# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? loop_ _publ_author_address _publ_author_footnote ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; ; ? # Address 2 ; ; ? # Footnote 2 ; _publ_contact_author_address ; School of Chemistry, University of Edinburgh, Joseph Black Building, King's Buildings, West Mains Road, Edinburgh, EH9 3JJ , UK. ; _publ_contact_author_email anna.collins@ed.ac.uk _publ_contact_author_fax '+44 131 000000' _publ_contact_author_phone '+44 131 650 4806' _publ_contact_author_name 'Anna Collins' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_section_title # Title of paper - generally just the systematic or trivial name ; ? ; _publ_author_name A.Collins data_EB7166 _database_code_depnum_ccdc_archive 'CCDC 636071' _audit_creation_date 07-05-16 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'eb6166 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.6159(3) _cell_length_b 13.0159(2) _cell_length_c 14.5850(3) _cell_angle_alpha 105.6790(10) _cell_angle_beta 92.6250(10) _cell_angle_gamma 105.1690(10) _cell_volume 2207.95(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 1 # Given Formula = C80 H108 Mn6 N8 O26 # Dc = 1.45 Fooo = 1000.00 Mu = 9.11 M = 963.67 # Found Formula = C82 H108 Mn6 N6 O26 # Dc = 1.45 FOOO = 1000.00 Mu = 9.10 M = 961.68 _chemical_formula_sum 'C82 H108 Mn6 N6 O26' _chemical_formula_moiety 'CC78 H96 Mn6 N6 O24, 2(C2 H6 O)' _chemical_compound_source ? _chemical_formula_weight 1923.35 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.910 # Sheldrick geometric approximatio 0.79 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.96 _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/2\q # 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 'SIR92 (Altomare et al., 1994)' _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 26717 _reflns_number_total 10575 _diffrn_reflns_av_R_equivalents 0.035 # Number of reflections with Friedels Law is 10575 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11761 _diffrn_reflns_theta_min 1.462 _diffrn_reflns_theta_max 29.017 _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.245 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -17 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 1.14 _oxford_diffrn_Wilson_scale 6.02 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.79 _refine_diff_density_max 1.47 _refine_ls_number_reflns 10575 _refine_ls_number_restraints 0 _refine_ls_number_parameters 541 #_refine_ls_R_factor_ref 0.0557 _refine_ls_wR_factor_ref 0.0903 _refine_ls_goodness_of_fit_ref 0.8854 #_reflns_number_all 10575 _refine_ls_R_factor_all 0.0557 _refine_ls_wR_factor_all 0.0903 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7795 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_gt 0.0867 _refine_ls_shift/su_max 0.001687 # 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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; The asymmetric unit contains half of the Mn6 complex. This comprises 6 manganese atoms, 3 nitrogen atoms, 12 oxygen atoms, 41 carbons and 48 hydrogens. These include 2 ethanol ligands and one water ligand. There is also one molecule of ethanol solvent per asymmetric unit. Large atomic motion is associated with the positions of ethyl chains. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. 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, N---H in the range 0.86--0.89 N---H to 0.86 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. 912_ALERT_3_A # Missing FCF Reflections Above STH/L=0.6 ...... 1145 The data is complete to Acta recommendations. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.999 4633 4630 3 23.01 0.550 0.998 6161 6148 13 25.24 0.600 0.996 7994 7961 33 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.987 10163 10028 135 29.02 0.683 0.900 11753 10575 1178 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.66 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.44 Ratio This is associated with a flexible ethyl chain that is likely to display atomic motion. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89 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. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 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. 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. 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 1.05036(2) 0.60763(2) 1.09418(2) 0.0138 1.0000 Uani . . . . . . Mn2 Mn 1.03900(2) 0.37577(2) 1.14599(2) 0.0146 1.0000 Uani . . . . . . Mn3 Mn 1.27711(2) 0.55320(3) 1.15385(2) 0.0148 1.0000 Uani . . . . . . O4 O 1.12170(11) 0.51596(11) 1.13672(10) 0.0149 1.0000 Uani . . . . . . O5 O 0.98839(11) 0.68787(11) 1.02436(10) 0.0158 1.0000 Uani . . . . . . C6 C 1.01024(17) 0.79951(17) 1.06368(15) 0.0169 1.0000 Uani . . . . . . C7 C 0.92544(18) 0.84816(18) 1.05601(16) 0.0200 1.0000 Uani . . . . . . C8 C 0.94290(19) 0.96125(18) 1.09383(17) 0.0234 1.0000 Uani . . . . . . C9 C 1.04579(19) 1.02868(18) 1.14103(17) 0.0245 1.0000 Uani . . . . . . C10 C 1.13093(18) 0.98168(18) 1.14719(17) 0.0230 1.0000 Uani . . . . . . C11 C 1.11681(17) 0.86701(17) 1.10878(15) 0.0175 1.0000 Uani . . . . . . C12 C 1.21249(17) 0.82263(17) 1.11258(15) 0.0179 1.0000 Uani . . . . . . N13 N 1.19776(14) 0.71929(14) 1.10840(12) 0.0159 1.0000 Uani . . . . . . O14 O 1.28876(11) 0.67994(12) 1.10607(11) 0.0181 1.0000 Uani . . . . . . C15 C 1.32704(19) 0.89750(19) 1.1158(2) 0.0302 1.0000 Uani . . . . . . C16 C 1.3432(3) 0.9252(3) 1.0221(3) 0.0621 1.0000 Uani . . . . . . O17 O 0.94518(12) 0.24490(12) 1.16032(11) 0.0189 1.0000 Uani . . . . . . C18 C 0.86430(17) 0.24774(17) 1.21616(15) 0.0181 1.0000 Uani . . . . . . C19 C 0.83828(19) 0.16735(18) 1.26530(17) 0.0246 1.0000 Uani . . . . . . C20 C 0.7568(2) 0.1655(2) 1.32513(19) 0.0322 1.0000 Uani . . . . . . C21 C 0.6984(2) 0.2436(2) 1.33760(19) 0.0328 1.0000 Uani . . . . . . C22 C 0.72153(19) 0.3226(2) 1.28948(17) 0.0256 1.0000 Uani . . . . . . C23 C 0.80401(17) 0.32776(17) 1.22776(15) 0.0184 1.0000 Uani . . . . . . C24 C 0.81944(17) 0.40961(17) 1.17380(15) 0.0172 1.0000 Uani . . . . . . N25 N 0.90464(13) 0.42366(14) 1.12748(12) 0.0149 1.0000 Uani . . . . . . O26 O 0.91192(11) 0.48943(11) 1.06544(10) 0.0156 1.0000 Uani . . . . . . C27 C 0.73623(17) 0.47389(19) 1.17205(16) 0.0217 1.0000 Uani . . . . . . C28 C 0.62699(19) 0.4026(2) 1.11057(17) 0.0297 1.0000 Uani . . . . . . O29 O 1.43250(11) 0.58653(12) 1.17631(11) 0.0191 1.0000 Uani . . . . . . C30 C 1.48387(16) 0.57759(17) 1.25501(15) 0.0179 1.0000 Uani . . . . . . C31 C 1.58491(17) 0.65599(18) 1.29670(17) 0.0227 1.0000 Uani . . . . . . C32 C 1.64517(19) 0.6501(2) 1.37570(17) 0.0271 1.0000 Uani . . . . . . C33 C 1.60516(19) 0.5641(2) 1.41519(17) 0.0267 1.0000 Uani . . . . . . C34 C 1.50560(18) 0.4854(2) 1.37525(17) 0.0256 1.0000 Uani . . . . . . C35 C 1.44208(17) 0.48979(18) 1.29548(16) 0.0200 1.0000 Uani . . . . . . C36 C 1.33743(18) 0.40226(18) 1.25681(16) 0.0219 1.0000 Uani . . . . . . N37 N 1.26372(14) 0.41895(14) 1.20235(12) 0.0167 1.0000 Uani . . . . . . O38 O 1.17022(11) 0.33212(12) 1.16459(11) 0.0192 1.0000 Uani . . . . . . C39 C 1.3138(2) 0.2944(2) 1.2836(2) 0.0373 1.0000 Uani . . . 1 1 . C40 C 1.3885(2) 0.2266(2) 1.2424(2) 0.0484 1.0000 Uani . . . 1 1 . O41 O 1.00091(12) 0.69368(12) 1.22322(11) 0.0222 1.0000 Uani . . . . . . C42 C 1.01990(17) 0.71345(17) 1.31288(16) 0.0188 1.0000 Uani . . . . . . O43 O 1.08462(13) 0.67686(13) 1.35513(11) 0.0249 1.0000 Uani . . . . . . C44 C 0.95933(17) 0.78619(17) 1.37447(16) 0.0191 1.0000 Uani . . . . . . C45 C 0.89903(19) 0.84238(19) 1.33527(17) 0.0255 1.0000 Uani . . . . . . C46 C 0.8438(2) 0.9091(2) 1.39347(19) 0.0309 1.0000 Uani . . . . . . C47 C 0.8476(2) 0.9209(2) 1.49072(18) 0.0295 1.0000 Uani . . . . . . C48 C 0.9083(2) 0.8652(2) 1.52922(18) 0.0299 1.0000 Uani . . . . . . C49 C 0.96480(19) 0.79857(19) 1.47224(16) 0.0257 1.0000 Uani . . . . . . C50 C 0.7850(2) 0.9919(2) 1.5534(2) 0.0464 1.0000 Uani . . . . . . O51 O 1.28266(12) 0.66613(12) 1.30194(11) 0.0226 1.0000 Uani . . . . . . C52 C 1.3541(2) 0.7783(2) 1.33166(18) 0.0302 1.0000 Uani . . . . . . C53 C 1.4000(3) 0.8128(3) 1.4352(2) 0.0476 1.0000 Uani . . . . . . O54 O 1.05426(13) 0.45635(12) 1.30348(11) 0.0232 1.0000 Uani . . . . . . C55 C 1.0640(2) 0.4146(2) 1.38354(17) 0.0293 1.0000 Uani . . . . . . C56 C 1.1576(2) 0.4905(2) 1.45779(19) 0.0403 1.0000 Uani . . . . . . O57 O 0.40757(14) 0.32013(14) 0.93099(13) 0.0347 1.0000 Uani . . . . . . C58 C 0.4062(2) 0.2137(2) 0.9404(2) 0.0365 1.0000 Uani . . . . . . C59 C 0.3666(2) 0.1224(2) 0.8481(2) 0.0425 1.0000 Uani . . . . . . O60 O 1.26948(12) 0.43408(12) 1.01279(11) 0.0234 1.0000 Uani . . . . . . H71 H 0.8596 0.8053 1.0236 0.0236 1.0000 Uiso R . . . . . H81 H 0.8853 0.9921 1.0871 0.0289 1.0000 Uiso R . . . . . H91 H 1.0602 1.1067 1.1675 0.0292 1.0000 Uiso R . . . . . H101 H 1.1975 1.0274 1.1786 0.0258 1.0000 Uiso R . . . . . H151 H 1.3400 0.9635 1.1700 0.0372 1.0000 Uiso R . . . . . H152 H 1.3824 0.8615 1.1298 0.0365 1.0000 Uiso R . . . . . H161 H 1.4171 0.9751 1.0266 0.1039 1.0000 Uiso R . . . . . H162 H 1.2894 0.9581 1.0061 0.1048 1.0000 Uiso R . . . . . H163 H 1.3379 0.8579 0.9708 0.1041 1.0000 Uiso R . . . . . H191 H 0.8767 0.1169 1.2565 0.0312 1.0000 Uiso R . . . . . H201 H 0.7391 0.1118 1.3580 0.0424 1.0000 Uiso R . . . . . H211 H 0.6431 0.2428 1.3781 0.0441 1.0000 Uiso R . . . . . H221 H 0.6810 0.3746 1.2973 0.0325 1.0000 Uiso R . . . . . H271 H 0.7248 0.5043 1.2381 0.0274 1.0000 Uiso R . . . . . H272 H 0.7675 0.5360 1.1485 0.0274 1.0000 Uiso R . . . . . H281 H 0.5793 0.4487 1.1095 0.0468 1.0000 Uiso R . . . . . H282 H 0.5905 0.3427 1.1364 0.0454 1.0000 Uiso R . . . . . H283 H 0.6376 0.3695 1.0442 0.0453 1.0000 Uiso R . . . . . H311 H 1.6106 0.7123 1.2702 0.0271 1.0000 Uiso R . . . . . H321 H 1.7107 0.7037 1.4018 0.0304 1.0000 Uiso R . . . . . H331 H 1.6420 0.5603 1.4677 0.0319 1.0000 Uiso R . . . . . H341 H 1.4775 0.4288 1.4038 0.0319 1.0000 Uiso R . . . . . H391 H 1.3185 0.3012 1.3537 0.0465 1.0000 Uiso R . . 1 1 . H392 H 1.2384 0.2499 1.2706 0.0439 1.0000 Uiso R . . 1 1 . H401 H 1.3728 0.1589 1.2678 0.0714 1.0000 Uiso R . . 1 1 . H402 H 1.4673 0.2738 1.2636 0.0720 1.0000 Uiso R . . 1 1 . H403 H 1.3687 0.2042 1.1696 0.0717 1.0000 Uiso R . . 1 1 . H451 H 0.8971 0.8346 1.2710 0.0309 1.0000 Uiso R . . . . . H461 H 0.8017 0.9452 1.3668 0.0383 1.0000 Uiso R . . . . . H481 H 0.9101 0.8718 1.5931 0.0331 1.0000 Uiso R . . . . . H491 H 1.0058 0.7607 1.4997 0.0318 1.0000 Uiso R . . . . . H501 H 0.8091 1.0086 1.6202 0.0672 1.0000 Uiso R . . . . . H502 H 0.7952 1.0600 1.5394 0.0669 1.0000 Uiso R . . . . . H503 H 0.7090 0.9534 1.5408 0.0667 1.0000 Uiso R . . . . . H521 H 1.4157 0.7815 1.2911 0.0340 1.0000 Uiso R . . . . . H522 H 1.3130 0.8289 1.3199 0.0332 1.0000 Uiso R . . . . . H531 H 1.4488 0.8886 1.4524 0.0671 1.0000 Uiso R . . . . . H532 H 1.4413 0.7619 1.4434 0.0658 1.0000 Uiso R . . . . . H533 H 1.3398 0.8093 1.4745 0.0658 1.0000 Uiso R . . . . . H551 H 1.0777 0.3419 1.3581 0.0361 1.0000 Uiso R . . . . . H552 H 0.9957 0.4035 1.4117 0.0370 1.0000 Uiso R . . . . . H561 H 1.1611 0.4589 1.5109 0.0616 1.0000 Uiso R . . . . . H562 H 1.2287 0.5005 1.4326 0.0612 1.0000 Uiso R . . . . . H563 H 1.1432 0.5651 1.4824 0.0601 1.0000 Uiso R . . . . . H581 H 0.4803 0.2168 0.9653 0.0454 1.0000 Uiso R . . . . . H582 H 0.3591 0.1991 0.9876 0.0459 1.0000 Uiso R . . . . . H591 H 0.3578 0.0513 0.8604 0.0628 1.0000 Uiso R . . . . . H592 H 0.4203 0.1322 0.8010 0.0615 1.0000 Uiso R . . . . . H593 H 0.2966 0.1257 0.8232 0.0618 1.0000 Uiso R . . . . . H9 H 1.0582 0.5217 1.3239 0.0331 1.0000 Uiso R . . . . . H19 H 0.4601 0.3463 0.9052 0.0538 1.0000 Uiso R . . . . . H28 H 1.2237 0.6686 1.3139 0.0324 1.0000 Uiso R . . . . . H40 H 1.3092 0.4000 0.9892 0.0349 1.0000 Uiso R . . . . . H58 H 1.2054 0.4041 0.9887 0.0348 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 0.01178(15) 0.01303(15) 0.01660(16) 0.00449(12) -0.00003(12) 0.00386(12) Mn2 0.01157(15) 0.01407(15) 0.01886(17) 0.00585(13) 0.00066(12) 0.00378(12) Mn3 0.01110(15) 0.01496(16) 0.01894(17) 0.00561(13) 0.00050(12) 0.00424(12) O4 0.0119(7) 0.0151(7) 0.0186(7) 0.0062(6) 0.0007(6) 0.0043(6) O5 0.0181(7) 0.0130(7) 0.0157(7) 0.0031(6) -0.0013(6) 0.0051(6) C6 0.0209(11) 0.0154(10) 0.0151(10) 0.0049(8) 0.0026(8) 0.0056(8) C7 0.0179(10) 0.0210(11) 0.0213(11) 0.0055(9) 0.0003(9) 0.0069(9) C8 0.0235(11) 0.0225(11) 0.0271(12) 0.0063(10) 0.0026(9) 0.0127(10) C9 0.0298(13) 0.0139(10) 0.0288(13) 0.0030(9) 0.0021(10) 0.0084(9) C10 0.0199(11) 0.0159(11) 0.0300(13) 0.0043(9) -0.0004(9) 0.0028(9) C11 0.0166(10) 0.0158(10) 0.0210(11) 0.0060(9) 0.0033(8) 0.0052(8) C12 0.0153(10) 0.0164(10) 0.0207(11) 0.0037(9) 0.0018(8) 0.0043(8) N13 0.0142(8) 0.0165(9) 0.0172(9) 0.0039(7) 0.0018(7) 0.0058(7) O14 0.0134(7) 0.0191(7) 0.0257(8) 0.0090(6) 0.0048(6) 0.0083(6) C15 0.0182(11) 0.0185(11) 0.0549(17) 0.0124(11) 0.0039(11) 0.0056(9) C16 0.0367(17) 0.079(2) 0.095(3) 0.062(2) 0.0321(18) 0.0156(17) O17 0.0170(7) 0.0155(7) 0.0264(8) 0.0081(6) 0.0074(6) 0.0054(6) C18 0.0157(10) 0.0186(11) 0.0190(11) 0.0064(9) 0.0020(8) 0.0025(8) C19 0.0272(12) 0.0213(11) 0.0302(13) 0.0118(10) 0.0066(10) 0.0099(10) C20 0.0376(14) 0.0320(14) 0.0374(15) 0.0216(12) 0.0164(12) 0.0134(11) C21 0.0318(14) 0.0414(15) 0.0363(15) 0.0223(12) 0.0192(11) 0.0152(12) C22 0.0262(12) 0.0318(13) 0.0258(12) 0.0128(10) 0.0086(10) 0.0145(10) C23 0.0178(10) 0.0187(10) 0.0181(11) 0.0054(9) 0.0015(8) 0.0042(9) C24 0.0152(10) 0.0161(10) 0.0182(11) 0.0026(8) -0.0015(8) 0.0038(8) N25 0.0131(8) 0.0142(8) 0.0176(9) 0.0061(7) -0.0001(7) 0.0032(7) O26 0.0145(7) 0.0164(7) 0.0172(7) 0.0078(6) 0.0004(6) 0.0038(6) C27 0.0206(11) 0.0266(12) 0.0239(12) 0.0109(10) 0.0076(9) 0.0125(9) C28 0.0205(12) 0.0449(15) 0.0276(13) 0.0126(11) 0.0052(10) 0.0136(11) O29 0.0120(7) 0.0230(8) 0.0243(8) 0.0093(7) 0.0010(6) 0.0062(6) C30 0.0132(10) 0.0202(11) 0.0206(11) 0.0031(9) 0.0018(8) 0.0081(8) C31 0.0165(11) 0.0214(11) 0.0296(13) 0.0066(10) 0.0022(9) 0.0053(9) C32 0.0185(11) 0.0271(12) 0.0280(13) -0.0010(10) -0.0040(9) 0.0041(10) C33 0.0214(12) 0.0375(14) 0.0205(12) 0.0070(10) -0.0047(9) 0.0098(10) C34 0.0203(11) 0.0311(13) 0.0279(13) 0.0130(11) 0.0012(10) 0.0072(10) C35 0.0158(10) 0.0208(11) 0.0225(12) 0.0049(9) -0.0010(9) 0.0055(9) C36 0.0188(11) 0.0215(11) 0.0267(12) 0.0101(10) -0.0024(9) 0.0058(9) N37 0.0129(8) 0.0156(9) 0.0209(9) 0.0049(7) 0.0018(7) 0.0032(7) O38 0.0124(7) 0.0151(7) 0.0276(8) 0.0051(6) -0.0024(6) 0.0020(6) C39 0.0252(13) 0.0313(14) 0.0555(18) 0.0215(13) -0.0148(12) 0.0024(11) C40 0.0444(17) 0.0330(15) 0.065(2) 0.0125(15) -0.0007(15) 0.0098(13) O41 0.0256(8) 0.0228(8) 0.0192(8) 0.0041(7) 0.0044(6) 0.0102(7) C42 0.0175(10) 0.0131(10) 0.0235(12) 0.0036(9) 0.0033(9) 0.0020(8) O43 0.0265(9) 0.0264(9) 0.0250(9) 0.0063(7) 0.0037(7) 0.0142(7) C44 0.0174(10) 0.0143(10) 0.0217(11) 0.0014(9) 0.0045(9) 0.0017(8) C45 0.0286(12) 0.0234(12) 0.0258(13) 0.0065(10) 0.0057(10) 0.0097(10) C46 0.0273(13) 0.0256(13) 0.0438(16) 0.0113(11) 0.0056(11) 0.0132(11) C47 0.0224(12) 0.0237(12) 0.0366(14) -0.0015(11) 0.0106(10) 0.0066(10) C48 0.0277(13) 0.0334(14) 0.0218(12) -0.0005(10) 0.0062(10) 0.0057(11) C49 0.0252(12) 0.0275(12) 0.0235(12) 0.0057(10) 0.0025(10) 0.0080(10) C50 0.0376(16) 0.0386(16) 0.057(2) -0.0023(14) 0.0177(14) 0.0147(13) O51 0.0174(8) 0.0219(8) 0.0261(9) 0.0034(7) 0.0034(6) 0.0052(6) C52 0.0310(13) 0.0257(13) 0.0292(13) 0.0022(10) 0.0039(11) 0.0060(11) C53 0.0488(18) 0.0467(18) 0.0363(17) -0.0011(14) -0.0052(14) 0.0102(15) O54 0.0318(9) 0.0184(8) 0.0192(8) 0.0056(6) -0.0006(7) 0.0076(7) C55 0.0341(14) 0.0343(14) 0.0225(12) 0.0137(11) 0.0026(10) 0.0096(11) C56 0.0404(16) 0.0565(18) 0.0264(14) 0.0156(13) -0.0048(12) 0.0157(14) O57 0.0279(9) 0.0352(10) 0.0458(11) 0.0131(9) 0.0169(8) 0.0133(8) C58 0.0298(14) 0.0427(16) 0.0396(16) 0.0153(13) 0.0069(12) 0.0109(12) C59 0.0441(17) 0.0342(15) 0.0457(18) 0.0129(13) 0.0012(13) 0.0048(13) O60 0.0196(8) 0.0276(8) 0.0228(8) 0.0029(7) 0.0017(6) 0.0114(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4169(3) 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 . O26 2_767 2.4634(14) yes Mn1 . Mn1 2_767 3.2662(6) yes Mn1 . Mn2 . 3.2734(4) yes Mn1 . Mn3 . 3.2571(4) yes Mn1 . O4 . 1.8788(13) yes Mn1 . O5 . 1.9151(14) yes Mn1 . N13 . 2.0002(17) yes Mn1 . O26 . 1.9419(14) yes Mn1 . O41 . 2.1260(15) yes Mn2 . O5 2_767 2.3743(14) yes Mn2 . Mn3 . 3.2504(4) yes Mn2 . O4 . 1.8937(14) yes Mn2 . O17 . 1.8724(14) yes Mn2 . N25 . 1.9840(16) yes Mn2 . O38 . 1.9161(14) yes Mn2 . O54 . 2.2283(15) yes Mn3 . O4 . 1.8798(13) yes Mn3 . O14 . 1.9319(14) yes Mn3 . O29 . 1.8863(14) yes Mn3 . N37 . 2.0266(17) yes Mn3 . O51 . 2.2465(15) yes Mn3 . O60 . 2.1968(15) yes O5 . C6 . 1.357(2) yes C6 . C7 . 1.393(3) yes C6 . C11 . 1.414(3) yes C7 . C8 . 1.378(3) yes C7 . H71 . 0.897 no C8 . C9 . 1.387(3) yes C8 . H81 . 0.931 no C9 . C10 . 1.379(3) yes C9 . H91 . 0.948 no C10 . C11 . 1.405(3) yes C10 . H101 . 0.908 no C11 . C12 . 1.473(3) yes C12 . N13 . 1.293(3) yes C12 . C15 . 1.508(3) yes N13 . O14 . 1.372(2) yes C15 . C16 . 1.513(4) yes C15 . H151 . 0.968 no C15 . H152 . 0.979 no C16 . H161 . 0.975 no C16 . H162 . 0.944 no C16 . H163 . 0.971 no O17 . C18 . 1.336(2) yes C18 . C19 . 1.401(3) yes C18 . C23 . 1.422(3) yes C19 . C20 . 1.378(3) yes C19 . H191 . 0.899 no C20 . C21 . 1.383(3) yes C20 . H201 . 0.936 no C21 . C22 . 1.374(3) yes C21 . H211 . 0.934 no C22 . C23 . 1.407(3) yes C22 . H221 . 0.937 no C23 . C24 . 1.467(3) yes C24 . N25 . 1.295(3) yes C24 . C27 . 1.507(3) yes N25 . O26 . 1.395(2) yes C27 . C28 . 1.527(3) yes C27 . H271 . 0.970 no C27 . H272 . 0.961 no C28 . H281 . 0.957 no C28 . H282 . 0.973 no C28 . H283 . 0.979 no O29 . C30 . 1.340(2) yes C30 . C31 . 1.396(3) yes C30 . C35 . 1.418(3) yes C31 . C32 . 1.382(3) yes C31 . H311 . 0.912 no C32 . C33 . 1.385(3) yes C32 . H321 . 0.917 no C33 . C34 . 1.379(3) yes C33 . H331 . 0.897 no C34 . C35 . 1.405(3) yes C34 . H341 . 0.941 no C35 . C36 . 1.468(3) yes C36 . N37 . 1.294(3) yes C36 . C39 . 1.516(3) yes N37 . O38 . 1.371(2) yes C39 . C40 . 1.493(4) yes C39 . H391 . 1.000 no C39 . H392 . 0.956 no C40 . H401 . 1.023 no C40 . H402 . 1.006 no C40 . H403 . 1.022 no O41 . C42 . 1.261(3) yes C42 . O43 . 1.261(3) yes C42 . C44 . 1.506(3) yes C44 . C45 . 1.385(3) yes C44 . C49 . 1.387(3) yes C45 . C46 . 1.390(3) yes C45 . H451 . 0.914 no C46 . C47 . 1.382(4) yes C46 . H461 . 0.930 no C47 . C48 . 1.378(4) yes C47 . C50 . 1.518(3) yes C48 . C49 . 1.393(3) yes C48 . H481 . 0.911 no C49 . H491 . 0.945 no C50 . H501 . 0.955 no C50 . H502 . 0.940 no C50 . H503 . 0.942 no O51 . C52 . 1.437(3) yes O51 . H28 . 0.778 no C52 . C53 . 1.494(4) yes C52 . H521 . 0.997 no C52 . H522 . 0.981 no C53 . H531 . 0.975 no C53 . H532 . 0.972 no C53 . H533 . 0.972 no O54 . C55 . 1.428(3) yes O54 . H9 . 0.809 no C55 . C56 . 1.496(3) yes C55 . H551 . 0.983 no C55 . H552 . 0.965 no C56 . H561 . 0.975 no C56 . H562 . 0.976 no C56 . H563 . 1.007 no O57 . C58 . 1.424(3) yes O57 . H19 . 0.818 no C58 . C59 . 1.496(4) yes C58 . H581 . 0.974 no C58 . H582 . 0.955 no C59 . H591 . 0.969 no C59 . H592 . 0.997 no C59 . H593 . 0.956 no O60 . H40 . 0.785 no O60 . H58 . 0.815 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 O26 2_767 Mn1 . Mn1 2_767 36.32(3) yes O26 2_767 Mn1 . Mn2 . 85.44(3) yes Mn1 2_767 Mn1 . Mn2 . 69.118(11) yes O26 2_767 Mn1 . Mn3 . 79.94(3) yes Mn1 2_767 Mn1 . Mn3 . 98.843(13) yes Mn2 . Mn1 . Mn3 . 59.699(9) yes O26 2_767 Mn1 . O4 . 84.03(5) yes Mn1 2_767 Mn1 . O4 . 85.41(4) yes Mn2 . Mn1 . O4 . 29.94(4) yes Mn3 . Mn1 . O4 . 29.95(4) yes O26 2_767 Mn1 . O5 . 83.44(5) yes Mn1 2_767 Mn1 . O5 . 85.55(4) yes Mn2 . Mn1 . O5 . 149.66(4) yes Mn3 . Mn1 . O5 . 144.29(4) yes O4 . Mn1 . O5 . 167.35(6) yes O26 2_767 Mn1 . N13 . 87.92(6) yes Mn1 2_767 Mn1 . N13 . 124.24(5) yes Mn2 . Mn1 . N13 . 118.89(5) yes Mn3 . Mn1 . N13 . 59.32(5) yes O4 . Mn1 . N13 . 88.96(6) yes O26 2_767 Mn1 . O26 . 85.03(5) yes Mn1 2_767 Mn1 . O26 . 48.71(4) yes Mn2 . Mn1 . O26 . 60.09(4) yes Mn3 . Mn1 . O26 . 118.70(4) yes O4 . Mn1 . O26 . 89.84(6) yes O26 2_767 Mn1 . O41 . 173.11(5) yes Mn1 2_767 Mn1 . O41 . 139.92(4) yes Mn2 . Mn1 . O41 . 98.09(4) yes Mn3 . Mn1 . O41 . 106.95(4) yes O4 . Mn1 . O41 . 101.99(6) yes O5 . Mn1 . N13 . 88.84(6) yes O5 . Mn1 . O26 . 90.83(6) yes N13 . Mn1 . O26 . 172.93(7) yes O5 . Mn1 . O41 . 90.62(6) yes N13 . Mn1 . O41 . 95.48(6) yes O26 . Mn1 . O41 . 91.58(6) yes O5 2_767 Mn2 . Mn1 . 78.92(3) yes O5 2_767 Mn2 . Mn3 . 93.39(3) yes Mn1 . Mn2 . Mn3 . 59.901(9) yes O5 2_767 Mn2 . O4 . 87.88(5) yes Mn1 . Mn2 . O4 . 29.68(4) yes Mn3 . Mn2 . O4 . 30.40(4) yes O5 2_767 Mn2 . O17 . 94.36(6) yes Mn1 . Mn2 . O17 . 145.16(5) yes Mn3 . Mn2 . O17 . 154.90(5) yes O4 . Mn2 . O17 . 173.59(6) yes O5 2_767 Mn2 . N25 . 82.80(6) yes Mn1 . Mn2 . N25 . 57.94(5) yes Mn3 . Mn2 . N25 . 117.26(5) yes O4 . Mn2 . N25 . 86.91(6) yes O17 . Mn2 . N25 . 87.41(6) yes O5 2_767 Mn2 . O38 . 97.53(6) yes Mn1 . Mn2 . O38 . 121.21(4) yes Mn3 . Mn2 . O38 . 61.83(4) yes O4 . Mn2 . O38 . 92.19(6) yes O17 . Mn2 . O38 . 93.47(6) yes O5 2_767 Mn2 . O54 . 171.25(5) yes Mn1 . Mn2 . O54 . 93.16(4) yes Mn3 . Mn2 . O54 . 85.73(4) yes O4 . Mn2 . O54 . 86.98(6) yes O17 . Mn2 . O54 . 90.04(6) yes N25 . Mn2 . O38 . 179.03(7) yes N25 . Mn2 . O54 . 89.85(6) yes O38 . Mn2 . O54 . 89.74(6) yes Mn2 . Mn3 . Mn1 . 60.400(9) yes Mn2 . Mn3 . O4 . 30.65(4) yes Mn1 . Mn3 . O4 . 29.93(4) yes Mn2 . Mn3 . O14 . 121.32(4) yes Mn1 . Mn3 . O14 . 61.54(4) yes O4 . Mn3 . O14 . 91.41(6) yes Mn2 . Mn3 . O29 . 146.79(5) yes Mn1 . Mn3 . O29 . 152.80(5) yes O4 . Mn3 . O29 . 176.85(6) yes O14 . Mn3 . O29 . 91.44(6) yes Mn2 . Mn3 . N37 . 58.21(5) yes Mn1 . Mn3 . N37 . 118.09(5) yes O4 . Mn3 . N37 . 88.20(6) yes O14 . Mn3 . N37 . 179.26(7) yes O29 . Mn3 . N37 . 88.97(6) yes Mn2 . Mn3 . O51 . 97.58(4) yes Mn1 . Mn3 . O51 . 87.92(4) yes O4 . Mn3 . O51 . 90.67(6) yes O14 . Mn3 . O51 . 88.09(6) yes O29 . Mn3 . O51 . 88.07(6) yes Mn2 . Mn3 . O60 . 80.22(4) yes Mn1 . Mn3 . O60 . 93.36(4) yes O4 . Mn3 . O60 . 88.80(6) yes O14 . Mn3 . O60 . 95.42(6) yes O29 . Mn3 . O60 . 92.27(6) yes N37 . Mn3 . O51 . 92.54(6) yes N37 . Mn3 . O60 . 83.94(6) yes O51 . Mn3 . O60 . 176.46(6) yes Mn2 . O4 . Mn3 . 118.94(7) yes Mn2 . O4 . Mn1 . 120.38(7) yes Mn3 . O4 . Mn1 . 120.12(7) yes Mn2 2_767 O5 . Mn1 . 119.34(6) yes Mn2 2_767 O5 . C6 . 115.52(12) yes Mn1 . O5 . C6 . 117.78(12) yes O5 . C6 . C7 . 118.35(19) yes O5 . C6 . C11 . 121.81(18) yes C7 . C6 . C11 . 119.81(19) yes C6 . C7 . C8 . 121.0(2) yes C6 . C7 . H71 . 119.0 no C8 . C7 . H71 . 119.9 no C7 . C8 . C9 . 120.2(2) yes C7 . C8 . H81 . 119.5 no C9 . C8 . H81 . 120.3 no C8 . C9 . C10 . 119.2(2) yes C8 . C9 . H91 . 122.0 no C10 . C9 . H91 . 118.8 no C9 . C10 . C11 . 122.3(2) yes C9 . C10 . H101 . 117.7 no C11 . C10 . H101 . 120.0 no C6 . C11 . C10 . 117.43(19) yes C6 . C11 . C12 . 122.75(18) yes C10 . C11 . C12 . 119.76(19) yes C11 . C12 . N13 . 120.29(19) yes C11 . C12 . C15 . 119.13(18) yes N13 . C12 . C15 . 120.49(18) yes Mn1 . N13 . C12 . 124.96(14) yes Mn1 . N13 . O14 . 116.62(12) yes C12 . N13 . O14 . 118.22(17) yes N13 . O14 . Mn3 . 116.26(11) yes C12 . C15 . C16 . 111.5(2) yes C12 . C15 . H151 . 108.9 no C16 . C15 . H151 . 112.3 no C12 . C15 . H152 . 109.7 no C16 . C15 . H152 . 109.6 no H151 . C15 . H152 . 104.5 no C15 . C16 . H161 . 109.9 no C15 . C16 . H162 . 111.2 no H161 . C16 . H162 . 109.9 no C15 . C16 . H163 . 109.8 no H161 . C16 . H163 . 106.9 no H162 . C16 . H163 . 108.9 no Mn2 . O17 . C18 . 121.26(13) yes O17 . C18 . C19 . 117.79(19) yes O17 . C18 . C23 . 123.29(18) yes C19 . C18 . C23 . 118.93(19) yes C18 . C19 . C20 . 121.3(2) yes C18 . C19 . H191 . 117.7 no C20 . C19 . H191 . 121.1 no C19 . C20 . C21 . 120.2(2) yes C19 . C20 . H201 . 121.5 no C21 . C20 . H201 . 118.3 no C20 . C21 . C22 . 119.7(2) yes C20 . C21 . H211 . 120.7 no C22 . C21 . H211 . 119.7 no C21 . C22 . C23 . 122.1(2) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 118.5 no C18 . C23 . C22 . 117.80(19) yes C18 . C23 . C24 . 122.85(19) yes C22 . C23 . C24 . 119.24(19) yes C23 . C24 . N25 . 118.46(18) yes C23 . C24 . C27 . 120.00(18) yes N25 . C24 . C27 . 121.54(19) yes Mn2 . N25 . C24 . 126.62(14) yes Mn2 . N25 . O26 . 114.17(11) yes C24 . N25 . O26 . 118.80(16) yes N25 . O26 . Mn1 2_767 111.36(10) yes N25 . O26 . Mn1 . 112.12(10) yes Mn1 2_767 O26 . Mn1 . 94.97(5) yes C24 . C27 . C28 . 112.79(19) yes C24 . C27 . H271 . 107.0 no C28 . C27 . H271 . 111.0 no C24 . C27 . H272 . 109.1 no C28 . C27 . H272 . 109.7 no H271 . C27 . H272 . 107.0 no C27 . C28 . H281 . 108.8 no C27 . C28 . H282 . 111.2 no H281 . C28 . H282 . 108.9 no C27 . C28 . H283 . 111.9 no H281 . C28 . H283 . 107.7 no H282 . C28 . H283 . 108.2 no Mn3 . O29 . C30 . 122.16(13) yes O29 . C30 . C31 . 118.37(19) yes O29 . C30 . C35 . 122.84(18) yes C31 . C30 . C35 . 118.76(19) yes C30 . C31 . C32 . 121.9(2) yes C30 . C31 . H311 . 117.8 no C32 . C31 . H311 . 120.2 no C31 . C32 . C33 . 119.6(2) yes C31 . C32 . H321 . 119.6 no C33 . C32 . H321 . 120.9 no C32 . C33 . C34 . 119.6(2) yes C32 . C33 . H331 . 120.8 no C34 . C33 . H331 . 119.6 no C33 . C34 . C35 . 122.1(2) yes C33 . C34 . H341 . 119.3 no C35 . C34 . H341 . 118.6 no C30 . C35 . C34 . 118.0(2) yes C30 . C35 . C36 . 123.29(19) yes C34 . C35 . C36 . 118.7(2) yes C35 . C36 . N37 . 119.74(19) yes C35 . C36 . C39 . 120.24(19) yes N37 . C36 . C39 . 120.0(2) yes Mn3 . N37 . C36 . 127.40(15) yes Mn3 . N37 . O38 . 115.26(12) yes C36 . N37 . O38 . 116.97(17) yes N37 . O38 . Mn2 . 114.55(11) yes C36 . C39 . C40 . 111.8(2) yes C36 . C39 . H391 . 116.5 no C40 . C39 . H391 . 106.7 no C36 . C39 . H392 . 115.9 no C40 . C39 . H392 . 110.8 no H391 . C39 . H392 . 93.6 no C39 . C40 . H401 . 107.7 no C39 . C40 . H402 . 108.4 no H401 . C40 . H402 . 110.8 no C39 . C40 . H403 . 105.7 no H401 . C40 . H403 . 111.9 no H402 . C40 . H403 . 112.1 no Mn1 . O41 . C42 . 140.25(14) yes O41 . C42 . O43 . 125.5(2) yes O41 . C42 . C44 . 117.12(19) yes O43 . C42 . C44 . 117.37(19) yes C42 . C44 . C45 . 121.0(2) yes C42 . C44 . C49 . 119.8(2) yes C45 . C44 . C49 . 119.2(2) yes C44 . C45 . C46 . 120.0(2) yes C44 . C45 . H451 . 118.4 no C46 . C45 . H451 . 121.6 no C45 . C46 . C47 . 121.3(2) yes C45 . C46 . H461 . 120.1 no C47 . C46 . H461 . 118.7 no C46 . C47 . C48 . 118.3(2) yes C46 . C47 . C50 . 120.9(2) yes C48 . C47 . C50 . 120.7(2) yes C47 . C48 . C49 . 121.3(2) yes C47 . C48 . H481 . 118.7 no C49 . C48 . H481 . 120.0 no C48 . C49 . C44 . 119.9(2) yes C48 . C49 . H491 . 120.2 no C44 . C49 . H491 . 119.8 no C47 . C50 . H501 . 112.3 no C47 . C50 . H502 . 110.6 no H501 . C50 . H502 . 107.4 no C47 . C50 . H503 . 108.7 no H501 . C50 . H503 . 109.2 no H502 . C50 . H503 . 108.6 no Mn3 . O51 . C52 . 120.87(13) yes Mn3 . O51 . H28 . 111.6 no C52 . O51 . H28 . 107.5 no O51 . C52 . C53 . 111.4(2) yes O51 . C52 . H521 . 107.7 no C53 . C52 . H521 . 109.9 no O51 . C52 . H522 . 109.5 no C53 . C52 . H522 . 110.3 no H521 . C52 . H522 . 108.1 no C52 . C53 . H531 . 109.0 no C52 . C53 . H532 . 107.7 no H531 . C53 . H532 . 110.2 no C52 . C53 . H533 . 109.6 no H531 . C53 . H533 . 109.9 no H532 . C53 . H533 . 110.3 no Mn2 . O54 . C55 . 131.62(14) yes Mn2 . O54 . H9 . 120.3 no C55 . O54 . H9 . 108.0 no O54 . C55 . C56 . 111.6(2) yes O54 . C55 . H551 . 106.4 no C56 . C55 . H551 . 109.8 no O54 . C55 . H552 . 110.6 no C56 . C55 . H552 . 110.0 no H551 . C55 . H552 . 108.4 no C55 . C56 . H561 . 108.7 no C55 . C56 . H562 . 112.3 no H561 . C56 . H562 . 108.5 no C55 . C56 . H563 . 109.0 no H561 . C56 . H563 . 108.9 no H562 . C56 . H563 . 109.3 no C58 . O57 . H19 . 112.7 no O57 . C58 . C59 . 112.8(2) yes O57 . C58 . H581 . 108.8 no C59 . C58 . H581 . 110.6 no O57 . C58 . H582 . 108.0 no C59 . C58 . H582 . 109.7 no H581 . C58 . H582 . 106.7 no C58 . C59 . H591 . 109.3 no C58 . C59 . H592 . 110.2 no H591 . C59 . H592 . 110.3 no C58 . C59 . H593 . 108.2 no H591 . C59 . H593 . 109.5 no H592 . C59 . H593 . 109.4 no Mn3 . O60 . H40 . 133.8 no Mn3 . O60 . H58 . 110.4 no H40 . O60 . H58 . 111.8 no data_eb6170 _database_code_depnum_ccdc_archive 'CCDC 636072' _audit_creation_date 07-05-16 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'eb6170 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.7121(4) _cell_length_b 13.1980(4) _cell_length_c 15.2785(5) _cell_angle_alpha 75.593(2) _cell_angle_beta 78.672(2) _cell_angle_gamma 68.389(2) _cell_volume 2292.53(13) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 1 # Given Formula = C88 H120 Mn6 N6 O24 # Dc = 1.43 Fooo = 1016.00 Mu = 8.77 M = 987.76 # Found Formula = C88 H104.00 Mn6 N6 O24 # Dc = 1.42 FOOO = 1016.00 Mu = 8.77 M = 979.69 _chemical_formula_sum 'C88 H104.00 Mn6 N6 O24' _chemical_formula_moiety 'C88 H104.00 Mn6 N6 O24' _chemical_compound_source ? _chemical_formula_weight 1959.39 _cell_measurement_reflns_used 6935 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1016.000 _exptl_absorpt_coefficient_mu 0.877 # Sheldrick geometric approximatio 0.80 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.97 _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_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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 48307 _reflns_number_total 12813 _diffrn_reflns_av_R_equivalents 0.040 # Number of reflections with Friedels Law is 12813 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14023 _diffrn_reflns_theta_min 1.385 _diffrn_reflns_theta_max 30.528 _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 27.780 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 18 _reflns_limit_k_min -17 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 1.44 _oxford_diffrn_Wilson_scale 5.14 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.85 _refine_diff_density_max 0.91 _refine_ls_number_reflns 12813 _refine_ls_number_restraints 0 _refine_ls_number_parameters 595 #_refine_ls_R_factor_ref 0.0701 _refine_ls_wR_factor_ref 0.1025 _refine_ls_goodness_of_fit_ref 0.8978 #_reflns_number_all 12813 _refine_ls_R_factor_all 0.0701 _refine_ls_wR_factor_all 0.1025 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8669 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_gt 0.0957 _refine_ls_shift/su_max 0.001115 # 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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; There is a single molcule in the unit cell, positioned on an inversion centre. The structure contains a Mn6 complex which has three ethylsalicylaldoxime (C~9~H~8~NO~2~) ligands, one adamantane carboxylate (C~11~H~15~O~2~) ligand and three ethanol ligands. Two of these ethanol ligands are disorder, and in these cases the terminal carbon atom has been modelled over mulitple atomic sites. In one case, the carbon is located at two sites (C60 and C61), with almost equal occupancies, and in the other the carbon has been positioned at three sites (C64, C65 and C66). In addition, one of the ethyl groups of the salicylaldomixe ligands is disordered at the terminal methyl group, and has been modelled over two atomic sites (C28 and C29). See the refinement details for the placement of hydrogen atoms on these carbons. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. Most H atoms were located in a difference Fourier map, but were positioned geometrically. Exceptions to this were the hydroxy hydrogens of the ethanol ligands, which were located from the difference Fourier map, and hydrogen atoms on the disordered ethyl groups. Hydrogen atoms were positioned geometrically on C28 and C29, but have been omitted for C27 (in the ethyl group). Similarly, hydrogen atoms were placed geometrically on C60 and C61, but in this case, due to the orientations of these carbon atoms, one of the two hydrogen atoms on C59 of the ethyl group are approximately coincident, and this hydrogen atom has been positioned using the Fourier map. The remaining hydrogen atom on C59 (which would be split over two sites, in the directions of C60 and C61) has not been modelled. Hydrogen atoms have not been placed on atoms C63-C66 due to the nature of the disorder. 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, N---H in the range 0.86--0.89 N---H to 0.86 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. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.43 Ratio 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C63 This atom may be disordered. It is attached to a carbon atom that has been modelled as three-fold disordered, and it is possible to model this atom over two atomic sites successfully. However, as the nature of the bonding between C63 and the attached methyl group then becomes difficult to determine, the atom was modelled as occupying a single atomic site but with a large adp. 432_ALERT_2_A Short Inter X...Y Contact C61 .. C61 .. 2.28 Ang. 432_ALERT_2_A Short Inter X...Y Contact C65 .. C65 .. 2.82 Ang. These atoms are both partially occupied. The unfavourable short contact may be a driving force towards the disorder present in there groups. 912_ALERT_3_A # Missing FCF Reflections Above STH/L=0.6 ...... 1206 911_ALERT_3_C # Missing FCF Refl. Between TH(Min) & STH/L=0.6 5 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 4802 4802 0 23.01 0.550 1.000 6386 6386 0 25.24 0.600 0.999 8299 8294 5 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.997 10531 10495 36 29.84 0.700 0.947 13181 12478 703 30.53 0.715 0.914 14024 12813 1211 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.07 Ratio 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O62 The atom is attached to a carbon atom that may be disordered, but has been modelled as a singly occupied atomic site (see above). 413_ALERT_2_B Short Inter XH3 .. XHn H573 .. H601 .. 2.06 Ang. The contact involves a disordered group, where the hydrogen atoms had to be placed geometrically. 213_ALERT_2_C Atom C53 has ADP max/min Ratio ............. 3.30 prolat 213_ALERT_2_C Atom C63 has ADP max/min Ratio ............. 3.60 prolat 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C53 This is at the tip of a ligand and therefore is probably caused by increased atomic motion at this point. 301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. Disorder is common in these types of structure, and here affects the flexible ethyl chains. 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? Not all hydrogen atoms have been placed for disordered ethyl groups. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 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. 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. 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 0.00958(3) 0.58757(3) 0.90684(2) 0.0169 1.0000 Uani . . . . . . Mn2 Mn -0.02655(3) 0.37216(3) 0.86296(2) 0.0180 1.0000 Uani . . . . . . Mn3 Mn 0.20992(3) 0.42279(3) 0.78694(2) 0.0198 1.0000 Uani . . . . . . O4 O 0.06175(12) 0.46419(12) 0.84976(10) 0.0187 1.0000 Uani . . . . . . O5 O -0.02235(12) 0.69584(12) 0.98157(10) 0.0198 1.0000 Uani . . . . . . C6 C -0.01174(19) 0.79627(18) 0.94196(15) 0.0208 1.0000 Uani . . . . . . C7 C -0.0892(2) 0.89017(19) 0.97366(16) 0.0253 1.0000 Uani . . . . . . C8 C -0.0850(2) 0.99503(19) 0.93474(17) 0.0290 1.0000 Uani . . . . . . C9 C -0.0032(2) 1.0091(2) 0.86288(17) 0.0299 1.0000 Uani . . . . . . C10 C 0.0755(2) 0.9172(2) 0.83335(18) 0.0304 1.0000 Uani . . . . . . C11 C 0.07591(19) 0.80857(18) 0.87197(16) 0.0236 1.0000 Uani . . . . . . C12 C 0.16927(19) 0.71342(19) 0.84288(17) 0.0255 1.0000 Uani . . . . . . N13 N 0.15418(15) 0.61915(15) 0.85255(13) 0.0214 1.0000 Uani . . . . . . O14 O 0.24575(12) 0.53100(12) 0.82978(11) 0.0235 1.0000 Uani . . . . . . C15 C 0.2835(2) 0.7259(2) 0.8048(2) 0.0420 1.0000 Uani . . . . . . C16 C 0.3338(3) 0.7526(3) 0.8733(3) 0.0637 1.0000 Uani . . . . . . O17 O 0.35617(13) 0.37540(14) 0.72466(12) 0.0283 1.0000 Uani . . . . . . C18 C 0.3776(2) 0.3446(2) 0.64486(17) 0.0273 1.0000 Uani . . . . . . C19 C 0.4652(2) 0.3710(2) 0.58203(19) 0.0357 1.0000 Uani . . . . . . C20 C 0.4932(3) 0.3399(3) 0.4992(2) 0.0495 1.0000 Uani . . . . . . C21 C 0.4385(3) 0.2795(3) 0.4760(2) 0.0671 1.0000 Uani . . . . . . C22 C 0.3532(3) 0.2504(3) 0.5376(2) 0.0557 1.0000 Uani . . . . . . C23 C 0.3202(2) 0.2830(2) 0.62185(17) 0.0327 1.0000 Uani . . . . . . C24 C 0.2293(2) 0.2494(2) 0.68406(17) 0.0286 1.0000 Uani . . . . . . N25 N 0.17541(15) 0.30359(15) 0.74858(13) 0.0211 1.0000 Uani . . . . . . O26 O 0.09605(13) 0.26330(12) 0.80687(10) 0.0223 1.0000 Uani . . . . . . C27 C 0.2002(2) 0.1505(3) 0.6756(2) 0.0435 1.0000 Uani . . . . . . C28 C 0.2791(10) 0.0634(9) 0.6770(8) 0.0578 0.2957 Uani . . . . . . C29 C 0.0947(3) 0.1787(4) 0.6350(3) 0.0429 0.7043 Uani . . . . . . O30 O -0.12024(13) 0.28675(12) 0.88121(11) 0.0229 1.0000 Uani . . . . . . C31 C -0.22847(19) 0.33373(19) 0.86398(16) 0.0233 1.0000 Uani . . . . . . C32 C -0.2741(2) 0.2756(2) 0.82529(19) 0.0327 1.0000 Uani . . . . . . C33 C -0.3842(2) 0.3195(2) 0.8031(2) 0.0397 1.0000 Uani . . . . . . C34 C -0.4542(2) 0.4232(2) 0.8208(2) 0.0393 1.0000 Uani . . . . . . C35 C -0.4122(2) 0.4805(2) 0.86139(19) 0.0321 1.0000 Uani . . . . . . C36 C -0.29948(19) 0.43857(19) 0.88414(16) 0.0238 1.0000 Uani . . . . . . C37 C -0.26081(18) 0.50363(18) 0.92758(15) 0.0211 1.0000 Uani . . . . . . N38 N -0.15259(15) 0.48197(15) 0.92555(12) 0.0182 1.0000 Uani . . . . . . O39 O -0.11739(12) 0.53931(12) 0.97303(10) 0.0186 1.0000 Uani . . . . . . C40 C -0.34571(19) 0.59737(19) 0.96941(17) 0.0264 1.0000 Uani . . . . . . C41 C -0.3616(2) 0.7067(2) 0.9013(2) 0.0385 1.0000 Uani . . . . . . O42 O -0.09066(14) 0.71103(13) 0.81101(11) 0.0269 1.0000 Uani . . . . . . C43 C -0.10558(19) 0.73706(19) 0.72807(16) 0.0239 1.0000 Uani . . . . . . O44 O -0.06645(15) 0.67089(13) 0.67321(11) 0.0308 1.0000 Uani . . . . . . C45 C -0.1749(2) 0.85691(19) 0.69084(16) 0.0275 1.0000 Uani . . . . . . C46 C -0.2670(3) 0.8584(2) 0.6385(2) 0.0501 1.0000 Uani . . . . . . C47 C -0.3345(3) 0.9785(3) 0.5982(3) 0.0688 1.0000 Uani . . . . . . C48 C -0.3902(3) 1.0437(3) 0.6751(3) 0.0617 1.0000 Uani . . . . . . C49 C -0.2974(3) 1.0441(2) 0.72471(19) 0.0409 1.0000 Uani . . . . . . C50 C -0.2303(2) 0.9246(2) 0.76555(17) 0.0310 1.0000 Uani . . . . . . C51 C -0.0946(3) 0.9112(2) 0.62380(19) 0.0442 1.0000 Uani . . . . . . C52 C -0.1620(4) 1.0312(2) 0.5829(2) 0.0620 1.0000 Uani . . . . . . C53 C -0.2548(4) 1.0304(3) 0.5325(2) 0.0877 1.0000 Uani . . . . . . C54 C -0.2168(3) 1.0973(2) 0.6594(2) 0.0532 1.0000 Uani . . . . . . O55 O 0.15175(14) 0.54658(13) 0.66334(11) 0.0300 1.0000 Uani . . . . . . C56 C 0.2084(3) 0.6255(3) 0.6198(2) 0.0490 1.0000 Uani . . . . . . C57 C 0.2041(4) 0.6560(4) 0.5212(2) 0.0798 1.0000 Uani . . . . . . O58 O -0.09025(14) 0.46994(14) 0.73122(11) 0.0295 1.0000 Uani . . . . . . C59 C -0.1284(3) 0.4507(3) 0.6568(2) 0.0554 1.0000 Uani . . . . . . C60 C -0.2394(7) 0.5324(6) 0.6378(6) 0.0786 0.5078 Uani . . . . . . C61 C -0.0565(9) 0.4835(8) 0.5660(4) 0.0850 0.4922 Uani . . . . . . O62 O 0.26869(15) 0.27908(14) 0.91082(12) 0.0333 1.0000 Uani . . . . . . C63 C 0.3434(4) 0.1677(3) 0.9068(5) 0.1127 1.0000 Uani . . . . . . C64 C 0.3834(10) 0.1063(10) 0.8678(8) 0.0446 0.2610 Uani . . . . . . C65 C 0.4144(8) 0.0884(7) 0.9567(6) 0.0606 0.3940 Uani . . . . . . C66 C 0.4487(8) 0.1515(8) 0.8807(8) 0.0590 0.3450 Uani . . . . . . H71 H -0.1428 0.8825 1.0210 0.0296 1.0000 Uiso R . . . . . H81 H -0.1380 1.0559 0.9577 0.0342 1.0000 Uiso R . . . . . H91 H 0.0011 1.0794 0.8364 0.0367 1.0000 Uiso R . . . . . H101 H 0.1294 0.9266 0.7861 0.0370 1.0000 Uiso R . . . . . H151 H 0.2806 0.7799 0.7449 0.0526 1.0000 Uiso R . . . . . H152 H 0.3377 0.6624 0.7828 0.0525 1.0000 Uiso R . . . . . H161 H 0.4087 0.7604 0.8445 0.0989 1.0000 Uiso R . . . . . H162 H 0.2812 0.8202 0.8968 0.0994 1.0000 Uiso R . . . . . H163 H 0.3490 0.6851 0.9252 0.0990 1.0000 Uiso R . . . . . H191 H 0.5031 0.4087 0.5984 0.0400 1.0000 Uiso R . . . . . H201 H 0.5506 0.3590 0.4581 0.0569 1.0000 Uiso R . . . . . H211 H 0.4573 0.2590 0.4195 0.0840 1.0000 Uiso R . . . . . H221 H 0.3151 0.2099 0.5225 0.0722 1.0000 Uiso R . . . . . H281 H 0.2587 0.0134 0.6547 0.0999 0.2957 Uiso R . . . . . H282 H 0.2944 0.0339 0.7381 0.0998 0.2957 Uiso R . . . . . H283 H 0.3441 0.0763 0.6409 0.0999 0.2957 Uiso R . . . . . H291 H 0.0802 0.1146 0.6341 0.0694 0.7043 Uiso R . . . . . H292 H 0.0323 0.2239 0.6683 0.0692 0.7043 Uiso R . . . . . H293 H 0.1036 0.2170 0.5745 0.0694 0.7043 Uiso R . . . . . H321 H -0.2286 0.2077 0.8129 0.0405 1.0000 Uiso R . . . . . H331 H -0.4130 0.2817 0.7748 0.0500 1.0000 Uiso R . . . . . H341 H -0.5278 0.4532 0.8053 0.0497 1.0000 Uiso R . . . . . H351 H -0.4597 0.5501 0.8736 0.0392 1.0000 Uiso R . . . . . H401 H -0.3217 0.6006 1.0227 0.0333 1.0000 Uiso R . . . . . H402 H -0.4175 0.5849 0.9862 0.0327 1.0000 Uiso R . . . . . H411 H -0.4194 0.7649 0.9259 0.0560 1.0000 Uiso R . . . . . H412 H -0.2932 0.7246 0.8860 0.0556 1.0000 Uiso R . . . . . H413 H -0.3822 0.7028 0.8448 0.0556 1.0000 Uiso R . . . . . H461 H -0.3174 0.8237 0.6798 0.0593 1.0000 Uiso R . . . . . H462 H -0.2308 0.8188 0.5903 0.0594 1.0000 Uiso R . . . . . H471 H -0.3957 0.9781 0.5678 0.0822 1.0000 Uiso R . . . . . H481 H -0.4313 1.1197 0.6469 0.0676 1.0000 Uiso R . . . . . H482 H -0.4433 1.0090 0.7169 0.0679 1.0000 Uiso R . . . . . H491 H -0.3328 1.0867 0.7720 0.0455 1.0000 Uiso R . . . . . H501 H -0.1734 0.9249 0.8002 0.0356 1.0000 Uiso R . . . . . H502 H -0.2821 0.8919 0.8077 0.0366 1.0000 Uiso R . . . . . H511 H -0.0334 0.9083 0.6554 0.0505 1.0000 Uiso R . . . . . H512 H -0.0618 0.8708 0.5744 0.0499 1.0000 Uiso R . . . . . H521 H -0.1097 1.0641 0.5402 0.0657 1.0000 Uiso R . . . . . H531 H -0.2995 1.1051 0.5057 0.0911 1.0000 Uiso R . . . . . H532 H -0.2202 0.9890 0.4838 0.0912 1.0000 Uiso R . . . . . H541 H -0.1578 1.0980 0.6914 0.0596 1.0000 Uiso R . . . . . H542 H -0.2636 1.1731 0.6337 0.0588 1.0000 Uiso R . . . . . H551 H 0.0843 0.5752 0.6684 0.0420 1.0000 Uiso R . . . . . H561 H 0.1747 0.6989 0.6438 0.0568 1.0000 Uiso R . . . . . H562 H 0.2878 0.5923 0.6329 0.0577 1.0000 Uiso R . . . . . H571 H 0.2451 0.7113 0.4971 0.1239 1.0000 Uiso R . . . . . H572 H 0.1229 0.6891 0.5104 0.1231 1.0000 Uiso R . . . . . H573 H 0.2410 0.5858 0.4974 0.1247 1.0000 Uiso R . . . . . H581 H -0.0751 0.5260 0.7156 0.0466 1.0000 Uiso R . . . . . H591 H -0.1296 0.3741 0.6693 0.0745 1.0000 Uiso R . . . . . H601 H -0.2659 0.5167 0.5897 0.1248 0.5078 Uiso R . . . . . H602 H -0.2933 0.5309 0.6905 0.1250 0.5078 Uiso R . . . . . H603 H -0.2332 0.6034 0.6193 0.1250 0.5078 Uiso R . . . . . H611 H -0.0909 0.4810 0.5164 0.1510 0.4922 Uiso R . . . . . H612 H -0.0563 0.5575 0.5619 0.1507 0.4922 Uiso R . . . . . H613 H 0.0181 0.4322 0.5665 0.1510 0.4922 Uiso R . . . . . H58 H 0.2150 0.2802 0.9528 0.0541 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 0.01594(16) 0.01402(16) 0.02142(17) -0.00416(12) -0.00373(12) -0.00459(13) Mn2 0.01523(16) 0.01599(17) 0.02421(17) -0.00643(13) -0.00325(13) -0.00464(13) Mn3 0.01555(16) 0.01720(17) 0.02742(18) -0.00738(14) -0.00195(13) -0.00454(13) O4 0.0170(7) 0.0173(8) 0.0230(8) -0.0056(6) -0.0030(6) -0.0059(6) O5 0.0205(8) 0.0151(7) 0.0237(8) -0.0038(6) -0.0054(6) -0.0044(6) C6 0.0229(11) 0.0160(11) 0.0256(11) -0.0049(9) -0.0089(9) -0.0053(9) C7 0.0266(12) 0.0207(12) 0.0287(12) -0.0069(9) -0.0045(10) -0.0063(10) C8 0.0335(13) 0.0157(11) 0.0369(14) -0.0084(10) -0.0090(11) -0.0025(10) C9 0.0348(14) 0.0169(12) 0.0398(14) -0.0042(10) -0.0067(11) -0.0105(10) C10 0.0289(13) 0.0234(13) 0.0396(14) -0.0066(11) 0.0003(11) -0.0113(11) C11 0.0217(11) 0.0172(11) 0.0339(13) -0.0067(9) -0.0036(10) -0.0075(9) C12 0.0205(11) 0.0232(12) 0.0348(13) -0.0074(10) -0.0009(10) -0.0097(10) N13 0.0162(9) 0.0187(10) 0.0286(10) -0.0072(8) -0.0023(7) -0.0035(7) O14 0.0155(7) 0.0186(8) 0.0366(9) -0.0103(7) -0.0013(7) -0.0037(6) C15 0.0257(13) 0.0288(14) 0.075(2) -0.0194(14) 0.0082(13) -0.0136(12) C16 0.0325(17) 0.057(2) 0.109(3) -0.026(2) -0.0124(18) -0.0137(16) O17 0.0169(8) 0.0287(9) 0.0410(10) -0.0140(8) 0.0004(7) -0.0068(7) C18 0.0205(11) 0.0226(12) 0.0348(13) -0.0084(10) 0.0004(10) -0.0025(10) C19 0.0280(13) 0.0298(14) 0.0442(16) -0.0078(12) 0.0058(12) -0.0087(11) C20 0.0416(17) 0.060(2) 0.0427(17) -0.0092(15) 0.0132(14) -0.0216(16) C21 0.065(2) 0.107(3) 0.0428(19) -0.036(2) 0.0231(17) -0.045(2) C22 0.0502(19) 0.088(3) 0.0465(18) -0.0387(18) 0.0141(15) -0.0364(19) C23 0.0270(13) 0.0397(15) 0.0317(13) -0.0135(11) 0.0021(10) -0.0100(11) C24 0.0239(12) 0.0352(14) 0.0315(13) -0.0159(11) 0.0002(10) -0.0109(11) N25 0.0166(9) 0.0201(10) 0.0252(10) -0.0046(8) -0.0014(7) -0.0051(8) O26 0.0198(8) 0.0194(8) 0.0280(8) -0.0075(6) 0.0010(6) -0.0071(6) C27 0.0343(15) 0.0472(18) 0.064(2) -0.0405(16) 0.0109(14) -0.0205(14) C28 0.074(8) 0.060(7) 0.069(8) -0.046(6) 0.021(6) -0.049(7) C29 0.039(2) 0.051(3) 0.051(3) -0.026(2) 0.0003(19) -0.022(2) O30 0.0172(7) 0.0177(8) 0.0355(9) -0.0061(7) -0.0060(7) -0.0057(6) C31 0.0181(11) 0.0206(11) 0.0333(13) -0.0069(10) -0.0058(9) -0.0062(9) C32 0.0270(13) 0.0227(13) 0.0524(17) -0.0153(12) -0.0116(12) -0.0041(10) C33 0.0287(14) 0.0323(15) 0.067(2) -0.0205(14) -0.0192(13) -0.0070(12) C34 0.0216(12) 0.0364(15) 0.067(2) -0.0211(14) -0.0147(12) -0.0052(11) C35 0.0186(11) 0.0263(13) 0.0540(17) -0.0152(12) -0.0094(11) -0.0031(10) C36 0.0171(10) 0.0221(12) 0.0346(13) -0.0078(10) -0.0051(9) -0.0066(9) C37 0.0188(11) 0.0192(11) 0.0263(11) -0.0048(9) -0.0034(9) -0.0070(9) N38 0.0169(9) 0.0177(9) 0.0231(9) -0.0055(7) -0.0042(7) -0.0074(7) O39 0.0171(7) 0.0203(8) 0.0223(8) -0.0069(6) -0.0041(6) -0.0081(6) C40 0.0175(11) 0.0262(13) 0.0382(14) -0.0139(10) -0.0033(10) -0.0056(10) C41 0.0262(13) 0.0258(14) 0.0607(19) -0.0100(13) -0.0085(13) -0.0027(11) O42 0.0256(9) 0.0238(9) 0.0290(9) 0.0004(7) -0.0097(7) -0.0058(7) C43 0.0200(11) 0.0213(12) 0.0299(12) 0.0001(9) -0.0070(9) -0.0077(9) O44 0.0327(10) 0.0228(9) 0.0328(9) -0.0055(7) -0.0074(8) -0.0029(7) C45 0.0343(13) 0.0201(12) 0.0260(12) -0.0016(9) -0.0127(10) -0.0040(10) C46 0.056(2) 0.0303(15) 0.064(2) -0.0162(14) -0.0403(17) 0.0063(14) C47 0.083(3) 0.0372(18) 0.080(3) -0.0188(18) -0.062(2) 0.0174(18) C48 0.059(2) 0.0321(17) 0.079(3) -0.0118(16) -0.0354(19) 0.0165(15) C49 0.0581(19) 0.0212(13) 0.0351(15) -0.0064(11) -0.0110(13) -0.0005(13) C50 0.0407(15) 0.0230(13) 0.0277(13) -0.0029(10) -0.0073(11) -0.0085(11) C51 0.063(2) 0.0272(14) 0.0336(15) -0.0016(11) 0.0067(14) -0.0136(14) C52 0.104(3) 0.0253(15) 0.0355(17) 0.0012(13) 0.0100(18) -0.0113(17) C53 0.157(4) 0.0331(19) 0.0366(19) -0.0029(15) -0.040(2) 0.021(2) C54 0.088(3) 0.0217(14) 0.0401(17) 0.0002(12) -0.0067(17) -0.0120(16) O55 0.0243(9) 0.0257(9) 0.0346(10) -0.0004(7) -0.0015(7) -0.0068(7) C56 0.0450(18) 0.0461(18) 0.0519(19) 0.0034(15) -0.0032(15) -0.0204(15) C57 0.109(4) 0.088(3) 0.051(2) 0.018(2) -0.020(2) -0.058(3) O58 0.0376(10) 0.0269(9) 0.0295(9) -0.0028(7) -0.0140(8) -0.0139(8) C59 0.082(3) 0.070(2) 0.0358(17) -0.0083(16) -0.0180(16) -0.046(2) C60 0.100(6) 0.063(5) 0.089(6) 0.000(4) -0.064(5) -0.030(5) C61 0.156(9) 0.114(7) 0.032(4) -0.017(4) -0.001(4) -0.103(7) O62 0.0396(10) 0.0246(9) 0.0366(10) -0.0049(8) -0.0146(8) -0.0075(8) C63 0.053(3) 0.033(2) 0.207(6) 0.013(3) -0.015(3) 0.0142(19) C64 0.042(7) 0.031(6) 0.042(6) -0.014(5) -0.013(5) 0.019(5) C65 0.074(6) 0.037(5) 0.067(6) -0.003(4) -0.040(5) -0.003(4) C66 0.027(5) 0.049(6) 0.092(8) -0.016(6) 0.006(5) -0.007(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4603(4) 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 . O39 2_567 2.4124(15) yes Mn1 . Mn1 2_567 3.2208(7) yes Mn1 . Mn2 . 3.2822(5) yes Mn1 . Mn3 . 3.2621(5) yes Mn1 . O4 . 1.8803(15) yes Mn1 . O5 . 1.9269(15) yes Mn1 . N13 . 2.0085(18) yes Mn1 . O39 . 1.9567(15) yes Mn1 . O42 . 2.1068(16) yes Mn2 . O5 2_567 2.4376(15) yes Mn2 . Mn3 . 3.2486(5) yes Mn2 . O4 . 1.8892(15) yes Mn2 . O26 . 1.9148(15) yes Mn2 . O30 . 1.8627(15) yes Mn2 . N38 . 1.9897(18) yes Mn2 . O58 . 2.2250(16) yes Mn3 . O4 . 1.8868(15) yes Mn3 . O14 . 1.9330(15) yes Mn3 . O17 . 1.8702(16) yes Mn3 . N25 . 2.0198(19) yes Mn3 . O55 . 2.2150(17) yes Mn3 . O62 . 2.3373(17) yes O5 . C6 . 1.357(3) yes C6 . C7 . 1.397(3) yes C6 . C11 . 1.411(3) yes C7 . C8 . 1.380(3) yes C7 . H71 . 0.904 no C8 . C9 . 1.383(3) yes C8 . H81 . 0.933 no C9 . C10 . 1.371(3) yes C9 . H91 . 0.932 no C10 . C11 . 1.406(3) yes C10 . H101 . 0.910 no C11 . C12 . 1.468(3) yes C12 . N13 . 1.296(3) yes C12 . C15 . 1.507(3) yes N13 . O14 . 1.369(2) yes C15 . C16 . 1.496(4) yes C15 . H151 . 1.007 no C15 . H152 . 0.957 no C16 . H161 . 0.999 no C16 . H162 . 1.000 no C16 . H163 . 1.020 no O17 . C18 . 1.327(3) yes C18 . C19 . 1.408(3) yes C18 . C23 . 1.413(4) yes C19 . C20 . 1.368(4) yes C19 . H191 . 0.911 no C20 . C21 . 1.375(5) yes C20 . H201 . 0.930 no C21 . C22 . 1.392(4) yes C21 . H211 . 0.929 no C22 . C23 . 1.395(4) yes C22 . H221 . 0.932 no C23 . C24 . 1.474(3) yes C24 . N25 . 1.295(3) yes C24 . C27 . 1.522(4) yes N25 . O26 . 1.378(2) yes C27 . C28 . 1.214(12) yes C27 . C29 . 1.473(5) yes C28 . H281 . 0.945 no C28 . H282 . 0.946 no C28 . H283 . 0.946 no C29 . H291 . 0.934 no C29 . H292 . 0.942 no C29 . H293 . 0.944 no O30 . C31 . 1.334(3) yes C31 . C32 . 1.401(3) yes C31 . C36 . 1.417(3) yes C32 . C33 . 1.379(3) yes C32 . H321 . 0.913 no C33 . C34 . 1.389(4) yes C33 . H331 . 0.935 no C34 . C35 . 1.379(3) yes C34 . H341 . 0.926 no C35 . C36 . 1.413(3) yes C35 . H351 . 0.936 no C36 . C37 . 1.464(3) yes C37 . N38 . 1.294(3) yes C37 . C40 . 1.498(3) yes N38 . O39 . 1.396(2) yes C40 . C41 . 1.526(3) yes C40 . H401 . 0.939 no C40 . H402 . 0.961 no C41 . H411 . 0.944 no C41 . H412 . 0.954 no C41 . H413 . 0.967 no O42 . C43 . 1.261(3) yes C43 . O44 . 1.262(3) yes C43 . C45 . 1.525(3) yes C45 . C46 . 1.534(4) yes C45 . C50 . 1.524(3) yes C45 . C51 . 1.538(4) yes C46 . C47 . 1.532(4) yes C46 . H461 . 0.965 no C46 . H462 . 0.953 no C47 . C48 . 1.534(5) yes C47 . C53 . 1.507(6) yes C47 . H471 . 0.983 no C48 . C49 . 1.524(4) yes C48 . H481 . 0.975 no C48 . H482 . 0.993 no C49 . C50 . 1.528(3) yes C49 . C54 . 1.522(4) yes C49 . H491 . 0.963 no C50 . H501 . 0.978 no C50 . H502 . 0.969 no C51 . C52 . 1.533(4) yes C51 . H511 . 0.978 no C51 . H512 . 0.970 no C52 . C53 . 1.535(6) yes C52 . C54 . 1.534(4) yes C52 . H521 . 0.977 no C53 . H531 . 0.970 no C53 . H532 . 0.970 no C54 . H541 . 0.976 no C54 . H542 . 0.984 no O55 . C56 . 1.438(3) yes O55 . H551 . 0.796 no C56 . C57 . 1.466(4) yes C56 . H561 . 1.032 no C56 . H562 . 0.980 no C57 . H571 . 1.004 no C57 . H572 . 0.992 no C57 . H573 . 0.996 no O58 . C59 . 1.429(3) yes O58 . H581 . 0.801 no C59 . C60 . 1.458(8) yes C59 . C61 . 1.563(7) yes C59 . H591 . 0.986 no C60 . H601 . 0.960 no C60 . H602 . 0.949 no C60 . H603 . 0.937 no C61 . H611 . 0.960 no C61 . H612 . 0.963 no C61 . H613 . 0.941 no O62 . C63 . 1.435(4) yes O62 . H58 . 0.838 no C63 . C64 . 1.044(11) yes C63 . C65 . 1.292(9) yes C63 . C66 . 1.272(10) yes C64 . C65 . 1.427(14) yes C64 . C66 . 1.254(16) yes C65 . C66 . 1.348(13) yes 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 O39 2_567 Mn1 . Mn1 2_567 37.28(3) yes O39 2_567 Mn1 . Mn2 . 87.22(4) yes Mn1 2_567 Mn1 . Mn2 . 70.276(13) yes O39 2_567 Mn1 . Mn3 . 80.52(4) yes Mn1 2_567 Mn1 . Mn3 . 99.622(15) yes Mn2 . Mn1 . Mn3 . 59.523(10) yes O39 2_567 Mn1 . O4 . 84.59(6) yes Mn1 2_567 Mn1 . O4 . 85.63(5) yes Mn2 . Mn1 . O4 . 29.53(4) yes Mn3 . Mn1 . O4 . 30.07(4) yes O39 2_567 Mn1 . O5 . 84.37(6) yes Mn1 2_567 Mn1 . O5 . 86.88(5) yes Mn2 . Mn1 . O5 . 151.41(5) yes Mn3 . Mn1 . O5 . 144.53(5) yes O4 . Mn1 . O5 . 168.75(6) yes O39 2_567 Mn1 . N13 . 85.85(6) yes Mn1 2_567 Mn1 . N13 . 123.12(6) yes Mn2 . Mn1 . N13 . 118.23(5) yes Mn3 . Mn1 . N13 . 58.78(5) yes O4 . Mn1 . N13 . 88.69(7) yes O39 2_567 Mn1 . O39 . 85.59(6) yes Mn1 2_567 Mn1 . O39 . 48.31(4) yes Mn2 . Mn1 . O39 . 60.28(4) yes Mn3 . Mn1 . O39 . 118.57(4) yes O4 . Mn1 . O39 . 89.48(6) yes O39 2_567 Mn1 . O42 . 173.86(6) yes Mn1 2_567 Mn1 . O42 . 141.79(5) yes Mn2 . Mn1 . O42 . 97.84(5) yes Mn3 . Mn1 . O42 . 105.03(5) yes O4 . Mn1 . O42 . 101.53(6) yes O5 . Mn1 . N13 . 88.38(7) yes O5 . Mn1 . O39 . 91.80(6) yes N13 . Mn1 . O39 . 171.38(7) yes O5 . Mn1 . O42 . 89.53(6) yes N13 . Mn1 . O42 . 94.75(7) yes O39 . Mn1 . O42 . 93.88(6) yes O5 2_567 Mn2 . Mn1 . 78.09(4) yes O5 2_567 Mn2 . Mn3 . 93.01(4) yes Mn1 . Mn2 . Mn3 . 59.930(10) yes O5 2_567 Mn2 . O4 . 86.30(6) yes Mn1 . Mn2 . O4 . 29.38(4) yes Mn3 . Mn2 . O4 . 30.63(4) yes O5 2_567 Mn2 . O26 . 98.09(6) yes Mn1 . Mn2 . O26 . 121.38(5) yes Mn3 . Mn2 . O26 . 61.96(5) yes O4 . Mn2 . O26 . 92.49(6) yes O5 2_567 Mn2 . O30 . 92.29(6) yes Mn1 . Mn2 . O30 . 146.96(5) yes Mn3 . Mn2 . O30 . 152.97(5) yes O4 . Mn2 . O30 . 176.34(7) yes O26 . Mn2 . O30 . 91.05(7) yes O5 2_567 Mn2 . N38 . 79.93(6) yes Mn1 . Mn2 . N38 . 58.77(5) yes Mn3 . Mn2 . N38 . 118.44(5) yes O4 . Mn2 . N38 . 87.84(7) yes O26 . Mn2 . N38 . 177.97(7) yes O5 2_567 Mn2 . O58 . 167.30(6) yes Mn1 . Mn2 . O58 . 91.40(4) yes Mn3 . Mn2 . O58 . 87.75(5) yes O4 . Mn2 . O58 . 87.94(6) yes O26 . Mn2 . O58 . 93.46(7) yes O30 . Mn2 . N38 . 88.58(7) yes O30 . Mn2 . O58 . 92.77(7) yes N38 . Mn2 . O58 . 88.55(7) yes Mn2 . Mn3 . Mn1 . 60.547(10) yes Mn2 . Mn3 . O4 . 30.67(4) yes Mn1 . Mn3 . O4 . 29.95(4) yes Mn2 . Mn3 . O14 . 121.01(5) yes Mn1 . Mn3 . O14 . 61.47(4) yes O4 . Mn3 . O14 . 91.17(6) yes Mn2 . Mn3 . O17 . 146.69(5) yes Mn1 . Mn3 . O17 . 152.62(5) yes O4 . Mn3 . O17 . 177.33(7) yes O14 . Mn3 . O17 . 91.31(7) yes Mn2 . Mn3 . N25 . 58.51(5) yes Mn1 . Mn3 . N25 . 118.58(5) yes O4 . Mn3 . N25 . 88.71(7) yes O14 . Mn3 . N25 . 176.80(7) yes O17 . Mn3 . N25 . 88.76(7) yes Mn2 . Mn3 . O55 . 97.64(4) yes Mn1 . Mn3 . O55 . 87.99(4) yes O4 . Mn3 . O55 . 91.59(6) yes O14 . Mn3 . O55 . 90.31(7) yes O17 . Mn3 . O55 . 89.37(7) yes Mn2 . Mn3 . O62 . 79.94(5) yes Mn1 . Mn3 . O62 . 95.28(5) yes O4 . Mn3 . O62 . 88.91(6) yes O14 . Mn3 . O62 . 95.41(6) yes O17 . Mn3 . O62 . 89.88(7) yes N25 . Mn3 . O55 . 92.89(7) yes N25 . Mn3 . O62 . 81.39(7) yes O55 . Mn3 . O62 . 174.24(6) yes Mn2 . O4 . Mn3 . 118.70(8) yes Mn2 . O4 . Mn1 . 121.08(8) yes Mn3 . O4 . Mn1 . 119.98(8) yes Mn2 2_567 O5 . Mn1 . 117.63(7) yes Mn2 2_567 O5 . C6 . 114.60(12) yes Mn1 . O5 . C6 . 118.83(13) yes O5 . C6 . C7 . 118.3(2) yes O5 . C6 . C11 . 122.43(19) yes C7 . C6 . C11 . 119.2(2) yes C6 . C7 . C8 . 121.2(2) yes C6 . C7 . H71 . 119.7 no C8 . C7 . H71 . 119.0 no C7 . C8 . C9 . 120.2(2) yes C7 . C8 . H81 . 119.0 no C9 . C8 . H81 . 120.8 no C8 . C9 . C10 . 118.9(2) yes C8 . C9 . H91 . 121.1 no C10 . C9 . H91 . 119.9 no C9 . C10 . C11 . 122.8(2) yes C9 . C10 . H101 . 118.8 no C11 . C10 . H101 . 118.3 no C6 . C11 . C10 . 117.4(2) yes C6 . C11 . C12 . 122.7(2) yes C10 . C11 . C12 . 119.8(2) yes C11 . C12 . N13 . 120.2(2) yes C11 . C12 . C15 . 119.1(2) yes N13 . C12 . C15 . 120.7(2) yes Mn1 . N13 . C12 . 125.42(15) yes Mn1 . N13 . O14 . 116.42(13) yes C12 . N13 . O14 . 118.01(18) yes N13 . O14 . Mn3 . 115.43(12) yes C12 . C15 . C16 . 111.4(3) yes C12 . C15 . H151 . 112.3 no C16 . C15 . H151 . 112.9 no C12 . C15 . H152 . 113.9 no C16 . C15 . H152 . 108.9 no H151 . C15 . H152 . 96.7 no C15 . C16 . H161 . 107.9 no C15 . C16 . H162 . 111.9 no H161 . C16 . H162 . 112.3 no C15 . C16 . H163 . 106.5 no H161 . C16 . H163 . 107.9 no H162 . C16 . H163 . 110.1 no Mn3 . O17 . C18 . 123.52(15) yes O17 . C18 . C19 . 117.9(2) yes O17 . C18 . C23 . 123.2(2) yes C19 . C18 . C23 . 118.9(2) yes C18 . C19 . C20 . 120.9(3) yes C18 . C19 . H191 . 118.1 no C20 . C19 . H191 . 121.0 no C19 . C20 . C21 . 120.9(3) yes C19 . C20 . H201 . 119.9 no C21 . C20 . H201 . 119.3 no C20 . C21 . C22 . 119.3(3) yes C20 . C21 . H211 . 120.6 no C22 . C21 . H211 . 120.1 no C21 . C22 . C23 . 121.5(3) yes C21 . C22 . H221 . 120.1 no C23 . C22 . H221 . 118.3 no C18 . C23 . C22 . 118.5(2) yes C18 . C23 . C24 . 122.7(2) yes C22 . C23 . C24 . 118.8(2) yes C23 . C24 . N25 . 119.1(2) yes C23 . C24 . C27 . 121.3(2) yes N25 . C24 . C27 . 119.6(2) yes Mn3 . N25 . C24 . 128.19(16) yes Mn3 . N25 . O26 . 115.43(13) yes C24 . N25 . O26 . 115.56(19) yes N25 . O26 . Mn2 . 114.76(12) yes C24 . C27 . C28 . 115.8(5) yes C24 . C27 . C29 . 115.2(3) yes C28 . C27 . C29 . 125.2(6) yes C27 . C28 . H281 . 109.5 no C27 . C28 . H282 . 107.9 no H281 . C28 . H282 . 109.8 no C27 . C28 . H283 . 109.7 no H281 . C28 . H283 . 110.0 no H282 . C28 . H283 . 109.8 no C27 . C29 . H291 . 110.8 no C27 . C29 . H292 . 110.4 no H291 . C29 . H292 . 108.9 no C27 . C29 . H293 . 108.5 no H291 . C29 . H293 . 108.5 no H292 . C29 . H293 . 109.7 no Mn2 . O30 . C31 . 120.70(14) yes O30 . C31 . C32 . 118.2(2) yes O30 . C31 . C36 . 123.1(2) yes C32 . C31 . C36 . 118.7(2) yes C31 . C32 . C33 . 121.9(2) yes C31 . C32 . H321 . 118.7 no C33 . C32 . H321 . 119.4 no C32 . C33 . C34 . 120.1(2) yes C32 . C33 . H331 . 121.4 no C34 . C33 . H331 . 118.6 no C33 . C34 . C35 . 119.1(2) yes C33 . C34 . H341 . 120.1 no C35 . C34 . H341 . 120.8 no C34 . C35 . C36 . 122.4(2) yes C34 . C35 . H351 . 118.9 no C36 . C35 . H351 . 118.8 no C31 . C36 . C35 . 117.9(2) yes C31 . C36 . C37 . 122.7(2) yes C35 . C36 . C37 . 119.4(2) yes C36 . C37 . N38 . 118.9(2) yes C36 . C37 . C40 . 120.14(19) yes N38 . C37 . C40 . 120.9(2) yes Mn2 . N38 . C37 . 127.21(15) yes Mn2 . N38 . O39 . 114.75(12) yes C37 . N38 . O39 . 118.03(17) yes N38 . O39 . Mn1 2_567 110.57(11) yes N38 . O39 . Mn1 . 113.54(11) yes Mn1 2_567 O39 . Mn1 . 94.41(6) yes C37 . C40 . C41 . 109.9(2) yes C37 . C40 . H401 . 110.3 no C41 . C40 . H401 . 110.5 no C37 . C40 . H402 . 109.5 no C41 . C40 . H402 . 109.2 no H401 . C40 . H402 . 107.4 no C40 . C41 . H411 . 109.8 no C40 . C41 . H412 . 111.8 no H411 . C41 . H412 . 108.6 no C40 . C41 . H413 . 111.1 no H411 . C41 . H413 . 108.9 no H412 . C41 . H413 . 106.4 no Mn1 . O42 . C43 . 142.76(16) yes O42 . C43 . O44 . 124.6(2) yes O42 . C43 . C45 . 118.0(2) yes O44 . C43 . C45 . 117.4(2) yes C43 . C45 . C46 . 109.5(2) yes C43 . C45 . C50 . 112.44(19) yes C46 . C45 . C50 . 109.6(2) yes C43 . C45 . C51 . 108.3(2) yes C46 . C45 . C51 . 108.2(2) yes C50 . C45 . C51 . 108.7(2) yes C45 . C46 . C47 . 109.8(2) yes C45 . C46 . H461 . 108.9 no C47 . C46 . H461 . 109.9 no C45 . C46 . H462 . 108.6 no C47 . C46 . H462 . 109.0 no H461 . C46 . H462 . 110.6 no C46 . C47 . C48 . 109.4(3) yes C46 . C47 . C53 . 109.1(3) yes C48 . C47 . C53 . 110.4(3) yes C46 . C47 . H471 . 108.7 no C48 . C47 . H471 . 107.8 no C53 . C47 . H471 . 111.4 no C47 . C48 . C49 . 109.1(3) yes C47 . C48 . H481 . 107.1 no C49 . C48 . H481 . 109.3 no C47 . C48 . H482 . 109.1 no C49 . C48 . H482 . 111.4 no H481 . C48 . H482 . 110.7 no C48 . C49 . C50 . 109.1(2) yes C48 . C49 . C54 . 110.6(3) yes C50 . C49 . C54 . 109.4(2) yes C48 . C49 . H491 . 108.6 no C50 . C49 . H491 . 110.4 no C54 . C49 . H491 . 108.8 no C49 . C50 . C45 . 110.4(2) yes C49 . C50 . H501 . 109.2 no C45 . C50 . H501 . 111.4 no C49 . C50 . H502 . 108.7 no C45 . C50 . H502 . 109.5 no H501 . C50 . H502 . 107.6 no C45 . C51 . C52 . 109.9(3) yes C45 . C51 . H511 . 109.4 no C52 . C51 . H511 . 111.2 no C45 . C51 . H512 . 109.3 no C52 . C51 . H512 . 107.9 no H511 . C51 . H512 . 109.1 no C51 . C52 . C53 . 108.9(3) yes C51 . C52 . C54 . 109.4(3) yes C53 . C52 . C54 . 109.8(3) yes C51 . C52 . H521 . 108.7 no C53 . C52 . H521 . 109.8 no C54 . C52 . H521 . 110.2 no C52 . C53 . C47 . 109.8(3) yes C52 . C53 . H531 . 111.3 no C47 . C53 . H531 . 108.0 no C52 . C53 . H532 . 109.9 no C47 . C53 . H532 . 110.0 no H531 . C53 . H532 . 107.9 no C52 . C54 . C49 . 109.0(3) yes C52 . C54 . H541 . 109.9 no C49 . C54 . H541 . 110.5 no C52 . C54 . H542 . 109.5 no C49 . C54 . H542 . 106.6 no H541 . C54 . H542 . 111.3 no Mn3 . O55 . C56 . 121.09(16) yes Mn3 . O55 . H551 . 111.5 no C56 . O55 . H551 . 111.8 no O55 . C56 . C57 . 112.4(3) yes O55 . C56 . H561 . 113.5 no C57 . C56 . H561 . 106.3 no O55 . C56 . H562 . 107.7 no C57 . C56 . H562 . 110.0 no H561 . C56 . H562 . 106.7 no C56 . C57 . H571 . 106.6 no C56 . C57 . H572 . 107.9 no H571 . C57 . H572 . 111.5 no C56 . C57 . H573 . 106.5 no H571 . C57 . H573 . 113.7 no H572 . C57 . H573 . 110.4 no Mn2 . O58 . C59 . 137.19(18) yes Mn2 . O58 . H581 . 112.0 no C59 . O58 . H581 . 109.1 no O58 . C59 . C60 . 110.7(4) yes O58 . C59 . C61 . 109.7(4) yes C60 . C59 . C61 . 98.9(5) yes O58 . C59 . H591 . 110.3 no C60 . C59 . H591 . 111.7 no C61 . C59 . H591 . 115.1 no C59 . C60 . H601 . 110.0 no C59 . C60 . H602 . 110.4 no H601 . C60 . H602 . 108.9 no C59 . C60 . H603 . 109.5 no H601 . C60 . H603 . 108.4 no H602 . C60 . H603 . 109.6 no C59 . C61 . H611 . 108.2 no C59 . C61 . H612 . 108.8 no H611 . C61 . H612 . 110.4 no C59 . C61 . H613 . 108.4 no H611 . C61 . H613 . 110.4 no H612 . C61 . H613 . 110.6 no Mn3 . O62 . C63 . 126.5(3) yes Mn3 . O62 . H58 . 111.0 no C63 . O62 . H58 . 111.5 no O62 . C63 . C64 . 147.7(9) yes O62 . C63 . C65 . 137.3(7) yes C64 . C63 . C65 . 74.5(7) yes O62 . C63 . C66 . 118.5(6) yes C64 . C63 . C66 . 64.7(9) yes C65 . C63 . C66 . 63.4(7) yes C63 . C64 . C65 . 60.7(7) yes C63 . C64 . C66 . 66.5(9) yes C65 . C64 . C66 . 59.9(8) yes C64 . C65 . C63 . 44.8(5) yes C64 . C65 . C66 . 53.6(8) yes C63 . C65 . C66 . 57.6(6) yes C65 . C66 . C63 . 59.0(6) yes C65 . C66 . C64 . 66.4(8) yes C63 . C66 . C64 . 48.8(6) yes