# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'P G Edwards' _publ_contact_author_email EDWARDSPG@CARDIFF.AC.UK _publ_section_title ; Manganese Complexes of Phosphino-?-phosphido Ligands ; loop_ _publ_author_name 'P G Edwards' 'Ekkehardt Hahn' 'Benson M Kariuki' 'Matthieu Limon' 'Paul Newman' 'Andreas Stasch' # Attachment 'Figure 1.CIF' data_ASPGE01 _database_code_depnum_ccdc_archive 'CCDC 714222' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H14 Mn2 O6 P4, C4 H8 O' _chemical_formula_sum 'C22 H22 Mn2 O7 P4' _chemical_formula_weight 632.16 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' 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 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 9.3011(19) _cell_length_b 19.035(4) _cell_length_c 14.797(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.99(3) _cell_angle_gamma 90.00 _cell_volume 2609.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 257 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 26.99 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.763 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5598 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2842 _reflns_number_gt 2574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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. Analysis of carbonyl ligand ADPs suggests possible substitutional disorder but refinement is satistactory for single occupancy. ; _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^)+(0.0248P)^2^+2.5062P] 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 2842 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Mn1 Mn 0.07852(2) 0.267328(12) 0.051716(16) 0.02252(8) Uani 1 1 d . . . P1 P 0.24850(4) 0.17938(2) 0.03279(3) 0.02248(10) Uani 1 1 d . . . O1 O -0.10868(16) 0.18012(7) 0.15823(10) 0.0462(4) Uani 1 1 d . . . C1 C 0.15400(17) 0.10822(8) -0.03029(11) 0.0239(3) Uani 1 1 d . . . H1 H 0.3021(19) 0.1448(10) 0.1053(12) 0.030(5) Uiso 1 1 d . . . P2 P -0.02880(5) 0.21738(2) -0.07626(3) 0.02655(11) Uani 1 1 d . . . O2 O -0.10824(16) 0.39346(7) 0.04138(11) 0.0494(4) Uani 1 1 d . . . C2 C 0.02718(18) 0.12598(8) -0.08369(11) 0.0251(3) Uani 1 1 d . . . O3 O 0.22898(16) 0.31556(8) 0.22495(9) 0.0449(3) Uani 1 1 d . . . C3 C -0.04847(19) 0.07532(9) -0.13649(11) 0.0296(4) Uani 1 1 d . . . H3 H -0.1334 0.0876 -0.1734 0.036 Uiso 1 1 calc R . . O4 O 0.5000 -0.12439(11) -0.2500 0.0509(5) Uani 1 2 d S . . C4 C 0.0018(2) 0.00653(9) -0.13460(12) 0.0325(4) Uani 1 1 d . . . H4 H -0.0503 -0.0286 -0.1694 0.039 Uiso 1 1 calc R . . C5 C 0.1270(2) -0.01113(9) -0.08248(12) 0.0312(4) Uani 1 1 d . . . H5 H 0.1606 -0.0583 -0.0819 0.037 Uiso 1 1 calc R . . C6 C 0.20434(19) 0.03938(8) -0.03092(12) 0.0279(3) Uani 1 1 d . . . H6 H 0.2914 0.0270 0.0038 0.034 Uiso 1 1 calc R . . C7 C -0.0365(2) 0.21366(9) 0.11602(12) 0.0303(4) Uani 1 1 d . . . C8 C -0.03733(19) 0.34405(9) 0.04443(12) 0.0314(4) Uani 1 1 d . . . C9 C 0.17388(19) 0.29707(9) 0.15678(12) 0.0294(4) Uani 1 1 d . . . C10 C 0.6025(2) -0.08093(13) -0.28888(15) 0.0513(5) Uani 1 1 d . . . H10A H 0.5885 -0.0830 -0.3559 0.062 Uiso 1 1 calc R . . H10B H 0.7018 -0.0966 -0.2693 0.062 Uiso 1 1 calc R . . C11 C 0.5788(3) -0.00769(15) -0.2566(2) 0.0707(8) Uani 1 1 d . . . H11A H 0.6377 0.0020 -0.1989 0.085 Uiso 1 1 calc R . . H11B H 0.6019 0.0274 -0.3025 0.085 Uiso 1 1 calc R . . H2A H -0.172(2) 0.2134(11) -0.0824(14) 0.040(6) Uiso 1 1 d . . . H2B H -0.008(2) 0.2431(11) -0.1594(14) 0.043(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.02320(14) 0.01838(13) 0.02586(14) -0.00110(9) 0.00144(10) -0.00008(9) P1 0.0241(2) 0.0183(2) 0.0247(2) 0.00121(15) -0.00006(16) 0.00055(15) O1 0.0555(9) 0.0362(7) 0.0498(8) -0.0048(6) 0.0215(7) -0.0166(7) C1 0.0273(8) 0.0209(7) 0.0242(8) 0.0018(6) 0.0063(6) -0.0019(6) P2 0.0268(2) 0.0221(2) 0.0296(2) 0.00007(17) -0.00403(17) 0.00075(16) O2 0.0508(9) 0.0346(7) 0.0632(10) 0.0011(7) 0.0071(7) 0.0204(7) C2 0.0297(8) 0.0217(8) 0.0244(8) 0.0015(6) 0.0052(6) -0.0016(6) O3 0.0561(9) 0.0480(8) 0.0294(7) -0.0046(6) -0.0027(6) -0.0150(7) C3 0.0326(9) 0.0297(9) 0.0265(8) -0.0004(7) 0.0022(7) -0.0067(7) O4 0.0509(12) 0.0484(12) 0.0552(13) 0.000 0.0144(10) 0.000 C4 0.0438(10) 0.0257(8) 0.0295(9) -0.0066(7) 0.0106(8) -0.0108(8) C5 0.0404(10) 0.0191(8) 0.0361(9) -0.0024(7) 0.0150(8) -0.0023(7) C6 0.0314(9) 0.0218(8) 0.0315(9) 0.0014(7) 0.0080(7) 0.0004(7) C7 0.0342(9) 0.0229(8) 0.0339(9) -0.0068(7) 0.0042(7) -0.0014(7) C8 0.0319(9) 0.0279(9) 0.0346(9) -0.0010(7) 0.0044(7) -0.0014(7) C9 0.0336(9) 0.0245(8) 0.0310(9) 0.0006(7) 0.0072(7) -0.0042(7) C10 0.0441(12) 0.0658(15) 0.0466(12) -0.0006(11) 0.0190(10) 0.0029(11) C11 0.0635(17) 0.0646(16) 0.088(2) -0.0038(15) 0.0326(15) -0.0141(13) _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 C7 1.8084(19) . ? Mn1 C9 1.8123(19) . ? Mn1 C8 1.8125(18) . ? Mn1 P2 2.2710(7) . ? Mn1 P1 2.3361(6) . ? Mn1 P1 2.3518(7) 7 ? P1 C1 1.8264(17) . ? P1 Mn1 2.3518(7) 7 ? O1 C7 1.150(2) . ? C1 C6 1.392(2) . ? C1 C2 1.403(2) . ? P2 C2 1.8221(17) . ? O2 C8 1.147(2) . ? C2 C3 1.393(2) . ? O3 C9 1.146(2) . ? C3 C4 1.390(3) . ? O4 C10 1.421(2) 2_654 ? O4 C10 1.421(2) . ? C4 C5 1.382(3) . ? C5 C6 1.389(2) . ? C10 C11 1.496(3) . ? C11 C11 1.495(5) 2_654 ? 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 C7 Mn1 C9 89.59(8) . . ? C7 Mn1 C8 96.35(8) . . ? C9 Mn1 C8 92.49(8) . . ? C7 Mn1 P2 87.99(6) . . ? C9 Mn1 P2 173.18(6) . . ? C8 Mn1 P2 94.12(6) . . ? C7 Mn1 P1 95.50(6) . . ? C9 Mn1 P1 92.34(6) . . ? C8 Mn1 P1 167.23(6) . . ? P2 Mn1 P1 81.55(3) . . ? C7 Mn1 P1 170.66(6) . 7 ? C9 Mn1 P1 90.86(6) . 7 ? C8 Mn1 P1 92.95(6) . 7 ? P2 Mn1 P1 90.49(2) . 7 ? P1 Mn1 P1 75.16(2) . 7 ? C1 P1 Mn1 106.98(6) . . ? C1 P1 Mn1 111.67(5) . 7 ? Mn1 P1 Mn1 104.84(2) . 7 ? C6 C1 C2 119.34(15) . . ? C6 C1 P1 123.67(13) . . ? C2 C1 P1 116.93(12) . . ? C2 P2 Mn1 110.05(6) . . ? C3 C2 C1 120.55(15) . . ? C3 C2 P2 124.18(13) . . ? C1 C2 P2 115.26(12) . . ? C4 C3 C2 119.23(16) . . ? C10 O4 C10 108.8(2) 2_654 . ? C5 C4 C3 120.43(16) . . ? C4 C5 C6 120.62(16) . . ? C5 C6 C1 119.81(17) . . ? O1 C7 Mn1 178.82(16) . . ? O2 C8 Mn1 178.26(17) . . ? O3 C9 Mn1 177.15(16) . . ? O4 C10 C11 106.88(18) . . ? C11 C11 C10 102.41(16) 2_654 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.520 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.051 # Attachment 'Figure 2.CIF' data_pge0832b _database_code_depnum_ccdc_archive 'CCDC 714223' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H14 Mn2 O6 P4' _chemical_formula_sum 'C18 H14 Mn2 O6 P4' _chemical_formula_weight 560.05 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' 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 tetragonal _symmetry_space_group_name_H-M I41/a _symmetry_space_group_name_Hall -I4ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 21.6710(4) _cell_length_b 21.6710(4) _cell_length_c 19.1310(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8984.5(3) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4105 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6718 _exptl_absorpt_correction_T_max 0.7615 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8603 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5135 _reflns_number_gt 4105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0379P)^2^+16.2782P] 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 5135 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.06025(12) 0.97554(12) 0.75309(13) 0.0259(6) Uani 1 1 d . . . C2 C 1.01593(12) 0.97576(12) 0.70051(13) 0.0235(5) Uani 1 1 d . . . C3 C 1.03496(13) 0.97293(12) 0.63069(14) 0.0297(6) Uani 1 1 d . . . H3 H 1.0053 0.9743 0.5941 0.036 Uiso 1 1 calc R . . C4 C 1.09728(15) 0.96815(14) 0.61505(16) 0.0387(7) Uani 1 1 d . . . H4 H 1.1100 0.9648 0.5677 0.046 Uiso 1 1 calc R . . C5 C 1.14104(14) 0.96819(16) 0.66769(17) 0.0434(8) Uani 1 1 d . . . H5 H 1.1836 0.9655 0.6562 0.052 Uiso 1 1 calc R . . C6 C 1.12316(13) 0.97218(14) 0.73659(16) 0.0363(7) Uani 1 1 d . . . H6 H 1.1533 0.9726 0.7727 0.044 Uiso 1 1 calc R . . C7 C 0.96381(13) 1.12287(12) 0.86379(15) 0.0311(6) Uani 1 1 d . . . C8 C 1.00439(12) 1.14758(13) 0.81448(15) 0.0318(6) Uani 1 1 d . . . C9 C 1.05434(13) 1.18373(14) 0.83630(18) 0.0406(7) Uani 1 1 d . . . H9 H 1.0826 1.1998 0.8030 0.049 Uiso 1 1 calc R . . C10 C 1.06224(14) 1.19581(16) 0.90672(19) 0.0484(9) Uani 1 1 d . . . H10 H 1.0959 1.2206 0.9216 0.058 Uiso 1 1 calc R . . C11 C 1.02180(15) 1.17221(15) 0.95579(19) 0.0460(8) Uani 1 1 d . . . H11 H 1.0275 1.1812 1.0040 0.055 Uiso 1 1 calc R . . C12 C 0.97284(14) 1.13530(14) 0.93463(16) 0.0380(7) Uani 1 1 d . . . H12 H 0.9455 1.1185 0.9684 0.046 Uiso 1 1 calc R . . C13 C 0.94403(13) 0.88270(14) 0.84024(15) 0.0330(6) Uani 1 1 d . . . C14 C 0.84633(13) 0.94941(13) 0.83917(15) 0.0314(6) Uani 1 1 d . . . C15 C 0.92571(13) 0.97120(14) 0.93997(15) 0.0342(6) Uani 1 1 d . . . C16 C 0.86136(14) 1.16035(15) 0.72157(16) 0.0385(7) Uani 1 1 d . . . C17 C 0.89709(14) 1.08272(14) 0.61777(16) 0.0365(7) Uani 1 1 d . . . C18 C 0.81901(14) 1.04709(14) 0.71419(15) 0.0358(7) Uani 1 1 d . . . O1 O 0.95290(11) 0.83099(10) 0.83614(13) 0.0515(6) Uani 1 1 d . . . O2 O 0.79478(10) 0.93807(11) 0.83661(12) 0.0478(6) Uani 1 1 d . . . O3 O 0.92356(12) 0.97750(12) 0.99941(11) 0.0552(6) Uani 1 1 d . . . O4 O 0.84129(12) 1.20886(11) 0.72900(14) 0.0582(7) Uani 1 1 d . . . O5 O 0.89800(12) 1.08170(12) 0.55813(12) 0.0580(7) Uani 1 1 d . . . O6 O 0.77151(10) 1.02408(12) 0.71442(13) 0.0542(7) Uani 1 1 d . . . P1 P 1.03125(3) 0.98004(3) 0.84231(4) 0.02635(16) Uani 1 1 d . . . H1A H 1.0411 1.0211 0.8621 0.032 Uiso 1 1 calc R . . H1B H 1.0519 0.9484 0.8714 0.032 Uiso 1 1 calc R . . P2 P 0.93512(3) 0.98403(3) 0.72613(3) 0.02303(15) Uani 1 1 d . . . H2 H 0.9092 0.9536 0.6999 0.028 Uiso 1 1 calc R . . P3 P 0.90424(3) 1.06982(3) 0.83208(4) 0.02620(16) Uani 1 1 d . . . H3A H 0.8641 1.0791 0.8557 0.031 Uiso 1 1 calc R . . P4 P 0.98754(3) 1.12954(3) 0.72350(4) 0.03183(18) Uani 1 1 d . . . H4A H 1.0198 1.1016 0.7050 0.038 Uiso 1 1 calc R . . H4B H 0.9883 1.1680 0.6956 0.038 Uiso 1 1 calc R . . Mn1 Mn 0.927987(18) 0.964903(18) 0.84551(2) 0.02396(11) Uani 1 1 d . . . Mn2 Mn 0.894122(19) 1.083979(19) 0.71249(2) 0.02694(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0243(13) 0.0295(14) 0.0240(13) 0.0015(11) 0.0013(11) 0.0006(11) C2 0.0250(13) 0.0246(13) 0.0209(12) -0.0005(10) 0.0021(10) -0.0001(10) C3 0.0380(15) 0.0289(14) 0.0221(13) 0.0008(11) 0.0014(12) 0.0013(12) C4 0.0445(17) 0.0421(17) 0.0294(15) 0.0009(13) 0.0116(14) 0.0018(14) C5 0.0297(15) 0.054(2) 0.0470(19) 0.0121(16) 0.0128(14) 0.0043(14) C6 0.0248(14) 0.0498(18) 0.0343(16) 0.0084(14) -0.0012(12) 0.0017(13) C7 0.0294(14) 0.0272(14) 0.0367(16) -0.0058(12) -0.0022(12) 0.0029(11) C8 0.0277(14) 0.0283(14) 0.0394(16) -0.0078(12) -0.0041(12) 0.0016(11) C9 0.0265(15) 0.0408(17) 0.054(2) -0.0083(15) -0.0006(14) -0.0033(13) C10 0.0305(16) 0.050(2) 0.064(2) -0.0208(18) -0.0114(16) -0.0018(14) C11 0.0423(18) 0.0474(19) 0.048(2) -0.0163(16) -0.0118(16) 0.0058(15) C12 0.0386(17) 0.0385(16) 0.0370(16) -0.0086(14) -0.0032(13) 0.0032(13) C13 0.0318(15) 0.0376(17) 0.0295(15) 0.0036(13) -0.0044(12) -0.0029(12) C14 0.0313(15) 0.0291(14) 0.0338(16) 0.0075(12) 0.0025(12) 0.0015(12) C15 0.0339(16) 0.0410(17) 0.0276(15) 0.0044(13) 0.0027(12) 0.0027(13) C16 0.0358(16) 0.0408(18) 0.0388(17) 0.0008(14) -0.0091(14) 0.0036(14) C17 0.0363(16) 0.0385(16) 0.0346(17) 0.0067(13) -0.0064(13) -0.0004(13) C18 0.0335(16) 0.0385(16) 0.0354(16) 0.0097(13) -0.0062(13) 0.0036(13) O1 0.0649(16) 0.0318(12) 0.0577(15) -0.0022(11) -0.0120(13) 0.0041(11) O2 0.0296(12) 0.0515(14) 0.0624(15) 0.0192(12) 0.0004(11) -0.0070(10) O3 0.0665(16) 0.0767(18) 0.0223(11) 0.0009(11) 0.0049(11) 0.0035(13) O4 0.0628(16) 0.0390(13) 0.0728(18) -0.0109(12) -0.0225(13) 0.0171(12) O5 0.0667(17) 0.0774(18) 0.0301(13) 0.0064(12) -0.0047(12) 0.0011(14) O6 0.0318(12) 0.0646(16) 0.0662(17) 0.0283(13) -0.0143(11) -0.0105(11) P1 0.0243(3) 0.0346(4) 0.0202(3) 0.0003(3) -0.0039(3) 0.0019(3) P2 0.0218(3) 0.0271(3) 0.0202(3) -0.0012(3) -0.0036(3) -0.0012(3) P3 0.0239(3) 0.0287(4) 0.0260(4) -0.0027(3) 0.0011(3) 0.0018(3) P4 0.0312(4) 0.0303(4) 0.0340(4) 0.0033(3) 0.0011(3) -0.0038(3) Mn1 0.0240(2) 0.0281(2) 0.0198(2) 0.00120(16) 0.00042(16) -0.00019(16) Mn2 0.0254(2) 0.0285(2) 0.0269(2) 0.00273(17) -0.00434(17) 0.00149(16) _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 C1 C2 1.391(4) . ? C1 C6 1.401(4) . ? C1 P1 1.822(3) . ? C2 C3 1.399(4) . ? C2 P2 1.827(3) . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(5) . ? C4 H4 0.9500 . ? C5 C6 1.377(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.395(4) . ? C7 C8 1.397(4) . ? C7 P3 1.832(3) . ? C8 C9 1.400(4) . ? C8 P4 1.821(3) . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.382(5) . ? C10 H10 0.9500 . ? C11 C12 1.389(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 O1 1.140(4) . ? C13 Mn1 1.818(3) . ? C14 O2 1.145(3) . ? C14 Mn1 1.805(3) . ? C15 O3 1.146(4) . ? C15 Mn1 1.813(3) . ? C16 O4 1.147(4) . ? C16 Mn2 1.809(3) . ? C17 O5 1.141(4) . ? C17 Mn2 1.813(3) . ? C18 O6 1.144(4) . ? C18 Mn2 1.814(3) . ? P1 Mn1 2.2625(8) . ? P1 H1A 0.9900 . ? P1 H1B 0.9900 . ? P2 Mn1 2.3262(7) . ? P2 Mn2 2.3556(8) . ? P2 H2 1.0000 . ? P3 Mn2 2.3188(8) . ? P3 Mn1 2.3452(8) . ? P3 H3A 1.0000 . ? P4 Mn2 2.2621(8) . ? P4 H4A 0.9900 . ? P4 H4B 0.9900 . ? 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 C2 C1 C6 120.6(2) . . ? C2 C1 P1 116.06(19) . . ? C6 C1 P1 123.3(2) . . ? C1 C2 C3 119.1(2) . . ? C1 C2 P2 117.91(19) . . ? C3 C2 P2 122.9(2) . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 119.5(3) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 119.6(3) . . ? C12 C7 P3 122.8(2) . . ? C8 C7 P3 117.4(2) . . ? C7 C8 C9 120.0(3) . . ? C7 C8 P4 115.9(2) . . ? C9 C8 P4 124.1(2) . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.9(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.1(3) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? O1 C13 Mn1 178.5(3) . . ? O2 C14 Mn1 177.8(3) . . ? O3 C15 Mn1 177.4(3) . . ? O4 C16 Mn2 178.2(3) . . ? O5 C17 Mn2 178.9(3) . . ? O6 C18 Mn2 179.1(3) . . ? C1 P1 Mn1 111.03(9) . . ? C1 P1 H1A 109.4 . . ? Mn1 P1 H1A 109.4 . . ? C1 P1 H1B 109.4 . . ? Mn1 P1 H1B 109.4 . . ? H1A P1 H1B 108.0 . . ? C2 P2 Mn1 108.03(8) . . ? C2 P2 Mn2 114.96(9) . . ? Mn1 P2 Mn2 104.33(3) . . ? C2 P2 H2 109.8 . . ? Mn1 P2 H2 109.8 . . ? Mn2 P2 H2 109.8 . . ? C7 P3 Mn2 108.08(10) . . ? C7 P3 Mn1 114.67(9) . . ? Mn2 P3 Mn1 104.90(3) . . ? C7 P3 H3A 109.7 . . ? Mn2 P3 H3A 109.7 . . ? Mn1 P3 H3A 109.7 . . ? C8 P4 Mn2 111.24(10) . . ? C8 P4 H4A 109.4 . . ? Mn2 P4 H4A 109.4 . . ? C8 P4 H4B 109.4 . . ? Mn2 P4 H4B 109.4 . . ? H4A P4 H4B 108.0 . . ? C14 Mn1 C15 93.11(13) . . ? C14 Mn1 C13 90.09(13) . . ? C15 Mn1 C13 97.71(13) . . ? C14 Mn1 P1 174.09(10) . . ? C15 Mn1 P1 92.46(10) . . ? C13 Mn1 P1 87.21(9) . . ? C14 Mn1 P2 91.86(9) . . ? C15 Mn1 P2 165.24(10) . . ? C13 Mn1 P2 96.17(9) . . ? P1 Mn1 P2 83.22(3) . . ? C14 Mn1 P3 87.58(9) . . ? C15 Mn1 P3 91.73(10) . . ? C13 Mn1 P3 170.38(9) . . ? P1 Mn1 P3 94.22(3) . . ? P2 Mn1 P3 74.59(3) . . ? C16 Mn2 C17 97.10(14) . . ? C16 Mn2 C18 92.83(14) . . ? C17 Mn2 C18 92.47(14) . . ? C16 Mn2 P4 86.73(10) . . ? C17 Mn2 P4 93.89(10) . . ? C18 Mn2 P4 173.63(10) . . ? C16 Mn2 P3 93.64(10) . . ? C17 Mn2 P3 168.70(10) . . ? C18 Mn2 P3 90.51(9) . . ? P4 Mn2 P3 83.18(3) . . ? C16 Mn2 P2 168.09(10) . . ? C17 Mn2 P2 94.79(10) . . ? C18 Mn2 P2 86.06(9) . . ? P4 Mn2 P2 93.06(3) . . ? P3 Mn2 P2 74.53(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.558 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.074