# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Xintao Wu' _publ_contact_author_email WXT@FJIRSM.AC.CN _publ_section_title ; Syntheses, crystal structures, thermal stabilities, luminescence and magnetism of two 3D pillared metal phosphonates ; loop_ _publ_author_name 'Xintao Wu' 'Rui-Biao Fu' 'Sheng-min Hu' # Attachment '1.CIF' data_f1 _database_code_depnum_ccdc_archive 'CCDC 727228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H16 Mn3 N3 O12 P2' _chemical_formula_weight 705.11 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' Mn Mn 0.3368 0.7283 '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 8.652(3) _cell_length_b 10.293(3) _cell_length_c 14.164(4) _cell_angle_alpha 106.843(3) _cell_angle_beta 97.861(2) _cell_angle_gamma 100.576(3) _cell_volume 1162.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2715 _cell_measurement_theta_min 2.1280 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.817 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6209 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _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 9018 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5242 _reflns_number_gt 4164 _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^)+(0.0510P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5242 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Mn1 Mn 0.50234(3) 0.24997(3) 0.492470(19) 0.01512(9) Uani 1 1 d . . . Mn2 Mn 1.10024(3) 0.22290(3) 0.602373(18) 0.01241(9) Uani 1 1 d . . . Mn3 Mn 0.89808(3) 0.27355(3) 0.397821(18) 0.01248(9) Uani 1 1 d . . . P1 P 0.73986(5) 0.54011(5) 0.48886(3) 0.01042(11) Uani 1 1 d . . . P2 P 0.73716(5) 0.03582(5) 0.48653(3) 0.01031(11) Uani 1 1 d . . . O1 O 0.59395(14) 0.58016(13) 0.44555(9) 0.0154(3) Uani 1 1 d . . . O2 O 1.10539(14) 0.38231(13) 0.53176(9) 0.0139(3) Uani 1 1 d . . . O3 O 0.72487(14) 0.38212(13) 0.45668(9) 0.0134(3) Uani 1 1 d . . . O4 O 1.06388(15) 0.40825(14) 0.33598(9) 0.0156(3) Uani 1 1 d . . . H2 H 1.069(3) 0.497(3) 0.3404(17) 0.028(6) Uiso 1 1 d . . . O5 O 0.65479(15) 0.79968(14) 0.65236(9) 0.0178(3) Uani 1 1 d . . . O6 O 1.07761(15) 0.15877(13) 0.32291(9) 0.0155(3) Uani 1 1 d . . . O7 O 0.59262(14) 0.07457(13) 0.43999(9) 0.0151(3) Uani 1 1 d . . . O8 O 0.27678(14) 0.12174(13) 0.54162(9) 0.0136(3) Uani 1 1 d . . . O9 O 0.89344(14) 0.11223(13) 0.46622(9) 0.0145(3) Uani 1 1 d . . . O10 O 0.92907(15) 0.09047(15) 0.66322(9) 0.0154(3) Uani 1 1 d . . . H4 H 0.920(3) 0.004(3) 0.6613(19) 0.036(7) Uiso 1 1 d . . . O11 O 0.65411(15) 0.30023(14) 0.64048(9) 0.0171(3) Uani 1 1 d . . . O12 O 0.92134(14) 0.34011(13) 0.67421(9) 0.0161(3) Uani 1 1 d . . . N1 N 1.25452(19) 0.3204(2) 0.75753(12) 0.0245(4) Uani 1 1 d . . . N2 N 0.7272(2) 0.16492(19) 0.24958(12) 0.0237(4) Uani 1 1 d . . . N3 N 0.8661(4) 0.2958(4) -0.0287(2) 0.0841(10) Uani 1 1 d . . . C1 C 0.7786(2) 0.60596(19) 0.62770(12) 0.0124(3) Uani 1 1 d . . . H1 H 0.700(2) 0.563(2) 0.6529(15) 0.014(5) Uiso 1 1 d . . . C2 C 0.7841(2) 0.76104(19) 0.65623(12) 0.0127(3) Uani 1 1 d . . . C3 C 0.7732(2) 0.10578(19) 0.62496(12) 0.0119(3) Uani 1 1 d . . . H3 H 0.686(2) 0.065(2) 0.6504(14) 0.011(5) Uiso 1 1 d . . . C4 C 0.7824(2) 0.26076(19) 0.65058(12) 0.0118(3) Uani 1 1 d . . . C5 C 1.4112(3) 0.3464(4) 0.77298(17) 0.0650(11) Uani 1 1 d . . . H5 H 1.452(3) 0.316(3) 0.718(2) 0.073(9) Uiso 1 1 d . . . C6 C 1.5117(3) 0.4161(4) 0.86575(17) 0.0665(11) Uani 1 1 d . . . H6 H 1.627(4) 0.440(4) 0.872(3) 0.110(13) Uiso 1 1 d . . . C7 C 1.4486(2) 0.4617(2) 0.94925(14) 0.0241(5) Uani 1 1 d . . . C8 C 1.2846(3) 0.4294(4) 0.93390(16) 0.0523(8) Uani 1 1 d . . . H7 H 1.238(4) 0.457(3) 0.992(2) 0.082(10) Uiso 1 1 d . . . C9 C 1.1929(3) 0.3591(3) 0.83892(16) 0.0484(8) Uani 1 1 d . . . H8 H 1.072(4) 0.323(4) 0.826(3) 0.106(12) Uiso 1 1 d . . . C10 C 0.6411(4) 0.2314(3) 0.20321(19) 0.0525(8) Uani 1 1 d . . . H9 H 0.639(4) 0.326(4) 0.242(2) 0.082(11) Uiso 1 1 d . . . C11 C 0.5524(4) 0.1708(3) 0.1064(2) 0.0598(9) Uani 1 1 d . . . H20 H 0.494(4) 0.227(3) 0.080(2) 0.071(9) Uiso 1 1 d . . . C12 C 0.5464(3) 0.0343(2) 0.05270(14) 0.0268(5) Uani 1 1 d . . . C13 C 0.6326(3) -0.0347(3) 0.10215(18) 0.0453(7) Uani 1 1 d . . . H21 H 0.634(3) -0.129(3) 0.067(2) 0.066(9) Uiso 1 1 d . . . C14 C 0.7201(3) 0.0335(3) 0.19900(18) 0.0436(6) Uani 1 1 d . . . H22 H 0.791(3) -0.019(3) 0.2298(19) 0.059(8) Uiso 1 1 d . . . C15 C 0.9588(5) 0.3001(5) 0.0563(3) 0.0852(12) Uani 1 1 d . . . H23 H 0.983(5) 0.402(5) 0.112(3) 0.125(15) Uiso 1 1 d . . . C16 C 1.0109(5) 0.1890(4) 0.0709(3) 0.0726(10) Uani 1 1 d . . . H24 H 1.081(4) 0.200(4) 0.135(2) 0.090(12) Uiso 1 1 d . . . C17 C 0.9726(3) 0.0617(3) -0.00594(19) 0.0553(8) Uani 1 1 d . . . C18 C 0.8757(5) 0.0580(5) -0.0939(2) 0.0738(11) Uani 1 1 d . . . H25 H 0.842(4) -0.028(4) -0.146(3) 0.099(13) Uiso 1 1 d . . . C19 C 0.8265(5) 0.1742(5) -0.1007(3) 0.0839(12) Uani 1 1 d . . . H26 H 0.762(4) 0.169(4) -0.166(3) 0.105(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 Mn1 0.01121(16) 0.01195(17) 0.02132(16) 0.00375(12) 0.00056(11) 0.00529(12) Mn2 0.01002(15) 0.01285(16) 0.01388(14) 0.00393(11) 0.00104(10) 0.00315(11) Mn3 0.01020(15) 0.01251(16) 0.01404(14) 0.00390(11) 0.00079(10) 0.00288(11) P1 0.0091(2) 0.0076(2) 0.0140(2) 0.00313(17) 0.00185(16) 0.00158(17) P2 0.0090(2) 0.0077(2) 0.0142(2) 0.00342(17) 0.00213(16) 0.00210(17) O1 0.0127(6) 0.0124(7) 0.0206(6) 0.0044(5) 0.0018(5) 0.0046(5) O2 0.0105(6) 0.0128(7) 0.0181(6) 0.0054(5) 0.0034(5) 0.0010(5) O3 0.0121(6) 0.0079(6) 0.0188(6) 0.0031(5) 0.0031(5) 0.0013(5) O4 0.0136(6) 0.0100(7) 0.0224(7) 0.0061(5) -0.0013(5) 0.0030(5) O5 0.0141(6) 0.0174(7) 0.0204(6) 0.0022(5) 0.0022(5) 0.0071(5) O6 0.0132(6) 0.0104(7) 0.0224(6) 0.0051(5) 0.0031(5) 0.0021(5) O7 0.0127(6) 0.0122(7) 0.0201(6) 0.0044(5) 0.0016(5) 0.0044(5) O8 0.0117(6) 0.0076(6) 0.0207(6) 0.0037(5) 0.0033(5) 0.0018(5) O9 0.0111(6) 0.0134(7) 0.0190(6) 0.0060(5) 0.0035(5) 0.0011(5) O10 0.0128(6) 0.0119(7) 0.0211(6) 0.0067(5) -0.0009(5) 0.0031(5) O11 0.0129(6) 0.0171(7) 0.0213(6) 0.0036(6) 0.0030(5) 0.0080(5) O12 0.0126(6) 0.0104(7) 0.0242(7) 0.0058(5) 0.0023(5) 0.0008(5) N1 0.0160(8) 0.0363(11) 0.0157(8) 0.0023(7) -0.0007(6) 0.0056(8) N2 0.0225(9) 0.0255(10) 0.0177(8) 0.0028(7) -0.0020(6) 0.0037(7) N3 0.111(3) 0.091(3) 0.0573(18) 0.0204(18) 0.0336(17) 0.032(2) C1 0.0116(8) 0.0109(9) 0.0151(8) 0.0050(7) 0.0026(6) 0.0022(7) C2 0.0137(9) 0.0133(9) 0.0104(7) 0.0028(7) 0.0019(6) 0.0038(7) C3 0.0098(8) 0.0110(9) 0.0154(8) 0.0048(7) 0.0021(6) 0.0031(7) C4 0.0140(9) 0.0115(9) 0.0106(7) 0.0033(7) 0.0030(6) 0.0044(7) C5 0.0168(12) 0.132(3) 0.0195(11) -0.0101(15) 0.0038(9) 0.0082(15) C6 0.0146(12) 0.132(3) 0.0230(12) -0.0095(15) 0.0021(9) 0.0025(15) C7 0.0172(10) 0.0326(13) 0.0170(9) 0.0026(9) -0.0012(8) 0.0041(9) C8 0.0212(12) 0.098(3) 0.0187(10) -0.0045(13) 0.0021(9) 0.0081(13) C9 0.0179(12) 0.088(2) 0.0210(10) -0.0024(12) -0.0007(9) 0.0044(12) C10 0.069(2) 0.0375(16) 0.0338(13) -0.0068(12) -0.0244(12) 0.0270(15) C11 0.087(2) 0.0382(17) 0.0358(14) -0.0063(12) -0.0309(14) 0.0315(16) C12 0.0252(11) 0.0286(12) 0.0190(10) 0.0021(9) -0.0046(8) 0.0035(9) C13 0.0628(18) 0.0257(14) 0.0317(12) -0.0014(11) -0.0170(11) 0.0094(13) C14 0.0583(17) 0.0298(14) 0.0317(12) 0.0047(11) -0.0180(11) 0.0117(12) C15 0.102(3) 0.076(3) 0.063(2) 0.008(2) 0.012(2) 0.010(2) C16 0.080(3) 0.072(3) 0.0493(19) 0.0121(18) -0.0001(17) 0.001(2) C17 0.0580(18) 0.071(2) 0.0330(13) 0.0130(14) 0.0213(12) 0.0038(16) C18 0.099(3) 0.085(3) 0.0331(16) 0.0058(18) 0.0195(16) 0.027(2) C19 0.099(3) 0.120(4) 0.0419(19) 0.025(2) 0.0263(19) 0.041(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 Mn1 O7 2.0786(14) . ? Mn1 O1 2.0898(14) 2_666 ? Mn1 O5 2.1661(14) 2_666 ? Mn1 O11 2.1807(14) . ? Mn1 O3 2.3492(13) . ? Mn1 O8 2.4481(13) . ? Mn2 O8 2.1405(13) 1_655 ? Mn2 O2 2.1520(13) . ? Mn2 N1 2.2464(17) . ? Mn2 O10 2.2544(14) . ? Mn2 O9 2.2918(13) . ? Mn2 O12 2.3003(13) . ? Mn3 O3 2.1462(13) . ? Mn3 O9 2.1485(13) . ? Mn3 N2 2.2423(17) . ? Mn3 O4 2.2505(14) . ? Mn3 O2 2.2739(13) . ? Mn3 O6 2.3091(13) . ? P1 O1 1.5052(13) . ? P1 O3 1.5317(14) . ? P1 O2 1.5379(13) 2_766 ? P1 C1 1.8446(18) . ? P2 O7 1.5057(13) . ? P2 O8 1.5310(14) 2_656 ? P2 O9 1.5416(13) . ? P2 C3 1.8419(18) . ? O1 Mn1 2.0898(14) 2_666 ? O2 P1 1.5379(12) 2_766 ? O4 C1 1.438(2) 2_766 ? O5 C2 1.254(2) . ? O5 Mn1 2.1661(14) 2_666 ? O6 C2 1.264(2) 2_766 ? O8 P2 1.5310(14) 2_656 ? O8 Mn2 2.1405(13) 1_455 ? O10 C3 1.437(2) . ? O11 C4 1.254(2) . ? O12 C4 1.263(2) . ? N1 C5 1.307(3) . ? N1 C9 1.324(3) . ? N2 C14 1.321(3) . ? N2 C10 1.330(3) . ? N3 C19 1.316(5) . ? N3 C15 1.336(5) . ? C1 O4 1.438(2) 2_766 ? C1 C2 1.519(3) . ? C2 O6 1.264(2) 2_766 ? C3 C4 1.514(3) . ? C5 C6 1.382(3) . ? C6 C7 1.366(3) . ? C7 C8 1.368(3) . ? C7 C7 1.488(4) 2_867 ? C8 C9 1.377(3) . ? C10 C11 1.378(3) . ? C11 C12 1.378(3) . ? C12 C13 1.376(3) . ? C12 C12 1.492(4) 2_655 ? C13 C14 1.382(3) . ? C15 C16 1.362(5) . ? C16 C17 1.389(5) . ? C17 C18 1.390(4) . ? C17 C17 1.480(6) 2_755 ? C18 C19 1.365(6) . ? 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 O7 Mn1 O1 175.30(4) . 2_666 ? O7 Mn1 O5 91.19(5) . 2_666 ? O1 Mn1 O5 91.33(5) 2_666 2_666 ? O7 Mn1 O11 89.85(5) . . ? O1 Mn1 O11 87.53(5) 2_666 . ? O5 Mn1 O11 178.23(4) 2_666 . ? O7 Mn1 O3 88.30(5) . . ? O1 Mn1 O3 95.36(5) 2_666 . ? O5 Mn1 O3 96.46(5) 2_666 . ? O11 Mn1 O3 85.00(5) . . ? O7 Mn1 O8 93.48(5) . . ? O1 Mn1 O8 82.70(5) 2_666 . ? O5 Mn1 O8 86.89(5) 2_666 . ? O11 Mn1 O8 91.61(5) . . ? O3 Mn1 O8 176.17(4) . . ? O8 Mn2 O2 101.39(5) 1_655 . ? O8 Mn2 N1 93.73(6) 1_655 . ? O2 Mn2 N1 107.91(6) . . ? O8 Mn2 O10 113.43(5) 1_655 . ? O2 Mn2 O10 140.06(5) . . ? N1 Mn2 O10 89.31(6) . . ? O8 Mn2 O9 96.83(5) 1_655 . ? O2 Mn2 O9 79.70(5) . . ? N1 Mn2 O9 165.52(5) . . ? O10 Mn2 O9 77.41(5) . . ? O8 Mn2 O12 176.95(5) 1_655 . ? O2 Mn2 O12 78.38(5) . . ? N1 Mn2 O12 83.49(6) . . ? O10 Mn2 O12 67.86(5) . . ? O9 Mn2 O12 86.13(5) . . ? O3 Mn3 O9 104.39(5) . . ? O3 Mn3 N2 91.20(6) . . ? O9 Mn3 N2 103.06(6) . . ? O3 Mn3 O4 109.82(5) . . ? O9 Mn3 O4 141.17(5) . . ? N2 Mn3 O4 94.17(6) . . ? O3 Mn3 O2 97.25(5) . . ? O9 Mn3 O2 80.18(5) . . ? N2 Mn3 O2 169.94(5) . . ? O4 Mn3 O2 77.85(5) . . ? O3 Mn3 O6 175.66(4) . . ? O9 Mn3 O6 79.01(5) . . ? N2 Mn3 O6 85.35(6) . . ? O4 Mn3 O6 67.89(5) . . ? O2 Mn3 O6 85.95(5) . . ? O1 P1 O3 113.47(7) . . ? O1 P1 O2 111.79(7) . 2_766 ? O3 P1 O2 111.79(7) . 2_766 ? O1 P1 C1 110.35(8) . . ? O3 P1 C1 107.59(8) . . ? O2 P1 C1 101.05(8) 2_766 . ? O7 P2 O8 114.05(7) . 2_656 ? O7 P2 O9 111.47(7) . . ? O8 P2 O9 111.88(7) 2_656 . ? O7 P2 C3 110.65(7) . . ? O8 P2 C3 107.00(8) 2_656 . ? O9 P2 C3 100.90(7) . . ? P1 O1 Mn1 129.23(8) . 2_666 ? P1 O2 Mn2 123.10(7) 2_766 . ? P1 O2 Mn3 116.92(7) 2_766 . ? Mn2 O2 Mn3 100.28(5) . . ? P1 O3 Mn3 126.64(7) . . ? P1 O3 Mn1 115.90(7) . . ? Mn3 O3 Mn1 117.09(6) . . ? C1 O4 Mn3 104.51(10) 2_766 . ? C2 O5 Mn1 119.28(11) . 2_666 ? C2 O6 Mn3 111.26(11) 2_766 . ? P2 O7 Mn1 129.57(8) . . ? P2 O8 Mn2 123.81(7) 2_656 1_455 ? P2 O8 Mn1 114.73(6) 2_656 . ? Mn2 O8 Mn1 121.04(6) 1_455 . ? P2 O9 Mn3 122.12(7) . . ? P2 O9 Mn2 116.72(7) . . ? Mn3 O9 Mn2 99.83(5) . . ? C3 O10 Mn2 104.60(10) . . ? C4 O11 Mn1 121.30(11) . . ? C4 O12 Mn2 110.62(11) . . ? C5 N1 C9 115.65(19) . . ? C5 N1 Mn2 122.14(14) . . ? C9 N1 Mn2 122.18(14) . . ? C14 N2 C10 116.4(2) . . ? C14 N2 Mn3 120.68(15) . . ? C10 N2 Mn3 122.57(16) . . ? C19 N3 C15 115.4(4) . . ? O4 C1 C2 107.54(14) 2_766 . ? O4 C1 P1 107.59(11) 2_766 . ? C2 C1 P1 105.91(11) . . ? O5 C2 O6 125.06(17) . 2_766 ? O5 C2 C1 119.05(16) . . ? O6 C2 C1 115.77(15) 2_766 . ? O10 C3 C4 107.30(14) . . ? O10 C3 P2 107.40(11) . . ? C4 C3 P2 105.91(11) . . ? O11 C4 O12 124.83(17) . . ? O11 C4 C3 118.54(16) . . ? O12 C4 C3 116.44(15) . . ? N1 C5 C6 124.4(2) . . ? C7 C6 C5 120.1(2) . . ? C6 C7 C8 115.6(2) . . ? C6 C7 C7 122.3(2) . 2_867 ? C8 C7 C7 122.1(2) . 2_867 ? C7 C8 C9 120.7(2) . . ? N1 C9 C8 123.5(2) . . ? N2 C10 C11 123.1(3) . . ? C12 C11 C10 120.7(2) . . ? C13 C12 C11 115.8(2) . . ? C13 C12 C12 121.9(3) . 2_655 ? C11 C12 C12 122.3(3) . 2_655 ? C12 C13 C14 120.2(2) . . ? N2 C14 C13 123.8(2) . . ? N3 C15 C16 124.3(4) . . ? C15 C16 C17 120.4(3) . . ? C16 C17 C18 114.9(3) . . ? C16 C17 C17 122.5(3) . 2_755 ? C18 C17 C17 122.6(4) . 2_755 ? C19 C18 C17 120.4(4) . . ? N3 C19 C18 124.6(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 O4 H2 O12 0.89(3) 1.74(3) 2.617(2) 170(2) 2_766 O10 H4 O6 0.87(3) 1.75(3) 2.620(2) 171(2) 2_756 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.435 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.082 # Attachment '2.CIF' data_f2 _database_code_depnum_ccdc_archive 'CCDC 727229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H20 Co3 N3 O14 P2' _chemical_formula_weight 753.11 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 triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9725(11) _cell_length_b 10.5369(10) _cell_length_c 14.1184(16) _cell_angle_alpha 90.477(4) _cell_angle_beta 109.924(4) _cell_angle_gamma 98.596(4) _cell_volume 1376.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3288 _cell_measurement_theta_min 3.0755 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.976 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8306 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear Version 1.35 (Rigaku Corporation)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _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 10558 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6190 _reflns_number_gt 5212 _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^)+(0.0762P)^2^+4.3448P] 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 6190 _refine_ls_number_parameters 517 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.58392(5) 0.27034(5) 0.00512(4) 0.01938(15) Uani 1 1 d . . . Co2 Co 0.04168(5) 0.17515(5) -0.10084(4) 0.01571(15) Uani 1 1 d . . . Co3 Co 0.13496(5) 0.31672(5) 0.12657(4) 0.01554(15) Uani 1 1 d . . . P1 P -0.16151(10) 0.09710(9) 0.03292(7) 0.0136(2) Uani 1 1 d . . . P2 P 0.31476(10) 0.41666(9) -0.01550(8) 0.0143(2) Uani 1 1 d . . . O1 O -0.0035(3) 0.1551(3) 0.0483(2) 0.0178(5) Uani 1 1 d . . . O2 O -0.1719(3) -0.0399(2) 0.0664(2) 0.0175(5) Uani 1 1 d . . . O3 O -0.2396(3) 0.1807(3) 0.0743(2) 0.0219(6) Uani 1 1 d . . . O4 O -0.1548(3) 0.0374(3) -0.1507(2) 0.0209(6) Uani 1 1 d . . . O5 O -0.1317(3) 0.2843(3) -0.1490(2) 0.0201(6) Uani 1 1 d . . . O6 O 0.6558(3) 0.2869(3) -0.1302(2) 0.0232(6) Uani 1 1 d . . . O7 O 0.1692(3) 0.3354(3) -0.0227(2) 0.0171(5) Uani 1 1 d . . . O8 O 0.4008(3) 0.3518(3) -0.0648(2) 0.0200(6) Uani 1 1 d . . . O9 O 0.2903(3) 0.5504(3) -0.0500(2) 0.0200(6) Uani 1 1 d . . . O10 O 0.3164(3) 0.4686(3) 0.1700(2) 0.0191(6) Uani 1 1 d . . . O11 O 0.3144(3) 0.2221(3) 0.1700(2) 0.0209(6) Uani 1 1 d . . . O12 O 0.5148(4) 0.2334(3) 0.1318(3) 0.0363(9) Uani 1 1 d . . . O13 O -0.0039(3) 0.4463(3) 0.1007(3) 0.0274(7) Uani 1 1 d . . . O14 O 0.4521(4) 0.0967(3) -0.0652(3) 0.0395(9) Uani 1 1 d . . . C1 C -0.2445(4) 0.0909(4) -0.1054(3) 0.0178(7) Uani 1 1 d . . . H1A H -0.3432 0.0430 -0.1288 0.021 Uiso 1 1 calc R . . C2 C 0.7585(4) 0.2311(4) -0.1317(3) 0.0168(7) Uani 1 1 d . . . C3 C 0.4071(4) 0.4218(4) 0.1218(3) 0.0179(7) Uani 1 1 d . . . H3A H 0.5034 0.4743 0.1429 0.022 Uiso 1 1 calc R . . C4 C 0.4145(4) 0.2816(4) 0.1444(3) 0.0197(8) Uani 1 1 d . . . N1 N 0.0654(4) 0.1979(4) -0.2437(3) 0.0269(8) Uani 0.70 1 d P . 1 C5 C 0.0927(11) 0.1078(8) -0.2940(6) 0.046(2) Uani 0.70 1 d P . 1 H5A H 0.1084 0.0306 -0.2639 0.055 Uiso 0.70 1 calc PR . 1 C6 C 0.0999(11) 0.1192(8) -0.3893(6) 0.046(2) Uani 0.70 1 d P . 1 H6A H 0.1188 0.0499 -0.4212 0.055 Uiso 0.70 1 calc PR . 1 C7 C 0.0805(6) 0.2267(5) -0.4366(4) 0.0339(11) Uani 0.70 1 d P . 1 C8 C 0.0578(16) 0.3276(10) -0.3819(8) 0.079(4) Uani 0.70 1 d P . 1 H8A H 0.0487 0.4073 -0.4090 0.095 Uiso 0.70 1 calc PR . 1 C9 C 0.0489(13) 0.3085(9) -0.2880(7) 0.063(3) Uani 0.70 1 d P . 1 H9A H 0.0305 0.3759 -0.2537 0.076 Uiso 0.70 1 calc PR . 1 N1A N 0.0654(4) 0.1979(4) -0.2437(3) 0.0269(8) Uani 0.30 1 d P . 2 C5A C 0.1878(18) 0.203(2) -0.2614(13) 0.040(4) Uani 0.30 1 d P . 2 H5AA H 0.2726 0.2007 -0.2073 0.048 Uiso 0.30 1 calc PR . 2 C6A C 0.1943(19) 0.211(2) -0.3581(14) 0.045(5) Uani 0.30 1 d P . 2 H6AA H 0.2809 0.2046 -0.3678 0.053 Uiso 0.30 1 calc PR . 2 C7A C 0.0805(6) 0.2267(5) -0.4366(4) 0.0339(11) Uani 0.30 1 d P . 2 C8A C -0.0519(19) 0.204(2) -0.4216(13) 0.046(5) Uani 0.30 1 d P . 2 H8AA H -0.1372 0.1983 -0.4767 0.055 Uiso 0.30 1 calc PR . 2 C9A C -0.058(2) 0.190(2) -0.3270(12) 0.046(5) Uani 0.30 1 d P . 2 H9AA H -0.1474 0.1752 -0.3187 0.056 Uiso 0.30 1 calc PR . 2 N2 N 0.1073(4) 0.2788(4) 0.2682(3) 0.0273(8) Uani 0.70 1 d P . 1 C10 C -0.0004(9) 0.3156(9) 0.2930(6) 0.046(2) Uani 0.70 1 d P . 1 H10A H -0.0702 0.3531 0.2450 0.056 Uiso 0.70 1 calc PR . 1 C11 C -0.0111(10) 0.2994(10) 0.3880(6) 0.053(2) Uani 0.70 1 d P . 1 H11A H -0.0867 0.3272 0.4023 0.064 Uiso 0.70 1 calc PR . 1 C12 C 0.0891(6) 0.2426(5) 0.4613(4) 0.0356(11) Uani 0.70 1 d P . 1 C13 C 0.1807(10) 0.1843(9) 0.4279(6) 0.047(2) Uani 0.70 1 d P . 1 H13A H 0.2388 0.1310 0.4692 0.056 Uiso 0.70 1 calc PR . 1 C14 C 0.1861(10) 0.2056(9) 0.3316(6) 0.047(2) Uani 0.70 1 d P . 1 H14A H 0.2495 0.1655 0.3112 0.056 Uiso 0.70 1 calc PR . 1 N2A N 0.1073(4) 0.2788(4) 0.2682(3) 0.0273(8) Uani 0.30 1 d P . 2 C10A C 0.045(3) 0.1769(18) 0.2939(14) 0.049(5) Uani 0.30 1 d P . 2 H10B H 0.0026 0.1092 0.2452 0.059 Uiso 0.30 1 calc PR . 2 C11A C 0.036(3) 0.1596(19) 0.3888(15) 0.058(6) Uani 0.30 1 d P . 2 H11B H -0.0132 0.0817 0.3993 0.070 Uiso 0.30 1 calc PR . 2 C12A C 0.0891(6) 0.2426(5) 0.4613(4) 0.0356(11) Uani 0.30 1 d P . 2 C13A C 0.167(3) 0.366(2) 0.4412(15) 0.079(10) Uani 0.30 1 d P . 2 H13B H 0.2140 0.4308 0.4917 0.095 Uiso 0.30 1 calc PR . 2 C14A C 0.166(3) 0.379(2) 0.3433(13) 0.061(7) Uani 0.30 1 d P . 2 H14B H 0.2069 0.4570 0.3270 0.073 Uiso 0.30 1 calc PR . 2 N3 N 0.4167(13) 0.0760(12) 0.7205(8) 0.089(4) Uani 0.50 1 d PGU A 1 C15 C 0.4103(13) -0.0542(11) 0.6931(9) 0.096(5) Uani 0.50 1 d PGU A 1 H15A H 0.3874 -0.1180 0.7327 0.115 Uiso 0.50 1 calc PR A 1 C16 C 0.4384(15) -0.0876(11) 0.6058(10) 0.095(6) Uani 0.50 1 d PGU A 1 H16A H 0.4342 -0.1736 0.5878 0.113 Uiso 0.50 1 calc PR A 1 C17 C 0.4730(16) 0.0091(13) 0.5458(8) 0.091(6) Uani 0.50 1 d PG . 1 C18 C 0.4794(17) 0.1392(12) 0.5732(9) 0.107(7) Uani 0.50 1 d PG A 1 H18A H 0.5022 0.2031 0.5335 0.128 Uiso 0.50 1 calc PR A 1 C19 C 0.4512(15) 0.1727(11) 0.6605(10) 0.102(7) Uani 0.50 1 d PG A 1 H19A H 0.4554 0.2586 0.6786 0.123 Uiso 0.50 1 calc PR A 1 N4 N 0.3020(18) -0.1079(17) 0.5084(18) 0.063(6) Uani 0.25 1 d PG B 2 C21 C 0.324(2) -0.1334(18) 0.4193(14) 0.094(14) Uani 0.25 1 d PG B 2 H21A H 0.2934 -0.0813 0.3657 0.112 Uiso 0.25 1 calc PR B 2 C22 C 0.390(2) -0.2360(17) 0.4095(11) 0.064(8) Uani 0.25 1 d PG B 2 H22A H 0.4044 -0.2531 0.3493 0.077 Uiso 0.25 1 calc PR B 2 C23 C 0.4345(17) -0.3131(16) 0.4888(11) 0.040(5) Uani 0.25 1 d PG . 2 C24 C 0.413(2) -0.2877(19) 0.5780(14) 0.092(13) Uani 0.25 1 d PG . 2 C25 C 0.347(2) -0.185(2) 0.5877(17) 0.106(15) Uani 0.25 1 d PG B 2 H25A H 0.3322 -0.1679 0.6479 0.128 Uiso 0.25 1 calc PR B 2 N5 N 0.698(2) -0.5963(16) 0.4762(12) 0.079(9) Uani 0.25 1 d PG . 2 C26 C 0.678(2) -0.5665(16) 0.5635(11) 0.075(10) Uani 0.25 1 d PG . 2 C27 C 0.5942(17) -0.4769(15) 0.5660(10) 0.049(6) Uani 0.25 1 d PG . 2 C28 C 0.5311(16) -0.4171(14) 0.4812(10) 0.039(5) Uani 0.25 1 d PGU . 2 C29 C 0.5516(17) -0.4469(16) 0.3940(10) 0.050(6) Uani 0.25 1 d PGU . 2 H29A H 0.5083 -0.4059 0.3359 0.060 Uiso 0.25 1 calc PR . 2 C30 C 0.6352(19) -0.5365(17) 0.3915(10) 0.052(6) Uani 0.25 1 d PGU . 2 H30A H 0.6492 -0.5569 0.3317 0.063 Uiso 0.25 1 calc PR . 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 0.0163(3) 0.0146(3) 0.0338(3) 0.0063(2) 0.0152(2) 0.00665(19) Co2 0.0172(3) 0.0161(3) 0.0166(3) 0.0028(2) 0.0081(2) 0.00570(19) Co3 0.0163(3) 0.0155(3) 0.0177(3) 0.0025(2) 0.0092(2) 0.00339(19) P1 0.0129(4) 0.0122(4) 0.0190(5) 0.0028(3) 0.0089(4) 0.0040(3) P2 0.0126(4) 0.0126(4) 0.0209(5) 0.0037(4) 0.0092(4) 0.0037(3) O1 0.0137(12) 0.0171(13) 0.0249(15) 0.0008(11) 0.0106(11) 0.0002(10) O2 0.0171(12) 0.0132(12) 0.0262(15) 0.0052(11) 0.0115(11) 0.0051(10) O3 0.0231(14) 0.0201(14) 0.0291(16) 0.0044(12) 0.0140(12) 0.0117(11) O4 0.0273(15) 0.0163(13) 0.0225(15) 0.0009(11) 0.0119(12) 0.0064(11) O5 0.0201(13) 0.0161(13) 0.0272(15) 0.0056(11) 0.0111(12) 0.0054(10) O6 0.0224(14) 0.0194(14) 0.0347(17) 0.0074(12) 0.0159(13) 0.0094(11) O7 0.0147(12) 0.0154(12) 0.0223(14) 0.0017(11) 0.0089(11) 0.0004(10) O8 0.0187(13) 0.0212(14) 0.0250(15) 0.0023(11) 0.0119(12) 0.0080(11) O9 0.0179(13) 0.0151(13) 0.0281(15) 0.0057(11) 0.0090(11) 0.0035(10) O10 0.0209(13) 0.0178(13) 0.0228(14) 0.0018(11) 0.0119(11) 0.0055(10) O11 0.0229(14) 0.0172(13) 0.0281(15) 0.0088(11) 0.0141(12) 0.0075(11) O12 0.0407(19) 0.0403(19) 0.052(2) 0.0297(17) 0.0364(17) 0.0296(16) O13 0.0223(14) 0.0227(15) 0.0429(19) 0.0093(14) 0.0150(14) 0.0120(12) O14 0.0289(17) 0.0179(15) 0.084(3) -0.0002(16) 0.0366(19) 0.0005(12) C1 0.0172(17) 0.0142(17) 0.024(2) 0.0026(15) 0.0088(15) 0.0042(13) C2 0.0196(18) 0.0181(18) 0.0145(18) 0.0029(14) 0.0069(14) 0.0064(14) C3 0.0155(17) 0.0193(18) 0.0215(19) 0.0030(15) 0.0090(15) 0.0039(14) C4 0.0184(18) 0.0225(19) 0.023(2) 0.0090(16) 0.0091(15) 0.0111(15) N1 0.035(2) 0.032(2) 0.0204(18) 0.0069(15) 0.0155(16) 0.0122(16) C5 0.094(7) 0.032(4) 0.032(4) 0.008(3) 0.040(4) 0.023(4) C6 0.081(6) 0.041(4) 0.029(4) 0.005(3) 0.034(4) 0.015(4) C7 0.043(3) 0.046(3) 0.023(2) 0.011(2) 0.020(2) 0.016(2) C8 0.165(13) 0.064(6) 0.052(6) 0.033(5) 0.073(8) 0.069(8) C9 0.133(9) 0.048(5) 0.048(5) 0.026(4) 0.066(6) 0.053(6) N1A 0.035(2) 0.032(2) 0.0204(18) 0.0069(15) 0.0155(16) 0.0122(16) C5A 0.030(8) 0.078(14) 0.023(8) 0.020(8) 0.016(7) 0.020(9) C6A 0.028(8) 0.077(14) 0.038(10) 0.010(9) 0.020(8) 0.017(9) C7A 0.043(3) 0.046(3) 0.023(2) 0.011(2) 0.020(2) 0.016(2) C8A 0.029(8) 0.089(16) 0.020(8) 0.008(9) 0.007(7) 0.014(9) C9A 0.039(9) 0.090(16) 0.019(8) 0.020(9) 0.012(7) 0.031(10) N2 0.035(2) 0.035(2) 0.0197(18) 0.0088(15) 0.0163(16) 0.0129(16) C10 0.045(4) 0.081(6) 0.030(4) 0.024(4) 0.025(3) 0.031(4) C11 0.061(5) 0.089(7) 0.030(4) 0.018(4) 0.031(4) 0.038(5) C12 0.045(3) 0.049(3) 0.022(2) 0.010(2) 0.021(2) 0.016(2) C13 0.070(6) 0.062(5) 0.031(4) 0.025(4) 0.033(4) 0.042(5) C14 0.069(6) 0.062(5) 0.030(4) 0.018(4) 0.033(4) 0.036(5) N2A 0.035(2) 0.035(2) 0.0197(18) 0.0088(15) 0.0163(16) 0.0129(16) C10A 0.089(16) 0.031(9) 0.025(9) -0.008(7) 0.027(10) -0.014(9) C11A 0.12(2) 0.037(10) 0.037(11) 0.003(8) 0.050(13) 0.004(11) C12A 0.045(3) 0.049(3) 0.022(2) 0.010(2) 0.021(2) 0.016(2) C13A 0.14(2) 0.061(14) 0.024(9) -0.022(9) 0.046(13) -0.061(15) C14A 0.110(19) 0.049(11) 0.020(8) -0.011(8) 0.036(10) -0.034(12) N3 0.074(7) 0.115(9) 0.079(8) -0.021(7) 0.026(6) 0.024(7) C15 0.075(8) 0.067(8) 0.117(10) 0.036(7) -0.004(7) 0.012(6) C16 0.120(10) 0.086(9) 0.087(9) 0.016(7) 0.043(8) 0.028(8) C17 0.129(17) 0.096(13) 0.043(8) -0.009(9) 0.016(9) 0.034(12) C18 0.16(2) 0.087(14) 0.105(16) 0.030(12) 0.079(16) 0.030(14) C19 0.143(19) 0.098(14) 0.075(12) -0.017(11) 0.065(13) -0.019(13) N4 0.050(13) 0.049(13) 0.10(2) 0.018(13) 0.030(13) 0.021(10) C21 0.063(18) 0.08(2) 0.09(3) 0.009(19) -0.047(18) 0.037(17) C22 0.09(2) 0.054(15) 0.024(11) 0.002(10) -0.012(12) 0.030(15) C23 0.028(9) 0.041(11) 0.029(10) -0.005(9) -0.019(8) 0.013(8) C24 0.08(2) 0.09(2) 0.15(4) 0.05(2) 0.08(2) 0.06(2) C25 0.09(3) 0.10(3) 0.17(5) -0.01(3) 0.10(3) 0.02(2) N5 0.11(2) 0.066(16) 0.046(13) -0.025(12) -0.002(14) 0.057(16) C26 0.08(2) 0.041(14) 0.063(18) 0.012(13) -0.030(15) 0.028(14) C27 0.052(13) 0.043(12) 0.029(11) -0.008(9) -0.015(10) 0.008(10) C28 0.030(7) 0.042(8) 0.032(8) -0.005(7) -0.005(6) 0.001(6) C29 0.048(9) 0.053(9) 0.036(8) -0.001(7) -0.006(7) 0.018(7) C30 0.056(9) 0.057(9) 0.036(9) -0.012(7) 0.002(7) 0.020(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 O9 2.067(3) 2_665 ? Co1 O3 2.070(3) 1_655 ? Co1 O8 2.074(3) . ? Co1 O14 2.103(3) . ? Co1 O12 2.144(3) . ? Co1 O6 2.257(3) . ? Co2 O7 2.014(3) . ? Co2 O2 2.022(3) 2 ? Co2 N1 2.121(4) . ? Co2 O5 2.140(3) . ? Co2 O4 2.153(3) . ? Co2 O1 2.303(3) . ? Co3 O13 2.036(3) . ? Co3 O1 2.063(3) . ? Co3 O11 2.091(3) . ? Co3 O10 2.138(3) . ? Co3 N2 2.142(4) . ? Co3 O7 2.252(3) . ? P1 O3 1.494(3) . ? P1 O2 1.522(3) . ? P1 O1 1.543(3) . ? P1 C1 1.839(4) . ? P2 O8 1.504(3) . ? P2 O9 1.522(3) . ? P2 O7 1.542(3) . ? P2 C3 1.837(4) . ? O2 Co2 2.022(3) 2 ? O3 Co1 2.070(3) 1_455 ? O4 C1 1.436(5) . ? O5 C2 1.255(5) 1_455 ? O6 C2 1.260(5) . ? O9 Co1 2.067(3) 2_665 ? O10 C3 1.439(5) . ? O11 C4 1.258(5) . ? O12 C4 1.249(5) . ? C1 C2 1.524(5) 1_455 ? C2 O5 1.255(5) 1_655 ? C2 C1 1.524(5) 1_655 ? C3 C4 1.521(5) . ? N1 C5 1.295(8) . ? N1 C9 1.333(9) . ? C5 C6 1.377(10) . ? C6 C7 1.326(9) . ? C7 C8 1.398(10) . ? C7 C12 1.483(6) 1_554 ? C8 C9 1.372(11) . ? C5A C6A 1.39(2) . ? C8A C9A 1.37(2) . ? N2 C14 1.314(9) . ? N2 C10 1.344(8) . ? C10 C11 1.390(10) . ? C11 C12 1.383(10) . ? C12 C13 1.375(9) . ? C12 C7 1.483(6) 1_556 ? C13 C14 1.397(10) . ? C10A C11A 1.39(2) . ? C13A C14A 1.39(2) . ? N3 C15 1.408(7) . ? N3 C19 1.408(7) . ? C15 C16 1.407(7) . ? C16 C17 1.409(7) . ? C17 C18 1.408(7) . ? C17 C17 1.58(3) 2_656 ? C18 C19 1.408(7) . ? N4 C21 1.377(10) . ? N4 C25 1.378(10) . ? C21 C22 1.377(10) . ? C22 C23 1.378(10) . ? C23 C24 1.378(10) . ? C23 C26 1.55(3) 2_646 ? C23 C28 1.59(2) . ? C23 N5 1.73(3) 2_646 ? C24 C25 1.377(10) . ? C24 N5 1.52(3) 2_646 ? C24 C30 1.93(4) 2_646 ? N5 C30 1.357(9) . ? N5 C26 1.358(9) . ? N5 C24 1.52(6) 2_646 ? N5 C23 1.73(6) 2_646 ? C26 C27 1.358(9) . ? C26 C23 1.55(6) 2_646 ? C26 C28 1.94(4) 2_646 ? C27 C28 1.358(9) . ? C27 C28 1.50(3) 2_646 ? C27 C29 1.82(4) 2_646 ? C28 C29 1.357(9) . ? C28 C27 1.50(3) 2_646 ? C28 C28 1.91(3) 2_646 ? C28 C26 1.94(4) 2_646 ? C29 C30 1.358(9) . ? C29 C27 1.82(3) 2_646 ? C30 C24 1.93(6) 2_646 ? 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 O9 Co1 O3 91.14(11) 2_665 1_655 ? O9 Co1 O8 91.52(11) 2_665 . ? O3 Co1 O8 177.26(11) 1_655 . ? O9 Co1 O14 170.40(14) 2_665 . ? O3 Co1 O14 92.89(13) 1_655 . ? O8 Co1 O14 84.58(13) . . ? O9 Co1 O12 100.92(14) 2_665 . ? O3 Co1 O12 88.94(12) 1_655 . ? O8 Co1 O12 89.92(11) . . ? O14 Co1 O12 87.87(15) . . ? O9 Co1 O6 84.17(11) 2_665 . ? O3 Co1 O6 87.84(11) 1_655 . ? O8 Co1 O6 93.08(11) . . ? O14 Co1 O6 87.28(13) . . ? O12 Co1 O6 174.03(12) . . ? O7 Co2 O2 103.76(11) . 2 ? O7 Co2 N1 101.01(13) . . ? O2 Co2 N1 92.45(13) 2 . ? O7 Co2 O5 87.92(11) . . ? O2 Co2 O5 167.95(11) 2 . ? N1 Co2 O5 88.17(13) . . ? O7 Co2 O4 153.58(11) . . ? O2 Co2 O4 94.21(11) 2 . ? N1 Co2 O4 97.35(13) . . ? O5 Co2 O4 73.78(10) . . ? O7 Co2 O1 80.35(10) . . ? O2 Co2 O1 91.79(10) 2 . ? N1 Co2 O1 175.11(12) . . ? O5 Co2 O1 87.18(10) . . ? O4 Co2 O1 79.89(10) . . ? O13 Co3 O1 100.51(12) . . ? O13 Co3 O11 166.27(12) . . ? O1 Co3 O11 93.17(11) . . ? O13 Co3 O10 90.95(11) . . ? O1 Co3 O10 158.98(11) . . ? O11 Co3 O10 75.68(11) . . ? O13 Co3 N2 90.44(14) . . ? O1 Co3 N2 95.71(13) . . ? O11 Co3 N2 89.31(13) . . ? O10 Co3 N2 101.82(13) . . ? O13 Co3 O7 94.90(12) . . ? O1 Co3 O7 80.59(10) . . ? O11 Co3 O7 86.16(10) . . ? O10 Co3 O7 80.92(10) . . ? N2 Co3 O7 173.97(13) . . ? O3 P1 O2 113.85(16) . . ? O3 P1 O1 114.60(16) . . ? O2 P1 O1 110.94(15) . . ? O3 P1 C1 106.76(17) . . ? O2 P1 C1 108.34(17) . . ? O1 P1 C1 101.30(16) . . ? O8 P2 O9 114.50(16) . . ? O8 P2 O7 114.14(16) . . ? O9 P2 O7 109.41(15) . . ? O8 P2 C3 107.84(17) . . ? O9 P2 C3 110.80(17) . . ? O7 P2 C3 99.05(16) . . ? P1 O1 Co3 134.35(17) . . ? P1 O1 Co2 113.19(15) . . ? Co3 O1 Co2 97.92(10) . . ? P1 O2 Co2 136.42(16) . 2 ? P1 O3 Co1 131.94(19) . 1_455 ? C1 O4 Co2 102.7(2) . . ? C2 O5 Co2 112.1(2) 1_455 . ? C2 O6 Co1 118.8(3) . . ? P2 O7 Co2 137.08(17) . . ? P2 O7 Co3 113.95(15) . . ? Co2 O7 Co3 101.07(11) . . ? P2 O8 Co1 127.71(18) . . ? P2 O9 Co1 132.21(17) . 2_665 ? C3 O10 Co3 101.1(2) . . ? C4 O11 Co3 110.6(2) . . ? C4 O12 Co1 122.7(3) . . ? O4 C1 C2 107.0(3) . 1_455 ? O4 C1 P1 109.7(3) . . ? C2 C1 P1 105.0(3) 1_455 . ? O5 C2 O6 124.6(4) 1_655 . ? O5 C2 C1 116.5(3) 1_655 1_655 ? O6 C2 C1 118.8(3) . 1_655 ? O10 C3 C4 108.5(3) . . ? O10 C3 P2 108.2(2) . . ? C4 C3 P2 104.2(3) . . ? O12 C4 O11 125.3(4) . . ? O12 C4 C3 117.9(3) . . ? O11 C4 C3 116.7(3) . . ? C5 N1 C9 116.1(5) . . ? C5 N1 Co2 123.6(4) . . ? C9 N1 Co2 120.2(4) . . ? N1 C5 C6 124.0(7) . . ? C7 C6 C5 121.5(7) . . ? C6 C7 C8 115.6(6) . . ? C6 C7 C12 122.8(5) . 1_554 ? C8 C7 C12 121.6(5) . 1_554 ? C9 C8 C7 119.8(8) . . ? N1 C9 C8 123.0(7) . . ? C14 N2 C10 115.7(5) . . ? C14 N2 Co3 121.3(4) . . ? C10 N2 Co3 122.7(4) . . ? N2 C10 C11 122.2(7) . . ? C12 C11 C10 121.0(7) . . ? C13 C12 C11 115.1(6) . . ? C13 C12 C7 122.6(5) . 1_556 ? C11 C12 C7 121.6(5) . 1_556 ? C12 C13 C14 119.7(7) . . ? N2 C14 C13 124.2(7) . . ? C15 N3 C19 120.0 . . ? C16 C15 N3 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 C17 112.9(17) . 2_656 ? C16 C17 C17 126.7(17) . 2_656 ? C19 C18 C17 120.0 . . ? C18 C19 N3 120.0 . . ? C21 N4 C25 120.0 . . ? C22 C21 N4 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 C26 105.9(15) . 2_646 ? C22 C23 C26 95.3(15) . 2_646 ? C24 C23 C28 120.7(11) . . ? C22 C23 C28 118.6(12) . . ? C26 C23 C28 76.3(12) 2_646 . ? C24 C23 N5 57.3(11) . 2_646 ? C22 C23 N5 117.1(10) . 2_646 ? C26 C23 N5 48.6(12) 2_646 2_646 ? C28 C23 N5 102.0(12) . 2_646 ? C25 C24 C23 120.0 . . ? C25 C24 N5 110.9(10) . 2_646 ? C23 C24 N5 73.0(13) . 2_646 ? C25 C24 C30 127.3(13) . 2_646 ? C23 C24 C30 97.9(13) . 2_646 ? N5 C24 C30 44.3(14) 2_646 2_646 ? C24 C25 N4 120.0 . . ? C30 N5 C26 120.0 . . ? C30 N5 C24 84(2) . 2_646 ? C26 N5 C24 109(3) . 2_646 ? C30 N5 C23 109.2(18) . 2_646 ? C26 N5 C23 59(2) . 2_646 ? C24 N5 C23 49.7(18) 2_646 2_646 ? C27 C26 N5 120.0 . . ? C27 C26 C23 103.2(19) . 2_646 ? N5 C26 C23 73(2) . 2_646 ? C27 C26 C28 50.5(12) . 2_646 ? N5 C26 C28 101.4(12) . 2_646 ? C23 C26 C28 52.7(19) 2_646 2_646 ? C28 C27 C26 120.0 . . ? C28 C27 C28 83.4(15) . 2_646 ? C26 C27 C28 85.2(17) . 2_646 ? C28 C27 C29 106.2(18) . 2_646 ? C26 C27 C29 107.7(19) . 2_646 ? C28 C27 C29 47.1(10) 2_646 2_646 ? C29 C28 C27 120.0 . . ? C29 C28 C27 78.6(15) . 2_646 ? C27 C28 C27 96.6(17) . 2_646 ? C29 C28 C23 122.3(11) . . ? C27 C28 C23 117.7(11) . . ? C27 C28 C23 95.2(13) 2_646 . ? C29 C28 C28 101.6(12) . 2_646 ? C27 C28 C28 51.5(13) . 2_646 ? C27 C28 C28 45.0(9) 2_646 2_646 ? C23 C28 C28 113.7(12) . 2_646 ? C29 C28 C26 101.4(15) . 2_646 ? C27 C28 C26 116.0(18) . 2_646 ? C27 C28 C26 44.3(8) 2_646 2_646 ? C23 C28 C26 51.0(11) . 2_646 ? C28 C28 C26 75.4(11) 2_646 2_646 ? C28 C29 C30 120.0 . . ? C28 C29 C27 54.2(12) . 2_646 ? C30 C29 C27 107.7(14) . 2_646 ? N5 C30 C29 120.0 . . ? N5 C30 C24 51.5(19) . 2_646 ? C29 C30 C24 121.5(18) . 2_646 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.195 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.140