# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'A. Carty' 'Todd Graham' 'Konstantin A. Udachin' _publ_contact_author_name 'Prof Arthur J. Carty' _publ_contact_author_address ; Steacie Institute for Molecular Sciences National Research Council of Canada 100 Sussex Drive Ottawa ON K1A 0R6 CANADA ; _publ_contact_author_email ACARTY@PCO-BCP.GC.CA _publ_requested_journal 'Chemical Communications' _publ_section_title ; Reactivity of Electrophilic m2-Phosphinidene Complexes with Heterocumulenes: Formation of the First s-p-Aminophosphaimine Complexes [Mn2(CO)8{m-h1,h2-P(NiPr2)=NR}] and Diazoalkane Insertions into Metal-Phosphorus Bonds. ; data_tg21 _database_code_depnum_ccdc_archive 'CCDC 269679' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 Mn2 N3 O8.50 P' _chemical_formula_weight 696.40 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)/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 12.1027(16) _cell_length_b 20.563(3) _cell_length_c 13.6644(18) _cell_angle_alpha 90.00 _cell_angle_beta 111.888(2) _cell_angle_gamma 90.00 _cell_volume 3155.5(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 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.7730 _exptl_absorpt_correction_T_max 0.9562 _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 33326 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.38 _reflns_number_total 7871 _reflns_number_gt 6622 _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^)+(0.0473P)^2^+1.3950P] 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 7871 _refine_ls_number_parameters 416 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.48412(2) 0.349294(12) 0.329151(18) 0.01796(7) Uani 1 1 d . . . Mn2 Mn 0.29841(2) 0.309961(11) 0.133406(18) 0.01721(7) Uani 1 1 d . . . P1 P 0.41163(3) 0.437421(19) 0.23872(3) 0.01597(9) Uani 1 1 d . . . O1 O 0.65823(14) 0.33501(8) 0.22246(13) 0.0439(4) Uani 1 1 d . . . O2 O 0.52462(14) 0.21179(7) 0.40162(12) 0.0392(3) Uani 1 1 d . . . O3 O 0.65328(13) 0.40647(7) 0.52602(10) 0.0368(3) Uani 1 1 d . . . O4 O 0.28091(12) 0.35448(6) 0.40271(10) 0.0282(3) Uani 1 1 d . . . O5 O 0.22791(13) 0.21476(7) 0.26600(11) 0.0346(3) Uani 1 1 d . . . O6 O 0.40023(12) 0.38373(6) -0.00263(10) 0.0302(3) Uani 1 1 d . . . O7 O 0.11817(12) 0.25600(7) -0.06080(11) 0.0369(3) Uani 1 1 d . . . O8 O 0.47086(12) 0.21067(6) 0.12460(11) 0.0337(3) Uani 1 1 d . . . N1 N 0.48339(12) 0.50330(6) 0.23179(10) 0.0189(3) Uani 1 1 d . . . N2 N 0.27433(12) 0.45089(6) 0.17219(10) 0.0180(3) Uani 1 1 d . . . N3 N 0.20764(12) 0.39247(6) 0.15552(10) 0.0165(3) Uani 1 1 d . . . C1 C 0.59175(17) 0.34057(9) 0.26278(14) 0.0272(4) Uani 1 1 d . . . C2 C 0.50837(16) 0.26433(9) 0.37221(14) 0.0262(4) Uani 1 1 d . . . C3 C 0.58817(15) 0.38414(9) 0.44930(13) 0.0245(3) Uani 1 1 d . . . C4 C 0.35711(15) 0.35232(8) 0.37272(12) 0.0211(3) Uani 1 1 d . . . C5 C 0.25180(15) 0.25404(8) 0.21837(13) 0.0236(3) Uani 1 1 d . . . C6 C 0.36113(15) 0.35910(8) 0.05182(13) 0.0210(3) Uani 1 1 d . . . C7 C 0.18473(15) 0.27810(9) 0.01495(13) 0.0241(3) Uani 1 1 d . . . C8 C 0.40396(16) 0.24846(8) 0.13002(13) 0.0237(3) Uani 1 1 d . . . C9 C 0.09950(14) 0.40087(8) 0.15153(11) 0.0174(3) Uani 1 1 d . . . C10 C 0.05503(14) 0.46474(8) 0.17355(12) 0.0188(3) Uani 1 1 d . . . C11 C 0.11379(16) 0.49924(9) 0.26700(13) 0.0255(3) Uani 1 1 d . . . H11 H 0.1841 0.4819 0.3187 0.031 Uiso 1 1 calc R . . C12 C 0.06982(17) 0.55843(9) 0.28426(15) 0.0296(4) Uani 1 1 d . . . H12 H 0.1101 0.5814 0.3480 0.035 Uiso 1 1 calc R . . C13 C -0.03239(17) 0.58455(9) 0.20948(15) 0.0282(4) Uani 1 1 d . . . H13 H -0.0615 0.6255 0.2212 0.034 Uiso 1 1 calc R . . C14 C -0.09155(16) 0.55044(9) 0.11763(14) 0.0280(4) Uani 1 1 d . . . H14 H -0.1616 0.5682 0.0661 0.034 Uiso 1 1 calc R . . C15 C -0.04959(15) 0.49048(9) 0.09998(13) 0.0233(3) Uani 1 1 d . . . H15 H -0.0923 0.4669 0.0375 0.028 Uiso 1 1 calc R . . C16 C 0.01335(14) 0.34564(8) 0.12587(13) 0.0197(3) Uani 1 1 d . . . C17 C -0.00500(16) 0.31298(9) 0.20786(14) 0.0275(4) Uani 1 1 d . . . H17 H 0.0401 0.3245 0.2789 0.033 Uiso 1 1 calc R . . C18 C -0.08887(18) 0.26366(10) 0.18610(17) 0.0348(4) Uani 1 1 d . . . H18 H -0.1000 0.2410 0.2423 0.042 Uiso 1 1 calc R . . C19 C -0.15644(17) 0.24741(10) 0.08268(17) 0.0364(5) Uani 1 1 d . . . H19 H -0.2141 0.2137 0.0680 0.044 Uiso 1 1 calc R . . C20 C -0.14003(17) 0.28020(9) 0.00082(16) 0.0327(4) Uani 1 1 d . . . H20 H -0.1867 0.2690 -0.0701 0.039 Uiso 1 1 calc R . . C21 C -0.05543(16) 0.32956(9) 0.02167(14) 0.0256(4) Uani 1 1 d . . . H21 H -0.0447 0.3521 -0.0348 0.031 Uiso 1 1 calc R . . C22 C 0.61388(14) 0.50661(8) 0.29676(12) 0.0209(3) Uani 1 1 d . . . H22 H 0.6382 0.4627 0.3289 0.025 Uiso 1 1 calc R . . C23 C 0.68632(17) 0.52022(11) 0.22921(16) 0.0349(4) Uani 1 1 d . . . H23C H 0.6666 0.5636 0.1977 0.042 Uiso 1 1 calc R . . H23B H 0.6678 0.4875 0.1732 0.042 Uiso 1 1 calc R . . H23A H 0.7714 0.5183 0.2731 0.042 Uiso 1 1 calc R . . C24 C 0.63891(18) 0.55450(10) 0.38712(16) 0.0365(5) Uani 1 1 d . . . H24C H 0.5808 0.5482 0.4206 0.044 Uiso 1 1 calc R . . H24B H 0.6327 0.5990 0.3599 0.044 Uiso 1 1 calc R . . H24A H 0.7194 0.5472 0.4391 0.044 Uiso 1 1 calc R . . C25 C 0.42878(15) 0.56382(8) 0.17132(13) 0.0220(3) Uani 1 1 d . . . H25 H 0.4953 0.5956 0.1841 0.026 Uiso 1 1 calc R . . C26 C 0.34034(17) 0.59580(9) 0.21163(14) 0.0276(4) Uani 1 1 d . . . H26C H 0.3748 0.5979 0.2888 0.033 Uiso 1 1 calc R . . H26B H 0.2668 0.5702 0.1892 0.033 Uiso 1 1 calc R . . H26A H 0.3225 0.6399 0.1828 0.033 Uiso 1 1 calc R . . C27 C 0.37664(16) 0.55145(9) 0.05309(13) 0.0255(4) Uani 1 1 d . . . H27C H 0.3062 0.5236 0.0358 0.031 Uiso 1 1 calc R . . H27B H 0.4362 0.5298 0.0316 0.031 Uiso 1 1 calc R . . H27A H 0.3539 0.5929 0.0157 0.031 Uiso 1 1 calc R . . O1A O -0.0474(2) 0.50218(15) 0.4693(2) 0.0319(6) Uani 0.50 1 d PD A -11 C1A C 0.0367(6) 0.5475(4) 0.5332(6) 0.0391(17) Uani 0.50 1 d PD A -11 H1A2 H 0.1092 0.5470 0.5159 0.047 Uiso 0.50 1 calc PR A -11 H1A1 H 0.0597 0.5360 0.6086 0.047 Uiso 0.50 1 calc PR A -11 C2A C -0.0195(4) 0.6146(2) 0.5128(4) 0.0449(11) Uani 0.50 1 d PD A -11 H2A3 H -0.0865 0.6159 0.5366 0.054 Uiso 0.50 1 calc PR A -11 H2A2 H -0.0482 0.6241 0.4371 0.054 Uiso 0.50 1 calc PR A -11 H2A1 H 0.0399 0.6471 0.5514 0.054 Uiso 0.50 1 calc PR A -11 C3A C 0.0021(5) 0.4388(4) 0.4747(6) 0.0330(15) Uani 0.50 1 d PD A -11 H3A2 H 0.0362 0.4240 0.5489 0.040 Uiso 0.50 1 calc PR A -11 H3A1 H 0.0667 0.4397 0.4467 0.040 Uiso 0.50 1 calc PR A -11 C4A C -0.0944(4) 0.3926(2) 0.4105(4) 0.0409(10) Uani 0.50 1 d PD A -11 H4A3 H -0.1229 0.4053 0.3360 0.049 Uiso 0.50 1 calc PR A -11 H4A2 H -0.1607 0.3943 0.4352 0.049 Uiso 0.50 1 calc PR A -11 H4A1 H -0.0626 0.3483 0.4185 0.049 Uiso 0.50 1 calc PR A -11 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 0.01637(13) 0.01528(13) 0.02061(12) 0.00219(8) 0.00501(9) 0.00139(9) Mn2 0.01712(13) 0.01403(12) 0.02005(12) -0.00059(8) 0.00644(9) -0.00007(9) P1 0.01473(19) 0.01388(19) 0.01792(17) 0.00000(13) 0.00448(14) -0.00079(14) O1 0.0354(8) 0.0459(9) 0.0603(10) -0.0068(7) 0.0292(8) 0.0008(7) O2 0.0442(9) 0.0218(7) 0.0510(8) 0.0113(6) 0.0170(7) 0.0075(6) O3 0.0316(7) 0.0454(8) 0.0241(6) -0.0002(6) -0.0001(5) -0.0059(6) O4 0.0266(7) 0.0326(7) 0.0275(6) -0.0016(5) 0.0125(5) -0.0027(5) O5 0.0387(8) 0.0259(7) 0.0441(8) 0.0069(6) 0.0212(6) -0.0031(6) O6 0.0351(7) 0.0281(7) 0.0333(7) 0.0038(5) 0.0197(6) 0.0013(6) O7 0.0292(7) 0.0429(8) 0.0340(7) -0.0176(6) 0.0065(6) -0.0037(6) O8 0.0323(7) 0.0226(7) 0.0464(8) -0.0027(6) 0.0147(6) 0.0082(6) N1 0.0155(6) 0.0160(6) 0.0212(6) 0.0014(5) 0.0024(5) -0.0013(5) N2 0.0153(6) 0.0146(6) 0.0223(6) -0.0002(5) 0.0050(5) -0.0019(5) N3 0.0161(6) 0.0149(6) 0.0165(6) 0.0002(5) 0.0038(5) -0.0010(5) C1 0.0252(9) 0.0208(9) 0.0346(9) -0.0004(7) 0.0100(7) 0.0027(7) C2 0.0254(9) 0.0217(9) 0.0305(8) 0.0030(7) 0.0094(7) 0.0029(7) C3 0.0218(8) 0.0247(9) 0.0248(8) 0.0056(6) 0.0062(6) 0.0016(7) C4 0.0232(8) 0.0165(8) 0.0198(7) 0.0018(6) 0.0037(6) -0.0010(6) C5 0.0240(8) 0.0200(8) 0.0270(8) -0.0017(6) 0.0098(7) 0.0005(7) C6 0.0205(8) 0.0173(8) 0.0239(7) -0.0021(6) 0.0068(6) 0.0021(6) C7 0.0215(8) 0.0228(8) 0.0290(8) -0.0028(7) 0.0105(7) 0.0016(7) C8 0.0252(9) 0.0180(8) 0.0259(8) -0.0011(6) 0.0072(7) -0.0007(7) C9 0.0152(7) 0.0182(8) 0.0166(6) 0.0015(5) 0.0033(5) 0.0002(6) C10 0.0157(7) 0.0180(8) 0.0239(7) 0.0001(6) 0.0088(6) -0.0004(6) C11 0.0194(8) 0.0279(9) 0.0268(8) -0.0030(7) 0.0060(6) 0.0032(7) C12 0.0255(9) 0.0301(10) 0.0337(9) -0.0116(7) 0.0117(7) -0.0017(7) C13 0.0273(9) 0.0209(9) 0.0422(10) -0.0007(7) 0.0198(8) 0.0032(7) C14 0.0232(9) 0.0265(9) 0.0334(9) 0.0059(7) 0.0093(7) 0.0076(7) C15 0.0184(8) 0.0247(9) 0.0249(8) -0.0001(6) 0.0059(6) 0.0013(6) C16 0.0145(7) 0.0175(8) 0.0253(8) -0.0004(6) 0.0052(6) 0.0013(6) C17 0.0248(9) 0.0278(9) 0.0288(8) 0.0034(7) 0.0087(7) -0.0031(7) C18 0.0292(10) 0.0297(10) 0.0463(11) 0.0075(8) 0.0149(8) -0.0058(8) C19 0.0235(9) 0.0247(10) 0.0560(12) -0.0009(8) 0.0091(9) -0.0082(8) C20 0.0243(9) 0.0265(9) 0.0382(10) -0.0070(8) 0.0011(7) -0.0045(8) C21 0.0225(9) 0.0228(9) 0.0279(8) -0.0019(7) 0.0051(7) -0.0015(7) C22 0.0158(7) 0.0189(8) 0.0240(7) 0.0002(6) 0.0027(6) -0.0024(6) C23 0.0194(9) 0.0481(12) 0.0357(10) 0.0109(9) 0.0087(7) -0.0034(8) C24 0.0283(10) 0.0321(10) 0.0377(10) -0.0133(8) -0.0010(8) -0.0019(8) C25 0.0205(8) 0.0150(7) 0.0266(8) 0.0035(6) 0.0042(6) -0.0024(6) C26 0.0305(9) 0.0169(8) 0.0327(9) -0.0002(7) 0.0088(7) 0.0028(7) C27 0.0246(9) 0.0243(9) 0.0253(8) 0.0056(6) 0.0069(7) -0.0010(7) O1A 0.0257(13) 0.0299(16) 0.0359(14) -0.0014(11) 0.0067(10) 0.0030(12) C1A 0.026(4) 0.052(5) 0.037(3) 0.003(3) 0.009(3) -0.006(3) C2A 0.042(3) 0.041(3) 0.056(3) -0.010(2) 0.023(2) -0.009(2) C3A 0.024(3) 0.041(4) 0.033(2) 0.007(2) 0.009(3) 0.008(3) C4A 0.038(2) 0.037(2) 0.049(2) -0.0018(18) 0.0174(19) 0.0035(18) _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 C3 1.8037(18) . ? Mn1 C2 1.8320(18) . ? Mn1 C4 1.8449(18) . ? Mn1 C1 1.8525(19) . ? Mn1 P1 2.1845(5) . ? Mn1 Mn2 2.8945(4) . ? Mn2 C8 1.8103(18) . ? Mn2 C7 1.8116(17) . ? Mn2 C6 1.8631(17) . ? Mn2 C5 1.8646(18) . ? Mn2 N3 2.1034(13) . ? P1 N2 1.5931(14) . ? P1 N1 1.6309(14) . ? O1 C1 1.138(2) . ? O2 C2 1.144(2) . ? O3 C3 1.147(2) . ? O4 C4 1.141(2) . ? O5 C5 1.140(2) . ? O6 C6 1.139(2) . ? O7 C7 1.142(2) . ? O8 C8 1.144(2) . ? N1 C22 1.497(2) . ? N1 C25 1.504(2) . ? N2 N3 1.4176(18) . ? N3 C9 1.301(2) . ? C9 C10 1.492(2) . ? C9 C16 1.492(2) . ? C10 C15 1.395(2) . ? C10 C11 1.401(2) . ? C11 C12 1.383(3) . ? C12 C13 1.386(3) . ? C13 C14 1.382(3) . ? C14 C15 1.388(2) . ? C16 C17 1.393(2) . ? C16 C21 1.395(2) . ? C17 C18 1.387(3) . ? C18 C19 1.384(3) . ? C19 C20 1.382(3) . ? C20 C21 1.394(3) . ? C22 C23 1.517(2) . ? C22 C24 1.519(2) . ? C25 C27 1.521(2) . ? C25 C26 1.523(3) . ? O1A C1A 1.416(8) . ? O1A C3A 1.425(7) . ? C1A C2A 1.517(8) . ? C3A C4A 1.507(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mn1 C2 96.47(8) . . ? C3 Mn1 C4 94.35(8) . . ? C2 Mn1 C4 88.94(8) . . ? C3 Mn1 C1 95.99(8) . . ? C2 Mn1 C1 90.41(8) . . ? C4 Mn1 C1 169.65(8) . . ? C3 Mn1 P1 100.50(6) . . ? C2 Mn1 P1 162.80(6) . . ? C4 Mn1 P1 86.98(5) . . ? C1 Mn1 P1 90.62(6) . . ? C3 Mn1 Mn2 172.01(6) . . ? C2 Mn1 Mn2 90.37(6) . . ? C4 Mn1 Mn2 81.62(5) . . ? C1 Mn1 Mn2 88.06(6) . . ? P1 Mn1 Mn2 72.502(15) . . ? C8 Mn2 C7 91.87(8) . . ? C8 Mn2 C6 85.11(8) . . ? C7 Mn2 C6 90.27(8) . . ? C8 Mn2 C5 88.01(8) . . ? C7 Mn2 C5 91.60(8) . . ? C6 Mn2 C5 172.93(7) . . ? C8 Mn2 N3 168.08(7) . . ? C7 Mn2 N3 99.01(6) . . ? C6 Mn2 N3 89.98(6) . . ? C5 Mn2 N3 96.46(6) . . ? C8 Mn2 Mn1 84.64(5) . . ? C7 Mn2 Mn1 175.00(6) . . ? C6 Mn2 Mn1 92.99(5) . . ? C5 Mn2 Mn1 84.72(5) . . ? N3 Mn2 Mn1 84.78(4) . . ? N2 P1 N1 106.69(7) . . ? N2 P1 Mn1 125.49(5) . . ? N1 P1 Mn1 127.71(5) . . ? C22 N1 C25 116.02(12) . . ? C22 N1 P1 118.04(10) . . ? C25 N1 P1 125.79(11) . . ? N3 N2 P1 110.77(10) . . ? C9 N3 N2 113.45(13) . . ? C9 N3 Mn2 132.24(11) . . ? N2 N3 Mn2 114.21(9) . . ? O1 C1 Mn1 179.6(2) . . ? O2 C2 Mn1 178.31(17) . . ? O3 C3 Mn1 179.23(18) . . ? O4 C4 Mn1 177.93(14) . . ? O5 C5 Mn2 172.89(16) . . ? O6 C6 Mn2 173.48(15) . . ? O7 C7 Mn2 175.98(16) . . ? O8 C8 Mn2 177.45(16) . . ? N3 C9 C10 122.77(14) . . ? N3 C9 C16 120.84(14) . . ? C10 C9 C16 116.38(13) . . ? C15 C10 C11 118.74(15) . . ? C15 C10 C9 119.18(14) . . ? C11 C10 C9 122.06(14) . . ? C12 C11 C10 120.27(16) . . ? C11 C12 C13 120.65(17) . . ? C14 C13 C12 119.39(17) . . ? C13 C14 C15 120.62(16) . . ? C14 C15 C10 120.29(16) . . ? C17 C16 C21 119.55(16) . . ? C17 C16 C9 118.99(15) . . ? C21 C16 C9 121.26(15) . . ? C18 C17 C16 120.23(17) . . ? C19 C18 C17 120.14(18) . . ? C20 C19 C18 120.00(18) . . ? C19 C20 C21 120.40(17) . . ? C20 C21 C16 119.65(17) . . ? N1 C22 C23 111.63(13) . . ? N1 C22 C24 110.98(14) . . ? C23 C22 C24 112.93(16) . . ? N1 C25 C27 111.63(13) . . ? N1 C25 C26 112.50(14) . . ? C27 C25 C26 112.77(14) . . ? C1A O1A C3A 112.2(4) . . ? O1A C1A C2A 108.3(5) . . ? O1A C3A C4A 109.0(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.569 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.073 data_tg29 _database_code_depnum_ccdc_archive 'CCDC 269680' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H42 Co2 N O4 P3' _chemical_formula_weight 799.51 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.170(6) _cell_length_b 10.6655(19) _cell_length_c 23.493(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.347(3) _cell_angle_gamma 90.00 _cell_volume 7385(2) _cell_formula_units_Z 8 _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 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.6168 _exptl_absorpt_correction_T_max 0.9485 _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 45123 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 29.57 _reflns_number_total 10308 _reflns_number_gt 7709 _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^)+(0.0443P)^2^+5.9264P] 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 10308 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.109009(9) 0.28979(2) 0.290132(11) 0.01930(7) Uani 1 1 d . . . Co2 Co 0.152107(8) 0.42996(2) 0.381818(10) 0.01760(6) Uani 1 1 d . . . P1 P 0.124814(16) 0.44036(5) 0.23274(2) 0.01809(10) Uani 1 1 d . . . P2 P 0.202337(16) 0.51068(5) 0.33718(2) 0.01714(10) Uani 1 1 d . . . P3 P 0.093242(17) 0.31652(5) 0.37354(2) 0.02010(10) Uani 1 1 d . . . O1 O 0.19735(5) 0.16889(15) 0.30423(7) 0.0361(4) Uani 1 1 d . . . O2 O 0.04980(6) 0.10350(16) 0.22196(8) 0.0454(4) Uani 1 1 d . . . O3 O 0.20487(6) 0.34855(18) 0.49401(7) 0.0407(4) Uani 1 1 d . . . O4 O 0.10308(5) 0.65895(15) 0.39366(7) 0.0327(3) Uani 1 1 d . . . N1 N 0.07507(6) 0.22425(17) 0.42121(7) 0.0274(4) Uani 1 1 d . . . C2A C 0.05230(7) 0.3701(2) 0.31501(9) 0.0231(4) Uani 1 1 d . . . H2A H 0.0502(7) 0.453(2) 0.3064(9) 0.023(6) Uiso 1 1 d . . . H2 H 0.0232(8) 0.325(2) 0.3038(10) 0.028(6) Uiso 1 1 d . . . C1 C 0.16291(7) 0.21815(19) 0.30052(8) 0.0257(4) Uani 1 1 d . . . C2 C 0.07361(8) 0.17548(19) 0.24813(9) 0.0283(4) Uani 1 1 d . . . C3 C 0.18518(7) 0.3743(2) 0.44804(9) 0.0259(4) Uani 1 1 d . . . C4 C 0.12198(7) 0.56931(19) 0.38575(8) 0.0223(4) Uani 1 1 d . . . C5 C 0.18308(6) 0.50226(19) 0.25692(8) 0.0200(4) Uani 1 1 d . . . H5B H 0.1844 0.5873 0.2405 0.024 Uiso 1 1 calc R . . H5A H 0.2042 0.4481 0.2411 0.024 Uiso 1 1 calc R . . C6 C 0.08953(6) 0.58026(18) 0.22054(8) 0.0204(4) Uani 1 1 d . . . C7 C 0.04769(7) 0.5748(2) 0.18134(10) 0.0308(5) Uani 1 1 d . . . H7 H 0.0382 0.4985 0.1615 0.037 Uiso 1 1 calc R . . C8 C 0.01995(8) 0.6790(2) 0.17100(11) 0.0364(5) Uani 1 1 d . . . H8 H -0.0081 0.6747 0.1435 0.044 Uiso 1 1 calc R . . C9 C 0.03300(7) 0.7899(2) 0.20069(10) 0.0316(5) Uani 1 1 d . . . H9 H 0.0140 0.8618 0.1934 0.038 Uiso 1 1 calc R . . C10 C 0.07374(7) 0.7955(2) 0.24090(9) 0.0277(4) Uani 1 1 d . . . H10 H 0.0824 0.8708 0.2619 0.033 Uiso 1 1 calc R . . C11 C 0.10204(7) 0.69152(18) 0.25066(8) 0.0234(4) Uani 1 1 d . . . H11 H 0.1301 0.6963 0.2781 0.028 Uiso 1 1 calc R . . C12 C 0.12882(6) 0.39326(19) 0.15870(8) 0.0218(4) Uani 1 1 d . . . C13 C 0.12931(8) 0.4796(2) 0.11448(9) 0.0307(5) Uani 1 1 d . . . H13 H 0.1243 0.5659 0.1208 0.037 Uiso 1 1 calc R . . C14 C 0.13711(8) 0.4405(2) 0.06114(9) 0.0363(5) Uani 1 1 d . . . H14 H 0.1377 0.5005 0.0314 0.044 Uiso 1 1 calc R . . C15 C 0.14400(8) 0.3160(2) 0.05084(9) 0.0361(5) Uani 1 1 d . . . H15 H 0.1488 0.2900 0.0140 0.043 Uiso 1 1 calc R . . C16 C 0.14386(8) 0.2291(2) 0.09413(9) 0.0353(5) Uani 1 1 d . . . H16 H 0.1490 0.1430 0.0874 0.042 Uiso 1 1 calc R . . C17 C 0.13620(7) 0.2676(2) 0.14777(9) 0.0286(4) Uani 1 1 d . . . H17 H 0.1360 0.2072 0.1774 0.034 Uiso 1 1 calc R . . C18 C 0.25945(6) 0.44272(18) 0.34593(8) 0.0188(4) Uani 1 1 d . . . C19 C 0.29002(7) 0.49185(19) 0.31507(9) 0.0243(4) Uani 1 1 d . . . H19 H 0.2819 0.5638 0.2913 0.029 Uiso 1 1 calc R . . C20 C 0.33220(7) 0.43712(19) 0.31858(9) 0.0269(4) Uani 1 1 d . . . H20 H 0.3526 0.4706 0.2968 0.032 Uiso 1 1 calc R . . C21 C 0.34453(7) 0.3337(2) 0.35388(9) 0.0270(4) Uani 1 1 d . . . H21 H 0.3734 0.2959 0.3564 0.032 Uiso 1 1 calc R . . C22 C 0.31483(8) 0.2856(2) 0.38544(10) 0.0343(5) Uani 1 1 d . . . H22 H 0.3235 0.2153 0.4101 0.041 Uiso 1 1 calc R . . C23 C 0.27224(7) 0.3396(2) 0.38136(9) 0.0288(5) Uani 1 1 d . . . H23 H 0.2519 0.3055 0.4030 0.035 Uiso 1 1 calc R . . C24 C 0.21601(6) 0.67515(18) 0.35519(8) 0.0199(4) Uani 1 1 d . . . C25 C 0.22510(7) 0.76597(19) 0.31657(9) 0.0258(4) Uani 1 1 d . . . H25 H 0.2241 0.7444 0.2771 0.031 Uiso 1 1 calc R . . C26 C 0.23569(7) 0.8881(2) 0.33560(10) 0.0295(5) Uani 1 1 d . . . H26 H 0.2415 0.9493 0.3088 0.035 Uiso 1 1 calc R . . C27 C 0.23780(7) 0.9216(2) 0.39276(10) 0.0305(5) Uani 1 1 d . . . H27 H 0.2453 1.0051 0.4053 0.037 Uiso 1 1 calc R . . C28 C 0.22891(8) 0.8326(2) 0.43169(10) 0.0314(5) Uani 1 1 d . . . H28 H 0.2303 0.8547 0.4712 0.038 Uiso 1 1 calc R . . C29 C 0.21798(7) 0.7109(2) 0.41295(9) 0.0261(4) Uani 1 1 d . . . H29 H 0.2117 0.6506 0.4399 0.031 Uiso 1 1 calc R . . C30 C 0.08905(8) 0.0889(2) 0.43002(10) 0.0357(5) Uani 1 1 d . . . C31 C 0.09564(10) 0.0538(3) 0.49453(11) 0.0525(8) Uani 1 1 d . . . H31B H 0.0992 -0.0383 0.4984 0.063 Uiso 1 1 calc R . . H31A H 0.1241 0.0927 0.5162 0.063 Uiso 1 1 calc R . . C32 C 0.05729(11) 0.0937(3) 0.52234(12) 0.0610(9) Uani 1 1 d . . . H32B H 0.0648 0.0731 0.5644 0.073 Uiso 1 1 calc R . . H32A H 0.0293 0.0481 0.5041 0.073 Uiso 1 1 calc R . . C33 C 0.04961(9) 0.2331(3) 0.51450(10) 0.0526(8) Uani 1 1 d . . . H33B H 0.0771 0.2777 0.5355 0.063 Uiso 1 1 calc R . . H33A H 0.0241 0.2577 0.5326 0.063 Uiso 1 1 calc R . . C34 C 0.03899(8) 0.2759(3) 0.45062(10) 0.0365(5) Uani 1 1 d . . . C35 C 0.13456(9) 0.0654(2) 0.41368(13) 0.0493(7) Uani 1 1 d . . . H35C H 0.1562 0.1306 0.4310 0.059 Uiso 1 1 calc R . . H35B H 0.1306 0.0674 0.3712 0.059 Uiso 1 1 calc R . . H35A H 0.1462 -0.0169 0.4283 0.059 Uiso 1 1 calc R . . C36 C 0.05383(9) 0.0025(2) 0.39205(12) 0.0453(6) Uani 1 1 d . . . H36C H 0.0454 0.0368 0.3525 0.054 Uiso 1 1 calc R . . H36B H 0.0268 -0.0031 0.4088 0.054 Uiso 1 1 calc R . . H36A H 0.0669 -0.0813 0.3906 0.054 Uiso 1 1 calc R . . C37 C -0.00916(8) 0.2364(3) 0.41988(11) 0.0464(7) Uani 1 1 d . . . H37C H -0.0122 0.1452 0.4225 0.056 Uiso 1 1 calc R . . H37B H -0.0147 0.2615 0.3788 0.056 Uiso 1 1 calc R . . H37A H -0.0313 0.2773 0.4387 0.056 Uiso 1 1 calc R . . C38 C 0.04042(9) 0.4194(3) 0.45148(11) 0.0434(6) Uani 1 1 d . . . H38C H 0.0292 0.4515 0.4119 0.052 Uiso 1 1 calc R . . H38B H 0.0717 0.4476 0.4659 0.052 Uiso 1 1 calc R . . H38A H 0.0213 0.4510 0.4772 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02279(13) 0.01691(13) 0.01800(12) 0.00057(9) 0.00389(9) 0.00106(10) Co2 0.01712(12) 0.01914(13) 0.01715(12) 0.00205(9) 0.00505(9) -0.00022(10) P1 0.0190(2) 0.0182(2) 0.0170(2) 0.00138(17) 0.00367(17) 0.00247(18) P2 0.0164(2) 0.0184(2) 0.0169(2) 0.00273(17) 0.00420(16) 0.00100(18) P3 0.0196(2) 0.0208(2) 0.0201(2) 0.00180(18) 0.00459(18) -0.00096(19) O1 0.0352(9) 0.0343(9) 0.0383(9) -0.0027(7) 0.0067(7) 0.0138(7) O2 0.0537(11) 0.0282(9) 0.0472(10) -0.0065(8) -0.0050(8) -0.0082(8) O3 0.0368(9) 0.0624(12) 0.0223(8) 0.0130(7) 0.0049(6) 0.0087(8) O4 0.0343(8) 0.0279(8) 0.0368(8) -0.0035(6) 0.0095(7) 0.0056(7) N1 0.0252(9) 0.0331(10) 0.0243(8) 0.0053(7) 0.0061(7) -0.0072(8) C2A 0.0201(9) 0.0230(10) 0.0255(10) 0.0011(8) 0.0033(7) 0.0023(8) C1 0.0341(11) 0.0217(10) 0.0208(9) 0.0013(7) 0.0049(8) 0.0032(9) C2 0.0364(12) 0.0203(10) 0.0267(10) 0.0015(8) 0.0036(9) 0.0031(9) C3 0.0233(10) 0.0321(11) 0.0240(10) 0.0041(8) 0.0092(8) 0.0007(8) C4 0.0224(9) 0.0249(10) 0.0199(9) -0.0008(7) 0.0052(7) -0.0024(8) C5 0.0182(9) 0.0254(10) 0.0166(8) 0.0026(7) 0.0042(7) 0.0001(7) C6 0.0204(9) 0.0193(9) 0.0222(9) 0.0053(7) 0.0064(7) 0.0024(7) C7 0.0250(10) 0.0264(11) 0.0374(12) 0.0009(9) -0.0011(9) 0.0021(9) C8 0.0227(11) 0.0376(13) 0.0452(13) 0.0057(10) -0.0014(9) 0.0067(9) C9 0.0295(11) 0.0273(11) 0.0394(12) 0.0091(9) 0.0104(9) 0.0105(9) C10 0.0317(11) 0.0215(10) 0.0317(11) 0.0021(8) 0.0108(9) 0.0045(9) C11 0.0235(10) 0.0233(10) 0.0241(10) 0.0022(7) 0.0064(7) 0.0026(8) C12 0.0208(9) 0.0270(10) 0.0163(8) 0.0003(7) 0.0014(7) 0.0020(8) C13 0.0355(12) 0.0295(11) 0.0276(11) 0.0033(8) 0.0077(9) -0.0011(9) C14 0.0402(13) 0.0470(15) 0.0223(10) 0.0073(9) 0.0075(9) -0.0010(11) C15 0.0358(12) 0.0541(16) 0.0190(10) -0.0051(9) 0.0067(9) -0.0001(11) C16 0.0430(13) 0.0379(13) 0.0246(11) -0.0069(9) 0.0065(9) 0.0056(11) C17 0.0346(11) 0.0312(11) 0.0196(9) -0.0003(8) 0.0046(8) 0.0065(9) C18 0.0172(8) 0.0208(9) 0.0179(8) 0.0000(7) 0.0027(7) 0.0009(7) C19 0.0240(10) 0.0194(10) 0.0309(10) 0.0039(8) 0.0091(8) 0.0011(8) C20 0.0225(10) 0.0247(10) 0.0364(11) -0.0011(8) 0.0125(8) -0.0016(8) C21 0.0217(10) 0.0343(12) 0.0249(10) -0.0027(8) 0.0044(8) 0.0086(9) C22 0.0327(11) 0.0405(13) 0.0315(11) 0.0153(10) 0.0110(9) 0.0169(10) C23 0.0278(10) 0.0346(12) 0.0268(10) 0.0129(9) 0.0119(8) 0.0101(9) C24 0.0152(8) 0.0189(9) 0.0252(9) 0.0021(7) 0.0037(7) 0.0016(7) C25 0.0290(10) 0.0236(10) 0.0284(10) 0.0030(8) 0.0144(8) 0.0034(8) C26 0.0309(11) 0.0194(10) 0.0419(12) 0.0064(9) 0.0161(9) 0.0036(9) C27 0.0279(11) 0.0213(10) 0.0412(12) -0.0013(9) 0.0045(9) -0.0019(9) C28 0.0359(12) 0.0272(11) 0.0272(11) -0.0011(8) -0.0019(9) -0.0017(9) C29 0.0271(10) 0.0257(10) 0.0229(9) 0.0038(8) 0.0000(8) -0.0032(8) C30 0.0376(12) 0.0313(12) 0.0348(12) 0.0120(9) 0.0000(9) -0.0103(10) C31 0.0577(17) 0.0516(17) 0.0399(14) 0.0240(12) -0.0079(12) -0.0240(14) C32 0.0605(18) 0.086(2) 0.0329(14) 0.0207(14) 0.0015(12) -0.0366(17) C33 0.0438(15) 0.089(2) 0.0275(12) 0.0053(13) 0.0128(11) -0.0212(15) C34 0.0269(11) 0.0566(16) 0.0282(11) 0.0002(10) 0.0110(9) -0.0108(11) C35 0.0476(15) 0.0310(13) 0.0698(19) 0.0225(13) 0.0134(13) 0.0087(12) C36 0.0513(15) 0.0346(14) 0.0455(14) 0.0055(11) 0.0003(12) -0.0133(12) C37 0.0253(12) 0.0709(19) 0.0430(14) 0.0027(13) 0.0074(10) -0.0100(12) C38 0.0411(14) 0.0557(17) 0.0394(13) -0.0104(12) 0.0224(11) -0.0022(12) _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 C1 1.766(2) . ? Co1 C2 1.775(2) . ? Co1 C2A 2.105(2) . ? Co1 P3 2.1321(6) . ? Co1 P1 2.2135(6) . ? Co1 Co2 2.7143(5) . ? Co2 C4 1.755(2) . ? Co2 C3 1.762(2) . ? Co2 P3 2.1232(6) . ? Co2 P2 2.1948(6) . ? P1 C6 1.8196(19) . ? P1 C12 1.8392(19) . ? P1 C5 1.8498(19) . ? P2 C24 1.831(2) . ? P2 C18 1.8400(19) . ? P2 C5 1.8525(18) . ? P3 N1 1.6691(17) . ? P3 C2A 1.737(2) . ? O1 C1 1.151(2) . ? O2 C2 1.138(3) . ? O3 C3 1.149(2) . ? O4 C4 1.148(2) . ? N1 C30 1.506(3) . ? N1 C34 1.512(3) . ? C6 C11 1.392(3) . ? C6 C7 1.396(3) . ? C7 C8 1.381(3) . ? C8 C9 1.387(3) . ? C9 C10 1.382(3) . ? C10 C11 1.389(3) . ? C12 C13 1.391(3) . ? C12 C17 1.391(3) . ? C13 C14 1.388(3) . ? C14 C15 1.373(4) . ? C15 C16 1.377(3) . ? C16 C17 1.391(3) . ? C18 C23 1.383(3) . ? C18 C19 1.392(3) . ? C19 C20 1.386(3) . ? C20 C21 1.382(3) . ? C21 C22 1.378(3) . ? C22 C23 1.392(3) . ? C24 C25 1.394(3) . ? C24 C29 1.398(3) . ? C25 C26 1.392(3) . ? C26 C27 1.378(3) . ? C27 C28 1.384(3) . ? C28 C29 1.387(3) . ? C30 C35 1.523(4) . ? C30 C31 1.532(3) . ? C30 C36 1.539(3) . ? C31 C32 1.507(5) . ? C32 C33 1.510(5) . ? C33 C34 1.535(3) . ? C34 C38 1.532(4) . ? C34 C37 1.536(3) . ? 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 Co1 C2 101.91(10) . . ? C1 Co1 C2A 156.49(8) . . ? C2 Co1 C2A 90.33(9) . . ? C1 Co1 P3 108.10(7) . . ? C2 Co1 P3 112.14(7) . . ? C2A Co1 P3 48.40(6) . . ? C1 Co1 P1 94.94(7) . . ? C2 Co1 P1 110.01(7) . . ? C2A Co1 P1 99.65(6) . . ? P3 Co1 P1 125.62(2) . . ? C1 Co1 Co2 81.83(7) . . ? C2 Co1 Co2 161.57(7) . . ? C2A Co1 Co2 80.53(6) . . ? P3 Co1 Co2 50.222(18) . . ? P1 Co1 Co2 87.41(2) . . ? C4 Co2 C3 116.14(9) . . ? C4 Co2 P3 93.15(7) . . ? C3 Co2 P3 101.16(7) . . ? C4 Co2 P2 96.39(7) . . ? C3 Co2 P2 103.63(7) . . ? P3 Co2 P2 146.02(2) . . ? C4 Co2 Co1 110.04(6) . . ? C3 Co2 Co1 126.87(7) . . ? P3 Co2 Co1 50.511(16) . . ? P2 Co2 Co1 95.70(2) . . ? C6 P1 C12 103.27(9) . . ? C6 P1 C5 103.96(9) . . ? C12 P1 C5 97.91(8) . . ? C6 P1 Co1 119.73(6) . . ? C12 P1 Co1 116.38(7) . . ? C5 P1 Co1 112.72(6) . . ? C24 P2 C18 101.09(8) . . ? C24 P2 C5 106.73(9) . . ? C18 P2 C5 100.20(8) . . ? C24 P2 Co2 114.19(6) . . ? C18 P2 Co2 121.19(6) . . ? C5 P2 Co2 111.65(6) . . ? N1 P3 C2A 116.44(10) . . ? N1 P3 Co2 131.51(6) . . ? C2A P3 Co2 108.92(8) . . ? N1 P3 Co1 135.05(7) . . ? C2A P3 Co1 64.98(7) . . ? Co2 P3 Co1 79.27(2) . . ? C30 N1 C34 119.60(18) . . ? C30 N1 P3 122.34(15) . . ? C34 N1 P3 117.63(15) . . ? P3 C2A Co1 66.62(7) . . ? O1 C1 Co1 176.24(18) . . ? O2 C2 Co1 177.8(2) . . ? O3 C3 Co2 172.7(2) . . ? O4 C4 Co2 173.84(17) . . ? P1 C5 P2 113.61(10) . . ? C11 C6 C7 118.67(18) . . ? C11 C6 P1 122.22(15) . . ? C7 C6 P1 119.06(15) . . ? C8 C7 C6 120.7(2) . . ? C7 C8 C9 120.1(2) . . ? C10 C9 C8 119.7(2) . . ? C9 C10 C11 120.2(2) . . ? C10 C11 C6 120.46(19) . . ? C13 C12 C17 118.18(19) . . ? C13 C12 P1 122.62(16) . . ? C17 C12 P1 118.89(15) . . ? C14 C13 C12 120.4(2) . . ? C15 C14 C13 120.7(2) . . ? C14 C15 C16 119.8(2) . . ? C15 C16 C17 119.8(2) . . ? C12 C17 C16 121.1(2) . . ? C23 C18 C19 118.83(18) . . ? C23 C18 P2 120.96(15) . . ? C19 C18 P2 120.17(14) . . ? C20 C19 C18 120.84(18) . . ? C21 C20 C19 119.83(19) . . ? C22 C21 C20 119.81(19) . . ? C21 C22 C23 120.4(2) . . ? C18 C23 C22 120.30(19) . . ? C25 C24 C29 117.96(18) . . ? C25 C24 P2 125.54(15) . . ? C29 C24 P2 116.49(15) . . ? C26 C25 C24 120.31(19) . . ? C27 C26 C25 121.0(2) . . ? C26 C27 C28 119.4(2) . . ? C27 C28 C29 119.9(2) . . ? C28 C29 C24 121.38(19) . . ? N1 C30 C35 111.34(18) . . ? N1 C30 C31 110.1(2) . . ? C35 C30 C31 106.0(2) . . ? N1 C30 C36 110.86(18) . . ? C35 C30 C36 107.7(2) . . ? C31 C30 C36 110.76(19) . . ? C32 C31 C30 114.2(2) . . ? C31 C32 C33 109.7(2) . . ? C32 C33 C34 114.0(2) . . ? N1 C34 C38 110.42(18) . . ? N1 C34 C33 108.6(2) . . ? C38 C34 C33 106.5(2) . . ? N1 C34 C37 112.7(2) . . ? C38 C34 C37 107.5(2) . . ? C33 C34 C37 110.9(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.043 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.074 data_tg28 _database_code_depnum_ccdc_archive 'CCDC 275483' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 Mn4 N4 O16 P2' _chemical_formula_weight 1112.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 8.8228(11) _cell_length_b 9.7766(12) _cell_length_c 28.072(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.045(2) _cell_angle_gamma 90.00 _cell_volume 2403.1(5) _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 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.164 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.5938 _exptl_absorpt_correction_T_max 0.7216 _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 29121 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 29.60 _reflns_number_total 6717 _reflns_number_gt 6257 _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^)+(0.0307P)^2^+0.7213P] 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 6717 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 P1 P 0.87008(3) 0.20555(3) 0.135744(9) 0.01817(6) Uani 1 1 d . . . N1 N 1.00071(10) 0.08644(9) 0.14626(3) 0.02118(17) Uani 1 1 d . . . N2 N 0.70147(10) 0.14672(9) 0.13168(3) 0.02061(16) Uani 1 1 d . . . Mn1 Mn 0.660387(18) 0.254882(17) 0.066617(6) 0.02181(5) Uani 1 1 d . . . Mn2 Mn 0.890556(18) 0.421929(16) 0.119651(6) 0.02220(5) Uani 1 1 d . . . O1 O 0.38778(11) 0.11009(12) 0.02045(4) 0.0456(3) Uani 1 1 d . . . O2 O 0.86674(12) 0.07683(12) 0.01633(4) 0.0441(3) Uani 1 1 d . . . O3 O 0.66144(15) 0.43845(14) -0.01667(4) 0.0579(3) Uani 1 1 d . . . O4 O 0.45196(10) 0.44843(9) 0.11053(4) 0.03345(19) Uani 1 1 d . . . O5 O 1.08074(13) 0.36040(13) 0.04107(4) 0.0497(3) Uani 1 1 d . . . O6 O 0.75778(13) 0.66732(10) 0.06738(4) 0.0482(3) Uani 1 1 d . . . O7 O 1.15505(11) 0.54522(10) 0.17913(4) 0.0439(2) Uani 1 1 d . . . O8 O 0.69627(12) 0.46960(12) 0.19760(4) 0.0459(3) Uani 1 1 d . . . C1 C 0.49350(14) 0.16372(13) 0.03903(4) 0.0305(2) Uani 1 1 d . . . C2 C 0.78961(13) 0.14160(14) 0.03674(4) 0.0299(2) Uani 1 1 d . . . C3 C 0.66109(15) 0.36908(15) 0.01608(5) 0.0366(3) Uani 1 1 d . . . C4 C 0.53427(13) 0.37676(12) 0.09506(4) 0.0257(2) Uani 1 1 d . . . C5 C 1.00938(14) 0.38306(13) 0.07115(5) 0.0324(2) Uani 1 1 d . . . C6 C 0.81067(15) 0.57292(12) 0.08682(5) 0.0331(3) Uani 1 1 d . . . C7 C 1.05188(14) 0.49815(12) 0.15595(5) 0.0312(2) Uani 1 1 d . . . C8 C 0.76773(14) 0.45222(12) 0.16700(5) 0.0296(2) Uani 1 1 d . . . C9 C 1.15320(13) 0.11388(12) 0.17441(5) 0.0279(2) Uani 1 1 d . . . H9 H 1.2012 0.0225 0.1820 0.033 Uiso 1 1 calc R . . C10 C 1.26125(14) 0.19148(13) 0.14604(6) 0.0371(3) Uani 1 1 d . . . H10A H 1.2655 0.1461 0.1151 0.045 Uiso 1 1 calc R . . H10B H 1.3635 0.1930 0.1641 0.045 Uiso 1 1 calc R . . H10C H 1.2244 0.2854 0.1406 0.045 Uiso 1 1 calc R . . C11 C 1.13590(16) 0.18106(14) 0.22237(5) 0.0368(3) Uani 1 1 d . . . H11A H 1.0926 0.2728 0.2168 0.044 Uiso 1 1 calc R . . H11B H 1.2362 0.1879 0.2415 0.044 Uiso 1 1 calc R . . H11C H 1.0678 0.1257 0.2396 0.044 Uiso 1 1 calc R . . C12 C 0.96867(13) -0.05949(11) 0.13319(4) 0.0239(2) Uani 1 1 d . . . H12 H 0.8657 -0.0632 0.1139 0.029 Uiso 1 1 calc R . . C13 C 1.08450(15) -0.11333(14) 0.10163(5) 0.0344(3) Uani 1 1 d . . . H13A H 1.0858 -0.0535 0.0737 0.041 Uiso 1 1 calc R . . H13B H 1.0559 -0.2061 0.0908 0.041 Uiso 1 1 calc R . . H13C H 1.1862 -0.1150 0.1201 0.041 Uiso 1 1 calc R . . C14 C 0.96226(15) -0.14804(12) 0.17744(5) 0.0321(2) Uani 1 1 d . . . H14A H 1.0650 -0.1565 0.1950 0.039 Uiso 1 1 calc R . . H14B H 0.9235 -0.2390 0.1676 0.039 Uiso 1 1 calc R . . H14C H 0.8942 -0.1057 0.1983 0.039 Uiso 1 1 calc R . . C15 C 0.63440(12) 0.03507(11) 0.15283(4) 0.0234(2) Uani 1 1 d . . . C16 C 0.63141(14) 0.03427(14) 0.20243(5) 0.0330(3) Uani 1 1 d . . . H16 H 0.6763 0.1074 0.2215 0.040 Uiso 1 1 calc R . . C17 C 0.56270(17) -0.07353(18) 0.22390(6) 0.0491(4) Uani 1 1 d . . . H17 H 0.5610 -0.0738 0.2577 0.059 Uiso 1 1 calc R . . C18 C 0.49711(17) -0.17983(17) 0.19661(8) 0.0552(5) Uani 1 1 d . . . H18 H 0.4499 -0.2530 0.2115 0.066 Uiso 1 1 calc R . . C19 C 0.50004(15) -0.17990(14) 0.14747(7) 0.0466(4) Uani 1 1 d . . . H19 H 0.4556 -0.2538 0.1287 0.056 Uiso 1 1 calc R . . C20 C 0.56775(13) -0.07233(12) 0.12524(5) 0.0317(3) Uani 1 1 d . . . H20 H 0.5684 -0.0724 0.0914 0.038 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 P1 0.01947(11) 0.01684(11) 0.01801(12) 0.00042(8) 0.00153(9) 0.00079(9) N1 0.0200(4) 0.0179(4) 0.0252(4) -0.0004(3) 0.0012(3) 0.0018(3) N2 0.0210(4) 0.0195(4) 0.0210(4) 0.0023(3) 0.0012(3) 0.0000(3) Mn1 0.02150(8) 0.02490(9) 0.01855(8) 0.00210(6) 0.00051(6) -0.00066(6) Mn2 0.02200(8) 0.01685(8) 0.02736(9) 0.00207(6) 0.00140(6) -0.00043(5) O1 0.0328(5) 0.0484(6) 0.0518(6) -0.0138(5) -0.0091(4) -0.0044(4) O2 0.0361(5) 0.0661(7) 0.0310(5) -0.0162(5) 0.0085(4) 0.0042(5) O3 0.0597(7) 0.0731(8) 0.0392(6) 0.0292(6) -0.0003(5) -0.0062(6) O4 0.0307(4) 0.0310(4) 0.0386(5) 0.0021(4) 0.0041(4) 0.0058(3) O5 0.0467(6) 0.0585(7) 0.0483(6) 0.0019(5) 0.0239(5) -0.0082(5) O6 0.0506(6) 0.0297(5) 0.0616(7) 0.0152(5) -0.0044(5) 0.0043(4) O7 0.0322(5) 0.0299(4) 0.0654(7) -0.0089(5) -0.0110(5) -0.0015(4) O8 0.0416(5) 0.0536(6) 0.0444(6) -0.0207(5) 0.0126(4) -0.0044(5) C1 0.0287(5) 0.0338(6) 0.0283(6) -0.0031(5) 0.0005(4) 0.0021(5) C2 0.0273(5) 0.0412(6) 0.0207(5) -0.0028(5) 0.0013(4) -0.0032(5) C3 0.0349(6) 0.0450(7) 0.0287(6) 0.0091(5) -0.0006(5) -0.0024(5) C4 0.0253(5) 0.0237(5) 0.0267(5) 0.0060(4) -0.0021(4) -0.0011(4) C5 0.0306(6) 0.0293(6) 0.0376(7) 0.0058(5) 0.0057(5) -0.0051(5) C6 0.0304(6) 0.0248(5) 0.0430(7) 0.0050(5) 0.0002(5) -0.0020(4) C7 0.0289(5) 0.0196(5) 0.0443(7) -0.0006(5) 0.0010(5) 0.0022(4) C8 0.0282(5) 0.0243(5) 0.0356(6) -0.0064(4) 0.0002(5) -0.0009(4) C9 0.0215(5) 0.0233(5) 0.0369(6) 0.0010(4) -0.0044(4) 0.0026(4) C10 0.0202(5) 0.0312(6) 0.0601(9) 0.0022(6) 0.0059(5) 0.0011(4) C11 0.0404(7) 0.0333(6) 0.0327(6) 0.0003(5) -0.0115(5) 0.0001(5) C12 0.0240(5) 0.0186(4) 0.0295(5) -0.0035(4) 0.0052(4) 0.0016(4) C13 0.0317(6) 0.0330(6) 0.0401(7) -0.0094(5) 0.0105(5) 0.0056(5) C14 0.0340(6) 0.0208(5) 0.0425(7) 0.0061(5) 0.0088(5) 0.0046(4) C15 0.0177(4) 0.0214(5) 0.0317(6) 0.0060(4) 0.0058(4) 0.0036(4) C16 0.0297(6) 0.0374(6) 0.0337(6) 0.0106(5) 0.0116(5) 0.0100(5) C17 0.0378(7) 0.0587(10) 0.0553(9) 0.0325(8) 0.0236(7) 0.0163(7) C18 0.0296(7) 0.0477(9) 0.0909(14) 0.0400(9) 0.0189(7) 0.0026(6) C19 0.0250(6) 0.0264(6) 0.0875(12) 0.0148(7) 0.0025(6) -0.0031(5) C20 0.0228(5) 0.0230(5) 0.0488(7) 0.0038(5) 0.0019(5) -0.0004(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 P1 N2 1.5860(9) . ? P1 N1 1.6395(9) . ? P1 Mn2 2.1753(4) . ? P1 Mn1 2.5574(4) . ? N1 C12 1.4915(13) . ? N1 C9 1.4986(14) . ? N2 C15 1.4072(13) . ? N2 Mn1 2.1031(9) . ? Mn1 C3 1.8059(13) . ? Mn1 C1 1.8118(13) . ? Mn1 C2 1.8612(13) . ? Mn1 C4 1.8744(12) . ? Mn1 Mn2 2.8750(3) . ? Mn2 C7 1.8066(13) . ? Mn2 C6 1.8347(13) . ? Mn2 C8 1.8391(13) . ? Mn2 C5 1.8567(14) . ? O1 C1 1.1392(16) . ? O2 C2 1.1349(16) . ? O3 C3 1.1428(17) . ? O4 C4 1.1333(15) . ? O5 C5 1.1352(17) . ? O6 C6 1.1423(16) . ? O7 C7 1.1481(16) . ? O8 C8 1.1389(17) . ? C9 C10 1.5182(18) . ? C9 C11 1.5223(19) . ? C12 C14 1.5209(17) . ? C12 C13 1.5260(16) . ? C15 C20 1.3917(17) . ? C15 C16 1.3957(17) . ? C16 C17 1.3897(19) . ? C17 C18 1.376(3) . ? C18 C19 1.383(3) . ? C19 C20 1.3941(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 N2 P1 N1 112.82(5) . . ? N2 P1 Mn2 116.03(3) . . ? N1 P1 Mn2 130.82(4) . . ? N2 P1 Mn1 55.17(3) . . ? N1 P1 Mn1 134.24(4) . . ? Mn2 P1 Mn1 74.324(10) . . ? C12 N1 C9 115.58(8) . . ? C12 N1 P1 121.82(7) . . ? C9 N1 P1 122.25(7) . . ? C15 N2 P1 133.64(8) . . ? C15 N2 Mn1 136.05(7) . . ? P1 N2 Mn1 86.58(4) . . ? C3 Mn1 C1 92.82(6) . . ? C3 Mn1 C2 87.28(6) . . ? C1 Mn1 C2 91.45(5) . . ? C3 Mn1 C4 90.06(6) . . ? C1 Mn1 C4 90.06(5) . . ? C2 Mn1 C4 177.00(5) . . ? C3 Mn1 N2 167.49(5) . . ? C1 Mn1 N2 99.69(5) . . ? C2 Mn1 N2 92.42(5) . . ? C4 Mn1 N2 89.87(4) . . ? C3 Mn1 P1 129.85(4) . . ? C1 Mn1 P1 134.90(4) . . ? C2 Mn1 P1 78.67(4) . . ? C4 Mn1 P1 102.04(4) . . ? N2 Mn1 P1 38.25(2) . . ? C3 Mn1 Mn2 89.16(5) . . ? C1 Mn1 Mn2 170.46(4) . . ? C2 Mn1 Mn2 97.96(4) . . ? C4 Mn1 Mn2 80.61(4) . . ? N2 Mn1 Mn2 78.49(3) . . ? P1 Mn1 Mn2 46.758(9) . . ? C7 Mn2 C6 100.31(6) . . ? C7 Mn2 C8 91.10(6) . . ? C6 Mn2 C8 90.54(6) . . ? C7 Mn2 C5 91.23(6) . . ? C6 Mn2 C5 90.74(6) . . ? C8 Mn2 C5 177.10(5) . . ? C7 Mn2 P1 111.33(4) . . ? C6 Mn2 P1 148.24(4) . . ? C8 Mn2 P1 86.28(4) . . ? C5 Mn2 P1 91.26(4) . . ? C7 Mn2 Mn1 169.73(4) . . ? C6 Mn2 Mn1 89.63(4) . . ? C8 Mn2 Mn1 91.40(4) . . ? C5 Mn2 Mn1 86.02(4) . . ? P1 Mn2 Mn1 58.918(10) . . ? O1 C1 Mn1 177.48(13) . . ? O2 C2 Mn1 176.24(12) . . ? O3 C3 Mn1 178.22(15) . . ? O4 C4 Mn1 176.44(11) . . ? O5 C5 Mn2 179.05(13) . . ? O6 C6 Mn2 177.88(14) . . ? O7 C7 Mn2 179.26(12) . . ? O8 C8 Mn2 177.36(12) . . ? N1 C9 C10 113.18(10) . . ? N1 C9 C11 111.27(10) . . ? C10 C9 C11 112.70(11) . . ? N1 C12 C14 111.63(9) . . ? N1 C12 C13 110.64(9) . . ? C14 C12 C13 111.87(10) . . ? C20 C15 C16 119.51(11) . . ? C20 C15 N2 121.41(11) . . ? C16 C15 N2 119.05(11) . . ? C17 C16 C15 119.97(14) . . ? C18 C17 C16 120.50(16) . . ? C17 C18 C19 119.84(13) . . ? C18 C19 C20 120.51(15) . . ? C15 C20 C19 119.67(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.60 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.324 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.076 data_tgg25 _database_code_depnum_ccdc_archive 'CCDC 275484' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H23 Mn2 N2 O8 P Si' _chemical_formula_weight 552.31 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' Si Si 0.0817 0.0704 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7307(13) _cell_length_b 10.5029(8) _cell_length_c 15.5917(13) _cell_angle_alpha 90.00 _cell_angle_beta 113.0100(10) _cell_angle_gamma 90.00 _cell_volume 2371.1(3) _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 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.7099 _exptl_absorpt_correction_T_max 0.9412 _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 26467 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.25 _reflns_number_total 5835 _reflns_number_gt 5434 _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^)+(0.0284P)^2^+0.8282P] 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 5835 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.180875(11) 0.456641(16) 0.186823(11) 0.01633(5) Uani 1 1 d . . . Mn2 Mn 0.376948(11) 0.429676(16) 0.293225(11) 0.01714(5) Uani 1 1 d . . . P1 P 0.285486(18) 0.56000(2) 0.325935(19) 0.01540(6) Uani 1 1 d . . . Si4 Si 0.12732(2) 0.45931(3) 0.38840(2) 0.01896(7) Uani 1 1 d . . . N1 N 0.29655(6) 0.71502(9) 0.34461(6) 0.01740(17) Uani 1 1 d . . . N2 N 0.19239(6) 0.50525(9) 0.32632(6) 0.01825(18) Uani 1 1 d . . . O1 O -0.02125(6) 0.42775(10) 0.08871(7) 0.0379(2) Uani 1 1 d . . . O2 O 0.19655(6) 0.17486(8) 0.22040(7) 0.02958(19) Uani 1 1 d . . . O3 O 0.22303(7) 0.39962(9) 0.02205(6) 0.0309(2) Uani 1 1 d . . . O4 O 0.14396(6) 0.72548(8) 0.11991(6) 0.02832(19) Uani 1 1 d . . . O5 O 0.34532(7) 0.24324(10) 0.42274(7) 0.0356(2) Uani 1 1 d . . . O6 O 0.40385(7) 0.21422(10) 0.18247(7) 0.0382(2) Uani 1 1 d . . . O7 O 0.56556(6) 0.46550(10) 0.43559(7) 0.0334(2) Uani 1 1 d . . . O8 O 0.41843(7) 0.60380(10) 0.16331(6) 0.0331(2) Uani 1 1 d . . . C1 C 0.05672(8) 0.43755(11) 0.12888(9) 0.0245(2) Uani 1 1 d . . . C2 C 0.19434(8) 0.28261(11) 0.21320(8) 0.0216(2) Uani 1 1 d . . . C3 C 0.20698(8) 0.42227(11) 0.08589(8) 0.0219(2) Uani 1 1 d . . . C4 C 0.16176(7) 0.62543(11) 0.14907(7) 0.0199(2) Uani 1 1 d . . . C5 C 0.35510(8) 0.31426(11) 0.37244(8) 0.0237(2) Uani 1 1 d . . . C6 C 0.39391(8) 0.29696(12) 0.22493(9) 0.0251(2) Uani 1 1 d . . . C7 C 0.49301(8) 0.45143(11) 0.37993(8) 0.0226(2) Uani 1 1 d . . . C8 C 0.40056(8) 0.54054(11) 0.21326(8) 0.0222(2) Uani 1 1 d . . . C9 C 0.22214(8) 0.78495(11) 0.36197(8) 0.0206(2) Uani 1 1 d . . . H9 H 0.1650 0.7320 0.3340 0.025 Uiso 1 1 calc R . . C10 C 0.24305(9) 0.79389(12) 0.46587(9) 0.0279(2) Uani 1 1 d . . . H10A H 0.2639 0.7108 0.4951 0.033 Uiso 1 1 calc R . . H10B H 0.1871 0.8193 0.4747 0.033 Uiso 1 1 calc R . . H10C H 0.2916 0.8573 0.4946 0.033 Uiso 1 1 calc R . . C11 C 0.19865(9) 0.91486(11) 0.31547(9) 0.0261(2) Uani 1 1 d . . . H11A H 0.2518 0.9718 0.3428 0.031 Uiso 1 1 calc R . . H11B H 0.1455 0.9506 0.3252 0.031 Uiso 1 1 calc R . . H11C H 0.1834 0.9058 0.2485 0.031 Uiso 1 1 calc R . . C12 C 0.38257(8) 0.77729(11) 0.34756(8) 0.0221(2) Uani 1 1 d . . . H12 H 0.4251 0.7067 0.3473 0.027 Uiso 1 1 calc R . . C13 C 0.36778(9) 0.85781(13) 0.26086(10) 0.0298(3) Uani 1 1 d . . . H13A H 0.3275 0.8118 0.2051 0.036 Uiso 1 1 calc R . . H13B H 0.4275 0.8741 0.2569 0.036 Uiso 1 1 calc R . . H13C H 0.3389 0.9389 0.2652 0.036 Uiso 1 1 calc R . . C14 C 0.43317(9) 0.85237(13) 0.43694(10) 0.0314(3) Uani 1 1 d . . . H14A H 0.3963 0.9268 0.4386 0.038 Uiso 1 1 calc R . . H14B H 0.4932 0.8805 0.4386 0.038 Uiso 1 1 calc R . . H14C H 0.4425 0.7980 0.4910 0.038 Uiso 1 1 calc R . . C15 C 0.07294(9) 0.30150(12) 0.34618(9) 0.0292(3) Uani 1 1 d . . . H15A H 0.0331 0.3073 0.2798 0.035 Uiso 1 1 calc R . . H15B H 0.0360 0.2763 0.3814 0.035 Uiso 1 1 calc R . . H15C H 0.1212 0.2379 0.3551 0.035 Uiso 1 1 calc R . . C16 C 0.03235(9) 0.57496(13) 0.37263(11) 0.0320(3) Uani 1 1 d . . . H16A H 0.0588 0.6578 0.3982 0.038 Uiso 1 1 calc R . . H16B H -0.0056 0.5438 0.4053 0.038 Uiso 1 1 calc R . . H16C H -0.0061 0.5840 0.3061 0.038 Uiso 1 1 calc R . . C17 C 0.20260(10) 0.44460(13) 0.51437(9) 0.0309(3) Uani 1 1 d . . . H17A H 0.2497 0.3794 0.5226 0.037 Uiso 1 1 calc R . . H17B H 0.1650 0.4202 0.5492 0.037 Uiso 1 1 calc R . . H17C H 0.2327 0.5264 0.5376 0.037 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 0.01504(8) 0.01724(8) 0.01629(8) 0.00007(6) 0.00566(6) -0.00113(6) Mn2 0.01487(8) 0.01811(8) 0.01841(8) -0.00018(6) 0.00648(6) 0.00146(6) P1 0.01445(12) 0.01580(12) 0.01617(13) 0.00038(9) 0.00623(10) 0.00001(9) Si4 0.01731(14) 0.02138(15) 0.01997(15) 0.00271(11) 0.00921(12) -0.00019(11) N1 0.0162(4) 0.0163(4) 0.0205(4) -0.0010(3) 0.0081(3) -0.0006(3) N2 0.0172(4) 0.0206(4) 0.0177(4) 0.0004(3) 0.0076(3) -0.0016(3) O1 0.0199(4) 0.0488(6) 0.0379(5) 0.0061(4) 0.0036(4) -0.0065(4) O2 0.0338(5) 0.0202(4) 0.0336(5) 0.0005(4) 0.0119(4) -0.0025(3) O3 0.0431(5) 0.0285(5) 0.0258(4) -0.0026(4) 0.0185(4) -0.0002(4) O4 0.0352(5) 0.0237(4) 0.0254(4) 0.0041(3) 0.0112(4) 0.0048(4) O5 0.0325(5) 0.0340(5) 0.0390(5) 0.0145(4) 0.0125(4) 0.0014(4) O6 0.0306(5) 0.0367(5) 0.0451(6) -0.0173(5) 0.0124(4) 0.0032(4) O7 0.0208(4) 0.0439(6) 0.0293(5) 0.0026(4) 0.0032(4) -0.0028(4) O8 0.0329(5) 0.0413(5) 0.0268(4) 0.0057(4) 0.0134(4) -0.0047(4) C1 0.0225(6) 0.0259(6) 0.0243(6) 0.0034(4) 0.0082(5) -0.0021(4) C2 0.0206(5) 0.0244(6) 0.0195(5) -0.0017(4) 0.0076(4) -0.0027(4) C3 0.0232(5) 0.0179(5) 0.0231(5) 0.0000(4) 0.0075(4) -0.0020(4) C4 0.0187(5) 0.0242(5) 0.0175(5) -0.0014(4) 0.0079(4) 0.0002(4) C5 0.0185(5) 0.0229(5) 0.0271(6) 0.0015(5) 0.0061(4) 0.0029(4) C6 0.0175(5) 0.0278(6) 0.0287(6) -0.0030(5) 0.0074(4) 0.0013(4) C7 0.0217(5) 0.0245(6) 0.0228(6) 0.0020(4) 0.0099(5) 0.0017(4) C8 0.0175(5) 0.0272(6) 0.0203(5) -0.0018(4) 0.0055(4) 0.0013(4) C9 0.0201(5) 0.0195(5) 0.0240(5) -0.0004(4) 0.0105(4) 0.0029(4) C10 0.0345(6) 0.0270(6) 0.0257(6) -0.0018(5) 0.0157(5) 0.0048(5) C11 0.0265(6) 0.0208(5) 0.0307(6) 0.0020(5) 0.0108(5) 0.0046(4) C12 0.0183(5) 0.0198(5) 0.0291(6) -0.0010(4) 0.0103(4) -0.0029(4) C13 0.0275(6) 0.0283(6) 0.0387(7) 0.0065(5) 0.0186(5) -0.0020(5) C14 0.0239(6) 0.0272(6) 0.0380(7) -0.0077(5) 0.0064(5) -0.0058(5) C15 0.0306(6) 0.0274(6) 0.0326(6) 0.0006(5) 0.0154(5) -0.0086(5) C16 0.0237(6) 0.0338(7) 0.0439(8) 0.0050(6) 0.0191(6) 0.0053(5) C17 0.0329(7) 0.0370(7) 0.0220(6) 0.0056(5) 0.0101(5) -0.0027(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 C3 1.8113(12) . ? Mn1 C1 1.8143(12) . ? Mn1 C4 1.8551(12) . ? Mn1 C2 1.8674(12) . ? Mn1 N2 2.1717(9) . ? Mn1 P1 2.4084(3) . ? Mn1 Mn2 2.8888(3) . ? Mn2 C7 1.8120(12) . ? Mn2 C6 1.8358(12) . ? Mn2 C8 1.8466(12) . ? Mn2 C5 1.8560(12) . ? Mn2 P1 2.1857(3) . ? P1 N2 1.5756(9) . ? P1 N1 1.6512(9) . ? Si4 N2 1.7297(9) . ? Si4 C17 1.8617(13) . ? Si4 C15 1.8633(13) . ? Si4 C16 1.8656(13) . ? N1 C12 1.4873(13) . ? N1 C9 1.4935(13) . ? O1 C1 1.1431(15) . ? O2 C2 1.1364(15) . ? O3 C3 1.1435(15) . ? O4 C4 1.1357(15) . ? O5 C5 1.1356(15) . ? O6 C6 1.1397(15) . ? O7 C7 1.1416(15) . ? O8 C8 1.1394(15) . ? C9 C11 1.5213(16) . ? C9 C10 1.5247(16) . ? C12 C14 1.5265(17) . ? C12 C13 1.5333(17) . ? 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 C3 Mn1 C1 96.36(5) . . ? C3 Mn1 C4 88.77(5) . . ? C1 Mn1 C4 86.46(5) . . ? C3 Mn1 C2 87.22(5) . . ? C1 Mn1 C2 90.50(5) . . ? C4 Mn1 C2 174.67(5) . . ? C3 Mn1 N2 163.45(4) . . ? C1 Mn1 N2 100.18(5) . . ? C4 Mn1 N2 91.88(4) . . ? C2 Mn1 N2 92.96(4) . . ? C3 Mn1 P1 124.41(4) . . ? C1 Mn1 P1 136.21(4) . . ? C4 Mn1 P1 79.86(3) . . ? C2 Mn1 P1 105.31(4) . . ? N2 Mn1 P1 39.82(2) . . ? C3 Mn1 Mn2 85.74(4) . . ? C1 Mn1 Mn2 167.17(4) . . ? C4 Mn1 Mn2 106.27(3) . . ? C2 Mn1 Mn2 76.93(3) . . ? N2 Mn1 Mn2 78.20(2) . . ? P1 Mn1 Mn2 47.680(8) . . ? C7 Mn2 C6 101.30(5) . . ? C7 Mn2 C8 90.82(5) . . ? C6 Mn2 C8 88.51(5) . . ? C7 Mn2 C5 88.89(5) . . ? C6 Mn2 C5 89.82(6) . . ? C8 Mn2 C5 178.21(5) . . ? C7 Mn2 P1 108.07(4) . . ? C6 Mn2 P1 150.34(4) . . ? C8 Mn2 P1 95.00(4) . . ? C5 Mn2 P1 86.77(4) . . ? C7 Mn2 Mn1 162.61(4) . . ? C6 Mn2 Mn1 96.08(4) . . ? C8 Mn2 Mn1 90.10(4) . . ? C5 Mn2 Mn1 90.71(4) . . ? P1 Mn2 Mn1 54.562(9) . . ? N2 P1 N1 113.15(5) . . ? N2 P1 Mn2 118.04(4) . . ? N1 P1 Mn2 128.69(3) . . ? N2 P1 Mn1 61.97(3) . . ? N1 P1 Mn1 126.23(4) . . ? Mn2 P1 Mn1 77.758(11) . . ? N2 Si4 C17 110.00(5) . . ? N2 Si4 C15 109.93(5) . . ? C17 Si4 C15 108.28(6) . . ? N2 Si4 C16 111.30(5) . . ? C17 Si4 C16 109.84(7) . . ? C15 Si4 C16 107.41(6) . . ? C12 N1 C9 123.10(9) . . ? C12 N1 P1 118.09(7) . . ? C9 N1 P1 118.74(7) . . ? P1 N2 Si4 149.12(6) . . ? P1 N2 Mn1 78.21(4) . . ? Si4 N2 Mn1 131.22(5) . . ? O1 C1 Mn1 176.83(11) . . ? O2 C2 Mn1 173.21(11) . . ? O3 C3 Mn1 179.41(11) . . ? O4 C4 Mn1 174.42(10) . . ? O5 C5 Mn2 177.36(11) . . ? O6 C6 Mn2 179.52(11) . . ? O7 C7 Mn2 178.91(11) . . ? O8 C8 Mn2 176.07(11) . . ? N1 C9 C11 114.60(9) . . ? N1 C9 C10 111.35(9) . . ? C11 C9 C10 111.25(10) . . ? N1 C12 C14 113.51(10) . . ? N1 C12 C13 113.11(9) . . ? C14 C12 C13 111.42(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.406 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.046 data_tg19 _database_code_depnum_ccdc_archive 'CCDC 275485' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Mn2 N O8 P' _chemical_formula_weight 465.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6736(7) _cell_length_b 9.5035(9) _cell_length_c 15.4285(15) _cell_angle_alpha 104.344(2) _cell_angle_beta 96.656(2) _cell_angle_gamma 97.440(2) _cell_volume 928.81(16) _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 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 1.486 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.5238 _exptl_absorpt_correction_T_max 0.8656 _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 11559 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 29.58 _reflns_number_total 5109 _reflns_number_gt 4614 _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^)+(0.0312P)^2^+0.2097P] 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 5109 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.29866(3) 0.728387(19) 0.154830(12) 0.02009(5) Uani 1 1 d . . . Mn2 Mn 0.25356(3) 0.842082(19) 0.344246(12) 0.02111(5) Uani 1 1 d . . . P1 P 0.16824(4) 0.62926(3) 0.250468(19) 0.01928(7) Uani 1 1 d . . . N1 N 0.12103(15) 0.45680(11) 0.24946(7) 0.02308(19) Uani 1 1 d . . . O1 O 0.67817(15) 0.61930(11) 0.21151(7) 0.0310(2) Uani 1 1 d . . . O2 O 0.54127(17) 0.99704(13) 0.13032(11) 0.0521(3) Uani 1 1 d . . . O3 O -0.08428(16) 0.82712(12) 0.08838(7) 0.0365(2) Uani 1 1 d . . . O4 O 0.25889(17) 0.51565(13) -0.02371(7) 0.0400(2) Uani 1 1 d . . . O5 O 0.64396(15) 0.76369(12) 0.41865(7) 0.0358(2) Uani 1 1 d . . . O6 O 0.10836(17) 0.85534(13) 0.51968(7) 0.0392(2) Uani 1 1 d . . . O7 O 0.48485(19) 1.13631(12) 0.35336(9) 0.0485(3) Uani 1 1 d . . . O8 O -0.12554(16) 0.95412(12) 0.28763(7) 0.0344(2) Uani 1 1 d . . . C1 C 0.53442(19) 0.66298(13) 0.19022(8) 0.0238(2) Uani 1 1 d . . . C2 C 0.4499(2) 0.89554(15) 0.14113(11) 0.0322(3) Uani 1 1 d . . . C3 C 0.0595(2) 0.79073(14) 0.11639(8) 0.0258(2) Uani 1 1 d . . . C4 C 0.27529(19) 0.59963(15) 0.04544(9) 0.0272(2) Uani 1 1 d . . . C5 C 0.49477(19) 0.79143(14) 0.38869(8) 0.0259(2) Uani 1 1 d . . . C6 C 0.1661(2) 0.85189(14) 0.45228(8) 0.0278(2) Uani 1 1 d . . . C7 C 0.3969(2) 1.02359(15) 0.35009(10) 0.0322(3) Uani 1 1 d . . . C8 C 0.0170(2) 0.90788(13) 0.30677(8) 0.0256(2) Uani 1 1 d . . . C9 C 0.0874(2) 0.40158(15) 0.32974(9) 0.0295(3) Uani 1 1 d . . . H9 H 0.0689 0.2917 0.3090 0.035 Uiso 1 1 calc R . . C10 C 0.2726(2) 0.45087(17) 0.40376(9) 0.0352(3) Uani 1 1 d . . . H10A H 0.3966 0.4339 0.3771 0.042 Uiso 1 1 calc R . . H10B H 0.2581 0.3945 0.4486 0.042 Uiso 1 1 calc R . . H10C H 0.2825 0.5560 0.4333 0.042 Uiso 1 1 calc R . . C11 C -0.1089(2) 0.44029(18) 0.36335(10) 0.0377(3) Uani 1 1 d . . . H11A H -0.0964 0.5475 0.3856 0.045 Uiso 1 1 calc R . . H11B H -0.1334 0.3952 0.4126 0.045 Uiso 1 1 calc R . . H11C H -0.2237 0.4032 0.3135 0.045 Uiso 1 1 calc R . . C12 C 0.1033(2) 0.34210(14) 0.16059(9) 0.0274(2) Uani 1 1 d . . . H12 H 0.1099 0.3952 0.1123 0.033 Uiso 1 1 calc R . . C13 C -0.1013(2) 0.24065(17) 0.13854(10) 0.0383(3) Uani 1 1 d . . . H13A H -0.1094 0.1820 0.1825 0.046 Uiso 1 1 calc R . . H13B H -0.1149 0.1749 0.0775 0.046 Uiso 1 1 calc R . . H13C H -0.2118 0.2994 0.1414 0.046 Uiso 1 1 calc R . . C14 C 0.2831(2) 0.26033(18) 0.16033(11) 0.0409(3) Uani 1 1 d . . . H14A H 0.4108 0.3311 0.1760 0.049 Uiso 1 1 calc R . . H14B H 0.2778 0.1942 0.1000 0.049 Uiso 1 1 calc R . . H14C H 0.2773 0.2027 0.2048 0.049 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 0.01945(9) 0.01944(9) 0.02155(9) 0.00528(7) 0.00410(6) 0.00340(6) Mn2 0.02178(9) 0.01876(9) 0.02063(9) 0.00180(7) 0.00083(6) 0.00442(6) P1 0.01971(13) 0.01778(13) 0.01989(13) 0.00389(10) 0.00340(10) 0.00336(10) N1 0.0232(5) 0.0201(4) 0.0267(5) 0.0070(4) 0.0042(4) 0.0045(4) O1 0.0265(5) 0.0356(5) 0.0318(5) 0.0080(4) 0.0041(4) 0.0109(4) O2 0.0335(6) 0.0345(6) 0.0997(10) 0.0339(7) 0.0205(6) 0.0063(5) O3 0.0340(5) 0.0465(6) 0.0327(5) 0.0124(5) 0.0036(4) 0.0177(4) O4 0.0436(6) 0.0439(6) 0.0276(5) -0.0010(4) 0.0067(4) 0.0089(5) O5 0.0301(5) 0.0401(5) 0.0367(5) 0.0096(4) -0.0014(4) 0.0109(4) O6 0.0435(6) 0.0500(6) 0.0246(5) 0.0060(4) 0.0070(4) 0.0155(5) O7 0.0457(6) 0.0272(5) 0.0658(8) 0.0140(5) -0.0109(6) -0.0039(5) O8 0.0327(5) 0.0367(5) 0.0319(5) 0.0032(4) -0.0001(4) 0.0153(4) C1 0.0246(6) 0.0230(5) 0.0230(5) 0.0044(4) 0.0054(4) 0.0026(4) C2 0.0242(6) 0.0279(6) 0.0485(8) 0.0141(6) 0.0095(5) 0.0076(5) C3 0.0278(6) 0.0278(6) 0.0225(5) 0.0065(5) 0.0062(4) 0.0058(5) C4 0.0259(6) 0.0298(6) 0.0267(6) 0.0077(5) 0.0056(5) 0.0060(5) C5 0.0271(6) 0.0247(5) 0.0238(5) 0.0029(5) 0.0030(5) 0.0042(5) C6 0.0280(6) 0.0280(6) 0.0242(5) 0.0011(5) -0.0003(5) 0.0084(5) C7 0.0300(6) 0.0257(6) 0.0368(7) 0.0055(5) -0.0051(5) 0.0047(5) C8 0.0293(6) 0.0226(5) 0.0221(5) 0.0005(4) 0.0027(4) 0.0052(5) C9 0.0333(7) 0.0290(6) 0.0307(6) 0.0145(5) 0.0075(5) 0.0058(5) C10 0.0418(8) 0.0387(7) 0.0281(6) 0.0120(6) 0.0045(5) 0.0123(6) C11 0.0368(7) 0.0471(8) 0.0368(7) 0.0188(7) 0.0153(6) 0.0104(6) C12 0.0312(6) 0.0215(5) 0.0272(6) 0.0031(5) 0.0034(5) 0.0033(5) C13 0.0399(8) 0.0337(7) 0.0344(7) 0.0051(6) -0.0001(6) -0.0054(6) C14 0.0446(8) 0.0406(8) 0.0377(7) 0.0031(6) 0.0073(6) 0.0211(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 Mn1 C4 1.7990(13) . ? Mn1 C1 1.8391(12) . ? Mn1 C2 1.8405(14) . ? Mn1 C3 1.8570(13) . ? Mn1 P1 2.1439(4) . ? Mn1 Mn2 2.9193(4) . ? Mn2 C6 1.8139(14) . ? Mn2 C7 1.8369(14) . ? Mn2 C5 1.8443(13) . ? Mn2 C8 1.8547(13) . ? Mn2 P1 2.1376(4) . ? P1 N1 1.6242(10) . ? N1 C9 1.4886(15) . ? N1 C12 1.5069(16) . ? O1 C1 1.1394(15) . ? O2 C2 1.1318(17) . ? O3 C3 1.1364(16) . ? O4 C4 1.1470(17) . ? O5 C5 1.1384(16) . ? O6 C6 1.1445(17) . ? O7 C7 1.1395(18) . ? O8 C8 1.1371(16) . ? C9 C10 1.5195(19) . ? C9 C11 1.5195(19) . ? C12 C14 1.5116(18) . ? C12 C13 1.5157(19) . ? 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 C4 Mn1 C1 89.07(6) . . ? C4 Mn1 C2 103.24(6) . . ? C1 Mn1 C2 90.51(6) . . ? C4 Mn1 C3 89.50(6) . . ? C1 Mn1 C3 178.57(5) . . ? C2 Mn1 C3 89.98(6) . . ? C4 Mn1 P1 112.07(4) . . ? C1 Mn1 P1 85.86(4) . . ? C2 Mn1 P1 144.41(5) . . ? C3 Mn1 P1 94.53(4) . . ? C4 Mn1 Mn2 158.96(4) . . ? C1 Mn1 Mn2 90.04(4) . . ? C2 Mn1 Mn2 97.78(5) . . ? C3 Mn1 Mn2 91.23(4) . . ? P1 Mn1 Mn2 46.922(10) . . ? C6 Mn2 C7 107.85(6) . . ? C6 Mn2 C5 89.64(6) . . ? C7 Mn2 C5 88.37(6) . . ? C6 Mn2 C8 88.24(6) . . ? C7 Mn2 C8 88.23(6) . . ? C5 Mn2 C8 175.25(5) . . ? C6 Mn2 P1 113.29(4) . . ? C7 Mn2 P1 138.84(5) . . ? C5 Mn2 P1 90.91(4) . . ? C8 Mn2 P1 93.84(4) . . ? C6 Mn2 Mn1 159.97(4) . . ? C7 Mn2 Mn1 91.91(5) . . ? C5 Mn2 Mn1 94.25(4) . . ? C8 Mn2 Mn1 89.18(4) . . ? P1 Mn2 Mn1 47.104(9) . . ? N1 P1 Mn2 140.12(4) . . ? N1 P1 Mn1 129.61(4) . . ? Mn2 P1 Mn1 85.974(14) . . ? C9 N1 C12 116.53(10) . . ? C9 N1 P1 125.04(9) . . ? C12 N1 P1 118.41(8) . . ? O1 C1 Mn1 178.46(11) . . ? O2 C2 Mn1 178.20(16) . . ? O3 C3 Mn1 176.39(11) . . ? O4 C4 Mn1 178.81(13) . . ? O5 C5 Mn2 177.77(12) . . ? O6 C6 Mn2 178.59(13) . . ? O7 C7 Mn2 179.58(14) . . ? O8 C8 Mn2 176.51(11) . . ? N1 C9 C10 111.96(11) . . ? N1 C9 C11 111.28(10) . . ? C10 C9 C11 112.93(12) . . ? N1 C12 C14 110.38(11) . . ? N1 C12 C13 111.34(11) . . ? C14 C12 C13 112.98(12) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.532 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.058