# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Taylor, Stephanie' 'McIntosh, Ruaraidh' 'Beavers, Christine' 'Teat, Simon' 'Piligkos, Stergios' 'Dalgarno, Scott' 'Brechin, Euan' _publ_contact_author_name 'Dalgarno, Scott' _publ_contact_author_email S.J.Dalgarno@hw.ac.uk _publ_section_title ; Calix[4]arene supported clusters: A dimer of [MnIII2MnII2] dimers ; # Attachment '- CC.CIF' data_MnPhos _database_code_depnum_ccdc_archive 'CCDC 797183' #TrackingRef '- CC.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Mn2PhosphinateTBC4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H162 Mn4 N4 O20 P2' _chemical_formula_weight 2202.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 '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 0.2237 0.8587 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1013 0.1134 '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 12.5734(7) _cell_length_b 13.2559(8) _cell_length_c 20.3034(12) _cell_angle_alpha 74.747(2) _cell_angle_beta 73.160(2) _cell_angle_gamma 64.054(2) _cell_volume 2875.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3945 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 24.00 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9372 _exptl_absorpt_correction_T_max 0.9617 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker Apex II CCD ' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21865 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _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 3.21 _diffrn_reflns_theta_max 24.08 _reflns_number_total 7023 _reflns_number_gt 4662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. One ligand on Mn2 was found to be a partial occupancy MeOH 0.5 (refined) and partial occupancy H2O. This disorder was modelled successfully. Restratints were applied due to this disorder, and also to the thermal parameters of the phenyl ring of the phosphinate ligand. Disorder could not be modelled in this case. The crystals were found to be weakly diffracting, even with synchrotron radiation and long exposure, with drop off in diffraction beyond 0.95 A resolution. The absence of H atoms on the MeOH and H2O ligands accounts for the difference in reported and calculated formulae. These could not be located. ; _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^)+(0.1187P)^2^+8.4442P] 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 7023 _refine_ls_number_parameters 637 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2247 _refine_ls_wR_factor_gt 0.1962 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.79195(9) 0.19168(10) 0.14577(5) 0.0286(4) Uani 1 1 d . . . P1 P 1.01529(18) 0.17612(19) 0.00632(10) 0.0343(6) Uani 1 1 d D . . O1 O 0.8597(4) 0.2878(4) 0.1566(2) 0.0301(12) Uani 1 1 d . . . N1 N 0.5644(5) 0.1929(5) 0.3637(3) 0.0290(15) Uani 1 1 d . . . C1 C 0.7293(6) 0.4272(6) 0.2299(4) 0.0275(18) Uani 1 1 d . A . Mn2 Mn 0.79120(10) 0.08846(10) 0.01479(5) 0.0300(4) Uani 1 1 d . . . O2 O 0.9295(4) 0.0571(4) 0.1710(2) 0.0303(12) Uani 1 1 d . . . N2 N 0.6366(5) -0.1311(5) 0.0183(3) 0.0353(16) Uani 1 1 d . A . C2 C 0.7035(6) 0.4653(7) 0.2934(4) 0.0301(19) Uani 1 1 d . . . H2 H 0.6362 0.5342 0.3017 0.036 Uiso 1 1 calc R . . O3 O 0.7269(4) 0.0968(4) 0.1250(2) 0.0289(12) Uani 1 1 d . A . C3 C 0.7721(6) 0.4065(7) 0.3443(4) 0.0312(19) Uani 1 1 d . . . O4 O 0.6604(4) 0.3212(4) 0.1113(2) 0.0299(12) Uani 1 1 d . A . C4 C 0.8674(6) 0.3035(7) 0.3308(4) 0.0314(19) Uani 1 1 d . . . H4 H 0.9151 0.2609 0.3652 0.038 Uiso 1 1 calc R . . O5 O 0.6808(4) 0.1813(4) 0.2545(2) 0.0289(12) Uani 1 1 d . . . C5 C 0.8959(6) 0.2605(6) 0.2706(4) 0.0276(18) Uani 1 1 d . . . O6 O 0.8909(4) 0.1728(4) 0.0349(2) 0.0286(12) Uani 1 1 d . A . C6 C 0.8285(6) 0.3247(6) 0.2182(4) 0.0269(18) Uani 1 1 d . . . O7 O 1.1038(4) 0.0859(5) -0.0368(2) 0.0350(13) Uani 1 1 d . . . C7 C 0.9951(6) 0.1447(6) 0.2613(4) 0.0317(19) Uani 1 1 d . . . H7A H 1.0568 0.1296 0.2877 0.038 Uiso 1 1 calc R . . H7B H 1.0344 0.1449 0.2114 0.038 Uiso 1 1 calc R . . O8 O 0.6496(4) 0.0375(5) 0.0093(3) 0.0370(14) Uani 1 1 d . A . C8 C 0.9485(6) 0.0491(6) 0.2860(4) 0.0282(18) Uani 1 1 d . . . O9 O 0.8713(5) 0.0834(5) -0.0979(3) 0.0447(15) Uani 1 1 d . A . C9 C 0.9326(6) 0.0014(7) 0.3558(4) 0.0321(19) Uani 1 1 d . . . H9 H 0.9546 0.0271 0.3874 0.039 Uiso 1 1 calc R . . O10 O 0.6652(5) 0.2676(5) -0.0115(3) 0.0513(16) Uani 0.50 1 d P A 1 C10 C 0.8855(6) -0.0828(6) 0.3819(4) 0.0304(19) Uani 1 1 d . . . C11 C 0.8562(6) -0.1187(7) 0.3337(4) 0.0302(18) Uani 1 1 d . . . H11 H 0.8255 -0.1768 0.3498 0.036 Uiso 1 1 calc R . . C12 C 0.8693(6) -0.0745(6) 0.2633(4) 0.0277(18) Uani 1 1 d . . . C13 C 0.9165(6) 0.0113(6) 0.2391(4) 0.0290(18) Uani 1 1 d . . . C14 C 0.8323(6) -0.1133(7) 0.2126(4) 0.0328(19) Uani 1 1 d . . . H14A H 0.8533 -0.1962 0.2252 0.039 Uiso 1 1 calc R . . H14B H 0.8783 -0.0988 0.1650 0.039 Uiso 1 1 calc R . . C15 C 0.6974(6) -0.0528(6) 0.2124(4) 0.0258(18) Uani 1 1 d . A . C16 C 0.6184(6) -0.1022(6) 0.2541(3) 0.0273(18) Uani 1 1 d . . . H16 H 0.6508 -0.1759 0.2800 0.033 Uiso 1 1 calc R . . C17 C 0.4913(6) -0.0477(6) 0.2597(4) 0.0266(18) Uani 1 1 d . . . C18 C 0.4488(6) 0.0606(6) 0.2222(4) 0.0266(18) Uani 1 1 d . . . H18 H 0.3641 0.1005 0.2259 0.032 Uiso 1 1 calc R . . C19 C 0.5245(6) 0.1145(6) 0.1793(4) 0.0256(17) Uani 1 1 d . A . C20 C 0.6509(6) 0.0536(6) 0.1721(3) 0.0240(17) Uani 1 1 d . . . C21 C 0.4728(6) 0.2333(6) 0.1405(4) 0.0294(18) Uani 1 1 d . . . H21A H 0.3912 0.2479 0.1352 0.035 Uiso 1 1 calc R A . H21B H 0.5236 0.2364 0.0931 0.035 Uiso 1 1 calc R . . C22 C 0.4627(6) 0.3289(6) 0.1732(3) 0.0238(17) Uani 1 1 d . A . C23 C 0.3567(6) 0.3829(6) 0.2190(3) 0.0269(18) Uani 1 1 d . . . H23 H 0.2926 0.3580 0.2291 0.032 Uiso 1 1 calc R A . C24 C 0.3404(6) 0.4711(6) 0.2506(4) 0.0301(18) Uani 1 1 d . A . C25 C 0.4364(6) 0.5048(6) 0.2354(4) 0.0265(17) Uani 1 1 d . . . H25 H 0.4276 0.5646 0.2566 0.032 Uiso 1 1 calc R A . C26 C 0.5444(6) 0.4549(6) 0.1906(3) 0.0246(17) Uani 1 1 d . A . C27 C 0.5566(6) 0.3672(6) 0.1578(3) 0.0287(18) Uani 1 1 d . . . C28 C 0.6483(6) 0.4922(6) 0.1774(4) 0.0287(18) Uani 1 1 d . . . H28A H 0.6968 0.4803 0.1299 0.034 Uiso 1 1 calc R A . H28B H 0.6152 0.5744 0.1795 0.034 Uiso 1 1 calc R . . C29 C 0.7472(7) 0.4532(8) 0.4116(4) 0.041(2) Uani 1 1 d . . . C30 C 0.6282(9) 0.5500(9) 0.4236(5) 0.084(4) Uani 1 1 d . . . H30A H 0.6144 0.5717 0.4689 0.127 Uiso 1 1 calc R . . H30B H 0.5640 0.5271 0.4234 0.127 Uiso 1 1 calc R . . H30C H 0.6278 0.6147 0.3866 0.127 Uiso 1 1 calc R . . C31 C 0.8515(10) 0.4782(10) 0.4123(5) 0.073(3) Uani 1 1 d . . . H31A H 0.8549 0.5429 0.3761 0.110 Uiso 1 1 calc R . . H31B H 0.9265 0.4115 0.4034 0.110 Uiso 1 1 calc R . . H31C H 0.8415 0.4967 0.4580 0.110 Uiso 1 1 calc R . . C32 C 0.7385(10) 0.3580(9) 0.4766(5) 0.065(3) Uani 1 1 d . . . H32A H 0.8140 0.2904 0.4724 0.098 Uiso 1 1 calc R . . H32B H 0.6712 0.3382 0.4781 0.098 Uiso 1 1 calc R . . H32C H 0.7249 0.3865 0.5195 0.098 Uiso 1 1 calc R . . C33 C 0.8649(7) -0.1347(7) 0.4595(4) 0.037(2) Uani 1 1 d . . . C34 C 0.9050(10) -0.0894(10) 0.5045(5) 0.074(3) Uani 1 1 d . . . H34A H 0.8973 -0.1309 0.5521 0.111 Uiso 1 1 calc R . . H34B H 0.8543 -0.0084 0.5049 0.111 Uiso 1 1 calc R . . H34C H 0.9895 -0.0992 0.4857 0.111 Uiso 1 1 calc R . . C35 C 0.9224(12) -0.2611(9) 0.4702(5) 0.087(4) Uani 1 1 d . . . H35A H 1.0104 -0.2856 0.4563 0.130 Uiso 1 1 calc R . . H35B H 0.8940 -0.2900 0.4419 0.130 Uiso 1 1 calc R . . H35C H 0.9009 -0.2910 0.5195 0.130 Uiso 1 1 calc R . . C36 C 0.7274(9) -0.1026(10) 0.4865(5) 0.071(3) Uani 1 1 d . . . H36A H 0.6961 -0.1259 0.4567 0.107 Uiso 1 1 calc R . . H36B H 0.6865 -0.0202 0.4855 0.107 Uiso 1 1 calc R . . H36C H 0.7127 -0.1413 0.5344 0.107 Uiso 1 1 calc R . . C37 C 0.4108(6) -0.1084(6) 0.3068(4) 0.0297(18) Uani 1 1 d . . . C38 C 0.4303(7) -0.1385(7) 0.3822(4) 0.039(2) Uani 1 1 d . . . H38A H 0.5161 -0.1838 0.3827 0.059 Uiso 1 1 calc R . . H38B H 0.3828 -0.1824 0.4110 0.059 Uiso 1 1 calc R . . H38C H 0.4045 -0.0685 0.4009 0.059 Uiso 1 1 calc R . . C39 C 0.4434(7) -0.2184(6) 0.2800(4) 0.040(2) Uani 1 1 d . . . H39A H 0.4181 -0.1997 0.2354 0.059 Uiso 1 1 calc R . . H39B H 0.4020 -0.2640 0.3140 0.059 Uiso 1 1 calc R . . H39C H 0.5309 -0.2618 0.2734 0.059 Uiso 1 1 calc R . . C40 C 0.2769(6) -0.0349(7) 0.3076(4) 0.038(2) Uani 1 1 d . . . H40A H 0.2539 0.0341 0.3267 0.057 Uiso 1 1 calc R . . H40B H 0.2284 -0.0777 0.3367 0.057 Uiso 1 1 calc R . . H40C H 0.2626 -0.0141 0.2600 0.057 Uiso 1 1 calc R . . C41 C 0.2177(6) 0.5314(6) 0.2968(4) 0.0331(19) Uani 1 1 d . . . C42 C 0.1183(8) 0.5840(9) 0.2543(5) 0.063(3) Uani 1 1 d . A . H42A H 0.1114 0.5237 0.2385 0.094 Uiso 1 1 calc R . . H42B H 0.1385 0.6366 0.2138 0.094 Uiso 1 1 calc R . . H42C H 0.0413 0.6253 0.2834 0.094 Uiso 1 1 calc R . . C43 C 0.2169(8) 0.6296(8) 0.3240(5) 0.061(3) Uani 1 1 d . A . H43A H 0.1360 0.6695 0.3501 0.092 Uiso 1 1 calc R . . H43B H 0.2391 0.6828 0.2846 0.092 Uiso 1 1 calc R . . H43C H 0.2752 0.5993 0.3547 0.092 Uiso 1 1 calc R . . C44 C 0.1891(9) 0.4479(8) 0.3580(5) 0.068(3) Uani 1 1 d . A . H44A H 0.2533 0.4140 0.3849 0.102 Uiso 1 1 calc R . . H44B H 0.1832 0.3880 0.3412 0.102 Uiso 1 1 calc R . . H44C H 0.1121 0.4873 0.3878 0.102 Uiso 1 1 calc R . . C45 C 0.6436(6) 0.2186(7) 0.3097(4) 0.0302(18) Uani 1 1 d . . . H45 H 0.6739 0.2702 0.3144 0.036 Uiso 1 1 calc R . . C46 C 0.5197(7) 0.2465(7) 0.4251(4) 0.043(2) Uani 1 1 d . . . H46A H 0.5556 0.3016 0.4190 0.064 Uiso 1 1 calc R . . H46B H 0.5415 0.1886 0.4658 0.064 Uiso 1 1 calc R . . H46C H 0.4316 0.2857 0.4321 0.064 Uiso 1 1 calc R . . C47 C 0.5159(8) 0.1146(8) 0.3606(4) 0.050(2) Uani 1 1 d . . . H47A H 0.4310 0.1560 0.3569 0.076 Uiso 1 1 calc R . . H47B H 0.5221 0.0578 0.4030 0.076 Uiso 1 1 calc R . . H47C H 0.5616 0.0765 0.3199 0.076 Uiso 1 1 calc R . . C48 C 1.0014(10) 0.3130(9) -0.0426(6) 0.0709(13) Uani 1 1 d . . . C49 C 0.9128(10) 0.4073(8) -0.0165(6) 0.0709(13) Uani 1 1 d . . . H49 H 0.8581 0.3993 0.0261 0.085 Uiso 1 1 calc R . . C50 C 0.9031(10) 0.5142(9) -0.0524(5) 0.0709(13) Uani 1 1 d . . . H50 H 0.8405 0.5795 -0.0346 0.085 Uiso 1 1 calc R . . C51 C 0.9826(9) 0.5274(9) -0.1132(5) 0.0709(13) Uani 1 1 d . . . H51 H 0.9761 0.6013 -0.1369 0.085 Uiso 1 1 calc R . . C52 C 1.0697(10) 0.4349(8) -0.1392(6) 0.0709(13) Uani 1 1 d . . . H52 H 1.1238 0.4432 -0.1820 0.085 Uiso 1 1 calc R . . C53 C 1.0799(10) 0.3288(9) -0.1035(5) 0.0709(13) Uani 1 1 d . . . H53 H 1.1434 0.2642 -0.1215 0.085 Uiso 1 1 calc R . . C54 C 0.6297(9) -0.0477(9) 0.0447(6) 0.0709(13) Uani 1 1 d . . . H54 H 0.6083 -0.0522 0.0940 0.085 Uiso 1 1 calc R A . C55 C 0.6071(9) -0.2239(8) 0.0619(5) 0.059(3) Uani 1 1 d . . . H55A H 0.5775 -0.2097 0.1102 0.088 Uiso 1 1 calc R A . H55B H 0.6794 -0.2946 0.0593 0.088 Uiso 1 1 calc R . . H55C H 0.5444 -0.2306 0.0459 0.088 Uiso 1 1 calc R . . C56 C 0.6727(8) -0.1313(8) -0.0569(4) 0.050(2) Uani 1 1 d . . . H56A H 0.6896 -0.0635 -0.0801 0.075 Uiso 1 1 calc R A . H56B H 0.6073 -0.1310 -0.0741 0.075 Uiso 1 1 calc R . . H56C H 0.7455 -0.1995 -0.0668 0.075 Uiso 1 1 calc R . . C57 C 0.7991(8) 0.1127(9) -0.1486(4) 0.056(3) Uani 1 1 d . . . H57A H 0.8089 0.0433 -0.1626 0.083 Uiso 1 1 calc R A . H57B H 0.8251 0.1615 -0.1895 0.083 Uiso 1 1 calc R . . H57C H 0.7141 0.1532 -0.1283 0.083 Uiso 1 1 calc R . . C58 C 0.6750(15) 0.3553(16) -0.0632(8) 0.0513(16) Uani 0.50 1 d P A 1 H58A H 0.7586 0.3495 -0.0754 0.077 Uiso 0.50 1 calc PR A 1 H58B H 0.6214 0.4278 -0.0469 0.077 Uiso 0.50 1 calc PR A 1 H58C H 0.6521 0.3513 -0.1044 0.077 Uiso 0.50 1 calc PR A 1 O10A O 0.6652(5) 0.2676(5) -0.0115(3) 0.0513(16) Uani 0.50 1 d P A 2 H1P H 1.052(7) 0.169(7) 0.067(3) 0.062 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 Mn1 0.0214(6) 0.0473(8) 0.0213(6) -0.0176(5) 0.0016(5) -0.0141(6) P1 0.0285(11) 0.0572(15) 0.0262(11) -0.0253(10) 0.0072(9) -0.0223(10) O1 0.022(3) 0.052(3) 0.024(3) -0.019(3) 0.003(2) -0.019(2) N1 0.027(3) 0.040(4) 0.022(3) -0.015(3) -0.001(3) -0.011(3) C1 0.024(4) 0.039(5) 0.027(4) -0.010(4) -0.002(3) -0.018(4) Mn2 0.0247(6) 0.0519(8) 0.0193(6) -0.0183(6) 0.0032(5) -0.0181(6) O2 0.022(3) 0.049(3) 0.019(3) -0.014(2) 0.001(2) -0.012(2) N2 0.035(4) 0.041(4) 0.039(4) -0.018(3) -0.012(3) -0.014(3) C2 0.021(4) 0.046(5) 0.033(4) -0.028(4) 0.004(3) -0.016(4) O3 0.026(3) 0.052(3) 0.017(3) -0.016(2) 0.002(2) -0.022(3) C3 0.021(4) 0.048(5) 0.029(4) -0.021(4) -0.002(3) -0.011(4) O4 0.025(3) 0.047(3) 0.023(3) -0.018(2) 0.005(2) -0.018(2) C4 0.027(4) 0.047(5) 0.022(4) -0.011(4) -0.007(3) -0.012(4) O5 0.024(3) 0.044(3) 0.019(3) -0.017(2) 0.002(2) -0.012(2) C5 0.015(4) 0.045(5) 0.028(4) -0.017(4) 0.000(3) -0.012(4) O6 0.026(3) 0.047(3) 0.019(3) -0.017(2) 0.005(2) -0.019(2) C6 0.018(4) 0.045(5) 0.025(4) -0.017(4) 0.004(3) -0.017(4) O7 0.028(3) 0.054(4) 0.025(3) -0.020(3) 0.004(2) -0.016(3) C7 0.018(4) 0.050(5) 0.029(4) -0.015(4) -0.003(3) -0.010(4) O8 0.024(3) 0.058(4) 0.038(3) -0.026(3) -0.007(2) -0.013(3) C8 0.016(4) 0.038(5) 0.028(4) -0.019(4) -0.002(3) -0.002(3) O9 0.031(3) 0.078(4) 0.026(3) -0.020(3) -0.004(2) -0.016(3) C9 0.020(4) 0.044(5) 0.031(5) -0.022(4) -0.005(3) -0.001(4) O10 0.036(3) 0.075(4) 0.031(3) 0.008(3) -0.007(3) -0.020(3) C10 0.018(4) 0.038(5) 0.032(5) -0.021(4) -0.007(3) 0.002(4) C11 0.019(4) 0.040(5) 0.027(4) -0.011(4) 0.000(3) -0.006(3) C12 0.019(4) 0.037(5) 0.025(4) -0.014(4) -0.001(3) -0.006(4) C13 0.016(4) 0.040(5) 0.023(4) -0.018(4) 0.001(3) 0.001(3) C14 0.026(4) 0.045(5) 0.029(4) -0.016(4) 0.000(3) -0.013(4) C15 0.022(4) 0.042(5) 0.019(4) -0.019(4) 0.004(3) -0.014(4) C16 0.024(4) 0.036(5) 0.020(4) -0.013(3) -0.006(3) -0.004(4) C17 0.023(4) 0.036(5) 0.021(4) -0.016(4) -0.002(3) -0.008(4) C18 0.018(4) 0.037(5) 0.025(4) -0.019(4) -0.002(3) -0.005(4) C19 0.027(4) 0.033(4) 0.022(4) -0.013(3) -0.004(3) -0.012(4) C20 0.028(4) 0.037(5) 0.015(4) -0.017(4) 0.000(3) -0.014(4) C21 0.023(4) 0.050(5) 0.022(4) -0.013(4) -0.002(3) -0.017(4) C22 0.024(4) 0.030(4) 0.020(4) -0.008(3) -0.006(3) -0.010(3) C23 0.019(4) 0.042(5) 0.023(4) -0.004(4) -0.003(3) -0.016(4) C24 0.027(4) 0.039(5) 0.025(4) -0.012(4) -0.006(3) -0.009(4) C25 0.028(4) 0.028(4) 0.023(4) -0.010(3) -0.010(3) -0.004(3) C26 0.028(4) 0.031(4) 0.017(4) -0.008(3) -0.005(3) -0.012(3) C27 0.028(4) 0.044(5) 0.017(4) -0.007(4) -0.005(3) -0.014(4) C28 0.022(4) 0.036(5) 0.028(4) -0.014(4) -0.003(3) -0.008(3) C29 0.031(5) 0.065(6) 0.032(5) -0.027(4) 0.000(4) -0.016(4) C30 0.079(8) 0.088(8) 0.053(6) -0.054(6) -0.031(6) 0.031(6) C31 0.089(8) 0.094(9) 0.067(7) -0.041(6) -0.020(6) -0.045(7) C32 0.084(8) 0.077(7) 0.044(6) -0.025(5) -0.008(5) -0.033(6) C33 0.038(5) 0.038(5) 0.024(4) -0.017(4) -0.006(4) 0.000(4) C34 0.093(8) 0.107(9) 0.040(6) -0.004(6) -0.026(6) -0.052(7) C35 0.139(11) 0.062(8) 0.043(6) -0.012(5) -0.014(7) -0.026(7) C36 0.056(6) 0.106(9) 0.035(6) -0.016(6) 0.005(5) -0.023(6) C37 0.022(4) 0.036(5) 0.034(4) -0.015(4) -0.001(3) -0.012(4) C38 0.037(5) 0.042(5) 0.033(5) -0.012(4) -0.001(4) -0.012(4) C39 0.038(5) 0.033(5) 0.046(5) -0.014(4) -0.006(4) -0.010(4) C40 0.026(4) 0.042(5) 0.041(5) -0.010(4) 0.002(4) -0.013(4) C41 0.025(4) 0.036(5) 0.039(5) -0.018(4) 0.002(4) -0.011(4) C42 0.036(5) 0.066(7) 0.074(7) -0.022(6) -0.005(5) -0.007(5) C43 0.037(5) 0.065(7) 0.079(7) -0.036(6) 0.013(5) -0.020(5) C44 0.056(6) 0.059(7) 0.066(7) -0.024(6) 0.025(5) -0.017(5) C45 0.021(4) 0.046(5) 0.028(5) -0.013(4) -0.002(4) -0.015(4) C46 0.040(5) 0.053(6) 0.037(5) -0.024(4) 0.008(4) -0.020(4) C47 0.065(6) 0.071(7) 0.028(5) -0.024(5) 0.014(4) -0.043(5) C48 0.078(3) 0.061(2) 0.073(3) -0.036(2) 0.035(2) -0.043(2) C49 0.078(3) 0.061(2) 0.073(3) -0.036(2) 0.035(2) -0.043(2) C50 0.078(3) 0.061(2) 0.073(3) -0.036(2) 0.035(2) -0.043(2) C51 0.078(3) 0.061(2) 0.073(3) -0.036(2) 0.035(2) -0.043(2) C52 0.078(3) 0.061(2) 0.073(3) -0.036(2) 0.035(2) -0.043(2) C53 0.078(3) 0.061(2) 0.073(3) -0.036(2) 0.035(2) -0.043(2) C54 0.078(3) 0.061(2) 0.073(3) -0.036(2) 0.035(2) -0.043(2) C55 0.073(7) 0.049(6) 0.062(7) -0.006(5) -0.018(5) -0.029(5) C56 0.053(6) 0.067(6) 0.042(5) -0.035(5) -0.003(4) -0.024(5) C57 0.040(5) 0.085(7) 0.037(5) -0.021(5) -0.006(4) -0.014(5) C58 0.036(3) 0.075(4) 0.031(3) 0.008(3) -0.007(3) -0.020(3) O10A 0.036(3) 0.075(4) 0.031(3) 0.008(3) -0.007(3) -0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.897(5) . ? Mn1 O4 1.930(5) . ? Mn1 O2 1.941(5) . ? Mn1 O3 1.951(5) . ? Mn1 O5 2.251(5) . ? Mn1 O6 2.253(4) . ? P1 O7 1.501(5) . ? P1 O6 1.518(5) . ? P1 C48 1.784(11) . ? P1 H1P 1.40(2) . ? O1 C6 1.354(8) . ? N1 C45 1.334(9) . ? N1 C47 1.436(10) . ? N1 C46 1.443(9) . ? C1 C6 1.405(10) . ? C1 C2 1.405(10) . ? C1 C28 1.516(10) . ? Mn2 O7 2.101(5) 2_755 ? Mn2 O3 2.162(4) . ? Mn2 O6 2.180(5) . ? Mn2 O8 2.202(5) . ? Mn2 O9 2.223(5) . ? Mn2 O10 2.228(6) . ? O2 C13 1.349(8) . ? N2 C54 1.311(11) . ? N2 C55 1.438(11) . ? N2 C56 1.461(10) . ? C2 C3 1.388(11) . ? C2 H2 0.9500 . ? O3 C20 1.348(8) . ? C3 C4 1.397(10) . ? C3 C29 1.540(10) . ? O4 C27 1.363(8) . ? C4 C5 1.373(10) . ? C4 H4 0.9500 . ? O5 C45 1.228(8) . ? C5 C6 1.409(10) . ? C5 C7 1.512(10) . ? O7 Mn2 2.101(5) 2_755 ? C7 C8 1.531(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O8 C54 1.253(11) . ? C8 C9 1.388(10) . ? C8 C13 1.403(10) . ? O9 C57 1.434(10) . ? C9 C10 1.401(11) . ? C9 H9 0.9500 . ? O10 C58 1.370(17) . ? C10 C11 1.388(10) . ? C10 C33 1.541(11) . ? C11 C12 1.385(10) . ? C11 H11 0.9500 . ? C12 C13 1.420(11) . ? C12 C14 1.519(10) . ? C14 C15 1.527(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.386(10) . ? C15 C20 1.396(10) . ? C16 C17 1.421(10) . ? C16 H16 0.9500 . ? C17 C18 1.384(10) . ? C17 C37 1.527(10) . ? C18 C19 1.400(10) . ? C18 H18 0.9500 . ? C19 C20 1.416(10) . ? C19 C21 1.507(10) . ? C21 C22 1.523(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.396(10) . ? C22 C27 1.406(10) . ? C23 C24 1.389(10) . ? C23 H23 0.9500 . ? C24 C25 1.391(10) . ? C24 C41 1.541(10) . ? C25 C26 1.387(10) . ? C25 H25 0.9500 . ? C26 C27 1.417(10) . ? C26 C28 1.521(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.489(12) . ? C29 C31 1.492(12) . ? C29 C32 1.584(13) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.489(13) . ? C33 C34 1.507(12) . ? C33 C36 1.548(12) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C40 1.530(10) . ? C37 C39 1.536(10) . ? C37 C38 1.540(10) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C44 1.505(12) . ? C41 C42 1.529(12) . ? C41 C43 1.538(12) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.369(13) . ? C48 C53 1.373(13) . ? C49 C50 1.383(14) . ? C49 H49 0.9500 . ? C50 C51 1.371(13) . ? C50 H50 0.9500 . ? C51 C52 1.345(13) . ? C51 H51 0.9500 . ? C52 C53 1.371(14) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? 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 O1 Mn1 O4 91.1(2) . . ? O1 Mn1 O2 91.3(2) . . ? O4 Mn1 O2 174.2(2) . . ? O1 Mn1 O3 174.5(2) . . ? O4 Mn1 O3 87.1(2) . . ? O2 Mn1 O3 90.1(2) . . ? O1 Mn1 O5 97.06(18) . . ? O4 Mn1 O5 92.25(18) . . ? O2 Mn1 O5 92.73(19) . . ? O3 Mn1 O5 88.21(18) . . ? O1 Mn1 O6 95.33(18) . . ? O4 Mn1 O6 89.24(19) . . ? O2 Mn1 O6 85.25(19) . . ? O3 Mn1 O6 79.46(18) . . ? O5 Mn1 O6 167.49(18) . . ? O7 P1 O6 115.7(3) . . ? O7 P1 C48 109.6(4) . . ? O6 P1 C48 109.7(4) . . ? O7 P1 H1P 113(3) . . ? O6 P1 H1P 102(3) . . ? C48 P1 H1P 106(3) . . ? C6 O1 Mn1 119.4(4) . . ? C45 N1 C47 120.3(6) . . ? C45 N1 C46 121.8(6) . . ? C47 N1 C46 117.9(6) . . ? C6 C1 C2 118.2(7) . . ? C6 C1 C28 121.1(6) . . ? C2 C1 C28 120.7(6) . . ? O7 Mn2 O3 90.51(19) 2_755 . ? O7 Mn2 O6 104.78(19) 2_755 . ? O3 Mn2 O6 76.81(17) . . ? O7 Mn2 O8 86.4(2) 2_755 . ? O3 Mn2 O8 93.15(18) . . ? O6 Mn2 O8 164.81(18) . . ? O7 Mn2 O9 89.4(2) 2_755 . ? O3 Mn2 O9 174.71(19) . . ? O6 Mn2 O9 98.09(19) . . ? O8 Mn2 O9 92.13(19) . . ? O7 Mn2 O10 173.4(2) 2_755 . ? O3 Mn2 O10 91.0(2) . . ? O6 Mn2 O10 81.8(2) . . ? O8 Mn2 O10 87.1(2) . . ? O9 Mn2 O10 89.6(2) . . ? C13 O2 Mn1 115.2(4) . . ? C54 N2 C55 121.3(8) . . ? C54 N2 C56 120.6(8) . . ? C55 N2 C56 118.0(7) . . ? C3 C2 C1 122.9(7) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C20 O3 Mn1 123.9(4) . . ? C20 O3 Mn2 129.5(4) . . ? Mn1 O3 Mn2 106.5(2) . . ? C2 C3 C4 116.5(6) . . ? C2 C3 C29 122.1(7) . . ? C4 C3 C29 121.3(7) . . ? C27 O4 Mn1 118.4(4) . . ? C5 C4 C3 123.4(7) . . ? C5 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? C45 O5 Mn1 145.6(5) . . ? C4 C5 C6 118.8(7) . . ? C4 C5 C7 120.7(7) . . ? C6 C5 C7 120.5(6) . . ? P1 O6 Mn2 135.7(3) . . ? P1 O6 Mn1 123.3(3) . . ? Mn2 O6 Mn1 96.16(18) . . ? O1 C6 C1 120.0(6) . . ? O1 C6 C5 119.9(6) . . ? C1 C6 C5 120.1(6) . . ? P1 O7 Mn2 134.9(3) . 2_755 ? C5 C7 C8 112.8(6) . . ? C5 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C5 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C54 O8 Mn2 126.0(7) . . ? C9 C8 C13 118.7(7) . . ? C9 C8 C7 120.4(7) . . ? C13 C8 C7 120.8(7) . . ? C57 O9 Mn2 122.2(5) . . ? C8 C9 C10 123.0(7) . . ? C8 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C58 O10 Mn2 133.2(8) . . ? C11 C10 C9 116.5(7) . . ? C11 C10 C33 120.0(7) . . ? C9 C10 C33 123.5(7) . . ? C12 C11 C10 123.6(7) . . ? C12 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? C11 C12 C13 118.1(7) . . ? C11 C12 C14 122.0(7) . . ? C13 C12 C14 119.9(6) . . ? O2 C13 C8 120.0(7) . . ? O2 C13 C12 119.8(6) . . ? C8 C13 C12 120.1(7) . . ? C12 C14 C15 112.5(6) . . ? C12 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? C12 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C20 118.9(6) . . ? C16 C15 C14 120.0(7) . . ? C20 C15 C14 121.1(6) . . ? C15 C16 C17 122.9(7) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 116.1(7) . . ? C18 C17 C37 124.4(6) . . ? C16 C17 C37 119.5(7) . . ? C17 C18 C19 123.3(6) . . ? C17 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C18 C19 C20 118.3(7) . . ? C18 C19 C21 120.9(6) . . ? C20 C19 C21 120.8(6) . . ? O3 C20 C15 119.7(6) . . ? O3 C20 C19 120.1(7) . . ? C15 C20 C19 120.2(6) . . ? C19 C21 C22 116.5(6) . . ? C19 C21 H21A 108.2 . . ? C22 C21 H21A 108.2 . . ? C19 C21 H21B 108.2 . . ? C22 C21 H21B 108.2 . . ? H21A C21 H21B 107.3 . . ? C23 C22 C27 118.1(6) . . ? C23 C22 C21 119.9(6) . . ? C27 C22 C21 122.0(6) . . ? C24 C23 C22 123.2(7) . . ? C24 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C23 C24 C25 117.0(6) . . ? C23 C24 C41 120.1(7) . . ? C25 C24 C41 122.8(7) . . ? C26 C25 C24 122.9(7) . . ? C26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C25 C26 C27 118.6(6) . . ? C25 C26 C28 121.0(6) . . ? C27 C26 C28 120.5(6) . . ? O4 C27 C22 120.9(6) . . ? O4 C27 C26 118.9(6) . . ? C22 C27 C26 120.1(6) . . ? C1 C28 C26 112.3(6) . . ? C1 C28 H28A 109.2 . . ? C26 C28 H28A 109.2 . . ? C1 C28 H28B 109.2 . . ? C26 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C31 113.9(9) . . ? C30 C29 C3 113.2(7) . . ? C31 C29 C3 109.4(7) . . ? C30 C29 C32 104.3(8) . . ? C31 C29 C32 106.5(8) . . ? C3 C29 C32 109.1(7) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C34 110.0(8) . . ? C35 C33 C10 112.0(7) . . ? C34 C33 C10 113.4(7) . . ? C35 C33 C36 106.5(9) . . ? C34 C33 C36 106.5(7) . . ? C10 C33 C36 108.0(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C17 C37 C40 111.8(6) . . ? C17 C37 C39 108.9(6) . . ? C40 C37 C39 108.6(6) . . ? C17 C37 C38 110.5(6) . . ? C40 C37 C38 108.1(6) . . ? C39 C37 C38 108.9(6) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C44 C41 C42 109.8(8) . . ? C44 C41 C43 108.8(7) . . ? C42 C41 C43 106.4(7) . . ? C44 C41 C24 110.0(7) . . ? C42 C41 C24 110.0(6) . . ? C43 C41 C24 111.8(6) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O5 C45 N1 125.5(7) . . ? O5 C45 H45 117.3 . . ? N1 C45 H45 117.3 . . ? N1 C46 H46A 109.5 . . ? N1 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N1 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N1 C47 H47A 109.5 . . ? N1 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N1 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C53 118.0(10) . . ? C49 C48 P1 118.8(7) . . ? C53 C48 P1 123.1(8) . . ? C48 C49 C50 119.7(9) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C51 C50 C49 121.0(9) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C52 C51 C50 119.5(10) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C53 119.6(9) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C48 122.1(9) . . ? C52 C53 H53 118.9 . . ? C48 C53 H53 118.9 . . ? O8 C54 N2 124.3(10) . . ? O8 C54 H54 117.9 . . ? N2 C54 H54 117.9 . . ? N2 C55 H55A 109.5 . . ? N2 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N2 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N2 C56 H56A 109.5 . . ? N2 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N2 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O9 C57 H57A 109.5 . . ? O9 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O9 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.406 _refine_diff_density_min -1.676 _refine_diff_density_rms 0.099