# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_rrmur302 _database_code_depnum_ccdc_archive 'CCDC 751230' #TrackingRef '- Complex 2.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Ni hydrozone complex' ; _chemical_name_common "'Ni hydrozone complex'" _chemical_melting_point ? _chemical_formula_moiety 'C32 H25 N2 Ni O2 P' _chemical_formula_sum 'C32 H25 N2 Ni O2 P' _chemical_formula_weight 559.20 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6153(2) _cell_length_b 10.18390(10) _cell_length_c 17.6301(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.0130(10) _cell_angle_gamma 90.00 _cell_volume 2620.45(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9772 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 33.4 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8122 _exptl_absorpt_correction_T_max 0.8850 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 SMART APEX II CCD area-detector' _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 35579 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 33.41 _reflns_number_total 9769 _reflns_number_gt 5533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0873P)^2^+1.7888P] 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 9769 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Ni1 Ni 0.77246(2) -0.10348(3) 0.835011(19) 0.03506(12) Uani 1 1 d . . . P1 P 0.73827(5) 0.10589(6) 0.81287(4) 0.03242(15) Uani 1 1 d . . . O1 O 0.82871(16) -0.0656(2) 0.92659(12) 0.0461(5) Uani 1 1 d . . . O2 O 0.72346(15) -0.1417(2) 0.74106(12) 0.0452(5) Uani 1 1 d . . . N2 N 0.76037(17) -0.3525(2) 0.77572(13) 0.0398(5) Uani 1 1 d . . . N1 N 0.79113(16) -0.2827(2) 0.84088(13) 0.0364(5) Uani 1 1 d . . . C21 C 0.82710(18) 0.1863(3) 0.76154(14) 0.0330(5) Uani 1 1 d . . . C9 C 0.6879(2) -0.3147(3) 0.65189(16) 0.0402(6) Uani 1 1 d . . . C27 C 0.7253(2) 0.2133(3) 0.89381(16) 0.0389(6) Uani 1 1 d . . . C6 C 0.8658(2) -0.2864(3) 0.96483(16) 0.0380(6) Uani 1 1 d . . . C15 C 0.63342(19) 0.1252(3) 0.75409(15) 0.0363(6) Uani 1 1 d . . . C1 C 0.8662(2) -0.1501(3) 0.97540(16) 0.0394(6) Uani 1 1 d . . . C25 C 0.9081(2) 0.3789(3) 0.72384(19) 0.0479(7) Uani 1 1 d . . . H25 H 0.9151 0.4697 0.7250 0.058 Uiso 1 1 calc R . . C26 C 0.8392(2) 0.3210(3) 0.76261(17) 0.0417(6) Uani 1 1 d . . . H26 H 0.8004 0.3732 0.7899 0.050 Uiso 1 1 calc R . . C20 C 0.6238(2) 0.2163(3) 0.69615(18) 0.0491(7) Uani 1 1 d . . . H20 H 0.6727 0.2700 0.6850 0.059 Uiso 1 1 calc R . . C22 C 0.8856(2) 0.1099(3) 0.71925(18) 0.0434(6) Uani 1 1 d . . . H22 H 0.8778 0.0193 0.7170 0.052 Uiso 1 1 calc R . . C32 C 0.7989(3) 0.2243(3) 0.94718(19) 0.0506(8) Uani 1 1 d . . . H32 H 0.8523 0.1766 0.9410 0.061 Uiso 1 1 calc R . . C5 C 0.9079(3) -0.3686(3) 1.0208(2) 0.0541(8) Uani 1 1 d . . . H5 H 0.9073 -0.4591 1.0137 0.065 Uiso 1 1 calc R . . C8 C 0.7262(2) -0.2685(3) 0.72651(16) 0.0384(6) Uani 1 1 d . . . C7 C 0.8268(2) -0.3479(3) 0.89740(17) 0.0413(6) Uani 1 1 d . . . H7 H 0.8273 -0.4390 0.8945 0.050 Uiso 1 1 calc R . . C28 C 0.6467(3) 0.2847(4) 0.9042(2) 0.0576(9) Uani 1 1 d . . . H28 H 0.5965 0.2772 0.8699 0.069 Uiso 1 1 calc R . . C23 C 0.9543(2) 0.1681(4) 0.6810(2) 0.0544(8) Uani 1 1 d . . . H23 H 0.9931 0.1168 0.6531 0.065 Uiso 1 1 calc R . . C24 C 0.9662(2) 0.3036(4) 0.6836(2) 0.0529(8) Uani 1 1 d . . . H24 H 1.0132 0.3427 0.6583 0.063 Uiso 1 1 calc R . . C10 C 0.6996(2) -0.4407(3) 0.62703(19) 0.0520(8) Uani 1 1 d . . . H10 H 0.7334 -0.4996 0.6575 0.062 Uiso 1 1 calc R . . C2 C 0.9095(3) -0.1004(3) 1.04206(19) 0.0529(8) Uani 1 1 d . . . H2 H 0.9109 -0.0101 1.0498 0.063 Uiso 1 1 calc R . . C3 C 0.9500(3) -0.1814(4) 1.09618(19) 0.0571(9) Uani 1 1 d . . . H3 H 0.9777 -0.1453 1.1401 0.069 Uiso 1 1 calc R . . C18 C 0.4686(2) 0.1491(5) 0.6704(2) 0.0622(10) Uani 1 1 d . . . H18 H 0.4133 0.1575 0.6423 0.075 Uiso 1 1 calc R . . C16 C 0.5596(2) 0.0454(4) 0.7692(2) 0.0526(8) Uani 1 1 d . . . H16 H 0.5653 -0.0172 0.8076 0.063 Uiso 1 1 calc R . . C11 C 0.6621(3) -0.4820(4) 0.5576(2) 0.0617(9) Uani 1 1 d . . . H11 H 0.6696 -0.5684 0.5419 0.074 Uiso 1 1 calc R . . C4 C 0.9500(3) -0.3162(4) 1.0862(2) 0.0624(10) Uani 1 1 d . . . H4 H 0.9779 -0.3708 1.1229 0.075 Uiso 1 1 calc R . . C14 C 0.6377(3) -0.2271(4) 0.6058(2) 0.0674(11) Uani 1 1 d . . . H14 H 0.6286 -0.1413 0.6218 0.081 Uiso 1 1 calc R . . C19 C 0.5406(3) 0.2276(4) 0.6545(2) 0.0627(10) Uani 1 1 d . . . H19 H 0.5342 0.2890 0.6156 0.075 Uiso 1 1 calc R . . C31 C 0.7924(3) 0.3063(4) 1.0093(2) 0.0660(11) Uani 1 1 d . . . H31 H 0.8408 0.3119 1.0456 0.079 Uiso 1 1 calc R . . C30 C 0.7152(4) 0.3787(4) 1.0176(2) 0.0761(13) Uani 1 1 d . . . H30 H 0.7118 0.4357 1.0585 0.091 Uiso 1 1 calc R . . C17 C 0.4768(2) 0.0593(4) 0.7268(2) 0.0616(9) Uani 1 1 d . . . H17 H 0.4271 0.0065 0.7374 0.074 Uiso 1 1 calc R . . C12 C 0.6142(3) -0.3957(4) 0.5122(2) 0.0708(11) Uani 1 1 d . . . H12 H 0.5900 -0.4228 0.4649 0.085 Uiso 1 1 calc R . . C29 C 0.6432(3) 0.3677(5) 0.9661(3) 0.0763(13) Uani 1 1 d . . . H29 H 0.5906 0.4168 0.9727 0.092 Uiso 1 1 calc R . . C13 C 0.6011(3) -0.2689(5) 0.5354(2) 0.0828(14) Uani 1 1 d . . . H13 H 0.5677 -0.2107 0.5041 0.099 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 Ni1 0.0424(2) 0.02850(16) 0.03388(19) 0.00086(13) -0.00201(14) 0.00211(14) P1 0.0359(3) 0.0280(3) 0.0333(3) 0.0011(2) 0.0012(3) 0.0020(3) O1 0.0643(14) 0.0343(10) 0.0381(10) -0.0022(8) -0.0125(10) 0.0067(9) O2 0.0567(13) 0.0301(9) 0.0482(12) 0.0039(8) -0.0034(10) 0.0083(9) N2 0.0450(13) 0.0352(11) 0.0381(12) -0.0009(10) -0.0079(10) 0.0028(10) N1 0.0410(13) 0.0320(11) 0.0360(12) -0.0018(9) 0.0004(10) -0.0041(9) C21 0.0319(13) 0.0343(12) 0.0324(12) 0.0031(10) -0.0026(10) 0.0001(10) C9 0.0423(15) 0.0440(15) 0.0339(13) -0.0023(11) -0.0014(11) -0.0039(12) C27 0.0495(16) 0.0345(13) 0.0330(13) 0.0016(10) 0.0051(11) 0.0008(12) C6 0.0375(14) 0.0384(13) 0.0375(14) 0.0045(11) -0.0032(11) 0.0012(11) C15 0.0371(14) 0.0370(13) 0.0348(13) -0.0038(10) 0.0009(10) 0.0042(11) C1 0.0432(15) 0.0394(13) 0.0352(14) -0.0003(11) 0.0003(11) 0.0049(12) C25 0.0504(18) 0.0418(16) 0.0512(18) 0.0063(13) -0.0010(14) -0.0121(13) C26 0.0455(16) 0.0358(13) 0.0438(15) -0.0021(11) 0.0034(12) -0.0004(12) C20 0.0451(17) 0.0577(19) 0.0438(16) 0.0083(14) -0.0047(13) -0.0004(14) C22 0.0465(16) 0.0379(14) 0.0463(16) 0.0016(12) 0.0060(13) 0.0062(12) C32 0.061(2) 0.0415(15) 0.0482(17) 0.0019(13) -0.0094(15) -0.0018(14) C5 0.060(2) 0.0412(16) 0.059(2) 0.0090(14) -0.0148(16) -0.0001(14) C8 0.0428(15) 0.0357(13) 0.0362(13) -0.0012(11) -0.0017(11) -0.0005(11) C7 0.0491(16) 0.0288(12) 0.0452(16) 0.0016(11) -0.0044(13) 0.0011(12) C28 0.056(2) 0.061(2) 0.056(2) -0.0124(16) 0.0062(16) 0.0118(16) C23 0.0476(18) 0.059(2) 0.058(2) 0.0016(16) 0.0162(15) 0.0100(15) C24 0.0441(17) 0.062(2) 0.0534(19) 0.0138(16) 0.0070(14) -0.0073(15) C10 0.062(2) 0.0473(17) 0.0456(17) -0.0052(14) -0.0067(15) 0.0015(15) C2 0.065(2) 0.0493(17) 0.0432(16) -0.0068(14) -0.0119(15) 0.0056(15) C3 0.062(2) 0.067(2) 0.0405(17) -0.0037(15) -0.0152(15) 0.0082(17) C18 0.0405(18) 0.093(3) 0.052(2) -0.008(2) -0.0086(15) 0.0090(19) C16 0.0442(17) 0.0561(19) 0.0573(19) 0.0069(16) 0.0013(14) -0.0036(15) C11 0.072(2) 0.062(2) 0.0497(19) -0.0152(17) -0.0046(17) -0.0028(19) C4 0.073(2) 0.062(2) 0.0506(19) 0.0119(16) -0.0169(17) 0.0074(18) C14 0.096(3) 0.053(2) 0.051(2) -0.0039(16) -0.018(2) 0.015(2) C19 0.052(2) 0.086(3) 0.0486(19) 0.0103(18) -0.0097(15) 0.0100(19) C31 0.099(3) 0.054(2) 0.0441(18) -0.0051(15) -0.0094(19) -0.018(2) C30 0.116(4) 0.065(2) 0.050(2) -0.0199(18) 0.026(2) -0.013(2) C17 0.0377(17) 0.078(3) 0.070(2) -0.009(2) 0.0019(16) -0.0079(17) C12 0.081(3) 0.083(3) 0.0463(19) -0.0182(19) -0.0126(19) 0.001(2) C29 0.080(3) 0.078(3) 0.073(3) -0.029(2) 0.022(2) 0.011(2) C13 0.107(4) 0.082(3) 0.056(2) -0.002(2) -0.037(2) 0.019(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 Ni1 O2 1.812(2) . ? Ni1 O1 1.814(2) . ? Ni1 N1 1.848(2) . ? Ni1 P1 2.2199(7) . ? P1 C15 1.815(3) . ? P1 C27 1.816(3) . ? P1 C21 1.816(3) . ? O1 C1 1.316(3) . ? O2 C8 1.317(3) . ? N2 C8 1.300(4) . ? N2 N1 1.405(3) . ? N1 C7 1.285(4) . ? C21 C26 1.383(4) . ? C21 C22 1.400(4) . ? C9 C10 1.370(4) . ? C9 C14 1.390(5) . ? C9 C8 1.479(4) . ? C27 C28 1.380(5) . ? C27 C32 1.397(4) . ? C6 C1 1.400(4) . ? C6 C5 1.410(4) . ? C6 C7 1.435(4) . ? C15 C20 1.381(4) . ? C15 C16 1.389(4) . ? C1 C2 1.400(4) . ? C25 C24 1.370(5) . ? C25 C26 1.379(4) . ? C20 C19 1.391(5) . ? C22 C23 1.375(5) . ? C32 C31 1.385(5) . ? C5 C4 1.385(5) . ? C28 C29 1.384(5) . ? C23 C24 1.390(5) . ? C10 C11 1.381(5) . ? C2 C3 1.371(5) . ? C3 C4 1.384(5) . ? C18 C17 1.352(6) . ? C18 C19 1.363(6) . ? C16 C17 1.395(5) . ? C11 C12 1.358(6) . ? C14 C13 1.391(5) . ? C31 C30 1.362(7) . ? C30 C29 1.356(7) . ? C12 C13 1.371(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 O2 Ni1 O1 176.34(10) . . ? O2 Ni1 N1 83.63(9) . . ? O1 Ni1 N1 95.82(10) . . ? O2 Ni1 P1 88.35(7) . . ? O1 Ni1 P1 92.27(7) . . ? N1 Ni1 P1 171.86(7) . . ? C15 P1 C27 105.26(13) . . ? C15 P1 C21 105.71(12) . . ? C27 P1 C21 103.12(13) . . ? C15 P1 Ni1 112.35(9) . . ? C27 P1 Ni1 118.19(9) . . ? C21 P1 Ni1 111.13(9) . . ? C1 O1 Ni1 126.64(19) . . ? C8 O2 Ni1 111.97(17) . . ? C8 N2 N1 107.9(2) . . ? C7 N1 N2 118.2(2) . . ? C7 N1 Ni1 127.3(2) . . ? N2 N1 Ni1 114.48(17) . . ? C26 C21 C22 118.5(3) . . ? C26 C21 P1 122.3(2) . . ? C22 C21 P1 119.1(2) . . ? C10 C9 C14 119.0(3) . . ? C10 C9 C8 122.4(3) . . ? C14 C9 C8 118.7(3) . . ? C28 C27 C32 119.1(3) . . ? C28 C27 P1 123.0(2) . . ? C32 C27 P1 118.0(2) . . ? C1 C6 C5 119.8(3) . . ? C1 C6 C7 122.8(2) . . ? C5 C6 C7 117.4(3) . . ? C20 C15 C16 119.0(3) . . ? C20 C15 P1 123.1(2) . . ? C16 C15 P1 117.9(2) . . ? O1 C1 C2 117.8(3) . . ? O1 C1 C6 124.2(3) . . ? C2 C1 C6 117.9(3) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 120.9(3) . . ? C15 C20 C19 119.9(3) . . ? C23 C22 C21 120.3(3) . . ? C31 C32 C27 119.9(4) . . ? C4 C5 C6 120.8(3) . . ? N2 C8 O2 122.0(3) . . ? N2 C8 C9 119.9(3) . . ? O2 C8 C9 118.1(2) . . ? N1 C7 C6 123.0(3) . . ? C27 C28 C29 119.5(4) . . ? C22 C23 C24 120.3(3) . . ? C25 C24 C23 119.6(3) . . ? C9 C10 C11 121.3(3) . . ? C3 C2 C1 121.7(3) . . ? C2 C3 C4 120.8(3) . . ? C17 C18 C19 120.6(3) . . ? C15 C16 C17 119.9(3) . . ? C12 C11 C10 119.6(4) . . ? C3 C4 C5 119.0(3) . . ? C9 C14 C13 119.4(4) . . ? C18 C19 C20 120.4(4) . . ? C30 C31 C32 120.2(4) . . ? C29 C30 C31 120.1(4) . . ? C18 C17 C16 120.3(4) . . ? C11 C12 C13 120.7(3) . . ? C30 C29 C28 121.2(4) . . ? C12 C13 C14 120.1(4) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.321 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.087 data_cobhs _database_code_depnum_ccdc_archive 'CCDC 896151' #TrackingRef 'cobhs.cif' # start Validation Reply Form _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The data was collected from a poor quality crystal resulting with limited resolution. ; _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 21.66 Deg. RESPONSE: The data was collected from a poor quality crystal resulting with limited resolution. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H111.20 Co3 N8 O17.60 P4' _chemical_formula_weight 2343.72 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.5181(5) _cell_length_b 14.2200(6) _cell_length_c 19.9005(9) _cell_angle_alpha 77.689(3) _cell_angle_beta 84.636(3) _cell_angle_gamma 79.795(3) _cell_volume 2857.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4053 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 61.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1217 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 0.8685 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'APEX II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30411 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 21.66 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 6655 _reflns_number_gt 4074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; APEX-II(BRUKER-NONIUS, 2003) ; _computing_data_reduction APEX-II _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _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^)+(0.0463P)^2^+12.7386P] 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 6655 _refine_ls_number_parameters 727 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.2063 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _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 0.52556(11) 0.26394(9) 0.79616(6) 0.0568(4) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 1.0000 0.0524(5) Uani 1 2 d S . . P1 P 0.3295(2) 0.70109(17) 0.90511(12) 0.0533(7) Uani 1 1 d . . . P2 P 0.1061(3) 0.2555(2) 0.43481(15) 0.0755(8) Uani 1 1 d . . . C1 C 0.3838(8) 0.2410(7) 0.9127(4) 0.051(2) Uani 1 1 d . . . C2 C 0.3352(9) 0.1926(6) 0.9811(4) 0.056(2) Uani 1 1 d . . . C3 C 0.4059(9) 0.1105(6) 1.0186(5) 0.060(2) Uani 1 1 d . . . H3 H 0.4889 0.0872 1.0024 0.072 Uiso 1 1 calc R . . C4 C 0.3537(11) 0.0620(7) 1.0808(5) 0.079(3) Uani 1 1 d . . . H4 H 0.4021 0.0066 1.1058 0.095 Uiso 1 1 calc R . . C5 C 0.2315(13) 0.0955(9) 1.1052(6) 0.090(3) Uani 1 1 d . . . H5 H 0.1967 0.0626 1.1464 0.109 Uiso 1 1 calc R . . C6 C 0.1615(11) 0.1773(8) 1.0687(5) 0.081(3) Uani 1 1 d . . . H6 H 0.0792 0.2003 1.0859 0.097 Uiso 1 1 calc R . . C7 C 0.2094(9) 0.2269(7) 1.0070(5) 0.064(3) Uani 1 1 d . . . H7 H 0.1598 0.2822 0.9827 0.077 Uiso 1 1 calc R . . C8 C 0.3416(8) 0.4371(6) 0.7812(4) 0.050(2) Uani 1 1 d . . . H8 H 0.2713 0.4760 0.7988 0.060 Uiso 1 1 calc R . . C9 C 0.3894(8) 0.4717(6) 0.7121(4) 0.051(2) Uani 1 1 d . . . C10 C 0.3320(9) 0.5640(7) 0.6763(5) 0.064(3) Uani 1 1 d . . . H10 H 0.2620 0.5982 0.6978 0.076 Uiso 1 1 calc R . . C11 C 0.3740(10) 0.6050(8) 0.6123(5) 0.076(3) Uani 1 1 d . . . H11 H 0.3339 0.6660 0.5903 0.091 Uiso 1 1 calc R . . C12 C 0.4793(11) 0.5536(8) 0.5799(5) 0.079(3) Uani 1 1 d . . . H12 H 0.5091 0.5799 0.5356 0.094 Uiso 1 1 calc R . . C13 C 0.5383(9) 0.4646(7) 0.6133(5) 0.069(3) Uani 1 1 d . . . H13 H 0.6080 0.4319 0.5905 0.083 Uiso 1 1 calc R . . C14 C 0.4988(8) 0.4195(7) 0.6810(5) 0.058(2) Uani 1 1 d . . . C15 C 0.4732(10) 0.1236(7) 0.7415(4) 0.057(2) Uani 1 1 d . . . C16 C 0.3975(10) 0.0661(7) 0.7133(5) 0.063(3) Uani 1 1 d . . . C17 C 0.2680(11) 0.1010(8) 0.7000(5) 0.079(3) Uani 1 1 d . . . H17 H 0.2291 0.1609 0.7099 0.095 Uiso 1 1 calc R . . C18 C 0.1982(12) 0.0478(10) 0.6725(6) 0.098(4) Uani 1 1 d . . . H18 H 0.1121 0.0723 0.6635 0.117 Uiso 1 1 calc R . . C19 C 0.2516(15) -0.0400(12) 0.6581(6) 0.110(4) Uani 1 1 d . . . H19 H 0.2019 -0.0761 0.6405 0.132 Uiso 1 1 calc R . . C20 C 0.3805(14) -0.0760(9) 0.6697(6) 0.103(4) Uani 1 1 d . . . H20 H 0.4184 -0.1355 0.6588 0.123 Uiso 1 1 calc R . . C21 C 0.4522(11) -0.0232(8) 0.6974(5) 0.074(3) Uani 1 1 d . . . H21 H 0.5386 -0.0477 0.7055 0.089 Uiso 1 1 calc R . . C22 C 0.7700(9) 0.1487(6) 0.7811(4) 0.057(2) Uani 1 1 d . . . H22 H 0.8207 0.0941 0.7682 0.068 Uiso 1 1 calc R . . C23 C 0.8349(8) 0.2128(6) 0.8061(4) 0.053(2) Uani 1 1 d . . . C24 C 0.9704(9) 0.1899(7) 0.8069(5) 0.064(3) Uani 1 1 d . . . H24 H 1.0118 0.1340 0.7919 0.077 Uiso 1 1 calc R . . C25 C 1.0435(10) 0.2467(7) 0.8286(5) 0.074(3) Uani 1 1 d . . . H25 H 1.1332 0.2305 0.8273 0.089 Uiso 1 1 calc R . . C26 C 0.9822(10) 0.3285(7) 0.8525(5) 0.074(3) Uani 1 1 d . . . H26 H 1.0305 0.3673 0.8684 0.088 Uiso 1 1 calc R . . C27 C 0.8496(9) 0.3525(7) 0.8526(5) 0.065(3) Uani 1 1 d . . . H27 H 0.8096 0.4087 0.8677 0.078 Uiso 1 1 calc R . . C28 C 0.7731(9) 0.2950(6) 0.8310(4) 0.054(2) Uani 1 1 d . . . C29 C 0.2777(8) 0.8183(6) 0.9244(5) 0.054(2) Uani 1 1 d . . . C30 C 0.2298(10) 0.8253(7) 0.9902(5) 0.073(3) Uani 1 1 d . . . H30 H 0.2318 0.7691 1.0243 0.088 Uiso 1 1 calc R . . C31 C 0.1795(11) 0.9132(8) 1.0058(6) 0.085(3) Uani 1 1 d . . . H31 H 0.1456 0.9162 1.0503 0.102 Uiso 1 1 calc R . . C32 C 0.1779(9) 0.9973(7) 0.9573(6) 0.073(3) Uani 1 1 d . . . H32 H 0.1418 1.0571 0.9683 0.087 Uiso 1 1 calc R . . C33 C 0.2296(10) 0.9925(7) 0.8928(6) 0.080(3) Uani 1 1 d . . . H33 H 0.2324 1.0495 0.8599 0.096 Uiso 1 1 calc R . . C34 C 0.2781(10) 0.9035(7) 0.8758(5) 0.077(3) Uani 1 1 d . . . H34 H 0.3114 0.9009 0.8311 0.092 Uiso 1 1 calc R . . C35 C 0.4561(8) 0.7125(6) 0.8374(5) 0.052(2) Uani 1 1 d . . . C36 C 0.5568(9) 0.7587(7) 0.8448(5) 0.065(3) Uani 1 1 d . . . H36 H 0.5550 0.7896 0.8817 0.078 Uiso 1 1 calc R . . C37 C 0.6609(9) 0.7586(8) 0.7967(5) 0.073(3) Uani 1 1 d . . . H37 H 0.7288 0.7903 0.8010 0.088 Uiso 1 1 calc R . . C38 C 0.6644(10) 0.7124(8) 0.7430(5) 0.083(3) Uani 1 1 d . . . H38 H 0.7351 0.7123 0.7112 0.099 Uiso 1 1 calc R . . C39 C 0.5657(10) 0.6666(9) 0.7356(6) 0.088(3) Uani 1 1 d . . . H39 H 0.5684 0.6351 0.6989 0.106 Uiso 1 1 calc R . . C40 C 0.4607(9) 0.6669(8) 0.7830(5) 0.075(3) Uani 1 1 d . . . H40 H 0.3925 0.6359 0.7778 0.090 Uiso 1 1 calc R . . C41 C 0.1939(9) 0.6685(7) 0.8720(5) 0.062(3) Uani 1 1 d . . . C42 C 0.1422(10) 0.7195(8) 0.8096(5) 0.078(3) Uani 1 1 d . . . H42 H 0.1784 0.7717 0.7834 0.094 Uiso 1 1 calc R . . C43 C 0.0335(11) 0.6904(11) 0.7868(7) 0.099(4) Uani 1 1 d . . . H43 H -0.0004 0.7216 0.7448 0.118 Uiso 1 1 calc R . . C44 C -0.0190(12) 0.6168(11) 0.8274(9) 0.105(4) Uani 1 1 d . . . H44 H -0.0895 0.5974 0.8123 0.126 Uiso 1 1 calc R . . C45 C 0.0264(11) 0.5699(9) 0.8891(8) 0.099(4) Uani 1 1 d . . . H45 H -0.0142 0.5209 0.9164 0.119 Uiso 1 1 calc R . . C46 C 0.1339(9) 0.5956(7) 0.9111(6) 0.074(3) Uani 1 1 d . . . H46 H 0.1660 0.5627 0.9533 0.088 Uiso 1 1 calc R . . C47 C -0.0229(9) 0.2188(8) 0.4964(5) 0.069(3) Uani 1 1 d . . . C48 C -0.0642(11) 0.1355(9) 0.4938(6) 0.097(4) Uani 1 1 d . . . H48 H -0.0315 0.1022 0.4588 0.117 Uiso 1 1 calc R . . C49 C -0.1553(13) 0.0988(10) 0.5430(8) 0.117(5) Uani 1 1 d . . . H49 H -0.1847 0.0416 0.5408 0.140 Uiso 1 1 calc R . . C50 C -0.2011(12) 0.1481(13) 0.5946(8) 0.111(5) Uani 1 1 d . . . H50 H -0.2594 0.1225 0.6287 0.134 Uiso 1 1 calc R . . C51 C -0.1638(12) 0.2314(12) 0.5967(6) 0.106(4) Uani 1 1 d . . . H51 H -0.1992 0.2652 0.6310 0.128 Uiso 1 1 calc R . . C52 C -0.0724(11) 0.2691(9) 0.5483(6) 0.091(3) Uani 1 1 d . . . H52 H -0.0448 0.3269 0.5505 0.110 Uiso 1 1 calc R . . C53 C 0.2487(11) 0.2376(10) 0.4819(7) 0.092(4) Uani 1 1 d . . . C54 C 0.3517(15) 0.1694(11) 0.4704(9) 0.147(6) Uani 1 1 d . . . H54 H 0.3499 0.1304 0.4386 0.176 Uiso 1 1 calc R . . C55 C 0.461(3) 0.160(3) 0.5083(14) 0.222(19) Uani 1 1 d . . . H55 H 0.5336 0.1159 0.4985 0.267 Uiso 1 1 calc R . . C56 C 0.467(3) 0.207(3) 0.5549(14) 0.22(2) Uani 1 1 d . . . H56 H 0.5395 0.1924 0.5808 0.262 Uiso 1 1 calc R . . C57 C 0.3674(18) 0.2796(15) 0.5679(8) 0.154(8) Uani 1 1 d . . . H57 H 0.3740 0.3176 0.5997 0.185 Uiso 1 1 calc R . . C58 C 0.2554(13) 0.2934(12) 0.5309(8) 0.122(5) Uani 1 1 d . . . H58 H 0.1852 0.3402 0.5392 0.147 Uiso 1 1 calc R . . C59 C 0.0708(10) 0.3835(8) 0.4025(5) 0.070(3) Uani 1 1 d . . . C60 C 0.1710(12) 0.4348(9) 0.3760(6) 0.091(3) Uani 1 1 d . . . H60 H 0.2561 0.4038 0.3814 0.109 Uiso 1 1 calc R . . C61 C 0.1471(14) 0.5296(10) 0.3424(6) 0.105(4) Uani 1 1 d . . . H61 H 0.2156 0.5631 0.3259 0.126 Uiso 1 1 calc R . . C62 C 0.0236(17) 0.5752(10) 0.3328(6) 0.109(4) Uani 1 1 d . . . H62 H 0.0077 0.6384 0.3070 0.131 Uiso 1 1 calc R . . C63 C -0.0763(14) 0.5287(11) 0.3607(8) 0.121(5) Uani 1 1 d . . . H63 H -0.1609 0.5613 0.3565 0.146 Uiso 1 1 calc R . . C64 C -0.0523(12) 0.4315(9) 0.3959(7) 0.113(4) Uani 1 1 d . . . H64 H -0.1212 0.3997 0.4149 0.135 Uiso 1 1 calc R . . N1 N 0.3302(7) 0.3301(5) 0.8858(4) 0.0552(19) Uani 1 1 d . . . N2 N 0.3877(6) 0.3573(5) 0.8207(3) 0.0514(18) Uani 1 1 d . . . N3 N 0.5977(7) 0.0936(5) 0.7473(3) 0.0570(19) Uani 1 1 d . . . N4 N 0.6477(8) 0.1596(5) 0.7745(3) 0.0517(18) Uani 1 1 d . . . O1 O 0.4832(5) 0.1907(4) 0.8847(3) 0.0588(16) Uani 1 1 d . . . O2 O 0.5636(6) 0.3362(4) 0.7086(3) 0.0645(17) Uani 1 1 d . . . O3 O 0.4131(5) 0.2054(4) 0.7600(3) 0.0668(18) Uani 1 1 d . . . O4 O 0.6425(5) 0.3209(4) 0.8343(3) 0.0602(16) Uani 1 1 d . . . O5 O 0.3738(5) 0.6261(4) 0.9666(3) 0.0597(16) Uani 1 1 d . . . O8 O 0.1249(7) 0.1997(5) 0.3793(4) 0.098(2) Uani 1 1 d . . . O1W O 0.1506(12) 0.0679(8) 0.2871(5) 0.133(4) Uani 0.80 1 d P . . H1WA H 0.1424 0.1086 0.3151 0.199 Uiso 0.80 1 d PR . . H1WB H 0.2156 0.0265 0.2784 0.199 Uiso 0.80 1 d PR . . O2W O 0.3478(6) 0.4209(4) 1.0035(3) 0.0757(19) Uani 1 1 d . . . H2WA H 0.3428 0.3950 0.9692 0.114 Uiso 1 1 d R . . H2WB H 0.3418 0.3800 1.0412 0.114 Uiso 1 1 d R . . O3W O 0.5503(6) 0.4751(4) 0.8986(3) 0.079(2) Uani 1 1 d . . . H3WA H 0.5787 0.4273 0.8790 0.119 Uiso 1 1 d R . . H3WB H 0.5430 0.5286 0.8693 0.119 Uiso 1 1 d 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 0.0529(8) 0.0514(8) 0.0584(8) -0.0074(6) 0.0075(6) 0.0020(6) Co2 0.0418(10) 0.0434(10) 0.0670(12) -0.0108(8) -0.0010(8) 0.0055(8) P1 0.0431(14) 0.0499(14) 0.0601(16) -0.0083(12) 0.0029(11) 0.0046(11) P2 0.0652(18) 0.084(2) 0.074(2) -0.0103(16) 0.0106(14) -0.0178(15) C1 0.045(5) 0.058(6) 0.057(6) -0.020(5) 0.011(5) -0.020(5) C2 0.059(6) 0.050(6) 0.060(6) -0.016(5) 0.015(5) -0.016(5) C3 0.072(6) 0.042(5) 0.063(6) -0.016(5) 0.005(5) 0.000(5) C4 0.100(9) 0.068(7) 0.062(7) -0.005(6) 0.004(6) -0.013(6) C5 0.112(10) 0.085(9) 0.073(8) -0.017(7) 0.021(7) -0.024(8) C6 0.089(8) 0.076(8) 0.077(8) -0.022(6) 0.027(7) -0.019(7) C7 0.061(6) 0.060(6) 0.071(7) -0.016(5) 0.014(5) -0.012(5) C8 0.044(5) 0.051(6) 0.052(6) -0.006(5) -0.007(4) -0.004(4) C9 0.052(6) 0.054(6) 0.046(5) -0.014(5) 0.007(4) -0.008(5) C10 0.053(6) 0.062(7) 0.072(7) -0.005(5) -0.008(5) -0.006(5) C11 0.079(8) 0.076(7) 0.066(7) 0.005(6) -0.015(6) -0.013(6) C12 0.077(8) 0.085(8) 0.069(7) 0.003(6) -0.006(6) -0.022(6) C13 0.061(6) 0.079(7) 0.062(7) -0.008(6) 0.011(5) -0.010(6) C14 0.048(6) 0.065(7) 0.061(6) -0.012(5) 0.005(5) -0.011(5) C15 0.064(7) 0.059(6) 0.045(6) -0.001(5) 0.005(5) -0.019(6) C16 0.069(7) 0.063(7) 0.054(6) -0.009(5) 0.008(5) -0.016(6) C17 0.081(8) 0.076(7) 0.082(8) -0.023(6) 0.007(6) -0.015(7) C18 0.080(8) 0.110(10) 0.117(10) -0.047(9) -0.009(7) -0.022(8) C19 0.112(12) 0.133(13) 0.106(10) -0.035(9) -0.015(9) -0.058(10) C20 0.111(11) 0.097(10) 0.106(10) -0.030(8) -0.017(8) -0.014(8) C21 0.083(8) 0.069(7) 0.072(7) -0.014(6) -0.010(6) -0.012(6) C22 0.051(6) 0.053(6) 0.058(6) -0.001(5) 0.002(5) -0.002(5) C23 0.047(6) 0.046(6) 0.061(6) 0.002(5) -0.005(4) -0.007(5) C24 0.049(6) 0.060(6) 0.077(7) -0.008(5) -0.005(5) 0.002(5) C25 0.054(6) 0.063(7) 0.099(8) -0.007(6) -0.015(6) -0.003(6) C26 0.066(7) 0.062(7) 0.092(8) -0.009(6) -0.017(6) -0.011(6) C27 0.065(7) 0.052(6) 0.077(7) -0.016(5) -0.004(5) 0.000(5) C28 0.064(7) 0.042(6) 0.047(5) 0.004(4) 0.004(5) -0.005(5) C29 0.042(5) 0.063(6) 0.052(6) -0.010(5) -0.002(4) 0.006(4) C30 0.097(8) 0.046(6) 0.068(7) -0.006(5) 0.010(6) -0.004(5) C31 0.103(9) 0.067(8) 0.082(8) -0.020(7) 0.029(6) -0.017(6) C32 0.064(7) 0.054(7) 0.095(9) -0.023(6) 0.007(6) 0.010(5) C33 0.098(8) 0.048(7) 0.079(8) -0.003(5) -0.007(6) 0.019(6) C34 0.091(8) 0.060(7) 0.060(6) 0.001(6) 0.010(5) 0.015(6) C35 0.042(5) 0.047(5) 0.062(6) -0.010(5) -0.004(4) 0.008(4) C36 0.056(6) 0.073(7) 0.069(7) -0.023(5) 0.002(5) -0.012(5) C37 0.050(6) 0.093(8) 0.082(8) -0.025(6) 0.011(6) -0.028(5) C38 0.054(7) 0.120(10) 0.075(8) -0.035(7) 0.016(6) -0.007(6) C39 0.055(7) 0.135(10) 0.083(8) -0.044(7) 0.010(6) -0.017(7) C40 0.046(6) 0.097(8) 0.088(8) -0.030(7) 0.008(6) -0.017(5) C41 0.052(6) 0.058(6) 0.067(7) -0.015(5) 0.015(5) 0.006(5) C42 0.052(7) 0.100(8) 0.075(8) -0.019(7) 0.002(6) 0.005(6) C43 0.053(8) 0.131(12) 0.107(10) -0.041(9) -0.026(7) 0.032(7) C44 0.060(8) 0.093(10) 0.168(15) -0.050(10) -0.015(10) 0.003(8) C45 0.056(8) 0.079(8) 0.161(13) -0.022(9) -0.012(8) -0.008(6) C46 0.043(6) 0.063(7) 0.111(9) -0.023(6) 0.003(6) 0.005(5) C47 0.052(6) 0.081(8) 0.071(7) -0.008(6) 0.001(5) -0.013(6) C48 0.084(9) 0.102(10) 0.104(9) -0.025(8) 0.029(7) -0.022(7) C49 0.094(10) 0.102(10) 0.153(13) -0.016(10) 0.025(10) -0.040(8) C50 0.064(8) 0.141(14) 0.107(11) 0.015(10) 0.013(8) -0.015(9) C51 0.081(9) 0.144(13) 0.081(9) -0.015(9) 0.021(7) -0.004(9) C52 0.074(8) 0.117(10) 0.087(8) -0.033(8) 0.009(7) -0.019(7) C53 0.073(9) 0.096(10) 0.093(10) 0.014(7) 0.010(7) -0.026(8) C54 0.084(11) 0.129(13) 0.182(16) 0.036(11) 0.007(11) 0.016(10) C55 0.101(17) 0.28(4) 0.20(3) 0.11(3) -0.01(2) 0.025(19) C56 0.082(15) 0.31(4) 0.18(3) 0.15(3) -0.03(2) -0.03(2) C57 0.120(14) 0.23(2) 0.105(12) 0.054(13) -0.032(12) -0.096(14) C58 0.073(9) 0.176(15) 0.109(11) 0.015(11) -0.012(9) -0.044(9) C59 0.062(7) 0.090(8) 0.057(6) -0.010(5) 0.000(5) -0.014(6) C60 0.087(9) 0.079(8) 0.096(9) -0.006(7) 0.016(7) -0.009(7) C61 0.110(11) 0.107(11) 0.096(10) -0.012(8) 0.002(8) -0.029(9) C62 0.134(13) 0.094(10) 0.096(10) 0.009(7) -0.040(9) -0.023(10) C63 0.094(10) 0.106(11) 0.163(14) 0.002(10) -0.061(10) -0.018(9) C64 0.073(9) 0.092(10) 0.166(13) 0.005(9) -0.037(8) -0.018(7) N1 0.053(5) 0.044(5) 0.062(5) -0.010(4) 0.016(4) -0.005(4) N2 0.054(5) 0.053(5) 0.045(4) -0.009(4) 0.008(4) -0.008(4) N3 0.048(5) 0.063(5) 0.055(5) -0.008(4) 0.006(4) -0.002(4) N4 0.071(6) 0.043(4) 0.041(4) -0.010(3) 0.003(4) -0.011(4) O1 0.053(4) 0.052(4) 0.065(4) -0.011(3) 0.008(3) 0.003(3) O2 0.063(4) 0.056(4) 0.066(4) -0.007(3) 0.007(3) 0.003(3) O3 0.059(4) 0.060(4) 0.063(4) 0.001(3) 0.012(3) 0.014(3) O4 0.047(4) 0.058(4) 0.067(4) -0.011(3) 0.004(3) 0.007(3) O5 0.060(4) 0.048(4) 0.060(4) 0.000(3) -0.002(3) 0.006(3) O8 0.097(6) 0.110(6) 0.095(5) -0.044(5) 0.038(4) -0.033(5) O1W 0.182(12) 0.112(8) 0.112(8) -0.035(7) -0.009(8) -0.027(8) O2W 0.068(4) 0.059(4) 0.096(5) -0.012(4) -0.005(4) -0.001(3) O3W 0.089(5) 0.066(4) 0.075(4) -0.021(3) -0.009(4) 0.017(4) _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 O3 1.837(7) . ? Co1 O2 1.873(6) . ? Co1 N4 1.880(7) . ? Co1 O4 1.880(6) . ? Co1 N2 1.888(7) . ? Co1 O1 1.903(6) . ? Co2 O5 2.057(5) . ? Co2 O5 2.057(5) 2_667 ? Co2 O2W 2.102(6) 2_667 ? Co2 O2W 2.102(6) . ? Co2 O3W 2.126(6) . ? Co2 O3W 2.126(6) 2_667 ? P1 O5 1.492(6) . ? P1 C29 1.770(9) . ? P1 C41 1.795(10) . ? P1 C35 1.806(9) . ? P2 O8 1.471(7) . ? P2 C59 1.780(10) . ? P2 C53 1.795(13) . ? P2 C47 1.812(10) . ? C1 O1 1.308(9) . ? C1 N1 1.313(10) . ? C1 C2 1.476(11) . ? C2 C3 1.378(11) . ? C2 C7 1.416(12) . ? C3 C4 1.398(12) . ? C3 H3 0.9300 . ? C4 C5 1.371(14) . ? C4 H4 0.9300 . ? C5 C6 1.364(14) . ? C5 H5 0.9300 . ? C6 C7 1.378(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N2 1.280(9) . ? C8 C9 1.433(11) . ? C8 H8 0.9300 . ? C9 C10 1.413(11) . ? C9 C14 1.422(11) . ? C10 C11 1.351(12) . ? C10 H10 0.9300 . ? C11 C12 1.399(13) . ? C11 H11 0.9300 . ? C12 C13 1.367(13) . ? C12 H12 0.9300 . ? C13 C14 1.421(12) . ? C13 H13 0.9300 . ? C14 O2 1.295(10) . ? C15 N3 1.311(11) . ? C15 O3 1.329(10) . ? C15 C16 1.459(13) . ? C16 C21 1.386(13) . ? C16 C17 1.394(13) . ? C17 C18 1.364(14) . ? C17 H17 0.9300 . ? C18 C19 1.353(16) . ? C18 H18 0.9300 . ? C19 C20 1.383(16) . ? C19 H19 0.9300 . ? C20 C21 1.375(14) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 N4 1.283(10) . ? C22 C23 1.422(12) . ? C22 H22 0.9300 . ? C23 C28 1.397(12) . ? C23 C24 1.406(11) . ? C24 C25 1.363(12) . ? C24 H24 0.9300 . ? C25 C26 1.382(13) . ? C25 H25 0.9300 . ? C26 C27 1.376(12) . ? C26 H26 0.9300 . ? C27 C28 1.397(12) . ? C27 H27 0.9300 . ? C28 O4 1.357(10) . ? C29 C30 1.377(12) . ? C29 C34 1.380(12) . ? C30 C31 1.356(12) . ? C30 H30 0.9300 . ? C31 C32 1.367(13) . ? C31 H31 0.9300 . ? C32 C33 1.357(13) . ? C32 H32 0.9300 . ? C33 C34 1.377(12) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C40 1.369(12) . ? C35 C36 1.376(12) . ? C36 C37 1.386(12) . ? C36 H36 0.9300 . ? C37 C38 1.363(13) . ? C37 H37 0.9300 . ? C38 C39 1.353(14) . ? C38 H38 0.9300 . ? C39 C40 1.383(13) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C46 1.370(12) . ? C41 C42 1.402(12) . ? C42 C43 1.424(15) . ? C42 H42 0.9300 . ? C43 C44 1.347(16) . ? C43 H43 0.9300 . ? C44 C45 1.352(17) . ? C44 H44 0.9300 . ? C45 C46 1.382(14) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.344(14) . ? C47 C52 1.389(14) . ? C48 C49 1.391(16) . ? C48 H48 0.9300 . ? C49 C50 1.368(17) . ? C49 H49 0.9300 . ? C50 C51 1.323(17) . ? C50 H50 0.9300 . ? C51 C52 1.389(15) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.357(17) . ? C53 C58 1.394(17) . ? C54 C55 1.40(3) . ? C54 H54 0.9300 . ? C55 C56 1.27(5) . ? C55 H55 0.9300 . ? C56 C57 1.38(4) . ? C56 H56 0.9300 . ? C57 C58 1.410(18) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 C64 1.357(14) . ? C59 C60 1.387(14) . ? C60 C61 1.362(15) . ? C60 H60 0.9300 . ? C61 C62 1.356(16) . ? C61 H61 0.9300 . ? C62 C63 1.353(17) . ? C62 H62 0.9300 . ? C63 C64 1.401(16) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? N1 N2 1.385(9) . ? N3 N4 1.377(9) . ? O1W H1WA 0.8745 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8502 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8506 . ? 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 O3 Co1 O2 90.5(3) . . ? O3 Co1 N4 83.1(3) . . ? O2 Co1 N4 88.4(3) . . ? O3 Co1 O4 178.6(3) . . ? O2 Co1 O4 90.4(3) . . ? N4 Co1 O4 95.9(3) . . ? O3 Co1 N2 90.8(3) . . ? O2 Co1 N2 96.0(3) . . ? N4 Co1 N2 172.6(3) . . ? O4 Co1 N2 90.1(3) . . ? O3 Co1 O1 88.5(3) . . ? O2 Co1 O1 178.8(3) . . ? N4 Co1 O1 92.2(3) . . ? O4 Co1 O1 90.7(3) . . ? N2 Co1 O1 83.3(3) . . ? O5 Co2 O5 180.0 . 2_667 ? O5 Co2 O2W 91.3(2) . 2_667 ? O5 Co2 O2W 88.7(2) 2_667 2_667 ? O5 Co2 O2W 88.7(2) . . ? O5 Co2 O2W 91.3(2) 2_667 . ? O2W Co2 O2W 180.0 2_667 . ? O5 Co2 O3W 93.3(2) . . ? O5 Co2 O3W 86.7(2) 2_667 . ? O2W Co2 O3W 92.4(3) 2_667 . ? O2W Co2 O3W 87.6(3) . . ? O5 Co2 O3W 86.7(2) . 2_667 ? O5 Co2 O3W 93.3(2) 2_667 2_667 ? O2W Co2 O3W 87.6(3) 2_667 2_667 ? O2W Co2 O3W 92.4(3) . 2_667 ? O3W Co2 O3W 180.0 . 2_667 ? O5 P1 C29 112.7(4) . . ? O5 P1 C41 109.8(4) . . ? C29 P1 C41 106.7(4) . . ? O5 P1 C35 111.7(3) . . ? C29 P1 C35 107.2(4) . . ? C41 P1 C35 108.5(4) . . ? O8 P2 C59 112.1(5) . . ? O8 P2 C53 112.1(6) . . ? C59 P2 C53 105.4(6) . . ? O8 P2 C47 111.1(5) . . ? C59 P2 C47 109.0(5) . . ? C53 P2 C47 107.0(5) . . ? O1 C1 N1 124.9(7) . . ? O1 C1 C2 115.5(8) . . ? N1 C1 C2 119.6(8) . . ? C3 C2 C7 118.7(8) . . ? C3 C2 C1 121.5(8) . . ? C7 C2 C1 119.6(8) . . ? C2 C3 C4 120.3(9) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.5(10) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.5(10) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 121.8(10) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C2 119.2(9) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? N2 C8 C9 125.5(8) . . ? N2 C8 H8 117.2 . . ? C9 C8 H8 117.2 . . ? C10 C9 C14 119.3(8) . . ? C10 C9 C8 118.7(8) . . ? C14 C9 C8 121.8(8) . . ? C11 C10 C9 123.2(9) . . ? C11 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C10 C11 C12 118.4(9) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C13 C12 C11 120.1(10) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 123.4(9) . . ? C12 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? O2 C14 C13 118.4(8) . . ? O2 C14 C9 126.0(8) . . ? C13 C14 C9 115.6(8) . . ? N3 C15 O3 122.3(9) . . ? N3 C15 C16 119.2(9) . . ? O3 C15 C16 118.5(9) . . ? C21 C16 C17 118.1(10) . . ? C21 C16 C15 121.5(10) . . ? C17 C16 C15 120.5(10) . . ? C18 C17 C16 120.3(10) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 121.3(12) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 119.8(12) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 119.6(12) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C16 120.9(11) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? N4 C22 C23 125.8(8) . . ? N4 C22 H22 117.1 . . ? C23 C22 H22 117.1 . . ? C28 C23 C24 118.4(9) . . ? C28 C23 C22 124.5(8) . . ? C24 C23 C22 117.1(9) . . ? C25 C24 C23 122.5(9) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C24 C25 C26 119.0(9) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 119.8(10) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 122.1(9) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? O4 C28 C23 122.5(9) . . ? O4 C28 C27 119.3(8) . . ? C23 C28 C27 118.2(9) . . ? C30 C29 C34 118.0(8) . . ? C30 C29 P1 118.7(7) . . ? C34 C29 P1 123.2(7) . . ? C31 C30 C29 120.7(9) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 121.1(10) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C33 C32 C31 119.1(9) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.3(9) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 120.6(9) . . ? C33 C34 H34 119.7 . . ? C29 C34 H34 119.7 . . ? C40 C35 C36 119.5(8) . . ? C40 C35 P1 121.1(7) . . ? C36 C35 P1 119.0(7) . . ? C35 C36 C37 119.2(9) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 120.5(9) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 120.4(10) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 119.6(10) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C35 C40 C39 120.7(10) . . ? C35 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C46 C41 C42 118.9(10) . . ? C46 C41 P1 118.8(8) . . ? C42 C41 P1 122.1(8) . . ? C41 C42 C43 119.1(11) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 118.6(12) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? C43 C44 C45 122.7(13) . . ? C43 C44 H44 118.6 . . ? C45 C44 H44 118.6 . . ? C44 C45 C46 119.4(12) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 121.1(11) . . ? C41 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C48 C47 C52 119.8(10) . . ? C48 C47 P2 117.4(9) . . ? C52 C47 P2 122.6(9) . . ? C47 C48 C49 120.5(12) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 119.0(13) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C51 C50 C49 121.0(13) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C50 C51 C52 120.8(13) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C47 C52 C51 118.7(12) . . ? C47 C52 H52 120.6 . . ? C51 C52 H52 120.6 . . ? C54 C53 C58 119.1(15) . . ? C54 C53 P2 120.4(14) . . ? C58 C53 P2 120.6(11) . . ? C53 C54 C55 118(2) . . ? C53 C54 H54 121.2 . . ? C55 C54 H54 121.2 . . ? C56 C55 C54 124(4) . . ? C56 C55 H55 117.9 . . ? C54 C55 H55 117.9 . . ? C55 C56 C57 121(4) . . ? C55 C56 H56 119.4 . . ? C57 C56 H56 119.4 . . ? C56 C57 C58 117(2) . . ? C56 C57 H57 121.5 . . ? C58 C57 H57 121.5 . . ? C53 C58 C57 120.7(17) . . ? C53 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? C64 C59 C60 118.0(10) . . ? C64 C59 P2 122.1(9) . . ? C60 C59 P2 119.5(8) . . ? C61 C60 C59 121.3(11) . . ? C61 C60 H60 119.4 . . ? C59 C60 H60 119.4 . . ? C62 C61 C60 120.1(13) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C63 C62 C61 120.0(13) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.0(13) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C59 C64 C63 120.4(12) . . ? C59 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C1 N1 N2 108.7(6) . . ? C8 N2 N1 120.1(7) . . ? C8 N2 Co1 125.4(6) . . ? N1 N2 Co1 114.3(5) . . ? C15 N3 N4 108.6(7) . . ? C22 N4 N3 120.0(7) . . ? C22 N4 Co1 125.1(7) . . ? N3 N4 Co1 114.9(6) . . ? C1 O1 Co1 108.5(5) . . ? C14 O2 Co1 125.0(5) . . ? C15 O3 Co1 111.0(6) . . ? C28 O4 Co1 125.4(6) . . ? P1 O5 Co2 144.8(4) . . ? H1WA O1W H1WB 129.4 . . ? Co2 O2W H2WA 117.5 . . ? Co2 O2W H2WB 112.5 . . ? H2WA O2W H2WB 110.9 . . ? Co2 O3W H3WA 138.3 . . ? Co2 O3W H3WB 110.9 . . ? H3WA O3W H3WB 110.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 13.4(12) . . . . ? N1 C1 C2 C3 -164.1(8) . . . . ? O1 C1 C2 C7 -162.2(8) . . . . ? N1 C1 C2 C7 20.3(13) . . . . ? C7 C2 C3 C4 0.4(14) . . . . ? C1 C2 C3 C4 -175.3(8) . . . . ? C2 C3 C4 C5 0.0(15) . . . . ? C3 C4 C5 C6 -0.7(17) . . . . ? C4 C5 C6 C7 1.0(17) . . . . ? C5 C6 C7 C2 -0.6(16) . . . . ? C3 C2 C7 C6 -0.1(14) . . . . ? C1 C2 C7 C6 175.7(9) . . . . ? N2 C8 C9 C10 -176.8(8) . . . . ? N2 C8 C9 C14 -1.9(14) . . . . ? C14 C9 C10 C11 1.8(14) . . . . ? C8 C9 C10 C11 176.8(9) . . . . ? C9 C10 C11 C12 0.1(15) . . . . ? C10 C11 C12 C13 -0.9(15) . . . . ? C11 C12 C13 C14 -0.1(16) . . . . ? C12 C13 C14 O2 -178.2(9) . . . . ? C12 C13 C14 C9 1.9(14) . . . . ? C10 C9 C14 O2 177.5(8) . . . . ? C8 C9 C14 O2 2.6(14) . . . . ? C10 C9 C14 C13 -2.6(13) . . . . ? C8 C9 C14 C13 -177.5(8) . . . . ? N3 C15 C16 C21 4.9(13) . . . . ? O3 C15 C16 C21 -175.6(8) . . . . ? N3 C15 C16 C17 -173.4(8) . . . . ? O3 C15 C16 C17 6.1(12) . . . . ? C21 C16 C17 C18 0.5(15) . . . . ? C15 C16 C17 C18 178.8(9) . . . . ? C16 C17 C18 C19 0.6(18) . . . . ? C17 C18 C19 C20 -2(2) . . . . ? C18 C19 C20 C21 1.6(19) . . . . ? C19 C20 C21 C16 -0.6(17) . . . . ? C17 C16 C21 C20 -0.5(15) . . . . ? C15 C16 C21 C20 -178.8(9) . . . . ? N4 C22 C23 C28 3.6(14) . . . . ? N4 C22 C23 C24 -177.6(8) . . . . ? C28 C23 C24 C25 -2.3(13) . . . . ? C22 C23 C24 C25 178.8(8) . . . . ? C23 C24 C25 C26 1.7(15) . . . . ? C24 C25 C26 C27 -1.3(15) . . . . ? C25 C26 C27 C28 1.7(15) . . . . ? C24 C23 C28 O4 -177.9(7) . . . . ? C22 C23 C28 O4 0.9(13) . . . . ? C24 C23 C28 C27 2.5(12) . . . . ? C22 C23 C28 C27 -178.6(8) . . . . ? C26 C27 C28 O4 178.0(8) . . . . ? C26 C27 C28 C23 -2.4(13) . . . . ? O5 P1 C29 C30 -27.4(9) . . . . ? C41 P1 C29 C30 93.3(8) . . . . ? C35 P1 C29 C30 -150.7(8) . . . . ? O5 P1 C29 C34 155.3(8) . . . . ? C41 P1 C29 C34 -84.0(9) . . . . ? C35 P1 C29 C34 32.0(9) . . . . ? C34 C29 C30 C31 2.7(15) . . . . ? P1 C29 C30 C31 -174.7(8) . . . . ? C29 C30 C31 C32 -1.6(17) . . . . ? C30 C31 C32 C33 -1.2(17) . . . . ? C31 C32 C33 C34 2.7(17) . . . . ? C32 C33 C34 C29 -1.6(17) . . . . ? C30 C29 C34 C33 -1.2(15) . . . . ? P1 C29 C34 C33 176.2(8) . . . . ? O5 P1 C35 C40 98.8(8) . . . . ? C29 P1 C35 C40 -137.2(7) . . . . ? C41 P1 C35 C40 -22.4(8) . . . . ? O5 P1 C35 C36 -74.0(8) . . . . ? C29 P1 C35 C36 50.0(8) . . . . ? C41 P1 C35 C36 164.8(7) . . . . ? C40 C35 C36 C37 0.3(13) . . . . ? P1 C35 C36 C37 173.2(7) . . . . ? C35 C36 C37 C38 -0.8(15) . . . . ? C36 C37 C38 C39 0.6(17) . . . . ? C37 C38 C39 C40 0.1(17) . . . . ? C36 C35 C40 C39 0.3(15) . . . . ? P1 C35 C40 C39 -172.5(8) . . . . ? C38 C39 C40 C35 -0.5(17) . . . . ? O5 P1 C41 C46 12.1(8) . . . . ? C29 P1 C41 C46 -110.4(7) . . . . ? C35 P1 C41 C46 134.5(7) . . . . ? O5 P1 C41 C42 -172.2(7) . . . . ? C29 P1 C41 C42 65.4(8) . . . . ? C35 P1 C41 C42 -49.8(8) . . . . ? C46 C41 C42 C43 -3.6(13) . . . . ? P1 C41 C42 C43 -179.3(7) . . . . ? C41 C42 C43 C44 2.3(16) . . . . ? C42 C43 C44 C45 0.6(19) . . . . ? C43 C44 C45 C46 -2.3(19) . . . . ? C42 C41 C46 C45 1.9(14) . . . . ? P1 C41 C46 C45 177.8(8) . . . . ? C44 C45 C46 C41 1.0(16) . . . . ? O8 P2 C47 C48 14.1(10) . . . . ? C59 P2 C47 C48 138.0(9) . . . . ? C53 P2 C47 C48 -108.5(10) . . . . ? O8 P2 C47 C52 -170.8(9) . . . . ? C59 P2 C47 C52 -46.8(10) . . . . ? C53 P2 C47 C52 66.7(10) . . . . ? C52 C47 C48 C49 -0.5(18) . . . . ? P2 C47 C48 C49 174.7(10) . . . . ? C47 C48 C49 C50 -1(2) . . . . ? C48 C49 C50 C51 3(2) . . . . ? C49 C50 C51 C52 -3(2) . . . . ? C48 C47 C52 C51 0.2(17) . . . . ? P2 C47 C52 C51 -174.8(9) . . . . ? C50 C51 C52 C47 1.5(19) . . . . ? O8 P2 C53 C54 -8.0(12) . . . . ? C59 P2 C53 C54 -130.2(10) . . . . ? C47 P2 C53 C54 113.9(11) . . . . ? O8 P2 C53 C58 172.1(9) . . . . ? C59 P2 C53 C58 49.9(11) . . . . ? C47 P2 C53 C58 -66.0(11) . . . . ? C58 C53 C54 C55 -1(2) . . . . ? P2 C53 C54 C55 179.2(16) . . . . ? C53 C54 C55 C56 4(5) . . . . ? C54 C55 C56 C57 -6(6) . . . . ? C55 C56 C57 C58 5(5) . . . . ? C54 C53 C58 C57 0.2(19) . . . . ? P2 C53 C58 C57 -179.9(9) . . . . ? C56 C57 C58 C53 -2(2) . . . . ? O8 P2 C59 C64 92.1(10) . . . . ? C53 P2 C59 C64 -145.8(10) . . . . ? C47 P2 C59 C64 -31.3(11) . . . . ? O8 P2 C59 C60 -80.7(9) . . . . ? C53 P2 C59 C60 41.4(10) . . . . ? C47 P2 C59 C60 155.9(9) . . . . ? C64 C59 C60 C61 -2.2(17) . . . . ? P2 C59 C60 C61 170.9(9) . . . . ? C59 C60 C61 C62 -1.4(19) . . . . ? C60 C61 C62 C63 4(2) . . . . ? C61 C62 C63 C64 -4(2) . . . . ? C60 C59 C64 C63 2.7(19) . . . . ? P2 C59 C64 C63 -170.2(10) . . . . ? C62 C63 C64 C59 0(2) . . . . ? O1 C1 N1 N2 5.8(12) . . . . ? C2 C1 N1 N2 -177.0(7) . . . . ? C9 C8 N2 N1 -177.8(7) . . . . ? C9 C8 N2 Co1 -2.3(12) . . . . ? C1 N1 N2 C8 172.2(8) . . . . ? C1 N1 N2 Co1 -3.7(8) . . . . ? O3 Co1 N2 C8 -86.1(7) . . . . ? O2 Co1 N2 C8 4.5(7) . . . . ? N4 Co1 N2 C8 -121(2) . . . . ? O4 Co1 N2 C8 94.9(7) . . . . ? O1 Co1 N2 C8 -174.4(7) . . . . ? O3 Co1 N2 N1 89.6(6) . . . . ? O2 Co1 N2 N1 -179.8(5) . . . . ? N4 Co1 N2 N1 54(3) . . . . ? O4 Co1 N2 N1 -89.4(5) . . . . ? O1 Co1 N2 N1 1.2(5) . . . . ? O3 C15 N3 N4 0.2(10) . . . . ? C16 C15 N3 N4 179.7(7) . . . . ? C23 C22 N4 N3 177.8(7) . . . . ? C23 C22 N4 Co1 0.5(12) . . . . ? C15 N3 N4 C22 -175.7(7) . . . . ? C15 N3 N4 Co1 1.8(8) . . . . ? O3 Co1 N4 C22 175.0(7) . . . . ? O2 Co1 N4 C22 84.3(7) . . . . ? O4 Co1 N4 C22 -5.9(7) . . . . ? N2 Co1 N4 C22 -149(2) . . . . ? O1 Co1 N4 C22 -96.8(7) . . . . ? O3 Co1 N4 N3 -2.4(5) . . . . ? O2 Co1 N4 N3 -93.1(5) . . . . ? O4 Co1 N4 N3 176.7(5) . . . . ? N2 Co1 N4 N3 33(3) . . . . ? O1 Co1 N4 N3 85.8(5) . . . . ? N1 C1 O1 Co1 -4.8(10) . . . . ? C2 C1 O1 Co1 177.9(6) . . . . ? O3 Co1 O1 C1 -89.4(5) . . . . ? O2 Co1 O1 C1 -56(12) . . . . ? N4 Co1 O1 C1 -172.5(6) . . . . ? O4 Co1 O1 C1 91.6(5) . . . . ? N2 Co1 O1 C1 1.6(5) . . . . ? C13 C14 O2 Co1 -178.8(6) . . . . ? C9 C14 O2 Co1 1.1(13) . . . . ? O3 Co1 O2 C14 87.0(7) . . . . ? N4 Co1 O2 C14 170.1(7) . . . . ? O4 Co1 O2 C14 -94.0(7) . . . . ? N2 Co1 O2 C14 -3.9(7) . . . . ? O1 Co1 O2 C14 54(12) . . . . ? N3 C15 O3 Co1 -2.1(10) . . . . ? C16 C15 O3 Co1 178.4(6) . . . . ? O2 Co1 O3 C15 90.6(5) . . . . ? N4 Co1 O3 C15 2.3(5) . . . . ? O4 Co1 O3 C15 -40(11) . . . . ? N2 Co1 O3 C15 -173.4(5) . . . . ? O1 Co1 O3 C15 -90.1(5) . . . . ? C23 C28 O4 Co1 -8.9(11) . . . . ? C27 C28 O4 Co1 170.7(6) . . . . ? O3 Co1 O4 C28 53(11) . . . . ? O2 Co1 O4 C28 -78.4(6) . . . . ? N4 Co1 O4 C28 10.0(6) . . . . ? N2 Co1 O4 C28 -174.4(6) . . . . ? O1 Co1 O4 C28 102.3(6) . . . . ? C29 P1 O5 Co2 -147.8(6) . . . . ? C41 P1 O5 Co2 93.4(7) . . . . ? C35 P1 O5 Co2 -27.1(8) . . . . ? O5 Co2 O5 P1 -6(18) 2_667 . . . ? O2W Co2 O5 P1 80.0(7) 2_667 . . . ? O2W Co2 O5 P1 -100.0(7) . . . . ? O3W Co2 O5 P1 -12.5(7) . . . . ? O3W Co2 O5 P1 167.5(7) 2_667 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 21.66 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.775 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.074