# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _audit_creation_date 09-02-10 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 'eb7138 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 'Euan Brechin' _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 EBRECHIN@STAFFMAIL.ED.AC.UK _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_name _publ_author_address _publ_author_footnote # Author 1 # Author 2 E.Brechin ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; A.Collins ; ? # Address 2 ; ; ? # Footnote 2 ; S.Datta '' '' S.Hill '' '' R.Inglis '' '' L.F.Jones '' '' C.Milios '' '' S.Parsons '' '' S.Perlepes '' '' S.Piligkos '' '' W.Wernsdorfer '' '' _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. ; # Attachment '[13]CCDC706504.cif' data_EB8048 _database_code_depnum_ccdc_archive 'CCDC 706504' _cell_length_a 12.2582(4) _cell_length_b 12.3804(4) _cell_length_c 14.8895(5) _cell_angle_alpha 91.749(2) _cell_angle_beta 107.077(2) _cell_angle_gamma 115.261(2) _cell_volume 1921.47(12) _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' 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' 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' _cell_formula_units_Z 1 # Given Formula = C65 H92 Mn6 N6 O27 # Dc = 1.49 Fooo = 880.00 Mu = 10.37 M = 859.52 # Found Formula = C65 H90 Mn6 N6 O26 # Dc = 1.47 FOOO = 880.00 Mu = 10.35 M = 850.51 _chemical_formula_sum 'C65 H92 Mn6 N6 O27' _chemical_formula_weight 1719.04 _cell_measurement_reflns_used 9822 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description 'rhombohedral plate' _exptl_crystal_colour black _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.037 # 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 0.75 _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 41182 _reflns_number_total 10653 _diffrn_reflns_av_R_equivalents 0.058 # Number of reflections with Friedels Law is 10653 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11754 _diffrn_reflns_theta_min 1.849 _diffrn_reflns_theta_max 30.529 _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.781 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min -17 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _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 -0.76 _refine_diff_density_max 1.05 # 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 10620 _refine_ls_number_restraints 18 _refine_ls_number_parameters 487 _oxford_refine_ls_R_factor_ref 0.0670 _refine_ls_wR_factor_ref 0.1220 _refine_ls_goodness_of_fit_ref 1.0096 _refine_ls_shift/su_max 0.001148 # The values computed from all data _oxford_reflns_number_all 10620 _refine_ls_R_factor_all 0.0670 _refine_ls_wR_factor_all 0.1220 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8300 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_gt 0.1136 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.71P] ,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 0.55577(4) 0.10802(4) 0.58808(3) 0.0201 1.0000 Uani . . . . . . . Mn2 Mn 0.31547(4) 0.02170(4) 0.66632(3) 0.0230 1.0000 Uani . . . . . . . Mn3 Mn 0.44933(4) -0.15286(4) 0.65972(3) 0.0217 1.0000 Uani . . . . . . . O4 O 0.44372(17) -0.00523(17) 0.64042(12) 0.0224 1.0000 Uani . . . . . . . O5 O 0.64020(18) 0.21135(18) 0.51182(13) 0.0240 1.0000 Uani . . . . . . . C6 C 0.7027(3) 0.3324(3) 0.54479(17) 0.0237 1.0000 Uani . . . . . . . C7 C 0.8245(3) 0.3983(3) 0.5386(2) 0.0300 1.0000 Uani . . . . . . . C8 C 0.8932(3) 0.5213(3) 0.5718(2) 0.0335 1.0000 Uani . . . . . . . C9 C 0.8410(3) 0.5830(3) 0.6114(2) 0.0335 1.0000 Uani . . . . . . . C10 C 0.7194(3) 0.5189(3) 0.6159(2) 0.0300 1.0000 Uani . . . . . . . C11 C 0.6485(3) 0.3938(3) 0.58336(18) 0.0245 1.0000 Uani . . . . . . . C12 C 0.5196(3) 0.3297(3) 0.59100(18) 0.0236 1.0000 Uani . . . . . . . N13 N 0.4753(2) 0.2166(2) 0.59976(15) 0.0236 1.0000 Uani . . . . . . . O14 O 0.35530(18) 0.16303(19) 0.60692(14) 0.0266 1.0000 Uani . . . . . . . C15 C 0.4385(3) 0.3929(3) 0.5903(2) 0.0336 1.0000 Uani . . . . . . . O16 O 0.18427(19) 0.0412(2) 0.69402(14) 0.0299 1.0000 Uani . . . . . . . C17 C 0.1708(3) 0.0277(3) 0.77953(19) 0.0274 1.0000 Uani . . . . . . . C18 C 0.1427(3) 0.1094(3) 0.8236(2) 0.0348 1.0000 Uani . . . . . . . C19 C 0.1276(3) 0.1006(3) 0.9113(2) 0.0397 1.0000 Uani . . . . . . . C20 C 0.1401(3) 0.0105(3) 0.9589(2) 0.0376 1.0000 Uani . . . . . . . C21 C 0.1655(3) -0.0729(3) 0.9165(2) 0.0313 1.0000 Uani . . . . . . . C22 C 0.1815(2) -0.0668(3) 0.82643(19) 0.0253 1.0000 Uani . . . . . . . C23 C 0.2105(3) -0.1567(3) 0.78641(19) 0.0262 1.0000 Uani . . . . . . . N24 N 0.2705(2) -0.1289(2) 0.72546(15) 0.0238 1.0000 Uani . . . . . . . O25 O 0.29443(18) -0.21693(18) 0.68905(14) 0.0262 1.0000 Uani . . . . . . . C26 C 0.1698(3) -0.2796(3) 0.8153(2) 0.0352 1.0000 Uani . . . . . . . O27 O 0.46703(18) -0.29507(18) 0.67703(14) 0.0260 1.0000 Uani . . . . . . . C28 C 0.5800(3) -0.2872(3) 0.72844(19) 0.0249 1.0000 Uani . . . . . . . C29 C 0.5814(3) -0.3713(3) 0.7899(2) 0.0315 1.0000 Uani . . . . . . . C30 C 0.6957(3) -0.3675(3) 0.8458(2) 0.0369 1.0000 Uani . . . . . . . C31 C 0.8113(3) -0.2809(3) 0.8421(2) 0.0351 1.0000 Uani . . . . . . . C32 C 0.8128(3) -0.1988(3) 0.7821(2) 0.0293 1.0000 Uani . . . . . . . C33 C 0.6983(3) -0.1999(3) 0.72347(18) 0.0240 1.0000 Uani . . . . . . . C34 C 0.7051(3) -0.1129(3) 0.65807(18) 0.0237 1.0000 Uani . . . . . . . N35 N 0.6101(2) -0.0871(2) 0.62799(15) 0.0221 1.0000 Uani . . . . . . . O36 O 0.61537(17) -0.00982(17) 0.56163(12) 0.0223 1.0000 Uani . . . . . . . C37 C 0.8186(3) -0.0554(3) 0.6262(2) 0.0341 1.0000 Uani . . . . . . . C38 C 0.7611(3) 0.2197(3) 0.79982(19) 0.0244 1.0000 Uani . . . . . . . O39 O 0.7155(2) 0.1974(2) 0.71000(14) 0.0342 1.0000 Uani . . . . . . . O40 O 0.7022(2) 0.1658(2) 0.85430(15) 0.0325 1.0000 Uani . . . . . . . C41 C 0.8961(3) 0.3230(3) 0.8440(2) 0.0304 1.0000 Uani . . . . . . . C42 C 0.8815(4) 0.4399(3) 0.8459(3) 0.0600 1.0000 Uani . . . . . . . C43 C 0.9769(3) 0.3262(5) 0.7825(3) 0.0619 1.0000 Uani . . . . . . . C44 C 0.9600(3) 0.3121(3) 0.9453(2) 0.0419 1.0000 Uani . . . . . . . O45 O 0.4601(2) 0.1371(2) 0.80822(14) 0.0315 1.0000 Uani . . . . . . . C46 C 0.4803(4) 0.2554(4) 0.8421(3) 0.0527 1.0000 Uani . . . . . . . O47 O 0.1748(2) -0.1125(2) 0.53172(14) 0.0339 1.0000 Uani . U . . . . . C48 C 0.0410(11) -0.1578(11) 0.4964(8) 0.0988 0.5000 Uani . U . 1 1 . . O49 O 0.5647(2) -0.07638(19) 0.81408(13) 0.0292 1.0000 Uani . . . . . . . C50 C 0.5284(3) -0.1246(3) 0.8928(2) 0.0393 1.0000 Uani . . . . . . . O51 O -0.0645(5) -0.1592(7) 0.4229(5) 0.0697 0.5000 Uani . U . 1 2 . . C52 C -0.1282(9) -0.2706(12) 0.3904(7) 0.0815 0.5000 Uani . U . 1 2 . . O53 O -0.2755(6) -0.5323(6) 0.2560(5) 0.0743 0.5000 Uani . U . 1 1 . . C54 C -0.2086(7) -0.4482(7) 0.3308(5) 0.0417 0.5000 Uani . U . 1 1 . . H261 H 0.1680 -0.3360 0.7701 0.0592 1.0000 Uiso R . . . . . . H263 H 0.2265 -0.2749 0.8764 0.0592 1.0000 Uiso R . . . . . . H262 H 0.0865 -0.3089 0.8190 0.0593 1.0000 Uiso R . . . . . . H181 H 0.1368 0.1716 0.7933 0.0508 1.0000 Uiso R . . . . . . H153 H 0.3609 0.3507 0.5374 0.0588 1.0000 Uiso R . . . . . . H152 H 0.4189 0.3876 0.6476 0.0587 1.0000 Uiso R . . . . . . H151 H 0.4822 0.4762 0.5842 0.0584 1.0000 Uiso R . . . . . . H101 H 0.6847 0.5602 0.6424 0.0400 1.0000 Uiso R . . . . . . H91 H 0.8882 0.6660 0.6350 0.0405 1.0000 Uiso R . . . . . . H81 H 0.9748 0.5655 0.5688 0.0434 1.0000 Uiso R . . . . . . H71 H 0.8591 0.3573 0.5119 0.0421 1.0000 Uiso R . . . . . . H321 H 0.8920 -0.1398 0.7812 0.0395 1.0000 Uiso R . . . . . . H311 H 0.8881 -0.2761 0.8809 0.0473 1.0000 Uiso R . . . . . . H373 H 0.7894 -0.0672 0.5581 0.0586 1.0000 Uiso R . . . . . . H372 H 0.8653 0.0302 0.6512 0.0588 1.0000 Uiso R . . . . . . H371 H 0.8736 -0.0913 0.6465 0.0589 1.0000 Uiso R . . . . . . H291 H 0.5041 -0.4306 0.7927 0.0444 1.0000 Uiso R . . . . . . H211 H 0.1720 -0.1355 0.9476 0.0408 1.0000 Uiso R . . . . . . H301 H 0.6930 -0.4250 0.8856 0.0527 1.0000 Uiso R . . . . . . H201 H 0.1318 0.0049 1.0193 0.0509 1.0000 Uiso R . . . . . . H441 H 1.0460 0.3771 0.9702 0.0576 1.0000 Uiso R . . . . . . H443 H 0.9124 0.3175 0.9854 0.0579 1.0000 Uiso R . . . . . . H442 H 0.9611 0.2351 0.9446 0.0581 1.0000 Uiso R . . . . . . H191 H 0.1109 0.1568 0.9398 0.0532 1.0000 Uiso R . . . . . . H421 H 0.9647 0.5092 0.8761 0.0807 1.0000 Uiso R . . . . . . H422 H 0.8268 0.4356 0.8829 0.0813 1.0000 Uiso R . . . . . . H423 H 0.8440 0.4492 0.7817 0.0810 1.0000 Uiso R . . . . . . H432 H 1.0618 0.3923 0.8113 0.0915 1.0000 Uiso R . . . . . . H431 H 0.9805 0.2506 0.7791 0.0917 1.0000 Uiso R . . . . . . H433 H 0.9387 0.3371 0.7196 0.0916 1.0000 Uiso R . . . . . . H451 H 0.5301 0.1421 0.8194 0.0521 1.0000 Uiso R . . . . . . H502 H 0.4660 -0.2078 0.8725 0.0575 1.0000 Uiso R . . . . . . H491 H 0.6081 -0.0024 0.8253 0.0466 1.0000 Uiso R . . . . . . H503 H 0.6011 -0.1170 0.9439 0.0583 1.0000 Uiso R . . . . . . H461 H 0.5232 0.2786 0.9101 0.0800 1.0000 Uiso R . . . . . . H463 H 0.4005 0.2579 0.8267 0.0802 1.0000 Uiso R . . . . . . H462 H 0.5307 0.3132 0.8115 0.0803 1.0000 Uiso R . . . . . . H501 H 0.4916 -0.0807 0.9155 0.0584 1.0000 Uiso R . . . . . . H471 H 0.2005 -0.1243 0.4900 0.0561 1.0000 Uiso R . . . . . . H482 H 0.0157 -0.1206 0.5395 0.1053 0.5000 Uiso R . . 1 1 . . H481 H 0.0005 -0.2449 0.4940 0.1052 0.5000 Uiso R . . 1 1 . . H483 H 0.0102 -0.1409 0.4325 0.1050 0.5000 Uiso R . . 1 1 . . H511 H -0.0915 -0.1149 0.3985 0.1258 0.5000 Uiso R . . 1 2 . . H542 H -0.1948 -0.3724 0.3117 0.0548 0.5000 Uiso R . . 1 1 . . H541 H -0.1288 -0.4474 0.3593 0.0551 0.5000 Uiso R . . 1 1 . . H543 H -0.2524 -0.4615 0.3744 0.0546 0.5000 Uiso R . . 1 1 . . H472 H 0.1221 -0.0993 0.4938 0.0562 0.5000 Uiso R . . 1 2 . . H523 H -0.0718 -0.3036 0.3836 0.1512 0.5000 Uiso R . . 1 2 . . H521 H -0.1695 -0.3107 0.4341 0.1511 0.5000 Uiso R . . 1 2 . . H522 H -0.1921 -0.2859 0.3289 0.1511 0.5000 Uiso R . . 1 2 . . H531 H -0.3300 -0.5814 0.2750 0.0761 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 0.02359(19) 0.0285(2) 0.01818(17) 0.00825(15) 0.01091(15) 0.01800(17) Mn2 0.0258(2) 0.0337(2) 0.02323(19) 0.01206(17) 0.01450(16) 0.02118(18) Mn3 0.02463(19) 0.0295(2) 0.02126(18) 0.00974(16) 0.01156(15) 0.01879(17) O4 0.0269(9) 0.0322(10) 0.0209(8) 0.0104(8) 0.0135(7) 0.0209(8) O5 0.0285(9) 0.0299(10) 0.0217(8) 0.0081(8) 0.0130(8) 0.0173(8) C6 0.0270(12) 0.0345(15) 0.0173(11) 0.0107(10) 0.0096(10) 0.0190(12) C7 0.0320(14) 0.0379(16) 0.0305(14) 0.0118(12) 0.0171(12) 0.0205(13) C8 0.0298(14) 0.0395(17) 0.0338(15) 0.0090(13) 0.0141(12) 0.0157(13) C9 0.0373(16) 0.0321(16) 0.0320(14) 0.0082(12) 0.0128(13) 0.0159(13) C10 0.0373(15) 0.0346(16) 0.0267(13) 0.0102(12) 0.0121(12) 0.0229(13) C11 0.0269(12) 0.0304(14) 0.0229(12) 0.0098(11) 0.0092(10) 0.0182(11) C12 0.0284(13) 0.0308(14) 0.0207(11) 0.0084(10) 0.0103(10) 0.0200(11) N13 0.0262(11) 0.0330(12) 0.0215(10) 0.0091(9) 0.0121(9) 0.0194(10) O14 0.0265(9) 0.0360(11) 0.0319(10) 0.0148(9) 0.0168(8) 0.0222(9) C15 0.0365(15) 0.0373(17) 0.0423(16) 0.0139(14) 0.0176(13) 0.0271(14) O16 0.0312(10) 0.0455(12) 0.0298(10) 0.0157(9) 0.0175(8) 0.0273(10) C17 0.0232(12) 0.0403(16) 0.0264(13) 0.0087(12) 0.0122(11) 0.0186(12) C18 0.0334(15) 0.0452(18) 0.0407(16) 0.0109(14) 0.0189(13) 0.0269(14) C19 0.0384(17) 0.051(2) 0.0402(17) 0.0024(15) 0.0199(14) 0.0262(16) C20 0.0369(16) 0.058(2) 0.0300(14) 0.0069(14) 0.0190(13) 0.0271(16) C21 0.0300(14) 0.0429(17) 0.0263(13) 0.0097(12) 0.0148(11) 0.0176(13) C22 0.0219(12) 0.0356(15) 0.0254(12) 0.0081(11) 0.0136(10) 0.0154(11) C23 0.0230(12) 0.0339(15) 0.0253(12) 0.0090(11) 0.0100(10) 0.0148(11) N24 0.0253(11) 0.0331(13) 0.0213(10) 0.0078(9) 0.0107(9) 0.0186(10) O25 0.0291(10) 0.0314(10) 0.0292(9) 0.0093(8) 0.0160(8) 0.0194(9) C26 0.0379(16) 0.0369(17) 0.0408(16) 0.0172(14) 0.0236(14) 0.0186(14) O27 0.0280(9) 0.0292(10) 0.0292(9) 0.0092(8) 0.0118(8) 0.0188(8) C28 0.0316(13) 0.0301(14) 0.0247(12) 0.0087(11) 0.0112(11) 0.0231(12) C29 0.0399(16) 0.0344(16) 0.0333(14) 0.0146(12) 0.0166(13) 0.0252(14) C30 0.0506(19) 0.0439(18) 0.0337(15) 0.0206(14) 0.0181(14) 0.0337(16) C31 0.0377(16) 0.0454(18) 0.0303(14) 0.0125(13) 0.0072(12) 0.0287(15) C32 0.0327(14) 0.0374(16) 0.0264(13) 0.0099(12) 0.0099(11) 0.0234(13) C33 0.0299(13) 0.0302(14) 0.0194(11) 0.0066(10) 0.0095(10) 0.0196(12) C34 0.0249(12) 0.0312(14) 0.0220(11) 0.0072(10) 0.0089(10) 0.0182(11) N35 0.0257(11) 0.0288(12) 0.0203(10) 0.0093(9) 0.0101(8) 0.0182(9) O36 0.0269(9) 0.0315(10) 0.0204(8) 0.0107(7) 0.0122(7) 0.0208(8) C37 0.0289(14) 0.0529(19) 0.0340(15) 0.0211(14) 0.0143(12) 0.0273(14) C38 0.0273(13) 0.0272(13) 0.0255(12) 0.0058(10) 0.0080(10) 0.0188(11) O39 0.0358(11) 0.0415(13) 0.0238(9) 0.0057(9) 0.0081(9) 0.0177(10) O40 0.0303(10) 0.0368(12) 0.0306(10) 0.0065(9) 0.0124(9) 0.0141(9) C41 0.0276(13) 0.0386(16) 0.0236(13) 0.0094(12) 0.0071(11) 0.0147(12) C42 0.069(3) 0.034(2) 0.058(2) 0.0111(18) 0.005(2) 0.0167(19) C43 0.0324(18) 0.108(4) 0.0414(19) 0.019(2) 0.0173(16) 0.025(2) C44 0.0350(16) 0.051(2) 0.0283(15) 0.0145(14) 0.0033(13) 0.0136(15) O45 0.0294(10) 0.0385(12) 0.0326(10) 0.0034(9) 0.0129(9) 0.0194(9) C46 0.046(2) 0.053(2) 0.062(2) -0.0085(19) 0.0162(19) 0.0272(18) O47 0.0339(11) 0.0502(14) 0.0259(10) 0.0094(9) 0.0116(9) 0.0254(10) C48 0.091(6) 0.086(6) 0.071(6) -0.003(5) 0.031(5) -0.004(5) O49 0.0348(11) 0.0321(11) 0.0246(9) 0.0086(8) 0.0127(8) 0.0168(9) C50 0.0410(17) 0.049(2) 0.0238(14) 0.0115(14) 0.0114(13) 0.0170(15) O51 0.028(3) 0.102(5) 0.083(4) 0.058(4) 0.006(3) 0.040(3) C52 0.044(4) 0.147(8) 0.083(6) 0.072(6) 0.036(4) 0.056(5) O53 0.073(4) 0.060(4) 0.078(4) 0.033(3) 0.030(3) 0.016(3) C54 0.048(4) 0.055(4) 0.035(3) 0.016(3) 0.017(3) 0.033(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4650(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 . O36 2_656 2.3999(19) yes Mn1 . Mn1 2_656 3.2012(8) yes Mn1 . Mn2 . 3.2529(5) yes Mn1 . Mn3 . 3.2716(6) yes Mn1 . O4 . 1.8740(18) yes Mn1 . O5 . 1.9093(18) yes Mn1 . N13 . 2.007(2) yes Mn1 . O36 . 1.9650(18) yes Mn1 . O39 . 2.072(2) yes Mn2 . Mn3 . 3.2375(6) yes Mn2 . O4 . 1.8780(18) yes Mn2 . O14 . 1.9239(19) yes Mn2 . O16 . 1.8784(19) yes Mn2 . N24 . 2.016(2) yes Mn2 . O45 . 2.259(2) yes Mn2 . O47 . 2.252(2) yes Mn3 . O5 2_656 2.4114(18) yes Mn3 . O4 . 1.8857(19) yes Mn3 . O25 . 1.9100(19) yes Mn3 . O27 . 1.8799(19) yes Mn3 . N35 . 1.993(2) yes Mn3 . O49 . 2.235(2) yes O5 . C6 . 1.352(3) yes C6 . C7 . 1.396(4) yes C6 . C11 . 1.407(4) yes C7 . C8 . 1.374(4) yes C7 . H71 . 0.931 no C8 . C9 . 1.397(4) yes C8 . H81 . 0.929 no C9 . C10 . 1.381(4) yes C9 . H91 . 0.930 no C10 . C11 . 1.395(4) yes C10 . H101 . 0.933 no C11 . C12 . 1.476(4) yes C12 . N13 . 1.295(3) yes C12 . C15 . 1.503(4) yes N13 . O14 . 1.370(3) yes C15 . H153 . 0.953 no C15 . H152 . 0.950 no C15 . H151 . 0.961 no O16 . C17 . 1.338(3) yes C17 . C18 . 1.400(4) yes C17 . C22 . 1.414(4) yes C18 . C19 . 1.374(4) yes C18 . H181 . 0.923 no C19 . C20 . 1.378(5) yes C19 . H191 . 0.929 no C20 . C21 . 1.382(4) yes C20 . H201 . 0.936 no C21 . C22 . 1.411(3) yes C21 . H211 . 0.935 no C22 . C23 . 1.463(4) yes C23 . N24 . 1.296(3) yes C23 . C26 . 1.505(4) yes N24 . O25 . 1.378(3) yes C26 . H261 . 0.943 no C26 . H263 . 0.952 no C26 . H262 . 0.946 no O27 . C28 . 1.331(3) yes C28 . C29 . 1.409(4) yes C28 . C33 . 1.417(4) yes C29 . C30 . 1.384(4) yes C29 . H291 . 0.933 no C30 . C31 . 1.384(5) yes C30 . H301 . 0.936 no C31 . C32 . 1.371(4) yes C31 . H311 . 0.924 no C32 . C33 . 1.413(4) yes C32 . H321 . 0.937 no C33 . C34 . 1.467(3) yes C34 . N35 . 1.296(3) yes C34 . C37 . 1.494(4) yes N35 . O36 . 1.392(3) yes C37 . H373 . 0.954 no C37 . H372 . 0.961 no C37 . H371 . 0.942 no C38 . O39 . 1.258(3) yes C38 . O40 . 1.261(3) yes C38 . C41 . 1.520(4) yes C41 . C42 . 1.533(5) yes C41 . C43 . 1.523(5) yes C41 . C44 . 1.521(4) yes C42 . H421 . 0.969 no C42 . H422 . 0.971 no C42 . H423 . 0.966 no C43 . H432 . 0.962 no C43 . H431 . 0.957 no C43 . H433 . 0.959 no C44 . H441 . 0.961 no C44 . H443 . 0.968 no C44 . H442 . 0.959 no O45 . C46 . 1.425(4) yes O45 . H451 . 0.800 no C46 . H461 . 0.962 no C46 . H463 . 0.952 no C46 . H462 . 0.953 no O47 . C48 . 1.405(12) yes O47 . H471 . 0.809 no O47 . H471 . 0.809 no O47 . H472 . 0.803 no C48 . H482 . 0.969 no C48 . H481 . 0.970 no C48 . H483 . 0.980 no O49 . C50 . 1.431(3) yes O49 . H491 . 0.819 no C50 . H502 . 0.954 no C50 . H503 . 0.953 no C50 . H501 . 0.950 no O51 . C52 . 1.251(13) yes O51 . H511 . 0.801 no C52 . H523 . 0.967 no C52 . H521 . 0.961 no C52 . H522 . 0.964 no O53 . C54 . 1.288(9) yes O53 . H531 . 0.820 no C54 . H542 . 0.948 no C54 . H541 . 0.940 no C54 . H543 . 0.935 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 O36 2_656 Mn1 . Mn1 2_656 37.77(4) yes O36 2_656 Mn1 . Mn2 . 81.48(4) yes Mn1 2_656 Mn1 . Mn2 . 100.775(19) yes O36 2_656 Mn1 . Mn3 . 87.51(4) yes Mn1 2_656 Mn1 . Mn3 . 70.458(16) yes Mn2 . Mn1 . Mn3 . 59.498(12) yes O36 2_656 Mn1 . O4 . 84.95(7) yes Mn1 2_656 Mn1 . O4 . 86.13(6) yes Mn2 . Mn1 . O4 . 29.93(6) yes Mn3 . Mn1 . O4 . 29.62(6) yes O36 2_656 Mn1 . O5 . 83.61(7) yes Mn1 2_656 Mn1 . O5 . 86.06(6) yes Mn2 . Mn1 . O5 . 144.83(6) yes Mn3 . Mn1 . O5 . 151.07(6) yes O4 . Mn1 . O5 . 168.39(8) yes O36 2_656 Mn1 . N13 . 86.44(8) yes Mn1 2_656 Mn1 . N13 . 124.20(7) yes Mn2 . Mn1 . N13 . 59.04(6) yes Mn3 . Mn1 . N13 . 118.47(6) yes O4 . Mn1 . N13 . 88.85(8) yes O36 2_656 Mn1 . O36 . 86.19(7) yes Mn1 2_656 Mn1 . O36 . 48.42(5) yes Mn2 . Mn1 . O36 . 119.05(5) yes Mn3 . Mn1 . O36 . 60.53(5) yes O4 . Mn1 . O36 . 89.86(8) yes O36 2_656 Mn1 . O39 . 174.52(7) yes Mn1 2_656 Mn1 . O39 . 139.50(7) yes Mn2 . Mn1 . O39 . 104.00(6) yes Mn3 . Mn1 . O39 . 95.52(6) yes O4 . Mn1 . O39 . 99.94(8) yes O5 . Mn1 . N13 . 88.45(8) yes O5 . Mn1 . O36 . 91.37(8) yes N13 . Mn1 . O36 . 172.60(9) yes O5 . Mn1 . O39 . 91.58(8) yes N13 . Mn1 . O39 . 96.08(9) yes O36 . Mn1 . O39 . 91.32(8) yes Mn1 . Mn2 . Mn3 . 60.539(12) yes Mn1 . Mn2 . O4 . 29.86(6) yes Mn3 . Mn2 . O4 . 30.73(6) yes Mn1 . Mn2 . O14 . 61.98(5) yes Mn3 . Mn2 . O14 . 121.79(6) yes O4 . Mn2 . O14 . 91.65(8) yes Mn1 . Mn2 . O16 . 152.94(7) yes Mn3 . Mn2 . O16 . 146.46(7) yes O4 . Mn2 . O16 . 177.20(9) yes O14 . Mn2 . O16 . 91.11(8) yes Mn1 . Mn2 . N24 . 118.15(6) yes Mn3 . Mn2 . N24 . 58.12(6) yes O4 . Mn2 . N24 . 88.40(8) yes O14 . Mn2 . N24 . 178.59(9) yes O16 . Mn2 . N24 . 88.82(9) yes Mn1 . Mn2 . O45 . 86.54(5) yes Mn3 . Mn2 . O45 . 94.53(5) yes O4 . Mn2 . O45 . 89.29(8) yes O14 . Mn2 . O45 . 90.53(8) yes O16 . Mn2 . O45 . 91.17(8) yes Mn1 . Mn2 . O47 . 93.87(5) yes Mn3 . Mn2 . O47 . 79.65(6) yes O4 . Mn2 . O47 . 87.62(8) yes O14 . Mn2 . O47 . 95.84(8) yes O16 . Mn2 . O47 . 91.61(9) yes N24 . Mn2 . O45 . 90.87(8) yes N24 . Mn2 . O47 . 82.75(8) yes O45 . Mn2 . O47 . 172.99(8) yes O5 2_656 Mn3 . Mn2 . 93.95(5) yes O5 2_656 Mn3 . Mn1 . 77.31(5) yes Mn2 . Mn3 . Mn1 . 59.964(12) yes O5 2_656 Mn3 . O4 . 86.06(7) yes Mn2 . Mn3 . O4 . 30.59(5) yes Mn1 . Mn3 . O4 . 29.42(5) yes O5 2_656 Mn3 . O25 . 99.39(7) yes Mn2 . Mn3 . O25 . 62.25(6) yes Mn1 . Mn3 . O25 . 121.63(6) yes O4 . Mn3 . O25 . 92.70(8) yes O5 2_656 Mn3 . O27 . 93.35(8) yes Mn2 . Mn3 . O27 . 153.83(6) yes Mn1 . Mn3 . O27 . 146.20(6) yes O4 . Mn3 . O27 . 175.53(8) yes O25 . Mn3 . O27 . 91.76(8) yes O5 2_656 Mn3 . N35 . 80.13(8) yes Mn2 . Mn3 . N35 . 117.94(7) yes Mn1 . Mn3 . N35 . 58.48(6) yes O4 . Mn3 . N35 . 87.46(8) yes O25 . Mn3 . N35 . 179.48(9) yes O5 2_656 Mn3 . O49 . 169.65(7) yes Mn2 . Mn3 . O49 . 88.25(6) yes Mn1 . Mn3 . O49 . 95.16(5) yes O4 . Mn3 . O49 . 90.77(8) yes O25 . Mn3 . O49 . 90.59(8) yes O27 . Mn3 . N35 . 88.07(9) yes O27 . Mn3 . O49 . 89.04(8) yes N35 . Mn3 . O49 . 89.90(8) yes Mn3 . O4 . Mn2 . 118.67(9) yes Mn3 . O4 . Mn1 . 120.96(9) yes Mn2 . O4 . Mn1 . 120.22(10) yes Mn3 2_656 O5 . Mn1 . 119.14(9) yes Mn3 2_656 O5 . C6 . 115.06(14) yes Mn1 . O5 . C6 . 117.99(15) yes O5 . C6 . C7 . 118.4(2) yes O5 . C6 . C11 . 122.4(2) yes C7 . C6 . C11 . 119.2(3) yes C6 . C7 . C8 . 121.1(3) yes C6 . C7 . H71 . 118.8 no C8 . C7 . H71 . 120.2 no C7 . C8 . C9 . 120.2(3) yes C7 . C8 . H81 . 121.5 no C9 . C8 . H81 . 118.4 no C8 . C9 . C10 . 119.1(3) yes C8 . C9 . H91 . 120.1 no C10 . C9 . H91 . 120.7 no C9 . C10 . C11 . 121.6(3) yes C9 . C10 . H101 . 119.0 no C11 . C10 . H101 . 119.4 no C6 . C11 . C10 . 118.8(3) yes C6 . C11 . C12 . 121.9(3) yes C10 . C11 . C12 . 119.3(3) yes C11 . C12 . N13 . 119.6(2) yes C11 . C12 . C15 . 121.6(2) yes N13 . C12 . C15 . 118.8(2) yes Mn1 . N13 . C12 . 126.15(18) yes Mn1 . N13 . O14 . 116.99(17) yes C12 . N13 . O14 . 116.4(2) yes N13 . O14 . Mn2 . 116.03(15) yes C12 . C15 . H153 . 107.4 no C12 . C15 . H152 . 108.8 no H153 . C15 . H152 . 109.0 no C12 . C15 . H151 . 110.8 no H153 . C15 . H151 . 110.3 no H152 . C15 . H151 . 110.5 no Mn2 . O16 . C17 . 120.28(17) yes O16 . C17 . C18 . 118.5(3) yes O16 . C17 . C22 . 122.7(3) yes C18 . C17 . C22 . 118.7(3) yes C17 . C18 . C19 . 121.5(3) yes C17 . C18 . H181 . 118.7 no C19 . C18 . H181 . 119.8 no C18 . C19 . C20 . 120.6(3) yes C18 . C19 . H191 . 120.0 no C20 . C19 . H191 . 119.4 no C19 . C20 . C21 . 119.3(3) yes C19 . C20 . H201 . 121.1 no C21 . C20 . H201 . 119.5 no C20 . C21 . C22 . 121.6(3) yes C20 . C21 . H211 . 119.8 no C22 . C21 . H211 . 118.5 no C17 . C22 . C21 . 118.2(3) yes C17 . C22 . C23 . 122.9(2) yes C21 . C22 . C23 . 118.9(3) yes C22 . C23 . N24 . 118.8(3) yes C22 . C23 . C26 . 120.2(2) yes N24 . C23 . C26 . 120.9(3) yes Mn2 . N24 . C23 . 127.2(2) yes Mn2 . N24 . O25 . 115.70(15) yes C23 . N24 . O25 . 116.7(2) yes N24 . O25 . Mn3 . 113.56(15) yes C23 . C26 . H261 . 110.8 no C23 . C26 . H263 . 110.7 no H261 . C26 . H263 . 109.3 no C23 . C26 . H262 . 110.1 no H261 . C26 . H262 . 108.0 no H263 . C26 . H262 . 107.8 no Mn3 . O27 . C28 . 119.85(18) yes O27 . C28 . C29 . 118.1(3) yes O27 . C28 . C33 . 123.4(2) yes C29 . C28 . C33 . 118.5(2) yes C28 . C29 . C30 . 121.0(3) yes C28 . C29 . H291 . 119.5 no C30 . C29 . H291 . 119.5 no C29 . C30 . C31 . 120.4(3) yes C29 . C30 . H301 . 118.7 no C31 . C30 . H301 . 120.9 no C30 . C31 . C32 . 119.9(3) yes C30 . C31 . H311 . 120.8 no C32 . C31 . H311 . 119.3 no C31 . C32 . C33 . 121.5(3) yes C31 . C32 . H321 . 118.9 no C33 . C32 . H321 . 119.6 no C28 . C33 . C32 . 118.7(2) yes C28 . C33 . C34 . 122.1(2) yes C32 . C33 . C34 . 119.3(2) yes C33 . C34 . N35 . 118.6(2) yes C33 . C34 . C37 . 120.9(2) yes N35 . C34 . C37 . 120.5(2) yes Mn3 . N35 . C34 . 127.56(18) yes Mn3 . N35 . O36 . 114.86(15) yes C34 . N35 . O36 . 117.5(2) yes N35 . O36 . Mn1 2_656 112.09(14) yes N35 . O36 . Mn1 . 112.11(13) yes Mn1 2_656 O36 . Mn1 . 93.81(7) yes C34 . C37 . H373 . 108.8 no C34 . C37 . H372 . 110.6 no H373 . C37 . H372 . 108.8 no C34 . C37 . H371 . 110.6 no H373 . C37 . H371 . 108.8 no H372 . C37 . H371 . 109.3 no O39 . C38 . O40 . 125.1(3) yes O39 . C38 . C41 . 116.1(2) yes O40 . C38 . C41 . 118.8(2) yes Mn1 . O39 . C38 . 147.8(2) yes C38 . C41 . C42 . 105.9(3) yes C38 . C41 . C43 . 110.4(3) yes C42 . C41 . C43 . 109.3(3) yes C38 . C41 . C44 . 111.4(2) yes C42 . C41 . C44 . 109.5(3) yes C43 . C41 . C44 . 110.2(3) yes C41 . C42 . H421 . 109.7 no C41 . C42 . H422 . 108.8 no H421 . C42 . H422 . 108.8 no C41 . C42 . H423 . 110.1 no H421 . C42 . H423 . 109.4 no H422 . C42 . H423 . 110.0 no C41 . C43 . H432 . 109.4 no C41 . C43 . H431 . 107.9 no H432 . C43 . H431 . 110.2 no C41 . C43 . H433 . 110.2 no H432 . C43 . H433 . 109.4 no H431 . C43 . H433 . 109.7 no C41 . C44 . H441 . 109.2 no C41 . C44 . H443 . 109.8 no H441 . C44 . H443 . 109.2 no C41 . C44 . H442 . 109.3 no H441 . C44 . H442 . 110.3 no H443 . C44 . H442 . 108.9 no Mn2 . O45 . C46 . 124.1(2) yes Mn2 . O45 . H451 . 114.9 no C46 . O45 . H451 . 105.4 no O45 . C46 . H461 . 111.5 no O45 . C46 . H463 . 110.1 no H461 . C46 . H463 . 108.9 no O45 . C46 . H462 . 109.9 no H461 . C46 . H462 . 109.0 no H463 . C46 . H462 . 107.3 no Mn2 . O47 . C48 . 127.9(5) yes Mn2 . O47 . H471 . 119.2 no C48 . O47 . H471 . 110.6 no Mn2 . O47 . H471 . 119.2 no Mn2 . O47 . H472 . 121.8 no H471 . O47 . H472 . 90.4 no O47 . C48 . H482 . 108.8 no O47 . C48 . H481 . 109.4 no H482 . C48 . H481 . 108.5 no O47 . C48 . H483 . 112.6 no H482 . C48 . H483 . 108.6 no H481 . C48 . H483 . 108.9 no Mn3 . O49 . C50 . 125.54(18) yes Mn3 . O49 . H491 . 113.8 no C50 . O49 . H491 . 113.5 no O49 . C50 . H502 . 110.1 no O49 . C50 . H503 . 111.0 no H502 . C50 . H503 . 110.0 no O49 . C50 . H501 . 109.2 no H502 . C50 . H501 . 108.3 no H503 . C50 . H501 . 108.2 no C52 . O51 . H511 . 118.1 no O51 . C52 . H523 . 109.7 no O51 . C52 . H521 . 109.4 no H523 . C52 . H521 . 108.6 no O51 . C52 . H522 . 110.9 no H523 . C52 . H522 . 108.8 no H521 . C52 . H522 . 109.5 no C54 . O53 . H531 . 100.6 no O53 . C54 . H542 . 108.5 no O53 . C54 . H541 . 109.9 no H542 . C54 . H541 . 109.0 no O53 . C54 . H543 . 110.0 no H542 . C54 . H543 . 109.6 no H541 . C54 . H543 . 109.8 no data_1 _database_code_depnum_ccdc_archive 'CCDC 706505' _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 positioned geometrically. Those attached to O atoms were positioned along lokely hydrogen bond directions. Hydrogen positions were not refined. The majority of the structure was routine, however one ligand was substitutionally disordered and refined as a 1:1 ratio of ethanol:water. This had an associated affect on the solvent, which has been modelled as two half-occupancy ethanol molecules. The occupancies of these ligands and of the carbon atoms of the part-occupancy ethanol ligand were initially refined but were later fixed at 0.5 as the refined values were very close to this. One of the solvent molecules has the hydroxy group disordered over two positions with an occupancies of these atoms and the attached H atoms fixed at 0.25. Checkcif alerts 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.53 Ratio 415_ALERT_2_B Short Inter D-H..H-X H391 .. H1081 .. 1.92 Ang. 432_ALERT_2_B Short Inter X...Y Contact C28 .. O107 .. 2.75 Ang. No action. 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? These arise from rounding errors. 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.02 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.25 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C110 No action. 245_ALERT_2_C U(iso) H1051 Smaller than U(eq) C110 by ... 0.01 AngSq 245_ALERT_2_C U(iso) H1052 Smaller than U(eq) C110 by ... 0.01 AngSq 245_ALERT_2_C U(iso) H1053 Smaller than U(eq) C110 by ... 0.01 AngSq These H atoms are bonded to C105. 301_ALERT_3_C Main Residue Disorder ......................... 9.00 Perc. Disordered ligands are common in these types of Mn6 materials. 313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O107 313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O108 Only 2 bonds for O107 and O108 are listed within the cif's atom bonding loop. This may arise because of close contacts of different parts of disordered groups. 371_ALERT_2_C Long C(sp2)-C(sp1) Bond C55 - C58 ... 1.43 Ang. This bond is not long, when compared to other C-C single bonds attached to a Ph ring at one end and a alkyne group at the other. The CSD finds 18 such structures with a mean bond length of 1.44(2)\%A. 432_ALERT_2_C Short Inter X...Y Contact C39 .. O108 .. 3.01 Ang. The O108 atom is a minor occupancy atom (only 0.25 occupancy). 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 30 No action. 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 2 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 4 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 12 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 2 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 4360 4358 2 23.01 0.550 1.000 5815 5813 2 25.24 0.600 0.999 7539 7533 6 #----------------------------------------------------------- ACTA Min. Res. --- 26.37 0.625 0.998 8525 8507 18 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 20 U(IJ)'S 0.0, 0.0050000 = C(25) TO C(28) DISTANCE 1.500000 , 0.050000 = C(109) TO C(110) DISTANCE 1.500000 , 0.050000 = C(101) TO C(102) U(IJ)'S 0.0, 0.010000 = C(109) TO C(110) U(IJ)'S 0.0, 0.010000 = C(301) TO C(310) ; _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 12.1777(3) _cell_length_b 12.3384(2) _cell_length_c 14.4043(3) _cell_angle_alpha 84.4970(10) _cell_angle_beta 89.042(2) _cell_angle_gamma 75.2140(10) _cell_volume 2082.91(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C80 H96 Mn6 N6 O26 # Dc = 1.50 Fooo = 977.00 Mu = 9.63 M = 943.62 # Found Formula = C80 H97.00 Mn6 N6 O26 # Dc = 1.51 FOOO = 977.00 Mu = 9.63 M = 944.12 _chemical_formula_sum 'C80 H97.00 Mn6 N6 O26' _chemical_formula_moiety 'C80 H97.00 Mn6 N6 O26' _chemical_compound_source ? _chemical_formula_weight 1888.24 _cell_measurement_reflns_used 5772 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 977.000 _exptl_absorpt_coefficient_mu 0.963 # Sheldrick geometric approximatio 0.77 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.93 _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 49999 _reflns_number_total 8507 _diffrn_reflns_av_R_equivalents 0.054 # Number of reflections with Friedels Law is 8507 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8519 _diffrn_reflns_theta_min 1.730 _diffrn_reflns_theta_max 26.371 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.371 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 1.58 _oxford_diffrn_Wilson_scale 78.14 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.62 _refine_diff_density_max 0.81 # 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 8507 _refine_ls_number_restraints 20 _refine_ls_number_parameters 595 _oxford_refine_ls_R_factor_ref 0.0584 _refine_ls_wR_factor_ref 0.1085 _refine_ls_goodness_of_fit_ref 0.8922 _refine_ls_shift/su_max 0.001025 # The values computed from all data _oxford_reflns_number_all 8507 _refine_ls_R_factor_all 0.0584 _refine_ls_wR_factor_all 0.1085 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5460 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_gt 0.0880 # 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: 7.94 12.2 5.96 1.50 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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 1.00979(3) 0.90436(3) 0.08730(3) 0.0179 1.0000 Uani . . . . . . . O2 O 1.08368(15) 1.02827(15) 0.06219(13) 0.0205 1.0000 Uani . . . . . . . N3 N 1.05291(19) 1.10756(18) 0.12710(15) 0.0206 1.0000 Uani . . . . . . . Mn4 Mn 0.88920(3) 1.14952(3) 0.15785(3) 0.0211 1.0000 Uani . . . . . . . O5 O 0.88505(15) 1.00077(15) 0.13965(13) 0.0202 1.0000 Uani . . . . . . . Mn6 Mn 0.74571(3) 0.96202(3) 0.15789(3) 0.0197 1.0000 Uani . . . . . . . O7 O 0.80634(15) 0.82257(16) 0.10262(14) 0.0242 1.0000 Uani . . . . . . . N8 N 0.92259(18) 0.78658(19) 0.09822(15) 0.0209 1.0000 Uani . . . . . . . C9 C 0.9648(2) 0.6800(2) 0.09337(19) 0.0232 1.0000 Uani . . . . . . . C10 C 1.0889(2) 0.6363(2) 0.08518(19) 0.0236 1.0000 Uani . . . . . . . C11 C 1.1588(2) 0.7020(2) 0.04336(19) 0.0231 1.0000 Uani . . . . . . . O12 O 1.11756(16) 0.81139(15) 0.01161(13) 0.0224 1.0000 Uani . . . . . . . C13 C 1.2744(2) 0.6529(2) 0.0319(2) 0.0263 1.0000 Uani . . . . . . . C14 C 1.3218(2) 0.5429(3) 0.0651(2) 0.0318 1.0000 Uani . . . . . . . C15 C 1.2551(3) 0.4781(2) 0.1099(2) 0.0317 1.0000 Uani . . . . . . . C16 C 1.1401(3) 0.5244(2) 0.1185(2) 0.0280 1.0000 Uani . . . . . . . C17 C 0.8877(3) 0.6031(3) 0.0939(3) 0.0343 1.0000 Uani . . . . . . . O18 O 0.60380(16) 0.93051(17) 0.17613(14) 0.0259 1.0000 Uani . . . . . . . C19 C 0.5356(2) 0.9576(2) 0.24821(19) 0.0240 1.0000 Uani . . . . . . . C20 C 0.5308(3) 1.0524(3) 0.2969(2) 0.0311 1.0000 Uani . . . . . . . C21 C 0.4567(3) 1.0718(3) 0.3728(3) 0.0405 1.0000 Uani . . . . . . . C22 C 0.3853(3) 1.0036(3) 0.3981(3) 0.0428 1.0000 Uani . . . . . . . C23 C 0.3866(3) 0.9136(3) 0.3477(2) 0.0373 1.0000 Uani . . . . . . . C24 C 0.4613(3) 0.8896(3) 0.2750(2) 0.0305 1.0000 Uani . . . . . . . C25 C 0.5963(3) 1.1351(3) 0.2680(3) 0.0407 1.0000 Uani . U . . . . . N26 N 0.6821(2) 1.10849(19) 0.21380(17) 0.0245 1.0000 Uani . . . . . . . O27 O 0.73162(17) 1.19399(17) 0.18433(16) 0.0304 1.0000 Uani . . . . . . . C28 C 0.5590(4) 1.2523(4) 0.2971(4) 0.0722 1.0000 Uani . U . . . . . O29 O 0.80117(17) 0.87687(18) 0.29980(15) 0.0301 1.0000 Uani . . . . . . . O32 O 0.68896(17) 1.06691(19) 0.02376(15) 0.0308 1.0000 Uani . . . . . . . O37 O 0.90307(17) 1.29375(17) 0.17545(15) 0.0294 1.0000 Uani . . . . . . . C38 C 0.9883(3) 1.3047(2) 0.2276(2) 0.0295 1.0000 Uani . . . . . . . C39 C 0.9658(3) 1.3895(3) 0.2891(3) 0.0393 1.0000 Uani . . . . . . . C40 C 1.0501(4) 1.4048(3) 0.3453(3) 0.0507 1.0000 Uani . . . . . . . C41 C 1.1590(4) 1.3371(4) 0.3415(3) 0.0518 1.0000 Uani . . . . . . . C42 C 1.1835(3) 1.2548(3) 0.2808(3) 0.0417 1.0000 Uani . . . . . . . C43 C 1.0999(3) 1.2368(3) 0.2223(2) 0.0287 1.0000 Uani . . . . . . . C44 C 1.1321(2) 1.1481(2) 0.1582(2) 0.0251 1.0000 Uani . . . . . . . C45 C 1.2519(3) 1.1073(3) 0.1283(2) 0.0371 1.0000 Uani . . . . . . . O46 O 0.93387(19) 1.08907(17) 0.30453(14) 0.0306 1.0000 Uani . . . . . . . C47 C 0.9018(3) 1.1386(3) 0.3894(2) 0.0347 1.0000 Uani . . . . . . . C48 C 0.8383(3) 1.0714(3) 0.4526(2) 0.0448 1.0000 Uani . . . . . . . O49 O 1.11346(17) 0.83617(17) 0.20715(14) 0.0271 1.0000 Uani . . . . . . . C50 C 1.0965(2) 0.8131(2) 0.2919(2) 0.0248 1.0000 Uani . . . . . . . O51 O 1.01847(17) 0.86847(17) 0.34033(15) 0.0293 1.0000 Uani . . . . . . . C52 C 1.1774(2) 0.7106(2) 0.3413(2) 0.0242 1.0000 Uani . . . . . . . C53 C 1.2690(3) 0.6488(3) 0.2954(2) 0.0319 1.0000 Uani . . . . . . . C54 C 1.3417(3) 0.5546(3) 0.3418(2) 0.0384 1.0000 Uani . . . . . . . C55 C 1.3237(3) 0.5221(3) 0.4349(2) 0.0331 1.0000 Uani . . . . . . . C56 C 1.2312(3) 0.5848(3) 0.4804(2) 0.0357 1.0000 Uani . . . . . . . C57 C 1.1585(3) 0.6779(3) 0.4341(2) 0.0316 1.0000 Uani . . . . . . . C58 C 1.3975(3) 0.4248(3) 0.4835(3) 0.0423 1.0000 Uani . . . . . . . C59 C 1.4546(4) 0.3442(3) 0.5261(3) 0.0587 1.0000 Uani . . . . . . . C300 C 0.7674(7) 0.7930(7) 0.3620(7) 0.0436 0.5320 Uani . . . 1 2 . . C301 C 0.7942(10) 0.7609(10) 0.3235(7) 0.0471 0.4680 Uani . U . 1 1 . . C310 C 0.8041(11) 0.7357(10) 0.4253(7) 0.0701 0.4680 Uani . U . 1 1 . . C311 C 0.8475(7) 0.6821(6) 0.3688(7) 0.0528 0.5320 Uani . . . 1 2 . . H131 H 1.3187 0.6963 0.0021 0.0329 1.0000 Uiso . . . . . . . H141 H 1.3985 0.5124 0.0583 0.0364 1.0000 Uiso . . . . . . . H151 H 1.2875 0.4040 0.1334 0.0372 1.0000 Uiso . . . . . . . H161 H 1.0950 0.4805 0.1476 0.0347 1.0000 Uiso . . . . . . . H171 H 0.9290 0.5278 0.0874 0.0533 1.0000 Uiso . . . . . . . H172 H 0.8454 0.6073 0.1490 0.0534 1.0000 Uiso . . . . . . . H173 H 0.8368 0.6281 0.0428 0.0534 1.0000 Uiso . . . . . . . H211 H 0.4563 1.1323 0.4063 0.0514 1.0000 Uiso . . . . . . . H221 H 0.3374 1.0177 0.4487 0.0532 1.0000 Uiso . . . . . . . H231 H 0.3380 0.8676 0.3628 0.0456 1.0000 Uiso . . . . . . . H241 H 0.4634 0.8282 0.2428 0.0377 1.0000 Uiso . . . . . . . H391 H 0.8928 1.4350 0.2910 0.0504 1.0000 Uiso . . . . . . . H401 H 1.0326 1.4608 0.3856 0.0675 1.0000 Uiso . . . . . . . H411 H 1.2155 1.3467 0.3794 0.0699 1.0000 Uiso . . . . . . . H421 H 1.2563 1.2102 0.2772 0.0530 1.0000 Uiso . . . . . . . H451 H 1.2974 1.1538 0.1455 0.0601 1.0000 Uiso . . . . . . . H452 H 1.2546 1.1042 0.0624 0.0593 1.0000 Uiso . . . . . . . H453 H 1.2807 1.0334 0.1573 0.0600 1.0000 Uiso . . . . . . . H472 H 0.9682 1.1452 0.4216 0.0459 1.0000 Uiso . . . . . . . H471 H 0.8529 1.2125 0.3733 0.0457 1.0000 Uiso . . . . . . . H483 H 0.8162 1.1076 0.5084 0.0747 1.0000 Uiso . . . . . . . H481 H 0.8853 0.9965 0.4676 0.0749 1.0000 Uiso . . . . . . . H482 H 0.7711 1.0671 0.4201 0.0746 1.0000 Uiso . . . . . . . H531 H 1.2826 0.6691 0.2337 0.0389 1.0000 Uiso . . . . . . . H541 H 1.4024 0.5130 0.3111 0.0450 1.0000 Uiso . . . . . . . H561 H 1.2189 0.5659 0.5423 0.0446 1.0000 Uiso . . . . . . . H571 H 1.0966 0.7193 0.4641 0.0372 1.0000 Uiso . . . . . . . H591 H 1.4994 0.2802 0.5579 0.0691 1.0000 Uiso . . . . . . . H3002 H 0.7583 0.8185 0.4231 0.0505 0.5320 Uiso . . . 1 2 . . H3001 H 0.6944 0.7879 0.3408 0.0500 0.5320 Uiso . . . 1 2 . . H3011 H 0.8568 0.7093 0.2949 0.0511 0.4680 Uiso . . . 1 1 . . H3012 H 0.7242 0.7505 0.3017 0.0510 0.4680 Uiso . . . 1 1 . . H3113 H 0.8165 0.6276 0.4032 0.0808 0.5320 Uiso . . . 1 2 . . H3111 H 0.9164 0.6856 0.3979 0.0812 0.5320 Uiso . . . 1 2 . . H3112 H 0.8656 0.6602 0.3068 0.0812 0.5320 Uiso . . . 1 2 . . H291 H 0.8675 0.8709 0.3123 0.0469 1.0000 Uiso . . . . . . . H461 H 0.9636 1.0229 0.3160 0.0466 1.0000 Uiso . . . . . . . C101 C 0.5849(5) 1.1148(6) -0.0285(5) 0.0358 0.5000 Uani D . . 2 1 . . C102 C 0.4955(6) 1.1810(7) 0.0295(6) 0.0450 0.5000 Uani D . . 2 1 . . H1011 H 0.6005 1.1634 -0.0814 0.0419 0.5000 Uiso . . . 2 1 . . H1012 H 0.5589 1.0555 -0.0503 0.0420 0.5000 Uiso . . . 2 1 . . H1021 H 0.4260 1.2021 -0.0048 0.0670 0.5000 Uiso . . . 2 1 . . H1022 H 0.5149 1.2468 0.0473 0.0668 0.5000 Uiso . . . 2 1 . . H1023 H 0.4848 1.1351 0.0851 0.0670 0.5000 Uiso . . . 2 1 . . H321 H 0.7363 1.0812 -0.0104 0.0474 1.0000 Uiso . . . . . . . H322 H 0.6208 1.0898 0.0100 0.0379 0.5000 Uiso . . . 2 2 . . H281 H 0.4957 1.2575 0.3375 0.1070 0.5000 Uiso . . . . . . . H282 H 0.6204 1.2666 0.3311 0.1070 0.5000 Uiso . . . . . . . H283 H 0.5406 1.3043 0.2447 0.1070 0.5000 Uiso . . . . . . . H284 H 0.6104 1.2939 0.2742 0.1068 0.5000 Uiso . . . . . . . H285 H 0.5606 1.2472 0.3646 0.1068 0.5000 Uiso . . . . . . . H286 H 0.4850 1.2866 0.2759 0.1068 0.5000 Uiso . . . . . . . C109 C 0.3647(8) 1.5015(8) -0.1816(7) 0.0614 0.5000 Uani D U . 3 . . . O107 O 0.4205(10) 1.5838(10) -0.1590(9) 0.0609 0.2500 Uani . . . 3 1 . . O108 O 0.2847(8) 1.5499(7) -0.2445(7) 0.0399 0.2500 Uani . . . 3 2 . . C110 C 0.4236(10) 1.3855(10) -0.1949(11) 0.0819 0.5000 Uani D U . 3 . . . H1091 H 0.4196 1.5438 -0.1846 0.0783 0.2500 Uiso . . . 3 2 . . H1092 H 0.3298 1.5035 -0.1223 0.0783 0.2500 Uiso . . . 3 2 . . H1093 H 0.3254 1.5303 -0.2392 0.0783 0.2500 Uiso . . . 3 1 . . H1094 H 0.3108 1.4983 -0.1338 0.0783 0.2500 Uiso . . . 3 1 . . O103 O 0.4859(4) 1.1699(5) -0.0429(5) 0.0527 0.5000 Uani . . . 2 2 . . C104 C 0.4260(6) 1.2821(7) -0.0338(6) 0.0497 0.5000 Uani . . . 2 2 . . C105 C 0.4155(6) 1.3595(8) -0.1244(8) 0.0548 0.5000 Uani . . . 2 2 . . H1041 H 0.4669 1.3099 0.0123 0.0630 0.5000 Uiso . . . 2 2 . . H1042 H 0.3508 1.2830 -0.0107 0.0629 0.5000 Uiso . . . 2 2 . . H1031 H 0.4506 1.1201 -0.0725 0.0500 1.0000 Uiso . . . . . . . H1101 H 0.3686 1.3460 -0.2087 0.0972 0.5000 Uiso . . . 3 . . . H1102 H 0.4751 1.3842 -0.2441 0.0972 0.5000 Uiso . . . 3 . . . H1103 H 0.4622 1.3508 -0.1386 0.0972 0.5000 Uiso . . . 3 . . . H1051 H 0.3751 1.4332 -0.1134 0.0683 0.5000 Uiso . . . 2 2 . . H1052 H 0.4900 1.3602 -0.1462 0.0683 0.5000 Uiso . . . 2 2 . . H1053 H 0.3773 1.3318 -0.1699 0.0683 0.5000 Uiso . . . 2 2 . . H1071 H 0.3774 1.6468 -0.1667 0.0709 0.2500 Uiso . . . 3 1 . . H1081 H 0.2300 1.5954 -0.2245 0.0476 0.2500 Uiso . . . 3 2 . . H3101 H 0.7998 0.6606 0.4415 0.0901 0.4680 Uiso . . . 1 1 . . H3102 H 0.8750 0.7444 0.4452 0.0901 0.4680 Uiso . . . 1 1 . . H3103 H 0.7442 0.7863 0.4539 0.0901 0.4680 Uiso . . . 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 0.01513(19) 0.01804(19) 0.0203(2) -0.00121(15) 0.00210(14) -0.00436(15) O2 0.0184(9) 0.0218(9) 0.0216(9) -0.0033(7) 0.0026(7) -0.0057(7) N3 0.0218(11) 0.0194(11) 0.0201(11) -0.0013(8) 0.0042(8) -0.0049(9) Mn4 0.0181(2) 0.0190(2) 0.0277(2) -0.00427(16) 0.00519(16) -0.00678(15) O5 0.0166(9) 0.0197(9) 0.0247(10) -0.0036(7) 0.0021(7) -0.0051(7) Mn6 0.01515(19) 0.0200(2) 0.0244(2) -0.00268(15) 0.00246(15) -0.00503(15) O7 0.0160(9) 0.0251(10) 0.0330(11) -0.0061(8) 0.0009(8) -0.0068(7) N8 0.0176(10) 0.0246(11) 0.0198(11) -0.0019(9) 0.0019(8) -0.0040(9) C9 0.0234(13) 0.0228(13) 0.0244(14) -0.0014(10) 0.0010(10) -0.0079(11) C10 0.0238(13) 0.0222(13) 0.0238(14) -0.0040(10) -0.0009(11) -0.0037(11) C11 0.0240(13) 0.0221(13) 0.0222(13) -0.0023(10) -0.0012(10) -0.0038(10) O12 0.0217(9) 0.0205(9) 0.0235(10) 0.0012(7) 0.0034(7) -0.0038(7) C13 0.0206(13) 0.0266(14) 0.0298(15) -0.0006(11) 0.0039(11) -0.0033(11) C14 0.0208(14) 0.0314(15) 0.0389(17) -0.0043(13) 0.0019(12) 0.0017(12) C15 0.0304(15) 0.0231(14) 0.0375(17) 0.0000(12) 0.0011(13) -0.0005(12) C16 0.0294(15) 0.0237(14) 0.0309(15) -0.0009(11) 0.0035(12) -0.0079(11) C17 0.0256(15) 0.0254(15) 0.054(2) -0.0073(13) 0.0021(13) -0.0087(12) O18 0.0179(9) 0.0305(10) 0.0314(11) -0.0060(8) 0.0036(8) -0.0090(8) C19 0.0187(12) 0.0290(14) 0.0237(14) 0.0022(11) -0.0001(10) -0.0063(11) C20 0.0246(14) 0.0351(16) 0.0351(16) -0.0065(13) 0.0092(12) -0.0096(12) C21 0.0356(17) 0.048(2) 0.0422(19) -0.0142(16) 0.0141(15) -0.0156(15) C22 0.0393(19) 0.053(2) 0.0388(19) -0.0039(16) 0.0183(15) -0.0177(16) C23 0.0286(16) 0.0403(18) 0.0423(19) 0.0094(14) 0.0085(13) -0.0127(13) C24 0.0272(15) 0.0287(15) 0.0352(16) 0.0028(12) 0.0006(12) -0.0089(12) C25 0.0298(15) 0.0356(17) 0.063(2) -0.0219(16) 0.0228(15) -0.0153(13) N26 0.0210(11) 0.0229(11) 0.0311(13) -0.0014(10) 0.0033(9) -0.0090(9) O27 0.0222(10) 0.0228(10) 0.0473(13) -0.0051(9) 0.0107(9) -0.0075(8) C28 0.060(2) 0.052(2) 0.116(3) -0.043(2) 0.053(2) -0.0260(19) O29 0.0257(10) 0.0320(11) 0.0327(11) 0.0058(9) -0.0027(8) -0.0108(9) O32 0.0196(9) 0.0411(12) 0.0287(11) 0.0034(9) 0.0008(8) -0.0047(9) O37 0.0282(10) 0.0230(10) 0.0405(12) -0.0075(9) 0.0053(9) -0.0114(8) C38 0.0380(16) 0.0275(15) 0.0298(15) -0.0050(12) 0.0093(12) -0.0205(13) C39 0.049(2) 0.0320(16) 0.0430(19) -0.0090(14) 0.0156(15) -0.0203(15) C40 0.075(3) 0.049(2) 0.042(2) -0.0224(17) 0.0133(19) -0.036(2) C41 0.064(3) 0.061(2) 0.045(2) -0.0208(19) 0.0001(18) -0.038(2) C42 0.046(2) 0.048(2) 0.0381(18) -0.0101(15) -0.0024(15) -0.0237(16) C43 0.0343(16) 0.0303(15) 0.0275(15) -0.0032(12) 0.0021(12) -0.0190(12) C44 0.0229(13) 0.0290(14) 0.0245(14) 0.0000(11) 0.0001(11) -0.0096(11) C45 0.0251(15) 0.052(2) 0.0388(18) -0.0120(15) -0.0007(13) -0.0151(14) O46 0.0431(12) 0.0245(10) 0.0244(10) -0.0045(8) 0.0067(9) -0.0085(9) C47 0.0477(19) 0.0372(17) 0.0243(15) -0.0081(13) 0.0096(13) -0.0187(14) C48 0.061(2) 0.054(2) 0.0293(17) -0.0105(15) 0.0179(16) -0.0319(19) O49 0.0244(10) 0.0303(10) 0.0252(10) 0.0023(8) -0.0054(8) -0.0057(8) C50 0.0242(14) 0.0248(14) 0.0272(14) -0.0019(11) -0.0031(11) -0.0096(11) O51 0.0257(10) 0.0297(11) 0.0306(11) 0.0003(8) 0.0005(8) -0.0045(8) C52 0.0236(13) 0.0232(13) 0.0264(14) -0.0027(11) -0.0030(11) -0.0070(11) C53 0.0311(16) 0.0370(16) 0.0245(15) -0.0011(12) -0.0024(12) -0.0033(13) C54 0.0333(17) 0.0368(17) 0.0380(18) -0.0075(14) -0.0026(14) 0.0056(14) C55 0.0400(17) 0.0278(15) 0.0313(16) -0.0008(12) -0.0115(13) -0.0084(13) C56 0.0440(18) 0.0334(16) 0.0287(16) 0.0018(13) -0.0035(13) -0.0094(14) C57 0.0355(16) 0.0290(15) 0.0297(16) -0.0030(12) 0.0013(13) -0.0069(13) C58 0.046(2) 0.0387(19) 0.0396(19) -0.0014(15) -0.0084(15) -0.0064(15) C59 0.068(3) 0.040(2) 0.057(3) 0.0097(18) -0.021(2) 0.0026(19) C300 0.037(4) 0.039(4) 0.048(5) 0.020(4) 0.007(4) -0.007(3) C301 0.067(6) 0.057(6) 0.028(5) -0.002(4) -0.003(4) -0.036(5) C310 0.093(7) 0.078(6) 0.050(5) 0.009(5) 0.004(5) -0.047(5) C311 0.055(4) 0.023(3) 0.075(6) 0.012(4) 0.007(4) -0.007(3) C101 0.029(3) 0.041(4) 0.032(3) 0.000(3) -0.010(3) 0.001(3) C102 0.020(3) 0.063(5) 0.049(5) -0.001(4) 0.005(3) -0.008(3) C109 0.053(5) 0.056(5) 0.085(6) -0.027(4) 0.009(4) -0.026(4) O107 0.055(7) 0.047(6) 0.077(8) -0.002(6) -0.008(6) -0.007(5) O108 0.029(5) 0.028(4) 0.060(6) -0.015(4) -0.009(4) 0.003(4) C110 0.063(6) 0.068(6) 0.110(8) -0.003(6) 0.012(6) -0.012(5) O103 0.034(3) 0.050(3) 0.073(4) -0.026(3) -0.020(3) 0.002(2) C104 0.030(3) 0.057(5) 0.066(5) -0.021(4) -0.004(3) -0.012(3) C105 0.027(4) 0.065(5) 0.078(6) -0.029(5) 0.003(4) -0.014(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.11687(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 . O2 2_775 2.4247(19) yes Mn1 . Mn1 2_775 3.2475(8) yes Mn1 . O2 . 1.9655(18) yes Mn1 . Mn4 . 3.2574(5) yes Mn1 . O5 . 1.8714(18) yes Mn1 . N8 . 2.001(2) yes Mn1 . O12 . 1.9107(19) yes Mn1 . O49 . 2.1294(19) yes O2 . N3 . 1.396(3) yes N3 . Mn4 . 1.981(2) yes N3 . C44 . 1.298(4) yes Mn4 . O12 2_775 2.4410(19) yes Mn4 . O5 . 1.8919(18) yes Mn4 . Mn6 . 3.2355(6) yes Mn4 . O27 . 1.899(2) yes Mn4 . O37 . 1.871(2) yes Mn4 . O46 . 2.201(2) yes O5 . Mn6 . 1.8848(18) yes Mn6 . O7 . 1.932(2) yes Mn6 . O18 . 1.8748(19) yes Mn6 . N26 . 2.015(2) yes Mn6 . O29 . 2.238(2) yes Mn6 . O32 . 2.235(2) yes O7 . N8 . 1.374(3) yes N8 . C9 . 1.292(4) yes C9 . C10 . 1.475(4) yes C9 . C17 . 1.496(4) yes C10 . C11 . 1.410(4) yes C10 . C16 . 1.403(4) yes C11 . O12 . 1.352(3) yes C11 . C13 . 1.397(4) yes C13 . C14 . 1.374(4) yes C13 . H131 . 0.926 no C14 . C15 . 1.390(5) yes C14 . H141 . 0.921 no C15 . C16 . 1.379(4) yes C15 . H151 . 0.931 no C16 . H161 . 0.934 no C17 . H171 . 0.950 no C17 . H172 . 0.937 no C17 . H173 . 0.946 no O18 . C19 . 1.332(3) yes C19 . C20 . 1.408(4) yes C19 . C24 . 1.409(4) yes C20 . C21 . 1.405(4) yes C20 . C25 . 1.474(4) yes C21 . C22 . 1.379(5) yes C21 . H211 . 0.925 no C22 . C23 . 1.381(5) yes C22 . H221 . 0.927 no C23 . C24 . 1.379(4) yes C23 . H231 . 0.929 no C24 . H241 . 0.920 no C25 . N26 . 1.287(4) yes C25 . C28 . 1.499(5) yes N26 . O27 . 1.374(3) yes C28 . H281 . 0.951 no C28 . H282 . 0.962 no C28 . H283 . 0.933 no C28 . H284 . 0.943 no C28 . H285 . 0.969 no C28 . H286 . 0.935 no O29 . C301 . 1.463(10) yes O29 . H291 . 0.814 no O29 . C300 . 1.438(8) yes O29 . H291 . 0.814 no O32 . C101 . 1.445(6) yes O32 . H321 . 0.794 no O32 . H321 . 0.794 no O32 . H322 . 0.826 no O37 . C38 . 1.333(4) yes C38 . C39 . 1.407(4) yes C38 . C43 . 1.407(4) yes C39 . C40 . 1.379(6) yes C39 . H391 . 0.923 no C40 . C41 . 1.378(6) yes C40 . H401 . 0.926 no C41 . C42 . 1.374(5) yes C41 . H411 . 0.924 no C42 . C43 . 1.406(4) yes C42 . H421 . 0.920 no C43 . C44 . 1.472(4) yes C44 . C45 . 1.488(4) yes C45 . H451 . 0.944 no C45 . H452 . 0.953 no C45 . H453 . 0.947 no O46 . C47 . 1.423(4) yes O46 . H461 . 0.806 no C47 . C48 . 1.508(4) yes C47 . H472 . 0.964 no C47 . H471 . 0.962 no C48 . H483 . 0.957 no C48 . H481 . 0.960 no C48 . H482 . 0.966 no O49 . C50 . 1.252(4) yes C50 . O51 . 1.263(4) yes C50 . C52 . 1.514(4) yes C52 . C53 . 1.378(4) yes C52 . C57 . 1.391(4) yes C53 . C54 . 1.389(4) yes C53 . H531 . 0.923 no C54 . C55 . 1.392(5) yes C54 . H541 . 0.919 no C55 . C56 . 1.387(5) yes C55 . C58 . 1.432(5) yes C56 . C57 . 1.379(4) yes C56 . H561 . 0.919 no C57 . H571 . 0.924 no C58 . C59 . 1.180(5) yes C59 . H591 . 0.923 no C300 . C311 . 1.459(11) yes C300 . H3002 . 0.959 no C300 . H3001 . 0.964 no C301 . C310 . 1.471(13) yes C301 . H3011 . 0.973 no C301 . H3012 . 0.956 no C310 . H3101 . 0.948 no C310 . H3102 . 0.950 no C310 . H3103 . 0.947 no C311 . H3113 . 0.949 no C311 . H3111 . 0.957 no C311 . H3112 . 0.964 no C101 . C102 . 1.482(10) yes C101 . H1011 . 0.970 no C101 . H1012 . 0.949 no C102 . H1021 . 0.951 no C102 . H1022 . 0.960 no C102 . H1023 . 0.963 no C109 . C110 . 1.457(14) yes C109 . O107 . 1.423(15) yes C109 . H1093 . 0.955 no C109 . H1094 . 0.949 no C109 . O108 . 1.325(14) yes C109 . H1091 . 0.947 no C109 . H1092 . 0.947 no O107 . H1071 . 0.817 no O108 . H1081 . 0.822 no C110 . H1101 . 0.956 no C110 . H1102 . 0.937 no C110 . H1103 . 0.951 no O103 . C104 . 1.407(9) yes O103 . H1031 . 0.968 no C104 . C105 . 1.528(14) yes C104 . H1041 . 0.974 no C104 . H1042 . 0.967 no C105 . H1051 . 0.944 no C105 . H1052 . 0.957 no C105 . H1053 . 0.947 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 2_775 Mn1 . Mn1 2_775 37.09(4) yes O2 2_775 Mn1 . O2 . 85.16(7) yes Mn1 2_775 Mn1 . O2 . 48.07(5) yes O2 2_775 Mn1 . Mn4 . 87.85(4) yes Mn1 2_775 Mn1 . Mn4 . 71.123(15) yes O2 . Mn1 . Mn4 . 60.78(5) yes O2 2_775 Mn1 . O5 . 86.45(7) yes Mn1 2_775 Mn1 . O5 . 87.83(6) yes O2 . Mn1 . O5 . 90.79(8) yes Mn4 . Mn1 . O5 . 30.23(5) yes O2 2_775 Mn1 . N8 . 87.56(8) yes Mn1 2_775 Mn1 . N8 . 124.64(7) yes O2 . Mn1 . N8 . 172.67(9) yes Mn4 . Mn1 . N8 . 118.10(6) yes O5 . Mn1 . N8 . 87.87(8) yes O2 2_775 Mn1 . O12 . 82.12(7) yes Mn1 2_775 Mn1 . O12 . 84.81(6) yes O2 . Mn1 . O12 . 91.13(8) yes Mn4 . Mn1 . O12 . 150.95(6) yes O5 . Mn1 . O12 . 168.20(8) yes O2 2_775 Mn1 . O49 . 171.67(7) yes Mn1 2_775 Mn1 . O49 . 139.82(6) yes O2 . Mn1 . O49 . 92.39(8) yes Mn4 . Mn1 . O49 . 97.93(6) yes O5 . Mn1 . O49 . 101.57(8) yes N8 . Mn1 . O12 . 88.75(9) yes N8 . Mn1 . O49 . 94.94(8) yes O12 . Mn1 . O49 . 89.98(8) yes Mn1 2_775 O2 . Mn1 . 94.84(7) yes Mn1 2_775 O2 . N3 . 112.02(14) yes Mn1 . O2 . N3 . 111.79(14) yes O2 . N3 . Mn4 . 115.13(16) yes O2 . N3 . C44 . 117.6(2) yes Mn4 . N3 . C44 . 127.23(19) yes N3 . Mn4 . O12 2_775 78.75(8) yes N3 . Mn4 . Mn1 . 58.79(7) yes O12 2_775 Mn4 . Mn1 . 77.31(4) yes N3 . Mn4 . O5 . 88.15(8) yes O12 2_775 Mn4 . O5 . 87.38(7) yes Mn1 . Mn4 . O5 . 29.87(5) yes N3 . Mn4 . Mn6 . 119.13(7) yes O12 2_775 Mn4 . Mn6 . 93.83(5) yes Mn1 . Mn4 . Mn6 . 60.636(12) yes O5 . Mn4 . Mn6 . 30.99(5) yes N3 . Mn4 . O27 . 178.08(9) yes O12 2_775 Mn4 . O27 . 99.80(8) yes Mn1 . Mn4 . O27 . 122.24(6) yes O5 . Mn4 . O27 . 93.05(8) yes Mn6 . Mn4 . O27 . 62.09(6) yes N3 . Mn4 . O37 . 88.37(9) yes O12 2_775 Mn4 . O37 . 92.55(8) yes Mn1 . Mn4 . O37 . 146.79(7) yes O5 . Mn4 . O37 . 176.47(9) yes Mn6 . Mn4 . O37 . 152.48(7) yes N3 . Mn4 . O46 . 89.00(9) yes O12 2_775 Mn4 . O46 . 166.84(7) yes Mn1 . Mn4 . O46 . 92.31(5) yes O5 . Mn4 . O46 . 87.45(8) yes Mn6 . Mn4 . O46 . 87.93(6) yes O27 . Mn4 . O37 . 90.44(9) yes O27 . Mn4 . O46 . 92.55(9) yes O37 . Mn4 . O46 . 91.87(9) yes Mn4 . O5 . Mn1 . 119.89(9) yes Mn4 . O5 . Mn6 . 117.90(9) yes Mn1 . O5 . Mn6 . 121.53(10) yes O5 . Mn6 . Mn4 . 31.12(5) yes O5 . Mn6 . O7 . 90.55(8) yes Mn4 . Mn6 . O7 . 121.01(6) yes O5 . Mn6 . O18 . 177.37(9) yes Mn4 . Mn6 . O18 . 146.31(6) yes O7 . Mn6 . O18 . 91.87(8) yes O5 . Mn6 . N26 . 89.33(9) yes Mn4 . Mn6 . N26 . 58.78(7) yes O7 . Mn6 . N26 . 179.24(9) yes O18 . Mn6 . N26 . 88.24(9) yes O5 . Mn6 . O29 . 91.23(8) yes Mn4 . Mn6 . O29 . 96.41(5) yes O7 . Mn6 . O29 . 90.75(8) yes O18 . Mn6 . O29 . 89.78(8) yes N26 . Mn6 . O29 . 90.00(9) yes O5 . Mn6 . O32 . 86.50(8) yes Mn4 . Mn6 . O32 . 78.26(6) yes O7 . Mn6 . O32 . 95.93(8) yes O18 . Mn6 . O32 . 92.21(8) yes N26 . Mn6 . O32 . 83.31(9) yes O29 . Mn6 . O32 . 172.96(8) yes Mn6 . O7 . N8 . 116.37(15) yes O7 . N8 . Mn1 . 117.42(16) yes O7 . N8 . C9 . 116.5(2) yes Mn1 . N8 . C9 . 125.77(19) yes N8 . C9 . C10 . 119.3(2) yes N8 . C9 . C17 . 119.8(2) yes C10 . C9 . C17 . 120.8(2) yes C9 . C10 . C11 . 122.6(2) yes C9 . C10 . C16 . 119.4(3) yes C11 . C10 . C16 . 118.0(3) yes C10 . C11 . O12 . 122.2(2) yes C10 . C11 . C13 . 119.6(3) yes O12 . C11 . C13 . 118.1(2) yes C11 . O12 . Mn4 2_775 115.16(16) yes C11 . O12 . Mn1 . 117.73(16) yes Mn4 2_775 O12 . Mn1 . 120.28(9) yes C11 . C13 . C14 . 120.8(3) yes C11 . C13 . H131 . 118.6 no C14 . C13 . H131 . 120.6 no C13 . C14 . C15 . 120.4(3) yes C13 . C14 . H141 . 119.7 no C15 . C14 . H141 . 119.8 no C14 . C15 . C16 . 119.3(3) yes C14 . C15 . H151 . 120.4 no C16 . C15 . H151 . 120.3 no C10 . C16 . C15 . 121.8(3) yes C10 . C16 . H161 . 118.9 no C15 . C16 . H161 . 119.3 no C9 . C17 . H171 . 111.4 no C9 . C17 . H172 . 109.5 no H171 . C17 . H172 . 110.9 no C9 . C17 . H173 . 108.0 no H171 . C17 . H173 . 108.5 no H172 . C17 . H173 . 108.4 no Mn6 . O18 . C19 . 125.44(18) yes O18 . C19 . C20 . 123.8(3) yes O18 . C19 . C24 . 117.9(3) yes C20 . C19 . C24 . 118.3(3) yes C19 . C20 . C21 . 118.8(3) yes C19 . C20 . C25 . 122.3(3) yes C21 . C20 . C25 . 118.8(3) yes C20 . C21 . C22 . 121.8(3) yes C20 . C21 . H211 . 118.5 no C22 . C21 . H211 . 119.7 no C21 . C22 . C23 . 119.2(3) yes C21 . C22 . H221 . 120.4 no C23 . C22 . H221 . 120.4 no C22 . C23 . C24 . 120.5(3) yes C22 . C23 . H231 . 120.4 no C24 . C23 . H231 . 119.1 no C19 . C24 . C23 . 121.3(3) yes C19 . C24 . H241 . 118.5 no C23 . C24 . H241 . 120.1 no C20 . C25 . N26 . 120.0(3) yes C20 . C25 . C28 . 120.1(3) yes N26 . C25 . C28 . 119.9(3) yes Mn6 . N26 . C25 . 128.7(2) yes Mn6 . N26 . O27 . 115.44(16) yes C25 . N26 . O27 . 115.6(2) yes N26 . O27 . Mn4 . 115.87(16) yes C25 . C28 . H281 . 109.1 no C25 . C28 . H282 . 108.3 no H281 . C28 . H282 . 108.4 no C25 . C28 . H283 . 110.1 no H281 . C28 . H283 . 110.9 no H282 . C28 . H283 . 109.9 no C25 . C28 . H284 . 109.6 no H281 . C28 . H284 . 140.9 no H282 . C28 . H284 . 53.3 no H283 . C28 . H284 . 59.4 no C25 . C28 . H285 . 108.0 no H281 . C28 . H285 . 53.3 no H282 . C28 . H285 . 58.0 no H283 . C28 . H285 . 141.9 no H284 . C28 . H285 . 108.5 no C25 . C28 . H286 . 110.1 no H281 . C28 . H286 . 58.6 no H282 . C28 . H286 . 141.6 no H283 . C28 . H286 . 55.4 no H284 . C28 . H286 . 111.5 no H285 . C28 . H286 . 109.1 no Mn6 . O29 . C301 . 119.4(4) yes Mn6 . O29 . H291 . 114.6 no C301 . O29 . H291 . 100.6 no Mn6 . O29 . C300 . 135.0(4) yes Mn6 . O29 . H291 . 114.6 no C300 . O29 . H291 . 105.5 no Mn6 . O32 . C101 . 138.6(3) yes Mn6 . O32 . H321 . 118.0 no C101 . O32 . H321 . 103.3 no Mn6 . O32 . H321 . 118.0 no Mn6 . O32 . H322 . 120.9 no H321 . O32 . H322 . 121.1 no Mn4 . O37 . C38 . 119.31(19) yes O37 . C38 . C39 . 118.3(3) yes O37 . C38 . C43 . 122.9(3) yes C39 . C38 . C43 . 118.8(3) yes C38 . C39 . C40 . 121.1(3) yes C38 . C39 . H391 . 118.3 no C40 . C39 . H391 . 120.6 no C39 . C40 . C41 . 120.2(3) yes C39 . C40 . H401 . 119.2 no C41 . C40 . H401 . 120.6 no C40 . C41 . C42 . 119.8(4) yes C40 . C41 . H411 . 120.4 no C42 . C41 . H411 . 119.9 no C41 . C42 . C43 . 121.7(4) yes C41 . C42 . H421 . 120.2 no C43 . C42 . H421 . 118.1 no C38 . C43 . C42 . 118.4(3) yes C38 . C43 . C44 . 122.7(3) yes C42 . C43 . C44 . 119.0(3) yes C43 . C44 . N3 . 118.3(3) yes C43 . C44 . C45 . 121.0(3) yes N3 . C44 . C45 . 120.7(3) yes C44 . C45 . H451 . 111.8 no C44 . C45 . H452 . 109.8 no H451 . C45 . H452 . 109.6 no C44 . C45 . H453 . 107.8 no H451 . C45 . H453 . 109.4 no H452 . C45 . H453 . 108.4 no Mn4 . O46 . C47 . 132.29(19) yes Mn4 . O46 . H461 . 117.1 no C47 . O46 . H461 . 109.3 no O46 . C47 . C48 . 112.1(3) yes O46 . C47 . H472 . 110.0 no C48 . C47 . H472 . 109.4 no O46 . C47 . H471 . 107.2 no C48 . C47 . H471 . 108.9 no H472 . C47 . H471 . 109.3 no C47 . C48 . H483 . 110.2 no C47 . C48 . H481 . 109.7 no H483 . C48 . H481 . 110.4 no C47 . C48 . H482 . 108.4 no H483 . C48 . H482 . 109.1 no H481 . C48 . H482 . 109.0 no Mn1 . O49 . C50 . 135.85(19) yes O49 . C50 . O51 . 125.8(3) yes O49 . C50 . C52 . 117.3(3) yes O51 . C50 . C52 . 116.9(3) yes C50 . C52 . C53 . 120.9(3) yes C50 . C52 . C57 . 119.5(3) yes C53 . C52 . C57 . 119.6(3) yes C52 . C53 . C54 . 120.0(3) yes C52 . C53 . H531 . 120.8 no C54 . C53 . H531 . 119.3 no C53 . C54 . C55 . 120.6(3) yes C53 . C54 . H541 . 120.0 no C55 . C54 . H541 . 119.4 no C54 . C55 . C56 . 118.9(3) yes C54 . C55 . C58 . 121.3(3) yes C56 . C55 . C58 . 119.8(3) yes C55 . C56 . C57 . 120.4(3) yes C55 . C56 . H561 . 120.3 no C57 . C56 . H561 . 119.3 no C52 . C57 . C56 . 120.4(3) yes C52 . C57 . H571 . 119.1 no C56 . C57 . H571 . 120.5 no C55 . C58 . C59 . 177.1(5) yes C58 . C59 . H591 . 178.4 no O29 . C300 . C311 . 114.7(7) yes O29 . C300 . H3002 . 108.5 no C311 . C300 . H3002 . 108.0 no O29 . C300 . H3001 . 107.3 no C311 . C300 . H3001 . 110.1 no H3002 . C300 . H3001 . 108.1 no O29 . C301 . C310 . 108.6(8) yes O29 . C301 . H3011 . 109.7 no C310 . C301 . H3011 . 108.5 no O29 . C301 . H3012 . 110.8 no C310 . C301 . H3012 . 110.4 no H3011 . C301 . H3012 . 108.8 no C301 . C310 . H3101 . 109.3 no C301 . C310 . H3102 . 109.0 no H3101 . C310 . H3102 . 109.7 no C301 . C310 . H3103 . 109.2 no H3101 . C310 . H3103 . 109.9 no H3102 . C310 . H3103 . 109.8 no C300 . C311 . H3113 . 111.3 no C300 . C311 . H3111 . 109.8 no H3113 . C311 . H3111 . 109.8 no C300 . C311 . H3112 . 108.8 no H3113 . C311 . H3112 . 109.4 no H3111 . C311 . H3112 . 107.7 no O32 . C101 . C102 . 111.6(5) yes O32 . C101 . H1011 . 108.7 no C102 . C101 . H1011 . 109.3 no O32 . C101 . H1012 . 108.7 no C102 . C101 . H1012 . 109.1 no H1011 . C101 . H1012 . 109.4 no C101 . C102 . H1021 . 108.7 no C101 . C102 . H1022 . 111.8 no H1021 . C102 . H1022 . 110.1 no C101 . C102 . H1023 . 109.6 no H1021 . C102 . H1023 . 107.9 no H1022 . C102 . H1023 . 108.7 no O107 . C109 . H1093 . 106.1 no O107 . C109 . H1094 . 105.8 no H1093 . C109 . H1094 . 109.1 no O108 . C109 . H1091 . 107.9 no O108 . C109 . H1092 . 107.5 no H1091 . C109 . H1092 . 110.0 no C109 . C110 . H1101 . 108.7 no C109 . C110 . H1102 . 109.8 no H1101 . C110 . H1102 . 110.0 no C109 . C110 . H1103 . 108.9 no H1101 . C110 . H1103 . 108.9 no H1102 . C110 . H1103 . 110.5 no C104 . O103 . H1031 . 120.5 no O103 . C104 . C105 . 114.0(7) yes O103 . C104 . H1041 . 106.7 no C105 . C104 . H1041 . 109.1 no O103 . C104 . H1042 . 108.9 no C105 . C104 . H1042 . 109.0 no H1041 . C104 . H1042 . 109.0 no C104 . C105 . H1051 . 109.6 no C104 . C105 . H1052 . 108.9 no H1051 . C105 . H1052 . 109.4 no C104 . C105 . H1053 . 109.4 no H1051 . C105 . H1053 . 110.3 no H1052 . C105 . H1053 . 109.2 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 . O108 2_685 142 0.92 2.23 3.014(7) yes C45 . H452 . O7 2_775 154 0.95 2.51 3.396(7) yes C45 . H452 . O32 2_775 127 0.95 2.49 3.162(7) yes O29 . H291 . O51 . 176 0.81 1.88 2.693(7) yes O46 . H461 . O51 . 174 0.81 1.85 2.656(7) yes O32 . H321 . O2 2_775 134 0.79 2.41 3.014(7) yes O32 . H321 . O12 2_775 138 0.79 2.47 3.112(7) yes C101 . H322 . O32 . 140 0.71 0.83 1.445(7) yes O32 . H322 . C102 . 147 0.83 1.69 2.421(7) yes O32 . H322 . O103 . 163 0.83 1.82 2.625(7) yes C28 . H283 . O107 2_685 149 0.93 1.91 2.753(7) yes C28 . H284 . O107 2_685 125 0.94 2.10 2.753(7) yes C28 . H284 . O108 2_685 163 0.94 2.57 3.481(7) yes O103 . H1031 . O18 2_675 153 0.97 1.86 2.763(7) yes C110 . H1103 . O103 . 136 0.95 2.46 3.218(7) yes C110 . H1103 . C104 . 136 0.95 1.77 2.535(7) yes C105 . H1051 . O107 . 127 0.94 2.11 2.781(7) yes O107 . H1071 . O27 2_685 179 0.82 2.07 2.884(7) yes O108 . H1081 . O37 2_685 180 0.82 2.00 2.825(7) yes # Attachment '[22]CCDC706506.cif' data_EB7218 _database_code_depnum_ccdc_archive 'CCDC 706506' _cell_length_a 11.9218(2) _cell_length_b 12.0379(2) _cell_length_c 13.6675(3) _cell_angle_alpha 85.793(1) _cell_angle_beta 85.319(1) _cell_angle_gamma 75.513(1) _cell_volume 1889.92(6) _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' 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 1 # Found Formula = C68 H74.50 Cl4 Mn6 N6 O24.50 # Dc = 1.62 FOOO = 938.50 Mu = 11.94 M = 919.62 _chemical_formula_sum 'C68 H74.50 Cl4 Mn6 N6 O24.50' _chemical_formula_moiety 'C68 H74.50 Cl4 Mn6 N6 O24.50' _chemical_compound_source ? _chemical_formula_weight 1839.24 _cell_measurement_reflns_used 9330 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 938.500 _exptl_absorpt_coefficient_mu 1.194 # Sheldrick geometric approximatio 0.74 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.84 _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 22561 _reflns_number_total 7715 _diffrn_reflns_av_R_equivalents 0.035 # Number of reflections with Friedels Law is 7715 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7729 _diffrn_reflns_theta_min 1.768 _diffrn_reflns_theta_max 26.371 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.371 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -14 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 1.46 _oxford_diffrn_Wilson_scale 37.85 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.50 _refine_diff_density_max 0.68 # 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 7715 _refine_ls_number_restraints 0 _refine_ls_number_parameters 505 _oxford_refine_ls_R_factor_ref 0.0443 _refine_ls_wR_factor_ref 0.0780 _refine_ls_goodness_of_fit_ref 0.8767 _refine_ls_shift/su_max 0.001289 # The values computed from all data _oxford_reflns_number_all 7715 _refine_ls_R_factor_all 0.0443 _refine_ls_wR_factor_all 0.0780 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6111 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_gt 0.0749 # 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 0.49208(3) 1.09995(3) 0.41628(3) 0.0163 1.0000 Uani . . . . . . . Mn2 Mn 0.60367(3) 0.85472(3) 0.31815(3) 0.0179 1.0000 Uani . . . . . . . Mn3 Mn 0.75913(3) 1.03950(3) 0.32043(3) 0.0181 1.0000 Uani . . . . . . . O4 O 0.61511(13) 1.00203(13) 0.34690(11) 0.0180 1.0000 Uani . . . . . . . O5 O 0.38570(14) 1.19711(13) 0.50579(11) 0.0196 1.0000 Uani . . . . . . . C6 C 0.3443(2) 1.30876(19) 0.47750(17) 0.0205 1.0000 Uani . . . . . . . C7 C 0.2309(2) 1.3626(2) 0.50734(18) 0.0242 1.0000 Uani . . . . . . . C8 C 0.1804(2) 1.4737(2) 0.4744(2) 0.0293 1.0000 Uani . . . . . . . C9 C 0.2438(2) 1.5336(2) 0.4115(2) 0.0325 1.0000 Uani . . . . . . . C10 C 0.3591(2) 1.4851(2) 0.3869(2) 0.0296 1.0000 Uani . . . . . . . C11 C 0.4134(2) 1.3731(2) 0.42019(18) 0.0216 1.0000 Uani . . . . . . . C12 C 0.5391(2) 1.3289(2) 0.39810(17) 0.0207 1.0000 Uani . . . . . . . N13 N 0.58272(16) 1.21902(16) 0.39723(14) 0.0188 1.0000 Uani . . . . . . . O14 O 0.70105(14) 1.18147(13) 0.38420(12) 0.0218 1.0000 Uani . . . . . . . C15 C 0.6169(2) 1.4092(2) 0.3781(2) 0.0313 1.0000 Uani . . . . . . . O16 O 0.58493(14) 0.71170(14) 0.29116(13) 0.0236 1.0000 Uani . . . . . . . C17 C 0.4931(2) 0.7024(2) 0.24602(18) 0.0223 1.0000 Uani . . . . . . . C18 C 0.5098(2) 0.6180(2) 0.17744(19) 0.0298 1.0000 Uani . . . . . . . C19 C 0.4197(3) 0.6011(2) 0.1288(2) 0.0352 1.0000 Uani . . . . . . . C20 C 0.3083(3) 0.6686(3) 0.1469(2) 0.0359 1.0000 Uani . . . . . . . C21 C 0.2901(2) 0.7517(2) 0.21432(19) 0.0302 1.0000 Uani . . . . . . . C22 C 0.3796(2) 0.7713(2) 0.26577(17) 0.0217 1.0000 Uani . . . . . . . C23 C 0.3537(2) 0.8590(2) 0.33887(17) 0.0209 1.0000 Uani . . . . . . . N24 N 0.43739(17) 0.89770(15) 0.36637(14) 0.0172 1.0000 Uani . . . . . . . O25 O 0.41260(13) 0.97471(13) 0.44138(11) 0.0173 1.0000 Uani . . . . . . . C26 C 0.2326(2) 0.9023(2) 0.3813(2) 0.0335 1.0000 Uani . . . . . . . O27 O 0.90539(14) 1.06946(15) 0.30019(13) 0.0257 1.0000 Uani . . . . . . . C28 C 0.9793(2) 1.0421(2) 0.22181(18) 0.0237 1.0000 Uani . . . . . . . C29 C 1.0560(2) 1.1119(2) 0.1957(2) 0.0310 1.0000 Uani . . . . . . . C30 C 1.1381(2) 1.0883(3) 0.1178(2) 0.0360 1.0000 Uani . . . . . . . C31 C 1.1455(2) 0.9943(3) 0.0633(2) 0.0352 1.0000 Uani . . . . . . . C32 C 1.0705(2) 0.9252(2) 0.0874(2) 0.0311 1.0000 Uani . . . . . . . C33 C 0.9864(2) 0.9457(2) 0.16627(19) 0.0237 1.0000 Uani . . . . . . . C34 C 0.9123(2) 0.8653(2) 0.19084(18) 0.0229 1.0000 Uani . . . . . . . N35 N 0.82052(17) 0.89331(16) 0.25032(15) 0.0202 1.0000 Uani . . . . . . . O36 O 0.76271(14) 0.80891(13) 0.27440(13) 0.0238 1.0000 Uani . . . . . . . C37 C 0.9446(2) 0.7490(2) 0.1491(2) 0.0373 1.0000 Uani . . . . . . . O38 O 0.38289(15) 1.16563(15) 0.30035(12) 0.0249 1.0000 Uani . . . . . . . C39 C 0.3912(2) 1.2032(2) 0.21315(18) 0.0219 1.0000 Uani . . . . . . . O40 O 0.47310(15) 1.16734(15) 0.15034(13) 0.0274 1.0000 Uani . . . . . . . C41 C 0.2900(2) 1.29917(19) 0.17988(18) 0.0197 1.0000 Uani . . . . . . . C42 C 0.1924(2) 1.3312(2) 0.24360(18) 0.0249 1.0000 Uani . . . . . . . C43 C 0.0975(2) 1.4128(2) 0.21145(19) 0.0276 1.0000 Uani . . . . . . . C44 C 0.0988(2) 1.4654(2) 0.11770(19) 0.0256 1.0000 Uani . . . . . . . C45 C 0.1982(2) 1.4344(2) 0.05703(18) 0.0236 1.0000 Uani . . . . . . . C46 C 0.2942(2) 1.3515(2) 0.08613(18) 0.0219 1.0000 Uani . . . . . . . Cl47 Cl -0.02804(7) 1.45028(8) 0.28820(6) 0.0491 1.0000 Uani . . . . . . . Cl48 Cl 0.20027(6) 1.50345(6) -0.05914(5) 0.0387 1.0000 Uani . . . . . . . O49 O 0.54905(16) 0.92901(14) 0.16971(12) 0.0276 1.0000 Uani . . . . . . . C50 C 0.5948(3) 0.8832(3) 0.0782(2) 0.0438 1.0000 Uani . . . . . . . O51 O 0.70184(15) 1.12980(14) 0.17468(12) 0.0262 1.0000 Uani . . . . . . . C52 C 0.7287(3) 1.2356(2) 0.1387(2) 0.0380 1.0000 Uani . . . . . . . O53 O 0.81719(15) 0.92001(15) 0.45374(12) 0.0271 1.0000 Uani . . . . . . . C54 C 0.9353(3) 0.8569(4) 0.4811(4) 0.0507 0.7500 Uani . . . 1 1 . . O55 O 1.0074(6) 0.8754(6) 0.5387(6) 0.0342 0.2500 Uani . . . 1 2 . . C56 C 1.0535(11) 0.7577(10) 0.5304(10) 0.0480 0.2500 Uani . . . 1 2 . . H211 H 0.2170 0.7984 0.2230 0.0368 1.0000 Uiso R . . . . . . H201 H 0.2480 0.6574 0.1135 0.0444 1.0000 Uiso R . . . . . . H191 H 0.4335 0.5447 0.0849 0.0436 1.0000 Uiso R . . . . . . H181 H 0.5834 0.5720 0.1660 0.0346 1.0000 Uiso R . . . . . . H291 H 1.0500 1.1742 0.2315 0.0381 1.0000 Uiso R . . . . . . H371 H 1.0223 0.7135 0.1611 0.0573 1.0000 Uiso R . . . . . . H372 H 0.8977 0.7022 0.1785 0.0566 1.0000 Uiso R . . . . . . H373 H 0.9406 0.7549 0.0790 0.0568 1.0000 Uiso R . . . . . . H152 H 0.6856 1.3800 0.4079 0.0486 1.0000 Uiso R . . . . . . H151 H 0.5845 1.4815 0.4013 0.0477 1.0000 Uiso R . . . . . . H153 H 0.6382 1.4182 0.3099 0.0486 1.0000 Uiso R . . . . . . H71 H 0.1902 1.3241 0.5504 0.0285 1.0000 Uiso R . . . . . . H81 H 0.1043 1.5066 0.4945 0.0331 1.0000 Uiso R . . . . . . H91 H 0.2104 1.6050 0.3868 0.0360 1.0000 Uiso R . . . . . . H421 H 0.1905 1.2982 0.3069 0.0297 1.0000 Uiso R . . . . . . H441 H 0.0329 1.5185 0.0967 0.0298 1.0000 Uiso R . . . . . . H461 H 0.3599 1.3305 0.0424 0.0259 1.0000 Uiso R . . . . . . H101 H 0.4047 1.5268 0.3478 0.0341 1.0000 Uiso R . . . . . . H321 H 1.0734 0.8622 0.0482 0.0357 1.0000 Uiso R . . . . . . H261 H 0.1832 0.8608 0.3621 0.0526 1.0000 Uiso R . . . . . . H262 H 0.2077 0.9769 0.3588 0.0518 1.0000 Uiso R . . . . . . H263 H 0.2309 0.9010 0.4498 0.0513 1.0000 Uiso R . . . . . . H301 H 1.1873 1.1351 0.1026 0.0447 1.0000 Uiso R . . . . . . H311 H 1.1985 0.9807 0.0090 0.0431 1.0000 Uiso R . . . . . . H491 H 0.5251 0.9977 0.1621 0.0399 1.0000 Uiso R . . . . . . H531 H 0.7627 0.8977 0.4829 0.0407 1.0000 Uiso R . . . . . . H511 H 0.6324 1.1436 0.1687 0.0390 1.0000 Uiso R . . . . . . H503 H 0.5297 0.8642 0.0462 0.0643 1.0000 Uiso R . . . . . . H522 H 0.7203 1.2479 0.0698 0.0584 1.0000 Uiso R . . . . . . H502 H 0.6523 0.8131 0.0914 0.0643 1.0000 Uiso R . . . . . . H521 H 0.8037 1.2380 0.1518 0.0586 1.0000 Uiso R . . . . . . H501 H 0.6266 0.9344 0.0349 0.0651 1.0000 Uiso R . . . . . . H523 H 0.6781 1.2992 0.1676 0.0586 1.0000 Uiso R . . . . . . H532 H 0.8808 0.9067 0.4736 0.0421 1.0000 Uiso R . . 1 2 . . H541 H 0.9952 0.8985 0.4586 0.0713 0.7500 Uiso R . . 1 1 . . H542 H 0.9425 0.8412 0.5520 0.0713 0.7500 Uiso R . . 1 1 . . H543 H 0.9593 0.7824 0.4519 0.0719 0.7500 Uiso R . . 1 1 . . H563 H 1.1264 0.7355 0.5591 0.0740 0.2500 Uiso R . . 1 2 . . H562 H 1.0649 0.7412 0.4629 0.0741 0.2500 Uiso R . . 1 2 . . H561 H 1.0015 0.7157 0.5629 0.0738 0.2500 Uiso R . . 1 2 . . H551 H 1.0305 0.8763 0.5935 0.0529 0.2500 Uiso R . . 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 0.01756(19) 0.01452(17) 0.01590(18) 0.00000(14) 0.00223(14) -0.00379(14) Mn2 0.01717(19) 0.01575(18) 0.02077(19) -0.00196(14) 0.00217(15) -0.00484(14) Mn3 0.01719(19) 0.01777(18) 0.01977(19) -0.00163(14) 0.00193(14) -0.00574(14) O4 0.0173(8) 0.0171(8) 0.0196(8) -0.0023(7) 0.0034(7) -0.0054(7) O5 0.0242(9) 0.0164(8) 0.0166(8) 0.0011(7) 0.0029(7) -0.0035(7) C6 0.0261(13) 0.0160(11) 0.0185(12) -0.0027(9) -0.0024(10) -0.0028(10) C7 0.0265(14) 0.0247(13) 0.0210(13) -0.0006(10) 0.0024(10) -0.0072(11) C8 0.0233(14) 0.0264(14) 0.0341(15) -0.0040(12) 0.0008(11) 0.0010(11) C9 0.0346(16) 0.0189(13) 0.0372(16) 0.0060(12) 0.0007(13) 0.0033(11) C10 0.0358(16) 0.0195(13) 0.0319(15) 0.0039(11) 0.0031(12) -0.0071(11) C11 0.0244(13) 0.0187(12) 0.0204(12) -0.0018(10) 0.0023(10) -0.0037(10) C12 0.0260(13) 0.0183(12) 0.0178(12) -0.0007(9) 0.0016(10) -0.0065(10) N13 0.0175(10) 0.0198(10) 0.0186(10) -0.0014(8) 0.0013(8) -0.0045(8) O14 0.0172(9) 0.0200(8) 0.0282(9) -0.0040(7) 0.0009(7) -0.0047(7) C15 0.0284(15) 0.0186(13) 0.0474(18) -0.0022(12) 0.0041(13) -0.0089(11) O16 0.0218(9) 0.0171(8) 0.0329(10) -0.0034(7) -0.0002(8) -0.0067(7) C17 0.0265(14) 0.0194(12) 0.0236(13) 0.0003(10) 0.0031(10) -0.0121(10) C18 0.0321(15) 0.0273(14) 0.0313(15) -0.0076(11) 0.0117(12) -0.0122(12) C19 0.0445(18) 0.0361(16) 0.0303(15) -0.0131(13) 0.0047(13) -0.0192(14) C20 0.0355(17) 0.0470(18) 0.0308(16) -0.0089(13) -0.0045(13) -0.0180(14) C21 0.0281(15) 0.0366(15) 0.0274(14) -0.0052(12) -0.0025(11) -0.0098(12) C22 0.0256(13) 0.0231(12) 0.0183(12) -0.0017(10) 0.0019(10) -0.0102(10) C23 0.0202(13) 0.0220(12) 0.0194(12) 0.0018(10) -0.0020(10) -0.0039(10) N24 0.0213(11) 0.0147(9) 0.0152(10) -0.0002(8) 0.0010(8) -0.0045(8) O25 0.0204(9) 0.0156(8) 0.0156(8) -0.0020(6) 0.0017(7) -0.0045(7) C26 0.0206(14) 0.0453(17) 0.0367(16) -0.0186(13) -0.0008(12) -0.0076(12) O27 0.0206(9) 0.0306(10) 0.0286(10) -0.0056(8) 0.0039(7) -0.0118(8) C28 0.0191(13) 0.0277(13) 0.0241(13) 0.0018(11) -0.0004(10) -0.0066(10) C29 0.0290(15) 0.0346(15) 0.0334(15) -0.0052(12) 0.0019(12) -0.0153(12) C30 0.0312(16) 0.0443(17) 0.0388(17) -0.0023(14) 0.0068(13) -0.0242(13) C31 0.0299(15) 0.0451(17) 0.0317(16) -0.0029(13) 0.0126(12) -0.0157(13) C32 0.0299(15) 0.0298(14) 0.0333(15) -0.0046(12) 0.0059(12) -0.0086(12) C33 0.0171(12) 0.0239(13) 0.0286(14) 0.0005(11) 0.0016(10) -0.0037(10) C34 0.0223(13) 0.0185(12) 0.0266(13) -0.0005(10) 0.0021(10) -0.0042(10) N35 0.0206(11) 0.0168(10) 0.0236(11) -0.0006(8) 0.0010(9) -0.0062(8) O36 0.0204(9) 0.0169(8) 0.0342(10) -0.0027(7) 0.0061(8) -0.0071(7) C37 0.0306(16) 0.0284(15) 0.0527(19) -0.0136(14) 0.0170(14) -0.0102(12) O38 0.0271(10) 0.0277(9) 0.0190(9) 0.0033(7) -0.0049(7) -0.0053(8) C39 0.0258(14) 0.0186(12) 0.0232(13) -0.0015(10) -0.0058(11) -0.0078(10) O40 0.0262(10) 0.0273(9) 0.0241(9) 0.0019(8) -0.0010(8) 0.0010(8) C41 0.0211(12) 0.0165(11) 0.0225(13) -0.0018(10) -0.0047(10) -0.0052(9) C42 0.0280(14) 0.0257(13) 0.0204(13) -0.0018(10) -0.0021(11) -0.0052(11) C43 0.0249(14) 0.0304(14) 0.0253(14) -0.0060(11) 0.0035(11) -0.0030(11) C44 0.0235(13) 0.0226(13) 0.0290(14) -0.0026(11) -0.0060(11) -0.0007(10) C45 0.0309(14) 0.0223(12) 0.0190(13) 0.0023(10) -0.0049(11) -0.0089(11) C46 0.0216(13) 0.0225(12) 0.0221(13) -0.0015(10) 0.0003(10) -0.0068(10) Cl47 0.0314(4) 0.0718(6) 0.0311(4) -0.0037(4) 0.0069(3) 0.0090(4) Cl48 0.0318(4) 0.0449(4) 0.0330(4) 0.0187(3) -0.0027(3) -0.0032(3) O49 0.0389(11) 0.0210(9) 0.0203(9) -0.0016(7) 0.0016(8) -0.0038(8) C50 0.067(2) 0.0378(17) 0.0231(15) -0.0062(13) 0.0089(15) -0.0085(16) O51 0.0266(10) 0.0263(9) 0.0262(10) 0.0047(8) 0.0001(8) -0.0095(8) C52 0.0461(19) 0.0330(16) 0.0361(17) 0.0094(13) -0.0001(14) -0.0161(14) O53 0.0185(9) 0.0335(10) 0.0285(10) -0.0001(8) 0.0011(7) -0.0064(8) C54 0.027(2) 0.041(2) 0.074(3) 0.012(2) -0.008(2) 0.0061(18) O55 0.026(4) 0.042(5) 0.037(4) -0.016(4) -0.019(3) -0.002(3) C56 0.048(8) 0.033(7) 0.064(9) -0.009(6) -0.028(7) -0.005(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.15466(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 . O25 2_676 2.3402(16) yes Mn1 . Mn1 2_676 3.1779(7) yes Mn1 . Mn2 . 3.2570(5) yes Mn1 . O4 . 1.8740(15) yes Mn1 . O5 . 1.9203(16) yes Mn1 . N13 . 1.9910(19) yes Mn1 . O25 . 1.9684(15) yes Mn1 . O38 . 2.1138(17) yes Mn2 . O5 2_676 2.4465(16) yes Mn2 . Mn3 . 3.2351(5) yes Mn2 . O4 . 1.8840(15) yes Mn2 . O16 . 1.8572(16) yes Mn2 . N24 . 1.9888(19) yes Mn2 . O36 . 1.8966(16) yes Mn2 . O49 . 2.2356(17) yes Mn3 . O4 . 1.8827(15) yes Mn3 . O14 . 1.9203(16) yes Mn3 . O27 . 1.8624(17) yes Mn3 . N35 . 2.0098(19) yes Mn3 . O51 . 2.2693(17) yes Mn3 . O53 . 2.2784(17) yes O5 . C6 . 1.350(3) yes C6 . C7 . 1.387(3) yes C6 . C11 . 1.420(3) yes C7 . C8 . 1.380(3) yes C7 . H71 . 0.907 no C8 . C9 . 1.380(4) yes C8 . H81 . 0.922 no C9 . C10 . 1.376(4) yes C9 . H91 . 0.906 no C10 . C11 . 1.402(3) yes C10 . H101 . 0.940 no C11 . C12 . 1.474(3) yes C12 . N13 . 1.295(3) yes C12 . C15 . 1.496(3) yes N13 . O14 . 1.370(2) yes C15 . H152 . 0.923 no C15 . H151 . 0.927 no C15 . H153 . 0.951 no O16 . C17 . 1.332(3) yes C17 . C18 . 1.400(3) yes C17 . C22 . 1.415(3) yes C18 . C19 . 1.372(4) yes C18 . H181 . 0.921 no C19 . C20 . 1.386(4) yes C19 . H191 . 0.914 no C20 . C21 . 1.374(4) yes C20 . H201 . 0.925 no C21 . C22 . 1.401(3) yes C21 . H211 . 0.916 no C22 . C23 . 1.466(3) yes C23 . N24 . 1.293(3) yes C23 . C26 . 1.491(3) yes N24 . O25 . 1.397(2) yes C26 . H261 . 0.925 no C26 . H262 . 0.912 no C26 . H263 . 0.935 no O27 . C28 . 1.336(3) yes C28 . C29 . 1.398(3) yes C28 . C33 . 1.414(3) yes C29 . C30 . 1.381(4) yes C29 . H291 . 0.910 no C30 . C31 . 1.380(4) yes C30 . H301 . 0.912 no C31 . C32 . 1.372(4) yes C31 . H311 . 0.931 no C32 . C33 . 1.403(3) yes C32 . H321 . 0.952 no C33 . C34 . 1.470(3) yes C34 . N35 . 1.297(3) yes C34 . C37 . 1.499(3) yes N35 . O36 . 1.371(2) yes C37 . H371 . 0.940 no C37 . H372 . 0.938 no C37 . H373 . 0.959 no O38 . C39 . 1.249(3) yes C39 . O40 . 1.258(3) yes C39 . C41 . 1.521(3) yes C41 . C42 . 1.386(3) yes C41 . C46 . 1.389(3) yes C42 . C43 . 1.379(3) yes C42 . H421 . 0.926 no C43 . C44 . 1.388(3) yes C43 . Cl47 . 1.737(3) yes C44 . C45 . 1.377(3) yes C44 . H441 . 0.930 no C45 . C46 . 1.381(3) yes C45 . Cl48 . 1.738(2) yes C46 . H461 . 0.939 no O49 . C50 . 1.416(3) yes O49 . H491 . 0.806 no C50 . H503 . 1.002 no C50 . H502 . 0.961 no C50 . H501 . 0.948 no O51 . C52 . 1.433(3) yes O51 . H511 . 0.813 no C52 . H522 . 0.952 no C52 . H521 . 0.934 no C52 . H523 . 0.938 no O53 . C54 . 1.486(4) yes O53 . H531 . 0.826 no O53 . H531 . 0.826 no O53 . H532 . 0.800 no C54 . H541 . 0.988 no C54 . H542 . 0.981 no C54 . H543 . 0.974 no O55 . C56 . 1.395(13) yes O55 . H551 . 0.820 no C56 . H563 . 0.951 no C56 . H562 . 0.949 no C56 . H561 . 0.957 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O25 2_676 Mn1 . Mn1 2_676 38.12(4) yes O25 2_676 Mn1 . Mn2 . 88.71(4) yes Mn1 2_676 Mn1 . Mn2 . 71.323(13) yes O25 2_676 Mn1 . O4 . 86.66(6) yes Mn1 2_676 Mn1 . O4 . 87.75(5) yes Mn2 . Mn1 . O4 . 30.01(5) yes O25 2_676 Mn1 . O5 . 83.57(6) yes Mn1 2_676 Mn1 . O5 . 86.93(5) yes Mn2 . Mn1 . O5 . 152.81(5) yes O4 . Mn1 . O5 . 169.49(7) yes O25 2_676 Mn1 . N13 . 90.41(7) yes Mn1 2_676 Mn1 . N13 . 128.51(6) yes Mn2 . Mn1 . N13 . 117.53(6) yes O4 . Mn1 . N13 . 87.58(7) yes O5 . Mn1 . N13 . 88.65(7) yes O25 2_676 Mn1 . O25 . 85.34(6) yes Mn1 2_676 Mn1 . O25 . 47.22(5) yes Mn2 . Mn1 . O25 . 60.64(4) yes O4 . Mn1 . O25 . 90.34(6) yes O5 . Mn1 . O25 . 92.68(6) yes O25 2_676 Mn1 . O38 . 171.39(6) yes Mn1 2_676 Mn1 . O38 . 135.71(5) yes Mn2 . Mn1 . O38 . 94.00(5) yes O4 . Mn1 . O38 . 99.77(7) yes O5 . Mn1 . O38 . 90.36(7) yes N13 . Mn1 . O25 . 175.38(7) yes N13 . Mn1 . O38 . 95.56(7) yes O25 . Mn1 . O38 . 88.86(7) yes O5 2_676 Mn2 . Mn1 . 77.46(4) yes O5 2_676 Mn2 . Mn3 . 93.92(4) yes Mn1 . Mn2 . Mn3 . 60.451(11) yes O5 2_676 Mn2 . O4 . 87.30(6) yes Mn1 . Mn2 . O4 . 29.84(5) yes Mn3 . Mn2 . O4 . 30.80(5) yes O5 2_676 Mn2 . O16 . 92.48(7) yes Mn1 . Mn2 . O16 . 147.58(5) yes Mn3 . Mn2 . O16 . 151.86(5) yes O4 . Mn2 . O16 . 177.32(7) yes O5 2_676 Mn2 . N24 . 77.94(7) yes Mn1 . Mn2 . N24 . 59.19(5) yes Mn3 . Mn2 . N24 . 119.44(6) yes O4 . Mn2 . N24 . 88.64(7) yes O16 . Mn2 . N24 . 88.70(7) yes O5 2_676 Mn2 . O36 . 100.83(7) yes Mn1 . Mn2 . O36 . 122.07(5) yes Mn3 . Mn2 . O36 . 61.96(5) yes O4 . Mn2 . O36 . 92.75(7) yes O16 . Mn2 . O36 . 89.92(7) yes O5 2_676 Mn2 . O49 . 165.30(6) yes Mn1 . Mn2 . O49 . 91.54(4) yes Mn3 . Mn2 . O49 . 88.94(5) yes O4 . Mn2 . O49 . 87.83(7) yes O16 . Mn2 . O49 . 91.75(7) yes N24 . Mn2 . O36 . 178.11(7) yes N24 . Mn2 . O49 . 88.09(7) yes O36 . Mn2 . O49 . 93.25(7) yes Mn2 . Mn3 . O4 . 30.82(5) yes Mn2 . Mn3 . O14 . 121.31(5) yes O4 . Mn3 . O14 . 90.77(7) yes Mn2 . Mn3 . O27 . 147.49(6) yes O4 . Mn3 . O27 . 176.41(7) yes O14 . Mn3 . O27 . 90.34(7) yes Mn2 . Mn3 . N35 . 59.50(6) yes O4 . Mn3 . N35 . 89.93(7) yes O14 . Mn3 . N35 . 178.47(8) yes O27 . Mn3 . N35 . 89.04(8) yes Mn2 . Mn3 . O51 . 94.60(4) yes O4 . Mn3 . O51 . 91.00(7) yes O14 . Mn3 . O51 . 90.03(7) yes O27 . Mn3 . O51 . 92.41(7) yes N35 . Mn3 . O51 . 88.61(7) yes Mn2 . Mn3 . O53 . 77.70(4) yes O4 . Mn3 . O53 . 85.64(6) yes O14 . Mn3 . O53 . 99.50(7) yes O27 . Mn3 . O53 . 90.81(7) yes N35 . Mn3 . O53 . 81.91(7) yes O51 . Mn3 . O53 . 169.93(6) yes Mn2 . O4 . Mn3 . 118.38(8) yes Mn2 . O4 . Mn1 . 120.15(8) yes Mn3 . O4 . Mn1 . 120.91(8) yes Mn2 2_676 O5 . Mn1 . 117.96(7) yes Mn2 2_676 O5 . C6 . 118.14(13) yes Mn1 . O5 . C6 . 118.38(14) yes O5 . C6 . C7 . 118.5(2) yes O5 . C6 . C11 . 122.3(2) yes C7 . C6 . C11 . 119.1(2) yes C6 . C7 . C8 . 121.3(2) yes C6 . C7 . H71 . 118.8 no C8 . C7 . H71 . 119.9 no C7 . C8 . C9 . 119.8(2) yes C7 . C8 . H81 . 119.3 no C9 . C8 . H81 . 120.9 no C8 . C9 . C10 . 119.9(2) yes C8 . C9 . H91 . 120.5 no C10 . C9 . H91 . 119.5 no C9 . C10 . C11 . 121.6(2) yes C9 . C10 . H101 . 120.9 no C11 . C10 . H101 . 117.5 no C6 . C11 . C10 . 117.8(2) yes C6 . C11 . C12 . 122.9(2) yes C10 . C11 . C12 . 119.3(2) yes C11 . C12 . N13 . 119.4(2) yes C11 . C12 . C15 . 120.8(2) yes N13 . C12 . C15 . 119.8(2) yes Mn1 . N13 . C12 . 125.30(17) yes Mn1 . N13 . O14 . 117.28(13) yes C12 . N13 . O14 . 117.41(19) yes N13 . O14 . Mn3 . 116.26(13) yes C12 . C15 . H152 . 110.1 no C12 . C15 . H151 . 113.0 no H152 . C15 . H151 . 107.3 no C12 . C15 . H153 . 112.2 no H152 . C15 . H153 . 105.6 no H151 . C15 . H153 . 108.3 no Mn2 . O16 . C17 . 120.83(15) yes O16 . C17 . C18 . 118.0(2) yes O16 . C17 . C22 . 123.4(2) yes C18 . C17 . C22 . 118.6(2) yes C17 . C18 . C19 . 121.9(3) yes C17 . C18 . H181 . 118.4 no C19 . C18 . H181 . 119.7 no C18 . C19 . C20 . 120.1(3) yes C18 . C19 . H191 . 119.6 no C20 . C19 . H191 . 120.3 no C19 . C20 . C21 . 118.9(3) yes C19 . C20 . H201 . 119.7 no C21 . C20 . H201 . 121.3 no C20 . C21 . C22 . 122.7(3) yes C20 . C21 . H211 . 118.1 no C22 . C21 . H211 . 119.1 no C17 . C22 . C21 . 117.8(2) yes C17 . C22 . C23 . 122.2(2) yes C21 . C22 . C23 . 120.0(2) yes C22 . C23 . N24 . 119.1(2) yes C22 . C23 . C26 . 120.3(2) yes N24 . C23 . C26 . 120.6(2) yes Mn2 . N24 . C23 . 127.36(16) yes Mn2 . N24 . O25 . 114.35(13) yes C23 . N24 . O25 . 118.22(19) yes Mn1 2_676 O25 . N24 . 112.83(11) yes Mn1 2_676 O25 . Mn1 . 94.66(6) yes N24 . O25 . Mn1 . 112.49(12) yes C23 . C26 . H261 . 111.9 no C23 . C26 . H262 . 107.3 no H261 . C26 . H262 . 108.9 no C23 . C26 . H263 . 110.7 no H261 . C26 . H263 . 110.3 no H262 . C26 . H263 . 107.6 no Mn3 . O27 . C28 . 125.84(16) yes O27 . C28 . C29 . 117.4(2) yes O27 . C28 . C33 . 123.9(2) yes C29 . C28 . C33 . 118.7(2) yes C28 . C29 . C30 . 121.6(3) yes C28 . C29 . H291 . 117.9 no C30 . C29 . H291 . 120.5 no C29 . C30 . C31 . 120.0(3) yes C29 . C30 . H301 . 119.7 no C31 . C30 . H301 . 120.3 no C30 . C31 . C32 . 119.3(3) yes C30 . C31 . H311 . 119.8 no C32 . C31 . H311 . 120.8 no C31 . C32 . C33 . 122.5(3) yes C31 . C32 . H321 . 119.4 no C33 . C32 . H321 . 118.1 no C28 . C33 . C32 . 117.9(2) yes C28 . C33 . C34 . 122.4(2) yes C32 . C33 . C34 . 119.7(2) yes C33 . C34 . N35 . 120.4(2) yes C33 . C34 . C37 . 119.9(2) yes N35 . C34 . C37 . 119.7(2) yes Mn3 . N35 . C34 . 128.54(17) yes Mn3 . N35 . O36 . 115.54(14) yes C34 . N35 . O36 . 115.72(19) yes N35 . O36 . Mn2 . 117.84(13) yes C34 . C37 . H371 . 109.0 no C34 . C37 . H372 . 111.1 no H371 . C37 . H372 . 108.4 no C34 . C37 . H373 . 111.2 no H371 . C37 . H373 . 106.3 no H372 . C37 . H373 . 110.7 no Mn1 . O38 . C39 . 138.66(17) yes O38 . C39 . O40 . 126.4(2) yes O38 . C39 . C41 . 116.1(2) yes O40 . C39 . C41 . 117.5(2) yes C39 . C41 . C42 . 118.9(2) yes C39 . C41 . C46 . 120.4(2) yes C42 . C41 . C46 . 120.6(2) yes C41 . C42 . C43 . 119.1(2) yes C41 . C42 . H421 . 120.7 no C43 . C42 . H421 . 120.2 no C42 . C43 . C44 . 121.4(2) yes C42 . C43 . Cl47 . 120.0(2) yes C44 . C43 . Cl47 . 118.6(2) yes C43 . C44 . C45 . 118.2(2) yes C43 . C44 . H441 . 120.1 no C45 . C44 . H441 . 121.8 no C44 . C45 . C46 . 122.0(2) yes C44 . C45 . Cl48 . 117.81(19) yes C46 . C45 . Cl48 . 120.2(2) yes C41 . C46 . C45 . 118.7(2) yes C41 . C46 . H461 . 121.3 no C45 . C46 . H461 . 120.1 no Mn2 . O49 . C50 . 126.39(17) yes Mn2 . O49 . H491 . 118.5 no C50 . O49 . H491 . 109.3 no O49 . C50 . H503 . 107.4 no O49 . C50 . H502 . 107.6 no H503 . C50 . H502 . 108.5 no O49 . C50 . H501 . 113.7 no H503 . C50 . H501 . 108.7 no H502 . C50 . H501 . 110.8 no Mn3 . O51 . C52 . 122.88(16) yes Mn3 . O51 . H511 . 114.5 no C52 . O51 . H511 . 102.2 no O51 . C52 . H522 . 110.8 no O51 . C52 . H521 . 112.2 no H522 . C52 . H521 . 109.1 no O51 . C52 . H523 . 111.9 no H522 . C52 . H523 . 106.0 no H521 . C52 . H523 . 106.5 no Mn3 . O53 . C54 . 130.5(2) yes Mn3 . O53 . H531 . 111.8 no C54 . O53 . H531 . 115.9 no Mn3 . O53 . H531 . 111.8 no Mn3 . O53 . H532 . 124.3 no H531 . O53 . H532 . 123.6 no O53 . C54 . H541 . 112.8 no O53 . C54 . H542 . 114.3 no H541 . C54 . H542 . 105.5 no O53 . C54 . H543 . 111.3 no H541 . C54 . H543 . 106.4 no H542 . C54 . H543 . 106.1 no C56 . O55 . H551 . 94.6 no O55 . C56 . H563 . 109.3 no O55 . C56 . H562 . 109.4 no H563 . C56 . H562 . 108.9 no O55 . C56 . H561 . 110.1 no H563 . C56 . H561 . 109.9 no H562 . C56 . H561 . 109.3 no # Attachment '[3]CCDC706507.cif' data_EB7192 _database_code_depnum_ccdc_archive 'CCDC 706507' _cell_length_a 11.9177(3) _cell_length_b 12.7405(3) _cell_length_c 13.5095(3) _cell_angle_alpha 80.875(1) _cell_angle_beta 77.238(1) _cell_angle_gamma 80.941(1) _cell_volume 1959.23(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Found Formula = C72 H84 Mn6 N6 O28 # Dc = 1.53 FOOO = 932.00 Mu = 10.22 M = 905.53 _chemical_formula_sum 'C72 H84 Mn6 N6 O28' _chemical_formula_moiety 'C68 H68 Mn6 N6 O24, 2(C2 H6 O), 2(H2 O)' _chemical_compound_source 'Leigh Jones' _chemical_formula_weight 1811.05 _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 1.022 # Sheldrick geometric approximatio 0.81 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.92 _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 33921 _reflns_number_total 10895 _diffrn_reflns_av_R_equivalents 0.042 # Number of reflections with Friedels Law is 10895 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11505 _diffrn_reflns_theta_min 1.558 _diffrn_reflns_theta_max 30.073 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.968 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 16 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _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 -0.69 _refine_diff_density_max 0.89 # 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 10866 _refine_ls_number_restraints 0 _refine_ls_number_parameters 505 _oxford_refine_ls_R_factor_ref 0.0602 _refine_ls_wR_factor_ref 0.1068 _refine_ls_goodness_of_fit_ref 0.9321 _refine_ls_shift/su_max 0.001854 # The values computed from all data _oxford_reflns_number_all 10866 _refine_ls_R_factor_all 0.0602 _refine_ls_wR_factor_all 0.1068 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8549 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_gt 0.0991 # 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 0.94384(3) 0.59232(3) -0.24118(3) 0.0182 1.0000 Uani . . . . . . . Mn2 Mn 0.89171(3) 0.44842(3) -0.02788(2) 0.0166 1.0000 Uani . . . . . . . Mn3 Mn 1.02667(3) 0.33653(3) -0.22938(3) 0.0184 1.0000 Uani . . . . . . . O1 O 0.97115(13) 0.45950(12) -0.16407(11) 0.0176 1.0000 Uani . . . . . . . O2 O 0.94797(16) 0.72734(14) -0.31707(13) 0.0265 1.0000 Uani . . . . . . . C3 C 0.9299(2) 0.82534(19) -0.28957(19) 0.0227 1.0000 Uani . . . . . . . C4 C 0.9354(2) 0.9139(2) -0.3665(2) 0.0335 1.0000 Uani . . . . . . . C5 C 0.9215(3) 1.0165(2) -0.3417(2) 0.0388 1.0000 Uani . . . . . . . C6 C 0.8980(3) 1.0369(2) -0.2405(2) 0.0378 1.0000 Uani . . . . . . . C7 C 0.8894(2) 0.9515(2) -0.1642(2) 0.0309 1.0000 Uani . . . . . . . C8 C 0.9060(2) 0.84533(18) -0.18671(19) 0.0222 1.0000 Uani . . . . . . . C9 C 0.90182(19) 0.76067(18) -0.10266(18) 0.0205 1.0000 Uani . . . . . . . N10 N 0.91870(16) 0.66003(15) -0.11186(14) 0.0190 1.0000 Uani . . . . . . . O11 O 0.91820(14) 0.59249(12) -0.02039(12) 0.0192 1.0000 Uani . . . . . . . O12 O 0.81967(15) 0.43926(13) 0.11059(12) 0.0218 1.0000 Uani . . . . . . . C13 C 0.7587(2) 0.36207(19) 0.16486(17) 0.0197 1.0000 Uani . . . . . . . C14 C 0.6789(2) 0.3856(2) 0.25429(18) 0.0259 1.0000 Uani . . . . . . . C15 C 0.6166(2) 0.3079(2) 0.31466(19) 0.0297 1.0000 Uani . . . . . . . C16 C 0.6332(2) 0.2042(2) 0.2906(2) 0.0315 1.0000 Uani . . . . . . . C17 C 0.7115(2) 0.1791(2) 0.20325(19) 0.0278 1.0000 Uani . . . . . . . C18 C 0.7729(2) 0.25788(19) 0.13824(18) 0.0218 1.0000 Uani . . . . . . . C19 C 0.8499(2) 0.22493(19) 0.04635(18) 0.0225 1.0000 Uani . . . . . . . N20 N 0.90158(17) 0.29045(15) -0.02569(14) 0.0192 1.0000 Uani . . . . . . . O21 O 0.97621(15) 0.24421(13) -0.10497(12) 0.0243 1.0000 Uani . . . . . . . O22 O 1.10031(16) 0.21522(14) -0.28853(13) 0.0266 1.0000 Uani . . . . . . . C23 C 1.1710(2) 0.2072(2) -0.37899(18) 0.0237 1.0000 Uani . . . . . . . C24 C 1.2312(3) 0.1062(2) -0.3978(2) 0.0324 1.0000 Uani . . . . . . . C25 C 1.3066(3) 0.0928(2) -0.4894(2) 0.0401 1.0000 Uani . . . . . . . C26 C 1.3245(3) 0.1793(3) -0.5656(2) 0.0378 1.0000 Uani . . . . . . . C27 C 1.2656(2) 0.2783(2) -0.54938(19) 0.0305 1.0000 Uani . . . . . . . C28 C 1.1885(2) 0.2949(2) -0.45621(18) 0.0240 1.0000 Uani . . . . . . . C29 C 1.1315(2) 0.4029(2) -0.44541(18) 0.0239 1.0000 Uani . . . . . . . N30 N 1.06848(17) 0.43192(16) -0.36133(15) 0.0210 1.0000 Uani . . . . . . . O31 O 1.02080(16) 0.53758(14) -0.36574(13) 0.0262 1.0000 Uani . . . . . . . O32 O 0.76865(15) 0.57779(14) -0.23018(13) 0.0245 1.0000 Uani . . . . . . . O33 O 0.72961(14) 0.48117(14) -0.07556(13) 0.0241 1.0000 Uani . . . . . . . C34 C 0.7087(2) 0.51762(19) -0.16273(18) 0.0215 1.0000 Uani . . . . . . . C35 C 0.6001(2) 0.4904(2) -0.1889(2) 0.0295 1.0000 Uani . . . . . . . C36 C 0.5342(2) 0.4130(2) -0.1071(2) 0.0308 1.0000 Uani . . . . . . . C37 C 0.5909(2) 0.2988(2) -0.0986(2) 0.0274 1.0000 Uani . . . . . . . C38 C 0.5423(2) 0.2216(2) -0.01106(19) 0.0256 1.0000 Uani . . . . . . . C39 C 0.4402(2) 0.2495(2) 0.0589(2) 0.0275 1.0000 Uani . . . . . . . C40 C 0.3982(2) 0.1752(2) 0.1398(2) 0.0306 1.0000 Uani . . . . . . . C41 C 0.4551(2) 0.0722(2) 0.1535(2) 0.0307 1.0000 Uani . . . . . . . H41 H 0.9462 0.9021 -0.4346 0.0362 1.0000 Uiso R . . . . . . C42 C 0.5575(2) 0.0448(2) 0.0839(2) 0.0330 1.0000 Uani . . . . . . . C43 C 0.5998(2) 0.1182(2) 0.0031(2) 0.0306 1.0000 Uani . . . . . . . C44 C 0.4088(3) -0.0091(2) 0.2405(2) 0.0416 1.0000 Uani . . . . . . . O45 O 0.67507(17) 0.26765(16) -0.16220(15) 0.0375 1.0000 Uani . . . . . . . O46 O 0.86712(15) 0.33827(15) -0.28734(13) 0.0287 1.0000 Uani . . . . . . . O47 O 1.19926(15) 0.36192(15) -0.19775(14) 0.0274 1.0000 Uani . . . . . . . C48 C 1.2917(2) 0.2816(2) -0.1760(3) 0.0401 1.0000 Uani . . . . . . . C49 C 1.3942(3) 0.2837(3) -0.2633(3) 0.0536 1.0000 Uani . . . . . . . O50 O 1.1156(3) 0.04135(19) -0.0967(2) 0.0717 1.0000 Uani . . . . . . . O51 O 1.10359(18) 0.72294(17) -0.52386(14) 0.0381 1.0000 Uani . . . . . . . H51 H 0.9266 1.0737 -0.3948 0.0420 1.0000 Uiso R . . . . . . C52 C 1.2004(3) 0.7307(3) -0.4835(2) 0.0506 1.0000 Uani . . . . . . . C53 C 1.3001(3) 0.7576(4) -0.5647(3) 0.0633 1.0000 Uani . . . . . . . H61 H 0.8882 1.1064 -0.2249 0.0427 1.0000 Uiso R . . . . . . H71 H 0.8742 0.9640 -0.0957 0.0363 1.0000 Uiso R . . . . . . H91 H 0.8887 0.7804 -0.0367 0.0251 1.0000 Uiso R . . . . . . H141 H 0.6689 0.4547 0.2726 0.0307 1.0000 Uiso R . . . . . . H151 H 0.5639 0.3248 0.3721 0.0337 1.0000 Uiso R . . . . . . H161 H 0.5934 0.1510 0.3324 0.0365 1.0000 Uiso R . . . . . . H171 H 0.7235 0.1102 0.1861 0.0337 1.0000 Uiso R . . . . . . H191 H 0.8635 0.1534 0.0385 0.0267 1.0000 Uiso R . . . . . . H241 H 1.2201 0.0472 -0.3473 0.0379 1.0000 Uiso R . . . . . . H251 H 1.3458 0.0254 -0.5001 0.0460 1.0000 Uiso R . . . . . . H261 H 1.3750 0.1707 -0.6276 0.0439 1.0000 Uiso R . . . . . . H271 H 1.2755 0.3358 -0.6007 0.0361 1.0000 Uiso R . . . . . . H291 H 1.1376 0.4554 -0.5017 0.0294 1.0000 Uiso R . . . . . . H351 H 0.5494 0.5577 -0.1963 0.0370 1.0000 Uiso R . . . . . . H352 H 0.6226 0.4611 -0.2538 0.0371 1.0000 Uiso R . . . . . . H361 H 0.4572 0.4140 -0.1218 0.0371 1.0000 Uiso R . . . . . . H362 H 0.5259 0.4360 -0.0415 0.0375 1.0000 Uiso R . . . . . . H391 H 0.3994 0.3171 0.0514 0.0318 1.0000 Uiso R . . . . . . H401 H 0.3321 0.1952 0.1850 0.0362 1.0000 Uiso R . . . . . . H421 H 0.5971 -0.0235 0.0923 0.0384 1.0000 Uiso R . . . . . . H431 H 0.6667 0.0992 -0.0428 0.0381 1.0000 Uiso R . . . . . . H441 H 0.3382 0.0198 0.2792 0.0613 1.0000 Uiso R . . . . . . H442 H 0.3945 -0.0718 0.2154 0.0605 1.0000 Uiso R . . . . . . H443 H 0.4620 -0.0312 0.2852 0.0609 1.0000 Uiso R . . . . . . H461 H 0.8759 0.3184 -0.3442 0.0441 1.0000 Uiso R . . . . . . H462 H 0.8097 0.3161 -0.2534 0.0440 1.0000 Uiso R . . . . . . H471 H 1.1891 0.4094 -0.1635 0.0420 1.0000 Uiso R . . . . . . H481 H 1.2646 0.2127 -0.1643 0.0500 1.0000 Uiso R . . . . . . H482 H 1.3133 0.2948 -0.1137 0.0497 1.0000 Uiso R . . . . . . H491 H 1.4533 0.2273 -0.2465 0.0828 1.0000 Uiso R . . . . . . H492 H 1.4231 0.3524 -0.2735 0.0822 1.0000 Uiso R . . . . . . H493 H 1.3714 0.2708 -0.3235 0.0825 1.0000 Uiso R . . . . . . H501 H 1.0573 0.0778 -0.0684 0.1084 1.0000 Uiso R . . . . . . H502 H 1.0920 0.0450 -0.1506 0.1094 1.0000 Uiso R . . . . . . H511 H 1.0638 0.6882 -0.4789 0.0588 1.0000 Uiso R . . . . . . H521 H 1.2213 0.6606 -0.4498 0.0634 1.0000 Uiso R . . . . . . H522 H 1.1829 0.7832 -0.4358 0.0633 1.0000 Uiso R . . . . . . H531 H 1.3275 0.6952 -0.5988 0.0952 1.0000 Uiso R . . . . . . H532 H 1.2781 0.8159 -0.6129 0.0955 1.0000 Uiso R . . . . . . H533 H 1.3615 0.7740 -0.5354 0.0943 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 0.02078(17) 0.01679(17) 0.01614(16) 0.00121(12) -0.00364(13) -0.00319(13) Mn2 0.01937(17) 0.01542(16) 0.01491(15) -0.00032(12) -0.00350(12) -0.00335(12) Mn3 0.02083(17) 0.01731(17) 0.01648(16) -0.00199(13) -0.00214(13) -0.00319(13) O1 0.0200(8) 0.0164(7) 0.0159(7) 0.0008(6) -0.0038(6) -0.0034(6) O2 0.0342(10) 0.0202(8) 0.0220(8) 0.0035(7) -0.0021(7) -0.0047(7) C3 0.0193(11) 0.0176(11) 0.0273(12) 0.0037(9) -0.0014(9) -0.0018(9) C4 0.0373(15) 0.0261(13) 0.0271(13) 0.0080(10) 0.0026(11) 0.0017(11) C5 0.0431(17) 0.0223(13) 0.0407(16) 0.0117(12) 0.0009(13) -0.0020(12) C6 0.0456(17) 0.0190(13) 0.0434(16) 0.0008(11) -0.0027(14) -0.0018(11) C7 0.0364(15) 0.0193(12) 0.0345(14) -0.0005(10) -0.0057(12) -0.0011(10) C8 0.0184(11) 0.0170(11) 0.0296(12) 0.0019(9) -0.0061(9) -0.0007(8) C9 0.0190(11) 0.0204(11) 0.0228(11) -0.0013(9) -0.0075(9) -0.0018(8) N10 0.0191(9) 0.0186(9) 0.0190(9) 0.0023(7) -0.0063(7) -0.0030(7) O11 0.0262(8) 0.0154(7) 0.0165(7) 0.0020(6) -0.0073(6) -0.0039(6) O12 0.0261(9) 0.0222(8) 0.0160(7) 0.0000(6) -0.0015(6) -0.0060(7) C13 0.0187(10) 0.0246(11) 0.0168(10) 0.0008(8) -0.0072(8) -0.0037(9) C14 0.0236(12) 0.0295(13) 0.0232(11) -0.0013(10) -0.004(1) -0.0021(10) C15 0.0222(12) 0.0394(15) 0.0232(12) 0.0008(11) 0.0002(10) -0.0023(11) C16 0.0293(13) 0.0383(15) 0.0251(12) 0.0053(11) -0.0011(10) -0.0145(11) C17 0.0293(13) 0.0272(13) 0.0274(12) 0.0012(10) -0.0046(10) -0.0111(10) C18 0.0202(11) 0.0246(12) 0.0204(11) 0.0009(9) -0.0047(9) -0.0052(9) C19 0.0273(12) 0.0190(11) 0.0223(11) -0.0020(9) -0.0058(9) -0.0054(9) N20 0.0205(9) 0.0203(9) 0.0178(9) -0.0033(7) -0.0055(7) -0.0023(7) O21 0.0328(9) 0.0174(8) 0.0199(8) -0.0038(6) 0.0014(7) -0.0023(7) O22 0.0325(10) 0.0213(9) 0.0233(8) -0.0045(7) 0.0019(7) -0.0040(7) C23 0.0227(11) 0.0279(13) 0.0218(11) -0.0068(9) -0.0041(9) -0.0037(9) C24 0.0399(15) 0.0272(13) 0.0275(13) -0.0050(11) -0.0037(11) 0.0011(11) C25 0.0444(17) 0.0368(16) 0.0342(15) -0.0134(13) -0.0001(13) 0.0077(13) C26 0.0344(15) 0.0473(18) 0.0275(13) -0.0128(12) 0.0030(12) 0.0023(13) C27 0.0283(13) 0.0409(16) 0.0215(12) -0.0050(11) -0.0026(10) -0.0040(11) C28 0.0209(11) 0.0324(13) 0.0199(11) -0.0077(10) -0.0048(9) -0.0016(10) C29 0.0234(12) 0.0308(13) 0.0180(10) -0.0011(9) -0.0045(9) -0.0061(10) N30 0.0218(10) 0.0216(10) 0.0201(9) -0.0022(8) -0.0038(8) -0.0053(8) O31 0.0338(10) 0.0214(9) 0.0200(8) -0.0005(7) -0.0014(7) -0.0014(7) O32 0.0230(9) 0.0234(9) 0.0272(9) 0.0044(7) -0.0100(7) -0.0041(7) O33 0.0198(8) 0.0280(9) 0.0235(8) 0.0006(7) -0.0051(7) -0.0032(7) C34 0.0177(10) 0.0204(11) 0.0259(11) -0.0028(9) -0.0062(9) 0.0016(8) C35 0.0243(12) 0.0344(14) 0.0327(13) 0.0003(11) -0.0113(11) -0.0092(10) C36 0.0212(12) 0.0325(14) 0.0398(15) -0.0051(12) -0.0040(11) -0.0097(10) C37 0.0231(12) 0.0338(14) 0.0280(12) -0.0092(11) -0.0024(10) -0.0104(10) C38 0.0207(11) 0.0315(13) 0.0262(12) -0.0065(10) -0.0034(9) -0.0076(10) C39 0.0220(12) 0.0294(13) 0.0308(13) -0.0070(10) -0.0038(10) -0.0010(10) C40 0.0237(12) 0.0393(15) 0.0281(13) -0.0056(11) -0.0009(10) -0.0074(11) C41 0.0324(14) 0.0331(14) 0.0287(13) -0.0052(11) -0.0059(11) -0.0103(11) C42 0.0320(14) 0.0269(13) 0.0392(15) -0.0073(11) -0.0059(12) 0.0000(11) C43 0.0233(12) 0.0334(14) 0.0358(14) -0.0128(11) -0.0020(11) -0.0025(10) C44 0.0508(19) 0.0366(16) 0.0352(16) -0.0020(13) -0.0025(14) -0.0108(14) O45 0.0347(11) 0.0377(11) 0.0367(11) -0.0098(9) 0.0084(9) -0.0115(9) O46 0.0235(9) 0.0397(11) 0.0252(9) -0.0097(8) -0.0007(7) -0.0111(8) O47 0.0213(9) 0.0310(10) 0.0317(9) -0.0108(8) -0.0074(7) 0.0011(7) C48 0.0303(15) 0.0354(16) 0.058(2) 0.0034(14) -0.0228(14) -0.0042(12) C49 0.0276(15) 0.062(2) 0.076(3) -0.036(2) -0.0122(16) 0.0105(15) O50 0.110(2) 0.0391(14) 0.0675(18) -0.0126(13) -0.0400(17) 0.0243(15) O51 0.0356(11) 0.0569(14) 0.0232(9) 0.0020(9) -0.0050(8) -0.0188(10) C52 0.0359(17) 0.087(3) 0.0336(16) -0.0006(17) -0.0117(13) -0.0210(17) C53 0.0337(18) 0.114(4) 0.0432(19) 0.006(2) -0.0072(15) -0.027(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3235(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 . Mn2 . 3.1533(5) yes Mn1 . O1 . 1.8633(15) yes Mn1 . O2 . 1.8595(17) yes Mn1 . N10 . 2.0128(19) yes Mn1 . O31 . 1.9100(17) yes Mn1 . O32 . 2.0956(17) yes Mn2 . O11 2_765 2.4499(17) yes Mn2 . Mn2 2_765 3.3464(7) yes Mn2 . Mn3 . 3.2563(5) yes Mn2 . O1 . 1.8686(15) yes Mn2 . O11 . 1.9325(16) yes Mn2 . O12 . 1.8715(16) yes Mn2 . N20 . 1.9933(19) yes Mn2 . O33 . 2.1289(17) yes Mn3 . O1 . 1.8774(15) yes Mn3 . O21 . 1.9285(17) yes Mn3 . O22 . 1.8581(17) yes Mn3 . N30 . 2.004(2) yes Mn3 . O46 . 2.2064(18) yes Mn3 . O47 . 2.2715(18) yes O2 . C3 . 1.331(3) yes C3 . C4 . 1.407(3) yes C3 . C8 . 1.411(3) yes C4 . C5 . 1.378(4) yes C4 . H41 . 0.932 no C5 . C6 . 1.391(4) yes C5 . H51 . 0.936 no C6 . C7 . 1.374(4) yes C6 . H61 . 0.927 no C7 . C8 . 1.407(3) yes C7 . H71 . 0.937 no C8 . C9 . 1.435(3) yes C9 . N10 . 1.288(3) yes C9 . H91 . 0.938 no N10 . O11 . 1.389(2) yes O12 . C13 . 1.339(3) yes C13 . C14 . 1.404(3) yes C13 . C18 . 1.405(3) yes C14 . C15 . 1.379(4) yes C14 . H141 . 0.935 no C15 . C16 . 1.384(4) yes C15 . H151 . 0.915 no C16 . C17 . 1.380(3) yes C16 . H161 . 0.930 no C17 . C18 . 1.408(3) yes C17 . H171 . 0.925 no C18 . C19 . 1.449(3) yes C19 . N20 . 1.289(3) yes C19 . H191 . 0.919 no N20 . O21 . 1.378(2) yes O22 . C23 . 1.331(3) yes C23 . C24 . 1.403(3) yes C23 . C28 . 1.410(3) yes C24 . C25 . 1.377(4) yes C24 . H241 . 0.936 no C25 . C26 . 1.392(4) yes C25 . H251 . 0.927 no C26 . C27 . 1.368(4) yes C26 . H261 . 0.928 no C27 . C28 . 1.409(3) yes C27 . H271 . 0.928 no C28 . C29 . 1.450(3) yes C29 . N30 . 1.288(3) yes C29 . H291 . 0.927 no N30 . O31 . 1.374(2) yes O32 . C34 . 1.262(3) yes O33 . C34 . 1.259(3) yes C34 . C35 . 1.518(3) yes C35 . C36 . 1.525(4) yes C35 . H351 . 0.973 no C35 . H352 . 0.973 no C36 . C37 . 1.504(4) yes C36 . H361 . 0.978 no C36 . H362 . 0.956 no C37 . C38 . 1.486(4) yes C37 . O45 . 1.226(3) yes C38 . C39 . 1.401(3) yes C38 . C43 . 1.391(4) yes C39 . C40 . 1.385(4) yes C39 . H391 . 0.921 no C40 . C41 . 1.383(4) yes C40 . H401 . 0.912 no C41 . C42 . 1.400(4) yes C41 . C44 . 1.506(4) yes C42 . C43 . 1.378(4) yes C42 . H421 . 0.926 no C43 . H431 . 0.921 no C44 . H441 . 0.941 no C44 . H442 . 0.968 no C44 . H443 . 0.951 no O46 . H461 . 0.827 no O46 . H462 . 0.800 no O47 . C48 . 1.428(3) yes O47 . H471 . 0.797 no C48 . C49 . 1.499(4) yes C48 . H481 . 0.960 no C48 . H482 . 0.978 no C49 . H491 . 0.961 no C49 . H492 . 0.970 no C49 . H493 . 0.957 no O50 . H501 . 0.826 no O50 . H502 . 0.829 no O51 . C52 . 1.403(3) yes O51 . H511 . 0.802 no C52 . C53 . 1.471(4) yes C52 . H521 . 0.958 no C52 . H522 . 0.970 no C53 . H531 . 0.960 no C53 . H532 . 0.951 no C53 . H533 . 0.969 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 . O1 . 32.38(5) yes Mn2 . Mn1 . O2 . 149.75(6) yes O1 . Mn1 . O2 . 168.15(8) yes Mn2 . Mn1 . N10 . 60.80(5) yes O1 . Mn1 . N10 . 88.21(7) yes O2 . Mn1 . N10 . 89.59(8) yes Mn2 . Mn1 . O31 . 123.81(5) yes O1 . Mn1 . O31 . 92.06(7) yes O2 . Mn1 . O31 . 86.09(7) yes N10 . Mn1 . O31 . 160.19(8) yes Mn2 . Mn1 . O32 . 79.46(5) yes O1 . Mn1 . O32 . 93.01(7) yes O2 . Mn1 . O32 . 98.79(7) yes N10 . Mn1 . O32 . 95.38(7) yes O31 . Mn1 . O32 . 104.38(8) yes O11 2_765 Mn2 . Mn1 . 103.08(4) yes O11 2_765 Mn2 . Mn2 2_765 34.79(4) yes Mn1 . Mn2 . Mn2 2_765 85.677(14) yes O11 2_765 Mn2 . Mn3 . 83.39(4) yes Mn1 . Mn2 . Mn3 . 60.747(11) yes Mn2 2_765 Mn2 . Mn3 . 100.795(15) yes O11 2_765 Mn2 . O1 . 87.16(6) yes Mn1 . Mn2 . O1 . 32.28(5) yes Mn2 2_765 Mn2 . O1 . 87.81(5) yes Mn3 . Mn2 . O1 . 29.70(5) yes O11 2_765 Mn2 . O11 . 81.12(6) yes Mn1 . Mn2 . O11 . 65.32(5) yes Mn2 2_765 Mn2 . O11 . 46.33(5) yes Mn3 . Mn2 . O11 . 118.05(5) yes O1 . Mn2 . O11 . 89.81(7) yes O11 2_765 Mn2 . O12 . 89.87(6) yes Mn1 . Mn2 . O12 . 147.85(5) yes Mn2 2_765 Mn2 . O12 . 88.96(5) yes Mn3 . Mn2 . O12 . 151.10(5) yes O1 . Mn2 . O12 . 176.72(7) yes O11 2_765 Mn2 . N20 . 84.97(7) yes Mn1 . Mn2 . N20 . 118.58(6) yes Mn2 2_765 Mn2 . N20 . 119.76(6) yes Mn3 . Mn2 . N20 . 60.02(5) yes O1 . Mn2 . N20 . 89.66(7) yes O11 2_765 Mn2 . O33 . 177.62(6) yes Mn1 . Mn2 . O33 . 75.62(5) yes Mn2 2_765 Mn2 . O33 . 146.30(5) yes Mn3 . Mn2 . O33 . 94.23(5) yes O1 . Mn2 . O33 . 90.74(7) yes O11 . Mn2 . O12 . 88.35(7) yes O11 . Mn2 . N20 . 166.09(8) yes O12 . Mn2 . N20 . 91.47(7) yes O11 . Mn2 . O33 . 100.02(7) yes O12 . Mn2 . O33 . 92.25(7) yes N20 . Mn2 . O33 . 93.89(7) yes Mn2 . Mn3 . O1 . 29.55(5) yes Mn2 . Mn3 . O21 . 62.06(5) yes O1 . Mn3 . O21 . 91.54(7) yes Mn2 . Mn3 . O22 . 149.96(6) yes O1 . Mn3 . O22 . 172.26(8) yes O21 . Mn3 . O22 . 88.40(7) yes Mn2 . Mn3 . N30 . 118.00(6) yes O1 . Mn3 . N30 . 88.74(7) yes O21 . Mn3 . N30 . 175.98(8) yes O22 . Mn3 . N30 . 91.86(8) yes Mn2 . Mn3 . O46 . 94.05(5) yes O1 . Mn3 . O46 . 94.39(7) yes O21 . Mn3 . O46 . 94.02(7) yes O22 . Mn3 . O46 . 93.33(8) yes N30 . Mn3 . O46 . 81.96(7) yes Mn2 . Mn3 . O47 . 89.87(4) yes O1 . Mn3 . O47 . 83.45(7) yes O21 . Mn3 . O47 . 97.84(7) yes O22 . Mn3 . O47 . 88.89(7) yes N30 . Mn3 . O47 . 86.18(7) yes O46 . Mn3 . O47 . 167.99(7) yes Mn3 . O1 . Mn2 . 120.75(8) yes Mn3 . O1 . Mn1 . 120.16(8) yes Mn2 . O1 . Mn1 . 115.34(8) yes Mn1 . O2 . C3 . 132.10(16) yes O2 . C3 . C4 . 118.7(2) yes O2 . C3 . C8 . 123.3(2) yes C4 . C3 . C8 . 118.0(2) yes C3 . C4 . C5 . 120.6(3) yes C3 . C4 . H41 . 118.9 no C5 . C4 . H41 . 120.4 no C4 . C5 . C6 . 121.7(3) yes C4 . C5 . H51 . 118.5 no C6 . C5 . H51 . 119.8 no C5 . C6 . C7 . 118.4(3) yes C5 . C6 . H61 . 120.8 no C7 . C6 . H61 . 120.8 no C6 . C7 . C8 . 121.5(3) yes C6 . C7 . H71 . 119.4 no C8 . C7 . H71 . 119.1 no C3 . C8 . C7 . 119.7(2) yes C3 . C8 . C9 . 122.4(2) yes C7 . C8 . C9 . 117.8(2) yes C8 . C9 . N10 . 124.6(2) yes C8 . C9 . H91 . 117.3 no N10 . C9 . H91 . 118.0 no Mn1 . N10 . C9 . 127.62(16) yes Mn1 . N10 . O11 . 117.82(13) yes C9 . N10 . O11 . 114.56(19) yes N10 . O11 . Mn2 2_765 113.58(12) yes N10 . O11 . Mn2 . 113.47(12) yes Mn2 2_765 O11 . Mn2 . 98.88(6) yes Mn2 . O12 . C13 . 127.10(15) yes O12 . C13 . C14 . 118.4(2) yes O12 . C13 . C18 . 123.2(2) yes C14 . C13 . C18 . 118.4(2) yes C13 . C14 . C15 . 120.7(2) yes C13 . C14 . H141 . 119.0 no C15 . C14 . H141 . 120.4 no C14 . C15 . C16 . 121.2(2) yes C14 . C15 . H151 . 119.7 no C16 . C15 . H151 . 119.2 no C15 . C16 . C17 . 119.2(2) yes C15 . C16 . H161 . 121.5 no C17 . C16 . H161 . 119.3 no C16 . C17 . C18 . 120.8(2) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 119.0 no C17 . C18 . C13 . 119.8(2) yes C17 . C18 . C19 . 116.8(2) yes C13 . C18 . C19 . 123.5(2) yes C18 . C19 . N20 . 123.7(2) yes C18 . C19 . H191 . 118.8 no N20 . C19 . H191 . 117.5 no Mn2 . N20 . C19 . 126.33(16) yes Mn2 . N20 . O21 . 117.84(14) yes C19 . N20 . O21 . 115.69(19) yes N20 . O21 . Mn3 . 117.71(13) yes Mn3 . O22 . C23 . 129.75(16) yes O22 . C23 . C24 . 118.0(2) yes O22 . C23 . C28 . 123.3(2) yes C24 . C23 . C28 . 118.7(2) yes C23 . C24 . C25 . 120.8(3) yes C23 . C24 . H241 . 119.5 no C25 . C24 . H241 . 119.7 no C24 . C25 . C26 . 120.6(3) yes C24 . C25 . H251 . 119.4 no C26 . C25 . H251 . 120.0 no C25 . C26 . C27 . 119.5(3) yes C25 . C26 . H261 . 121.0 no C27 . C26 . H261 . 119.5 no C26 . C27 . C28 . 121.3(3) yes C26 . C27 . H271 . 119.8 no C28 . C27 . H271 . 118.9 no C23 . C28 . C27 . 119.1(2) yes C23 . C28 . C29 . 123.6(2) yes C27 . C28 . C29 . 117.3(2) yes C28 . C29 . N30 . 124.0(2) yes C28 . C29 . H291 . 119.9 no N30 . C29 . H291 . 116.1 no Mn3 . N30 . C29 . 126.35(18) yes Mn3 . N30 . O31 . 117.74(13) yes C29 . N30 . O31 . 115.8(2) yes N30 . O31 . Mn1 . 118.61(13) yes Mn1 . O32 . C34 . 125.98(15) yes Mn2 . O33 . C34 . 129.07(15) yes O32 . C34 . O33 . 125.7(2) yes O32 . C34 . C35 . 116.4(2) yes O33 . C34 . C35 . 117.8(2) yes C34 . C35 . C36 . 114.3(2) yes C34 . C35 . H351 . 106.1 no C36 . C35 . H351 . 107.9 no C34 . C35 . H352 . 107.8 no C36 . C35 . H352 . 110.5 no H351 . C35 . H352 . 110.1 no C35 . C36 . C37 . 115.2(2) yes C35 . C36 . H361 . 108.5 no C37 . C36 . H361 . 108.1 no C35 . C36 . H362 . 109.3 no C37 . C36 . H362 . 106.5 no H361 . C36 . H362 . 109.2 no C36 . C37 . C38 . 118.7(2) yes C36 . C37 . O45 . 121.9(2) yes C38 . C37 . O45 . 119.4(2) yes C37 . C38 . C39 . 122.2(2) yes C37 . C38 . C43 . 119.4(2) yes C39 . C38 . C43 . 118.4(2) yes C38 . C39 . C40 . 120.3(2) yes C38 . C39 . H391 . 120.6 no C40 . C39 . H391 . 119.1 no C39 . C40 . C41 . 121.3(2) yes C39 . C40 . H401 . 119.0 no C41 . C40 . H401 . 119.7 no C40 . C41 . C42 . 118.2(3) yes C40 . C41 . C44 . 121.4(3) yes C42 . C41 . C44 . 120.4(3) yes C41 . C42 . C43 . 120.8(3) yes C41 . C42 . H421 . 119.3 no C43 . C42 . H421 . 119.8 no C38 . C43 . C42 . 121.0(2) yes C38 . C43 . H431 . 118.8 no C42 . C43 . H431 . 120.2 no C41 . C44 . H441 . 110.8 no C41 . C44 . H442 . 111.0 no H441 . C44 . H442 . 107.6 no C41 . C44 . H443 . 110.9 no H441 . C44 . H443 . 107.9 no H442 . C44 . H443 . 108.5 no Mn3 . O46 . H461 . 116.3 no Mn3 . O46 . H462 . 123.7 no H461 . O46 . H462 . 106.4 no Mn3 . O47 . C48 . 127.33(17) yes Mn3 . O47 . H471 . 109.3 no C48 . O47 . H471 . 112.5 no O47 . C48 . C49 . 110.9(3) yes O47 . C48 . H481 . 108.7 no C49 . C48 . H481 . 109.6 no O47 . C48 . H482 . 108.3 no C49 . C48 . H482 . 110.2 no H481 . C48 . H482 . 109.0 no C48 . C49 . H491 . 108.3 no C48 . C49 . H492 . 109.5 no H491 . C49 . H492 . 109.8 no C48 . C49 . H493 . 109.1 no H491 . C49 . H493 . 108.9 no H492 . C49 . H493 . 111.1 no H501 . O50 . H502 . 94.2 no C52 . O51 . H511 . 104.3 no O51 . C52 . C53 . 111.7(3) yes O51 . C52 . H521 . 105.8 no C53 . C52 . H521 . 107.5 no O51 . C52 . H522 . 111.6 no C53 . C52 . H522 . 109.3 no H521 . C52 . H522 . 110.8 no C52 . C53 . H531 . 106.6 no C52 . C53 . H532 . 111.4 no H531 . C53 . H532 . 109.0 no C52 . C53 . H533 . 110.5 no H531 . C53 . H533 . 108.9 no H532 . C53 . H533 . 110.4 no # Attachment '[4]CCDC706508.cif' data_EB8006 _database_code_depnum_ccdc_archive 'CCDC 706508' _cell_length_a 12.1880(3) _cell_length_b 12.2015(3) _cell_length_c 13.3261(3) _cell_angle_alpha 101.143(1) _cell_angle_beta 96.929(1) _cell_angle_gamma 106.861(1) _cell_volume 1827.56(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C72 H68 Mn6 N14 O20 # Dc = 1.62 Fooo = 776.00 Mu = 10.90 M = 889.49 # Found Formula = C60 H50 Mn6 N8 O20 # Dc = 1.39 FOOO = 776.00 Mu = 10.75 M = 766.33 _chemical_formula_sum 'C72 H68 Mn6 N14 O20' _chemical_formula_weight 1778.98 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.29 _exptl_crystal_density_diffrn 1.62 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.090 # Sheldrick geometric approximatio 0.76 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.85 _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 27345 _reflns_number_total 7457 _diffrn_reflns_av_R_equivalents 0.041 # Number of reflections with Friedels Law is 7457 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7474 _diffrn_reflns_theta_min 1.778 _diffrn_reflns_theta_max 26.371 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.371 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -15 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 1.49 _oxford_diffrn_Wilson_scale 6.87 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.50 _refine_diff_density_max 0.51 # 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 7428 _refine_ls_number_restraints 0 _refine_ls_number_parameters 424 _oxford_refine_ls_R_factor_ref 0.0478 _refine_ls_wR_factor_ref 0.0883 _refine_ls_goodness_of_fit_ref 0.8895 _refine_ls_shift/su_max 0.000342 # The values computed from all data _oxford_reflns_number_all 7428 _refine_ls_R_factor_all 0.0478 _refine_ls_wR_factor_all 0.0883 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5865 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_gt 0.0850 # 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^ + 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. 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 0.44849(3) 0.02262(3) 0.24033(3) 0.0182 1.0000 Uani . . . . . . . Mn2 Mn 0.53912(3) 0.14222(3) 0.06269(3) 0.0183 1.0000 Uani . . . . . . . Mn3 Mn 0.29594(3) 0.16102(3) 0.12919(3) 0.0192 1.0000 Uani . . . . . . . O4 O 0.41704(15) 0.09543(14) 0.13419(13) 0.0180 1.0000 Uani . . . . . . . O5 O 0.46301(16) -0.07318(16) 0.33036(14) 0.0242 1.0000 Uani . . . . . . . C6 C 0.5538(2) -0.1047(2) 0.3627(2) 0.0205 1.0000 Uani . . . . . . . C7 C 0.5582(2) -0.1411(2) 0.4563(2) 0.0250 1.0000 Uani . . . . . . . C8 C 0.6487(3) -0.1780(2) 0.4918(2) 0.0288 1.0000 Uani . . . . . . . C9 C 0.7394(3) -0.1787(3) 0.4373(2) 0.0316 1.0000 Uani . . . . . . . C10 C 0.7363(2) -0.1428(2) 0.3454(2) 0.0280 1.0000 Uani . . . . . . . C11 C 0.6444(2) -0.1054(2) 0.30655(19) 0.0213 1.0000 Uani . . . . . . . C12 C 0.6464(2) -0.0694(2) 0.2099(2) 0.0211 1.0000 Uani . . . . . . . N13 N 0.57507(18) -0.02005(18) 0.17460(15) 0.0191 1.0000 Uani . . . . . . . O14 O 0.58851(15) 0.00649(15) 0.07928(13) 0.0199 1.0000 Uani . . . . . . . O15 O 0.65160(16) 0.17792(15) -0.02034(14) 0.0245 1.0000 Uani . . . . . . . C16 C 0.6857(2) 0.2713(2) -0.0609(2) 0.0225 1.0000 Uani . . . . . . . C17 C 0.7889(3) 0.2906(3) -0.1014(2) 0.0334 1.0000 Uani . . . . . . . C18 C 0.8270(3) 0.3855(3) -0.1450(3) 0.0424 1.0000 Uani . . . . . . . C19 C 0.7648(3) 0.4646(3) -0.1489(3) 0.0415 1.0000 Uani . . . . . . . C20 C 0.6629(3) 0.4460(3) -0.1109(2) 0.0355 1.0000 Uani . . . . . . . C21 C 0.6212(2) 0.3490(2) -0.0669(2) 0.0249 1.0000 Uani . . . . . . . C22 C 0.5103(2) 0.3329(2) -0.0333(2) 0.0251 1.0000 Uani . . . . . . . N23 N 0.46561(19) 0.25467(19) 0.01582(16) 0.0216 1.0000 Uani . . . . . . . O24 O 0.35489(16) 0.24778(17) 0.03196(15) 0.0273 1.0000 Uani . . . . . . . O25 O 0.16924(16) 0.21864(17) 0.12036(15) 0.0275 1.0000 Uani . . . . . . . C26 C 0.0817(2) 0.2065(2) 0.1725(2) 0.0223 1.0000 Uani . . . . . . . C27 C -0.0028(2) 0.2600(2) 0.1490(2) 0.0280 1.0000 Uani . . . . . . . C28 C -0.0979(2) 0.2467(2) 0.1974(2) 0.0301 1.0000 Uani . . . . . . . C29 C -0.1119(2) 0.1815(3) 0.2728(2) 0.0325 1.0000 Uani . . . . . . . C30 C -0.0286(2) 0.1300(2) 0.2986(2) 0.0296 1.0000 Uani . . . . . . . C31 C 0.0681(2) 0.1407(2) 0.2497(2) 0.0234 1.0000 Uani . . . . . . . C32 C 0.1486(2) 0.0815(2) 0.2792(2) 0.0242 1.0000 Uani . . . . . . . N33 N 0.23925(19) 0.08023(18) 0.23953(16) 0.0210 1.0000 Uani . . . . . . . O34 O 0.30191(16) 0.01560(16) 0.27827(14) 0.0258 1.0000 Uani . . . . . . . C35 C 0.7088(2) 0.3710(2) 0.3801(2) 0.0257 1.0000 Uani . . . . . . . C36 C 0.6928(3) 0.3872(3) 0.4825(2) 0.0398 1.0000 Uani . . . . . . . C37 C 0.7626(3) 0.4870(3) 0.5572(3) 0.0514 1.0000 Uani . . . . . . . C38 C 0.8497(3) 0.5703(3) 0.5309(3) 0.0542 1.0000 Uani . . . . . . . C39 C 0.8657(3) 0.5556(3) 0.4289(3) 0.0569 1.0000 Uani . . . . . . . C40 C 0.7948(3) 0.4569(3) 0.3539(3) 0.0397 1.0000 Uani . . . . . . . C41 C 0.6350(2) 0.2620(2) 0.3001(2) 0.0215 1.0000 Uani . . . . . . . O42 O 0.57049(16) 0.18050(15) 0.33330(13) 0.0235 1.0000 Uani . . . . . . . O43 O 0.64453(15) 0.25794(15) 0.20618(13) 0.0227 1.0000 Uani . . . . . . . N44 N 0.4029(2) 0.3324(2) 0.26376(19) 0.0319 1.0000 Uani . . . . . . . C45 C 0.4568(3) 0.4262(3) 0.3034(2) 0.0334 1.0000 Uani . . . . . . . C46 C 0.5259(3) 0.5483(3) 0.3553(3) 0.0557 1.0000 Uani . . . . . . . O47 O 0.19106(17) -0.00247(17) 0.00619(15) 0.0350 1.0000 Uani . . . . . . . H361 H 0.6345 0.3314 0.5007 0.0452 1.0000 Uiso R . . . . . . H371 H 0.7510 0.4957 0.6249 0.0574 1.0000 Uiso R . . . . . . H381 H 0.8975 0.6397 0.5798 0.0575 1.0000 Uiso R . . . . . . H391 H 0.9275 0.6124 0.4094 0.0608 1.0000 Uiso R . . . . . . H401 H 0.8051 0.4502 0.2849 0.0452 1.0000 Uiso R . . . . . . H321 H 0.1330 0.0393 0.3324 0.0299 1.0000 Uiso R . . . . . . H271 H 0.0058 0.3055 0.0991 0.0347 1.0000 Uiso R . . . . . . H281 H -0.1532 0.2814 0.1794 0.0370 1.0000 Uiso R . . . . . . H291 H -0.1773 0.1719 0.3068 0.0381 1.0000 Uiso R . . . . . . H301 H -0.0348 0.0870 0.3529 0.0363 1.0000 Uiso R . . . . . . H101 H 0.7966 -0.1440 0.3068 0.0345 1.0000 Uiso R . . . . . . H91 H 0.8037 -0.2028 0.4606 0.0387 1.0000 Uiso R . . . . . . H81 H 0.6501 -0.2041 0.5540 0.0337 1.0000 Uiso R . . . . . . H71 H 0.4999 -0.1375 0.4946 0.0290 1.0000 Uiso R . . . . . . H221 H 0.4658 0.3840 -0.0492 0.0329 1.0000 Uiso R . . . . . . H201 H 0.6214 0.4997 -0.1125 0.0462 1.0000 Uiso R . . . . . . H191 H 0.7926 0.5314 -0.1763 0.0525 1.0000 Uiso R . . . . . . H181 H 0.8977 0.3943 -0.1718 0.0537 1.0000 Uiso R . . . . . . H171 H 0.8331 0.2403 -0.0993 0.0437 1.0000 Uiso R . . . . . . H463 H 0.5495 0.5537 0.4276 0.0777 1.0000 Uiso R . . . . . . H461 H 0.5917 0.5698 0.3246 0.0780 1.0000 Uiso R . . . . . . H462 H 0.4820 0.5994 0.3502 0.0775 1.0000 Uiso R . . . . . . H121 H 0.7014 -0.0839 0.1716 0.0253 1.0000 Uiso R . . . . . . H471 H 0.1264 -0.0347 0.0110 0.0513 1.0000 Uiso R . . . . . . H472 H 0.2266 -0.0422 -0.0158 0.0504 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 0.0209(2) 0.0205(2) 0.0169(2) 0.00689(16) 0.00718(16) 0.00929(17) Mn2 0.0213(2) 0.0206(2) 0.0173(2) 0.00713(16) 0.00795(16) 0.01003(17) Mn3 0.0204(2) 0.0233(2) 0.0185(2) 0.00750(16) 0.00772(16) 0.01076(17) O4 0.0203(9) 0.0196(9) 0.0179(9) 0.0075(7) 0.0066(7) 0.0089(7) O5 0.0257(10) 0.0284(10) 0.0245(10) 0.0122(8) 0.0094(8) 0.0123(8) C6 0.0234(14) 0.0166(12) 0.0197(13) 0.0030(10) 0.0003(11) 0.0062(11) C7 0.0306(16) 0.0238(14) 0.0212(14) 0.0064(11) 0.0074(12) 0.0077(12) C8 0.0393(17) 0.0257(14) 0.0193(14) 0.0080(11) 0.0006(13) 0.0076(13) C9 0.0351(17) 0.0339(16) 0.0280(15) 0.0103(13) -0.0010(13) 0.0155(14) C10 0.0271(15) 0.0306(15) 0.0270(15) 0.0070(12) 0.0045(12) 0.0105(13) C11 0.0250(14) 0.0222(13) 0.0169(13) 0.0040(10) 0.0009(11) 0.0094(11) C12 0.0217(14) 0.0220(13) 0.0208(13) 0.0029(11) 0.0051(11) 0.0097(11) N13 0.0234(12) 0.0224(11) 0.0118(10) 0.0042(9) 0.0061(9) 0.0065(9) O14 0.0271(10) 0.0245(9) 0.0132(8) 0.0073(7) 0.0068(8) 0.0130(8) O15 0.0284(11) 0.0256(10) 0.0273(10) 0.0128(8) 0.0143(8) 0.0126(8) C16 0.0273(15) 0.0236(13) 0.0176(13) 0.0068(11) 0.0070(11) 0.0075(12) C17 0.0322(17) 0.0379(17) 0.0387(18) 0.0192(14) 0.0152(14) 0.0141(14) C18 0.0353(18) 0.049(2) 0.052(2) 0.0278(17) 0.0244(16) 0.0098(16) C19 0.045(2) 0.0385(18) 0.049(2) 0.0261(16) 0.0216(17) 0.0099(16) C20 0.0378(18) 0.0367(17) 0.0409(18) 0.0221(15) 0.0159(15) 0.0138(14) C21 0.0295(15) 0.0253(14) 0.0233(14) 0.0103(11) 0.0095(12) 0.0092(12) C22 0.0309(16) 0.0278(14) 0.0228(14) 0.0109(12) 0.0090(12) 0.0140(12) N23 0.0222(12) 0.0258(12) 0.0199(11) 0.0053(9) 0.0076(9) 0.0110(10) O24 0.0254(10) 0.0363(11) 0.0329(11) 0.0188(9) 0.0146(9) 0.0187(9) O25 0.0244(10) 0.0368(11) 0.0329(11) 0.0170(9) 0.0123(9) 0.0188(9) C26 0.0198(14) 0.0225(13) 0.0223(14) 0.0014(11) 0.0052(11) 0.0056(11) C27 0.0277(15) 0.0285(15) 0.0306(16) 0.0066(12) 0.0063(13) 0.0131(13) C28 0.0233(15) 0.0303(15) 0.0387(17) 0.0045(13) 0.0074(13) 0.0133(13) C29 0.0222(15) 0.0349(16) 0.0413(18) 0.0031(14) 0.0138(13) 0.0113(13) C30 0.0261(15) 0.0294(15) 0.0349(16) 0.0090(13) 0.0120(13) 0.0083(13) C31 0.0194(14) 0.0230(13) 0.0256(14) 0.0011(11) 0.0065(11) 0.0057(11) C32 0.0240(15) 0.0264(14) 0.0237(14) 0.0071(11) 0.0085(12) 0.0079(12) N33 0.0214(12) 0.0228(11) 0.0210(11) 0.0062(9) 0.0043(9) 0.0095(9) O34 0.0258(10) 0.0328(11) 0.0300(11) 0.0182(9) 0.0120(9) 0.0166(9) C35 0.0267(15) 0.0202(13) 0.0285(15) 0.0021(11) 0.0020(12) 0.0087(12) C36 0.049(2) 0.0347(17) 0.0282(16) 0.0018(14) 0.0042(15) 0.0073(15) C37 0.070(3) 0.043(2) 0.0293(18) -0.0050(15) 0.0001(18) 0.0117(19) C38 0.050(2) 0.0368(19) 0.054(2) -0.0170(17) -0.0059(19) 0.0064(17) C39 0.046(2) 0.0312(18) 0.075(3) -0.0074(18) 0.015(2) -0.0053(16) C40 0.0386(19) 0.0312(16) 0.0434(19) -0.0004(14) 0.0142(16) 0.0056(14) C41 0.0192(13) 0.0235(13) 0.0247(14) 0.0040(11) 0.0048(11) 0.0120(11) O42 0.0278(10) 0.0241(10) 0.0175(9) 0.0044(8) 0.0044(8) 0.0071(8) O43 0.0217(10) 0.0252(10) 0.0205(10) 0.0036(8) 0.0056(8) 0.0071(8) N44 0.0347(15) 0.0285(13) 0.0336(14) 0.0040(11) 0.0054(12) 0.0148(12) C45 0.0371(18) 0.0305(16) 0.0343(17) 0.0026(14) 0.0031(14) 0.0182(14) C46 0.054(2) 0.0302(18) 0.070(3) -0.0068(17) -0.010(2) 0.0138(17) O47 0.0266(11) 0.0378(12) 0.0349(12) -0.0030(9) 0.0049(9) 0.0099(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3720(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . Mn2 . 3.1598(5) yes Mn1 . Mn3 . 3.2596(5) yes Mn1 . O4 . 1.8679(17) yes Mn1 . O5 . 1.8569(18) yes Mn1 . N13 . 2.009(2) yes Mn1 . O34 . 1.8975(18) yes Mn1 . O42 . 2.1043(18) yes Mn2 . O14 2_655 2.3701(17) yes Mn2 . Mn3 . 3.2514(5) yes Mn2 . O4 . 1.8727(17) yes Mn2 . O14 . 1.9601(17) yes Mn2 . O15 . 1.8706(18) yes Mn2 . N23 . 1.996(2) yes Mn2 . O43 . 2.1475(18) yes Mn3 . O4 . 1.8722(17) yes Mn3 . O24 . 1.9051(18) yes Mn3 . O25 . 1.8738(18) yes Mn3 . N33 . 2.005(2) yes Mn3 . N44 . 2.386(2) yes Mn3 . O47 . 2.2475(19) yes O5 . C6 . 1.324(3) yes C6 . C7 . 1.403(3) yes C6 . C11 . 1.407(4) yes C7 . C8 . 1.374(4) yes C7 . H71 . 0.931 no C8 . C9 . 1.395(4) yes C8 . H81 . 0.944 no C9 . C10 . 1.378(4) yes C9 . H91 . 0.953 no C10 . C11 . 1.407(4) yes C10 . H101 . 0.949 no C11 . C12 . 1.439(3) yes C12 . N13 . 1.286(3) yes C12 . H121 . 0.926 no N13 . O14 . 1.387(2) yes O15 . C16 . 1.334(3) yes C16 . C17 . 1.403(4) yes C16 . C21 . 1.404(4) yes C17 . C18 . 1.382(4) yes C17 . H171 . 0.928 no C18 . C19 . 1.394(4) yes C18 . H181 . 0.957 no C19 . C20 . 1.372(4) yes C19 . H191 . 0.948 no C20 . C21 . 1.412(4) yes C20 . H201 . 0.938 no C21 . C22 . 1.446(4) yes C22 . N23 . 1.289(3) yes C22 . H221 . 0.972 no N23 . O24 . 1.373(3) yes O25 . C26 . 1.330(3) yes C26 . C27 . 1.406(4) yes C26 . C31 . 1.419(4) yes C27 . C28 . 1.377(4) yes C27 . H271 . 0.942 no C28 . C29 . 1.393(4) yes C28 . H281 . 0.926 no C29 . C30 . 1.383(4) yes C29 . H291 . 0.952 no C30 . C31 . 1.400(4) yes C30 . H301 . 0.971 no C31 . C32 . 1.438(4) yes C32 . N33 . 1.284(3) yes C32 . H321 . 0.959 no N33 . O34 . 1.372(3) yes C35 . C36 . 1.387(4) yes C35 . C40 . 1.383(4) yes C35 . C41 . 1.496(3) yes C36 . C37 . 1.387(4) yes C36 . H361 . 0.923 no C37 . C38 . 1.373(5) yes C37 . H371 . 0.921 no C38 . C39 . 1.381(5) yes C38 . H381 . 0.943 no C39 . C40 . 1.386(4) yes C39 . H391 . 0.964 no C40 . H401 . 0.933 no C41 . O42 . 1.266(3) yes C41 . O43 . 1.264(3) yes N44 . C45 . 1.126(4) yes C45 . C46 . 1.462(4) yes C46 . H463 . 0.955 no C46 . H461 . 0.938 no C46 . H462 . 0.939 no O47 . H471 . 0.789 no O47 . H472 . 0.778 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 . 60.838(12) yes Mn2 . Mn1 . O4 . 32.40(5) yes Mn3 . Mn1 . O4 . 29.40(5) yes Mn2 . Mn1 . O5 . 149.07(6) yes Mn3 . Mn1 . O5 . 149.63(6) yes O4 . Mn1 . O5 . 170.27(8) yes Mn2 . Mn1 . N13 . 60.79(6) yes Mn3 . Mn1 . N13 . 119.97(6) yes O4 . Mn1 . N13 . 90.61(8) yes O5 . Mn1 . N13 . 88.48(8) yes Mn2 . Mn1 . O34 . 123.06(6) yes Mn3 . Mn1 . O34 . 62.44(5) yes O4 . Mn1 . O34 . 90.77(7) yes O5 . Mn1 . O34 . 87.21(8) yes N13 . Mn1 . O34 . 162.38(8) yes Mn2 . Mn1 . O42 . 80.78(5) yes Mn3 . Mn1 . O42 . 92.89(5) yes O4 . Mn1 . O42 . 92.26(7) yes O5 . Mn1 . O42 . 97.43(8) yes N13 . Mn1 . O42 . 90.74(8) yes O34 . Mn1 . O42 . 106.76(8) yes O14 2_655 Mn2 . Mn1 . 96.62(4) yes O14 2_655 Mn2 . Mn3 . 82.95(4) yes Mn1 . Mn2 . Mn3 . 61.098(12) yes O14 2_655 Mn2 . O4 . 83.90(7) yes Mn1 . Mn2 . O4 . 32.31(5) yes Mn3 . Mn2 . O4 . 29.74(5) yes O14 2_655 Mn2 . O14 . 79.19(7) yes Mn1 . Mn2 . O14 . 64.39(5) yes Mn3 . Mn2 . O14 . 119.55(5) yes O4 . Mn2 . O14 . 90.85(7) yes O14 2_655 Mn2 . O15 . 90.45(7) yes Mn1 . Mn2 . O15 . 149.63(6) yes Mn3 . Mn2 . O15 . 149.27(6) yes O4 . Mn2 . O15 . 174.34(8) yes O14 . Mn2 . O15 . 88.24(7) yes O14 2_655 Mn2 . N23 . 87.65(7) yes Mn1 . Mn2 . N23 . 119.04(6) yes Mn3 . Mn2 . N23 . 59.23(6) yes O4 . Mn2 . N23 . 88.96(8) yes O14 . Mn2 . N23 . 166.78(8) yes O14 2_655 Mn2 . O43 . 170.92(6) yes Mn1 . Mn2 . O43 . 74.40(5) yes Mn3 . Mn2 . O43 . 93.62(5) yes O4 . Mn2 . O43 . 88.96(7) yes O14 . Mn2 . O43 . 95.36(7) yes O15 . Mn2 . N23 . 90.65(8) yes O15 . Mn2 . O43 . 96.68(7) yes N23 . Mn2 . O43 . 97.86(8) yes Mn2 . Mn3 . Mn1 . 58.064(11) yes Mn2 . Mn3 . O4 . 29.75(5) yes Mn1 . Mn3 . O4 . 29.33(5) yes Mn2 . Mn3 . O24 . 62.74(5) yes Mn1 . Mn3 . O24 . 120.52(6) yes O4 . Mn3 . O24 . 92.39(7) yes Mn2 . Mn3 . O25 . 151.40(6) yes Mn1 . Mn3 . O25 . 150.30(6) yes O4 . Mn3 . O25 . 176.92(8) yes O24 . Mn3 . O25 . 88.65(8) yes Mn2 . Mn3 . N33 . 117.66(6) yes Mn1 . Mn3 . N33 . 59.62(6) yes O4 . Mn3 . N33 . 88.29(8) yes O24 . Mn3 . N33 . 175.93(9) yes O25 . Mn3 . N33 . 90.88(8) yes Mn2 . Mn3 . N44 . 89.85(6) yes Mn1 . Mn3 . N44 . 86.98(6) yes O4 . Mn3 . N44 . 93.88(8) yes O24 . Mn3 . N44 . 87.53(8) yes O25 . Mn3 . N44 . 89.06(8) yes Mn2 . Mn3 . O47 . 91.68(5) yes Mn1 . Mn3 . O47 . 92.77(5) yes O4 . Mn3 . O47 . 86.84(7) yes O24 . Mn3 . O47 . 94.29(8) yes O25 . Mn3 . O47 . 90.20(8) yes N33 . Mn3 . N44 . 88.42(8) yes N33 . Mn3 . O47 . 89.76(8) yes N44 . Mn3 . O47 . 178.02(8) yes Mn2 . O4 . Mn3 . 120.50(9) yes Mn2 . O4 . Mn1 . 115.28(9) yes Mn3 . O4 . Mn1 . 121.27(9) yes Mn1 . O5 . C6 . 129.80(17) yes O5 . C6 . C7 . 118.2(2) yes O5 . C6 . C11 . 123.1(2) yes C7 . C6 . C11 . 118.7(2) yes C6 . C7 . C8 . 120.6(3) yes C6 . C7 . H71 . 118.5 no C8 . C7 . H71 . 120.9 no C7 . C8 . C9 . 121.3(3) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 118.6 no C8 . C9 . C10 . 118.7(3) yes C8 . C9 . H91 . 123.1 no C10 . C9 . H91 . 118.2 no C9 . C10 . C11 . 121.3(3) yes C9 . C10 . H101 . 119.8 no C11 . C10 . H101 . 118.9 no C6 . C11 . C10 . 119.3(2) yes C6 . C11 . C12 . 122.2(2) yes C10 . C11 . C12 . 118.4(2) yes C11 . C12 . N13 . 123.1(2) yes C11 . C12 . H121 . 117.6 no N13 . C12 . H121 . 119.3 no Mn1 . N13 . C12 . 128.07(18) yes Mn1 . N13 . O14 . 116.83(15) yes C12 . N13 . O14 . 115.1(2) yes N13 . O14 . Mn2 2_655 112.63(13) yes N13 . O14 . Mn2 . 112.24(13) yes Mn2 2_655 O14 . Mn2 . 100.81(7) yes Mn2 . O15 . C16 . 129.65(16) yes O15 . C16 . C17 . 118.4(2) yes O15 . C16 . C21 . 122.7(2) yes C17 . C16 . C21 . 118.8(2) yes C16 . C17 . C18 . 120.5(3) yes C16 . C17 . H171 . 121.0 no C18 . C17 . H171 . 118.6 no C17 . C18 . C19 . 120.9(3) yes C17 . C18 . H181 . 117.0 no C19 . C18 . H181 . 122.1 no C18 . C19 . C20 . 119.3(3) yes C18 . C19 . H191 . 120.9 no C20 . C19 . H191 . 119.8 no C19 . C20 . C21 . 121.0(3) yes C19 . C20 . H201 . 119.5 no C21 . C20 . H201 . 119.5 no C20 . C21 . C16 . 119.5(3) yes C20 . C21 . C22 . 117.3(3) yes C16 . C21 . C22 . 123.2(2) yes C21 . C22 . N23 . 124.5(3) yes C21 . C22 . H221 . 118.1 no N23 . C22 . H221 . 117.5 no Mn2 . N23 . C22 . 126.23(19) yes Mn2 . N23 . O24 . 119.00(15) yes C22 . N23 . O24 . 114.7(2) yes N23 . O24 . Mn3 . 117.31(14) yes Mn3 . O25 . C26 . 130.82(17) yes O25 . C26 . C27 . 118.5(2) yes O25 . C26 . C31 . 123.4(2) yes C27 . C26 . C31 . 118.1(2) yes C26 . C27 . C28 . 121.2(3) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 119.6 no C27 . C28 . C29 . 120.9(3) yes C27 . C28 . H281 . 119.4 no C29 . C28 . H281 . 119.7 no C28 . C29 . C30 . 119.0(3) yes C28 . C29 . H291 . 121.5 no C30 . C29 . H291 . 119.6 no C29 . C30 . C31 . 121.4(3) yes C29 . C30 . H301 . 120.5 no C31 . C30 . H301 . 118.1 no C26 . C31 . C30 . 119.5(3) yes C26 . C31 . C32 . 122.8(2) yes C30 . C31 . C32 . 117.7(3) yes C31 . C32 . N33 . 125.1(3) yes C31 . C32 . H321 . 117.3 no N33 . C32 . H321 . 117.5 no Mn3 . N33 . C32 . 126.98(19) yes Mn3 . N33 . O34 . 118.17(15) yes C32 . N33 . O34 . 114.9(2) yes N33 . O34 . Mn1 . 119.32(14) yes C36 . C35 . C40 . 118.6(3) yes C36 . C35 . C41 . 120.4(3) yes C40 . C35 . C41 . 120.9(3) yes C35 . C36 . C37 . 120.6(3) yes C35 . C36 . H361 . 119.5 no C37 . C36 . H361 . 119.9 no C36 . C37 . C38 . 120.3(3) yes C36 . C37 . H371 . 119.2 no C38 . C37 . H371 . 120.5 no C37 . C38 . C39 . 119.6(3) yes C37 . C38 . H381 . 122.1 no C39 . C38 . H381 . 118.3 no C38 . C39 . C40 . 120.1(3) yes C38 . C39 . H391 . 120.7 no C40 . C39 . H391 . 119.2 no C39 . C40 . C35 . 120.7(3) yes C39 . C40 . H401 . 118.8 no C35 . C40 . H401 . 120.5 no C35 . C41 . O42 . 116.7(2) yes C35 . C41 . O43 . 117.5(2) yes O42 . C41 . O43 . 125.7(2) yes Mn1 . O42 . C41 . 125.77(16) yes Mn2 . O43 . C41 . 132.01(17) yes Mn3 . N44 . C45 . 160.4(3) yes N44 . C45 . C46 . 179.5(3) yes C45 . C46 . H463 . 109.2 no C45 . C46 . H461 . 108.3 no H463 . C46 . H461 . 110.0 no C45 . C46 . H462 . 111.3 no H463 . C46 . H462 . 107.6 no H461 . C46 . H462 . 110.5 no Mn3 . O47 . H471 . 118.3 no Mn3 . O47 . H472 . 115.0 no H471 . O47 . H472 . 117.0 no # Attachment '[5]CCDC706509.cif' data_EB8017 _database_code_depnum_ccdc_archive 'CCDC 706509' _cell_length_a 12.7404(3) _cell_length_b 15.4280(4) _cell_length_c 19.0456(5) _cell_angle_alpha 90.075(2) _cell_angle_beta 103.2920(10) _cell_angle_gamma 98.8750(10) _cell_volume 3597.04(16) _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 = C64 H80 Mn6 N6 O24 # Dc = 1.52 Fooo = 1696.00 Mu = 11.01 M = 1646.93 # Found Formula = C64 H80 Mn6 N6 O24 # Dc = 1.52 FOOO = 1696.00 Mu = 11.01 M = 1646.93 _chemical_formula_sum 'C64 H80 Mn6 N6 O24' _chemical_formula_weight 1646.93 _cell_measurement_reflns_used 9898 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.26 _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.101 # Sheldrick geometric approximatio 0.83 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.92 _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 48617 _reflns_number_total 20054 _diffrn_reflns_av_R_equivalents 0.042 # Number of reflections with Friedels Law is 20054 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 22087 _diffrn_reflns_theta_min 1.763 _diffrn_reflns_theta_max 30.571 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 27.820 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min -22 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _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 -0.73 _refine_diff_density_max 0.75 # 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 20003 _refine_ls_number_restraints 24 _refine_ls_number_parameters 910 _oxford_refine_ls_R_factor_ref 0.0739 _refine_ls_wR_factor_ref 0.1305 _refine_ls_goodness_of_fit_ref 1.0171 _refine_ls_shift/su_max 0.000604 # The values computed from all data _oxford_reflns_number_all 20003 _refine_ls_R_factor_all 0.0739 _refine_ls_wR_factor_all 0.1305 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 15709 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_gt 0.1191 # 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^ + 0.61P] ,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 0.17142(4) 0.23387(3) 0.03183(2) 0.0216 1.0000 Uani . . . . . . . Mn2 Mn 0.15719(4) 0.08926(3) 0.15593(2) 0.0180 1.0000 Uani . . . . . . . Mn3 Mn 0.12895(4) 0.02528(3) -0.00652(2) 0.0213 1.0000 Uani . . . . . . . O4 O 0.13818(18) 0.11843(13) 0.05920(11) 0.0209 1.0000 Uani . . . . . . . O5 O 0.1882(2) 0.34929(15) 0.00401(12) 0.0317 1.0000 Uani . . . . . . . C6 C 0.2327(3) 0.4219(2) 0.04450(17) 0.0245 1.0000 Uani . . . . . . . C7 C 0.2662(3) 0.4975(2) 0.00942(19) 0.0314 1.0000 Uani . . . . . . . C8 C 0.3098(3) 0.5752(2) 0.0486(2) 0.0342 1.0000 Uani . . . . . . . C9 C 0.3210(3) 0.5807(2) 0.1226(2) 0.0333 1.0000 Uani . . . . . . . C10 C 0.2876(3) 0.5067(2) 0.15729(17) 0.0236 1.0000 Uani . . . . . . . C11 C 0.2442(2) 0.42623(19) 0.11959(16) 0.0192 1.0000 Uani . . . . . . . C12 C 0.2183(3) 0.35132(19) 0.16115(16) 0.0200 1.0000 Uani . . . . . . . N13 N 0.1919(2) 0.27187(16) 0.13542(13) 0.0193 1.0000 Uani . . . . . . . O14 O 0.1757(2) 0.20924(14) 0.18505(11) 0.0243 1.0000 Uani . . . . . . . O15 O 0.1540(2) 0.06036(14) 0.25015(11) 0.0246 1.0000 Uani . . . . . . . C16 C 0.1491(3) -0.0171(2) 0.28040(16) 0.0212 1.0000 Uani . . . . . . . C17 C 0.1797(3) -0.0195(2) 0.35593(17) 0.0265 1.0000 Uani . . . . . . . C18 C 0.1755(3) -0.0980(2) 0.39043(17) 0.0273 1.0000 Uani . . . . . . . C19 C 0.1416(3) -0.1779(2) 0.35161(18) 0.0288 1.0000 Uani . . . . . . . C20 C 0.1105(3) -0.1776(2) 0.27790(17) 0.0251 1.0000 Uani . . . . . . . C21 C 0.1140(3) -0.0982(2) 0.24114(16) 0.0211 1.0000 Uani . . . . . . . C22 C 0.0805(3) -0.1027(2) 0.16385(16) 0.0215 1.0000 Uani . . . . . . . N23 N 0.0906(2) -0.03571(17) 0.12434(13) 0.0206 1.0000 Uani . . . . . . . O24 O 0.05045(19) -0.05280(14) 0.05113(11) 0.0229 1.0000 Uani . . . . . . . O25 O 0.1079(2) -0.06889(15) -0.07333(12) 0.0283 1.0000 Uani . . . . . . . C26 C 0.1410(3) -0.0724(2) -0.13450(17) 0.0245 1.0000 Uani . . . . . . . C27 C 0.1410(3) -0.1540(2) -0.16599(19) 0.0316 1.0000 Uani . . . . . . . C28 C 0.1714(3) -0.1616(3) -0.2303(2) 0.0385 1.0000 Uani . . . . . . . C29 C 0.2011(4) -0.0873(3) -0.2665(2) 0.0412 1.0000 Uani . . . . . . . C30 C 0.2018(3) -0.0062(3) -0.2366(2) 0.0336 1.0000 Uani . . . . . . . C31 C 0.1731(3) 0.0036(2) -0.17068(17) 0.0229 1.0000 Uani . . . . . . . C32 C 0.1785(3) 0.0917(2) -0.14265(17) 0.0248 1.0000 Uani . . . . . . . N33 N 0.1664(2) 0.11064(17) -0.07932(14) 0.0222 1.0000 Uani . . . . . . . O34 O 0.1680(2) 0.19818(15) -0.06526(12) 0.0293 1.0000 Uani . . . . . . . C35 C 0.4492(3) -0.0199(2) 0.13218(19) 0.0298 1.0000 Uani . . . . . . . C36 C 0.4867(3) -0.0321(3) 0.2138(2) 0.0335 1.0000 Uani . . . . . . . C37 C 0.4083(3) -0.1016(2) 0.2411(2) 0.0356 1.0000 Uani . . . . . . . C38 C 0.3879(5) -0.1885(3) 0.1987(2) 0.0503 1.0000 Uani . . . . . . . C39 C 0.3530(4) -0.1765(3) 0.1174(2) 0.0478 1.0000 Uani . . . . . . . C40 C 0.4340(4) -0.1090(3) 0.0922(2) 0.0419 1.0000 Uani . . . . . . . C41 C 0.5332(3) 0.0471(3) 0.1055(2) 0.0452 1.0000 Uani . . . . . . . C42 C 0.3412(3) 0.0166(2) 0.11302(17) 0.0237 1.0000 Uani . . . . . . . O43 O 0.31747(18) 0.06189(14) 0.16164(12) 0.0234 1.0000 Uani . . . . . . . O44 O 0.2838(2) -0.00012(15) 0.05036(12) 0.0279 1.0000 Uani . . . . . . . O45 O -0.0105(2) 0.23403(17) 0.01500(16) 0.0409 1.0000 Uani . U . . . . . C46 C -0.0731(4) 0.3017(3) 0.0077(3) 0.0676 1.0000 Uani . U . . . . . O47 O 0.3554(2) 0.2397(2) 0.06053(15) 0.0438 1.0000 Uani . U . . . . . C48 C 0.4238(4) 0.2629(4) 0.0134(3) 0.0760 1.0000 Uani . U . . . . . O49 O 0.4473(2) 0.22252(17) 0.20351(15) 0.0369 1.0000 Uani . . . . . . . C50 C 0.5592(3) 0.2302(3) 0.2430(2) 0.0421 1.0000 Uani . . . . . . . Mn101 Mn 0.21045(4) 0.47060(3) 0.37425(2) 0.0161 1.0000 Uani . . . . . . . Mn102 Mn 0.25504(4) 0.49038(3) 0.54914(2) 0.0150 1.0000 Uani . . . . . . . Mn103 Mn 0.41908(3) 0.40456(3) 0.48014(2) 0.0137 1.0000 Uani . . . . . . . O104 O 0.30100(16) 0.46663(13) 0.46679(10) 0.0158 1.0000 Uani . . . . . . . O105 O 0.13409(19) 0.49053(16) 0.28215(12) 0.0257 1.0000 Uani . . . . . . . C106 C 0.0564(2) 0.5399(2) 0.26133(16) 0.0210 1.0000 Uani . . . . . . . C107 C 0.0263(3) 0.5582(2) 0.18782(17) 0.0266 1.0000 Uani . . . . . . . C108 C -0.0565(3) 0.6069(2) 0.16235(18) 0.0289 1.0000 Uani . . . . . . . C109 C -0.1121(3) 0.6381(2) 0.20900(19) 0.0274 1.0000 Uani . . . . . . . C110 C -0.0837(3) 0.6209(2) 0.28137(18) 0.0231 1.0000 Uani . . . . . . . C111 C 0.0013(2) 0.5739(2) 0.30916(17) 0.0198 1.0000 Uani . . . . . . . C112 C 0.0274(2) 0.56204(19) 0.38628(16) 0.0190 1.0000 Uani . . . . . . . N113 N 0.1078(2) 0.52411(17) 0.41921(13) 0.0183 1.0000 Uani . . . . . . . O114 O 0.12206(17) 0.52114(15) 0.49326(11) 0.0216 1.0000 Uani . . . . . . . O115 O 0.22236(17) 0.54509(14) 0.62696(11) 0.0204 1.0000 Uani . . . . . . . C116 C 0.2733(2) 0.55216(19) 0.69604(16) 0.0192 1.0000 Uani . . . . . . . C117 C 0.2196(3) 0.5812(2) 0.74626(18) 0.0237 1.0000 Uani . . . . . . . C118 C 0.2674(3) 0.5878(2) 0.81880(19) 0.0305 1.0000 Uani . . . . . . . C119 C 0.3718(3) 0.5679(3) 0.84439(19) 0.0368 1.0000 Uani . . . . . . . C120 C 0.4276(3) 0.5423(3) 0.79632(18) 0.0317 1.0000 Uani . . . . . . . C121 C 0.3806(3) 0.5340(2) 0.72171(16) 0.0216 1.0000 Uani . . . . . . . C122 C 0.4465(2) 0.5112(2) 0.67391(15) 0.0183 1.0000 Uani . . . . . . . N123 N 0.41077(19) 0.49557(15) 0.60550(13) 0.0149 1.0000 Uani . . . . . . . O124 O 0.48717(16) 0.47756(13) 0.56871(10) 0.0152 1.0000 Uani . . . . . . . O125 O 0.53653(16) 0.34110(13) 0.48711(11) 0.0181 1.0000 Uani . . . . . . . C126 C 0.5193(2) 0.25745(19) 0.46226(16) 0.0189 1.0000 Uani . . . . . . . H181 H 0.1949 -0.0975 0.4400 0.0313 1.0000 Uiso R . . . . . . C127 C 0.5813(3) 0.1977(2) 0.50004(18) 0.0242 1.0000 Uani . . . . . . . C128 C 0.5660(3) 0.1112(2) 0.4750(2) 0.0299 1.0000 Uani . . . . . . . C129 C 0.4902(3) 0.0812(2) 0.4118(2) 0.0312 1.0000 Uani . . . . . . . C130 C 0.4289(3) 0.1392(2) 0.37306(18) 0.0266 1.0000 Uani . . . . . . . C131 C 0.4421(3) 0.22740(19) 0.39751(16) 0.0194 1.0000 Uani . . . . . . . C132 C 0.3753(2) 0.2842(2) 0.35379(16) 0.0202 1.0000 Uani . . . . . . . N133 N 0.36018(19) 0.35748(16) 0.37867(13) 0.0163 1.0000 Uani . . . . . . . O134 O 0.30085(17) 0.40887(14) 0.33110(11) 0.0183 1.0000 Uani . . . . . . . C135 C 0.2615(3) 0.2211(2) 0.62220(18) 0.0251 1.0000 Uani . . . . . . . C136 C 0.1396(3) 0.1869(2) 0.61548(19) 0.0282 1.0000 Uani . . . . . . . C137 C 0.0844(3) 0.1448(3) 0.5419(2) 0.0372 1.0000 Uani . . . . . . . C138 C 0.1401(3) 0.0695(3) 0.5241(3) 0.0444 1.0000 Uani . . . . . . . C139 C 0.2611(3) 0.1028(2) 0.5279(2) 0.0373 1.0000 Uani . . . . . . . C140 C 0.3180(3) 0.1475(2) 0.6010(2) 0.0327 1.0000 Uani . . . . . . . C141 C 0.3181(3) 0.2553(3) 0.69994(19) 0.0331 1.0000 Uani . . . . . . . C142 C 0.2753(3) 0.3016(2) 0.57495(17) 0.0208 1.0000 Uani . . . . . . . O143 O 0.21596(18) 0.36033(14) 0.57834(12) 0.0220 1.0000 Uani . . . . . . . O144 O 0.34693(19) 0.30663(14) 0.53900(12) 0.0232 1.0000 Uani . . . . . . . O145 O 0.1105(2) 0.34027(16) 0.38571(14) 0.0355 1.0000 Uani . U . . . . . C146 C 0.0916(4) 0.2648(3) 0.3411(3) 0.0674 1.0000 Uani . U . . . . . O147 O 0.30468(18) 0.61269(14) 0.38225(12) 0.0240 1.0000 Uani . U . . . . . C148 C 0.3420(3) 0.6591(2) 0.32653(19) 0.0322 1.0000 Uani . U . . . . . O149 O 0.9072(14) 0.3269(11) 0.4062(10) 0.0332 0.1642 Uani . . . 1 1 . . C150 C 0.8478(4) 0.2670(3) 0.4366(3) 0.0477 1.0000 Uani . . . . . . . O151 O 0.9429(3) 0.3311(2) 0.4509(2) 0.0359 0.8358 Uani . . . 1 2 . . H1221 H 0.5191 0.5085 0.6932 0.0219 1.0000 Uiso R . . . . . . H1171 H 0.1504 0.5941 0.7301 0.0278 1.0000 Uiso R . . . . . . H1181 H 0.2298 0.6049 0.8510 0.0377 1.0000 Uiso R . . . . . . H1191 H 0.4039 0.5726 0.8933 0.0449 1.0000 Uiso R . . . . . . H1201 H 0.4989 0.5311 0.8134 0.0383 1.0000 Uiso R . . . . . . H1362 H 0.1337 0.1418 0.6513 0.0350 1.0000 Uiso R . . . . . . H1361 H 0.1036 0.2356 0.6255 0.0351 1.0000 Uiso R . . . . . . H1371 H 0.0071 0.1216 0.5418 0.0450 1.0000 Uiso R . . . . . . H1372 H 0.0885 0.1905 0.5065 0.0448 1.0000 Uiso R . . . . . . H1382 H 0.1345 0.0252 0.5606 0.0538 1.0000 Uiso R . . . . . . H1381 H 0.1037 0.0435 0.4756 0.0540 1.0000 Uiso R . . . . . . H1391 H 0.2981 0.0538 0.5202 0.0483 1.0000 Uiso R . . . . . . H1392 H 0.2672 0.1446 0.4897 0.0477 1.0000 Uiso R . . . . . . H1401 H 0.3172 0.1030 0.6374 0.0423 1.0000 Uiso R . . . . . . H1402 H 0.3943 0.1717 0.6023 0.0410 1.0000 Uiso R . . . . . . H1413 H 0.3119 0.2085 0.7342 0.0488 1.0000 Uiso R . . . . . . H1411 H 0.2849 0.3031 0.7135 0.0499 1.0000 Uiso R . . . . . . H1412 H 0.3956 0.2765 0.7035 0.0500 1.0000 Uiso R . . . . . . H1321 H 0.3423 0.2675 0.3071 0.0233 1.0000 Uiso R . . . . . . H1071 H 0.0631 0.5374 0.1562 0.0322 1.0000 Uiso R . . . . . . H1081 H -0.0754 0.6177 0.1136 0.0329 1.0000 Uiso R . . . . . . H1091 H -0.1681 0.6694 0.1923 0.0319 1.0000 Uiso R . . . . . . H1101 H -0.1218 0.6407 0.3123 0.0274 1.0000 Uiso R . . . . . . H1121 H -0.0154 0.5835 0.4142 0.0224 1.0000 Uiso R . . . . . . H1301 H 0.3782 0.1201 0.3310 0.0312 1.0000 Uiso R . . . . . . H1291 H 0.4808 0.0236 0.3960 0.0371 1.0000 Uiso R . . . . . . H1281 H 0.6078 0.0733 0.5019 0.0362 1.0000 Uiso R . . . . . . H1271 H 0.6311 0.2160 0.5427 0.0287 1.0000 Uiso R . . . . . . H171 H 0.2029 0.0325 0.3824 0.0303 1.0000 Uiso R . . . . . . H191 H 0.1408 -0.2303 0.3752 0.0330 1.0000 Uiso R . . . . . . H201 H 0.0872 -0.2301 0.2515 0.0279 1.0000 Uiso R . . . . . . H221 H 0.0512 -0.1573 0.1405 0.0250 1.0000 Uiso R . . . . . . H361 H 0.5581 -0.0506 0.2222 0.0400 1.0000 Uiso R . . . . . . H362 H 0.4928 0.0233 0.2406 0.0396 1.0000 Uiso R . . . . . . H371 H 0.4382 -0.1099 0.2916 0.0420 1.0000 Uiso R . . . . . . H372 H 0.3390 -0.0806 0.2365 0.0421 1.0000 Uiso R . . . . . . H381 H 0.4543 -0.2133 0.2092 0.0580 1.0000 Uiso R . . . . . . H382 H 0.3312 -0.2276 0.2138 0.0580 1.0000 Uiso R . . . . . . H391 H 0.3475 -0.2319 0.0913 0.0561 1.0000 Uiso R . . . . . . H392 H 0.2817 -0.1579 0.1072 0.0562 1.0000 Uiso R . . . . . . H402 H 0.5033 -0.1294 0.1011 0.0518 1.0000 Uiso R . . . . . . H401 H 0.4080 -0.1025 0.0405 0.0519 1.0000 Uiso R . . . . . . H412 H 0.6011 0.0242 0.1120 0.0690 1.0000 Uiso R . . . . . . H413 H 0.5467 0.1024 0.1323 0.0688 1.0000 Uiso R . . . . . . H411 H 0.5066 0.0559 0.0545 0.0689 1.0000 Uiso R . . . . . . H301 H 0.2227 0.0438 -0.2605 0.0409 1.0000 Uiso R . . . . . . H291 H 0.2208 -0.0919 -0.3107 0.0518 1.0000 Uiso R . . . . . . H281 H 0.1721 -0.2173 -0.2491 0.0476 1.0000 Uiso R . . . . . . H271 H 0.1200 -0.2040 -0.1430 0.0379 1.0000 Uiso R . . . . . . H321 H 0.1911 0.1387 -0.1718 0.0281 1.0000 Uiso R . . . . . . H121 H 0.2203 0.3613 0.2088 0.0228 1.0000 Uiso R . . . . . . H71 H 0.2593 0.4951 -0.0402 0.0371 1.0000 Uiso R . . . . . . H81 H 0.3326 0.6251 0.0251 0.0399 1.0000 Uiso R . . . . . . H91 H 0.3490 0.6330 0.1485 0.0389 1.0000 Uiso R . . . . . . H101 H 0.2942 0.5091 0.2066 0.0277 1.0000 Uiso R . . . . . . H1471 H 0.3510 0.6230 0.4184 0.0344 1.0000 Uiso R . . . . . . H491 H 0.4206 0.1707 0.2034 0.0532 1.0000 Uiso R . . . . . . H471 H 0.3885 0.2410 0.1026 0.0648 1.0000 Uiso R . . . . . . H1451 H 0.0561 0.3392 0.4015 0.0539 1.0000 Uiso R . . . . . . H1483 H 0.2877 0.6480 0.2824 0.0494 1.0000 Uiso R . . . . . . H1481 H 0.3574 0.7209 0.3375 0.0490 1.0000 Uiso R . . . . . . H1482 H 0.4067 0.6409 0.3194 0.0489 1.0000 Uiso R . . . . . . H502 H 0.5790 0.2813 0.2749 0.0606 1.0000 Uiso R . . . . . . H503 H 0.5688 0.1792 0.2717 0.0605 1.0000 Uiso R . . . . . . H501 H 0.6067 0.2330 0.2099 0.0606 1.0000 Uiso R . . . . . . H451 H -0.0420 0.1878 0.0237 0.0589 1.0000 Uiso R . . . . . . H1491 H 0.8540 0.3197 0.3721 0.0540 0.1642 Uiso R . . 1 1 . . H1511 H 0.9139 0.3730 0.4539 0.0562 0.8358 Uiso R . . 1 2 . . H1501 H 0.8678 0.2097 0.4388 0.0710 0.8358 Uiso R . . 1 2 . . H1505 H 0.8065 0.2734 0.4722 0.0712 0.8358 Uiso R . . 1 2 . . H1504 H 0.8034 0.2742 0.3898 0.0709 0.8358 Uiso R . . 1 2 . . H1503 H 0.8748 0.2717 0.4881 0.0710 0.1642 Uiso R . . 1 1 . . H1502 H 0.7729 0.2759 0.4246 0.0710 0.1642 Uiso R . . 1 1 . . H1506 H 0.8525 0.2097 0.4193 0.0710 0.1642 Uiso R . . 1 1 . . H1463 H 0.0785 0.2809 0.2916 0.1016 1.0000 Uiso R . . . . . . H463 H -0.0672 0.3294 0.0548 0.1051 1.0000 Uiso R . . . . . . H461 H -0.0460 0.3467 -0.0214 0.1052 1.0000 Uiso R . . . . . . H481 H 0.4394 0.3272 0.0133 0.1116 1.0000 Uiso R . . . . . . H482 H 0.3896 0.2416 -0.0360 0.1113 1.0000 Uiso R . . . . . . H1462 H 0.0303 0.2232 0.3478 0.1009 1.0000 Uiso R . . . . . . H1461 H 0.1549 0.2368 0.3500 0.1018 1.0000 Uiso R . . . . . . H462 H -0.1488 0.2795 -0.0129 0.1054 1.0000 Uiso R . . . . . . H483 H 0.4919 0.2400 0.0307 0.1111 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 0.0316(3) 0.0156(2) 0.0133(2) 0.00047(16) 0.00169(18) -0.00415(18) Mn2 0.0232(2) 0.0154(2) 0.0132(2) 0.00099(16) 0.00257(17) -0.00163(16) Mn3 0.0299(3) 0.0166(2) 0.0138(2) -0.00083(16) 0.00315(18) -0.00419(18) O4 0.0296(12) 0.0161(10) 0.0135(10) 0.0016(8) 0.0019(8) -0.0027(8) O5 0.0558(17) 0.0182(11) 0.0128(10) -0.0001(8) -0.0010(10) -0.0056(11) C6 0.0313(17) 0.0171(14) 0.0219(15) 0.0019(12) 0.0033(13) -0.0017(12) C7 0.049(2) 0.0217(16) 0.0214(16) 0.0014(13) 0.0088(15) -0.0019(15) C8 0.051(2) 0.0197(16) 0.0302(19) 0.0033(13) 0.0106(17) -0.0021(15) C9 0.050(2) 0.0169(15) 0.0297(18) -0.0047(13) 0.0098(16) -0.0039(14) C10 0.0309(17) 0.0200(14) 0.0187(14) -0.0014(11) 0.0041(12) 0.0029(12) C11 0.0204(14) 0.0156(13) 0.0201(14) 0.0015(11) 0.0024(11) 0.0015(10) C12 0.0243(15) 0.0175(13) 0.0165(14) -0.0008(11) 0.0022(11) 0.0020(11) N13 0.0246(13) 0.0179(12) 0.0142(11) 0.0020(9) 0.0036(10) 0.0012(10) O14 0.0373(13) 0.0179(10) 0.0156(10) 0.0021(8) 0.0053(9) -0.0006(9) O15 0.0370(13) 0.0203(11) 0.0144(10) 0.0021(8) 0.0043(9) 0.0003(9) C16 0.0226(15) 0.0223(15) 0.0179(14) 0.0039(11) 0.0058(11) -0.0011(11) C17 0.0303(17) 0.0275(16) 0.0183(15) 0.0016(12) 0.0050(13) -0.0046(13) C18 0.0291(17) 0.0333(18) 0.0156(14) 0.0047(13) 0.0017(12) -0.0016(14) C19 0.0303(18) 0.0267(17) 0.0255(17) 0.0096(13) 0.0022(13) -0.0011(13) C20 0.0282(17) 0.0220(15) 0.0199(15) 0.0022(12) 0.0004(12) -0.0041(12) C21 0.0209(14) 0.0230(15) 0.0165(14) 0.0032(11) 0.0019(11) -0.0022(11) C22 0.0234(15) 0.0205(14) 0.0187(14) 0.0008(11) 0.0055(12) -0.0030(11) N23 0.0237(13) 0.0211(12) 0.0139(12) 0.0006(9) 0.0021(10) -0.0028(10) O24 0.0310(12) 0.0191(10) 0.0130(10) -0.0005(8) -0.0002(9) -0.0051(9) O25 0.0421(15) 0.0208(11) 0.0207(11) -0.0039(9) 0.0117(10) -0.0059(10) C26 0.0235(15) 0.0258(16) 0.0215(15) -0.0032(12) 0.0016(12) 0.0013(12) C27 0.044(2) 0.0234(16) 0.0270(18) 0.0010(13) 0.0096(15) 0.0013(15) C28 0.051(2) 0.0303(19) 0.038(2) -0.0086(16) 0.0188(18) 0.0057(17) C29 0.056(3) 0.042(2) 0.031(2) -0.0054(17) 0.0205(19) 0.0095(19) C30 0.042(2) 0.0336(19) 0.0278(18) 0.0038(15) 0.0152(16) 0.0031(16) C31 0.0253(16) 0.0250(15) 0.0179(14) 0.0019(12) 0.0057(12) 0.0010(12) C32 0.0296(17) 0.0217(15) 0.0196(15) 0.0016(12) 0.0037(12) -0.0037(12) N33 0.0279(14) 0.0184(12) 0.0161(12) 0.0008(9) 0.0012(10) -0.0034(10) O34 0.0521(16) 0.0176(11) 0.0149(10) -0.0004(8) 0.0069(10) -0.0033(10) C35 0.0330(19) 0.0309(18) 0.0284(18) 0.0018(14) 0.0108(14) 0.0085(14) C36 0.0298(19) 0.039(2) 0.0311(19) -0.0002(15) 0.0020(15) 0.0100(15) C37 0.046(2) 0.0312(19) 0.0276(18) 0.0067(15) 0.0052(16) 0.0068(16) C38 0.087(4) 0.0260(19) 0.033(2) 0.0086(16) 0.004(2) 0.008(2) C39 0.086(4) 0.0215(18) 0.034(2) 0.0019(15) 0.008(2) 0.011(2) C40 0.056(3) 0.042(2) 0.033(2) -0.0001(17) 0.0073(18) 0.028(2) C41 0.035(2) 0.053(3) 0.049(3) 0.003(2) 0.0192(19) -0.0013(19) C42 0.0286(17) 0.0196(14) 0.0224(15) 0.0015(12) 0.0073(13) 0.0004(12) O43 0.0250(12) 0.0227(11) 0.0204(11) -0.0023(9) 0.0036(9) -0.0003(9) O44 0.0344(13) 0.0273(12) 0.0201(11) -0.0027(9) 0.0020(10) 0.0060(10) O45 0.0319(14) 0.0240(13) 0.0613(19) 0.0057(12) 0.0012(13) 0.0027(11) C46 0.059(3) 0.045(3) 0.109(4) 0.024(3) 0.033(3) 0.020(2) O47 0.0327(15) 0.064(2) 0.0331(15) 0.0069(13) 0.0103(12) -0.0012(13) C48 0.051(3) 0.118(5) 0.056(3) -0.016(3) 0.024(3) -0.013(3) O49 0.0332(14) 0.0312(14) 0.0408(16) -0.0050(11) 0.0032(12) -0.0038(11) C50 0.029(2) 0.041(2) 0.051(3) -0.0035(19) 0.0071(18) -0.0081(16) Mn101 0.0147(2) 0.0208(2) 0.0127(2) -0.00080(16) 0.00188(15) 0.00456(16) Mn102 0.0142(2) 0.0182(2) 0.0129(2) -0.00108(15) 0.00354(15) 0.00309(15) Mn103 0.01303(19) 0.01479(19) 0.01283(19) -0.00147(15) 0.00232(15) 0.00225(15) O104 0.0170(10) 0.0190(10) 0.0115(9) 0.0016(7) 0.0023(7) 0.0049(8) O105 0.0236(12) 0.0381(13) 0.0157(10) -0.0002(9) -0.0013(9) 0.0145(10) C106 0.0155(13) 0.0276(15) 0.0179(14) 0.0037(12) 0.0005(11) 0.0029(11) C107 0.0248(16) 0.0372(18) 0.0175(15) 0.0033(13) 0.0011(12) 0.0098(14) C108 0.0268(17) 0.0363(19) 0.0194(15) 0.0088(13) -0.0034(13) 0.0057(14) C109 0.0239(16) 0.0273(16) 0.0282(17) 0.0049(13) -0.0014(13) 0.0065(13) C110 0.0208(15) 0.0212(14) 0.0265(16) 0.0030(12) 0.0031(12) 0.0040(11) C111 0.0164(13) 0.0198(14) 0.0220(15) 0.0011(11) 0.0032(11) 0.0014(11) C112 0.0134(13) 0.0216(14) 0.0211(14) -0.0032(11) 0.0032(11) 0.0015(10) N113 0.0160(12) 0.0217(12) 0.0163(12) -0.0017(9) 0.0036(9) 0.0007(9) O114 0.0192(10) 0.0330(12) 0.0143(10) 0.0006(9) 0.0038(8) 0.0099(9) O115 0.0209(11) 0.0268(11) 0.0143(10) -0.0046(8) 0.0043(8) 0.0058(8) C116 0.0201(14) 0.0184(13) 0.0184(14) -0.0005(11) 0.0053(11) -0.0001(11) C117 0.0206(15) 0.0237(15) 0.0264(16) -0.0061(12) 0.0097(12) -0.0037(11) C118 0.0363(19) 0.0352(19) 0.0248(17) -0.0061(14) 0.0179(15) 0.0037(15) C119 0.041(2) 0.056(2) 0.0151(16) -0.0054(15) 0.0085(15) 0.0090(18) C120 0.0282(18) 0.049(2) 0.0173(15) -0.0022(14) 0.0034(13) 0.0071(15) C121 0.0257(16) 0.0234(15) 0.0159(14) -0.0028(11) 0.0075(12) 0.0013(12) C122 0.0147(13) 0.0244(14) 0.0147(13) -0.0022(11) 0.0014(10) 0.0024(10) N123 0.0171(11) 0.0146(11) 0.0141(11) -0.0009(8) 0.0066(9) 0.0010(9) O124 0.0127(9) 0.0201(10) 0.0133(9) -0.0028(7) 0.0040(7) 0.0023(7) O125 0.0169(10) 0.0184(10) 0.0179(10) -0.0033(8) 0.0012(8) 0.0034(8) C126 0.0205(14) 0.0164(13) 0.0210(14) 0.0003(11) 0.0078(11) 0.0023(11) C127 0.0246(16) 0.0224(15) 0.0244(16) -0.0009(12) 0.0003(12) 0.0079(12) C128 0.0329(18) 0.0223(16) 0.0339(19) 0.0017(14) 0.0026(15) 0.0106(13) C129 0.039(2) 0.0167(15) 0.037(2) -0.0015(13) 0.0051(16) 0.0058(13) C130 0.0307(17) 0.0215(15) 0.0265(17) -0.0068(12) 0.0055(13) 0.0027(13) C131 0.0237(15) 0.0156(13) 0.0186(14) -0.0055(11) 0.0054(11) 0.0014(11) C132 0.0202(14) 0.0225(14) 0.0159(13) -0.0028(11) 0.0017(11) 0.0013(11) N133 0.0149(11) 0.0181(11) 0.0153(11) -0.0018(9) 0.0034(9) 0.0004(9) O134 0.0206(10) 0.0217(10) 0.0133(9) -0.0007(8) 0.0034(8) 0.0061(8) C135 0.0272(16) 0.0217(15) 0.0283(17) 0.0043(12) 0.0105(13) 0.0038(12) C136 0.0317(18) 0.0219(15) 0.0344(19) -0.0006(13) 0.0168(15) 0.0012(13) C137 0.034(2) 0.035(2) 0.043(2) -0.0072(17) 0.0150(17) -0.0035(16) C138 0.046(2) 0.0281(19) 0.061(3) -0.0153(18) 0.024(2) -0.0068(17) C139 0.041(2) 0.0252(17) 0.053(2) -0.0041(16) 0.0273(19) 0.0029(15) C140 0.037(2) 0.0238(16) 0.044(2) 0.0087(15) 0.0183(17) 0.0110(14) C141 0.0320(19) 0.039(2) 0.0289(18) 0.0067(15) 0.0071(15) 0.0066(15) C142 0.0207(14) 0.0190(14) 0.0210(14) -0.0011(11) 0.0035(11) 0.0002(11) O143 0.0222(11) 0.0200(10) 0.0254(11) 0.0019(9) 0.0106(9) 0.0011(8) O144 0.0267(12) 0.0196(10) 0.0269(12) 0.0045(9) 0.0128(9) 0.0048(9) O145 0.0350(14) 0.0286(13) 0.0436(15) -0.0139(11) 0.0206(12) -0.0097(10) C146 0.062(3) 0.054(3) 0.089(4) -0.040(3) 0.046(3) -0.027(2) O147 0.0237(11) 0.0242(11) 0.0212(11) 0.0039(9) 0.0009(9) 0.0012(9) C148 0.042(2) 0.0274(17) 0.0276(17) 0.0044(14) 0.0130(15) -0.0001(15) O149 0.032(9) 0.036(9) 0.040(10) 0.026(8) 0.017(8) 0.019(7) C150 0.041(2) 0.036(2) 0.064(3) 0.008(2) 0.011(2) 0.0020(18) O151 0.0289(18) 0.0312(17) 0.051(2) -0.0002(17) 0.0150(16) 0.0076(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.32023(17) 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 . 3.2684(7) yes Mn1 . O4 . 1.869(2) yes Mn1 . O5 . 1.853(2) yes Mn1 . N13 . 2.004(2) yes Mn1 . O34 . 1.918(2) yes Mn1 . O45 . 2.266(3) yes Mn1 . O47 . 2.269(3) yes Mn2 . O4 . 1.867(2) yes Mn2 . O14 . 1.895(2) yes Mn2 . O15 . 1.858(2) yes Mn2 . N23 . 2.014(3) yes Mn2 . O43 . 2.127(2) yes Mn3 . O24 2_555 2.352(2) yes Mn3 . O4 . 1.877(2) yes Mn3 . O24 . 1.948(2) yes Mn3 . O25 . 1.876(2) yes Mn3 . N33 . 2.000(3) yes Mn3 . O44 . 2.116(2) yes O5 . C6 . 1.331(4) yes C6 . C7 . 1.404(4) yes C6 . C11 . 1.404(4) yes C7 . C8 . 1.380(5) yes C7 . H71 . 0.928 no C8 . C9 . 1.385(5) yes C8 . H81 . 0.932 no C9 . C10 . 1.379(5) yes C9 . H91 . 0.922 no C10 . C11 . 1.402(4) yes C10 . H101 . 0.923 no C11 . C12 . 1.441(4) yes C12 . N13 . 1.285(4) yes C12 . H121 . 0.914 no N13 . O14 . 1.378(3) yes O15 . C16 . 1.327(4) yes C16 . C17 . 1.403(4) yes C16 . C21 . 1.412(4) yes C17 . C18 . 1.378(5) yes C17 . H171 . 0.919 no C18 . C19 . 1.393(5) yes C18 . H181 . 0.919 no C19 . C20 . 1.368(4) yes C19 . H191 . 0.925 no C20 . C21 . 1.412(4) yes C20 . H201 . 0.923 no C21 . C22 . 1.434(4) yes C22 . N23 . 1.288(4) yes C22 . H221 . 0.933 no N23 . O24 . 1.380(3) yes O25 . C26 . 1.331(4) yes C26 . C27 . 1.394(4) yes C26 . C31 . 1.414(4) yes C27 . C28 . 1.377(5) yes C27 . H271 . 0.921 no C28 . C29 . 1.387(6) yes C28 . H281 . 0.932 no C29 . C30 . 1.372(5) yes C29 . H291 . 0.938 no C30 . C31 . 1.400(4) yes C30 . H301 . 0.931 no C31 . C32 . 1.445(4) yes C32 . N33 . 1.289(4) yes C32 . H321 . 0.931 no N33 . O34 . 1.373(3) yes C35 . C36 . 1.538(5) yes C35 . C40 . 1.534(5) yes C35 . C41 . 1.544(5) yes C35 . C42 . 1.534(5) yes C36 . C37 . 1.527(5) yes C36 . H361 . 0.973 no C36 . H362 . 0.979 no C37 . C38 . 1.520(5) yes C37 . H371 . 0.965 no C37 . H372 . 0.972 no C38 . C39 . 1.528(5) yes C38 . H381 . 0.962 no C38 . H382 . 0.966 no C39 . C40 . 1.509(6) yes C39 . H391 . 0.973 no C39 . H392 . 0.971 no C40 . H402 . 0.962 no C40 . H401 . 0.975 no C41 . H412 . 0.966 no C41 . H413 . 0.965 no C41 . H411 . 0.969 no C42 . O43 . 1.276(4) yes C42 . O44 . 1.251(4) yes O45 . C46 . 1.396(5) yes O45 . H451 . 0.799 no C46 . H463 . 0.975 no C46 . H461 . 0.962 no C46 . H462 . 0.962 no O47 . C48 . 1.399(5) yes O47 . H471 . 0.814 no C48 . H481 . 0.980 no C48 . H482 . 0.975 no C48 . H483 . 0.975 no O49 . C50 . 1.438(4) yes O49 . H491 . 0.819 no C50 . H502 . 0.958 no C50 . H503 . 0.966 no C50 . H501 . 0.967 no Mn101 . Mn103 . 3.2475(6) yes Mn101 . O104 . 1.878(2) yes Mn101 . O105 . 1.851(2) yes Mn101 . N113 . 1.993(3) yes Mn101 . O134 . 1.918(2) yes Mn101 . O145 . 2.248(2) yes Mn101 . O147 . 2.318(2) yes Mn102 . Mn103 . 3.1560(6) yes Mn102 . O104 . 1.850(2) yes Mn102 . O114 . 1.910(2) yes Mn102 . O115 . 1.863(2) yes Mn102 . N123 . 2.017(2) yes Mn102 . O143 . 2.099(2) yes Mn103 . O124 2_666 2.333(2) yes Mn103 . Mn103 2_666 3.3014(8) yes Mn103 . O104 . 1.875(2) yes Mn103 . O124 . 1.9717(19) yes Mn103 . O125 . 1.891(2) yes Mn103 . N133 . 1.997(2) yes Mn103 . O144 . 2.106(2) yes O105 . C106 . 1.330(4) yes C106 . C107 . 1.405(4) yes C106 . C111 . 1.416(4) yes C107 . C108 . 1.387(4) yes C107 . H1071 . 0.928 no C108 . C109 . 1.384(5) yes C108 . H1081 . 0.926 no C109 . C110 . 1.379(4) yes C109 . H1091 . 0.920 no C110 . C111 . 1.400(4) yes C110 . H1101 . 0.923 no C111 . C112 . 1.448(4) yes C112 . N113 . 1.295(4) yes C112 . H1121 . 0.936 no N113 . O114 . 1.382(3) yes O115 . C116 . 1.323(3) yes C116 . C117 . 1.407(4) yes C116 . C121 . 1.414(4) yes C117 . C118 . 1.372(5) yes C117 . H1171 . 0.917 no C118 . C119 . 1.389(5) yes C118 . H1181 . 0.922 no C119 . C120 . 1.373(5) yes C119 . H1191 . 0.925 no C120 . C121 . 1.407(4) yes C120 . H1201 . 0.934 no C121 . C122 . 1.448(4) yes C122 . N123 . 1.287(3) yes C122 . H1221 . 0.920 no N123 . O124 . 1.383(3) yes O125 . C126 . 1.342(3) yes C126 . C127 . 1.398(4) yes C126 . C131 . 1.416(4) yes C127 . C128 . 1.387(4) yes C127 . H1271 . 0.921 no C128 . C129 . 1.387(5) yes C128 . H1281 . 0.927 no C129 . C130 . 1.381(5) yes C129 . H1291 . 0.918 no C130 . C131 . 1.410(4) yes C130 . H1301 . 0.922 no C131 . C132 . 1.446(4) yes C132 . N133 . 1.283(4) yes C132 . H1321 . 0.910 no N133 . O134 . 1.376(3) yes C135 . C136 . 1.537(5) yes C135 . C140 . 1.535(5) yes C135 . C141 . 1.543(5) yes C135 . C142 . 1.546(4) yes C136 . C137 . 1.511(5) yes C136 . H1362 . 0.981 no C136 . H1361 . 0.980 no C137 . C138 . 1.527(5) yes C137 . H1371 . 0.993 no C137 . H1372 . 0.981 no C138 . C139 . 1.533(5) yes C138 . H1382 . 0.983 no C138 . H1381 . 0.986 no C139 . C140 . 1.523(5) yes C139 . H1391 . 0.979 no C139 . H1392 . 0.981 no C140 . H1401 . 0.977 no C140 . H1402 . 0.980 no C141 . H1413 . 0.980 no C141 . H1411 . 0.968 no C141 . H1412 . 0.978 no C142 . O143 . 1.277(4) yes C142 . O144 . 1.254(4) yes O145 . C146 . 1.398(4) yes O145 . H1451 . 0.813 no C146 . H1463 . 0.958 no C146 . H1462 . 0.965 no C146 . H1461 . 0.954 no O147 . C148 . 1.412(4) yes O147 . H1471 . 0.795 no C148 . H1483 . 0.953 no C148 . H1481 . 0.957 no C148 . H1482 . 0.948 no O149 . C150 . 1.322(16) yes O149 . H1491 . 0.817 no C150 . H1503 . 0.960 no C150 . H1502 . 0.961 no C150 . H1506 . 0.959 no C150 . O151 . 1.412(5) yes C150 . H1501 . 0.956 no C150 . H1505 . 0.962 no C150 . H1504 . 0.956 no O151 . H1511 . 0.801 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 . O4 . 28.96(6) yes Mn2 . Mn1 . O5 . 150.77(7) yes O4 . Mn1 . O5 . 173.63(12) yes Mn2 . Mn1 . N13 . 59.16(7) yes O4 . Mn1 . N13 . 87.72(10) yes O5 . Mn1 . N13 . 91.64(10) yes Mn2 . Mn1 . O34 . 120.93(7) yes O4 . Mn1 . O34 . 93.07(9) yes O5 . Mn1 . O34 . 88.23(10) yes N13 . Mn1 . O34 . 174.04(11) yes Mn2 . Mn1 . O45 . 89.19(7) yes O4 . Mn1 . O45 . 84.32(10) yes O5 . Mn1 . O45 . 89.34(11) yes N13 . Mn1 . O45 . 89.44(11) yes O34 . Mn1 . O45 . 96.52(11) yes Mn2 . Mn1 . O47 . 88.25(8) yes O4 . Mn1 . O47 . 96.00(11) yes O5 . Mn1 . O47 . 90.24(12) yes N13 . Mn1 . O47 . 84.58(11) yes O34 . Mn1 . O47 . 89.47(11) yes O45 . Mn1 . O47 . 173.98(11) yes Mn1 . Mn2 . O4 . 29.00(6) yes Mn1 . Mn2 . O14 . 62.73(7) yes O4 . Mn2 . O14 . 90.94(9) yes Mn1 . Mn2 . O15 . 151.20(7) yes O4 . Mn2 . O15 . 171.49(11) yes O14 . Mn2 . O15 . 88.50(10) yes Mn1 . Mn2 . N23 . 118.37(7) yes O4 . Mn2 . N23 . 89.46(10) yes O14 . Mn2 . N23 . 162.82(11) yes O15 . Mn2 . N23 . 88.58(10) yes Mn1 . Mn2 . O43 . 93.43(6) yes O4 . Mn2 . O43 . 92.50(10) yes O14 . Mn2 . O43 . 105.43(10) yes O15 . Mn2 . O43 . 95.84(10) yes N23 . Mn2 . O43 . 91.71(10) yes O24 2_555 Mn3 . O4 . 84.04(9) yes O24 2_555 Mn3 . O24 . 79.15(9) yes O4 . Mn3 . O24 . 89.57(9) yes O24 2_555 Mn3 . O25 . 91.81(10) yes O4 . Mn3 . O25 . 175.55(11) yes O24 . Mn3 . O25 . 88.08(10) yes O24 2_555 Mn3 . N33 . 84.56(10) yes O4 . Mn3 . N33 . 90.24(10) yes O24 . Mn3 . N33 . 163.65(11) yes O25 . Mn3 . N33 . 90.95(10) yes O24 2_555 Mn3 . O44 . 170.58(9) yes O4 . Mn3 . O44 . 90.06(9) yes O24 . Mn3 . O44 . 93.51(10) yes O25 . Mn3 . O44 . 93.85(10) yes N33 . Mn3 . O44 . 102.84(11) yes Mn3 . O4 . Mn1 . 119.37(11) yes Mn3 . O4 . Mn2 . 115.71(11) yes Mn1 . O4 . Mn2 . 122.04(11) yes Mn1 . O5 . C6 . 128.8(2) yes O5 . C6 . C7 . 117.7(3) yes O5 . C6 . C11 . 122.9(3) yes C7 . C6 . C11 . 119.3(3) yes C6 . C7 . C8 . 120.1(3) yes C6 . C7 . H71 . 119.8 no C8 . C7 . H71 . 120.1 no C7 . C8 . C9 . 121.3(3) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 119.0 no C8 . C9 . C10 . 118.9(3) yes C8 . C9 . H91 . 121.1 no C10 . C9 . H91 . 120.0 no C9 . C10 . C11 . 121.6(3) yes C9 . C10 . H101 . 120.1 no C11 . C10 . H101 . 118.3 no C6 . C11 . C10 . 118.8(3) yes C6 . C11 . C12 . 123.6(3) yes C10 . C11 . C12 . 117.5(3) yes C11 . C12 . N13 . 124.2(3) yes C11 . C12 . H121 . 117.6 no N13 . C12 . H121 . 118.1 no Mn1 . N13 . C12 . 125.8(2) yes Mn1 . N13 . O14 . 119.04(17) yes C12 . N13 . O14 . 115.1(2) yes N13 . O14 . Mn2 . 118.47(17) yes Mn2 . O15 . C16 . 130.2(2) yes O15 . C16 . C17 . 118.6(3) yes O15 . C16 . C21 . 123.9(3) yes C17 . C16 . C21 . 117.5(3) yes C16 . C17 . C18 . 121.2(3) yes C16 . C17 . H171 . 118.8 no C18 . C17 . H171 . 120.0 no C17 . C18 . C19 . 121.2(3) yes C17 . C18 . H181 . 119.3 no C19 . C18 . H181 . 119.5 no C18 . C19 . C20 . 118.9(3) yes C18 . C19 . H191 . 120.6 no C20 . C19 . H191 . 120.6 no C19 . C20 . C21 . 121.1(3) yes C19 . C20 . H201 . 119.7 no C21 . C20 . H201 . 119.1 no C16 . C21 . C20 . 120.1(3) yes C16 . C21 . C22 . 121.8(3) yes C20 . C21 . C22 . 118.1(3) yes C21 . C22 . N23 . 123.6(3) yes C21 . C22 . H221 . 118.6 no N23 . C22 . H221 . 117.8 no Mn2 . N23 . C22 . 128.3(2) yes Mn2 . N23 . O24 . 116.67(18) yes C22 . N23 . O24 . 115.0(2) yes Mn3 2_555 O24 . N23 . 114.59(18) yes Mn3 2_555 O24 . Mn3 . 100.85(9) yes N23 . O24 . Mn3 . 112.54(16) yes Mn3 . O25 . C26 . 129.6(2) yes O25 . C26 . C27 . 119.2(3) yes O25 . C26 . C31 . 122.7(3) yes C27 . C26 . C31 . 118.1(3) yes C26 . C27 . C28 . 121.7(3) yes C26 . C27 . H271 . 118.8 no C28 . C27 . H271 . 119.5 no C27 . C28 . C29 . 120.3(3) yes C27 . C28 . H281 . 119.3 no C29 . C28 . H281 . 120.4 no C28 . C29 . C30 . 119.0(4) yes C28 . C29 . H291 . 120.9 no C30 . C29 . H291 . 120.1 no C29 . C30 . C31 . 121.9(4) yes C29 . C30 . H301 . 119.1 no C31 . C30 . H301 . 119.0 no C26 . C31 . C30 . 119.0(3) yes C26 . C31 . C32 . 123.1(3) yes C30 . C31 . C32 . 117.9(3) yes C31 . C32 . N33 . 124.6(3) yes C31 . C32 . H321 . 118.9 no N33 . C32 . H321 . 116.5 no Mn3 . N33 . C32 . 126.5(2) yes Mn3 . N33 . O34 . 118.08(19) yes C32 . N33 . O34 . 115.0(3) yes N33 . O34 . Mn1 . 117.47(18) yes C36 . C35 . C40 . 108.9(3) yes C36 . C35 . C41 . 110.9(3) yes C40 . C35 . C41 . 110.2(3) yes C36 . C35 . C42 . 111.9(3) yes C40 . C35 . C42 . 108.9(3) yes C41 . C35 . C42 . 105.9(3) yes C35 . C36 . C37 . 112.2(3) yes C35 . C36 . H361 . 107.3 no C37 . C36 . H361 . 108.9 no C35 . C36 . H362 . 110.4 no C37 . C36 . H362 . 108.5 no H361 . C36 . H362 . 109.6 no C36 . C37 . C38 . 112.1(3) yes C36 . C37 . H371 . 108.9 no C38 . C37 . H371 . 110.0 no C36 . C37 . H372 . 108.7 no C38 . C37 . H372 . 108.6 no H371 . C37 . H372 . 108.5 no C37 . C38 . C39 . 111.7(3) yes C37 . C38 . H381 . 108.4 no C39 . C38 . H381 . 109.3 no C37 . C38 . H382 . 108.8 no C39 . C38 . H382 . 109.3 no H381 . C38 . H382 . 109.4 no C38 . C39 . C40 . 111.3(4) yes C38 . C39 . H391 . 110.0 no C40 . C39 . H391 . 108.5 no C38 . C39 . H392 . 108.1 no C40 . C39 . H392 . 109.8 no H391 . C39 . H392 . 109.0 no C35 . C40 . C39 . 111.8(3) yes C35 . C40 . H402 . 108.7 no C39 . C40 . H402 . 108.8 no C35 . C40 . H401 . 109.8 no C39 . C40 . H401 . 108.7 no H402 . C40 . H401 . 109.2 no C35 . C41 . H412 . 109.1 no C35 . C41 . H413 . 110.9 no H412 . C41 . H413 . 108.8 no C35 . C41 . H411 . 109.7 no H412 . C41 . H411 . 108.4 no H413 . C41 . H411 . 110.0 no C35 . C42 . O43 . 117.8(3) yes C35 . C42 . O44 . 116.8(3) yes O43 . C42 . O44 . 125.3(3) yes Mn2 . O43 . C42 . 123.0(2) yes Mn3 . O44 . C42 . 135.1(2) yes Mn1 . O45 . C46 . 132.4(3) yes Mn1 . O45 . H451 . 112.0 no C46 . O45 . H451 . 114.0 no O45 . C46 . H463 . 110.1 no O45 . C46 . H461 . 110.4 no H463 . C46 . H461 . 106.6 no O45 . C46 . H462 . 110.8 no H463 . C46 . H462 . 108.4 no H461 . C46 . H462 . 110.5 no Mn1 . O47 . C48 . 124.9(3) yes Mn1 . O47 . H471 . 120.2 no C48 . O47 . H471 . 113.0 no O47 . C48 . H481 . 108.2 no O47 . C48 . H482 . 112.2 no H481 . C48 . H482 . 107.7 no O47 . C48 . H483 . 109.0 no H481 . C48 . H483 . 109.2 no H482 . C48 . H483 . 110.5 no C50 . O49 . H491 . 106.7 no O49 . C50 . H502 . 110.8 no O49 . C50 . H503 . 109.5 no H502 . C50 . H503 . 108.3 no O49 . C50 . H501 . 110.0 no H502 . C50 . H501 . 110.1 no H503 . C50 . H501 . 108.1 no Mn103 . Mn101 . O104 . 30.05(6) yes Mn103 . Mn101 . O105 . 149.80(7) yes O104 . Mn101 . O105 . 171.40(10) yes Mn103 . Mn101 . N113 . 118.15(7) yes O104 . Mn101 . N113 . 88.60(9) yes O105 . Mn101 . N113 . 91.93(10) yes Mn103 . Mn101 . O134 . 62.10(6) yes O104 . Mn101 . O134 . 92.03(9) yes O105 . Mn101 . O134 . 88.23(9) yes N113 . Mn101 . O134 . 174.72(10) yes Mn103 . Mn101 . O145 . 88.51(8) yes O104 . Mn101 . O145 . 92.08(10) yes O105 . Mn101 . O145 . 96.52(11) yes N113 . Mn101 . O145 . 86.57(10) yes O134 . Mn101 . O145 . 88.17(9) yes Mn103 . Mn101 . O147 . 90.77(6) yes O104 . Mn101 . O147 . 81.96(8) yes O105 . Mn101 . O147 . 89.54(10) yes N113 . Mn101 . O147 . 84.21(9) yes O134 . Mn101 . O147 . 101.08(9) yes O145 . Mn101 . O147 . 169.12(9) yes Mn103 . Mn102 . O104 . 32.32(6) yes Mn103 . Mn102 . O114 . 122.86(6) yes O104 . Mn102 . O114 . 91.66(9) yes Mn103 . Mn102 . O115 . 150.68(7) yes O104 . Mn102 . O115 . 164.65(10) yes O114 . Mn102 . O115 . 85.88(9) yes Mn103 . Mn102 . N123 . 60.90(7) yes O104 . Mn102 . N123 . 88.08(9) yes O114 . Mn102 . N123 . 163.18(10) yes O115 . Mn102 . N123 . 89.93(9) yes Mn103 . Mn102 . O143 . 81.23(6) yes O104 . Mn102 . O143 . 97.90(9) yes O114 . Mn102 . O143 . 105.88(9) yes O115 . Mn102 . O143 . 97.35(9) yes N123 . Mn102 . O143 . 90.81(9) yes O124 2_666 Mn103 . Mn102 . 103.97(5) yes O124 2_666 Mn103 . Mn101 . 81.63(5) yes Mn102 . Mn103 . Mn101 . 61.050(13) yes O124 2_666 Mn103 . Mn103 2_666 36.05(5) yes Mn102 . Mn103 . Mn103 2_666 85.338(18) yes Mn101 . Mn103 . Mn103 2_666 99.11(2) yes O124 2_666 Mn103 . O104 . 87.69(8) yes Mn102 . Mn103 . O104 . 31.85(6) yes Mn101 . Mn103 . O104 . 30.11(6) yes Mn103 2_666 Mn103 . O104 . 87.34(6) yes O124 2_666 Mn103 . O124 . 80.19(8) yes Mn102 . Mn103 . O124 . 65.05(6) yes Mn101 . Mn103 . O124 . 115.94(6) yes Mn103 2_666 Mn103 . O124 . 44.14(6) yes O104 . Mn103 . O124 . 88.29(8) yes O124 2_666 Mn103 . O125 . 90.97(8) yes Mn102 . Mn103 . O125 . 151.75(7) yes Mn101 . Mn103 . O125 . 146.26(6) yes Mn103 2_666 Mn103 . O125 . 93.57(6) yes O104 . Mn103 . O125 . 176.34(9) yes O124 2_666 Mn103 . N133 . 86.32(9) yes Mn102 . Mn103 . N133 . 115.49(7) yes Mn101 . Mn103 . N133 . 57.92(7) yes Mn103 2_666 Mn103 . N133 . 122.30(7) yes O104 . Mn103 . N133 . 87.60(9) yes O124 2_666 Mn103 . O144 . 171.63(8) yes Mn102 . Mn103 . O144 . 73.28(6) yes Mn101 . Mn103 . O144 . 103.34(6) yes Mn103 2_666 Mn103 . O144 . 135.66(7) yes O104 . Mn103 . O144 . 93.36(9) yes O124 . Mn103 . O125 . 94.84(8) yes O124 . Mn103 . N133 . 166.05(10) yes O125 . Mn103 . N133 . 88.91(9) yes O124 . Mn103 . O144 . 91.53(9) yes O125 . Mn103 . O144 . 88.47(9) yes N133 . Mn103 . O144 . 102.01(10) yes Mn101 . O104 . Mn103 . 119.84(10) yes Mn101 . O104 . Mn102 . 121.50(11) yes Mn103 . O104 . Mn102 . 115.82(10) yes Mn101 . O105 . C106 . 129.5(2) yes O105 . C106 . C107 . 118.3(3) yes O105 . C106 . C111 . 123.4(3) yes C107 . C106 . C111 . 118.3(3) yes C106 . C107 . C108 . 121.1(3) yes C106 . C107 . H1071 . 119.0 no C108 . C107 . H1071 . 119.9 no C107 . C108 . C109 . 120.5(3) yes C107 . C108 . H1081 . 119.5 no C109 . C108 . H1081 . 119.9 no C108 . C109 . C110 . 119.3(3) yes C108 . C109 . H1091 . 121.0 no C110 . C109 . H1091 . 119.7 no C109 . C110 . C111 . 121.6(3) yes C109 . C110 . H1101 . 119.3 no C111 . C110 . H1101 . 119.1 no C106 . C111 . C110 . 119.2(3) yes C106 . C111 . C112 . 123.4(3) yes C110 . C111 . C112 . 117.4(3) yes C111 . C112 . N113 . 123.5(3) yes C111 . C112 . H1121 . 118.6 no N113 . C112 . H1121 . 117.9 no Mn101 . N113 . C112 . 126.9(2) yes Mn101 . N113 . O114 . 117.85(18) yes C112 . N113 . O114 . 115.3(2) yes N113 . O114 . Mn102 . 118.60(17) yes Mn102 . O115 . C116 . 130.4(2) yes O115 . C116 . C117 . 118.7(3) yes O115 . C116 . C121 . 123.0(3) yes C117 . C116 . C121 . 118.3(3) yes C116 . C117 . C118 . 121.3(3) yes C116 . C117 . H1171 . 119.0 no C118 . C117 . H1171 . 119.7 no C117 . C118 . C119 . 120.6(3) yes C117 . C118 . H1181 . 119.9 no C119 . C118 . H1181 . 119.5 no C118 . C119 . C120 . 119.4(3) yes C118 . C119 . H1191 . 120.4 no C120 . C119 . H1191 . 120.2 no C119 . C120 . C121 . 121.5(3) yes C119 . C120 . H1201 . 119.3 no C121 . C120 . H1201 . 119.2 no C116 . C121 . C120 . 118.9(3) yes C116 . C121 . C122 . 122.6(3) yes C120 . C121 . C122 . 118.4(3) yes C121 . C122 . N123 . 124.3(3) yes C121 . C122 . H1221 . 118.4 no N123 . C122 . H1221 . 117.2 no Mn102 . N123 . C122 . 126.2(2) yes Mn102 . N123 . O124 . 118.01(16) yes C122 . N123 . O124 . 115.7(2) yes Mn103 2_666 O124 . N123 . 117.49(15) yes Mn103 2_666 O124 . Mn103 . 99.81(8) yes N123 . O124 . Mn103 . 111.94(15) yes Mn103 . O125 . C126 . 120.99(18) yes O125 . C126 . C127 . 119.5(3) yes O125 . C126 . C131 . 122.3(3) yes C127 . C126 . C131 . 118.2(3) yes C126 . C127 . C128 . 120.6(3) yes C126 . C127 . H1271 . 119.3 no C128 . C127 . H1271 . 120.0 no C127 . C128 . C129 . 121.5(3) yes C127 . C128 . H1281 . 118.2 no C129 . C128 . H1281 . 120.3 no C128 . C129 . C130 . 118.9(3) yes C128 . C129 . H1291 . 120.5 no C130 . C129 . H1291 . 120.5 no C129 . C130 . C131 . 120.8(3) yes C129 . C130 . H1301 . 119.8 no C131 . C130 . H1301 . 119.5 no C126 . C131 . C130 . 119.9(3) yes C126 . C131 . C132 . 122.5(3) yes C130 . C131 . C132 . 117.5(3) yes C131 . C132 . N133 . 122.3(3) yes C131 . C132 . H1321 . 119.1 no N133 . C132 . H1321 . 118.6 no Mn103 . N133 . C132 . 125.4(2) yes Mn103 . N133 . O134 . 117.26(17) yes C132 . N133 . O134 . 117.3(2) yes N133 . O134 . Mn101 . 113.12(16) yes C136 . C135 . C140 . 109.9(3) yes C136 . C135 . C141 . 111.0(3) yes C140 . C135 . C141 . 109.4(3) yes C136 . C135 . C142 . 110.1(3) yes C140 . C135 . C142 . 111.3(3) yes C141 . C135 . C142 . 105.0(3) yes C135 . C136 . C137 . 112.3(3) yes C135 . C136 . H1362 . 108.0 no C137 . C136 . H1362 . 107.5 no C135 . C136 . H1361 . 109.0 no C137 . C136 . H1361 . 110.3 no H1362 . C136 . H1361 . 109.7 no C136 . C137 . C138 . 111.6(3) yes C136 . C137 . H1371 . 108.4 no C138 . C137 . H1371 . 109.2 no C136 . C137 . H1372 . 107.3 no C138 . C137 . H1372 . 109.8 no H1371 . C137 . H1372 . 110.7 no C137 . C138 . C139 . 110.1(3) yes C137 . C138 . H1382 . 107.5 no C139 . C138 . H1382 . 108.9 no C137 . C138 . H1381 . 110.4 no C139 . C138 . H1381 . 110.2 no H1382 . C138 . H1381 . 109.8 no C138 . C139 . C140 . 111.3(3) yes C138 . C139 . H1391 . 110.1 no C140 . C139 . H1391 . 108.5 no C138 . C139 . H1392 . 109.3 no C140 . C139 . H1392 . 109.4 no H1391 . C139 . H1392 . 108.3 no C135 . C140 . C139 . 113.5(3) yes C135 . C140 . H1401 . 107.5 no C139 . C140 . H1401 . 107.6 no C135 . C140 . H1402 . 108.7 no C139 . C140 . H1402 . 111.0 no H1401 . C140 . H1402 . 108.3 no C135 . C141 . H1413 . 110.8 no C135 . C141 . H1411 . 110.3 no H1413 . C141 . H1411 . 108.5 no C135 . C141 . H1412 . 110.1 no H1413 . C141 . H1412 . 108.4 no H1411 . C141 . H1412 . 108.6 no C135 . C142 . O143 . 117.0(3) yes C135 . C142 . O144 . 118.1(3) yes O143 . C142 . O144 . 124.8(3) yes Mn102 . O143 . C142 . 123.2(2) yes Mn103 . O144 . C142 . 135.5(2) yes Mn101 . O145 . C146 . 127.7(3) yes Mn101 . O145 . H1451 . 119.0 no C146 . O145 . H1451 . 106.0 no O145 . C146 . H1463 . 109.4 no O145 . C146 . H1462 . 112.5 no H1463 . C146 . H1462 . 109.0 no O145 . C146 . H1461 . 110.2 no H1463 . C146 . H1461 . 106.8 no H1462 . C146 . H1461 . 108.8 no Mn101 . O147 . C148 . 126.9(2) yes Mn101 . O147 . H1471 . 113.0 no C148 . O147 . H1471 . 107.9 no O147 . C148 . H1483 . 109.7 no O147 . C148 . H1481 . 111.3 no H1483 . C148 . H1481 . 108.9 no O147 . C148 . H1482 . 111.1 no H1483 . C148 . H1482 . 107.9 no H1481 . C148 . H1482 . 107.9 no C150 . O149 . H1491 . 84.3 no O149 . C150 . H1503 . 109.6 no O149 . C150 . H1502 . 109.8 no H1503 . C150 . H1502 . 109.4 no O149 . C150 . H1506 . 109.4 no H1503 . C150 . H1506 . 109.4 no H1502 . C150 . H1506 . 109.3 no O151 . C150 . H1501 . 109.7 no O151 . C150 . H1505 . 109.4 no H1501 . C150 . H1505 . 109.1 no O151 . C150 . H1504 . 110.3 no H1501 . C150 . H1504 . 109.4 no H1505 . C150 . H1504 . 108.8 no C150 . O151 . H1511 . 97.7 no # Attachment '[8]CCDC706510.cif' data_EB8041 _database_code_depnum_ccdc_archive 'CCDC 706510' _cell_length_a 13.521(2) _cell_length_b 13.6880(19) _cell_length_c 13.814(2) _cell_angle_alpha 112.975(9) _cell_angle_beta 95.825(9) _cell_angle_gamma 118.889(7) _cell_volume 1923.0(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C40 H50 Mn6 N6 O20 # Dc = 1.09 Fooo = 900.00 Mu = 10.08 M = 632.22 # Found Formula = C70 H96 Mn6 N6 O24 # Dc = 1.50 FOOO = 900.00 Mu = 10.34 M = 867.56 _chemical_formula_sum 'C70 H96 Mn6 N6 O24' _chemical_formula_weight 1735.13 _cell_measurement_reflns_used 6464 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.034 # Sheldrick geometric approximatio 0.81 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.88 _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 '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 17799 _reflns_number_total 10695 _diffrn_reflns_av_R_equivalents 0.0864 # Number of reflections with Friedels Law is 1 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9714 _diffrn_reflns_theta_min 1.716 _diffrn_reflns_theta_max 28.403 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.279 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min -17 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _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 -0.96 _refine_diff_density_max 1.27 # 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 10695 _refine_ls_number_restraints 6 _refine_ls_number_parameters 479 _oxford_refine_ls_R_factor_ref 0.0828 _refine_ls_wR_factor_ref 0.1886 _refine_ls_goodness_of_fit_ref 1.0423 _refine_ls_shift/su_max 0.000360 # The values computed from all data _oxford_reflns_number_all 10695 _refine_ls_R_factor_all 0.0828 _refine_ls_wR_factor_all 0.1886 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9800 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_gt 0.1800 # 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^ +15.83P] ,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 0.49416(7) 0.10045(7) 0.61005(7) 0.0137 1.0000 Uani . . . . . . . Mn2 Mn 0.27749(7) -0.11226(8) 0.64749(7) 0.0170 1.0000 Uani . . . . . . . Mn3 Mn 0.52567(7) -0.09725(8) 0.66488(7) 0.0159 1.0000 Uani . . . . . . . O4 O 0.4370(3) -0.0281(3) 0.6493(3) 0.0156 1.0000 Uani . . . . . . . O5 O 0.5334(3) 0.2067(4) 0.5429(3) 0.0184 1.0000 Uani . . . . . . . C6 C 0.5190(5) 0.3042(5) 0.5802(5) 0.0175 1.0000 Uani . . . . . . . C7 C 0.6014(5) 0.4162(5) 0.5791(5) 0.0226 1.0000 Uani . . . . . . . C8 C 0.5927(5) 0.5194(5) 0.6129(5) 0.0241 1.0000 Uani . . . . . . . C9 C 0.4995(5) 0.5150(5) 0.6499(6) 0.0261 1.0000 Uani . . . . . . . C10 C 0.4174(5) 0.4054(6) 0.6503(6) 0.0275 1.0000 Uani . . . . . . . C11 C 0.4212(5) 0.2975(5) 0.6148(5) 0.0211 1.0000 Uani . . . . . . . C12 C 0.3250(5) 0.1794(6) 0.6099(5) 0.0222 1.0000 Uani . . . . . . . N13 N 0.3419(4) 0.0942(4) 0.6074(4) 0.0173 1.0000 Uani . . . . . . . O14 O 0.2450(3) -0.0161(4) 0.5953(4) 0.0209 1.0000 Uani . . . . . . . C15 C 0.2048(6) 0.1617(7) 0.6078(7) 0.0346 1.0000 Uani . . . . . . . C16 C 0.1344(6) 0.1384(9) 0.5007(8) 0.0487 1.0000 Uani . . . . . . . O17 O 0.1180(3) -0.2049(4) 0.6405(4) 0.0243 1.0000 Uani . . . . . . . C18 C 0.0838(5) -0.2428(5) 0.7136(5) 0.0231 1.0000 Uani . . . . . . . C19 C -0.0221(6) -0.2578(6) 0.7280(6) 0.0301 1.0000 Uani . U . . . . . C20 C -0.0636(6) -0.2971(6) 0.8030(6) 0.0318 1.0000 Uani . U . . . . . C21 C -0.0001(7) -0.3193(6) 0.8645(6) 0.0346 1.0000 Uani . . . . . . . C22 C 0.1034(6) -0.3086(6) 0.8496(5) 0.0276 1.0000 Uani . . . . . . . C23 C 0.1486(5) -0.2710(5) 0.7736(5) 0.0231 1.0000 Uani . . . . . . . C24 C 0.2516(5) -0.2727(5) 0.7525(5) 0.0221 1.0000 Uani . . . . . . . N25 N 0.3087(4) -0.2150(4) 0.7006(4) 0.0201 1.0000 Uani . . . . . . . O26 O 0.3940(3) -0.2349(4) 0.6705(4) 0.0219 1.0000 Uani . . . . . . . C27 C 0.2856(5) -0.3510(6) 0.7807(6) 0.0274 1.0000 Uani . . . . . . . C28 C 0.1974(6) -0.4951(6) 0.7003(6) 0.0334 1.0000 Uani . . . . . . . O29 O 0.6198(3) -0.1590(4) 0.6775(4) 0.0207 1.0000 Uani . . . . . . . C30 C 0.7363(5) -0.0796(5) 0.7416(5) 0.0193 1.0000 Uani . . . . . . . C31 C 0.7828(5) -0.1226(6) 0.7988(5) 0.0259 1.0000 Uani . . . . . . . C32 C 0.9030(6) -0.0451(6) 0.8680(5) 0.0266 1.0000 Uani . . . . . . . C33 C 0.9796(5) 0.0748(6) 0.8793(6) 0.0297 1.0000 Uani . . . . . . . C34 C 0.9359(5) 0.1171(6) 0.8231(5) 0.0242 1.0000 Uani . . . . . . . C35 C 0.8149(5) 0.0431(5) 0.7536(5) 0.0208 1.0000 Uani . . . . . . . C36 C 0.7755(5) 0.0928(5) 0.6928(5) 0.0209 1.0000 Uani . . . . . . . N37 N 0.6601(4) 0.0393(4) 0.6496(4) 0.0160 1.0000 Uani . . . . . . . O38 O 0.6247(3) 0.0810(4) 0.5851(3) 0.0174 1.0000 Uani . . . . . . . C39 C 0.8663(4) 0.2059(5) 0.6855(5) 0.0206 1.0000 Uani . . . . . . . C40 C 0.8888(5) 0.3301(6) 0.7771(6) 0.0289 1.0000 Uani . . . . . . . C41 C 0.6109(5) 0.3021(5) 0.8752(5) 0.0204 1.0000 Uani . . . . . . . O42 O 0.5975(3) 0.2664(4) 0.7726(3) 0.0227 1.0000 Uani . . . . . . . O43 O 0.5784(4) 0.2281(4) 0.9158(4) 0.0285 1.0000 Uani . . . . . . . C44 C 0.6724(5) 0.4465(5) 0.9576(5) 0.0234 1.0000 Uani . . . . . . . C45 C 0.6062(6) 0.4606(6) 1.0407(6) 0.0321 1.0000 Uani . . . . . . . C46 C 0.6723(7) 0.5167(6) 0.8950(6) 0.0396 1.0000 Uani . . . . . . . C47 C 0.8030(5) 0.5010(6) 1.0227(6) 0.0320 1.0000 Uani . . . . . . . O48 O 0.3394(4) 0.0376(4) 0.8293(4) 0.0280 1.0000 Uani . . . . . . . C49 C 0.2785(8) 0.0955(8) 0.8705(8) 0.0520 1.0000 Uani . . . . . . . O50 O 0.2226(3) -0.2798(4) 0.4766(3) 0.0222 1.0000 Uani . . . . . . . C51 C 0.1356(5) -0.4104(5) 0.4439(5) 0.0252 1.0000 Uani . . . . . . . O52 O 0.6008(4) 0.0317(4) 0.8480(4) 0.0295 1.0000 Uani . . . . . . . C53 C 0.6178(7) 0.0042(7) 0.9342(6) 0.0364 1.0000 Uani . . . . . . . H71 H 0.6658 0.4208 0.5544 0.0243 1.0000 Uiso R . . . . . . H81 H 0.6499 0.5938 0.6108 0.0266 1.0000 Uiso R . . . . . . H91 H 0.4925 0.5858 0.6744 0.0328 1.0000 Uiso R . . . . . . H151 H 0.2193 0.2369 0.6689 0.0497 1.0000 Uiso R . . . . . . H152 H 0.1570 0.0892 0.6163 0.0497 1.0000 Uiso R . . . . . . H161 H 0.0600 0.1273 0.5039 0.0542 1.0000 Uiso R . . . . . . H162 H 0.1808 0.2106 0.4915 0.0542 1.0000 Uiso R . . . . . . H163 H 0.1184 0.0629 0.4388 0.0542 1.0000 Uiso R . . . . . . H191 H -0.0668 -0.2422 0.6856 0.0393 1.0000 Uiso R . . . . . . H201 H -0.1359 -0.3069 0.8123 0.0436 1.0000 Uiso R . . . . . . H211 H -0.0278 -0.3439 0.9169 0.0456 1.0000 Uiso R . . . . . . H221 H 0.1464 -0.3250 0.8927 0.0347 1.0000 Uiso R . . . . . . H271 H 0.2894 -0.3324 0.8553 0.0383 1.0000 Uiso R . . . . . . H272 H 0.3630 -0.3266 0.7761 0.0383 1.0000 Uiso R . . . . . . H281 H 0.2233 -0.5395 0.7215 0.0455 1.0000 Uiso R . . . . . . H282 H 0.1197 -0.5211 0.7045 0.0455 1.0000 Uiso R . . . . . . H283 H 0.1933 -0.5153 0.6253 0.0455 1.0000 Uiso R . . . . . . H311 H 0.7312 -0.2064 0.7884 0.0304 1.0000 Uiso R . . . . . . H321 H 0.9321 -0.0738 0.9086 0.0320 1.0000 Uiso R . . . . . . H331 H 1.0630 0.1270 0.9244 0.0300 1.0000 Uiso R . . . . . . H341 H 0.9891 0.2005 0.8330 0.0291 1.0000 Uiso R . . . . . . H391 H 0.9397 0.2115 0.6933 0.0233 1.0000 Uiso R . . . . . . H392 H 0.8356 0.1945 0.6141 0.0233 1.0000 Uiso R . . . . . . H401 H 0.9463 0.4012 0.7712 0.0315 1.0000 Uiso R . . . . . . H402 H 0.9196 0.3418 0.8485 0.0315 1.0000 Uiso R . . . . . . H403 H 0.8154 0.3247 0.7693 0.0315 1.0000 Uiso R . . . . . . H451 H 0.6431 0.5494 1.0926 0.0376 1.0000 Uiso R . . . . . . H452 H 0.6103 0.4189 1.0806 0.0376 1.0000 Uiso R . . . . . . H453 H 0.5239 0.4214 1.0000 0.0376 1.0000 Uiso R . . . . . . H461 H 0.7112 0.6059 0.9473 0.0443 1.0000 Uiso R . . . . . . H462 H 0.7143 0.5072 0.8448 0.0443 1.0000 Uiso R . . . . . . H463 H 0.5911 0.4803 0.8535 0.0443 1.0000 Uiso R . . . . . . H471 H 0.8447 0.5907 1.0746 0.0294 1.0000 Uiso R . . . . . . H472 H 0.8016 0.4575 1.0625 0.0294 1.0000 Uiso R . . . . . . H473 H 0.8434 0.4883 0.9715 0.0294 1.0000 Uiso R . . . . . . H481 H 0.4010 0.0603 0.8744 0.0329 1.0000 Uiso R . . . . . . H491 H 0.2093 0.0606 0.8098 0.0606 1.0000 Uiso R . . . . . . H492 H 0.2538 0.0774 0.9269 0.0606 1.0000 Uiso R . . . . . . H493 H 0.3306 0.1863 0.9016 0.0606 1.0000 Uiso R . . . . . . H501 H 0.2543 -0.2646 0.4321 0.0239 1.0000 Uiso R . . . . . . H511 H 0.1073 -0.4124 0.5038 0.0261 1.0000 Uiso R . . . . . . H512 H 0.1711 -0.4574 0.4283 0.0261 1.0000 Uiso R . . . . . . H513 H 0.0696 -0.4485 0.3786 0.0261 1.0000 Uiso R . . . . . . H521 H 0.6234 0.1066 0.8697 0.0358 1.0000 Uiso R . . . . . . H571 H 0.3539 0.4027 0.6757 0.0362 1.0000 Uiso R . . . . . . H651 H 0.5890 -0.0843 0.9003 0.0485 1.0000 Uiso R . . . . . . H652 H 0.7011 0.0566 0.9798 0.0485 1.0000 Uiso R . . . . . . H653 H 0.5731 0.0200 0.9796 0.0485 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 0.0130(3) 0.0151(4) 0.0147(4) 0.0081(3) 0.0075(3) 0.0081(3) Mn2 0.0153(4) 0.0168(4) 0.0201(4) 0.0106(3) 0.0104(3) 0.0082(3) Mn3 0.0142(4) 0.0155(4) 0.0168(4) 0.0085(3) 0.0055(3) 0.0074(3) O4 0.0138(16) 0.0154(17) 0.0194(19) 0.0103(15) 0.0091(14) 0.0078(14) O5 0.0196(18) 0.0200(18) 0.021(2) 0.0138(16) 0.0104(15) 0.0117(16) C6 0.017(2) 0.019(2) 0.016(3) 0.008(2) 0.005(2) 0.011(2) C7 0.021(3) 0.019(3) 0.022(3) 0.007(2) 0.009(2) 0.011(2) C8 0.023(3) 0.013(2) 0.028(3) 0.010(2) 0.004(2) 0.005(2) C9 0.030(3) 0.018(3) 0.031(3) 0.011(2) 0.008(3) 0.017(2) C10 0.020(3) 0.035(3) 0.037(4) 0.021(3) 0.014(3) 0.019(3) C11 0.019(2) 0.021(3) 0.028(3) 0.016(2) 0.011(2) 0.012(2) C12 0.016(2) 0.031(3) 0.025(3) 0.016(3) 0.011(2) 0.015(2) N13 0.0135(19) 0.020(2) 0.020(2) 0.0139(19) 0.0089(18) 0.0078(18) O14 0.0180(18) 0.0187(18) 0.028(2) 0.0130(17) 0.0134(16) 0.0096(16) C15 0.023(3) 0.036(4) 0.062(5) 0.033(4) 0.022(3) 0.020(3) C16 0.030(4) 0.058(5) 0.052(5) 0.022(4) 0.009(3) 0.027(4) O17 0.0162(18) 0.026(2) 0.032(2) 0.0174(19) 0.0133(17) 0.0102(16) C18 0.022(3) 0.015(2) 0.028(3) 0.009(2) 0.014(2) 0.008(2) C19 0.030(3) 0.029(3) 0.044(3) 0.024(2) 0.024(2) 0.019(2) C20 0.032(3) 0.028(3) 0.046(3) 0.023(2) 0.033(3) 0.017(2) C21 0.049(4) 0.033(3) 0.034(4) 0.022(3) 0.033(3) 0.024(3) C22 0.038(3) 0.023(3) 0.025(3) 0.015(2) 0.018(3) 0.016(3) C23 0.024(3) 0.016(2) 0.022(3) 0.007(2) 0.011(2) 0.007(2) C24 0.023(3) 0.015(2) 0.018(3) 0.005(2) 0.008(2) 0.006(2) N25 0.023(2) 0.020(2) 0.015(2) 0.0077(19) 0.0072(18) 0.0113(19) O26 0.0215(18) 0.0216(19) 0.028(2) 0.0164(17) 0.0142(17) 0.0115(16) C27 0.027(3) 0.035(3) 0.031(3) 0.026(3) 0.016(3) 0.017(3) C28 0.042(4) 0.031(3) 0.038(4) 0.019(3) 0.019(3) 0.026(3) O29 0.0151(17) 0.0169(18) 0.029(2) 0.0107(17) 0.0070(16) 0.0091(15) C30 0.019(2) 0.014(2) 0.020(3) 0.005(2) 0.004(2) 0.010(2) C31 0.027(3) 0.021(3) 0.026(3) 0.011(2) 0.007(2) 0.012(2) C32 0.035(3) 0.025(3) 0.019(3) 0.006(2) 0.001(2) 0.022(3) C33 0.024(3) 0.021(3) 0.026(3) 0.003(2) -0.006(2) 0.011(2) C34 0.021(3) 0.025(3) 0.026(3) 0.013(2) 0.008(2) 0.013(2) C35 0.023(3) 0.020(3) 0.016(3) 0.007(2) 0.005(2) 0.012(2) C36 0.022(3) 0.021(3) 0.018(3) 0.009(2) 0.010(2) 0.012(2) N37 0.020(2) 0.017(2) 0.015(2) 0.0082(17) 0.0084(17) 0.0136(18) O38 0.0159(17) 0.0202(18) 0.021(2) 0.0108(16) 0.0099(15) 0.0123(15) C39 0.010(2) 0.023(3) 0.020(3) 0.008(2) 0.001(2) 0.007(2) C40 0.017(3) 0.022(3) 0.034(4) 0.011(3) 0.003(2) 0.006(2) C41 0.019(2) 0.021(3) 0.022(3) 0.010(2) 0.009(2) 0.013(2) O42 0.0207(18) 0.0211(19) 0.017(2) 0.0070(16) 0.0060(15) 0.0083(16) O43 0.034(2) 0.021(2) 0.024(2) 0.0113(18) 0.0103(18) 0.0115(18) C44 0.027(3) 0.020(3) 0.018(3) 0.008(2) 0.005(2) 0.013(2) C45 0.037(3) 0.031(3) 0.029(3) 0.011(3) 0.012(3) 0.024(3) C46 0.053(4) 0.025(3) 0.032(4) 0.015(3) 0.005(3) 0.018(3) C47 0.023(3) 0.029(3) 0.028(3) 0.013(3) 0.002(3) 0.007(3) O48 0.028(2) 0.027(2) 0.025(2) 0.0092(18) 0.0137(18) 0.0155(18) C49 0.052(5) 0.045(5) 0.045(5) 0.011(4) 0.017(4) 0.028(4) O50 0.0219(19) 0.0175(18) 0.022(2) 0.0105(17) 0.0077(16) 0.0078(16) C51 0.022(3) 0.020(3) 0.028(3) 0.013(2) 0.008(2) 0.008(2) O52 0.044(3) 0.026(2) 0.017(2) 0.0096(18) 0.0081(19) 0.021(2) C53 0.050(4) 0.035(4) 0.027(4) 0.017(3) 0.018(3) 0.025(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4809(9) loop_ _oxford_twin_element_scale_factors 0.6647(14) 0.3353(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 . O38 2_656 2.461(4) yes Mn1 . Mn1 2_656 3.2897(17) yes Mn1 . Mn2 . 3.2510(11) yes Mn1 . Mn3 . 3.2753(12) yes Mn1 . O4 . 1.872(4) yes Mn1 . O5 . 1.915(4) yes Mn1 . N13 . 2.015(5) yes Mn1 . O38 . 1.952(4) yes Mn1 . O42 . 2.115(4) yes Mn2 . Mn3 . 3.2392(12) yes Mn2 . O4 . 1.883(3) yes Mn2 . O14 . 1.918(4) yes Mn2 . O17 . 1.868(4) yes Mn2 . N25 . 2.003(5) yes Mn2 . O48 . 2.260(4) yes Mn2 . O50 . 2.271(4) yes Mn3 . O5 2_656 2.478(4) yes Mn3 . O4 . 1.892(4) yes Mn3 . O26 . 1.904(4) yes Mn3 . O29 . 1.864(4) yes Mn3 . N37 . 1.987(4) yes Mn3 . O52 . 2.193(4) yes O5 . C6 . 1.348(6) yes C6 . C7 . 1.401(8) yes C6 . C11 . 1.426(8) yes C7 . C8 . 1.373(8) yes C7 . H71 . 0.950 no C8 . C9 . 1.391(9) yes C8 . H81 . 0.950 no C9 . C10 . 1.372(8) yes C9 . H91 . 0.950 no C10 . C11 . 1.392(9) yes C10 . H571 . 0.950 no C11 . C12 . 1.473(7) yes C12 . N13 . 1.281(8) yes C12 . C15 . 1.519(8) yes N13 . O14 . 1.368(5) yes C15 . C16 . 1.499(11) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no O17 . C18 . 1.333(7) yes C18 . C19 . 1.392(8) yes C18 . C23 . 1.424(9) yes C19 . C20 . 1.393(9) yes C19 . H191 . 0.950 no C20 . C21 . 1.363(11) yes C20 . H201 . 0.950 no C21 . C22 . 1.380(9) yes C21 . H211 . 0.950 no C22 . C23 . 1.411(8) yes C22 . H221 . 0.950 no C23 . C24 . 1.460(8) yes C24 . N25 . 1.304(7) yes C24 . C27 . 1.510(8) yes N25 . O26 . 1.374(6) yes C27 . C28 . 1.515(9) yes C27 . H271 . 0.950 no C27 . H272 . 0.950 no C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H283 . 0.950 no O29 . C30 . 1.325(6) yes C30 . C31 . 1.408(8) yes C30 . C35 . 1.414(7) yes C31 . C32 . 1.381(8) yes C31 . H311 . 0.950 no C32 . C33 . 1.383(9) yes C32 . H321 . 0.950 no C33 . C34 . 1.370(8) yes C33 . H331 . 0.950 no C34 . C35 . 1.394(8) yes C34 . H341 . 0.950 no C35 . C36 . 1.469(8) yes C36 . N37 . 1.301(7) yes C36 . C39 . 1.492(7) yes N37 . O38 . 1.387(6) yes C39 . C40 . 1.525(9) yes C39 . H391 . 0.950 no C39 . H392 . 0.950 no C40 . H401 . 0.950 no C40 . H402 . 0.950 no C40 . H403 . 0.950 no C41 . O42 . 1.266(7) yes C41 . O43 . 1.263(7) yes C41 . C44 . 1.535(8) yes C44 . C45 . 1.535(9) yes C44 . C46 . 1.524(9) yes C44 . C47 . 1.539(8) yes C45 . H451 . 0.950 no C45 . H452 . 0.950 no C45 . H453 . 0.950 no C46 . H461 . 0.950 no C46 . H462 . 0.950 no C46 . H463 . 0.950 no C47 . H471 . 0.950 no C47 . H472 . 0.950 no C47 . H473 . 0.950 no O48 . C49 . 1.415(9) yes O48 . H481 . 0.820 no C49 . H491 . 0.950 no C49 . H492 . 0.950 no C49 . H493 . 0.950 no O50 . C51 . 1.419(6) yes O50 . H501 . 0.820 no C51 . H511 . 0.950 no C51 . H512 . 0.950 no C51 . H513 . 0.950 no O52 . C53 . 1.411(8) yes O52 . H521 . 0.820 no C53 . H651 . 0.950 no C53 . H652 . 0.950 no C53 . H653 . 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 O38 2_656 Mn1 . Mn1 2_656 36.19(8) yes O38 2_656 Mn1 . Mn2 . 79.27(9) yes Mn1 2_656 Mn1 . Mn2 . 98.12(4) yes O38 2_656 Mn1 . Mn3 . 86.22(9) yes Mn1 2_656 Mn1 . Mn3 . 69.92(3) yes Mn2 . Mn1 . Mn3 . 59.51(3) yes O38 2_656 Mn1 . O4 . 84.91(15) yes Mn1 2_656 Mn1 . O4 . 86.05(12) yes Mn2 . Mn1 . O4 . 30.14(11) yes Mn3 . Mn1 . O4 . 29.70(11) yes O38 2_656 Mn1 . O5 . 84.80(15) yes Mn1 2_656 Mn1 . O5 . 86.28(13) yes Mn2 . Mn1 . O5 . 145.29(12) yes Mn3 . Mn1 . O5 . 149.97(12) yes O4 . Mn1 . O5 . 169.65(17) yes O38 2_656 Mn1 . N13 . 85.51(16) yes Mn1 2_656 Mn1 . N13 . 121.69(14) yes Mn2 . Mn1 . N13 . 59.58(12) yes Mn3 . Mn1 . N13 . 119.02(13) yes O4 . Mn1 . N13 . 89.37(16) yes O38 2_656 Mn1 . O38 . 84.29(15) yes Mn1 2_656 Mn1 . O38 . 48.10(12) yes Mn2 . Mn1 . O38 . 118.22(11) yes Mn3 . Mn1 . O38 . 60.30(11) yes O4 . Mn1 . O38 . 89.76(15) yes O38 2_656 Mn1 . O42 . 175.33(15) yes Mn1 2_656 Mn1 . O42 . 144.60(12) yes Mn2 . Mn1 . O42 . 104.13(11) yes Mn3 . Mn1 . O42 . 98.26(12) yes O4 . Mn1 . O42 . 99.64(16) yes O5 . Mn1 . N13 . 88.76(17) yes O5 . Mn1 . O38 . 90.28(16) yes N13 . Mn1 . O38 . 169.79(19) yes O5 . Mn1 . O42 . 90.63(16) yes N13 . Mn1 . O42 . 93.44(18) yes O38 . Mn1 . O42 . 96.73(16) yes Mn1 . Mn2 . Mn3 . 60.62(3) yes Mn1 . Mn2 . O4 . 29.94(11) yes Mn3 . Mn2 . O4 . 30.99(11) yes Mn1 . Mn2 . O14 . 61.78(11) yes Mn3 . Mn2 . O14 . 121.82(11) yes O4 . Mn2 . O14 . 91.70(15) yes Mn1 . Mn2 . O17 . 152.03(14) yes Mn3 . Mn2 . O17 . 146.40(13) yes O4 . Mn2 . O17 . 176.66(18) yes O14 . Mn2 . O17 . 90.30(17) yes Mn1 . Mn2 . N25 . 118.97(13) yes Mn3 . Mn2 . N25 . 58.85(13) yes O4 . Mn2 . N25 . 89.05(17) yes O14 . Mn2 . N25 . 179.10(18) yes O17 . Mn2 . N25 . 88.93(19) yes Mn1 . Mn2 . O48 . 90.77(11) yes Mn3 . Mn2 . O48 . 96.63(12) yes O4 . Mn2 . O48 . 91.00(16) yes O14 . Mn2 . O48 . 91.54(18) yes O17 . Mn2 . O48 . 91.62(18) yes Mn1 . Mn2 . O50 . 93.56(10) yes Mn3 . Mn2 . O50 . 78.33(11) yes O4 . Mn2 . O50 . 88.61(15) yes O14 . Mn2 . O50 . 97.86(16) yes O17 . Mn2 . O50 . 88.46(17) yes N25 . Mn2 . O48 . 88.96(18) yes N25 . Mn2 . O50 . 81.65(17) yes O48 . Mn2 . O50 . 170.60(16) yes O5 2_656 Mn3 . Mn2 . 91.41(9) yes O5 2_656 Mn3 . Mn1 . 78.65(9) yes Mn2 . Mn3 . Mn1 . 59.87(2) yes O5 2_656 Mn3 . O4 . 87.27(15) yes Mn2 . Mn3 . O4 . 30.83(10) yes Mn1 . Mn3 . O4 . 29.35(10) yes O5 2_656 Mn3 . O26 . 96.93(15) yes Mn2 . Mn3 . O26 . 61.71(13) yes Mn1 . Mn3 . O26 . 121.21(13) yes O4 . Mn3 . O26 . 92.54(16) yes O5 2_656 Mn3 . O29 . 91.43(16) yes Mn2 . Mn3 . O29 . 152.58(12) yes Mn1 . Mn3 . O29 . 147.13(12) yes O4 . Mn3 . O29 . 176.47(16) yes O26 . Mn3 . O29 . 90.87(17) yes O5 2_656 Mn3 . N37 . 79.78(16) yes Mn2 . Mn3 . N37 . 118.72(14) yes Mn1 . Mn3 . N37 . 58.93(13) yes O4 . Mn3 . N37 . 87.93(17) yes O26 . Mn3 . N37 . 176.66(19) yes O5 2_656 Mn3 . O52 . 169.49(14) yes Mn2 . Mn3 . O52 . 91.29(13) yes Mn1 . Mn3 . O52 . 93.98(12) yes O4 . Mn3 . O52 . 89.86(17) yes O26 . Mn3 . O52 . 93.29(18) yes O29 . Mn3 . N37 . 88.61(17) yes O29 . Mn3 . O52 . 90.84(18) yes N37 . Mn3 . O52 . 90.02(18) yes Mn3 . O4 . Mn2 . 118.17(18) yes Mn3 . O4 . Mn1 . 120.95(18) yes Mn2 . O4 . Mn1 . 119.93(19) yes Mn3 2_656 O5 . Mn1 . 117.23(18) yes Mn3 2_656 O5 . C6 . 110.5(3) yes Mn1 . O5 . C6 . 120.2(3) yes O5 . C6 . C7 . 118.0(5) yes O5 . C6 . C11 . 124.0(5) yes C7 . C6 . C11 . 117.9(5) yes C6 . C7 . C8 . 122.4(5) yes C6 . C7 . H71 . 118.6 no C8 . C7 . H71 . 118.9 no C7 . C8 . C9 . 119.9(5) yes C7 . C8 . H81 . 120.4 no C9 . C8 . H81 . 119.7 no C8 . C9 . C10 . 118.3(5) yes C8 . C9 . H91 . 121.2 no C10 . C9 . H91 . 120.5 no C9 . C10 . C11 . 123.8(6) yes C9 . C10 . H571 . 118.1 no C11 . C10 . H571 . 118.1 no C6 . C11 . C10 . 117.6(5) yes C6 . C11 . C12 . 121.5(5) yes C10 . C11 . C12 . 120.9(5) yes C11 . C12 . N13 . 121.3(5) yes C11 . C12 . C15 . 117.9(5) yes N13 . C12 . C15 . 120.9(5) yes Mn1 . N13 . C12 . 126.7(4) yes Mn1 . N13 . O14 . 116.0(4) yes C12 . N13 . O14 . 117.1(4) yes N13 . O14 . Mn2 . 117.7(3) yes C12 . C15 . C16 . 113.7(6) yes C12 . C15 . H151 . 109.0 no C16 . C15 . H151 . 108.5 no C12 . C15 . H152 . 108.2 no C16 . C15 . H152 . 108.0 no H151 . C15 . H152 . 109.5 no C15 . C16 . H161 . 110.0 no C15 . C16 . H162 . 109.0 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.4 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Mn2 . O17 . C18 . 125.1(4) yes O17 . C18 . C19 . 116.9(6) yes O17 . C18 . C23 . 123.0(5) yes C19 . C18 . C23 . 120.1(6) yes C18 . C19 . C20 . 120.2(6) yes C18 . C19 . H191 . 119.8 no C20 . C19 . H191 . 119.9 no C19 . C20 . C21 . 120.4(6) yes C19 . C20 . H201 . 119.6 no C21 . C20 . H201 . 119.9 no C20 . C21 . C22 . 120.4(6) yes C20 . C21 . H211 . 119.9 no C22 . C21 . H211 . 119.6 no C21 . C22 . C23 . 121.5(6) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 119.1 no C18 . C23 . C22 . 117.2(6) yes C18 . C23 . C24 . 122.9(5) yes C22 . C23 . C24 . 119.7(6) yes C23 . C24 . N25 . 120.0(5) yes C23 . C24 . C27 . 120.5(5) yes N25 . C24 . C27 . 119.2(5) yes Mn2 . N25 . C24 . 127.6(4) yes Mn2 . N25 . O26 . 115.5(3) yes C24 . N25 . O26 . 116.7(5) yes N25 . O26 . Mn3 . 115.8(3) yes C24 . C27 . C28 . 112.9(5) yes C24 . C27 . H271 . 108.8 no C28 . C27 . H271 . 109.4 no C24 . C27 . H272 . 108.3 no C28 . C27 . H272 . 107.9 no H271 . C27 . H272 . 109.5 no C27 . C28 . H281 . 109.3 no C27 . C28 . H282 . 108.8 no H281 . C28 . H282 . 109.5 no C27 . C28 . H283 . 110.3 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no Mn3 . O29 . C30 . 121.5(3) yes O29 . C30 . C31 . 117.2(5) yes O29 . C30 . C35 . 123.6(5) yes C31 . C30 . C35 . 119.2(5) yes C30 . C31 . C32 . 120.7(5) yes C30 . C31 . H311 . 119.5 no C32 . C31 . H311 . 119.8 no C31 . C32 . C33 . 119.9(6) yes C31 . C32 . H321 . 119.7 no C33 . C32 . H321 . 120.4 no C32 . C33 . C34 . 120.0(5) yes C32 . C33 . H331 . 120.2 no C34 . C33 . H331 . 119.7 no C33 . C34 . C35 . 122.1(5) yes C33 . C34 . H341 . 119.1 no C35 . C34 . H341 . 118.8 no C30 . C35 . C34 . 118.0(5) yes C30 . C35 . C36 . 122.8(5) yes C34 . C35 . C36 . 119.1(5) yes C35 . C36 . N37 . 118.5(5) yes C35 . C36 . C39 . 120.6(5) yes N37 . C36 . C39 . 120.9(5) yes Mn3 . N37 . C36 . 127.5(4) yes Mn3 . N37 . O38 . 115.0(3) yes C36 . N37 . O38 . 117.4(4) yes N37 . O38 . Mn1 2_656 108.5(3) yes N37 . O38 . Mn1 . 114.3(3) yes Mn1 2_656 O38 . Mn1 . 95.71(15) yes C36 . C39 . C40 . 110.3(5) yes C36 . C39 . H391 . 109.5 no C40 . C39 . H391 . 110.1 no C36 . C39 . H392 . 109.0 no C40 . C39 . H392 . 108.6 no H391 . C39 . H392 . 109.5 no C39 . C40 . H401 . 109.5 no C39 . C40 . H402 . 108.7 no H401 . C40 . H402 . 109.5 no C39 . C40 . H403 . 110.2 no H401 . C40 . H403 . 109.5 no H402 . C40 . H403 . 109.5 no O42 . C41 . O43 . 125.1(5) yes O42 . C41 . C44 . 117.9(5) yes O43 . C41 . C44 . 117.0(5) yes Mn1 . O42 . C41 . 141.3(4) yes C41 . C44 . C45 . 108.7(5) yes C41 . C44 . C46 . 111.1(5) yes C45 . C44 . C46 . 110.9(6) yes C41 . C44 . C47 . 106.6(5) yes C45 . C44 . C47 . 109.1(5) yes C46 . C44 . C47 . 110.3(5) yes C44 . C45 . H451 . 110.0 no C44 . C45 . H452 . 109.2 no H451 . C45 . H452 . 109.5 no C44 . C45 . H453 . 109.2 no H451 . C45 . H453 . 109.5 no H452 . C45 . H453 . 109.5 no C44 . C46 . H461 . 109.8 no C44 . C46 . H462 . 109.3 no H461 . C46 . H462 . 109.5 no C44 . C46 . H463 . 109.3 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no C44 . C47 . H471 . 109.4 no C44 . C47 . H472 . 109.3 no H471 . C47 . H472 . 109.5 no C44 . C47 . H473 . 109.8 no H471 . C47 . H473 . 109.5 no H472 . C47 . H473 . 109.5 no Mn2 . O48 . C49 . 124.0(5) yes Mn2 . O48 . H481 . 118.3 no C49 . O48 . H481 . 117.6 no O48 . C49 . H491 . 108.7 no O48 . C49 . H492 . 109.6 no H491 . C49 . H492 . 109.5 no O48 . C49 . H493 . 110.0 no H491 . C49 . H493 . 109.5 no H492 . C49 . H493 . 109.5 no Mn2 . O50 . C51 . 122.4(3) yes Mn2 . O50 . H501 . 119.0 no C51 . O50 . H501 . 118.6 no O50 . C51 . H511 . 108.7 no O50 . C51 . H512 . 110.1 no H511 . C51 . H512 . 109.5 no O50 . C51 . H513 . 109.6 no H511 . C51 . H513 . 109.5 no H512 . C51 . H513 . 109.5 no Mn3 . O52 . C53 . 128.8(4) yes Mn3 . O52 . H521 . 116.0 no C53 . O52 . H521 . 115.2 no O52 . C53 . H651 . 108.5 no O52 . C53 . H652 . 110.6 no H651 . C53 . H652 . 109.5 no O52 . C53 . H653 . 109.3 no H651 . C53 . H653 . 109.5 no H652 . C53 . H653 . 109.5 no