q P2 O1Q 115(3) 10_556 . ? O1Q P2 O2Q 110.7(11) 10_556 3 ? O1Q P2 O2Q 110.7(11) . 3 ? O1Q P2 O2Q 110.7(11) 10_556 . ? O1Q P2 O2Q 110.7(11) . . ? O2Q P2 O2Q 97.7(11) 3 . ? O1Q O1Q P2 170(6) 9 . ? 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 N1 H1A O3 0.89 1.90 2.788(9) 171.2 . N1 H1B O1 0.90 1.98 2.872(6) 171.1 11 O2Q H2 O3 0.83 1.69 2.528(13) 178.8 9_556 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.723 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.123 # Attachment '- DEL-2.cif' data_feng1 _database_code_depnum_ccdc_archive 'CCDC 885308' #TrackingRef '- DEL-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H28 Co5 N5 O20 P5' _chemical_formula_weight 915.81 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' P P 0.1023 0.0942 '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' 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 Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 13.361(7) _cell_length_b 13.789(7) _cell_length_c 14.017(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2582(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 3.549 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4078 _exptl_absorpt_correction_T_max 0.7005 _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 18493 _diffrn_reflns_av_R_equivalents 0.1037 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5023 _reflns_number_gt 4244 _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^)+(0.0966P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(3) _refine_ls_number_reflns 5023 _refine_ls_number_parameters 355 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1748 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _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 1.62686(11) 0.75941(11) 0.98491(10) 0.0219(4) Uani 1 1 d . . . Co2 Co 1.62796(10) 0.72493(11) 0.73757(10) 0.0215(4) Uani 1 1 d . . . Co3 Co 1.93519(8) 0.75931(11) 0.85827(15) 0.0233(3) Uani 1 1 d . . . Co4 Co 1.75806(10) 1.12628(10) 0.84276(10) 0.0210(3) Uani 1 1 d . . . Co5 Co 1.77641(9) 0.36778(10) 0.87807(10) 0.0203(3) Uani 1 1 d . . . P1 P 1.6072(2) 0.7610(2) 1.2163(2) 0.0239(6) Uani 1 1 d . . . P2 P 1.6127(2) 0.7179(2) 0.5065(2) 0.0206(6) Uani 1 1 d . . . P3 P 1.74337(18) 0.88880(18) 0.8325(2) 0.0195(6) Uani 1 1 d . . . P4 P 1.75989(18) 0.60777(19) 0.8842(2) 0.0192(6) Uani 1 1 d . . . P5 P 1.43049(15) 0.7416(2) 0.8620(3) 0.0206(5) Uani 1 1 d . . . O1 O 1.6020(6) 0.7986(5) 1.1133(7) 0.042(2) Uani 1 1 d . . . O2 O 1.6192(5) 0.8473(5) 1.2852(5) 0.0267(17) Uani 1 1 d . . . O3 O 1.5096(5) 0.7075(7) 1.2411(7) 0.036(2) Uani 1 1 d . . . O4 O 1.6967(5) 0.6919(5) 1.2260(6) 0.0286(18) Uani 1 1 d . . . O5 O 1.6126(5) 0.6806(5) 0.6078(7) 0.0294(16) Uani 1 1 d . . . O6 O 1.6910(5) 0.7992(6) 0.4973(6) 0.0287(18) Uani 1 1 d . . . O7 O 1.5070(6) 0.7536(6) 0.4798(7) 0.0307(19) Uani 1 1 d . . . O8 O 1.6407(6) 0.6326(6) 0.4418(6) 0.0316(18) Uani 1 1 d . . . O9 O 1.6584(5) 0.8706(5) 0.9024(6) 0.0297(18) Uani 1 1 d . . . O10 O 1.7307(5) 0.8257(5) 0.7435(7) 0.0294(19) Uani 1 1 d . . . O11 O 1.8445(5) 0.8690(5) 0.8782(6) 0.0275(16) Uani 1 1 d . . . O12 O 1.7381(5) 0.9940(5) 0.7981(7) 0.0288(19) Uani 1 1 d . . . O13 O 1.7385(5) 0.6679(5) 0.9749(6) 0.0267(18) Uani 1 1 d . . . O14 O 1.6727(5) 0.6142(5) 0.8141(5) 0.0262(16) Uani 1 1 d . . . O15 O 1.8571(5) 0.6429(5) 0.8359(6) 0.0274(17) Uani 1 1 d . . . O16 O 1.7742(6) 0.5027(5) 0.9165(6) 0.0277(18) Uani 1 1 d . . . O17 O 1.4951(5) 0.7085(6) 0.9443(6) 0.0256(17) Uani 1 1 d . . . O18 O 1.4932(5) 0.7636(5) 0.7734(6) 0.0230(17) Uani 1 1 d . . . O19 O 1.3724(5) 0.8334(6) 0.8906(6) 0.0300(18) Uani 1 1 d . . . O20 O 1.3590(5) 0.6583(5) 0.8367(6) 0.0266(17) Uani 1 1 d . . . N1 N 1.5000 0.5000 0.8482(14) 0.045(4) Uani 1 2 d S . . H1A H 1.5586 0.5304 0.8380 0.054 Uiso 0.50 1 d PR . . H1B H 1.4508 0.5446 0.8460 0.054 Uiso 0.50 1 d PR . . H1C H 1.5007 0.4716 0.9061 0.054 Uiso 0.50 1 d PR . . H1D H 1.4900 0.4551 0.8026 0.054 Uiso 0.50 1 d PR . . N2 N 2.0000 1.0000 0.8716(19) 0.072(7) Uani 1 2 d S . . H2A H 1.9443 0.9634 0.8711 0.086 Uiso 0.50 1 d PR . . H2B H 2.0507 0.9634 0.8937 0.086 Uiso 0.50 1 d PR . . H2C H 1.9909 1.0513 0.9103 0.086 Uiso 0.50 1 d PR . . H2D H 2.0139 1.0199 0.8119 0.086 Uiso 0.50 1 d PR . . N3 N 0.3623(7) 0.7073(7) 0.6163(10) 0.046(3) Uani 1 1 d D . . H3A H 0.3078 0.7456 0.6122 0.055 Uiso 1 1 d R . . H3B H 0.4062 0.7246 0.5707 0.055 Uiso 1 1 d R . . H3C H 0.3918 0.7166 0.6733 0.055 Uiso 1 1 d R . . N4 N 0.8674(7) 0.6927(8) 0.6037(10) 0.051(3) Uani 1 1 d D . . H4A H 0.8058 0.7149 0.6177 0.062 Uiso 1 1 d R . . H4B H 0.8847 0.7097 0.5439 0.062 Uiso 1 1 d R . . H4C H 0.9128 0.7173 0.6445 0.062 Uiso 1 1 d R . . N5 N 1.5000 1.0000 0.8369(9) 0.031(3) Uani 1 2 d SD . . H5A H 1.4912 1.0567 0.8675 0.037 Uiso 0.50 1 d PR . . H5B H 1.5587 0.9748 0.8564 0.037 Uiso 0.50 1 d PR . . H5C H 1.4515 0.9592 0.8564 0.037 Uiso 0.50 1 d PR . . N6 N 2.0000 0.5000 0.8797(11) 0.034(3) Uani 1 2 d SD . . H6A H 2.0605 0.5101 0.8534 0.041 Uiso 0.50 1 d PR . . H6B H 1.9579 0.5464 0.8592 0.041 Uiso 0.50 1 d PR . . H6C H 1.9763 0.4426 0.8592 0.041 Uiso 0.50 1 d PR . . N7 N 1.2687(7) 0.5190(7) 1.1062(9) 0.045(3) Uani 1 1 d D . . H7A H 1.2569 0.5833 1.1051 0.054 Uiso 1 1 d R . . H7B H 1.2481 0.4905 1.1605 0.054 Uiso 1 1 d R . . H7C H 1.2435 0.4878 1.0552 0.054 Uiso 1 1 d R . . C3 C 0.3399(13) 0.6035(10) 0.6055(16) 0.079(6) Uani 1 1 d D . . H3D H 0.4026 0.5667 0.6031 0.118 Uiso 1 1 calc R . . H3E H 0.3023 0.5931 0.5464 0.118 Uiso 1 1 calc R . . H3F H 0.2998 0.5814 0.6599 0.118 Uiso 1 1 calc R . . C4 C 0.8608(12) 0.5850(10) 0.6114(14) 0.074(5) Uani 1 1 d D . . H4D H 0.9283 0.5572 0.6101 0.111 Uiso 1 1 calc R . . H4E H 0.8219 0.5595 0.5576 0.111 Uiso 1 1 calc R . . H4F H 0.8278 0.5675 0.6714 0.111 Uiso 1 1 calc R . . C5 C 1.5000 1.0000 0.7311(11) 0.044(4) Uani 1 2 d SD . . H5D H 1.4549 1.0508 0.7078 0.066 Uiso 0.50 1 calc PR . . H5E H 1.4771 0.9368 0.7078 0.066 Uiso 0.50 1 calc PR . . H5F H 1.5680 1.0124 0.7078 0.066 Uiso 0.50 1 calc PR . . C6 C 2.0000 0.5000 0.9851(11) 0.038(4) Uani 1 2 d SD . . H6D H 2.0687 0.4923 1.0084 0.056 Uiso 0.50 1 calc PR . . H6E H 1.9588 0.4462 1.0084 0.056 Uiso 0.50 1 calc PR . . H6F H 1.9725 0.5615 1.0084 0.056 Uiso 0.50 1 calc PR . . C7 C 1.3786(8) 0.5308(9) 1.1007(10) 0.048(3) Uani 1 1 d D . . H7D H 1.3957 0.5696 1.0444 0.073 Uiso 1 1 calc R . . H7E H 1.4102 0.4668 1.0957 0.073 Uiso 1 1 calc R . . H7F H 1.4027 0.5637 1.1582 0.073 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 0.0204(8) 0.0376(8) 0.0076(8) 0.0022(6) 0.0008(6) 0.0015(5) Co2 0.0191(7) 0.0367(8) 0.0089(8) 0.0007(5) 0.0000(6) -0.0010(5) Co3 0.0218(6) 0.0341(7) 0.0139(6) 0.0034(6) -0.0009(8) -0.0011(6) Co4 0.0233(6) 0.0285(7) 0.0113(8) -0.0004(6) -0.0014(5) 0.0004(5) Co5 0.0205(6) 0.0291(7) 0.0113(8) 0.0003(6) 0.0007(5) -0.0012(5) P1 0.0229(14) 0.0424(16) 0.0065(15) -0.0025(11) 0.0010(11) 0.0041(11) P2 0.0204(13) 0.0348(14) 0.0068(14) -0.0010(10) 0.0002(11) -0.0016(11) P3 0.0198(11) 0.0273(13) 0.0116(15) 0.0010(11) 0.0001(11) -0.0015(10) P4 0.0199(11) 0.0261(13) 0.0117(15) 0.0000(10) 0.0012(11) 0.0009(9) P5 0.0153(10) 0.0342(13) 0.0122(11) 0.0001(10) 0.0016(13) 0.0001(10) O1 0.059(5) 0.057(4) 0.009(4) -0.002(4) 0.002(5) 0.028(4) O2 0.027(4) 0.035(4) 0.018(4) -0.006(3) -0.003(3) 0.008(3) O3 0.022(4) 0.060(6) 0.026(5) -0.014(4) 0.004(4) -0.005(4) O4 0.034(4) 0.036(4) 0.016(5) 0.000(3) -0.001(3) -0.001(3) O5 0.042(4) 0.038(4) 0.007(4) 0.003(3) 0.002(4) -0.007(3) O6 0.021(4) 0.048(4) 0.016(5) 0.004(3) -0.006(3) -0.004(3) O7 0.022(4) 0.047(4) 0.023(5) -0.010(4) -0.006(3) 0.000(3) O8 0.037(4) 0.043(4) 0.015(4) -0.009(3) 0.000(3) -0.001(3) O9 0.031(4) 0.045(4) 0.013(4) 0.006(3) 0.006(3) 0.000(3) O10 0.028(4) 0.033(4) 0.027(5) -0.002(3) -0.001(3) -0.006(3) O11 0.026(3) 0.039(4) 0.017(4) -0.004(3) -0.004(3) 0.007(3) O12 0.040(4) 0.035(4) 0.011(5) 0.002(3) -0.005(3) -0.006(3) O13 0.030(4) 0.031(4) 0.019(5) -0.013(3) 0.002(3) 0.005(3) O14 0.024(4) 0.039(4) 0.016(4) 0.004(3) -0.003(3) 0.002(3) O15 0.022(3) 0.040(4) 0.020(4) -0.001(3) 0.002(3) -0.004(3) O16 0.042(4) 0.028(4) 0.014(4) -0.002(3) 0.000(3) 0.003(3) O17 0.020(4) 0.050(5) 0.007(4) 0.007(3) -0.006(3) -0.006(3) O18 0.021(4) 0.042(4) 0.006(4) 0.001(3) 0.002(3) 0.001(3) O19 0.030(4) 0.045(5) 0.016(5) -0.009(4) -0.005(3) 0.006(3) O20 0.018(3) 0.039(4) 0.022(5) 0.002(3) 0.005(3) -0.001(3) N1 0.043(7) 0.028(7) 0.064(13) 0.000 0.000 -0.004(6) N2 0.028(7) 0.022(8) 0.17(2) 0.000 0.000 -0.006(6) N3 0.030(5) 0.084(7) 0.023(7) 0.001(6) 0.003(6) 0.006(5) N4 0.031(6) 0.109(9) 0.014(6) -0.018(7) 0.000(5) -0.005(5) N5 0.042(7) 0.035(7) 0.016(8) 0.000 0.000 -0.002(6) N6 0.025(6) 0.025(7) 0.054(10) 0.000 0.000 0.001(5) N7 0.050(6) 0.074(7) 0.010(5) -0.005(6) 0.006(5) -0.004(5) C3 0.112(13) 0.081(10) 0.044(11) -0.030(9) 0.040(11) -0.046(10) C4 0.110(13) 0.101(12) 0.011(7) 0.001(8) 0.007(9) -0.037(10) C5 0.040(9) 0.051(11) 0.041(12) 0.000 0.000 0.002(8) C6 0.019(7) 0.052(10) 0.042(11) 0.000 0.000 0.002(7) C7 0.039(7) 0.069(8) 0.038(8) -0.003(7) 0.000(6) -0.009(6) _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 1.908(10) . ? Co1 O13 1.958(7) . ? Co1 O9 1.966(8) . ? Co1 O17 1.979(7) . ? Co2 O5 1.930(9) . ? Co2 O18 1.944(7) . ? Co2 O10 1.955(7) . ? Co2 O14 1.960(7) . ? Co3 O15 1.939(7) . ? Co3 O11 1.958(7) . ? Co3 O7 1.963(9) 3_565 ? Co3 O3 1.973(9) 3_564 ? Co4 O8 1.940(8) 4_855 ? Co4 O12 1.946(7) . ? Co4 O19 1.949(7) 2_875 ? Co4 O4 1.965(8) 4_854 ? Co5 O2 1.928(7) 4_844 ? Co5 O20 1.933(7) 2_865 ? Co5 O16 1.938(7) . ? Co5 O6 1.969(8) 4_845 ? P1 O4 1.535(8) . ? P1 O1 1.536(10) . ? P1 O3 1.539(8) . ? P1 O2 1.541(8) . ? P2 O5 1.511(9) . ? P2 O8 1.532(8) . ? P2 O6 1.539(8) . ? P2 O7 1.542(8) . ? P3 O11 1.520(7) . ? P3 O9 1.520(8) . ? P3 O10 1.530(9) . ? P3 O12 1.531(7) . ? P4 O14 1.527(8) . ? P4 O16 1.529(7) . ? P4 O15 1.544(8) . ? P4 O13 1.544(8) . ? P5 O17 1.510(8) . ? P5 O18 1.530(8) . ? P5 O20 1.536(7) . ? P5 O19 1.538(8) . ? O2 Co5 1.928(7) 4_855 ? O3 Co3 1.973(9) 3_465 ? O4 Co4 1.965(8) 4_845 ? O6 Co5 1.969(8) 4_854 ? O7 Co3 1.963(9) 3_464 ? O8 Co4 1.940(8) 4_844 ? O19 Co4 1.949(7) 2_875 ? O20 Co5 1.933(7) 2_865 ? N3 C3 1.470(12) . ? N4 C4 1.492(13) . ? N5 C5 1.483(14) . ? N6 C6 1.477(14) . ? N7 C7 1.479(11) . ? 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 O13 112.5(3) . . ? O1 Co1 O9 111.8(3) . . ? O13 Co1 O9 107.3(3) . . ? O1 Co1 O17 102.5(4) . . ? O13 Co1 O17 115.4(3) . . ? O9 Co1 O17 107.3(3) . . ? O5 Co2 O18 103.4(3) . . ? O5 Co2 O10 109.9(3) . . ? O18 Co2 O10 116.4(3) . . ? O5 Co2 O14 107.5(3) . . ? O18 Co2 O14 110.8(3) . . ? O10 Co2 O14 108.4(3) . . ? O15 Co3 O11 109.2(3) . . ? O15 Co3 O7 109.1(3) . 3_565 ? O11 Co3 O7 104.4(4) . 3_565 ? O15 Co3 O3 109.1(4) . 3_564 ? O11 Co3 O3 104.6(3) . 3_564 ? O7 Co3 O3 119.8(3) 3_565 3_564 ? O8 Co4 O12 111.6(3) 4_855 . ? O8 Co4 O19 111.4(3) 4_855 2_875 ? O12 Co4 O19 104.8(3) . 2_875 ? O8 Co4 O4 111.1(3) 4_855 4_854 ? O12 Co4 O4 101.9(3) . 4_854 ? O19 Co4 O4 115.5(3) 2_875 4_854 ? O2 Co5 O20 116.6(3) 4_844 2_865 ? O2 Co5 O16 109.9(3) 4_844 . ? O20 Co5 O16 104.3(3) 2_865 . ? O2 Co5 O6 110.0(3) 4_844 4_845 ? O20 Co5 O6 111.9(3) 2_865 4_845 ? O16 Co5 O6 103.2(4) . 4_845 ? O4 P1 O1 109.2(5) . . ? O4 P1 O3 110.0(5) . . ? O1 P1 O3 109.6(5) . . ? O4 P1 O2 110.1(4) . . ? O1 P1 O2 109.5(5) . . ? O3 P1 O2 108.5(5) . . ? O5 P2 O8 107.2(5) . . ? O5 P2 O6 109.1(4) . . ? O8 P2 O6 110.1(5) . . ? O5 P2 O7 109.7(5) . . ? O8 P2 O7 109.0(5) . . ? O6 P2 O7 111.7(4) . . ? O11 P3 O9 111.3(5) . . ? O11 P3 O10 109.9(4) . . ? O9 P3 O10 110.4(4) . . ? O11 P3 O12 110.1(4) . . ? O9 P3 O12 109.0(4) . . ? O10 P3 O12 106.1(5) . . ? O14 P4 O16 109.9(4) . . ? O14 P4 O15 110.0(5) . . ? O16 P4 O15 108.8(4) . . ? O14 P4 O13 110.9(4) . . ? O16 P4 O13 106.8(5) . . ? O15 P4 O13 110.4(4) . . ? O17 P5 O18 111.5(3) . . ? O17 P5 O20 107.8(5) . . ? O18 P5 O20 107.6(5) . . ? O17 P5 O19 109.7(5) . . ? O18 P5 O19 108.9(5) . . ? O20 P5 O19 111.2(4) . . ? P1 O1 Co1 141.6(5) . . ? P1 O2 Co5 127.7(4) . 4_855 ? P1 O3 Co3 120.3(5) . 3_465 ? P1 O4 Co4 126.8(5) . 4_845 ? P2 O5 Co2 141.1(4) . . ? P2 O6 Co5 124.8(5) . 4_854 ? P2 O7 Co3 129.0(5) . 3_464 ? P2 O8 Co4 129.0(5) . 4_844 ? P3 O9 Co1 131.9(5) . . ? P3 O10 Co2 121.1(5) . . ? P3 O11 Co3 129.0(5) . . ? P3 O12 Co4 141.3(6) . . ? P4 O13 Co1 123.1(5) . . ? P4 O14 Co2 129.1(4) . . ? P4 O15 Co3 129.9(5) . . ? P4 O16 Co5 146.0(6) . . ? P5 O17 Co1 128.4(5) . . ? P5 O18 Co2 131.5(5) . . ? P5 O19 Co4 126.6(5) . 2_875 ? P5 O20 Co5 130.7(5) . 2_865 ? 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 N1 H1A O14 0.90 1.94 2.834(8) 171.1 . N1 H1B O20 0.90 2.00 2.887(7) 171.0 . N1 H1C O17 0.90 2.54 3.175(12) 127.9 2_865 N1 H1D O14 0.90 2.38 2.834(8) 111.3 2_865 N2 H2A O11 0.90 1.87 2.755(7) 169.3 . N2 H2B O8 0.90 1.91 2.801(12) 169.6 3_565 N2 H2C O8 0.90 2.13 2.801(12) 130.5 4_855 N3 H3A O4 0.90 2.34 3.032(13) 133.2 3_364 N3 H3A O13 0.90 2.45 3.102(14) 129.9 3_364 N3 H3B O7 0.90 1.90 2.794(15) 175.0 1_455 N3 H3C O18 0.90 2.06 2.917(15) 160.0 1_455 N3 H3C O20 0.90 2.47 3.163(16) 134.4 1_455 N4 H4A O10 0.90 2.54 3.247(14) 135.9 1_455 N4 H4A O6 0.90 2.56 3.152(13) 124.0 1_455 N4 H4B O19 0.90 2.24 3.010(15) 143.8 3_464 N4 H4B O17 0.90 2.32 3.123(15) 148.1 3_464 N4 H4C O3 0.90 2.14 3.035(14) 172.7 3_464 N4 H4C O1 0.90 2.57 3.140(13) 121.4 3_464 N5 H5A O9 0.90 2.29 2.917(9) 126.6 2_875 N5 H5A O19 0.90 2.39 2.958(9) 121.0 2_875 N5 H5B O9 0.90 2.06 2.917(9) 157.8 . N5 H5B O12 0.90 2.55 3.228(8) 133.1 . N5 H5C O19 0.90 2.09 2.958(9) 162.4 . N6 H6A O2 0.90 2.32 2.954(10) 127.1 3_564 N6 H6A O16 0.90 2.39 3.062(8) 131.9 2_965 N6 H6B O15 0.90 1.92 2.812(8) 170.3 . N6 H6C O2 0.90 2.10 2.954(10) 157.0 4_844 N7 H7A O10 0.90 2.34 2.924(14) 122.7 3_465 N7 H7A O6 0.90 2.38 3.113(13) 138.1 3_465 N7 H7B O12 0.90 1.95 2.728(16) 144.3 3_465 N7 H7C O16 0.90 1.96 2.736(16) 143.1 2_865 N7 H7C O13 0.90 2.44 3.169(14) 138.7 2_865 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.500 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.241 # Attachment '- DEL-3.cif' data_feng3 _database_code_depnum_ccdc_archive 'CCDC 885309' #TrackingRef '- DEL-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H44 Co10 N10 O40 P10' _chemical_formula_weight 1831.54 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' P P 0.1023 0.0942 '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 Tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 9.880(2) _cell_length_b 9.880(2) _cell_length_c 13.333(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1301.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 952 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 3.521 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6348 _exptl_absorpt_correction_T_max 0.6479 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14337 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0097 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1270 _reflns_number_gt 1268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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 '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^)+(0.0609P)^2^+6.9168P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(4) _refine_ls_number_reflns 1270 _refine_ls_number_parameters 114 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.003 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 0.64064(7) 0.39604(7) 0.19823(6) 0.0179(2) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 0.5000 0.0180(3) Uani 1 4 d S . . P1 P 0.38461(15) 0.32716(14) 0.32088(11) 0.0192(3) Uani 1 1 d . . . P2 P 0.5000 0.5000 0.0000 0.0188(6) Uani 1 4 d S . . O1 O 0.5588(5) 0.3858(5) 0.0648(3) 0.0285(10) Uani 1 1 d . . . O2 O 0.8165(4) 0.3101(4) 0.1788(4) 0.0291(10) Uani 1 1 d . . . O3 O 0.6765(5) 0.5830(4) 0.2380(3) 0.0295(10) Uani 1 1 d . . . O4 O 0.5366(4) 0.3050(5) 0.3012(4) 0.0301(10) Uani 1 1 d . . . O5 O 0.3668(5) 0.3931(5) 0.4247(3) 0.0320(10) Uani 1 1 d . . . N1 N 0.5000 0.0000 0.7399(12) 0.092(5) Uani 1 2 d S . . H1A H 0.4467 0.0515 0.7792 0.110 Uiso 0.50 1 d PR . . H1B H 0.4497 -0.0521 0.6989 0.110 Uiso 0.50 1 d PR . . N2Q N 0.170(2) 0.316(3) 0.5583(17) 0.083(10) Uani 0.38 1 d PD . . H2QC H 0.1703 0.2847 0.6218 0.125 Uiso 0.38 1 d PR . . H2QD H 0.1618 0.2454 0.5156 0.125 Uiso 0.38 1 d PR . . H2QE H 0.2487 0.3590 0.5460 0.125 Uiso 0.38 1 d PR . . N3Q N -0.1712(13) 0.3101(12) 0.4357(9) 0.017(3) Uani 0.38 1 d PDU . . H3QC H -0.2188 0.2671 0.3878 0.025 Uiso 0.38 1 d PR . . H3QD H -0.1173 0.2504 0.4675 0.025 Uiso 0.38 1 d PR . . H3QE H -0.2285 0.3477 0.4802 0.025 Uiso 0.38 1 d PR . . C1Q C 0.035(4) 0.434(3) 0.5401(17) 0.082(11) Uani 0.38 1 d PDU . . H1QA H 0.0464 0.5029 0.5901 0.098 Uiso 0.38 1 d PR . . H1QB H -0.0444 0.3842 0.5583 0.098 Uiso 0.38 1 d PR . . C2Q C 0.0000 0.5000 0.4499(12) 0.098(10) Uani 0.75 2 d SPDU . . H2QA H 0.0822 0.5226 0.4154 0.118 Uiso 0.38 1 d PR . . H2QB H -0.0461 0.5829 0.4655 0.118 Uiso 0.38 1 d PR . . C3Q C -0.0831(19) 0.4184(18) 0.3871(11) 0.030(4) Uani 0.38 1 d PDU . . H3QA H -0.1424 0.4786 0.3515 0.036 Uiso 0.38 1 d PR . . H3QB H -0.0255 0.3763 0.3382 0.036 Uiso 0.38 1 d PR . . 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 0.0186(4) 0.0164(4) 0.0188(4) 0.0022(3) 0.0018(3) 0.0028(3) Co2 0.0179(5) 0.0179(5) 0.0182(8) 0.000 0.000 0.000 P1 0.0204(7) 0.0177(7) 0.0194(7) 0.0006(5) -0.0002(6) -0.0058(5) P2 0.0201(9) 0.0201(9) 0.0163(14) 0.000 0.000 0.000 O1 0.042(3) 0.024(2) 0.019(2) 0.0026(18) -0.0045(19) 0.0073(19) O2 0.023(2) 0.022(2) 0.042(2) 0.003(2) 0.003(2) 0.0077(17) O3 0.039(3) 0.019(2) 0.031(2) -0.0032(19) 0.008(2) -0.0004(18) O4 0.021(2) 0.039(2) 0.031(2) 0.010(2) 0.0012(19) -0.0049(18) O5 0.030(2) 0.040(3) 0.025(2) -0.0127(19) 0.0032(19) -0.012(2) N1 0.113(12) 0.087(10) 0.076(9) 0.000 0.000 -0.020(10) N2Q 0.079(16) 0.11(2) 0.062(13) -0.070(15) 0.047(13) -0.077(15) N3Q 0.029(7) 0.011(5) 0.010(5) -0.007(4) 0.003(5) 0.007(5) C1Q 0.13(3) 0.064(17) 0.052(13) -0.027(13) 0.001(17) -0.05(2) C2Q 0.120(19) 0.13(2) 0.044(9) 0.000 0.000 0.116(17) C3Q 0.041(10) 0.034(9) 0.014(6) -0.012(7) -0.007(7) 0.024(8) _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 1.936(4) . ? Co1 O2 1.951(4) . ? Co1 O3 1.954(4) . ? Co1 O1 1.957(5) . ? Co2 O5 1.963(5) . ? Co2 O5 1.963(5) 2_665 ? Co2 O5 1.963(5) 4_656 ? Co2 O5 1.963(5) 3_566 ? P1 O2 1.514(4) 6_455 ? P1 O4 1.540(4) . ? P1 O3 1.541(4) 2_665 ? P1 O5 1.541(4) . ? P2 O1 1.535(4) 3_565 ? P2 O1 1.535(4) 4_655 ? P2 O1 1.535(4) 2_665 ? P2 O1 1.535(4) . ? O2 P1 1.514(4) 6 ? O3 P1 1.541(4) 2_665 ? N2Q C1Q 1.79(5) . ? N3Q C3Q 1.52(2) . ? C1Q C2Q 1.41(2) . ? C1Q C1Q 1.49(7) 2_565 ? C2Q C1Q 1.41(2) 2_565 ? C2Q C3Q 1.423(17) . ? C2Q C3Q 1.423(17) 2_565 ? 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 O2 111.39(19) . . ? O4 Co1 O3 110.1(2) . . ? O2 Co1 O3 106.6(2) . . ? O4 Co1 O1 113.7(2) . . ? O2 Co1 O1 103.0(2) . . ? O3 Co1 O1 111.7(2) . . ? O5 Co2 O5 118.5(3) . 2_665 ? O5 Co2 O5 105.14(13) . 4_656 ? O5 Co2 O5 105.14(13) 2_665 4_656 ? O5 Co2 O5 105.14(13) . 3_566 ? O5 Co2 O5 105.14(13) 2_665 3_566 ? O5 Co2 O5 118.5(3) 4_656 3_566 ? O2 P1 O4 107.9(3) 6_455 . ? O2 P1 O3 110.1(3) 6_455 2_665 ? O4 P1 O3 110.0(3) . 2_665 ? O2 P1 O5 109.0(3) 6_455 . ? O4 P1 O5 109.0(3) . . ? O3 P1 O5 110.9(3) 2_665 . ? O1 P2 O1 111.6(3) 3_565 4_655 ? O1 P2 O1 108.44(16) 3_565 2_665 ? O1 P2 O1 108.44(16) 4_655 2_665 ? O1 P2 O1 108.44(16) 3_565 . ? O1 P2 O1 108.44(16) 4_655 . ? O1 P2 O1 111.6(3) 2_665 . ? P2 O1 Co1 129.0(3) . . ? P1 O2 Co1 141.7(3) 6 . ? P1 O3 Co1 131.9(3) 2_665 . ? P1 O4 Co1 124.9(3) . . ? P1 O5 Co2 127.6(3) . . ? C2Q C1Q C1Q 58.3(14) . 2_565 ? C2Q C1Q N2Q 127(2) . . ? C1Q C1Q N2Q 158(3) 2_565 . ? C1Q C2Q C1Q 63(3) 2_565 . ? C1Q C2Q C3Q 128.3(16) 2_565 . ? C1Q C2Q C3Q 112.4(13) . . ? C1Q C2Q C3Q 112.4(13) 2_565 2_565 ? C1Q C2Q C3Q 128.3(16) . 2_565 ? C3Q C2Q C3Q 107.9(19) . 2_565 ? C2Q C3Q N3Q 118.5(12) . . ? 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 N1 H1A O2 0.90 1.96 2.825(8) 161.0 3_566 N1 H1A O4 0.90 2.65 3.144(6) 115.3 7 N2Q H2QC O3 0.90 2.07 2.89(3) 151.6 8_445 N2Q H2QD O1 0.90 1.97 2.804(18) 154.2 6_455 N2Q H2QE O5 0.90 2.02 2.74(2) 136.1 . N3Q H3QD O1 0.90 2.24 2.985(14) 139.7 6_455 N3Q H3QE O5 0.90 2.07 2.930(13) 159.2 4_556 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.746 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.152