# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Sullivan, Alice' _publ_contact_author_name 'Sullivan, Alice' _publ_contact_author_email a.c.sullivan@qmul.ac.uk _publ_section_title ; N-carbazolylmethylphosphonic acid - synthesis, metal coordination, emissive aggregate formation and spectroscopic features. ; # Attachment '- mncarmp.cif' data_mncarmp _database_code_depnum_ccdc_archive 'CCDC 779813' #TrackingRef '- mncarmp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H24 Mn N2 O7 P2' _chemical_formula_weight 593.35 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.373(2) _cell_length_b 4.7525(4) _cell_length_c 29.191(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.101(3) _cell_angle_gamma 90.00 _cell_volume 2436.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5633 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8337 _exptl_absorpt_correction_T_max 0.9928 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M.,2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_reflns_number 18437 _diffrn_reflns_av_R_equivalents 0.1148 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3445 _reflns_number_gt 2641 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) &PLUTON (Spek,A.L.,1990)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0000P)^2^+23.2487P] 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 3445 _refine_ls_number_parameters 359 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1167 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.003 _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 0.6345(4) 0.7466(15) 0.3624(3) 0.0164(18) Uani 1 1 d . . . C2 C 0.5646(5) 0.7127(16) 0.3290(3) 0.024(2) Uani 1 1 d . . . H2 H 0.5217 0.8211 0.3300 0.029 Uiso 1 1 calc R . . C3 C 0.5600(5) 0.5110(18) 0.2936(3) 0.027(2) Uani 1 1 d . . . H3 H 0.5123 0.4777 0.2703 0.033 Uiso 1 1 calc R . . C4 C 0.6222(5) 0.3598(18) 0.2914(3) 0.028(2) Uani 1 1 d . . . H4 H 0.6170 0.2267 0.2663 0.033 Uiso 1 1 calc R . . C5 C 0.6919(5) 0.3960(17) 0.3244(3) 0.027(2) Uani 1 1 d . . . H5 H 0.7344 0.2876 0.3226 0.033 Uiso 1 1 calc R . . C6 C 0.6996(5) 0.5955(16) 0.3609(3) 0.023(2) Uani 1 1 d . . . C7 C 0.7627(5) 0.6926(17) 0.4006(3) 0.024(2) Uani 1 1 d . . . C8 C 0.8396(5) 0.6270(19) 0.4174(3) 0.031(2) Uani 1 1 d . . . H8 H 0.8603 0.4844 0.4021 0.037 Uiso 1 1 calc R . . C9 C 0.8858(5) 0.769(2) 0.4561(3) 0.038(2) Uani 1 1 d . . . H9 H 0.9387 0.7266 0.4672 0.046 Uiso 1 1 calc R . . C10 C 0.8551(5) 0.974(2) 0.4789(3) 0.036(2) Uani 1 1 d . . . H10 H 0.8879 1.0696 0.5057 0.043 Uiso 1 1 calc R . . C11 C 0.7785(5) 1.0434(19) 0.4641(3) 0.029(2) Uani 1 1 d . . . H11 H 0.7583 1.1831 0.4802 0.035 Uiso 1 1 calc R . . C12 C 0.7322(5) 0.8997(17) 0.4245(3) 0.026(2) Uani 1 1 d . . . C13 C 0.6048(5) 1.1252(16) 0.4152(3) 0.0198(19) Uani 1 1 d . . . H13A H 0.5657 1.1877 0.3857 0.024 Uiso 1 1 calc R . . H13B H 0.6349 1.2928 0.4295 0.024 Uiso 1 1 calc R . . C14 C 0.8310(4) 0.5888(15) 0.6569(3) 0.0180(19) Uani 1 1 d . . . C15 C 0.8172(5) 0.6559(18) 0.6092(3) 0.026(2) Uani 1 1 d . . . H15 H 0.7793 0.7898 0.5942 0.032 Uiso 1 1 calc R . . C16 C 0.8597(5) 0.5240(19) 0.5840(3) 0.030(2) Uani 1 1 d . . . H16 H 0.8518 0.5717 0.5513 0.037 Uiso 1 1 calc R . . C17 C 0.9143(5) 0.3213(17) 0.6052(3) 0.029(2) Uani 1 1 d . . . H17 H 0.9424 0.2307 0.5868 0.035 Uiso 1 1 calc R . . C18 C 0.9277(4) 0.2522(17) 0.6533(3) 0.025(2) Uani 1 1 d . . . H18 H 0.9653 0.1166 0.6680 0.030 Uiso 1 1 calc R . . C19 C 0.8851(4) 0.3842(17) 0.6800(3) 0.022(2) Uani 1 1 d . . . C20 C 0.8851(4) 0.3727(16) 0.7287(3) 0.0199(19) Uani 1 1 d . . . C21 C 0.9271(5) 0.2160(17) 0.7689(3) 0.027(2) Uani 1 1 d . . . H21 H 0.9638 0.0815 0.7660 0.033 Uiso 1 1 calc R . . C22 C 0.9142(5) 0.2612(18) 0.8119(3) 0.029(2) Uani 1 1 d . . . H22 H 0.9424 0.1563 0.8390 0.035 Uiso 1 1 calc R . . C23 C 0.8609(5) 0.4572(17) 0.8172(3) 0.026(2) Uani 1 1 d . . . H23 H 0.8537 0.4846 0.8478 0.032 Uiso 1 1 calc R . . C24 C 0.8184(5) 0.6121(17) 0.7786(3) 0.027(2) Uani 1 1 d . . . H24 H 0.7819 0.7456 0.7822 0.032 Uiso 1 1 calc R . . C25 C 0.8304(4) 0.5669(16) 0.7345(3) 0.022(2) Uani 1 1 d . . . C26 C 0.7406(4) 0.9186(16) 0.6822(3) 0.026(2) Uani 1 1 d . . . H26A H 0.7533 1.0633 0.6613 0.031 Uiso 1 1 calc R . . H26B H 0.7433 1.0088 0.7132 0.031 Uiso 1 1 calc R . . Mn1 Mn 0.58071(7) 0.5128(2) 0.54004(4) 0.0162(3) Uani 1 1 d . . . N1 N 0.6549(4) 0.9287(13) 0.4016(2) 0.0188(16) Uani 1 1 d . . . N2 N 0.7974(4) 0.6950(13) 0.6905(2) 0.0227(16) Uani 1 1 d . . . O1 O 0.4885(3) 0.8082(10) 0.42782(18) 0.0168(12) Uani 1 1 d D . . O2 O 0.5271(3) 1.2586(10) 0.47596(18) 0.0166(12) Uani 1 1 d . . . O3 O 0.6111(3) 0.8214(10) 0.49439(16) 0.0136(12) Uani 1 1 d . . . O4 O 0.6809(3) 0.2470(12) 0.5515(2) 0.0285(14) Uani 1 1 d D . . O5 O 0.5938(3) 1.0558(10) 0.65260(18) 0.0190(12) Uani 1 1 d . . . O6 O 0.6284(3) 0.5759(10) 0.68974(19) 0.0208(13) Uani 1 1 d D . . O7 O 0.6368(3) 0.6692(11) 0.60686(18) 0.0207(13) Uani 1 1 d . . . P1 P 0.55677(11) 0.9986(4) 0.45651(7) 0.0152(5) Uani 1 1 d . . . P2 P 0.64427(12) 0.7979(4) 0.65459(7) 0.0178(5) Uani 1 1 d . . . H41W H 0.669(4) 0.081(11) 0.540(3) 0.03(3) Uiso 1 1 d D . . H42W H 0.728(3) 0.27(2) 0.565(4) 0.11(5) Uiso 1 1 d D . . H61 H 0.615(7) 0.404(14) 0.677(4) 0.10(5) Uiso 1 1 d D . . H71 H 0.460(4) 0.859(18) 0.397(2) 0.04(3) Uiso 1 1 d 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 0.026(5) 0.010(4) 0.015(4) 0.001(3) 0.010(4) 0.003(4) C2 0.030(5) 0.020(4) 0.026(5) 0.003(4) 0.017(4) 0.006(4) C3 0.029(5) 0.022(5) 0.029(5) -0.003(4) 0.007(4) 0.003(4) C4 0.045(6) 0.025(5) 0.015(5) -0.002(4) 0.013(4) -0.006(5) C5 0.037(6) 0.023(5) 0.028(5) 0.005(4) 0.021(5) 0.007(4) C6 0.031(5) 0.020(4) 0.022(5) 0.002(4) 0.014(4) 0.004(4) C7 0.032(5) 0.022(5) 0.022(5) 0.006(4) 0.012(4) 0.004(4) C8 0.027(5) 0.037(5) 0.027(5) -0.001(4) 0.006(4) 0.008(4) C9 0.027(5) 0.054(7) 0.033(6) 0.009(5) 0.007(4) -0.005(5) C10 0.030(5) 0.044(6) 0.031(5) 0.006(5) 0.004(4) -0.004(5) C11 0.035(5) 0.036(5) 0.020(5) -0.001(4) 0.015(4) -0.002(4) C12 0.030(5) 0.025(5) 0.024(5) 0.008(4) 0.011(4) 0.003(4) C13 0.030(5) 0.020(4) 0.015(4) 0.003(3) 0.015(4) 0.007(4) C14 0.015(4) 0.018(4) 0.025(5) -0.001(4) 0.013(4) -0.003(3) C15 0.017(5) 0.037(5) 0.021(5) -0.002(4) -0.001(4) 0.001(4) C16 0.028(5) 0.035(5) 0.031(5) 0.001(5) 0.014(4) -0.007(5) C17 0.026(5) 0.027(5) 0.038(6) -0.017(4) 0.015(4) -0.006(4) C18 0.013(5) 0.028(5) 0.032(5) -0.003(4) 0.004(4) 0.004(4) C19 0.018(5) 0.024(5) 0.024(5) 0.000(4) 0.006(4) -0.002(4) C20 0.014(5) 0.021(4) 0.023(5) -0.004(4) 0.003(4) -0.006(4) C21 0.023(5) 0.023(5) 0.035(6) 0.003(4) 0.006(4) -0.006(4) C22 0.023(5) 0.030(5) 0.030(6) 0.002(4) 0.001(4) -0.005(4) C23 0.029(5) 0.030(5) 0.021(5) 0.003(4) 0.008(4) -0.012(4) C24 0.023(5) 0.023(5) 0.035(6) -0.004(4) 0.010(4) -0.006(4) C25 0.022(5) 0.020(5) 0.023(5) 0.004(4) 0.005(4) -0.004(4) C26 0.023(5) 0.017(4) 0.034(5) 0.002(4) 0.004(4) 0.004(4) Mn1 0.0210(7) 0.0122(6) 0.0150(6) -0.0001(5) 0.0048(5) 0.0005(6) N1 0.024(4) 0.021(4) 0.015(4) 0.004(3) 0.012(3) 0.005(3) N2 0.022(4) 0.017(4) 0.025(4) -0.002(3) 0.000(3) 0.004(3) O1 0.021(3) 0.016(3) 0.011(3) 0.002(2) 0.003(2) -0.005(2) O2 0.020(3) 0.010(3) 0.021(3) -0.003(2) 0.008(2) 0.001(2) O3 0.021(3) 0.009(3) 0.009(3) 0.000(2) 0.002(2) -0.002(2) O4 0.023(4) 0.021(3) 0.037(4) -0.010(3) 0.002(3) 0.000(3) O5 0.019(3) 0.012(3) 0.022(3) -0.003(2) -0.002(2) 0.006(2) O6 0.031(3) 0.013(3) 0.020(3) 0.000(2) 0.009(3) -0.003(2) O7 0.024(3) 0.021(3) 0.014(3) -0.001(2) 0.001(2) 0.002(3) P1 0.0229(12) 0.0099(10) 0.0139(11) -0.0005(9) 0.0071(8) -0.0004(10) P2 0.0211(12) 0.0137(11) 0.0174(12) 0.0014(9) 0.0038(9) 0.0004(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.374(11) . ? C1 N1 1.395(9) . ? C1 C6 1.408(11) . ? C2 C3 1.395(11) . ? C2 H2 0.9500 . ? C3 C4 1.368(11) . ? C3 H3 0.9500 . ? C4 C5 1.368(12) . ? C4 H4 0.9500 . ? C5 C6 1.402(11) . ? C5 H5 0.9500 . ? C6 C7 1.455(12) . ? C7 C8 1.388(11) . ? C7 C12 1.412(11) . ? C8 C9 1.373(12) . ? C8 H8 0.9500 . ? C9 C10 1.391(13) . ? C9 H9 0.9500 . ? C10 C11 1.386(12) . ? C10 H10 0.9500 . ? C11 C12 1.397(12) . ? C11 H11 0.9500 . ? C12 N1 1.387(10) . ? C13 N1 1.447(9) . ? C13 P1 1.794(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.376(11) . ? C14 N2 1.398(10) . ? C14 C19 1.412(11) . ? C15 C16 1.373(11) . ? C15 H15 0.9500 . ? C16 C17 1.397(12) . ? C16 H16 0.9500 . ? C17 C18 1.394(12) . ? C17 H17 0.9500 . ? C18 C19 1.403(11) . ? C18 H18 0.9500 . ? C19 C20 1.422(11) . ? C20 C25 1.411(11) . ? C20 C21 1.413(11) . ? C21 C22 1.362(12) . ? C21 H21 0.9500 . ? C22 C23 1.393(12) . ? C22 H22 0.9500 . ? C23 C24 1.379(11) . ? C23 H23 0.9500 . ? C24 C25 1.386(11) . ? C24 H24 0.9500 . ? C25 N2 1.389(10) . ? C26 N2 1.459(10) . ? C26 P2 1.809(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? Mn1 O7 2.058(5) . ? Mn1 O3 2.162(5) . ? Mn1 O4 2.176(6) . ? Mn1 O2 2.185(5) 3_676 ? Mn1 O2 2.201(5) 1_545 ? Mn1 O1 2.351(5) 3_666 ? Mn1 Mn1 3.193(2) 3_666 ? O1 P1 1.573(5) . ? O1 Mn1 2.351(5) 3_666 ? O1 H71 0.94(5) . ? O2 P1 1.526(5) . ? O2 Mn1 2.185(5) 3_676 ? O2 Mn1 2.201(5) 1_565 ? O3 P1 1.510(5) . ? O4 H41W 0.86(4) . ? O4 H42W 0.85(5) . ? O5 P2 1.527(5) . ? O6 P2 1.558(5) . ? O6 H61 0.90(5) . ? O7 P2 1.491(5) . ? 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 N1 128.7(7) . . ? C2 C1 C6 122.8(7) . . ? N1 C1 C6 108.5(7) . . ? C1 C2 C3 116.6(8) . . ? C1 C2 H2 121.7 . . ? C3 C2 H2 121.7 . . ? C4 C3 C2 121.8(8) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 121.5(8) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C4 C5 C6 119.0(8) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C5 C6 C1 118.2(8) . . ? C5 C6 C7 134.4(8) . . ? C1 C6 C7 107.3(7) . . ? C8 C7 C12 119.6(8) . . ? C8 C7 C6 134.4(8) . . ? C12 C7 C6 106.0(7) . . ? C9 C8 C7 119.8(8) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.9(9) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 122.3(9) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 117.2(8) . . ? C10 C11 H11 121.4 . . ? C12 C11 H11 121.4 . . ? N1 C12 C11 129.6(8) . . ? N1 C12 C7 109.3(7) . . ? C11 C12 C7 121.0(8) . . ? N1 C13 P1 116.5(5) . . ? N1 C13 H13A 108.2 . . ? P1 C13 H13A 108.2 . . ? N1 C13 H13B 108.2 . . ? P1 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? C15 C14 N2 129.6(7) . . ? C15 C14 C19 122.5(7) . . ? N2 C14 C19 107.9(7) . . ? C16 C15 C14 118.1(8) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C15 C16 C17 121.7(8) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C18 119.9(8) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 119.5(8) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C14 118.2(7) . . ? C18 C19 C20 134.5(8) . . ? C14 C19 C20 107.3(7) . . ? C25 C20 C19 107.8(7) . . ? C25 C20 C21 118.6(8) . . ? C19 C20 C21 133.6(8) . . ? C22 C21 C20 118.8(8) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 121.8(8) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C24 C23 C22 121.0(8) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 118.0(8) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? N2 C25 C24 130.3(8) . . ? N2 C25 C20 107.9(7) . . ? C24 C25 C20 121.8(7) . . ? N2 C26 P2 113.7(5) . . ? N2 C26 H26A 108.8 . . ? P2 C26 H26A 108.8 . . ? N2 C26 H26B 108.8 . . ? P2 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? O7 Mn1 O3 101.0(2) . . ? O7 Mn1 O4 84.1(2) . . ? O3 Mn1 O4 97.4(2) . . ? O7 Mn1 O2 101.1(2) . 3_676 ? O3 Mn1 O2 85.00(19) . 3_676 ? O4 Mn1 O2 173.7(2) . 3_676 ? O7 Mn1 O2 167.9(2) . 1_545 ? O3 Mn1 O2 88.90(18) . 1_545 ? O4 Mn1 O2 87.7(2) . 1_545 ? O2 Mn1 O2 86.57(19) 3_676 1_545 ? O7 Mn1 O1 92.0(2) . 3_666 ? O3 Mn1 O1 162.55(18) . 3_666 ? O4 Mn1 O1 95.4(2) . 3_666 ? O2 Mn1 O1 81.10(19) 3_676 3_666 ? O2 Mn1 O1 79.82(18) 1_545 3_666 ? O7 Mn1 Mn1 143.71(16) . 3_666 ? O3 Mn1 Mn1 85.82(13) . 3_666 ? O4 Mn1 Mn1 130.73(17) . 3_666 ? O2 Mn1 Mn1 43.48(13) 3_676 3_666 ? O2 Mn1 Mn1 43.09(13) 1_545 3_666 ? O1 Mn1 Mn1 76.84(13) 3_666 3_666 ? C12 N1 C1 108.9(6) . . ? C12 N1 C13 125.3(7) . . ? C1 N1 C13 125.8(6) . . ? C25 N2 C14 109.2(6) . . ? C25 N2 C26 124.7(7) . . ? C14 N2 C26 126.0(7) . . ? P1 O1 Mn1 126.9(3) . 3_666 ? P1 O1 H71 120(5) . . ? Mn1 O1 H71 110(5) 3_666 . ? P1 O2 Mn1 136.4(3) . 3_676 ? P1 O2 Mn1 129.8(3) . 1_565 ? Mn1 O2 Mn1 93.43(18) 3_676 1_565 ? P1 O3 Mn1 126.5(3) . . ? Mn1 O4 H41W 112(5) . . ? Mn1 O4 H42W 134(7) . . ? H41W O4 H42W 114(7) . . ? P2 O6 H61 115(8) . . ? P2 O7 Mn1 156.4(3) . . ? O3 P1 O2 114.3(3) . . ? O3 P1 O1 108.7(3) . . ? O2 P1 O1 110.3(3) . . ? O3 P1 C13 109.3(3) . . ? O2 P1 C13 106.2(3) . . ? O1 P1 C13 107.9(3) . . ? O7 P2 O5 114.0(3) . . ? O7 P2 O6 110.7(3) . . ? O5 P2 O6 109.8(3) . . ? O7 P2 C26 110.8(4) . . ? O5 P2 C26 105.4(3) . . ? O6 P2 C26 105.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -179.3(7) . . . . ? C6 C1 C2 C3 2.2(12) . . . . ? C1 C2 C3 C4 -1.7(12) . . . . ? C2 C3 C4 C5 1.1(13) . . . . ? C3 C4 C5 C6 -0.9(12) . . . . ? C4 C5 C6 C1 1.3(12) . . . . ? C4 C5 C6 C7 -179.0(9) . . . . ? C2 C1 C6 C5 -2.0(12) . . . . ? N1 C1 C6 C5 179.2(7) . . . . ? C2 C1 C6 C7 178.2(7) . . . . ? N1 C1 C6 C7 -0.6(9) . . . . ? C5 C6 C7 C8 0.8(17) . . . . ? C1 C6 C7 C8 -179.4(9) . . . . ? C5 C6 C7 C12 -179.8(9) . . . . ? C1 C6 C7 C12 -0.1(9) . . . . ? C12 C7 C8 C9 -1.7(13) . . . . ? C6 C7 C8 C9 177.6(9) . . . . ? C7 C8 C9 C10 1.2(14) . . . . ? C8 C9 C10 C11 -0.1(14) . . . . ? C9 C10 C11 C12 -0.5(13) . . . . ? C10 C11 C12 N1 -178.9(8) . . . . ? C10 C11 C12 C7 -0.1(12) . . . . ? C8 C7 C12 N1 -179.8(7) . . . . ? C6 C7 C12 N1 0.7(9) . . . . ? C8 C7 C12 C11 1.2(12) . . . . ? C6 C7 C12 C11 -178.3(7) . . . . ? N2 C14 C15 C16 178.5(8) . . . . ? C19 C14 C15 C16 -2.1(12) . . . . ? C14 C15 C16 C17 1.7(13) . . . . ? C15 C16 C17 C18 -1.1(13) . . . . ? C16 C17 C18 C19 1.0(12) . . . . ? C17 C18 C19 C14 -1.4(12) . . . . ? C17 C18 C19 C20 -177.6(9) . . . . ? C15 C14 C19 C18 2.0(12) . . . . ? N2 C14 C19 C18 -178.5(7) . . . . ? C15 C14 C19 C20 179.2(7) . . . . ? N2 C14 C19 C20 -1.3(9) . . . . ? C18 C19 C20 C25 177.3(9) . . . . ? C14 C19 C20 C25 0.8(9) . . . . ? C18 C19 C20 C21 -2.1(16) . . . . ? C14 C19 C20 C21 -178.6(8) . . . . ? C25 C20 C21 C22 -1.0(11) . . . . ? C19 C20 C21 C22 178.3(9) . . . . ? C20 C21 C22 C23 0.0(12) . . . . ? C21 C22 C23 C24 0.6(13) . . . . ? C22 C23 C24 C25 -0.1(12) . . . . ? C23 C24 C25 N2 -178.4(8) . . . . ? C23 C24 C25 C20 -1.0(12) . . . . ? C19 C20 C25 N2 0.0(9) . . . . ? C21 C20 C25 N2 179.5(7) . . . . ? C19 C20 C25 C24 -177.9(7) . . . . ? C21 C20 C25 C24 1.6(12) . . . . ? C11 C12 N1 C1 177.8(8) . . . . ? C7 C12 N1 C1 -1.1(9) . . . . ? C11 C12 N1 C13 0.2(13) . . . . ? C7 C12 N1 C13 -178.6(7) . . . . ? C2 C1 N1 C12 -177.6(8) . . . . ? C6 C1 N1 C12 1.1(8) . . . . ? C2 C1 N1 C13 -0.1(12) . . . . ? C6 C1 N1 C13 178.6(7) . . . . ? P1 C13 N1 C12 -91.8(8) . . . . ? P1 C13 N1 C1 91.1(8) . . . . ? C24 C25 N2 C14 176.8(8) . . . . ? C20 C25 N2 C14 -0.8(8) . . . . ? C24 C25 N2 C26 0.6(13) . . . . ? C20 C25 N2 C26 -177.0(7) . . . . ? C15 C14 N2 C25 -179.2(8) . . . . ? C19 C14 N2 C25 1.3(8) . . . . ? C15 C14 N2 C26 -3.1(13) . . . . ? C19 C14 N2 C26 177.5(7) . . . . ? P2 C26 N2 C25 -101.2(8) . . . . ? P2 C26 N2 C14 83.2(9) . . . . ? O7 Mn1 O3 P1 -122.0(3) . . . . ? O4 Mn1 O3 P1 152.6(3) . . . . ? O2 Mn1 O3 P1 -21.6(3) 3_676 . . . ? O2 Mn1 O3 P1 65.0(3) 1_545 . . . ? O1 Mn1 O3 P1 15.6(9) 3_666 . . . ? Mn1 Mn1 O3 P1 22.0(3) 3_666 . . . ? O3 Mn1 O7 P2 113.0(8) . . . . ? O4 Mn1 O7 P2 -150.6(9) . . . . ? O2 Mn1 O7 P2 26.0(9) 3_676 . . . ? O2 Mn1 O7 P2 -102.7(12) 1_545 . . . ? O1 Mn1 O7 P2 -55.4(9) 3_666 . . . ? Mn1 Mn1 O7 P2 14.9(10) 3_666 . . . ? Mn1 O3 P1 O2 81.4(4) . . . . ? Mn1 O3 P1 O1 -42.3(4) . . . . ? Mn1 O3 P1 C13 -159.9(4) . . . . ? Mn1 O2 P1 O3 -142.5(4) 3_676 . . . ? Mn1 O2 P1 O3 28.7(5) 1_565 . . . ? Mn1 O2 P1 O1 -19.6(5) 3_676 . . . ? Mn1 O2 P1 O1 151.6(3) 1_565 . . . ? Mn1 O2 P1 C13 97.0(5) 3_676 . . . ? Mn1 O2 P1 C13 -91.8(4) 1_565 . . . ? Mn1 O1 P1 O3 45.8(4) 3_666 . . . ? Mn1 O1 P1 O2 -80.3(4) 3_666 . . . ? Mn1 O1 P1 C13 164.1(4) 3_666 . . . ? N1 C13 P1 O3 40.4(7) . . . . ? N1 C13 P1 O2 164.1(6) . . . . ? N1 C13 P1 O1 -77.6(6) . . . . ? Mn1 O7 P2 O5 -47.3(9) . . . . ? Mn1 O7 P2 O6 77.1(9) . . . . ? Mn1 O7 P2 C26 -166.0(8) . . . . ? N2 C26 P2 O7 -60.5(7) . . . . ? N2 C26 P2 O5 175.8(6) . . . . ? N2 C26 P2 O6 59.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.506 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.108