# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Dalton Trans. _journal_coden_cambridge 0182 _journal_year 2007 _journal_page_first 153 _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 C.J.Milios A.Prescimone A.Mishra S.Parsons W.Wernsdorfer G.Christou S.P.Perlepes E.K.Brechin # 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 # Attachment 'Complex_2.cif' data_EB8072 _database_code_depnum_ccdc_archive 'CCDC 756186' #TrackingRef 'Complex_2.cif' _audit_creation_date 08-04-14 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8072 in C2/c' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H60 Mn4 N8 O16, 3(C4 H10 O)' _chemical_compound_source 'Ross Inglis, RI885' _exptl_crystal_recrystallization_method ; Diffusion of MeCN and Et~2~O. ; _publ_section_exptl_refinement ; The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. Checkcif alerts 601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 537.00 A**3 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The solvent region was treated by the van der Sluis and Spek method, accounting for 581 e/cell. This corresponds to 2 molecules of Et~2~O per formula unit and F(000), M, mu, D and the formulae have been calculated on this assumption. 912_ALERT_3_A # Missing FCF Reflections Above STh/L= 0.600 1241 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 3 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 9130 9127 3 23.01 0.550 1.000 12168 12165 3 25.24 0.600 1.000 15808 15805 3 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 1.000 20093 20089 4 29.84 0.700 0.970 25102 24346 756 30.46 0.713 0.953 26496 25252 1244 061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.58 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay, changes in the volume of the crystal illuminated, etc. 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 3 No action taken. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.43 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.39 Ratio 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 8 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 20 No action. ; #end of refcif _cell_length_a 21.8339(5) _cell_length_b 20.0435(4) _cell_length_c 39.9737(9) _cell_angle_alpha 90 _cell_angle_beta 92.985(1) _cell_angle_gamma 90 _cell_volume 17469.9(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-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 8 # Given Formula = C100 H90 Mn4 N8 O19 # Dc = 1.47 Fooo = 7312.00 Mu = 6.44 M = 1927.57 # Found Formula = C92 H70 Mn4 N8 O17 # Dc = 1.35 FOOO = 7312.00 Mu = 6.36 M = 1779.32 _chemical_formula_sum 'C100 H90 Mn4 N8 O19' _chemical_formula_weight 1927.57 _cell_measurement_reflns_used 9190 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 7312 _exptl_absorpt_coefficient_mu 0.644 # Sheldrick geometric approximatio 0.89 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.91 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _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_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction '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 101048 _reflns_number_total 25252 _diffrn_reflns_av_R_equivalents 0.086 # Number of reflections with Friedels Law is 25252 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 26546 _diffrn_reflns_theta_min 1.020 _diffrn_reflns_theta_max 30.457 _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.325 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 56 _reflns_limit_h_min -31 _reflns_limit_h_max 31 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 56 _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 -1.36 _refine_diff_density_max 1.35 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 25252 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1090 _oxford_refine_ls_R_factor_ref 0.1338 _refine_ls_wR_factor_ref 0.2186 _refine_ls_goodness_of_fit_ref 1.0005 _refine_ls_shift/su_max 0.000440 # The values computed from all data _oxford_reflns_number_all 25252 _refine_ls_R_factor_all 0.1338 _refine_ls_wR_factor_all 0.2186 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 14760 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_gt 0.1630 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept Unit Weights _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./2F ; # 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. 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., 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.31561(3) 0.03632(4) 0.099923(18) 0.0166 1.0000 Uani . . . . . . . Mn2 Mn 0.23315(3) -0.11675(4) 0.108220(18) 0.0161 1.0000 Uani . . . . . . . Mn3 Mn 0.25632(3) -0.03536(4) 0.186507(19) 0.0188 1.0000 Uani . . . . . . . Mn4 Mn 0.16781(3) 0.06582(4) 0.129508(18) 0.0160 1.0000 Uani . . . . . . . O5 O 0.29235(16) 0.10643(17) 0.06864(9) 0.0210 1.0000 Uani . . . . . . . C6 C 0.3311(2) 0.1373(2) 0.04892(13) 0.0208 1.0000 Uani . . . . . . . C7 C 0.3163(2) 0.2044(3) 0.03872(14) 0.0241 1.0000 Uani . . . . . . . C8 C 0.3531(3) 0.2391(3) 0.01923(15) 0.0292 1.0000 Uani . . . . . . . C9 C 0.4095(2) 0.2126(3) 0.00904(14) 0.0260 1.0000 Uani . . . . . . . C10 C 0.4256(2) 0.1466(3) 0.01877(13) 0.0232 1.0000 Uani . . . . . . . C11 C 0.3829(2) 0.1070(3) 0.03666(13) 0.0222 1.0000 Uani . . . . . . . C12 C 0.3926(2) 0.0352(3) 0.03835(13) 0.0230 1.0000 Uani . . . . . . . N13 N 0.36480(19) -0.0037(2) 0.05783(11) 0.0204 1.0000 Uani . . . . . . . O14 O 0.37848(18) -0.07109(18) 0.05262(11) 0.0292 1.0000 Uani . . . . . . . C15 C 0.4509(3) 0.2509(3) -0.00912(14) 0.0294 1.0000 Uani . . . . . . . C16 C 0.5062(3) 0.2261(3) -0.01664(15) 0.0327 1.0000 Uani . . . . . . . C17 C 0.5238(3) 0.1620(3) -0.00615(15) 0.0316 1.0000 Uani . . . . . . . C18 C 0.4843(2) 0.1231(3) 0.01088(14) 0.0256 1.0000 Uani . . . . . . . O19 O 0.38504(16) 0.08006(18) 0.11773(10) 0.0238 1.0000 Uani . . . . . . . C20 C 0.4391(2) 0.0538(3) 0.12665(13) 0.0219 1.0000 Uani . . . . . . . C21 C 0.4918(3) 0.0946(3) 0.12402(17) 0.0321 1.0000 Uani . . . . . . . C22 C 0.5485(3) 0.0717(3) 0.13280(16) 0.0342 1.0000 Uani . . . . . . . C23 C 0.5583(2) 0.0060(3) 0.14509(15) 0.0296 1.0000 Uani . . . . . . . C24 C 0.5066(2) -0.0360(3) 0.14914(14) 0.0266 1.0000 Uani . . . . . . . C25 C 0.4466(2) -0.0114(3) 0.13889(13) 0.0219 1.0000 Uani . . . . . . . C26 C 0.3935(2) -0.0523(2) 0.14409(12) 0.0186 1.0000 Uani . . . . . . . N27 N 0.34009(18) -0.0417(2) 0.12939(10) 0.0181 1.0000 Uani . . . . . . . O28 O 0.29392(15) -0.08187(16) 0.14140(9) 0.0182 1.0000 Uani . . . . . . . C29 C 0.6176(3) -0.0182(3) 0.15390(16) 0.0363 1.0000 Uani . . . . . . . C30 C 0.6267(3) -0.0807(4) 0.16649(16) 0.0376 1.0000 Uani . . . . . . . C31 C 0.5765(3) -0.1213(3) 0.17078(16) 0.0366 1.0000 Uani . . . . . . . C32 C 0.5177(3) -0.1005(3) 0.16234(15) 0.0306 1.0000 Uani . . . . . . . O33 O 0.29466(15) -0.15429(17) 0.08169(9) 0.0194 1.0000 Uani . . . . . . . C34 C 0.2892(2) -0.2126(3) 0.06592(13) 0.0229 1.0000 Uani . . . . . . . C35 C 0.3197(3) -0.2195(3) 0.03550(14) 0.0276 1.0000 Uani . . . . . . . C36 C 0.3174(3) -0.2768(3) 0.01774(16) 0.0333 1.0000 Uani . . . . . . . C37 C 0.2826(3) -0.3317(3) 0.02764(15) 0.0297 1.0000 Uani . . . . . . . C38 C 0.2514(3) -0.3268(3) 0.05763(14) 0.0262 1.0000 Uani . . . . . . . C39 C 0.2579(2) -0.2681(3) 0.07814(14) 0.0262 1.0000 Uani . . . . . . . C40 C 0.2362(3) -0.2694(3) 0.11193(14) 0.0278 1.0000 Uani . . . . . . . N41 N 0.2320(2) -0.2177(2) 0.13036(11) 0.0224 1.0000 Uani . . . . . . . O42 O 0.2124(2) -0.2336(2) 0.16222(10) 0.0349 1.0000 Uani . . . . . . . C43 C 0.2752(3) -0.3891(3) 0.00714(16) 0.0349 1.0000 Uani . . . . . . . C44 C 0.2374(3) -0.4396(3) 0.01544(17) 0.0390 1.0000 Uani . . . . . . . C45 C 0.2060(4) -0.4352(3) 0.04471(19) 0.0478 1.0000 Uani . . . . . . . C46 C 0.2122(4) -0.3809(3) 0.06560(18) 0.0428 1.0000 Uani . . . . . . . O47 O 0.16858(16) -0.14320(18) 0.07846(9) 0.0214 1.0000 Uani . . . . . . . C48 C 0.1162(2) -0.1704(3) 0.08752(12) 0.0198 1.0000 Uani . . . . . . . C49 C 0.0903(3) -0.2214(3) 0.06643(13) 0.0245 1.0000 Uani . . . . . . . C50 C 0.0337(3) -0.2459(3) 0.07153(14) 0.0260 1.0000 Uani . . . . . . . C51 C -0.0001(2) -0.2241(3) 0.09858(13) 0.0233 1.0000 Uani . . . . . . . C52 C 0.0260(2) -0.1780(3) 0.12180(12) 0.0200 1.0000 Uani . . . . . . . C53 C 0.0853(2) -0.1508(2) 0.11566(12) 0.0172 1.0000 Uani . . . . . . . C54 C 0.1108(2) -0.1001(2) 0.13724(12) 0.0196 1.0000 Uani . . . . . . . N55 N 0.16816(18) -0.08298(19) 0.13791(10) 0.0161 1.0000 Uani . . . . . . . O56 O 0.18162(15) -0.02724(16) 0.15754(9) 0.0185 1.0000 Uani . . . . . . . C57 C -0.0601(3) -0.2493(3) 0.10350(17) 0.0325 1.0000 Uani . . . . . . . C58 C -0.0908(3) -0.2311(4) 0.13049(19) 0.0417 1.0000 Uani . . . . . . . C59 C -0.0642(3) -0.1870(4) 0.15406(18) 0.0422 1.0000 Uani . . . . . . . C60 C -0.0074(2) -0.1612(3) 0.14983(16) 0.0310 1.0000 Uani . . . . . . . O61 O 0.23678(18) -0.12300(18) 0.20058(9) 0.0248 1.0000 Uani . . . . . . . C62 C 0.2459(2) -0.1440(3) 0.23214(13) 0.0237 1.0000 Uani . . . . . . . C63 C 0.2751(3) -0.2067(3) 0.23685(14) 0.0283 1.0000 Uani . . . . . . . C64 C 0.2825(3) -0.2341(3) 0.26778(15) 0.0290 1.0000 Uani . . . . . . . C65 C 0.2611(2) -0.2017(3) 0.29631(13) 0.0251 1.0000 Uani . . . . . . . C66 C 0.2327(2) -0.1380(3) 0.29239(13) 0.0227 1.0000 Uani . . . . . . . C67 C 0.2259(2) -0.1081(3) 0.25952(13) 0.0222 1.0000 Uani . . . . . . . C68 C 0.1960(2) -0.0439(3) 0.25517(13) 0.0255 1.0000 Uani . . . . . . . N69 N 0.1996(2) -0.0078(2) 0.22914(11) 0.0235 1.0000 Uani . . . . . . . O70 O 0.1656(2) 0.0515(2) 0.23099(11) 0.0382 1.0000 Uani . . . . . . . C71 C 0.2673(3) -0.2309(3) 0.32815(14) 0.0288 1.0000 Uani . . . . . . . C72 C 0.2468(3) -0.2002(3) 0.35585(14) 0.0320 1.0000 Uani . . . . . . . C73 C 0.2193(3) -0.1367(3) 0.35209(15) 0.0335 1.0000 Uani . . . . . . . C74 C 0.2128(2) -0.1064(3) 0.32151(14) 0.0273 1.0000 Uani . . . . . . . O75 O 0.33156(17) -0.0352(2) 0.21084(10) 0.0269 1.0000 Uani . . . . . . . C76 C 0.3588(2) 0.0157(3) 0.22624(13) 0.0239 1.0000 Uani . . . . . . . C77 C 0.4018(3) 0.0004(4) 0.25317(15) 0.0361 1.0000 Uani . . . . . . . C78 C 0.4318(3) 0.0493(4) 0.27045(17) 0.0442 1.0000 Uani . . . . . . . C79 C 0.4216(3) 0.1177(4) 0.26292(14) 0.0373 1.0000 Uani . . . . . . . C80 C 0.3814(2) 0.1356(3) 0.23521(14) 0.0280 1.0000 Uani . . . . . . . C81 C 0.3509(2) 0.0827(3) 0.21632(13) 0.0225 1.0000 Uani . . . . . . . C82 C 0.3153(2) 0.0977(3) 0.18596(12) 0.0212 1.0000 Uani . . . . . . . N83 N 0.27679(18) 0.0573(2) 0.17140(10) 0.0192 1.0000 Uani . . . . . . . O84 O 0.25577(15) 0.07722(17) 0.13935(9) 0.0190 1.0000 Uani . . . . . . . C85 C 0.4495(3) 0.1688(4) 0.28267(18) 0.0492 1.0000 Uani . . . . . . . C86 C 0.4381(4) 0.2339(5) 0.2760(2) 0.0572 1.0000 Uani . . . . . . . C87 C 0.3994(4) 0.2517(4) 0.2484(2) 0.0513 1.0000 Uani . . . . . . . C88 C 0.3717(3) 0.2033(3) 0.22844(16) 0.0348 1.0000 Uani . . . . . . . O89 O 0.14589(16) 0.11372(18) 0.16859(9) 0.0220 1.0000 Uani . . . . . . . C90 C 0.0945(2) 0.1506(2) 0.16719(13) 0.0207 1.0000 Uani . . . . . . . C91 C 0.0573(3) 0.1475(3) 0.19566(15) 0.0326 1.0000 Uani . . . . . . . C92 C 0.0019(3) 0.1794(3) 0.19511(18) 0.0409 1.0000 Uani . . . . . . . C93 C -0.0203(3) 0.2162(3) 0.16684(17) 0.0312 1.0000 Uani . . . . . . . C94 C 0.0169(2) 0.2226(3) 0.13918(14) 0.0255 1.0000 Uani . . . . . . . C95 C 0.0763(2) 0.1913(2) 0.14036(13) 0.0201 1.0000 Uani . . . . . . . C96 C 0.1174(2) 0.2046(2) 0.11339(13) 0.0206 1.0000 Uani . . . . . . . N97 N 0.1605(2) 0.1655(2) 0.10595(11) 0.0213 1.0000 Uani . . . . . . . O98 O 0.19495(19) 0.18990(19) 0.08022(10) 0.0300 1.0000 Uani . . . . . . . C99 C -0.0796(3) 0.2444(3) 0.1651(2) 0.0397 1.0000 Uani . . . . . . . C100 C -0.1017(3) 0.2765(3) 0.1377(2) 0.0426 1.0000 Uani . . . . . . . C101 C -0.0654(3) 0.2838(3) 0.11004(19) 0.0412 1.0000 Uani . . . . . . . C102 C -0.0072(3) 0.2572(3) 0.11074(17) 0.0327 1.0000 Uani . . . . . . . O103 O 0.08606(15) 0.04670(18) 0.11546(9) 0.0200 1.0000 Uani . . . . . . . C104 C 0.0627(2) 0.0585(2) 0.08490(13) 0.0201 1.0000 Uani . . . . . . . C105 C 0.0005(2) 0.0796(3) 0.08136(14) 0.0260 1.0000 Uani . . . . . . . C106 C -0.0273(2) 0.0903(3) 0.05047(14) 0.0262 1.0000 Uani . . . . . . . C107 C 0.0052(2) 0.0822(2) 0.02079(13) 0.0221 1.0000 Uani . . . . . . . C108 C 0.0675(2) 0.0635(2) 0.02316(13) 0.0223 1.0000 Uani . . . . . . . C109 C 0.0958(2) 0.0496(2) 0.05591(12) 0.0167 1.0000 Uani . . . . . . . C110 C 0.1557(2) 0.0209(2) 0.05901(11) 0.0168 1.0000 Uani . . . . . . . N111 N 0.18957(18) 0.0224(2) 0.08637(10) 0.0159 1.0000 Uani . . . . . . . O112 O 0.24295(14) -0.01571(16) 0.08616(9) 0.0171 1.0000 Uani . . . . . . . C113 C -0.0235(3) 0.0950(3) -0.01115(14) 0.0278 1.0000 Uani . . . . . . . C114 C 0.0088(3) 0.0896(3) -0.03952(15) 0.0320 1.0000 Uani . . . . . . . C115 C 0.0710(3) 0.0734(3) -0.03693(14) 0.0317 1.0000 Uani . . . . . . . C116 C 0.1000(3) 0.0602(3) -0.00640(14) 0.0267 1.0000 Uani . . . . . . . O117 O 0.1434(2) 0.4173(2) 0.05501(12) 0.0382 1.0000 Uani . . . . . . . C118 C 0.0865(3) 0.4059(3) 0.06900(17) 0.0395 1.0000 Uani . . . . . . . C119 C 0.0459(4) 0.4655(4) 0.06167(18) 0.0495 1.0000 Uani . . . . . . . C120 C 0.1863(4) 0.3663(4) 0.06261(19) 0.0465 1.0000 Uani . . . . . . . C121 C 0.2457(4) 0.3834(4) 0.0483(2) 0.0578 1.0000 Uani . . . . . . . H1051 H -0.0215 0.0860 0.1003 0.0310 1.0000 Uiso R . . . . . . H1061 H -0.0683 0.1026 0.0486 0.0309 1.0000 Uiso R . . . . . . H1101 H 0.1706 0.0000 0.0404 0.0200 1.0000 Uiso R . . . . . . H491 H 0.1120 -0.2380 0.0490 0.0291 1.0000 Uiso R . . . . . . H501 H 0.0171 -0.2776 0.0570 0.0312 1.0000 Uiso R . . . . . . H541 H 0.0853 -0.0782 0.1513 0.0239 1.0000 Uiso R . . . . . . H261 H 0.3979 -0.0885 0.1589 0.0220 1.0000 Uiso R . . . . . . H211 H 0.4872 0.1379 0.1160 0.0389 1.0000 Uiso R . . . . . . H221 H 0.5824 0.0996 0.1307 0.0410 1.0000 Uiso R . . . . . . H321 H 0.4850 -0.1291 0.1652 0.0360 1.0000 Uiso R . . . . . . H311 H 0.5827 -0.1638 0.1795 0.0429 1.0000 Uiso R . . . . . . H301 H 0.6662 -0.0958 0.1722 0.0450 1.0000 Uiso R . . . . . . H291 H 0.6514 0.0090 0.1509 0.0429 1.0000 Uiso R . . . . . . H821 H 0.3203 0.1396 0.1763 0.0249 1.0000 Uiso R . . . . . . H771 H 0.4090 -0.0439 0.2589 0.0431 1.0000 Uiso R . . . . . . H781 H 0.4598 0.0378 0.2877 0.0519 1.0000 Uiso R . . . . . . H881 H 0.3459 0.2157 0.2101 0.0408 1.0000 Uiso R . . . . . . H871 H 0.3919 0.2962 0.2435 0.0608 1.0000 Uiso R . . . . . . H861 H 0.4562 0.2667 0.2897 0.0679 1.0000 Uiso R . . . . . . H851 H 0.4762 0.1574 0.3006 0.0580 1.0000 Uiso R . . . . . . H711 H 0.2858 -0.2724 0.3303 0.0338 1.0000 Uiso R . . . . . . H721 H 0.2507 -0.2203 0.3767 0.0378 1.0000 Uiso R . . . . . . H731 H 0.2058 -0.1150 0.3707 0.0398 1.0000 Uiso R . . . . . . H741 H 0.1953 -0.0645 0.3200 0.0328 1.0000 Uiso R . . . . . . H641 H 0.3020 -0.2749 0.2703 0.0336 1.0000 Uiso R . . . . . . H631 H 0.2893 -0.2292 0.2184 0.0339 1.0000 Uiso R . . . . . . H681 H 0.1733 -0.0280 0.2725 0.0311 1.0000 Uiso R . . . . . . H601 H 0.0096 -0.1320 0.1656 0.0370 1.0000 Uiso R . . . . . . H591 H -0.0853 -0.1754 0.1727 0.0511 1.0000 Uiso R . . . . . . H581 H -0.1300 -0.2475 0.1335 0.0498 1.0000 Uiso R . . . . . . H571 H -0.0781 -0.2785 0.0880 0.0390 1.0000 Uiso R . . . . . . H361 H 0.3387 -0.2802 -0.0015 0.0399 1.0000 Uiso R . . . . . . H351 H 0.3413 -0.1839 0.0276 0.0330 1.0000 Uiso R . . . . . . H431 H 0.2968 -0.3921 -0.0121 0.0420 1.0000 Uiso R . . . . . . H441 H 0.2324 -0.4767 0.0018 0.0469 1.0000 Uiso R . . . . . . H451 H 0.1804 -0.4699 0.0504 0.0580 1.0000 Uiso R . . . . . . H461 H 0.1909 -0.3796 0.0851 0.0520 1.0000 Uiso R . . . . . . H401 H 0.2250 -0.3105 0.1208 0.0340 1.0000 Uiso R . . . . . . H1161 H 0.1414 0.0492 -0.0053 0.0320 1.0000 Uiso R . . . . . . H1151 H 0.0931 0.0717 -0.0561 0.0380 1.0000 Uiso R . . . . . . H1141 H -0.0105 0.0964 -0.0604 0.0378 1.0000 Uiso R . . . . . . H1131 H -0.0647 0.1070 -0.0130 0.0327 1.0000 Uiso R . . . . . . H1021 H 0.0165 0.2622 0.0924 0.0390 1.0000 Uiso R . . . . . . H1011 H -0.0803 0.3061 0.0912 0.0481 1.0000 Uiso R . . . . . . H1001 H -0.1412 0.2940 0.1371 0.0507 1.0000 Uiso R . . . . . . H991 H -0.1037 0.2404 0.1833 0.0479 1.0000 Uiso R . . . . . . H921 H -0.0219 0.1768 0.2136 0.0500 1.0000 Uiso R . . . . . . H911 H 0.0712 0.1240 0.2146 0.0392 1.0000 Uiso R . . . . . . H961 H 0.1119 0.2438 0.1011 0.0250 1.0000 Uiso R . . . . . . H121 H 0.4202 0.0166 0.0242 0.0279 1.0000 Uiso R . . . . . . H181 H 0.4959 0.0805 0.0175 0.0310 1.0000 Uiso R . . . . . . H171 H 0.5624 0.1456 -0.0107 0.0377 1.0000 Uiso R . . . . . . H161 H 0.5328 0.2518 -0.0288 0.0399 1.0000 Uiso R . . . . . . H151 H 0.4396 0.2937 -0.0159 0.0360 1.0000 Uiso R . . . . . . H81 H 0.3413 0.2816 0.0120 0.0349 1.0000 Uiso R . . . . . . H71 H 0.2806 0.2240 0.0456 0.0291 1.0000 Uiso R . . . . . . H1182 H 0.0928 0.4000 0.0932 0.0469 1.0000 Uiso R . . . . . . H1181 H 0.0680 0.3657 0.0595 0.0468 1.0000 Uiso R . . . . . . H1192 H 0.0067 0.4581 0.0709 0.0740 1.0000 Uiso R . . . . . . H1191 H 0.0653 0.5049 0.0718 0.0740 1.0000 Uiso R . . . . . . H1193 H 0.0414 0.4715 0.0378 0.0738 1.0000 Uiso R . . . . . . H1201 H 0.1923 0.3628 0.0867 0.0549 1.0000 Uiso R . . . . . . H1202 H 0.1713 0.3241 0.0537 0.0550 1.0000 Uiso R . . . . . . H1211 H 0.2753 0.3491 0.0534 0.0869 1.0000 Uiso R . . . . . . H1213 H 0.2612 0.4247 0.0579 0.0868 1.0000 Uiso R . . . . . . H1212 H 0.2408 0.3885 0.0247 0.0869 1.0000 Uiso R . . . . . . H981 H 0.2236 0.1641 0.0779 0.0450 1.0000 Uiso R . . . . . . H701 H 0.1677 0.0654 0.2119 0.0568 1.0000 Uiso R . . . . . . H421 H 0.2204 -0.2018 0.1743 0.0530 1.0000 Uiso R . . . . . . H141 H 0.3503 -0.0921 0.0602 0.0440 1.0000 Uiso R . . . . . . 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 0.0150(3) 0.0133(3) 0.0214(3) 0.0015(3) -0.0006(2) 0.0001(3) Mn2 0.0151(3) 0.0134(3) 0.0196(3) 0.0001(3) 0.0016(2) -0.0004(3) Mn3 0.0196(3) 0.0166(3) 0.0199(3) 0.0017(3) -0.0018(3) 0.0018(3) Mn4 0.0151(3) 0.0143(3) 0.0182(3) -0.0003(3) -0.0019(2) 0.0014(3) O5 0.0198(16) 0.0166(17) 0.0268(18) 0.0070(14) 0.0024(13) 0.0025(13) C6 0.026(2) 0.013(2) 0.023(2) 0.0004(17) -0.0029(18) -0.0029(18) C7 0.019(2) 0.021(2) 0.032(3) 0.006(2) 0.0032(19) 0.0008(19) C8 0.031(3) 0.018(2) 0.039(3) 0.010(2) 0.002(2) -0.001(2) C9 0.026(3) 0.023(3) 0.029(3) 0.001(2) 0.001(2) -0.008(2) C10 0.025(2) 0.022(2) 0.023(2) -0.0019(19) 0.0052(19) -0.009(2) C11 0.023(2) 0.021(2) 0.022(2) 0.0003(19) 0.0000(18) -0.0028(19) C12 0.022(2) 0.020(2) 0.028(2) -0.004(2) 0.0041(19) -0.0033(19) N13 0.0194(19) 0.0128(19) 0.029(2) 0.0005(16) 0.0009(16) -0.0013(15) O14 0.033(2) 0.0118(17) 0.045(2) 0.0000(16) 0.0143(17) -0.0002(15) C15 0.040(3) 0.021(3) 0.028(3) 0.003(2) 0.010(2) -0.003(2) C16 0.038(3) 0.029(3) 0.033(3) -0.006(2) 0.012(2) -0.014(2) C17 0.029(3) 0.032(3) 0.035(3) -0.007(2) 0.011(2) -0.004(2) C18 0.028(3) 0.019(2) 0.030(3) -0.003(2) 0.007(2) -0.005(2) O19 0.0204(17) 0.0180(17) 0.033(2) 0.0030(15) -0.0015(14) -0.0002(14) C20 0.019(2) 0.020(2) 0.026(2) -0.0056(19) 0.0013(18) 0.0006(18) C21 0.022(2) 0.022(3) 0.053(4) -0.002(2) 0.001(2) -0.006(2) C22 0.022(3) 0.037(3) 0.044(3) -0.008(3) -0.003(2) -0.004(2) C23 0.018(2) 0.037(3) 0.033(3) -0.007(2) -0.004(2) 0.004(2) C24 0.019(2) 0.031(3) 0.030(3) -0.011(2) -0.0058(19) 0.006(2) C25 0.018(2) 0.023(2) 0.024(2) -0.0010(19) -0.0047(18) 0.0007(19) C26 0.019(2) 0.017(2) 0.020(2) 0.0001(17) -0.0033(17) 0.0037(17) N27 0.0167(18) 0.0154(19) 0.0224(19) -0.0012(15) 0.0024(15) -0.0029(15) O28 0.0171(15) 0.0139(16) 0.0238(17) 0.0024(13) 0.0042(13) 0.0024(12) C29 0.023(3) 0.043(4) 0.042(3) -0.009(3) -0.007(2) 0.002(2) C30 0.019(3) 0.054(4) 0.038(3) -0.006(3) -0.006(2) 0.006(3) C31 0.032(3) 0.038(3) 0.039(3) -0.004(3) -0.008(2) 0.015(3) C32 0.023(2) 0.033(3) 0.036(3) -0.003(2) -0.007(2) 0.003(2) O33 0.0195(16) 0.0147(16) 0.0247(17) -0.0029(13) 0.0068(13) -0.0002(13) C34 0.021(2) 0.020(2) 0.027(3) -0.0007(19) 0.0046(19) 0.0023(19) C35 0.029(3) 0.021(3) 0.034(3) -0.003(2) 0.010(2) -0.005(2) C36 0.038(3) 0.029(3) 0.033(3) -0.006(2) 0.013(2) -0.003(2) C37 0.031(3) 0.026(3) 0.032(3) -0.009(2) 0.001(2) 0.001(2) C38 0.028(3) 0.019(2) 0.032(3) -0.005(2) 0.007(2) -0.004(2) C39 0.025(2) 0.023(3) 0.031(3) -0.003(2) 0.002(2) -0.002(2) C40 0.038(3) 0.016(2) 0.030(3) 0.002(2) 0.008(2) -0.002(2) N41 0.027(2) 0.018(2) 0.023(2) 0.0027(16) 0.0043(17) 0.0005(17) O42 0.061(3) 0.0211(19) 0.0237(19) -0.0003(15) 0.0123(19) -0.0035(19) C43 0.046(4) 0.026(3) 0.034(3) -0.014(2) 0.008(3) -0.002(3) C44 0.054(4) 0.017(3) 0.046(4) -0.008(2) -0.001(3) -0.003(3) C45 0.063(5) 0.026(3) 0.056(4) -0.011(3) 0.019(4) -0.017(3) C46 0.063(5) 0.022(3) 0.044(4) -0.006(3) 0.015(3) -0.011(3) O47 0.0198(16) 0.0225(18) 0.0220(17) -0.0009(14) 0.0021(13) -0.0032(14) C48 0.018(2) 0.020(2) 0.021(2) 0.0038(18) -0.0008(17) -0.0016(18) C49 0.031(3) 0.020(2) 0.023(2) -0.0050(19) 0.001(2) -0.002(2) C50 0.030(3) 0.022(3) 0.025(3) -0.003(2) -0.006(2) -0.005(2) C51 0.025(2) 0.019(2) 0.026(3) 0.0042(19) 0.0013(19) 0.0001(19) C52 0.017(2) 0.022(2) 0.021(2) -0.0001(18) 0.0009(17) 0.0012(18) C53 0.018(2) 0.015(2) 0.019(2) -0.0018(16) 0.0004(16) 0.0012(17) C54 0.020(2) 0.020(2) 0.019(2) 0.0031(18) 0.0061(17) 0.0014(18) N55 0.0168(18) 0.0128(18) 0.0185(18) -0.0034(14) 0.0000(14) -0.0013(14) O56 0.0179(15) 0.0131(15) 0.0241(17) -0.0067(13) -0.0029(13) 0.0015(12) C57 0.026(3) 0.023(3) 0.047(4) 0.000(2) -0.006(2) -0.005(2) C58 0.018(3) 0.045(4) 0.062(4) -0.005(3) 0.007(3) -0.005(3) C59 0.029(3) 0.050(4) 0.048(4) -0.007(3) 0.014(3) -0.005(3) C60 0.019(2) 0.035(3) 0.039(3) -0.006(2) 0.004(2) -0.004(2) O61 0.034(2) 0.0162(17) 0.0241(18) 0.0017(14) 0.0003(15) 0.0026(15) C62 0.024(2) 0.022(2) 0.025(2) 0.005(2) 0.0001(19) 0.000(2) C63 0.035(3) 0.023(3) 0.028(3) 0.002(2) 0.004(2) 0.004(2) C64 0.034(3) 0.020(3) 0.032(3) 0.006(2) -0.004(2) 0.008(2) C65 0.022(2) 0.028(3) 0.025(2) 0.004(2) -0.0049(19) -0.004(2) C66 0.017(2) 0.025(3) 0.026(2) 0.001(2) -0.0027(18) -0.0038(19) C67 0.022(2) 0.020(2) 0.023(2) 0.0015(19) -0.0023(18) -0.0048(19) C68 0.025(2) 0.028(3) 0.023(2) 0.001(2) 0.0018(19) 0.003(2) N69 0.024(2) 0.024(2) 0.022(2) 0.0020(17) -0.0007(16) 0.0059(17) O70 0.052(3) 0.031(2) 0.031(2) 0.0093(18) 0.0073(19) 0.023(2) C71 0.031(3) 0.027(3) 0.027(3) 0.007(2) -0.008(2) -0.005(2) C72 0.031(3) 0.039(3) 0.025(3) 0.016(2) -0.006(2) -0.005(2) C73 0.029(3) 0.043(4) 0.029(3) -0.002(2) 0.001(2) -0.002(3) C74 0.023(2) 0.028(3) 0.030(3) 0.005(2) 0.000(2) 0.003(2) O75 0.0196(17) 0.031(2) 0.0298(19) 0.0023(16) -0.0047(14) 0.0045(15) C76 0.018(2) 0.033(3) 0.021(2) 0.004(2) -0.0009(18) -0.006(2) C77 0.033(3) 0.044(4) 0.029(3) 0.013(3) -0.013(2) -0.003(3) C78 0.032(3) 0.065(5) 0.033(3) 0.011(3) -0.015(3) -0.005(3) C79 0.027(3) 0.064(4) 0.021(3) -0.002(3) -0.004(2) -0.008(3) C80 0.022(2) 0.039(3) 0.022(2) -0.004(2) -0.0030(19) -0.003(2) C81 0.017(2) 0.028(3) 0.022(2) -0.0019(19) -0.0044(17) 0.0022(19) C82 0.023(2) 0.019(2) 0.020(2) -0.0016(18) -0.0008(18) 0.0023(19) N83 0.0157(18) 0.019(2) 0.022(2) 0.0016(15) -0.0050(15) -0.0018(15) O84 0.0163(15) 0.0170(16) 0.0231(17) 0.0022(13) -0.0052(12) -0.0006(13) C85 0.038(4) 0.074(6) 0.034(3) -0.015(3) -0.011(3) -0.016(4) C86 0.045(4) 0.071(6) 0.054(5) -0.035(4) -0.008(3) -0.019(4) C87 0.049(4) 0.045(4) 0.058(5) -0.019(4) -0.010(4) -0.002(3) C88 0.028(3) 0.035(3) 0.041(3) -0.015(3) -0.010(2) -0.004(2) O89 0.0248(17) 0.0222(18) 0.0188(16) -0.0009(14) -0.0020(13) 0.0038(14) C90 0.017(2) 0.018(2) 0.026(2) -0.0031(19) 0.0013(18) 0.0035(18) C91 0.033(3) 0.035(3) 0.031(3) 0.006(2) 0.009(2) 0.009(2) C92 0.029(3) 0.042(4) 0.054(4) 0.013(3) 0.020(3) 0.014(3) C93 0.022(3) 0.021(3) 0.051(4) 0.003(2) 0.000(2) 0.002(2) C94 0.024(2) 0.016(2) 0.036(3) -0.003(2) -0.008(2) 0.0057(19) C95 0.023(2) 0.013(2) 0.024(2) -0.0028(17) -0.0001(18) -0.0003(18) C96 0.020(2) 0.015(2) 0.028(2) 0.0032(18) -0.0006(18) 0.0038(18) N97 0.023(2) 0.020(2) 0.021(2) -0.0004(16) 0.0007(16) -0.0005(16) O98 0.035(2) 0.0215(19) 0.035(2) 0.0076(16) 0.0085(17) 0.0105(16) C99 0.023(3) 0.032(3) 0.065(5) 0.007(3) 0.007(3) 0.006(2) C100 0.022(3) 0.029(3) 0.076(5) -0.001(3) -0.006(3) 0.004(2) C101 0.035(3) 0.031(3) 0.055(4) 0.002(3) -0.021(3) 0.009(3) C102 0.027(3) 0.027(3) 0.043(3) -0.005(2) -0.008(2) 0.007(2) O103 0.0160(15) 0.0200(17) 0.0238(17) -0.0009(13) -0.0007(13) -0.0020(13) C104 0.018(2) 0.016(2) 0.026(2) -0.0001(18) -0.0046(18) -0.0037(17) C105 0.016(2) 0.029(3) 0.032(3) -0.002(2) -0.0010(19) 0.001(2) C106 0.016(2) 0.024(3) 0.038(3) 0.000(2) -0.006(2) 0.0003(19) C107 0.022(2) 0.014(2) 0.029(3) 0.0033(18) -0.0109(19) 0.0012(18) C108 0.023(2) 0.012(2) 0.030(3) 0.0007(18) -0.0128(19) -0.0006(18) C109 0.017(2) 0.011(2) 0.021(2) 0.0012(16) -0.0063(16) 0.0010(16) C110 0.023(2) 0.012(2) 0.016(2) -0.0018(15) -0.0005(16) -0.0017(17) N111 0.0155(17) 0.0155(18) 0.0166(18) -0.0001(14) 0.0003(14) 0.0004(14) O112 0.0133(14) 0.0134(15) 0.0248(17) 0.0027(13) 0.0013(12) 0.0036(12) C113 0.031(3) 0.022(3) 0.029(3) 0.008(2) -0.012(2) 0.000(2) C114 0.038(3) 0.024(3) 0.032(3) 0.006(2) -0.019(2) -0.004(2) C115 0.043(3) 0.027(3) 0.024(3) 0.002(2) -0.006(2) -0.002(2) C116 0.028(3) 0.024(3) 0.028(3) 0.004(2) -0.003(2) 0.001(2) O117 0.044(3) 0.028(2) 0.043(3) 0.0037(19) 0.002(2) 0.0018(19) C118 0.047(4) 0.035(3) 0.036(3) -0.004(3) 0.002(3) -0.014(3) C119 0.055(4) 0.057(5) 0.037(4) -0.008(3) 0.003(3) 0.003(4) C120 0.060(5) 0.032(3) 0.047(4) 0.004(3) -0.010(3) 0.001(3) C121 0.052(5) 0.040(4) 0.081(6) -0.001(4) 0.004(4) 0.004(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.09221(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 . O5 . 1.931(3) yes Mn1 . N13 . 2.195(4) yes Mn1 . O19 . 1.860(4) yes Mn1 . N27 . 2.013(4) yes Mn1 . O84 . 2.253(4) yes Mn1 . O112 . 1.954(3) yes Mn2 . O28 . 1.956(4) yes Mn2 . O33 . 1.909(3) yes Mn2 . N41 . 2.210(4) yes Mn2 . O47 . 1.873(4) yes Mn2 . N55 . 2.014(4) yes Mn2 . O112 . 2.223(3) yes Mn3 . O28 . 2.224(3) yes Mn3 . O56 . 1.957(3) yes Mn3 . O61 . 1.900(4) yes Mn3 . N69 . 2.227(5) yes Mn3 . O75 . 1.865(4) yes Mn3 . N83 . 2.010(4) yes Mn4 . O56 . 2.189(4) yes Mn4 . O84 . 1.954(3) yes Mn4 . O89 . 1.915(4) yes Mn4 . N97 . 2.211(4) yes Mn4 . O103 . 1.882(3) yes Mn4 . N111 . 2.010(4) yes O5 . C6 . 1.338(6) yes C6 . C7 . 1.437(7) yes C6 . C11 . 1.395(7) yes C7 . C8 . 1.343(7) yes C7 . H71 . 0.927 no C8 . C9 . 1.419(8) yes C8 . H81 . 0.932 no C9 . C10 . 1.419(8) yes C9 . C15 . 1.415(7) yes C10 . C11 . 1.442(7) yes C10 . C18 . 1.415(7) yes C11 . C12 . 1.457(7) yes C12 . N13 . 1.278(6) yes C12 . H121 . 0.926 no N13 . O14 . 1.400(5) yes O14 . H141 . 0.817 no C15 . C16 . 1.353(8) yes C15 . H151 . 0.929 no C16 . C17 . 1.399(9) yes C16 . H161 . 0.931 no C17 . C18 . 1.370(7) yes C17 . H171 . 0.932 no C18 . H181 . 0.926 no O19 . C20 . 1.324(6) yes C20 . C21 . 1.419(7) yes C20 . C25 . 1.403(7) yes C21 . C22 . 1.350(8) yes C21 . H211 . 0.929 no C22 . C23 . 1.418(9) yes C22 . H221 . 0.935 no C23 . C24 . 1.425(8) yes C23 . C29 . 1.410(8) yes C24 . C25 . 1.438(7) yes C24 . C32 . 1.413(8) yes C25 . C26 . 1.445(7) yes C26 . N27 . 1.295(6) yes C26 . H261 . 0.937 no N27 . O28 . 1.395(5) yes C29 . C30 . 1.360(10) yes C29 . H291 . 0.929 no C30 . C31 . 1.383(9) yes C30 . H301 . 0.931 no C31 . C32 . 1.376(8) yes C31 . H311 . 0.927 no C32 . H321 . 0.927 no O33 . C34 . 1.330(6) yes C34 . C35 . 1.423(7) yes C34 . C39 . 1.406(7) yes C35 . C36 . 1.351(8) yes C35 . H351 . 0.920 no C36 . C37 . 1.406(8) yes C36 . H361 . 0.924 no C37 . C38 . 1.412(8) yes C37 . C43 . 1.416(8) yes C38 . C39 . 1.437(7) yes C38 . C46 . 1.427(8) yes C39 . C40 . 1.455(8) yes C40 . N41 . 1.277(7) yes C40 . H401 . 0.934 no N41 . O42 . 1.401(6) yes O42 . H421 . 0.813 no C43 . C44 . 1.358(9) yes C43 . H431 . 0.925 no C44 . C45 . 1.389(10) yes C44 . H441 . 0.925 no C45 . C46 . 1.374(9) yes C45 . H451 . 0.929 no C46 . H461 . 0.931 no O47 . C48 . 1.334(6) yes C48 . C49 . 1.422(7) yes C48 . C53 . 1.398(7) yes C49 . C50 . 1.355(8) yes C49 . H491 . 0.925 no C50 . C51 . 1.411(8) yes C50 . H501 . 0.921 no C51 . C52 . 1.409(7) yes C51 . C57 . 1.427(8) yes C52 . C53 . 1.437(7) yes C52 . C60 . 1.410(7) yes C53 . C54 . 1.426(7) yes C54 . N55 . 1.297(6) yes C54 . H541 . 0.923 no N55 . O56 . 1.388(5) yes C57 . C58 . 1.350(9) yes C57 . H571 . 0.926 no C58 . C59 . 1.397(10) yes C58 . H581 . 0.930 no C59 . C60 . 1.361(8) yes C59 . H591 . 0.927 no C60 . H601 . 0.925 no O61 . C62 . 1.335(6) yes C62 . C63 . 1.416(7) yes C62 . C67 . 1.399(7) yes C63 . C64 . 1.356(8) yes C63 . H631 . 0.933 no C64 . C65 . 1.412(8) yes C64 . H641 . 0.926 no C65 . C66 . 1.426(8) yes C65 . C71 . 1.401(7) yes C66 . C67 . 1.445(7) yes C66 . C74 . 1.413(8) yes C67 . C68 . 1.450(7) yes C68 . N69 . 1.274(7) yes C68 . H681 . 0.928 no N69 . O70 . 1.406(6) yes O70 . H701 . 0.814 no C71 . C72 . 1.363(9) yes C71 . H711 . 0.927 no C72 . C73 . 1.411(9) yes C72 . H721 . 0.926 no C73 . C74 . 1.366(8) yes C73 . H731 . 0.924 no C74 . H741 . 0.925 no O75 . C76 . 1.317(7) yes C76 . C77 . 1.425(7) yes C76 . C81 . 1.408(8) yes C77 . C78 . 1.350(9) yes C77 . H771 . 0.927 no C78 . C79 . 1.419(11) yes C78 . H781 . 0.927 no C79 . C80 . 1.423(8) yes C79 . C85 . 1.411(9) yes C80 . C81 . 1.445(7) yes C80 . C88 . 1.398(9) yes C81 . C82 . 1.438(7) yes C82 . N83 . 1.286(6) yes C82 . H821 . 0.933 no N83 . O84 . 1.396(5) yes C85 . C86 . 1.352(12) yes C85 . H851 . 0.928 no C86 . C87 . 1.401(11) yes C86 . H861 . 0.931 no C87 . C88 . 1.373(9) yes C87 . H871 . 0.926 no C88 . H881 . 0.937 no O89 . C90 . 1.343(6) yes C90 . C91 . 1.434(7) yes C90 . C95 . 1.388(7) yes C91 . C92 . 1.367(8) yes C91 . H911 . 0.931 no C92 . C93 . 1.413(9) yes C92 . H921 . 0.927 no C93 . C94 . 1.411(9) yes C93 . C99 . 1.412(8) yes C94 . C95 . 1.439(7) yes C94 . C102 . 1.411(8) yes C95 . C96 . 1.463(7) yes C96 . N97 . 1.272(6) yes C96 . H961 . 0.930 no N97 . O98 . 1.394(6) yes O98 . H981 . 0.820 no C99 . C100 . 1.337(10) yes C99 . H991 . 0.925 no C100 . C101 . 1.404(11) yes C100 . H1001 . 0.928 no C101 . C102 . 1.376(8) yes C101 . H1011 . 0.921 no C102 . H1021 . 0.924 no O103 . C104 . 1.321(6) yes C104 . C105 . 1.421(7) yes C104 . C109 . 1.408(7) yes C105 . C106 . 1.365(8) yes C105 . H1051 . 0.927 no C106 . C107 . 1.423(8) yes C106 . H1061 . 0.929 no C107 . C108 . 1.410(7) yes C107 . C113 . 1.416(7) yes C108 . C109 . 1.445(6) yes C108 . C116 . 1.411(8) yes C109 . C110 . 1.429(6) yes C110 . N111 . 1.288(6) yes C110 . H1101 . 0.928 no N111 . O112 . 1.394(5) yes C113 . C114 . 1.370(9) yes C113 . H1131 . 0.931 no C114 . C115 . 1.395(9) yes C114 . H1141 . 0.924 no C115 . C116 . 1.371(7) yes C115 . H1151 . 0.929 no C116 . H1161 . 0.928 no O117 . C118 . 1.408(8) yes O117 . C120 . 1.409(8) yes C118 . C119 . 1.507(10) yes C118 . H1182 . 0.979 no C118 . H1181 . 0.970 no C119 . H1192 . 0.962 no C119 . H1191 . 0.973 no C119 . H1193 . 0.960 no C120 . C121 . 1.485(11) yes C120 . H1201 . 0.967 no C120 . H1202 . 0.967 no C121 . H1211 . 0.957 no C121 . H1213 . 0.966 no C121 . H1212 . 0.951 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 O5 . Mn1 . N13 . 83.83(16) yes O5 . Mn1 . O19 . 94.95(16) yes N13 . Mn1 . O19 . 92.53(16) yes O5 . Mn1 . N27 . 175.45(16) yes N13 . Mn1 . N27 . 92.22(16) yes O19 . Mn1 . N27 . 87.47(16) yes O5 . Mn1 . O84 . 92.62(14) yes N13 . Mn1 . O84 . 173.71(14) yes O19 . Mn1 . O84 . 92.96(15) yes N27 . Mn1 . O84 . 91.10(14) yes O5 . Mn1 . O112 . 91.37(14) yes N13 . Mn1 . O112 . 90.66(15) yes O19 . Mn1 . O112 . 173.19(16) yes N27 . Mn1 . O112 . 86.39(15) yes O84 . Mn1 . O112 . 84.22(13) yes O28 . Mn2 . O33 . 92.62(14) yes O28 . Mn2 . N41 . 94.45(15) yes O33 . Mn2 . N41 . 83.38(16) yes O28 . Mn2 . O47 . 173.41(15) yes O33 . Mn2 . O47 . 93.64(15) yes N41 . Mn2 . O47 . 88.33(16) yes O28 . Mn2 . N55 . 87.37(15) yes O33 . Mn2 . N55 . 176.14(16) yes N41 . Mn2 . N55 . 92.77(16) yes O47 . Mn2 . N55 . 86.52(16) yes O28 . Mn2 . O112 . 82.39(13) yes O33 . Mn2 . O112 . 93.08(14) yes N41 . Mn2 . O112 . 175.16(15) yes O47 . Mn2 . O112 . 95.20(14) yes N55 . Mn2 . O112 . 90.74(14) yes O28 . Mn3 . O56 . 83.49(13) yes O28 . Mn3 . O61 . 87.16(14) yes O56 . Mn3 . O61 . 93.39(16) yes O28 . Mn3 . N69 . 165.34(15) yes O56 . Mn3 . N69 . 87.31(15) yes O61 . Mn3 . N69 . 82.00(17) yes O28 . Mn3 . O75 . 94.09(15) yes O56 . Mn3 . O75 . 173.03(17) yes O61 . Mn3 . O75 . 93.03(17) yes N69 . Mn3 . O75 . 96.30(17) yes O28 . Mn3 . N83 . 92.65(15) yes O56 . Mn3 . N83 . 86.38(15) yes O61 . Mn3 . N83 . 179.72(17) yes N69 . Mn3 . N83 . 98.15(17) yes O75 . Mn3 . N83 . 87.20(17) yes O56 . Mn4 . O84 . 83.61(13) yes O56 . Mn4 . O89 . 92.48(14) yes O84 . Mn4 . O89 . 93.55(15) yes O56 . Mn4 . N97 . 173.28(14) yes O84 . Mn4 . N97 . 91.64(15) yes O89 . Mn4 . N97 . 83.04(16) yes O56 . Mn4 . O103 . 94.73(14) yes O84 . Mn4 . O103 . 172.20(16) yes O89 . Mn4 . O103 . 94.14(15) yes N97 . Mn4 . O103 . 90.60(16) yes O56 . Mn4 . N111 . 92.16(14) yes O84 . Mn4 . N111 . 87.11(15) yes O89 . Mn4 . N111 . 175.35(16) yes N97 . Mn4 . N111 . 92.34(16) yes O103 . Mn4 . N111 . 85.34(16) yes Mn1 . O5 . C6 . 124.4(3) yes O5 . C6 . C7 . 117.4(5) yes O5 . C6 . C11 . 123.7(4) yes C7 . C6 . C11 . 118.8(5) yes C6 . C7 . C8 . 121.1(5) yes C6 . C7 . H71 . 119.6 no C8 . C7 . H71 . 119.4 no C7 . C8 . C9 . 121.9(5) yes C7 . C8 . H81 . 119.2 no C9 . C8 . H81 . 118.9 no C8 . C9 . C10 . 118.5(5) yes C8 . C9 . C15 . 122.1(5) yes C10 . C9 . C15 . 119.3(5) yes C9 . C10 . C11 . 119.4(5) yes C9 . C10 . C18 . 117.6(5) yes C11 . C10 . C18 . 122.9(5) yes C10 . C11 . C6 . 119.5(5) yes C10 . C11 . C12 . 118.1(5) yes C6 . C11 . C12 . 122.1(5) yes C11 . C12 . N13 . 124.0(5) yes C11 . C12 . H121 . 117.8 no N13 . C12 . H121 . 118.2 no Mn1 . N13 . C12 . 120.7(4) yes Mn1 . N13 . O14 . 125.7(3) yes C12 . N13 . O14 . 112.7(4) yes N13 . O14 . H141 . 105.8 no C9 . C15 . C16 . 121.1(5) yes C9 . C15 . H151 . 118.9 no C16 . C15 . H151 . 120.0 no C15 . C16 . C17 . 120.4(5) yes C15 . C16 . H161 . 120.0 no C17 . C16 . H161 . 119.6 no C16 . C17 . C18 . 120.0(5) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 119.8 no C10 . C18 . C17 . 121.5(5) yes C10 . C18 . H181 . 118.8 no C17 . C18 . H181 . 119.7 no Mn1 . O19 . C20 . 127.8(3) yes O19 . C20 . C21 . 117.8(5) yes O19 . C20 . C25 . 123.4(5) yes C21 . C20 . C25 . 118.8(5) yes C20 . C21 . C22 . 121.4(6) yes C20 . C21 . H211 . 119.4 no C22 . C21 . H211 . 119.1 no C21 . C22 . C23 . 121.7(6) yes C21 . C22 . H221 . 119.6 no C23 . C22 . H221 . 118.8 no C22 . C23 . C24 . 118.8(5) yes C22 . C23 . C29 . 121.7(6) yes C24 . C23 . C29 . 119.5(6) yes C23 . C24 . C25 . 118.7(5) yes C23 . C24 . C32 . 117.5(5) yes C25 . C24 . C32 . 123.8(5) yes C24 . C25 . C20 . 120.5(5) yes C24 . C25 . C26 . 119.4(5) yes C20 . C25 . C26 . 119.9(4) yes C25 . C26 . N27 . 123.5(4) yes C25 . C26 . H261 . 118.1 no N27 . C26 . H261 . 118.4 no Mn1 . N27 . C26 . 126.8(3) yes Mn1 . N27 . O28 . 118.4(3) yes C26 . N27 . O28 . 113.4(4) yes Mn3 . O28 . N27 . 109.9(3) yes Mn3 . O28 . Mn2 . 115.69(15) yes N27 . O28 . Mn2 . 116.7(3) yes C23 . C29 . C30 . 121.5(6) yes C23 . C29 . H291 . 119.4 no C30 . C29 . H291 . 119.1 no C29 . C30 . C31 . 119.2(6) yes C29 . C30 . H301 . 120.3 no C31 . C30 . H301 . 120.5 no C30 . C31 . C32 . 121.7(6) yes C30 . C31 . H311 . 119.2 no C32 . C31 . H311 . 119.0 no C24 . C32 . C31 . 120.6(6) yes C24 . C32 . H321 . 119.5 no C31 . C32 . H321 . 119.9 no Mn2 . O33 . C34 . 124.1(3) yes O33 . C34 . C35 . 117.1(5) yes O33 . C34 . C39 . 124.3(5) yes C35 . C34 . C39 . 118.5(5) yes C34 . C35 . C36 . 121.7(5) yes C34 . C35 . H351 . 119.3 no C36 . C35 . H351 . 119.0 no C35 . C36 . C37 . 121.6(5) yes C35 . C36 . H361 . 119.6 no C37 . C36 . H361 . 118.8 no C36 . C37 . C38 . 118.4(5) yes C36 . C37 . C43 . 121.3(6) yes C38 . C37 . C43 . 120.2(6) yes C37 . C38 . C39 . 120.2(5) yes C37 . C38 . C46 . 117.2(5) yes C39 . C38 . C46 . 122.5(5) yes C38 . C39 . C34 . 119.0(5) yes C38 . C39 . C40 . 119.2(5) yes C34 . C39 . C40 . 121.6(5) yes C39 . C40 . N41 . 123.9(5) yes C39 . C40 . H401 . 118.3 no N41 . C40 . H401 . 117.8 no Mn2 . N41 . C40 . 120.6(4) yes Mn2 . N41 . O42 . 125.6(3) yes C40 . N41 . O42 . 112.0(4) yes N41 . O42 . H421 . 107.1 no C37 . C43 . C44 . 121.0(6) yes C37 . C43 . H431 . 119.1 no C44 . C43 . H431 . 119.9 no C43 . C44 . C45 . 119.5(6) yes C43 . C44 . H441 . 120.6 no C45 . C44 . H441 . 119.9 no C44 . C45 . C46 . 121.6(6) yes C44 . C45 . H451 . 119.3 no C46 . C45 . H451 . 119.1 no C38 . C46 . C45 . 120.5(6) yes C38 . C46 . H461 . 119.9 no C45 . C46 . H461 . 119.5 no Mn2 . O47 . C48 . 124.8(3) yes O47 . C48 . C49 . 116.9(5) yes O47 . C48 . C53 . 124.0(4) yes C49 . C48 . C53 . 119.1(5) yes C48 . C49 . C50 . 120.6(5) yes C48 . C49 . H491 . 120.0 no C50 . C49 . H491 . 119.4 no C49 . C50 . C51 . 121.4(5) yes C49 . C50 . H501 . 119.2 no C51 . C50 . H501 . 119.4 no C50 . C51 . C52 . 119.8(5) yes C50 . C51 . C57 . 121.1(5) yes C52 . C51 . C57 . 119.0(5) yes C51 . C52 . C53 . 118.3(4) yes C51 . C52 . C60 . 118.1(5) yes C53 . C52 . C60 . 123.6(5) yes C52 . C53 . C48 . 120.4(4) yes C52 . C53 . C54 . 119.6(4) yes C48 . C53 . C54 . 119.8(4) yes C53 . C54 . N55 . 123.2(4) yes C53 . C54 . H541 . 118.5 no N55 . C54 . H541 . 118.3 no Mn2 . N55 . C54 . 127.4(3) yes Mn2 . N55 . O56 . 117.9(3) yes C54 . N55 . O56 . 113.6(4) yes Mn4 . O56 . N55 . 112.2(3) yes Mn4 . O56 . Mn3 . 117.52(16) yes N55 . O56 . Mn3 . 114.4(3) yes C51 . C57 . C58 . 120.8(6) yes C51 . C57 . H571 . 119.4 no C58 . C57 . H571 . 119.8 no C57 . C58 . C59 . 120.2(6) yes C57 . C58 . H581 . 120.4 no C59 . C58 . H581 . 119.4 no C58 . C59 . C60 . 120.4(6) yes C58 . C59 . H591 . 119.7 no C60 . C59 . H591 . 119.9 no C52 . C60 . C59 . 121.4(6) yes C52 . C60 . H601 . 119.2 no C59 . C60 . H601 . 119.4 no Mn3 . O61 . C62 . 123.2(3) yes O61 . C62 . C63 . 116.7(5) yes O61 . C62 . C67 . 122.6(5) yes C63 . C62 . C67 . 120.6(5) yes C62 . C63 . C64 . 120.8(5) yes C62 . C63 . H631 . 119.4 no C64 . C63 . H631 . 119.8 no C63 . C64 . C65 . 121.4(5) yes C63 . C64 . H641 . 119.3 no C65 . C64 . H641 . 119.3 no C64 . C65 . C66 . 118.9(5) yes C64 . C65 . C71 . 121.4(5) yes C66 . C65 . C71 . 119.7(5) yes C65 . C66 . C67 . 119.7(5) yes C65 . C66 . C74 . 117.5(5) yes C67 . C66 . C74 . 122.8(5) yes C66 . C67 . C62 . 118.5(5) yes C66 . C67 . C68 . 120.1(5) yes C62 . C67 . C68 . 121.4(5) yes C67 . C68 . N69 . 123.7(5) yes C67 . C68 . H681 . 118.0 no N69 . C68 . H681 . 118.3 no Mn3 . N69 . C68 . 123.0(4) yes Mn3 . N69 . O70 . 124.5(3) yes C68 . N69 . O70 . 112.4(4) yes N69 . O70 . H701 . 100.5 no C65 . C71 . C72 . 121.9(6) yes C65 . C71 . H711 . 118.6 no C72 . C71 . H711 . 119.4 no C71 . C72 . C73 . 118.5(5) yes C71 . C72 . H721 . 121.0 no C73 . C72 . H721 . 120.5 no C72 . C73 . C74 . 121.3(6) yes C72 . C73 . H731 . 119.3 no C74 . C73 . H731 . 119.4 no C66 . C74 . C73 . 121.1(5) yes C66 . C74 . H741 . 119.7 no C73 . C74 . H741 . 119.2 no Mn3 . O75 . C76 . 127.5(3) yes O75 . C76 . C77 . 116.7(5) yes O75 . C76 . C81 . 124.1(5) yes C77 . C76 . C81 . 119.1(5) yes C76 . C77 . C78 . 120.8(6) yes C76 . C77 . H771 . 119.3 no C78 . C77 . H771 . 119.9 no C77 . C78 . C79 . 121.9(6) yes C77 . C78 . H781 . 118.9 no C79 . C78 . H781 . 119.3 no C78 . C79 . C80 . 119.5(6) yes C78 . C79 . C85 . 121.6(6) yes C80 . C79 . C85 . 118.9(7) yes C79 . C80 . C81 . 118.1(6) yes C79 . C80 . C88 . 118.4(6) yes C81 . C80 . C88 . 123.4(5) yes C80 . C81 . C76 . 120.4(5) yes C80 . C81 . C82 . 120.1(5) yes C76 . C81 . C82 . 119.4(5) yes C81 . C82 . N83 . 124.1(5) yes C81 . C82 . H821 . 117.9 no N83 . C82 . H821 . 118.0 no Mn3 . N83 . C82 . 126.7(3) yes Mn3 . N83 . O84 . 118.2(3) yes C82 . N83 . O84 . 114.2(4) yes Mn1 . O84 . N83 . 111.3(3) yes Mn1 . O84 . Mn4 . 114.60(16) yes N83 . O84 . Mn4 . 115.1(3) yes C79 . C85 . C86 . 121.3(7) yes C79 . C85 . H851 . 119.2 no C86 . C85 . H851 . 119.5 no C85 . C86 . C87 . 119.9(6) yes C85 . C86 . H861 . 119.7 no C87 . C86 . H861 . 120.4 no C86 . C87 . C88 . 120.4(8) yes C86 . C87 . H871 . 120.1 no C88 . C87 . H871 . 119.5 no C80 . C88 . C87 . 121.0(6) yes C80 . C88 . H881 . 119.2 no C87 . C88 . H881 . 119.8 no Mn4 . O89 . C90 . 119.1(3) yes O89 . C90 . C91 . 116.8(5) yes O89 . C90 . C95 . 124.1(5) yes C91 . C90 . C95 . 119.2(5) yes C90 . C91 . C92 . 120.3(6) yes C90 . C91 . H911 . 119.6 no C92 . C91 . H911 . 120.1 no C91 . C92 . C93 . 121.5(6) yes C91 . C92 . H921 . 119.6 no C93 . C92 . H921 . 118.9 no C92 . C93 . C94 . 119.1(5) yes C92 . C93 . C99 . 121.6(6) yes C94 . C93 . C99 . 119.2(6) yes C93 . C94 . C95 . 119.3(5) yes C93 . C94 . C102 . 118.0(5) yes C95 . C94 . C102 . 122.6(5) yes C94 . C95 . C90 . 120.2(5) yes C94 . C95 . C96 . 118.8(5) yes C90 . C95 . C96 . 121.0(4) yes C95 . C96 . N97 . 123.3(5) yes C95 . C96 . H961 . 118.4 no N97 . C96 . H961 . 118.3 no Mn4 . N97 . C96 . 119.7(4) yes Mn4 . N97 . O98 . 127.0(3) yes C96 . N97 . O98 . 113.0(4) yes N97 . O98 . H981 . 107.9 no C93 . C99 . C100 . 121.7(7) yes C93 . C99 . H991 . 119.0 no C100 . C99 . H991 . 119.3 no C99 . C100 . C101 . 120.0(6) yes C99 . C100 . H1001 . 120.0 no C101 . C100 . H1001 . 120.1 no C100 . C101 . C102 . 120.2(6) yes C100 . C101 . H1011 . 120.3 no C102 . C101 . H1011 . 119.5 no C94 . C102 . C101 . 120.8(6) yes C94 . C102 . H1021 . 119.4 no C101 . C102 . H1021 . 119.8 no Mn4 . O103 . C104 . 123.7(3) yes O103 . C104 . C105 . 117.8(5) yes O103 . C104 . C109 . 123.2(4) yes C105 . C104 . C109 . 118.9(4) yes C104 . C105 . C106 . 121.0(5) yes C104 . C105 . H1051 . 119.5 no C106 . C105 . H1051 . 119.5 no C105 . C106 . C107 . 121.2(5) yes C105 . C106 . H1061 . 119.8 no C107 . C106 . H1061 . 118.9 no C106 . C107 . C108 . 119.7(5) yes C106 . C107 . C113 . 121.0(5) yes C108 . C107 . C113 . 119.2(5) yes C107 . C108 . C109 . 118.5(5) yes C107 . C108 . C116 . 118.8(5) yes C109 . C108 . C116 . 122.7(5) yes C108 . C109 . C104 . 120.5(4) yes C108 . C109 . C110 . 120.1(4) yes C104 . C109 . C110 . 119.1(4) yes C109 . C110 . N111 . 123.2(4) yes C109 . C110 . H1101 . 118.0 no N111 . C110 . H1101 . 118.8 no Mn4 . N111 . C110 . 126.0(3) yes Mn4 . N111 . O112 . 118.5(3) yes C110 . N111 . O112 . 115.2(4) yes Mn2 . O112 . N111 . 113.5(2) yes Mn2 . O112 . Mn1 . 117.91(15) yes N111 . O112 . Mn1 . 111.9(3) yes C107 . C113 . C114 . 120.7(5) yes C107 . C113 . H1131 . 119.9 no C114 . C113 . H1131 . 119.5 no C113 . C114 . C115 . 119.8(5) yes C113 . C114 . H1141 . 120.4 no C115 . C114 . H1141 . 119.8 no C114 . C115 . C116 . 120.9(6) yes C114 . C115 . H1151 . 119.6 no C116 . C115 . H1151 . 119.4 no C108 . C116 . C115 . 120.5(5) yes C108 . C116 . H1161 . 120.2 no C115 . C116 . H1161 . 119.4 no C118 . O117 . C120 . 112.7(5) yes O117 . C118 . C119 . 108.4(6) yes O117 . C118 . H1182 . 109.4 no C119 . C118 . H1182 . 109.8 no O117 . C118 . H1181 . 109.7 no C119 . C118 . H1181 . 110.7 no H1182 . C118 . H1181 . 108.8 no C118 . C119 . H1192 . 109.2 no C118 . C119 . H1191 . 108.9 no H1192 . C119 . H1191 . 110.0 no C118 . C119 . H1193 . 108.7 no H1192 . C119 . H1193 . 110.6 no H1191 . C119 . H1193 . 109.4 no O117 . C120 . C121 . 109.5(6) yes O117 . C120 . H1201 . 108.8 no C121 . C120 . H1201 . 108.9 no O117 . C120 . H1202 . 110.3 no C121 . C120 . H1202 . 110.2 no H1201 . C120 . H1202 . 109.1 no C120 . C121 . H1211 . 110.3 no C120 . C121 . H1213 . 110.0 no H1211 . C121 . H1213 . 108.2 no C120 . C121 . H1212 . 110.6 no H1211 . C121 . H1212 . 109.3 no H1213 . C121 . H1212 . 108.6 no # Attachment 'Complex_3.CIF' data_c2ms96rp _database_code_depnum_ccdc_archive 'CCDC 756187' #TrackingRef 'Complex_3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H76 Mn4 N8 O16, 0.75(C2 H3 N)' _chemical_formula_sum 'C73.50 H78.25 Mn4 N8.75 O16' _chemical_formula_weight 1559.96 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 13.140(4) _cell_length_b 49.51(3) _cell_length_c 22.596(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.37(3) _cell_angle_gamma 90.00 _cell_volume 14544(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18589 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6468 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _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 'Xcalibur PX KM4CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64602 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.1695 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 62 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 27.06 _reflns_number_total 30962 _reflns_number_gt 14093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30962 _refine_ls_number_parameters 1913 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1668 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.005 _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 0.79299(5) 0.304076(13) 0.83913(2) 0.03284(17) Uani 1 1 d . . . Mn2 Mn 0.54794(5) 0.322455(13) 0.76306(2) 0.03403(17) Uani 1 1 d . . . Mn3 Mn 0.67414(5) 0.272801(14) 0.68560(2) 0.04215(19) Uani 1 1 d . . . Mn4 Mn 0.62182(5) 0.247634(13) 0.82370(2) 0.03765(18) Uani 1 1 d . . . Mn5 Mn -0.03792(5) 0.069033(14) 0.82929(2) 0.03797(18) Uani 1 1 d . . . Mn6 Mn -0.09080(5) 0.040792(14) 0.68489(2) 0.03636(18) Uani 1 1 d . . . Mn7 Mn 0.13484(5) 0.081507(14) 0.70027(2) 0.03685(18) Uani 1 1 d . . . Mn8 Mn 0.16892(5) 0.027261(14) 0.80298(2) 0.03658(18) Uani 1 1 d . . . O11 O 0.9166(2) 0.31434(6) 0.81545(10) 0.0367(7) Uani 1 1 d . . . O21 O 0.7280(2) 0.25512(5) 0.77420(10) 0.0372(7) Uani 1 1 d . . . N11 N 0.8157(3) 0.26766(7) 0.80247(12) 0.0326(9) Uani 1 1 d . . . C11 C 1.0002(3) 0.29881(10) 0.82630(15) 0.0349(11) Uani 1 1 d . . . C21 C 0.9968(3) 0.27051(10) 0.81729(15) 0.0341(11) Uani 1 1 d . . . C31 C 1.0905(4) 0.25619(10) 0.82741(16) 0.0434(12) Uani 1 1 d . . . H31 H 1.0901 0.2372 0.8213 0.052 Uiso 1 1 calc R . . C41 C 1.1818(4) 0.26888(11) 0.84580(16) 0.0412(12) Uani 1 1 d . . . H41 H 1.2439 0.2588 0.8527 0.049 Uiso 1 1 calc R . . C51 C 1.1837(3) 0.29677(11) 0.85444(16) 0.0445(13) Uani 1 1 d . . . H51 H 1.2471 0.3057 0.8672 0.053 Uiso 1 1 calc R . . C61 C 1.0937(4) 0.31138(9) 0.84455(15) 0.0382(11) Uani 1 1 d . . . H61 H 1.0957 0.3304 0.8503 0.046 Uiso 1 1 calc R . . C71 C 0.9023(3) 0.25637(9) 0.79501(15) 0.0346(11) Uani 1 1 d . . . C81 C 0.9053(3) 0.22925(9) 0.76492(18) 0.0478(13) Uani 1 1 d . . . H81A H 0.9687 0.2280 0.7462 0.057 Uiso 1 1 calc R . . H81B H 0.8457 0.2278 0.7327 0.057 Uiso 1 1 calc R . . C91 C 0.9026(4) 0.20578(9) 0.80789(19) 0.0613(14) Uani 1 1 d . . . H91A H 0.9035 0.1887 0.7860 0.092 Uiso 1 1 calc R . . H91B H 0.8398 0.2068 0.8265 0.092 Uiso 1 1 calc R . . H91C H 0.9629 0.2067 0.8390 0.092 Uiso 1 1 calc R . . O12 O 0.7751(2) 0.33815(5) 0.87570(10) 0.0334(7) Uani 1 1 d . . . O22 O 0.8442(2) 0.26848(6) 0.95868(10) 0.0394(7) Uani 1 1 d . . . H22 H 0.8053 0.2592 0.9338 0.059 Uiso 1 1 calc R . . N12 N 0.8631(2) 0.29341(7) 0.93305(13) 0.0321(9) Uani 1 1 d . . . C12 C 0.8587(3) 0.35061(9) 0.90293(16) 0.0299(10) Uani 1 1 d . . . C22 C 0.9290(3) 0.33795(9) 0.94817(15) 0.0308(10) Uani 1 1 d . . . C32 C 1.0166(3) 0.35194(9) 0.97337(16) 0.0347(11) Uani 1 1 d . . . H32 H 1.0642 0.3433 1.0031 0.042 Uiso 1 1 calc R . . C42 C 1.0362(3) 0.37786(9) 0.95643(17) 0.0376(11) Uani 1 1 d . . . H42 H 1.0966 0.3870 0.9741 0.045 Uiso 1 1 calc R . . C52 C 0.9670(4) 0.39036(9) 0.91348(17) 0.0419(12) Uani 1 1 d . . . H52 H 0.9794 0.4083 0.9017 0.050 Uiso 1 1 calc R . . C62 C 0.8801(3) 0.37706(9) 0.88748(17) 0.0382(11) Uani 1 1 d . . . H62 H 0.8332 0.3861 0.8581 0.046 Uiso 1 1 calc R . . C72 C 0.9100(3) 0.31043(9) 0.97004(16) 0.0310(11) Uani 1 1 d . . . C82 C 0.9383(3) 0.30373(9) 1.03522(15) 0.0409(12) Uani 1 1 d . . . H82A H 1.0056 0.3120 1.0506 0.049 Uiso 1 1 calc R . . H82B H 0.9449 0.2839 1.0401 0.049 Uiso 1 1 calc R . . C92 C 0.8580(4) 0.31403(10) 1.07074(18) 0.0693(16) Uani 1 1 d . . . H92A H 0.8790 0.3100 1.1132 0.104 Uiso 1 1 calc R . . H92B H 0.7921 0.3052 1.0568 0.104 Uiso 1 1 calc R . . H92C H 0.8506 0.3336 1.0653 0.104 Uiso 1 1 calc R . . O13 O 0.4126(2) 0.32402(5) 0.77758(10) 0.0368(7) Uani 1 1 d . . . O23 O 0.6611(2) 0.28988(5) 0.85665(9) 0.0315(7) Uani 1 1 d . . . N13 N 0.5820(2) 0.30854(6) 0.84783(12) 0.0301(8) Uani 1 1 d . . . C13 C 0.3909(3) 0.33681(9) 0.82613(17) 0.0352(11) Uani 1 1 d . . . C23 C 0.4468(3) 0.33279(8) 0.88379(16) 0.0328(11) Uani 1 1 d . . . C33 C 0.4135(3) 0.34561(9) 0.93267(17) 0.0413(12) Uani 1 1 d . . . H33 H 0.4493 0.3425 0.9718 0.050 Uiso 1 1 calc R . . C43 C 0.3297(3) 0.36263(9) 0.9250(2) 0.0475(13) Uani 1 1 d . . . H43 H 0.3085 0.3714 0.9586 0.057 Uiso 1 1 calc R . . C53 C 0.2765(3) 0.36698(9) 0.8685(2) 0.0473(12) Uani 1 1 d . . . H53 H 0.2190 0.3788 0.8633 0.057 Uiso 1 1 calc R . . C63 C 0.3063(3) 0.35429(9) 0.81993(18) 0.0416(12) Uani 1 1 d . . . H63 H 0.2688 0.3574 0.7813 0.050 Uiso 1 1 calc R . . C73 C 0.5368(3) 0.31472(8) 0.89380(16) 0.0327(11) Uani 1 1 d . . . C83 C 0.5748(3) 0.30361(9) 0.95480(16) 0.0440(12) Uani 1 1 d . . . H83A H 0.5861 0.3188 0.9834 0.053 Uiso 1 1 calc R . . H83B H 0.6421 0.2948 0.9538 0.053 Uiso 1 1 calc R . . C93 C 0.5026(4) 0.28338(9) 0.97776(17) 0.0545(14) Uani 1 1 d . . . H93A H 0.5354 0.2759 1.0160 0.082 Uiso 1 1 calc R . . H93B H 0.4876 0.2687 0.9486 0.082 Uiso 1 1 calc R . . H93C H 0.4385 0.2925 0.9834 0.082 Uiso 1 1 calc R . . O14 O 0.5157(2) 0.33537(6) 0.68305(10) 0.0382(7) Uani 1 1 d . . . O24 O 0.6371(2) 0.37583(5) 0.83245(10) 0.0404(7) Uani 1 1 d . . . H24A H 0.6792 0.3636 0.8445 0.061 Uiso 1 1 calc R . . N14 N 0.5673(2) 0.36627(7) 0.78380(12) 0.0329(9) Uani 1 1 d . . . C14 C 0.4418(3) 0.35402(10) 0.67004(17) 0.0388(12) Uani 1 1 d . . . C24 C 0.4367(3) 0.37780(10) 0.70372(16) 0.0388(11) Uani 1 1 d . . . C34 C 0.3558(3) 0.39581(9) 0.68604(17) 0.0466(12) Uani 1 1 d . . . H34 H 0.3505 0.4118 0.7087 0.056 Uiso 1 1 calc R . . C44 C 0.2840(4) 0.39095(11) 0.6367(2) 0.0617(15) Uani 1 1 d . . . H44 H 0.2289 0.4032 0.6260 0.074 Uiso 1 1 calc R . . C54 C 0.2924(4) 0.36833(11) 0.6031(2) 0.0616(15) Uani 1 1 d . . . H54 H 0.2448 0.3654 0.5678 0.074 Uiso 1 1 calc R . . C64 C 0.3684(4) 0.34991(10) 0.61981(17) 0.0502(13) Uani 1 1 d . . . H64 H 0.3713 0.3340 0.5967 0.060 Uiso 1 1 calc R . . C74 C 0.5125(3) 0.38535(9) 0.75653(17) 0.0347(11) Uani 1 1 d . . . C84 C 0.5239(3) 0.41403(9) 0.77858(18) 0.0447(12) Uani 1 1 d . . . H84A H 0.5003 0.4264 0.7449 0.054 Uiso 1 1 calc R . . H84B H 0.5976 0.4177 0.7920 0.054 Uiso 1 1 calc R . . C94 C 0.4634(3) 0.42023(9) 0.83024(18) 0.0544(13) Uani 1 1 d . . . H94A H 0.4771 0.4389 0.8438 0.082 Uiso 1 1 calc R . . H94B H 0.4848 0.4078 0.8634 0.082 Uiso 1 1 calc R . . H94C H 0.3896 0.4180 0.8165 0.082 Uiso 1 1 calc R . . O15 O 0.8008(2) 0.26789(7) 0.65965(12) 0.0551(9) Uani 1 1 d . . . O25 O 0.69482(19) 0.32083(5) 0.75808(10) 0.0359(7) Uani 1 1 d . . . N15 N 0.7207(3) 0.31017(8) 0.70518(13) 0.0488(11) Uani 1 1 d . . . C15 C 0.8343(4) 0.28529(13) 0.6227(2) 0.0557(15) Uani 1 1 d . . . C25 C 0.8231(4) 0.31308(12) 0.62712(18) 0.0515(14) Uani 1 1 d . . . C35 C 0.8602(4) 0.33040(12) 0.5848(2) 0.0706(16) Uani 1 1 d . . . H35 H 0.8510 0.3494 0.5869 0.085 Uiso 1 1 calc R . . C45 C 0.9102(4) 0.31926(14) 0.5400(2) 0.0734(17) Uani 1 1 d . . . H45 H 0.9350 0.3306 0.5113 0.088 Uiso 1 1 calc R . . C55 C 0.9231(4) 0.29150(15) 0.5380(2) 0.0816(19) Uani 1 1 d . . . H55 H 0.9580 0.2841 0.5078 0.098 Uiso 1 1 calc R . . C65 C 0.8878(4) 0.27472(12) 0.5773(2) 0.0678(16) Uani 1 1 d . . . H65 H 0.8986 0.2558 0.5747 0.081 Uiso 1 1 calc R . . C75 C 0.7805(3) 0.32540(10) 0.67776(18) 0.0463(13) Uani 1 1 d . . . C85 C 0.8073(4) 0.35371(10) 0.69809(18) 0.0539(14) Uani 1 1 d . . . H85A H 0.8753 0.3585 0.6872 0.065 Uiso 1 1 calc R . . H85B H 0.8125 0.3546 0.7422 0.065 Uiso 1 1 calc R . . C95 C 0.7278(4) 0.37406(10) 0.6703(2) 0.0738(16) Uani 1 1 d . . . H95A H 0.7481 0.3922 0.6848 0.111 Uiso 1 1 calc R . . H95B H 0.6606 0.3696 0.6816 0.111 Uiso 1 1 calc R . . H95C H 0.7234 0.3735 0.6267 0.111 Uiso 1 1 calc R . . O16 O 0.6305(2) 0.23716(6) 0.66124(10) 0.0446(8) Uani 1 1 d . . . O26 O 0.5476(2) 0.30736(6) 0.58243(10) 0.0463(8) Uani 1 1 d . . . H26A H 0.5397 0.3150 0.6147 0.069 Uiso 1 1 calc R . . N16 N 0.5934(3) 0.28213(8) 0.59473(14) 0.0444(10) Uani 1 1 d . . . C16 C 0.6606(3) 0.22693(10) 0.61186(17) 0.0432(12) Uani 1 1 d . . . C26 C 0.6428(3) 0.24014(9) 0.55609(17) 0.0394(11) Uani 1 1 d . . . C36 C 0.6713(3) 0.22693(10) 0.50632(18) 0.0499(13) Uani 1 1 d . . . H36 H 0.6596 0.2357 0.4685 0.060 Uiso 1 1 calc R . . C46 C 0.7160(3) 0.20158(11) 0.51035(19) 0.0528(14) Uani 1 1 d . . . H46 H 0.7340 0.1930 0.4757 0.063 Uiso 1 1 calc R . . C56 C 0.7340(3) 0.18888(10) 0.56507(19) 0.0522(14) Uani 1 1 d . . . H56 H 0.7662 0.1717 0.5685 0.063 Uiso 1 1 calc R . . C66 C 0.7052(3) 0.20116(10) 0.61495(18) 0.0504(13) Uani 1 1 d . . . H66 H 0.7159 0.1919 0.6522 0.061 Uiso 1 1 calc R . . C76 C 0.5947(3) 0.26716(10) 0.54762(17) 0.0420(12) Uani 1 1 d . . . C86 C 0.5519(3) 0.27700(9) 0.48625(15) 0.0438(12) Uani 1 1 d . . . H86A H 0.4946 0.2897 0.4889 0.053 Uiso 1 1 calc R . . H86B H 0.5245 0.2615 0.4611 0.053 Uiso 1 1 calc R . . C96 C 0.6364(4) 0.29123(10) 0.45750(18) 0.0590(15) Uani 1 1 d . . . H96A H 0.6057 0.2998 0.4200 0.088 Uiso 1 1 calc R . . H96B H 0.6877 0.2779 0.4492 0.088 Uiso 1 1 calc R . . H96C H 0.6695 0.3050 0.4849 0.088 Uiso 1 1 calc R . . O17 O 0.5112(2) 0.24142(6) 0.86450(10) 0.0397(8) Uani 1 1 d . . . O27 O 0.5497(2) 0.28145(6) 0.72156(10) 0.0365(7) Uani 1 1 d . . . N17 N 0.5173(3) 0.26047(7) 0.75548(12) 0.0359(9) Uani 1 1 d . . . C17 C 0.4276(4) 0.22837(9) 0.83922(18) 0.0409(12) Uani 1 1 d . . . C27 C 0.3797(3) 0.23340(9) 0.78019(17) 0.0393(12) Uani 1 1 d . . . C37 C 0.2915(4) 0.21905(10) 0.75840(19) 0.0497(13) Uani 1 1 d . . . H37 H 0.2589 0.2224 0.7187 0.060 Uiso 1 1 calc R . . C47 C 0.2499(4) 0.20030(10) 0.7921(2) 0.0556(14) Uani 1 1 d . . . H47 H 0.1897 0.1907 0.7759 0.067 Uiso 1 1 calc R . . C57 C 0.2962(4) 0.19550(10) 0.8495(2) 0.0561(14) Uani 1 1 d . . . H57 H 0.2669 0.1827 0.8734 0.067 Uiso 1 1 calc R . . C67 C 0.3836(4) 0.20889(10) 0.87286(19) 0.0497(13) Uani 1 1 d . . . H67 H 0.4153 0.2050 0.9124 0.060 Uiso 1 1 calc R . . C77 C 0.4203(4) 0.25412(9) 0.74374(16) 0.0385(12) Uani 1 1 d . . . C87 C 0.3509(3) 0.26769(9) 0.69339(16) 0.0474(13) Uani 1 1 d . . . H87A H 0.3693 0.2871 0.6921 0.057 Uiso 1 1 calc R . . H87B H 0.2788 0.2665 0.7011 0.057 Uiso 1 1 calc R . . C97 C 0.3595(4) 0.25494(10) 0.63361(18) 0.0688(16) Uani 1 1 d . . . H97A H 0.3184 0.2653 0.6017 0.103 Uiso 1 1 calc R . . H97B H 0.3339 0.2363 0.6331 0.103 Uiso 1 1 calc R . . H97C H 0.4316 0.2549 0.6272 0.103 Uiso 1 1 calc R . . O18 O 0.7205(2) 0.23434(6) 0.88721(10) 0.0394(7) Uani 1 1 d . . . O28 O 0.5937(2) 0.19750(6) 0.73328(12) 0.0579(9) Uani 1 1 d . . . H28A H 0.6060 0.2104 0.7112 0.087 Uiso 1 1 calc R . . N18 N 0.6198(3) 0.20488(7) 0.79298(15) 0.0426(10) Uani 1 1 d . . . C18 C 0.6948(3) 0.21319(10) 0.91964(18) 0.0416(12) Uani 1 1 d . . . C28 C 0.6507(3) 0.18913(10) 0.8934(2) 0.0467(12) Uani 1 1 d . . . C38 C 0.6261(4) 0.16868(10) 0.9323(2) 0.0601(14) Uani 1 1 d . . . H38 H 0.5960 0.1524 0.9157 0.072 Uiso 1 1 calc R . . C48 C 0.6440(4) 0.17138(11) 0.9929(2) 0.0640(15) Uani 1 1 d . . . H48 H 0.6260 0.1572 1.0179 0.077 Uiso 1 1 calc R . . C58 C 0.6883(4) 0.19476(12) 1.0177(2) 0.0612(15) Uani 1 1 d . . . H58 H 0.7011 0.1968 1.0599 0.073 Uiso 1 1 calc R . . C68 C 0.7140(3) 0.21516(10) 0.98143(18) 0.0513(13) Uani 1 1 d . . . H68 H 0.7458 0.2310 0.9992 0.062 Uiso 1 1 calc R . . C78 C 0.6266(3) 0.18424(10) 0.8279(2) 0.0449(12) Uani 1 1 d . . . C88 C 0.6080(4) 0.15630(10) 0.8054(2) 0.0639(15) Uani 1 1 d . . . H88A H 0.6425 0.1433 0.8352 0.077 Uiso 1 1 calc R . . H88B H 0.6376 0.1540 0.7678 0.077 Uiso 1 1 calc R . . C98 C 0.4931(5) 0.15044(11) 0.7939(2) 0.0812(18) Uani 1 1 d . . . H98A H 0.4819 0.1318 0.7798 0.122 Uiso 1 1 calc R . . H98B H 0.4595 0.1629 0.7635 0.122 Uiso 1 1 calc R . . H98C H 0.4639 0.1528 0.8311 0.122 Uiso 1 1 calc R . . O19 O -0.0642(2) 0.10512(6) 0.84304(11) 0.0444(8) Uani 1 1 d . . . O29 O 0.1664(2) 0.06667(6) 0.79495(10) 0.0366(7) Uani 1 1 d . . . N19 N 0.1105(3) 0.07956(7) 0.83381(13) 0.0381(9) Uani 1 1 d . A . C19 C -0.0092(4) 0.11782(10) 0.88957(19) 0.0478(13) Uani 1 1 d . . . C29 C 0.0981(4) 0.11477(10) 0.90444(18) 0.0558(14) Uani 1 1 d . A . C39 C 0.1484(4) 0.12810(11) 0.9554(2) 0.0670(16) Uani 1 1 d . . . H39 H 0.2207 0.1262 0.9659 0.080 Uiso 1 1 calc R . . C49 C 0.0944(5) 0.14377(11) 0.9902(2) 0.0761(18) Uani 1 1 d . . . H49 H 0.1285 0.1520 1.0256 0.091 Uiso 1 1 calc R . . C59 C -0.0108(5) 0.14749(11) 0.9732(2) 0.0694(16) Uani 1 1 d . . . H59 H -0.0474 0.1590 0.9963 0.083 Uiso 1 1 calc R . . C69 C -0.0625(4) 0.13495(9) 0.92397(19) 0.0535(14) Uani 1 1 d . . . H69 H -0.1342 0.1378 0.9130 0.064 Uiso 1 1 calc R . . C79 C 0.1568(4) 0.09861(10) 0.86774(18) 0.0517(14) Uani 1 1 d D . . C89 C 0.2677(4) 0.10691(19) 0.8637(3) 0.054(3) Uiso 0.736(9) 1 d PD A 1 H89A H 0.2832 0.1045 0.8225 0.065 Uiso 0.736(9) 1 calc PR A 1 H89B H 0.2793 0.1261 0.8755 0.065 Uiso 0.736(9) 1 calc PR A 1 C99 C 0.3349(5) 0.08846(15) 0.9068(3) 0.072(3) Uani 0.736(9) 1 d PD A 1 H99A H 0.4075 0.0928 0.9061 0.108 Uiso 0.736(9) 1 calc PR A 1 H99B H 0.3220 0.0696 0.8947 0.108 Uiso 0.736(9) 1 calc PR A 1 H99C H 0.3185 0.0910 0.9473 0.108 Uiso 0.736(9) 1 calc PR A 1 C817 C 0.2745(5) 0.0976(3) 0.8794(8) 0.022(5) Uiso 0.264(9) 1 d PD A 2 H8ZA H 0.3001 0.0943 0.9222 0.027 Uiso 0.264(9) 1 calc PR A 2 H8ZB H 0.3018 0.0835 0.8550 0.027 Uiso 0.264(9) 1 calc PR A 2 C917 C 0.3032(16) 0.1257(3) 0.8604(8) 0.069(7) Uiso 0.264(9) 1 d PD A 2 H9ZA H 0.3782 0.1277 0.8671 0.104 Uiso 0.264(9) 1 calc PR A 2 H9ZB H 0.2723 0.1393 0.8839 0.104 Uiso 0.264(9) 1 calc PR A 2 H9ZC H 0.2775 0.1283 0.8178 0.104 Uiso 0.264(9) 1 calc PR A 2 O110 O -0.1760(2) 0.05850(5) 0.83155(10) 0.0385(8) Uani 1 1 d . . . O210 O 0.0698(2) 0.04852(6) 0.95848(10) 0.0525(9) Uani 1 1 d . . . H210 H 0.1081 0.0429 0.9345 0.079 Uiso 1 1 calc R . . N110 N -0.0209(3) 0.05847(7) 0.92667(13) 0.0408(10) Uani 1 1 d . . . C110 C -0.2300(4) 0.07067(9) 0.87022(17) 0.0388(12) Uani 1 1 d . . . C210 C -0.1906(4) 0.07376(9) 0.93172(17) 0.0434(12) Uani 1 1 d . . . C310 C -0.2547(4) 0.08685(9) 0.96760(18) 0.0483(13) Uani 1 1 d . . . H310 H -0.2295 0.0898 1.0087 0.058 Uiso 1 1 calc R . . C410 C -0.3520(4) 0.09546(9) 0.9456(2) 0.0512(13) Uani 1 1 d . . . H410 H -0.3932 0.1041 0.9713 0.061 Uiso 1 1 calc R . . C510 C -0.3901(4) 0.09160(9) 0.8859(2) 0.0498(13) Uani 1 1 d . . . H510 H -0.4579 0.0973 0.8705 0.060 Uiso 1 1 calc R . . C610 C -0.3290(4) 0.07945(9) 0.84878(18) 0.0430(12) Uani 1 1 d . . . H610 H -0.3551 0.0770 0.8077 0.052 Uiso 1 1 calc R . . C710 C -0.0905(4) 0.06363(9) 0.95991(16) 0.0396(12) Uani 1 1 d . . . C810 C -0.0680(4) 0.05901(9) 1.02697(16) 0.0497(13) Uani 1 1 d . . . H81C H -0.0292 0.0419 1.0349 0.060 Uiso 1 1 calc R . . H81D H -0.1336 0.0572 1.0432 0.060 Uiso 1 1 calc R . . C910 C -0.0051(4) 0.08242(10) 1.05895(17) 0.0623(15) Uani 1 1 d . . . H91D H 0.0107 0.0784 1.1018 0.093 Uiso 1 1 calc R . . H91E H -0.0452 0.0992 1.0533 0.093 Uiso 1 1 calc R . . H91F H 0.0591 0.0846 1.0422 0.093 Uiso 1 1 calc R . . O111 O -0.0999(2) 0.00743(6) 0.64693(10) 0.0408(8) Uani 1 1 d . . . O211 O 0.00165(19) 0.03216(5) 0.80918(9) 0.0354(7) Uani 1 1 d . . . N111 N -0.0653(2) 0.02021(7) 0.76334(12) 0.0312(9) Uani 1 1 d . . . C111 C -0.1566(3) -0.01249(9) 0.66444(17) 0.0390(11) Uani 1 1 d . . . C211 C -0.1617(3) -0.01839(9) 0.72502(16) 0.0356(11) Uani 1 1 d . . . C311 C -0.2254(3) -0.03937(9) 0.73876(17) 0.0389(11) Uani 1 1 d . . . H311 H -0.2293 -0.0433 0.7795 0.047 Uiso 1 1 calc R . . C411 C -0.2822(3) -0.05431(9) 0.69502(19) 0.0492(13) Uani 1 1 d . . . H411 H -0.3277 -0.0679 0.7051 0.059 Uiso 1 1 calc R . . C511 C -0.2726(4) -0.04936(10) 0.6357(2) 0.0530(13) Uani 1 1 d . . . H511 H -0.3083 -0.0605 0.6052 0.064 Uiso 1 1 calc R . . C611 C -0.2124(3) -0.02872(10) 0.62050(18) 0.0496(13) Uani 1 1 d . . . H611 H -0.2083 -0.0253 0.5795 0.060 Uiso 1 1 calc R . . C711 C -0.0981(3) -0.00395(9) 0.77357(16) 0.0312(10) Uani 1 1 d . . . C811 C -0.0705(3) -0.01681(8) 0.83433(15) 0.0364(11) Uani 1 1 d . . . H8FA H 0.0015 -0.0122 0.8505 0.044 Uiso 1 1 calc R . . H8FB H -0.0751 -0.0367 0.8301 0.044 Uiso 1 1 calc R . . C911 C -0.1416(3) -0.00745(9) 0.87871(16) 0.0468(12) Uani 1 1 d . . . H9FA H -0.1228 -0.0168 0.9169 0.070 Uiso 1 1 calc R . . H9FB H -0.2131 -0.0116 0.8625 0.070 Uiso 1 1 calc R . . H9FC H -0.1341 0.0121 0.8850 0.070 Uiso 1 1 calc R . . O112 O -0.1205(2) 0.06080(6) 0.61290(10) 0.0401(8) Uani 1 1 d . . . O212 O -0.3005(2) 0.03762(6) 0.73764(10) 0.0473(8) Uani 1 1 d . . . H212 H -0.2614 0.0441 0.7669 0.071 Uiso 1 1 calc R . . N112 N -0.2598(3) 0.04301(7) 0.68445(13) 0.0382(9) Uani 1 1 d . . . C112 C -0.1997(3) 0.05715(8) 0.56895(16) 0.0344(11) Uani 1 1 d . . . C212 C -0.2980(3) 0.04743(8) 0.57854(15) 0.0329(11) Uani 1 1 d . . . C312 C -0.3720(3) 0.04424(8) 0.52779(17) 0.0379(11) Uani 1 1 d . . . H312 H -0.4374 0.0372 0.5328 0.046 Uiso 1 1 calc R . . C412 C -0.3542(3) 0.05081(9) 0.47119(17) 0.0421(12) Uani 1 1 d . . . H412 H -0.4062 0.0480 0.4379 0.050 Uiso 1 1 calc R . . C512 C -0.2601(4) 0.06154(9) 0.46311(16) 0.0439(12) Uani 1 1 d . . . H512 H -0.2483 0.0671 0.4245 0.053 Uiso 1 1 calc R . . C612 C -0.1837(3) 0.06410(8) 0.51128(15) 0.0398(12) Uani 1 1 d . . . H612 H -0.1184 0.0708 0.5051 0.048 Uiso 1 1 calc R . . C712 C -0.3295(3) 0.04205(9) 0.63764(17) 0.0372(11) Uani 1 1 d . . . C812 C -0.4398(3) 0.03539(9) 0.64257(17) 0.0430(12) Uani 1 1 d . . . H8EA H -0.4856 0.0452 0.6111 0.052 Uiso 1 1 calc R . . H8EB H -0.4557 0.0415 0.6819 0.052 Uiso 1 1 calc R . . C912 C -0.4607(3) 0.00537(10) 0.63605(18) 0.0564(14) Uani 1 1 d . . . H9EA H -0.5328 0.0018 0.6398 0.085 Uiso 1 1 calc R . . H9EB H -0.4159 -0.0044 0.6674 0.085 Uiso 1 1 calc R . . H9EC H -0.4468 -0.0007 0.5967 0.085 Uiso 1 1 calc R . . O113 O 0.1757(2) 0.11687(6) 0.71601(10) 0.0379(7) Uani 1 1 d . . . O213 O -0.0703(2) 0.07425(6) 0.73130(10) 0.0368(7) Uani 1 1 d . . . N113 N -0.0092(3) 0.09363(8) 0.70833(12) 0.0370(9) Uani 1 1 d . . . C113 C 0.1241(3) 0.13762(10) 0.68879(16) 0.0380(11) Uani 1 1 d . . . C213 C 0.0161(4) 0.13966(9) 0.68239(17) 0.0423(12) Uani 1 1 d . . . C313 C -0.0313(4) 0.16329(10) 0.65751(18) 0.0511(13) Uani 1 1 d . . . H313 H -0.1038 0.1651 0.6551 0.061 Uiso 1 1 calc R . . C413 C 0.0238(4) 0.18368(10) 0.63671(18) 0.0549(14) Uani 1 1 d . . . H413 H -0.0098 0.1993 0.6190 0.066 Uiso 1 1 calc R . . C513 C 0.1295(4) 0.18114(10) 0.64194(17) 0.0508(13) Uani 1 1 d . . . H513 H 0.1686 0.1952 0.6275 0.061 Uiso 1 1 calc R . . C613 C 0.1791(3) 0.15863(9) 0.66775(17) 0.0420(12) Uani 1 1 d . . . H613 H 0.2519 0.1575 0.6712 0.050 Uiso 1 1 calc R . . C713 C -0.0480(3) 0.11779(10) 0.70170(16) 0.0405(12) Uani 1 1 d . . . C813 C -0.1575(3) 0.12432(10) 0.71111(18) 0.0524(13) Uani 1 1 d . . . H8AA H -0.1775 0.1128 0.7433 0.063 Uiso 1 1 calc R . . H8AB H -0.1620 0.1434 0.7233 0.063 Uiso 1 1 calc R . . C913 C -0.2300(3) 0.11935(10) 0.65338(19) 0.0663(15) Uani 1 1 d . . . H9AA H -0.2966 0.1279 0.6559 0.099 Uiso 1 1 calc R . . H9AB H -0.2396 0.0999 0.6472 0.099 Uiso 1 1 calc R . . H9AC H -0.2005 0.1271 0.6198 0.099 Uiso 1 1 calc R . . O114 O 0.27041(19) 0.07028(6) 0.69248(10) 0.0375(7) Uani 1 1 d . . . O214 O 0.0330(2) 0.08568(7) 0.56400(10) 0.0645(10) Uani 1 1 d . . . H214 H -0.0099 0.0778 0.5822 0.097 Uiso 1 1 calc R . . N114 N 0.1268(3) 0.08772(8) 0.60146(13) 0.0454(10) Uani 1 1 d . B . C114 C 0.3349(3) 0.08575(8) 0.66587(16) 0.0343(11) Uani 1 1 d . . . C214 C 0.3065(3) 0.09645(9) 0.60737(16) 0.0401(12) Uani 1 1 d . B . C314 C 0.3830(3) 0.10983(9) 0.58191(16) 0.0460(13) Uani 1 1 d . . . H314 H 0.3668 0.1167 0.5424 0.055 Uiso 1 1 calc R . . C414 C 0.4812(4) 0.11349(10) 0.61191(18) 0.0576(15) Uani 1 1 d . . . H414 H 0.5315 0.1226 0.5931 0.069 Uiso 1 1 calc R . . C514 C 0.5053(3) 0.10391(9) 0.66903(18) 0.0500(13) Uani 1 1 d . . . H514 H 0.5721 0.1068 0.6905 0.060 Uiso 1 1 calc R . . C614 C 0.4326(3) 0.09010(9) 0.69553(16) 0.0384(11) Uani 1 1 d . . . H614 H 0.4505 0.0835 0.7351 0.046 Uiso 1 1 calc R . . C714 C 0.2032(4) 0.09331(10) 0.57324(17) 0.0504(14) Uani 1 1 d D . . C814 C 0.1899(6) 0.09456(18) 0.5041(2) 0.046(2) Uani 0.738(10) 1 d PD B 1 H81E H 0.2562 0.0911 0.4895 0.055 Uiso 0.738(10) 1 calc PR B 1 H81F H 0.1391 0.0810 0.4863 0.055 Uiso 0.738(10) 1 calc PR B 1 C914 C 0.1524(5) 0.12287(14) 0.4883(3) 0.056(3) Uani 0.738(10) 1 d PD B 1 H91G H 0.1422 0.1251 0.4447 0.084 Uiso 0.738(10) 1 calc PR B 1 H91H H 0.2036 0.1360 0.5065 0.084 Uiso 0.738(10) 1 calc PR B 1 H91I H 0.0871 0.1259 0.5034 0.084 Uiso 0.738(10) 1 calc PR B 1 C818 C 0.1733(17) 0.1077(3) 0.5123(4) 0.033(7) Uiso 0.262(10) 1 d PD B 2 H8XA H 0.1003 0.1133 0.5055 0.039 Uiso 0.262(10) 1 calc PR B 2 H8XB H 0.2184 0.1233 0.5072 0.039 Uiso 0.262(10) 1 calc PR B 2 C918 C 0.1939(16) 0.0838(4) 0.4741(10) 0.068(8) Uiso 0.262(10) 1 d PD B 2 H9XA H 0.1795 0.0888 0.4318 0.101 Uiso 0.262(10) 1 calc PR B 2 H9XB H 0.1495 0.0687 0.4819 0.101 Uiso 0.262(10) 1 calc PR B 2 H9XC H 0.2662 0.0784 0.4839 0.101 Uiso 0.262(10) 1 calc PR B 2 O115 O 0.1636(2) -0.01017(6) 0.80350(10) 0.0387(7) Uani 1 1 d . . . O215 O 0.07929(19) 0.04489(6) 0.68362(9) 0.0338(7) Uani 1 1 d . . . N115 N 0.1413(2) 0.02472(7) 0.71239(12) 0.0335(9) Uani 1 1 d . . . C115 C 0.2215(3) -0.02420(10) 0.77017(16) 0.0391(12) Uani 1 1 d . . . C215 C 0.2262(3) -0.01738(9) 0.70977(16) 0.0367(11) Uani 1 1 d . . . C315 C 0.2885(3) -0.03358(10) 0.67880(18) 0.0450(13) Uani 1 1 d . . . H315 H 0.2928 -0.0294 0.6382 0.054 Uiso 1 1 calc R . . C415 C 0.3434(4) -0.05510(10) 0.70468(19) 0.0487(13) Uani 1 1 d . . . H415 H 0.3852 -0.0656 0.6826 0.058 Uiso 1 1 calc R . . C515 C 0.3366(3) -0.06113(9) 0.76316(19) 0.0480(13) Uani 1 1 d . . . H515 H 0.3736 -0.0761 0.7815 0.058 Uiso 1 1 calc R . . C615 C 0.2775(4) -0.04596(10) 0.79554(18) 0.0442(12) Uani 1 1 d . . . H615 H 0.2750 -0.0505 0.8362 0.053 Uiso 1 1 calc R . . C715 C 0.1673(3) 0.00472(10) 0.67993(16) 0.0365(12) Uani 1 1 d . . . C815 C 0.1372(3) 0.00491(10) 0.61215(16) 0.0485(13) Uani 1 1 d . . . H8DE H 0.1313 -0.0139 0.5973 0.058 Uiso 1 1 calc R . . H8DB H 0.0690 0.0136 0.6020 0.058 Uiso 1 1 calc R . . C915 C 0.2152(4) 0.01993(10) 0.58108(17) 0.0635(15) Uani 1 1 d . . . H9DA H 0.1892 0.0215 0.5383 0.095 Uiso 1 1 calc R . . H9DB H 0.2803 0.0099 0.5863 0.095 Uiso 1 1 calc R . . H9DC H 0.2265 0.0380 0.5986 0.095 Uiso 1 1 calc R . . O116 O 0.2016(2) 0.02949(6) 0.88787(10) 0.0371(7) Uani 1 1 d . . . O216 O 0.3885(2) 0.03617(6) 0.76044(10) 0.0438(8) Uani 1 1 d . . . H216 H 0.3498 0.0470 0.7393 0.066 Uiso 1 1 calc R . . N116 N 0.3395(2) 0.02694(7) 0.80709(12) 0.0360(9) Uani 1 1 d . . . C116 C 0.2664(4) 0.01154(9) 0.91791(16) 0.0399(12) Uani 1 1 d . . . C216 C 0.3618(3) 0.00400(9) 0.90122(16) 0.0388(12) Uani 1 1 d . . . C316 C 0.4209(3) -0.01506(9) 0.93620(16) 0.0471(13) Uani 1 1 d . . . H316 H 0.4848 -0.0203 0.9248 0.057 Uiso 1 1 calc R . . C416 C 0.3915(4) -0.02655(9) 0.98603(17) 0.0496(13) Uani 1 1 d . . . H416 H 0.4332 -0.0398 1.0081 0.060 Uiso 1 1 calc R . . C516 C 0.3005(4) -0.01847(9) 1.00354(17) 0.0474(13) Uani 1 1 d . . . H516 H 0.2802 -0.0256 1.0390 0.057 Uiso 1 1 calc R . . C616 C 0.2380(3) 0.00010(9) 0.96964(16) 0.0441(13) Uani 1 1 d . . . H616 H 0.1744 0.0052 0.9818 0.053 Uiso 1 1 calc R . . C716 C 0.4044(3) 0.01578(8) 0.84924(15) 0.0361(11) Uani 1 1 d . . . C816 C 0.5159(3) 0.01380(9) 0.84411(16) 0.0427(12) Uani 1 1 d . . . H8EC H 0.5555 0.0112 0.8845 0.051 Uiso 1 1 calc R . . H8ED H 0.5388 0.0309 0.8277 0.051 Uiso 1 1 calc R . . C916 C 0.5390(3) -0.00952(9) 0.80385(17) 0.0535(13) Uani 1 1 d . . . H9CA H 0.6115 -0.0089 0.7982 0.080 Uiso 1 1 calc R . . H9CB H 0.4954 -0.0079 0.7649 0.080 Uiso 1 1 calc R . . H9CC H 0.5249 -0.0267 0.8225 0.080 Uiso 1 1 calc R . . N1R N 1.0995(10) 0.2499(3) 0.6424(6) 0.097(6) Uani 0.434(8) 1 d P C 1 C1R C 1.0931(10) 0.2709(4) 0.6577(6) 0.061(5) Uani 0.434(8) 1 d P C 1 C2R C 1.0866(11) 0.2987(5) 0.6780(5) 0.071(5) Uani 0.434(8) 1 d P C 1 H2RA H 1.0711 0.2989 0.7191 0.107 Uiso 0.434(8) 1 calc PR C 1 H2RB H 1.0319 0.3082 0.6519 0.107 Uiso 0.434(8) 1 calc PR C 1 H2RC H 1.1524 0.3079 0.6766 0.107 Uiso 0.434(8) 1 calc PR C 1 N2R N 1.0633(14) 0.3720(3) 0.7157(12) 0.290(15) Uani 0.566(8) 1 d P C 2 C3R C 1.0876(10) 0.3521(6) 0.6977(6) 0.128(8) Uani 0.566(8) 1 d P C 2 C4R C 1.1237(12) 0.3217(5) 0.6894(5) 0.136(7) Uani 0.566(8) 1 d P C 2 H4RA H 1.1175 0.3174 0.6466 0.164 Uiso 0.566(8) 1 calc PR C 2 H4RB H 1.0801 0.3093 0.7086 0.204 Uiso 0.566(8) 1 calc PR C 2 H4RC H 1.1955 0.3196 0.7078 0.204 Uiso 0.566(8) 1 calc PR C 2 N3R N 0.9606(10) 0.3978(3) 0.5625(6) 0.118(5) Uani 0.50 1 d P . . C5R C 0.9090(16) 0.4166(4) 0.5714(10) 0.139(8) Uani 0.50 1 d P . . C6R C 0.8238(12) 0.4370(3) 0.5608(5) 0.111(5) Uani 0.50 1 d P . . H6RA H 0.8167 0.4461 0.5986 0.167 Uiso 0.50 1 calc PR . . H6RB H 0.7592 0.4279 0.5454 0.167 Uiso 0.50 1 calc PR . . H6RC H 0.8400 0.4504 0.5316 0.167 Uiso 0.50 1 calc PR . . 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 0.0331(4) 0.0345(5) 0.0313(3) -0.0017(3) 0.0060(3) 0.0090(3) Mn2 0.0364(4) 0.0352(5) 0.0307(3) 0.0021(3) 0.0058(3) 0.0098(3) Mn3 0.0445(5) 0.0514(5) 0.0302(3) -0.0041(3) 0.0043(3) 0.0119(4) Mn4 0.0440(5) 0.0355(5) 0.0324(3) -0.0017(3) 0.0019(3) 0.0088(4) Mn5 0.0430(5) 0.0432(5) 0.0286(3) -0.0002(3) 0.0081(3) -0.0153(4) Mn6 0.0371(4) 0.0462(5) 0.0256(3) 0.0036(3) 0.0041(3) -0.0130(4) Mn7 0.0379(4) 0.0457(5) 0.0272(3) 0.0058(3) 0.0058(3) -0.0124(4) Mn8 0.0408(4) 0.0461(5) 0.0233(3) 0.0023(3) 0.0062(3) -0.0131(4) O11 0.0339(19) 0.041(2) 0.0348(15) 0.0023(13) 0.0048(12) 0.0104(16) O21 0.0378(19) 0.038(2) 0.0344(15) -0.0040(13) -0.0002(12) 0.0084(16) N11 0.027(2) 0.038(3) 0.0318(18) -0.0042(16) 0.0017(15) 0.009(2) C11 0.032(3) 0.052(4) 0.022(2) 0.005(2) 0.0078(18) 0.004(3) C21 0.033(3) 0.044(3) 0.026(2) 0.001(2) 0.0082(18) 0.015(3) C31 0.044(3) 0.051(4) 0.039(2) 0.004(2) 0.015(2) 0.009(3) C41 0.036(3) 0.049(4) 0.041(2) 0.013(2) 0.015(2) 0.012(3) C51 0.031(3) 0.065(4) 0.040(3) 0.010(2) 0.0123(19) -0.007(3) C61 0.039(3) 0.042(3) 0.036(2) 0.008(2) 0.0152(19) 0.002(3) C71 0.034(3) 0.037(3) 0.032(2) 0.004(2) 0.0023(19) 0.008(2) C81 0.050(3) 0.042(3) 0.051(3) -0.010(3) 0.007(2) 0.017(3) C91 0.064(4) 0.048(4) 0.071(3) -0.011(3) 0.006(3) 0.011(3) O12 0.0321(18) 0.0309(19) 0.0368(15) -0.0023(13) 0.0036(12) 0.0062(15) O22 0.047(2) 0.029(2) 0.0403(16) 0.0023(14) 0.0002(13) -0.0043(16) N12 0.036(2) 0.026(2) 0.0363(19) -0.0007(17) 0.0095(16) 0.0076(19) C12 0.034(3) 0.028(3) 0.030(2) -0.004(2) 0.0110(19) 0.009(2) C22 0.038(3) 0.028(3) 0.029(2) -0.004(2) 0.0136(19) 0.006(2) C32 0.032(3) 0.040(3) 0.033(2) -0.004(2) 0.0058(18) 0.007(2) C42 0.033(3) 0.037(3) 0.044(3) -0.011(2) 0.011(2) -0.002(3) C52 0.048(3) 0.031(3) 0.049(3) 0.002(2) 0.016(2) 0.007(3) C62 0.032(3) 0.037(3) 0.045(3) -0.004(2) 0.003(2) 0.005(3) C72 0.023(3) 0.042(3) 0.030(2) -0.003(2) 0.0101(17) 0.008(2) C82 0.042(3) 0.044(3) 0.036(2) -0.001(2) 0.0028(19) -0.009(2) C92 0.108(5) 0.064(4) 0.042(3) 0.002(3) 0.030(3) 0.017(3) O13 0.0361(19) 0.040(2) 0.0348(15) 0.0017(14) 0.0070(12) 0.0059(15) O23 0.0299(18) 0.0304(19) 0.0338(14) -0.0005(12) 0.0037(11) 0.0099(15) N13 0.028(2) 0.025(2) 0.0374(19) -0.0017(16) 0.0029(15) -0.0038(18) C13 0.026(3) 0.038(3) 0.042(3) 0.007(2) 0.0082(19) 0.004(2) C23 0.032(3) 0.026(3) 0.044(2) -0.003(2) 0.0161(19) 0.001(2) C33 0.036(3) 0.047(3) 0.042(2) 0.001(2) 0.012(2) 0.001(3) C43 0.034(3) 0.052(4) 0.062(3) -0.011(3) 0.025(2) 0.002(3) C53 0.036(3) 0.041(3) 0.066(3) 0.009(3) 0.013(2) 0.010(3) C63 0.031(3) 0.046(3) 0.049(3) 0.003(2) 0.011(2) 0.004(3) C73 0.026(3) 0.036(3) 0.036(2) -0.002(2) 0.0056(18) -0.003(2) C83 0.044(3) 0.058(4) 0.032(2) -0.002(2) 0.0116(19) 0.015(3) C93 0.086(4) 0.049(3) 0.032(2) -0.002(2) 0.022(2) -0.007(3) O14 0.041(2) 0.041(2) 0.0323(15) 0.0058(13) 0.0052(12) 0.0146(16) O24 0.0326(19) 0.038(2) 0.0488(17) 0.0000(14) 0.0009(13) 0.0122(15) N14 0.029(2) 0.042(3) 0.0275(18) 0.0034(17) 0.0036(15) 0.004(2) C14 0.043(3) 0.039(3) 0.036(2) 0.008(2) 0.013(2) 0.009(3) C24 0.035(3) 0.047(3) 0.034(2) 0.010(2) 0.0044(19) 0.008(3) C34 0.050(3) 0.045(3) 0.046(3) 0.004(2) 0.008(2) 0.013(3) C44 0.052(4) 0.070(4) 0.057(3) 0.001(3) -0.013(2) 0.022(3) C54 0.072(4) 0.059(4) 0.048(3) -0.007(3) -0.013(2) 0.017(3) C64 0.057(4) 0.051(4) 0.040(3) -0.003(2) -0.002(2) 0.012(3) C74 0.036(3) 0.029(3) 0.043(2) 0.006(2) 0.017(2) 0.003(2) C84 0.039(3) 0.035(3) 0.059(3) 0.008(2) 0.002(2) 0.009(2) C94 0.054(3) 0.043(3) 0.063(3) -0.013(3) 0.002(2) 0.011(3) O15 0.053(2) 0.069(3) 0.0454(18) -0.0068(17) 0.0137(15) 0.0167(19) O25 0.0380(19) 0.041(2) 0.0297(14) -0.0006(13) 0.0066(12) 0.0080(15) N15 0.040(3) 0.080(3) 0.028(2) 0.006(2) 0.0111(16) 0.023(2) C15 0.039(3) 0.081(5) 0.048(3) -0.014(3) 0.007(2) 0.004(3) C25 0.046(3) 0.070(4) 0.041(3) -0.006(3) 0.016(2) 0.002(3) C35 0.066(4) 0.085(5) 0.066(3) 0.006(3) 0.026(3) 0.007(3) C45 0.071(4) 0.100(5) 0.057(3) -0.001(4) 0.032(3) 0.000(4) C55 0.083(5) 0.109(6) 0.058(4) -0.015(4) 0.027(3) 0.013(4) C65 0.056(4) 0.097(5) 0.055(3) -0.017(3) 0.025(3) 0.008(3) C75 0.041(3) 0.053(4) 0.044(3) -0.003(3) 0.004(2) 0.013(3) C85 0.067(4) 0.051(4) 0.049(3) 0.008(3) 0.026(2) 0.010(3) C95 0.088(5) 0.056(4) 0.085(4) 0.008(3) 0.038(3) 0.008(4) O16 0.055(2) 0.043(2) 0.0349(16) -0.0099(14) 0.0034(13) 0.0122(16) O26 0.059(2) 0.042(2) 0.0386(16) 0.0021(15) 0.0118(13) 0.0153(18) N16 0.048(3) 0.045(3) 0.042(2) 0.0024(19) 0.0091(17) 0.011(2) C16 0.039(3) 0.056(4) 0.033(2) -0.003(2) -0.0031(19) 0.019(3) C26 0.038(3) 0.038(3) 0.041(3) -0.008(2) 0.002(2) 0.001(2) C36 0.048(3) 0.063(4) 0.036(3) -0.012(2) 0.000(2) 0.003(3) C46 0.043(3) 0.070(4) 0.044(3) -0.018(3) 0.003(2) 0.013(3) C56 0.037(3) 0.068(4) 0.047(3) -0.019(3) -0.009(2) 0.018(3) C66 0.046(3) 0.059(4) 0.042(3) -0.007(2) -0.009(2) 0.020(3) C76 0.049(3) 0.049(4) 0.030(2) -0.005(2) 0.014(2) -0.001(3) C86 0.044(3) 0.054(4) 0.034(2) -0.002(2) 0.005(2) 0.007(3) C96 0.064(4) 0.074(4) 0.041(3) -0.002(2) 0.016(2) -0.005(3) O17 0.048(2) 0.039(2) 0.0321(15) 0.0023(13) 0.0053(13) 0.0118(17) O27 0.043(2) 0.035(2) 0.0295(14) -0.0019(13) 0.0007(12) 0.0070(15) N17 0.047(3) 0.035(3) 0.0260(18) 0.0009(16) 0.0076(16) 0.012(2) C17 0.039(3) 0.037(3) 0.047(3) -0.007(2) 0.008(2) 0.004(3) C27 0.041(3) 0.040(3) 0.037(2) -0.003(2) 0.010(2) 0.006(3) C37 0.050(4) 0.050(4) 0.049(3) -0.007(3) 0.006(2) 0.005(3) C47 0.050(4) 0.057(4) 0.060(3) -0.014(3) 0.010(3) -0.003(3) C57 0.051(4) 0.055(4) 0.068(3) 0.002(3) 0.029(3) 0.006(3) C67 0.055(4) 0.052(4) 0.045(3) 0.004(3) 0.016(2) 0.016(3) C77 0.039(3) 0.040(3) 0.036(2) -0.012(2) 0.002(2) 0.008(3) C87 0.052(3) 0.047(3) 0.041(3) -0.002(2) -0.004(2) -0.003(3) C97 0.078(4) 0.070(4) 0.056(3) -0.007(3) 0.000(3) 0.019(3) O18 0.047(2) 0.031(2) 0.0384(16) 0.0016(14) 0.0008(13) 0.0067(16) O28 0.085(3) 0.046(2) 0.0423(18) -0.0161(15) 0.0093(15) 0.0025(19) N18 0.047(3) 0.034(3) 0.046(2) -0.0039(19) 0.0030(17) 0.010(2) C18 0.047(3) 0.037(3) 0.041(3) 0.008(2) 0.004(2) 0.012(3) C28 0.048(3) 0.032(3) 0.059(3) 0.008(3) 0.004(2) 0.006(3) C38 0.062(4) 0.043(4) 0.073(4) 0.007(3) 0.000(3) -0.007(3) C48 0.074(4) 0.052(4) 0.063(3) 0.018(3) -0.003(3) -0.007(3) C58 0.071(4) 0.066(4) 0.044(3) 0.012(3) 0.001(2) -0.007(3) C68 0.058(4) 0.049(4) 0.046(3) 0.011(2) 0.003(2) -0.002(3) C78 0.046(3) 0.031(3) 0.058(3) -0.004(3) 0.007(2) 0.005(3) C88 0.084(5) 0.038(4) 0.072(3) -0.008(3) 0.020(3) 0.000(3) C98 0.097(5) 0.054(4) 0.091(4) -0.024(3) 0.009(3) -0.017(4) O19 0.046(2) 0.046(2) 0.0414(16) -0.0056(15) 0.0086(13) -0.0192(17) O29 0.0371(18) 0.049(2) 0.0253(14) -0.0037(13) 0.0093(12) -0.0084(16) N19 0.041(2) 0.045(3) 0.0290(18) -0.0050(17) 0.0067(16) -0.013(2) C19 0.057(4) 0.041(3) 0.048(3) -0.002(2) 0.020(2) -0.021(3) C29 0.061(4) 0.063(4) 0.046(3) -0.024(3) 0.016(2) -0.029(3) C39 0.065(4) 0.076(4) 0.062(3) -0.025(3) 0.016(3) -0.026(3) C49 0.094(5) 0.079(5) 0.056(3) -0.033(3) 0.015(3) -0.028(4) C59 0.085(5) 0.056(4) 0.073(4) -0.026(3) 0.029(3) -0.025(4) C69 0.055(4) 0.049(4) 0.059(3) -0.016(3) 0.020(3) -0.026(3) C79 0.047(3) 0.067(4) 0.043(3) -0.015(3) 0.015(2) -0.020(3) C99 0.029(5) 0.100(7) 0.085(5) -0.021(4) 0.006(4) -0.022(5) O110 0.043(2) 0.045(2) 0.0289(14) -0.0014(13) 0.0116(13) -0.0119(16) O210 0.050(2) 0.080(3) 0.0291(15) -0.0006(15) 0.0092(13) -0.0003(19) N110 0.042(3) 0.052(3) 0.0278(18) 0.0003(17) 0.0044(17) -0.010(2) C110 0.051(3) 0.029(3) 0.040(3) 0.003(2) 0.016(2) -0.019(3) C210 0.052(3) 0.046(3) 0.035(2) 0.001(2) 0.016(2) -0.011(3) C310 0.066(4) 0.041(3) 0.040(3) -0.001(2) 0.014(2) -0.007(3) C410 0.068(4) 0.033(3) 0.059(3) 0.000(2) 0.031(3) 0.000(3) C510 0.048(3) 0.040(3) 0.062(3) 0.012(2) 0.010(2) 0.003(3) C610 0.048(3) 0.042(3) 0.040(3) 0.004(2) 0.010(2) -0.011(3) C710 0.055(3) 0.038(3) 0.028(2) 0.000(2) 0.011(2) -0.012(3) C810 0.062(4) 0.054(4) 0.036(2) -0.001(2) 0.019(2) -0.005(3) C910 0.065(4) 0.084(4) 0.038(3) -0.008(3) 0.009(2) -0.012(3) O111 0.047(2) 0.047(2) 0.0287(14) -0.0036(14) 0.0080(12) -0.0177(17) O211 0.0372(18) 0.043(2) 0.0250(14) 0.0024(13) 0.0009(11) -0.0168(15) N111 0.033(2) 0.033(3) 0.0275(18) -0.0031(16) 0.0032(14) -0.0155(19) C111 0.034(3) 0.048(3) 0.036(2) -0.007(2) 0.0058(19) -0.007(3) C211 0.039(3) 0.037(3) 0.031(2) -0.001(2) 0.0087(19) -0.006(2) C311 0.044(3) 0.033(3) 0.040(2) 0.000(2) 0.007(2) -0.006(3) C411 0.047(3) 0.046(4) 0.057(3) -0.007(3) 0.014(2) -0.020(3) C511 0.053(4) 0.046(4) 0.057(3) -0.018(3) -0.002(2) -0.017(3) C611 0.050(3) 0.058(4) 0.040(3) -0.005(2) 0.002(2) -0.019(3) C711 0.031(3) 0.034(3) 0.031(2) -0.003(2) 0.0114(18) -0.004(2) C811 0.039(3) 0.037(3) 0.033(2) 0.005(2) 0.0075(18) -0.012(2) C911 0.053(3) 0.054(3) 0.036(2) 0.003(2) 0.012(2) -0.009(3) O112 0.0368(19) 0.053(2) 0.0283(14) 0.0069(13) -0.0023(12) -0.0189(16) O212 0.045(2) 0.067(2) 0.0311(15) -0.0004(14) 0.0086(13) -0.0232(17) N112 0.043(2) 0.046(3) 0.0272(19) 0.0001(16) 0.0100(16) -0.013(2) C112 0.042(3) 0.031(3) 0.030(2) 0.0015(19) 0.0019(19) -0.006(2) C212 0.043(3) 0.026(3) 0.028(2) -0.0027(19) 0.0011(19) -0.008(2) C312 0.036(3) 0.034(3) 0.044(3) -0.001(2) 0.005(2) -0.004(2) C412 0.045(3) 0.043(3) 0.035(2) -0.002(2) -0.005(2) -0.005(3) C512 0.058(4) 0.045(3) 0.028(2) 0.002(2) 0.003(2) -0.008(3) C612 0.043(3) 0.043(3) 0.032(2) 0.002(2) 0.0020(19) -0.013(2) C712 0.040(3) 0.035(3) 0.038(2) -0.003(2) 0.008(2) -0.005(2) C812 0.036(3) 0.054(4) 0.040(2) -0.003(2) 0.0091(19) -0.006(3) C912 0.038(3) 0.069(4) 0.061(3) 0.011(3) 0.001(2) -0.023(3) O113 0.0373(19) 0.037(2) 0.0386(15) 0.0065(14) 0.0015(13) -0.0072(16) O213 0.0387(19) 0.045(2) 0.0278(14) 0.0086(13) 0.0092(12) -0.0166(16) N113 0.038(2) 0.045(3) 0.0278(18) 0.0087(18) 0.0049(15) -0.014(2) C113 0.038(3) 0.045(3) 0.032(2) 0.007(2) 0.011(2) -0.008(3) C213 0.048(3) 0.039(3) 0.040(2) 0.015(2) 0.007(2) -0.005(3) C313 0.037(3) 0.061(4) 0.055(3) 0.013(3) 0.004(2) -0.012(3) C413 0.044(4) 0.058(4) 0.062(3) 0.024(3) 0.004(2) -0.009(3) C513 0.051(4) 0.051(4) 0.052(3) 0.013(3) 0.014(2) -0.017(3) C613 0.038(3) 0.044(3) 0.045(3) 0.001(2) 0.008(2) -0.013(3) C713 0.035(3) 0.048(4) 0.038(2) 0.009(2) 0.0031(19) -0.010(3) C813 0.036(3) 0.061(4) 0.059(3) 0.025(3) 0.001(2) -0.008(3) C913 0.044(3) 0.076(4) 0.080(4) 0.003(3) 0.011(3) -0.016(3) O114 0.0322(18) 0.050(2) 0.0314(14) 0.0076(13) 0.0079(12) -0.0126(16) O214 0.043(2) 0.113(3) 0.0336(16) 0.0238(17) -0.0069(13) -0.032(2) N114 0.035(3) 0.068(3) 0.0308(19) 0.0127(18) -0.0027(16) -0.019(2) C114 0.043(3) 0.027(3) 0.035(2) 0.001(2) 0.013(2) -0.008(2) C214 0.038(3) 0.052(3) 0.030(2) 0.002(2) 0.0047(19) -0.012(2) C314 0.044(3) 0.061(4) 0.032(2) 0.014(2) 0.005(2) -0.016(3) C414 0.049(4) 0.080(4) 0.044(3) 0.016(3) 0.008(2) -0.024(3) C514 0.039(3) 0.063(4) 0.046(3) 0.013(2) 0.000(2) -0.018(3) C614 0.039(3) 0.047(3) 0.029(2) 0.003(2) 0.0028(19) -0.010(3) C714 0.047(3) 0.072(4) 0.031(2) 0.012(2) 0.003(2) -0.014(3) C814 0.049(5) 0.058(6) 0.035(4) -0.009(4) 0.018(3) -0.011(5) C914 0.049(5) 0.076(6) 0.043(4) 0.029(4) 0.010(3) 0.009(4) O115 0.046(2) 0.042(2) 0.0293(14) 0.0012(13) 0.0092(12) -0.0123(16) O215 0.0345(18) 0.042(2) 0.0254(14) 0.0057(13) 0.0065(11) -0.0065(16) N115 0.032(2) 0.041(3) 0.0262(18) 0.0090(18) 0.0016(15) -0.012(2) C115 0.037(3) 0.052(4) 0.028(2) -0.002(2) 0.0051(19) -0.023(3) C215 0.037(3) 0.042(3) 0.030(2) 0.000(2) 0.0043(19) -0.010(2) C315 0.047(3) 0.055(4) 0.034(2) -0.007(2) 0.008(2) -0.019(3) C415 0.050(3) 0.048(4) 0.048(3) -0.005(2) 0.005(2) -0.005(3) C515 0.053(3) 0.042(3) 0.046(3) 0.005(2) -0.002(2) -0.009(3) C615 0.049(3) 0.047(4) 0.036(2) 0.001(2) 0.004(2) -0.015(3) C715 0.033(3) 0.052(3) 0.024(2) -0.004(2) 0.0055(18) -0.017(3) C815 0.044(3) 0.068(4) 0.035(2) 0.000(2) 0.008(2) 0.005(3) C915 0.075(4) 0.080(4) 0.037(3) 0.004(2) 0.012(2) -0.011(3) O116 0.0422(19) 0.046(2) 0.0229(14) 0.0047(13) 0.0051(12) -0.0054(16) O216 0.043(2) 0.059(2) 0.0308(15) 0.0185(14) 0.0102(12) -0.0069(17) N116 0.039(2) 0.047(3) 0.0235(17) 0.0024(17) 0.0099(15) -0.010(2) C116 0.055(3) 0.044(3) 0.020(2) 0.001(2) 0.005(2) -0.019(3) C216 0.040(3) 0.052(3) 0.025(2) 0.003(2) 0.0042(19) -0.015(3) C316 0.047(3) 0.065(4) 0.030(2) 0.012(2) 0.006(2) -0.007(3) C416 0.058(4) 0.053(4) 0.036(2) 0.012(2) 0.001(2) -0.014(3) C516 0.059(4) 0.053(4) 0.030(2) 0.013(2) 0.004(2) -0.020(3) C616 0.046(3) 0.060(4) 0.028(2) -0.001(2) 0.009(2) -0.019(3) C716 0.047(3) 0.036(3) 0.023(2) 0.0009(19) 0.0017(19) -0.016(2) C816 0.031(3) 0.060(4) 0.036(2) 0.013(2) 0.0020(19) -0.014(2) C916 0.053(3) 0.061(4) 0.049(3) 0.009(3) 0.015(2) -0.005(3) N1R 0.086(10) 0.060(10) 0.131(11) 0.022(9) -0.029(7) -0.020(9) C1R 0.043(8) 0.082(14) 0.052(8) 0.020(9) -0.013(6) -0.016(10) C2R 0.045(10) 0.124(18) 0.043(8) -0.003(9) 0.002(6) -0.001(10) N2R 0.101(15) 0.101(14) 0.63(4) 0.094(18) -0.086(16) -0.033(11) C3R 0.029(8) 0.24(3) 0.111(10) 0.023(14) -0.007(6) -0.009(13) C4R 0.114(14) 0.22(2) 0.073(9) -0.040(12) 0.016(8) -0.018(17) N3R 0.084(11) 0.142(14) 0.131(10) 0.055(10) 0.027(7) -0.051(9) C5R 0.112(19) 0.090(16) 0.234(19) 0.022(16) 0.089(15) -0.040(13) C6R 0.159(15) 0.067(11) 0.105(10) -0.048(8) 0.007(9) -0.056(10) _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 O11 1.853(3) . ? Mn1 O12 1.908(3) . ? Mn1 O23 1.963(3) . ? Mn1 N11 2.025(3) . ? Mn1 O25 2.240(3) . ? Mn1 N12 2.250(3) . ? Mn2 O13 1.857(3) . ? Mn2 O14 1.907(2) . ? Mn2 O25 1.951(3) . ? Mn2 N13 2.023(3) . ? Mn2 N14 2.226(4) . ? Mn2 O27 2.238(3) . ? Mn3 O15 1.860(3) . ? Mn3 O16 1.911(3) . ? Mn3 O27 1.976(3) . ? Mn3 N15 1.979(4) . ? Mn3 O21 2.205(2) . ? Mn3 N16 2.218(3) . ? Mn4 O17 1.857(3) . ? Mn4 O18 1.906(3) . ? Mn4 O21 1.946(3) . ? Mn4 N17 2.013(3) . ? Mn4 N18 2.226(4) . ? Mn4 O23 2.255(3) . ? Mn5 O19 1.854(3) . ? Mn5 O110 1.896(3) . ? Mn5 O211 1.969(3) . ? Mn5 N19 2.006(3) . ? Mn5 O213 2.208(2) . ? Mn5 N110 2.241(3) . ? Mn6 O111 1.857(3) . ? Mn6 O112 1.896(2) . ? Mn6 O213 1.958(3) . ? Mn6 N111 2.030(3) . ? Mn6 N112 2.222(4) . ? Mn6 O215 2.248(3) . ? Mn7 O113 1.851(3) . ? Mn7 O114 1.899(3) . ? Mn7 O215 1.970(3) . ? Mn7 N113 2.019(4) . ? Mn7 N114 2.241(3) . ? Mn7 O29 2.243(2) . ? Mn8 O115 1.854(3) . ? Mn8 O116 1.907(2) . ? Mn8 O29 1.959(3) . ? Mn8 N115 2.030(3) . ? Mn8 N116 2.230(3) . ? Mn8 O211 2.236(3) . ? O11 C11 1.334(5) . ? O21 N11 1.382(4) . ? N11 C71 1.300(5) . ? C11 C61 1.385(5) . ? C11 C21 1.416(6) . ? C21 C31 1.411(5) . ? C21 C71 1.451(6) . ? C31 C41 1.364(5) . ? C31 H31 0.9500 . ? C41 C51 1.394(6) . ? C41 H41 0.9500 . ? C51 C61 1.376(5) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C71 C81 1.508(5) . ? C81 C91 1.518(5) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? O12 C12 1.330(4) . ? O22 N12 1.401(4) . ? O22 H22 0.8400 . ? N12 C72 1.280(5) . ? C12 C62 1.394(5) . ? C12 C22 1.420(5) . ? C22 C32 1.392(5) . ? C22 C72 1.483(5) . ? C32 C42 1.374(5) . ? C32 H32 0.9500 . ? C42 C52 1.377(5) . ? C42 H42 0.9500 . ? C52 C62 1.374(5) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C72 C82 1.503(5) . ? C82 C92 1.504(5) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? O13 C13 1.333(4) . ? O23 N13 1.384(4) . ? N13 C73 1.306(4) . ? C13 C63 1.400(5) . ? C13 C23 1.413(5) . ? C23 C33 1.398(5) . ? C23 C73 1.473(5) . ? C33 C43 1.378(5) . ? C33 H33 0.9500 . ? C43 C53 1.380(5) . ? C43 H43 0.9500 . ? C53 C63 1.371(5) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C73 C83 1.500(5) . ? C83 C93 1.521(5) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? O14 C14 1.341(5) . ? O24 N14 1.407(4) . ? O24 H24A 0.8400 . ? N14 C74 1.289(5) . ? C14 C64 1.394(5) . ? C14 C24 1.409(6) . ? C24 C34 1.400(5) . ? C24 C74 1.486(5) . ? C34 C44 1.372(5) . ? C34 H34 0.9500 . ? C44 C54 1.366(6) . ? C44 H44 0.9500 . ? C54 C64 1.364(6) . ? C54 H54 0.9500 . ? C64 H64 0.9500 . ? C74 C84 1.505(5) . ? C84 C94 1.536(5) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? O15 C15 1.320(6) . ? O25 N15 1.394(4) . ? N15 C75 1.308(5) . ? C15 C25 1.389(6) . ? C15 C65 1.425(6) . ? C25 C35 1.423(6) . ? C25 C75 1.477(6) . ? C35 C45 1.397(6) . ? C35 H35 0.9500 . ? C45 C55 1.387(7) . ? C45 H45 0.9500 . ? C55 C65 1.346(7) . ? C55 H55 0.9500 . ? C65 H65 0.9500 . ? C75 C85 1.501(6) . ? C85 C95 1.519(6) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? O16 C16 1.337(4) . ? O26 N16 1.397(4) . ? O26 H26A 0.8400 . ? N16 C76 1.299(4) . ? C16 C66 1.402(6) . ? C16 C26 1.409(5) . ? C26 C36 1.398(5) . ? C26 C76 1.480(6) . ? C36 C46 1.383(6) . ? C36 H36 0.9500 . ? C46 C56 1.377(6) . ? C46 H46 0.9500 . ? C56 C66 1.381(5) . ? C56 H56 0.9500 . ? C66 H66 0.9500 . ? C76 C86 1.500(5) . ? C86 C96 1.536(5) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? O17 C17 1.329(5) . ? O27 N17 1.394(4) . ? N17 C77 1.301(5) . ? C17 C67 1.403(6) . ? C17 C27 1.411(5) . ? C27 C37 1.388(6) . ? C27 C77 1.464(6) . ? C37 C47 1.364(6) . ? C37 H37 0.9500 . ? C47 C57 1.372(6) . ? C47 H47 0.9500 . ? C57 C67 1.365(6) . ? C57 H57 0.9500 . ? C67 H67 0.9500 . ? C77 C87 1.509(5) . ? C87 C97 1.510(5) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? O18 C18 1.349(5) . ? O28 N18 1.391(4) . ? O28 H28A 0.8400 . ? N18 C78 1.287(5) . ? C18 C68 1.386(5) . ? C18 C28 1.416(6) . ? C28 C38 1.409(6) . ? C28 C78 1.488(6) . ? C38 C48 1.361(6) . ? C38 H38 0.9500 . ? C48 C58 1.378(6) . ? C48 H48 0.9500 . ? C58 C68 1.373(6) . ? C58 H58 0.9500 . ? C68 H68 0.9500 . ? C78 C88 1.482(6) . ? C88 C98 1.523(6) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? O19 C19 1.342(5) . ? O29 N19 1.381(4) . ? N19 C79 1.308(5) . ? C19 C69 1.405(6) . ? C19 C29 1.409(6) . ? C29 C39 1.406(6) . ? C29 C79 1.452(6) . ? C39 C49 1.373(6) . ? C39 H39 0.9500 . ? C49 C59 1.392(7) . ? C49 H49 0.9500 . ? C59 C69 1.365(6) . ? C59 H59 0.9500 . ? C69 H69 0.9500 . ? C79 C89 1.530(6) . ? C79 C817 1.532(7) . ? C89 C99 1.520(8) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C817 C917 1.520(9) . ? C817 H8ZA 0.9900 . ? C817 H8ZB 0.9900 . ? C917 H9ZA 0.9800 . ? C917 H9ZB 0.9800 . ? C917 H9ZC 0.9800 . ? O110 C110 1.345(5) . ? O210 N110 1.389(4) . ? O210 H210 0.8400 . ? N110 C710 1.291(5) . ? C110 C610 1.389(6) . ? C110 C210 1.419(5) . ? C210 C310 1.409(6) . ? C210 C710 1.465(6) . ? C310 C410 1.371(6) . ? C310 H310 0.9500 . ? C410 C510 1.382(5) . ? C410 H410 0.9500 . ? C510 C610 1.380(5) . ? C510 H510 0.9500 . ? C610 H610 0.9500 . ? C710 C810 1.518(5) . ? C810 C910 1.541(6) . ? C810 H81C 0.9900 . ? C810 H81D 0.9900 . ? C910 H91D 0.9800 . ? C910 H91E 0.9800 . ? C910 H91F 0.9800 . ? O111 C111 1.330(5) . ? O211 N111 1.390(4) . ? N111 C711 1.304(5) . ? C111 C611 1.399(5) . ? C111 C211 1.411(5) . ? C211 C311 1.397(5) . ? C211 C711 1.464(5) . ? C311 C411 1.366(5) . ? C311 H311 0.9500 . ? C411 C511 1.387(5) . ? C411 H411 0.9500 . ? C511 C611 1.366(6) . ? C511 H511 0.9500 . ? C611 H611 0.9500 . ? C711 C811 1.509(5) . ? C811 C911 1.538(5) . ? C811 H8FA 0.9900 . ? C811 H8FB 0.9900 . ? C911 H9FA 0.9800 . ? C911 H9FB 0.9800 . ? C911 H9FC 0.9800 . ? O112 C112 1.342(4) . ? O212 N112 1.410(3) . ? O212 H212 0.8400 . ? N112 C712 1.295(5) . ? C112 C612 1.393(5) . ? C112 C212 1.424(5) . ? C212 C312 1.400(5) . ? C212 C712 1.479(5) . ? C312 C412 1.372(5) . ? C312 H312 0.9500 . ? C412 C512 1.383(5) . ? C412 H412 0.9500 . ? C512 C612 1.375(5) . ? C512 H512 0.9500 . ? C612 H612 0.9500 . ? C712 C812 1.507(5) . ? C812 C912 1.515(6) . ? C812 H8EA 0.9900 . ? C812 H8EB 0.9900 . ? C912 H9EA 0.9800 . ? C912 H9EB 0.9800 . ? C912 H9EC 0.9800 . ? O113 C113 1.331(5) . ? O213 N113 1.399(4) . ? N113 C713 1.301(5) . ? C113 C613 1.389(5) . ? C113 C213 1.409(6) . ? C213 C313 1.404(6) . ? C213 C713 1.476(6) . ? C313 C413 1.365(6) . ? C313 H313 0.9500 . ? C413 C513 1.382(6) . ? C413 H413 0.9500 . ? C513 C613 1.377(6) . ? C513 H513 0.9500 . ? C613 H613 0.9500 . ? C713 C813 1.519(6) . ? C813 C913 1.519(5) . ? C813 H8AA 0.9900 . ? C813 H8AB 0.9900 . ? C913 H9AA 0.9800 . ? C913 H9AB 0.9800 . ? C913 H9AC 0.9800 . ? O114 C114 1.347(4) . ? O214 N114 1.393(4) . ? O214 H214 0.8400 . ? N114 C714 1.295(5) . ? C114 C614 1.377(5) . ? C114 C214 1.422(5) . ? C214 C314 1.395(5) . ? C214 C714 1.469(6) . ? C314 C414 1.379(5) . ? C314 H314 0.9500 . ? C414 C514 1.368(5) . ? C414 H414 0.9500 . ? C514 C614 1.379(5) . ? C514 H514 0.9500 . ? C614 H614 0.9500 . ? C714 C814 1.548(6) . ? C714 C818 1.548(6) . ? C814 C914 1.512(8) . ? C814 H81E 0.9900 . ? C814 H81F 0.9900 . ? C914 H91G 0.9800 . ? C914 H91H 0.9800 . ? C914 H91I 0.9800 . ? C818 C918 1.511(8) . ? C818 H8XA 0.9900 . ? C818 H8XB 0.9900 . ? C918 H9XA 0.9800 . ? C918 H9XB 0.9800 . ? C918 H9XC 0.9800 . ? O115 C115 1.340(5) . ? O215 N115 1.389(4) . ? N115 C715 1.307(5) . ? C115 C615 1.382(6) . ? C115 C215 1.416(5) . ? C215 C315 1.404(6) . ? C215 C715 1.448(6) . ? C315 C415 1.369(6) . ? C315 H315 0.9500 . ? C415 C515 1.370(5) . ? C415 H415 0.9500 . ? C515 C615 1.366(6) . ? C515 H515 0.9500 . ? C615 H615 0.9500 . ? C715 C815 1.525(5) . ? C815 C915 1.519(5) . ? C815 H8DE 0.9900 . ? C815 H8DB 0.9900 . ? C915 H9DA 0.9800 . ? C915 H9DB 0.9800 . ? C915 H9DC 0.9800 . ? O116 C116 1.345(5) . ? O216 N116 1.390(3) . ? O216 H216 0.8400 . ? N116 C716 1.305(5) . ? C116 C616 1.398(5) . ? C116 C216 1.411(6) . ? C216 C316 1.392(5) . ? C216 C716 1.491(5) . ? C316 C416 1.366(5) . ? C316 H316 0.9500 . ? C416 C516 1.374(6) . ? C416 H416 0.9500 . ? C516 C616 1.387(6) . ? C516 H516 0.9500 . ? C616 H616 0.9500 . ? C716 C816 1.490(5) . ? C816 C916 1.528(5) . ? C816 H8EC 0.9900 . ? C816 H8ED 0.9900 . ? C916 H9CA 0.9800 . ? C916 H9CB 0.9800 . ? C916 H9CC 0.9800 . ? N1R C1R 1.105(18) . ? C1R C2R 1.46(2) . ? C2R H2RA 0.9800 . ? C2R H2RB 0.9800 . ? C2R H2RC 0.9800 . ? N2R C3R 1.13(2) . ? C3R C4R 1.60(2) . ? C4R H4RA 0.9800 . ? C4R H4RB 0.9800 . ? C4R H4RC 0.9800 . ? N3R C5R 1.187(18) . ? C5R C6R 1.50(2) . ? C6R H6RA 0.9800 . ? C6R H6RB 0.9800 . ? C6R H6RC 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 O11 Mn1 O12 92.92(12) . . ? O11 Mn1 O23 173.10(11) . . ? O12 Mn1 O23 93.52(11) . . ? O11 Mn1 N11 86.46(13) . . ? O12 Mn1 N11 178.15(12) . . ? O23 Mn1 N11 87.18(13) . . ? O11 Mn1 O25 94.99(11) . . ? O12 Mn1 O25 86.23(10) . . ? O23 Mn1 O25 82.95(10) . . ? N11 Mn1 O25 95.57(11) . . ? O11 Mn1 N12 94.63(12) . . ? O12 Mn1 N12 81.85(11) . . ? O23 Mn1 N12 88.75(11) . . ? N11 Mn1 N12 96.45(12) . . ? O25 Mn1 N12 165.03(10) . . ? O13 Mn2 O14 93.85(12) . . ? O13 Mn2 O25 173.21(10) . . ? O14 Mn2 O25 92.54(11) . . ? O13 Mn2 N13 86.14(12) . . ? O14 Mn2 N13 179.70(13) . . ? O25 Mn2 N13 87.48(12) . . ? O13 Mn2 N14 90.31(12) . . ? O14 Mn2 N14 82.85(12) . . ? O25 Mn2 N14 88.19(12) . . ? N13 Mn2 N14 97.45(12) . . ? O13 Mn2 O27 100.40(11) . . ? O14 Mn2 O27 85.49(11) . . ? O25 Mn2 O27 82.40(11) . . ? N13 Mn2 O27 94.22(11) . . ? N14 Mn2 O27 164.66(10) . . ? O15 Mn3 O16 91.92(13) . . ? O15 Mn3 O27 172.03(12) . . ? O16 Mn3 O27 94.98(12) . . ? O15 Mn3 N15 86.03(14) . . ? O16 Mn3 N15 176.14(12) . . ? O27 Mn3 N15 87.30(13) . . ? O15 Mn3 O21 92.91(12) . . ? O16 Mn3 O21 86.45(11) . . ? O27 Mn3 O21 83.56(10) . . ? N15 Mn3 O21 96.91(12) . . ? O15 Mn3 N16 93.73(13) . . ? O16 Mn3 N16 80.94(13) . . ? O27 Mn3 N16 91.29(12) . . ? N15 Mn3 N16 95.92(14) . . ? O21 Mn3 N16 165.92(13) . . ? O17 Mn4 O18 93.72(12) . . ? O17 Mn4 O21 174.38(11) . . ? O18 Mn4 O21 91.87(12) . . ? O17 Mn4 N17 86.34(13) . . ? O18 Mn4 N17 178.15(13) . . ? O21 Mn4 N17 88.06(13) . . ? O17 Mn4 N18 91.29(13) . . ? O18 Mn4 N18 83.25(13) . . ? O21 Mn4 N18 88.79(12) . . ? N17 Mn4 N18 94.90(14) . . ? O17 Mn4 O23 98.52(11) . . ? O18 Mn4 O23 88.49(11) . . ? O21 Mn4 O23 82.19(10) . . ? N17 Mn4 O23 93.33(12) . . ? N18 Mn4 O23 167.57(12) . . ? O19 Mn5 O110 93.35(12) . . ? O19 Mn5 O211 173.50(11) . . ? O110 Mn5 O211 92.13(12) . . ? O19 Mn5 N19 86.81(14) . . ? O110 Mn5 N19 175.49(11) . . ? O211 Mn5 N19 88.00(13) . . ? O19 Mn5 O213 92.40(11) . . ? O110 Mn5 O213 90.78(10) . . ? O211 Mn5 O213 84.02(10) . . ? N19 Mn5 O213 93.71(11) . . ? O19 Mn5 N110 93.14(12) . . ? O110 Mn5 N110 82.46(12) . . ? O211 Mn5 N110 91.04(12) . . ? N19 Mn5 N110 93.03(13) . . ? O213 Mn5 N110 171.49(11) . . ? O111 Mn6 O112 94.42(12) . . ? O111 Mn6 O213 173.97(12) . . ? O112 Mn6 O213 90.73(12) . . ? O111 Mn6 N111 87.03(13) . . ? O112 Mn6 N111 177.12(13) . . ? O213 Mn6 N111 87.97(12) . . ? O111 Mn6 N112 92.55(12) . . ? O112 Mn6 N112 83.65(12) . . ? O213 Mn6 N112 91.15(12) . . ? N111 Mn6 N112 93.81(12) . . ? O111 Mn6 O215 94.12(11) . . ? O112 Mn6 O215 91.32(10) . . ? O213 Mn6 O215 82.59(10) . . ? N111 Mn6 O215 91.06(11) . . ? N112 Mn6 O215 171.94(12) . . ? O113 Mn7 O114 92.58(12) . . ? O113 Mn7 O215 175.14(12) . . ? O114 Mn7 O215 92.26(12) . . ? O113 Mn7 N113 87.18(14) . . ? O114 Mn7 N113 179.69(15) . . ? O215 Mn7 N113 87.98(14) . . ? O113 Mn7 N114 91.83(12) . . ? O114 Mn7 N114 81.76(12) . . ? O215 Mn7 N114 88.50(11) . . ? N113 Mn7 N114 98.06(13) . . ? O113 Mn7 O29 96.79(10) . . ? O114 Mn7 O29 86.94(10) . . ? O215 Mn7 O29 83.84(10) . . ? N113 Mn7 O29 93.28(11) . . ? N114 Mn7 O29 166.08(12) . . ? O115 Mn8 O116 93.14(11) . . ? O115 Mn8 O29 174.55(10) . . ? O116 Mn8 O29 91.93(11) . . ? O115 Mn8 N115 86.75(13) . . ? O116 Mn8 N115 177.31(13) . . ? O29 Mn8 N115 88.29(12) . . ? O115 Mn8 N116 91.79(12) . . ? O116 Mn8 N116 83.15(11) . . ? O29 Mn8 N116 90.80(12) . . ? N115 Mn8 N116 94.17(12) . . ? O115 Mn8 O211 94.00(11) . . ? O116 Mn8 O211 90.58(10) . . ? O29 Mn8 O211 83.95(10) . . ? N115 Mn8 O211 92.11(12) . . ? N116 Mn8 O211 171.69(11) . . ? C11 O11 Mn1 121.4(3) . . ? N11 O21 Mn4 116.09(19) . . ? N11 O21 Mn3 112.2(2) . . ? Mn4 O21 Mn3 115.81(13) . . ? C71 N11 O21 115.7(3) . . ? C71 N11 Mn1 128.3(3) . . ? O21 N11 Mn1 115.2(2) . . ? O11 C11 C61 117.8(4) . . ? O11 C11 C21 122.4(4) . . ? C61 C11 C21 119.7(4) . . ? C31 C21 C11 117.8(4) . . ? C31 C21 C71 119.8(4) . . ? C11 C21 C71 122.3(4) . . ? C41 C31 C21 121.7(5) . . ? C41 C31 H31 119.1 . . ? C21 C31 H31 119.1 . . ? C31 C41 C51 119.7(4) . . ? C31 C41 H41 120.2 . . ? C51 C41 H41 120.2 . . ? C61 C51 C41 120.1(4) . . ? C61 C51 H51 120.0 . . ? C41 C51 H51 120.0 . . ? C51 C61 C11 121.1(5) . . ? C51 C61 H61 119.5 . . ? C11 C61 H61 119.5 . . ? N11 C71 C21 117.9(4) . . ? N11 C71 C81 121.5(4) . . ? C21 C71 C81 120.6(4) . . ? C71 C81 C91 112.9(3) . . ? C71 C81 H81A 109.0 . . ? C91 C81 H81A 109.0 . . ? C71 C81 H81B 109.0 . . ? C91 C81 H81B 109.0 . . ? H81A C81 H81B 107.8 . . ? C81 C91 H91A 109.5 . . ? C81 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C81 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C12 O12 Mn1 117.7(2) . . ? N12 O22 H22 109.5 . . ? C72 N12 O22 114.1(3) . . ? C72 N12 Mn1 123.6(3) . . ? O22 N12 Mn1 121.6(2) . . ? O12 C12 C62 120.1(4) . . ? O12 C12 C22 122.3(4) . . ? C62 C12 C22 117.5(4) . . ? C32 C22 C12 119.1(4) . . ? C32 C22 C72 119.4(4) . . ? C12 C22 C72 121.5(4) . . ? C42 C32 C22 121.9(4) . . ? C42 C32 H32 119.1 . . ? C22 C32 H32 119.1 . . ? C32 C42 C52 119.0(4) . . ? C32 C42 H42 120.5 . . ? C52 C42 H42 120.5 . . ? C62 C52 C42 120.6(4) . . ? C62 C52 H52 119.7 . . ? C42 C52 H52 119.7 . . ? C52 C62 C12 121.9(4) . . ? C52 C62 H62 119.1 . . ? C12 C62 H62 119.1 . . ? N12 C72 C22 118.4(3) . . ? N12 C72 C82 121.5(4) . . ? C22 C72 C82 120.0(4) . . ? C72 C82 C92 110.8(4) . . ? C72 C82 H82A 109.5 . . ? C92 C82 H82A 109.5 . . ? C72 C82 H82B 109.5 . . ? C92 C82 H82B 109.5 . . ? H82A C82 H82B 108.1 . . ? C82 C92 H92A 109.5 . . ? C82 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C82 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C13 O13 Mn2 119.4(2) . . ? N13 O23 Mn1 113.5(2) . . ? N13 O23 Mn4 116.2(2) . . ? Mn1 O23 Mn4 115.61(12) . . ? C73 N13 O23 117.5(3) . . ? C73 N13 Mn2 127.6(3) . . ? O23 N13 Mn2 114.9(2) . . ? O13 C13 C63 118.2(3) . . ? O13 C13 C23 123.2(4) . . ? C63 C13 C23 118.6(4) . . ? C33 C23 C13 118.9(4) . . ? C33 C23 C73 119.4(4) . . ? C13 C23 C73 121.7(3) . . ? C43 C33 C23 121.0(4) . . ? C43 C33 H33 119.5 . . ? C23 C33 H33 119.5 . . ? C33 C43 C53 120.0(4) . . ? C33 C43 H43 120.0 . . ? C53 C43 H43 120.0 . . ? C63 C53 C43 120.3(4) . . ? C63 C53 H53 119.9 . . ? C43 C53 H53 119.9 . . ? C53 C63 C13 121.2(4) . . ? C53 C63 H63 119.4 . . ? C13 C63 H63 119.4 . . ? N13 C73 C23 117.9(3) . . ? N13 C73 C83 121.0(4) . . ? C23 C73 C83 121.1(3) . . ? C73 C83 C93 114.4(4) . . ? C73 C83 H83A 108.6 . . ? C93 C83 H83A 108.6 . . ? C73 C83 H83B 108.6 . . ? C93 C83 H83B 108.6 . . ? H83A C83 H83B 107.6 . . ? C83 C93 H93A 109.5 . . ? C83 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C83 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C14 O14 Mn2 119.5(2) . . ? N14 O24 H24A 109.5 . . ? C74 N14 O24 112.5(3) . . ? C74 N14 Mn2 125.1(3) . . ? O24 N14 Mn2 122.3(2) . . ? O14 C14 C64 118.1(4) . . ? O14 C14 C24 123.2(4) . . ? C64 C14 C24 118.7(4) . . ? C34 C24 C14 118.2(4) . . ? C34 C24 C74 117.4(4) . . ? C14 C24 C74 124.4(4) . . ? C44 C34 C24 121.6(4) . . ? C44 C34 H34 119.2 . . ? C24 C34 H34 119.2 . . ? C54 C44 C34 119.6(5) . . ? C54 C44 H44 120.2 . . ? C34 C44 H44 120.2 . . ? C64 C54 C44 120.6(4) . . ? C64 C54 H54 119.7 . . ? C44 C54 H54 119.7 . . ? C54 C64 C14 121.3(5) . . ? C54 C64 H64 119.3 . . ? C14 C64 H64 119.3 . . ? N14 C74 C24 117.5(4) . . ? N14 C74 C84 120.7(4) . . ? C24 C74 C84 121.7(4) . . ? C74 C84 C94 113.8(3) . . ? C74 C84 H84A 108.8 . . ? C94 C84 H84A 108.8 . . ? C74 C84 H84B 108.8 . . ? C94 C84 H84B 108.8 . . ? H84A C84 H84B 107.7 . . ? C84 C94 H94A 109.5 . . ? C84 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C84 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C15 O15 Mn3 120.7(3) . . ? N15 O25 Mn2 115.6(2) . . ? N15 O25 Mn1 112.2(2) . . ? Mn2 O25 Mn1 115.14(11) . . ? C75 N15 O25 115.2(4) . . ? C75 N15 Mn3 128.4(3) . . ? O25 N15 Mn3 116.1(3) . . ? O15 C15 C25 123.5(4) . . ? O15 C15 C65 117.4(5) . . ? C25 C15 C65 119.0(5) . . ? C15 C25 C35 119.9(4) . . ? C15 C25 C75 121.4(4) . . ? C35 C25 C75 118.5(5) . . ? C45 C35 C25 119.5(5) . . ? C45 C35 H35 120.3 . . ? C25 C35 H35 120.3 . . ? C55 C45 C35 119.2(5) . . ? C55 C45 H45 120.4 . . ? C35 C45 H45 120.4 . . ? C65 C55 C45 122.3(5) . . ? C65 C55 H55 118.9 . . ? C45 C55 H55 118.9 . . ? C55 C65 C15 120.1(6) . . ? C55 C65 H65 120.0 . . ? C15 C65 H65 120.0 . . ? N15 C75 C25 116.8(5) . . ? N15 C75 C85 121.6(4) . . ? C25 C75 C85 121.6(4) . . ? C75 C85 C95 112.1(4) . . ? C75 C85 H85A 109.2 . . ? C95 C85 H85A 109.2 . . ? C75 C85 H85B 109.2 . . ? C95 C85 H85B 109.2 . . ? H85A C85 H85B 107.9 . . ? C85 C95 H95A 109.5 . . ? C85 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C85 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C16 O16 Mn3 118.5(3) . . ? N16 O26 H26A 109.5 . . ? C76 N16 O26 113.8(3) . . ? C76 N16 Mn3 125.3(3) . . ? O26 N16 Mn3 120.3(2) . . ? O16 C16 C66 118.4(4) . . ? O16 C16 C26 122.7(4) . . ? C66 C16 C26 118.7(4) . . ? C36 C26 C16 118.3(4) . . ? C36 C26 C76 118.6(4) . . ? C16 C26 C76 123.2(4) . . ? C46 C36 C26 122.2(4) . . ? C46 C36 H36 118.9 . . ? C26 C36 H36 118.9 . . ? C56 C46 C36 119.3(4) . . ? C56 C46 H46 120.4 . . ? C36 C46 H46 120.4 . . ? C46 C56 C66 120.0(5) . . ? C46 C56 H56 120.0 . . ? C66 C56 H56 120.0 . . ? C56 C66 C16 121.5(4) . . ? C56 C66 H66 119.3 . . ? C16 C66 H66 119.3 . . ? N16 C76 C26 117.8(4) . . ? N16 C76 C86 121.6(4) . . ? C26 C76 C86 120.6(4) . . ? C76 C86 C96 110.1(4) . . ? C76 C86 H86A 109.6 . . ? C96 C86 H86A 109.6 . . ? C76 C86 H86B 109.6 . . ? C96 C86 H86B 109.6 . . ? H86A C86 H86B 108.2 . . ? C86 C96 H96A 109.5 . . ? C86 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C86 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C17 O17 Mn4 121.7(2) . . ? N17 O27 Mn3 113.7(2) . . ? N17 O27 Mn2 115.04(19) . . ? Mn3 O27 Mn2 115.38(13) . . ? C77 N17 O27 115.9(3) . . ? C77 N17 Mn4 128.2(3) . . ? O27 N17 Mn4 115.3(3) . . ? O17 C17 C67 118.7(4) . . ? O17 C17 C27 123.1(4) . . ? C67 C17 C27 118.1(5) . . ? C37 C27 C17 118.6(4) . . ? C37 C27 C77 120.9(4) . . ? C17 C27 C77 120.4(4) . . ? C47 C37 C27 122.2(4) . . ? C47 C37 H37 118.9 . . ? C27 C37 H37 118.9 . . ? C37 C47 C57 119.2(5) . . ? C37 C47 H47 120.4 . . ? C57 C47 H47 120.4 . . ? C67 C57 C47 120.9(5) . . ? C67 C57 H57 119.5 . . ? C47 C57 H57 119.5 . . ? C57 C67 C17 121.0(4) . . ? C57 C67 H67 119.5 . . ? C17 C67 H67 119.5 . . ? N17 C77 C27 118.7(4) . . ? N17 C77 C87 120.9(4) . . ? C27 C77 C87 120.4(4) . . ? C77 C87 C97 111.9(4) . . ? C77 C87 H87A 109.2 . . ? C97 C87 H87A 109.2 . . ? C77 C87 H87B 109.2 . . ? C97 C87 H87B 109.2 . . ? H87A C87 H87B 107.9 . . ? C87 C97 H97A 109.5 . . ? C87 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C87 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C18 O18 Mn4 118.7(3) . . ? N18 O28 H28A 109.5 . . ? C78 N18 O28 111.8(4) . . ? C78 N18 Mn4 124.6(3) . . ? O28 N18 Mn4 122.8(3) . . ? O18 C18 C68 118.0(4) . . ? O18 C18 C28 123.0(4) . . ? C68 C18 C28 119.0(4) . . ? C38 C28 C18 117.4(4) . . ? C38 C28 C78 118.0(5) . . ? C18 C28 C78 124.6(4) . . ? C48 C38 C28 122.4(5) . . ? C48 C38 H38 118.8 . . ? C28 C38 H38 118.8 . . ? C38 C48 C58 119.5(5) . . ? C38 C48 H48 120.3 . . ? C58 C48 H48 120.3 . . ? C68 C58 C48 120.1(4) . . ? C68 C58 H58 119.9 . . ? C48 C58 H58 119.9 . . ? C58 C68 C18 121.6(5) . . ? C58 C68 H68 119.2 . . ? C18 C68 H68 119.2 . . ? N18 C78 C88 122.5(4) . . ? N18 C78 C28 117.8(4) . . ? C88 C78 C28 119.6(4) . . ? C78 C88 C98 110.2(4) . . ? C78 C88 H88A 109.6 . . ? C98 C88 H88A 109.6 . . ? C78 C88 H88B 109.6 . . ? C98 C88 H88B 109.6 . . ? H88A C88 H88B 108.1 . . ? C88 C98 H98A 109.5 . . ? C88 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C88 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C19 O19 Mn5 119.4(3) . . ? N19 O29 Mn8 113.8(2) . . ? N19 O29 Mn7 114.4(2) . . ? Mn8 O29 Mn7 114.37(11) . . ? C79 N19 O29 117.4(3) . . ? C79 N19 Mn5 125.6(3) . . ? O29 N19 Mn5 116.8(2) . . ? O19 C19 C69 117.5(5) . . ? O19 C19 C29 122.9(4) . . ? C69 C19 C29 119.7(4) . . ? C39 C29 C19 118.7(4) . . ? C39 C29 C79 120.1(5) . . ? C19 C29 C79 121.2(4) . . ? C49 C39 C29 120.9(5) . . ? C49 C39 H39 119.5 . . ? C29 C39 H39 119.5 . . ? C39 C49 C59 119.4(5) . . ? C39 C49 H49 120.3 . . ? C59 C49 H49 120.3 . . ? C69 C59 C49 121.4(5) . . ? C69 C59 H59 119.3 . . ? C49 C59 H59 119.3 . . ? C59 C69 C19 119.8(5) . . ? C59 C69 H69 120.1 . . ? C19 C69 H69 120.1 . . ? N19 C79 C29 119.4(4) . . ? N19 C79 C89 121.7(5) . . ? C29 C79 C89 118.4(5) . . ? N19 C79 C817 116.7(7) . . ? C29 C79 C817 121.7(7) . . ? C99 C89 C79 105.7(6) . . ? C99 C89 H89A 110.6 . . ? C79 C89 H89A 110.6 . . ? C99 C89 H89B 110.6 . . ? C79 C89 H89B 110.6 . . ? H89A C89 H89B 108.7 . . ? C89 C99 H99A 109.5 . . ? C89 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C89 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C917 C817 C79 101.9(11) . . ? C917 C817 H8ZA 111.4 . . ? C79 C817 H8ZA 111.4 . . ? C917 C817 H8ZB 111.4 . . ? C79 C817 H8ZB 111.4 . . ? H8ZA C817 H8ZB 109.2 . . ? C817 C917 H9ZA 109.5 . . ? C817 C917 H9ZB 109.5 . . ? H9ZA C917 H9ZB 109.5 . . ? C817 C917 H9ZC 109.5 . . ? H9ZA C917 H9ZC 109.5 . . ? H9ZB C917 H9ZC 109.5 . . ? C110 O110 Mn5 119.4(2) . . ? N110 O210 H210 109.5 . . ? C710 N110 O210 113.3(3) . . ? C710 N110 Mn5 123.2(3) . . ? O210 N110 Mn5 123.1(2) . . ? O110 C110 C610 118.0(4) . . ? O110 C110 C210 122.2(4) . . ? C610 C110 C210 119.8(4) . . ? C310 C210 C110 116.7(5) . . ? C310 C210 C710 118.8(4) . . ? C110 C210 C710 124.5(4) . . ? C410 C310 C210 122.5(4) . . ? C410 C310 H310 118.7 . . ? C210 C310 H310 118.7 . . ? C310 C410 C510 119.9(4) . . ? C310 C410 H410 120.1 . . ? C510 C410 H410 120.1 . . ? C610 C510 C410 119.5(5) . . ? C610 C510 H510 120.2 . . ? C410 C510 H510 120.3 . . ? C510 C610 C110 121.5(4) . . ? C510 C610 H610 119.2 . . ? C110 C610 H610 119.2 . . ? N110 C710 C210 118.9(4) . . ? N110 C710 C810 119.9(4) . . ? C210 C710 C810 121.2(4) . . ? C710 C810 C910 111.6(3) . . ? C710 C810 H81C 109.3 . . ? C910 C810 H81C 109.3 . . ? C710 C810 H81D 109.3 . . ? C910 C810 H81D 109.3 . . ? H81C C810 H81D 108.0 . . ? C810 C910 H91D 109.5 . . ? C810 C910 H91E 109.5 . . ? H91D C910 H91E 109.5 . . ? C810 C910 H91F 109.5 . . ? H91D C910 H91F 109.5 . . ? H91E C910 H91F 109.5 . . ? C111 O111 Mn6 121.6(2) . . ? N111 O211 Mn5 114.0(2) . . ? N111 O211 Mn8 115.4(2) . . ? Mn5 O211 Mn8 114.21(12) . . ? C711 N111 O211 116.6(3) . . ? C711 N111 Mn6 126.8(3) . . ? O211 N111 Mn6 116.3(2) . . ? O111 C111 C611 118.2(4) . . ? O111 C111 C211 123.3(4) . . ? C611 C111 C211 118.4(4) . . ? C311 C211 C111 118.9(4) . . ? C311 C211 C711 119.4(3) . . ? C111 C211 C711 121.6(4) . . ? C411 C311 C211 121.6(4) . . ? C411 C311 H311 119.2 . . ? C211 C311 H311 119.2 . . ? C311 C411 C511 119.1(4) . . ? C311 C411 H411 120.4 . . ? C511 C411 H411 120.4 . . ? C611 C511 C411 120.8(4) . . ? C611 C511 H511 119.6 . . ? C411 C511 H511 119.6 . . ? C511 C611 C111 120.9(4) . . ? C511 C611 H611 119.5 . . ? C111 C611 H611 119.5 . . ? N111 C711 C211 118.8(3) . . ? N111 C711 C811 120.4(3) . . ? C211 C711 C811 120.7(4) . . ? C711 C811 C911 112.2(3) . . ? C711 C811 H8FA 109.2 . . ? C911 C811 H8FA 109.2 . . ? C711 C811 H8FB 109.2 . . ? C911 C811 H8FB 109.2 . . ? H8FA C811 H8FB 107.9 . . ? C811 C911 H9FA 109.5 . . ? C811 C911 H9FB 109.5 . . ? H9FA C911 H9FB 109.5 . . ? C811 C911 H9FC 109.5 . . ? H9FA C911 H9FC 109.5 . . ? H9FB C911 H9FC 109.5 . . ? C112 O112 Mn6 127.3(2) . . ? N112 O212 H212 109.5 . . ? C712 N112 O212 112.2(3) . . ? C712 N112 Mn6 126.1(3) . . ? O212 N112 Mn6 119.3(2) . . ? O112 C112 C612 116.9(4) . . ? O112 C112 C212 123.7(3) . . ? C612 C112 C212 119.3(3) . . ? C312 C212 C112 116.8(3) . . ? C312 C212 C712 117.8(4) . . ? C112 C212 C712 125.3(3) . . ? C412 C312 C212 123.0(4) . . ? C412 C312 H312 118.5 . . ? C212 C312 H312 118.5 . . ? C312 C412 C512 119.4(4) . . ? C312 C412 H412 120.3 . . ? C512 C412 H412 120.3 . . ? C612 C512 C412 119.7(4) . . ? C612 C512 H512 120.2 . . ? C412 C512 H512 120.2 . . ? C512 C612 C112 121.7(4) . . ? C512 C612 H612 119.1 . . ? C112 C612 H612 119.1 . . ? N112 C712 C212 118.3(4) . . ? N112 C712 C812 121.4(3) . . ? C212 C712 C812 120.3(3) . . ? C712 C812 C912 111.7(4) . . ? C712 C812 H8EA 109.3 . . ? C912 C812 H8EA 109.3 . . ? C712 C812 H8EB 109.3 . . ? C912 C812 H8EB 109.3 . . ? H8EA C812 H8EB 107.9 . . ? C812 C912 H9EA 109.5 . . ? C812 C912 H9EB 109.5 . . ? H9EA C912 H9EB 109.5 . . ? C812 C912 H9EC 109.5 . . ? H9EA C912 H9EC 109.5 . . ? H9EB C912 H9EC 109.5 . . ? C113 O113 Mn7 121.8(2) . . ? N113 O213 Mn6 115.0(2) . . ? N113 O213 Mn5 114.52(19) . . ? Mn6 O213 Mn5 115.44(13) . . ? C713 N113 O213 115.9(3) . . ? C713 N113 Mn7 128.4(3) . . ? O213 N113 Mn7 115.2(3) . . ? O113 C113 C613 118.7(4) . . ? O113 C113 C213 122.7(4) . . ? C613 C113 C213 118.5(4) . . ? C313 C213 C113 118.8(4) . . ? C313 C213 C713 119.4(4) . . ? C113 C213 C713 121.8(4) . . ? C413 C313 C213 121.8(5) . . ? C413 C313 H313 119.1 . . ? C213 C313 H313 119.1 . . ? C313 C413 C513 118.7(5) . . ? C313 C413 H413 120.7 . . ? C513 C413 H413 120.7 . . ? C613 C513 C413 121.2(4) . . ? C613 C513 H513 119.4 . . ? C413 C513 H513 119.4 . . ? C513 C613 C113 120.9(4) . . ? C513 C613 H613 119.6 . . ? C113 C613 H613 119.6 . . ? N113 C713 C213 118.5(4) . . ? N113 C713 C813 122.9(4) . . ? C213 C713 C813 118.6(4) . . ? C913 C813 C713 109.5(4) . . ? C913 C813 H8AA 109.8 . . ? C713 C813 H8AA 109.8 . . ? C913 C813 H8AB 109.8 . . ? C713 C813 H8AB 109.8 . . ? H8AA C813 H8AB 108.2 . . ? C813 C913 H9AA 109.5 . . ? C813 C913 H9AB 109.5 . . ? H9AA C913 H9AB 109.5 . . ? C813 C913 H9AC 109.5 . . ? H9AA C913 H9AC 109.5 . . ? H9AB C913 H9AC 109.5 . . ? C114 O114 Mn7 122.3(3) . . ? N114 O214 H214 109.5 . . ? C714 N114 O214 113.4(3) . . ? C714 N114 Mn7 126.3(3) . . ? O214 N114 Mn7 120.3(2) . . ? O114 C114 C614 118.3(3) . . ? O114 C114 C214 122.0(4) . . ? C614 C114 C214 119.6(4) . . ? C314 C214 C114 116.9(4) . . ? C314 C214 C714 120.0(4) . . ? C114 C214 C714 123.1(4) . . ? C414 C314 C214 122.5(4) . . ? C414 C314 H314 118.7 . . ? C214 C314 H314 118.7 . . ? C514 C414 C314 119.3(4) . . ? C514 C414 H414 120.3 . . ? C314 C414 H414 120.3 . . ? C414 C514 C614 120.1(4) . . ? C414 C514 H514 119.9 . . ? C614 C514 H514 119.9 . . ? C114 C614 C514 121.4(4) . . ? C114 C614 H614 119.3 . . ? C514 C614 H614 119.3 . . ? N114 C714 C214 119.2(4) . . ? N114 C714 C814 121.6(4) . . ? C214 C714 C814 119.0(4) . . ? N114 C714 C818 114.9(9) . . ? C214 C714 C818 120.9(9) . . ? C914 C814 C714 105.1(6) . . ? C914 C814 H81E 110.7 . . ? C714 C814 H81E 110.7 . . ? C914 C814 H81F 110.7 . . ? C714 C814 H81F 110.7 . . ? H81E C814 H81F 108.8 . . ? C814 C914 H91G 109.5 . . ? C814 C914 H91H 109.5 . . ? H91G C914 H91H 109.5 . . ? C814 C914 H91I 109.5 . . ? H91G C914 H91I 109.5 . . ? H91H C914 H91I 109.5 . . ? C918 C818 C714 96.0(12) . . ? C918 C818 H8XA 112.5 . . ? C714 C818 H8XA 112.5 . . ? C918 C818 H8XB 112.5 . . ? C714 C818 H8XB 112.5 . . ? H8XA C818 H8XB 110.1 . . ? C818 C918 H9XA 109.5 . . ? C818 C918 H9XB 109.5 . . ? H9XA C918 H9XB 109.5 . . ? C818 C918 H9XC 109.5 . . ? H9XA C918 H9XC 109.5 . . ? H9XB C918 H9XC 109.5 . . ? C115 O115 Mn8 119.3(3) . . ? N115 O215 Mn7 113.3(2) . . ? N115 O215 Mn6 116.47(19) . . ? Mn7 O215 Mn6 114.96(13) . . ? C715 N115 O215 117.8(3) . . ? C715 N115 Mn8 126.1(3) . . ? O215 N115 Mn8 115.7(2) . . ? O115 C115 C615 118.9(4) . . ? O115 C115 C215 121.7(4) . . ? C615 C115 C215 119.4(4) . . ? C315 C215 C115 117.0(4) . . ? C315 C215 C715 120.7(4) . . ? C115 C215 C715 122.2(4) . . ? C415 C315 C215 122.7(4) . . ? C415 C315 H315 118.6 . . ? C215 C315 H315 118.6 . . ? C315 C415 C515 118.5(4) . . ? C315 C415 H415 120.7 . . ? C515 C415 H415 120.7 . . ? C615 C515 C415 121.2(5) . . ? C615 C515 H515 119.4 . . ? C415 C515 H515 119.4 . . ? C515 C615 C115 121.1(4) . . ? C515 C615 H615 119.5 . . ? C115 C615 H615 119.5 . . ? N115 C715 C215 118.5(3) . . ? N115 C715 C815 120.5(4) . . ? C215 C715 C815 121.0(4) . . ? C915 C815 C715 111.9(4) . . ? C915 C815 H8DE 109.2 . . ? C715 C815 H8DE 109.2 . . ? C915 C815 H8DB 109.2 . . ? C715 C815 H8DB 109.2 . . ? H8DE C815 H8DB 107.9 . . ? C815 C915 H9DA 109.5 . . ? C815 C915 H9DB 109.5 . . ? H9DA C915 H9DB 109.5 . . ? C815 C915 H9DC 109.5 . . ? H9DA C915 H9DC 109.5 . . ? H9DB C915 H9DC 109.5 . . ? C116 O116 Mn8 120.2(2) . . ? N116 O216 H216 109.5 . . ? C716 N116 O216 111.6(3) . . ? C716 N116 Mn8 125.4(3) . . ? O216 N116 Mn8 122.7(2) . . ? O116 C116 C616 117.6(4) . . ? O116 C116 C216 124.2(3) . . ? C616 C116 C216 118.2(4) . . ? C316 C216 C116 118.1(4) . . ? C316 C216 C716 118.0(4) . . ? C116 C216 C716 123.8(4) . . ? C416 C316 C216 123.3(4) . . ? C416 C316 H316 118.4 . . ? C216 C316 H316 118.4 . . ? C316 C416 C516 118.6(4) . . ? C316 C416 H416 120.7 . . ? C516 C416 H416 120.7 . . ? C416 C516 C616 120.3(4) . . ? C416 C516 H516 119.8 . . ? C616 C516 H516 119.8 . . ? C516 C616 C116 121.4(4) . . ? C516 C616 H616 119.3 . . ? C116 C616 H616 119.3 . . ? N116 C716 C816 121.1(3) . . ? N116 C716 C216 117.4(4) . . ? C816 C716 C216 121.4(4) . . ? C716 C816 C916 112.3(3) . . ? C716 C816 H8EC 109.1 . . ? C916 C816 H8EC 109.1 . . ? C716 C816 H8ED 109.1 . . ? C916 C816 H8ED 109.1 . . ? H8EC C816 H8ED 107.9 . . ? C816 C916 H9CA 109.5 . . ? C816 C916 H9CB 109.5 . . ? H9CA C916 H9CB 109.5 . . ? C816 C916 H9CC 109.5 . . ? H9CA C916 H9CC 109.5 . . ? H9CB C916 H9CC 109.5 . . ? N1R C1R C2R 179.0(17) . . ? N2R C3R C4R 166(2) . . ? C3R C4R H4RA 109.5 . . ? C3R C4R H4RB 109.5 . . ? H4RA C4R H4RB 109.5 . . ? C3R C4R H4RC 109.5 . . ? H4RA C4R H4RC 109.5 . . ? H4RB C4R H4RC 109.5 . . ? N3R C5R C6R 159(2) . . ? C5R C6R H6RA 109.5 . . ? C5R C6R H6RB 109.5 . . ? H6RA C6R H6RB 109.5 . . ? C5R C6R H6RC 109.5 . . ? H6RA C6R H6RC 109.5 . . ? H6RB C6R H6RC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 C11 C21 C31 177.0(3) . . . . ? C61 C11 C21 C31 -0.1(5) . . . . ? O11 C11 C21 C71 0.6(5) . . . . ? C61 C11 C21 C71 -176.5(3) . . . . ? C11 C21 C31 C41 0.6(5) . . . . ? C71 C21 C31 C41 177.1(3) . . . . ? C21 C31 C41 C51 -0.6(5) . . . . ? C31 C41 C51 C61 0.1(5) . . . . ? C41 C51 C61 C11 0.3(5) . . . . ? O11 C11 C61 C51 -177.6(3) . . . . ? C21 C11 C61 C51 -0.4(5) . . . . ? O21 N11 C71 C21 172.4(3) . . . . ? O21 N11 C71 C81 -8.4(5) . . . . ? C31 C21 C71 N11 160.3(3) . . . . ? C11 C21 C71 N11 -23.4(5) . . . . ? C31 C21 C71 C81 -18.9(5) . . . . ? C11 C21 C71 C81 157.4(3) . . . . ? N11 C71 C81 C91 -85.7(5) . . . . ? C21 C71 C81 C91 93.5(5) . . . . ? O12 C12 C22 C32 178.0(3) . . . . ? C62 C12 C22 C32 -2.1(5) . . . . ? O12 C12 C22 C72 -3.4(5) . . . . ? C62 C12 C22 C72 176.6(3) . . . . ? C12 C22 C32 C42 1.1(5) . . . . ? C72 C22 C32 C42 -177.5(3) . . . . ? C22 C32 C42 C52 0.2(6) . . . . ? C32 C42 C52 C62 -0.6(6) . . . . ? C42 C52 C62 C12 -0.4(6) . . . . ? O12 C12 C62 C52 -178.3(3) . . . . ? C22 C12 C62 C52 1.8(5) . . . . ? O22 N12 C72 C22 -176.9(3) . . . . ? O22 N12 C72 C82 -1.5(5) . . . . ? C32 C22 C72 N12 -148.2(4) . . . . ? C12 C22 C72 N12 33.1(5) . . . . ? C32 C22 C72 C82 36.3(5) . . . . ? C12 C22 C72 C82 -142.3(4) . . . . ? N12 C72 C82 C92 -95.7(5) . . . . ? C22 C72 C82 C92 79.7(5) . . . . ? O13 C13 C23 C33 -175.3(4) . . . . ? C63 C13 C23 C33 2.3(6) . . . . ? O13 C13 C23 C73 2.5(6) . . . . ? C63 C13 C23 C73 -180.0(4) . . . . ? C13 C23 C33 C43 -2.1(6) . . . . ? C73 C23 C33 C43 -180.0(4) . . . . ? C23 C33 C43 C53 0.8(7) . . . . ? C33 C43 C53 C63 0.5(7) . . . . ? C43 C53 C63 C13 -0.3(7) . . . . ? O13 C13 C63 C53 176.6(4) . . . . ? C23 C13 C63 C53 -1.1(6) . . . . ? O23 N13 C73 C23 -174.9(3) . . . . ? O23 N13 C73 C83 4.7(5) . . . . ? C33 C23 C73 N13 -162.9(4) . . . . ? C13 C23 C73 N13 19.3(6) . . . . ? C33 C23 C73 C83 17.5(6) . . . . ? C13 C23 C73 C83 -160.3(4) . . . . ? N13 C73 C83 C93 -111.2(4) . . . . ? C23 C73 C83 C93 68.4(5) . . . . ? O14 C14 C24 C34 -179.8(4) . . . . ? C64 C14 C24 C34 1.9(6) . . . . ? O14 C14 C24 C74 1.1(6) . . . . ? C64 C14 C24 C74 -177.1(4) . . . . ? C14 C24 C34 C44 -1.2(7) . . . . ? C74 C24 C34 C44 178.0(4) . . . . ? C24 C34 C44 C54 -1.4(7) . . . . ? C34 C44 C54 C64 3.2(8) . . . . ? C44 C54 C64 C14 -2.5(8) . . . . ? O14 C14 C64 C54 -178.5(4) . . . . ? C24 C14 C64 C54 -0.2(7) . . . . ? O24 N14 C74 C24 179.2(3) . . . . ? O24 N14 C74 C84 -2.1(5) . . . . ? C34 C24 C74 N14 159.8(4) . . . . ? C14 C24 C74 N14 -21.2(6) . . . . ? C34 C24 C74 C84 -19.0(6) . . . . ? C14 C24 C74 C84 160.1(4) . . . . ? N14 C74 C84 C94 -82.2(5) . . . . ? C24 C74 C84 C94 96.5(4) . . . . ? O15 C15 C25 C35 -179.0(4) . . . . ? C65 C15 C25 C35 3.2(7) . . . . ? O15 C15 C25 C75 5.7(8) . . . . ? C65 C15 C25 C75 -172.0(4) . . . . ? C15 C25 C35 C45 -1.8(8) . . . . ? C75 C25 C35 C45 173.6(4) . . . . ? C25 C35 C45 C55 -0.3(8) . . . . ? C35 C45 C55 C65 0.9(9) . . . . ? C45 C55 C65 C15 0.5(9) . . . . ? O15 C15 C65 C55 179.5(5) . . . . ? C25 C15 C65 C55 -2.6(7) . . . . ? O25 N15 C75 C25 170.4(3) . . . . ? O25 N15 C75 C85 -7.5(6) . . . . ? C15 C25 C75 N15 -24.3(7) . . . . ? C35 C25 C75 N15 160.4(4) . . . . ? C15 C25 C75 C85 153.7(5) . . . . ? C35 C25 C75 C85 -21.6(6) . . . . ? N15 C75 C85 C95 -86.9(5) . . . . ? C25 C75 C85 C95 95.2(5) . . . . ? O16 C16 C26 C36 -175.9(4) . . . . ? C66 C16 C26 C36 -0.4(6) . . . . ? O16 C16 C26 C76 3.6(6) . . . . ? C66 C16 C26 C76 179.0(4) . . . . ? C16 C26 C36 C46 0.0(7) . . . . ? C76 C26 C36 C46 -179.5(4) . . . . ? C26 C36 C46 C56 -0.5(7) . . . . ? C36 C46 C56 C66 1.6(7) . . . . ? C46 C56 C66 C16 -2.1(7) . . . . ? O16 C16 C66 C56 177.1(4) . . . . ? C26 C16 C66 C56 1.5(7) . . . . ? O26 N16 C76 C26 179.3(3) . . . . ? O26 N16 C76 C86 1.1(6) . . . . ? C36 C26 C76 N16 -162.2(4) . . . . ? C16 C26 C76 N16 18.3(6) . . . . ? C36 C26 C76 C86 16.1(6) . . . . ? C16 C26 C76 C86 -163.4(4) . . . . ? N16 C76 C86 C96 90.1(5) . . . . ? C26 C76 C86 C96 -88.1(5) . . . . ? O17 C17 C27 C37 -178.7(4) . . . . ? C67 C17 C27 C37 0.5(6) . . . . ? O17 C17 C27 C77 -1.2(7) . . . . ? C67 C17 C27 C77 178.0(4) . . . . ? C17 C27 C37 C47 -0.2(7) . . . . ? C77 C27 C37 C47 -177.7(4) . . . . ? C27 C37 C47 C57 0.5(7) . . . . ? C37 C47 C57 C67 -1.1(7) . . . . ? C47 C57 C67 C17 1.5(7) . . . . ? O17 C17 C67 C57 178.1(4) . . . . ? C27 C17 C67 C57 -1.1(7) . . . . ? O27 N17 C77 C27 -176.3(3) . . . . ? O27 N17 C77 C87 4.1(5) . . . . ? C37 C27 C77 N17 -156.8(4) . . . . ? C17 C27 C77 N17 25.7(6) . . . . ? C37 C27 C77 C87 22.8(6) . . . . ? C17 C27 C77 C87 -154.7(4) . . . . ? N17 C77 C87 C97 82.3(5) . . . . ? C27 C77 C87 C97 -97.3(5) . . . . ? O18 C18 C28 C38 -179.1(4) . . . . ? C68 C18 C28 C38 1.7(6) . . . . ? O18 C18 C28 C78 -0.5(7) . . . . ? C68 C18 C28 C78 -179.6(4) . . . . ? C18 C28 C38 C48 -0.4(7) . . . . ? C78 C28 C38 C48 -179.2(4) . . . . ? C28 C38 C48 C58 -0.5(8) . . . . ? C38 C48 C58 C68 0.1(8) . . . . ? C48 C58 C68 C18 1.2(8) . . . . ? O18 C18 C68 C58 178.6(4) . . . . ? C28 C18 C68 C58 -2.1(7) . . . . ? O28 N18 C78 C88 -0.2(6) . . . . ? O28 N18 C78 C28 -178.0(3) . . . . ? C38 C28 C78 N18 159.8(4) . . . . ? C18 C28 C78 N18 -18.9(7) . . . . ? C38 C28 C78 C88 -18.1(6) . . . . ? C18 C28 C78 C88 163.2(4) . . . . ? N18 C78 C88 C98 -81.4(5) . . . . ? C28 C78 C88 C98 96.4(5) . . . . ? O19 C19 C29 C39 -177.6(4) . . . . ? C69 C19 C29 C39 3.0(7) . . . . ? O19 C19 C29 C79 3.4(7) . . . . ? C69 C19 C29 C79 -176.0(4) . . . . ? C19 C29 C39 C49 0.1(8) . . . . ? C79 C29 C39 C49 179.1(5) . . . . ? C29 C39 C49 C59 -3.0(8) . . . . ? C39 C49 C59 C69 2.9(8) . . . . ? C49 C59 C69 C19 0.2(8) . . . . ? O19 C19 C69 C59 177.4(4) . . . . ? C29 C19 C69 C59 -3.1(7) . . . . ? O29 N19 C79 C29 173.2(4) . . . . ? O29 N19 C79 C89 1.5(7) . . . . ? O29 N19 C79 C817 -23.0(9) . . . . ? C39 C29 C79 N19 157.2(4) . . . . ? C19 C29 C79 N19 -23.8(7) . . . . ? C39 C29 C79 C89 -30.8(7) . . . . ? C19 C29 C79 C89 148.2(5) . . . . ? C39 C29 C79 C817 -5.8(10) . . . . ? C19 C29 C79 C817 173.2(8) . . . . ? N19 C79 C89 C99 -88.4(6) . . . . ? C29 C79 C89 C99 99.8(6) . . . . ? C817 C79 C89 C99 -5(2) . . . . ? N19 C79 C817 C917 126.0(9) . . . . ? C29 C79 C817 C917 -70.5(13) . . . . ? C89 C79 C817 C917 17.1(17) . . . . ? O110 C110 C210 C310 -180.0(4) . . . . ? C610 C110 C210 C310 -2.5(6) . . . . ? O110 C110 C210 C710 -1.8(7) . . . . ? C610 C110 C210 C710 175.7(4) . . . . ? C110 C210 C310 C410 2.3(7) . . . . ? C710 C210 C310 C410 -175.9(4) . . . . ? C210 C310 C410 C510 -0.6(7) . . . . ? C310 C410 C510 C610 -1.0(7) . . . . ? C410 C510 C610 C110 0.8(7) . . . . ? O110 C110 C610 C510 178.6(4) . . . . ? C210 C110 C610 C510 1.0(7) . . . . ? O210 N110 C710 C210 -178.8(4) . . . . ? O210 N110 C710 C810 0.8(5) . . . . ? C310 C210 C710 N110 -161.3(4) . . . . ? C110 C210 C710 N110 20.6(7) . . . . ? C310 C210 C710 C810 19.1(6) . . . . ? C110 C210 C710 C810 -159.0(4) . . . . ? N110 C710 C810 C910 80.1(5) . . . . ? C210 C710 C810 C910 -100.3(5) . . . . ? O111 C111 C211 C311 178.5(4) . . . . ? C611 C111 C211 C311 -2.8(6) . . . . ? O111 C111 C211 C711 -4.4(6) . . . . ? C611 C111 C211 C711 174.2(4) . . . . ? C111 C211 C311 C411 0.3(6) . . . . ? C711 C211 C311 C411 -176.7(4) . . . . ? C211 C311 C411 C511 3.1(7) . . . . ? C311 C411 C511 C611 -4.2(7) . . . . ? C411 C511 C611 C111 1.7(7) . . . . ? O111 C111 C611 C511 -179.5(4) . . . . ? C211 C111 C611 C511 1.8(7) . . . . ? O211 N111 C711 C211 -174.8(3) . . . . ? O211 N111 C711 C811 4.9(5) . . . . ? C311 C211 C711 N111 -158.3(4) . . . . ? C111 C211 C711 N111 24.7(6) . . . . ? C311 C211 C711 C811 22.0(6) . . . . ? C111 C211 C711 C811 -155.0(4) . . . . ? N111 C711 C811 C911 82.5(5) . . . . ? C211 C711 C811 C911 -97.8(4) . . . . ? O112 C112 C212 C312 -178.8(4) . . . . ? C612 C112 C212 C312 3.0(6) . . . . ? O112 C112 C212 C712 5.0(7) . . . . ? C612 C112 C212 C712 -173.2(4) . . . . ? C112 C212 C312 C412 -2.1(6) . . . . ? C712 C212 C312 C412 174.4(4) . . . . ? C212 C312 C412 C512 -1.2(6) . . . . ? C312 C412 C512 C612 3.6(7) . . . . ? C412 C512 C612 C112 -2.6(7) . . . . ? O112 C112 C612 C512 -179.1(4) . . . . ? C212 C112 C612 C512 -0.7(6) . . . . ? O212 N112 C712 C212 179.7(3) . . . . ? O212 N112 C712 C812 -0.8(6) . . . . ? C312 C212 C712 N112 175.0(4) . . . . ? C112 C212 C712 N112 -8.8(6) . . . . ? C312 C212 C712 C812 -4.5(6) . . . . ? C112 C212 C712 C812 171.7(4) . . . . ? N112 C712 C812 C912 -91.4(5) . . . . ? C212 C712 C812 C912 88.1(5) . . . . ? O113 C113 C213 C313 174.7(4) . . . . ? C613 C113 C213 C313 -2.8(6) . . . . ? O113 C113 C213 C713 -4.6(6) . . . . ? C613 C113 C213 C713 177.9(4) . . . . ? C113 C213 C313 C413 3.3(6) . . . . ? C713 C213 C313 C413 -177.3(4) . . . . ? C213 C313 C413 C513 -1.8(7) . . . . ? C313 C413 C513 C613 -0.3(7) . . . . ? C413 C513 C613 C113 0.7(6) . . . . ? O113 C113 C613 C513 -176.8(3) . . . . ? C213 C113 C613 C513 0.9(6) . . . . ? O213 N113 C713 C213 175.0(3) . . . . ? O213 N113 C713 C813 -6.9(5) . . . . ? C313 C213 C713 N113 160.6(4) . . . . ? C113 C213 C713 N113 -20.1(6) . . . . ? C313 C213 C713 C813 -17.6(6) . . . . ? C113 C213 C713 C813 161.8(4) . . . . ? N113 C713 C813 C913 -86.8(5) . . . . ? C213 C713 C813 C913 91.3(5) . . . . ? O114 C114 C214 C314 -173.5(4) . . . . ? C614 C114 C214 C314 3.3(6) . . . . ? O114 C114 C214 C714 4.7(7) . . . . ? C614 C114 C214 C714 -178.5(4) . . . . ? C114 C214 C314 C414 -2.0(7) . . . . ? C714 C214 C314 C414 179.7(5) . . . . ? C214 C314 C414 C514 -0.5(8) . . . . ? C314 C414 C514 C614 1.8(7) . . . . ? O114 C114 C614 C514 174.8(4) . . . . ? C214 C114 C614 C514 -2.2(7) . . . . ? C414 C514 C614 C114 -0.4(7) . . . . ? O214 N114 C714 C214 179.1(4) . . . . ? O214 N114 C714 C814 -5.7(7) . . . . ? O214 N114 C714 C818 23.8(9) . . . . ? C314 C214 C714 N114 -161.4(4) . . . . ? C114 C214 C714 N114 20.3(7) . . . . ? C314 C214 C714 C814 23.3(7) . . . . ? C114 C214 C714 C814 -154.9(5) . . . . ? C314 C214 C714 C818 -7.7(9) . . . . ? C114 C214 C714 C818 174.1(8) . . . . ? N114 C714 C814 C914 85.0(6) . . . . ? C214 C714 C814 C914 -99.8(6) . . . . ? C818 C714 C814 C914 2(2) . . . . ? N114 C714 C818 C918 -108.5(14) . . . . ? C214 C714 C818 C918 96.7(15) . . . . ? C814 C714 C818 C918 2.7(14) . . . . ? O115 C115 C215 C315 -179.5(4) . . . . ? C615 C115 C215 C315 0.2(6) . . . . ? O115 C115 C215 C715 -1.4(6) . . . . ? C615 C115 C215 C715 178.3(4) . . . . ? C115 C215 C315 C415 -0.1(6) . . . . ? C715 C215 C315 C415 -178.2(4) . . . . ? C215 C315 C415 C515 0.4(7) . . . . ? C315 C415 C515 C615 -0.7(6) . . . . ? C415 C515 C615 C115 0.9(7) . . . . ? O115 C115 C615 C515 179.1(4) . . . . ? C215 C115 C615 C515 -0.6(6) . . . . ? O215 N115 C715 C215 -175.9(3) . . . . ? O215 N115 C715 C815 4.8(5) . . . . ? C315 C215 C715 N115 -155.6(4) . . . . ? C115 C215 C715 N115 26.4(6) . . . . ? C315 C215 C715 C815 23.7(6) . . . . ? C115 C215 C715 C815 -154.3(4) . . . . ? N115 C715 C815 C915 86.3(5) . . . . ? C215 C715 C815 C915 -93.0(5) . . . . ? O116 C116 C216 C316 -179.4(4) . . . . ? C616 C116 C216 C316 2.0(6) . . . . ? O116 C116 C216 C716 2.3(6) . . . . ? C616 C116 C216 C716 -176.4(4) . . . . ? C116 C216 C316 C416 -0.7(6) . . . . ? C716 C216 C316 C416 177.7(4) . . . . ? C216 C316 C416 C516 -1.7(7) . . . . ? C316 C416 C516 C616 2.8(7) . . . . ? C416 C516 C616 C116 -1.5(6) . . . . ? O116 C116 C616 C516 -179.6(4) . . . . ? C216 C116 C616 C516 -0.9(6) . . . . ? O216 N116 C716 C816 -0.5(5) . . . . ? O216 N116 C716 C216 -177.7(3) . . . . ? C316 C216 C716 N116 159.9(4) . . . . ? C116 C216 C716 N116 -21.8(6) . . . . ? C316 C216 C716 C816 -17.3(6) . . . . ? C116 C216 C716 C816 161.0(4) . . . . ? N116 C716 C816 C916 -79.4(5) . . . . ? C216 C716 C816 C916 97.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.672 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.069