# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- KF_KOH_combined.cif' _audit_creation_date 11-09-20 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'kf in P -1' _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'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. ; _publ_contact_author_name 'Cedric Desroches' _publ_contact_author_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Nowhere, Nowhere, NO1 4T, UK. ; _publ_contact_author_phone '+44 1865 000000' _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_email cedric.desroches@univ-lyon1.fr _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_section_title # Title of paper - generally just the systematic or trivial name ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_address _publ_author_footnote # Author 1 # Author 2 ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; ; ? # Address 2 ; ; ? # Footnote 2 ; _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 (Cooper et al, 2010). Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; _publ_author_name 'Cedric Desroches' # 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)" # data_KF _database_code_depnum_ccdc_archive 'CCDC 824786' #TrackingRef '- KF_KOH_combined.cif' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 12.1491(6) _cell_length_b 12.9634(7) _cell_length_c 17.3393(9) _cell_angle_alpha 72.172(5) _cell_angle_beta 81.666(4) _cell_angle_gamma 64.773(5) _cell_volume 2351.4(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' 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' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C50 H50 F0.50 K1 Mn2 O8 S4 # Dc = 1.51 Fooo = 1111.33 Mu = 8.60 M = 1065.66 # Found Formula = C42.65 H54.59 F0.50 K0.50 Mn2 O14.65 S4 # Dc = 1.51 FOOO = 1111.33 Mu = 8.27 M = 1068.80 _chemical_formula_sum 'C85.30 H109.18 F K Mn4 O29.30 S8' _chemical_formula_moiety 'C82 H96 F K Mn4 O26 S8, 3.3(C H4 O' _chemical_compound_source ? _chemical_formula_weight 2137.62 _cell_measurement_reflns_used 20983 _cell_measurement_theta_min 3.3178 _cell_measurement_theta_max 29.5545 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.074 _exptl_crystal_size_mid 0.164 _exptl_crystal_size_max 0.239 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1111.328 _exptl_absorpt_coefficient_mu 0.827 # Sheldrick geometric approximatio 0.87 0.94 _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.4685 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 100 _diffrn_reflns_number 59479 _reflns_number_total 11882 _diffrn_reflns_av_R_equivalents 0.065 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 11882 # Theoretical number of reflections is about 26495 _diffrn_reflns_theta_min 3.324 _diffrn_reflns_theta_max 29.617 _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 26.665 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -15 _reflns_limit_h_max 16 _reflns_limit_k_min -16 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _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 difmap _refine_diff_density_min -1.38 _refine_diff_density_max 2.48 # 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 11882 _refine_ls_number_restraints 9 _refine_ls_number_parameters 590 _oxford_refine_ls_R_factor_ref 0.0795 _refine_ls_wR_factor_ref 0.1617 _refine_ls_goodness_of_fit_ref 1.0042 _refine_ls_shift/su_max 0.0006035 _refine_ls_shift/su_mean 0.0000319 # The values computed from all data _oxford_reflns_number_all 11882 _refine_ls_R_factor_all 0.0795 _refine_ls_wR_factor_all 0.1617 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9549 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_gt 0.1279 # 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: 680. 0.104E+04 547. 145. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Oxford Diffraction, (2010). CrysAlisPro. Oxford Diffraction, (2006). Gemini User Manual. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 0.61756(5) 0.37966(5) 0.42726(3) 0.0137 1.0000 Uani . . . . . . F2 F 0.5000 0.5000 0.5000 0.0152 1.0000 Uani S . . . . . Mn3 Mn 0.65283(5) 0.53583(5) 0.51679(3) 0.0136 1.0000 Uani . . . . . . O4 O 0.6705(2) 0.5342(2) 0.38873(15) 0.0169 1.0000 Uani . . . . . . C5 C 0.6870(3) 0.6030(3) 0.3194(2) 0.0152 1.0000 Uani . . . . . . C6 C 0.6806(3) 0.5866(3) 0.2427(2) 0.0178 1.0000 Uani . . . . . . S7 S 0.64951(8) 0.47093(8) 0.23245(5) 0.0154 1.0000 Uani . . . . . . O8 O 0.6832(2) 0.3737(2) 0.30483(16) 0.0173 1.0000 Uani . . . . . . O9 O 0.7068(2) 0.4441(2) 0.15825(16) 0.0205 1.0000 Uani . . . . . . C10 C 0.4909(3) 0.5306(3) 0.2193(2) 0.0155 1.0000 Uani . . . . . . C11 C 0.4077(3) 0.5335(3) 0.2869(2) 0.0144 1.0000 Uani . . . . . . O12 O 0.4409(2) 0.4869(2) 0.36228(15) 0.0161 1.0000 Uani . . . . . . C13 C 0.2842(3) 0.5924(3) 0.2622(2) 0.0151 1.0000 Uani . . . . . . S14 S 0.16139(8) 0.62052(8) 0.33241(5) 0.0143 1.0000 Uani . . . . . . O15 O 0.8075(2) 0.4756(2) 0.59347(15) 0.0159 1.0000 Uani . . . . . . O16 O 0.0545(2) 0.6420(2) 0.29341(16) 0.0186 1.0000 Uani . . . . . . C17 C 0.8569(3) 0.2486(3) 0.6466(2) 0.0158 1.0000 Uani . . . . . . C18 C 0.9283(3) 0.1468(3) 0.7032(2) 0.0172 1.0000 Uani . . . . . . C19 C 0.9507(3) 0.0343(3) 0.7002(2) 0.0167 1.0000 Uani . . . . . . C20 C 1.0260(3) -0.0742(3) 0.7655(2) 0.0186 1.0000 Uani . . . . . . C21 C 1.0336(4) -0.1885(4) 0.7537(3) 0.0299 1.0000 Uani . . . . . . C22 C 0.9656(4) -0.0626(4) 0.8489(3) 0.0279 1.0000 Uani . . . . . . C23 C 1.1551(4) -0.0814(4) 0.7626(3) 0.0279 1.0000 Uani . . . . . . C24 C 0.9018(3) 0.0291(3) 0.6345(2) 0.0167 1.0000 Uani . . . . . . C25 C 0.8298(3) 0.1296(3) 0.5773(2) 0.0154 1.0000 Uani . . . . . . C26 C 0.8006(3) 0.2467(3) 0.5810(2) 0.0130 1.0000 Uani . . . . . . O27 O 0.7311(2) 0.3423(2) 0.52875(16) 0.0157 1.0000 Uani . . . . . . S28 S 0.76941(8) 0.09842(8) 0.50502(5) 0.0138 1.0000 Uani . . . . . . O29 O 0.7391(2) 0.1956(2) 0.43221(16) 0.0175 1.0000 Uani . . . . . . O30 O 0.8539(2) -0.0157(2) 0.49497(16) 0.0169 1.0000 Uani . . . . . . C31 C 0.6362(3) 0.0833(3) 0.5512(2) 0.0151 1.0000 Uani . . . . . . C32 C 0.5207(3) 0.1816(3) 0.54636(19) 0.0123 1.0000 Uani . . . . . . O33 O 0.5024(2) 0.2896(2) 0.50471(16) 0.0169 1.0000 Uani . . . . . . C34 C 0.4280(3) 0.1476(3) 0.5924(2) 0.0153 1.0000 Uani . . . . . . S35 S 0.27907(8) 0.25063(8) 0.60462(5) 0.0155 1.0000 Uani . . . . . . C36 C 0.7140(3) 0.7023(3) 0.3116(2) 0.0168 1.0000 Uani . . . . . . C37 C 0.7291(3) 0.7766(3) 0.2370(2) 0.0185 1.0000 Uani . . . . . . C38 C 0.7180(3) 0.7595(4) 0.1636(2) 0.0204 1.0000 Uani . . . . . . C39 C 0.6941(4) 0.6628(3) 0.1685(2) 0.0197 1.0000 Uani . . . . . . C40 C 0.7292(4) 0.8471(4) 0.0831(3) 0.0266 1.0000 Uani . . . . . . C41 C 0.8564(4) 0.8471(4) 0.0763(3) 0.0328 1.0000 Uani . . . . . . C42 C 0.7096(5) 0.8142(5) 0.0102(3) 0.0370 1.0000 Uani . . . . . . C43 C 0.6318(5) 0.9707(4) 0.0823(3) 0.0358 1.0000 Uani . . . . . . O44 O 0.7542(2) 0.6482(2) 0.46632(16) 0.0170 1.0000 Uani . . . . . . O45 O 0.2004(2) 0.1889(2) 0.62546(17) 0.0205 1.0000 Uani . . . . . . C46 C 0.4490(3) 0.0322(3) 0.6377(2) 0.0188 1.0000 Uani . . . . . . C47 C 0.5631(3) -0.0604(3) 0.6432(2) 0.0188 1.0000 Uani . . . . . . C48 C 0.6548(3) -0.0309(3) 0.5977(2) 0.0169 1.0000 Uani . . . . . . C49 C 0.5910(4) -0.1849(3) 0.6980(2) 0.0213 1.0000 Uani . . . . . . C50 C 0.6681(5) -0.2768(4) 0.6522(3) 0.0362 1.0000 Uani . . . . . . C51 C 0.4763(5) -0.2046(4) 0.7292(4) 0.0395 1.0000 Uani . . . . . . C52 C 0.6640(6) -0.2032(5) 0.7698(3) 0.0422 1.0000 Uani . . . . . . C53 C 0.2495(3) 0.6397(3) 0.1816(2) 0.0176 1.0000 Uani . . . . . . C54 C 0.3334(4) 0.6348(3) 0.1176(2) 0.0191 1.0000 Uani . . . . . . C55 C 0.4545(3) 0.5794(3) 0.1387(2) 0.0178 1.0000 Uani . . . . . . C56 C 0.2896(4) 0.6911(4) 0.0300(2) 0.0202 1.0000 Uani . . . . . . C57 C 0.3950(4) 0.6878(4) -0.0304(2) 0.0302 1.0000 Uani . . . . . . C58 C 0.2238(4) 0.6235(4) 0.0114(3) 0.0292 1.0000 Uani . . . . . . C59 C 0.2011(4) 0.8206(4) 0.0206(3) 0.0260 1.0000 Uani . . . . . . K60 K 1.0000 0.5000 0.5000 0.0244 1.0000 Uani S . . . . . C61 C 1.0058(14) 0.4760(13) 0.1695(9) 0.0982 0.6480 Uani D U . . . . O62 O 0.9465(12) 0.4825(10) 0.0963(8) 0.1126 0.6480 Uani D U . . . . C63 C 1.0147(4) 0.7108(4) 0.5886(3) 0.0298 1.0000 Uani D . . . . . O64 O 0.9672(3) 0.7060(3) 0.5190(2) 0.0342 1.0000 Uani D . . . . . C65 C 0.3881(4) 0.8609(5) 0.2392(3) 0.0389 1.0000 Uani D . . . . . O66 O 0.3738(4) 0.8633(4) 0.1570(3) 0.0568 1.0000 Uani D . . . . . H181 H 0.9624 0.1557 0.7440 0.0207 1.0000 Uiso R . . . . . H212 H 1.0799 -0.2550 0.7962 0.0450 1.0000 Uiso R . . . . . H211 H 0.9535 -0.1867 0.7544 0.0448 1.0000 Uiso R . . . . . H213 H 1.0724 -0.1991 0.7025 0.0446 1.0000 Uiso R . . . . . H222 H 1.0088 -0.1334 0.8908 0.0419 1.0000 Uiso R . . . . . H221 H 0.8822 -0.0517 0.8489 0.0418 1.0000 Uiso R . . . . . H223 H 0.9681 0.0045 0.8601 0.0418 1.0000 Uiso R . . . . . H231 H 1.2027 -0.1500 0.8038 0.0418 1.0000 Uiso R . . . . . H233 H 1.1925 -0.0871 0.7100 0.0420 1.0000 Uiso R . . . . . H232 H 1.1536 -0.0120 0.7726 0.0418 1.0000 Uiso R . . . . . H241 H 0.9177 -0.0460 0.6286 0.0200 1.0000 Uiso R . . . . . H371 H 0.7480 0.8391 0.2371 0.0222 1.0000 Uiso R . . . . . H391 H 0.6884 0.6465 0.1209 0.0238 1.0000 Uiso R . . . . . H411 H 0.8640 0.9035 0.0270 0.0490 1.0000 Uiso R . . . . . H412 H 0.8706 0.8674 0.1219 0.0489 1.0000 Uiso R . . . . . H413 H 0.9171 0.7698 0.0753 0.0488 1.0000 Uiso R . . . . . H421 H 0.7173 0.8719 -0.0388 0.0558 1.0000 Uiso R . . . . . H422 H 0.7699 0.7367 0.0092 0.0558 1.0000 Uiso R . . . . . H423 H 0.6291 0.8155 0.0129 0.0557 1.0000 Uiso R . . . . . H431 H 0.6344 1.0254 0.0301 0.0539 1.0000 Uiso R . . . . . H432 H 0.6486 0.9964 0.1243 0.0539 1.0000 Uiso R . . . . . H433 H 0.5525 0.9690 0.0913 0.0537 1.0000 Uiso R . . . . . H461 H 0.3830 0.0183 0.6654 0.0228 1.0000 Uiso R . . . . . H481 H 0.7334 -0.0903 0.5986 0.0199 1.0000 Uiso R . . . . . H501 H 0.6857 -0.3555 0.6883 0.0538 1.0000 Uiso R . . . . . H503 H 0.6237 -0.2655 0.6057 0.0541 1.0000 Uiso R . . . . . H502 H 0.7437 -0.2685 0.6340 0.0540 1.0000 Uiso R . . . . . H511 H 0.4980 -0.2843 0.7650 0.0590 1.0000 Uiso R . . . . . H512 H 0.4340 -0.1963 0.6832 0.0588 1.0000 Uiso R . . . . . H513 H 0.4260 -0.1475 0.7588 0.0590 1.0000 Uiso R . . . . . H521 H 0.6893 -0.2847 0.8028 0.0630 1.0000 Uiso R . . . . . H522 H 0.6115 -0.1504 0.8017 0.0630 1.0000 Uiso R . . . . . H523 H 0.7351 -0.1857 0.7499 0.0630 1.0000 Uiso R . . . . . H531 H 0.1655 0.6751 0.1707 0.0215 1.0000 Uiso R . . . . . H551 H 0.5135 0.5751 0.0975 0.0208 1.0000 Uiso R . . . . . H571 H 0.3644 0.7230 -0.0843 0.0450 1.0000 Uiso R . . . . . H573 H 0.4368 0.7307 -0.0205 0.0448 1.0000 Uiso R . . . . . H572 H 0.4518 0.6069 -0.0261 0.0448 1.0000 Uiso R . . . . . H581 H 0.1947 0.6603 -0.0436 0.0441 1.0000 Uiso R . . . . . H583 H 0.2802 0.5420 0.0163 0.0440 1.0000 Uiso R . . . . . H582 H 0.1562 0.6262 0.0487 0.0439 1.0000 Uiso R . . . . . H591 H 0.1795 0.8593 -0.0356 0.0389 1.0000 Uiso R . . . . . H592 H 0.2396 0.8609 0.0384 0.0391 1.0000 Uiso R . . . . . H593 H 0.1285 0.8252 0.0525 0.0391 1.0000 Uiso R . . . . . H631 H 0.9495 0.7355 0.6272 0.0437 1.0000 Uiso R . . . . . H633 H 1.0536 0.7653 0.5722 0.0440 1.0000 Uiso R . . . . . H651 H 0.4466 0.8922 0.2388 0.0585 1.0000 Uiso R . . . . . H652 H 0.3121 0.9089 0.2588 0.0583 1.0000 Uiso R . . . . . H632 H 1.0733 0.6328 0.6136 0.0442 1.0000 Uiso R . . . . . H653 H 0.4150 0.7816 0.2741 0.0583 1.0000 Uiso R . . . . . H661 H 0.4050 0.7949 0.1536 0.0855 1.0000 Uiso R . . . . . H641 H 0.9280 0.7738 0.4919 0.0513 1.0000 Uiso R . . . . . H621 H 0.9718 0.5246 0.0595 0.1653 0.6480 Uiso R . . . . . H611 H 0.9770 0.4272 0.2124 0.1981 0.6480 Uiso R . . . . . H612 H 0.9957 0.5444 0.1843 0.1981 0.6480 Uiso R . . . . . H613 H 1.0896 0.4331 0.1593 0.1981 0.6480 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 0.0122(2) 0.0143(3) 0.0134(3) -0.00380(19) 0.00110(18) -0.0047(2) F2 0.0121(13) 0.0140(13) 0.0171(14) -0.0043(11) 0.0016(11) -0.0035(11) Mn3 0.0118(2) 0.0135(3) 0.0142(3) -0.00323(19) 0.00101(18) -0.0048(2) O4 0.0180(12) 0.0175(12) 0.0144(12) -0.0015(10) 0.0042(9) -0.0099(10) C5 0.0113(15) 0.0174(16) 0.0134(15) -0.0013(12) 0.0001(12) -0.0049(13) C6 0.0146(16) 0.0194(17) 0.0167(17) -0.0017(13) -0.0005(12) -0.0066(13) S7 0.0139(4) 0.0165(4) 0.0133(4) -0.0040(3) 0.0020(3) -0.0045(3) O8 0.0171(12) 0.0170(12) 0.0161(12) -0.0052(10) 0.0019(9) -0.0054(10) O9 0.0183(13) 0.0218(13) 0.0167(12) -0.0078(10) 0.0052(10) -0.0037(11) C10 0.0150(15) 0.0138(15) 0.0159(16) -0.0051(12) 0.0018(12) -0.0042(13) C11 0.0189(16) 0.0115(15) 0.0129(15) -0.0045(12) 0.0008(12) -0.0057(13) O12 0.0142(11) 0.0183(12) 0.0140(11) -0.0036(10) -0.0005(9) -0.0054(10) C13 0.0142(15) 0.0162(16) 0.0144(15) -0.0048(12) 0.0031(12) -0.0063(13) S14 0.0126(4) 0.0159(4) 0.0144(4) -0.0047(3) 0.0007(3) -0.0058(3) O15 0.0161(12) 0.0162(12) 0.0145(11) -0.0042(9) 0.0020(9) -0.0066(10) O16 0.0120(11) 0.0232(13) 0.0204(13) -0.0066(10) -0.0013(10) -0.0061(10) C17 0.0142(15) 0.0145(16) 0.0176(16) -0.0039(13) 0.0017(12) -0.0057(13) C18 0.0171(16) 0.0197(17) 0.0152(16) -0.0035(13) -0.0026(13) -0.0080(14) C19 0.0141(15) 0.0163(16) 0.0156(16) -0.0037(13) 0.0017(12) -0.0034(13) C20 0.0171(16) 0.0161(17) 0.0176(17) -0.0018(13) -0.0025(13) -0.0034(13) C21 0.034(2) 0.0177(19) 0.032(2) -0.0018(16) -0.0143(18) -0.0044(17) C22 0.027(2) 0.026(2) 0.0200(19) -0.0007(16) -0.0014(15) -0.0045(17) C23 0.0189(18) 0.030(2) 0.029(2) -0.0015(17) -0.0081(16) -0.0064(16) C24 0.0150(15) 0.0149(16) 0.0173(16) -0.0048(13) 0.0027(13) -0.0042(13) C25 0.0152(15) 0.0149(16) 0.0153(15) -0.0039(13) 0.0029(12) -0.0064(13) C26 0.0133(15) 0.0137(15) 0.0118(14) -0.0035(12) 0.0006(11) -0.0055(12) O27 0.0160(12) 0.0136(12) 0.0172(12) -0.0052(9) -0.0017(9) -0.0046(9) S28 0.0121(4) 0.0135(4) 0.0151(4) -0.0054(3) 0.0022(3) -0.0043(3) O29 0.0181(12) 0.0177(12) 0.0159(12) -0.0057(10) 0.0024(10) -0.0066(10) O30 0.0152(12) 0.0146(12) 0.0187(12) -0.0086(10) 0.0023(9) -0.0021(10) C31 0.0138(15) 0.0157(16) 0.0153(15) -0.0035(13) -0.0003(12) -0.0060(13) C32 0.0137(15) 0.0128(15) 0.0092(14) -0.0001(11) -0.0034(11) -0.0052(12) O33 0.0143(12) 0.0133(12) 0.0192(12) -0.0009(10) 0.0004(9) -0.0046(10) C34 0.0162(16) 0.0133(15) 0.0151(15) -0.0028(12) -0.0011(12) -0.0054(13) S35 0.0118(4) 0.0152(4) 0.0176(4) -0.0027(3) 0.0013(3) -0.0053(3) C36 0.0143(15) 0.0178(17) 0.0143(16) -0.0025(13) 0.0019(12) -0.0048(13) C37 0.0173(16) 0.0198(17) 0.0179(17) -0.0005(13) 0.0002(13) -0.0104(14) C38 0.0176(17) 0.0229(18) 0.0171(17) -0.0018(14) 0.0009(13) -0.0079(14) C39 0.0220(18) 0.0221(18) 0.0138(16) -0.0032(14) 0.0026(13) -0.0098(15) C40 0.028(2) 0.025(2) 0.0218(19) 0.0016(16) 0.0014(16) -0.0131(17) C41 0.035(2) 0.038(3) 0.024(2) -0.0007(18) 0.0069(18) -0.021(2) C42 0.056(3) 0.041(3) 0.0163(19) 0.0018(18) -0.0004(19) -0.028(2) C43 0.037(3) 0.030(2) 0.028(2) 0.0056(18) 0.0033(19) -0.012(2) O44 0.0120(11) 0.0175(12) 0.0198(12) -0.0034(10) -0.0020(9) -0.0053(10) O45 0.0150(12) 0.0187(13) 0.0259(14) -0.0028(11) 0.0014(10) -0.0078(10) C46 0.0166(16) 0.0208(18) 0.0185(16) -0.0048(14) 0.0029(13) -0.0086(14) C47 0.0194(17) 0.0171(17) 0.0195(17) -0.0042(13) -0.0011(13) -0.0071(14) C48 0.0153(16) 0.0136(16) 0.0202(17) -0.0050(13) 0.0007(13) -0.0043(13) C49 0.0183(17) 0.0184(18) 0.0247(19) -0.0023(14) 0.0007(14) -0.0078(14) C50 0.038(3) 0.018(2) 0.045(3) -0.0064(19) 0.014(2) -0.0109(19) C51 0.031(2) 0.025(2) 0.056(3) -0.001(2) 0.010(2) -0.0148(19) C52 0.055(3) 0.034(3) 0.035(3) 0.005(2) -0.015(2) -0.021(2) C53 0.0176(16) 0.0200(17) 0.0151(16) -0.0052(13) -0.0003(13) -0.0073(14) C54 0.0199(17) 0.0196(17) 0.0156(16) -0.0034(13) -0.0008(13) -0.0069(14) C55 0.0210(17) 0.0168(16) 0.0144(16) -0.0027(13) 0.0020(13) -0.0085(14) C56 0.0188(17) 0.0240(19) 0.0135(16) -0.0042(14) 0.0003(13) -0.0055(14) C57 0.024(2) 0.041(3) 0.0160(18) -0.0037(17) -0.0006(15) -0.0074(18) C58 0.031(2) 0.035(2) 0.0224(19) -0.0120(17) -0.0007(16) -0.0118(19) C59 0.0217(19) 0.026(2) 0.0218(19) 0.0006(16) -0.0039(15) -0.0050(16) K60 0.0150(5) 0.0246(6) 0.0304(6) -0.0047(5) 0.0042(4) -0.0084(4) C61 0.088(8) 0.066(7) 0.138(11) -0.001(7) -0.006(8) -0.045(6) O62 0.124(8) 0.087(6) 0.123(9) -0.028(6) 0.005(7) -0.042(6) C63 0.027(2) 0.035(2) 0.032(2) -0.0149(19) 0.0055(17) -0.0148(19) O64 0.0329(17) 0.0335(18) 0.0374(18) -0.0061(14) -0.0076(14) -0.0148(14) C65 0.025(2) 0.047(3) 0.047(3) -0.020(2) 0.007(2) -0.014(2) O66 0.066(3) 0.051(3) 0.056(3) -0.022(2) -0.010(2) -0.019(2) _refine_ls_extinction_coef 124(9) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 2.108(16) 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 . Mn3 2_666 3.0971(8) yes Mn1 . F2 . 2.2018(5) yes Mn1 . Mn3 . 3.0900(8) yes Mn1 . O4 . 2.242(3) yes Mn1 . O8 . 2.169(3) yes Mn1 . O12 . 2.238(3) yes Mn1 . O27 . 2.202(3) yes Mn1 . O29 . 2.188(3) yes Mn1 . O33 . 2.238(3) yes F2 . Mn3 2_666 2.1732(5) yes F2 . Mn3 . 2.1732(5) yes Mn3 . O33 2_666 2.206(3) yes Mn3 . O12 2_666 2.235(3) yes Mn3 . O4 . 2.205(3) yes Mn3 . O15 . 2.178(3) yes Mn3 . O27 . 2.224(3) yes Mn3 . O44 . 2.200(3) yes O4 . C5 . 1.307(4) yes C5 . C6 . 1.426(5) yes C5 . C36 . 1.423(5) yes C6 . S7 . 1.757(4) yes C6 . C39 . 1.399(5) yes S7 . O8 . 1.439(3) yes S7 . O9 . 1.438(3) yes S7 . C10 . 1.764(4) yes C10 . C11 . 1.431(5) yes C10 . C55 . 1.396(5) yes C11 . O12 . 1.303(4) yes C11 . C13 . 1.424(5) yes C13 . S14 . 1.767(4) yes C13 . C53 . 1.390(5) yes S14 . C17 2_666 1.759(4) yes S14 . O15 2_666 1.451(3) yes S14 . O16 . 1.432(3) yes C17 . C18 . 1.391(5) yes C17 . C26 . 1.421(5) yes C18 . C19 . 1.381(5) yes C18 . H181 . 0.928 no C19 . C20 . 1.524(5) yes C19 . C24 . 1.389(5) yes C20 . C21 . 1.520(6) yes C20 . C22 . 1.544(6) yes C20 . C23 . 1.526(5) yes C21 . H212 . 0.960 no C21 . H211 . 0.961 no C21 . H213 . 0.962 no C22 . H222 . 0.968 no C22 . H221 . 0.961 no C22 . H223 . 0.961 no C23 . H231 . 0.963 no C23 . H233 . 0.968 no C23 . H232 . 0.959 no C24 . C25 . 1.391(5) yes C24 . H241 . 0.944 no C25 . C26 . 1.425(5) yes C25 . S28 . 1.761(4) yes C26 . O27 . 1.308(4) yes S28 . O29 . 1.443(3) yes S28 . O30 . 1.443(3) yes S28 . C31 . 1.760(4) yes C31 . C32 . 1.430(5) yes C31 . C48 . 1.389(5) yes C32 . O33 . 1.302(4) yes C32 . C34 . 1.431(5) yes C34 . S35 . 1.762(4) yes C34 . C46 . 1.390(5) yes S35 . C36 2_666 1.764(4) yes S35 . O44 2_666 1.450(3) yes S35 . O45 . 1.435(3) yes C36 . C37 . 1.397(5) yes C37 . C38 . 1.392(5) yes C37 . H371 . 0.932 no C38 . C39 . 1.379(5) yes C38 . C40 . 1.537(5) yes C39 . H391 . 0.932 no C40 . C41 . 1.532(6) yes C40 . C42 . 1.529(6) yes C40 . C43 . 1.531(7) yes C41 . H411 . 0.963 no C41 . H412 . 0.964 no C41 . H413 . 0.962 no C42 . H421 . 0.969 no C42 . H422 . 0.962 no C42 . H423 . 0.965 no C43 . H431 . 0.969 no C43 . H432 . 0.966 no C43 . H433 . 0.962 no C46 . C47 . 1.387(5) yes C46 . H461 . 0.930 no C47 . C48 . 1.390(5) yes C47 . C49 . 1.520(5) yes C48 . H481 . 0.936 no C49 . C50 . 1.530(6) yes C49 . C51 . 1.516(6) yes C49 . C52 . 1.534(6) yes C50 . H501 . 0.969 no C50 . H503 . 0.973 no C50 . H502 . 0.967 no C51 . H511 . 0.972 no C51 . H512 . 0.965 no C51 . H513 . 0.970 no C52 . H521 . 0.970 no C52 . H522 . 0.970 no C52 . H523 . 0.975 no C53 . C54 . 1.391(5) yes C53 . H531 . 0.943 no C54 . C55 . 1.382(5) yes C54 . C56 . 1.533(5) yes C55 . H551 . 0.932 no C56 . C57 . 1.526(6) yes C56 . C58 . 1.534(6) yes C56 . C59 . 1.531(6) yes C57 . H571 . 0.958 no C57 . H573 . 0.960 no C57 . H572 . 0.966 no C58 . H581 . 0.969 no C58 . H583 . 0.969 no C58 . H582 . 0.965 no C59 . H591 . 0.966 no C59 . H592 . 0.968 no C59 . H593 . 0.961 no K60 . O64 2_766 2.644(3) yes K60 . O64 . 2.644(3) yes C61 . O62 . 1.512(9) yes C61 . H611 . 0.950 no C61 . H612 . 0.950 no C61 . H613 . 0.950 no O62 . H621 . 0.820 no C63 . O64 . 1.439(5) yes C63 . H631 . 0.969 no C63 . H633 . 0.963 no C63 . H632 . 0.962 no O64 . H641 . 0.821 no C65 . O66 . 1.451(6) yes C65 . H651 . 0.955 no C65 . H652 . 0.952 no C65 . H653 . 0.958 no O66 . H661 . 0.819 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 Mn3 2_666 Mn1 . F2 . 44.561(14) yes Mn3 2_666 Mn1 . Mn3 . 89.25(2) yes F2 . Mn1 . Mn3 . 44.690(14) yes Mn3 2_666 Mn1 . O4 . 109.26(7) yes F2 . Mn1 . O4 . 74.94(7) yes Mn3 . Mn1 . O4 . 45.50(7) yes Mn3 2_666 Mn1 . O8 . 125.45(7) yes F2 . Mn1 . O8 . 143.08(7) yes Mn3 . Mn1 . O8 . 123.92(7) yes O4 . Mn1 . O8 . 79.63(10) yes Mn3 2_666 Mn1 . O12 . 46.14(7) yes F2 . Mn1 . O12 . 73.74(7) yes Mn3 . Mn1 . O12 . 107.19(7) yes O4 . Mn1 . O12 . 91.90(10) yes O8 . Mn1 . O12 . 80.89(10) yes Mn3 2_666 Mn1 . O27 . 109.09(7) yes F2 . Mn1 . O27 . 75.09(7) yes Mn3 . Mn1 . O27 . 46.00(7) yes O4 . Mn1 . O27 . 78.36(10) yes O8 . Mn1 . O27 . 125.24(10) yes Mn3 2_666 Mn1 . O29 . 124.77(7) yes F2 . Mn1 . O29 . 144.39(7) yes Mn3 . Mn1 . O29 . 125.94(7) yes O4 . Mn1 . O29 . 125.88(10) yes O8 . Mn1 . O29 . 72.54(10) yes Mn3 2_666 Mn1 . O33 . 45.40(7) yes F2 . Mn1 . O33 . 74.61(7) yes Mn3 . Mn1 . O33 . 109.00(7) yes O4 . Mn1 . O33 . 149.55(10) yes O8 . Mn1 . O33 . 126.89(10) yes O12 . Mn1 . O27 . 148.78(10) yes O12 . Mn1 . O29 . 126.80(10) yes O27 . Mn1 . O29 . 81.27(10) yes O12 . Mn1 . O33 . 79.76(9) yes O27 . Mn1 . O33 . 93.67(10) yes O29 . Mn1 . O33 . 80.82(10) yes Mn3 2_666 F2 . Mn1 . 90.13(2) yes Mn3 2_666 F2 . Mn1 2_666 89.87(2) yes Mn1 . F2 . Mn1 2_666 179.995 yes Mn3 2_666 F2 . Mn3 . 179.995 yes Mn1 . F2 . Mn3 . 89.87(2) yes Mn1 2_666 F2 . Mn3 . 90.13(2) yes F2 . Mn3 . O33 2_666 75.83(7) yes F2 . Mn3 . O12 2_666 74.34(7) yes O33 2_666 Mn3 . O12 2_666 80.51(10) yes F2 . Mn3 . Mn1 . 45.441(14) yes O33 2_666 Mn3 . Mn1 . 110.41(7) yes O12 2_666 Mn3 . Mn1 . 108.30(7) yes F2 . Mn3 . Mn1 2_666 45.308(14) yes O33 2_666 Mn3 . Mn1 2_666 46.26(7) yes O12 2_666 Mn3 . Mn1 2_666 46.21(7) yes Mn1 . Mn3 . Mn1 2_666 90.75(2) yes F2 . Mn3 . O4 . 76.25(7) yes O33 2_666 Mn3 . O4 . 94.02(10) yes O12 2_666 Mn3 . O4 . 150.55(10) yes Mn1 . Mn3 . O4 . 46.48(7) yes Mn1 2_666 Mn3 . O4 . 110.71(7) yes F2 . Mn3 . O15 . 143.88(7) yes O33 2_666 Mn3 . O15 . 125.94(10) yes O12 2_666 Mn3 . O15 . 81.11(9) yes Mn1 . Mn3 . O15 . 123.61(7) yes Mn1 2_666 Mn3 . O15 . 125.53(7) yes F2 . Mn3 . O27 . 75.21(7) yes O33 2_666 Mn3 . O27 . 151.04(10) yes O12 2_666 Mn3 . O27 . 92.14(10) yes Mn1 . Mn3 . O27 . 45.42(7) yes Mn1 2_666 Mn3 . O27 . 110.00(7) yes F2 . Mn3 . O44 . 145.22(7) yes O33 2_666 Mn3 . O44 . 81.52(10) yes O12 2_666 Mn3 . O44 . 127.52(10) yes Mn1 . Mn3 . O44 . 124.18(7) yes Mn1 2_666 Mn3 . O44 . 126.31(7) yes O4 . Mn3 . O15 . 123.66(10) yes O4 . Mn3 . O27 . 78.68(10) yes O15 . Mn3 . O27 . 79.72(10) yes O4 . Mn3 . O44 . 79.43(10) yes O15 . Mn3 . O44 . 70.85(10) yes O27 . Mn3 . O44 . 123.61(10) yes Mn3 . O4 . Mn1 . 88.02(9) yes Mn3 . O4 . C5 . 136.0(2) yes Mn1 . O4 . C5 . 135.3(2) yes O4 . C5 . C6 . 123.8(3) yes O4 . C5 . C36 . 123.9(3) yes C6 . C5 . C36 . 112.3(3) yes C5 . C6 . S7 . 123.0(3) yes C5 . C6 . C39 . 123.6(4) yes S7 . C6 . C39 . 113.4(3) yes C6 . S7 . O8 . 110.03(17) yes C6 . S7 . O9 . 107.49(17) yes O8 . S7 . O9 . 116.17(16) yes C6 . S7 . C10 . 105.68(17) yes O8 . S7 . C10 . 109.78(16) yes O9 . S7 . C10 . 107.14(17) yes Mn1 . O8 . S7 . 126.87(16) yes S7 . C10 . C11 . 121.8(3) yes S7 . C10 . C55 . 114.6(3) yes C11 . C10 . C55 . 123.6(3) yes C10 . C11 . O12 . 124.0(3) yes C10 . C11 . C13 . 112.2(3) yes O12 . C11 . C13 . 123.8(3) yes Mn3 2_666 O12 . Mn1 . 87.65(9) yes Mn3 2_666 O12 . C11 . 136.2(2) yes Mn1 . O12 . C11 . 135.9(2) yes C11 . C13 . S14 . 122.3(3) yes C11 . C13 . C53 . 123.5(3) yes S14 . C13 . C53 . 114.1(3) yes C13 . S14 . C17 2_666 105.59(17) yes C13 . S14 . O15 2_666 109.70(16) yes C17 2_666 S14 . O15 2_666 109.02(16) yes C13 . S14 . O16 . 108.00(17) yes C17 2_666 S14 . O16 . 108.91(17) yes O15 2_666 S14 . O16 . 115.18(16) yes Mn3 . O15 . S14 2_666 126.42(15) yes S14 2_666 C17 . C18 . 112.8(3) yes S14 2_666 C17 . C26 . 123.7(3) yes C18 . C17 . C26 . 123.4(3) yes C17 . C18 . C19 . 122.5(3) yes C17 . C18 . H181 . 118.1 no C19 . C18 . H181 . 119.4 no C18 . C19 . C20 . 120.4(3) yes C18 . C19 . C24 . 115.5(3) yes C20 . C19 . C24 . 124.2(3) yes C19 . C20 . C21 . 112.0(3) yes C19 . C20 . C22 . 108.7(3) yes C21 . C20 . C22 . 108.4(3) yes C19 . C20 . C23 . 109.4(3) yes C21 . C20 . C23 . 108.1(3) yes C22 . C20 . C23 . 110.3(3) yes C20 . C21 . H212 . 110.1 no C20 . C21 . H211 . 110.4 no H212 . C21 . H211 . 108.8 no C20 . C21 . H213 . 110.4 no H212 . C21 . H213 . 108.7 no H211 . C21 . H213 . 108.5 no C20 . C22 . H222 . 109.9 no C20 . C22 . H221 . 109.9 no H222 . C22 . H221 . 109.4 no C20 . C22 . H223 . 109.6 no H222 . C22 . H223 . 108.9 no H221 . C22 . H223 . 109.1 no C20 . C23 . H231 . 109.4 no C20 . C23 . H233 . 110.3 no H231 . C23 . H233 . 109.4 no C20 . C23 . H232 . 110.1 no H231 . C23 . H232 . 108.8 no H233 . C23 . H232 . 108.8 no C19 . C24 . C25 . 123.1(3) yes C19 . C24 . H241 . 118.5 no C25 . C24 . H241 . 118.4 no C24 . C25 . C26 . 122.6(3) yes C24 . C25 . S28 . 113.9(3) yes C26 . C25 . S28 . 123.4(3) yes C25 . C26 . C17 . 112.8(3) yes C25 . C26 . O27 . 123.6(3) yes C17 . C26 . O27 . 123.6(3) yes Mn1 . O27 . Mn3 . 88.57(9) yes Mn1 . O27 . C26 . 135.4(2) yes Mn3 . O27 . C26 . 135.4(2) yes C25 . S28 . O29 . 110.44(16) yes C25 . S28 . O30 . 107.64(16) yes O29 . S28 . O30 . 115.97(16) yes C25 . S28 . C31 . 104.72(17) yes O29 . S28 . C31 . 109.84(16) yes O30 . S28 . C31 . 107.60(17) yes Mn1 . O29 . S28 . 124.97(15) yes S28 . C31 . C32 . 122.9(3) yes S28 . C31 . C48 . 114.1(3) yes C32 . C31 . C48 . 122.8(3) yes C31 . C32 . O33 . 123.6(3) yes C31 . C32 . C34 . 112.4(3) yes O33 . C32 . C34 . 124.0(3) yes Mn3 2_666 O33 . Mn1 . 88.34(9) yes Mn3 2_666 O33 . C32 . 136.0(2) yes Mn1 . O33 . C32 . 135.6(2) yes C32 . C34 . S35 . 122.9(3) yes C32 . C34 . C46 . 123.5(3) yes S35 . C34 . C46 . 113.3(3) yes C36 2_666 S35 . C34 . 104.98(17) yes C36 2_666 S35 . O44 2_666 108.83(17) yes C34 . S35 . O44 2_666 110.02(16) yes C36 2_666 S35 . O45 . 108.58(17) yes C34 . S35 . O45 . 108.00(17) yes O44 2_666 S35 . O45 . 115.87(16) yes S35 2_666 C36 . C5 . 122.9(3) yes S35 2_666 C36 . C37 . 113.5(3) yes C5 . C36 . C37 . 123.4(3) yes C36 . C37 . C38 . 122.3(4) yes C36 . C37 . H371 . 118.2 no C38 . C37 . H371 . 119.5 no C37 . C38 . C39 . 116.0(3) yes C37 . C38 . C40 . 120.5(4) yes C39 . C38 . C40 . 123.5(4) yes C6 . C39 . C38 . 122.3(4) yes C6 . C39 . H391 . 118.6 no C38 . C39 . H391 . 119.1 no C38 . C40 . C41 . 109.0(3) yes C38 . C40 . C42 . 111.8(4) yes C41 . C40 . C42 . 109.0(4) yes C38 . C40 . C43 . 108.5(3) yes C41 . C40 . C43 . 110.3(4) yes C42 . C40 . C43 . 108.2(4) yes C40 . C41 . H411 . 110.1 no C40 . C41 . H412 . 110.3 no H411 . C41 . H412 . 109.2 no C40 . C41 . H413 . 109.9 no H411 . C41 . H413 . 108.4 no H412 . C41 . H413 . 109.0 no C40 . C42 . H421 . 108.6 no C40 . C42 . H422 . 110.0 no H421 . C42 . H422 . 109.3 no C40 . C42 . H423 . 110.1 no H421 . C42 . H423 . 108.8 no H422 . C42 . H423 . 110.0 no C40 . C43 . H431 . 109.0 no C40 . C43 . H432 . 109.1 no H431 . C43 . H432 . 109.3 no C40 . C43 . H433 . 110.2 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 109.7 no Mn3 . O44 . S35 2_666 125.62(15) yes C34 . C46 . C47 . 122.6(3) yes C34 . C46 . H461 . 117.5 no C47 . C46 . H461 . 119.8 no C46 . C47 . C48 . 115.3(3) yes C46 . C47 . C49 . 123.7(3) yes C48 . C47 . C49 . 120.9(3) yes C47 . C48 . C31 . 123.3(3) yes C47 . C48 . H481 . 118.8 no C31 . C48 . H481 . 117.8 no C47 . C49 . C50 . 110.3(3) yes C47 . C49 . C51 . 112.2(3) yes C50 . C49 . C51 . 108.3(4) yes C47 . C49 . C52 . 108.0(3) yes C50 . C49 . C52 . 108.6(4) yes C51 . C49 . C52 . 109.5(4) yes C49 . C50 . H501 . 109.0 no C49 . C50 . H503 . 109.7 no H501 . C50 . H503 . 109.6 no C49 . C50 . H502 . 109.8 no H501 . C50 . H502 . 109.2 no H503 . C50 . H502 . 109.5 no C49 . C51 . H511 . 109.5 no C49 . C51 . H512 . 107.9 no H511 . C51 . H512 . 109.1 no C49 . C51 . H513 . 109.8 no H511 . C51 . H513 . 109.4 no H512 . C51 . H513 . 111.1 no C49 . C52 . H521 . 109.2 no C49 . C52 . H522 . 108.1 no H521 . C52 . H522 . 109.4 no C49 . C52 . H523 . 109.7 no H521 . C52 . H523 . 110.0 no H522 . C52 . H523 . 110.3 no C13 . C53 . C54 . 122.6(3) yes C13 . C53 . H531 . 117.8 no C54 . C53 . H531 . 119.6 no C53 . C54 . C55 . 116.0(3) yes C53 . C54 . C56 . 120.2(3) yes C55 . C54 . C56 . 123.8(3) yes C10 . C55 . C54 . 122.2(3) yes C10 . C55 . H551 . 119.2 no C54 . C55 . H551 . 118.6 no C54 . C56 . C57 . 111.8(3) yes C54 . C56 . C58 . 108.9(3) yes C57 . C56 . C58 . 109.1(3) yes C54 . C56 . C59 . 109.0(3) yes C57 . C56 . C59 . 108.6(3) yes C58 . C56 . C59 . 109.4(3) yes C56 . C57 . H571 . 109.5 no C56 . C57 . H573 . 110.7 no H571 . C57 . H573 . 109.0 no C56 . C57 . H572 . 110.2 no H571 . C57 . H572 . 108.3 no H573 . C57 . H572 . 109.2 no C56 . C58 . H581 . 108.8 no C56 . C58 . H583 . 109.5 no H581 . C58 . H583 . 109.0 no C56 . C58 . H582 . 109.8 no H581 . C58 . H582 . 109.9 no H583 . C58 . H582 . 109.9 no C56 . C59 . H591 . 109.7 no C56 . C59 . H592 . 109.4 no H591 . C59 . H592 . 109.1 no C56 . C59 . H593 . 110.6 no H591 . C59 . H593 . 109.1 no H592 . C59 . H593 . 109.0 no O64 2_766 K60 . O64 . 179.996 yes O62 . C61 . H611 . 102.5 no O62 . C61 . H612 . 122.9 no H611 . C61 . H612 . 109.5 no O62 . C61 . H613 . 102.2 no H611 . C61 . H613 . 109.5 no H612 . C61 . H613 . 109.5 no C61 . O62 . H621 . 102.1 no O64 . C63 . H631 . 110.1 no O64 . C63 . H633 . 110.0 no H631 . C63 . H633 . 109.8 no O64 . C63 . H632 . 108.4 no H631 . C63 . H632 . 109.1 no H633 . C63 . H632 . 109.4 no C63 . O64 . K60 . 120.5(3) yes C63 . O64 . H641 . 109.3 no K60 . O64 . H641 . 130.1 no O66 . C65 . H651 . 108.7 no O66 . C65 . H652 . 109.0 no H651 . C65 . H652 . 109.3 no O66 . C65 . H653 . 111.0 no H651 . C65 . H653 . 109.4 no H652 . C65 . H653 . 109.4 no C65 . O66 . H661 . 108.1 no 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 O64 . H641 . O30 1_565 140.78(10) 0.821 2.499 3.178(7) yes O64 . H641 . O45 2_666 120.79(10) 0.821 2.546 3.049(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 20/09/11 at 10:46:23 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) H ( 213,X'S) RIDE C ( 22,X'S) H ( 222,X'S) H ( 221,X'S) H ( 223,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 233,X'S) H ( 232,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S) RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S) RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 503,X'S) H ( 502,X'S) RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) H ( 513,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) H ( 523,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 573,X'S) H ( 572,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 583,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) H ( 593,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) H ( 613,X'S) RIDE O ( 62,X'S) H ( 621,X'S) RIDE C ( 63,X'S) H ( 631,X'S) H ( 633,X'S) H ( 632,X'S) RIDE O ( 64,X'S) H ( 641,X'S) RIDE C ( 65,X'S) H ( 651,X'S) H ( 652,X'S) H ( 653,X'S) RIDE O ( 66,X'S) H ( 661,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 20/09/11 at 10:46:23 # #LIST 16 NO U(IJ)'S 0.0, 0.010000 = C(61) TO O(62) DISTANCE 1.550000 , 0.010000 = C(61) TO O(62) DISTANCE 1.550000 , 0.010000 = C(65) TO O(66) DISTANCE 1.550000 , 0.010000 = C(63) TO O(64) END ; data_KOH _database_code_depnum_ccdc_archive 'CCDC 835636' #TrackingRef '- KF_KOH_combined.cif' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 12.2087(4) _cell_length_b 18.8106(5) _cell_length_c 22.2153(7) _cell_angle_alpha 90 _cell_angle_beta 105.222(3) _cell_angle_gamma 90 _cell_volume 4922.8(3) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c ' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x,-y,z+1/2 -x,y,-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' 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 '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 = C59.33 K4 Mn2.67 O10.67 S2 # Dc = 1.27 Fooo = 2231.10 Mu = 8.74 M = 937.73 # Found Formula = C57.02 H74.08 K0.67 Mn2.67 O20.35 S5.33 # Dc = 1.45 FOOO = 2231.10 Mu = 7.89 M = 1071.56 _chemical_formula_sum 'C85.53 H111.12 K Mn4 O30.53 S8' _chemical_formula_moiety ; C82 H97 K Mn4 O27 S8, C0.61 H2.46 O0.61, 2.92(C H4 O) ; _chemical_compound_source ? _chemical_formula_weight 2143.13 _cell_measurement_reflns_used 67367 _cell_measurement_theta_min 3.3770 _cell_measurement_theta_max 29.9878 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.134 _exptl_crystal_size_mid 0.239 _exptl_crystal_size_max 0.261 _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2231.6 _exptl_absorpt_coefficient_mu 0.789 # Sheldrick geometric approximatio 0.83 0.90 _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.4685 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 100 _diffrn_reflns_number 263202 _reflns_number_total 13520 _diffrn_reflns_av_R_equivalents 0.059 # Number of reflections without Friedels Law is 26095 # Number of reflections with Friedels Law is 13520 # Theoretical number of reflections is about 14444 _diffrn_reflns_theta_min 3.385 _diffrn_reflns_theta_max 30.065 _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 26.758 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _oxford_diffrn_Wilson_B_factor 1.46 _oxford_diffrn_Wilson_scale 0.17 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.31 _refine_diff_density_max 1.49 # 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 13519 _refine_ls_number_restraints 556 _refine_ls_number_parameters 714 _oxford_refine_ls_R_factor_ref 0.0757 _refine_ls_wR_factor_ref 0.1197 _refine_ls_goodness_of_fit_ref 1.0487 _refine_ls_shift/su_max 0.0148131 _refine_ls_shift/su_mean 0.0000689 # The values computed from all data _oxford_reflns_number_all 13519 _refine_ls_R_factor_all 0.0757 _refine_ls_wR_factor_all 0.1197 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11032 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_gt 0.1016 # 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: 0.140E+04 0.211E+04 0.111E+04 270. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Oxford Diffraction, (2010). CrysAlisPro. Oxford Diffraction, (2006). Gemini User Manual. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 0.00121(4) 0.24963(2) 0.34814(2) 0.0139 1.0000 Uani . . . . . . O2 O -0.00194(18) 0.18231(11) 0.42561(9) 0.0177 1.0000 Uani . . . . . . S3 S 0.00181(6) 0.10531(4) 0.42670(3) 0.0153 1.0000 Uani . . . . . . O4 O -0.00805(19) 0.07265(11) 0.48326(10) 0.0198 1.0000 Uani . . . . . . C5 C -0.1066(2) 0.07046(15) 0.36468(13) 0.0184 1.0000 Uani . . . . . . C6 C -0.1658(2) 0.11124(15) 0.31170(13) 0.0158 1.0000 Uani . . . . . . O7 O -0.14541(18) 0.17821(11) 0.30428(10) 0.0199 1.0000 Uani . . . . . . Mn8 Mn -0.18651(4) 0.25016(2) 0.22322(2) 0.0148 1.0000 Uani . . . . . . O9 O -0.15086(18) 0.32040(10) 0.15058(10) 0.0170 1.0000 Uani . . . . . . C10 C -0.1628(2) 0.38931(15) 0.14228(12) 0.0143 1.0000 Uani . . . . . . C11 C -0.0998(2) 0.42998(15) 0.10888(13) 0.0172 1.0000 Uani . . . . . . S12 S 0.00070(6) 0.39380(4) 0.07318(3) 0.0156 1.0000 Uani . . . . . . O13 O -0.00613(19) 0.31693(11) 0.07264(10) 0.0187 1.0000 Uani . . . . . . O14 O -0.0149(2) 0.42724(12) 0.01328(10) 0.0216 1.0000 Uani . . . . . . C15 C 0.1322(2) 0.42159(15) 0.12134(14) 0.0171 1.0000 Uani . . . . . . C16 C 0.1767(2) 0.38847(15) 0.18020(14) 0.0172 1.0000 Uani . . . . . . O17 O 0.13200(17) 0.33280(11) 0.19896(10) 0.0170 1.0000 Uani . . . . . . C18 C 0.2747(2) 0.42308(15) 0.21669(14) 0.0182 1.0000 Uani . . . . . . S19 S 0.33455(6) 0.39738(4) 0.29418(3) 0.0171 1.0000 Uani . . . . . . C20 C 0.2406(2) 0.43096(16) 0.33537(14) 0.0192 1.0000 Uani . . . . . . C21 C 0.2525(4) 0.5038(4) 0.3455(3) 0.0216 0.6009 Uani . U . 1 1 . C22 C 0.2413(6) 0.5064(5) 0.3374(5) 0.0281 0.3991 Uani . U . 1 2 . C23 C 0.1881(5) 0.5427(4) 0.3766(3) 0.0218 0.6009 Uani . U . 1 1 . C24 C 0.1705(7) 0.5433(6) 0.3645(5) 0.0284 0.3991 Uani . U . 1 2 . C25 C 0.1101(4) 0.5049(4) 0.3980(4) 0.0215 0.6009 Uani . U . 1 1 . C26 C 0.1081(6) 0.5015(6) 0.3973(6) 0.0280 0.3991 Uani . U . 1 2 . H251 H 0.0707 0.5263 0.4234 0.0177 0.6009 Uiso R . . 1 1 . H261 H 0.0584 0.5260 0.4149 0.0170 0.3991 Uiso R . . 1 2 . C27 C 0.2064(5) 0.6220(3) 0.3881(3) 0.0350 0.6009 Uani . U . 1 1 . C28 C 0.1626(7) 0.6263(5) 0.3620(4) 0.0283 0.3991 Uani . U . 1 2 . C29 C 0.1389(5) 0.6543(4) 0.4222(4) 0.0548 0.3991 Uani . . . 1 2 . C30 C 0.1030(4) 0.6583(4) 0.4003(4) 0.0622 0.6009 Uani . . . 1 1 . H302 H 0.1132 0.7088 0.4019 0.0869 0.6009 Uiso R . . 1 1 . H291 H 0.1203 0.7039 0.4171 0.0830 0.3991 Uiso R . . 1 2 . H301 H 0.0901 0.6421 0.4388 0.0870 0.6009 Uiso R . . 1 1 . H293 H 0.0761 0.6288 0.4304 0.0830 0.3991 Uiso R . . 1 2 . H303 H 0.0372 0.6474 0.3672 0.0870 0.6009 Uiso R . . 1 1 . H292 H 0.2061 0.6479 0.4564 0.0831 0.3991 Uiso R . . 1 2 . C31 C 0.2690(4) 0.6590(4) 0.3558(4) 0.0354 0.3991 Uani . U . 1 2 . C32 C 0.2247(4) 0.6583(3) 0.3290(3) 0.0544 0.6009 Uani . . . 1 1 . H322 H 0.2303 0.7088 0.3360 0.0908 0.6009 Uiso R . . 1 1 . H313 H 0.2782 0.7052 0.3751 0.0818 0.3991 Uiso R . . 1 2 . H323 H 0.2934 0.6419 0.3204 0.0910 0.6009 Uiso R . . 1 1 . H312 H 0.2652 0.6636 0.3121 0.0821 0.3991 Uiso R . . 1 2 . H321 H 0.1618 0.6489 0.2936 0.0907 0.6009 Uiso R . . 1 1 . H311 H 0.3330 0.6303 0.3759 0.0821 0.3991 Uiso R . . 1 2 . C33 C 0.3133(4) 0.6336(3) 0.4417(4) 0.0816 0.6009 Uani . . . 1 1 . H332 H 0.3345 0.6831 0.4417 0.1100 0.6009 Uiso R . . 1 1 . H331 H 0.2941 0.6224 0.4800 0.1099 0.6009 Uiso R . . 1 1 . H333 H 0.3747 0.6038 0.4371 0.1099 0.6009 Uiso R . . 1 1 . C34 C 0.0631(5) 0.6466(4) 0.3062(4) 0.0951 0.3991 Uani . . . 1 2 . H343 H 0.0425 0.6956 0.3094 0.1320 0.3991 Uiso R . . 1 2 . H341 H -0.0004 0.6162 0.3054 0.1320 0.3991 Uiso R . . 1 2 . H342 H 0.0880 0.6397 0.2691 0.1320 0.3991 Uiso R . . 1 2 . H211 H 0.3098 0.5280 0.3325 0.0258 0.6009 Uiso R . . 1 1 . H221 H 0.2903 0.5305 0.3185 0.0251 0.3991 Uiso R . . 1 2 . O35 O 0.33773(17) 0.31996(11) 0.29758(10) 0.0182 1.0000 Uani . . . . . . O36 O 0.44187(18) 0.43262(12) 0.31674(11) 0.0226 1.0000 Uani . . . . . . C37 C 0.3236(2) 0.48292(15) 0.19665(15) 0.0201 1.0000 Uani . . . . . . C38 C 0.2778(2) 0.51320(16) 0.13836(15) 0.0214 1.0000 Uani . . . . . . C39 C 0.1802(2) 0.48093(16) 0.10115(15) 0.0213 1.0000 Uani . . . . . . H391 H 0.1475 0.4988 0.0632 0.0257 1.0000 Uiso R . . . . . C40 C 0.3253(3) 0.57997(17) 0.11527(17) 0.0278 1.0000 Uani . . . . . . C41 C 0.3529(3) 0.5640(2) 0.05334(19) 0.0450 1.0000 Uani . . . . . . H413 H 0.3848 0.6054 0.0403 0.0686 1.0000 Uiso R . . . . . H411 H 0.2858 0.5520 0.0227 0.0676 1.0000 Uiso R . . . . . H412 H 0.4075 0.5260 0.0585 0.0678 1.0000 Uiso R . . . . . C42 C 0.2364(3) 0.63979(17) 0.1065(2) 0.0384 1.0000 Uani . . . . . . H422 H 0.2642 0.6819 0.0897 0.0576 1.0000 Uiso R . . . . . H423 H 0.1669 0.6244 0.0778 0.0581 1.0000 Uiso R . . . . . H421 H 0.2227 0.6504 0.1465 0.0577 1.0000 Uiso R . . . . . C43 C 0.4333(3) 0.60585(19) 0.1618(2) 0.0388 1.0000 Uani . . . . . . H431 H 0.4631 0.6470 0.1442 0.0581 1.0000 Uiso R . . . . . H432 H 0.4910 0.5684 0.1700 0.0580 1.0000 Uiso R . . . . . H433 H 0.4186 0.6200 0.2015 0.0577 1.0000 Uiso R . . . . . H371 H 0.3887 0.5028 0.2234 0.0251 1.0000 Uiso R . . . . . O44 O -0.13343(17) 0.16887(11) 0.16146(9) 0.0171 1.0000 Uani . . . . . . C45 C -0.1763(2) 0.11125(15) 0.13159(13) 0.0162 1.0000 Uani . . . . . . C46 C -0.1301(2) 0.07629(15) 0.08715(13) 0.0177 1.0000 Uani . . . . . . C47 C -0.1775(3) 0.01539(16) 0.05509(14) 0.0206 1.0000 Uani . . . . . . C48 C -0.2753(3) -0.01586(16) 0.06380(15) 0.0228 1.0000 Uani . . . . . . C49 C -0.3224(2) 0.01608(16) 0.10756(14) 0.0207 1.0000 Uani . . . . . . C50 C -0.2753(2) 0.07727(15) 0.14038(13) 0.0182 1.0000 Uani . . . . . . S51 S -0.33803(6) 0.10486(4) 0.19877(3) 0.0162 1.0000 Uani . . . . . . O52 O -0.33725(17) 0.18238(11) 0.20187(10) 0.0174 1.0000 Uani . . . . . . C53 C -0.2506(3) 0.07080(15) 0.26874(14) 0.0189 1.0000 Uani . . . . . . C54 C -0.2707(3) -0.00097(17) 0.27743(15) 0.0267 1.0000 Uani . . . . . . C55 C -0.2093(3) -0.03919(18) 0.32888(16) 0.0300 1.0000 Uani . . . . . . C56 C -0.1280(3) -0.00138(16) 0.37232(15) 0.0253 1.0000 Uani . . . . . . H561 H -0.0873 -0.0255 0.4073 0.0307 1.0000 Uiso R . . . . . C57 C -0.2323(4) -0.11789(19) 0.3378(2) 0.0457 1.0000 Uani . . . . . . C58 C -0.3086(4) -0.1527(3) 0.2827(3) 0.0723 0.6512 Uani . . . 2 1 . C59 C -0.2382(5) -0.1559(4) 0.2723(4) 0.0888 0.3488 Uani . . . 2 2 . H583 H -0.2821 -0.1444 0.2463 0.1110 0.6512 Uiso R . . 2 1 . H591 H -0.2917 -0.1311 0.2397 0.1250 0.3488 Uiso R . . 2 2 . H592 H -0.2618 -0.2048 0.2736 0.1250 0.3488 Uiso R . . 2 2 . H593 H -0.1639 -0.1540 0.2649 0.1250 0.3488 Uiso R . . 2 2 . H582 H -0.3120 -0.2033 0.2887 0.1109 0.6512 Uiso R . . 2 1 . H581 H -0.3845 -0.1340 0.2746 0.1110 0.6512 Uiso R . . 2 1 . C60 C -0.1185(4) -0.1593(3) 0.3562(4) 0.0659 0.6512 Uani . . . 2 1 . C61 C -0.1485(5) -0.1527(4) 0.3839(4) 0.0770 0.3488 Uani . . . 2 2 . H601 H -0.1327 -0.2082 0.3646 0.0990 0.6512 Uiso R . . 2 1 . H611 H -0.1651 -0.2028 0.3824 0.1150 0.3488 Uiso R . . 2 2 . H602 H -0.0703 -0.1379 0.3930 0.0990 0.6512 Uiso R . . 2 1 . H613 H -0.0750 -0.1451 0.3772 0.1150 0.3488 Uiso R . . 2 2 . H612 H -0.1495 -0.1342 0.4243 0.1150 0.3488 Uiso R . . 2 2 . H603 H -0.0824 -0.1572 0.3221 0.0990 0.6512 Uiso R . . 2 1 . C62 C -0.2828(4) -0.1232(3) 0.3955(3) 0.0702 0.6512 Uani . . . 2 1 . C63 C -0.3530(5) -0.1240(4) 0.3481(4) 0.0856 0.3488 Uani . . . 2 2 . H621 H -0.3563 -0.1004 0.3871 0.1090 0.6512 Uiso R . . 2 1 . H631 H -0.3656 -0.0861 0.3744 0.1170 0.3488 Uiso R . . 2 2 . H632 H -0.3611 -0.1686 0.3678 0.1170 0.3488 Uiso R . . 2 2 . H633 H -0.4101 -0.1210 0.3088 0.1170 0.3488 Uiso R . . 2 2 . H622 H -0.2913 -0.1724 0.4053 0.1089 0.6512 Uiso R . . 2 1 . H623 H -0.2312 -0.1009 0.4309 0.1090 0.6512 Uiso R . . 2 1 . H541 H -0.3266 -0.0256 0.2473 0.0325 1.0000 Uiso R . . . . . O64 O -0.44746(18) 0.07183(12) 0.18761(10) 0.0218 1.0000 Uani . . . . . . H491 H -0.3878 -0.0025 0.1150 0.0266 1.0000 Uiso R . . . . . C65 C -0.3223(3) -0.08436(18) 0.02915(17) 0.0286 1.0000 Uani . . . . . . C66 C -0.3420(3) -0.07365(19) -0.04126(17) 0.0360 1.0000 Uani . . . . . . H661 H -0.3697 -0.1177 -0.0636 0.0547 1.0000 Uiso R . . . . . H662 H -0.3965 -0.0367 -0.0553 0.0556 1.0000 Uiso R . . . . . H663 H -0.2715 -0.0587 -0.0508 0.0545 1.0000 Uiso R . . . . . C67 C -0.2342(3) -0.14388(18) 0.05085(19) 0.0390 1.0000 Uani . . . . . . H672 H -0.2604 -0.1875 0.0295 0.0589 1.0000 Uiso R . . . . . H673 H -0.1621 -0.1304 0.0435 0.0594 1.0000 Uiso R . . . . . H671 H -0.2243 -0.1516 0.0954 0.0585 1.0000 Uiso R . . . . . C68 C -0.4339(3) -0.1074(2) 0.0419(2) 0.0459 1.0000 Uani . . . . . . H682 H -0.4609 -0.1512 0.0196 0.0689 1.0000 Uiso R . . . . . H683 H -0.4918 -0.0720 0.0279 0.0691 1.0000 Uiso R . . . . . H681 H -0.4245 -0.1147 0.0858 0.0686 1.0000 Uiso R . . . . . H471 H -0.1413 -0.0044 0.0272 0.0257 1.0000 Uiso R . . . . . O69 O 0.000000(7) 0.2539(2) 0.250000(7) 0.0270 1.0000 Uani S T . . . . H691 H 0.0000 0.2109 0.2500 0.0406 1.0000 Uiso RS . . . . . K70 K -0.5000 0.24436(7) 0.2500 0.0506 1.0000 Uani S T . . . . O71 O -0.3433(5) 0.2455(4) 0.3417(3) 0.0567 0.5000 Uani . . . 3 1 . O72 O -0.4055(6) 0.2502(4) 0.3781(3) 0.0773 0.5000 Uani . . . 3 2 . C73 C -0.3396(4) 0.2866(4) 0.3984(4) 0.0575 0.5000 Uani . . . 3 1 . C74 C -0.2789(5) 0.2589(4) 0.4044(4) 0.0863 0.5000 Uani . . . 3 2 . H743 H -0.2536 0.2982 0.3838 0.1220 0.5000 Uiso R . . 3 2 . H731 H -0.2618 0.2945 0.4209 0.0800 0.5000 Uiso R . . 3 1 . H741 H -0.2432 0.2157 0.3966 0.1223 0.5000 Uiso R . . 3 2 . H742 H -0.2605 0.2683 0.4485 0.1220 0.5000 Uiso R . . 3 2 . H733 H -0.3761 0.2621 0.4258 0.0801 0.5000 Uiso R . . 3 1 . H732 H -0.3740 0.3322 0.3890 0.0798 0.5000 Uiso R . . 3 1 . O75 O 0.6375(5) 0.2739(3) 0.0554(3) 0.1807 0.9150 Uani D U . . . . C76 C 0.6846(4) 0.2322(4) 0.0139(3) 0.1800 0.9150 Uani D U . . . . O77 O 0.000000(10) 0.9730(6) 0.250000(10) 0.1459 0.6140 Uani DS TU . . . . C78 C -0.0759(5) 0.9212(5) 0.2049(5) 0.1457 0.3070 Uani D U . . . . O79 O 0.4574(6) 0.3109(4) 0.0308(4) 0.1277 0.5433 Uani D U . . . . C80 C 0.4439(5) 0.3907(4) 0.0359(4) 0.1278 0.5433 Uani D U . . . . H711 H -0.2880 0.2212 0.3409 0.0751 0.5000 Uiso R . . 3 1 . H721 H -0.4460 0.2477 0.4022 0.1036 0.5000 Uiso R . . 3 2 . H791 H 0.4406 0.2917 0.0603 0.1588 0.5433 Uiso R . . . . . H751 H 0.6963 0.2858 0.0808 0.1762 0.9150 Uiso R . . . . . H781 H -0.1297 0.9459 0.1730 0.2146 0.3070 Uiso R . . . . . H782 H -0.1146 0.8922 0.2277 0.2146 0.3070 Uiso R . . . . . H783 H -0.0296 0.8922 0.1865 0.2146 0.3070 Uiso R . . . . . H801 H 0.4631 0.4137 0.0020 0.1632 0.5433 Uiso R . . . . . H802 H 0.4923 0.4072 0.0741 0.1632 0.5433 Uiso R . . . . . H803 H 0.3672 0.4010 0.0348 0.1632 0.5433 Uiso R . . . . . H761 H 0.6262 0.2139 -0.0197 0.2226 0.9150 Uiso R . . . . . H762 H 0.7321 0.2629 -0.0021 0.2226 0.9150 Uiso R . . . . . H763 H 0.7284 0.1941 0.0358 0.2226 0.9150 Uiso R . . . . . H771 H -0.0279 0.9812 0.2792 0.2239 0.3070 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 0.0162(2) 0.01235(19) 0.01296(19) -0.00011(14) 0.00318(15) -0.00028(14) O2 0.0250(10) 0.0137(9) 0.0148(9) -0.0005(7) 0.0060(8) -0.0005(8) S3 0.0194(3) 0.0124(3) 0.0138(3) 0.0010(2) 0.0039(2) -0.0007(2) O4 0.0267(11) 0.0179(10) 0.0157(10) 0.0029(8) 0.0071(8) -0.0014(8) C5 0.0228(14) 0.0145(12) 0.0169(13) 0.0015(10) 0.0035(11) -0.0038(10) C6 0.0169(12) 0.0159(12) 0.0157(12) 0.0007(10) 0.0063(10) -0.0016(10) O7 0.0246(11) 0.0140(9) 0.0186(10) 0.0038(8) 0.0011(8) -0.0043(8) Mn8 0.0153(2) 0.0138(2) 0.0149(2) 0.00062(15) 0.00312(15) -0.00020(15) O9 0.0216(10) 0.0116(9) 0.0188(10) 0.0012(7) 0.0070(8) 0.0013(7) C10 0.0153(12) 0.0150(12) 0.0119(11) 0.0010(9) 0.0021(9) -0.0002(9) C11 0.0188(13) 0.0143(12) 0.0180(13) 0.0016(10) 0.0039(10) -0.0003(10) S12 0.0203(3) 0.0126(3) 0.0143(3) 0.0013(2) 0.0051(2) 0.0000(2) O13 0.0268(11) 0.0138(9) 0.0162(9) 0.0005(7) 0.0066(8) 0.0006(8) O14 0.0324(12) 0.0186(10) 0.0147(10) 0.0030(8) 0.0079(9) -0.0006(9) C15 0.0180(13) 0.0144(12) 0.0200(13) -0.0006(10) 0.0069(11) -0.0002(10) C16 0.0186(13) 0.0149(12) 0.0192(13) -0.0006(10) 0.0073(10) 0.0011(10) O17 0.0192(10) 0.0128(9) 0.0193(10) 0.0006(7) 0.0055(8) -0.0030(7) C18 0.0181(13) 0.0148(12) 0.0227(14) 0.0016(10) 0.0072(11) 0.0010(10) S19 0.0153(3) 0.0146(3) 0.0212(3) -0.0008(2) 0.0046(3) -0.0006(2) C20 0.0181(13) 0.0169(13) 0.0225(14) -0.0043(11) 0.0054(11) -0.0029(10) C21 0.022(2) 0.013(2) 0.033(2) -0.0068(17) 0.0128(17) -0.0032(16) C22 0.033(3) 0.017(3) 0.037(3) 0.004(3) 0.015(3) -0.001(3) C23 0.0229(19) 0.013(2) 0.033(2) -0.0069(16) 0.0124(16) -0.0027(16) C24 0.034(3) 0.017(3) 0.037(3) 0.004(3) 0.015(3) -0.001(3) C25 0.023(2) 0.012(2) 0.032(2) -0.0072(17) 0.0126(17) -0.0021(17) C26 0.033(3) 0.017(3) 0.037(3) 0.004(3) 0.015(3) -0.001(3) C27 0.042(3) 0.015(2) 0.057(4) -0.006(2) 0.028(3) -0.004(2) C28 0.033(3) 0.017(3) 0.037(3) 0.004(2) 0.015(3) -0.001(2) C29 0.082(10) 0.016(6) 0.083(11) -0.016(6) 0.053(9) 0.003(6) C30 0.077(6) 0.014(3) 0.123(10) 0.007(5) 0.076(7) 0.004(4) C31 0.042(3) 0.015(2) 0.058(4) -0.006(3) 0.029(3) -0.004(2) C32 0.087(7) 0.024(3) 0.063(6) 0.003(4) 0.039(5) -0.002(4) C33 0.077(7) 0.030(4) 0.112(9) -0.035(5) -0.021(6) -0.013(4) C34 0.108(13) 0.025(6) 0.111(14) 0.003(7) -0.044(11) 0.020(7) O35 0.0162(9) 0.0155(9) 0.0236(10) -0.0006(8) 0.0065(8) 0.0013(7) O36 0.0166(10) 0.0219(11) 0.0282(11) -0.0016(9) 0.0039(9) -0.0024(8) C37 0.0181(13) 0.0132(12) 0.0300(16) 0.0018(11) 0.0080(12) -0.0008(10) C38 0.0191(13) 0.0155(13) 0.0295(16) 0.0035(11) 0.0064(12) 0.0022(11) C39 0.0235(14) 0.0168(13) 0.0250(15) 0.0044(11) 0.0089(12) 0.0012(11) C40 0.0243(15) 0.0187(14) 0.0389(19) 0.0079(13) 0.0057(14) -0.0033(12) C41 0.052(3) 0.039(2) 0.050(3) 0.0105(19) 0.023(2) -0.0118(19) C42 0.0294(18) 0.0155(15) 0.062(3) 0.0096(16) -0.0018(17) -0.0011(13) C43 0.0258(17) 0.0271(18) 0.057(3) 0.0189(17) -0.0010(16) -0.0080(14) O44 0.0190(10) 0.0145(9) 0.0176(9) -0.0038(7) 0.0048(8) -0.0044(7) C45 0.0172(12) 0.0128(12) 0.0169(12) 0.0011(10) 0.0014(10) 0.0016(10) C46 0.0191(13) 0.0165(13) 0.0164(13) -0.0020(10) 0.0026(10) -0.0001(10) C47 0.0260(15) 0.0167(13) 0.0184(13) -0.0036(11) 0.0043(11) 0.0005(11) C48 0.0284(15) 0.0165(13) 0.0227(14) -0.0036(11) 0.0052(12) -0.0015(11) C49 0.0229(14) 0.0170(13) 0.0212(14) -0.0031(11) 0.0038(11) -0.0026(11) C50 0.0216(14) 0.0142(12) 0.0176(13) -0.0017(10) 0.0031(11) -0.0015(10) S51 0.0166(3) 0.0148(3) 0.0167(3) -0.0008(2) 0.0034(2) -0.0018(2) O52 0.0162(9) 0.0140(9) 0.0216(10) -0.0003(8) 0.0041(8) 0.0012(7) C53 0.0235(14) 0.0148(13) 0.0177(13) 0.0005(10) 0.0044(11) -0.0008(11) C54 0.0361(18) 0.0181(14) 0.0231(15) 0.0003(12) 0.0026(13) -0.0083(13) C55 0.0392(19) 0.0163(14) 0.0285(17) 0.0018(12) -0.0016(14) -0.0081(13) C56 0.0344(17) 0.0153(13) 0.0231(15) 0.0032(11) 0.0021(13) -0.0031(12) C57 0.064(3) 0.0165(16) 0.043(2) 0.0059(15) -0.010(2) -0.0169(17) C58 0.101(8) 0.025(4) 0.060(6) 0.007(3) -0.034(5) -0.030(4) C59 0.17(3) 0.022(7) 0.056(10) 0.005(6) -0.007(14) -0.017(11) C60 0.063(5) 0.018(3) 0.101(9) -0.003(4) -0.006(6) 0.001(3) C61 0.098(16) 0.020(7) 0.079(14) 0.011(8) -0.036(12) -0.017(8) C62 0.106(8) 0.031(4) 0.078(6) 0.007(4) 0.032(6) -0.034(4) C63 0.109(16) 0.048(9) 0.088(14) 0.020(9) 0.005(12) -0.044(10) O64 0.0176(10) 0.0241(11) 0.0227(11) -0.0010(9) 0.0038(8) -0.0047(8) C65 0.0311(17) 0.0221(15) 0.0324(17) -0.0116(13) 0.0077(14) -0.0063(13) C66 0.041(2) 0.0295(18) 0.0327(19) -0.0133(15) 0.0012(16) -0.0048(15) C67 0.052(2) 0.0175(16) 0.043(2) -0.0046(15) 0.0039(18) 0.0000(15) C68 0.044(2) 0.033(2) 0.066(3) -0.025(2) 0.024(2) -0.0205(18) O69 0.0139(14) 0.051(2) 0.0156(14) 0.0000 0.0029(11) 0.0000 K70 0.0532(8) 0.0292(6) 0.0905(11) 0.0000 0.0565(8) 0.0000 O71 0.056(4) 0.058(4) 0.057(4) -0.010(4) 0.018(4) 0.004(3) O72 0.118(8) 0.043(4) 0.051(5) -0.004(4) -0.012(5) 0.022(5) C73 0.065(7) 0.044(6) 0.068(8) 0.024(5) 0.025(6) 0.016(5) C74 0.136(14) 0.083(10) 0.038(6) 0.008(6) 0.020(7) -0.060(10) O75 0.263(9) 0.072(4) 0.115(5) 0.006(3) -0.114(6) -0.018(5) C76 0.262(9) 0.071(4) 0.114(5) 0.007(3) -0.114(6) -0.019(5) O77 0.131(13) 0.191(19) 0.120(13) 0.0000 0.039(10) 0.0000 C78 0.131(13) 0.191(19) 0.119(13) -0.0001(10) 0.039(10) -0.0001(10) O79 0.147(9) 0.102(7) 0.137(8) -0.026(7) 0.042(7) -0.008(7) C80 0.147(9) 0.102(7) 0.137(8) -0.026(7) 0.042(7) -0.008(7) _refine_ls_extinction_coef 129(8) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 2.432(14) 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 . O9 4_555 2.255(2) yes Mn1 . O13 4_555 2.156(2) yes Mn1 . O44 4_555 2.267(2) yes Mn1 . O17 4_555 2.301(2) yes Mn1 . Mn8 4_555 3.0845(6) yes Mn1 . O2 . 2.145(2) yes Mn1 . O7 . 2.246(2) yes Mn1 . Mn8 . 3.1006(6) yes Mn1 . O69 . 2.1778(5) yes O2 . S3 . 1.449(2) yes S3 . C46 4_555 1.760(3) yes S3 . O4 . 1.432(2) yes S3 . C5 . 1.767(3) yes C5 . C6 . 1.432(4) yes C5 . C56 . 1.395(4) yes C6 . O7 . 1.303(3) yes C6 . C53 . 1.429(4) yes O7 . Mn8 . 2.203(2) yes Mn8 . O35 4_555 2.213(2) yes Mn8 . O17 4_555 2.290(2) yes Mn8 . O9 . 2.215(2) yes Mn8 . O44 . 2.260(2) yes Mn8 . O52 . 2.186(2) yes Mn8 . O69 . 2.1984(5) yes O9 . C10 . 1.312(3) yes C10 . C20 4_555 1.418(4) yes C10 . C11 . 1.423(4) yes C11 . C25 4_555 1.420(7) yes C11 . S12 . 1.764(3) yes C11 . C26 4_555 1.354(11) yes C11 . S12 . 1.764(3) yes S12 . O13 . 1.448(2) yes S12 . O14 . 1.439(2) yes S12 . C15 . 1.759(3) yes C15 . C16 . 1.421(4) yes C15 . C39 . 1.389(4) yes C16 . O17 . 1.299(3) yes C16 . C18 . 1.415(4) yes C18 . S19 . 1.752(3) yes C18 . C37 . 1.400(4) yes S19 . C20 . 1.762(3) yes S19 . O35 . 1.458(2) yes S19 . O36 . 1.436(2) yes C20 . C21 . 1.389(7) yes C20 . C22 . 1.419(11) yes C21 . C23 . 1.384(9) yes C21 . H211 . 0.941 no C22 . C24 . 1.366(14) yes C22 . H221 . 0.934 no C23 . C25 . 1.369(10) yes C23 . C27 . 1.521(8) yes C24 . C26 . 1.422(16) yes C24 . C28 . 1.564(14) yes C25 . H251 . 0.923 no C26 . H261 . 0.925 no C27 . C30 . 1.520(8) yes C27 . C32 . 1.548(10) yes C27 . C33 . 1.534(9) yes C28 . C29 . 1.534(13) yes C28 . C31 . 1.476(10) yes C28 . C34 . 1.537(11) yes C29 . H291 . 0.960 no C29 . H293 . 0.961 no C29 . H292 . 0.968 no C30 . H302 . 0.959 no C30 . H301 . 0.957 no C30 . H303 . 0.958 no C31 . H313 . 0.962 no C31 . H312 . 0.964 no C31 . H311 . 0.959 no C32 . H322 . 0.964 no C32 . H323 . 0.958 no C32 . H321 . 0.961 no C33 . H332 . 0.968 no C33 . H331 . 0.963 no C33 . H333 . 0.963 no C34 . H343 . 0.963 no C34 . H341 . 0.960 no C34 . H342 . 0.959 no C37 . C38 . 1.390(4) yes C37 . H371 . 0.937 no C38 . C39 . 1.398(4) yes C38 . C40 . 1.528(4) yes C39 . H391 . 0.899 no C40 . C41 . 1.529(6) yes C40 . C42 . 1.540(5) yes C40 . C43 . 1.525(5) yes C41 . H413 . 0.948 no C41 . H411 . 0.945 no C41 . H412 . 0.964 no C42 . H422 . 0.973 no C42 . H423 . 0.962 no C42 . H421 . 0.969 no C43 . H431 . 0.978 no C43 . H432 . 0.980 no C43 . H433 . 0.983 no O44 . C45 . 1.307(3) yes C45 . C46 . 1.421(4) yes C45 . C50 . 1.425(4) yes C46 . C47 . 1.392(4) yes C47 . C48 . 1.389(4) yes C47 . H471 . 0.929 no C48 . C49 . 1.389(4) yes C48 . C65 . 1.533(4) yes C49 . C50 . 1.402(4) yes C49 . H491 . 0.925 no C50 . S51 . 1.749(3) yes S51 . O52 . 1.460(2) yes S51 . C53 . 1.759(3) yes S51 . O64 . 1.435(2) yes C53 . C54 . 1.395(4) yes C54 . C55 . 1.391(4) yes C54 . H541 . 0.942 no C55 . C56 . 1.385(4) yes C55 . C57 . 1.529(5) yes C56 . H561 . 0.924 no C57 . C58 . 1.482(7) yes C57 . C60 . 1.551(7) yes C57 . C62 . 1.563(8) yes C57 . C59 . 1.606(11) yes C57 . C61 . 1.405(8) yes C57 . C63 . 1.554(8) yes C58 . H583 . 0.960 no C58 . H582 . 0.964 no C58 . H581 . 0.963 no C59 . H591 . 0.960 no C59 . H592 . 0.966 no C59 . H593 . 0.964 no C60 . H601 . 0.965 no C60 . H602 . 0.961 no C60 . H603 . 0.972 no C61 . H611 . 0.962 no C61 . H613 . 0.960 no C61 . H612 . 0.964 no C62 . H621 . 0.967 no C62 . H622 . 0.964 no C62 . H623 . 0.965 no C63 . H631 . 0.960 no C63 . H632 . 0.964 no C63 . H633 . 0.964 no C65 . C66 . 1.532(5) yes C65 . C67 . 1.539(5) yes C65 . C68 . 1.525(5) yes C66 . H661 . 0.978 no C66 . H662 . 0.955 no C66 . H663 . 0.981 no C67 . H672 . 0.960 no C67 . H673 . 0.970 no C67 . H671 . 0.975 no C68 . H682 . 0.972 no C68 . H683 . 0.961 no C68 . H681 . 0.962 no O69 . H691 . 0.808 no K70 . O71 4_455 2.401(6) yes K70 . O71 . 2.401(6) yes K70 . O72 . 2.778(7) yes O71 . C73 . 1.466(10) yes O71 . H711 . 0.820 no O72 . C74 . 1.511(8) yes O72 . H721 . 0.820 no C73 . H731 . 0.961 no C73 . H733 . 0.962 no C73 . H732 . 0.954 no C74 . H743 . 0.963 no C74 . H741 . 0.960 no C74 . H742 . 0.961 no O75 . C76 . 1.440(9) yes O75 . H751 . 0.820 no C76 . H761 . 0.950 no C76 . H762 . 0.950 no C76 . H763 . 0.950 no O77 . C78 4_555 1.525(9) yes O77 . H771 4_555 0.824 no O77 . C78 . 1.525(9) yes O77 . H771 . 0.824 no C78 . H781 . 0.950 no C78 . H782 . 0.950 no C78 . H783 . 0.950 no O79 . C80 . 1.518(10) yes O79 . H791 . 0.820 no C80 . H801 . 0.950 no C80 . H802 . 0.950 no C80 . H803 . 0.950 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 O9 4_555 Mn1 . O13 4_555 78.12(8) yes O9 4_555 Mn1 . O44 4_555 78.59(7) yes O13 4_555 Mn1 . O44 4_555 127.03(8) yes O9 4_555 Mn1 . O17 4_555 94.47(7) yes O13 4_555 Mn1 . O17 4_555 80.61(8) yes O44 4_555 Mn1 . O17 4_555 148.06(7) yes O9 4_555 Mn1 . Mn8 4_555 45.84(5) yes O13 4_555 Mn1 . Mn8 4_555 123.41(6) yes O44 4_555 Mn1 . Mn8 4_555 46.95(5) yes O17 4_555 Mn1 . Mn8 4_555 106.88(5) yes O9 4_555 Mn1 . O2 . 121.57(8) yes O13 4_555 Mn1 . O2 . 72.20(8) yes O44 4_555 Mn1 . O2 . 80.97(8) yes O17 4_555 Mn1 . O2 . 127.36(8) yes Mn8 4_555 Mn1 . O2 . 125.75(6) yes O9 4_555 Mn1 . O7 . 155.46(8) yes O13 4_555 Mn1 . O7 . 123.62(8) yes O44 4_555 Mn1 . O7 . 93.69(8) yes O17 4_555 Mn1 . O7 . 79.73(7) yes Mn8 4_555 Mn1 . O7 . 112.81(6) yes O9 4_555 Mn1 . Mn8 . 114.55(6) yes O13 4_555 Mn1 . Mn8 . 125.76(6) yes O44 4_555 Mn1 . Mn8 . 107.17(5) yes O17 4_555 Mn1 . Mn8 . 47.37(5) yes Mn8 4_555 Mn1 . Mn8 . 90.548(16) yes O9 4_555 Mn1 . O69 . 77.48(8) yes O13 4_555 Mn1 . O69 . 141.90(12) yes O44 4_555 Mn1 . O69 . 75.43(9) yes O17 4_555 Mn1 . O69 . 72.63(9) yes Mn8 4_555 Mn1 . O69 . 45.455(12) yes O2 . Mn1 . O7 . 79.32(8) yes O2 . Mn1 . Mn8 . 123.72(6) yes O7 . Mn1 . Mn8 . 45.24(5) yes O2 . Mn1 . O69 . 145.91(12) yes O7 . Mn1 . O69 . 78.04(9) yes Mn8 . Mn1 . O69 . 45.153(12) yes Mn1 . O2 . S3 . 126.60(12) yes C46 4_555 S3 . O2 . 109.44(13) yes C46 4_555 S3 . O4 . 107.69(13) yes O2 . S3 . O4 . 115.71(13) yes C46 4_555 S3 . C5 . 105.49(14) yes O2 . S3 . C5 . 110.12(13) yes O4 . S3 . C5 . 107.87(13) yes S3 . C5 . C6 . 123.7(2) yes S3 . C5 . C56 . 113.0(2) yes C6 . C5 . C56 . 123.3(3) yes C5 . C6 . O7 . 123.4(3) yes C5 . C6 . C53 . 112.6(2) yes O7 . C6 . C53 . 124.0(3) yes Mn1 . O7 . C6 . 132.88(18) yes Mn1 . O7 . Mn8 . 88.37(7) yes C6 . O7 . Mn8 . 133.43(19) yes O35 4_555 Mn8 . O7 . 122.25(8) yes O35 4_555 Mn8 . O17 4_555 79.40(8) yes O7 . Mn8 . O17 4_555 80.87(8) yes O35 4_555 Mn8 . Mn1 4_555 125.37(6) yes O7 . Mn8 . Mn1 4_555 112.20(6) yes O17 4_555 Mn8 . Mn1 4_555 106.45(5) yes O35 4_555 Mn8 . Mn1 . 124.66(6) yes O7 . Mn8 . Mn1 . 46.38(5) yes O17 4_555 Mn8 . Mn1 . 47.66(5) yes Mn1 4_555 Mn8 . Mn1 . 89.451(16) yes O35 4_555 Mn8 . O9 . 78.86(8) yes O7 . Mn8 . O9 . 156.32(8) yes O17 4_555 Mn8 . O9 . 94.09(8) yes Mn1 4_555 Mn8 . O9 . 46.90(5) yes Mn1 . Mn8 . O9 . 114.42(6) yes O35 4_555 Mn8 . O44 . 129.14(8) yes O7 . Mn8 . O44 . 92.32(8) yes O17 4_555 Mn8 . O44 . 147.65(7) yes Mn1 4_555 Mn8 . O44 . 47.15(5) yes Mn1 . Mn8 . O44 . 106.19(5) yes O35 4_555 Mn8 . O52 . 72.07(8) yes O7 . Mn8 . O52 . 79.46(8) yes O17 4_555 Mn8 . O52 . 128.38(8) yes Mn1 4_555 Mn8 . O52 . 125.17(6) yes Mn1 . Mn8 . O52 . 125.07(6) yes O35 4_555 Mn8 . O69 . 141.76(12) yes O7 . Mn8 . O69 . 78.53(9) yes O17 4_555 Mn8 . O69 . 72.47(9) yes Mn1 4_555 Mn8 . O69 . 44.912(13) yes Mn1 . Mn8 . O69 . 44.617(13) yes O9 . Mn8 . O44 . 79.56(7) yes O9 . Mn8 . O52 . 120.34(8) yes O44 . Mn8 . O52 . 80.39(7) yes O9 . Mn8 . O69 . 77.89(8) yes O44 . Mn8 . O69 . 75.18(9) yes O52 . Mn8 . O69 . 146.17(12) yes Mn8 . O9 . Mn1 4_555 87.26(7) yes Mn8 . O9 . C10 . 130.99(18) yes Mn1 4_555 O9 . C10 . 130.15(18) yes C20 4_555 C10 . O9 . 123.8(3) yes C20 4_555 C10 . C11 . 112.9(2) yes O9 . C10 . C11 . 123.3(3) yes C10 . C11 . C25 4_555 123.0(4) yes C10 . C11 . S12 . 124.2(2) yes C25 4_555 C11 . S12 . 112.8(3) yes C10 . C11 . C26 4_555 123.5(5) yes C10 . C11 . S12 . 124.2(2) yes C26 4_555 C11 . S12 . 112.3(5) yes C11 . S12 . O13 . 110.09(13) yes C11 . S12 . O14 . 107.96(14) yes O13 . S12 . O14 . 115.83(13) yes C11 . S12 . C15 . 104.10(13) yes O13 . S12 . C15 . 110.07(13) yes O14 . S12 . C15 . 108.12(14) yes Mn1 4_555 O13 . S12 . 126.18(13) yes S12 . C15 . C16 . 119.8(2) yes S12 . C15 . C39 . 116.0(2) yes C16 . C15 . C39 . 123.9(3) yes C15 . C16 . O17 . 123.8(3) yes C15 . C16 . C18 . 112.8(3) yes O17 . C16 . C18 . 123.4(3) yes Mn8 4_555 O17 . Mn1 4_555 84.97(7) yes Mn8 4_555 O17 . C16 . 136.55(18) yes Mn1 4_555 O17 . C16 . 135.12(19) yes C16 . C18 . S19 . 120.5(2) yes C16 . C18 . C37 . 123.7(3) yes S19 . C18 . C37 . 115.6(2) yes C18 . S19 . C20 . 104.54(14) yes C18 . S19 . O35 . 108.96(13) yes C20 . S19 . O35 . 110.08(14) yes C18 . S19 . O36 . 108.79(14) yes C20 . S19 . O36 . 108.19(14) yes O35 . S19 . O36 . 115.68(13) yes S19 . C20 . C10 4_555 124.8(2) yes S19 . C20 . C21 . 112.5(3) yes C10 4_555 C20 . C21 . 122.6(4) yes S19 . C20 . C10 4_555 124.8(2) yes S19 . C20 . C22 . 112.0(5) yes C10 4_555 C20 . C22 . 122.7(5) yes C20 . C21 . C23 . 123.6(5) yes C20 . C21 . H211 . 118.8 no C23 . C21 . H211 . 117.6 no C20 . C22 . C24 . 121.5(8) yes C20 . C22 . H221 . 118.1 no C24 . C22 . H221 . 120.4 no C21 . C23 . C25 . 115.9(6) yes C21 . C23 . C27 . 121.7(6) yes C25 . C23 . C27 . 122.4(6) yes C22 . C24 . C26 . 115.6(9) yes C22 . C24 . C28 . 122.1(9) yes C26 . C24 . C28 . 122.3(9) yes C11 4_555 C25 . C23 . 121.8(6) yes C11 4_555 C25 . H251 . 116.9 no C23 . C25 . H251 . 120.4 no C24 . C26 . C11 4_555 122.2(10) yes C24 . C26 . H261 . 116.1 no C11 4_555 C26 . H261 . 119.9 no C23 . C27 . C30 . 112.2(5) yes C23 . C27 . C32 . 109.7(5) yes C30 . C27 . C32 . 105.4(5) yes C23 . C27 . C33 . 109.1(5) yes C30 . C27 . C33 . 112.1(6) yes C32 . C27 . C33 . 108.3(5) yes C24 . C28 . C29 . 109.6(8) yes C24 . C28 . C31 . 111.9(7) yes C29 . C28 . C31 . 108.0(7) yes C24 . C28 . C34 . 107.8(7) yes C29 . C28 . C34 . 109.1(6) yes C31 . C28 . C34 . 110.5(7) yes C28 . C29 . H291 . 108.9 no C28 . C29 . H293 . 109.7 no H291 . C29 . H293 . 109.3 no C28 . C29 . H292 . 109.1 no H291 . C29 . H292 . 109.7 no H293 . C29 . H292 . 110.0 no C27 . C30 . H302 . 110.2 no C27 . C30 . H301 . 110.8 no H302 . C30 . H301 . 109.5 no C27 . C30 . H303 . 109.6 no H302 . C30 . H303 . 108.3 no H301 . C30 . H303 . 108.4 no C28 . C31 . H313 . 109.7 no C28 . C31 . H312 . 108.6 no H313 . C31 . H312 . 109.7 no C28 . C31 . H311 . 110.6 no H313 . C31 . H311 . 108.5 no H312 . C31 . H311 . 109.7 no C27 . C32 . H322 . 108.4 no C27 . C32 . H323 . 110.9 no H322 . C32 . H323 . 108.8 no C27 . C32 . H321 . 110.6 no H322 . C32 . H321 . 108.7 no H323 . C32 . H321 . 109.3 no C27 . C33 . H332 . 108.0 no C27 . C33 . H331 . 107.5 no H332 . C33 . H331 . 109.9 no C27 . C33 . H333 . 111.3 no H332 . C33 . H333 . 110.1 no H331 . C33 . H333 . 110.2 no C28 . C34 . H343 . 110.2 no C28 . C34 . H341 . 109.3 no H343 . C34 . H341 . 110.3 no C28 . C34 . H342 . 107.2 no H343 . C34 . H342 . 110.0 no H341 . C34 . H342 . 109.9 no Mn8 4_555 O35 . S19 . 124.91(12) yes C18 . C37 . C38 . 121.7(3) yes C18 . C37 . H371 . 118.8 no C38 . C37 . H371 . 119.6 no C37 . C38 . C39 . 116.4(3) yes C37 . C38 . C40 . 123.7(3) yes C39 . C38 . C40 . 119.9(3) yes C38 . C39 . C15 . 121.6(3) yes C38 . C39 . H391 . 119.5 no C15 . C39 . H391 . 118.9 no C38 . C40 . C41 . 109.5(3) yes C38 . C40 . C42 . 109.0(3) yes C41 . C40 . C42 . 110.1(3) yes C38 . C40 . C43 . 111.8(3) yes C41 . C40 . C43 . 108.5(3) yes C42 . C40 . C43 . 107.9(3) yes C40 . C41 . H413 . 108.5 no C40 . C41 . H411 . 109.9 no H413 . C41 . H411 . 109.0 no C40 . C41 . H412 . 110.4 no H413 . C41 . H412 . 108.6 no H411 . C41 . H412 . 110.4 no C40 . C42 . H422 . 109.7 no C40 . C42 . H423 . 109.6 no H422 . C42 . H423 . 109.0 no C40 . C42 . H421 . 108.6 no H422 . C42 . H421 . 110.4 no H423 . C42 . H421 . 109.5 no C40 . C43 . H431 . 109.1 no C40 . C43 . H432 . 110.4 no H431 . C43 . H432 . 108.6 no C40 . C43 . H433 . 111.5 no H431 . C43 . H433 . 108.6 no H432 . C43 . H433 . 108.6 no Mn8 . O44 . Mn1 4_555 85.90(7) yes Mn8 . O44 . C45 . 136.81(18) yes Mn1 4_555 O44 . C45 . 135.11(19) yes O44 . C45 . C46 . 123.9(3) yes O44 . C45 . C50 . 122.9(3) yes C46 . C45 . C50 . 113.2(2) yes C45 . C46 . S3 4_555 120.8(2) yes C45 . C46 . C47 . 123.3(3) yes S3 4_555 C46 . C47 . 115.8(2) yes C46 . C47 . C48 . 122.3(3) yes C46 . C47 . H471 . 117.7 no C48 . C47 . H471 . 120.0 no C47 . C48 . C49 . 116.3(3) yes C47 . C48 . C65 . 120.5(3) yes C49 . C48 . C65 . 123.1(3) yes C48 . C49 . C50 . 122.0(3) yes C48 . C49 . H491 . 119.8 no C50 . C49 . H491 . 118.2 no C45 . C50 . C49 . 122.9(3) yes C45 . C50 . S51 . 121.4(2) yes C49 . C50 . S51 . 115.5(2) yes C50 . S51 . O52 . 109.44(13) yes C50 . S51 . C53 . 105.36(14) yes O52 . S51 . C53 . 109.09(13) yes C50 . S51 . O64 . 108.19(14) yes O52 . S51 . O64 . 115.79(13) yes C53 . S51 . O64 . 108.46(14) yes Mn8 . O52 . S51 . 125.98(12) yes C6 . C53 . S51 . 124.2(2) yes C6 . C53 . C54 . 123.1(3) yes S51 . C53 . C54 . 112.7(2) yes C53 . C54 . C55 . 122.5(3) yes C53 . C54 . H541 . 119.9 no C55 . C54 . H541 . 117.6 no C54 . C55 . C56 . 116.1(3) yes C54 . C55 . C57 . 122.0(3) yes C56 . C55 . C57 . 121.9(3) yes C5 . C56 . C55 . 122.4(3) yes C5 . C56 . H561 . 120.1 no C55 . C56 . H561 . 117.6 no C55 . C57 . C58 . 114.6(4) yes C55 . C57 . C60 . 109.7(4) yes C58 . C57 . C60 . 108.7(5) yes C55 . C57 . C62 . 107.1(4) yes C58 . C57 . C62 . 110.6(4) yes C60 . C57 . C62 . 105.7(4) yes C55 . C57 . C59 . 106.2(4) yes C55 . C57 . C61 . 115.0(4) yes C59 . C57 . C61 . 107.7(5) yes C55 . C57 . C63 . 107.7(4) yes C59 . C57 . C63 . 106.4(5) yes C61 . C57 . C63 . 113.3(5) yes C57 . C58 . H583 . 110.3 no C57 . C58 . H582 . 111.2 no H583 . C58 . H582 . 108.3 no C57 . C58 . H581 . 111.0 no H583 . C58 . H581 . 107.7 no H582 . C58 . H581 . 108.2 no C57 . C59 . H591 . 109.1 no C57 . C59 . H592 . 109.9 no H591 . C59 . H592 . 109.6 no C57 . C59 . H593 . 108.7 no H591 . C59 . H593 . 109.6 no H592 . C59 . H593 . 109.9 no C57 . C60 . H601 . 109.6 no C57 . C60 . H602 . 108.6 no H601 . C60 . H602 . 109.7 no C57 . C60 . H603 . 109.5 no H601 . C60 . H603 . 109.3 no H602 . C60 . H603 . 110.2 no C57 . C61 . H611 . 108.9 no C57 . C61 . H613 . 110.4 no H611 . C61 . H613 . 109.7 no C57 . C61 . H612 . 109.0 no H611 . C61 . H612 . 109.3 no H613 . C61 . H612 . 109.4 no C57 . C62 . H621 . 111.0 no C57 . C62 . H622 . 109.6 no H621 . C62 . H622 . 108.7 no C57 . C62 . H623 . 109.1 no H621 . C62 . H623 . 109.8 no H622 . C62 . H623 . 108.6 no C57 . C63 . H631 . 110.1 no C57 . C63 . H632 . 110.1 no H631 . C63 . H632 . 108.5 no C57 . C63 . H633 . 110.5 no H631 . C63 . H633 . 108.4 no H632 . C63 . H633 . 109.1 no C48 . C65 . C66 . 109.9(3) yes C48 . C65 . C67 . 108.4(3) yes C66 . C65 . C67 . 109.0(3) yes C48 . C65 . C68 . 112.4(3) yes C66 . C65 . C68 . 108.6(3) yes C67 . C65 . C68 . 108.6(3) yes C65 . C66 . H661 . 110.3 no C65 . C66 . H662 . 109.8 no H661 . C66 . H662 . 109.4 no C65 . C66 . H663 . 110.3 no H661 . C66 . H663 . 109.8 no H662 . C66 . H663 . 107.2 no C65 . C67 . H672 . 110.6 no C65 . C67 . H673 . 110.3 no H672 . C67 . H673 . 109.8 no C65 . C67 . H671 . 108.4 no H672 . C67 . H671 . 108.1 no H673 . C67 . H671 . 109.5 no C65 . C68 . H682 . 110.3 no C65 . C68 . H683 . 111.1 no H682 . C68 . H683 . 107.4 no C65 . C68 . H681 . 110.8 no H682 . C68 . H681 . 109.2 no H683 . C68 . H681 . 107.9 no Mn8 . O69 . Mn8 4_555 176.3(2) yes Mn8 . O69 . Mn1 4_555 89.633(18) yes Mn8 4_555 O69 . Mn1 4_555 90.230(19) yes Mn8 . O69 . Mn1 . 90.230(19) yes Mn8 4_555 O69 . Mn1 . 89.633(18) yes Mn1 4_555 O69 . Mn1 . 175.8(2) yes Mn8 . O69 . H691 . 88.2 no Mn8 4_555 O69 . H691 . 88.2 no Mn1 4_555 O69 . H691 . 87.9 no Mn1 . O69 . H691 . 87.9 no O71 4_455 K70 . O71 . 178.9(3) yes K70 . O71 . C73 . 124.9(4) yes K70 . O71 . H711 . 116.9 no C73 . O71 . H711 . 118.3 no C74 . O72 . H721 . 118.9 no C74 . O72 . K70 . 120.5(5) yes H721 . O72 . K70 . 120.5 no O71 . C73 . H731 . 109.4 no O71 . C73 . H733 . 112.1 no H731 . C73 . H733 . 107.7 no O71 . C73 . H732 . 111.9 no H731 . C73 . H732 . 107.0 no H733 . C73 . H732 . 108.5 no O72 . C74 . H743 . 108.8 no O72 . C74 . H741 . 107.8 no H743 . C74 . H741 . 110.2 no O72 . C74 . H742 . 110.9 no H743 . C74 . H742 . 109.0 no H741 . C74 . H742 . 110.1 no C76 . O75 . H751 . 99.6 no O75 . C76 . H761 . 110.9 no O75 . C76 . H762 . 107.1 no H761 . C76 . H762 . 109.5 no O75 . C76 . H763 . 110.4 no H761 . C76 . H763 . 109.5 no H762 . C76 . H763 . 109.5 no C78 4_555 O77 . H771 4_555 109.4 no C78 4_555 O77 . C78 . 100.6(9) yes H771 4_555 O77 . C78 . 84.7 no C78 4_555 O77 . H771 . 84.7 no H771 4_555 O77 . H771 . 158.4 no C78 . O77 . H771 . 109.4 no O77 . C78 . H781 . 111.1 no O77 . C78 . H782 . 108.5 no H781 . C78 . H782 . 109.5 no O77 . C78 . H783 . 108.8 no H781 . C78 . H783 . 109.5 no H782 . C78 . H783 . 109.5 no C80 . O79 . H791 . 108.7 no O79 . C80 . H801 . 109.7 no O79 . C80 . H802 . 109.6 no H801 . C80 . H802 . 109.5 no O79 . C80 . H803 . 109.1 no H801 . C80 . H803 . 109.5 no H802 . C80 . H803 . 109.5 no 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 C39 . H391 . O14 2_565 156.02(9) 0.899 2.449 3.290(7) yes C42 . H423 . O14 2_565 166.10(10) 0.962 2.551 3.493(7) yes C56 . H561 . O4 2_556 167.97(9) 0.924 2.563 3.472(7) yes C59 . H593 . C78 1_545 134.4(2) 0.964 2.385 3.136(7) yes C47 . H471 . O4 3_554 162.21(8) 0.929 2.465 3.362(7) yes C73 . H743 . C16 4_555 138.6(6) 1.198 2.546 3.535(7) yes C74 . H743 . C16 4_555 171.71(19) 0.963 2.546 3.502(7) yes O72 . H733 . O79 4_555 123.8(6) 1.050 1.806 2.545(7) yes C73 . H733 . O79 4_555 120.4(3) 0.962 1.806 2.439(7) yes O71 . H711 . O7 . 157.92(18) 0.820 2.256 3.032(7) yes O72 . H721 . O79 4_555 130.2(3) 0.820 1.937 2.545(7) yes O79 . H791 . O72 4_555 179.3(4) 0.820 1.725 2.545(7) yes O79 . H791 . C73 4_555 144.6(4) 0.820 1.724 2.439(7) yes O79 . H791 . C74 4_555 141.1(3) 0.820 2.389 3.070(7) yes O75 . H751 . O9 1_655 177.7(2) 0.820 2.188 3.008(7) yes C78 . H782 . C59 1_565 165.9(3) 0.950 2.206 3.136(7) yes C78 . H783 . C60 4_565 167.0(2) 0.950 2.452 3.385(7) yes C80 . H802 . O36 4_655 159.17(18) 0.950 2.395 3.300(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 20/09/11 at 17:32:07 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 293,X'S) H ( 292,X'S) RIDE C ( 30,X'S) H ( 302,X'S) H ( 301,X'S) H ( 303,X'S) RIDE C ( 31,X'S) H ( 313,X'S) H ( 312,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 322,X'S) H ( 323,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 332,X'S) H ( 331,X'S) H ( 333,X'S) RIDE C ( 34,X'S) H ( 343,X'S) H ( 341,X'S) H ( 342,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 41,X'S) H ( 413,X'S) H ( 411,X'S) H ( 412,X'S) RIDE C ( 42,X'S) H ( 422,X'S) H ( 423,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S) RIDE C ( 47,X'S) H ( 471,X'S) RIDE C ( 49,X'S) H ( 491,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 58,X'S) H ( 583,X'S) H ( 582,X'S) H ( 581,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) H ( 593,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) H ( 603,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 613,X'S) H ( 612,X'S) RIDE C ( 62,X'S) H ( 621,X'S) H ( 622,X'S) H ( 623,X'S) RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S) H ( 633,X'S) RIDE C ( 66,X'S) H ( 661,X'S) H ( 662,X'S) H ( 663,X'S) RIDE C ( 67,X'S) H ( 672,X'S) H ( 673,X'S) H ( 671,X'S) RIDE C ( 68,X'S) H ( 682,X'S) H ( 683,X'S) H ( 681,X'S) RIDE O ( 69,X'S) H ( 691,X'S) RIDE O ( 71,X'S) H ( 711,X'S) RIDE O ( 72,X'S) H ( 721,X'S) RIDE C ( 73,X'S) H ( 731,X'S) H ( 733,X'S) H ( 732,X'S) RIDE C ( 74,X'S) H ( 743,X'S) H ( 741,X'S) H ( 742,X'S) RIDE O ( 75,X'S) H ( 751,X'S) RIDE C ( 76,X'S) H ( 761,X'S) H ( 762,X'S) H ( 763,X'S) RIDE O ( 77,X'S) H ( 771,X'S) RIDE C ( 78,X'S) H ( 781,X'S) H ( 782,X'S) H ( 783,X'S) RIDE O ( 79,X'S) H ( 791,X'S) RIDE C ( 80,X'S) H ( 801,X'S) H ( 802,X'S) H ( 803,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 20/09/11 at 17:32:07 # #LIST 16 U(IJ)'S 0.0, 0.0010000 = C(31) TO C(27) DISTANCE 1.550000 , 0.020000 = O(75) TO C(76) DISTANCE 1.550000 , 0.020000 = O(77) TO C(78) DISTANCE 1.550000 , 0.020000 = O(79) TO C(80) U(IJ)'S 0.0, 0.0010000 = O(75) TO C(76) U(IJ)'S 0.0, 0.0010000 = O(77) TO C(78) U(IJ)'S 0.0, 0.0010000 = O(79) TO C(80) U(IJ)'S 0.0, 0.0010000 = C(26) TO C(28) U(IJ)'S 0.0, 0.0010000 = C(24) TO C(28) U(IJ)'S 0.0, 0.0010000 = C(22) TO C(28) U(IJ)'S 0.0, 0.0010000 = C(25) TO C(23) U(IJ)'S 0.0, 0.0010000 = C(21) TO C(23) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE) LIMIT 0.001000000 X LIMIT 0.001000000 Y LIMIT 0.001000000 Z REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE) END ;