Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_MnTPPlCl _database_code_depnum_ccdc_archive 'CCDC 251021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '5,10,15,20-tetraphenylporpholactonato Manganese(III) chloride' ; _chemical_name_common ;'5,10,15,20-tetraphenylporpholactonato Manganese(iii) chloride' ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H27 Cl4 Mn N4 O2' _chemical_formula_weight 840.44 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.031(9) _cell_length_b 21.864(16) _cell_length_c 14.551(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.581(13) _cell_angle_gamma 90.00 _cell_volume 3736(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2279 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.44 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.5474 _exptl_absorpt_correction_T_max 0.9864 _exptl_absorpt_process_details ? _exptl_special_details ; 'Ratio of minimum to maximum apparent transmission: 0.554977' ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24320 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.1306 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6568 _reflns_number_gt 3650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms were placed in ideal positions on pyrrole and phenyl carbons and were refined isotropically. The solvent disorder (four chloroform per unit cell) was refined as a diffuse contribution without specific atom positions using the SQUEEZE program, but the density, absorption coefficient and other parameters reflect the full formula. Some disorder was observed in the lactone ring; the model reflects the primary orientation (~45%). The remaining occupancy was evenly distributed through seven other positions in the porphyrin ring. Due the fractional contribution of each position, the disordered was not modelled. The second oxygen in the lactone ring has a refined occupancy of 0.84. This results from the sum of thefractional contribution of the disordered oxygen (~0.45) and the disordered carbon (~0.55) at that position. This sum results in 0.86, which is within 5% of the refined value. The highest Q peak of 1.35 on the difference map arises from the disordered oxazolone ring. ; _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^)+(0.1019P)^2^+0.0000P] 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 6568 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1811 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 C1 C -0.0573(4) 0.2318(2) 0.0637(4) 0.0459(13) Uani 1 1 d . . . C2 C -0.1297(5) 0.2624(3) 0.1152(4) 0.0515(14) Uani 1 1 d . . . H2 H -0.1656 0.2998 0.0997 0.062 Uiso 1 1 calc R . . C3 C -0.1366(4) 0.2278(3) 0.1895(4) 0.0496(14) Uani 1 1 d . . . H3 H -0.1793 0.2363 0.2342 0.059 Uiso 1 1 calc R . . C4 C -0.0653(4) 0.1744(2) 0.1875(3) 0.0409(12) Uani 1 1 d . . . C5 C -0.0388(4) 0.1316(2) 0.2585(3) 0.0416(12) Uani 1 1 d . . . C6 C 0.0318(4) 0.0811(2) 0.2513(3) 0.0415(12) Uani 1 1 d . . . C7 C 0.1332(5) -0.0045(3) 0.2940(4) 0.0455(13) Uani 1 1 d . . . C8 C 0.1326(4) 0.0106(2) 0.1997(3) 0.0377(11) Uani 1 1 d . . . C9 C 0.1842(4) -0.0258(2) 0.1422(3) 0.0391(12) Uani 1 1 d . . . C10 C 0.1813(4) -0.0109(2) 0.0488(3) 0.0360(11) Uani 1 1 d . . . C11 C 0.2129(4) -0.0501(2) -0.0191(3) 0.0414(12) Uani 1 1 d . . . H11 H 0.2368 -0.0905 -0.0092 0.050 Uiso 1 1 calc R . . C12 C 0.2023(4) -0.0189(2) -0.0997(3) 0.0402(12) Uani 1 1 d . . . H12 H 0.2176 -0.0338 -0.1556 0.048 Uiso 1 1 calc R . . C13 C 0.1639(4) 0.0405(2) -0.0851(3) 0.0396(12) Uani 1 1 d . . . C14 C 0.1538(4) 0.0887(2) -0.1511(3) 0.0395(11) Uani 1 1 d . . . C15 C 0.1129(4) 0.1470(2) -0.1337(3) 0.0401(12) Uani 1 1 d . . . C16 C 0.1123(3) 0.19874(14) -0.1917(2) 0.0513(14) Uani 1 1 d . . . H16 H 0.1407 0.2007 -0.2462 0.062 Uiso 1 1 calc R . . O1 O 0.0679(3) 0.04040(14) 0.3274(2) 0.064(2) Uani 0.837(14) 1 d PR . . O2 O 0.1907(3) -0.03232(14) 0.3578(2) 0.073(5) Uani 0.451(16) 1 d PR . . C17 C 0.0632(3) 0.24468(14) -0.1537(2) 0.0537(14) Uani 1 1 d R . . H17 H 0.0513 0.2843 -0.1771 0.064 Uiso 1 1 d R . . C18 C 0.0325(5) 0.2216(2) -0.0708(4) 0.0476(13) Uani 1 1 d . . . C19 C -0.0264(5) 0.2555(2) -0.0157(4) 0.0464(13) Uani 1 1 d . . . C20 C -0.0837(5) 0.1389(3) 0.3457(4) 0.0488(13) Uani 1 1 d . . . C21 C -0.1510(5) 0.0939(3) 0.3740(4) 0.0617(17) Uani 1 1 d . . . H21 H -0.1678 0.0585 0.3382 0.074 Uiso 1 1 calc R . . C22 C -0.1934(6) 0.1009(3) 0.4548(5) 0.077(2) Uani 1 1 d . . . H22 H -0.2370 0.0700 0.4733 0.092 Uiso 1 1 calc R . . C23 C -0.1708(7) 0.1536(4) 0.5077(5) 0.081(2) Uani 1 1 d . . . H23 H -0.2008 0.1589 0.5609 0.097 Uiso 1 1 calc R . . C24 C -0.1049(7) 0.1976(3) 0.4818(4) 0.075(2) Uani 1 1 d . . . H24 H -0.0890 0.2329 0.5180 0.090 Uiso 1 1 calc R . . C25 C -0.0599(6) 0.1907(3) 0.4008(4) 0.0636(16) Uani 1 1 d . . . H25 H -0.0140 0.2212 0.3843 0.076 Uiso 1 1 calc R . . C26 C 0.2415(4) -0.0840(2) 0.1791(3) 0.0405(12) Uani 1 1 d . . . C27 C 0.3553(5) -0.0934(3) 0.1800(4) 0.0548(15) Uani 1 1 d . . . H27 H 0.3966 -0.0630 0.1575 0.066 Uiso 1 1 calc R . . C28 C 0.4097(5) -0.1483(3) 0.2145(4) 0.0599(16) Uani 1 1 d . . . H28 H 0.4866 -0.1541 0.2160 0.072 Uiso 1 1 calc R . . C29 C 0.3473(5) -0.1931(3) 0.2462(4) 0.0565(15) Uani 1 1 d . . . H29 H 0.3822 -0.2298 0.2684 0.068 Uiso 1 1 calc R . . C30 C 0.2356(5) -0.1846(2) 0.2453(4) 0.0510(14) Uani 1 1 d . . . H30 H 0.1944 -0.2155 0.2668 0.061 Uiso 1 1 calc R . . C31 C 0.1827(4) -0.1306(2) 0.2129(3) 0.0433(12) Uani 1 1 d . . . H31 H 0.1063 -0.1251 0.2137 0.052 Uiso 1 1 calc R . . C32 C 0.1880(5) 0.0790(2) -0.2422(4) 0.0473(13) Uani 1 1 d . . . C33 C 0.2982(5) 0.0630(3) -0.2444(4) 0.0512(14) Uani 1 1 d . . . H33 H 0.3510 0.0567 -0.1882 0.061 Uiso 1 1 calc R . . C34 C 0.3315(6) 0.0561(3) -0.3299(5) 0.0624(16) Uani 1 1 d . . . H34 H 0.4057 0.0447 -0.3308 0.075 Uiso 1 1 calc R . . C35 C 0.2538(6) 0.0662(3) -0.4125(4) 0.0591(16) Uani 1 1 d . . . H35 H 0.2759 0.0628 -0.4697 0.071 Uiso 1 1 calc R . . C36 C 0.1458(6) 0.0810(3) -0.4111(4) 0.0691(18) Uani 1 1 d . . . H36 H 0.0940 0.0870 -0.4680 0.083 Uiso 1 1 calc R . . C37 C 0.1091(5) 0.0877(3) -0.3278(4) 0.0529(14) Uani 1 1 d . . . H37 H 0.0338 0.0978 -0.3285 0.063 Uiso 1 1 calc R . . C38 C -0.0532(5) 0.3209(3) -0.0445(4) 0.0571(16) Uani 1 1 d . . . C39 C -0.1377(8) 0.3369(3) -0.1174(5) 0.094(3) Uani 1 1 d . . . H39 H -0.1873 0.3069 -0.1476 0.113 Uiso 1 1 calc R . . C40 C -0.1528(9) 0.3970(4) -0.1489(5) 0.088(2) Uani 1 1 d . . . H40 H -0.2131 0.4068 -0.1985 0.106 Uiso 1 1 calc R . . C41 C -0.0847(7) 0.4385(4) -0.1102(6) 0.086(2) Uani 1 1 d . . . H41 H -0.0933 0.4780 -0.1345 0.104 Uiso 1 1 calc R . . C42 C 0.0036(7) 0.4265(4) -0.0314(8) 0.116(3) Uani 1 1 d . . . H42 H 0.0511 0.4577 -0.0023 0.139 Uiso 1 1 calc R . . C43 C 0.0181(6) 0.3671(3) 0.0019(6) 0.083(2) Uani 1 1 d . . . H43 H 0.0747 0.3580 0.0546 0.100 Uiso 1 1 calc R . . Cl1 Cl 0.25249(11) 0.17147(6) 0.13260(9) 0.0499(4) Uani 1 1 d . . . Mn1 Mn 0.08460(6) 0.11753(3) 0.06453(5) 0.0373(2) Uani 1 1 d . . . N1 N -0.0197(3) 0.17711(18) 0.1074(3) 0.0390(10) Uani 1 1 d . . . N2 N 0.0723(3) 0.06377(18) 0.1746(3) 0.0381(9) Uani 1 1 d . . . N3 N 0.1475(3) 0.04535(17) 0.0053(3) 0.0377(9) Uani 1 1 d . . . N4 N 0.0637(4) 0.16143(18) -0.0581(3) 0.0410(10) 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 0.047(3) 0.040(3) 0.052(3) 0.001(2) 0.015(3) 0.007(2) C2 0.050(3) 0.048(3) 0.057(3) -0.002(3) 0.012(3) 0.011(3) C3 0.044(3) 0.058(4) 0.050(3) -0.009(3) 0.019(3) 0.004(3) C4 0.040(3) 0.040(3) 0.045(3) -0.007(2) 0.017(2) 0.000(2) C5 0.045(3) 0.042(3) 0.041(3) -0.008(2) 0.017(2) -0.002(2) C6 0.047(3) 0.042(3) 0.035(3) -0.003(2) 0.008(2) 0.000(2) C7 0.046(3) 0.050(3) 0.042(3) 0.012(3) 0.013(2) 0.009(3) C8 0.039(3) 0.036(3) 0.040(3) 0.002(2) 0.011(2) 0.004(2) C9 0.036(3) 0.031(3) 0.050(3) 0.001(2) 0.009(2) 0.002(2) C10 0.033(3) 0.039(3) 0.036(3) -0.002(2) 0.008(2) 0.001(2) C11 0.037(3) 0.039(3) 0.050(3) -0.007(2) 0.014(2) 0.008(2) C12 0.043(3) 0.043(3) 0.037(3) -0.011(2) 0.014(2) 0.003(2) C13 0.035(3) 0.051(3) 0.034(3) -0.003(2) 0.010(2) 0.001(2) C14 0.037(3) 0.052(3) 0.033(3) -0.003(2) 0.013(2) -0.002(2) C15 0.041(3) 0.040(3) 0.040(3) -0.002(2) 0.011(2) -0.003(2) C16 0.059(4) 0.050(3) 0.048(3) -0.001(3) 0.021(3) 0.010(3) O1 0.068(4) 0.071(4) 0.056(3) -0.001(2) 0.019(3) 0.000(3) O2 0.100(9) 0.055(7) 0.073(8) 0.008(5) 0.040(6) 0.001(5) C17 0.075(4) 0.044(3) 0.047(3) 0.010(2) 0.021(3) 0.009(3) C18 0.063(4) 0.038(3) 0.044(3) -0.003(2) 0.016(3) 0.007(3) C19 0.055(3) 0.042(3) 0.044(3) 0.000(2) 0.015(3) 0.010(2) C20 0.059(3) 0.048(3) 0.044(3) -0.007(2) 0.022(3) 0.005(3) C21 0.076(4) 0.066(4) 0.055(4) -0.013(3) 0.040(3) -0.013(3) C22 0.084(5) 0.088(5) 0.072(4) -0.008(4) 0.048(4) -0.009(4) C23 0.100(6) 0.095(6) 0.058(4) -0.014(4) 0.038(4) 0.012(5) C24 0.104(6) 0.076(5) 0.054(4) -0.011(3) 0.038(4) -0.006(4) C25 0.074(4) 0.063(4) 0.060(4) -0.002(3) 0.027(3) -0.011(3) C26 0.048(3) 0.041(3) 0.034(3) -0.002(2) 0.011(2) 0.004(2) C27 0.044(3) 0.043(3) 0.081(4) 0.014(3) 0.019(3) -0.001(3) C28 0.048(3) 0.053(4) 0.079(4) 0.015(3) 0.015(3) 0.010(3) C29 0.059(4) 0.042(3) 0.066(4) 0.009(3) 0.007(3) 0.010(3) C30 0.065(4) 0.031(3) 0.059(3) 0.004(2) 0.016(3) 0.000(3) C31 0.044(3) 0.047(3) 0.044(3) -0.001(2) 0.020(2) 0.001(2) C32 0.059(3) 0.038(3) 0.049(3) -0.004(2) 0.022(3) -0.001(2) C33 0.053(3) 0.059(4) 0.048(3) -0.002(3) 0.025(3) -0.002(3) C34 0.066(4) 0.059(4) 0.072(4) -0.007(3) 0.037(4) -0.001(3) C35 0.072(4) 0.064(4) 0.052(4) 0.000(3) 0.036(3) -0.004(3) C36 0.091(5) 0.075(5) 0.044(4) -0.001(3) 0.022(3) -0.011(4) C37 0.064(4) 0.060(4) 0.038(3) 0.002(3) 0.018(3) 0.003(3) C38 0.071(4) 0.052(4) 0.052(4) 0.004(3) 0.023(3) 0.020(3) C39 0.135(7) 0.062(5) 0.069(5) -0.007(4) -0.017(5) 0.050(5) C40 0.124(7) 0.075(6) 0.061(5) 0.003(4) 0.013(5) 0.029(5) C41 0.097(6) 0.084(6) 0.094(6) 0.045(5) 0.054(5) 0.027(5) C42 0.069(5) 0.070(5) 0.212(11) 0.035(6) 0.036(6) 0.007(4) C43 0.055(4) 0.055(4) 0.135(7) 0.038(4) 0.011(4) 0.006(3) Cl1 0.0485(8) 0.0486(8) 0.0548(8) -0.0099(6) 0.0159(6) -0.0008(6) Mn1 0.0401(4) 0.0368(4) 0.0368(4) -0.0010(3) 0.0124(3) 0.0036(3) N1 0.040(2) 0.044(2) 0.035(2) -0.0027(18) 0.0112(19) 0.0031(19) N2 0.039(2) 0.039(2) 0.038(2) -0.0012(18) 0.0120(19) -0.0025(19) N3 0.041(2) 0.036(2) 0.037(2) -0.0043(17) 0.0111(19) 0.0024(18) N4 0.048(2) 0.042(3) 0.037(2) 0.0003(18) 0.017(2) 0.004(2) _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 N1 1.383(6) . ? C1 C19 1.389(7) . ? C1 C2 1.433(7) . ? C2 C3 1.337(7) . ? C3 C4 1.452(7) . ? C4 C5 1.379(7) . ? C4 N1 1.393(6) . ? C5 C6 1.412(7) . ? C5 C20 1.492(7) . ? C6 N2 1.364(6) . ? C6 O1 1.413(6) . ? C7 O2 1.195(6) . ? C7 O1 1.408(6) . ? C7 C8 1.411(7) . ? C8 N2 1.376(6) . ? C8 C9 1.394(6) . ? C9 C10 1.391(7) . ? C9 C26 1.490(7) . ? C10 N3 1.402(6) . ? C10 C11 1.422(6) . ? C11 C12 1.340(7) . ? C12 C13 1.411(7) . ? C13 N3 1.376(6) . ? C13 C14 1.413(7) . ? C14 C15 1.408(7) . ? C14 C32 1.486(7) . ? C15 N4 1.394(6) . ? C15 C16 1.411(6) . ? C16 C17 1.3441 . ? C17 C18 1.429(6) . ? C18 N4 1.370(6) . ? C18 C19 1.393(7) . ? C19 C38 1.505(8) . ? C20 C25 1.382(8) . ? C20 C21 1.392(8) . ? C21 C22 1.388(8) . ? C22 C23 1.380(10) . ? C23 C24 1.350(10) . ? C24 C25 1.409(8) . ? C26 C27 1.383(7) . ? C26 C31 1.390(7) . ? C27 C28 1.406(8) . ? C28 C29 1.374(8) . ? C29 C30 1.354(8) . ? C30 C31 1.376(7) . ? C32 C33 1.378(8) . ? C32 C37 1.406(8) . ? C33 C34 1.395(7) . ? C34 C35 1.370(9) . ? C35 C36 1.343(9) . ? C36 C37 1.385(8) . ? C38 C39 1.346(9) . ? C38 C43 1.400(9) . ? C39 C40 1.390(10) . ? C40 C41 1.270(11) . ? C41 C42 1.408(12) . ? C42 C43 1.382(10) . ? Cl1 Mn1 2.362(2) . ? Mn1 N4 1.993(4) . ? Mn1 N1 2.001(4) . ? Mn1 N2 2.018(4) . ? Mn1 N3 2.022(4) . ? 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 N1 C1 C19 125.9(5) . . ? N1 C1 C2 109.7(4) . . ? C19 C1 C2 124.3(5) . . ? C3 C2 C1 108.1(5) . . ? C2 C3 C4 107.3(4) . . ? C5 C4 N1 125.9(4) . . ? C5 C4 C3 124.8(4) . . ? N1 C4 C3 109.0(4) . . ? C4 C5 C6 121.4(4) . . ? C4 C5 C20 119.9(5) . . ? C6 C5 C20 118.8(5) . . ? N2 C6 C5 127.3(5) . . ? N2 C6 O1 111.3(4) . . ? C5 C6 O1 121.5(4) . . ? O2 C7 O1 111.1(4) . . ? O2 C7 C8 138.9(5) . . ? O1 C7 C8 106.7(4) . . ? N2 C8 C9 126.9(4) . . ? N2 C8 C7 110.2(4) . . ? C9 C8 C7 122.8(4) . . ? C10 C9 C8 122.2(4) . . ? C10 C9 C26 117.6(4) . . ? C8 C9 C26 120.2(4) . . ? C9 C10 N3 126.1(4) . . ? C9 C10 C11 125.7(4) . . ? N3 C10 C11 108.1(4) . . ? C12 C11 C10 108.2(4) . . ? C11 C12 C13 108.0(4) . . ? N3 C13 C12 109.6(4) . . ? N3 C13 C14 125.7(4) . . ? C12 C13 C14 124.5(4) . . ? C15 C14 C13 122.3(4) . . ? C15 C14 C32 117.8(4) . . ? C13 C14 C32 120.0(5) . . ? N4 C15 C14 124.9(4) . . ? N4 C15 C16 110.0(4) . . ? C14 C15 C16 125.1(4) . . ? C17 C16 C15 107.4(2) . . ? C7 O1 C6 105.5(3) . . ? C16 C17 C18 107.6(2) . . ? N4 C18 C19 126.3(5) . . ? N4 C18 C17 109.8(4) . . ? C19 C18 C17 123.8(4) . . ? C1 C19 C18 122.8(5) . . ? C1 C19 C38 120.4(5) . . ? C18 C19 C38 116.8(5) . . ? C25 C20 C21 117.9(5) . . ? C25 C20 C5 120.8(5) . . ? C21 C20 C5 121.2(5) . . ? C22 C21 C20 121.1(6) . . ? C23 C22 C21 120.0(7) . . ? C24 C23 C22 119.7(6) . . ? C23 C24 C25 120.9(6) . . ? C20 C25 C24 120.3(6) . . ? C27 C26 C31 117.8(5) . . ? C27 C26 C9 120.7(5) . . ? C31 C26 C9 121.5(5) . . ? C26 C27 C28 120.9(5) . . ? C29 C28 C27 118.9(5) . . ? C30 C29 C28 120.8(5) . . ? C29 C30 C31 120.3(5) . . ? C30 C31 C26 121.3(5) . . ? C33 C32 C37 118.8(5) . . ? C33 C32 C14 120.8(5) . . ? C37 C32 C14 120.4(5) . . ? C32 C33 C34 120.8(6) . . ? C35 C34 C33 119.4(6) . . ? C36 C35 C34 120.2(5) . . ? C35 C36 C37 122.2(6) . . ? C36 C37 C32 118.6(6) . . ? C39 C38 C43 118.0(6) . . ? C39 C38 C19 123.1(6) . . ? C43 C38 C19 118.7(5) . . ? C38 C39 C40 121.9(8) . . ? C41 C40 C39 120.2(8) . . ? C40 C41 C42 121.9(8) . . ? C43 C42 C41 118.4(9) . . ? C42 C43 C38 119.5(7) . . ? N4 Mn1 N1 90.02(16) . . ? N4 Mn1 N2 166.98(17) . . ? N1 Mn1 N2 88.40(16) . . ? N4 Mn1 N3 88.87(16) . . ? N1 Mn1 N3 163.61(16) . . ? N2 Mn1 N3 89.01(16) . . ? N4 Mn1 Cl1 93.70(13) . . ? N1 Mn1 Cl1 94.67(13) . . ? N2 Mn1 Cl1 99.31(12) . . ? N3 Mn1 Cl1 101.73(13) . . ? C1 N1 C4 105.8(4) . . ? C1 N1 Mn1 125.7(3) . . ? C4 N1 Mn1 128.4(3) . . ? C6 N2 C8 106.2(4) . . ? C6 N2 Mn1 126.0(3) . . ? C8 N2 Mn1 125.2(3) . . ? C13 N3 C10 106.0(4) . . ? C13 N3 Mn1 127.7(3) . . ? C10 N3 Mn1 126.2(3) . . ? C18 N4 C15 105.3(4) . . ? C18 N4 Mn1 124.1(3) . . ? C15 N4 Mn1 127.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.320 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.087 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.500 309.6 113.9 2 0.500 1.000 0.000 309.5 114.4 _platon_squeeze_details ; ? ;