# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Arthur Carty' _publ_contact_author_address ; Steacie Institute for Molecular Sciences National Research Council of Canada 100 Sussex Dr. Ottawa ON K1A 0R6 CANADA ; _publ_contact_author_email ACARTY@PCO-BCP.GC.CA _publ_section_title ; Reactivity of Electrophilic m-Phosphinidene Complexes with N-Heterocyclic Carbenes: Formation of the First Main Group Element Adducts of 'Abnormal Carbene' Ligands. ; loop_ _publ_author_name 'A. Carty' 'Todd Graham' 'Konstantin A. Udachin' # Attachment 'Compound 5 TG62.cif' data_tg62 _database_code_depnum_ccdc_archive 'CCDC 602520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H34 Mn2 N3 O8 P' _chemical_formula_weight 645.40 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9513(16) _cell_length_b 15.968(2) _cell_length_c 16.925(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.384(2) _cell_angle_gamma 90.00 _cell_volume 2911.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.7591 _exptl_absorpt_correction_T_max 0.9530 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _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 35996 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.58 _reflns_number_total 8136 _reflns_number_gt 6921 _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^)+(0.0350P)^2^+1.0960P] 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 8136 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Mn1 Mn 0.146424(17) 0.839396(12) 0.157101(12) 0.01718(5) Uani 1 1 d . . . Mn2 Mn 0.156754(18) 0.816506(12) -0.004849(11) 0.01684(5) Uani 1 1 d . . . P1 P 0.28838(3) 0.760988(19) 0.101686(18) 0.01359(6) Uani 1 1 d . . . O1 O 0.20281(13) 0.84569(8) 0.33351(7) 0.0414(3) Uani 1 1 d . . . O2 O -0.00353(11) 0.68686(8) 0.17285(8) 0.0389(3) Uani 1 1 d . . . O3 O -0.08844(9) 0.93542(7) 0.12646(7) 0.0337(2) Uani 1 1 d . . . O4 O 0.28853(9) 0.99854(6) 0.15524(7) 0.0274(2) Uani 1 1 d . . . O5 O -0.03477(10) 0.68212(7) -0.01924(8) 0.0372(3) Uani 1 1 d . . . O6 O -0.05937(10) 0.92987(7) -0.04862(6) 0.0302(2) Uani 1 1 d . . . O7 O 0.19485(12) 0.76699(8) -0.16561(7) 0.0389(3) Uani 1 1 d . . . O8 O 0.33964(11) 0.95273(7) -0.01250(7) 0.0345(3) Uani 1 1 d . . . N2 N 0.58912(10) 0.89152(7) 0.20088(6) 0.0180(2) Uani 1 1 d . . . N3 N 0.55136(10) 0.81728(7) 0.09027(7) 0.0176(2) Uani 1 1 d . . . N4 N 0.31225(10) 0.65649(7) 0.11516(6) 0.0181(2) Uani 1 1 d . . . C1 C 0.18248(13) 0.84237(9) 0.26420(9) 0.0256(3) Uani 1 1 d . . . C2 C 0.05601(13) 0.74385(9) 0.16386(9) 0.0258(3) Uani 1 1 d . . . C3 C 0.00381(12) 0.89868(9) 0.13792(9) 0.0241(3) Uani 1 1 d . . . C4 C 0.23474(12) 0.93690(8) 0.15272(8) 0.0200(2) Uani 1 1 d . . . C5 C 0.04134(13) 0.73215(9) -0.00931(9) 0.0245(3) Uani 1 1 d . . . C6 C 0.02610(13) 0.88772(8) -0.03100(8) 0.0228(3) Uani 1 1 d . . . C7 C 0.18169(14) 0.78550(9) -0.10157(8) 0.0250(3) Uani 1 1 d . . . C8 C 0.26892(13) 0.90149(9) -0.00650(8) 0.0226(3) Uani 1 1 d . . . C9 C 0.44695(11) 0.80778(8) 0.12847(7) 0.0152(2) Uani 1 1 d . . . C10 C 0.47556(11) 0.85396(8) 0.19715(7) 0.0162(2) Uani 1 1 d . . . H10 H 0.4243 0.8593 0.2366 0.019 Uiso 1 1 calc R . . C11 C 0.63187(12) 0.86811(9) 0.13574(8) 0.0208(3) Uani 1 1 d . . . H11 H 0.7092 0.8852 0.1231 0.025 Uiso 1 1 calc R . . C12 C 0.65017(12) 0.95481(9) 0.26141(8) 0.0211(3) Uani 1 1 d . . . C13 C 0.57290(15) 0.96299(12) 0.32682(10) 0.0352(4) Uani 1 1 d . . . H13A H 0.4893 0.9823 0.3032 0.042 Uiso 1 1 calc R . . H13B H 0.6119 1.0035 0.3670 0.042 Uiso 1 1 calc R . . H13C H 0.5675 0.9084 0.3525 0.042 Uiso 1 1 calc R . . C14 C 0.65448(15) 1.03788(9) 0.21760(9) 0.0297(3) Uani 1 1 d . . . H14A H 0.7062 1.0318 0.1763 0.036 Uiso 1 1 calc R . . H14B H 0.6898 1.0812 0.2561 0.036 Uiso 1 1 calc R . . H14C H 0.5702 1.0541 0.1922 0.036 Uiso 1 1 calc R . . C15 C 0.78081(13) 0.92409(10) 0.29646(9) 0.0282(3) Uani 1 1 d . . . H15A H 0.7757 0.8695 0.3221 0.034 Uiso 1 1 calc R . . H15B H 0.8213 0.9644 0.3364 0.034 Uiso 1 1 calc R . . H15C H 0.8292 0.9187 0.2533 0.034 Uiso 1 1 calc R . . C16 C 0.58941(12) 0.77606(9) 0.01753(9) 0.0237(3) Uani 1 1 d . . . C17 C 0.6484(2) 0.84107(13) -0.02852(13) 0.0542(6) Uani 1 1 d . . . H17A H 0.6608 0.8174 -0.0799 0.065 Uiso 1 1 calc R . . H17B H 0.7287 0.8579 0.0029 0.065 Uiso 1 1 calc R . . H17C H 0.5939 0.8901 -0.0384 0.065 Uiso 1 1 calc R . . C18 C 0.6824(2) 0.70747(15) 0.04920(13) 0.0548(6) Uani 1 1 d . . . H18A H 0.6425 0.6661 0.0789 0.066 Uiso 1 1 calc R . . H18B H 0.7536 0.7323 0.0850 0.066 Uiso 1 1 calc R . . H18C H 0.7109 0.6800 0.0040 0.066 Uiso 1 1 calc R . . C19 C 0.47919(15) 0.73842(12) -0.03603(10) 0.0385(4) Uani 1 1 d . . . H19A H 0.4246 0.7832 -0.0614 0.046 Uiso 1 1 calc R . . H19B H 0.4336 0.7029 -0.0041 0.046 Uiso 1 1 calc R . . H19C H 0.5072 0.7046 -0.0776 0.046 Uiso 1 1 calc R . . C20 C 0.37032(13) 0.61870(9) 0.19338(8) 0.0254(3) Uani 1 1 d . . . H20 H 0.3404 0.5595 0.1922 0.030 Uiso 1 1 calc R . . C21 C 0.33137(16) 0.65934(10) 0.26627(9) 0.0326(3) Uani 1 1 d . . . H21A H 0.3648 0.7164 0.2727 0.039 Uiso 1 1 calc R . . H21B H 0.3637 0.6265 0.3144 0.039 Uiso 1 1 calc R . . H21C H 0.2406 0.6614 0.2586 0.039 Uiso 1 1 calc R . . C22 C 0.51180(14) 0.61426(10) 0.20454(11) 0.0370(4) Uani 1 1 d . . . H22A H 0.5357 0.5846 0.1590 0.044 Uiso 1 1 calc R . . H22B H 0.5444 0.5843 0.2544 0.044 Uiso 1 1 calc R . . H22C H 0.5460 0.6711 0.2074 0.044 Uiso 1 1 calc R . . C23 C 0.26301(12) 0.59529(8) 0.05160(8) 0.0190(2) Uani 1 1 d . . . H23 H 0.2314 0.6278 0.0016 0.023 Uiso 1 1 calc R . . C24 C 0.15407(13) 0.54432(9) 0.07156(9) 0.0259(3) Uani 1 1 d . . . H24A H 0.1840 0.5065 0.1165 0.031 Uiso 1 1 calc R . . H24B H 0.1166 0.5115 0.0245 0.031 Uiso 1 1 calc R . . H24C H 0.0918 0.5824 0.0865 0.031 Uiso 1 1 calc R . . C25 C 0.36143(14) 0.53443(9) 0.03217(10) 0.0281(3) Uani 1 1 d . . . H25A H 0.4312 0.5661 0.0183 0.034 Uiso 1 1 calc R . . H25B H 0.3251 0.4990 -0.0133 0.034 Uiso 1 1 calc R . . H25C H 0.3910 0.4992 0.0791 0.034 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 Mn1 0.01310(9) 0.02010(10) 0.01906(10) -0.00102(7) 0.00480(7) -0.00091(7) Mn2 0.01768(9) 0.01514(9) 0.01606(9) 0.00060(7) -0.00135(7) 0.00123(7) P1 0.01158(13) 0.01406(14) 0.01485(14) 0.00144(10) 0.00158(11) -0.00065(10) O1 0.0567(8) 0.0466(7) 0.0221(5) -0.0028(5) 0.0101(5) -0.0087(6) O2 0.0350(6) 0.0344(6) 0.0513(7) -0.0027(5) 0.0183(5) -0.0144(5) O3 0.0177(5) 0.0417(6) 0.0432(6) 0.0015(5) 0.0098(4) 0.0054(4) O4 0.0230(5) 0.0202(5) 0.0383(6) -0.0006(4) 0.0034(4) 0.0007(4) O5 0.0248(5) 0.0319(6) 0.0512(7) -0.0018(5) -0.0033(5) -0.0075(4) O6 0.0305(5) 0.0262(5) 0.0290(5) -0.0050(4) -0.0078(4) 0.0097(4) O7 0.0589(8) 0.0353(6) 0.0209(5) -0.0036(4) 0.0031(5) 0.0121(5) O8 0.0446(7) 0.0274(6) 0.0317(6) 0.0037(4) 0.0079(5) -0.0121(5) N2 0.0150(5) 0.0196(5) 0.0196(5) -0.0021(4) 0.0033(4) -0.0031(4) N3 0.0146(5) 0.0188(5) 0.0206(5) -0.0036(4) 0.0061(4) -0.0022(4) N4 0.0195(5) 0.0146(5) 0.0184(5) 0.0020(4) -0.0017(4) -0.0002(4) C1 0.0259(7) 0.0267(7) 0.0256(7) -0.0014(5) 0.0086(5) -0.0049(5) C2 0.0210(6) 0.0296(7) 0.0283(7) -0.0041(6) 0.0086(5) -0.0011(5) C3 0.0177(6) 0.0286(7) 0.0272(7) -0.0023(5) 0.0077(5) -0.0026(5) C4 0.0160(5) 0.0225(6) 0.0215(6) -0.0007(5) 0.0037(5) 0.0051(5) C5 0.0202(6) 0.0237(7) 0.0268(7) 0.0007(5) -0.0030(5) 0.0026(5) C6 0.0263(7) 0.0201(6) 0.0194(6) -0.0031(5) -0.0033(5) 0.0014(5) C7 0.0308(7) 0.0188(6) 0.0229(6) 0.0000(5) -0.0016(5) 0.0047(5) C8 0.0300(7) 0.0203(6) 0.0165(6) 0.0020(5) 0.0016(5) 0.0011(5) C9 0.0122(5) 0.0158(6) 0.0177(6) 0.0012(4) 0.0032(4) -0.0002(4) C10 0.0130(5) 0.0173(6) 0.0183(6) 0.0019(4) 0.0030(4) -0.0008(4) C11 0.0156(6) 0.0234(6) 0.0243(6) -0.0052(5) 0.0065(5) -0.0044(5) C12 0.0206(6) 0.0230(6) 0.0194(6) -0.0049(5) 0.0028(5) -0.0067(5) C13 0.0335(8) 0.0473(10) 0.0274(7) -0.0157(7) 0.0122(6) -0.0148(7) C14 0.0362(8) 0.0213(7) 0.0296(7) -0.0027(6) 0.0001(6) -0.0043(6) C15 0.0231(7) 0.0325(8) 0.0260(7) 0.0012(6) -0.0035(5) -0.0082(6) C16 0.0200(6) 0.0247(7) 0.0291(7) -0.0112(5) 0.0118(5) -0.0047(5) C17 0.0787(15) 0.0483(11) 0.0478(11) -0.0226(9) 0.0439(11) -0.0339(10) C18 0.0465(11) 0.0643(13) 0.0517(12) -0.0200(10) 0.0040(9) 0.0290(10) C19 0.0289(8) 0.0540(11) 0.0357(8) -0.0240(8) 0.0138(7) -0.0127(7) C20 0.0285(7) 0.0187(6) 0.0248(7) 0.0072(5) -0.0062(5) -0.0015(5) C21 0.0453(9) 0.0301(8) 0.0194(6) 0.0085(6) -0.0024(6) -0.0057(7) C22 0.0290(8) 0.0286(8) 0.0457(9) 0.0050(7) -0.0137(7) 0.0049(6) C23 0.0187(6) 0.0158(6) 0.0217(6) -0.0004(5) 0.0018(5) -0.0014(4) C24 0.0229(6) 0.0208(7) 0.0331(7) 0.0015(5) 0.0026(6) -0.0062(5) C25 0.0294(7) 0.0215(7) 0.0339(8) -0.0014(6) 0.0071(6) 0.0050(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 Mn1 C1 1.7849(15) . ? Mn1 C3 1.8050(14) . ? Mn1 C2 1.8335(15) . ? Mn1 C4 1.8415(14) . ? Mn1 P1 2.3216(4) . ? Mn1 Mn2 2.7877(5) . ? Mn2 C7 1.7778(15) . ? Mn2 C6 1.8188(14) . ? Mn2 C8 1.8340(14) . ? Mn2 C5 1.8394(15) . ? Mn2 P1 2.2755(4) . ? P1 N4 1.6980(11) . ? P1 C9 1.8696(12) . ? O1 C1 1.1550(18) . ? O2 C2 1.1455(18) . ? O3 C3 1.1540(17) . ? O4 C4 1.1439(17) . ? O5 C5 1.1448(18) . ? O6 C6 1.1477(17) . ? O7 C7 1.1573(18) . ? O8 C8 1.1436(18) . ? N2 C11 1.3269(17) . ? N2 C10 1.3719(15) . ? N2 C12 1.5069(16) . ? N3 C11 1.3355(16) . ? N3 C9 1.4195(16) . ? N3 C16 1.5190(17) . ? N4 C23 1.4812(16) . ? N4 C20 1.4892(16) . ? C9 C10 1.3645(17) . ? C12 C13 1.515(2) . ? C12 C14 1.525(2) . ? C12 C15 1.5276(19) . ? C16 C19 1.499(2) . ? C16 C17 1.511(2) . ? C16 C18 1.526(2) . ? C20 C21 1.521(2) . ? C20 C22 1.528(2) . ? C23 C25 1.5304(19) . ? C23 C24 1.5313(18) . ? 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 C1 Mn1 C3 101.22(7) . . ? C1 Mn1 C2 88.96(7) . . ? C3 Mn1 C2 89.32(7) . . ? C1 Mn1 C4 89.81(6) . . ? C3 Mn1 C4 89.60(6) . . ? C2 Mn1 C4 178.18(6) . . ? C1 Mn1 P1 112.52(5) . . ? C3 Mn1 P1 146.19(5) . . ? C2 Mn1 P1 89.14(5) . . ? C4 Mn1 P1 92.57(4) . . ? C1 Mn1 Mn2 164.00(5) . . ? C3 Mn1 Mn2 94.54(5) . . ? C2 Mn1 Mn2 94.03(5) . . ? C4 Mn1 Mn2 87.51(4) . . ? P1 Mn1 Mn2 51.922(10) . . ? C7 Mn2 C6 101.23(6) . . ? C7 Mn2 C8 88.71(6) . . ? C6 Mn2 C8 91.91(6) . . ? C7 Mn2 C5 88.67(7) . . ? C6 Mn2 C5 86.75(6) . . ? C8 Mn2 C5 176.77(6) . . ? C7 Mn2 P1 116.14(5) . . ? C6 Mn2 P1 142.62(4) . . ? C8 Mn2 P1 88.28(4) . . ? C5 Mn2 P1 94.57(4) . . ? C7 Mn2 Mn1 169.14(4) . . ? C6 Mn2 Mn1 89.30(4) . . ? C8 Mn2 Mn1 93.66(4) . . ? C5 Mn2 Mn1 89.25(5) . . ? P1 Mn2 Mn1 53.427(12) . . ? N4 P1 C9 104.26(5) . . ? N4 P1 Mn2 123.33(4) . . ? C9 P1 Mn2 117.68(4) . . ? N4 P1 Mn1 125.02(4) . . ? C9 P1 Mn1 110.30(4) . . ? Mn2 P1 Mn1 74.651(15) . . ? C11 N2 C10 106.93(10) . . ? C11 N2 C12 125.03(11) . . ? C10 N2 C12 127.73(11) . . ? C11 N3 C9 107.75(10) . . ? C11 N3 C16 118.77(11) . . ? C9 N3 C16 133.16(10) . . ? C23 N4 C20 114.81(10) . . ? C23 N4 P1 121.58(8) . . ? C20 N4 P1 123.25(9) . . ? O1 C1 Mn1 178.03(15) . . ? O2 C2 Mn1 174.88(13) . . ? O3 C3 Mn1 178.66(14) . . ? O4 C4 Mn1 175.33(12) . . ? O5 C5 Mn2 173.59(13) . . ? O6 C6 Mn2 177.17(12) . . ? O7 C7 Mn2 177.81(13) . . ? O8 C8 Mn2 175.46(13) . . ? C10 C9 N3 104.49(10) . . ? C10 C9 P1 118.89(9) . . ? N3 C9 P1 136.18(9) . . ? C9 C10 N2 110.03(11) . . ? N2 C11 N3 110.78(11) . . ? N2 C12 C13 108.46(11) . . ? N2 C12 C14 107.56(11) . . ? C13 C12 C14 110.52(13) . . ? N2 C12 C15 108.56(11) . . ? C13 C12 C15 110.56(12) . . ? C14 C12 C15 111.06(12) . . ? C19 C16 C17 109.63(15) . . ? C19 C16 N3 110.82(11) . . ? C17 C16 N3 109.00(12) . . ? C19 C16 C18 109.79(15) . . ? C17 C16 C18 110.73(17) . . ? N3 C16 C18 106.84(13) . . ? N4 C20 C21 114.26(12) . . ? N4 C20 C22 112.93(12) . . ? C21 C20 C22 110.22(13) . . ? N4 C23 C25 113.37(11) . . ? N4 C23 C24 112.74(11) . . ? C25 C23 C24 108.47(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.563 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.055 data_tgg40 _database_code_depnum_ccdc_archive 'CCDC 602521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H68 Co2 N3 O5.50 P3' _chemical_formula_weight 1033.86 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 11.2872(10) _cell_length_b 11.6939(10) _cell_length_c 20.7381(18) _cell_angle_alpha 89.9240(10) _cell_angle_beta 74.9300(10) _cell_angle_gamma 75.5530(10) _cell_volume 2553.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.7687 _exptl_absorpt_correction_T_max 0.8903 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _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 31811 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 29.60 _reflns_number_total 14076 _reflns_number_gt 11305 _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^)+(0.0511P)^2^+1.1295P] 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 14076 _refine_ls_number_parameters 659 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.060 _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 O1B O 0.1766(13) 0.3977(11) -0.0436(8) 0.1075(15) Uani 0.22 1 d PD A -7 C1B C 0.0917(13) 0.3211(14) -0.0362(10) 0.097(3) Uani 0.22 1 d PD A -7 H1B1 H 0.0323 0.3439 -0.0645 0.117 Uiso 0.22 1 calc PR A -7 H1B2 H 0.0424 0.3227 0.0110 0.117 Uiso 0.22 1 calc PR A -7 C2B C 0.1790(15) 0.2059(11) -0.0588(9) 0.0793(17) Uani 0.22 1 d PD A -7 H2B1 H 0.1633 0.1492 -0.0241 0.095 Uiso 0.22 1 calc PR A -7 H2B2 H 0.1651 0.1761 -0.1001 0.095 Uiso 0.22 1 calc PR A -7 C3B C 0.3086(14) 0.2151(13) -0.0717(13) 0.101(2) Uani 0.22 1 d PD A -7 H3B1 H 0.3619 0.1684 -0.1136 0.121 Uiso 0.22 1 calc PR A -7 H3B2 H 0.3448 0.1850 -0.0344 0.121 Uiso 0.22 1 calc PR A -7 C4B C 0.3038(15) 0.3404(14) -0.0778(12) 0.109(3) Uani 0.22 1 d PD A -7 H4B1 H 0.3641 0.3635 -0.0565 0.131 Uiso 0.22 1 calc PR A -7 H4B2 H 0.3236 0.3594 -0.1253 0.131 Uiso 0.22 1 calc PR A -7 O1G O 0.154(2) 0.3569(18) -0.0169(13) 0.1075(15) Uani 0.13 1 d PD B -6 C1G C 0.028(2) 0.368(2) -0.0230(16) 0.097(3) Uani 0.13 1 d PD B -6 H1G1 H -0.0099 0.3083 0.0033 0.117 Uiso 0.13 1 calc PR B -6 H1G2 H 0.0295 0.3541 -0.0704 0.117 Uiso 0.13 1 calc PR B -6 C2G C -0.0486(19) 0.488(2) 0.0029(17) 0.0793(17) Uani 0.13 1 d PD B -6 H2G1 H -0.1168 0.5162 -0.0198 0.095 Uiso 0.13 1 calc PR B -6 H2G2 H -0.0872 0.4918 0.0517 0.095 Uiso 0.13 1 calc PR B -6 C3G C 0.044(3) 0.5596(16) -0.013(2) 0.101(2) Uani 0.13 1 d PD B -6 H3G1 H 0.0398 0.6077 0.0273 0.121 Uiso 0.13 1 calc PR B -6 H3G2 H 0.0282 0.6131 -0.0485 0.121 Uiso 0.13 1 calc PR B -6 C4G C 0.167(2) 0.473(2) -0.0356(18) 0.109(3) Uani 0.13 1 d PD B -6 H4G1 H 0.1997 0.4720 -0.0849 0.131 Uiso 0.13 1 calc PR B -6 H4G2 H 0.2293 0.4950 -0.0151 0.131 Uiso 0.13 1 calc PR B -6 O1F O 0.1156(12) 0.4337(12) 0.0268(7) 0.1075(15) Uani 0.24 1 d PD C -5 C1F C 0.067(2) 0.5593(13) 0.0214(12) 0.097(3) Uani 0.24 1 d PD C -5 H1F1 H 0.1374 0.5976 0.0070 0.117 Uiso 0.24 1 calc PR C -5 H1F2 H 0.0111 0.5977 0.0650 0.117 Uiso 0.24 1 calc PR C -5 C2F C -0.0055(18) 0.5689(12) -0.0288(9) 0.0793(17) Uani 0.24 1 d PD C -5 H2F1 H 0.0507 0.5641 -0.0747 0.095 Uiso 0.24 1 calc PR C -5 H2F2 H -0.0730 0.6440 -0.0211 0.095 Uiso 0.24 1 calc PR C -5 C3F C -0.060(2) 0.4663(16) -0.0180(15) 0.101(2) Uani 0.24 1 d PD C -5 H3F1 H -0.1480 0.4905 0.0108 0.121 Uiso 0.24 1 calc PR C -5 H3F2 H -0.0602 0.4310 -0.0612 0.121 Uiso 0.24 1 calc PR C -5 C4F C 0.0202(19) 0.3811(13) 0.0147(12) 0.109(3) Uani 0.24 1 d PD C -5 H4F1 H -0.0318 0.3615 0.0575 0.131 Uiso 0.24 1 calc PR C -5 H4F2 H 0.0609 0.3072 -0.0144 0.131 Uiso 0.24 1 calc PR C -5 O1S O 0.3283(7) 0.2584(7) -0.0239(4) 0.1075(15) Uani 0.43 1 d PD D -1 C1S C 0.4405(13) 0.1652(13) -0.0301(6) 0.097(3) Uani 0.43 1 d PD D -1 H1S1 H 0.4196 0.0997 -0.0029 0.117 Uiso 0.43 1 calc PR D -1 H1S2 H 0.5027 0.1946 -0.0133 0.117 Uiso 0.43 1 calc PR D -1 C2S C 0.4954(14) 0.1224(13) -0.1002(7) 0.0793(17) Uani 0.43 1 d PD D -1 H2S1 H 0.4606 0.0578 -0.1118 0.095 Uiso 0.43 1 calc PR D -1 H2S2 H 0.5891 0.0945 -0.1111 0.095 Uiso 0.43 1 calc PR D -1 C3S C 0.4537(15) 0.2327(13) -0.1354(6) 0.101(2) Uani 0.43 1 d PD D -1 H3S1 H 0.5276 0.2619 -0.1590 0.121 Uiso 0.43 1 calc PR D -1 H3S2 H 0.4089 0.2168 -0.1683 0.121 Uiso 0.43 1 calc PR D -1 C4S C 0.3697(12) 0.3169(9) -0.0826(5) 0.109(3) Uani 0.43 1 d PD D -1 H4S1 H 0.4142 0.3748 -0.0725 0.131 Uiso 0.43 1 calc PR D -1 H4S2 H 0.2952 0.3607 -0.0973 0.131 Uiso 0.43 1 calc PR D -1 O1T O 0.2906(8) 0.1535(9) -0.0533(5) 0.1075(15) Uani 0.34 1 d PD E -3 C1T C 0.4078(12) 0.1121(14) -0.0378(7) 0.097(3) Uani 0.34 1 d PD E -3 H1T1 H 0.4206 0.0280 -0.0274 0.117 Uiso 0.34 1 calc PR E -3 H1T2 H 0.4094 0.1587 0.0016 0.117 Uiso 0.34 1 calc PR E -3 C2T C 0.5081(13) 0.1251(17) -0.0964(10) 0.0793(17) Uani 0.34 1 d PD E -3 H2T1 H 0.5335 0.0568 -0.1297 0.095 Uiso 0.34 1 calc PR E -3 H2T2 H 0.5838 0.1346 -0.0835 0.095 Uiso 0.34 1 calc PR E -3 C3T C 0.4421(15) 0.2367(17) -0.1224(10) 0.101(2) Uani 0.34 1 d PD E -3 H3T1 H 0.4569 0.3072 -0.1026 0.121 Uiso 0.34 1 calc PR E -3 H3T2 H 0.4733 0.2349 -0.1718 0.121 Uiso 0.34 1 calc PR E -3 C4T C 0.3056(13) 0.2395(12) -0.1019(7) 0.109(3) Uani 0.34 1 d PD E -3 H4T1 H 0.2541 0.3192 -0.0824 0.131 Uiso 0.34 1 calc PR E -3 H4T2 H 0.2777 0.2198 -0.1411 0.131 Uiso 0.34 1 calc PR E -3 O1A O 0.570(2) -0.0140(17) -0.0608(10) 0.1075(15) Uani 0.13 1 d PD F -4 C1A C 0.463(3) 0.041(2) -0.0060(11) 0.097(3) Uani 0.13 1 d PD F -4 H1A1 H 0.4884 0.0355 0.0365 0.117 Uiso 0.13 1 calc PR F -4 H1A2 H 0.3943 0.0010 -0.0020 0.117 Uiso 0.13 1 calc PR F -4 C2A C 0.420(4) 0.165(2) -0.0194(14) 0.0793(17) Uani 0.13 1 d PD F -4 H2A1 H 0.3258 0.1918 -0.0054 0.095 Uiso 0.13 1 calc PR F -4 H2A2 H 0.4536 0.2163 0.0053 0.095 Uiso 0.13 1 calc PR F -4 C3A C 0.467(4) 0.172(2) -0.0916(15) 0.101(2) Uani 0.13 1 d PD F -4 H3A1 H 0.4938 0.2461 -0.1017 0.121 Uiso 0.13 1 calc PR F -4 H3A2 H 0.4017 0.1684 -0.1146 0.121 Uiso 0.13 1 calc PR F -4 C4A C 0.577(3) 0.068(2) -0.1126(12) 0.109(3) Uani 0.13 1 d PD F -4 H4A1 H 0.5762 0.0295 -0.1549 0.131 Uiso 0.13 1 calc PR F -4 H4A2 H 0.6572 0.0926 -0.1202 0.131 Uiso 0.13 1 calc PR F -4 Co1 Co 0.16469(2) 0.19850(2) 0.307544(11) 0.01629(6) Uani 1 1 d . . . Co2 Co 0.27284(2) 0.37931(2) 0.303411(11) 0.01602(6) Uani 1 1 d . . . P1 P 0.11763(4) 0.25400(4) 0.21518(2) 0.01983(9) Uani 1 1 d . . . P2 P 0.33238(4) 0.36869(4) 0.19447(2) 0.01911(9) Uani 1 1 d . . . P3 P 0.29832(4) 0.22696(4) 0.35976(2) 0.01482(8) Uani 1 1 d . . . O1 O -0.08539(12) 0.26058(13) 0.40287(7) 0.0290(3) Uani 1 1 d . . . O2 O 0.26170(14) -0.05217(13) 0.26862(8) 0.0361(3) Uani 1 1 d . . . O3 O 0.01276(13) 0.51786(12) 0.36290(8) 0.0343(3) Uani 1 1 d . . . O4 O 0.44219(14) 0.51543(14) 0.32649(8) 0.0358(3) Uani 1 1 d . . . N1 N 0.44223(13) 0.12953(13) 0.35384(7) 0.0183(3) Uani 1 1 d . . . N2 N 0.25317(12) 0.29573(12) 0.50633(7) 0.0159(3) Uani 1 1 d . . . N3 N 0.10977(12) 0.20256(12) 0.55029(7) 0.0161(3) Uani 1 1 d . . . C1 C 0.01445(16) 0.24011(15) 0.36558(8) 0.0199(3) Uani 1 1 d . . . C2 C 0.22924(16) 0.04909(17) 0.28281(9) 0.0234(3) Uani 1 1 d . . . C3 C 0.11553(16) 0.46288(15) 0.33682(9) 0.0216(3) Uani 1 1 d . . . C4 C 0.37631(16) 0.45889(16) 0.31712(9) 0.0230(3) Uani 1 1 d . . . C5 C 0.25153(16) 0.28486(18) 0.15246(9) 0.0252(4) Uani 1 1 d . . . H5A H 0.2206 0.3317 0.1176 0.030 Uiso 1 1 calc R . . H5B H 0.3116 0.2097 0.1307 0.030 Uiso 1 1 calc R . . C6 C 0.07342(16) 0.14325(18) 0.16956(9) 0.0246(4) Uani 1 1 d . . . C7 C -0.00109(19) 0.07390(18) 0.20651(10) 0.0291(4) Uani 1 1 d . . . H7 H -0.0280 0.0855 0.2539 0.035 Uiso 1 1 calc R . . C8 C -0.0362(2) -0.0117(2) 0.17466(12) 0.0363(5) Uani 1 1 d . . . H8 H -0.0887 -0.0567 0.2003 0.044 Uiso 1 1 calc R . . C9 C 0.0053(2) -0.0315(2) 0.10579(12) 0.0395(5) Uani 1 1 d . . . H9 H -0.0171 -0.0912 0.0841 0.047 Uiso 1 1 calc R . . C10 C 0.0797(2) 0.0360(2) 0.06874(11) 0.0406(5) Uani 1 1 d . . . H10 H 0.1084 0.0224 0.0214 0.049 Uiso 1 1 calc R . . C11 C 0.11275(18) 0.1234(2) 0.10000(10) 0.0330(5) Uani 1 1 d . . . H11 H 0.1626 0.1702 0.0739 0.040 Uiso 1 1 calc R . . C12 C -0.01534(16) 0.38446(18) 0.21992(9) 0.0246(4) Uani 1 1 d . . . C13 C -0.13652(17) 0.37825(19) 0.25505(10) 0.0288(4) Uani 1 1 d . . . H13 H -0.1485 0.3064 0.2737 0.035 Uiso 1 1 calc R . . C14 C -0.23977(18) 0.4756(2) 0.26304(11) 0.0359(5) Uani 1 1 d . . . H14 H -0.3222 0.4692 0.2859 0.043 Uiso 1 1 calc R . . C15 C -0.2241(2) 0.5805(2) 0.23833(13) 0.0451(6) Uani 1 1 d . . . H15 H -0.2952 0.6471 0.2445 0.054 Uiso 1 1 calc R . . C16 C -0.1049(2) 0.5897(3) 0.20437(16) 0.0580(8) Uani 1 1 d . . . H16 H -0.0933 0.6630 0.1877 0.070 Uiso 1 1 calc R . . C17 C -0.0007(2) 0.4904(2) 0.19440(14) 0.0463(6) Uani 1 1 d . . . H17 H 0.0810 0.4962 0.1697 0.056 Uiso 1 1 calc R . . C18 C 0.31136(17) 0.50824(17) 0.15209(9) 0.0262(4) Uani 1 1 d . . . C19 C 0.34641(19) 0.50647(19) 0.08215(9) 0.0311(4) Uani 1 1 d . . . H19 H 0.3843 0.4330 0.0565 0.037 Uiso 1 1 calc R . . C20 C 0.3265(2) 0.6104(2) 0.04982(11) 0.0432(6) Uani 1 1 d . . . H20 H 0.3500 0.6082 0.0023 0.052 Uiso 1 1 calc R . . C21 C 0.2721(3) 0.7175(2) 0.08710(13) 0.0576(8) Uani 1 1 d . . . H21 H 0.2563 0.7888 0.0651 0.069 Uiso 1 1 calc R . . C22 C 0.2407(3) 0.7210(2) 0.15602(13) 0.0569(8) Uani 1 1 d . . . H22 H 0.2058 0.7949 0.1814 0.068 Uiso 1 1 calc R . . C23 C 0.2600(2) 0.61638(19) 0.18862(10) 0.0386(5) Uani 1 1 d . . . H23 H 0.2378 0.6193 0.2361 0.046 Uiso 1 1 calc R . . C24 C 0.50153(16) 0.30774(17) 0.15124(8) 0.0221(3) Uani 1 1 d . . . C25 C 0.58353(18) 0.3781(2) 0.15469(10) 0.0303(4) Uani 1 1 d . . . H25 H 0.5502 0.4546 0.1772 0.036 Uiso 1 1 calc R . . C26 C 0.71347(19) 0.3372(2) 0.12554(10) 0.0380(5) Uani 1 1 d . . . H26 H 0.7681 0.3861 0.1280 0.046 Uiso 1 1 calc R . . C27 C 0.76304(19) 0.2262(2) 0.09326(11) 0.0410(6) Uani 1 1 d . . . H27 H 0.8517 0.1987 0.0729 0.049 Uiso 1 1 calc R . . C28 C 0.6842(2) 0.1558(2) 0.09057(12) 0.0409(5) Uani 1 1 d . . . H28 H 0.7187 0.0785 0.0690 0.049 Uiso 1 1 calc R . . C29 C 0.55365(18) 0.19598(18) 0.11910(10) 0.0305(4) Uani 1 1 d . . . H29 H 0.5000 0.1462 0.1164 0.037 Uiso 1 1 calc R . . C30 C 0.53236(16) 0.11745(16) 0.28634(8) 0.0223(3) Uani 1 1 d . . . H30 H 0.4840 0.1690 0.2583 0.027 Uiso 1 1 calc R . . C31 C 0.64482(18) 0.1684(2) 0.28536(10) 0.0324(4) Uani 1 1 d . . . H31A H 0.6138 0.2475 0.3084 0.039 Uiso 1 1 calc R . . H31B H 0.6913 0.1736 0.2389 0.039 Uiso 1 1 calc R . . H31C H 0.7015 0.1166 0.3081 0.039 Uiso 1 1 calc R . . C32 C 0.57494(18) -0.00623(18) 0.25079(9) 0.0290(4) Uani 1 1 d . . . H32A H 0.6267 -0.0608 0.2748 0.035 Uiso 1 1 calc R . . H32B H 0.6252 -0.0033 0.2048 0.035 Uiso 1 1 calc R . . H32C H 0.5001 -0.0338 0.2500 0.035 Uiso 1 1 calc R . . C33 C 0.46046(16) 0.04113(16) 0.40350(9) 0.0235(4) Uani 1 1 d . . . H33 H 0.4096 0.0828 0.4478 0.028 Uiso 1 1 calc R . . C34 C 0.59735(18) 0.0011(2) 0.40876(10) 0.0342(5) Uani 1 1 d . . . H34A H 0.6518 -0.0442 0.3673 0.041 Uiso 1 1 calc R . . H34B H 0.6005 -0.0487 0.4466 0.041 Uiso 1 1 calc R . . H34C H 0.6274 0.0707 0.4157 0.041 Uiso 1 1 calc R . . C35 C 0.4072(2) -0.06490(18) 0.39679(11) 0.0342(4) Uani 1 1 d . . . H35A H 0.3204 -0.0369 0.3925 0.041 Uiso 1 1 calc R . . H35B H 0.4065 -0.1102 0.4366 0.041 Uiso 1 1 calc R . . H35C H 0.4605 -0.1156 0.3570 0.041 Uiso 1 1 calc R . . C36 C 0.23125(14) 0.23815(14) 0.45241(8) 0.0157(3) Uani 1 1 d . . . C37 C 0.17790(15) 0.27281(14) 0.56327(8) 0.0165(3) Uani 1 1 d . . . H37 H 0.1737 0.3024 0.6067 0.020 Uiso 1 1 calc R . . C38 C 0.14146(15) 0.18095(15) 0.48203(8) 0.0172(3) Uani 1 1 d . . . H38 H 0.1063 0.1335 0.4590 0.021 Uiso 1 1 calc R . . C39 C 0.33156(17) 0.38328(16) 0.50562(9) 0.0208(3) Uani 1 1 d . . . C40 C 0.46247(17) 0.33305(17) 0.45805(10) 0.0257(4) Uani 1 1 d . . . H40A H 0.5042 0.2590 0.4741 0.031 Uiso 1 1 calc R . . H40B H 0.5136 0.3901 0.4562 0.031 Uiso 1 1 calc R . . H40C H 0.4540 0.3177 0.4132 0.031 Uiso 1 1 calc R . . C41 C 0.25936(19) 0.49948(16) 0.48458(10) 0.0268(4) Uani 1 1 d . . . H41A H 0.2436 0.4857 0.4413 0.032 Uiso 1 1 calc R . . H41B H 0.3099 0.5574 0.4806 0.032 Uiso 1 1 calc R . . H41C H 0.1781 0.5299 0.5183 0.032 Uiso 1 1 calc R . . C42 C 0.3438(2) 0.4011(2) 0.57625(10) 0.0333(5) Uani 1 1 d . . . H42A H 0.2601 0.4389 0.6061 0.040 Uiso 1 1 calc R . . H42B H 0.4014 0.4517 0.5757 0.040 Uiso 1 1 calc R . . H42C H 0.3779 0.3242 0.5923 0.040 Uiso 1 1 calc R . . C43 C 0.01202(15) 0.15829(15) 0.60029(8) 0.0188(3) Uani 1 1 d . . . C44 C -0.11748(16) 0.21721(18) 0.58944(10) 0.0274(4) Uani 1 1 d . . . H44A H -0.1347 0.3033 0.5966 0.033 Uiso 1 1 calc R . . H44B H -0.1834 0.1891 0.6212 0.033 Uiso 1 1 calc R . . H44C H -0.1175 0.1970 0.5436 0.033 Uiso 1 1 calc R . . C45 C 0.01609(18) 0.18963(17) 0.67103(9) 0.0245(4) Uani 1 1 d . . . H45A H 0.1019 0.1565 0.6757 0.029 Uiso 1 1 calc R . . H45B H -0.0443 0.1567 0.7036 0.029 Uiso 1 1 calc R . . H45C H -0.0068 0.2759 0.6792 0.029 Uiso 1 1 calc R . . C46 C 0.04578(18) 0.02431(16) 0.58831(9) 0.0241(4) Uani 1 1 d . . . H46A H 0.0483 0.0037 0.5421 0.029 Uiso 1 1 calc R . . H46B H -0.0184 -0.0071 0.6192 0.029 Uiso 1 1 calc R . . H46C H 0.1291 -0.0100 0.5959 0.029 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 O1B 0.115(4) 0.109(4) 0.096(4) 0.041(3) -0.026(3) -0.026(3) C1B 0.104(6) 0.134(8) 0.059(4) 0.024(5) -0.018(4) -0.044(5) C2B 0.096(4) 0.066(3) 0.077(3) -0.006(2) -0.031(3) -0.013(3) C3B 0.129(5) 0.079(4) 0.090(6) 0.022(4) -0.029(4) -0.020(4) C4B 0.144(8) 0.078(5) 0.093(5) 0.020(4) -0.046(5) 0.009(5) O1G 0.115(4) 0.109(4) 0.096(4) 0.041(3) -0.026(3) -0.026(3) C1G 0.104(6) 0.134(8) 0.059(4) 0.024(5) -0.018(4) -0.044(5) C2G 0.096(4) 0.066(3) 0.077(3) -0.006(2) -0.031(3) -0.013(3) C3G 0.129(5) 0.079(4) 0.090(6) 0.022(4) -0.029(4) -0.020(4) C4G 0.144(8) 0.078(5) 0.093(5) 0.020(4) -0.046(5) 0.009(5) O1F 0.115(4) 0.109(4) 0.096(4) 0.041(3) -0.026(3) -0.026(3) C1F 0.104(6) 0.134(8) 0.059(4) 0.024(5) -0.018(4) -0.044(5) C2F 0.096(4) 0.066(3) 0.077(3) -0.006(2) -0.031(3) -0.013(3) C3F 0.129(5) 0.079(4) 0.090(6) 0.022(4) -0.029(4) -0.020(4) C4F 0.144(8) 0.078(5) 0.093(5) 0.020(4) -0.046(5) 0.009(5) O1S 0.115(4) 0.109(4) 0.096(4) 0.041(3) -0.026(3) -0.026(3) C1S 0.104(6) 0.134(8) 0.059(4) 0.024(5) -0.018(4) -0.044(5) C2S 0.096(4) 0.066(3) 0.077(3) -0.006(2) -0.031(3) -0.013(3) C3S 0.129(5) 0.079(4) 0.090(6) 0.022(4) -0.029(4) -0.020(4) C4S 0.144(8) 0.078(5) 0.093(5) 0.020(4) -0.046(5) 0.009(5) O1T 0.115(4) 0.109(4) 0.096(4) 0.041(3) -0.026(3) -0.026(3) C1T 0.104(6) 0.134(8) 0.059(4) 0.024(5) -0.018(4) -0.044(5) C2T 0.096(4) 0.066(3) 0.077(3) -0.006(2) -0.031(3) -0.013(3) C3T 0.129(5) 0.079(4) 0.090(6) 0.022(4) -0.029(4) -0.020(4) C4T 0.144(8) 0.078(5) 0.093(5) 0.020(4) -0.046(5) 0.009(5) O1A 0.115(4) 0.109(4) 0.096(4) 0.041(3) -0.026(3) -0.026(3) C1A 0.104(6) 0.134(8) 0.059(4) 0.024(5) -0.018(4) -0.044(5) C2A 0.096(4) 0.066(3) 0.077(3) -0.006(2) -0.031(3) -0.013(3) C3A 0.129(5) 0.079(4) 0.090(6) 0.022(4) -0.029(4) -0.020(4) C4A 0.144(8) 0.078(5) 0.093(5) 0.020(4) -0.046(5) 0.009(5) Co1 0.01622(10) 0.01886(11) 0.01316(10) 0.00132(8) -0.00405(8) -0.00325(8) Co2 0.01581(10) 0.01723(11) 0.01301(10) 0.00351(8) -0.00189(8) -0.00269(8) P1 0.01610(19) 0.0280(2) 0.01370(19) 0.00164(16) -0.00388(15) -0.00281(16) P2 0.01697(19) 0.0234(2) 0.01345(19) 0.00391(16) -0.00170(15) -0.00129(16) P3 0.01488(17) 0.01657(19) 0.01205(18) 0.00258(14) -0.00270(14) -0.00326(14) O1 0.0218(6) 0.0322(7) 0.0275(7) -0.0002(6) 0.0009(5) -0.0046(5) O2 0.0398(8) 0.0230(7) 0.0440(9) -0.0049(6) -0.0125(7) -0.0039(6) O3 0.0236(6) 0.0237(7) 0.0447(9) -0.0018(6) 0.0041(6) -0.0003(5) O4 0.0336(7) 0.0434(9) 0.0346(8) 0.0025(7) -0.0048(6) -0.0223(7) N1 0.0165(6) 0.0212(7) 0.0141(6) 0.0051(5) -0.0026(5) -0.0009(5) N2 0.0178(6) 0.0159(6) 0.0149(6) 0.0019(5) -0.0037(5) -0.0066(5) N3 0.0168(6) 0.0172(7) 0.0133(6) 0.0023(5) -0.0017(5) -0.0047(5) C1 0.0230(8) 0.0203(8) 0.0171(8) 0.0011(6) -0.0072(6) -0.0051(6) C2 0.0224(8) 0.0264(9) 0.0215(8) -0.0004(7) -0.0073(7) -0.0052(7) C3 0.0233(8) 0.0180(8) 0.0210(8) 0.0047(6) -0.0026(6) -0.0045(6) C4 0.0227(8) 0.0260(9) 0.0177(8) 0.0049(7) -0.0011(6) -0.0057(7) C5 0.0199(8) 0.0391(11) 0.0154(8) 0.0021(7) -0.0042(6) -0.0063(7) C6 0.0196(8) 0.0340(10) 0.0187(8) -0.0025(7) -0.0077(6) -0.0017(7) C7 0.0313(9) 0.0325(10) 0.0246(9) -0.0002(8) -0.0114(8) -0.0060(8) C8 0.0422(11) 0.0333(11) 0.0399(12) 0.0010(9) -0.0222(10) -0.0095(9) C9 0.0390(11) 0.0374(12) 0.0422(13) -0.0140(10) -0.0216(10) 0.0013(9) C10 0.0290(10) 0.0601(15) 0.0272(10) -0.0170(10) -0.0097(8) 0.0009(10) C11 0.0223(9) 0.0526(13) 0.0216(9) -0.0067(9) -0.0055(7) -0.0053(8) C12 0.0199(8) 0.0336(10) 0.0188(8) 0.0017(7) -0.0079(6) -0.0011(7) C13 0.0227(8) 0.0374(11) 0.0249(9) -0.0038(8) -0.0068(7) -0.0045(8) C14 0.0209(9) 0.0522(14) 0.0294(10) -0.0100(9) -0.0074(8) 0.0006(8) C15 0.0311(11) 0.0503(15) 0.0448(13) -0.0010(11) -0.0151(10) 0.0114(10) C16 0.0404(13) 0.0463(15) 0.077(2) 0.0274(14) -0.0138(13) 0.0059(11) C17 0.0260(10) 0.0477(14) 0.0583(16) 0.0264(12) -0.0082(10) -0.0004(9) C18 0.0263(9) 0.0277(9) 0.0182(8) 0.0067(7) -0.0023(7) 0.0005(7) C19 0.0364(10) 0.0312(10) 0.0181(9) 0.0048(7) -0.0030(7) 0.0002(8) C20 0.0555(14) 0.0409(13) 0.0216(10) 0.0123(9) -0.0037(9) 0.0016(10) C21 0.083(2) 0.0348(13) 0.0333(13) 0.0170(10) -0.0010(12) 0.0094(13) C22 0.084(2) 0.0293(12) 0.0309(12) 0.0075(9) 0.0055(12) 0.0109(12) C23 0.0509(13) 0.0295(11) 0.0201(9) 0.0055(8) 0.0025(8) 0.0047(9) C24 0.0181(7) 0.0306(9) 0.0136(7) 0.0074(7) -0.0013(6) -0.0020(6) C25 0.0272(9) 0.0425(12) 0.0200(9) 0.0027(8) -0.0029(7) -0.0101(8) C26 0.0246(9) 0.0670(16) 0.0246(10) 0.0142(10) -0.0056(8) -0.0170(10) C27 0.0178(8) 0.0655(16) 0.0297(11) 0.0160(10) 0.0007(8) -0.0001(9) C28 0.0293(10) 0.0398(12) 0.0371(12) 0.0023(10) 0.0030(9) 0.0086(9) C29 0.0243(9) 0.0292(10) 0.0308(10) 0.0038(8) -0.0008(7) -0.0007(7) C30 0.0188(7) 0.0277(9) 0.0158(8) 0.0053(7) -0.0015(6) -0.0007(6) C31 0.0221(9) 0.0411(12) 0.0292(10) 0.0050(9) 0.0017(7) -0.0083(8) C32 0.0268(9) 0.0315(10) 0.0206(9) -0.0003(7) -0.0017(7) 0.0023(7) C33 0.0228(8) 0.0261(9) 0.0173(8) 0.0078(7) -0.0050(6) 0.0013(7) C34 0.0277(9) 0.0436(12) 0.0226(9) 0.0068(8) -0.0080(7) 0.0082(8) C35 0.0432(11) 0.0239(10) 0.0312(10) 0.0099(8) -0.0054(9) -0.0055(8) C36 0.0171(7) 0.0154(7) 0.0136(7) 0.0026(6) -0.0035(6) -0.0034(6) C37 0.0188(7) 0.0154(7) 0.0148(7) 0.0017(6) -0.0042(6) -0.0041(6) C38 0.0194(7) 0.0193(8) 0.0132(7) 0.0017(6) -0.0035(6) -0.0065(6) C39 0.0266(8) 0.0223(8) 0.0180(8) 0.0028(6) -0.0054(6) -0.0149(7) C40 0.0221(8) 0.0298(10) 0.0288(9) 0.0043(7) -0.0064(7) -0.0137(7) C41 0.0346(10) 0.0185(8) 0.0253(9) 0.0022(7) -0.0021(7) -0.0094(7) C42 0.0482(12) 0.0415(12) 0.0232(9) 0.0060(8) -0.0126(8) -0.0317(10) C43 0.0181(7) 0.0208(8) 0.0168(7) 0.0046(6) -0.0005(6) -0.0081(6) C44 0.0183(8) 0.0329(10) 0.0293(10) 0.0090(8) -0.0036(7) -0.0065(7) C45 0.0299(9) 0.0274(9) 0.0147(8) 0.0030(7) -0.0001(7) -0.0104(7) C46 0.0285(9) 0.0216(9) 0.0222(8) 0.0033(7) -0.0028(7) -0.0111(7) _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 O1B C4B 1.416(10) . ? O1B C1B 1.448(9) . ? C1B C2B 1.451(9) . ? C2B C3B 1.448(9) . ? C3B C4B 1.459(9) . ? O1G C4G 1.443(10) . ? O1G C1G 1.444(10) . ? C1G C2G 1.477(10) . ? C2G C3G 1.465(10) . ? C3G C4G 1.466(10) . ? O1F C4F 1.439(10) . ? O1F C1F 1.449(10) . ? C1F C2F 1.468(9) . ? C2F C3F 1.469(10) . ? C3F C4F 1.460(9) . ? O1S C4S 1.424(8) . ? O1S C1S 1.427(9) . ? C1S C2S 1.460(9) . ? C2S C3S 1.513(8) . ? C3S C4S 1.438(9) . ? O1T C1T 1.409(9) . ? O1T C4T 1.432(9) . ? C1T C2T 1.466(9) . ? C2T C3T 1.508(9) . ? C3T C4T 1.480(10) . ? O1A C4A 1.437(10) . ? O1A C1A 1.437(10) . ? C1A C2A 1.465(10) . ? C2A C3A 1.463(10) . ? C3A C4A 1.475(10) . ? Co1 C2 1.7376(19) . ? Co1 C1 1.7577(17) . ? Co1 P3 2.1585(5) . ? Co1 P1 2.1739(5) . ? Co1 Co2 2.6835(4) . ? Co2 C4 1.7397(19) . ? Co2 C3 1.7561(17) . ? Co2 P3 2.1298(5) . ? Co2 P2 2.1774(5) . ? P1 C5 1.8316(18) . ? P1 C12 1.8360(19) . ? P1 C6 1.8419(19) . ? P2 C24 1.8410(17) . ? P2 C18 1.8447(19) . ? P2 C5 1.8479(19) . ? P3 N1 1.7102(14) . ? P3 C36 1.8646(16) . ? O1 C1 1.157(2) . ? O2 C2 1.162(2) . ? O3 C3 1.164(2) . ? O4 C4 1.161(2) . ? N1 C33 1.474(2) . ? N1 C30 1.484(2) . ? N2 C37 1.334(2) . ? N2 C36 1.412(2) . ? N2 C39 1.509(2) . ? N3 C37 1.327(2) . ? N3 C38 1.374(2) . ? N3 C43 1.500(2) . ? C6 C11 1.396(3) . ? C6 C7 1.398(3) . ? C7 C8 1.389(3) . ? C8 C9 1.383(3) . ? C9 C10 1.383(4) . ? C10 C11 1.387(3) . ? C12 C17 1.377(3) . ? C12 C13 1.392(3) . ? C13 C14 1.385(3) . ? C14 C15 1.364(4) . ? C15 C16 1.377(4) . ? C16 C17 1.403(3) . ? C18 C23 1.385(3) . ? C18 C19 1.400(3) . ? C19 C20 1.385(3) . ? C20 C21 1.383(4) . ? C21 C22 1.378(3) . ? C22 C23 1.394(3) . ? C24 C29 1.383(3) . ? C24 C25 1.397(3) . ? C25 C26 1.391(3) . ? C26 C27 1.375(4) . ? C27 C28 1.365(4) . ? C28 C29 1.394(3) . ? C30 C31 1.526(3) . ? C30 C32 1.529(3) . ? C33 C35 1.528(3) . ? C33 C34 1.531(3) . ? C36 C38 1.366(2) . ? C39 C40 1.521(2) . ? C39 C42 1.526(3) . ? C39 C41 1.527(3) . ? C43 C46 1.522(2) . ? C43 C44 1.526(2) . ? C43 C45 1.528(2) . ? 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 C4B O1B C1B 113.3(10) . . ? O1B C1B C2B 102.3(9) . . ? C3B C2B C1B 109.8(9) . . ? C2B C3B C4B 106.5(10) . . ? O1B C4B C3B 103.3(10) . . ? C4G O1G C1G 99.2(16) . . ? O1G C1G C2G 107.4(12) . . ? C3G C2G C1G 103.7(10) . . ? C2G C3G C4G 104.7(10) . . ? O1G C4G C3G 109.6(11) . . ? C4F O1F C1F 104.6(10) . . ? O1F C1F C2F 106.1(10) . . ? C1F C2F C3F 102.7(10) . . ? C4F C3F C2F 106.9(9) . . ? O1F C4F C3F 107.9(9) . . ? C4S O1S C1S 99.2(7) . . ? O1S C1S C2S 109.3(9) . . ? C1S C2S C3S 101.6(8) . . ? C4S C3S C2S 104.5(8) . . ? O1S C4S C3S 110.5(8) . . ? C1T O1T C4T 107.5(8) . . ? O1T C1T C2T 107.7(9) . . ? C1T C2T C3T 101.1(9) . . ? C4T C3T C2T 105.3(9) . . ? O1T C4T C3T 107.0(8) . . ? C4A O1A C1A 107.3(11) . . ? O1A C1A C2A 107.7(11) . . ? C3A C2A C1A 106.2(11) . . ? C2A C3A C4A 104.6(11) . . ? O1A C4A C3A 108.8(11) . . ? C2 Co1 C1 117.80(8) . . ? C2 Co1 P3 99.73(6) . . ? C1 Co1 P3 106.13(6) . . ? C2 Co1 P1 97.26(6) . . ? C1 Co1 P1 101.32(6) . . ? P3 Co1 P1 135.725(19) . . ? C2 Co1 Co2 131.48(6) . . ? C1 Co1 Co2 108.13(6) . . ? P3 Co1 Co2 50.784(13) . . ? P1 Co1 Co2 87.995(15) . . ? C4 Co2 C3 109.39(8) . . ? C4 Co2 P3 106.71(6) . . ? C3 Co2 P3 106.63(6) . . ? C4 Co2 P2 97.46(6) . . ? C3 Co2 P2 113.10(6) . . ? P3 Co2 P2 122.52(2) . . ? C4 Co2 Co1 158.16(6) . . ? C3 Co2 Co1 83.44(6) . . ? P3 Co2 Co1 51.741(14) . . ? P2 Co2 Co1 93.236(15) . . ? C5 P1 C12 104.85(9) . . ? C5 P1 C6 102.42(8) . . ? C12 P1 C6 101.43(8) . . ? C5 P1 Co1 112.83(6) . . ? C12 P1 Co1 118.17(6) . . ? C6 P1 Co1 115.27(6) . . ? C24 P2 C18 96.61(8) . . ? C24 P2 C5 103.35(8) . . ? C18 P2 C5 101.33(9) . . ? C24 P2 Co2 118.98(6) . . ? C18 P2 Co2 117.99(6) . . ? C5 P2 Co2 115.42(6) . . ? N1 P3 C36 99.27(7) . . ? N1 P3 Co2 123.92(5) . . ? C36 P3 Co2 121.07(5) . . ? N1 P3 Co1 123.76(5) . . ? C36 P3 Co1 112.04(5) . . ? Co2 P3 Co1 77.475(16) . . ? C33 N1 C30 121.92(13) . . ? C33 N1 P3 121.98(11) . . ? C30 N1 P3 113.62(11) . . ? C37 N2 C36 108.58(13) . . ? C37 N2 C39 121.22(14) . . ? C36 N2 C39 129.72(13) . . ? C37 N3 C38 107.50(13) . . ? C37 N3 C43 126.67(14) . . ? C38 N3 C43 125.79(14) . . ? O1 C1 Co1 175.69(16) . . ? O2 C2 Co1 173.93(17) . . ? O3 C3 Co2 175.69(17) . . ? O4 C4 Co2 177.73(17) . . ? P1 C5 P2 108.68(9) . . ? C11 C6 C7 118.35(18) . . ? C11 C6 P1 123.25(16) . . ? C7 C6 P1 118.39(14) . . ? C8 C7 C6 120.77(19) . . ? C9 C8 C7 120.2(2) . . ? C8 C9 C10 119.6(2) . . ? C9 C10 C11 120.6(2) . . ? C10 C11 C6 120.5(2) . . ? C17 C12 C13 118.22(18) . . ? C17 C12 P1 123.58(15) . . ? C13 C12 P1 118.07(15) . . ? C14 C13 C12 120.8(2) . . ? C15 C14 C13 120.6(2) . . ? C14 C15 C16 119.9(2) . . ? C15 C16 C17 119.7(3) . . ? C12 C17 C16 120.8(2) . . ? C23 C18 C19 118.75(18) . . ? C23 C18 P2 120.87(14) . . ? C19 C18 P2 120.37(15) . . ? C20 C19 C18 120.8(2) . . ? C21 C20 C19 119.6(2) . . ? C22 C21 C20 120.2(2) . . ? C21 C22 C23 120.2(2) . . ? C18 C23 C22 120.3(2) . . ? C29 C24 C25 118.07(17) . . ? C29 C24 P2 124.96(15) . . ? C25 C24 P2 116.87(14) . . ? C26 C25 C24 120.7(2) . . ? C27 C26 C25 120.2(2) . . ? C28 C27 C26 119.65(19) . . ? C27 C28 C29 120.8(2) . . ? C24 C29 C28 120.6(2) . . ? N1 C30 C31 112.69(15) . . ? N1 C30 C32 115.41(15) . . ? C31 C30 C32 111.86(15) . . ? N1 C33 C35 114.56(15) . . ? N1 C33 C34 113.78(15) . . ? C35 C33 C34 111.18(16) . . ? C38 C36 N2 104.46(13) . . ? C38 C36 P3 121.33(12) . . ? N2 C36 P3 134.20(12) . . ? N3 C37 N2 109.92(14) . . ? C36 C38 N3 109.53(14) . . ? N2 C39 C40 108.67(14) . . ? N2 C39 C42 108.59(14) . . ? C40 C39 C42 109.65(16) . . ? N2 C39 C41 106.92(14) . . ? C40 C39 C41 113.12(15) . . ? C42 C39 C41 109.76(16) . . ? N3 C43 C46 107.52(13) . . ? N3 C43 C44 107.63(13) . . ? C46 C43 C44 112.03(15) . . ? N3 C43 C45 109.51(13) . . ? C46 C43 C45 109.22(14) . . ? C44 C43 C45 110.84(15) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 29.60 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.542 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.071