# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Euan Brechin' _publ_contact_author_address ; Department of Chemistry University of Edinburgh West Mains Raod Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_section_title ; A rare ferromagnetic manganese(III) cube. ; _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK loop_ _publ_author_name E.Brechin G.Christou C.J.Milios A.Mishra S.Parsons S.P.Perlepes A.Prescimone W.Wernsdorfer # Attachment 'eb6059.cif' data_eb6059 _database_code_depnum_ccdc_archive 'CCDC 616497' _audit_creation_date 06-06-12 _audit_creation_method CRYSTALS_ver_12.83 _chemical_compound_source ' C. Milios, CM1691' _exptl_crystal_recrystallization_method ; Slow evaporation of a CH3CN solution ; _oxford_structure_analysis_title 'eb6059 in P 1 21/c 1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.6720(4) _cell_length_b 19.6080(6) _cell_length_c 27.9570(9) _cell_angle_alpha 90 _cell_angle_beta 103.6350(10) _cell_angle_gamma 90 _cell_volume 7283.5(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C71 H74.50 Mn4 N11.50 O16 # Dc = 1.43 Fooo = 2912.00 Mu = 7.52 M = 1564.65 # Found Formula = C64 H60 Mn4 N8 O16 # Dc = 1.29 FOOO = 2912.00 Mu = 7.43 M = 1416.94 _chemical_formula_sum 'C71 H74.5 Mn4 N11.5 O16' _chemical_formula_moiety '[Mn4(MeSaO)4(MeSaOH)4].3.5(CH3CN)' _chemical_formula_weight 1563.1 _cell_measurement_reflns_used 8771 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_min 0.21 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_max 0.52 _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 0.743 # Sheldrick geometric approximatio 0.81 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 71703 _reflns_number_total 22020 _diffrn_reflns_av_R_equivalents 0.054 # Number of reflections with Friedels Law is 22020 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 22505 _diffrn_reflns_theta_min 1.499 _diffrn_reflns_theta_max 30.649 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.810 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 40 _reflns_limit_h_min -19 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 40 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.39 _refine_diff_density_max 0.72 _refine_ls_number_reflns 13218 _refine_ls_number_restraints 0 _refine_ls_number_parameters 829 #_refine_ls_R_factor_ref 0.0465 _refine_ls_wR_factor_ref 0.0475 _refine_ls_goodness_of_fit_ref 1.1297 #_reflns_number_all 21961 _refine_ls_R_factor_all 0.0830 _refine_ls_wR_factor_all 0.0540 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 13218 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_gt 0.0475 _refine_ls_shift/su_max 0.000909 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.90 0.914 1.62 ; # SQUEEZE RESULTS (APPEND TO CIF) 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 0.000 834.3 149.5 2 0.000 0.000 0.500 834.3 148.7 _platon_squeeze_details ; This equates to ca 7(CH3CN) molecules per formula unit (298 e/cell) ; _publ_section_exptl_refinement ; The hydrogens were placed geometrically, then refined subject to geometric restraints and finally constrained to ride on their host atoms. Disordered solved was treated with the Squeeae procedure (see above). Checkcif output: 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 493 A data collection strategy has been used aimed to achieve a complete data set. Some higher angle data were collected in the process, but these are generally weak, and were excluded from the refinement. (They are, however, included in the fcf file). #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 7625 7623 2 23.01 0.550 1.000 10145 10143 2 25.24 0.600 1.000 13187 13185 2 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 16762 16759 3 29.84 0.700 0.988 20933 20685 248 30.65 0.717 0.978 22515 22020 495 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.82 Sadabs corrects for all systematic errors that lead to disparities in the intensities of equivalent data. It is possible that the larger than expected range of transmission is accounted for by crystal decay or absorption by the mounting fibre. 232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn4 - O24 .. 5.23 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn4 - N15 .. 5.11 su Directly bonded N, O to Metal bonds often give rise to the above alert, as the metal atom usually exhibit a spherical anisotropic thermal parameter. 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C46 This is alert can be due to some thermal motion of the aromatic ring 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! Squeeze procedure used to treat solvent. see above. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.10 Ratio 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C68 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O11 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N12 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 1 911_ALERT_3_C # Missing FCF Refl. Between TH(Min) & STH/L=0.6 1 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 2 No action taken ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mn1 Mn 0.44289(2) 0.194236(17) 0.061188(11) 0.0205 1.0000 Uani . . . . . . Mn2 Mn 0.36978(2) 0.315516(16) 0.141125(12) 0.0202 1.0000 Uani . . . . . . Mn3 Mn 0.20324(2) 0.265794(16) 0.007877(12) 0.0205 1.0000 Uani . . . . . . Mn4 Mn 0.20343(2) 0.173968(16) 0.118095(12) 0.0206 1.0000 Uani . . . . . . O25 O 0.27706(11) 0.18120(7) 0.02937(5) 0.0213 1.0000 Uani . . . . . . O11 O 0.45237(11) 0.20747(9) -0.00471(6) 0.0261 1.0000 Uani . . . . . . O22 O 0.35828(11) 0.21633(8) 0.14562(5) 0.0216 1.0000 Uani . . . . . . O13 O 0.51022(11) 0.31579(8) 0.17039(6) 0.0247 1.0000 Uani . . . . . . O14 O 0.36564(12) 0.40890(8) 0.12882(6) 0.0259 1.0000 Uani . . . . . . O24 O 0.17897(11) 0.26252(7) 0.08479(6) 0.0221 1.0000 Uani . . . . . . O16 O 0.07690(11) 0.22045(8) -0.01205(6) 0.0244 1.0000 Uani . . . . . . O17 O 0.17138(13) 0.20633(8) 0.17684(6) 0.0277 1.0000 Uani . . . . . . O23 O 0.28145(14) 0.29584(10) 0.23756(6) 0.0359 1.0000 Uani . . . . . . N14 N 0.22007(13) 0.31748(9) 0.11416(6) 0.0211 1.0000 Uani . . . . . . O21 O 0.64159(13) 0.27871(11) 0.11772(7) 0.0378 1.0000 Uani . . . . . . O12 O 0.47913(12) 0.10286(8) 0.06177(6) 0.0276 1.0000 Uani . . . . . . O26 O 0.30081(13) 0.21891(12) -0.08196(6) 0.0397 1.0000 Uani . . . . . . O15 O 0.22974(12) 0.08507(8) 0.14193(6) 0.0264 1.0000 Uani . . . . . . O28 O 0.40213(11) 0.28842(8) 0.06891(5) 0.0223 1.0000 Uani . . . . . . N12 N 0.43416(13) 0.18045(9) 0.13098(7) 0.0219 1.0000 Uani . . . . . . N13 N 0.35836(15) 0.32546(10) 0.21965(7) 0.0272 1.0000 Uani . . . . . . O18 O 0.14577(12) 0.35110(8) -0.00934(6) 0.0285 1.0000 Uani . . . . . . O27 O -0.02261(13) 0.15992(10) 0.05003(7) 0.0336 1.0000 Uani . . . . . . N18 N 0.33512(13) 0.31553(9) 0.02818(6) 0.0216 1.0000 Uani . . . . . . N11 N 0.60363(14) 0.23636(10) 0.07766(7) 0.0262 1.0000 Uani . . . . . . C78 C 0.36182(17) 0.37272(11) 0.01146(8) 0.0256 1.0000 Uani . . . . . . N15 N 0.22743(13) 0.13798(9) 0.05473(7) 0.0209 1.0000 Uani . . . . . . N16 N 0.21212(14) 0.23869(10) -0.06981(7) 0.0276 1.0000 Uani . . . . . . C68 C 0.28893(18) 0.40752(11) -0.02771(9) 0.0275 1.0000 Uani . . . . . . C72 C 0.48799(17) 0.14018(11) 0.16326(8) 0.0251 1.0000 Uani . . . . . . N17 N 0.03496(14) 0.15616(10) 0.09846(7) 0.0265 1.0000 Uani . . . . . . C86 C 0.1438(2) 0.2065(2) -0.15513(10) 0.0497 1.0000 Uani . . . . . . C18 C 0.18436(18) 0.39495(11) -0.03629(8) 0.0268 1.0000 Uani . . . . . . C21 C 0.50624(18) 0.13232(14) -0.05951(9) 0.0311 1.0000 Uani . . . . . . C62 C 0.55933(17) 0.09445(11) 0.14857(9) 0.0265 1.0000 Uani . . . . . . C34 C 0.2731(2) 0.55618(13) 0.18130(11) 0.0389 1.0000 Uani . . . . . . C61 C 0.62995(17) 0.19158(12) 0.00288(8) 0.0253 1.0000 Uani . . . . . . C13 C 0.54835(17) 0.36966(12) 0.19876(8) 0.0266 1.0000 Uani . . . . . . C48 C 0.2556(2) 0.49294(15) -0.09210(10) 0.0420 1.0000 Uani . . . . . . C75 C 0.20800(15) 0.07706(11) 0.03695(8) 0.0232 1.0000 Uani . . . . . . C74 C 0.15886(17) 0.36691(11) 0.11685(9) 0.0267 1.0000 Uani . . . . . . C83 C 0.4192(2) 0.35577(16) 0.30605(10) 0.0430 1.0000 Uani . . . . . . C24 C 0.33555(19) 0.51247(12) 0.16408(9) 0.0315 1.0000 Uani . . . . . . C15 C 0.17712(16) 0.03428(11) 0.11640(9) 0.0254 1.0000 Uani . . . . . . C17 C 0.12843(19) 0.16264(12) 0.20270(9) 0.0299 1.0000 Uani . . . . . . C35 C 0.0777(2) -0.06754(13) 0.11612(12) 0.0393 1.0000 Uani . . . . . . C71 C 0.65963(16) 0.23628(12) 0.04647(9) 0.0273 1.0000 Uani . . . . . . C11 C 0.52863(16) 0.17676(12) -0.01977(8) 0.0242 1.0000 Uani . . . . . . C76 C 0.13466(18) 0.23291(13) -0.10610(8) 0.0294 1.0000 Uani . . . . . . C16 C 0.01104(17) 0.24484(11) -0.05187(9) 0.0269 1.0000 Uani . . . . . . C28 C 0.1178(2) 0.43160(13) -0.07275(10) 0.0349 1.0000 Uani . . . . . . C64 C 0.20007(18) 0.42979(12) 0.14144(10) 0.0297 1.0000 Uani . . . . . . C77 C -0.01402(17) 0.13314(13) 0.12911(10) 0.0317 1.0000 Uani . . . . . . C67 C 0.03922(19) 0.12682(13) 0.18130(10) 0.0322 1.0000 Uani . . . . . . C73 C 0.42508(18) 0.35569(12) 0.25312(8) 0.0281 1.0000 Uani . . . . . . C41 C 0.6814(2) 0.11825(15) -0.05678(10) 0.0358 1.0000 Uani . . . . . . C57 C -0.0002(2) 0.08241(16) 0.21147(12) 0.0451 1.0000 Uani . . . . . . C63 C 0.50893(18) 0.39087(12) 0.23876(9) 0.0296 1.0000 Uani . . . . . . C85 C 0.2344(2) 0.05813(13) -0.01020(10) 0.0331 1.0000 Uani . . . . . . C56 C -0.0385(2) 0.27732(19) -0.13687(12) 0.0520 1.0000 Uani . . . . . . C42 C 0.7016(2) 0.01631(14) 0.17117(11) 0.0379 1.0000 Uani . . . . . . C65 C 0.16187(16) 0.02853(11) 0.06484(9) 0.0256 1.0000 Uani . . . . . . C31 C 0.5817(2) 0.10288(14) -0.07773(9) 0.0352 1.0000 Uani . . . . . . C51 C 0.70501(17) 0.16186(13) -0.01721(9) 0.0304 1.0000 Uani . . . . . . C45 C 0.05936(19) -0.07213(12) 0.06557(11) 0.0359 1.0000 Uani . . . . . . C58 C 0.3226(2) 0.45743(14) -0.05663(9) 0.0357 1.0000 Uani . . . . . . C22 C 0.61433(18) 0.02759(13) 0.08635(10) 0.0316 1.0000 Uani . . . . . . C43 C 0.6355(2) 0.48065(15) 0.25638(11) 0.0432 1.0000 Uani . . . . . . C12 C 0.54908(17) 0.07680(11) 0.09821(9) 0.0261 1.0000 Uani . . . . . . C55 C 0.10302(17) -0.02505(11) 0.04011(10) 0.0296 1.0000 Uani . . . . . . C33 C 0.6745(2) 0.45857(15) 0.21833(11) 0.0421 1.0000 Uani . . . . . . C82 C 0.4735(2) 0.14044(15) 0.21472(10) 0.0409 1.0000 Uani . . . . . . C32 C 0.68804(19) -0.00201(13) 0.12226(11) 0.0369 1.0000 Uani . . . . . . C44 C 0.1747(2) 0.53715(15) 0.18042(13) 0.0480 1.0000 Uani . . . . . . C14 C 0.30148(18) 0.44835(11) 0.14452(8) 0.0260 1.0000 Uani . . . . . . C53 C 0.5544(2) 0.44699(14) 0.26648(10) 0.0398 1.0000 Uani . . . . . . C47 C 0.0468(3) 0.07267(18) 0.26067(12) 0.0518 1.0000 Uani . . . . . . C27 C 0.1735(2) 0.15331(15) 0.25240(10) 0.0383 1.0000 Uani . . . . . . C52 C 0.63690(19) 0.06408(13) 0.18356(10) 0.0342 1.0000 Uani . . . . . . C88 C 0.46330(18) 0.40274(13) 0.03288(9) 0.0324 1.0000 Uani . . . . . . C25 C 0.1362(2) -0.01607(13) 0.14182(10) 0.0346 1.0000 Uani . . . . . . C38 C 0.1532(2) 0.48012(14) -0.10032(10) 0.0410 1.0000 Uani . . . . . . C37 C 0.1338(2) 0.10868(18) 0.28146(11) 0.0488 1.0000 Uani . . . . . . C81 C 0.7519(2) 0.27956(17) 0.05308(12) 0.0463 1.0000 Uani . . . . . . C23 C 0.6318(2) 0.40371(14) 0.18931(10) 0.0361 1.0000 Uani . . . . . . C66 C 0.03569(18) 0.25208(12) -0.09791(10) 0.0314 1.0000 Uani . . . . . . C26 C -0.0861(2) 0.26105(14) -0.04761(12) 0.0389 1.0000 Uani . . . . . . C84 C 0.04922(19) 0.36008(14) 0.09217(11) 0.0374 1.0000 Uani . . . . . . C54 C 0.1391(2) 0.47518(14) 0.16044(13) 0.0431 1.0000 Uani . . . . . . C87 C -0.1217(2) 0.1106(2) 0.11268(13) 0.0543 1.0000 Uani . . . . . . C36 C -0.1576(2) 0.2847(2) -0.08740(16) 0.0598 1.0000 Uani . . . . . . C46 C -0.1332(3) 0.2936(2) -0.13168(16) 0.0723 1.0000 Uani . . . . . . H211 H 0.4388 0.1229 -0.0742 0.0381 1.0000 Uiso . . . . . . H341 H 0.2973 0.5986 0.1934 0.0470 1.0000 Uiso . . . . . . H481 H 0.2799 0.5255 -0.1105 0.0512 1.0000 Uiso . . . . . . H831 H 0.4815 0.3403 0.3266 0.0661 1.0000 Uiso . . . . . . H832 H 0.4070 0.4017 0.3160 0.0661 1.0000 Uiso . . . . . . H833 H 0.3654 0.3273 0.3105 0.0662 1.0000 Uiso . . . . . . H241 H 0.4014 0.5255 0.1655 0.0388 1.0000 Uiso . . . . . . H351 H 0.0496 -0.0998 0.1337 0.0464 1.0000 Uiso . . . . . . H281 H 0.0494 0.4229 -0.0779 0.0421 1.0000 Uiso . . . . . . H411 H 0.7319 0.0993 -0.0694 0.0450 1.0000 Uiso . . . . . . H571 H -0.0603 0.0593 0.1980 0.0577 1.0000 Uiso . . . . . . H561 H -0.0221 0.2838 -0.1666 0.0617 1.0000 Uiso . . . . . . H421 H 0.7528 -0.0029 0.1952 0.0460 1.0000 Uiso . . . . . . H311 H 0.5664 0.0729 -0.1037 0.0432 1.0000 Uiso . . . . . . H511 H 0.7718 0.1730 -0.0036 0.0390 1.0000 Uiso . . . . . . H451 H 0.0188 -0.1067 0.0487 0.0419 1.0000 Uiso . . . . . . H581 H 0.3914 0.4667 -0.0522 0.0440 1.0000 Uiso . . . . . . H221 H 0.6066 0.0147 0.0537 0.0401 1.0000 Uiso . . . . . . H431 H 0.6641 0.5168 0.2750 0.0502 1.0000 Uiso . . . . . . H551 H 0.0920 -0.0302 0.0062 0.0337 1.0000 Uiso . . . . . . H331 H 0.7299 0.4806 0.2122 0.0510 1.0000 Uiso . . . . . . H821 H 0.5147 0.1071 0.2348 0.0639 1.0000 Uiso . . . . . . H822 H 0.4915 0.1842 0.2300 0.0642 1.0000 Uiso . . . . . . H823 H 0.4041 0.1313 0.2143 0.0639 1.0000 Uiso . . . . . . H321 H 0.7296 -0.0348 0.1139 0.0470 1.0000 Uiso . . . . . . H441 H 0.1332 0.5666 0.1933 0.0610 1.0000 Uiso . . . . . . H531 H 0.5285 0.4619 0.2926 0.0481 1.0000 Uiso . . . . . . H471 H 0.0201 0.0418 0.2790 0.0678 1.0000 Uiso . . . . . . H271 H 0.2311 0.1783 0.2666 0.0471 1.0000 Uiso . . . . . . H521 H 0.6450 0.0770 0.2163 0.0422 1.0000 Uiso . . . . . . H251 H 0.1483 -0.0148 0.1761 0.0410 1.0000 Uiso . . . . . . H381 H 0.1067 0.5035 -0.1246 0.0487 1.0000 Uiso . . . . . . H371 H 0.1655 0.1023 0.3148 0.0611 1.0000 Uiso . . . . . . H811 H 0.7651 0.2908 0.0222 0.0748 1.0000 Uiso . . . . . . H812 H 0.8084 0.2535 0.0722 0.0749 1.0000 Uiso . . . . . . H813 H 0.7450 0.3203 0.0713 0.0750 1.0000 Uiso . . . . . . H231 H 0.6592 0.3892 0.1633 0.0438 1.0000 Uiso . . . . . . H261 H -0.1026 0.2565 -0.0173 0.0467 1.0000 Uiso . . . . . . H541 H 0.0739 0.4622 0.1604 0.0530 1.0000 Uiso . . . . . . H361 H -0.2227 0.2947 -0.0840 0.0729 1.0000 Uiso . . . . . . H461 H -0.1812 0.3098 -0.1584 0.0831 1.0000 Uiso . . . . . . H851 H 0.2173 0.0116 -0.0184 0.0530 1.0000 Uiso . . . . . . H852 H 0.3056 0.0632 -0.0070 0.0530 1.0000 Uiso . . . . . . H853 H 0.1980 0.0865 -0.0363 0.0529 1.0000 Uiso . . . . . . H881 H 0.4653 0.4473 0.0191 0.0497 1.0000 Uiso . . . . . . H882 H 0.4731 0.4061 0.0683 0.0498 1.0000 Uiso . . . . . . H883 H 0.5142 0.3745 0.0246 0.0493 1.0000 Uiso . . . . . . H841 H 0.0138 0.3997 0.0991 0.0548 1.0000 Uiso . . . . . . H842 H 0.0415 0.3564 0.0571 0.0550 1.0000 Uiso . . . . . . H843 H 0.0208 0.3207 0.1038 0.0553 1.0000 Uiso . . . . . . H861 H 0.0794 0.2017 -0.1772 0.0730 1.0000 Uiso . . . . . . H862 H 0.1845 0.2355 -0.1695 0.0731 1.0000 Uiso . . . . . . H863 H 0.1754 0.1628 -0.1504 0.0733 1.0000 Uiso . . . . . . H871 H -0.1467 0.0991 0.1410 0.0812 1.0000 Uiso . . . . . . H872 H -0.1603 0.1466 0.0941 0.0813 1.0000 Uiso . . . . . . H873 H -0.1233 0.0709 0.0918 0.0813 1.0000 Uiso . . . . . . H14 H 0.2444 0.2715 0.2174 0.0575 1.0000 Uiso . . . . . . H18 H 0.0153 0.1745 0.0332 0.0524 1.0000 Uiso . . . . . . H31 H 0.6023 0.2784 0.1358 0.0573 1.0000 Uiso . . . . . . H62 H 0.3458 0.2114 -0.0568 0.0603 1.0000 Uiso . . . . . . 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 0.01808(14) 0.02525(15) 0.01934(14) -0.00326(11) 0.00661(11) -0.00216(11) Mn2 0.01937(14) 0.02115(14) 0.02122(14) -0.00406(11) 0.00708(11) -0.00441(11) Mn3 0.01769(14) 0.02072(14) 0.02371(15) -0.00098(12) 0.00640(11) -0.00446(11) Mn4 0.02112(15) 0.01987(14) 0.02257(14) -0.00222(11) 0.00878(11) -0.00519(11) O25 0.0180(6) 0.0248(7) 0.0232(7) 0.0000(6) 0.0089(5) -0.0040(5) O11 0.0176(7) 0.0393(9) 0.0226(7) -0.0013(6) 0.0070(6) 0.0024(6) O22 0.0206(7) 0.0230(7) 0.0237(7) -0.0033(5) 0.0105(6) -0.0016(5) O13 0.0207(7) 0.0288(8) 0.0245(7) -0.0083(6) 0.0051(6) -0.0052(6) O14 0.0251(7) 0.0236(7) 0.0317(8) -0.0041(6) 0.0119(6) -0.0051(6) O24 0.0217(7) 0.0214(7) 0.0248(7) -0.0047(6) 0.0085(6) -0.0058(5) O16 0.0191(7) 0.0246(7) 0.0286(8) 0.0006(6) 0.0038(6) -0.0055(6) O17 0.0337(8) 0.0269(8) 0.0269(8) -0.0023(6) 0.0159(7) -0.0090(6) O23 0.0397(10) 0.0446(10) 0.0286(8) -0.0106(7) 0.0187(7) -0.0167(8) N14 0.0217(8) 0.0220(8) 0.0210(8) -0.0039(6) 0.0078(6) -0.0059(6) O21 0.0258(8) 0.0548(11) 0.0339(9) -0.0209(8) 0.0094(7) -0.0128(8) O12 0.0278(8) 0.0284(8) 0.0263(8) -0.0068(6) 0.0059(6) -0.0002(6) O26 0.0238(8) 0.0713(14) 0.0245(8) 0.0005(8) 0.0068(6) 0.0072(8) O15 0.0262(8) 0.0250(7) 0.0276(8) 0.0013(6) 0.0057(6) -0.0036(6) O28 0.0226(7) 0.0258(7) 0.0186(7) -0.0030(5) 0.0050(5) -0.0026(6) N12 0.0208(8) 0.0227(8) 0.0238(8) -0.0050(7) 0.0085(6) -0.0042(6) N13 0.0322(10) 0.0275(9) 0.0250(9) -0.0035(7) 0.0134(8) -0.0042(7) O18 0.0268(8) 0.0239(7) 0.0356(9) 0.0022(6) 0.0091(7) -0.0012(6) O27 0.0244(8) 0.0444(10) 0.0328(9) 0.0019(7) 0.0084(7) -0.0111(7) N18 0.0192(8) 0.0243(8) 0.0217(8) -0.0014(7) 0.0056(6) -0.0033(6) N11 0.0203(8) 0.0331(10) 0.0246(9) -0.0070(7) 0.0041(7) -0.0040(7) C78 0.0261(10) 0.0272(10) 0.0258(10) -0.0032(8) 0.0108(8) -0.0073(8) N15 0.0171(8) 0.0219(8) 0.0243(8) 0.0004(6) 0.0064(6) -0.0029(6) N16 0.0234(9) 0.0342(10) 0.0256(9) 0.0017(8) 0.0067(7) 0.0018(7) C68 0.0328(12) 0.0237(10) 0.0265(10) -0.0012(8) 0.0081(9) -0.0046(8) C72 0.0260(10) 0.0250(10) 0.0247(10) -0.0031(8) 0.0070(8) -0.0040(8) N17 0.0228(9) 0.0270(9) 0.0304(9) 0.0001(7) 0.0079(7) -0.0056(7) C86 0.0376(15) 0.087(2) 0.0233(12) 0.0018(13) 0.0044(10) 0.0011(15) C18 0.0306(11) 0.0228(10) 0.0277(10) -0.0040(8) 0.0083(9) -0.0030(8) C21 0.0268(11) 0.0428(13) 0.0239(10) -0.0014(9) 0.0063(8) 0.0065(9) C62 0.0241(10) 0.0268(10) 0.0293(11) 0.0003(8) 0.0080(8) -0.0009(8) C34 0.0420(14) 0.0271(11) 0.0469(15) -0.0146(10) 0.0091(12) -0.0038(10) C61 0.0225(10) 0.0307(10) 0.0237(10) 0.0013(8) 0.0071(8) 0.0004(8) C13 0.0243(10) 0.0297(11) 0.0241(10) -0.0057(8) 0.0023(8) -0.0047(8) C48 0.0567(17) 0.0368(13) 0.0351(13) 0.0087(11) 0.0158(12) -0.0047(12) C75 0.0169(9) 0.0253(10) 0.0277(10) -0.0032(8) 0.0055(8) 0.0003(7) C74 0.0228(10) 0.0250(10) 0.0342(11) -0.0011(8) 0.0104(9) -0.0023(8) C83 0.0542(17) 0.0524(16) 0.0245(11) -0.0096(11) 0.0136(11) -0.0072(13) C24 0.0349(12) 0.0256(10) 0.0330(12) -0.0049(9) 0.0058(10) -0.0050(9) C15 0.0202(9) 0.0210(9) 0.0350(11) 0.0029(8) 0.0063(8) -0.0003(7) C17 0.0347(12) 0.0295(11) 0.0309(11) 0.0007(9) 0.0188(10) -0.0058(9) C35 0.0341(13) 0.0250(11) 0.0572(17) 0.0125(11) 0.0077(12) -0.0064(9) C71 0.0174(9) 0.0320(11) 0.0327(11) -0.0022(9) 0.0061(8) -0.0010(8) C11 0.0221(10) 0.0328(11) 0.0195(9) 0.0030(8) 0.0084(7) 0.0024(8) C76 0.0270(11) 0.0351(12) 0.0249(10) 0.0070(9) 0.0039(8) -0.0008(9) C16 0.0217(10) 0.0201(9) 0.0377(12) -0.0014(8) 0.0047(9) -0.0046(7) C28 0.0367(13) 0.0308(12) 0.0364(13) -0.0016(10) 0.0068(10) 0.0028(10) C64 0.0263(11) 0.0271(10) 0.0375(12) -0.0052(9) 0.0112(9) -0.0015(8) C77 0.0233(11) 0.0336(12) 0.0412(13) 0.0040(10) 0.0134(9) -0.0067(9) C67 0.0296(11) 0.0347(12) 0.0379(13) 0.0045(10) 0.0190(10) -0.0035(9) C73 0.0338(12) 0.0287(10) 0.0216(10) -0.0058(8) 0.0065(8) 0.0005(9) C41 0.0318(12) 0.0456(14) 0.0329(12) 0.0010(10) 0.0133(10) 0.0158(11) C57 0.0402(15) 0.0500(16) 0.0509(17) 0.0105(13) 0.0225(13) -0.0131(12) C63 0.0291(11) 0.0318(11) 0.0273(11) -0.0073(9) 0.0053(9) -0.0046(9) C85 0.0359(13) 0.0317(12) 0.0349(12) -0.0119(10) 0.0144(10) -0.0031(10) C56 0.0359(14) 0.066(2) 0.0483(17) 0.0296(15) -0.0008(12) 0.0046(14) C42 0.0306(12) 0.0361(13) 0.0461(15) 0.0065(11) 0.0073(11) 0.0045(10) C65 0.0209(10) 0.0203(9) 0.0354(11) -0.0022(8) 0.0063(8) -0.0016(7) C31 0.0387(13) 0.0447(14) 0.0218(10) -0.0018(10) 0.0062(9) 0.0134(11) C51 0.0196(10) 0.0394(12) 0.0337(12) -0.0023(10) 0.0096(9) 0.0034(9) C45 0.0271(11) 0.0231(10) 0.0548(16) 0.0002(10) 0.0043(11) -0.0050(9) C58 0.0429(14) 0.0366(13) 0.0289(12) 0.0029(10) 0.0109(10) -0.0112(11) C22 0.0268(11) 0.0293(11) 0.0413(13) -0.0033(10) 0.0132(10) 0.0016(9) C43 0.0397(14) 0.0393(14) 0.0469(15) -0.0194(12) 0.0030(12) -0.0130(11) C12 0.0243(10) 0.0230(10) 0.0330(11) -0.0029(8) 0.0107(9) -0.0026(8) C55 0.0246(10) 0.0215(10) 0.0405(13) -0.0037(9) 0.0031(9) 0.0000(8) C33 0.0362(14) 0.0410(14) 0.0477(15) -0.0121(12) 0.0075(12) -0.0189(11) C82 0.0539(16) 0.0457(15) 0.0268(12) 0.0087(11) 0.0169(11) 0.0134(13) C32 0.0282(12) 0.0293(12) 0.0571(17) -0.0015(11) 0.0182(11) 0.0013(9) C44 0.0503(17) 0.0345(14) 0.0632(19) -0.0184(13) 0.0211(15) 0.0020(12) C14 0.0300(11) 0.0232(10) 0.0259(10) -0.0034(8) 0.0089(8) -0.0032(8) C53 0.0408(14) 0.0400(14) 0.0369(14) -0.0171(11) 0.0056(11) -0.0055(11) C47 0.0515(18) 0.0610(19) 0.0498(17) 0.0189(15) 0.0257(14) -0.0115(15) C27 0.0410(14) 0.0460(14) 0.0308(12) 0.0034(11) 0.0143(11) -0.0074(11) C52 0.0309(12) 0.0332(12) 0.0374(13) 0.0045(10) 0.0059(10) 0.0044(9) C88 0.0252(11) 0.0382(13) 0.0327(12) 0.0034(10) 0.0048(9) -0.0113(9) C25 0.0355(13) 0.0275(11) 0.0412(13) 0.0080(10) 0.0097(10) -0.0041(9) C38 0.0546(17) 0.0330(13) 0.0334(13) 0.0044(10) 0.0064(12) 0.0027(12) C37 0.0496(17) 0.0646(19) 0.0372(15) 0.0147(14) 0.0201(13) -0.0041(14) C81 0.0314(13) 0.0543(17) 0.0598(18) -0.0201(14) 0.0239(13) -0.0174(12) C23 0.0365(13) 0.0400(13) 0.0337(12) -0.0090(10) 0.0123(10) -0.0119(10) C66 0.0236(11) 0.0293(11) 0.0378(13) 0.0090(9) 0.0006(9) -0.0023(8) C26 0.0273(12) 0.0354(13) 0.0548(17) 0.0040(12) 0.0111(11) 0.0043(10) C84 0.0261(12) 0.0325(12) 0.0535(16) -0.0110(11) 0.0092(11) -0.0028(9) C54 0.0346(14) 0.0341(13) 0.0658(19) -0.0129(13) 0.0224(13) 0.0001(11) C87 0.0296(14) 0.081(2) 0.0528(18) 0.0114(17) 0.0100(12) -0.0229(14) C36 0.0269(14) 0.068(2) 0.082(3) 0.0211(19) 0.0088(15) 0.0170(14) C46 0.0351(16) 0.093(3) 0.079(3) 0.049(2) -0.0056(16) 0.0205(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2046(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . O25 . 2.2464(15) yes Mn1 . O11 . 1.8949(16) yes Mn1 . O12 . 1.8580(17) yes Mn1 . O28 . 1.9556(16) yes Mn1 . N12 . 2.0011(18) yes Mn1 . N11 . 2.2907(18) yes Mn2 . O22 . 1.9576(15) yes Mn2 . O13 . 1.9015(15) yes Mn2 . O14 . 1.8615(16) yes Mn2 . N14 . 2.0080(18) yes Mn2 . O28 . 2.2304(15) yes Mn2 . N13 . 2.2457(19) yes Mn3 . O25 . 1.9608(15) yes Mn3 . O24 . 2.2526(15) yes Mn3 . O16 . 1.9055(15) yes Mn3 . O18 . 1.8625(16) yes Mn3 . N18 . 2.0104(17) yes Mn3 . N16 . 2.267(2) yes Mn4 . O22 . 2.2352(15) yes Mn4 . O24 . 1.9614(16) yes Mn4 . O17 . 1.9056(16) yes Mn4 . O15 . 1.8706(16) yes Mn4 . N15 . 2.0044(18) yes Mn4 . N17 . 2.2655(19) yes O25 . N15 . 1.381(2) yes O11 . C11 . 1.354(3) yes O22 . N12 . 1.392(2) yes O13 . C13 . 1.350(3) yes O14 . C14 . 1.320(3) yes O24 . N14 . 1.391(2) yes O16 . C16 . 1.344(3) yes O17 . C17 . 1.342(3) yes O23 . N13 . 1.393(2) yes O23 . H14 . 0.816 no N14 . C74 . 1.294(3) yes O21 . N11 . 1.393(2) yes O21 . H31 . 0.820 no O12 . C12 . 1.324(3) yes O26 . N16 . 1.389(3) yes O26 . H62 . 0.831 no O15 . C15 . 1.333(3) yes O28 . N18 . 1.388(2) yes N12 . C72 . 1.291(3) yes N13 . C73 . 1.287(3) yes O18 . C18 . 1.331(3) yes O27 . N17 . 1.398(3) yes O27 . H18 . 0.828 no N18 . C78 . 1.300(3) yes N11 . C71 . 1.289(3) yes C78 . C68 . 1.464(3) yes C78 . C88 . 1.496(3) yes N15 . C75 . 1.297(3) yes N16 . C76 . 1.287(3) yes C68 . C18 . 1.414(3) yes C68 . C58 . 1.414(3) yes C72 . C62 . 1.454(3) yes C72 . C82 . 1.498(3) yes N17 . C77 . 1.287(3) yes C86 . C76 . 1.498(4) yes C86 . H861 . 0.953 no C86 . H862 . 0.949 no C86 . H863 . 0.953 no C18 . C28 . 1.395(4) yes C21 . C11 . 1.388(3) yes C21 . C31 . 1.380(3) yes C21 . H211 . 0.935 no C62 . C12 . 1.424(3) yes C62 . C52 . 1.395(3) yes C34 . C24 . 1.375(4) yes C34 . C44 . 1.391(4) yes C34 . H341 . 0.929 no C61 . C71 . 1.478(3) yes C61 . C11 . 1.411(3) yes C61 . C51 . 1.407(3) yes C13 . C63 . 1.413(3) yes C13 . C23 . 1.399(3) yes C48 . C58 . 1.371(4) yes C48 . C38 . 1.387(4) yes C48 . H481 . 0.929 no C75 . C85 . 1.493(3) yes C75 . C65 . 1.464(3) yes C74 . C64 . 1.459(3) yes C74 . C84 . 1.501(3) yes C83 . C73 . 1.501(3) yes C83 . H831 . 0.958 no C83 . H832 . 0.969 no C83 . H833 . 0.954 no C24 . C14 . 1.406(3) yes C24 . H241 . 0.927 no C15 . C65 . 1.412(3) yes C15 . C25 . 1.407(3) yes C17 . C67 . 1.412(3) yes C17 . C27 . 1.393(4) yes C35 . C45 . 1.379(4) yes C35 . C25 . 1.379(4) yes C35 . H351 . 0.937 no C71 . C81 . 1.495(3) yes C76 . C66 . 1.473(3) yes C16 . C66 . 1.412(4) yes C16 . C26 . 1.397(3) yes C28 . C38 . 1.382(4) yes C28 . H281 . 0.927 no C64 . C14 . 1.416(3) yes C64 . C54 . 1.406(3) yes C77 . C67 . 1.474(4) yes C77 . C87 . 1.502(4) yes C67 . C57 . 1.405(3) yes C73 . C63 . 1.473(3) yes C41 . C31 . 1.384(4) yes C41 . C51 . 1.375(4) yes C41 . H411 . 0.924 no C57 . C47 . 1.387(5) yes C57 . H571 . 0.936 no C63 . C53 . 1.404(3) yes C85 . H851 . 0.956 no C85 . H852 . 0.962 no C85 . H853 . 0.958 no C56 . C66 . 1.393(4) yes C56 . C46 . 1.374(5) yes C56 . H561 . 0.919 no C42 . C32 . 1.384(4) yes C42 . C52 . 1.387(4) yes C42 . H421 . 0.928 no C65 . C55 . 1.402(3) yes C31 . H311 . 0.920 no C51 . H511 . 0.929 no C45 . C55 . 1.384(4) yes C45 . H451 . 0.931 no C58 . H581 . 0.938 no C22 . C12 . 1.406(3) yes C22 . C32 . 1.372(4) yes C22 . H221 . 0.928 no C43 . C33 . 1.367(4) yes C43 . C53 . 1.376(4) yes C43 . H431 . 0.912 no C55 . H551 . 0.931 no C33 . C23 . 1.391(4) yes C33 . H331 . 0.923 no C82 . H821 . 0.954 no C82 . H822 . 0.964 no C82 . H823 . 0.963 no C32 . H321 . 0.924 no C44 . C54 . 1.377(4) yes C44 . H441 . 0.939 no C53 . H531 . 0.930 no C47 . C37 . 1.388(5) yes C47 . H471 . 0.923 no C27 . C37 . 1.389(4) yes C27 . H271 . 0.934 no C52 . H521 . 0.932 no C88 . H881 . 0.958 no C88 . H882 . 0.969 no C88 . H883 . 0.960 no C25 . H251 . 0.934 no C38 . H381 . 0.934 no C37 . H371 . 0.938 no C81 . H811 . 0.948 no C81 . H812 . 0.974 no C81 . H813 . 0.964 no C23 . H231 . 0.937 no C26 . C36 . 1.377(4) yes C26 . H261 . 0.932 no C84 . H841 . 0.959 no C84 . H842 . 0.965 no C84 . H843 . 0.956 no C54 . H541 . 0.927 no C87 . H871 . 0.961 no C87 . H872 . 0.959 no C87 . H873 . 0.970 no C36 . C46 . 1.367(6) yes C36 . H361 . 0.938 no C46 . H461 . 0.926 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O25 . Mn1 . O11 . 85.68(6) yes O25 . Mn1 . O12 . 97.81(6) yes O11 . Mn1 . O12 . 93.51(7) yes O25 . Mn1 . O28 . 82.18(6) yes O11 . Mn1 . O28 . 93.71(7) yes O12 . Mn1 . O28 . 172.76(7) yes O25 . Mn1 . N12 . 94.83(6) yes O11 . Mn1 . N12 . 179.50(7) yes O12 . Mn1 . N12 . 86.46(7) yes O28 . Mn1 . N12 . 86.33(7) yes O25 . Mn1 . N11 . 162.10(7) yes O11 . Mn1 . N11 . 82.17(7) yes O12 . Mn1 . N11 . 96.01(7) yes O28 . Mn1 . N11 . 85.54(7) yes N12 . Mn1 . N11 . 97.33(7) yes O22 . Mn2 . O13 . 93.63(7) yes O22 . Mn2 . O14 . 171.77(7) yes O13 . Mn2 . O14 . 93.46(7) yes O22 . Mn2 . N14 . 87.30(7) yes O13 . Mn2 . N14 . 176.45(7) yes O14 . Mn2 . N14 . 85.86(7) yes O22 . Mn2 . O28 . 81.80(6) yes O13 . Mn2 . O28 . 89.69(6) yes O14 . Mn2 . O28 . 94.07(6) yes N14 . Mn2 . O28 . 93.83(6) yes O22 . Mn2 . N13 . 89.91(7) yes O13 . Mn2 . N13 . 82.82(7) yes O14 . Mn2 . N13 . 95.12(7) yes N14 . Mn2 . N13 . 93.77(7) yes O28 . Mn2 . N13 . 168.47(7) yes O25 . Mn3 . O24 . 82.20(6) yes O25 . Mn3 . O16 . 93.47(6) yes O24 . Mn3 . O16 . 86.47(6) yes O25 . Mn3 . O18 . 173.84(7) yes O24 . Mn3 . O18 . 97.13(7) yes O16 . Mn3 . O18 . 92.60(7) yes O25 . Mn3 . N18 . 87.78(7) yes O24 . Mn3 . N18 . 93.92(6) yes O16 . Mn3 . N18 . 178.73(7) yes O18 . Mn3 . N18 . 86.15(7) yes O25 . Mn3 . N16 . 87.44(7) yes O24 . Mn3 . N16 . 163.97(6) yes O16 . Mn3 . N16 . 81.95(7) yes O18 . Mn3 . N16 . 94.45(7) yes N18 . Mn3 . N16 . 97.89(7) yes O22 . Mn4 . O24 . 82.88(6) yes O22 . Mn4 . O17 . 88.35(6) yes O24 . Mn4 . O17 . 93.80(7) yes O22 . Mn4 . O15 . 97.86(6) yes O24 . Mn4 . O15 . 172.33(7) yes O17 . Mn4 . O15 . 93.86(7) yes O22 . Mn4 . N15 . 95.51(6) yes O24 . Mn4 . N15 . 86.40(7) yes O17 . Mn4 . N15 . 176.13(7) yes O15 . Mn4 . N15 . 85.93(7) yes O22 . Mn4 . N17 . 165.26(6) yes O24 . Mn4 . N17 . 88.37(7) yes O17 . Mn4 . N17 . 80.39(7) yes O15 . Mn4 . N17 . 92.40(7) yes N15 . Mn4 . N17 . 95.76(7) yes Mn1 . O25 . Mn3 . 115.06(7) yes Mn1 . O25 . N15 . 116.01(11) yes Mn3 . O25 . N15 . 113.38(11) yes Mn1 . O11 . C11 . 118.40(14) yes Mn4 . O22 . Mn2 . 115.53(7) yes Mn4 . O22 . N12 . 114.95(11) yes Mn2 . O22 . N12 . 113.99(11) yes Mn2 . O13 . C13 . 117.77(14) yes Mn2 . O14 . C14 . 120.58(14) yes Mn3 . O24 . Mn4 . 115.56(7) yes Mn3 . O24 . N14 . 114.30(11) yes Mn4 . O24 . N14 . 113.94(12) yes Mn3 . O16 . C16 . 117.42(13) yes Mn4 . O17 . C17 . 118.06(14) yes N13 . O23 . H14 . 113.2 no O24 . N14 . Mn2 . 116.18(12) yes O24 . N14 . C74 . 115.96(18) yes Mn2 . N14 . C74 . 127.48(15) yes N11 . O21 . H31 . 108.5 no Mn1 . O12 . C12 . 121.43(14) yes N16 . O26 . H62 . 110.9 no Mn4 . O15 . C15 . 118.11(14) yes Mn2 . O28 . Mn1 . 116.57(7) yes Mn2 . O28 . N18 . 114.70(11) yes Mn1 . O28 . N18 . 114.92(11) yes O22 . N12 . Mn1 . 115.98(13) yes O22 . N12 . C72 . 116.43(17) yes Mn1 . N12 . C72 . 127.52(15) yes Mn2 . N13 . O23 . 123.18(14) yes Mn2 . N13 . C73 . 123.37(16) yes O23 . N13 . C73 . 113.34(18) yes Mn3 . O18 . C18 . 121.80(15) yes N17 . O27 . H18 . 106.4 no O28 . N18 . Mn3 . 114.86(12) yes O28 . N18 . C78 . 116.00(17) yes Mn3 . N18 . C78 . 128.77(16) yes Mn1 . N11 . O21 . 122.32(13) yes Mn1 . N11 . C71 . 123.93(15) yes O21 . N11 . C71 . 112.13(18) yes N18 . C78 . C68 . 118.1(2) yes N18 . C78 . C88 . 120.5(2) yes C68 . C78 . C88 . 121.3(2) yes O25 . N15 . Mn4 . 116.11(12) yes O25 . N15 . C75 . 116.71(17) yes Mn4 . N15 . C75 . 126.98(15) yes Mn3 . N16 . O26 . 123.13(14) yes Mn3 . N16 . C76 . 123.76(16) yes O26 . N16 . C76 . 112.72(19) yes C78 . C68 . C18 . 121.9(2) yes C78 . C68 . C58 . 119.6(2) yes C18 . C68 . C58 . 118.4(2) yes N12 . C72 . C62 . 119.3(2) yes N12 . C72 . C82 . 119.1(2) yes C62 . C72 . C82 . 121.5(2) yes Mn4 . N17 . O27 . 122.32(13) yes Mn4 . N17 . C77 . 123.46(17) yes O27 . N17 . C77 . 113.61(19) yes C76 . C86 . H861 . 111.2 no C76 . C86 . H862 . 111.4 no H861 . C86 . H862 . 109.2 no C76 . C86 . H863 . 108.5 no H861 . C86 . H863 . 108.7 no H862 . C86 . H863 . 107.8 no C68 . C18 . O18 . 122.4(2) yes C68 . C18 . C28 . 119.6(2) yes O18 . C18 . C28 . 117.9(2) yes C11 . C21 . C31 . 121.0(2) yes C11 . C21 . H211 . 119.0 no C31 . C21 . H211 . 120.0 no C72 . C62 . C12 . 120.9(2) yes C72 . C62 . C52 . 121.0(2) yes C12 . C62 . C52 . 118.1(2) yes C24 . C34 . C44 . 120.3(2) yes C24 . C34 . H341 . 119.2 no C44 . C34 . H341 . 120.5 no C71 . C61 . C11 . 122.81(19) yes C71 . C61 . C51 . 119.4(2) yes C11 . C61 . C51 . 117.8(2) yes O13 . C13 . C63 . 121.9(2) yes O13 . C13 . C23 . 118.8(2) yes C63 . C13 . C23 . 119.3(2) yes C58 . C48 . C38 . 120.3(2) yes C58 . C48 . H481 . 119.0 no C38 . C48 . H481 . 120.8 no N15 . C75 . C85 . 119.8(2) yes N15 . C75 . C65 . 118.01(19) yes C85 . C75 . C65 . 122.19(19) yes N14 . C74 . C64 . 118.5(2) yes N14 . C74 . C84 . 119.7(2) yes C64 . C74 . C84 . 121.7(2) yes C73 . C83 . H831 . 110.1 no C73 . C83 . H832 . 109.7 no H831 . C83 . H832 . 108.1 no C73 . C83 . H833 . 110.5 no H831 . C83 . H833 . 109.9 no H832 . C83 . H833 . 108.5 no C34 . C24 . C14 . 121.2(2) yes C34 . C24 . H241 . 119.3 no C14 . C24 . H241 . 119.5 no O15 . C15 . C65 . 122.53(19) yes O15 . C15 . C25 . 118.8(2) yes C65 . C15 . C25 . 118.6(2) yes O17 . C17 . C67 . 122.2(2) yes O17 . C17 . C27 . 118.3(2) yes C67 . C17 . C27 . 119.5(2) yes C45 . C35 . C25 . 121.6(2) yes C45 . C35 . H351 . 119.8 no C25 . C35 . H351 . 118.6 no C61 . C71 . N11 . 117.8(2) yes C61 . C71 . C81 . 119.9(2) yes N11 . C71 . C81 . 122.3(2) yes C61 . C11 . C21 . 119.8(2) yes C61 . C11 . O11 . 121.0(2) yes C21 . C11 . O11 . 119.2(2) yes C86 . C76 . N16 . 121.4(2) yes C86 . C76 . C66 . 120.6(2) yes N16 . C76 . C66 . 118.0(2) yes O16 . C16 . C66 . 122.2(2) yes O16 . C16 . C26 . 118.4(2) yes C66 . C16 . C26 . 119.4(2) yes C18 . C28 . C38 . 120.5(3) yes C18 . C28 . H281 . 118.7 no C38 . C28 . H281 . 120.8 no C74 . C64 . C14 . 120.6(2) yes C74 . C64 . C54 . 121.0(2) yes C14 . C64 . C54 . 118.2(2) yes N17 . C77 . C67 . 118.4(2) yes N17 . C77 . C87 . 121.7(2) yes C67 . C77 . C87 . 119.8(2) yes C77 . C67 . C17 . 123.6(2) yes C77 . C67 . C57 . 118.4(2) yes C17 . C67 . C57 . 118.0(2) yes C83 . C73 . N13 . 121.6(2) yes C83 . C73 . C63 . 119.6(2) yes N13 . C73 . C63 . 118.8(2) yes C31 . C41 . C51 . 119.8(2) yes C31 . C41 . H411 . 120.0 no C51 . C41 . H411 . 120.2 no C67 . C57 . C47 . 121.8(3) yes C67 . C57 . H571 . 118.9 no C47 . C57 . H571 . 119.3 no C73 . C63 . C13 . 123.0(2) yes C73 . C63 . C53 . 119.3(2) yes C13 . C63 . C53 . 117.7(2) yes C75 . C85 . H851 . 110.6 no C75 . C85 . H852 . 110.1 no H851 . C85 . H852 . 107.8 no C75 . C85 . H853 . 109.7 no H851 . C85 . H853 . 108.6 no H852 . C85 . H853 . 110.0 no C66 . C56 . C46 . 122.1(3) yes C66 . C56 . H561 . 118.0 no C46 . C56 . H561 . 119.9 no C32 . C42 . C52 . 118.5(2) yes C32 . C42 . H421 . 120.9 no C52 . C42 . H421 . 120.6 no C75 . C65 . C15 . 120.90(19) yes C75 . C65 . C55 . 119.6(2) yes C15 . C65 . C55 . 119.5(2) yes C41 . C31 . C21 . 120.0(2) yes C41 . C31 . H311 . 119.5 no C21 . C31 . H311 . 120.5 no C61 . C51 . C41 . 121.6(2) yes C61 . C51 . H511 . 118.6 no C41 . C51 . H511 . 119.8 no C35 . C45 . C55 . 119.2(2) yes C35 . C45 . H451 . 120.6 no C55 . C45 . H451 . 120.2 no C68 . C58 . C48 . 120.9(3) yes C68 . C58 . H581 . 120.7 no C48 . C58 . H581 . 118.4 no C12 . C22 . C32 . 121.0(2) yes C12 . C22 . H221 . 119.1 no C32 . C22 . H221 . 119.9 no C33 . C43 . C53 . 119.3(2) yes C33 . C43 . H431 . 119.9 no C53 . C43 . H431 . 120.9 no C62 . C12 . C22 . 118.7(2) yes C62 . C12 . O12 . 123.5(2) yes C22 . C12 . O12 . 117.8(2) yes C65 . C55 . C45 . 120.9(2) yes C65 . C55 . H551 . 121.3 no C45 . C55 . H551 . 117.8 no C43 . C33 . C23 . 120.8(2) yes C43 . C33 . H331 . 119.0 no C23 . C33 . H331 . 120.3 no C72 . C82 . H821 . 111.7 no C72 . C82 . H822 . 110.6 no H821 . C82 . H822 . 107.1 no C72 . C82 . H823 . 109.9 no H821 . C82 . H823 . 108.9 no H822 . C82 . H823 . 108.6 no C42 . C32 . C22 . 121.1(2) yes C42 . C32 . H321 . 118.9 no C22 . C32 . H321 . 120.0 no C34 . C44 . C54 . 119.4(3) yes C34 . C44 . H441 . 119.8 no C54 . C44 . H441 . 120.8 no C64 . C14 . C24 . 118.9(2) yes C64 . C14 . O14 . 123.2(2) yes C24 . C14 . O14 . 117.9(2) yes C63 . C53 . C43 . 122.4(2) yes C63 . C53 . H531 . 118.5 no C43 . C53 . H531 . 119.0 no C57 . C47 . C37 . 119.8(3) yes C57 . C47 . H471 . 119.4 no C37 . C47 . H471 . 120.9 no C17 . C27 . C37 . 121.6(3) yes C17 . C27 . H271 . 119.1 no C37 . C27 . H271 . 119.2 no C62 . C52 . C42 . 122.5(3) yes C62 . C52 . H521 . 117.9 no C42 . C52 . H521 . 119.7 no C78 . C88 . H881 . 108.0 no C78 . C88 . H882 . 109.2 no H881 . C88 . H882 . 109.7 no C78 . C88 . H883 . 109.5 no H881 . C88 . H883 . 109.8 no H882 . C88 . H883 . 110.6 no C15 . C25 . C35 . 120.1(2) yes C15 . C25 . H251 . 120.2 no C35 . C25 . H251 . 119.7 no C48 . C38 . C28 . 120.3(3) yes C48 . C38 . H381 . 121.2 no C28 . C38 . H381 . 118.4 no C27 . C37 . C47 . 119.4(3) yes C27 . C37 . H371 . 120.8 no C47 . C37 . H371 . 119.8 no C71 . C81 . H811 . 110.8 no C71 . C81 . H812 . 107.9 no H811 . C81 . H812 . 108.9 no C71 . C81 . H813 . 110.5 no H811 . C81 . H813 . 110.6 no H812 . C81 . H813 . 107.9 no C13 . C23 . C33 . 120.5(2) yes C13 . C23 . H231 . 119.7 no C33 . C23 . H231 . 119.8 no C76 . C66 . C16 . 122.8(2) yes C76 . C66 . C56 . 119.7(3) yes C16 . C66 . C56 . 117.5(2) yes C16 . C26 . C36 . 121.0(3) yes C16 . C26 . H261 . 119.7 no C36 . C26 . H261 . 119.3 no C74 . C84 . H841 . 109.4 no C74 . C84 . H842 . 109.4 no H841 . C84 . H842 . 109.1 no C74 . C84 . H843 . 111.0 no H841 . C84 . H843 . 108.6 no H842 . C84 . H843 . 109.4 no C64 . C54 . C44 . 121.9(3) yes C64 . C54 . H541 . 118.8 no C44 . C54 . H541 . 119.3 no C77 . C87 . H871 . 109.3 no C77 . C87 . H872 . 108.9 no H871 . C87 . H872 . 111.3 no C77 . C87 . H873 . 107.5 no H871 . C87 . H873 . 110.3 no H872 . C87 . H873 . 109.5 no C26 . C36 . C46 . 119.8(3) yes C26 . C36 . H361 . 119.9 no C46 . C36 . H361 . 120.3 no C56 . C46 . C36 . 120.2(3) yes C56 . C46 . H461 . 120.0 no C36 . C46 . H461 . 119.8 no