data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'M Dufton' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Saiti Datta' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Stephen Hill' '' '' 'Ross Inglis' '' '' 'Leigh F. Jones' '' '' 'Giannis Papaefstathiou' '' '' 'Spyros P. Perlepes' '' '' 'Stephanie M. Taylor' '' '' 'Wolfgang Wernsdorfer' '' '' _publ_contact_author_name 'Euan Brechin' _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_section_title ; Twisting, Bending, Stretching: Strategies for Making Ferromagnetic [MnIII3] Triangles ; _publ_contact_author_address ; Department of Chemistry, Joseph Black Building, West Mains Road, University of Edinburgh, Edinburgh, EH9 3JJ, UK. ; _publ_contact_author_phone '+44 131 650 4806' _publ_contact_letter ; ; _publ_requested_coeditor_name A.Prescimone@sms.ed.ac.uk _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_name_full ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_fax '+44 131 000000' _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_journal 'Section E' # Attachment 'Complex 2.cif' data_EB8178 _database_code_depnum_ccdc_archive 'CCDC 736436' _audit_creation_date 08-11-25 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8178 in P-3' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Cl1 Mn3 N6 O11. (C4 H10 O)' _chemical_compound_source 'Stephanie Taylor ST14' _exptl_crystal_recrystallization_method ; Diffusion of ether into MeOH solution ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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 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\%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. H atoms on C22 were added geometrically. The crystal was twinned. It was processed as a 2-component twin via the twin law: 1 0 0 1 1 0 0 0 -1 with each component accounting for approx. 50% of the reflections. Checkcif alerts 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.48 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.67 Ratio No action taken. There is disorder in the terminal methyl grouo of the 4-ethyl pyridine ligand (see below). 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 113.00 A**3 The solvent region was treated by the van der Sluis and Spek method, accounting for 73 e/cell. This corresponds approximately to 1 molecule of ether per formula unit and F(000), M, mu, D and the formulae have been calculated on this assumption. 063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.68 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O15 301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. The 4-ethyl pyridine has been modelled using two partially occupied atomic sites for the terminal methyl group. The occupancy of these two sites has been refined to the ratio 0.6:0.4. However, the electron density may be more continuous than this modelling implies, accouning for the large adps. 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 1 Reflections with [sin(\q/\l)]^2^ less than 0.01 were excluded from the refinement as these may be poorly measured in the vicinity of the beamstop. The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 1606 1606 0 23.01 0.550 1.000 2146 2146 0 25.24 0.600 1.000 2791 2791 0 #----------------------------------------------------------- ACTA Min. Res. --- 26.35 0.625 1.000 3149 3148 1 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 19 The following least squares restraints were applied: U(IJ)'S 0.0, 0.010000 = C(22) TO C(23) U(IJ)'S 0.0, 0.010000 = C(22) TO C(24) U(IJ)'S 0.0, 0.010000 = C(19) TO C(22) DISTANCE 1.500000 , 0.010000 = C(22) TO C(23) ; # 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 0.000 0.000 114.8 71.6 2 0.000 0.000 0.500 7.0 1.5 _platon_squeeze_details ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 15.9022(10) _cell_length_b 15.9022(10) _cell_length_c 10.5328(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2306.7(3) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P -3 ' _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y,x-y,z y,-x+y,-z -x+y,-x,z x-y,x,-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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 2 # Given Formula = C46 H52 Cl1.00 Mn3 N6 O12 # Dc = 1.56 Fooo = 1032.00 Mu = 9.37 M = 360.40 # Found Formula = C42 H42 Cl1 Mn3 N6 O11.00 # Dc = 1.45 FOOO = 1032.00 Mu = 9.30 M = 335.69 _chemical_formula_sum 'C46 H52 Cl1 Mn3 N6 O12' _chemical_formula_weight 1081.20 _cell_measurement_reflns_used 9790 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_min 0.24 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.68 _exptl_crystal_density_diffrn 1.56 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.937 # Sheldrick geometric approximatio 0.76 0.80 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.80 _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 '\f & \w scans' # 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 72611 _reflns_number_total 3148 _diffrn_reflns_av_R_equivalents 0.0519 # Number of reflections with Friedels Law is 3148 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3138 _diffrn_reflns_theta_min 1.479 _diffrn_reflns_theta_max 26.352 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.352 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -19 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _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 -0.49 _refine_diff_density_max 0.61 # 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 3135 _refine_ls_number_restraints 19 _refine_ls_number_parameters 200 _oxford_refine_ls_R_factor_ref 0.0540 _refine_ls_wR_factor_ref 0.1272 _refine_ls_goodness_of_fit_ref 1.1277 _refine_ls_shift/su_max 0.000873 # The values computed from all data _oxford_reflns_number_all 3135 _refine_ls_R_factor_all 0.0540 _refine_ls_wR_factor_all 0.1272 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3082 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_gt 0.1263 # 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^) + ( 0.05P)^2^ + 4.82P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.55489(3) 0.34469(3) 0.41645(5) 0.0258 1.0000 Uani . . . . . . . O2 O 0.90838(15) 0.55137(15) 0.3664(2) 0.0331 1.0000 Uani . . . . . . . C3 C 0.9363(2) 0.6445(2) 0.3583(3) 0.0261 1.0000 Uani . . . . . . . C4 C 1.0356(2) 0.7110(2) 0.3402(3) 0.0317 1.0000 Uani . . . . . . . C5 C 1.0687(2) 0.8090(2) 0.3279(4) 0.0386 1.0000 Uani . . . . . . . C6 C 1.0055(3) 0.8448(2) 0.3333(4) 0.0456 1.0000 Uani . . . . . . . C7 C 0.9080(3) 0.7810(2) 0.3510(4) 0.0384 1.0000 Uani . . . . . . . C8 C 0.8719(2) 0.6809(2) 0.3638(3) 0.0269 1.0000 Uani . . . . . . . C9 C 0.7689(2) 0.6185(2) 0.3818(3) 0.0269 1.0000 Uani . . . . . . . N10 N 0.72674(17) 0.52651(17) 0.4013(3) 0.0255 1.0000 Uani . . . . . . . O11 O 0.62843(15) 0.48245(15) 0.4171(3) 0.0364 1.0000 Uani . . . . . . . O12 O 0.6667 0.3333 0.4444(4) 0.0248 1.0000 Uani S T . . . . . Cl13 Cl 0.6667 0.3333 0.14096(15) 0.0407 1.0000 Uani S T . . . . . O14 O 0.6667 0.3333 0.0060(5) 0.0608 1.0000 Uani S T . . . . . O15 O 0.5892(2) 0.3473(2) 0.1880(3) 0.0515 1.0000 Uani . . . . . . . N16 N 0.51441(18) 0.34285(18) 0.6228(3) 0.0295 1.0000 Uani . . . . . . . C17 C 0.4840(3) 0.4047(3) 0.6561(4) 0.0372 1.0000 Uani . . . . . . . C18 C 0.4512(3) 0.4075(3) 0.7759(4) 0.0469 1.0000 Uani . . . . . . . C19 C 0.4473(3) 0.3439(4) 0.8681(4) 0.0521 1.0000 Uani . U . . . . . C20 C 0.4813(3) 0.2809(3) 0.8335(4) 0.0463 1.0000 Uani . . . . . . . C21 C 0.5135(2) 0.2831(2) 0.7131(4) 0.0352 1.0000 Uani . . . . . . . C22 C 0.4031(5) 0.3364(5) 0.9983(5) 0.0832 1.0000 Uani D U . . . . . C23 C 0.2923(7) 0.2589(10) 0.9933(10) 0.1171 0.600(11) Uani D U P 1 1 . . C24 C 0.3622(13) 0.4037(13) 1.0118(12) 0.0840 0.400(11) Uani . U P 1 2 . . H41 H 1.0800 0.6861 0.3372 0.0362 1.0000 Uiso R . . . . . . H51 H 1.1357 0.8525 0.3131 0.0433 1.0000 Uiso R . . . . . . H61 H 1.0292 0.9124 0.3216 0.0523 1.0000 Uiso R . . . . . . H71 H 0.8644 0.8054 0.3527 0.0441 1.0000 Uiso R . . . . . . H91 H 0.7294 0.6481 0.3785 0.0319 1.0000 Uiso R . . . . . . H171 H 0.4862 0.4487 0.5945 0.0490 1.0000 Uiso R . . . . . . H181 H 0.4308 0.4513 0.7941 0.0615 1.0000 Uiso R . . . . . . H201 H 0.4815 0.2368 0.8943 0.0595 1.0000 Uiso R . . . . . . H211 H 0.5351 0.2392 0.6899 0.0434 1.0000 Uiso R . . . . . . H232 H 0.2719 0.2459 1.0811 0.1398 0.600(11) Uiso R . P 1 1 . . H231 H 0.2928 0.2054 0.9544 0.1402 0.600(11) Uiso R . P 1 1 . . H233 H 0.2586 0.2839 0.9451 0.1403 0.600(11) Uiso R . P 1 1 . . H242 H 0.3309 0.3942 1.0929 0.1490 0.400(11) Uiso R . P 1 2 . . H241 H 0.4138 0.4702 1.0046 0.1489 0.400(11) Uiso R . P 1 2 . . H243 H 0.3158 0.3890 0.9455 0.1490 0.400(11) Uiso R . P 1 2 . . H221 H 0.4372 0.3205 1.0588 0.1145 0.600(11) Uiso R . P 1 1 . . H222 H 0.4081 0.3967 1.0203 0.1145 0.600(11) Uiso R . P 1 1 . . H223 H 0.4530 0.3544 1.0597 0.1145 0.400(11) Uiso R . P 1 2 . . H224 H 0.3530 0.2715 1.0133 0.1145 0.400(11) Uiso R . P 1 2 . . 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 0.0146(2) 0.0156(2) 0.0479(3) 0.00313(18) 0.00075(18) 0.00786(18) O2 0.0197(10) 0.0188(10) 0.0594(15) 0.0008(10) 0.0074(10) 0.0086(9) C3 0.0233(14) 0.0202(14) 0.0308(15) -0.0027(11) -0.0010(12) 0.0079(12) C4 0.0212(15) 0.0249(15) 0.0412(18) 0.0001(13) 0.0029(13) 0.0058(12) C5 0.0221(15) 0.0248(16) 0.056(2) 0.0007(15) 0.0027(14) 0.0019(13) C6 0.0316(18) 0.0186(15) 0.075(3) 0.0048(16) 0.0030(17) 0.0040(14) C7 0.0320(17) 0.0216(15) 0.061(2) 0.0028(14) 0.0018(15) 0.0126(14) C8 0.0247(15) 0.0180(14) 0.0343(16) -0.0007(11) -0.0010(12) 0.0078(12) C9 0.0242(15) 0.0190(13) 0.0385(17) 0.0003(12) 0.0002(12) 0.0116(12) N10 0.0158(11) 0.0188(12) 0.0397(14) 0.0011(10) 0.0038(10) 0.0071(10) O11 0.0167(10) 0.0190(10) 0.0744(17) 0.0049(10) 0.0081(10) 0.0096(9) O12 0.0159(10) 0.0159(10) 0.043(2) 0.0000 0.0000 0.0079(5) Cl13 0.0402(5) 0.0402(5) 0.0417(8) 0.0000 0.0000 0.0201(2) O14 0.071(2) 0.071(2) 0.041(3) 0.0000 0.0000 0.0353(11) O15 0.0475(16) 0.0670(19) 0.0509(16) 0.0156(14) 0.0048(13) 0.0368(15) N16 0.0183(12) 0.0215(12) 0.0483(16) 0.0010(11) 0.0021(11) 0.0096(10) C17 0.0340(17) 0.0328(17) 0.051(2) 0.0014(15) 0.0022(15) 0.0212(15) C18 0.050(2) 0.053(2) 0.052(2) -0.0145(18) -0.0096(18) 0.037(2) C19 0.056(2) 0.073(3) 0.040(2) -0.0085(19) -0.0094(18) 0.042(2) C20 0.046(2) 0.048(2) 0.048(2) 0.0021(17) -0.0094(17) 0.0262(18) C21 0.0250(15) 0.0243(15) 0.056(2) -0.0007(14) -0.0047(14) 0.0120(13) C22 0.101(4) 0.128(4) 0.043(2) -0.004(3) -0.001(2) 0.074(3) C23 0.101(7) 0.172(9) 0.056(5) -0.009(6) 0.020(5) 0.052(6) C24 0.112(8) 0.126(8) 0.045(6) 0.001(6) 0.016(6) 0.083(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3930(8) 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 . N10 3_655 2.001(2) yes Mn1 . O2 3_655 1.871(2) yes Mn1 . Mn1 3_655 3.2465(7) yes Mn1 . O11 . 1.899(2) yes Mn1 . O12 . 1.8974(7) yes Mn1 . O15 . 2.463(3) yes Mn1 . N16 . 2.263(3) yes O2 . C3 . 1.319(4) yes C3 . C4 . 1.406(4) yes C3 . C8 . 1.409(4) yes C4 . C5 . 1.379(5) yes C4 . H41 . 0.968 no C5 . C6 . 1.382(5) yes C5 . H51 . 0.950 no C6 . C7 . 1.376(5) yes C6 . H61 . 0.953 no C7 . C8 . 1.402(4) yes C7 . H71 . 0.949 no C8 . C9 . 1.441(4) yes C9 . N10 . 1.285(4) yes C9 . H91 . 0.955 no N10 . O11 . 1.366(3) yes Cl13 . O15 5_665 1.445(3) yes Cl13 . O15 3_655 1.445(3) yes Cl13 . O14 . 1.422(5) yes Cl13 . O15 . 1.445(3) yes N16 . C17 . 1.342(4) yes N16 . C21 . 1.339(4) yes C17 . C18 . 1.375(5) yes C17 . H171 . 0.942 no C18 . C19 . 1.381(6) yes C18 . H181 . 0.925 no C19 . C20 . 1.405(6) yes C19 . C22 . 1.518(6) yes C20 . C21 . 1.361(6) yes C20 . H201 . 0.951 no C21 . H211 . 0.950 no C22 . C23 . 1.567(8) yes C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . C24 . 1.512(15) yes C22 . H223 . 0.950 no C22 . H224 . 0.950 no C23 . H232 . 0.967 no C23 . H231 . 0.948 no C23 . H233 . 0.957 no C24 . H242 . 0.962 no C24 . H241 . 0.964 no C24 . H243 . 0.956 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 N10 3_655 Mn1 . O2 3_655 89.89(10) yes N10 3_655 Mn1 . Mn1 3_655 59.51(7) yes O2 3_655 Mn1 . Mn1 3_655 146.75(7) yes N10 3_655 Mn1 . O11 . 175.22(11) yes O2 3_655 Mn1 . O11 . 87.00(9) yes Mn1 3_655 Mn1 . O11 . 122.55(6) yes N10 3_655 Mn1 . O12 . 90.12(7) yes O2 3_655 Mn1 . O12 . 172.55(14) yes Mn1 3_655 Mn1 . O12 . 31.18(3) yes O11 . Mn1 . O12 . 92.48(7) yes N10 3_655 Mn1 . O15 . 87.28(11) yes O2 3_655 Mn1 . O15 . 85.80(10) yes Mn1 3_655 Mn1 . O15 . 80.43(6) yes O11 . Mn1 . O15 . 88.87(11) yes O12 . Mn1 . O15 . 86.76(13) yes N10 3_655 Mn1 . N16 . 92.58(10) yes O2 3_655 Mn1 . N16 . 90.34(10) yes Mn1 3_655 Mn1 . N16 . 102.82(7) yes O11 . Mn1 . N16 . 91.07(10) yes O12 . Mn1 . N16 . 97.10(13) yes O15 . Mn1 . N16 . 176.13(9) yes Mn1 5_665 O2 . C3 . 130.84(19) yes O2 . C3 . C4 . 118.4(3) yes O2 . C3 . C8 . 123.6(3) yes C4 . C3 . C8 . 118.0(3) yes C3 . C4 . C5 . 120.9(3) yes C3 . C4 . H41 . 118.1 no C5 . C4 . H41 . 121.0 no C4 . C5 . C6 . 121.1(3) yes C4 . C5 . H51 . 119.6 no C6 . C5 . H51 . 119.3 no C5 . C6 . C7 . 119.0(3) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 120.9 no C6 . C7 . C8 . 121.4(3) yes C6 . C7 . H71 . 119.0 no C8 . C7 . H71 . 119.6 no C3 . C8 . C7 . 119.5(3) yes C3 . C8 . C9 . 122.1(3) yes C7 . C8 . C9 . 118.3(3) yes C8 . C9 . N10 . 124.9(3) yes C8 . C9 . H91 . 117.2 no N10 . C9 . H91 . 117.9 no Mn1 5_665 N10 . C9 . 127.2(2) yes Mn1 5_665 N10 . O11 . 118.26(17) yes C9 . N10 . O11 . 114.5(2) yes N10 . O11 . Mn1 . 118.56(16) yes Mn1 . O12 . Mn1 5_665 117.64(6) yes Mn1 . O12 . Mn1 3_655 117.64(6) yes Mn1 5_665 O12 . Mn1 3_655 117.64(6) yes O15 5_665 Cl13 . O15 3_655 108.89(13) yes O15 5_665 Cl13 . O14 . 110.05(13) yes O15 3_655 Cl13 . O14 . 110.05(13) yes O15 5_665 Cl13 . O15 . 108.89(13) yes O15 3_655 Cl13 . O15 . 108.89(13) yes O14 . Cl13 . O15 . 110.05(13) yes Mn1 . O15 . Cl13 . 122.05(16) yes Mn1 . N16 . C17 . 116.5(2) yes Mn1 . N16 . C21 . 126.4(2) yes C17 . N16 . C21 . 117.0(3) yes N16 . C17 . C18 . 123.0(3) yes N16 . C17 . H171 . 118.1 no C18 . C17 . H171 . 118.8 no C17 . C18 . C19 . 120.1(4) yes C17 . C18 . H181 . 119.8 no C19 . C18 . H181 . 120.1 no C18 . C19 . C20 . 116.6(4) yes C18 . C19 . C22 . 122.9(4) yes C20 . C19 . C22 . 120.4(4) yes C19 . C20 . C21 . 119.8(4) yes C19 . C20 . H201 . 119.7 no C21 . C20 . H201 . 120.5 no C20 . C21 . N16 . 123.4(3) yes C20 . C21 . H211 . 119.3 no N16 . C21 . H211 . 117.3 no C19 . C22 . C23 . 109.1(5) yes C19 . C22 . H221 . 108.9 no C23 . C22 . H221 . 112.3 no C19 . C22 . H222 . 109.8 no C23 . C22 . H222 . 107.3 no H221 . C22 . H222 . 109.5 no C19 . C22 . C24 . 112.1(6) yes C19 . C22 . H223 . 107.9 no C24 . C22 . H223 . 108.2 no C19 . C22 . H224 . 109.8 no C24 . C22 . H224 . 109.3 no H223 . C22 . H224 . 109.5 no C22 . C23 . H232 . 105.1 no C22 . C23 . H231 . 102.1 no H232 . C23 . H231 . 112.0 no C22 . C23 . H233 . 109.5 no H232 . C23 . H233 . 113.5 no H231 . C23 . H233 . 113.6 no C22 . C24 . H242 . 110.1 no C22 . C24 . H241 . 109.7 no H242 . C24 . H241 . 109.5 no C22 . C24 . H243 . 108.1 no H242 . C24 . H243 . 109.6 no H241 . C24 . H243 . 109.9 no # Attachment 'Complex 4.cif' data_EB7157 _database_code_depnum_ccdc_archive 'CCDC 736437' _audit_creation_date 07-11-05 _audit_creation_method CRYSTALS_ver_12.85 _chemical_formula_moiety 'C47 H37 Mn3 N6 O9, 1.5(C5 H5 N)' _chemical_compound_source 'Ross Inglis, RI62' _chemical_name_systematic ? _chemical_melting_point ? #looking for refcif # 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'. _exptl_crystal_recrystallization_method ; Slow evaporation of pyridine/ethanol. ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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. 601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 345.00 A**3 The solvent region was treated by the van der Sluis and Spek method, accounting for 120 e/cell. This corresponds to 1.5 molecules of pyridine per formula unit and F(000), M, mu, D and the formulae have been calculated on this assumption. 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.595 83 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 2 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 The data are 99% complete to d=0.8\%A. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 5001 4998 3 23.01 0.550 0.998 6641 6625 16 25.01 0.595 0.990 8406 8323 83 #----------------------------------------------------------- ACTA Min. Res. --- 097_ALERT_2_C Maximum (Positive) Residual Density ............ 2.06 e/A** 154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 300 Deg. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.30 Ratio 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 15 No action taken. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 12 Thermal similarity restriants were applied to O2 (to Mn1; esd=0.001) and O14 (to O21; esd=0.001). ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 10.3147(5) _cell_length_b 15.4284(7) _cell_length_c 16.1150(8) _cell_angle_alpha 106.695(3) _cell_angle_beta 101.405(3) _cell_angle_gamma 94.588(3) _cell_volume 2382.2(2) _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 2 # Given Formula = C54.50 H44.50 Mn3 N7.50 O9 # Dc = 1.55 Fooo = 1016.00 Mu = 8.52 M = 1113.28 # Found Formula = C47 H37 Mn3 N6 O9 # Dc = 1.39 FOOO = 1016.00 Mu = 8.42 M = 994.63 _chemical_formula_sum 'C54.5 H44.5 Mn3 N7.5 O9' _chemical_formula_weight 1113.28 _cell_measurement_reflns_used 9655 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.43 _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.852 # Sheldrick geometric approximatio 0.71 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.90 _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 '\f & \w scans' # 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 8323 _reflns_number_total 8323 _diffrn_reflns_av_R_equivalents 0.073 # Number of reflections with Friedels Law is 8323 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8398 _diffrn_reflns_theta_min 1.356 _diffrn_reflns_theta_max 25.007 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.007 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -18 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 1.09 _oxford_diffrn_Wilson_scale 134.41 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.29 _refine_diff_density_max 2.06 # 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 8322 _refine_ls_number_restraints 12 _refine_ls_number_parameters 586 _oxford_refine_ls_R_factor_ref 0.1358 _refine_ls_wR_factor_ref 0.2433 _refine_ls_goodness_of_fit_ref 1.0691 _refine_ls_shift/su_max 0.000329 # The values computed from all data _oxford_reflns_number_all 8322 _refine_ls_R_factor_all 0.1358 _refine_ls_wR_factor_all 0.2433 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5686 _refine_ls_R_factor_gt 0.1029 _refine_ls_wR_factor_gt 0.2282 # 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^) + ( 0.09P)^2^ + 7.39P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. 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 # 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 0.500 341.8 118.4 2 0.457 0.918 0.477 6.8 0.7 3 0.543 0.082 0.523 6.8 0.6 _platon_squeeze_details ; ; 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 0.00408(12) 0.33329(8) 0.08257(8) 0.0202 1.0000 Uani . U . . . . . O2 O 0.1518(5) 0.2922(3) 0.1453(4) 0.0204 1.0000 Uani . U . . . . . Mn3 Mn 0.12819(13) 0.17110(8) 0.14901(9) 0.0230 1.0000 Uani . . . . . . . O4 O -0.0269(6) 0.1371(4) 0.0548(4) 0.0328 1.0000 Uani . . . . . . . N5 N -0.0788(7) 0.2024(4) 0.0202(5) 0.0263 1.0000 Uani . . . . . . . C6 C -0.1768(9) 0.1728(6) -0.0482(6) 0.0289 1.0000 Uani . . . . . . . C7 C -0.2494(8) 0.2308(6) -0.0913(6) 0.0267 1.0000 Uani . . . . . . . C8 C -0.2267(8) 0.3259(6) -0.0551(6) 0.0228 1.0000 Uani . . . . . . . O9 O -0.1400(5) 0.3720(4) 0.0185(4) 0.0258 1.0000 Uani . . . . . . . C10 C -0.3082(8) 0.3759(7) -0.1015(6) 0.0312 1.0000 Uani . . . . . . . C11 C -0.4045(9) 0.3327(7) -0.1784(7) 0.0394 1.0000 Uani . . . . . . . C12 C -0.4248(10) 0.2386(7) -0.2129(6) 0.0395 1.0000 Uani . . . . . . . C13 C -0.3477(9) 0.1890(6) -0.1701(6) 0.0369 1.0000 Uani . . . . . . . O14 O 0.0802(6) 0.0566(4) 0.1620(4) 0.0317 1.0000 Uani . U . . . . . C15 C 0.1173(9) 0.0200(6) 0.2267(6) 0.0309 1.0000 Uani . . . . . . . C16 C 0.2191(9) 0.0663(6) 0.3042(6) 0.0321 1.0000 Uani . . . . . . . C17 C 0.2836(9) 0.1578(7) 0.3207(5) 0.0320 1.0000 Uani . . . . . . . N18 N 0.2599(7) 0.2055(5) 0.2663(5) 0.0274 1.0000 Uani . . . . . . . O19 O 0.3343(6) 0.2904(4) 0.2935(4) 0.0278 1.0000 Uani . . . . . . . Mn20 Mn 0.23483(12) 0.38035(8) 0.25998(9) 0.0217 1.0000 Uani . . . . . . . O21 O 0.3130(6) 0.4634(4) 0.3727(4) 0.0320 1.0000 Uani . U . . . . . C22 C 0.3131(9) 0.5528(6) 0.4057(6) 0.0293 1.0000 Uani . . . . . . . C23 C 0.2510(8) 0.6066(6) 0.3559(6) 0.0285 1.0000 Uani . . . . . . . C24 C 0.1782(8) 0.5671(6) 0.2647(6) 0.0259 1.0000 Uani . . . . . . . N25 N 0.1545(6) 0.4809(4) 0.2207(4) 0.0211 1.0000 Uani . . . . . . . O26 O 0.0849(6) 0.4588(3) 0.1348(4) 0.0262 1.0000 Uani . . . . . . . C27 C 0.2602(10) 0.7017(6) 0.3964(7) 0.0405 1.0000 Uani . . . . . . . C28 C 0.3199(11) 0.7404(6) 0.4828(7) 0.0454 1.0000 Uani . . . . . . . C29 C 0.3772(10) 0.6882(7) 0.5339(7) 0.0401 1.0000 Uani . . . . . . . C30 C 0.3745(10) 0.5969(7) 0.4952(6) 0.0380 1.0000 Uani . . . . . . . O31 O 0.0604(6) 0.3290(5) 0.3013(4) 0.0395 1.0000 Uani . . . . . . . C32 C -0.0570(9) 0.3045(6) 0.2523(6) 0.0311 1.0000 Uani . . . . . . . O33 O -0.1034(6) 0.3293(4) 0.1866(4) 0.0317 1.0000 Uani . . . . . . . C34 C -0.1450(9) 0.2347(6) 0.2736(6) 0.0319 1.0000 Uani . . . . . . . C35 C -0.2857(8) 0.2197(6) 0.2386(6) 0.0309 1.0000 Uani . . . . . . . C36 C -0.3655(9) 0.1555(6) 0.2560(6) 0.0341 1.0000 Uani . . . . . . . C37 C -0.3115(10) 0.1000(6) 0.3058(6) 0.0342 1.0000 Uani . . . . . . . C38 C -0.1706(9) 0.1138(7) 0.3409(7) 0.0382 1.0000 Uani . . . . . . . C39 C -0.0924(10) 0.1820(7) 0.3232(6) 0.0386 1.0000 Uani . . . . . . . C40 C -0.1162(14) 0.0572(10) 0.3889(9) 0.0658 1.0000 Uani . . . . . . . C41 C -0.1963(16) -0.0069(10) 0.4052(10) 0.0763 1.0000 Uani . . . . . . . C42 C -0.3361(16) -0.0192(8) 0.3718(8) 0.0654 1.0000 Uani . . . . . . . C43 C -0.3900(12) 0.0324(7) 0.3252(8) 0.0528 1.0000 Uani . . . . . . . N44 N 0.4166(7) 0.4219(4) 0.2077(5) 0.0253 1.0000 Uani . . . . . . . C45 C 0.5393(9) 0.4426(6) 0.2589(7) 0.0346 1.0000 Uani . . . . . . . C46 C 0.6522(9) 0.4485(7) 0.2250(8) 0.0448 1.0000 Uani . . . . . . . C47 C 0.6384(9) 0.4301(7) 0.1366(7) 0.0398 1.0000 Uani . . . . . . . C48 C 0.5114(10) 0.4119(7) 0.0817(7) 0.0395 1.0000 Uani . . . . . . . C49 C 0.4031(9) 0.4073(6) 0.1210(6) 0.0314 1.0000 Uani . . . . . . . C50 C 0.2527(11) 0.0230(7) 0.3697(7) 0.0432 1.0000 Uani . . . . . . . C51 C 0.1883(11) -0.0636(6) 0.3583(7) 0.0437 1.0000 Uani . . . . . . . C52 C 0.0907(11) -0.1065(6) 0.2825(7) 0.0431 1.0000 Uani . . . . . . . C53 C 0.0542(10) -0.0658(6) 0.2184(7) 0.0377 1.0000 Uani . . . . . . . N54 N 0.2699(7) 0.1223(5) 0.0643(5) 0.0272 1.0000 Uani . . . . . . . C55 C 0.3901(9) 0.1689(6) 0.0726(7) 0.0328 1.0000 Uani . . . . . . . C56 C 0.4666(10) 0.1455(7) 0.0121(8) 0.0461 1.0000 Uani . . . . . . . C57 C 0.4186(11) 0.0712(8) -0.0620(8) 0.0548 1.0000 Uani . . . . . . . C58 C 0.2929(11) 0.0214(7) -0.0738(7) 0.0465 1.0000 Uani . . . . . . . C59 C 0.2237(10) 0.0501(6) -0.0087(6) 0.0329 1.0000 Uani . . . . . . . N60 N 0.1013(7) 0.3245(4) -0.0420(5) 0.0250 1.0000 Uani . . . . . . . C61 C 0.1778(9) 0.2617(6) -0.0713(6) 0.0320 1.0000 Uani . . . . . . . C62 C 0.2362(10) 0.2607(8) -0.1401(7) 0.0446 1.0000 Uani . . . . . . . C63 C 0.2168(10) 0.3251(8) -0.1825(7) 0.0502 1.0000 Uani . . . . . . . C64 C 0.1370(9) 0.3898(7) -0.1537(7) 0.0391 1.0000 Uani . . . . . . . C65 C 0.0825(8) 0.3880(6) -0.0835(6) 0.0284 1.0000 Uani . . . . . . . H61 H -0.2028 0.1101 -0.0721 0.0330 1.0000 Uiso R . . . . . . H101 H -0.2950 0.4397 -0.0790 0.0371 1.0000 Uiso R . . . . . . H111 H -0.4572 0.3668 -0.2066 0.0512 1.0000 Uiso R . . . . . . H121 H -0.4892 0.2088 -0.2657 0.0461 1.0000 Uiso R . . . . . . H131 H -0.3596 0.1254 -0.1938 0.0429 1.0000 Uiso R . . . . . . H171 H 0.3465 0.1846 0.3745 0.0381 1.0000 Uiso R . . . . . . H241 H 0.1450 0.6076 0.2358 0.0322 1.0000 Uiso R . . . . . . H271 H 0.2237 0.7376 0.3628 0.0402 1.0000 Uiso R . . . . . . H281 H 0.3233 0.8030 0.5093 0.0460 1.0000 Uiso R . . . . . . H291 H 0.4163 0.7155 0.5941 0.0450 1.0000 Uiso R . . . . . . H301 H 0.4149 0.5627 0.5288 0.0441 1.0000 Uiso R . . . . . . H351 H -0.3232 0.2543 0.2040 0.0312 1.0000 Uiso R . . . . . . H361 H -0.4577 0.1479 0.2349 0.0371 1.0000 Uiso R . . . . . . H391 H 0.0000 0.1925 0.3472 0.0501 1.0000 Uiso R . . . . . . H401 H -0.0240 0.0650 0.4109 0.0881 1.0000 Uiso R . . . . . . H411 H -0.1588 -0.0439 0.4372 0.0911 1.0000 Uiso R . . . . . . H421 H -0.3897 -0.0634 0.3838 0.0770 1.0000 Uiso R . . . . . . H431 H -0.4820 0.0243 0.3044 0.0581 1.0000 Uiso R . . . . . . H451 H 0.5486 0.4535 0.3204 0.0412 1.0000 Uiso R . . . . . . H461 H 0.7367 0.4655 0.2639 0.0572 1.0000 Uiso R . . . . . . H471 H 0.7127 0.4296 0.1128 0.0491 1.0000 Uiso R . . . . . . H481 H 0.4990 0.4032 0.0209 0.0511 1.0000 Uiso R . . . . . . H491 H 0.3176 0.3932 0.0853 0.0360 1.0000 Uiso R . . . . . . H501 H 0.3191 0.0531 0.4211 0.0521 1.0000 Uiso R . . . . . . H511 H 0.2102 -0.0920 0.4023 0.0492 1.0000 Uiso R . . . . . . H521 H 0.0497 -0.1646 0.2754 0.0521 1.0000 Uiso R . . . . . . H531 H -0.0131 -0.0959 0.1684 0.0461 1.0000 Uiso R . . . . . . H551 H 0.4228 0.2194 0.1232 0.0361 1.0000 Uiso R . . . . . . H561 H 0.5491 0.1792 0.0209 0.0531 1.0000 Uiso R . . . . . . H571 H 0.4684 0.0532 -0.1050 0.0600 1.0000 Uiso R . . . . . . H581 H 0.2579 -0.0291 -0.1240 0.0552 1.0000 Uiso R . . . . . . H591 H 0.1401 0.0181 -0.0153 0.0371 1.0000 Uiso R . . . . . . H611 H 0.1913 0.2173 -0.0436 0.0361 1.0000 Uiso R . . . . . . H621 H 0.2898 0.2165 -0.1583 0.0501 1.0000 Uiso R . . . . . . H631 H 0.2561 0.3249 -0.2301 0.0581 1.0000 Uiso R . . . . . . H641 H 0.1200 0.4336 -0.1825 0.0462 1.0000 Uiso R . . . . . . H651 H 0.0304 0.4322 -0.0629 0.0310 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 0.0171(6) 0.0147(6) 0.0271(7) 0.0079(5) 0.0005(5) -0.0004(5) O2 0.0182(11) 0.0138(11) 0.0276(11) 0.0084(10) 0.0000(10) -0.0005(10) Mn3 0.0227(7) 0.0151(6) 0.0292(8) 0.0093(5) -0.0002(5) -0.0018(5) O4 0.031(3) 0.019(3) 0.045(4) 0.016(3) -0.007(3) -0.001(3) N5 0.027(4) 0.016(4) 0.036(4) 0.011(3) 0.007(3) -0.002(3) C6 0.031(5) 0.017(4) 0.033(5) 0.004(4) 0.004(4) -0.010(4) C7 0.020(4) 0.029(5) 0.029(5) 0.010(4) 0.005(4) -0.008(4) C8 0.013(4) 0.030(5) 0.026(5) 0.013(4) 0.001(3) 0.001(3) O9 0.021(3) 0.023(3) 0.029(3) 0.008(3) -0.005(2) 0.002(2) C10 0.024(5) 0.035(5) 0.038(6) 0.017(4) 0.006(4) 0.007(4) C11 0.022(5) 0.055(7) 0.044(6) 0.031(5) -0.008(4) 0.004(4) C12 0.045(6) 0.039(6) 0.027(5) 0.015(4) -0.008(4) -0.016(5) C13 0.037(5) 0.027(5) 0.039(6) 0.009(4) -0.003(4) -0.011(4) O14 0.037(3) 0.019(2) 0.036(3) 0.011(2) 0.002(2) -0.0031(19) C15 0.043(5) 0.021(4) 0.044(6) 0.023(4) 0.023(5) 0.010(4) C16 0.038(5) 0.019(4) 0.043(6) 0.017(4) 0.005(4) 0.003(4) C17 0.033(5) 0.049(6) 0.011(4) 0.010(4) -0.004(4) 0.005(4) N18 0.029(4) 0.023(4) 0.028(4) 0.008(3) 0.001(3) 0.000(3) O19 0.025(3) 0.017(3) 0.035(4) 0.011(3) -0.009(3) -0.003(2) Mn20 0.0200(6) 0.0186(6) 0.0258(7) 0.0088(5) 0.0013(5) 0.0014(5) O21 0.037(3) 0.020(2) 0.036(3) 0.010(2) 0.003(2) -0.0024(19) C22 0.041(5) 0.027(5) 0.018(5) 0.003(4) 0.010(4) 0.004(4) C23 0.022(4) 0.031(5) 0.025(5) 0.002(4) -0.003(4) 0.001(4) C24 0.024(4) 0.026(5) 0.033(5) 0.012(4) 0.010(4) 0.013(4) N25 0.020(3) 0.015(3) 0.028(4) 0.006(3) 0.005(3) 0.002(3) O26 0.037(3) 0.009(3) 0.027(3) 0.005(2) -0.003(3) -0.001(2) C27 0.051(6) 0.015(4) 0.041(6) -0.004(4) -0.005(5) 0.004(4) C28 0.053(6) 0.019(5) 0.043(6) -0.013(4) 0.000(5) 0.000(4) C29 0.048(6) 0.031(5) 0.036(6) 0.005(4) 0.005(5) 0.010(5) C30 0.037(5) 0.051(6) 0.033(6) 0.023(5) 0.007(4) 0.011(5) O31 0.021(3) 0.060(5) 0.036(4) 0.020(3) -0.001(3) -0.002(3) C32 0.035(5) 0.040(5) 0.021(5) 0.012(4) 0.009(4) 0.001(4) O33 0.024(3) 0.044(4) 0.032(4) 0.017(3) 0.009(3) 0.006(3) C34 0.031(5) 0.032(5) 0.033(5) 0.009(4) 0.008(4) 0.007(4) C35 0.020(4) 0.031(5) 0.035(5) 0.007(4) -0.003(4) 0.003(4) C36 0.023(5) 0.031(5) 0.041(6) 0.003(4) 0.006(4) -0.003(4) C37 0.045(6) 0.025(5) 0.027(5) -0.002(4) 0.013(4) -0.001(4) C38 0.029(5) 0.048(6) 0.045(6) 0.023(5) 0.010(4) 0.013(4) C39 0.033(5) 0.053(6) 0.036(6) 0.021(5) 0.010(4) 0.006(5) C40 0.063(8) 0.090(10) 0.068(9) 0.053(8) 0.024(7) 0.019(7) C41 0.088(11) 0.080(10) 0.081(10) 0.053(9) 0.020(9) 0.020(8) C42 0.109(12) 0.043(7) 0.049(8) 0.021(6) 0.030(8) -0.010(7) C43 0.054(7) 0.042(6) 0.053(7) 0.007(6) 0.012(6) -0.014(5) N44 0.023(4) 0.012(3) 0.042(5) 0.013(3) 0.004(3) 0.003(3) C45 0.031(5) 0.034(5) 0.038(6) 0.012(4) 0.005(4) 0.004(4) C46 0.020(5) 0.049(6) 0.070(8) 0.026(6) 0.010(5) 0.007(4) C47 0.030(5) 0.035(5) 0.061(7) 0.014(5) 0.026(5) 0.006(4) C48 0.038(6) 0.036(6) 0.051(6) 0.016(5) 0.021(5) 0.008(4) C49 0.022(4) 0.024(5) 0.046(6) 0.013(4) -0.001(4) 0.002(4) C50 0.049(6) 0.042(6) 0.038(6) 0.017(5) 0.004(5) 0.003(5) C51 0.072(8) 0.018(5) 0.045(6) 0.021(4) 0.007(5) 0.000(5) C52 0.054(7) 0.020(5) 0.054(7) 0.016(5) 0.008(5) -0.006(4) C53 0.041(6) 0.029(5) 0.040(6) 0.014(4) 0.000(5) 0.000(4) N54 0.024(4) 0.024(4) 0.031(4) 0.008(3) 0.001(3) 0.009(3) C55 0.030(5) 0.017(4) 0.043(6) 0.006(4) -0.004(4) -0.001(4) C56 0.029(5) 0.040(6) 0.071(8) 0.020(6) 0.013(5) 0.005(4) C57 0.046(7) 0.058(8) 0.061(8) 0.011(6) 0.020(6) 0.022(6) C58 0.052(7) 0.041(6) 0.045(7) 0.010(5) 0.008(5) 0.017(5) C59 0.037(5) 0.021(5) 0.041(6) 0.013(4) 0.003(4) 0.003(4) N60 0.024(4) 0.017(3) 0.029(4) 0.006(3) -0.003(3) -0.003(3) C61 0.027(5) 0.026(5) 0.040(6) 0.014(4) -0.005(4) 0.006(4) C62 0.034(6) 0.049(7) 0.047(7) 0.009(5) 0.008(5) 0.014(5) C63 0.031(5) 0.078(8) 0.047(7) 0.025(6) 0.015(5) 0.000(5) C64 0.025(5) 0.056(7) 0.043(6) 0.029(5) 0.005(4) 0.001(4) C65 0.019(4) 0.025(5) 0.033(5) 0.009(4) -0.010(4) -0.003(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3054(5) 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 . O2 . 1.912(5) yes Mn1 . Mn3 . 3.2492(17) yes Mn1 . N5 . 2.009(7) yes Mn1 . O9 . 1.876(6) yes Mn1 . Mn20 . 3.1947(17) yes Mn1 . O26 . 1.919(5) yes Mn1 . O33 . 2.197(6) yes Mn1 . N60 . 2.390(7) yes O2 . Mn3 . 1.885(5) yes O2 . Mn20 . 1.934(5) yes Mn3 . O4 . 1.894(6) yes Mn3 . O14 . 1.878(6) yes Mn3 . N18 . 1.998(7) yes Mn3 . N54 . 2.223(7) yes O4 . N5 . 1.380(9) yes N5 . C6 . 1.281(11) yes C6 . C7 . 1.451(12) yes C6 . H61 . 0.926 no C7 . C8 . 1.395(12) yes C7 . C13 . 1.404(12) yes C8 . O9 . 1.307(9) yes C8 . C10 . 1.431(12) yes C10 . C11 . 1.378(12) yes C10 . H101 . 0.934 no C11 . C12 . 1.379(14) yes C11 . H111 . 0.930 no C12 . C13 . 1.371(14) yes C12 . H121 . 0.938 no C13 . H131 . 0.932 no O14 . C15 . 1.329(10) yes C15 . C16 . 1.421(13) yes C15 . C53 . 1.385(12) yes C16 . C17 . 1.439(12) yes C16 . C50 . 1.406(13) yes C17 . N18 . 1.299(11) yes C17 . H171 . 0.934 no N18 . O19 . 1.368(8) yes O19 . Mn20 . 1.927(6) yes Mn20 . O21 . 1.874(6) yes Mn20 . N25 . 2.014(7) yes Mn20 . O31 . 2.204(6) yes Mn20 . N44 . 2.319(7) yes O21 . C22 . 1.328(10) yes C22 . C23 . 1.416(12) yes C22 . C30 . 1.397(12) yes C23 . C24 . 1.439(12) yes C23 . C27 . 1.411(12) yes C24 . N25 . 1.292(10) yes C24 . H241 . 0.928 no N25 . O26 . 1.359(8) yes C27 . C28 . 1.341(13) yes C27 . H271 . 0.930 no C28 . C29 . 1.392(14) yes C28 . H281 . 0.932 no C29 . C30 . 1.363(13) yes C29 . H291 . 0.930 no C30 . H301 . 0.925 no O31 . C32 . 1.269(11) yes C32 . O33 . 1.248(10) yes C32 . C34 . 1.510(13) yes C34 . C35 . 1.423(12) yes C34 . C39 . 1.368(13) yes C35 . C36 . 1.362(13) yes C35 . H351 . 0.930 no C36 . C37 . 1.408(14) yes C36 . H361 . 0.930 no C37 . C38 . 1.425(13) yes C37 . C43 . 1.413(14) yes C38 . C39 . 1.402(13) yes C38 . C40 . 1.404(15) yes C39 . H391 . 0.937 no C40 . C41 . 1.354(18) yes C40 . H401 . 0.932 no C41 . C42 . 1.413(19) yes C41 . H411 . 0.931 no C42 . C43 . 1.324(17) yes C42 . H421 . 0.931 no C43 . H431 . 0.927 no N44 . C45 . 1.325(11) yes N44 . C49 . 1.327(12) yes C45 . C46 . 1.388(13) yes C45 . H451 . 0.939 no C46 . C47 . 1.345(14) yes C46 . H461 . 0.935 no C47 . C48 . 1.384(14) yes C47 . H471 . 0.923 no C48 . C49 . 1.395(13) yes C48 . H481 . 0.932 no C49 . H491 . 0.924 no C50 . C51 . 1.389(13) yes C50 . H501 . 0.935 no C51 . C52 . 1.374(14) yes C51 . H511 . 0.936 no C52 . C53 . 1.363(13) yes C52 . H521 . 0.926 no C53 . H531 . 0.926 no N54 . C55 . 1.345(11) yes N54 . C59 . 1.338(11) yes C55 . C56 . 1.360(14) yes C55 . H551 . 0.933 no C56 . C57 . 1.369(15) yes C56 . H561 . 0.924 no C57 . C58 . 1.402(15) yes C57 . H571 . 0.935 no C58 . C59 . 1.374(14) yes C58 . H581 . 0.932 no C59 . H591 . 0.930 no N60 . C61 . 1.339(11) yes N60 . C65 . 1.341(11) yes C61 . C62 . 1.358(14) yes C61 . H611 . 0.924 no C62 . C63 . 1.365(15) yes C62 . H621 . 0.931 no C63 . C64 . 1.381(15) yes C63 . H631 . 0.935 no C64 . C65 . 1.365(13) yes C64 . H641 . 0.933 no C65 . H651 . 0.930 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 O2 . Mn1 . Mn3 . 30.92(15) yes O2 . Mn1 . N5 . 89.4(3) yes Mn3 . Mn1 . N5 . 60.1(2) yes O2 . Mn1 . O9 . 178.7(3) yes Mn3 . Mn1 . O9 . 148.75(17) yes N5 . Mn1 . O9 . 89.9(3) yes O2 . Mn1 . Mn20 . 34.08(16) yes Mn3 . Mn1 . Mn20 . 59.31(4) yes N5 . Mn1 . Mn20 . 119.1(2) yes O9 . Mn1 . Mn20 . 147.06(18) yes O2 . Mn1 . O26 . 92.0(2) yes Mn3 . Mn1 . O26 . 121.86(18) yes N5 . Mn1 . O26 . 176.3(3) yes O9 . Mn1 . O26 . 88.6(2) yes Mn20 . Mn1 . O26 . 63.40(17) yes O2 . Mn1 . O33 . 89.5(2) yes Mn3 . Mn1 . O33 . 79.11(17) yes N5 . Mn1 . O33 . 87.1(3) yes O9 . Mn1 . O33 . 91.6(2) yes Mn20 . Mn1 . O33 . 75.79(16) yes O2 . Mn1 . N60 . 93.4(2) yes Mn3 . Mn1 . N60 . 100.52(17) yes N5 . Mn1 . N60 . 87.1(3) yes O9 . Mn1 . N60 . 85.4(2) yes Mn20 . Mn1 . N60 . 109.70(16) yes O26 . Mn1 . O33 . 96.3(3) yes O26 . Mn1 . N60 . 89.4(2) yes O33 . Mn1 . N60 . 173.5(2) yes Mn1 . O2 . Mn3 . 117.7(3) yes Mn1 . O2 . Mn20 . 112.3(3) yes Mn3 . O2 . Mn20 . 113.2(3) yes O2 . Mn3 . Mn1 . 31.42(16) yes O2 . Mn3 . O4 . 92.7(2) yes Mn1 . Mn3 . O4 . 62.57(17) yes O2 . Mn3 . O14 . 170.1(3) yes Mn1 . Mn3 . O14 . 142.5(2) yes O4 . Mn3 . O14 . 84.7(3) yes O2 . Mn3 . N18 . 91.3(3) yes Mn1 . Mn3 . N18 . 118.3(2) yes O4 . Mn3 . N18 . 166.2(3) yes O14 . Mn3 . N18 . 89.2(3) yes O2 . Mn3 . N54 . 95.1(3) yes Mn1 . Mn3 . N54 . 105.65(19) yes O4 . Mn3 . N54 . 95.9(3) yes O14 . Mn3 . N54 . 94.7(3) yes N18 . Mn3 . N54 . 97.0(3) yes Mn3 . O4 . N5 . 119.8(5) yes O4 . N5 . Mn1 . 117.2(5) yes O4 . N5 . C6 . 116.0(7) yes Mn1 . N5 . C6 . 126.9(6) yes N5 . C6 . C7 . 124.3(8) yes N5 . C6 . H61 . 118.1 no C7 . C6 . H61 . 117.6 no C6 . C7 . C8 . 121.8(7) yes C6 . C7 . C13 . 118.4(8) yes C8 . C7 . C13 . 119.8(8) yes C7 . C8 . O9 . 125.2(8) yes C7 . C8 . C10 . 116.8(8) yes O9 . C8 . C10 . 118.0(8) yes C8 . O9 . Mn1 . 129.1(5) yes C8 . C10 . C11 . 121.9(9) yes C8 . C10 . H101 . 118.8 no C11 . C10 . H101 . 119.3 no C10 . C11 . C12 . 120.2(9) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 119.7 no C11 . C12 . C13 . 119.2(8) yes C11 . C12 . H121 . 120.6 no C13 . C12 . H121 . 120.2 no C7 . C13 . C12 . 122.1(9) yes C7 . C13 . H131 . 118.3 no C12 . C13 . H131 . 119.5 no Mn3 . O14 . C15 . 133.2(6) yes O14 . C15 . C16 . 122.1(8) yes O14 . C15 . C53 . 118.8(9) yes C16 . C15 . C53 . 119.1(8) yes C15 . C16 . C17 . 122.6(8) yes C15 . C16 . C50 . 118.7(8) yes C17 . C16 . C50 . 118.6(8) yes C16 . C17 . N18 . 124.5(8) yes C16 . C17 . H171 . 117.5 no N18 . C17 . H171 . 118.0 no Mn3 . N18 . C17 . 128.3(6) yes Mn3 . N18 . O19 . 116.3(5) yes C17 . N18 . O19 . 115.4(7) yes N18 . O19 . Mn20 . 112.6(5) yes O2 . Mn20 . O19 . 90.5(2) yes O2 . Mn20 . Mn1 . 33.63(16) yes O19 . Mn20 . Mn1 . 123.28(17) yes O2 . Mn20 . O21 . 178.3(3) yes O19 . Mn20 . O21 . 88.6(3) yes Mn1 . Mn20 . O21 . 146.8(2) yes O2 . Mn20 . N25 . 90.7(2) yes O19 . Mn20 . N25 . 171.9(3) yes Mn1 . Mn20 . N25 . 59.37(19) yes O21 . Mn20 . N25 . 90.4(3) yes O2 . Mn20 . O31 . 84.2(2) yes O19 . Mn20 . O31 . 91.0(3) yes Mn1 . Mn20 . O31 . 77.84(17) yes O21 . Mn20 . O31 . 94.3(3) yes N25 . Mn20 . O31 . 97.1(3) yes O2 . Mn20 . N44 . 91.5(2) yes O19 . Mn20 . N44 . 86.5(2) yes Mn1 . Mn20 . N44 . 99.92(18) yes O21 . Mn20 . N44 . 89.9(3) yes N25 . Mn20 . N44 . 85.4(2) yes O31 . Mn20 . N44 . 175.0(3) yes Mn20 . O21 . C22 . 131.3(6) yes O21 . C22 . C23 . 123.8(8) yes O21 . C22 . C30 . 118.8(8) yes C23 . C22 . C30 . 117.4(8) yes C22 . C23 . C24 . 121.9(8) yes C22 . C23 . C27 . 119.4(8) yes C24 . C23 . C27 . 118.6(8) yes C23 . C24 . N25 . 125.6(8) yes C23 . C24 . H241 . 116.4 no N25 . C24 . H241 . 118.0 no Mn20 . N25 . C24 . 126.4(6) yes Mn20 . N25 . O26 . 117.1(5) yes C24 . N25 . O26 . 115.7(7) yes N25 . O26 . Mn1 . 114.7(4) yes C23 . C27 . C28 . 120.5(10) yes C23 . C27 . H271 . 119.5 no C28 . C27 . H271 . 119.9 no C27 . C28 . C29 . 120.9(9) yes C27 . C28 . H281 . 119.9 no C29 . C28 . H281 . 119.1 no C28 . C29 . C30 . 119.5(9) yes C28 . C29 . H291 . 120.2 no C30 . C29 . H291 . 120.3 no C22 . C30 . C29 . 122.1(9) yes C22 . C30 . H301 . 118.5 no C29 . C30 . H301 . 119.4 no Mn20 . O31 . C32 . 124.7(6) yes O31 . C32 . O33 . 126.3(8) yes O31 . C32 . C34 . 115.9(8) yes O33 . C32 . C34 . 117.7(8) yes Mn1 . O33 . C32 . 123.4(6) yes C32 . C34 . C35 . 120.2(8) yes C32 . C34 . C39 . 121.5(8) yes C35 . C34 . C39 . 118.2(9) yes C34 . C35 . C36 . 120.5(9) yes C34 . C35 . H351 . 119.5 no C36 . C35 . H351 . 120.0 no C35 . C36 . C37 . 121.4(9) yes C35 . C36 . H361 . 119.8 no C37 . C36 . H361 . 118.8 no C36 . C37 . C38 . 118.8(8) yes C36 . C37 . C43 . 123.5(10) yes C38 . C37 . C43 . 117.7(10) yes C37 . C38 . C39 . 118.0(9) yes C37 . C38 . C40 . 118.9(10) yes C39 . C38 . C40 . 123.0(10) yes C38 . C39 . C34 . 123.0(9) yes C38 . C39 . H391 . 118.6 no C34 . C39 . H391 . 118.4 no C38 . C40 . C41 . 120.7(12) yes C38 . C40 . H401 . 119.4 no C41 . C40 . H401 . 119.9 no C40 . C41 . C42 . 120.1(13) yes C40 . C41 . H411 . 119.8 no C42 . C41 . H411 . 120.1 no C41 . C42 . C43 . 120.4(12) yes C41 . C42 . H421 . 118.9 no C43 . C42 . H421 . 120.6 no C37 . C43 . C42 . 122.0(12) yes C37 . C43 . H431 . 118.3 no C42 . C43 . H431 . 119.7 no Mn20 . N44 . C45 . 121.4(6) yes Mn20 . N44 . C49 . 119.4(5) yes C45 . N44 . C49 . 117.9(8) yes N44 . C45 . C46 . 122.5(10) yes N44 . C45 . H451 . 117.6 no C46 . C45 . H451 . 119.9 no C45 . C46 . C47 . 119.5(9) yes C45 . C46 . H461 . 119.5 no C47 . C46 . H461 . 121.0 no C46 . C47 . C48 . 119.4(9) yes C46 . C47 . H471 . 120.4 no C48 . C47 . H471 . 120.2 no C47 . C48 . C49 . 117.5(10) yes C47 . C48 . H481 . 121.2 no C49 . C48 . H481 . 121.4 no C48 . C49 . N44 . 123.1(8) yes C48 . C49 . H491 . 119.0 no N44 . C49 . H491 . 117.9 no C16 . C50 . C51 . 120.5(9) yes C16 . C50 . H501 . 119.3 no C51 . C50 . H501 . 120.2 no C50 . C51 . C52 . 119.3(9) yes C50 . C51 . H511 . 120.4 no C52 . C51 . H511 . 120.4 no C51 . C52 . C53 . 121.7(9) yes C51 . C52 . H521 . 118.3 no C53 . C52 . H521 . 120.0 no C15 . C53 . C52 . 120.7(9) yes C15 . C53 . H531 . 119.5 no C52 . C53 . H531 . 119.8 no Mn3 . N54 . C55 . 124.3(6) yes Mn3 . N54 . C59 . 117.4(6) yes C55 . N54 . C59 . 117.3(8) yes N54 . C55 . C56 . 123.6(9) yes N54 . C55 . H551 . 117.7 no C56 . C55 . H551 . 118.7 no C55 . C56 . C57 . 118.6(10) yes C55 . C56 . H561 . 120.6 no C57 . C56 . H561 . 120.8 no C56 . C57 . C58 . 119.6(10) yes C56 . C57 . H571 . 120.9 no C58 . C57 . H571 . 119.5 no C57 . C58 . C59 . 117.4(10) yes C57 . C58 . H581 . 121.1 no C59 . C58 . H581 . 121.5 no C58 . C59 . N54 . 123.6(9) yes C58 . C59 . H591 . 118.6 no N54 . C59 . H591 . 117.8 no Mn1 . N60 . C61 . 124.0(6) yes Mn1 . N60 . C65 . 118.5(6) yes C61 . N60 . C65 . 117.5(8) yes N60 . C61 . C62 . 122.6(9) yes N60 . C61 . H611 . 118.5 no C62 . C61 . H611 . 118.9 no C61 . C62 . C63 . 119.9(10) yes C61 . C62 . H621 . 120.4 no C63 . C62 . H621 . 119.7 no C62 . C63 . C64 . 118.2(10) yes C62 . C63 . H631 . 120.7 no C64 . C63 . H631 . 121.1 no C63 . C64 . C65 . 119.2(10) yes C63 . C64 . H641 . 120.1 no C65 . C64 . H641 . 120.7 no C64 . C65 . N60 . 122.6(9) yes C64 . C65 . H651 . 119.6 no N60 . C65 . H651 . 117.8 no # Attachment 'Complex 7.cif' data_eb7066 _database_code_depnum_ccdc_archive 'CCDC 736438' _audit_creation_date 07-05-15 _audit_creation_method CRYSTALS_ver_12.84 _chemical_compound_source C.Milios _exptl_crystal_recrystallization_method ; Slow evaporation of a Methanol solution ; _oxford_structure_analysis_title 'eb7066bis in P2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 15.0333(7) _cell_length_b 8.6770(4) _cell_length_c 16.8357(8) _cell_angle_alpha 90 _cell_angle_beta 99.936(3) _cell_angle_gamma 90 _cell_volume 2163.18(18) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-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 2 # Given Formula = C39 H53 Mn3 N4 O16 # Dc = 1.53 Fooo = 1036.00 Mu = 9.38 M = 998.65 # Found Formula = C39 H53 Mn3 N4 O16 # Dc = 1.53 FOOO = 1036.00 Mu = 9.38 M = 998.65 _chemical_formula_sum 'C39 H53 Mn3 N4 O16' _chemical_formula_moiety '[Mn3O(EtSaO)3(AcO)(MeOH)5].EtSaOH' _chemical_formula_weight 998.65 _cell_measurement_reflns_used 5322 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 0.938 # Sheldrick geometric approximatio 0.83 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.88 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # 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 43215 _reflns_number_total 11916 _diffrn_reflns_av_R_equivalents 0.0964 # Number of reflections with Friedels Law is 6741 # Number of reflections without Friedels Law is 11916 # Theoretical number of reflections is about 6570 _diffrn_reflns_theta_min 1.996 _diffrn_reflns_theta_max 30.495 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.666 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 1.71 _oxford_diffrn_Wilson_scale 2.94 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.38 _refine_diff_density_max 0.61 _refine_ls_number_reflns 4708 _refine_ls_number_restraints 1 _refine_ls_number_parameters 560 #_refine_ls_R_factor_ref 0.0394 _refine_ls_wR_factor_ref 0.0401 _refine_ls_goodness_of_fit_ref 1.0985 #_reflns_number_all 6737 _refine_ls_R_factor_all 0.0707 _refine_ls_wR_factor_all 0.0417 # 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 4708 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_gt 0.0401 _refine_ls_shift/su_max 0.000584 _refine_ls_abs_structure_Flack 0.59(4) _refine_ls_abs_structure_details 'Flack (1983), 5175 Friedel-pairs' # 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 ad _refine_ls_structure_factor_coef F _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, 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: 1.81 -0.882 1.22 ; _publ_section_exptl_refinement ; H atoms placed geometrically after each cycle Oxidation states and charge balance: there are 3EtSaO ligands which are 2- charged each, 1 Acetate with a negative charge and 1 O2- that makes the number of negative charges equal to 9- There are 3 Mn atoms that must therefore be Mn(III) Checkcif output: 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 227 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 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 0.999 2452 2449 3 23.01 0.550 0.999 3261 3258 3 25.24 0.600 0.999 4202 4199 3 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.999 5298 5294 4 29.84 0.700 0.981 6594 6468 126 30.50 0.714 0.967 6971 6741 230 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.53 Ratio 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.33 Ratio These alerts are caused by the a terminal methyl group of one of the Ethanols molecules attached to the metals: it is not unexpected that such kind of terminal atoms have an higher thermal motions than the rest of the molecule 033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.59 914_ALERT_3_C No Bijvoet Pairs in FCF for Non-centro Structure ! The Flack parameter has been refined for completeness since the structure is not chiral. 026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 40 Perc. This might be an indication that the quality of the structure is not very high due to the presence of many weak data ; # 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. Flack, H. D. (1983). Acta Cryst. A39, 876-881. 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 0.42588(4) 0.41978(17) 0.75645(3) 0.0184 1.0000 Uani . . . . . . O2 O 0.30785(18) 0.3914(4) 0.77210(16) 0.0195 1.0000 Uani . . . . . . Mn3 Mn 0.27174(4) 0.45437(17) 0.86941(4) 0.0187 1.0000 Uani . . . . . . N4 N 0.1429(2) 0.4584(5) 0.81098(18) 0.0211 1.0000 Uani . . . . . . O5 O 0.1246(2) 0.3637(4) 0.74522(18) 0.0248 1.0000 Uani . . . . . . Mn6 Mn 0.21929(4) 0.32520(17) 0.68594(4) 0.0186 1.0000 Uani . . . . . . N7 N 0.3165(2) 0.2751(5) 0.6229(2) 0.0211 1.0000 Uani . . . . . . O8 O 0.39629(19) 0.3521(4) 0.64678(17) 0.0236 1.0000 Uani . . . . . . C9 C 0.3116(3) 0.1879(5) 0.5583(2) 0.0189 1.0000 Uani . . . . . . C10 C 0.2268(3) 0.1081(6) 0.5263(2) 0.0232 1.0000 Uani . . . . . . C11 C 0.1436(3) 0.1428(5) 0.5504(3) 0.0228 1.0000 Uani . . . . . . O12 O 0.1330(2) 0.2551(4) 0.60150(18) 0.0249 1.0000 Uani . . . . . . C13 C 0.0656(3) 0.0611(6) 0.5165(3) 0.0256 1.0000 Uani . . . . . . C14 C 0.0679(3) -0.0485(6) 0.4568(3) 0.0288 1.0000 Uani . . . . . . C15 C 0.1483(3) -0.0790(6) 0.4305(3) 0.0297 1.0000 Uani . . . . . . C16 C 0.2268(3) -0.0038(5) 0.4659(3) 0.0259 1.0000 Uani . . . . . . C17 C 0.3911(3) 0.1738(6) 0.5167(3) 0.0320 1.0000 Uani . . . . . . O18 O 0.2215(2) 0.5637(4) 0.6364(2) 0.0351 1.0000 Uani . . . . . . C19 C 0.1525(4) 0.6580(8) 0.6027(6) 0.0665 1.0000 Uani . . . . . . O20 O 0.2311(2) 0.0769(4) 0.74419(19) 0.0248 1.0000 Uani . . . . . . C21 C 0.1480(3) -0.0084(7) 0.7369(3) 0.0358 1.0000 Uani . . . . . . C22 C 0.0735(3) 0.5249(6) 0.8324(2) 0.0209 1.0000 Uani . . . . . . C23 C 0.0860(3) 0.6212(6) 0.9053(2) 0.0250 1.0000 Uani . . . . . . C24 C 0.1627(3) 0.6080(6) 0.9662(3) 0.0258 1.0000 Uani . . . . . . O25 O 0.2299(2) 0.5081(4) 0.96336(18) 0.0271 1.0000 Uani . . . . . . C26 C 0.1680(3) 0.6975(7) 1.0367(3) 0.0325 1.0000 Uani . . . . . . C27 C 0.1017(4) 0.8009(6) 1.0452(3) 0.0348 1.0000 Uani . . . . . . C28 C 0.0263(3) 0.8205(7) 0.9841(3) 0.0362 1.0000 Uani . . . . . . C29 C 0.0197(3) 0.7297(6) 0.9159(3) 0.0296 1.0000 Uani . . . . . . C30 C -0.0171(3) 0.4978(6) 0.7812(3) 0.0262 1.0000 Uani . . . . . . O31 O 0.39640(18) 0.4560(4) 0.91974(15) 0.0219 1.0000 Uani . . . . . . N32 N 0.4560(2) 0.4982(4) 0.8701(2) 0.0201 1.0000 Uani . . . . . . C33 C 0.5279(3) 0.5715(6) 0.9047(2) 0.0219 1.0000 Uani . . . . . . C34 C 0.5972(3) 0.6207(5) 0.8568(3) 0.0227 1.0000 Uani . . . . . . C35 C 0.6049(3) 0.5585(5) 0.7816(2) 0.0213 1.0000 Uani . . . . . . O36 O 0.54553(18) 0.4562(4) 0.74237(17) 0.0230 1.0000 Uani . . . . . . C37 C 0.6767(3) 0.6029(6) 0.7444(3) 0.0268 1.0000 Uani . . . . . . C38 C 0.7368(3) 0.7135(7) 0.7780(3) 0.0315 1.0000 Uani . . . . . . C39 C 0.7282(3) 0.7811(6) 0.8513(3) 0.0313 1.0000 Uani . . . . . . C40 C 0.6599(3) 0.7329(6) 0.8902(3) 0.0278 1.0000 Uani . . . . . . C41 C 0.5404(3) 0.6090(7) 0.9928(3) 0.0296 1.0000 Uani . . . . . . O42 O 0.2836(2) 0.7083(4) 0.83760(18) 0.0255 1.0000 Uani . . . . . . C43 C 0.3274(3) 0.8112(6) 0.8977(3) 0.0331 1.0000 Uani . . . . . . O44 O 0.2480(2) 0.2046(4) 0.89713(18) 0.0250 1.0000 Uani . . . . . . C45 C 0.1712(4) 0.1573(7) 0.9301(3) 0.0378 1.0000 Uani . . . . . . O46 O 0.4666(2) 0.1805(4) 0.7990(2) 0.0300 1.0000 Uani . . . . . . C47 C 0.5594(3) 0.1376(7) 0.8266(3) 0.0380 1.0000 Uani . . . . . . O48 O 0.3800(2) 0.6845(4) 0.71698(18) 0.0239 1.0000 Uani . . . . . . C49 C 0.4120(3) 0.8134(6) 0.6993(2) 0.0240 1.0000 Uani . . . . . . O50 O 0.3797(2) 0.9389(4) 0.7162(2) 0.0381 1.0000 Uani . . . . . . C51 C 0.4916(3) 0.8146(7) 0.6562(3) 0.0382 1.0000 Uani . . . . . . C52 C 0.2216(3) 0.5567(6) 0.3565(2) 0.0246 1.0000 Uani . . . . . . C53 C 0.1768(3) 0.5946(6) 0.2784(3) 0.0280 1.0000 Uani . . . . . . C54 C 0.0983(3) 0.5177(7) 0.2451(3) 0.0341 1.0000 Uani . . . . . . C55 C 0.0643(3) 0.4008(6) 0.2867(3) 0.0339 1.0000 Uani . . . . . . C56 C 0.1081(3) 0.3620(7) 0.3634(3) 0.0356 1.0000 Uani . . . . . . C57 C 0.1844(3) 0.4402(6) 0.3976(3) 0.0303 1.0000 Uani . . . . . . O58 O 0.2050(2) 0.7088(5) 0.23400(19) 0.0351 1.0000 Uani . . . . . . C59 C 0.3045(3) 0.6374(6) 0.3948(3) 0.0258 1.0000 Uani . . . . . . N60 N 0.3356(2) 0.7398(5) 0.3512(2) 0.0274 1.0000 Uani . . . . . . O61 O 0.4121(2) 0.8148(5) 0.39068(19) 0.0311 1.0000 Uani . . . . . . C62 C 0.3477(4) 0.6064(7) 0.4808(3) 0.0381 1.0000 Uani . . . . . . H131 H 0.0119 0.0807 0.5348 0.0318 1.0000 Uiso R . . . . . H141 H 0.0153 -0.0999 0.4348 0.0350 1.0000 Uiso R . . . . . H151 H 0.1500 -0.1497 0.3894 0.0342 1.0000 Uiso R . . . . . H161 H 0.2805 -0.0283 0.4487 0.0289 1.0000 Uiso R . . . . . H171 H 0.4076 0.0672 0.5135 0.0460 1.0000 Uiso R . . . . . H172 H 0.3764 0.2156 0.4631 0.0459 1.0000 Uiso R . . . . . H173 H 0.4408 0.2312 0.5464 0.0460 1.0000 Uiso R . . . . . H261 H 0.2173 0.6870 1.0778 0.0359 1.0000 Uiso R . . . . . H271 H 0.1059 0.8582 1.0925 0.0451 1.0000 Uiso R . . . . . H281 H -0.0177 0.8932 0.9896 0.0398 1.0000 Uiso R . . . . . H291 H -0.0307 0.7403 0.8762 0.0381 1.0000 Uiso R . . . . . H301 H -0.0625 0.5479 0.8053 0.0380 1.0000 Uiso R . . . . . H302 H -0.0162 0.5377 0.7283 0.0381 1.0000 Uiso R . . . . . H303 H -0.0279 0.3882 0.7783 0.0379 1.0000 Uiso R . . . . . H371 H 0.6840 0.5558 0.6965 0.0310 1.0000 Uiso R . . . . . H381 H 0.7834 0.7433 0.7517 0.0360 1.0000 Uiso R . . . . . H391 H 0.7675 0.8576 0.8737 0.0320 1.0000 Uiso R . . . . . H401 H 0.6549 0.7755 0.9394 0.0277 1.0000 Uiso R . . . . . H411 H 0.6028 0.5996 1.0171 0.0412 1.0000 Uiso R . . . . . H412 H 0.5223 0.7135 0.9991 0.0413 1.0000 Uiso R . . . . . H413 H 0.5052 0.5427 1.0206 0.0409 1.0000 Uiso R . . . . . H511 H 0.4803 0.8839 0.6113 0.0611 1.0000 Uiso R . . . . . H512 H 0.5032 0.7132 0.6378 0.0609 1.0000 Uiso R . . . . . H513 H 0.5432 0.8507 0.6924 0.0613 1.0000 Uiso R . . . . . H541 H 0.0681 0.5460 0.1942 0.0380 1.0000 Uiso R . . . . . H551 H 0.0124 0.3483 0.2632 0.0409 1.0000 Uiso R . . . . . H561 H 0.0848 0.2850 0.3921 0.0409 1.0000 Uiso R . . . . . H571 H 0.2128 0.4133 0.4496 0.0361 1.0000 Uiso R . . . . . H621 H 0.3756 0.6983 0.5048 0.0542 1.0000 Uiso R . . . . . H622 H 0.3928 0.5289 0.4812 0.0540 1.0000 Uiso R . . . . . H623 H 0.3031 0.5715 0.5114 0.0541 1.0000 Uiso R . . . . . H19 H 0.3111 0.7159 0.7994 0.0350 1.0000 Uiso R . . . . . H624 H 0.2521 0.1624 0.8547 0.0368 1.0000 Uiso R . . . . . H27 H 0.4439 0.1132 0.7688 0.0459 1.0000 Uiso R . . . . . H33 H 0.2700 0.6031 0.6557 0.0489 1.0000 Uiso R . . . . . H70 H 0.2658 0.0103 0.7335 0.0359 1.0000 Uiso R . . . . . H451 H 0.1717 0.0475 0.9366 0.0560 1.0000 Uiso R . . . . . H452 H 0.1174 0.1868 0.8945 0.0559 1.0000 Uiso R . . . . . H453 H 0.1718 0.2067 0.9812 0.0557 1.0000 Uiso R . . . . . H211 H 0.1558 -0.0952 0.7731 0.0539 1.0000 Uiso R . . . . . H212 H 0.1307 -0.0439 0.6825 0.0539 1.0000 Uiso R . . . . . H213 H 0.1014 0.0578 0.7504 0.0537 1.0000 Uiso R . . . . . H431 H 0.3396 0.9057 0.8735 0.0443 1.0000 Uiso R . . . . . H432 H 0.2882 0.8295 0.9356 0.0444 1.0000 Uiso R . . . . . H433 H 0.3828 0.7664 0.9242 0.0445 1.0000 Uiso R . . . . . H471 H 0.5607 0.0360 0.8487 0.0530 1.0000 Uiso R . . . . . H472 H 0.5918 0.1391 0.7818 0.0528 1.0000 Uiso R . . . . . H473 H 0.5860 0.2088 0.8668 0.0529 1.0000 Uiso R . . . . . H191 H 0.1766 0.7558 0.5898 0.0920 1.0000 Uiso R . . . . . H192 H 0.1206 0.6100 0.5546 0.0921 1.0000 Uiso R . . . . . H193 H 0.1127 0.6711 0.6412 0.0919 1.0000 Uiso R . . . . . H13 H 0.2565 0.7372 0.2535 0.0522 1.0000 Uiso R . . . . . H22 H 0.4326 0.8547 0.3531 0.0464 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 0.0161(3) 0.0231(3) 0.0150(3) -0.0028(2) 0.0003(2) -0.0016(2) O2 0.0180(13) 0.0250(17) 0.0147(12) -0.0027(11) 0.0007(10) -0.0015(12) Mn3 0.0177(3) 0.0234(4) 0.0142(3) -0.0005(2) 0.0010(2) 0.0011(3) N4 0.0202(15) 0.028(2) 0.0137(14) 0.0003(15) -0.0005(12) 0.0015(15) O5 0.0231(15) 0.0303(19) 0.0201(14) -0.0071(12) 0.0007(11) 0.0006(12) Mn6 0.0161(3) 0.0242(3) 0.0143(3) -0.0022(3) -0.0007(2) -0.0004(3) N7 0.0141(15) 0.030(2) 0.0178(15) -0.0008(14) -0.0016(12) -0.0024(14) O8 0.0185(13) 0.0333(19) 0.0182(13) -0.0059(13) 0.0008(10) -0.0035(13) C9 0.0218(19) 0.019(2) 0.0142(16) -0.0010(15) -0.0028(14) -0.0006(16) C10 0.024(2) 0.028(2) 0.0167(18) -0.0008(17) 0.0009(15) -0.0004(18) C11 0.025(2) 0.022(2) 0.0201(19) -0.0008(17) -0.0007(16) -0.0023(17) O12 0.0167(14) 0.0364(19) 0.0196(14) -0.0077(13) -0.0023(11) 0.0012(13) C13 0.020(2) 0.030(3) 0.025(2) -0.0019(18) -0.0010(16) -0.0009(18) C14 0.025(2) 0.027(2) 0.032(2) -0.006(2) -0.0023(16) -0.005(2) C15 0.029(2) 0.030(3) 0.026(2) -0.013(2) -0.0056(16) -0.001(2) C16 0.027(2) 0.023(2) 0.026(2) -0.0073(17) 0.0012(17) -0.0039(17) C17 0.028(2) 0.034(3) 0.033(2) -0.013(2) 0.0045(19) -0.004(2) O18 0.0272(17) 0.033(2) 0.0398(19) 0.0088(16) -0.0103(14) -0.0022(15) C19 0.038(3) 0.038(4) 0.111(6) 0.010(4) -0.022(4) 0.003(3) O20 0.0229(15) 0.0226(17) 0.0293(16) -0.0021(13) 0.0059(12) -0.0001(13) C21 0.033(2) 0.039(3) 0.034(2) 0.003(2) 0.001(2) -0.008(2) C22 0.0184(19) 0.028(2) 0.0171(18) 0.0025(17) 0.0041(14) 0.0012(17) C23 0.031(2) 0.029(2) 0.0159(18) -0.0002(17) 0.0088(16) 0.0009(19) C24 0.024(2) 0.032(3) 0.022(2) 0.0041(18) 0.0058(17) 0.0017(19) O25 0.0269(16) 0.035(2) 0.0185(14) -0.0009(13) 0.0008(12) 0.0070(14) C26 0.038(3) 0.038(3) 0.022(2) -0.006(2) 0.0066(19) 0.002(2) C27 0.044(3) 0.034(3) 0.028(2) -0.009(2) 0.013(2) 0.005(2) C28 0.039(3) 0.035(3) 0.037(3) -0.003(2) 0.013(2) 0.011(3) C29 0.032(2) 0.035(3) 0.024(2) 0.002(2) 0.0084(18) 0.009(2) C30 0.0184(19) 0.032(3) 0.028(2) 0.0007(18) 0.0037(16) -0.0005(17) O31 0.0192(12) 0.0297(17) 0.0158(12) 0.0013(13) 0.0005(10) 0.0004(13) N32 0.0180(16) 0.0226(19) 0.0192(16) 0.0000(13) 0.0015(13) 0.0005(13) C33 0.0231(19) 0.026(2) 0.0147(18) -0.0007(16) -0.0013(15) 0.0030(18) C34 0.0204(19) 0.021(2) 0.024(2) -0.0020(17) -0.0026(16) -0.0009(17) C35 0.0176(18) 0.022(2) 0.0228(19) 0.0006(17) -0.0016(15) -0.0016(16) O36 0.0178(12) 0.0269(16) 0.0239(13) -0.0040(13) 0.0025(10) -0.0024(13) C37 0.0179(19) 0.034(3) 0.027(2) -0.0038(19) -0.0002(17) -0.0039(18) C38 0.023(2) 0.040(3) 0.032(2) 0.000(2) 0.0059(18) -0.009(2) C39 0.028(2) 0.032(3) 0.032(2) -0.005(2) -0.0010(18) -0.0107(19) C40 0.026(2) 0.035(3) 0.020(2) -0.0054(19) -0.0033(16) -0.0036(19) C41 0.028(2) 0.043(3) 0.0161(19) -0.0033(19) -0.0008(16) -0.005(2) O42 0.0296(16) 0.0257(17) 0.0198(14) -0.0002(13) 0.0009(12) -0.0001(14) C43 0.042(3) 0.026(3) 0.029(2) -0.002(2) -0.0007(19) -0.001(2) O44 0.0250(15) 0.0274(18) 0.0223(14) 0.0025(13) 0.0032(12) 0.0043(14) C45 0.038(3) 0.041(3) 0.035(3) 0.007(2) 0.006(2) -0.006(2) O46 0.0270(16) 0.0279(19) 0.0339(17) -0.0013(15) 0.0021(13) 0.0042(14) C47 0.033(3) 0.039(3) 0.042(3) 0.007(2) 0.005(2) 0.008(2) O48 0.0263(16) 0.0224(17) 0.0223(14) -0.0004(13) 0.0024(12) -0.0020(13) C49 0.0216(19) 0.024(2) 0.0248(19) -0.0005(19) -0.0006(15) -0.0011(18) O50 0.0325(17) 0.0223(19) 0.060(2) -0.0031(18) 0.0099(16) 0.0004(16) C51 0.035(3) 0.036(3) 0.047(3) 0.015(3) 0.019(2) 0.007(2) C52 0.028(2) 0.028(2) 0.0182(19) 0.0007(17) 0.0043(16) 0.0027(18) C53 0.029(2) 0.026(2) 0.029(2) -0.0032(18) 0.0047(18) 0.0037(19) C54 0.032(2) 0.038(3) 0.030(2) -0.005(2) -0.0004(19) 0.002(2) C55 0.027(2) 0.033(3) 0.040(3) -0.010(2) 0.0004(19) 0.000(2) C56 0.035(3) 0.038(3) 0.035(3) 0.003(2) 0.008(2) -0.001(2) C57 0.035(2) 0.028(3) 0.027(2) 0.006(2) 0.0034(17) -0.005(2) O58 0.0374(19) 0.044(2) 0.0214(15) 0.0073(16) -0.0032(13) -0.0083(17) C59 0.023(2) 0.032(3) 0.022(2) 0.0015(18) 0.0028(16) 0.0041(19) N60 0.0189(17) 0.039(2) 0.0235(18) 0.0018(17) 0.0018(14) -0.0013(17) O61 0.0256(15) 0.040(2) 0.0281(15) 0.0034(16) 0.0054(12) -0.0032(16) C62 0.033(3) 0.049(4) 0.029(2) 0.015(2) -0.004(2) -0.006(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.6045(8) 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 . O2 . 1.855(3) yes Mn1 . O8 . 1.915(3) yes Mn1 . N32 . 2.007(3) yes Mn1 . O36 . 1.881(3) yes Mn1 . O46 . 2.246(4) yes Mn1 . O48 . 2.457(4) yes O2 . Mn3 . 1.893(3) yes O2 . Mn6 . 1.881(3) yes Mn3 . N4 . 2.016(3) yes Mn3 . O25 . 1.860(3) yes Mn3 . O31 . 1.919(3) yes Mn3 . O42 . 2.282(4) yes Mn3 . O44 . 2.258(4) yes N4 . O5 . 1.368(4) yes N4 . C22 . 1.296(5) yes O5 . Mn6 . 1.903(3) yes Mn6 . N7 . 1.997(4) yes Mn6 . O12 . 1.854(3) yes Mn6 . O18 . 2.234(4) yes Mn6 . O20 . 2.361(4) yes N7 . O8 . 1.371(4) yes N7 . C9 . 1.316(5) yes C9 . C10 . 1.469(6) yes C9 . C17 . 1.491(6) yes C10 . C11 . 1.412(6) yes C10 . C16 . 1.405(6) yes C11 . O12 . 1.328(5) yes C11 . C13 . 1.404(6) yes C13 . C14 . 1.389(7) yes C13 . H131 . 0.928 no C14 . C15 . 1.382(6) yes C14 . H141 . 0.928 no C15 . C16 . 1.389(6) yes C15 . H151 . 0.929 no C16 . H161 . 0.929 no C17 . H171 . 0.962 no C17 . H172 . 0.961 no C17 . H173 . 0.964 no O18 . C19 . 1.365(7) yes O18 . H33 . 0.820 no C19 . H191 . 0.962 no C19 . H192 . 0.962 no C19 . H193 . 0.961 no O20 . C21 . 1.438(6) yes O20 . H70 . 0.820 no C21 . H211 . 0.963 no C21 . H212 . 0.958 no C21 . H213 . 0.963 no C22 . C23 . 1.470(6) yes C22 . C30 . 1.500(6) yes C23 . C24 . 1.408(6) yes C23 . C29 . 1.405(7) yes C24 . O25 . 1.338(6) yes C24 . C26 . 1.410(7) yes C26 . C27 . 1.367(7) yes C26 . H261 . 0.926 no C27 . C28 . 1.403(7) yes C27 . H271 . 0.931 no C28 . C29 . 1.383(7) yes C28 . H281 . 0.930 no C29 . H291 . 0.924 no C30 . H301 . 0.957 no C30 . H302 . 0.958 no C30 . H303 . 0.964 no O31 . N32 . 1.376(4) yes N32 . C33 . 1.302(5) yes C33 . C34 . 1.485(6) yes C33 . C41 . 1.499(6) yes C34 . C35 . 1.400(6) yes C34 . C40 . 1.404(6) yes C35 . O36 . 1.348(5) yes C35 . C37 . 1.393(6) yes C37 . C38 . 1.371(7) yes C37 . H371 . 0.927 no C38 . C39 . 1.392(7) yes C38 . H381 . 0.928 no C39 . C40 . 1.374(7) yes C39 . H391 . 0.925 no C40 . H401 . 0.921 no C41 . H411 . 0.959 no C41 . H412 . 0.958 no C41 . H413 . 0.958 no O42 . C43 . 1.422(6) yes O42 . H19 . 0.825 no C43 . H431 . 0.947 no C43 . H432 . 0.954 no C43 . H433 . 0.956 no O44 . C45 . 1.424(6) yes O44 . H624 . 0.814 no C45 . H451 . 0.958 no C45 . H452 . 0.954 no C45 . H453 . 0.960 no O46 . C47 . 1.440(6) yes O46 . H27 . 0.810 no C47 . H471 . 0.956 no C47 . H472 . 0.965 no C47 . H473 . 0.953 no O48 . C49 . 1.272(6) yes C49 . O50 . 1.245(6) yes C49 . C51 . 1.504(6) yes C51 . H511 . 0.957 no C51 . H512 . 0.959 no C51 . H513 . 0.953 no C52 . C53 . 1.409(6) yes C52 . C57 . 1.395(7) yes C52 . C59 . 1.477(6) yes C53 . C54 . 1.387(7) yes C53 . O58 . 1.353(6) yes C54 . C55 . 1.380(8) yes C54 . H541 . 0.931 no C55 . C56 . 1.385(7) yes C55 . H551 . 0.931 no C56 . C57 . 1.372(7) yes C56 . H561 . 0.927 no C57 . H571 . 0.935 no O58 . H13 . 0.824 no C59 . N60 . 1.290(6) yes C59 . C62 . 1.505(6) yes N60 . O61 . 1.386(5) yes O61 . H22 . 0.826 no C62 . H621 . 0.957 no C62 . H622 . 0.954 no C62 . H623 . 0.963 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 O2 . Mn1 . O8 . 91.57(12) yes O2 . Mn1 . N32 . 88.49(13) yes O8 . Mn1 . N32 . 178.05(17) yes O2 . Mn1 . O36 . 177.80(17) yes O8 . Mn1 . O36 . 89.89(12) yes N32 . Mn1 . O36 . 90.00(13) yes O2 . Mn1 . O46 . 92.69(14) yes O8 . Mn1 . O46 . 91.66(14) yes N32 . Mn1 . O46 . 90.29(14) yes O36 . Mn1 . O46 . 88.91(14) yes O2 . Mn1 . O48 . 86.12(13) yes O8 . Mn1 . O48 . 91.06(13) yes N32 . Mn1 . O48 . 87.00(14) yes O36 . Mn1 . O48 . 92.21(14) yes O46 . Mn1 . O48 . 177.06(12) yes Mn1 . O2 . Mn3 . 120.57(15) yes Mn1 . O2 . Mn6 . 119.88(15) yes Mn3 . O2 . Mn6 . 119.01(15) yes O2 . Mn3 . N4 . 88.71(12) yes O2 . Mn3 . O25 . 176.33(16) yes N4 . Mn3 . O25 . 88.45(13) yes O2 . Mn3 . O31 . 88.87(12) yes N4 . Mn3 . O31 . 176.72(14) yes O25 . Mn3 . O31 . 94.06(13) yes O2 . Mn3 . O42 . 91.73(13) yes N4 . Mn3 . O42 . 88.63(14) yes O25 . Mn3 . O42 . 90.51(15) yes O31 . Mn3 . O42 . 89.24(14) yes O2 . Mn3 . O44 . 88.90(14) yes N4 . Mn3 . O44 . 86.81(15) yes O25 . Mn3 . O44 . 88.63(14) yes O31 . Mn3 . O44 . 95.36(13) yes O42 . Mn3 . O44 . 175.38(12) yes Mn3 . N4 . O5 . 115.2(2) yes Mn3 . N4 . C22 . 128.5(3) yes O5 . N4 . C22 . 115.7(3) yes N4 . O5 . Mn6 . 117.8(2) yes O5 . Mn6 . O2 . 92.05(13) yes O5 . Mn6 . N7 . 177.40(18) yes O2 . Mn6 . N7 . 89.49(13) yes O5 . Mn6 . O12 . 88.41(13) yes O2 . Mn6 . O12 . 178.60(18) yes N7 . Mn6 . O12 . 90.00(14) yes O5 . Mn6 . O18 . 95.40(15) yes O2 . Mn6 . O18 . 87.21(14) yes N7 . Mn6 . O18 . 86.77(15) yes O12 . Mn6 . O18 . 94.06(15) yes O5 . Mn6 . O20 . 87.21(13) yes O2 . Mn6 . O20 . 88.05(13) yes N7 . Mn6 . O20 . 90.74(15) yes O12 . Mn6 . O20 . 90.66(15) yes O18 . Mn6 . O20 . 174.66(12) yes Mn6 . N7 . O8 . 114.9(3) yes Mn6 . N7 . C9 . 128.5(3) yes O8 . N7 . C9 . 116.4(3) yes N7 . O8 . Mn1 . 118.6(2) yes N7 . C9 . C10 . 119.7(4) yes N7 . C9 . C17 . 120.0(4) yes C10 . C9 . C17 . 120.2(4) yes C9 . C10 . C11 . 123.3(4) yes C9 . C10 . C16 . 118.9(4) yes C11 . C10 . C16 . 117.7(4) yes C10 . C11 . O12 . 123.6(4) yes C10 . C11 . C13 . 119.6(4) yes O12 . C11 . C13 . 116.6(4) yes C11 . O12 . Mn6 . 126.3(3) yes C11 . C13 . C14 . 121.1(4) yes C11 . C13 . H131 . 119.1 no C14 . C13 . H131 . 119.8 no C13 . C14 . C15 . 119.7(4) yes C13 . C14 . H141 . 119.5 no C15 . C14 . H141 . 120.8 no C14 . C15 . C16 . 119.8(4) yes C14 . C15 . H151 . 120.2 no C16 . C15 . H151 . 119.9 no C10 . C16 . C15 . 122.0(4) yes C10 . C16 . H161 . 119.5 no C15 . C16 . H161 . 118.6 no C9 . C17 . H171 . 109.9 no C9 . C17 . H172 . 109.8 no H171 . C17 . H172 . 109.3 no C9 . C17 . H173 . 109.1 no H171 . C17 . H173 . 109.9 no H172 . C17 . H173 . 108.9 no Mn6 . O18 . C19 . 130.6(4) yes Mn6 . O18 . H33 . 107.9 no C19 . O18 . H33 . 118.3 no O18 . C19 . H191 . 109.5 no O18 . C19 . H192 . 108.8 no H191 . C19 . H192 . 110.1 no O18 . C19 . H193 . 107.9 no H191 . C19 . H193 . 110.5 no H192 . C19 . H193 . 109.9 no Mn6 . O20 . C21 . 115.6(3) yes Mn6 . O20 . H70 . 123.8 no C21 . O20 . H70 . 101.3 no O20 . C21 . H211 . 109.8 no O20 . C21 . H212 . 109.6 no H211 . C21 . H212 . 109.7 no O20 . C21 . H213 . 109.2 no H211 . C21 . H213 . 109.3 no H212 . C21 . H213 . 109.2 no N4 . C22 . C23 . 119.5(4) yes N4 . C22 . C30 . 117.7(4) yes C23 . C22 . C30 . 122.8(4) yes C22 . C23 . C24 . 122.2(4) yes C22 . C23 . C29 . 119.7(4) yes C24 . C23 . C29 . 118.2(4) yes C23 . C24 . O25 . 123.7(4) yes C23 . C24 . C26 . 119.3(4) yes O25 . C24 . C26 . 116.9(4) yes C24 . O25 . Mn3 . 124.1(3) yes C24 . C26 . C27 . 120.8(4) yes C24 . C26 . H261 . 119.8 no C27 . C26 . H261 . 119.4 no C26 . C27 . C28 . 121.0(5) yes C26 . C27 . H271 . 119.8 no C28 . C27 . H271 . 119.2 no C27 . C28 . C29 . 118.2(5) yes C27 . C28 . H281 . 120.6 no C29 . C28 . H281 . 121.2 no C23 . C29 . C28 . 122.4(4) yes C23 . C29 . H291 . 119.2 no C28 . C29 . H291 . 118.4 no C22 . C30 . H301 . 109.1 no C22 . C30 . H302 . 108.8 no H301 . C30 . H302 . 110.9 no C22 . C30 . H303 . 108.2 no H301 . C30 . H303 . 110.1 no H302 . C30 . H303 . 109.8 no Mn3 . O31 . N32 . 115.0(2) yes O31 . N32 . Mn1 . 115.2(2) yes O31 . N32 . C33 . 115.8(3) yes Mn1 . N32 . C33 . 128.7(3) yes N32 . C33 . C34 . 120.3(4) yes N32 . C33 . C41 . 120.1(4) yes C34 . C33 . C41 . 119.6(4) yes C33 . C34 . C35 . 123.7(4) yes C33 . C34 . C40 . 117.9(4) yes C35 . C34 . C40 . 118.4(4) yes C34 . C35 . O36 . 123.1(4) yes C34 . C35 . C37 . 119.4(4) yes O36 . C35 . C37 . 117.5(4) yes C35 . O36 . Mn1 . 128.0(3) yes C35 . C37 . C38 . 121.0(5) yes C35 . C37 . H371 . 119.1 no C38 . C37 . H371 . 120.0 no C37 . C38 . C39 . 120.3(5) yes C37 . C38 . H381 . 119.7 no C39 . C38 . H381 . 120.0 no C38 . C39 . C40 . 119.1(4) yes C38 . C39 . H391 . 120.9 no C40 . C39 . H391 . 120.1 no C34 . C40 . C39 . 121.7(4) yes C34 . C40 . H401 . 119.0 no C39 . C40 . H401 . 119.3 no C33 . C41 . H411 . 110.5 no C33 . C41 . H412 . 109.1 no H411 . C41 . H412 . 108.0 no C33 . C41 . H413 . 111.6 no H411 . C41 . H413 . 108.8 no H412 . C41 . H413 . 108.8 no Mn3 . O42 . C43 . 119.0(3) yes Mn3 . O42 . H19 . 109.2 no C43 . O42 . H19 . 105.7 no O42 . C43 . H431 . 109.8 no O42 . C43 . H432 . 108.5 no H431 . C43 . H432 . 109.3 no O42 . C43 . H433 . 109.7 no H431 . C43 . H433 . 109.6 no H432 . C43 . H433 . 110.1 no Mn3 . O44 . C45 . 121.7(3) yes Mn3 . O44 . H624 . 102.2 no C45 . O44 . H624 . 113.6 no O44 . C45 . H451 . 109.9 no O44 . C45 . H452 . 109.6 no H451 . C45 . H452 . 109.1 no O44 . C45 . H453 . 109.7 no H451 . C45 . H453 . 110.0 no H452 . C45 . H453 . 108.5 no Mn1 . O46 . C47 . 122.5(3) yes Mn1 . O46 . H27 . 113.8 no C47 . O46 . H27 . 107.2 no O46 . C47 . H471 . 108.5 no O46 . C47 . H472 . 109.6 no H471 . C47 . H472 . 109.8 no O46 . C47 . H473 . 109.0 no H471 . C47 . H473 . 110.0 no H472 . C47 . H473 . 109.8 no Mn1 . O48 . C49 . 141.8(3) yes O48 . C49 . O50 . 122.5(4) yes O48 . C49 . C51 . 118.9(4) yes O50 . C49 . C51 . 118.6(5) yes C49 . C51 . H511 . 109.7 no C49 . C51 . H512 . 110.7 no H511 . C51 . H512 . 109.8 no C49 . C51 . H513 . 108.8 no H511 . C51 . H513 . 108.3 no H512 . C51 . H513 . 109.6 no C53 . C52 . C57 . 117.7(4) yes C53 . C52 . C59 . 121.8(4) yes C57 . C52 . C59 . 120.5(4) yes C52 . C53 . C54 . 120.1(5) yes C52 . C53 . O58 . 122.9(4) yes C54 . C53 . O58 . 117.0(4) yes C53 . C54 . C55 . 120.8(5) yes C53 . C54 . H541 . 119.4 no C55 . C54 . H541 . 119.8 no C54 . C55 . C56 . 119.6(5) yes C54 . C55 . H551 . 120.0 no C56 . C55 . H551 . 120.4 no C55 . C56 . C57 . 119.9(5) yes C55 . C56 . H561 . 120.0 no C57 . C56 . H561 . 120.1 no C52 . C57 . C56 . 121.9(4) yes C52 . C57 . H571 . 119.3 no C56 . C57 . H571 . 118.8 no C53 . O58 . H13 . 111.2 no C52 . C59 . N60 . 116.1(4) yes C52 . C59 . C62 . 121.8(4) yes N60 . C59 . C62 . 122.0(4) yes C59 . N60 . O61 . 113.8(4) yes N60 . O61 . H22 . 102.6 no C59 . C62 . H621 . 110.1 no C59 . C62 . H622 . 108.7 no H621 . C62 . H622 . 109.0 no C59 . C62 . H623 . 110.3 no H621 . C62 . H623 . 109.2 no H622 . C62 . H623 . 109.5 no # Attachment 'Complex 10.cif' data_EB8160 _database_code_depnum_ccdc_archive 'CCDC 736439' _audit_creation_date 08-11-21 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 'eb8160 in C2/c' _chemical_name_systematic ? _chemical_melting_point ? _exptl_crystal_recrystallization_method ; Slow evaporation of pyridine solution ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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. Most H atoms were located in a difference map. Those attached to the disordered pyridine group were added 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. >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text #============================================================================== 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 123.00 A**3 The results from platon SQUEEZE indicate that the total number of electrons in the voids total 40 for the whole cell. Fourier difference maps do not show any significant peaks in the areas of these voids and so no further action has been taken. SQUEEZE output is shown below; _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 _platon_squeeze_void_content 1 0.000 1.015 0.250 125 8 ' ' 2 0.500 0.515 0.250 125 8 ' ' 3 0.074 0.111 0.144 8 0 ' ' 4 0.574 0.611 0.144 8 0 ' ' 5 0.500 0.836 0.250 15 1 ' ' 6 1.000 0.336 0.250 15 1 ' ' 7 0.426 0.611 0.356 8 0 ' ' 8 0.926 0.111 0.356 8 0 ' ' 9 0.000 -0.015 0.750 127 8 ' ' 10 0.500 0.485 0.750 127 8 ' ' 11 0.074 0.889 0.644 7 0 ' ' 12 0.574 0.389 0.644 7 0 ' ' 13 0.500 0.164 0.750 15 1 ' ' 14 1.000 0.664 0.750 15 1 ' ' 15 0.426 0.389 0.856 7 0 ' ' 16 0.926 0.889 0.856 7 0 ' ' 912_ALERT_3_B # Missing FCF Reflections Above STh/L= 0.600 143 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 3 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 6376 6376 0 23.01 0.550 1.000 8470 8470 0 25.24 0.600 1.000 11011 11008 3 #----------------------------------------------------------- ACTA Min. Res. --- 26.67 0.632 0.989 12850 12704 146 #============================================================================== 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.73 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.86 Ratio Checked - no further action 232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - O41 .. 9.98 su 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 7 No action taken 301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc. There is a pyridine ligand disordered over two positions by symmetry and forming a long Mn-N contact. The Mn-N distance is approximately 2.6\%A. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 36 No action taken #============================================================================== 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 25 The following restraints have been applied; U(IJ)'S 0.0, 0.010000 = C(51) TO C(52) U(IJ)'S 0.0, 0.010000 = O(45) TO C(450) U(IJ)'S 0.0, 0.010000 = C(85) TO C(84) U(IJ)'S 0.0, 0.010000 = O(45) TO C(45) VIBRATION 0.0, 0.020000 = O(45) TO C(450) #============================================================================== ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 31.6181(17) _cell_length_b 15.4746(8) _cell_length_c 27.5994(15) _cell_angle_alpha 90 _cell_angle_beta 115.719(2) _cell_angle_gamma 90 _cell_volume 12166.0(11) _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 4 # Given Formula = C121 H135 Mn6 N13 O24 # Dc = 1.36 Fooo = 5176.00 Mu = 6.78 M = 1242.52 # Found Formula = C121 H135 Mn6 N13 O24 # Dc = 1.36 FOOO = 5176.00 Mu = 6.78 M = 1242.52 _chemical_formula_sum 'C121 H135 Mn6 N13 O24' _chemical_formula_moiety 'C121 H135 Mn6 N13 O24' _chemical_compound_source ? _chemical_formula_weight 2485.04 _cell_measurement_reflns_used 9751 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_max 0.51 _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5176 _exptl_absorpt_coefficient_mu 0.678 # Sheldrick geometric approximatio 0.73 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.90 _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 61883 _reflns_number_total 12704 _diffrn_reflns_av_R_equivalents 0.055 # Number of reflections with Friedels Law is 12704 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12842 _diffrn_reflns_theta_min 1.430 _diffrn_reflns_theta_max 26.675 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.141 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min -39 _reflns_limit_h_max 35 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _oxford_diffrn_Wilson_B_factor 2.25 _oxford_diffrn_Wilson_scale 1150.04 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.67 _refine_diff_density_max 1.13 # 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 12704 _refine_ls_number_restraints 25 _refine_ls_number_parameters 766 _oxford_refine_ls_R_factor_ref 0.0888 _refine_ls_wR_factor_ref 0.1568 _refine_ls_goodness_of_fit_ref 0.9971 _refine_ls_shift/su_max 0.000644 # The values computed from all data _oxford_reflns_number_all 12704 _refine_ls_R_factor_all 0.0888 _refine_ls_wR_factor_all 0.1568 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9343 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_gt 0.1405 # 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^) + ( 0.05P)^2^ +81.41P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. (2008). Acta Cryst A64, 112-122. 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 0.23225(2) 0.56987(4) 0.36558(2) 0.0300 1.0000 Uani . . . . . . . Mn2 Mn 0.13244(2) 0.60173(4) 0.26817(2) 0.0262 1.0000 Uani . . . . . . . Mn3 Mn 0.14353(2) 0.45310(4) 0.35706(2) 0.0265 1.0000 Uani . . . . . . . O1 O 0.16750(9) 0.55256(17) 0.33733(10) 0.0275 1.0000 Uani . . . . . . . O11 O 0.29590(10) 0.59516(18) 0.39956(11) 0.0337 1.0000 Uani . . . . . . . C11 C 0.32167(14) 0.6574(2) 0.39348(15) 0.0306 1.0000 Uani . . . . . . . C12 C 0.37144(15) 0.6541(3) 0.42358(17) 0.0359 1.0000 Uani . . . . . . . C13 C 0.39738(16) 0.7213(3) 0.4168(2) 0.0478 1.0000 Uani . . . . . . . C14 C 0.37716(18) 0.7903(3) 0.3826(2) 0.0539 1.0000 Uani . . . . . . . C15 C 0.32985(17) 0.7932(3) 0.3537(2) 0.0468 1.0000 Uani . . . . . . . C16 C 0.30128(15) 0.7276(3) 0.35779(16) 0.0337 1.0000 Uani . . . . . . . O17 O 0.17552(9) 0.69578(18) 0.28368(11) 0.0322 1.0000 Uani . . . . . . . N17 N 0.22042(11) 0.6781(2) 0.32034(12) 0.0277 1.0000 Uani . . . . . . . C17 C 0.25164(15) 0.7333(3) 0.32337(16) 0.0331 1.0000 Uani . . . . . . . O21 O 0.09345(9) 0.64354(17) 0.19818(10) 0.0305 1.0000 Uani . . . . . . . C21 C 0.07612(13) 0.5940(3) 0.15452(15) 0.0290 1.0000 Uani . . . . . . . C22 C 0.07138(14) 0.6270(3) 0.10412(16) 0.0339 1.0000 Uani . . . . . . . C23 C 0.05667(15) 0.5693(3) 0.06127(16) 0.0390 1.0000 Uani . . . . . . . C24 C 0.04355(16) 0.4851(3) 0.06408(17) 0.0403 1.0000 Uani . . . . . . . C25 C 0.04345(14) 0.4559(3) 0.11123(16) 0.0356 1.0000 Uani . . . . . . . C26 C 0.06025(13) 0.5097(3) 0.15666(15) 0.0305 1.0000 Uani . . . . . . . O27 O 0.08405(9) 0.46111(17) 0.29502(10) 0.0297 1.0000 Uani . . . . . . . N27 N 0.08709(11) 0.5029(2) 0.25271(12) 0.0268 1.0000 Uani . . . . . . . C27 C 0.06155(13) 0.4732(3) 0.20592(15) 0.0296 1.0000 Uani . . . . . . . O31 O 0.11939(10) 0.35812(18) 0.37974(11) 0.0348 1.0000 Uani . . . . . . . C31 C 0.13832(14) 0.3072(2) 0.42226(15) 0.0288 1.0000 Uani . . . . . . . C32 C 0.11261(14) 0.2334(3) 0.42568(16) 0.0304 1.0000 Uani . . . . . . . C33 C 0.13314(15) 0.1828(3) 0.47175(17) 0.0348 1.0000 Uani . . . . . . . C34 C 0.17621(15) 0.2012(3) 0.51351(17) 0.0369 1.0000 Uani . . . . . . . C35 C 0.20113(15) 0.2714(3) 0.51017(17) 0.0372 1.0000 Uani . . . . . . . C36 C 0.18324(14) 0.3239(3) 0.46414(15) 0.0305 1.0000 Uani . . . . . . . N37 N 0.20569(11) 0.4403(2) 0.42017(13) 0.0287 1.0000 Uani . . . . . . . O37 O 0.24269(9) 0.48903(18) 0.42280(11) 0.0332 1.0000 Uani . . . . . . . C37 C 0.21464(14) 0.3899(3) 0.46080(16) 0.0323 1.0000 Uani . . . . . . . O40 O 0.17301(10) 0.52858(19) 0.23390(11) 0.0343 1.0000 Uani . . . . . . . C40 C 0.21559(14) 0.5083(2) 0.25469(15) 0.0292 1.0000 Uani . . . . . . . O41 O 0.24181(10) 0.50062(18) 0.30453(11) 0.0318 1.0000 Uani . . . . . . . C41 C 0.23880(14) 0.4936(2) 0.21751(16) 0.0302 1.0000 Uani . . . . . . . C42 C 0.21262(15) 0.5094(3) 0.16276(16) 0.0355 1.0000 Uani . . . . . . . C43 C 0.23422(16) 0.5003(3) 0.12813(17) 0.0389 1.0000 Uani . . . . . . . O43 O 0.21210(12) 0.5134(2) 0.07417(12) 0.0514 1.0000 Uani . . . . . . . O44 O 0.30262(14) 0.4681(2) 0.11495(15) 0.0576 1.0000 Uani . . . . . . . C44 C 0.28124(17) 0.4784(3) 0.14912(19) 0.0401 1.0000 Uani . . . . . . . O45 O 0.35289(12) 0.4430(2) 0.21979(16) 0.0574 1.0000 Uani . U . . . . . C45 C 0.30703(16) 0.4629(3) 0.2038(2) 0.0415 1.0000 Uani . U . . . . . C46 C 0.28529(15) 0.4705(3) 0.23847(18) 0.0350 1.0000 Uani . . . . . . . N51 N 0.2386(2) 0.6799(4) 0.4387(3) 0.0337 0.5000 Uani . . . . . . . C51 C 0.2558(4) 0.6526(7) 0.4898(4) 0.0453 0.5000 Uani . U . . . . . C52 C 0.2578(5) 0.7016(9) 0.5327(5) 0.0484 0.5000 Uani . U . . . . . C53 C 0.2411(4) 0.7842(8) 0.5216(4) 0.0533 0.5000 Uani . . . . . . . C54 C 0.2258(5) 0.8169(8) 0.4714(6) 0.0502 0.5000 Uani . . . . . . . C55 C 0.2245(4) 0.7616(6) 0.4304(4) 0.0424 0.5000 Uani . . . . . . . N61 N 0.09020(12) 0.6901(2) 0.30124(13) 0.0338 1.0000 Uani . . . . . . . C61 C 0.05150(15) 0.6652(3) 0.30483(17) 0.0399 1.0000 Uani . . . . . . . C62 C 0.02546(18) 0.7189(4) 0.3219(2) 0.0506 1.0000 Uani . . . . . . . C63 C 0.0405(2) 0.8016(4) 0.3365(2) 0.0640 1.0000 Uani . . . . . . . C64 C 0.0802(2) 0.8292(4) 0.3331(3) 0.0757 1.0000 Uani . . . . . . . C65 C 0.1036(2) 0.7716(3) 0.3155(2) 0.0575 1.0000 Uani . . . . . . . N71 N 0.17152(12) 0.3479(2) 0.31378(14) 0.0355 1.0000 Uani . . . . . . . C71 C 0.21629(17) 0.3227(3) 0.3333(2) 0.0445 1.0000 Uani . . . . . . . C72 C 0.23036(19) 0.2499(3) 0.3154(2) 0.0561 1.0000 Uani . . . . . . . C73 C 0.1971(2) 0.2017(3) 0.2754(2) 0.0585 1.0000 Uani . . . . . . . C74 C 0.1510(2) 0.2263(3) 0.2541(2) 0.0544 1.0000 Uani . . . . . . . C75 C 0.14026(16) 0.3005(3) 0.27493(18) 0.0415 1.0000 Uani . . . . . . . N81 N 0.11775(12) 0.5418(2) 0.40798(13) 0.0345 1.0000 Uani . . . . . . . C81 C 0.07694(16) 0.5291(3) 0.40955(18) 0.0444 1.0000 Uani . . . . . . . C82 C 0.06017(19) 0.5826(4) 0.4380(2) 0.0556 1.0000 Uani . . . . . . . C83 C 0.0869(2) 0.6504(4) 0.4661(2) 0.0621 1.0000 Uani . . . . . . . C84 C 0.1294(3) 0.6640(4) 0.4655(3) 0.0759 1.0000 Uani . U . . . . . C85 C 0.1427(2) 0.6082(4) 0.4349(3) 0.0652 1.0000 Uani . U . . . . . C120 C 0.39440(15) 0.5782(3) 0.46165(18) 0.0396 1.0000 Uani . . . . . . . C121 C 0.38301(19) 0.4934(3) 0.4296(2) 0.0527 1.0000 Uani . . . . . . . C122 C 0.37673(18) 0.5739(3) 0.50565(19) 0.0492 1.0000 Uani . . . . . . . C123 C 0.44793(18) 0.5868(4) 0.4901(3) 0.0673 1.0000 Uani . . . . . . . H131 H 0.4297 0.7205 0.4359 0.0537 1.0000 Uiso R . . . . . . H141 H 0.3958 0.8344 0.3799 0.0634 1.0000 Uiso R . . . . . . H151 H 0.3163 0.8394 0.3313 0.0551 1.0000 Uiso R . . . . . . H171 H 0.2412 0.7814 0.3015 0.0410 1.0000 Uiso R . . . . . . C220 C 0.08241(16) 0.7215(3) 0.09840(17) 0.0392 1.0000 Uani . . . . . . . C221 C 0.13509(16) 0.7397(3) 0.13142(19) 0.0466 1.0000 Uani . . . . . . . C222 C 0.0698(2) 0.7438(4) 0.03911(19) 0.0541 1.0000 Uani . . . . . . . C223 C 0.05299(16) 0.7807(3) 0.11567(17) 0.0413 1.0000 Uani . . . . . . . H231 H 0.0553 0.5896 0.0287 0.0479 1.0000 Uiso R . . . . . . H241 H 0.0343 0.4481 0.0344 0.0489 1.0000 Uiso R . . . . . . H251 H 0.0323 0.3999 0.1131 0.0441 1.0000 Uiso R . . . . . . H271 H 0.0428 0.4250 0.2034 0.0347 1.0000 Uiso R . . . . . . C320 C 0.06395(15) 0.2117(3) 0.38107(18) 0.0373 1.0000 Uani . . . . . . . C321 C 0.02957(17) 0.2843(3) 0.3762(2) 0.0547 1.0000 Uani . . . . . . . C322 C 0.06554(19) 0.2002(4) 0.32672(19) 0.0557 1.0000 Uani . . . . . . . C323 C 0.04375(19) 0.1282(3) 0.3925(2) 0.0566 1.0000 Uani . . . . . . . H331 H 0.1165 0.1342 0.4740 0.0446 1.0000 Uiso R . . . . . . H341 H 0.1885 0.1653 0.5433 0.0472 1.0000 Uiso R . . . . . . H351 H 0.2304 0.2850 0.5387 0.0445 1.0000 Uiso R . . . . . . H371 H 0.2440 0.3964 0.4897 0.0388 1.0000 Uiso R . . . . . . H421 H 0.1812 0.5252 0.1493 0.0443 1.0000 Uiso R . . . . . . C430 C 0.16301(18) 0.5282(4) 0.05128(19) 0.0573 1.0000 Uani . . . . . . . C440 C 0.3231(2) 0.5438(4) 0.1075(2) 0.0672 1.0000 Uani . . . . . . . C450 C 0.3798(2) 0.4207(5) 0.2744(3) 0.0787 1.0000 Uani . U . . . . . H461 H 0.3028 0.4604 0.2749 0.0456 1.0000 Uiso R . . . . . . H511 H 0.2664 0.5945 0.4968 0.0541 0.5000 Uiso R . . . . . . H521 H 0.2710 0.6794 0.5684 0.0736 0.5000 Uiso R . . . . . . H531 H 0.2404 0.8193 0.5495 0.0711 0.5000 Uiso R . . . . . . H541 H 0.2158 0.8753 0.4643 0.0701 0.5000 Uiso R . . . . . . H551 H 0.2127 0.7841 0.3949 0.0557 0.5000 Uiso R . . . . . . H611 H 0.0412 0.6088 0.2951 0.0490 1.0000 Uiso R . . . . . . H621 H -0.0016 0.6986 0.3228 0.0647 1.0000 Uiso R . . . . . . H631 H 0.0241 0.8389 0.3482 0.0880 1.0000 Uiso R . . . . . . H641 H 0.0909 0.8858 0.3421 0.1049 1.0000 Uiso R . . . . . . H651 H 0.1310 0.7902 0.3138 0.0781 1.0000 Uiso R . . . . . . H711 H 0.2391 0.3565 0.3598 0.0547 1.0000 Uiso R . . . . . . H721 H 0.2620 0.2340 0.3301 0.0718 1.0000 Uiso R . . . . . . H731 H 0.2058 0.1522 0.2628 0.0779 1.0000 Uiso R . . . . . . H741 H 0.1275 0.1951 0.2268 0.0679 1.0000 Uiso R . . . . . . H751 H 0.1090 0.3175 0.2601 0.0508 1.0000 Uiso R . . . . . . H811 H 0.0587 0.4816 0.3907 0.0550 1.0000 Uiso R . . . . . . H821 H 0.0308 0.5721 0.4374 0.0731 1.0000 Uiso R . . . . . . H831 H 0.0762 0.6869 0.4850 0.0843 1.0000 Uiso R . . . . . . H841 H 0.1490 0.7090 0.4852 0.1041 1.0000 Uiso R . . . . . . H851 H 0.1713 0.6185 0.4336 0.0852 1.0000 Uiso R . . . . . . H1211 H 0.3974 0.4460 0.4532 0.0806 1.0000 Uiso R . . . . . . H1212 H 0.3959 0.4962 0.4039 0.0804 1.0000 Uiso R . . . . . . H1213 H 0.3496 0.4847 0.4108 0.0806 1.0000 Uiso R . . . . . . H1221 H 0.3436 0.5633 0.4902 0.0685 1.0000 Uiso R . . . . . . H1222 H 0.3836 0.6281 0.5246 0.0687 1.0000 Uiso R . . . . . . H1223 H 0.3931 0.5287 0.5306 0.0685 1.0000 Uiso R . . . . . . H1231 H 0.4606 0.5874 0.4643 0.0919 1.0000 Uiso R . . . . . . H1232 H 0.4568 0.6389 0.5105 0.0918 1.0000 Uiso R . . . . . . H1233 H 0.4614 0.5391 0.5140 0.0917 1.0000 Uiso R . . . . . . H2211 H 0.1530 0.7035 0.1188 0.0729 1.0000 Uiso R . . . . . . H2212 H 0.1443 0.7270 0.1686 0.0726 1.0000 Uiso R . . . . . . H2213 H 0.1419 0.7996 0.1282 0.0728 1.0000 Uiso R . . . . . . H2221 H 0.0761 0.8043 0.0369 0.0847 1.0000 Uiso R . . . . . . H2222 H 0.0367 0.7319 0.0173 0.0845 1.0000 Uiso R . . . . . . H2223 H 0.0889 0.7085 0.0274 0.0849 1.0000 Uiso R . . . . . . H2231 H 0.0591 0.8405 0.1113 0.0604 1.0000 Uiso R . . . . . . H2232 H 0.0606 0.7725 0.1531 0.0605 1.0000 Uiso R . . . . . . H2233 H 0.0197 0.7699 0.0946 0.0608 1.0000 Uiso R . . . . . . H3211 H -0.0015 0.2690 0.3492 0.0795 1.0000 Uiso R . . . . . . H3212 H 0.0285 0.2931 0.4100 0.0799 1.0000 Uiso R . . . . . . H3213 H 0.0393 0.3369 0.3655 0.0798 1.0000 Uiso R . . . . . . H3221 H 0.0354 0.1806 0.3005 0.0817 1.0000 Uiso R . . . . . . H3222 H 0.0730 0.2542 0.3154 0.0821 1.0000 Uiso R . . . . . . H3223 H 0.0890 0.1584 0.3300 0.0819 1.0000 Uiso R . . . . . . H3231 H 0.0633 0.0797 0.3949 0.0797 1.0000 Uiso R . . . . . . H3232 H 0.0412 0.1340 0.4257 0.0800 1.0000 Uiso R . . . . . . H3233 H 0.0125 0.1185 0.3642 0.0794 1.0000 Uiso R . . . . . . H4301 H 0.1512 0.5312 0.0129 0.0889 1.0000 Uiso R . . . . . . H4302 H 0.1562 0.5819 0.0640 0.0889 1.0000 Uiso R . . . . . . H4303 H 0.1476 0.4817 0.0604 0.0888 1.0000 Uiso R . . . . . . H4401 H 0.3000 0.5893 0.0957 0.1107 1.0000 Uiso R . . . . . . H4402 H 0.3491 0.5596 0.1403 0.1111 1.0000 Uiso R . . . . . . H4403 H 0.3338 0.5322 0.0806 0.1109 1.0000 Uiso R . . . . . . H4501 H 0.3647 0.3740 0.2836 0.1340 1.0000 Uiso R . . . . . . H4502 H 0.3822 0.4712 0.2960 0.1338 1.0000 Uiso R . . . . . . H4503 H 0.4107 0.4036 0.2793 0.1335 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 0.0298(3) 0.0322(3) 0.0310(3) 0.0092(2) 0.0161(2) 0.0019(2) Mn2 0.0311(3) 0.0288(3) 0.0224(3) 0.0049(2) 0.0152(2) 0.0019(2) Mn3 0.0299(3) 0.0283(3) 0.0239(3) 0.0060(2) 0.0143(2) 0.0024(2) O1 0.0297(13) 0.0322(14) 0.0247(13) 0.0059(11) 0.0157(11) 0.0018(11) O11 0.0401(15) 0.0295(15) 0.0300(14) 0.0039(11) 0.0138(12) -0.0031(12) C11 0.038(2) 0.0256(19) 0.0297(19) -0.0048(15) 0.0164(17) -0.0042(16) C12 0.042(2) 0.032(2) 0.034(2) -0.0045(17) 0.0166(18) -0.0051(18) C13 0.036(2) 0.048(3) 0.051(3) 0.002(2) 0.011(2) -0.006(2) C14 0.048(3) 0.042(3) 0.067(3) 0.008(2) 0.021(3) -0.015(2) C15 0.054(3) 0.033(2) 0.051(3) 0.008(2) 0.020(2) -0.005(2) C16 0.041(2) 0.027(2) 0.034(2) -0.0009(16) 0.0163(18) -0.0036(17) O17 0.0326(14) 0.0334(15) 0.0306(14) 0.0085(12) 0.0138(12) 0.0018(12) N17 0.0328(17) 0.0277(16) 0.0264(16) 0.0004(13) 0.0165(13) 0.0032(13) C17 0.045(2) 0.027(2) 0.031(2) 0.0035(16) 0.0191(18) 0.0036(17) O21 0.0369(15) 0.0316(14) 0.0244(13) 0.0035(11) 0.0147(11) 0.0000(12) C21 0.0293(19) 0.037(2) 0.0227(18) 0.0030(15) 0.0127(15) 0.0014(16) C22 0.034(2) 0.043(2) 0.0265(19) 0.0040(17) 0.0159(17) -0.0041(18) C23 0.040(2) 0.054(3) 0.027(2) 0.0020(19) 0.0180(18) -0.003(2) C24 0.045(2) 0.046(3) 0.030(2) -0.0063(18) 0.0167(19) -0.002(2) C25 0.037(2) 0.038(2) 0.034(2) -0.0012(18) 0.0170(18) -0.0017(18) C26 0.0293(19) 0.035(2) 0.0286(19) 0.0048(16) 0.0141(16) 0.0022(16) O27 0.0305(14) 0.0344(15) 0.0276(13) 0.0079(11) 0.0158(11) 0.0012(11) N27 0.0270(16) 0.0304(17) 0.0262(16) 0.0079(13) 0.0145(13) 0.0049(13) C27 0.0300(19) 0.032(2) 0.0266(19) 0.0023(15) 0.0120(16) -0.0027(16) O31 0.0368(15) 0.0342(15) 0.0308(14) 0.0108(12) 0.0123(12) -0.0007(12) C31 0.037(2) 0.0251(19) 0.032(2) 0.0060(15) 0.0218(17) 0.0066(16) C32 0.033(2) 0.030(2) 0.032(2) 0.0050(16) 0.0179(17) 0.0045(16) C33 0.042(2) 0.029(2) 0.043(2) 0.0087(18) 0.028(2) 0.0057(17) C34 0.043(2) 0.043(2) 0.032(2) 0.0150(18) 0.0229(19) 0.0073(19) C35 0.037(2) 0.044(2) 0.030(2) 0.0079(18) 0.0146(18) 0.0038(19) C36 0.035(2) 0.031(2) 0.0292(19) 0.0064(16) 0.0170(17) 0.0050(16) N37 0.0308(16) 0.0282(17) 0.0284(16) 0.0024(13) 0.0142(13) -0.0002(13) O37 0.0323(14) 0.0362(15) 0.0306(14) 0.0066(12) 0.0131(12) -0.0050(12) C37 0.035(2) 0.036(2) 0.0268(19) 0.0043(16) 0.0148(16) 0.0002(17) O40 0.0345(15) 0.0463(17) 0.0286(14) -0.0009(12) 0.0198(12) 0.0027(13) C40 0.036(2) 0.0255(19) 0.032(2) -0.0031(15) 0.0209(17) -0.0053(16) O41 0.0365(15) 0.0366(15) 0.0273(14) -0.0030(12) 0.0185(12) 0.0030(12) C41 0.041(2) 0.0217(18) 0.036(2) -0.0042(15) 0.0241(18) -0.0041(16) C42 0.038(2) 0.041(2) 0.033(2) -0.0073(18) 0.0207(18) -0.0079(18) C43 0.054(3) 0.040(2) 0.032(2) -0.0085(18) 0.026(2) -0.010(2) O43 0.060(2) 0.071(2) 0.0343(17) -0.0082(16) 0.0318(16) -0.0099(18) O44 0.076(2) 0.060(2) 0.067(2) -0.0061(18) 0.059(2) -0.0012(19) C44 0.057(3) 0.035(2) 0.046(3) -0.0038(19) 0.039(2) -0.004(2) O45 0.054(2) 0.067(2) 0.069(2) 0.0196(19) 0.0430(18) 0.0194(17) C45 0.046(2) 0.034(2) 0.060(3) 0.006(2) 0.037(2) 0.0056(19) C46 0.044(2) 0.028(2) 0.043(2) 0.0031(17) 0.028(2) 0.0033(17) N51 0.046(4) 0.034(4) 0.026(3) -0.007(3) 0.021(3) -0.002(3) C51 0.063(6) 0.047(5) 0.029(4) -0.004(4) 0.022(4) 0.010(4) C52 0.073(7) 0.055(7) 0.028(5) -0.007(5) 0.032(5) 0.004(5) C53 0.071(7) 0.055(7) 0.049(6) -0.022(5) 0.041(6) -0.010(6) C54 0.084(10) 0.030(5) 0.056(8) -0.011(5) 0.048(8) 0.007(5) C55 0.063(6) 0.040(5) 0.035(5) -0.006(4) 0.032(5) -0.001(4) N61 0.0375(18) 0.0383(19) 0.0288(17) 0.0041(14) 0.0175(15) 0.0069(15) C61 0.042(2) 0.043(3) 0.037(2) 0.0047(19) 0.0202(19) 0.0050(19) C62 0.048(3) 0.061(3) 0.053(3) 0.000(2) 0.032(2) 0.006(2) C63 0.090(4) 0.052(3) 0.076(4) -0.006(3) 0.061(4) 0.012(3) C64 0.099(5) 0.047(3) 0.116(6) -0.019(3) 0.080(5) -0.005(3) C65 0.068(3) 0.046(3) 0.081(4) -0.014(3) 0.053(3) -0.009(3) N71 0.0369(19) 0.0362(19) 0.0394(19) 0.0017(15) 0.0223(16) 0.0023(15) C71 0.045(3) 0.037(2) 0.055(3) 0.002(2) 0.025(2) 0.003(2) C72 0.052(3) 0.046(3) 0.082(4) 0.003(3) 0.040(3) 0.011(2) C73 0.078(4) 0.039(3) 0.076(4) -0.006(3) 0.050(3) 0.007(3) C74 0.067(3) 0.045(3) 0.058(3) -0.011(2) 0.033(3) -0.006(2) C75 0.043(2) 0.042(2) 0.043(2) -0.001(2) 0.021(2) 0.004(2) N81 0.0425(19) 0.0370(19) 0.0307(17) 0.0037(15) 0.0223(15) 0.0034(15) C81 0.044(2) 0.054(3) 0.040(2) -0.004(2) 0.022(2) -0.002(2) C82 0.059(3) 0.074(4) 0.049(3) -0.001(3) 0.038(3) 0.014(3) C83 0.096(4) 0.057(3) 0.053(3) 0.001(3) 0.051(3) 0.020(3) C84 0.111(5) 0.049(3) 0.089(4) -0.031(3) 0.064(4) -0.021(3) C85 0.082(4) 0.055(3) 0.083(4) -0.025(3) 0.059(3) -0.023(3) C120 0.036(2) 0.035(2) 0.045(2) -0.0009(19) 0.0145(19) -0.0014(18) C121 0.065(3) 0.036(3) 0.061(3) -0.001(2) 0.031(3) 0.010(2) C122 0.057(3) 0.044(3) 0.037(2) 0.005(2) 0.012(2) 0.006(2) C123 0.046(3) 0.059(3) 0.080(4) 0.021(3) 0.012(3) 0.005(3) C220 0.045(2) 0.042(2) 0.032(2) 0.0072(18) 0.0188(19) -0.006(2) C221 0.046(3) 0.055(3) 0.045(3) 0.000(2) 0.026(2) -0.013(2) C222 0.075(4) 0.058(3) 0.036(2) 0.010(2) 0.030(2) -0.015(3) C223 0.047(3) 0.042(2) 0.033(2) 0.0107(19) 0.0153(19) 0.000(2) C320 0.040(2) 0.031(2) 0.044(2) 0.0049(18) 0.021(2) -0.0016(18) C321 0.039(3) 0.050(3) 0.071(4) 0.009(3) 0.020(2) 0.004(2) C322 0.061(3) 0.064(3) 0.038(3) -0.004(2) 0.018(2) -0.009(3) C323 0.054(3) 0.047(3) 0.059(3) 0.013(2) 0.015(3) -0.011(2) C430 0.059(3) 0.085(4) 0.035(2) -0.005(3) 0.026(2) -0.020(3) C440 0.068(4) 0.085(4) 0.069(4) 0.006(3) 0.049(3) -0.013(3) C450 0.051(3) 0.116(5) 0.080(4) 0.034(4) 0.038(3) 0.034(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.040235(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 . Mn2 . 3.1726(8) yes Mn1 . Mn3 . 3.2582(8) yes Mn1 . O1 . 1.867(3) yes Mn1 . O11 . 1.856(3) yes Mn1 . N17 . 2.024(3) yes Mn1 . O37 . 1.928(3) yes Mn1 . O41 . 2.126(3) yes Mn1 . N51 . 2.582(6) yes Mn2 . Mn3 . 3.2686(8) yes Mn2 . O1 . 1.901(3) yes Mn2 . O17 . 1.911(3) yes Mn2 . O21 . 1.898(3) yes Mn2 . N27 . 2.012(3) yes Mn2 . O40 . 2.208(3) yes Mn2 . N61 . 2.355(3) yes Mn3 . O1 . 1.897(3) yes Mn3 . O27 . 1.921(3) yes Mn3 . O31 . 1.884(3) yes Mn3 . N37 . 1.991(3) yes Mn3 . N71 . 2.403(3) yes Mn3 . N81 . 2.349(3) yes O11 . C11 . 1.319(5) yes C11 . C12 . 1.426(6) yes C11 . C16 . 1.420(6) yes C12 . C13 . 1.386(6) yes C12 . C120 . 1.533(6) yes C13 . C14 . 1.384(7) yes C13 . H131 . 0.923 no C14 . C15 . 1.357(7) yes C14 . H141 . 0.926 no C15 . C16 . 1.396(6) yes C15 . H151 . 0.920 no C16 . C17 . 1.442(6) yes O17 . N17 . 1.367(4) yes N17 . C17 . 1.280(5) yes C17 . H171 . 0.925 no O21 . C21 . 1.329(5) yes C21 . C22 . 1.427(5) yes C21 . C26 . 1.409(6) yes C22 . C23 . 1.391(6) yes C22 . C220 . 1.527(6) yes C23 . C24 . 1.380(6) yes C23 . H231 . 0.935 no C24 . C25 . 1.379(6) yes C24 . H241 . 0.937 no C25 . C26 . 1.403(6) yes C25 . H251 . 0.946 no C26 . C27 . 1.456(5) yes O27 . N27 . 1.374(4) yes N27 . C27 . 1.275(5) yes C27 . H271 . 0.937 no O31 . C31 . 1.321(4) yes C31 . C32 . 1.429(5) yes C31 . C36 . 1.412(6) yes C32 . C33 . 1.391(5) yes C32 . C320 . 1.534(6) yes C33 . C34 . 1.379(6) yes C33 . H331 . 0.935 no C34 . C35 . 1.368(6) yes C34 . H341 . 0.927 no C35 . C36 . 1.404(5) yes C35 . H351 . 0.941 no C36 . C37 . 1.454(5) yes N37 . O37 . 1.367(4) yes N37 . C37 . 1.293(5) yes C37 . H371 . 0.929 no O40 . C40 . 1.253(5) yes C40 . O41 . 1.266(5) yes C40 . C41 . 1.515(5) yes C41 . C42 . 1.394(6) yes C41 . C46 . 1.373(6) yes C42 . C43 . 1.402(5) yes C42 . H421 . 0.931 no C43 . O43 . 1.358(5) yes C43 . C44 . 1.383(6) yes O43 . C430 . 1.418(6) yes O44 . C44 . 1.388(5) yes O44 . C440 . 1.397(6) yes C44 . C45 . 1.389(7) yes O45 . C45 . 1.355(5) yes O45 . C450 . 1.416(7) yes C45 . C46 . 1.405(6) yes C46 . H461 . 0.927 no N51 . C51 . 1.340(11) yes N51 . C55 . 1.326(11) yes C51 . C52 . 1.385(14) yes C51 . H511 . 0.950 no C52 . C53 . 1.365(17) yes C52 . H521 . 0.950 no C53 . C54 . 1.351(18) yes C53 . H531 . 0.950 no C54 . C55 . 1.406(13) yes C54 . H541 . 0.950 no C55 . H551 . 0.950 no N61 . C61 . 1.327(5) yes N61 . C65 . 1.334(6) yes C61 . C62 . 1.388(6) yes C61 . H611 . 0.929 no C62 . C63 . 1.364(8) yes C62 . H621 . 0.923 no C63 . C64 . 1.367(8) yes C63 . H631 . 0.924 no C64 . C65 . 1.376(7) yes C64 . H641 . 0.933 no C65 . H651 . 0.930 no N71 . C71 . 1.336(6) yes N71 . C75 . 1.321(6) yes C71 . C72 . 1.380(7) yes C71 . H711 . 0.933 no C72 . C73 . 1.367(8) yes C72 . H721 . 0.933 no C73 . C74 . 1.367(8) yes C73 . H731 . 0.931 no C74 . C75 . 1.391(7) yes C74 . H741 . 0.931 no C75 . H751 . 0.929 no N81 . C81 . 1.324(6) yes N81 . C85 . 1.313(6) yes C81 . C82 . 1.394(6) yes C81 . H811 . 0.939 no C82 . C83 . 1.358(8) yes C82 . H821 . 0.938 no C83 . C84 . 1.370(8) yes C83 . H831 . 0.926 no C84 . C85 . 1.393(7) yes C84 . H841 . 0.935 no C85 . H851 . 0.933 no C120 . C121 . 1.535(6) yes C120 . C122 . 1.543(7) yes C120 . C123 . 1.531(7) yes C121 . H1211 . 0.956 no C121 . H1212 . 0.961 no C121 . H1213 . 0.963 no C122 . H1221 . 0.959 no C122 . H1222 . 0.963 no C122 . H1223 . 0.960 no C123 . H1231 . 0.955 no C123 . H1232 . 0.953 no C123 . H1233 . 0.959 no C220 . C221 . 1.539(6) yes C220 . C222 . 1.545(6) yes C220 . C223 . 1.523(6) yes C221 . H2211 . 0.963 no C221 . H2212 . 0.959 no C221 . H2213 . 0.964 no C222 . H2221 . 0.966 no C222 . H2222 . 0.972 no C222 . H2223 . 0.970 no C223 . H2231 . 0.963 no C223 . H2232 . 0.962 no C223 . H2233 . 0.971 no C320 . C321 . 1.528(6) yes C320 . C322 . 1.533(6) yes C320 . C323 . 1.533(6) yes C321 . H3211 . 0.970 no C321 . H3212 . 0.958 no C321 . H3213 . 0.962 no C322 . H3221 . 0.961 no C322 . H3222 . 0.958 no C322 . H3223 . 0.957 no C323 . H3231 . 0.956 no C323 . H3232 . 0.957 no C323 . H3233 . 0.970 no C430 . H4301 . 0.959 no C430 . H4302 . 0.962 no C430 . H4303 . 0.961 no C440 . H4401 . 0.963 no C440 . H4402 . 0.954 no C440 . H4403 . 0.955 no C450 . H4501 . 0.960 no C450 . H4502 . 0.965 no C450 . H4503 . 0.962 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 Mn2 . Mn1 . Mn3 . 61.081(18) yes Mn2 . Mn1 . O1 . 32.98(8) yes Mn3 . Mn1 . O1 . 30.30(8) yes Mn2 . Mn1 . O11 . 148.99(9) yes Mn3 . Mn1 . O11 . 149.79(9) yes O1 . Mn1 . O11 . 173.39(12) yes Mn2 . Mn1 . N17 . 59.95(9) yes Mn3 . Mn1 . N17 . 119.43(9) yes O1 . Mn1 . N17 . 89.17(12) yes O11 . Mn1 . N17 . 90.39(12) yes Mn2 . Mn1 . O37 . 123.29(8) yes Mn3 . Mn1 . O37 . 62.31(8) yes O1 . Mn1 . O37 . 90.92(11) yes O11 . Mn1 . O37 . 87.72(12) yes N17 . Mn1 . O37 . 164.23(13) yes Mn2 . Mn1 . O41 . 80.68(8) yes Mn3 . Mn1 . O41 . 94.43(8) yes O1 . Mn1 . O41 . 95.96(11) yes O11 . Mn1 . O41 . 90.62(12) yes N17 . Mn1 . O41 . 88.84(12) yes Mn2 . Mn1 . N51 . 105.74(16) yes Mn3 . Mn1 . N51 . 101.21(16) yes O1 . Mn1 . N51 . 96.90(18) yes O11 . Mn1 . N51 . 76.51(18) yes N17 . Mn1 . N51 . 82.39(18) yes O37 . Mn1 . O41 . 106.83(12) yes O37 . Mn1 . N51 . 81.94(18) yes O41 . Mn1 . N51 . 164.31(17) yes Mn1 . Mn2 . Mn3 . 60.752(18) yes Mn1 . Mn2 . O1 . 32.31(8) yes Mn3 . Mn2 . O1 . 30.57(8) yes Mn1 . Mn2 . O17 . 65.06(8) yes Mn3 . Mn2 . O17 . 122.28(8) yes O1 . Mn2 . O17 . 91.81(11) yes Mn1 . Mn2 . O21 . 152.03(8) yes Mn3 . Mn2 . O21 . 144.53(9) yes O1 . Mn2 . O21 . 175.10(12) yes O17 . Mn2 . O21 . 93.06(11) yes Mn1 . Mn2 . N27 . 114.64(9) yes Mn3 . Mn2 . N27 . 57.22(9) yes O1 . Mn2 . N27 . 87.71(12) yes O17 . Mn2 . N27 . 179.31(12) yes O21 . Mn2 . N27 . 87.42(12) yes Mn1 . Mn2 . O40 . 74.59(7) yes Mn3 . Mn2 . O40 . 93.89(8) yes O1 . Mn2 . O40 . 91.77(11) yes O17 . Mn2 . O40 . 89.79(12) yes O21 . Mn2 . O40 . 88.86(11) yes Mn1 . Mn2 . N61 . 106.54(8) yes Mn3 . Mn2 . N61 . 90.69(8) yes O1 . Mn2 . N61 . 91.44(11) yes O17 . Mn2 . N61 . 86.55(12) yes O21 . Mn2 . N61 . 88.24(12) yes N27 . Mn2 . O40 . 90.71(12) yes N27 . Mn2 . N61 . 92.98(12) yes O40 . Mn2 . N61 . 175.21(12) yes Mn1 . Mn3 . Mn2 . 58.166(17) yes Mn1 . Mn3 . O1 . 29.77(8) yes Mn2 . Mn3 . O1 . 30.65(8) yes Mn1 . Mn3 . O27 . 120.52(8) yes Mn2 . Mn3 . O27 . 62.67(8) yes O1 . Mn3 . O27 . 92.89(11) yes Mn1 . Mn3 . O31 . 150.33(9) yes Mn2 . Mn3 . O31 . 150.61(9) yes O1 . Mn3 . O31 . 176.72(12) yes O27 . Mn3 . O31 . 88.02(11) yes Mn1 . Mn3 . N37 . 60.00(9) yes Mn2 . Mn3 . N37 . 118.04(9) yes O1 . Mn3 . N37 . 88.06(12) yes O27 . Mn3 . N37 . 177.66(13) yes O31 . Mn3 . N37 . 91.16(12) yes Mn1 . Mn3 . N71 . 85.43(9) yes Mn2 . Mn3 . N71 . 92.65(9) yes O1 . Mn3 . N71 . 97.33(12) yes O27 . Mn3 . N71 . 91.72(12) yes O31 . Mn3 . N71 . 85.79(12) yes Mn1 . Mn3 . N81 . 98.29(9) yes Mn2 . Mn3 . N81 . 94.93(8) yes O1 . Mn3 . N81 . 89.05(12) yes O27 . Mn3 . N81 . 92.06(12) yes O31 . Mn3 . N81 . 87.77(13) yes N37 . Mn3 . N71 . 86.04(13) yes N37 . Mn3 . N81 . 90.10(13) yes N71 . Mn3 . N81 . 172.41(12) yes Mn2 . O1 . Mn3 . 118.78(14) yes Mn2 . O1 . Mn1 . 114.70(13) yes Mn3 . O1 . Mn1 . 119.93(13) yes Mn1 . O11 . C11 . 133.2(3) yes O11 . C11 . C12 . 119.1(4) yes O11 . C11 . C16 . 121.9(4) yes C12 . C11 . C16 . 119.0(4) yes C11 . C12 . C13 . 117.6(4) yes C11 . C12 . C120 . 120.1(4) yes C13 . C12 . C120 . 122.4(4) yes C12 . C13 . C14 . 123.0(4) yes C12 . C13 . H131 . 119.0 no C14 . C13 . H131 . 118.0 no C13 . C14 . C15 . 119.6(4) yes C13 . C14 . H141 . 120.2 no C15 . C14 . H141 . 120.3 no C14 . C15 . C16 . 120.9(4) yes C14 . C15 . H151 . 119.7 no C16 . C15 . H151 . 119.4 no C11 . C16 . C15 . 119.9(4) yes C11 . C16 . C17 . 122.7(4) yes C15 . C16 . C17 . 117.4(4) yes Mn2 . O17 . N17 . 115.1(2) yes O17 . N17 . Mn1 . 118.5(2) yes O17 . N17 . C17 . 116.0(3) yes Mn1 . N17 . C17 . 125.5(3) yes C16 . C17 . N17 . 126.2(4) yes C16 . C17 . H171 . 117.1 no N17 . C17 . H171 . 116.6 no Mn2 . O21 . C21 . 123.8(2) yes O21 . C21 . C22 . 120.3(4) yes O21 . C21 . C26 . 120.7(3) yes C22 . C21 . C26 . 118.9(4) yes C21 . C22 . C23 . 117.0(4) yes C21 . C22 . C220 . 120.7(4) yes C23 . C22 . C220 . 122.3(4) yes C22 . C23 . C24 . 123.8(4) yes C22 . C23 . H231 . 117.4 no C24 . C23 . H231 . 118.8 no C23 . C24 . C25 . 119.1(4) yes C23 . C24 . H241 . 121.0 no C25 . C24 . H241 . 119.9 no C24 . C25 . C26 . 119.6(4) yes C24 . C25 . H251 . 120.4 no C26 . C25 . H251 . 120.0 no C21 . C26 . C25 . 121.0(4) yes C21 . C26 . C27 . 122.2(4) yes C25 . C26 . C27 . 116.8(4) yes Mn3 . O27 . N27 . 112.7(2) yes O27 . N27 . Mn2 . 118.9(2) yes O27 . N27 . C27 . 116.4(3) yes Mn2 . N27 . C27 . 124.7(3) yes C26 . C27 . N27 . 123.7(4) yes C26 . C27 . H271 . 118.6 no N27 . C27 . H271 . 117.7 no Mn3 . O31 . C31 . 131.9(3) yes O31 . C31 . C32 . 118.9(4) yes O31 . C31 . C36 . 121.7(3) yes C32 . C31 . C36 . 119.4(3) yes C31 . C32 . C33 . 117.2(4) yes C31 . C32 . C320 . 121.6(3) yes C33 . C32 . C320 . 121.2(4) yes C32 . C33 . C34 . 123.2(4) yes C32 . C33 . H331 . 117.4 no C34 . C33 . H331 . 119.4 no C33 . C34 . C35 . 119.7(4) yes C33 . C34 . H341 . 120.0 no C35 . C34 . H341 . 120.3 no C34 . C35 . C36 . 120.2(4) yes C34 . C35 . H351 . 120.4 no C36 . C35 . H351 . 119.4 no C31 . C36 . C35 . 120.1(4) yes C31 . C36 . C37 . 123.2(3) yes C35 . C36 . C37 . 116.5(4) yes Mn3 . N37 . O37 . 119.3(2) yes Mn3 . N37 . C37 . 125.5(3) yes O37 . N37 . C37 . 115.3(3) yes N37 . O37 . Mn1 . 118.4(2) yes C36 . C37 . N37 . 125.5(4) yes C36 . C37 . H371 . 118.5 no N37 . C37 . H371 . 116.0 no Mn2 . O40 . C40 . 129.8(2) yes O40 . C40 . O41 . 126.0(3) yes O40 . C40 . C41 . 117.9(3) yes O41 . C40 . C41 . 116.1(3) yes Mn1 . O41 . C40 . 124.2(2) yes C40 . C41 . C42 . 118.3(4) yes C40 . C41 . C46 . 119.9(4) yes C42 . C41 . C46 . 121.7(4) yes C41 . C42 . C43 . 119.0(4) yes C41 . C42 . H421 . 120.5 no C43 . C42 . H421 . 120.4 no C42 . C43 . O43 . 124.1(4) yes C42 . C43 . C44 . 119.5(4) yes O43 . C43 . C44 . 116.4(4) yes C43 . O43 . C430 . 117.1(3) yes C44 . O44 . C440 . 113.5(4) yes O44 . C44 . C43 . 119.7(4) yes O44 . C44 . C45 . 119.3(4) yes C43 . C44 . C45 . 121.0(4) yes C45 . O45 . C450 . 117.8(4) yes C44 . C45 . O45 . 115.7(4) yes C44 . C45 . C46 . 119.7(4) yes O45 . C45 . C46 . 124.6(4) yes C45 . C46 . C41 . 119.0(4) yes C45 . C46 . H461 . 119.2 no C41 . C46 . H461 . 121.7 no Mn1 . N51 . C51 . 118.2(6) yes Mn1 . N51 . C55 . 126.0(6) yes C51 . N51 . C55 . 115.8(7) yes N51 . C51 . C52 . 125.1(10) yes N51 . C51 . H511 . 117.3 no C52 . C51 . H511 . 117.6 no C51 . C52 . C53 . 116.8(11) yes C51 . C52 . H521 . 121.6 no C53 . C52 . H521 . 121.6 no C52 . C53 . C54 . 120.8(10) yes C52 . C53 . H531 . 119.8 no C54 . C53 . H531 . 119.4 no C53 . C54 . C55 . 118.0(11) yes C53 . C54 . H541 . 120.5 no C55 . C54 . H541 . 121.5 no C54 . C55 . N51 . 123.4(9) yes C54 . C55 . H551 . 117.9 no N51 . C55 . H551 . 118.7 no Mn2 . N61 . C61 . 123.8(3) yes Mn2 . N61 . C65 . 120.1(3) yes C61 . N61 . C65 . 116.0(4) yes N61 . C61 . C62 . 123.6(5) yes N61 . C61 . H611 . 118.0 no C62 . C61 . H611 . 118.4 no C61 . C62 . C63 . 118.7(5) yes C61 . C62 . H621 . 120.1 no C63 . C62 . H621 . 121.2 no C62 . C63 . C64 . 119.1(5) yes C62 . C63 . H631 . 121.0 no C64 . C63 . H631 . 120.0 no C63 . C64 . C65 . 118.3(5) yes C63 . C64 . H641 . 120.9 no C65 . C64 . H641 . 120.8 no C64 . C65 . N61 . 124.4(5) yes C64 . C65 . H651 . 118.1 no N61 . C65 . H651 . 117.5 no Mn3 . N71 . C71 . 123.5(3) yes Mn3 . N71 . C75 . 118.2(3) yes C71 . N71 . C75 . 117.0(4) yes N71 . C71 . C72 . 123.0(5) yes N71 . C71 . H711 . 118.5 no C72 . C71 . H711 . 118.6 no C71 . C72 . C73 . 118.7(5) yes C71 . C72 . H721 . 120.6 no C73 . C72 . H721 . 120.7 no C72 . C73 . C74 . 119.9(5) yes C72 . C73 . H731 . 120.2 no C74 . C73 . H731 . 119.9 no C73 . C74 . C75 . 117.3(5) yes C73 . C74 . H741 . 122.2 no C75 . C74 . H741 . 120.5 no C74 . C75 . N71 . 124.2(4) yes C74 . C75 . H751 . 117.2 no N71 . C75 . H751 . 118.5 no Mn3 . N81 . C81 . 122.0(3) yes Mn3 . N81 . C85 . 121.1(3) yes C81 . N81 . C85 . 116.9(4) yes N81 . C81 . C82 . 123.0(5) yes N81 . C81 . H811 . 118.1 no C82 . C81 . H811 . 118.9 no C81 . C82 . C83 . 119.1(5) yes C81 . C82 . H821 . 120.2 no C83 . C82 . H821 . 120.7 no C82 . C83 . C84 . 118.8(5) yes C82 . C83 . H831 . 120.3 no C84 . C83 . H831 . 120.8 no C83 . C84 . C85 . 117.9(5) yes C83 . C84 . H841 . 120.9 no C85 . C84 . H841 . 121.1 no C84 . C85 . N81 . 124.2(5) yes C84 . C85 . H851 . 118.0 no N81 . C85 . H851 . 117.7 no C12 . C120 . C121 . 109.7(4) yes C12 . C120 . C122 . 110.3(4) yes C121 . C120 . C122 . 110.0(4) yes C12 . C120 . C123 . 112.0(4) yes C121 . C120 . C123 . 107.5(4) yes C122 . C120 . C123 . 107.3(4) yes C120 . C121 . H1211 . 109.9 no C120 . C121 . H1212 . 108.6 no H1211 . C121 . H1212 . 108.0 no C120 . C121 . H1213 . 111.1 no H1211 . C121 . H1213 . 110.2 no H1212 . C121 . H1213 . 109.0 no C120 . C122 . H1221 . 110.8 no C120 . C122 . H1222 . 108.4 no H1221 . C122 . H1222 . 109.6 no C120 . C122 . H1223 . 109.2 no H1221 . C122 . H1223 . 109.9 no H1222 . C122 . H1223 . 108.8 no C120 . C123 . H1231 . 110.2 no C120 . C123 . H1232 . 110.7 no H1231 . C123 . H1232 . 108.7 no C120 . C123 . H1233 . 110.3 no H1231 . C123 . H1233 . 108.4 no H1232 . C123 . H1233 . 108.5 no C22 . C220 . C221 . 110.6(4) yes C22 . C220 . C222 . 110.9(4) yes C221 . C220 . C222 . 107.6(4) yes C22 . C220 . C223 . 110.3(3) yes C221 . C220 . C223 . 110.8(4) yes C222 . C220 . C223 . 106.6(4) yes C220 . C221 . H2211 . 109.6 no C220 . C221 . H2212 . 110.1 no H2211 . C221 . H2212 . 108.2 no C220 . C221 . H2213 . 110.5 no H2211 . C221 . H2213 . 109.7 no H2212 . C221 . H2213 . 108.7 no C220 . C222 . H2221 . 108.5 no C220 . C222 . H2222 . 109.2 no H2221 . C222 . H2222 . 110.0 no C220 . C222 . H2223 . 108.4 no H2221 . C222 . H2223 . 110.3 no H2222 . C222 . H2223 . 110.3 no C220 . C223 . H2231 . 110.9 no C220 . C223 . H2232 . 110.8 no H2231 . C223 . H2232 . 107.0 no C220 . C223 . H2233 . 111.1 no H2231 . C223 . H2233 . 108.3 no H2232 . C223 . H2233 . 108.7 no C32 . C320 . C321 . 109.7(4) yes C32 . C320 . C322 . 111.3(4) yes C321 . C320 . C322 . 108.9(4) yes C32 . C320 . C323 . 112.4(4) yes C321 . C320 . C323 . 107.0(4) yes C322 . C320 . C323 . 107.3(4) yes C320 . C321 . H3211 . 109.5 no C320 . C321 . H3212 . 110.2 no H3211 . C321 . H3212 . 109.3 no C320 . C321 . H3213 . 109.7 no H3211 . C321 . H3213 . 108.8 no H3212 . C321 . H3213 . 109.3 no C320 . C322 . H3221 . 109.4 no C320 . C322 . H3222 . 109.6 no H3221 . C322 . H3222 . 109.5 no C320 . C322 . H3223 . 109.8 no H3221 . C322 . H3223 . 109.4 no H3222 . C322 . H3223 . 109.2 no C320 . C323 . H3231 . 111.2 no C320 . C323 . H3232 . 109.5 no H3231 . C323 . H3232 . 109.1 no C320 . C323 . H3233 . 109.5 no H3231 . C323 . H3233 . 109.6 no H3232 . C323 . H3233 . 107.9 no O43 . C430 . H4301 . 109.1 no O43 . C430 . H4302 . 110.6 no H4301 . C430 . H4302 . 108.5 no O43 . C430 . H4303 . 110.1 no H4301 . C430 . H4303 . 109.0 no H4302 . C430 . H4303 . 109.5 no O44 . C440 . H4401 . 109.3 no O44 . C440 . H4402 . 109.8 no H4401 . C440 . H4402 . 110.3 no O44 . C440 . H4403 . 107.4 no H4401 . C440 . H4403 . 110.3 no H4402 . C440 . H4403 . 109.6 no O45 . C450 . H4501 . 109.1 no O45 . C450 . H4502 . 108.1 no H4501 . C450 . H4502 . 111.1 no O45 . C450 . H4503 . 108.7 no H4501 . C450 . H4503 . 110.3 no H4502 . C450 . H4503 . 109.5 no # Attachment 'Complex 11.cif' data_eb7032 _database_code_depnum_ccdc_archive 'CCDC 736440' _audit_creation_date 07-03-05 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'eb7032 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.0732(5) _cell_length_b 13.8072(5) _cell_length_c 15.0103(6) _cell_angle_alpha 81.204(3) _cell_angle_beta 84.118(3) _cell_angle_gamma 72.351(2) _cell_volume 2547.00(17) _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 2 # Given Formula = C46 H64 Mn3 N3 O13 # Dc = 1.35 Fooo = 1080.00 Mu = 7.94 M = 1031.81 # Found Formula = C46 H64 Mn3 N3 O13 # Dc = 1.35 FOOO = 1080.00 Mu = 7.94 M = 1031.81 _chemical_formula_sum 'C47.5 H68 Mn3 N3 O14.5' _chemical_formula_moiety 'C46 H64 Mn3 N3 O13, 1.5(C H4 O)' _chemical_compound_source ? _chemical_formula_weight 1063.85 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description rhomb _exptl_crystal_colour black _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.794 # Sheldrick geometric approximatio 0.85 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.89 _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 14164 _reflns_number_total 14164 _diffrn_reflns_av_R_equivalents 0.047 # Number of reflections with Friedels Law is 14164 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 15609 _diffrn_reflns_theta_min 1.561 _diffrn_reflns_theta_max 30.549 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.050 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 18 _reflns_limit_k_min -19 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.03 _oxford_diffrn_Wilson_scale 10.22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.11 _refine_diff_density_max 1.36 _refine_ls_number_reflns 14162 _refine_ls_number_restraints 0 _refine_ls_number_parameters 586 #_refine_ls_R_factor_ref 0.1065 _refine_ls_wR_factor_ref 0.1936 _refine_ls_goodness_of_fit_ref 1.0056 #_reflns_number_all 14162 _refine_ls_R_factor_all 0.1065 _refine_ls_wR_factor_all 0.1936 # 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 9017 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_gt 0.1822 _refine_ls_shift/su_max 0.000208 # 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^) + ( 0.07P)^2^ + 5.39P] ,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. ; ? ; _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 ...... 1381 911_ALERT_3_B # Missing FCF Refl. Between TH(Min) & STH/L=0.6 54 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 1 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.991 5321 5274 47 23.01 0.550 0.993 7110 7060 50 25.24 0.600 0.994 9206 9151 55 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.992 11711 11618 93 29.84 0.700 0.938 14644 13739 905 30.55 0.715 0.908 15600 14164 1436 420_ALERT_2_B D-H Without Acceptor O16 - H161 ... ? There is disordered methanol solvent within the structure( not modelled; see below) and this probably acts as the acceptor. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.86 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 etc. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.05 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.28 Ratio 232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - O6 .. 7.07 su 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 59.00 A**3 The solvent region was treated by the van der Sluis and Spek method, accounting for 27e/cell. This corresponds to 1.5 molecules of methanol per formula unit. ; # 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 0.000 0.500 27.1 18.2 2 0.000 0.500 0.500 60.8 9.1 3 0.233 0.056 0.764 7.0 0.4 4 0.767 0.944 0.236 7.0 0.3 _platon_squeeze_details ; Voids 1 and 2 correspond to one and one half molecules of MeOH respectively. Voids 3 and 4 are neglible. ; _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 0.19929(5) 0.19748(5) 0.36541(4) 0.0288 1.0000 Uani . . . . . . Mn2 Mn -0.02229(5) 0.28258(4) 0.25817(4) 0.0279 1.0000 Uani . . . . . . Mn3 Mn 0.11605(5) 0.03959(4) 0.26914(4) 0.0256 1.0000 Uani . . . . . . O5 O 0.0974(2) 0.1726(2) 0.29741(18) 0.0285 1.0000 Uani . . . . . . O6 O 0.0951(3) 0.1619(3) 0.4944(2) 0.0580 1.0000 Uani . . . . . . O7 O 0.1262(2) 0.3410(2) 0.3590(2) 0.0442 1.0000 Uani . . . . . . O8 O -0.1405(2) 0.3933(2) 0.2222(2) 0.0353 1.0000 Uani . . . . . . O9 O -0.0910(2) 0.1908(2) 0.2237(2) 0.0339 1.0000 Uani . . . . . . O10 O 0.2292(2) -0.0188(2) 0.3514(2) 0.0348 1.0000 Uani . . . . . . O11 O 0.2988(2) 0.2107(2) 0.4402(2) 0.0336 1.0000 Uani . . . . . . O12 O 0.1040(2) -0.0923(2) 0.27152(18) 0.0299 1.0000 Uani . . . . . . O13 O 0.2050(2) 0.0299(2) 0.1462(2) 0.0371 1.0000 Uani . . . . . . O14 O 0.2568(2) 0.1694(2) 0.09632(19) 0.0332 1.0000 Uani . . . . . . O15 O 0.0652(2) 0.2983(2) 0.1251(2) 0.0359 1.0000 Uani . . . . . . O16 O -0.1011(3) 0.2635(3) 0.4058(2) 0.0554 1.0000 Uani . . . . . . O17 O 0.3068(2) 0.2228(2) 0.2430(2) 0.0341 1.0000 Uani . . . . . . N18 N 0.0404(3) 0.3796(3) 0.3047(3) 0.0351 1.0000 Uani . . . . . . N19 N -0.0254(3) 0.0943(2) 0.2127(2) 0.0301 1.0000 Uani . . . . . . N20 N 0.2821(3) 0.0501(3) 0.3676(2) 0.0301 1.0000 Uani . . . . . . C21 C -0.1957(6) 0.3411(5) 0.4267(5) 0.0810 1.0000 Uani . . . . . . C22 C -0.0334(4) -0.0944(4) 0.0715(4) 0.0488 1.0000 Uani . . . . . . C23 C 0.1119(5) 0.1782(5) 0.5828(4) 0.0646 1.0000 Uani . . . . . . C24 C 0.3368(5) 0.3138(4) 0.2142(4) 0.0520 1.0000 Uani . . . . . . C25 C -0.4199(4) 0.6001(4) 0.0819(4) 0.0567 1.0000 Uani . . . . . . C26 C 0.0075(4) 0.4776(3) 0.2906(4) 0.0427 1.0000 Uani . . . . . . C27 C -0.0848(4) 0.5384(3) 0.2416(3) 0.0375 1.0000 Uani . . . . . . C28 C -0.1574(3) 0.4944(3) 0.2105(3) 0.0326 1.0000 Uani . . . . . . C29 C -0.2492(3) 0.5586(3) 0.1664(3) 0.0345 1.0000 Uani . . . . . . C30 C -0.3283(4) 0.5150(3) 0.1294(3) 0.0369 1.0000 Uani . . . . . . C31 C -0.2689(4) 0.4434(4) 0.0590(3) 0.0425 1.0000 Uani . . . . . . C32 C -0.3800(4) 0.4554(4) 0.2065(3) 0.0454 1.0000 Uani . . . . . . C33 C -0.2639(4) 0.6643(3) 0.1562(3) 0.0418 1.0000 Uani . . . . . . C34 C -0.1939(4) 0.7080(4) 0.1865(4) 0.0473 1.0000 Uani . . . . . . C35 C -0.1042(4) 0.6462(4) 0.2284(4) 0.0468 1.0000 Uani . . . . . . C36 C 0.3823(3) 0.0131(3) 0.3795(3) 0.0314 1.0000 Uani . . . . . . C37 C 0.4495(3) 0.0734(3) 0.3984(3) 0.0294 1.0000 Uani . . . . . . C38 C 0.4049(3) 0.1699(3) 0.4310(3) 0.0303 1.0000 Uani . . . . . . C39 C 0.4749(3) 0.2201(3) 0.4574(3) 0.0322 1.0000 Uani . . . . . . C40 C 0.4298(4) 0.3182(3) 0.5033(3) 0.0380 1.0000 Uani . . . . . . C41 C 0.3638(4) 0.4064(3) 0.4370(3) 0.0465 1.0000 Uani . . . . . . C42 C 0.3589(4) 0.2991(4) 0.5882(3) 0.0467 1.0000 Uani . . . . . . C43 C 0.5196(4) 0.3546(4) 0.5322(4) 0.0524 1.0000 Uani . . . . . . C44 C 0.5839(4) 0.1765(3) 0.4418(3) 0.0386 1.0000 Uani . . . . . . C45 C 0.6279(4) 0.0846(4) 0.4041(3) 0.0422 1.0000 Uani . . . . . . C46 C 0.5612(4) 0.0324(3) 0.3857(3) 0.0366 1.0000 Uani . . . . . . C47 C 0.0786(3) -0.1244(3) 0.1990(3) 0.0296 1.0000 Uani . . . . . . C48 C -0.0049(4) -0.0599(3) 0.1464(3) 0.0369 1.0000 Uani . . . . . . C49 C -0.0619(4) 0.0435(3) 0.1644(3) 0.0382 1.0000 Uani . . . . . . C50 C 0.1336(3) -0.2242(3) 0.1776(3) 0.0312 1.0000 Uani . . . . . . C51 C 0.2254(4) -0.2959(3) 0.2333(3) 0.0340 1.0000 Uani . . . . . . C52 C 0.1865(4) -0.3149(3) 0.3318(3) 0.0442 1.0000 Uani . . . . . . C53 C 0.3177(4) -0.2481(3) 0.2266(3) 0.0416 1.0000 Uani . . . . . . C54 C 0.2707(4) -0.4004(3) 0.1985(3) 0.0447 1.0000 Uani . . . . . . C55 C 0.1031(4) -0.2530(3) 0.1013(3) 0.0391 1.0000 Uani . . . . . . C56 C 0.0206(4) -0.1905(4) 0.0489(4) 0.0493 1.0000 Uani . . . . . . C57 C 0.2541(3) 0.0793(3) 0.0907(3) 0.0294 1.0000 Uani . . . . . . C58 C 0.3152(3) 0.0291(3) 0.0112(3) 0.0266 1.0000 Uani . . . . . . C59 C 0.3811(3) 0.0765(3) -0.0453(3) 0.0291 1.0000 Uani . . . . . . C60 C 0.4379(3) 0.0325(3) -0.1201(3) 0.0321 1.0000 Uani . . . . . . C61 C 0.4270(3) -0.0607(3) -0.1355(3) 0.0362 1.0000 Uani . . . . . . C62 C 0.3621(4) -0.1102(3) -0.0798(3) 0.0360 1.0000 Uani . . . . . . C63 C 0.3054(3) -0.0641(3) -0.0053(3) 0.0314 1.0000 Uani . . . . . . C64 C 0.3541(5) -0.2117(4) -0.0971(4) 0.0537 1.0000 Uani . . . . . . C65 C 0.5084(4) 0.0854(4) -0.1808(3) 0.0446 1.0000 Uani . . . . . . C66 C 0.0559(4) 0.3868(3) 0.0606(3) 0.0437 1.0000 Uani . . . . . . H221 H -0.0906 -0.0531 0.0381 0.0599 1.0000 Uiso R . . . . . H251 H -0.4687 0.5697 0.0611 0.0808 1.0000 Uiso R . . . . . H252 H -0.4586 0.6471 0.1229 0.0809 1.0000 Uiso R . . . . . H253 H -0.3899 0.6353 0.0315 0.0808 1.0000 Uiso R . . . . . H261 H 0.0484 0.5127 0.3121 0.0552 1.0000 Uiso R . . . . . H311 H -0.2158 0.3850 0.0882 0.0669 1.0000 Uiso R . . . . . H312 H -0.2342 0.4795 0.0116 0.0666 1.0000 Uiso R . . . . . H313 H -0.3198 0.4200 0.0326 0.0671 1.0000 Uiso R . . . . . H321 H -0.3266 0.3973 0.2342 0.0690 1.0000 Uiso R . . . . . H322 H -0.4150 0.4984 0.2521 0.0690 1.0000 Uiso R . . . . . H323 H -0.4330 0.4321 0.1827 0.0689 1.0000 Uiso R . . . . . H331 H -0.3242 0.7074 0.1281 0.0488 1.0000 Uiso R . . . . . H341 H -0.2072 0.7783 0.1773 0.0583 1.0000 Uiso R . . . . . H351 H -0.0561 0.6742 0.2482 0.0567 1.0000 Uiso R . . . . . H361 H 0.4145 -0.0561 0.3752 0.0381 1.0000 Uiso R . . . . . H411 H 0.3383 0.4669 0.4655 0.0707 1.0000 Uiso R . . . . . H412 H 0.4085 0.4189 0.3837 0.0707 1.0000 Uiso R . . . . . H413 H 0.3028 0.3906 0.4202 0.0708 1.0000 Uiso R . . . . . H421 H 0.3310 0.3607 0.6152 0.0737 1.0000 Uiso R . . . . . H422 H 0.4022 0.2475 0.6299 0.0738 1.0000 Uiso R . . . . . H423 H 0.3003 0.2779 0.5730 0.0738 1.0000 Uiso R . . . . . H431 H 0.4882 0.4141 0.5616 0.0838 1.0000 Uiso R . . . . . H432 H 0.5645 0.3026 0.5729 0.0837 1.0000 Uiso R . . . . . H433 H 0.5622 0.3710 0.4793 0.0837 1.0000 Uiso R . . . . . H441 H 0.6311 0.2097 0.4559 0.0499 1.0000 Uiso R . . . . . H451 H 0.7017 0.0599 0.3929 0.0510 1.0000 Uiso R . . . . . H461 H 0.5901 -0.0311 0.3641 0.0432 1.0000 Uiso R . . . . . H491 H -0.1287 0.0764 0.1394 0.0450 1.0000 Uiso R . . . . . H521 H 0.2453 -0.3604 0.3646 0.0660 1.0000 Uiso R . . . . . H522 H 0.1289 -0.3445 0.3359 0.0658 1.0000 Uiso R . . . . . H523 H 0.1627 -0.2519 0.3562 0.0658 1.0000 Uiso R . . . . . H531 H 0.3764 -0.2936 0.2597 0.0609 1.0000 Uiso R . . . . . H532 H 0.2940 -0.1857 0.2525 0.0612 1.0000 Uiso R . . . . . H533 H 0.3421 -0.2350 0.1647 0.0607 1.0000 Uiso R . . . . . H541 H 0.3241 -0.4436 0.2377 0.0667 1.0000 Uiso R . . . . . H542 H 0.2135 -0.4309 0.1997 0.0669 1.0000 Uiso R . . . . . H543 H 0.3024 -0.3927 0.1383 0.0665 1.0000 Uiso R . . . . . H551 H 0.1383 -0.3181 0.0858 0.0491 1.0000 Uiso R . . . . . H561 H 0.0040 -0.2118 -0.0020 0.0650 1.0000 Uiso R . . . . . H591 H 0.3884 0.1379 -0.0325 0.0342 1.0000 Uiso R . . . . . H611 H 0.4648 -0.0908 -0.1854 0.0429 1.0000 Uiso R . . . . . H631 H 0.2608 -0.0956 0.0326 0.0378 1.0000 Uiso R . . . . . H641 H 0.2890 -0.2224 -0.0681 0.0851 1.0000 Uiso R . . . . . H642 H 0.4145 -0.2656 -0.0745 0.0850 1.0000 Uiso R . . . . . H643 H 0.3533 -0.2111 -0.1610 0.0848 1.0000 Uiso R . . . . . H651 H 0.5703 0.0374 -0.2047 0.0651 1.0000 Uiso R . . . . . H652 H 0.5318 0.1278 -0.1476 0.0650 1.0000 Uiso R . . . . . H653 H 0.4687 0.1278 -0.2300 0.0650 1.0000 Uiso R . . . . . H661 H 0.0914 0.3686 0.0035 0.0611 1.0000 Uiso R . . . . . H662 H 0.0886 0.4318 0.0825 0.0615 1.0000 Uiso R . . . . . H663 H -0.0190 0.4211 0.0533 0.0610 1.0000 Uiso R . . . . . H10 H -0.2279 0.3203 0.4842 0.1117 1.0000 Uiso R . . . . . H12 H 0.0453 0.2091 0.4724 0.0874 1.0000 Uiso R . . . . . H34 H -0.2449 0.3509 0.3800 0.1120 1.0000 Uiso R . . . . . H70 H -0.1801 0.4043 0.4285 0.1120 1.0000 Uiso R . . . . . H74 H 0.1267 0.2605 0.1202 0.0532 1.0000 Uiso R . . . . . H171 H 0.2908 0.2055 0.1955 0.0435 1.0000 Uiso R . . . . . H241 H 0.3559 0.3369 0.2655 0.0697 1.0000 Uiso R . . . . . H242 H 0.3972 0.3004 0.1709 0.0697 1.0000 Uiso R . . . . . H243 H 0.2774 0.3657 0.1871 0.0697 1.0000 Uiso R . . . . . H231 H 0.1706 0.1229 0.6088 0.0818 1.0000 Uiso R . . . . . H232 H 0.1299 0.2416 0.5804 0.0818 1.0000 Uiso R . . . . . H233 H 0.0482 0.1818 0.6223 0.0818 1.0000 Uiso R . . . . . H161 H -0.1171 0.2088 0.4033 0.0649 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 0.0277(3) 0.0257(3) 0.0332(3) -0.0098(2) -0.0051(2) -0.0038(2) Mn2 0.0247(3) 0.0222(3) 0.0358(3) -0.0089(2) -0.0034(2) -0.0023(2) Mn3 0.0260(3) 0.0226(3) 0.0280(3) -0.0042(2) -0.0035(2) -0.0059(2) O5 0.0268(14) 0.0252(13) 0.0327(15) -0.0091(11) -0.0033(11) -0.0032(11) O6 0.0410(19) 0.086(3) 0.044(2) -0.0219(19) -0.0026(16) -0.0075(19) O7 0.0334(16) 0.0343(16) 0.065(2) -0.0252(15) -0.0170(15) 0.0038(13) O8 0.0314(15) 0.0253(14) 0.0498(18) -0.0131(13) -0.0055(13) -0.0040(12) O9 0.0264(14) 0.0232(13) 0.0501(18) -0.0068(12) -0.0074(13) -0.0018(11) O10 0.0397(17) 0.0246(14) 0.0442(17) -0.0037(12) -0.0142(14) -0.0119(13) O11 0.0310(15) 0.0331(15) 0.0372(16) -0.0134(12) -0.0069(12) -0.0042(12) O12 0.0348(15) 0.0253(13) 0.0305(15) -0.0025(11) -0.0037(12) -0.0101(12) O13 0.0423(17) 0.0295(15) 0.0366(16) -0.0063(12) 0.0083(14) -0.0085(13) O14 0.0369(16) 0.0264(14) 0.0361(16) -0.0106(12) 0.0024(13) -0.0071(12) O15 0.0371(16) 0.0247(14) 0.0386(16) -0.0002(12) 0.0013(13) -0.0010(12) O16 0.042(2) 0.077(3) 0.045(2) -0.0196(19) 0.0091(16) -0.0126(19) O17 0.0393(16) 0.0286(14) 0.0369(16) -0.0075(12) -0.0058(13) -0.0110(13) N18 0.0284(18) 0.0293(18) 0.048(2) -0.0188(16) -0.0052(16) -0.0010(15) N19 0.0261(17) 0.0206(15) 0.042(2) -0.0050(14) -0.0058(14) -0.0033(13) N20 0.0354(19) 0.0259(16) 0.0310(17) -0.0041(13) -0.0083(15) -0.0097(14) C21 0.082(5) 0.074(4) 0.063(4) -0.014(3) 0.032(4) 0.005(4) C22 0.052(3) 0.031(2) 0.064(3) -0.011(2) -0.030(3) -0.002(2) C23 0.070(4) 0.080(4) 0.047(3) -0.020(3) 0.003(3) -0.025(3) C24 0.073(4) 0.040(3) 0.050(3) -0.009(2) 0.007(3) -0.030(3) C25 0.047(3) 0.048(3) 0.067(4) -0.013(3) -0.023(3) 0.006(2) C26 0.035(2) 0.034(2) 0.064(3) -0.023(2) -0.005(2) -0.0086(19) C27 0.036(2) 0.026(2) 0.050(3) -0.0148(18) -0.002(2) -0.0033(18) C28 0.029(2) 0.0246(19) 0.041(2) -0.0102(17) 0.0006(18) -0.0019(16) C29 0.034(2) 0.029(2) 0.038(2) -0.0100(17) 0.0008(18) -0.0028(17) C30 0.033(2) 0.0248(19) 0.047(3) -0.0087(18) -0.0069(19) 0.0040(17) C31 0.046(3) 0.037(2) 0.046(3) -0.016(2) -0.005(2) -0.009(2) C32 0.032(2) 0.050(3) 0.052(3) -0.010(2) 0.002(2) -0.008(2) C33 0.042(3) 0.030(2) 0.046(3) -0.0045(19) -0.010(2) 0.0013(19) C34 0.051(3) 0.025(2) 0.065(3) -0.011(2) -0.008(2) -0.004(2) C35 0.043(3) 0.033(2) 0.069(3) -0.019(2) -0.005(2) -0.010(2) C36 0.036(2) 0.0233(18) 0.032(2) -0.0073(16) -0.0076(17) -0.0021(17) C37 0.034(2) 0.0275(19) 0.0258(19) -0.0027(15) -0.0080(16) -0.0059(17) C38 0.032(2) 0.030(2) 0.029(2) -0.0028(16) -0.0070(16) -0.0081(17) C39 0.035(2) 0.029(2) 0.033(2) -0.0030(16) -0.0102(17) -0.0076(17) C40 0.042(2) 0.030(2) 0.044(3) -0.0064(18) -0.017(2) -0.0065(19) C41 0.058(3) 0.027(2) 0.053(3) -0.007(2) -0.021(2) -0.004(2) C42 0.059(3) 0.040(3) 0.044(3) -0.017(2) -0.005(2) -0.013(2) C43 0.051(3) 0.041(3) 0.072(4) -0.018(3) -0.021(3) -0.014(2) C44 0.037(2) 0.035(2) 0.046(3) -0.0042(19) -0.013(2) -0.0110(19) C45 0.030(2) 0.040(2) 0.055(3) -0.007(2) -0.008(2) -0.0052(19) C46 0.036(2) 0.032(2) 0.038(2) -0.0060(18) -0.0105(19) -0.0007(18) C47 0.031(2) 0.0254(19) 0.036(2) -0.0056(16) -0.0026(17) -0.0119(16) C48 0.035(2) 0.027(2) 0.049(3) -0.0079(18) -0.015(2) -0.0039(18) C49 0.032(2) 0.027(2) 0.055(3) -0.0037(19) -0.014(2) -0.0046(18) C50 0.033(2) 0.0244(19) 0.038(2) -0.0039(16) -0.0038(17) -0.0096(17) C51 0.038(2) 0.0215(18) 0.042(2) -0.0051(16) -0.0067(19) -0.0054(17) C52 0.055(3) 0.029(2) 0.044(3) 0.0040(19) -0.012(2) -0.008(2) C53 0.031(2) 0.034(2) 0.057(3) -0.002(2) -0.010(2) -0.0043(19) C54 0.051(3) 0.025(2) 0.051(3) -0.0045(19) -0.013(2) 0.002(2) C55 0.050(3) 0.0236(19) 0.043(3) -0.0058(17) -0.014(2) -0.0055(19) C56 0.062(3) 0.035(2) 0.054(3) -0.013(2) -0.028(3) -0.007(2) C57 0.030(2) 0.0257(19) 0.029(2) -0.0070(15) -0.0016(16) -0.0019(16) C58 0.0250(18) 0.0235(17) 0.0263(19) -0.0050(14) -0.0026(15) 0.0014(15) C59 0.029(2) 0.0257(18) 0.030(2) -0.0054(15) -0.0067(16) -0.0014(16) C60 0.029(2) 0.032(2) 0.029(2) -0.0012(16) -0.0061(16) 0.0013(17) C61 0.034(2) 0.038(2) 0.031(2) -0.0116(18) -0.0011(18) 0.0012(19) C62 0.035(2) 0.029(2) 0.040(2) -0.0110(17) -0.0072(19) 0.0022(18) C63 0.033(2) 0.0247(19) 0.035(2) -0.0048(16) 0.0002(17) -0.0056(17) C64 0.057(3) 0.036(3) 0.070(4) -0.024(2) -0.005(3) -0.008(2) C65 0.036(2) 0.054(3) 0.037(2) -0.007(2) 0.008(2) -0.007(2) C66 0.046(3) 0.030(2) 0.045(3) 0.0009(19) 0.004(2) 0.000(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3517(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 . Mn2 . 3.2675(9) yes Mn1 . Mn3 . 3.2785(8) yes Mn1 . O5 . 1.897(3) yes Mn1 . O6 . 2.328(4) yes Mn1 . O7 . 1.913(3) yes Mn1 . O11 . 1.869(3) yes Mn1 . O17 . 2.247(3) yes Mn1 . N20 . 1.991(3) yes Mn2 . O5 . 1.891(3) yes Mn2 . O8 . 1.871(3) yes Mn2 . O9 . 1.915(3) yes Mn2 . O15 . 2.212(3) yes Mn2 . O16 . 2.358(3) yes Mn2 . N18 . 2.005(3) yes Mn3 . O5 . 1.886(3) yes Mn3 . O10 . 1.926(3) yes Mn3 . O12 . 1.869(3) yes Mn3 . O13 . 2.077(3) yes Mn3 . N19 . 1.997(3) yes O6 . C23 . 1.428(6) yes O6 . H12 . 0.824 no O7 . N18 . 1.378(5) yes O8 . C28 . 1.333(5) yes O9 . N19 . 1.373(4) yes O10 . N20 . 1.395(4) yes O11 . C38 . 1.331(5) yes O12 . C47 . 1.343(5) yes O13 . C57 . 1.247(5) yes O14 . C57 . 1.271(5) yes O15 . C66 . 1.420(5) yes O15 . H74 . 0.818 no O16 . C21 . 1.412(7) yes O16 . H161 . 0.850 no O17 . C24 . 1.420(5) yes O17 . H171 . 0.850 no N18 . C26 . 1.280(6) yes N19 . C49 . 1.293(5) yes N20 . C36 . 1.274(5) yes C21 . H10 . 0.963 no C21 . H34 . 0.967 no C21 . H70 . 0.959 no C22 . C48 . 1.409(6) yes C22 . C56 . 1.377(6) yes C22 . H221 . 0.930 no C23 . H231 . 0.969 no C23 . H232 . 0.968 no C23 . H233 . 0.965 no C24 . H241 . 0.960 no C24 . H242 . 0.960 no C24 . H243 . 0.960 no C25 . C30 . 1.545(6) yes C25 . H251 . 0.961 no C25 . H252 . 0.958 no C25 . H253 . 0.951 no C26 . C27 . 1.442(7) yes C26 . H261 . 0.932 no C27 . C28 . 1.419(6) yes C27 . C35 . 1.418(6) yes C28 . C29 . 1.415(6) yes C29 . C30 . 1.528(6) yes C29 . C33 . 1.400(6) yes C30 . C31 . 1.544(6) yes C30 . C32 . 1.537(7) yes C31 . H311 . 0.970 no C31 . H312 . 0.960 no C31 . H313 . 0.964 no C32 . H321 . 0.960 no C32 . H322 . 0.962 no C32 . H323 . 0.966 no C33 . C34 . 1.382(7) yes C33 . H331 . 0.928 no C34 . C35 . 1.371(7) yes C34 . H341 . 0.924 no C35 . H351 . 0.924 no C36 . C37 . 1.453(6) yes C36 . H361 . 0.930 no C37 . C38 . 1.423(6) yes C37 . C46 . 1.402(6) yes C38 . C39 . 1.421(6) yes C39 . C40 . 1.541(6) yes C39 . C44 . 1.379(6) yes C40 . C41 . 1.544(6) yes C40 . C42 . 1.534(7) yes C40 . C43 . 1.533(6) yes C41 . H411 . 0.950 no C41 . H412 . 0.967 no C41 . H413 . 0.954 no C42 . H421 . 0.953 no C42 . H422 . 0.955 no C42 . H423 . 0.958 no C43 . H431 . 0.951 no C43 . H432 . 0.958 no C43 . H433 . 0.961 no C44 . C45 . 1.404(6) yes C44 . H441 . 0.929 no C45 . C46 . 1.359(6) yes C45 . H451 . 0.928 no C46 . H461 . 0.936 no C47 . C48 . 1.408(6) yes C47 . C50 . 1.417(5) yes C48 . C49 . 1.448(6) yes C49 . H491 . 0.940 no C50 . C51 . 1.533(6) yes C50 . C55 . 1.400(6) yes C51 . C52 . 1.523(6) yes C51 . C53 . 1.529(6) yes C51 . C54 . 1.535(6) yes C52 . H521 . 0.958 no C52 . H522 . 0.953 no C52 . H523 . 0.947 no C53 . H531 . 0.959 no C53 . H532 . 0.952 no C53 . H533 . 0.960 no C54 . H541 . 0.955 no C54 . H542 . 0.961 no C54 . H543 . 0.960 no C55 . C56 . 1.387(6) yes C55 . H551 . 0.930 no C56 . H561 . 0.926 no C57 . C58 . 1.505(5) yes C58 . C59 . 1.383(6) yes C58 . C63 . 1.392(5) yes C59 . C60 . 1.395(6) yes C59 . H591 . 0.931 no C60 . C61 . 1.392(6) yes C60 . C65 . 1.499(6) yes C61 . C62 . 1.384(7) yes C61 . H611 . 0.934 no C62 . C63 . 1.402(6) yes C62 . C64 . 1.500(6) yes C63 . H631 . 0.930 no C64 . H641 . 0.957 no C64 . H642 . 0.957 no C64 . H643 . 0.960 no C65 . H651 . 0.955 no C65 . H652 . 0.956 no C65 . H653 . 0.959 no C66 . H661 . 0.963 no C66 . H662 . 0.964 no C66 . H663 . 0.960 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 Mn2 . Mn1 . Mn3 . 60.168(18) yes Mn2 . Mn1 . O5 . 30.34(8) yes Mn3 . Mn1 . O5 . 29.83(8) yes Mn2 . Mn1 . O6 . 87.63(9) yes Mn3 . Mn1 . O6 . 88.00(10) yes O5 . Mn1 . O6 . 87.40(12) yes Mn2 . Mn1 . O7 . 62.87(9) yes Mn3 . Mn1 . O7 . 123.01(9) yes O5 . Mn1 . O7 . 93.20(12) yes O6 . Mn1 . O7 . 91.50(15) yes Mn2 . Mn1 . O11 . 153.16(9) yes Mn3 . Mn1 . O11 . 146.16(9) yes O5 . Mn1 . O11 . 174.39(13) yes O6 . Mn1 . O11 . 88.47(13) yes O7 . Mn1 . O11 . 90.71(13) yes Mn2 . Mn1 . O17 . 94.79(8) yes Mn3 . Mn1 . O17 . 91.16(7) yes O5 . Mn1 . O17 . 93.50(11) yes O6 . Mn1 . O17 . 176.62(13) yes O7 . Mn1 . O17 . 91.70(13) yes Mn2 . Mn1 . N20 . 118.31(10) yes Mn3 . Mn1 . N20 . 58.16(10) yes O5 . Mn1 . N20 . 87.99(12) yes O6 . Mn1 . N20 . 91.56(14) yes O7 . Mn1 . N20 . 176.77(15) yes O11 . Mn1 . O17 . 90.41(12) yes O11 . Mn1 . N20 . 88.32(13) yes O17 . Mn1 . N20 . 85.22(13) yes Mn1 . Mn2 . O5 . 30.45(8) yes Mn1 . Mn2 . O8 . 148.08(9) yes O5 . Mn2 . O8 . 178.33(12) yes Mn1 . Mn2 . O9 . 121.41(9) yes O5 . Mn2 . O9 . 91.66(12) yes O8 . Mn2 . O9 . 89.62(12) yes Mn1 . Mn2 . O15 . 92.88(8) yes O5 . Mn2 . O15 . 88.73(11) yes O8 . Mn2 . O15 . 92.25(12) yes O9 . Mn2 . O15 . 93.73(13) yes Mn1 . Mn2 . O16 . 82.16(9) yes O5 . Mn2 . O16 . 87.47(13) yes O8 . Mn2 . O16 . 91.47(14) yes O9 . Mn2 . O16 . 89.73(14) yes O15 . Mn2 . O16 . 174.93(12) yes Mn1 . Mn2 . N18 . 59.19(10) yes O5 . Mn2 . N18 . 89.44(13) yes O8 . Mn2 . N18 . 89.20(13) yes O9 . Mn2 . N18 . 174.66(15) yes O15 . Mn2 . N18 . 91.52(14) yes O16 . Mn2 . N18 . 85.10(15) yes Mn1 . Mn3 . O5 . 30.03(8) yes Mn1 . Mn3 . O10 . 62.28(8) yes O5 . Mn3 . O10 . 91.69(12) yes Mn1 . Mn3 . O12 . 148.11(9) yes O5 . Mn3 . O12 . 162.31(12) yes O10 . Mn3 . O12 . 87.78(12) yes Mn1 . Mn3 . O13 . 103.98(9) yes O5 . Mn3 . O13 . 106.08(12) yes O10 . Mn3 . O13 . 100.42(13) yes O12 . Mn3 . O13 . 91.39(12) yes Mn1 . Mn3 . N19 . 117.76(10) yes O5 . Mn3 . N19 . 87.81(12) yes O10 . Mn3 . N19 . 165.05(14) yes O12 . Mn3 . N19 . 88.18(13) yes O13 . Mn3 . N19 . 94.07(14) yes Mn1 . O5 . Mn2 . 119.22(14) yes Mn1 . O5 . Mn3 . 120.14(14) yes Mn2 . O5 . Mn3 . 120.64(14) yes Mn1 . O6 . C23 . 124.0(4) yes Mn1 . O6 . H12 . 86.7 no C23 . O6 . H12 . 110.4 no Mn1 . O7 . N18 . 117.4(2) yes Mn2 . O8 . C28 . 132.9(3) yes Mn2 . O9 . N19 . 115.8(2) yes Mn3 . O10 . N20 . 113.9(2) yes Mn1 . O11 . C38 . 125.4(3) yes Mn3 . O12 . C47 . 122.3(2) yes Mn3 . O13 . C57 . 141.0(3) yes Mn2 . O15 . C66 . 129.1(3) yes Mn2 . O15 . H74 . 116.6 no C66 . O15 . H74 . 108.2 no Mn2 . O16 . C21 . 116.5(4) yes Mn2 . O16 . H161 . 98.2 no C21 . O16 . H161 . 109.1 no Mn1 . O17 . C24 . 125.4(3) yes Mn1 . O17 . H171 . 113.9 no C24 . O17 . H171 . 105.5 no O7 . N18 . Mn2 . 119.4(3) yes O7 . N18 . C26 . 114.1(4) yes Mn2 . N18 . C26 . 126.4(3) yes O9 . N19 . Mn3 . 120.6(2) yes O9 . N19 . C49 . 115.5(3) yes Mn3 . N19 . C49 . 123.8(3) yes O10 . N20 . Mn1 . 118.8(2) yes O10 . N20 . C36 . 116.3(3) yes Mn1 . N20 . C36 . 124.9(3) yes O16 . C21 . H10 . 109.8 no O16 . C21 . H34 . 107.9 no H10 . C21 . H34 . 109.6 no O16 . C21 . H70 . 110.7 no H10 . C21 . H70 . 109.7 no H34 . C21 . H70 . 109.1 no C48 . C22 . C56 . 120.4(4) yes C48 . C22 . H221 . 120.1 no C56 . C22 . H221 . 119.4 no O6 . C23 . H231 . 110.6 no O6 . C23 . H232 . 110.5 no H231 . C23 . H232 . 108.1 no O6 . C23 . H233 . 110.9 no H231 . C23 . H233 . 108.3 no H232 . C23 . H233 . 108.4 no O17 . C24 . H241 . 109.1 no O17 . C24 . H242 . 109.9 no H241 . C24 . H242 . 109.5 no O17 . C24 . H243 . 109.4 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C30 . C25 . H251 . 109.4 no C30 . C25 . H252 . 110.4 no H251 . C25 . H252 . 108.8 no C30 . C25 . H253 . 109.1 no H251 . C25 . H253 . 109.2 no H252 . C25 . H253 . 110.0 no N18 . C26 . C27 . 126.0(4) yes N18 . C26 . H261 . 116.9 no C27 . C26 . H261 . 117.0 no C26 . C27 . C28 . 122.4(4) yes C26 . C27 . C35 . 117.5(4) yes C28 . C27 . C35 . 120.1(4) yes C27 . C28 . O8 . 120.9(4) yes C27 . C28 . C29 . 119.8(4) yes O8 . C28 . C29 . 119.3(4) yes C28 . C29 . C30 . 121.9(4) yes C28 . C29 . C33 . 117.2(4) yes C30 . C29 . C33 . 120.9(4) yes C25 . C30 . C29 . 112.1(4) yes C25 . C30 . C31 . 107.3(4) yes C29 . C30 . C31 . 109.7(4) yes C25 . C30 . C32 . 107.7(4) yes C29 . C30 . C32 . 110.2(4) yes C31 . C30 . C32 . 109.7(4) yes C30 . C31 . H311 . 109.5 no C30 . C31 . H312 . 110.3 no H311 . C31 . H312 . 109.7 no C30 . C31 . H313 . 109.6 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 108.3 no C30 . C32 . H321 . 110.7 no C30 . C32 . H322 . 110.6 no H321 . C32 . H322 . 108.4 no C30 . C32 . H323 . 109.2 no H321 . C32 . H323 . 109.3 no H322 . C32 . H323 . 108.6 no C29 . C33 . C34 . 123.6(4) yes C29 . C33 . H331 . 118.2 no C34 . C33 . H331 . 118.2 no C33 . C34 . C35 . 119.5(4) yes C33 . C34 . H341 . 119.9 no C35 . C34 . H341 . 120.6 no C27 . C35 . C34 . 119.9(4) yes C27 . C35 . H351 . 119.6 no C34 . C35 . H351 . 120.5 no N20 . C36 . C37 . 123.7(4) yes N20 . C36 . H361 . 118.3 no C37 . C36 . H361 . 118.0 no C36 . C37 . C38 . 121.8(4) yes C36 . C37 . C46 . 117.9(4) yes C38 . C37 . C46 . 120.3(4) yes C37 . C38 . O11 . 120.4(4) yes C37 . C38 . C39 . 119.2(4) yes O11 . C38 . C39 . 120.3(4) yes C38 . C39 . C40 . 120.8(4) yes C38 . C39 . C44 . 117.3(4) yes C40 . C39 . C44 . 121.9(4) yes C39 . C40 . C41 . 110.2(4) yes C39 . C40 . C42 . 110.4(4) yes C41 . C40 . C42 . 109.8(4) yes C39 . C40 . C43 . 111.9(4) yes C41 . C40 . C43 . 106.8(4) yes C42 . C40 . C43 . 107.6(4) yes C40 . C41 . H411 . 109.4 no C40 . C41 . H412 . 109.9 no H411 . C41 . H412 . 109.0 no C40 . C41 . H413 . 110.9 no H411 . C41 . H413 . 107.8 no H412 . C41 . H413 . 109.7 no C40 . C42 . H421 . 109.3 no C40 . C42 . H422 . 108.6 no H421 . C42 . H422 . 109.0 no C40 . C42 . H423 . 110.5 no H421 . C42 . H423 . 109.0 no H422 . C42 . H423 . 110.4 no C40 . C43 . H431 . 109.0 no C40 . C43 . H432 . 111.0 no H431 . C43 . H432 . 109.0 no C40 . C43 . H433 . 108.6 no H431 . C43 . H433 . 109.8 no H432 . C43 . H433 . 109.5 no C39 . C44 . C45 . 123.4(4) yes C39 . C44 . H441 . 118.9 no C45 . C44 . H441 . 117.7 no C44 . C45 . C46 . 119.1(4) yes C44 . C45 . H451 . 119.9 no C46 . C45 . H451 . 120.9 no C37 . C46 . C45 . 120.3(4) yes C37 . C46 . H461 . 119.9 no C45 . C46 . H461 . 119.8 no O12 . C47 . C48 . 119.8(4) yes O12 . C47 . C50 . 119.8(4) yes C48 . C47 . C50 . 120.4(4) yes C22 . C48 . C47 . 119.9(4) yes C22 . C48 . C49 . 117.7(4) yes C47 . C48 . C49 . 122.4(4) yes C48 . C49 . N19 . 123.5(4) yes C48 . C49 . H491 . 118.9 no N19 . C49 . H491 . 117.6 no C47 . C50 . C51 . 121.5(4) yes C47 . C50 . C55 . 116.9(4) yes C51 . C50 . C55 . 121.5(4) yes C50 . C51 . C52 . 110.7(4) yes C50 . C51 . C53 . 109.4(3) yes C52 . C51 . C53 . 109.9(4) yes C50 . C51 . C54 . 112.0(4) yes C52 . C51 . C54 . 107.6(4) yes C53 . C51 . C54 . 107.2(4) yes C51 . C52 . H521 . 108.7 no C51 . C52 . H522 . 109.8 no H521 . C52 . H522 . 109.9 no C51 . C52 . H523 . 109.4 no H521 . C52 . H523 . 109.4 no H522 . C52 . H523 . 109.6 no C51 . C53 . H531 . 109.9 no C51 . C53 . H532 . 109.5 no H531 . C53 . H532 . 108.2 no C51 . C53 . H533 . 110.5 no H531 . C53 . H533 . 109.1 no H532 . C53 . H533 . 109.6 no C51 . C54 . H541 . 108.7 no C51 . C54 . H542 . 108.9 no H541 . C54 . H542 . 108.9 no C51 . C54 . H543 . 110.5 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 110.2 no C50 . C55 . C56 . 123.4(4) yes C50 . C55 . H551 . 118.4 no C56 . C55 . H551 . 118.1 no C55 . C56 . C22 . 119.0(4) yes C55 . C56 . H561 . 120.7 no C22 . C56 . H561 . 120.2 no O14 . C57 . O13 . 124.7(4) yes O14 . C57 . C58 . 117.2(4) yes O13 . C57 . C58 . 118.1(4) yes C57 . C58 . C59 . 119.4(4) yes C57 . C58 . C63 . 120.3(4) yes C59 . C58 . C63 . 120.3(4) yes C58 . C59 . C60 . 120.7(4) yes C58 . C59 . H591 . 119.4 no C60 . C59 . H591 . 119.9 no C59 . C60 . C61 . 118.1(4) yes C59 . C60 . C65 . 119.8(4) yes C61 . C60 . C65 . 122.1(4) yes C60 . C61 . C62 . 122.5(4) yes C60 . C61 . H611 . 118.7 no C62 . C61 . H611 . 118.9 no C61 . C62 . C63 . 118.4(4) yes C61 . C62 . C64 . 121.1(4) yes C63 . C62 . C64 . 120.5(4) yes C62 . C63 . C58 . 120.0(4) yes C62 . C63 . H631 . 119.7 no C58 . C63 . H631 . 120.2 no C62 . C64 . H641 . 109.6 no C62 . C64 . H642 . 110.1 no H641 . C64 . H642 . 109.7 no C62 . C64 . H643 . 108.6 no H641 . C64 . H643 . 109.5 no H642 . C64 . H643 . 109.2 no C60 . C65 . H651 . 111.5 no C60 . C65 . H652 . 109.7 no H651 . C65 . H652 . 108.5 no C60 . C65 . H653 . 109.7 no H651 . C65 . H653 . 108.7 no H652 . C65 . H653 . 108.7 no O15 . C66 . H661 . 111.0 no O15 . C66 . H662 . 109.1 no H661 . C66 . H662 . 108.9 no O15 . C66 . H663 . 108.6 no H661 . C66 . H663 . 109.9 no H662 . C66 . H663 . 109.4 no # Attachment 'Complex 14.cif' data_Eb7063 _database_code_depnum_ccdc_archive 'CCDC 736441' _audit_creation_date 07-05-08 _audit_creation_method CRYSTALS_ver_12.84 _chemical_compound_source ' C.Milios reaction CM3552 ' _exptl_crystal_recrystallization_method ; Evaporation of ethanol solution ; _oxford_structure_analysis_title 'eb7063 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.6577(3) _cell_length_b 14.3628(3) _cell_length_c 15.5107(3) _cell_angle_alpha 76.2850(10) _cell_angle_beta 86.2710(10) _cell_angle_gamma 73.3250(10) _cell_volume 2831.55(10) _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' 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' 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' _cell_formula_units_Z 2 # Given Formula = C49 H65 Mn3 N4 O18 # Dc = 1.36 Fooo = 1140.00 Mu = 7.29 M = 1162.86 # Found Formula = C47 H57 Mn3 N4 O16 # Dc = 1.29 FOOO = 1140.00 Mu = 7.23 M = 1098.77 _chemical_formula_sum 'C49 H65 Mn3 N4 O18 ' _chemical_formula_moiety '[(Mn3O)(C9O2NH9)3(C7O2H5)2(C6O3NH16)(H20)2]' _chemical_formula_weight 1162.86 _cell_measurement_reflns_used 7021 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description rhombus _exptl_crystal_colour green _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.38 _exptl_crystal_density_diffrn 1.36 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 0.729 # Sheldrick geometric approximatio 0.86 0.94 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.94 _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 41137 _reflns_number_total 15881 _diffrn_reflns_av_R_equivalents 0.054 # Number of reflections with Friedels Law is 15881 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 17379 _diffrn_reflns_theta_min 1.846 _diffrn_reflns_theta_max 30.567 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 27.816 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min -19 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _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 -0.77 _refine_diff_density_max 0.76 _refine_ls_number_reflns 15879 _refine_ls_number_restraints 0 _refine_ls_number_parameters 631 #_refine_ls_R_factor_ref 0.0812 _refine_ls_wR_factor_ref 0.1574 _refine_ls_goodness_of_fit_ref 0.9471 #_reflns_number_all 15879 _refine_ls_R_factor_all 0.0812 _refine_ls_wR_factor_all 0.1574 # 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 9932 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_gt 0.1223 _refine_ls_shift/su_max 0.000244 # 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 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: 70.3 112. 67.8 29.1 6.21 ; 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 0.500 0.500 0.006 564.8 74.2 _platon_squeeze_details ; This amount to 1EtOH and 1 H2O per foumula unit. The values of F(000), Dcalc, M and mu have been calculated on this assumption. ; _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. Checkcif Output: 912_ALERT_3_A # Missing FCF Reflections Above STH/L=0.6 ...... 1501 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 4 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 7 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 5 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.999 5939 5933 6 23.01 0.550 0.999 7879 7872 7 25.24 0.600 0.999 10255 10244 11 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.997 13024 12987 37 29.84 0.700 0.948 16264 15411 853 30.57 0.716 0.913 17393 15881 1512 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.64 Ratio 220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.58 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.10 Ratio The atoms in question may be subject to large thermal motion due to freedom to move 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 applied (see above) 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C47 H57 Mn3 N4 O16 No action taken 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C73 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 .. N16 Numbering Scheme is sound # 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. 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. 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 Mn3 Mn 0.07807(3) 0.14073(3) 0.01471(3) 0.0181 1.0000 Uani . . . . . . Mn2 Mn 0.18230(3) 0.20540(3) -0.17655(3) 0.0192 1.0000 Uani . . . . . . Mn1 Mn 0.01350(3) 0.36921(3) -0.10186(3) 0.0187 1.0000 Uani . . . . . . O123 O 0.10404(16) 0.23988(14) -0.07937(13) 0.0196 1.0000 Uani . . . . . . O11 O 0.04150(17) 0.04974(14) 0.11230(13) 0.0227 1.0000 Uani . . . . . . C11 C 0.0387(2) 0.0645(2) 0.19432(19) 0.0225 1.0000 Uani . . . . . . C21 C 0.0667(3) -0.0196(2) 0.2650(2) 0.0279 1.0000 Uani . . . . . . C31 C 0.0703(3) -0.0101(3) 0.3511(2) 0.0325 1.0000 Uani . . . . . . C41 C 0.0446(3) 0.0839(3) 0.3702(2) 0.0327 1.0000 Uani . . . . . . C51 C 0.0136(3) 0.1671(2) 0.3018(2) 0.0290 1.0000 Uani . . . . . . C61 C 0.0083(2) 0.1608(2) 0.21383(19) 0.0226 1.0000 Uani . . . . . . C71 C -0.0340(2) 0.2525(2) 0.14538(19) 0.0222 1.0000 Uani . . . . . . N71 N -0.01696(19) 0.25075(17) 0.06246(16) 0.0210 1.0000 Uani . . . . . . O71 O -0.06713(16) 0.33409(15) -0.00006(14) 0.0232 1.0000 Uani . . . . . . C81 C -0.0987(3) 0.3462(2) 0.1705(2) 0.0258 1.0000 Uani . . . . . . C91 C -0.2053(3) 0.3435(3) 0.2003(4) 0.0526 1.0000 Uani . . . . . . N73 N 0.09217(19) 0.40632(17) -0.21197(15) 0.0197 1.0000 Uani . . . . . . O73 O 0.18865(16) 0.34238(15) -0.21471(14) 0.0224 1.0000 Uani . . . . . . C73 C 0.0645(2) 0.4794(2) -0.28083(18) 0.0210 1.0000 Uani . . . . . . C63 C -0.0387(2) 0.5478(2) -0.28376(19) 0.0239 1.0000 Uani . . . . . . C13 C -0.1016(2) 0.5550(2) -0.20789(19) 0.0235 1.0000 Uani . . . . . . O13 O -0.07173(16) 0.50013(14) -0.12643(14) 0.0222 1.0000 Uani . . . . . . C23 C -0.1980(3) 0.6246(3) -0.2170(2) 0.0355 1.0000 Uani . . . . . . C33 C -0.2325(3) 0.6853(3) -0.2990(3) 0.0484 1.0000 Uani . . . . . . C43 C -0.1729(4) 0.6780(3) -0.3735(3) 0.0489 1.0000 Uani . . . . . . C53 C -0.0771(3) 0.6106(2) -0.3657(2) 0.0343 1.0000 Uani . . . . . . C83 C 0.1370(3) 0.4908(2) -0.3571(2) 0.0278 1.0000 Uani . . . . . . C93 C 0.1317(3) 0.4264(3) -0.4211(2) 0.0372 1.0000 Uani . . . . . . O14 O 0.20219(18) 0.13472(17) 0.10012(15) 0.0284 1.0000 Uani . . . . . . C14 C 0.2736(2) 0.1705(2) 0.1071(2) 0.0238 1.0000 Uani . . . . . . C24 C 0.3375(2) 0.1252(3) 0.1904(2) 0.0297 1.0000 Uani . . . . . . C74 C 0.4304(3) 0.1446(3) 0.1969(2) 0.0384 1.0000 Uani . . . . . . C64 C 0.4885(3) 0.0997(4) 0.2743(3) 0.0519 1.0000 Uani . . . . . . C54 C 0.4530(3) 0.0396(4) 0.3442(3) 0.0578 1.0000 Uani . . . . . . C44 C 0.3611(3) 0.0207(4) 0.3375(2) 0.0479 1.0000 Uani . . . . . . C34 C 0.3025(3) 0.0633(3) 0.2605(2) 0.0345 1.0000 Uani . . . . . . O24 O 0.29584(18) 0.24038(17) 0.05010(15) 0.0282 1.0000 Uani . . . . . . O72 O 0.17012(16) 0.03755(14) -0.03627(13) 0.0209 1.0000 Uani . . . . . . C72 C 0.2026(2) -0.0089(2) -0.16869(18) 0.0205 1.0000 Uani . . . . . . C62 C 0.2195(2) 0.0150(2) -0.26548(19) 0.0239 1.0000 Uani . . . . . . C12 C 0.2485(2) 0.0996(2) -0.31016(19) 0.0257 1.0000 Uani . . . . . . O12 O 0.26781(17) 0.16424(16) -0.26837(14) 0.0245 1.0000 Uani . . . . . . C22 C 0.2612(3) 0.1186(3) -0.4026(2) 0.0324 1.0000 Uani . . . . . . C32 C 0.2443(3) 0.0548(3) -0.4504(2) 0.0424 1.0000 Uani . . . . . . C42 C 0.2163(3) -0.0297(3) -0.4071(3) 0.0431 1.0000 Uani . . . . . . C52 C 0.2043(3) -0.0489(3) -0.3167(2) 0.0350 1.0000 Uani . . . . . . C82 C 0.2104(2) -0.1145(2) -0.1193(2) 0.0245 1.0000 Uani . . . . . . C92 C 0.3215(3) -0.1799(2) -0.1092(2) 0.0334 1.0000 Uani . . . . . . O18 O -0.05364(18) 0.13324(15) -0.06429(14) 0.0249 1.0000 Uani . . . . . . O25 O -0.07984(17) 0.32164(16) -0.19211(14) 0.0254 1.0000 Uani . . . . . . C15 C -0.0395(2) 0.2879(2) -0.2586(2) 0.0233 1.0000 Uani . . . . . . O15 O 0.05174(17) 0.23825(16) -0.26356(14) 0.0263 1.0000 Uani . . . . . . C25 C -0.1074(2) 0.3059(2) -0.3372(2) 0.0263 1.0000 Uani . . . . . . C35 C -0.0705(3) 0.2613(2) -0.4076(2) 0.0310 1.0000 Uani . . . . . . C45 C -0.1340(3) 0.2759(3) -0.4791(2) 0.0414 1.0000 Uani . . . . . . C55 C -0.2333(4) 0.3346(4) -0.4803(3) 0.0501 1.0000 Uani . . . . . . C65 C -0.2703(3) 0.3796(4) -0.4114(3) 0.0557 1.0000 Uani . . . . . . C75 C -0.2074(3) 0.3657(3) -0.3396(2) 0.0418 1.0000 Uani . . . . . . O17 O 0.12207(17) 0.40528(15) -0.01827(14) 0.0256 1.0000 Uani . . . . . . O26 O 0.32790(16) 0.18577(15) -0.10260(13) 0.0237 1.0000 Uani . . . . . . C26 C 0.4224(3) 0.1091(2) -0.0898(2) 0.0284 1.0000 Uani . . . . . . C16 C 0.4823(3) 0.1170(3) -0.1747(2) 0.0327 1.0000 Uani . . . . . . N16 N 0.5076(2) 0.2145(2) -0.2033(2) 0.0378 1.0000 Uani . . . . . . C56 C 0.5787(3) 0.2303(3) -0.1415(3) 0.0420 1.0000 Uani . . . . . . C66 C 0.6768(3) 0.1470(3) -0.1186(3) 0.0427 1.0000 Uani . . . . . . O66 O 0.6546(2) 0.0675(2) -0.05586(19) 0.0416 1.0000 Uani . . . . . . C36 C 0.5468(3) 0.2304(5) -0.2967(3) 0.0612 1.0000 Uani . . . . . . C46 C 0.4700(4) 0.2305(6) -0.3632(3) 0.0748 1.0000 Uani . . . . . . O46 O 0.3747(2) 0.2997(3) -0.3548(2) 0.0698 1.0000 Uani . . . . . . N72 N 0.18314(19) 0.06264(17) -0.12702(15) 0.0197 1.0000 Uani . . . . . . H211 H 0.0834 -0.0844 0.2534 0.0326 1.0000 Uiso . . . . . . H311 H 0.0904 -0.0682 0.3977 0.0379 1.0000 Uiso . . . . . . H411 H 0.0486 0.0905 0.4293 0.0402 1.0000 Uiso . . . . . . H511 H -0.0050 0.2312 0.3150 0.0357 1.0000 Uiso . . . . . . H811 H -0.0639 0.3576 0.2196 0.0320 1.0000 Uiso . . . . . . H812 H -0.1040 0.4026 0.1183 0.0320 1.0000 Uiso . . . . . . H911 H -0.2423 0.4069 0.2154 0.0653 1.0000 Uiso . . . . . . H912 H -0.2017 0.2887 0.2526 0.0653 1.0000 Uiso . . . . . . H913 H -0.2414 0.3332 0.1523 0.0653 1.0000 Uiso . . . . . . H221 H 0.2815 0.1759 -0.4326 0.0370 1.0000 Uiso . . . . . . H321 H 0.2519 0.0689 -0.5130 0.0513 1.0000 Uiso . . . . . . H421 H 0.2055 -0.0741 -0.4397 0.0549 1.0000 Uiso . . . . . . H521 H 0.1850 -0.1071 -0.2875 0.0439 1.0000 Uiso . . . . . . H821 H 0.1715 -0.1436 -0.1522 0.0296 1.0000 Uiso . . . . . . H822 H 0.1804 -0.1137 -0.0595 0.0296 1.0000 Uiso . . . . . . H921 H 0.3231 -0.2478 -0.0768 0.0386 1.0000 Uiso . . . . . . H922 H 0.3516 -0.1816 -0.1681 0.0386 1.0000 Uiso . . . . . . H923 H 0.3605 -0.1520 -0.0763 0.0386 1.0000 Uiso . . . . . . H231 H -0.2404 0.6302 -0.1663 0.0400 1.0000 Uiso . . . . . . H331 H -0.2980 0.7325 -0.3039 0.0513 1.0000 Uiso . . . . . . H431 H -0.1976 0.7191 -0.4297 0.0524 1.0000 Uiso . . . . . . H531 H -0.0359 0.6065 -0.4171 0.0387 1.0000 Uiso . . . . . . H831 H 0.1192 0.5617 -0.3896 0.0324 1.0000 Uiso . . . . . . H832 H 0.2075 0.4706 -0.3335 0.0324 1.0000 Uiso . . . . . . H931 H 0.1799 0.4357 -0.4699 0.0431 1.0000 Uiso . . . . . . H932 H 0.0623 0.4462 -0.4451 0.0431 1.0000 Uiso . . . . . . H933 H 0.1497 0.3560 -0.3895 0.0431 1.0000 Uiso . . . . . . H341 H 0.2391 0.0500 0.2560 0.0381 1.0000 Uiso . . . . . . H441 H 0.3373 -0.0218 0.3858 0.0509 1.0000 Uiso . . . . . . H541 H 0.4921 0.0110 0.3973 0.0616 1.0000 Uiso . . . . . . H641 H 0.5530 0.1109 0.2786 0.0595 1.0000 Uiso . . . . . . H741 H 0.4541 0.1879 0.1493 0.0436 1.0000 Uiso . . . . . . H351 H -0.0018 0.2209 -0.4069 0.0370 1.0000 Uiso . . . . . . H451 H -0.1088 0.2451 -0.5271 0.0501 1.0000 Uiso . . . . . . H551 H -0.2765 0.3441 -0.5291 0.0594 1.0000 Uiso . . . . . . H651 H -0.3390 0.4202 -0.4127 0.0606 1.0000 Uiso . . . . . . H751 H -0.2330 0.3972 -0.2922 0.0469 1.0000 Uiso . . . . . . H161 H 0.5468 0.0623 -0.1660 0.0358 1.0000 Uiso . . . . . . H162 H 0.4414 0.1102 -0.2221 0.0358 1.0000 Uiso . . . . . . H261 H 0.4620 0.1169 -0.0421 0.0311 1.0000 Uiso . . . . . . H262 H 0.4089 0.0430 -0.0730 0.0311 1.0000 Uiso . . . . . . H361 H 0.5626 0.2955 -0.3124 0.0643 1.0000 Uiso . . . . . . H362 H 0.6100 0.1763 -0.3000 0.0643 1.0000 Uiso . . . . . . H461 H 0.4964 0.2489 -0.4240 0.0801 1.0000 Uiso . . . . . . H462 H 0.4607 0.1629 -0.3527 0.0801 1.0000 Uiso . . . . . . H561 H 0.5971 0.2925 -0.1697 0.0471 1.0000 Uiso . . . . . . H562 H 0.5416 0.2384 -0.0855 0.0471 1.0000 Uiso . . . . . . H661 H 0.7269 0.1712 -0.0933 0.0478 1.0000 Uiso . . . . . . H662 H 0.7055 0.1242 -0.1727 0.0478 1.0000 Uiso . . . . . . H16 H 0.4477 0.2630 -0.2033 0.0493 1.0000 Uiso . . . . . . H66 H 0.7087 0.0351 -0.0274 0.0570 1.0000 Uiso . . . . . . H46 H 0.3426 0.2591 -0.3289 0.0916 1.0000 Uiso . . . . . . H26 H 0.3177 0.2032 -0.0540 0.0333 1.0000 Uiso . . . . . . H17 H 0.1061 0.4352 0.0276 0.0377 1.0000 Uiso . . . . . . H18 H 0.1764 0.3537 0.0031 0.0377 1.0000 Uiso . . . . . . H19 H -0.0618 0.1918 -0.1040 0.0382 1.0000 Uiso . . . . . . H20 H -0.0498 0.0756 -0.0794 0.0382 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 Mn3 0.0251(2) 0.01208(17) 0.01589(18) -0.00365(13) 0.00223(15) -0.00364(15) Mn2 0.0236(2) 0.01446(18) 0.01635(18) -0.00195(14) 0.00172(15) -0.00187(15) Mn1 0.0223(2) 0.01140(17) 0.02042(19) -0.00282(14) 0.00012(15) -0.00232(14) O123 0.0251(10) 0.0129(8) 0.0172(9) -0.0009(7) 0.0019(7) -0.0025(7) O11 0.0352(11) 0.0156(8) 0.0187(9) -0.0061(7) 0.0035(8) -0.0084(8) C11 0.0293(14) 0.0195(12) 0.0196(12) -0.0058(10) 0.0019(11) -0.0075(11) C21 0.0410(18) 0.0223(13) 0.0183(13) -0.0016(10) 0.0032(12) -0.0087(12) C31 0.0429(19) 0.0306(15) 0.0211(14) -0.0021(12) -0.0003(13) -0.0089(14) C41 0.0441(19) 0.0362(17) 0.0202(14) -0.0098(12) -0.0013(13) -0.0119(15) C51 0.0374(17) 0.0305(15) 0.0214(13) -0.0105(11) -0.0013(12) -0.0088(13) C61 0.0299(15) 0.0189(12) 0.0191(12) -0.0050(10) 0.0030(11) -0.0071(11) C71 0.0261(14) 0.0201(12) 0.0237(13) -0.0096(10) 0.0021(11) -0.0082(10) N71 0.0280(12) 0.0139(9) 0.0204(11) -0.0040(8) 0.0018(9) -0.0050(9) O71 0.0268(10) 0.0151(8) 0.0241(10) -0.0021(7) 0.0017(8) -0.0026(7) C81 0.0369(17) 0.0172(12) 0.0259(14) -0.0109(10) 0.0020(12) -0.0070(11) C91 0.042(2) 0.0318(18) 0.089(3) -0.032(2) 0.018(2) -0.0076(16) N73 0.0239(12) 0.0148(10) 0.0190(10) -0.0021(8) -0.0029(9) -0.0042(8) O73 0.0210(10) 0.0180(9) 0.0237(10) 0.0008(7) -0.0009(8) -0.0026(7) C73 0.0297(14) 0.0156(11) 0.0191(12) -0.0022(9) -0.0037(10) -0.0089(10) C63 0.0333(15) 0.0146(11) 0.0222(13) -0.0040(9) -0.0100(11) -0.0023(10) C13 0.0299(15) 0.0177(12) 0.0240(13) -0.0072(10) -0.0100(11) -0.0042(11) O13 0.0265(10) 0.0135(8) 0.0234(10) -0.0032(7) -0.0035(8) -0.0007(7) C23 0.0352(18) 0.0328(16) 0.0320(16) -0.0140(13) -0.0129(14) 0.0090(14) C33 0.050(2) 0.042(2) 0.0364(19) -0.0174(16) -0.0214(17) 0.0247(17) C43 0.065(3) 0.0364(19) 0.0295(17) -0.0088(14) -0.0235(18) 0.0165(18) C53 0.048(2) 0.0269(15) 0.0219(14) -0.0074(12) -0.0110(13) 0.0031(14) C83 0.0354(17) 0.0233(13) 0.0224(13) -0.0007(11) -0.0008(12) -0.0084(12) C93 0.046(2) 0.0380(18) 0.0236(15) -0.0110(13) -0.0005(14) -0.0020(15) O14 0.0322(12) 0.0290(11) 0.0242(10) -0.0074(8) -0.0015(9) -0.0076(9) C14 0.0227(13) 0.0217(12) 0.0255(13) -0.0137(10) 0.0003(11) 0.0030(10) C24 0.0252(15) 0.0357(16) 0.0233(14) -0.0119(12) -0.0007(11) 0.0036(12) C74 0.0219(15) 0.055(2) 0.0323(17) -0.0132(16) -0.0026(13) 0.0026(15) C64 0.0270(18) 0.081(3) 0.041(2) -0.017(2) -0.0076(16) 0.0003(19) C54 0.034(2) 0.090(4) 0.0303(19) -0.013(2) -0.0080(15) 0.015(2) C44 0.038(2) 0.066(3) 0.0234(16) -0.0064(16) 0.0004(14) 0.0076(18) C34 0.0277(16) 0.0440(19) 0.0235(14) -0.0088(13) 0.0026(12) 0.0029(14) O24 0.0324(12) 0.0269(10) 0.0248(10) -0.0071(8) -0.0020(9) -0.0061(9) O72 0.0290(10) 0.0163(8) 0.0144(8) -0.0039(7) 0.0023(7) -0.0018(7) C72 0.0222(13) 0.0174(11) 0.0198(12) -0.0065(9) 0.0004(10) -0.0003(10) C62 0.0254(14) 0.0253(13) 0.0196(12) -0.0086(10) 0.0000(10) -0.0019(11) C12 0.0253(14) 0.0288(14) 0.0186(13) -0.0072(11) 0.0003(10) 0.0007(11) O12 0.0283(11) 0.0247(10) 0.0189(9) -0.0049(8) 0.0037(8) -0.0058(8) C22 0.0343(17) 0.0386(17) 0.0195(13) -0.0053(12) 0.0012(12) -0.0040(14) C32 0.048(2) 0.059(2) 0.0215(15) -0.0178(15) 0.0025(14) -0.0099(18) C42 0.053(2) 0.053(2) 0.0309(17) -0.0234(17) 0.0063(16) -0.0175(19) C52 0.0398(19) 0.0382(18) 0.0316(16) -0.0180(14) 0.0047(14) -0.0108(15) C82 0.0296(15) 0.0188(12) 0.0257(13) -0.0090(10) 0.0028(11) -0.0052(11) C92 0.0325(17) 0.0241(14) 0.0399(18) -0.0086(13) -0.0038(14) -0.0003(12) O18 0.0354(12) 0.0177(9) 0.0234(10) -0.0038(7) 0.0009(8) -0.0112(8) O25 0.0264(11) 0.0251(10) 0.0252(10) -0.0074(8) -0.0018(8) -0.0063(8) C15 0.0275(14) 0.0160(11) 0.0257(13) 0.0008(10) -0.0020(11) -0.0090(10) O15 0.0278(11) 0.0245(10) 0.0242(10) -0.0047(8) -0.0033(8) -0.0035(8) C25 0.0290(15) 0.0246(13) 0.0221(13) 0.0041(11) -0.0051(11) -0.0088(11) C35 0.0429(19) 0.0265(14) 0.0231(14) -0.0001(11) -0.0056(13) -0.0121(13) C45 0.056(2) 0.048(2) 0.0217(15) 0.0017(14) -0.0080(15) -0.0225(18) C55 0.054(2) 0.067(3) 0.0278(17) 0.0096(17) -0.0158(17) -0.027(2) C65 0.032(2) 0.083(3) 0.037(2) 0.007(2) -0.0135(16) -0.006(2) C75 0.0345(19) 0.053(2) 0.0301(17) -0.0002(15) -0.0030(14) -0.0068(16) O17 0.0300(11) 0.0198(9) 0.0256(10) -0.0084(8) -0.0064(8) -0.0008(8) O26 0.0242(10) 0.0223(9) 0.0202(9) -0.0061(7) 0.0007(8) 0.0011(8) C26 0.0285(15) 0.0247(13) 0.0245(14) -0.0030(11) -0.0040(11) 0.0030(11) C16 0.0250(15) 0.0387(17) 0.0258(15) -0.0071(13) -0.0020(12) 0.0046(13) N16 0.0250(14) 0.0449(17) 0.0287(14) 0.0047(12) -0.0004(11) 0.0028(12) C56 0.0338(19) 0.0362(18) 0.048(2) -0.0006(16) -0.0088(16) -0.0028(15) C66 0.0319(18) 0.046(2) 0.041(2) -0.0032(16) -0.0087(15) -0.0011(16) O66 0.0354(14) 0.0356(13) 0.0430(15) -0.0024(11) -0.0132(11) 0.0044(11) C36 0.0278(19) 0.102(4) 0.0310(19) 0.009(2) 0.0042(15) -0.002(2) C46 0.033(2) 0.138(6) 0.029(2) 0.006(3) 0.0065(17) -0.008(3) O46 0.0352(16) 0.089(3) 0.059(2) 0.0267(19) -0.0030(14) -0.0115(17) N72 0.0251(12) 0.0157(10) 0.0165(10) -0.0047(8) 0.0004(8) -0.0021(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4525(5) 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 Mn3 . Mn2 . 3.2546(6) yes Mn3 . O123 . 1.8762(19) yes Mn3 . O11 . 1.894(2) yes Mn3 . N71 . 1.996(2) yes Mn3 . O14 . 2.189(2) yes Mn3 . O72 . 1.9388(19) yes Mn3 . O18 . 2.282(2) yes Mn2 . Mn1 . 3.1662(6) yes Mn2 . O123 . 1.871(2) yes Mn2 . O73 . 1.941(2) yes Mn2 . O12 . 1.878(2) yes Mn2 . O15 . 2.180(2) yes Mn2 . O26 . 2.274(2) yes Mn2 . N72 . 2.009(2) yes Mn1 . O123 . 1.8794(19) yes Mn1 . O71 . 1.917(2) yes Mn1 . N73 . 2.003(2) yes Mn1 . O13 . 1.8702(19) yes Mn1 . O25 . 2.288(2) yes Mn1 . O17 . 2.271(2) yes O11 . C11 . 1.335(3) yes C11 . C21 . 1.404(4) yes C11 . C61 . 1.425(4) yes C21 . C31 . 1.379(4) yes C21 . H211 . 0.950 no C31 . C41 . 1.392(5) yes C31 . H311 . 0.950 no C41 . C51 . 1.379(5) yes C41 . H411 . 0.950 no C51 . C61 . 1.396(4) yes C51 . H511 . 0.950 no C61 . C71 . 1.475(4) yes C71 . N71 . 1.297(4) yes C71 . C81 . 1.506(4) yes N71 . O71 . 1.381(3) yes C81 . C91 . 1.508(5) yes C81 . H811 . 0.990 no C81 . H812 . 0.990 no C91 . H911 . 0.980 no C91 . H912 . 0.980 no C91 . H913 . 0.981 no N73 . O73 . 1.378(3) yes N73 . C73 . 1.295(3) yes C73 . C63 . 1.465(4) yes C73 . C83 . 1.502(4) yes C63 . C13 . 1.418(4) yes C63 . C53 . 1.405(4) yes C13 . O13 . 1.340(3) yes C13 . C23 . 1.397(4) yes C23 . C33 . 1.384(5) yes C23 . H231 . 0.951 no C33 . C43 . 1.375(6) yes C33 . H331 . 0.950 no C43 . C53 . 1.380(5) yes C43 . H431 . 0.950 no C53 . H531 . 0.950 no C83 . C93 . 1.526(5) yes C83 . H831 . 0.990 no C83 . H832 . 0.990 no C93 . H931 . 0.980 no C93 . H932 . 0.980 no C93 . H933 . 0.980 no O14 . C14 . 1.246(4) yes C14 . C24 . 1.509(4) yes C14 . O24 . 1.265(4) yes C24 . C74 . 1.389(5) yes C24 . C34 . 1.385(5) yes C74 . C64 . 1.395(5) yes C74 . H741 . 0.951 no C64 . C54 . 1.374(7) yes C64 . H641 . 0.949 no C54 . C44 . 1.373(7) yes C54 . H541 . 0.950 no C44 . C34 . 1.393(5) yes C44 . H441 . 0.950 no C34 . H341 . 0.950 no O72 . N72 . 1.381(3) yes C72 . C62 . 1.477(4) yes C72 . C82 . 1.505(4) yes C72 . N72 . 1.297(3) yes C62 . C12 . 1.398(4) yes C62 . C52 . 1.411(4) yes C12 . O12 . 1.342(4) yes C12 . C22 . 1.404(4) yes C22 . C32 . 1.382(5) yes C22 . H221 . 0.950 no C32 . C42 . 1.384(6) yes C32 . H321 . 0.950 no C42 . C52 . 1.372(5) yes C42 . H421 . 0.950 no C52 . H521 . 0.950 no C82 . C92 . 1.533(4) yes C82 . H821 . 0.990 no C82 . H822 . 0.990 no C92 . H921 . 0.980 no C92 . H922 . 0.980 no C92 . H923 . 0.980 no O18 . H19 . 0.900 no O18 . H20 . 0.900 no O25 . C15 . 1.269(4) yes C15 . O15 . 1.254(4) yes C15 . C25 . 1.508(4) yes C25 . C35 . 1.389(5) yes C25 . C75 . 1.386(5) yes C35 . C45 . 1.392(5) yes C35 . H351 . 0.951 no C45 . C55 . 1.375(7) yes C45 . H451 . 0.950 no C55 . C65 . 1.373(7) yes C55 . H551 . 0.950 no C65 . C75 . 1.393(6) yes C65 . H651 . 0.950 no C75 . H751 . 0.950 no O17 . H17 . 0.900 no O17 . H18 . 0.900 no O26 . C26 . 1.426(3) yes O26 . H26 . 0.840 no C26 . C16 . 1.502(5) yes C26 . H261 . 0.990 no C26 . H262 . 0.990 no C16 . N16 . 1.496(5) yes C16 . H161 . 0.990 no C16 . H162 . 0.990 no N16 . C56 . 1.505(5) yes N16 . C36 . 1.501(5) yes N16 . H16 . 0.910 no C56 . C66 . 1.515(5) yes C56 . H561 . 0.990 no C56 . H562 . 0.990 no C66 . O66 . 1.406(5) yes C66 . H661 . 0.990 no C66 . H662 . 0.990 no O66 . H66 . 0.840 no C36 . C46 . 1.517(7) yes C36 . H361 . 0.990 no C36 . H362 . 0.990 no C46 . O46 . 1.414(6) yes C46 . H461 . 0.990 no C46 . H462 . 0.990 no O46 . H46 . 0.840 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 Mn2 . Mn3 . O123 . 29.66(6) yes Mn2 . Mn3 . O11 . 155.15(6) yes O123 . Mn3 . O11 . 174.77(9) yes Mn2 . Mn3 . N71 . 116.58(7) yes O123 . Mn3 . N71 . 87.19(9) yes O11 . Mn3 . N71 . 87.72(9) yes Mn2 . Mn3 . O14 . 98.33(6) yes O123 . Mn3 . O14 . 95.93(9) yes O11 . Mn3 . O14 . 85.43(9) yes N71 . Mn3 . O14 . 91.36(9) yes Mn2 . Mn3 . O72 . 61.19(6) yes O123 . Mn3 . O72 . 90.62(8) yes O11 . Mn3 . O72 . 94.44(8) yes N71 . Mn3 . O72 . 177.70(9) yes O14 . Mn3 . O72 . 89.57(9) yes Mn2 . Mn3 . O18 . 86.22(6) yes O123 . Mn3 . O18 . 89.78(8) yes O11 . Mn3 . O18 . 88.97(8) yes N71 . Mn3 . O18 . 89.74(9) yes O14 . Mn3 . O18 . 174.24(8) yes O72 . Mn3 . O18 . 89.54(8) yes Mn3 . Mn2 . Mn1 . 60.756(13) yes Mn3 . Mn2 . O123 . 29.75(6) yes Mn1 . Mn2 . O123 . 32.49(6) yes Mn3 . Mn2 . O73 . 117.82(6) yes Mn1 . Mn2 . O73 . 62.84(6) yes O123 . Mn2 . O73 . 88.71(9) yes Mn3 . Mn2 . O12 . 147.45(7) yes Mn1 . Mn2 . O12 . 151.15(7) yes O123 . Mn2 . O12 . 175.93(9) yes O73 . Mn2 . O12 . 93.28(9) yes Mn3 . Mn2 . O15 . 99.83(6) yes Mn1 . Mn2 . O15 . 76.71(6) yes O123 . Mn2 . O15 . 95.12(9) yes O73 . Mn2 . O15 . 90.78(9) yes O12 . Mn2 . O15 . 88.41(9) yes Mn3 . Mn2 . O26 . 88.10(5) yes Mn1 . Mn2 . O26 . 104.89(5) yes O123 . Mn2 . O26 . 90.24(8) yes O73 . Mn2 . O26 . 82.72(8) yes O12 . Mn2 . O26 . 86.49(9) yes Mn3 . Mn2 . N72 . 59.47(7) yes Mn1 . Mn2 . N72 . 116.58(7) yes O123 . Mn2 . N72 . 88.99(9) yes O73 . Mn2 . N72 . 174.67(9) yes O12 . Mn2 . N72 . 88.72(9) yes O15 . Mn2 . O26 . 171.49(8) yes O15 . Mn2 . N72 . 94.22(9) yes O26 . Mn2 . N72 . 92.48(9) yes Mn2 . Mn1 . O123 . 32.33(6) yes Mn2 . Mn1 . O71 . 121.75(6) yes O123 . Mn1 . O71 . 91.61(8) yes Mn2 . Mn1 . N73 . 58.67(7) yes O123 . Mn1 . N73 . 89.35(9) yes O71 . Mn1 . N73 . 177.24(10) yes Mn2 . Mn1 . O13 . 146.01(7) yes O123 . Mn1 . O13 . 177.44(9) yes O71 . Mn1 . O13 . 90.59(9) yes N73 . Mn1 . O13 . 88.52(9) yes Mn2 . Mn1 . O25 . 77.62(6) yes O123 . Mn1 . O25 . 89.20(8) yes O71 . Mn1 . O25 . 92.36(9) yes N73 . Mn1 . O25 . 85.06(9) yes O13 . Mn1 . O25 . 92.03(8) yes Mn2 . Mn1 . O17 . 95.93(6) yes O123 . Mn1 . O17 . 85.61(8) yes O71 . Mn1 . O17 . 91.67(9) yes N73 . Mn1 . O17 . 90.99(9) yes O13 . Mn1 . O17 . 93.01(8) yes O25 . Mn1 . O17 . 173.51(8) yes Mn1 . O123 . Mn3 . 119.72(11) yes Mn1 . O123 . Mn2 . 115.18(10) yes Mn3 . O123 . Mn2 . 120.59(10) yes Mn3 . O11 . C11 . 120.63(18) yes O11 . C11 . C21 . 118.0(3) yes O11 . C11 . C61 . 123.5(3) yes C21 . C11 . C61 . 118.4(3) yes C11 . C21 . C31 . 121.3(3) yes C11 . C21 . H211 . 119.4 no C31 . C21 . H211 . 119.4 no C21 . C31 . C41 . 120.6(3) yes C21 . C31 . H311 . 119.7 no C41 . C31 . H311 . 119.7 no C31 . C41 . C51 . 118.8(3) yes C31 . C41 . H411 . 120.6 no C51 . C41 . H411 . 120.6 no C41 . C51 . C61 . 122.5(3) yes C41 . C51 . H511 . 118.7 no C61 . C51 . H511 . 118.8 no C11 . C61 . C51 . 118.3(3) yes C11 . C61 . C71 . 122.1(3) yes C51 . C61 . C71 . 119.4(3) yes C61 . C71 . N71 . 119.0(2) yes C61 . C71 . C81 . 120.9(2) yes N71 . C71 . C81 . 120.0(3) yes Mn3 . N71 . C71 . 126.7(2) yes Mn3 . N71 . O71 . 115.85(16) yes C71 . N71 . O71 . 117.5(2) yes N71 . O71 . Mn1 . 114.46(16) yes C71 . C81 . C91 . 114.5(3) yes C71 . C81 . H811 . 108.2 no C91 . C81 . H811 . 108.2 no C71 . C81 . H812 . 108.2 no C91 . C81 . H812 . 108.2 no H811 . C81 . H812 . 109.5 no C81 . C91 . H911 . 109.5 no C81 . C91 . H912 . 109.5 no H911 . C91 . H912 . 109.5 no C81 . C91 . H913 . 109.4 no H911 . C91 . H913 . 109.4 no H912 . C91 . H913 . 109.4 no Mn1 . N73 . O73 . 114.27(16) yes Mn1 . N73 . C73 . 129.5(2) yes O73 . N73 . C73 . 116.2(2) yes N73 . O73 . Mn2 . 109.40(16) yes N73 . C73 . C63 . 119.0(3) yes N73 . C73 . C83 . 119.8(3) yes C63 . C73 . C83 . 121.2(2) yes C73 . C63 . C13 . 123.4(2) yes C73 . C63 . C53 . 118.5(3) yes C13 . C63 . C53 . 118.1(3) yes C63 . C13 . O13 . 122.9(3) yes C63 . C13 . C23 . 119.2(3) yes O13 . C13 . C23 . 117.9(3) yes C13 . O13 . Mn1 . 124.72(18) yes C13 . C23 . C33 . 120.8(3) yes C13 . C23 . H231 . 119.6 no C33 . C23 . H231 . 119.6 no C23 . C33 . C43 . 120.7(3) yes C23 . C33 . H331 . 119.6 no C43 . C33 . H331 . 119.6 no C33 . C43 . C53 . 119.4(3) yes C33 . C43 . H431 . 120.3 no C53 . C43 . H431 . 120.3 no C63 . C53 . C43 . 121.9(3) yes C63 . C53 . H531 . 119.0 no C43 . C53 . H531 . 119.0 no C73 . C83 . C93 . 111.7(3) yes C73 . C83 . H831 . 108.9 no C93 . C83 . H831 . 108.9 no C73 . C83 . H832 . 108.9 no C93 . C83 . H832 . 108.9 no H831 . C83 . H832 . 109.4 no C83 . C93 . H931 . 109.5 no C83 . C93 . H932 . 109.5 no H931 . C93 . H932 . 109.5 no C83 . C93 . H933 . 109.5 no H931 . C93 . H933 . 109.5 no H932 . C93 . H933 . 109.5 no Mn3 . O14 . C14 . 144.9(2) yes O14 . C14 . C24 . 116.3(3) yes O14 . C14 . O24 . 125.1(3) yes C24 . C14 . O24 . 118.6(3) yes C14 . C24 . C74 . 120.8(3) yes C14 . C24 . C34 . 119.0(3) yes C74 . C24 . C34 . 120.2(3) yes C24 . C74 . C64 . 119.2(4) yes C24 . C74 . H741 . 120.4 no C64 . C74 . H741 . 120.4 no C74 . C64 . C54 . 120.5(4) yes C74 . C64 . H641 . 119.7 no C54 . C64 . H641 . 119.7 no C64 . C54 . C44 . 120.1(4) yes C64 . C54 . H541 . 120.0 no C44 . C54 . H541 . 120.0 no C54 . C44 . C34 . 120.4(4) yes C54 . C44 . H441 . 119.8 no C34 . C44 . H441 . 119.8 no C44 . C34 . C24 . 119.5(4) yes C44 . C34 . H341 . 120.3 no C24 . C34 . H341 . 120.2 no Mn3 . O72 . N72 . 115.67(15) yes C62 . C72 . C82 . 120.7(2) yes C62 . C72 . N72 . 118.5(2) yes C82 . C72 . N72 . 120.8(2) yes C72 . C62 . C12 . 123.2(3) yes C72 . C62 . C52 . 119.2(3) yes C12 . C62 . C52 . 117.6(3) yes C62 . C12 . O12 . 122.9(3) yes C62 . C12 . C22 . 120.1(3) yes O12 . C12 . C22 . 117.0(3) yes C12 . O12 . Mn2 . 120.46(19) yes C12 . C22 . C32 . 120.5(3) yes C12 . C22 . H221 . 119.7 no C32 . C22 . H221 . 119.7 no C22 . C32 . C42 . 120.1(3) yes C22 . C32 . H321 . 119.9 no C42 . C32 . H321 . 119.9 no C32 . C42 . C52 . 119.6(3) yes C32 . C42 . H421 . 120.2 no C52 . C42 . H421 . 120.2 no C62 . C52 . C42 . 122.1(3) yes C62 . C52 . H521 . 118.9 no C42 . C52 . H521 . 118.9 no C72 . C82 . C92 . 112.0(3) yes C72 . C82 . H821 . 108.8 no C92 . C82 . H821 . 108.8 no C72 . C82 . H822 . 108.8 no C92 . C82 . H822 . 108.8 no H821 . C82 . H822 . 109.5 no C82 . C92 . H921 . 109.4 no C82 . C92 . H922 . 109.5 no H921 . C92 . H922 . 109.5 no C82 . C92 . H923 . 109.4 no H921 . C92 . H923 . 109.5 no H922 . C92 . H923 . 109.5 no Mn3 . O18 . H19 . 98.0 no Mn3 . O18 . H20 . 118.5 no H19 . O18 . H20 . 123.4 no Mn1 . O25 . C15 . 121.19(19) yes O25 . C15 . O15 . 125.5(3) yes O25 . C15 . C25 . 117.6(3) yes O15 . C15 . C25 . 116.9(3) yes Mn2 . O15 . C15 . 131.2(2) yes C15 . C25 . C35 . 120.1(3) yes C15 . C25 . C75 . 120.6(3) yes C35 . C25 . C75 . 119.3(3) yes C25 . C35 . C45 . 120.1(3) yes C25 . C35 . H351 . 120.0 no C45 . C35 . H351 . 120.0 no C35 . C45 . C55 . 120.1(4) yes C35 . C45 . H451 . 120.0 no C55 . C45 . H451 . 119.9 no C45 . C55 . C65 . 120.3(4) yes C45 . C55 . H551 . 119.8 no C65 . C55 . H551 . 119.8 no C55 . C65 . C75 . 120.1(4) yes C55 . C65 . H651 . 119.9 no C75 . C65 . H651 . 120.0 no C65 . C75 . C25 . 120.1(4) yes C65 . C75 . H751 . 119.9 no C25 . C75 . H751 . 120.0 no Mn1 . O17 . H17 . 127.4 no Mn1 . O17 . H18 . 114.6 no H17 . O17 . H18 . 102.0 no Mn2 . O26 . C26 . 132.29(19) yes Mn2 . O26 . H26 . 113.9 no C26 . O26 . H26 . 104.1 no O26 . C26 . C16 . 109.1(2) yes O26 . C26 . H261 . 109.6 no C16 . C26 . H261 . 109.6 no O26 . C26 . H262 . 109.5 no C16 . C26 . H262 . 109.6 no H261 . C26 . H262 . 109.5 no C26 . C16 . N16 . 112.6(3) yes C26 . C16 . H161 . 108.7 no N16 . C16 . H161 . 108.7 no C26 . C16 . H162 . 108.7 no N16 . C16 . H162 . 108.7 no H161 . C16 . H162 . 109.5 no C16 . N16 . C56 . 114.4(3) yes C16 . N16 . C36 . 111.8(4) yes C56 . N16 . C36 . 110.8(3) yes C16 . N16 . H16 . 106.4 no C56 . N16 . H16 . 106.4 no C36 . N16 . H16 . 106.4 no N16 . C56 . C66 . 115.3(3) yes N16 . C56 . H561 . 108.0 no C66 . C56 . H561 . 108.0 no N16 . C56 . H562 . 108.0 no C66 . C56 . H562 . 108.0 no H561 . C56 . H562 . 109.4 no C56 . C66 . O66 . 108.5(3) yes C56 . C66 . H661 . 109.7 no O66 . C66 . H661 . 109.7 no C56 . C66 . H662 . 109.7 no O66 . C66 . H662 . 109.7 no H661 . C66 . H662 . 109.5 no C66 . O66 . H66 . 107.1 no N16 . C36 . C46 . 112.5(4) yes N16 . C36 . H361 . 108.7 no C46 . C36 . H361 . 108.7 no N16 . C36 . H362 . 108.7 no C46 . C36 . H362 . 108.7 no H361 . C36 . H362 . 109.4 no C36 . C46 . O46 . 111.0(5) yes C36 . C46 . H461 . 109.1 no O46 . C46 . H461 . 109.1 no C36 . C46 . H462 . 109.1 no O46 . C46 . H462 . 109.1 no H461 . C46 . H462 . 109.5 no C46 . O46 . H46 . 98.5 no O72 . N72 . Mn2 . 114.81(16) yes O72 . N72 . C72 . 117.2(2) yes Mn2 . N72 . C72 . 127.8(2) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O66 . H66 . O72 2_655 180 0.84 1.88 2.720(2) yes O46 . H46 . O12 . 180 0.84 1.96 2.802(2) yes O26 . H26 . O24 . 180 0.84 1.80 2.639(2) yes O17 . H17 . O13 2_565 180 0.90 1.94 2.840(2) yes O17 . H18 . O24 . 180 0.90 1.98 2.877(2) yes O18 . H19 . O25 . 180 0.90 1.99 2.894(2) yes O18 . H20 . O11 2_555 180 0.90 1.95 2.855(2) yes # Attachment 'Complex 16.cif' data_EB8142 _database_code_depnum_ccdc_archive 'CCDC 736442' _audit_creation_date 08-08-06 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8142 in P-3c1' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H48 Cl1 Mn3 N6 O11' _chemical_compound_source 'Ross Inglis, RI1351' _exptl_crystal_recrystallization_method ; Diffusion of Et~2~O into THF solution. ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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 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 \%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 912_ALERT_3_B # Missing FCF Reflections Above STh/L= 0.600 129 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 1580 1580 0 23.01 0.550 1.000 2102 2102 0 25.24 0.600 1.000 2719 2719 0 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 1.000 3464 3464 0 28.78 0.678 0.967 3897 3768 129 301_ALERT_3_C Main Residue Disorder ......................... 19.00 Perc. The disordered 3-picoline has been modelled over two sets of atomic sites, each with the occupancy set to 0.5. In earlier stages of refinement, the occupancy of these atomic sites was refined and found to be very close to 0.5. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.98 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.15 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C26 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C23 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 18 The following restraints were applied: U(IJ)'S 0.0, 0.010000 = C(23) TO C(27) U(IJ)'S 0.0, 0.010000 = C(22) TO C(26) U(IJ)'S 0.0, 0.010000 = C(25) TO C(29) ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 13.3429(2) _cell_length_b 13.3429(2) _cell_length_c 29.0999(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 4486.65(16) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P -3 c 1 ' _symmetry_space_group_name_Hall '-P 3 2"c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y,x-y,z y,-x+y,-z -x+y,-x,z x-y,x,-z -x+y,y,z+1/2 x-y,-y,-z+1/2 x,x-y,z+1/2 -x,-x+y,-z+1/2 -y,-x,z+1/2 y,x,-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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 = C45 H48 Cl1.00 Mn3 N6 O11 # Dc = 1.55 Fooo = 2160.00 Mu = 9.59 M = 349.72 # Found Formula = C45 H48 Cl1 Mn3 N6 O11 # Dc = 1.55 FOOO = 2160.00 Mu = 9.59 M = 349.72 _chemical_formula_sum 'C45 H48 Cl1 Mn3 N6 O11' _chemical_formula_weight 1049.15 _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour black _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_max 0.44 _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.959 # Sheldrick geometric approximatio 0.70 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.87 _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 '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 52744 _reflns_number_total 3768 _diffrn_reflns_av_R_equivalents 0.045 # Number of reflections with Friedels Law is 3768 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3896 _diffrn_reflns_theta_min 1.400 _diffrn_reflns_theta_max 28.785 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.921 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _reflns_limit_h_min -15 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 38 _oxford_diffrn_Wilson_B_factor 1.38 _oxford_diffrn_Wilson_scale 16.37 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.52 _refine_diff_density_max 0.98 # 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 3768 _refine_ls_number_restraints 18 _refine_ls_number_parameters 244 _oxford_refine_ls_R_factor_ref 0.0575 _refine_ls_wR_factor_ref 0.1039 _refine_ls_goodness_of_fit_ref 0.9627 _refine_ls_shift/su_max 0.000807 # The values computed from all data _oxford_reflns_number_all 3768 _refine_ls_R_factor_all 0.0575 _refine_ls_wR_factor_all 0.1039 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3098 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_gt 0.0927 # 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 ; # 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.50558(3) 0.23311(3) 0.360651(12) 0.0196 1.0000 Uani . . . . . . . O2 O 0.6667 0.3333 0.35111(9) 0.0186 1.0000 Uani S T . . . . . O3 O 0.35108(16) 0.13213(16) 0.37512(6) 0.0245 1.0000 Uani . . . . . . . C4 C 0.3109(2) 0.0516(2) 0.40788(8) 0.0224 1.0000 Uani . . . . . . . C5 C 0.1974(2) 0.0118(2) 0.42261(9) 0.0286 1.0000 Uani . . . . . . . C6 C 0.1483(3) -0.0704(3) 0.45662(9) 0.0322 1.0000 Uani . . . . . . . C7 C 0.2115(3) -0.1149(3) 0.47698(9) 0.0332 1.0000 Uani . . . . . . . C8 C 0.3218(3) -0.0799(2) 0.46201(9) 0.0290 1.0000 Uani . . . . . . . C9 C 0.3748(2) 0.0031(2) 0.42673(8) 0.0218 1.0000 Uani . . . . . . . C10 C 0.4881(2) 0.0288(2) 0.40884(8) 0.0229 1.0000 Uani . . . . . . . N11 N 0.53839(18) 0.10825(19) 0.37736(7) 0.0208 1.0000 Uani . . . . . . . O12 O 0.63696(16) 0.11847(16) 0.35762(6) 0.0249 1.0000 Uani . . . . . . . C13 C 0.5445(3) -0.0392(2) 0.42378(9) 0.0284 1.0000 Uani . . . . . . . C14 C 0.5030(3) -0.1487(3) 0.39556(11) 0.0427 1.0000 Uani . . . . . . . Cl15 Cl 0.6667 0.3333 0.46286(3) 0.0216 1.0000 Uani S T . . . . . O16 O 0.54903(16) 0.28494(17) 0.44604(6) 0.0256 1.0000 Uani . . . . . . . O17 O 0.6667 0.3333 0.51193(10) 0.0333 1.0000 Uani S T . . . . . N18 N 0.4623(2) 0.1827(2) 0.28576(7) 0.0278 1.0000 Uani . . . . . . . C19 C 0.3937(5) 0.2000(6) 0.2616(2) 0.0275 0.5000 Uani . . . 1 1 . . C20 C 0.3648(6) 0.1705(6) 0.2157(2) 0.0326 0.5000 Uani . . . 1 1 . . C21 C 0.4115(3) 0.1218(3) 0.19431(10) 0.0470 1.0000 Uani . . . . . . . C22 C 0.4935(5) 0.0925(6) 0.2183(2) 0.0335 0.5000 Uani . U . 1 1 . . C23 C 0.5156(5) 0.1249(6) 0.26363(19) 0.0282 0.5000 Uani . U . 1 1 . . C24 C 0.3488(6) 0.1396(6) 0.2701(2) 0.0314 0.5000 Uani . . . 1 2 . . C25 C 0.3198(7) 0.1119(6) 0.2247(2) 0.0354 0.5000 Uani . U . 1 2 . . C26 C 0.5138(7) 0.1765(9) 0.2098(3) 0.0646 0.5000 Uani . U . 1 2 . . C27 C 0.5365(7) 0.2033(8) 0.2561(2) 0.0516 0.5000 Uani . U . 1 2 . . C28 C 0.2801(7) 0.1920(8) 0.1915(2) 0.0547 0.5000 Uani . . . 1 1 . . C29 C 0.1940(7) 0.0597(7) 0.2089(3) 0.0579 0.5000 Uani . U . 1 2 . . H51 H 0.1568 0.0430 0.4093 0.0327 1.0000 Uiso R . . . . . . H61 H 0.0735 -0.0955 0.4660 0.0351 1.0000 Uiso R . . . . . . H71 H 0.1798 -0.1685 0.5003 0.0362 1.0000 Uiso R . . . . . . H81 H 0.3626 -0.1124 0.4747 0.0330 1.0000 Uiso R . . . . . . H131 H 0.5259 -0.0619 0.4559 0.0335 1.0000 Uiso R . . . . . . H132 H 0.6265 0.0085 0.4199 0.0335 1.0000 Uiso R . . . . . . H143 H 0.5426 -0.1886 0.4056 0.0701 1.0000 Uiso R . . . . . . H141 H 0.4201 -0.1997 0.3994 0.0709 1.0000 Uiso R . . . . . . H142 H 0.5215 -0.1288 0.3641 0.0704 1.0000 Uiso R . . . . . . H191 H 0.3584 0.2360 0.2759 0.0317 0.5000 Uiso R . . 1 1 . . H221 H 0.5270 0.0551 0.2033 0.0399 0.5000 Uiso R . . 1 1 . . H231 H 0.5659 0.1095 0.2800 0.0347 0.5000 Uiso R . . 1 1 . . H241 H 0.2922 0.1298 0.2905 0.0399 0.5000 Uiso R . . 1 2 . . H261 H 0.5751 0.1975 0.1899 0.0871 0.5000 Uiso R . . 1 2 . . H271 H 0.6131 0.2394 0.2654 0.0651 0.5000 Uiso R . . 1 2 . . H281 H 0.2736 0.1695 0.1600 0.0880 0.5000 Uiso R . . 1 1 . . H282 H 0.3034 0.2717 0.1929 0.0881 0.5000 Uiso R . . 1 1 . . H283 H 0.2061 0.1475 0.2061 0.0878 0.5000 Uiso R . . 1 1 . . H293 H 0.1448 0.0428 0.2349 0.0998 0.5000 Uiso R . . 1 2 . . H292 H 0.1727 -0.0091 0.1918 0.1000 0.5000 Uiso R . . 1 2 . . H291 H 0.1884 0.1148 0.1898 0.0998 0.5000 Uiso R . . 1 2 . . H211 H 0.3965 0.1023 0.1629 0.0471 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 0.0198(2) 0.0202(2) 0.01763(17) 0.00010(14) 0.00012(14) 0.00929(16) O2 0.0183(9) 0.0183(9) 0.0190(13) 0.0000 0.0000 0.0092(5) O3 0.0206(9) 0.0283(10) 0.0219(8) 0.0043(7) 0.0019(7) 0.0103(8) C4 0.0253(13) 0.0209(12) 0.0158(10) -0.0043(9) -0.0015(9) 0.0076(11) C5 0.0260(14) 0.0284(14) 0.0273(13) -0.0018(11) 0.0009(11) 0.0104(12) C6 0.0275(14) 0.0325(16) 0.0273(13) -0.0045(11) 0.0053(11) 0.0079(12) C7 0.0360(16) 0.0286(15) 0.0251(13) 0.0042(11) 0.0090(12) 0.0086(13) C8 0.0389(16) 0.0249(14) 0.0201(12) 0.0027(10) 0.0010(11) 0.0137(13) C9 0.0246(13) 0.0180(12) 0.0177(11) -0.0035(9) -0.0016(9) 0.0068(10) C10 0.0260(13) 0.0215(13) 0.0195(11) -0.0052(9) -0.0061(10) 0.0104(11) N11 0.0196(10) 0.0216(11) 0.0208(9) -0.0038(8) -0.0010(8) 0.0099(9) O12 0.0218(9) 0.0219(9) 0.0302(9) -0.0038(7) 0.0020(7) 0.0103(8) C13 0.0317(15) 0.0289(14) 0.0244(12) 0.0030(11) -0.0020(11) 0.0150(12) C14 0.063(2) 0.0395(18) 0.0390(17) -0.0087(14) -0.0161(16) 0.0354(18) Cl15 0.0249(3) 0.0249(3) 0.0152(4) 0.0000 0.0000 0.01243(16) O16 0.0231(9) 0.0292(10) 0.0228(8) -0.0004(8) 0.0017(7) 0.0117(8) O17 0.0428(13) 0.0428(13) 0.0144(14) 0.0000 0.0000 0.0214(7) N18 0.0281(12) 0.0264(12) 0.0194(10) 0.0011(9) 0.0008(9) 0.0066(10) C19 0.023(3) 0.030(3) 0.026(3) -0.004(3) 0.001(2) 0.011(3) C20 0.038(4) 0.030(4) 0.025(3) 0.003(3) -0.007(3) 0.013(3) C21 0.052(2) 0.050(2) 0.0160(12) -0.0049(13) -0.0037(13) 0.0080(18) C22 0.029(3) 0.046(4) 0.029(3) -0.005(3) 0.002(2) 0.021(3) C23 0.028(3) 0.041(3) 0.022(2) -0.010(2) -0.006(2) 0.023(3) C24 0.030(4) 0.038(4) 0.030(3) -0.004(3) -0.002(3) 0.021(3) C25 0.054(4) 0.034(3) 0.031(3) -0.007(3) -0.015(3) 0.032(3) C26 0.049(4) 0.101(6) 0.030(3) -0.013(4) 0.007(3) 0.027(5) C27 0.037(4) 0.081(5) 0.033(3) -0.010(4) -0.005(3) 0.026(4) C28 0.061(5) 0.073(6) 0.044(4) -0.012(4) -0.017(4) 0.044(5) C29 0.058(4) 0.072(5) 0.049(4) -0.019(4) -0.027(3) 0.037(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2662(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 . O12 5_665 1.9165(19) yes Mn1 . O2 . 1.9002(6) yes Mn1 . O3 . 1.8615(18) yes Mn1 . N11 . 1.983(2) yes Mn1 . O16 . 2.5667(18) yes Mn1 . N18 . 2.269(2) yes O3 . C4 . 1.332(3) yes C4 . C5 . 1.398(4) yes C4 . C9 . 1.414(4) yes C5 . C6 . 1.376(4) yes C5 . H51 . 0.918 no C6 . C7 . 1.383(4) yes C6 . H61 . 0.921 no C7 . C8 . 1.373(4) yes C7 . H71 . 0.921 no C8 . C9 . 1.413(3) yes C8 . H81 . 0.926 no C9 . C10 . 1.468(4) yes C10 . N11 . 1.305(3) yes C10 . C13 . 1.504(4) yes N11 . O12 . 1.378(3) yes C13 . C14 . 1.518(4) yes C13 . H131 . 0.975 no C13 . H132 . 0.959 no C14 . H143 . 0.965 no C14 . H141 . 0.972 no C14 . H142 . 0.950 no Cl15 . O16 3_655 1.4514(18) yes Cl15 . O16 5_665 1.4514(18) yes Cl15 . O16 . 1.4514(18) yes Cl15 . O17 . 1.428(3) yes N18 . C19 . 1.264(7) yes N18 . C23 . 1.437(6) yes N18 . C24 . 1.399(7) yes N18 . C27 . 1.237(7) yes C19 . C20 . 1.391(8) yes C19 . H191 . 0.924 no C20 . C21 . 1.268(8) yes C20 . C28 . 1.476(9) yes C21 . C22 . 1.504(7) yes C21 . H211 . 0.944 no C21 . C25 . 1.461(8) yes C21 . C26 . 1.267(9) yes C21 . H211 . 0.944 no C22 . C23 . 1.374(8) yes C22 . H221 . 0.928 no C23 . H231 . 0.925 no C24 . C25 . 1.375(9) yes C24 . H241 . 0.917 no C25 . C29 . 1.531(10) yes C26 . C27 . 1.387(10) yes C26 . H261 . 0.924 no C27 . H271 . 0.926 no C28 . H281 . 0.955 no C28 . H282 . 0.947 no C28 . H283 . 0.960 no C29 . H293 . 0.953 no C29 . H292 . 0.954 no C29 . H291 . 0.955 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 O12 5_665 Mn1 . O2 . 89.94(6) yes O12 5_665 Mn1 . O3 . 92.25(8) yes O2 . Mn1 . O3 . 174.92(9) yes O12 5_665 Mn1 . N11 . 168.07(8) yes O2 . Mn1 . N11 . 88.85(7) yes O3 . Mn1 . N11 . 88.07(9) yes O12 5_665 Mn1 . O16 . 85.31(7) yes O2 . Mn1 . O16 . 85.88(9) yes O3 . Mn1 . O16 . 89.73(7) yes N11 . Mn1 . O16 . 82.76(7) yes O12 5_665 Mn1 . N18 . 95.23(8) yes O2 . Mn1 . N18 . 95.69(10) yes O3 . Mn1 . N18 . 88.68(8) yes N11 . Mn1 . N18 . 96.71(8) yes O16 . Mn1 . N18 . 178.33(7) yes Mn1 3_655 O2 . Mn1 . 117.90(4) yes Mn1 3_655 O2 . Mn1 5_665 117.90(4) yes Mn1 . O2 . Mn1 5_665 117.90(4) yes Mn1 . O3 . C4 . 126.79(17) yes O3 . C4 . C5 . 116.6(2) yes O3 . C4 . C9 . 123.8(2) yes C5 . C4 . C9 . 119.6(2) yes C4 . C5 . C6 . 121.1(3) yes C4 . C5 . H51 . 118.2 no C6 . C5 . H51 . 120.7 no C5 . C6 . C7 . 120.0(3) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 119.9 no C6 . C7 . C8 . 119.8(3) yes C6 . C7 . H71 . 120.5 no C8 . C7 . H71 . 119.7 no C7 . C8 . C9 . 121.9(3) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 118.4 no C4 . C9 . C8 . 117.4(2) yes C4 . C9 . C10 . 122.8(2) yes C8 . C9 . C10 . 119.6(2) yes C9 . C10 . N11 . 119.3(2) yes C9 . C10 . C13 . 121.6(2) yes N11 . C10 . C13 . 119.0(2) yes Mn1 . N11 . C10 . 127.95(18) yes Mn1 . N11 . O12 . 114.54(15) yes C10 . N11 . O12 . 116.8(2) yes N11 . O12 . Mn1 3_655 113.20(14) yes C10 . C13 . C14 . 111.9(2) yes C10 . C13 . H131 . 109.6 no C14 . C13 . H131 . 107.9 no C10 . C13 . H132 . 108.3 no C14 . C13 . H132 . 108.8 no H131 . C13 . H132 . 110.4 no C13 . C14 . H143 . 109.2 no C13 . C14 . H141 . 110.6 no H143 . C14 . H141 . 109.0 no C13 . C14 . H142 . 109.4 no H143 . C14 . H142 . 107.9 no H141 . C14 . H142 . 110.6 no O16 3_655 Cl15 . O16 5_665 109.24(8) yes O16 3_655 Cl15 . O16 . 109.24(8) yes O16 5_665 Cl15 . O16 . 109.24(8) yes O16 3_655 Cl15 . O17 . 109.70(8) yes O16 5_665 Cl15 . O17 . 109.70(8) yes O16 . Cl15 . O17 . 109.70(8) yes Mn1 . O16 . Cl15 . 119.64(10) yes Mn1 . N18 . C19 . 125.5(3) yes Mn1 . N18 . C23 . 117.9(3) yes C19 . N18 . C23 . 116.6(4) yes Mn1 . N18 . C24 . 119.8(3) yes Mn1 . N18 . C27 . 123.2(4) yes C24 . N18 . C27 . 116.5(5) yes N18 . C19 . C20 . 127.3(6) yes N18 . C19 . H191 . 116.7 no C20 . C19 . H191 . 116.0 no C19 . C20 . C21 . 118.6(6) yes C19 . C20 . C28 . 122.2(7) yes C21 . C20 . C28 . 119.1(6) yes C20 . C21 . C22 . 120.9(4) yes C20 . C21 . H211 . 121.7 no C22 . C21 . H211 . 117.4 no C25 . C21 . C26 . 116.7(5) yes C25 . C21 . H211 . 120.5 no C26 . C21 . H211 . 121.6 no C21 . C22 . C23 . 115.7(5) yes C21 . C22 . H221 . 122.0 no C23 . C22 . H221 . 122.3 no N18 . C23 . C22 . 120.9(5) yes N18 . C23 . H231 . 119.8 no C22 . C23 . H231 . 119.4 no N18 . C24 . C25 . 121.7(6) yes N18 . C24 . H241 . 119.5 no C25 . C24 . H241 . 118.8 no C21 . C25 . C24 . 116.5(6) yes C21 . C25 . C29 . 122.6(5) yes C24 . C25 . C29 . 120.5(7) yes C21 . C26 . C27 . 121.9(7) yes C21 . C26 . H261 . 119.0 no C27 . C26 . H261 . 119.1 no C26 . C27 . N18 . 124.9(7) yes C26 . C27 . H271 . 117.4 no N18 . C27 . H271 . 117.7 no C20 . C28 . H281 . 110.7 no C20 . C28 . H282 . 110.2 no H281 . C28 . H282 . 108.7 no C20 . C28 . H283 . 108.6 no H281 . C28 . H283 . 109.0 no H282 . C28 . H283 . 109.6 no C25 . C29 . H293 . 109.8 no C25 . C29 . H292 . 109.0 no H293 . C29 . H292 . 110.5 no C25 . C29 . H291 . 108.3 no H293 . C29 . H291 . 109.6 no H292 . C29 . H291 . 109.6 no # Attachment 'Complex 17.cif' data_EB8143 _database_code_depnum_ccdc_archive 'CCDC 736443' _audit_creation_date 08-08-12 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'Eb8143 in R-3' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety ; C48 H54 Cl1 Mn3 N6 O11, 0.5(C H4 O), 0.5(C4 H10 O) ; _chemical_compound_source 'Ross Inglis, RI1404' _exptl_crystal_recrystallization_method ; Diffusion of Et~2~O into MeOH solution. ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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 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\%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_B Structure Contains Solvent Accessible VOIDS of . 163.00 A**3 The solvent region was treated by the van der Sluis and Spek method, accounting for 185 e/cell. This corresponds to 3 molecules of MeOH and 3 molecules of Et~2~O. and F(000), M, mu, D and the formulae have been calculated on this assumption. 912_ALERT_3_B # Missing FCF Reflections Above STh/L= 0.600 236 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 1756 1756 0 23.01 0.550 1.000 2354 2354 0 25.24 0.600 1.000 3039 3039 0 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.999 3863 3859 4 29.42 0.691 0.949 4600 4364 236 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.83 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.50 Ratio 301_ALERT_3_C Main Residue Disorder ......................... 8.00 Perc. The disorder has been modelled with partial occupancy of atomic sites. The occupancies of the two sets of positions were initially refined, but as they were found to be close to 0.5 they were subsequently fixed at this value. Restraints were applied to these disordered groups of atoms. 366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C17 - C18 ... 1.38 Ang. 366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C18 - C19 ... 1.38 Ang. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10 No action taken. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 25 U(IJ)'S 0.0, 0.010000 = C(18) TO C(210) U(IJ)'S 0.0, 0.010000 = C(18) TO C(211) DISTANCE 1.500000 , 0.050000 = C(211) TO C(220) U(IJ)'S 0.0, 0.010000 = C(210) TO C(221) U(IJ)'S 0.0, 0.010000 = C(211) TO C(220) ; # 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 0.000 0.500 164.4 61.3 2 0.333 0.667 0.167 168.3 61.6 3 0.667 0.333 0.833 168.3 61.6 _platon_squeeze_details ; Each solvent void is assumed to contain one molecule of MeOH and one molecule of Et~2~O. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 13.3010(3) _cell_length_b 13.3010(3) _cell_length_c 49.1441(19) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 7529.6(4) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/3,y+2/3,z+2/3 -x+1/3,-y+2/3,-z+2/3 x+2/3,y+1/3,z+1/3 -x+2/3,-y+1/3,-z+1/3 -y,x-y,z y,-x+y,-z -y+1/3,x-y+2/3,z+2/3 y+1/3,-x+y+2/3,-z+2/3 -y+2/3,x-y+1/3,z+1/3 y+2/3,-x+y+1/3,-z+1/3 -x+y,-x,z x-y,x,-z -x+y+1/3,-x+2/3,z+2/3 x-y+1/3,x+2/3,-z+2/3 -x+y+2/3,-x+1/3,z+1/3 x-y+2/3,x+1/3,-z+1/3 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 6 # Given Formula = C50.50 H61 Cl1.00 Mn3 N6 O12 # Dc = 1.51 Fooo = 3384.00 Mu = 8.66 M = 381.44 # Found Formula = C48 H54 Cl1 Mn3 N6 O11.00 # Dc = 1.44 FOOO = 3384.00 Mu = 8.61 M = 363.74 _chemical_formula_sum 'C50.5 H61 Cl1 Mn3 N6 O12' _chemical_formula_weight 1144.32 _cell_measurement_reflns_used 9881 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_min 0.23 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.49 _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 0.866 # Sheldrick geometric approximatio 0.79 0.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.82 _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 '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 52463 _reflns_number_total 4364 _diffrn_reflns_av_R_equivalents 0.034 # Number of reflections with Friedels Law is 4364 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4627 _diffrn_reflns_theta_min 1.243 _diffrn_reflns_theta_max 29.419 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.948 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 66 _reflns_limit_h_min -17 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 66 _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 -0.40 _refine_diff_density_max 0.52 # 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 4347 _refine_ls_number_restraints 25 _refine_ls_number_parameters 226 _oxford_refine_ls_R_factor_ref 0.0485 _refine_ls_wR_factor_ref 0.1056 _refine_ls_goodness_of_fit_ref 0.8834 _refine_ls_shift/su_max 0.002428 # The values computed from all data _oxford_reflns_number_all 4347 _refine_ls_R_factor_all 0.0485 _refine_ls_wR_factor_all 0.1056 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3343 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_gt 0.0909 # 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, 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: 6.38 9.43 4.45 1.11 ; # 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. 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.60653(2) 0.43416(2) 0.584303(6) 0.0180 1.0000 Uani . . . . . . . O2 O 0.85287(12) 0.54808(12) 0.58169(3) 0.0224 1.0000 Uani . . . . . . . N3 N 0.76555(14) 0.55882(14) 0.59392(3) 0.0194 1.0000 Uani . . . . . . . C4 C 0.79655(17) 0.64031(16) 0.61212(4) 0.0212 1.0000 Uani . . . . . . . C5 C 0.92244(18) 0.71013(18) 0.62000(4) 0.0271 1.0000 Uani . . . . . . . C6 C 0.9854(2) 0.8181(2) 0.60211(6) 0.0373 1.0000 Uani . . . . . . . C7 C 0.70975(17) 0.66652(16) 0.62317(4) 0.0217 1.0000 Uani . . . . . . . C8 C 0.59580(18) 0.61714(16) 0.61220(4) 0.0214 1.0000 Uani . . . . . . . O9 O 0.55553(13) 0.53759(13) 0.59262(3) 0.0243 1.0000 Uani . . . . . . . C10 C 0.52155(19) 0.65586(19) 0.62169(4) 0.0264 1.0000 Uani . . . . . . . C11 C 0.5564(2) 0.7389(2) 0.64175(5) 0.0306 1.0000 Uani . . . . . . . C12 C 0.6654(2) 0.7844(2) 0.65349(5) 0.0330 1.0000 Uani . . . . . . . C13 C 0.7408(2) 0.74922(18) 0.64414(4) 0.0278 1.0000 Uani . . . . . . . O14 O 0.6667 0.3333 0.57870(5) 0.0180 1.0000 Uani S T . . . . . N15 N 0.62524(16) 0.49231(16) 0.54012(3) 0.0241 1.0000 Uani . . . . . . . C16 C 0.5764(2) 0.41837(19) 0.51931(4) 0.0269 1.0000 Uani . . . . . . . C17 C 0.5988(2) 0.4539(2) 0.49246(5) 0.0347 1.0000 Uani . . . . . . . C18 C 0.6736(3) 0.5687(2) 0.48602(5) 0.0384 1.0000 Uani . U . . . . . C19 C 0.7228(2) 0.6445(2) 0.50756(5) 0.0404 1.0000 Uani . . . . . . . C20 C 0.6970(2) 0.6040(2) 0.53402(5) 0.0334 1.0000 Uani . . . . . . . Cl23 Cl 0.6667 0.3333 0.644399(15) 0.0204 1.0000 Uani S T . . . . . O24 O 0.59811(13) 0.38292(13) 0.63439(3) 0.0239 1.0000 Uani . . . . . . . O25 O 0.6667 0.3333 0.67343(5) 0.0313 1.0000 Uani S T . . . . . C210 C 0.6820(9) 0.5977(11) 0.4557(3) 0.0451 0.5000 Uani . U . 1 1 . . C211 C 0.7173(9) 0.6242(10) 0.4584(3) 0.0434 0.5000 Uani D U . 1 2 . . C220 C 0.7105(8) 0.5400(7) 0.43710(15) 0.0503 0.5000 Uani D U . 1 2 . . C221 C 0.7685(8) 0.5779(9) 0.44173(17) 0.0598 0.5000 Uani . U . 1 1 . . H51 H 0.9275 0.7301 0.6387 0.0346 1.0000 Uiso R . . . . . . H52 H 0.9573 0.6606 0.6178 0.0340 1.0000 Uiso R . . . . . . H63 H 1.0676 0.8567 0.6063 0.0568 1.0000 Uiso R . . . . . . H62 H 0.9587 0.8747 0.6065 0.0568 1.0000 Uiso R . . . . . . H61 H 0.9733 0.7970 0.5836 0.0571 1.0000 Uiso R . . . . . . H101 H 0.4475 0.6268 0.6132 0.0298 1.0000 Uiso R . . . . . . H111 H 0.5069 0.7650 0.6480 0.0332 1.0000 Uiso R . . . . . . H121 H 0.6854 0.8375 0.6680 0.0369 1.0000 Uiso R . . . . . . H131 H 0.8155 0.7810 0.6521 0.0314 1.0000 Uiso R . . . . . . H161 H 0.5207 0.3369 0.5236 0.0362 1.0000 Uiso R . . . . . . H171 H 0.5589 0.3936 0.4790 0.0472 1.0000 Uiso R . . . . . . H191 H 0.7736 0.7211 0.5045 0.0473 1.0000 Uiso R . . . . . . H201 H 0.7330 0.6583 0.5484 0.0385 1.0000 Uiso R . . . . . . H2101 H 0.7004 0.6770 0.4540 0.0641 0.5000 Uiso R . . 1 1 . . H2102 H 0.6073 0.5477 0.4467 0.0643 0.5000 Uiso R . . 1 1 . . H2111 H 0.7945 0.6931 0.4597 0.0588 0.5000 Uiso R . . 1 2 . . H2112 H 0.6633 0.6568 0.4513 0.0591 0.5000 Uiso R . . 1 2 . . H2203 H 0.7534 0.5776 0.4205 0.0718 0.5000 Uiso R . . 1 2 . . H2202 H 0.7592 0.5062 0.4451 0.0724 0.5000 Uiso R . . 1 2 . . H2201 H 0.6409 0.4789 0.4331 0.0722 0.5000 Uiso R . . 1 2 . . H2211 H 0.7986 0.6211 0.4251 0.1041 0.5000 Uiso R . . 1 1 . . H2212 H 0.8437 0.6140 0.4545 0.1039 0.5000 Uiso R . . 1 1 . . H2213 H 0.7497 0.5001 0.4390 0.1043 0.5000 Uiso R . . 1 1 . . 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 0.01804(14) 0.01771(14) 0.01894(14) -0.00065(10) -0.00065(10) 0.00946(11) O2 0.0215(7) 0.0203(6) 0.0259(7) 0.0021(5) 0.0039(5) 0.0107(5) N3 0.0192(7) 0.0186(7) 0.0209(7) 0.0031(6) 0.0018(6) 0.0098(6) C4 0.0240(9) 0.0186(8) 0.0201(8) 0.0017(7) -0.0011(7) 0.0100(7) C5 0.0247(9) 0.0256(10) 0.0293(10) -0.0069(8) -0.0066(8) 0.0113(8) C6 0.0284(11) 0.0271(11) 0.0473(14) -0.0019(10) 0.0035(10) 0.0070(9) C7 0.0258(9) 0.0173(8) 0.0203(8) 0.0019(7) 0.0016(7) 0.0095(7) C8 0.0278(9) 0.0189(8) 0.0192(8) 0.0020(7) 0.0001(7) 0.0131(7) O9 0.0255(7) 0.0253(7) 0.0270(7) -0.0056(6) -0.0055(5) 0.0164(6) C10 0.0327(11) 0.0271(10) 0.0249(10) 0.0035(8) 0.0038(8) 0.0191(9) C11 0.0402(12) 0.0297(10) 0.0280(10) 0.0015(8) 0.0082(9) 0.0221(9) C12 0.0431(13) 0.0286(10) 0.0266(10) -0.0054(8) 0.0039(9) 0.0174(10) C13 0.0316(10) 0.0250(9) 0.0243(9) -0.0030(8) -0.0002(8) 0.0122(8) O14 0.0180(6) 0.0180(6) 0.0179(10) 0.0000 0.0000 0.0090(3) N15 0.0284(8) 0.0261(8) 0.0206(8) 0.0018(6) 0.0005(6) 0.0156(7) C16 0.0308(10) 0.0287(10) 0.0251(10) -0.0019(8) -0.0021(8) 0.0177(9) C17 0.0500(14) 0.0437(13) 0.0232(10) -0.0014(9) -0.0019(9) 0.0330(12) C18 0.0568(15) 0.0522(14) 0.0237(10) 0.0119(10) 0.0088(10) 0.0404(13) C19 0.0478(14) 0.0346(12) 0.0372(13) 0.0148(10) 0.0093(11) 0.0193(11) C20 0.0403(12) 0.0279(11) 0.0278(11) 0.0051(8) -0.0005(9) 0.0139(10) Cl23 0.0219(2) 0.0219(2) 0.0174(3) 0.0000 0.0000 0.01095(11) O24 0.0253(7) 0.0258(7) 0.0238(7) 0.0007(5) 0.0009(5) 0.0152(6) O25 0.0391(9) 0.0391(9) 0.0159(11) 0.0000 0.0000 0.0195(5) C210 0.062(5) 0.068(6) 0.026(3) 0.016(4) 0.007(4) 0.048(4) C211 0.060(5) 0.047(4) 0.023(3) 0.011(3) 0.008(4) 0.027(3) C220 0.069(5) 0.056(4) 0.025(3) 0.005(2) 0.010(3) 0.030(4) C221 0.080(5) 0.089(6) 0.037(4) 0.023(4) 0.024(4) 0.062(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.054700(10) 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 . O2 7_655 1.9151(14) yes Mn1 . Mn1 13_665 3.2455(5) yes Mn1 . N3 . 1.9848(16) yes Mn1 . O9 . 1.8583(14) yes Mn1 . O14 . 1.8940(4) yes Mn1 . N15 . 2.2763(17) yes Mn1 . O24 . 2.5414(15) yes O2 . N3 . 1.377(2) yes N3 . C4 . 1.303(2) yes C4 . C5 . 1.504(3) yes C4 . C7 . 1.467(3) yes C5 . C6 . 1.528(3) yes C5 . H51 . 0.951 no C5 . H52 . 0.982 no C6 . H63 . 0.969 no C6 . H62 . 1.002 no C6 . H61 . 0.944 no C7 . C8 . 1.423(3) yes C7 . C13 . 1.410(3) yes C8 . O9 . 1.329(2) yes C8 . C10 . 1.402(3) yes C10 . C11 . 1.376(3) yes C10 . H101 . 0.957 no C11 . C12 . 1.387(4) yes C11 . H111 . 0.937 no C12 . C13 . 1.380(3) yes C12 . H121 . 0.942 no C13 . H131 . 0.948 no N15 . C16 . 1.340(3) yes N15 . C20 . 1.338(3) yes C16 . C17 . 1.383(3) yes C16 . H161 . 0.982 no C17 . C18 . 1.380(4) yes C17 . H171 . 0.966 no C18 . C19 . 1.380(4) yes C18 . C210 . 1.529(13) yes C18 . C19 . 1.380(4) yes C18 . C211 . 1.514(13) yes C19 . C20 . 1.383(3) yes C19 . H191 . 0.910 no C20 . H201 . 0.949 no Cl23 . O24 7_655 1.4526(14) yes Cl23 . O24 13_665 1.4526(14) yes Cl23 . O24 . 1.4526(14) yes Cl23 . O25 . 1.427(3) yes C210 . C221 . 1.472(16) yes C210 . H2101 . 0.959 no C210 . H2102 . 0.984 no C211 . C220 . 1.503(16) yes C211 . H2111 . 0.979 no C211 . H2112 . 1.066 no C220 . H2203 . 0.978 no C220 . H2202 . 1.034 no C220 . H2201 . 0.896 no C221 . H2211 . 0.966 no C221 . H2212 . 1.071 no C221 . H2213 . 0.945 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 O2 7_655 Mn1 . Mn1 13_665 120.37(4) yes O2 7_655 Mn1 . N3 . 169.60(6) yes Mn1 13_665 Mn1 . N3 . 57.54(5) yes O2 7_655 Mn1 . O9 . 93.12(6) yes Mn1 13_665 Mn1 . O9 . 145.09(5) yes N3 . Mn1 . O9 . 87.71(7) yes O2 7_655 Mn1 . O14 . 89.89(4) yes Mn1 13_665 Mn1 . O14 . 31.040(16) yes N3 . Mn1 . O14 . 88.58(5) yes O9 . Mn1 . O14 . 174.86(7) yes O2 7_655 Mn1 . N15 . 97.31(6) yes Mn1 13_665 Mn1 . N15 . 95.88(4) yes N3 . Mn1 . N15 . 93.07(7) yes O9 . Mn1 . N15 . 88.66(6) yes O14 . Mn1 . N15 . 95.09(8) yes O2 7_655 Mn1 . O24 . 86.58(6) yes Mn1 13_665 Mn1 . O24 . 82.96(3) yes N3 . Mn1 . O24 . 83.05(6) yes O9 . Mn1 . O24 . 90.12(6) yes O14 . Mn1 . O24 . 85.91(7) yes N15 . Mn1 . O24 . 175.97(6) yes Mn1 13_665 O2 . N3 . 112.21(10) yes O2 . N3 . Mn1 . 114.28(11) yes O2 . N3 . C4 . 116.96(16) yes Mn1 . N3 . C4 . 128.33(14) yes N3 . C4 . C5 . 118.80(18) yes N3 . C4 . C7 . 119.50(17) yes C5 . C4 . C7 . 121.59(17) yes C4 . C5 . C6 . 110.50(18) yes C4 . C5 . H51 . 108.9 no C6 . C5 . H51 . 111.4 no C4 . C5 . H52 . 108.1 no C6 . C5 . H52 . 110.3 no H51 . C5 . H52 . 107.5 no C5 . C6 . H63 . 108.7 no C5 . C6 . H62 . 110.5 no H63 . C6 . H62 . 106.6 no C5 . C6 . H61 . 110.1 no H63 . C6 . H61 . 109.8 no H62 . C6 . H61 . 111.0 no C4 . C7 . C8 . 122.25(17) yes C4 . C7 . C13 . 119.84(18) yes C8 . C7 . C13 . 117.77(19) yes C7 . C8 . O9 . 123.66(17) yes C7 . C8 . C10 . 119.19(18) yes O9 . C8 . C10 . 117.13(18) yes C8 . O9 . Mn1 . 126.72(13) yes C8 . C10 . C11 . 121.1(2) yes C8 . C10 . H101 . 118.5 no C11 . C10 . H101 . 120.3 no C10 . C11 . C12 . 120.5(2) yes C10 . C11 . H111 . 121.1 no C12 . C11 . H111 . 118.4 no C11 . C12 . C13 . 119.4(2) yes C11 . C12 . H121 . 118.9 no C13 . C12 . H121 . 121.6 no C7 . C13 . C12 . 121.9(2) yes C7 . C13 . H131 . 118.8 no C12 . C13 . H131 . 119.2 no Mn1 13_665 O14 . Mn1 7_655 117.92(3) yes Mn1 13_665 O14 . Mn1 . 117.92(3) yes Mn1 7_655 O14 . Mn1 . 117.92(3) yes Mn1 . N15 . C16 . 123.23(14) yes Mn1 . N15 . C20 . 119.15(15) yes C16 . N15 . C20 . 117.30(19) yes N15 . C16 . C17 . 122.3(2) yes N15 . C16 . H161 . 117.8 no C17 . C16 . H161 . 119.8 no C16 . C17 . C18 . 120.6(2) yes C16 . C17 . H171 . 115.6 no C18 . C17 . H171 . 123.7 no C17 . C18 . C19 . 116.6(2) yes C17 . C18 . C210 . 115.1(5) yes C19 . C18 . C210 . 128.0(5) yes C17 . C18 . C19 . 116.6(2) yes C17 . C18 . C211 . 129.3(5) yes C19 . C18 . C211 . 113.9(4) yes C18 . C19 . C20 . 120.2(2) yes C18 . C19 . H191 . 120.5 no C20 . C19 . H191 . 119.3 no C19 . C20 . N15 . 122.9(2) yes C19 . C20 . H201 . 118.0 no N15 . C20 . H201 . 119.1 no O24 7_655 Cl23 . O24 13_665 109.14(6) yes O24 7_655 Cl23 . O24 . 109.14(6) yes O24 13_665 Cl23 . O24 . 109.14(6) yes O24 7_655 Cl23 . O25 . 109.80(6) yes O24 13_665 Cl23 . O25 . 109.80(6) yes O24 . Cl23 . O25 . 109.80(6) yes Mn1 . O24 . Cl23 . 119.76(8) yes C18 . C210 . C221 . 112.0(9) yes C18 . C210 . H2101 . 107.9 no C221 . C210 . H2101 . 111.3 no C18 . C210 . H2102 . 110.4 no C221 . C210 . H2102 . 106.5 no H2101 . C210 . H2102 . 108.7 no C18 . C211 . C220 . 113.3(9) yes C18 . C211 . H2111 . 111.6 no C220 . C211 . H2111 . 112.7 no C18 . C211 . H2112 . 108.6 no C220 . C211 . H2112 . 105.9 no H2111 . C211 . H2112 . 104.1 no C211 . C220 . H2203 . 113.5 no C211 . C220 . H2202 . 103.9 no H2203 . C220 . H2202 . 102.1 no C211 . C220 . H2201 . 118.5 no H2203 . C220 . H2201 . 110.9 no H2202 . C220 . H2201 . 106.0 no C210 . C221 . H2211 . 114.7 no C210 . C221 . H2212 . 106.4 no H2211 . C221 . H2212 . 102.5 no C210 . C221 . H2213 . 117.4 no H2211 . C221 . H2213 . 109.6 no H2212 . C221 . H2213 . 104.5 no # Attachment 'Complex 18.cif' data_eb8176 _database_code_depnum_ccdc_archive 'CCDC 736444' _audit_creation_date 08-11-17 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8176 in R3c' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H66 Cl1 Mn3 N6 O11' _chemical_compound_source 'Ross Inglis, RI1737' _exptl_crystal_recrystallization_method ; Slow evaporation of MeOH solution ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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: ; The absolute configuration was arbitrarily assigned. The Flack parameter is close to 0, but is not well-determined enough to establish the absoluted configuration. 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 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.45 Ratio 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.22 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.35 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.47 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C122 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C124 Differences occur in groups contained tBu, where large amounts of motion is often observed. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.84 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. 063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.69 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 24 The second part molecule was labelled to be the same as the first, with an offset of 100 in the serial number. 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 4 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 1942 1942 0 23.01 0.550 1.000 2591 2591 0 25.24 0.600 1.000 3356 3356 0 #----------------------------------------------------------- ACTA Min. Res. --- 26.43 0.626 0.999 3809 3805 4 033_ALERT_2_G Flack Parameter Value Deviates 2 * su from zero. 0.04 The absolute configuration cannot therefore be determined from the data. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 13 The following LS restraints were applied U(IJ)'S 0.0, 0.010000 = C(24) TO C(27) U(IJ)'S 0.0, 0.010000 = C(24) to C(25) ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 19.5188(15) _cell_length_b 19.5188(15) _cell_length_c 50.368(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 16619(2) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R 3 c ' _symmetry_space_group_name_Hall 'R 3 -2"c' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/3,y+2/3,z+2/3 x+2/3,y+1/3,z+1/3 -y,x-y,z -y+1/3,x-y+2/3,z+2/3 -y+2/3,x-y+1/3,z+1/3 -x+y,-x,z -x+y+1/3,-x+2/3,z+2/3 -x+y+2/3,-x+1/3,z+1/3 -x+y,y,z+1/2 -x+y+1/3,y+2/3,z+7/6 -x+y+2/3,y+1/3,z+5/6 x,x-y,z+1/2 x+1/3,x-y+2/3,z+7/6 x+2/3,x-y+1/3,z+5/6 -y,-x,z+1/2 -y+1/3,-x+2/3,z+7/6 -y+2/3,-x+1/3,z+5/6 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 12 # Given Formula = C54 H66 Cl1 Mn3 N6 O11.00 # Dc = 1.41 Fooo = 7344.00 Mu = 7.85 M = 783.59 # Found Formula = C54 H66 Cl1 Mn3 N6 O11 # Dc = 1.41 FOOO = 7344.00 Mu = 7.85 M = 783.59 _chemical_formula_sum 'C54 H66 Cl1 Mn3 N6 O11' _chemical_formula_weight 1175.39 _cell_measurement_reflns_used 9897 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.69 _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 7344 _exptl_absorpt_coefficient_mu 0.785 # Sheldrick geometric approximatio 0.88 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.88 _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 59229 _reflns_number_total 7571 _diffrn_reflns_av_R_equivalents 0.054 # Number of reflections with Friedels Law is 3805 # Number of reflections without Friedels Law is 7571 # Theoretical number of reflections is about 3799 _diffrn_reflns_theta_min 1.451 _diffrn_reflns_theta_max 26.428 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.428 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 62 _reflns_limit_h_min -21 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min -62 _reflns_limit_l_max 62 _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 -0.98 _refine_diff_density_max 1.30 # 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 7543 _refine_ls_number_restraints 13 _refine_ls_number_parameters 452 _oxford_refine_ls_R_factor_ref 0.0443 _refine_ls_wR_factor_ref 0.0825 _refine_ls_goodness_of_fit_ref 0.7379 _refine_ls_shift/su_max 0.000805 # The values computed from all data _oxford_reflns_number_all 7543 _refine_ls_R_factor_all 0.0443 _refine_ls_wR_factor_all 0.0825 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6730 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_gt 0.0789 _refine_ls_abs_structure_Flack 0.039(15) _refine_ls_abs_structure_details 'Flack (1983), 3766 Friedel-pairs' # 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 ad _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^) + ( 0.00P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. Flack, H. D. (1983). Acta Cryst. A39, 876-881. 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 0.96726(3) 0.89167(3) 0.09177(3) 0.0232 1.0000 Uani . . . . . . . O2 O 1.0000 1.0000 0.09756(8) 0.0242 1.0000 Uani S T . . . . . O3 O 0.93793(15) 0.78823(15) 0.08276(6) 0.0324 1.0000 Uani . . . . . . . C4 C 0.9736(2) 0.7622(2) 0.06656(7) 0.0277 1.0000 Uani . . . . . . . C5 C 0.9281(3) 0.6862(2) 0.05565(8) 0.0355 1.0000 Uani . . . . . . . C6 C 0.9619(3) 0.6543(2) 0.03930(8) 0.0394 1.0000 Uani . . . . . . . C7 C 1.0414(3) 0.6957(2) 0.03375(9) 0.0426 1.0000 Uani . . . . . . . C8 C 1.0869(3) 0.7695(2) 0.04420(8) 0.0356 1.0000 Uani . . . . . . . C9 C 1.0560(2) 0.8052(2) 0.06082(7) 0.0296 1.0000 Uani . . . . . . . C10 C 1.1079(2) 0.8838(2) 0.07159(7) 0.0263 1.0000 Uani . . . . . . . N11 N 1.08015(17) 0.92171(17) 0.08484(6) 0.0245 1.0000 Uani . . . . . . . O12 O 0.85983(14) 0.86570(14) 0.09517(6) 0.0299 1.0000 Uani . . . . . . . C13 C 1.1961(2) 0.9251(2) 0.06631(9) 0.0365 1.0000 Uani . . . . . . . C14 C 1.2151(3) 0.9713(3) 0.04019(10) 0.0579 1.0000 Uani . . . . . . . Cl15 Cl 1.0000 1.0000 0.03429(4) 0.0254 1.0000 Uani S T . . . . . O16 O 0.96369(16) 0.91969(15) 0.04412(5) 0.0315 1.0000 Uani . . . . . . . O17 O 1.0000 1.0000 0.00595(9) 0.0339 1.0000 Uani S T . . . . . N18 N 0.96620(19) 0.85982(17) 0.13534(7) 0.0287 1.0000 Uani . . . . . . . C19 C 0.9223(3) 0.8725(2) 0.15271(8) 0.0388 1.0000 Uani . . . . . . . C20 C 0.9178(3) 0.8533(2) 0.17933(8) 0.0425 1.0000 Uani . . . . . . . C21 C 0.9590(2) 0.8184(2) 0.18891(8) 0.0349 1.0000 Uani . . . . . . . C22 C 1.0023(3) 0.8039(2) 0.17080(9) 0.0418 1.0000 Uani . . . . . . . C23 C 1.0047(2) 0.8245(2) 0.14453(9) 0.0378 1.0000 Uani . . . . . . . C24 C 0.9561(4) 0.7958(3) 0.21825(10) 0.0633 1.0000 Uani . U . . . . . C25 C 0.9162(4) 0.7037(3) 0.21987(11) 0.0829 1.0000 Uani . U . . . . . C26 C 0.9026(4) 0.8142(3) 0.23508(9) 0.0741 1.0000 Uani . . . . . . . C27 C 1.0344(4) 0.8409(5) 0.22919(12) 0.1168 1.0000 Uani . U . . . . . H81 H 1.1396 0.7973 0.0399 0.0476 1.0000 Uiso R . . . . . . H71 H 1.0640 0.6740 0.0226 0.0566 1.0000 Uiso R . . . . . . H61 H 0.9322 0.6056 0.0320 0.0506 1.0000 Uiso R . . . . . . H51 H 0.8763 0.6567 0.0595 0.0420 1.0000 Uiso R . . . . . . H131 H 1.2238 0.9605 0.0810 0.0465 1.0000 Uiso R . . . . . . H132 H 1.2143 0.8877 0.0655 0.0466 1.0000 Uiso R . . . . . . H143 H 1.2707 0.9946 0.0368 0.0888 1.0000 Uiso R . . . . . . H141 H 1.2029 1.0116 0.0418 0.0884 1.0000 Uiso R . . . . . . H142 H 1.1854 0.9379 0.0259 0.0890 1.0000 Uiso R . . . . . . H231 H 1.0348 0.8135 0.1324 0.0469 1.0000 Uiso R . . . . . . H221 H 1.0301 0.7807 0.1764 0.0515 1.0000 Uiso R . . . . . . H201 H 0.8875 0.8632 0.1904 0.0532 1.0000 Uiso R . . . . . . H191 H 0.8940 0.8955 0.1465 0.0508 1.0000 Uiso R . . . . . . H262 H 0.8992 0.7931 0.2531 0.0948 1.0000 Uiso R . . . . . . H261 H 0.9238 0.8716 0.2358 0.0954 1.0000 Uiso R . . . . . . H263 H 0.8505 0.7884 0.2274 0.0951 1.0000 Uiso R . . . . . . H252 H 0.9225 0.6917 0.2384 0.1434 1.0000 Uiso R . . . . . . H253 H 0.9459 0.6874 0.2081 0.1434 1.0000 Uiso R . . . . . . H251 H 0.8588 0.6782 0.2153 0.1429 1.0000 Uiso R . . . . . . H272 H 1.0321 0.8136 0.2460 0.1457 1.0000 Uiso R . . . . . . H271 H 1.0492 0.8973 0.2314 0.1428 1.0000 Uiso R . . . . . . H273 H 1.0686 0.8339 0.2169 0.1452 1.0000 Uiso R . . . . . . Mn101 Mn 0.44389(3) 0.72134(4) 0.01319(3) 0.0227 1.0000 Uani . . . . . . . O102 O 0.3333 0.6667 0.01848(9) 0.0236 1.0000 Uani S T . . . . . O103 O 0.55028(14) 0.77110(15) 0.00360(5) 0.0296 1.0000 Uani . . . . . . . C104 C 0.58083(19) 0.7487(2) -0.01550(8) 0.0249 1.0000 Uani . . . . . . . C105 C 0.6443(2) 0.8071(2) -0.02987(8) 0.0329 1.0000 Uani . . . . . . . C106 C 0.6815(2) 0.7890(2) -0.04951(9) 0.0358 1.0000 Uani . . . . . . . C107 C 0.6556(2) 0.7103(2) -0.05581(8) 0.0334 1.0000 Uani . . . . . . . C108 C 0.5935(2) 0.6515(2) -0.04179(8) 0.0297 1.0000 Uani . . . . . . . C109 C 0.5543(2) 0.6680(2) -0.02167(7) 0.0240 1.0000 Uani . . . . . . . C110 C 0.4864(2) 0.6033(2) -0.00807(7) 0.0230 1.0000 Uani . . . . . . . N111 N 0.43783(16) 0.61750(17) 0.00512(6) 0.0222 1.0000 Uani . . . . . . . O112 O 0.44653(13) 0.82114(14) 0.01696(5) 0.0257 1.0000 Uani . . . . . . . C113 C 0.4703(2) 0.5191(2) -0.00993(8) 0.0310 1.0000 Uani . . . . . . . C114 C 0.4115(3) 0.4728(2) -0.03201(10) 0.0490 1.0000 Uani . . . . . . . Cl115 Cl 0.3333 0.6667 -0.04436(4) 0.0256 1.0000 Uani S T . . . . . O116 O 0.41197(15) 0.72101(15) -0.03463(6) 0.0301 1.0000 Uani . . . . . . . O117 O 0.3333 0.6667 -0.07240(9) 0.0387 1.0000 Uani S T . . . . . N118 N 0.47647(19) 0.72225(19) 0.05637(6) 0.0297 1.0000 Uani . . . . . . . C119 C 0.5013(2) 0.6754(2) 0.06624(8) 0.0321 1.0000 Uani . . . . . . . C120 C 0.5281(2) 0.6800(2) 0.09167(8) 0.0306 1.0000 Uani . . . . . . . C121 C 0.5307(2) 0.7354(2) 0.10919(8) 0.0317 1.0000 Uani . . . . . . . C122 C 0.5066(4) 0.7856(3) 0.09886(9) 0.0631 1.0000 Uani . . . . . . . C123 C 0.4800(3) 0.7769(3) 0.07257(9) 0.0571 1.0000 Uani . . . . . . . C124 C 0.5615(3) 0.7428(3) 0.13718(8) 0.0382 1.0000 Uani . . . . . . . C125 C 0.5054(3) 0.6703(3) 0.15297(9) 0.0516 1.0000 Uani . . . . . . . C126 C 0.6431(3) 0.7502(4) 0.13644(10) 0.0669 1.0000 Uani . . . . . . . C127 C 0.5684(4) 0.8152(3) 0.15160(9) 0.0740 1.0000 Uani . . . . . . . H1131 H 0.5187 0.5184 -0.0129 0.0369 1.0000 Uiso R . . . . . . H1132 H 0.4486 0.4918 0.0065 0.0373 1.0000 Uiso R . . . . . . H1143 H 0.4029 0.4212 -0.0340 0.0698 1.0000 Uiso R . . . . . . H1142 H 0.4292 0.4999 -0.0484 0.0699 1.0000 Uiso R . . . . . . H1141 H 0.3620 0.4692 -0.0281 0.0695 1.0000 Uiso R . . . . . . H1051 H 0.6609 0.8586 -0.0258 0.0378 1.0000 Uiso R . . . . . . H1061 H 0.7221 0.8289 -0.0589 0.0398 1.0000 Uiso R . . . . . . H1071 H 0.6803 0.6968 -0.0690 0.0398 1.0000 Uiso R . . . . . . H1081 H 0.5758 0.5989 -0.0460 0.0358 1.0000 Uiso R . . . . . . H1191 H 0.5017 0.6385 0.0552 0.0409 1.0000 Uiso R . . . . . . H1201 H 0.5446 0.6453 0.0973 0.0397 1.0000 Uiso R . . . . . . H1252 H 0.5270 0.6732 0.1703 0.0876 1.0000 Uiso R . . . . . . H1253 H 0.4556 0.6685 0.1549 0.0878 1.0000 Uiso R . . . . . . H1251 H 0.4972 0.6227 0.1447 0.0878 1.0000 Uiso R . . . . . . H1273 H 0.5877 0.8175 0.1691 0.1197 1.0000 Uiso R . . . . . . H1272 H 0.6052 0.8619 0.1423 0.1198 1.0000 Uiso R . . . . . . H1271 H 0.5176 0.8120 0.1522 0.1196 1.0000 Uiso R . . . . . . H1263 H 0.6621 0.7538 0.1539 0.1012 1.0000 Uiso R . . . . . . H1262 H 0.6790 0.7976 0.1272 0.1015 1.0000 Uiso R . . . . . . H1261 H 0.6401 0.7056 0.1278 0.1013 1.0000 Uiso R . . . . . . H1221 H 0.5076 0.8253 0.1096 0.0897 1.0000 Uiso R . . . . . . H1231 H 0.4643 0.8111 0.0661 0.0838 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 0.0238(3) 0.0215(2) 0.0245(3) 0.0019(2) 0.0040(2) 0.0114(2) O2 0.0231(13) 0.0231(13) 0.026(2) 0.0000 0.0000 0.0115(6) O3 0.0340(15) 0.0241(13) 0.0381(16) 0.0027(11) 0.0110(12) 0.0137(11) C4 0.044(2) 0.0285(18) 0.0203(17) 0.0072(14) 0.0043(15) 0.0250(17) C5 0.046(2) 0.028(2) 0.033(2) 0.0025(16) -0.0048(18) 0.0190(19) C6 0.070(3) 0.0262(19) 0.031(2) -0.0023(16) -0.005(2) 0.030(2) C7 0.067(3) 0.041(2) 0.035(2) 0.0008(19) 0.006(2) 0.038(2) C8 0.047(2) 0.042(2) 0.032(2) 0.0056(18) 0.0029(18) 0.033(2) C9 0.042(2) 0.035(2) 0.0232(18) 0.0086(15) 0.0031(16) 0.0277(18) C10 0.0332(19) 0.0272(18) 0.0209(15) 0.0079(14) 0.0015(15) 0.0169(16) N11 0.0237(15) 0.0259(15) 0.0254(15) 0.0061(13) 0.0022(12) 0.0135(12) O12 0.0299(13) 0.0265(13) 0.0347(15) 0.0073(11) 0.0064(11) 0.0151(11) C13 0.030(2) 0.045(2) 0.043(2) 0.0072(19) 0.0048(18) 0.0254(19) C14 0.048(3) 0.068(3) 0.062(3) 0.029(3) 0.031(3) 0.032(3) Cl15 0.0278(4) 0.0278(4) 0.0207(7) 0.0000 0.0000 0.0139(2) O16 0.0348(15) 0.0293(14) 0.0272(13) -0.0027(11) -0.0010(12) 0.0137(12) O17 0.0418(17) 0.0418(17) 0.018(2) 0.0000 0.0000 0.0209(8) N18 0.0342(17) 0.0230(15) 0.0278(16) 0.0022(13) 0.0018(13) 0.0133(14) C19 0.054(3) 0.037(2) 0.038(2) 0.0043(18) 0.005(2) 0.032(2) C20 0.063(3) 0.040(2) 0.029(2) 0.0033(18) 0.008(2) 0.030(2) C21 0.039(2) 0.0244(18) 0.030(2) 0.0068(15) -0.0029(17) 0.0069(17) C22 0.043(2) 0.044(2) 0.043(2) 0.015(2) 0.0003(19) 0.025(2) C23 0.041(2) 0.035(2) 0.041(2) 0.0092(18) 0.0115(19) 0.0219(19) C24 0.082(3) 0.081(3) 0.030(2) 0.013(2) -0.010(2) 0.043(3) C25 0.118(4) 0.082(4) 0.046(3) 0.025(3) 0.003(3) 0.048(3) C26 0.098(5) 0.065(4) 0.028(2) 0.003(2) 0.004(3) 0.018(3) C27 0.089(4) 0.158(5) 0.050(3) 0.019(3) -0.021(3) 0.022(4) Mn101 0.0217(3) 0.0226(2) 0.0241(3) -0.0034(3) -0.0019(2) 0.0113(2) O102 0.0206(12) 0.0206(12) 0.029(2) 0.0000 0.0000 0.0103(6) O103 0.0209(12) 0.0251(13) 0.0378(14) -0.0097(11) 0.0023(11) 0.0077(11) C104 0.0189(16) 0.0253(18) 0.0311(19) -0.0014(14) -0.0047(14) 0.0114(14) C105 0.0245(18) 0.0209(17) 0.051(2) -0.0047(16) -0.0018(17) 0.0099(15) C106 0.0205(18) 0.030(2) 0.049(3) 0.0054(18) 0.0115(17) 0.0068(16) C107 0.0279(19) 0.041(2) 0.032(2) -0.0023(17) 0.0034(16) 0.0173(17) C108 0.035(2) 0.0235(18) 0.031(2) -0.0037(15) 0.0016(16) 0.0141(16) C109 0.0247(17) 0.0260(17) 0.0199(16) -0.0002(14) -0.0037(13) 0.0116(15) C110 0.0272(17) 0.0266(17) 0.0184(16) -0.0042(13) -0.0050(13) 0.0158(15) N111 0.0228(14) 0.0227(14) 0.0208(14) -0.0013(11) -0.0050(12) 0.0113(12) O112 0.0232(12) 0.0247(12) 0.0295(13) -0.0027(10) -0.0060(10) 0.0122(10) C113 0.0321(19) 0.0267(19) 0.038(2) 0.0052(16) 0.0106(16) 0.0172(16) C114 0.055(3) 0.028(2) 0.056(3) -0.012(2) 0.000(2) 0.015(2) Cl115 0.0277(4) 0.0277(4) 0.0215(7) 0.0000 0.0000 0.0138(2) O116 0.0284(14) 0.0286(13) 0.0290(14) 0.0006(11) 0.0014(11) 0.0111(11) O117 0.0426(17) 0.0426(17) 0.031(3) 0.0000 0.0000 0.0213(9) N118 0.0322(17) 0.0364(18) 0.0283(16) -0.0051(13) -0.0060(14) 0.0230(14) C119 0.040(2) 0.0297(19) 0.033(2) -0.0066(16) -0.0047(17) 0.0220(17) C120 0.036(2) 0.0316(19) 0.033(2) -0.0003(16) -0.0041(16) 0.0233(17) C121 0.040(2) 0.036(2) 0.0254(19) -0.0007(16) -0.0007(16) 0.0238(18) C122 0.122(5) 0.071(3) 0.034(2) -0.022(2) -0.031(3) 0.076(4) C123 0.107(4) 0.067(3) 0.035(2) -0.009(2) -0.017(3) 0.072(3) C124 0.056(3) 0.043(2) 0.0249(19) 0.0009(17) -0.0043(19) 0.031(2) C125 0.079(4) 0.064(3) 0.033(2) 0.005(2) 0.004(2) 0.052(3) C126 0.059(3) 0.111(5) 0.035(3) -0.002(3) -0.016(2) 0.046(3) C127 0.152(6) 0.058(3) 0.029(2) -0.013(2) -0.027(3) 0.066(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.077856(10) 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 . Mn1 7_675 3.2534(9) yes Mn1 . O2 . 1.9009(8) yes Mn1 . O3 . 1.859(3) yes Mn1 . N11 . 2.007(3) yes Mn1 . O12 . 1.903(3) yes Mn1 . O16 . 2.470(3) yes Mn1 . N18 . 2.278(3) yes O3 . C4 . 1.328(4) yes C4 . C5 . 1.404(5) yes C4 . C9 . 1.422(5) yes C5 . C6 . 1.383(5) yes C5 . H51 . 0.899 no C6 . C7 . 1.373(6) yes C6 . H61 . 0.907 no C7 . C8 . 1.365(6) yes C7 . H71 . 0.935 no C8 . C9 . 1.404(5) yes C8 . H81 . 0.917 no C9 . C10 . 1.457(5) yes C10 . N11 . 1.299(4) yes C10 . C13 . 1.516(5) yes N11 . O12 4_765 1.376(4) yes C13 . C14 . 1.532(5) yes C13 . H131 . 0.972 no C13 . H132 . 0.959 no C14 . H143 . 0.960 no C14 . H141 . 0.934 no C14 . H142 . 0.947 no Cl15 . O16 7_675 1.447(3) yes Cl15 . O16 4_765 1.447(3) yes Cl15 . O16 . 1.447(3) yes Cl15 . O17 . 1.428(4) yes N18 . C19 . 1.332(5) yes N18 . C23 . 1.331(5) yes C19 . C20 . 1.383(5) yes C19 . H191 . 0.922 no C20 . C21 . 1.376(6) yes C20 . H201 . 0.902 no C21 . C22 . 1.366(6) yes C21 . C24 . 1.535(6) yes C22 . C23 . 1.377(5) yes C22 . H221 . 0.908 no C23 . H231 . 0.944 no C24 . C25 . 1.563(8) yes C24 . C26 . 1.521(8) yes C24 . C27 . 1.439(8) yes C25 . H252 . 0.983 no C25 . H253 . 0.987 no C25 . H251 . 0.998 no C26 . H262 . 0.982 no C26 . H261 . 0.983 no C26 . H263 . 0.961 no C27 . H272 . 0.988 no C27 . H271 . 0.995 no C27 . H273 . 0.970 no Mn101 . Mn101 4_665 3.2370(9) yes Mn101 . Mn101 7_565 3.2370(9) yes Mn101 . O102 . 1.8878(8) yes Mn101 . O103 . 1.863(2) yes Mn101 . N111 . 2.012(3) yes Mn101 . O112 . 1.932(2) yes Mn101 . O116 . 2.487(3) yes Mn101 . N118 . 2.263(3) yes O103 . C104 . 1.317(4) yes C104 . C105 . 1.395(5) yes C104 . C109 . 1.424(5) yes C105 . C106 . 1.372(5) yes C105 . H1051 . 0.913 no C106 . C107 . 1.394(5) yes C106 . H1061 . 0.917 no C107 . C108 . 1.377(5) yes C107 . H1071 . 0.932 no C108 . C109 . 1.400(5) yes C108 . H1081 . 0.930 no C109 . C110 . 1.466(5) yes C110 . N111 . 1.295(4) yes C110 . C113 . 1.515(5) yes N111 . O112 7_565 1.378(3) yes C113 . C114 . 1.528(5) yes C113 . H1131 . 0.962 no C113 . H1132 . 0.961 no C114 . H1143 . 0.940 no C114 . H1142 . 0.947 no C114 . H1141 . 0.954 no Cl115 . O116 7_565 1.447(3) yes Cl115 . O116 4_665 1.446(3) yes Cl115 . O117 4_665 1.413(5) yes Cl115 . O116 . 1.447(3) yes N118 . C119 . 1.328(5) yes N118 . C123 . 1.317(5) yes C119 . C120 . 1.370(5) yes C119 . H1191 . 0.913 no C120 . C121 . 1.377(5) yes C120 . H1201 . 0.927 no C121 . C122 . 1.383(5) yes C121 . C124 . 1.511(5) yes C122 . C123 . 1.401(6) yes C122 . H1221 . 0.937 no C123 . H1231 . 0.924 no C124 . C125 . 1.512(6) yes C124 . C126 . 1.527(6) yes C124 . C127 . 1.534(6) yes C125 . H1252 . 0.960 no C125 . H1253 . 0.961 no C125 . H1251 . 0.955 no C126 . H1263 . 0.943 no C126 . H1262 . 0.957 no C126 . H1261 . 0.947 no C127 . H1273 . 0.953 no C127 . H1272 . 0.954 no C127 . H1271 . 0.961 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 Mn1 7_675 Mn1 . O2 . 31.16(3) yes Mn1 7_675 Mn1 . O3 . 148.16(9) yes O2 . Mn1 . O3 . 174.57(15) yes Mn1 7_675 Mn1 . N11 . 117.52(8) yes O2 . Mn1 . N11 . 89.56(9) yes O3 . Mn1 . N11 . 88.38(11) yes Mn1 7_675 Mn1 . O12 . 60.66(8) yes O2 . Mn1 . O12 . 89.73(8) yes O3 . Mn1 . O12 . 91.87(11) yes N11 . Mn1 . O12 . 174.93(11) yes Mn1 7_675 Mn1 . O16 . 76.40(6) yes O2 . Mn1 . O16 . 86.21(14) yes O3 . Mn1 . O16 . 88.61(11) yes N11 . Mn1 . O16 . 85.11(10) yes O12 . Mn1 . O16 . 89.84(10) yes Mn1 7_675 Mn1 . N18 . 105.06(8) yes O2 . Mn1 . N18 . 96.19(14) yes O3 . Mn1 . N18 . 89.03(11) yes N11 . Mn1 . N18 . 96.09(11) yes O12 . Mn1 . N18 . 88.97(11) yes O16 . Mn1 . N18 . 177.32(10) yes Mn1 7_675 O2 . Mn1 . 117.69(6) yes Mn1 7_675 O2 . Mn1 4_765 117.69(6) yes Mn1 . O2 . Mn1 4_765 117.69(6) yes Mn1 . O3 . C4 . 129.1(2) yes O3 . C4 . C5 . 117.9(4) yes O3 . C4 . C9 . 123.6(3) yes C5 . C4 . C9 . 118.4(3) yes C4 . C5 . C6 . 121.1(4) yes C4 . C5 . H51 . 120.5 no C6 . C5 . H51 . 118.4 no C5 . C6 . C7 . 120.7(4) yes C5 . C6 . H61 . 120.9 no C7 . C6 . H61 . 118.4 no C6 . C7 . C8 . 119.3(4) yes C6 . C7 . H71 . 120.5 no C8 . C7 . H71 . 120.2 no C7 . C8 . C9 . 122.6(4) yes C7 . C8 . H81 . 118.7 no C9 . C8 . H81 . 118.7 no C4 . C9 . C8 . 117.9(4) yes C4 . C9 . C10 . 122.2(3) yes C8 . C9 . C10 . 119.9(4) yes C9 . C10 . N11 . 121.5(3) yes C9 . C10 . C13 . 120.2(3) yes N11 . C10 . C13 . 118.2(3) yes O12 4_765 N11 . Mn1 . 113.7(2) yes O12 4_765 N11 . C10 . 117.1(3) yes Mn1 . N11 . C10 . 129.2(3) yes N11 7_675 O12 . Mn1 . 115.84(19) yes C10 . C13 . C14 . 109.9(3) yes C10 . C13 . H131 . 109.0 no C14 . C13 . H131 . 110.5 no C10 . C13 . H132 . 110.9 no C14 . C13 . H132 . 109.9 no H131 . C13 . H132 . 106.7 no C13 . C14 . H143 . 108.5 no C13 . C14 . H141 . 109.3 no H143 . C14 . H141 . 108.8 no C13 . C14 . H142 . 111.1 no H143 . C14 . H142 . 110.3 no H141 . C14 . H142 . 108.8 no O16 7_675 Cl15 . O16 4_765 108.93(12) yes O16 7_675 Cl15 . O16 . 108.93(12) yes O16 4_765 Cl15 . O16 . 108.93(11) yes O16 7_675 Cl15 . O17 . 110.01(11) yes O16 4_765 Cl15 . O17 . 110.01(11) yes O16 . Cl15 . O17 . 110.01(11) yes Mn1 . O16 . Cl15 . 121.30(15) yes Mn1 . N18 . C19 . 120.1(3) yes Mn1 . N18 . C23 . 123.1(3) yes C19 . N18 . C23 . 116.7(3) yes N18 . C19 . C20 . 123.1(4) yes N18 . C19 . H191 . 117.8 no C20 . C19 . H191 . 119.1 no C19 . C20 . C21 . 120.1(4) yes C19 . C20 . H201 . 120.1 no C21 . C20 . H201 . 119.8 no C20 . C21 . C22 . 116.3(4) yes C20 . C21 . C24 . 122.3(4) yes C22 . C21 . C24 . 121.4(4) yes C21 . C22 . C23 . 121.0(4) yes C21 . C22 . H221 . 118.7 no C23 . C22 . H221 . 120.3 no C22 . C23 . N18 . 122.7(4) yes C22 . C23 . H231 . 119.3 no N18 . C23 . H231 . 118.0 no C21 . C24 . C25 . 107.8(4) yes C21 . C24 . C26 . 113.6(4) yes C25 . C24 . C26 . 103.6(5) yes C21 . C24 . C27 . 108.5(5) yes C25 . C24 . C27 . 116.8(6) yes C26 . C24 . C27 . 106.7(5) yes C24 . C25 . H252 . 105.9 no C24 . C25 . H253 . 107.7 no H252 . C25 . H253 . 109.0 no C24 . C25 . H251 . 110.7 no H252 . C25 . H251 . 110.1 no H253 . C25 . H251 . 113.2 no C24 . C26 . H262 . 109.1 no C24 . C26 . H261 . 110.1 no H262 . C26 . H261 . 110.1 no C24 . C26 . H263 . 109.0 no H262 . C26 . H263 . 108.5 no H261 . C26 . H263 . 110.1 no C24 . C27 . H272 . 104.5 no C24 . C27 . H271 . 110.6 no H272 . C27 . H271 . 114.2 no C24 . C27 . H273 . 105.4 no H272 . C27 . H273 . 108.7 no H271 . C27 . H273 . 112.8 no Mn101 4_665 Mn101 . Mn101 7_565 60.000(4) yes Mn101 4_665 Mn101 . O102 . 30.98(3) yes Mn101 7_565 Mn101 . O102 . 30.98(3) yes Mn101 4_665 Mn101 . O103 . 148.31(9) yes Mn101 7_565 Mn101 . O103 . 145.20(9) yes O102 . Mn101 . O103 . 172.86(15) yes Mn101 4_665 Mn101 . N111 . 116.77(8) yes Mn101 7_565 Mn101 . N111 . 58.14(8) yes O102 . Mn101 . N111 . 89.10(9) yes O103 . Mn101 . N111 . 87.80(11) yes Mn101 4_665 Mn101 . O112 . 61.12(7) yes Mn101 7_565 Mn101 . O112 . 120.80(7) yes O102 . Mn101 . O112 . 90.16(7) yes O103 . Mn101 . O112 . 92.23(11) yes N111 . Mn101 . O112 . 173.77(12) yes Mn101 4_665 Mn101 . O116 . 75.57(6) yes Mn101 7_565 Mn101 . O116 . 82.65(6) yes O102 . Mn101 . O116 . 85.47(14) yes O103 . Mn101 . O116 . 87.86(10) yes N111 . Mn101 . O116 . 85.03(10) yes Mn101 4_665 Mn101 . N118 . 106.08(8) yes Mn101 7_565 Mn101 . N118 . 98.39(8) yes O102 . Mn101 . N118 . 96.10(15) yes O103 . Mn101 . N118 . 90.55(11) yes N111 . Mn101 . N118 . 94.41(11) yes O112 . Mn101 . O116 . 88.75(10) yes O112 . Mn101 . N118 . 91.83(11) yes O116 . Mn101 . N118 . 178.33(11) yes Mn101 7_565 O102 . Mn101 . 118.05(6) yes Mn101 7_565 O102 . Mn101 4_665 118.05(6) yes Mn101 . O102 . Mn101 4_665 118.05(6) yes Mn101 . O103 . C104 . 126.0(2) yes O103 . C104 . C105 . 118.2(3) yes O103 . C104 . C109 . 123.5(3) yes C105 . C104 . C109 . 118.2(3) yes C104 . C105 . C106 . 122.1(3) yes C104 . C105 . H1051 . 117.5 no C106 . C105 . H1051 . 120.3 no C105 . C106 . C107 . 120.1(3) yes C105 . C106 . H1061 . 119.8 no C107 . C106 . H1061 . 120.1 no C106 . C107 . C108 . 118.9(3) yes C106 . C107 . H1071 . 121.4 no C108 . C107 . H1071 . 119.7 no C107 . C108 . C109 . 122.4(3) yes C107 . C108 . H1081 . 119.2 no C109 . C108 . H1081 . 118.4 no C104 . C109 . C108 . 118.3(3) yes C104 . C109 . C110 . 121.5(3) yes C108 . C109 . C110 . 120.2(3) yes C109 . C110 . N111 . 119.9(3) yes C109 . C110 . C113 . 120.9(3) yes N111 . C110 . C113 . 119.2(3) yes O112 7_565 N111 . Mn101 . 113.7(2) yes O112 7_565 N111 . C110 . 116.6(3) yes Mn101 . N111 . C110 . 129.7(2) yes N111 4_665 O112 . Mn101 . 112.28(19) yes C110 . C113 . C114 . 111.9(3) yes C110 . C113 . H1131 . 110.7 no C114 . C113 . H1131 . 109.3 no C110 . C113 . H1132 . 110.1 no C114 . C113 . H1132 . 107.9 no H1131 . C113 . H1132 . 106.9 no C113 . C114 . H1143 . 113.0 no C113 . C114 . H1142 . 110.4 no H1143 . C114 . H1142 . 108.9 no C113 . C114 . H1141 . 109.2 no H1143 . C114 . H1141 . 108.1 no H1142 . C114 . H1141 . 107.1 no O116 7_565 Cl115 . O116 4_665 109.17(12) yes O116 7_565 Cl115 . O117 4_665 109.70(11) yes O116 4_665 Cl115 . O117 4_665 109.86(11) yes O116 7_565 Cl115 . O116 . 109.10(12) yes O116 4_665 Cl115 . O116 . 109.19(12) yes O117 4_665 Cl115 . O116 . 109.80(11) yes Mn101 . O116 . Cl115 4_665 120.13(15) yes Mn101 . O116 . Cl115 . 120.15(15) yes Mn101 . O116 . Cl115 7_565 120.16(15) yes Mn101 . N118 . C119 . 123.5(3) yes Mn101 . N118 . C123 . 120.2(3) yes C119 . N118 . C123 . 115.9(3) yes N118 . C119 . C120 . 124.3(3) yes N118 . C119 . H1191 . 117.8 no C120 . C119 . H1191 . 117.9 no C119 . C120 . C121 . 120.9(3) yes C119 . C120 . H1201 . 119.8 no C121 . C120 . H1201 . 119.3 no C120 . C121 . C122 . 115.1(4) yes C120 . C121 . C124 . 122.0(3) yes C122 . C121 . C124 . 122.9(3) yes C121 . C122 . C123 . 120.4(4) yes C121 . C122 . H1221 . 119.7 no C123 . C122 . H1221 . 120.0 no C122 . C123 . N118 . 123.4(4) yes C122 . C123 . H1231 . 118.9 no N118 . C123 . H1231 . 117.7 no C121 . C124 . C125 . 109.5(4) yes C121 . C124 . C126 . 109.5(4) yes C125 . C124 . C126 . 109.5(4) yes C121 . C124 . C127 . 112.2(3) yes C125 . C124 . C127 . 107.6(4) yes C126 . C124 . C127 . 108.6(4) yes C124 . C125 . H1252 . 109.5 no C124 . C125 . H1253 . 109.4 no H1252 . C125 . H1253 . 108.3 no C124 . C125 . H1251 . 111.9 no H1252 . C125 . H1251 . 108.0 no H1253 . C125 . H1251 . 109.6 no C124 . C126 . H1263 . 109.7 no C124 . C126 . H1262 . 109.1 no H1263 . C126 . H1262 . 108.3 no C124 . C126 . H1261 . 110.0 no H1263 . C126 . H1261 . 109.7 no H1262 . C126 . H1261 . 110.2 no C124 . C127 . H1273 . 109.3 no C124 . C127 . H1272 . 108.9 no H1273 . C127 . H1272 . 108.6 no C124 . C127 . H1271 . 110.0 no H1273 . C127 . H1271 . 110.1 no H1272 . C127 . H1271 . 109.8 no # Attachment 'Complex 21.cif' data_EB8175 _database_code_depnum_ccdc_archive 'CCDC 736445' _audit_creation_date 08-11-18 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8175 in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H48 Cl1 Mn3 N6 O11' _chemical_compound_source 'Stepahnie Taylor, ST53' _exptl_crystal_recrystallization_method ; Slow evaporation og MeOH solution ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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 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 912_ALERT_3_A # Missing FCF Reflections Above STh/L= 0.600 1119 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 5469 5469 0 23.01 0.550 1.000 7280 7280 0 25.24 0.600 1.000 9460 9460 0 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.999 12023 12016 7 29.84 0.700 0.927 14945 13849 1096 29.85 0.700 0.925 14969 13850 1119 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 2 Reflections with [sin(\q/\l)]^2^ less than 0.01 were excluded from the refinement as these may be poorly measured in the vicinity of the beamstop. 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.17 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.25 Ratio No action. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 13.9058(7) _cell_length_b 19.4110(9) _cell_length_c 19.4946(8) _cell_angle_alpha 90 _cell_angle_beta 96.588(3) _cell_angle_gamma 90 _cell_volume 5227.3(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 = C40 H50 Cl1 Mn6 N12 O20 # Dc = 1.76 Fooo = 2448.00 Mu = 15.44 M = 1383.93 # Found Formula = C57 H48 Cl1 Mn3 N6 O11 # Dc = 1.52 FOOO = 2448.00 Mu = 8.34 M = 1193.28 _chemical_formula_sum 'C57 H48 Cl1 Mn3 N6 O11' _chemical_formula_weight 1193.28 _cell_measurement_reflns_used 1014 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description wedge _exptl_crystal_colour black _exptl_crystal_size_min 0.22 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.37 _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.834 # Sheldrick geometric approximatio 0.83 0.83 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.83 _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 '\f & \w scans' # 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 71170 _reflns_number_total 13850 _diffrn_reflns_av_R_equivalents 0.041 # Number of reflections with Friedels Law is 13850 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 15045 _diffrn_reflns_theta_min 1.485 _diffrn_reflns_theta_max 29.853 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.062 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 1.29 _oxford_diffrn_Wilson_scale 34.58 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.60 _refine_diff_density_max 0.73 # 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 13807 _refine_ls_number_restraints 0 _refine_ls_number_parameters 703 _oxford_refine_ls_R_factor_ref 0.0692 _refine_ls_wR_factor_ref 0.1193 _refine_ls_goodness_of_fit_ref 1.0296 _refine_ls_shift/su_max 0.000891 # The values computed from all data _oxford_reflns_number_all 13807 _refine_ls_R_factor_all 0.0692 _refine_ls_wR_factor_all 0.1193 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12148 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_gt 0.1118 # 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^) + ( 0.02P)^2^ +16.60P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.54455(3) 0.67930(2) 0.22049(2) 0.0166 1.0000 Uani . . . . . . . O2 O 0.53959(14) 0.76911(9) 0.18388(9) 0.0170 1.0000 Uani . . . . . . . Mn3 Mn 0.47558(3) 0.78389(2) 0.09386(2) 0.0173 1.0000 Uani . . . . . . . O4 O 0.39672(15) 0.80070(10) 0.01112(10) 0.0238 1.0000 Uani . . . . . . . C5 C 0.3428(2) 0.85449(15) -0.00905(14) 0.0198 1.0000 Uani . . . . . . . C6 C 0.3474(2) 0.91897(14) 0.02550(13) 0.0189 1.0000 Uani . . . . . . . C7 C 0.4133(2) 0.93192(14) 0.08748(14) 0.0192 1.0000 Uani . . . . . . . N8 N 0.46945(17) 0.88420(12) 0.11648(11) 0.0188 1.0000 Uani . . . . . . . O9 O 0.53195(15) 0.90590(10) 0.17206(10) 0.0227 1.0000 Uani . . . . . . . Mn10 Mn 0.54680(3) 0.84378(2) 0.24763(2) 0.0173 1.0000 Uani . . . . . . . O11 O 0.53714(16) 0.91400(10) 0.31187(10) 0.0237 1.0000 Uani . . . . . . . C12 C 0.4917(2) 0.91020(15) 0.36803(15) 0.0229 1.0000 Uani . . . . . . . C13 C 0.4871(2) 0.84939(15) 0.40796(14) 0.0215 1.0000 Uani . . . . . . . C14 C 0.5269(2) 0.78360(15) 0.38710(14) 0.0199 1.0000 Uani . . . . . . . N15 N 0.55177(16) 0.77648(12) 0.32503(12) 0.0180 1.0000 Uani . . . . . . . O16 O 0.59275(14) 0.71472(10) 0.30986(9) 0.0194 1.0000 Uani . . . . . . . C17 C 0.5360(2) 0.72434(15) 0.43579(14) 0.0209 1.0000 Uani . . . . . . . C18 C 0.5915(2) 0.73027(17) 0.49985(15) 0.0260 1.0000 Uani . . . . . . . C19 C 0.5995(3) 0.67559(19) 0.54585(16) 0.0327 1.0000 Uani . . . . . . . C20 C 0.5498(3) 0.61515(18) 0.52909(17) 0.0352 1.0000 Uani . . . . . . . C21 C 0.4937(3) 0.60902(17) 0.46569(16) 0.0308 1.0000 Uani . . . . . . . C22 C 0.4880(2) 0.66277(16) 0.41874(15) 0.0242 1.0000 Uani . . . . . . . C23 C 0.4416(2) 0.85266(17) 0.46877(16) 0.0276 1.0000 Uani . . . . . . . C24 C 0.4007(2) 0.91281(19) 0.48950(17) 0.0330 1.0000 Uani . . . . . . . C25 C 0.4051(2) 0.97171(18) 0.44972(17) 0.0330 1.0000 Uani . . . . . . . C26 C 0.4490(2) 0.97066(17) 0.39016(17) 0.0294 1.0000 Uani . . . . . . . N27 N 0.70908(17) 0.86109(12) 0.25537(12) 0.0211 1.0000 Uani . . . . . . . C28 C 0.7441(2) 0.91462(16) 0.22224(15) 0.0251 1.0000 Uani . . . . . . . C29 C 0.8403(2) 0.93330(16) 0.23256(16) 0.0276 1.0000 Uani . . . . . . . C30 C 0.9026(2) 0.89701(17) 0.27931(17) 0.0293 1.0000 Uani . . . . . . . C31 C 0.8683(2) 0.84242(18) 0.31442(18) 0.0334 1.0000 Uani . . . . . . . C32 C 0.7715(2) 0.82593(16) 0.29995(16) 0.0269 1.0000 Uani . . . . . . . C33 C 0.9321(3) 0.8029(3) 0.3677(3) 0.0731 1.0000 Uani . . . . . . . C34 C 0.4167(2) 1.00212(14) 0.11945(14) 0.0190 1.0000 Uani . . . . . . . C35 C 0.4727(3) 1.05387(17) 0.09681(18) 0.0357 1.0000 Uani . . . . . . . C36 C 0.4695(3) 1.11944(19) 0.1245(2) 0.0424 1.0000 Uani . . . . . . . C37 C 0.4113(3) 1.13324(18) 0.17546(18) 0.0355 1.0000 Uani . . . . . . . C38 C 0.3567(3) 1.0820(2) 0.1982(2) 0.0499 1.0000 Uani . . . . . . . C39 C 0.3594(3) 1.01606(19) 0.1708(2) 0.0427 1.0000 Uani . . . . . . . C40 C 0.2877(2) 0.97321(16) -0.00180(16) 0.0270 1.0000 Uani . . . . . . . C41 C 0.2253(2) 0.96542(17) -0.06157(17) 0.0315 1.0000 Uani . . . . . . . C42 C 0.2201(2) 0.90216(17) -0.09545(15) 0.0274 1.0000 Uani . . . . . . . C43 C 0.2774(2) 0.84831(16) -0.06971(14) 0.0229 1.0000 Uani . . . . . . . O44 O 0.47437(15) 0.68640(10) 0.07723(9) 0.0204 1.0000 Uani . . . . . . . N45 N 0.46623(16) 0.64633(12) 0.13385(11) 0.0174 1.0000 Uani . . . . . . . C46 C 0.41382(19) 0.59098(14) 0.12409(14) 0.0178 1.0000 Uani . . . . . . . C47 C 0.4011(2) 0.54458(14) 0.18159(13) 0.0175 1.0000 Uani . . . . . . . C48 C 0.4598(2) 0.54863(14) 0.24565(14) 0.0182 1.0000 Uani . . . . . . . O49 O 0.53440(15) 0.59139(10) 0.25785(10) 0.0217 1.0000 Uani . . . . . . . C50 C 0.4422(2) 0.50292(15) 0.29858(15) 0.0236 1.0000 Uani . . . . . . . C51 C 0.3700(2) 0.45397(16) 0.28856(15) 0.0262 1.0000 Uani . . . . . . . C52 C 0.3117(2) 0.44982(16) 0.22584(15) 0.0257 1.0000 Uani . . . . . . . C53 C 0.3268(2) 0.49496(15) 0.17362(14) 0.0214 1.0000 Uani . . . . . . . C54 C 0.3627(2) 0.57559(14) 0.05422(14) 0.0192 1.0000 Uani . . . . . . . C55 C 0.3812(2) 0.51472(16) 0.02106(15) 0.0255 1.0000 Uani . . . . . . . C56 C 0.3319(3) 0.49907(18) -0.04333(16) 0.0320 1.0000 Uani . . . . . . . C57 C 0.2634(3) 0.54409(19) -0.07398(16) 0.0336 1.0000 Uani . . . . . . . C58 C 0.2450(2) 0.60506(19) -0.04117(16) 0.0322 1.0000 Uani . . . . . . . C59 C 0.2949(2) 0.62141(16) 0.02235(15) 0.0254 1.0000 Uani . . . . . . . N60 N 0.61017(18) 0.78882(13) 0.03805(12) 0.0234 1.0000 Uani . . . . . . . C61 C 0.6230(2) 0.73697(16) -0.00600(15) 0.0242 1.0000 Uani . . . . . . . C62 C 0.6945(2) 0.73525(17) -0.04984(16) 0.0271 1.0000 Uani . . . . . . . C63 C 0.7001(3) 0.6775(2) -0.09997(18) 0.0367 1.0000 Uani . . . . . . . C64 C 0.7589(2) 0.79002(18) -0.04535(18) 0.0342 1.0000 Uani . . . . . . . C65 C 0.7489(2) 0.84303(18) 0.0008(2) 0.0365 1.0000 Uani . . . . . . . C66 C 0.6725(2) 0.84143(17) 0.04028(17) 0.0290 1.0000 Uani . . . . . . . N67 N 0.69720(18) 0.65707(13) 0.19467(12) 0.0230 1.0000 Uani . . . . . . . C68 C 0.7528(2) 0.70728(16) 0.17370(15) 0.0254 1.0000 Uani . . . . . . . C69 C 0.8515(2) 0.70019(18) 0.16834(16) 0.0312 1.0000 Uani . . . . . . . C70 C 0.8926(3) 0.6370(2) 0.18625(19) 0.0375 1.0000 Uani . . . . . . . C71 C 0.8365(3) 0.58416(19) 0.2074(2) 0.0390 1.0000 Uani . . . . . . . C72 C 0.7397(2) 0.59648(17) 0.21127(17) 0.0309 1.0000 Uani . . . . . . . C73 C 0.9100(3) 0.7591(2) 0.1458(2) 0.0467 1.0000 Uani . . . . . . . Cl74 Cl 0.31745(5) 0.76707(4) 0.21834(4) 0.0240 1.0000 Uani . . . . . . . O75 O 0.32216(15) 0.76365(12) 0.14452(10) 0.0264 1.0000 Uani . . . . . . . O76 O 0.36492(16) 0.82977(11) 0.24465(11) 0.0283 1.0000 Uani . . . . . . . O77 O 0.21858(17) 0.76715(15) 0.23159(13) 0.0401 1.0000 Uani . . . . . . . O78 O 0.36803(17) 0.70845(12) 0.25148(11) 0.0295 1.0000 Uani . . . . . . . H181 H 0.6237 0.7715 0.5114 0.0308 1.0000 Uiso R . . . . . . H191 H 0.6388 0.6798 0.5873 0.0393 1.0000 Uiso R . . . . . . H201 H 0.5540 0.5785 0.5602 0.0430 1.0000 Uiso R . . . . . . H211 H 0.4594 0.5688 0.4544 0.0374 1.0000 Uiso R . . . . . . H221 H 0.4523 0.6578 0.3758 0.0284 1.0000 Uiso R . . . . . . H231 H 0.4391 0.8130 0.4950 0.0324 1.0000 Uiso R . . . . . . H241 H 0.3709 0.9138 0.5297 0.0398 1.0000 Uiso R . . . . . . H251 H 0.3782 1.0121 0.4634 0.0389 1.0000 Uiso R . . . . . . H261 H 0.4515 1.0100 0.3639 0.0348 1.0000 Uiso R . . . . . . H281 H 0.7009 0.9394 0.1915 0.0300 1.0000 Uiso R . . . . . . H291 H 0.8628 0.9701 0.2084 0.0330 1.0000 Uiso R . . . . . . H301 H 0.9683 0.9089 0.2876 0.0349 1.0000 Uiso R . . . . . . H321 H 0.7472 0.7890 0.3220 0.0318 1.0000 Uiso R . . . . . . H332 H 0.8964 0.7684 0.3874 0.1082 1.0000 Uiso R . . . . . . H331 H 0.9586 0.8329 0.4032 0.1088 1.0000 Uiso R . . . . . . H333 H 0.9834 0.7828 0.3469 0.1076 1.0000 Uiso R . . . . . . H351 H 0.5125 1.0451 0.0627 0.0440 1.0000 Uiso R . . . . . . H361 H 0.5068 1.1543 0.1087 0.0525 1.0000 Uiso R . . . . . . H371 H 0.4092 1.1775 0.1937 0.0418 1.0000 Uiso R . . . . . . H381 H 0.3177 1.0910 0.2326 0.0623 1.0000 Uiso R . . . . . . H391 H 0.3231 0.9813 0.1870 0.0538 1.0000 Uiso R . . . . . . H401 H 0.2903 1.0151 0.0213 0.0320 1.0000 Uiso R . . . . . . H411 H 0.1871 1.0024 -0.0785 0.0368 1.0000 Uiso R . . . . . . H421 H 0.1780 0.8964 -0.1349 0.0322 1.0000 Uiso R . . . . . . H431 H 0.2730 0.8062 -0.0924 0.0270 1.0000 Uiso R . . . . . . H501 H 0.4809 0.5062 0.3409 0.0277 1.0000 Uiso R . . . . . . H511 H 0.3599 0.4232 0.3240 0.0319 1.0000 Uiso R . . . . . . H521 H 0.2630 0.4170 0.2187 0.0308 1.0000 Uiso R . . . . . . H531 H 0.2878 0.4930 0.1322 0.0256 1.0000 Uiso R . . . . . . H551 H 0.4269 0.4844 0.0417 0.0304 1.0000 Uiso R . . . . . . H561 H 0.3453 0.4579 -0.0656 0.0389 1.0000 Uiso R . . . . . . H571 H 0.2293 0.5333 -0.1160 0.0399 1.0000 Uiso R . . . . . . H581 H 0.1993 0.6353 -0.0621 0.0378 1.0000 Uiso R . . . . . . H591 H 0.2826 0.6628 0.0438 0.0300 1.0000 Uiso R . . . . . . H611 H 0.5810 0.6992 -0.0066 0.0290 1.0000 Uiso R . . . . . . H631 H 0.7656 0.6673 -0.1052 0.0561 1.0000 Uiso R . . . . . . H633 H 0.6679 0.6905 -0.1441 0.0561 1.0000 Uiso R . . . . . . H632 H 0.6691 0.6372 -0.0846 0.0564 1.0000 Uiso R . . . . . . H641 H 0.8085 0.7917 -0.0733 0.0418 1.0000 Uiso R . . . . . . H651 H 0.7924 0.8790 0.0055 0.0439 1.0000 Uiso R . . . . . . H661 H 0.6635 0.8779 0.0699 0.0349 1.0000 Uiso R . . . . . . H681 H 0.7235 0.7494 0.1621 0.0308 1.0000 Uiso R . . . . . . H701 H 0.9584 0.6302 0.1839 0.0449 1.0000 Uiso R . . . . . . H711 H 0.8633 0.5419 0.2192 0.0472 1.0000 Uiso R . . . . . . H721 H 0.7021 0.5609 0.2259 0.0365 1.0000 Uiso R . . . . . . H733 H 0.9754 0.7557 0.1658 0.0726 1.0000 Uiso R . . . . . . H732 H 0.8842 0.8023 0.1586 0.0727 1.0000 Uiso R . . . . . . H731 H 0.9089 0.7584 0.0965 0.0724 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 0.0191(2) 0.01486(19) 0.01531(18) 0.00090(14) 0.00012(15) -0.00065(15) O2 0.0214(9) 0.0150(9) 0.0140(8) -0.0002(7) 0.0000(7) -0.0008(7) Mn3 0.0217(2) 0.01511(19) 0.01444(18) 0.00053(14) -0.00020(15) -0.00053(16) O4 0.0308(11) 0.0212(10) 0.0178(9) -0.0012(8) -0.0034(8) 0.0036(8) C5 0.0203(13) 0.0222(14) 0.0169(12) 0.0031(10) 0.0025(10) -0.0033(11) C6 0.0193(13) 0.0205(13) 0.0165(12) 0.0042(10) -0.0004(10) -0.0024(10) C7 0.0209(13) 0.0198(13) 0.0172(12) 0.0025(10) 0.0033(10) -0.0026(10) N8 0.0210(11) 0.0198(11) 0.0146(10) -0.0002(8) -0.0018(8) -0.0025(9) O9 0.0271(11) 0.0187(10) 0.0203(10) 0.0021(8) -0.0066(8) -0.0053(8) Mn10 0.0210(2) 0.01530(19) 0.01510(18) -0.00015(15) -0.00067(15) 0.00020(16) O11 0.0320(11) 0.0187(10) 0.0205(10) -0.0042(8) 0.0032(8) -0.0012(8) C12 0.0220(14) 0.0247(15) 0.0208(13) -0.0047(11) -0.0030(10) 0.0010(11) C13 0.0195(13) 0.0248(14) 0.0192(13) -0.0028(11) -0.0019(10) 0.0025(11) C14 0.0178(13) 0.0250(14) 0.0163(12) -0.0011(10) -0.0005(10) -0.0004(11) N15 0.0167(11) 0.0175(11) 0.0192(11) -0.0006(9) -0.0013(8) -0.0002(9) O16 0.0220(10) 0.0193(10) 0.0164(9) -0.0008(7) -0.0005(7) 0.0040(8) C17 0.0203(13) 0.0249(14) 0.0181(12) 0.0006(10) 0.0052(10) 0.0019(11) C18 0.0277(15) 0.0310(16) 0.0196(13) 0.0011(11) 0.0041(11) 0.0008(12) C19 0.0356(18) 0.0407(19) 0.0209(14) 0.0065(13) -0.0001(12) 0.0057(15) C20 0.048(2) 0.0333(18) 0.0252(15) 0.0109(13) 0.0084(14) 0.0044(15) C21 0.0403(19) 0.0273(16) 0.0265(15) -0.0008(12) 0.0113(13) -0.0048(14) C22 0.0249(14) 0.0283(15) 0.0200(13) 0.0013(11) 0.0054(11) 0.0006(12) C23 0.0245(15) 0.0322(17) 0.0259(15) -0.0018(12) 0.0022(12) 0.0007(13) C24 0.0293(17) 0.043(2) 0.0270(15) -0.0087(14) 0.0055(13) 0.0048(14) C25 0.0327(17) 0.0329(18) 0.0326(17) -0.0128(14) 0.0007(13) 0.0088(14) C26 0.0317(17) 0.0253(16) 0.0299(16) -0.0043(12) -0.0026(13) 0.0036(13) N27 0.0228(12) 0.0198(12) 0.0203(11) 0.0002(9) 0.0009(9) -0.0026(9) C28 0.0252(15) 0.0245(15) 0.0242(14) 0.0026(11) -0.0035(11) -0.0013(12) C29 0.0299(16) 0.0228(15) 0.0299(15) 0.0021(12) 0.0030(12) -0.0070(12) C30 0.0209(14) 0.0312(17) 0.0353(17) 0.0050(13) 0.0007(12) -0.0038(12) C31 0.0243(16) 0.0353(18) 0.0404(18) 0.0143(15) 0.0026(13) 0.0028(14) C32 0.0236(15) 0.0260(15) 0.0314(16) 0.0090(12) 0.0042(12) -0.0014(12) C33 0.0233(19) 0.090(4) 0.103(4) 0.071(3) -0.006(2) 0.000(2) C34 0.0202(13) 0.0167(13) 0.0191(12) 0.0020(10) -0.0012(10) 0.0023(10) C35 0.047(2) 0.0268(17) 0.0368(18) -0.0052(14) 0.0200(16) -0.0075(15) C36 0.057(2) 0.0247(17) 0.047(2) -0.0059(15) 0.0135(18) -0.0113(16) C37 0.046(2) 0.0242(16) 0.0345(17) -0.0092(13) -0.0033(15) 0.0046(14) C38 0.062(3) 0.041(2) 0.052(2) -0.0182(18) 0.030(2) -0.0045(19) C39 0.053(2) 0.0302(18) 0.050(2) -0.0085(16) 0.0304(19) -0.0116(16) C40 0.0314(16) 0.0193(14) 0.0282(15) 0.0007(11) -0.0066(12) 0.0010(12) C41 0.0308(17) 0.0271(16) 0.0336(17) 0.0050(13) -0.0090(13) 0.0034(13) C42 0.0262(15) 0.0314(16) 0.0226(14) 0.0015(12) -0.0063(11) -0.0050(13) C43 0.0257(14) 0.0251(15) 0.0173(12) -0.0019(11) -0.0008(11) -0.0046(12) O44 0.0295(11) 0.0172(9) 0.0145(9) 0.0026(7) 0.0027(8) -0.0024(8) N45 0.0184(11) 0.0179(11) 0.0158(10) 0.0009(8) 0.0012(8) 0.0010(9) C46 0.0179(12) 0.0169(13) 0.0184(12) -0.0006(10) 0.0017(10) 0.0015(10) C47 0.0197(13) 0.0167(12) 0.0164(12) -0.0011(9) 0.0032(10) 0.0002(10) C48 0.0186(13) 0.0157(12) 0.0206(13) -0.0008(10) 0.0032(10) 0.0020(10) O49 0.0250(10) 0.0164(9) 0.0223(10) 0.0037(7) -0.0035(8) -0.0014(8) C50 0.0285(15) 0.0226(14) 0.0197(13) 0.0024(11) 0.0024(11) 0.0020(12) C51 0.0305(16) 0.0252(15) 0.0243(14) 0.0049(11) 0.0096(12) -0.0015(12) C52 0.0288(16) 0.0232(15) 0.0263(14) -0.0021(11) 0.0081(12) -0.0081(12) C53 0.0216(14) 0.0232(14) 0.0195(13) -0.0004(10) 0.0023(10) -0.0015(11) C54 0.0193(13) 0.0202(13) 0.0178(12) 0.0013(10) 0.0012(10) -0.0043(10) C55 0.0298(16) 0.0241(15) 0.0231(14) -0.0008(11) 0.0050(12) -0.0013(12) C56 0.0434(19) 0.0304(17) 0.0226(14) -0.0060(12) 0.0058(13) -0.0058(14) C57 0.0387(19) 0.0414(19) 0.0192(14) -0.0006(13) -0.0037(13) -0.0073(15) C58 0.0298(17) 0.0383(18) 0.0263(15) 0.0055(13) -0.0057(12) -0.0022(14) C59 0.0261(15) 0.0251(15) 0.0241(14) -0.0010(11) -0.0001(11) -0.0004(12) N60 0.0251(13) 0.0241(13) 0.0208(11) 0.0024(9) 0.0015(9) -0.0019(10) C61 0.0260(15) 0.0254(15) 0.0209(13) 0.0004(11) 0.0017(11) -0.0021(12) C62 0.0222(14) 0.0318(16) 0.0270(15) 0.0042(12) 0.0016(12) 0.0040(12) C63 0.0323(18) 0.048(2) 0.0307(17) -0.0057(15) 0.0087(14) 0.0067(16) C64 0.0253(16) 0.0373(19) 0.0422(19) 0.0074(15) 0.0127(14) 0.0006(14) C65 0.0284(17) 0.0280(17) 0.054(2) 0.0045(15) 0.0069(15) -0.0057(14) C66 0.0277(16) 0.0243(15) 0.0347(16) 0.0001(13) 0.0028(13) -0.0032(12) N67 0.0250(12) 0.0229(12) 0.0207(11) -0.0030(9) 0.0014(9) 0.0035(10) C68 0.0289(15) 0.0256(15) 0.0223(13) -0.0015(11) 0.0046(11) 0.0003(12) C69 0.0291(16) 0.0381(18) 0.0272(15) -0.0069(13) 0.0068(12) -0.0039(14) C70 0.0260(17) 0.046(2) 0.0408(19) -0.0109(16) 0.0042(14) 0.0065(15) C71 0.0343(19) 0.0325(19) 0.050(2) -0.0033(16) 0.0019(16) 0.0139(15) C72 0.0311(17) 0.0233(15) 0.0381(18) -0.0015(13) 0.0034(13) 0.0043(13) C73 0.037(2) 0.052(2) 0.054(2) -0.0007(19) 0.0186(18) -0.0097(18) Cl74 0.0210(3) 0.0278(4) 0.0233(3) -0.0034(3) 0.0035(2) 0.0007(3) O75 0.0258(11) 0.0314(12) 0.0214(10) -0.0026(8) 0.0000(8) 0.0014(9) O76 0.0273(11) 0.0257(11) 0.0312(11) -0.0069(9) 0.0003(9) 0.0040(9) O77 0.0248(12) 0.0568(17) 0.0401(14) -0.0091(12) 0.0095(10) -0.0023(11) O78 0.0342(12) 0.0273(12) 0.0274(11) 0.0029(9) 0.0057(9) 0.0010(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.22453(9) 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 . O2 . 1.8821(19) yes Mn1 . Mn3 . 3.2546(6) yes Mn1 . O16 . 1.9207(19) yes Mn1 . N45 . 2.007(2) yes Mn1 . O49 . 1.867(2) yes Mn1 . N67 . 2.278(2) yes Mn1 . O78 . 2.655(2) yes O2 . Mn3 . 1.8962(18) yes O2 . Mn10 . 1.9043(18) yes Mn3 . O4 . 1.872(2) yes Mn3 . N8 . 2.000(2) yes Mn3 . Mn10 . 3.2614(6) yes Mn3 . O44 . 1.920(2) yes Mn3 . N60 . 2.272(3) yes Mn3 . O75 . 2.483(2) yes O4 . C5 . 1.319(3) yes C5 . C6 . 1.419(4) yes C5 . C43 . 1.412(4) yes C6 . C7 . 1.453(4) yes C6 . C40 . 1.407(4) yes C7 . N8 . 1.298(4) yes C7 . C34 . 1.497(4) yes N8 . O9 . 1.375(3) yes O9 . Mn10 . 1.897(2) yes Mn10 . O11 . 1.866(2) yes Mn10 . N15 . 1.991(2) yes Mn10 . N27 . 2.269(2) yes Mn10 . O76 . 2.538(2) yes O11 . C12 . 1.327(3) yes C12 . C13 . 1.419(4) yes C12 . C26 . 1.405(4) yes C13 . C14 . 1.467(4) yes C13 . C23 . 1.408(4) yes C14 . N15 . 1.304(3) yes C14 . C17 . 1.488(4) yes N15 . O16 . 1.374(3) yes C17 . C18 . 1.396(4) yes C17 . C22 . 1.390(4) yes C18 . C19 . 1.386(4) yes C18 . H181 . 0.932 no C19 . C20 . 1.381(5) yes C19 . H191 . 0.925 no C20 . C21 . 1.389(5) yes C20 . H201 . 0.932 no C21 . C22 . 1.384(4) yes C21 . H211 . 0.928 no C22 . H221 . 0.928 no C23 . C24 . 1.379(4) yes C23 . H231 . 0.927 no C24 . C25 . 1.387(5) yes C24 . H241 . 0.928 no C25 . C26 . 1.373(5) yes C25 . H251 . 0.923 no C26 . H261 . 0.923 no N27 . C28 . 1.344(4) yes N27 . C32 . 1.342(4) yes C28 . C29 . 1.378(4) yes C28 . H281 . 0.932 no C29 . C30 . 1.378(4) yes C29 . H291 . 0.930 no C30 . C31 . 1.377(4) yes C30 . H301 . 0.937 no C31 . C32 . 1.380(4) yes C31 . C33 . 1.498(5) yes C32 . H321 . 0.920 no C33 . H332 . 0.942 no C33 . H331 . 0.945 no C33 . H333 . 0.945 no C34 . C35 . 1.374(4) yes C34 . C39 . 1.376(4) yes C35 . C36 . 1.386(5) yes C35 . H351 . 0.928 no C36 . C37 . 1.377(5) yes C36 . H361 . 0.927 no C37 . C38 . 1.357(5) yes C37 . H371 . 0.932 no C38 . C39 . 1.389(5) yes C38 . H381 . 0.926 no C39 . H391 . 0.920 no C40 . C41 . 1.378(4) yes C40 . H401 . 0.929 no C41 . C42 . 1.392(5) yes C41 . H411 . 0.931 no C42 . C43 . 1.374(4) yes C42 . H421 . 0.919 no C43 . H431 . 0.927 no O44 . N45 . 1.366(3) yes N45 . C46 . 1.300(3) yes C46 . C47 . 1.464(4) yes C46 . C54 . 1.492(4) yes C47 . C48 . 1.413(4) yes C47 . C53 . 1.409(4) yes C48 . O49 . 1.329(3) yes C48 . C50 . 1.404(4) yes C50 . C51 . 1.379(4) yes C50 . H501 . 0.935 no C51 . C52 . 1.390(4) yes C51 . H511 . 0.937 no C52 . C53 . 1.377(4) yes C52 . H521 . 0.929 no C53 . H531 . 0.920 no C54 . C55 . 1.385(4) yes C54 . C59 . 1.390(4) yes C55 . C56 . 1.393(4) yes C55 . H551 . 0.924 no C56 . C57 . 1.377(5) yes C56 . H561 . 0.939 no C57 . C58 . 1.383(5) yes C57 . H571 . 0.922 no C58 . C59 . 1.385(4) yes C58 . H581 . 0.925 no C59 . H591 . 0.931 no N60 . C61 . 1.348(4) yes N60 . C66 . 1.337(4) yes C61 . C62 . 1.384(4) yes C61 . H611 . 0.936 no C62 . C63 . 1.495(5) yes C62 . C64 . 1.386(5) yes C63 . H631 . 0.949 no C63 . H633 . 0.957 no C63 . H632 . 0.956 no C64 . C65 . 1.385(5) yes C64 . H641 . 0.928 no C65 . C66 . 1.381(5) yes C65 . H651 . 0.922 no C66 . H661 . 0.931 no N67 . C68 . 1.337(4) yes N67 . C72 . 1.339(4) yes C68 . C69 . 1.395(4) yes C68 . H681 . 0.929 no C69 . C70 . 1.381(5) yes C69 . C73 . 1.499(5) yes C70 . C71 . 1.380(5) yes C70 . H701 . 0.931 no C71 . C72 . 1.378(5) yes C71 . H711 . 0.920 no C72 . H721 . 0.929 no C73 . H733 . 0.950 no C73 . H732 . 0.956 no C73 . H731 . 0.960 no Cl74 . O75 . 1.450(2) yes Cl74 . O76 . 1.450(2) yes Cl74 . O77 . 1.428(2) yes Cl74 . O78 . 1.450(2) 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 O2 . Mn1 . Mn3 . 30.65(6) yes O2 . Mn1 . O16 . 90.36(8) yes Mn3 . Mn1 . O16 . 120.43(6) yes O2 . Mn1 . N45 . 89.05(9) yes Mn3 . Mn1 . N45 . 58.41(7) yes O16 . Mn1 . N45 . 167.65(9) yes O2 . Mn1 . O49 . 173.43(9) yes Mn3 . Mn1 . O49 . 146.84(6) yes O16 . Mn1 . O49 . 90.43(9) yes N45 . Mn1 . O49 . 88.79(9) yes O2 . Mn1 . N67 . 94.94(9) yes Mn3 . Mn1 . N67 . 98.71(6) yes O16 . Mn1 . N67 . 91.79(8) yes N45 . Mn1 . N67 . 100.55(9) yes O49 . Mn1 . N67 . 91.56(9) yes O2 . Mn1 . O78 . 83.93(8) yes Mn3 . Mn1 . O78 . 80.79(5) yes O16 . Mn1 . O78 . 87.30(8) yes N45 . Mn1 . O78 . 80.37(8) yes O49 . Mn1 . O78 . 89.59(8) yes N67 . Mn1 . O78 . 178.54(8) yes Mn1 . O2 . Mn3 . 118.95(10) yes Mn1 . O2 . Mn10 . 117.42(9) yes Mn3 . O2 . Mn10 . 118.22(10) yes O2 . Mn3 . Mn1 . 30.40(6) yes O2 . Mn3 . O4 . 171.92(9) yes Mn1 . Mn3 . O4 . 148.73(7) yes O2 . Mn3 . N8 . 88.32(8) yes Mn1 . Mn3 . N8 . 117.15(6) yes O4 . Mn3 . N8 . 89.12(9) yes O2 . Mn3 . Mn10 . 30.97(6) yes Mn1 . Mn3 . Mn10 . 59.548(13) yes O4 . Mn3 . Mn10 . 144.67(6) yes N8 . Mn3 . Mn10 . 57.77(6) yes O2 . Mn3 . O44 . 90.07(8) yes Mn1 . Mn3 . O44 . 60.61(6) yes O4 . Mn3 . O44 . 91.91(9) yes N8 . Mn3 . O44 . 175.54(9) yes Mn10 . Mn3 . O44 . 120.16(6) yes O2 . Mn3 . N60 . 97.15(8) yes Mn1 . Mn3 . N60 . 101.67(6) yes O4 . Mn3 . N60 . 90.77(9) yes N8 . Mn3 . N60 . 97.06(9) yes Mn10 . Mn3 . N60 . 104.19(6) yes O2 . Mn3 . O75 . 86.65(8) yes Mn1 . Mn3 . O75 . 77.96(5) yes O4 . Mn3 . O75 . 85.70(8) yes N8 . Mn3 . O75 . 90.35(9) yes Mn10 . Mn3 . O75 . 82.82(5) yes O44 . Mn3 . N60 . 87.27(9) yes O44 . Mn3 . O75 . 85.40(8) yes N60 . Mn3 . O75 . 171.75(8) yes Mn3 . O4 . C5 . 130.66(18) yes O4 . C5 . C6 . 124.3(2) yes O4 . C5 . C43 . 118.2(3) yes C6 . C5 . C43 . 117.5(3) yes C5 . C6 . C7 . 122.5(3) yes C5 . C6 . C40 . 119.2(3) yes C7 . C6 . C40 . 118.3(3) yes C6 . C7 . N8 . 122.0(3) yes C6 . C7 . C34 . 119.4(2) yes N8 . C7 . C34 . 118.7(2) yes Mn3 . N8 . C7 . 129.58(19) yes Mn3 . N8 . O9 . 115.65(16) yes C7 . N8 . O9 . 114.7(2) yes N8 . O9 . Mn10 . 114.83(15) yes O2 . Mn10 . O9 . 89.09(8) yes O2 . Mn10 . Mn3 . 30.82(6) yes O9 . Mn10 . Mn3 . 61.20(6) yes O2 . Mn10 . O11 . 172.45(9) yes O9 . Mn10 . O11 . 92.69(9) yes Mn3 . Mn10 . O11 . 147.08(7) yes O2 . Mn10 . N15 . 89.42(9) yes O9 . Mn10 . N15 . 175.58(9) yes Mn3 . Mn10 . N15 . 116.31(7) yes O11 . Mn10 . N15 . 88.26(9) yes O2 . Mn10 . N27 . 97.68(8) yes O9 . Mn10 . N27 . 88.65(9) yes Mn3 . Mn10 . N27 . 107.98(6) yes O11 . Mn10 . N27 . 89.70(9) yes N15 . Mn10 . N27 . 95.68(9) yes O2 . Mn10 . O76 . 85.75(8) yes O9 . Mn10 . O76 . 91.77(8) yes Mn3 . Mn10 . O76 . 75.17(5) yes O11 . Mn10 . O76 . 86.87(8) yes N15 . Mn10 . O76 . 83.97(8) yes N27 . Mn10 . O76 . 176.56(8) yes Mn10 . O11 . C12 . 126.19(19) yes O11 . C12 . C13 . 123.7(3) yes O11 . C12 . C26 . 117.7(3) yes C13 . C12 . C26 . 118.6(3) yes C12 . C13 . C14 . 122.0(3) yes C12 . C13 . C23 . 118.5(3) yes C14 . C13 . C23 . 119.5(3) yes C13 . C14 . N15 . 119.9(3) yes C13 . C14 . C17 . 120.2(2) yes N15 . C14 . C17 . 119.9(3) yes Mn10 . N15 . C14 . 130.1(2) yes Mn10 . N15 . O16 . 112.86(16) yes C14 . N15 . O16 . 116.9(2) yes N15 . O16 . Mn1 . 113.41(15) yes C14 . C17 . C18 . 120.3(3) yes C14 . C17 . C22 . 120.6(3) yes C18 . C17 . C22 . 119.1(3) yes C17 . C18 . C19 . 120.7(3) yes C17 . C18 . H181 . 119.2 no C19 . C18 . H181 . 120.1 no C18 . C19 . C20 . 119.8(3) yes C18 . C19 . H191 . 119.5 no C20 . C19 . H191 . 120.7 no C19 . C20 . C21 . 119.9(3) yes C19 . C20 . H201 . 120.1 no C21 . C20 . H201 . 120.0 no C20 . C21 . C22 . 120.5(3) yes C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 119.3 no C17 . C22 . C21 . 120.0(3) yes C17 . C22 . H221 . 119.8 no C21 . C22 . H221 . 120.1 no C13 . C23 . C24 . 121.7(3) yes C13 . C23 . H231 . 118.3 no C24 . C23 . H231 . 120.0 no C23 . C24 . C25 . 119.2(3) yes C23 . C24 . H241 . 120.3 no C25 . C24 . H241 . 120.5 no C24 . C25 . C26 . 120.9(3) yes C24 . C25 . H251 . 119.6 no C26 . C25 . H251 . 119.5 no C12 . C26 . C25 . 121.1(3) yes C12 . C26 . H261 . 118.5 no C25 . C26 . H261 . 120.4 no Mn10 . N27 . C28 . 119.7(2) yes Mn10 . N27 . C32 . 122.13(19) yes C28 . N27 . C32 . 117.5(3) yes N27 . C28 . C29 . 122.2(3) yes N27 . C28 . H281 . 117.8 no C29 . C28 . H281 . 120.1 no C28 . C29 . C30 . 119.3(3) yes C28 . C29 . H291 . 120.4 no C30 . C29 . H291 . 120.3 no C29 . C30 . C31 . 119.6(3) yes C29 . C30 . H301 . 121.0 no C31 . C30 . H301 . 119.4 no C30 . C31 . C32 . 117.6(3) yes C30 . C31 . C33 . 121.8(3) yes C32 . C31 . C33 . 120.6(3) yes C31 . C32 . N27 . 123.8(3) yes C31 . C32 . H321 . 119.1 no N27 . C32 . H321 . 117.0 no C31 . C33 . H332 . 110.4 no C31 . C33 . H331 . 110.0 no H332 . C33 . H331 . 108.7 no C31 . C33 . H333 . 109.3 no H332 . C33 . H333 . 109.9 no H331 . C33 . H333 . 108.5 no C7 . C34 . C35 . 121.6(3) yes C7 . C34 . C39 . 119.3(3) yes C35 . C34 . C39 . 119.1(3) yes C34 . C35 . C36 . 120.1(3) yes C34 . C35 . H351 . 120.2 no C36 . C35 . H351 . 119.7 no C35 . C36 . C37 . 120.5(3) yes C35 . C36 . H361 . 119.8 no C37 . C36 . H361 . 119.7 no C36 . C37 . C38 . 119.4(3) yes C36 . C37 . H371 . 120.1 no C38 . C37 . H371 . 120.5 no C37 . C38 . C39 . 120.6(3) yes C37 . C38 . H381 . 119.6 no C39 . C38 . H381 . 119.8 no C38 . C39 . C34 . 120.3(3) yes C38 . C39 . H391 . 120.2 no C34 . C39 . H391 . 119.4 no C6 . C40 . C41 . 121.6(3) yes C6 . C40 . H401 . 118.9 no C41 . C40 . H401 . 119.5 no C40 . C41 . C42 . 119.4(3) yes C40 . C41 . H411 . 119.6 no C42 . C41 . H411 . 121.0 no C41 . C42 . C43 . 120.1(3) yes C41 . C42 . H421 . 119.9 no C43 . C42 . H421 . 120.0 no C5 . C43 . C42 . 122.1(3) yes C5 . C43 . H431 . 118.3 no C42 . C43 . H431 . 119.5 no Mn3 . O44 . N45 . 115.14(15) yes O44 . N45 . Mn1 . 114.29(16) yes O44 . N45 . C46 . 116.7(2) yes Mn1 . N45 . C46 . 128.89(19) yes N45 . C46 . C47 . 120.7(2) yes N45 . C46 . C54 . 120.0(2) yes C47 . C46 . C54 . 119.3(2) yes C46 . C47 . C48 . 122.3(2) yes C46 . C47 . C53 . 119.2(2) yes C48 . C47 . C53 . 118.5(2) yes C47 . C48 . O49 . 123.5(2) yes C47 . C48 . C50 . 118.9(3) yes O49 . C48 . C50 . 117.5(2) yes C48 . O49 . Mn1 . 126.41(17) yes C48 . C50 . C51 . 121.1(3) yes C48 . C50 . H501 . 118.4 no C51 . C50 . H501 . 120.5 no C50 . C51 . C52 . 120.4(3) yes C50 . C51 . H511 . 120.2 no C52 . C51 . H511 . 119.4 no C51 . C52 . C53 . 119.4(3) yes C51 . C52 . H521 . 120.9 no C53 . C52 . H521 . 119.8 no C47 . C53 . C52 . 121.7(3) yes C47 . C53 . H531 . 118.5 no C52 . C53 . H531 . 119.8 no C46 . C54 . C55 . 120.2(3) yes C46 . C54 . C59 . 120.5(3) yes C55 . C54 . C59 . 119.3(3) yes C54 . C55 . C56 . 120.5(3) yes C54 . C55 . H551 . 119.7 no C56 . C55 . H551 . 119.8 no C55 . C56 . C57 . 119.8(3) yes C55 . C56 . H561 . 119.9 no C57 . C56 . H561 . 120.3 no C56 . C57 . C58 . 119.8(3) yes C56 . C57 . H571 . 120.1 no C58 . C57 . H571 . 120.1 no C57 . C58 . C59 . 120.6(3) yes C57 . C58 . H581 . 119.5 no C59 . C58 . H581 . 119.9 no C54 . C59 . C58 . 119.8(3) yes C54 . C59 . H591 . 120.1 no C58 . C59 . H591 . 120.0 no Mn3 . N60 . C61 . 116.7(2) yes Mn3 . N60 . C66 . 125.7(2) yes C61 . N60 . C66 . 117.3(3) yes N60 . C61 . C62 . 124.6(3) yes N60 . C61 . H611 . 117.7 no C62 . C61 . H611 . 117.7 no C61 . C62 . C63 . 121.1(3) yes C61 . C62 . C64 . 116.6(3) yes C63 . C62 . C64 . 122.3(3) yes C62 . C63 . H631 . 110.5 no C62 . C63 . H633 . 109.6 no H631 . C63 . H633 . 108.3 no C62 . C63 . H632 . 110.4 no H631 . C63 . H632 . 109.6 no H633 . C63 . H632 . 108.5 no C62 . C64 . C65 . 119.9(3) yes C62 . C64 . H641 . 120.6 no C65 . C64 . H641 . 119.5 no C64 . C65 . C66 . 119.1(3) yes C64 . C65 . H651 . 120.9 no C66 . C65 . H651 . 120.0 no C65 . C66 . N60 . 122.4(3) yes C65 . C66 . H661 . 119.7 no N60 . C66 . H661 . 117.9 no Mn1 . N67 . C68 . 121.0(2) yes Mn1 . N67 . C72 . 120.6(2) yes C68 . N67 . C72 . 117.4(3) yes N67 . C68 . C69 . 124.0(3) yes N67 . C68 . H681 . 117.6 no C69 . C68 . H681 . 118.4 no C68 . C69 . C70 . 116.8(3) yes C68 . C69 . C73 . 121.2(3) yes C70 . C69 . C73 . 121.9(3) yes C69 . C70 . C71 . 120.2(3) yes C69 . C70 . H701 . 119.6 no C71 . C70 . H701 . 120.2 no C70 . C71 . C72 . 118.5(3) yes C70 . C71 . H711 . 120.7 no C72 . C71 . H711 . 120.8 no C71 . C72 . N67 . 123.1(3) yes C71 . C72 . H721 . 118.4 no N67 . C72 . H721 . 118.6 no C69 . C73 . H733 . 110.7 no C69 . C73 . H732 . 111.1 no H733 . C73 . H732 . 108.9 no C69 . C73 . H731 . 109.6 no H733 . C73 . H731 . 108.3 no H732 . C73 . H731 . 108.1 no O75 . Cl74 . O76 . 108.61(13) yes O75 . Cl74 . O77 . 109.49(14) yes O76 . Cl74 . O77 . 110.12(14) yes O75 . Cl74 . O78 . 109.35(13) yes O76 . Cl74 . O78 . 108.86(13) yes O77 . Cl74 . O78 . 110.38(15) yes Mn3 . O75 . Cl74 . 121.76(12) yes Mn10 . O76 . Cl74 . 120.67(12) yes Cl74 . O78 . Mn1 . 118.67(12) yes