# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Euan Brechin' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Anna Collins' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Ross Inglis' '' '' 'Leigh F Jones' '' '' 'Georgios Karotsis' '' '' 'Simon Parsons' '' '' ; S.Perlepes ; '' '' 'Wolfgang Wernsdorfer' '' '' _publ_contact_author_name 'Euan Brechin' _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_section_title ; Enhancing SMM properties via axial distortion of MnIII3 clusters ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_address ; School of Chemistry, University of Edinburgh, Joseph Black Building, King's Buildings, West Mains Road, Edinburgh, EH9 3JJ , UK. ; _publ_contact_author_fax '+44 131 000000' _publ_contact_author_phone '+44 131 650 4806' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures will be sent by e-mail. ; # Attachment '_1_.cif' data_EB8037 _database_code_depnum_ccdc_archive 'CCDC 694668' _audit_creation_date 08-07-04 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8037 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.2285(7) _cell_length_b 13.7060(7) _cell_length_c 15.0998(8) _cell_angle_alpha 85.868(3) _cell_angle_beta 65.017(2) _cell_angle_gamma 62.085(2) _cell_volume 2165.7(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Re -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C35 H55 Mn3 N3 O17 Re1 # Dc = 1.75 Fooo = 1144.00 Mu = 37.13 M = 1140.82 # Found Formula = C35 H55 Mn3 N3 O17 Re1 # Dc = 1.75 FOOO = 1144.00 Mu = 37.13 M = 1140.82 _chemical_formula_sum 'C35 H55 Mn3 N3 O17 Re1' _chemical_formula_moiety 'C29 H37 Mn3 N3 O14 Re, 3(C2 H6 O)' _chemical_compound_source ? _chemical_formula_weight 1140.82 _cell_measurement_reflns_used 9837 _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 0.07 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 3.713 # Sheldrick geometric approximatio 0.44 0.77 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.77 _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 29075 _reflns_number_total 8837 _diffrn_reflns_av_R_equivalents 0.049 # Number of reflections with Friedels Law is 8837 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8859 _diffrn_reflns_theta_min 1.506 _diffrn_reflns_theta_max 26.372 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.372 _diffrn_measured_fraction_theta_full 0.998 _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 -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -14 _reflns_limit_h_max 16 _reflns_limit_k_min -16 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 1.23 _oxford_diffrn_Wilson_scale 115.95 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.36 _refine_diff_density_max 1.66 # 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 8801 _refine_ls_number_restraints 13 _refine_ls_number_parameters 532 _oxford_refine_ls_R_factor_ref 0.0466 _refine_ls_wR_factor_ref 0.0875 _refine_ls_goodness_of_fit_ref 0.8736 _refine_ls_shift/su_max 0.001135 # The values computed from all data _oxford_reflns_number_all 8801 _refine_ls_R_factor_all 0.0466 _refine_ls_wR_factor_all 0.0875 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7639 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_gt 0.0839 # 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^) + ( 0.00P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; 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 C1 C 0.1701(5) 0.7814(4) 0.2115(4) 0.0196 1.0000 Uani . . . . . . . C2 C 0.0868(5) 0.8504(4) 0.1723(4) 0.0234 1.0000 Uani . . . . . . . C3 C 0.0752(5) 0.8083(4) 0.0989(4) 0.0239 1.0000 Uani . . . . . . . C4 C 0.1473(5) 0.6944(4) 0.0624(4) 0.0247 1.0000 Uani . . . . . . . C5 C 0.2280(5) 0.6241(4) 0.1018(4) 0.0229 1.0000 Uani . . . . . . . C6 C 0.2410(5) 0.6648(4) 0.1762(3) 0.0187 1.0000 Uani . . . . . . . C7 C 0.3287(5) 0.5857(4) 0.2159(3) 0.0181 1.0000 Uani . . . . . . . C8 C 0.3708(5) 0.4637(4) 0.2011(4) 0.0241 1.0000 Uani . . . . . . . C9 C 0.5027(5) 0.3993(4) 0.1142(4) 0.0309 1.0000 Uani . . . . . . . C10 C 0.8237(5) 0.3597(4) 0.2020(3) 0.0189 1.0000 Uani . . . . . . . C11 C 0.8764(5) 0.2456(4) 0.1731(4) 0.0219 1.0000 Uani . . . . . . . C12 C 1.0022(5) 0.1807(4) 0.1059(4) 0.0280 1.0000 Uani . . . . . . . C13 C 1.0794(5) 0.2296(5) 0.0655(4) 0.0305 1.0000 Uani . . . . . . . C14 C 1.0306(5) 0.3417(5) 0.0952(4) 0.0302 1.0000 Uani . . . . . . . C15 C 0.9019(5) 0.4106(4) 0.1644(4) 0.0223 1.0000 Uani . . . . . . . C16 C 0.8593(5) 0.5270(4) 0.1983(3) 0.0190 1.0000 Uani . . . . . . . C17 C 0.9513(5) 0.5697(4) 0.1807(4) 0.0257 1.0000 Uani . . . . . . . C18 C 0.9938(6) 0.5508(5) 0.2616(5) 0.0365 1.0000 Uani . . . . . . . C19 C 0.6244(5) 0.9812(4) 0.2014(4) 0.0206 1.0000 Uani . . . . . . . C20 C 0.7295(5) 0.9981(4) 0.1637(4) 0.0234 1.0000 Uani . . . . . . . C21 C 0.7525(5) 1.0548(4) 0.0842(4) 0.0280 1.0000 Uani . . . . . . . C22 C 0.6708(5) 1.0934(4) 0.0391(4) 0.0265 1.0000 Uani . . . . . . . C23 C 0.5662(5) 1.0777(4) 0.0774(4) 0.0278 1.0000 Uani . . . . . . . C24 C 0.5374(5) 1.0230(4) 0.1590(4) 0.0192 1.0000 Uani . . . . . . . C25 C 0.4218(5) 1.0123(4) 0.1990(4) 0.0218 1.0000 Uani . . . . . . . C26 C 0.3092(5) 1.0878(4) 0.1799(4) 0.0265 1.0000 Uani . . . . . . . C27 C 0.2175(6) 1.1933(5) 0.2569(5) 0.0495 1.0000 Uani . . . . . . . C28 C 0.1202(5) 0.8764(5) 0.5085(4) 0.0308 1.0000 Uani . . . . . . . C29 C 0.0787(7) 0.8831(6) 0.6175(4) 0.0478 1.0000 Uani . . . . . . . C30 C 0.8102(6) 0.4457(5) 0.4620(5) 0.0396 1.0000 Uani . . . . . . . C31 C 0.8901(7) 0.4132(7) 0.5143(6) 0.0649 1.0000 Uani . . . . . . . C32 C 0.5615(8) 0.2334(5) 0.3371(5) 0.0473 1.0000 Uani D U . . . . . C33 C 0.4371(7) 0.2353(6) 0.3904(5) 0.0569 1.0000 Uani . U . . . . . C34 C 0.2147(8) 0.1348(7) 0.6054(6) 0.0723 1.0000 Uani . . . . . . . C35 C 0.1522(10) 0.1500(8) 0.5460(8) 0.0960 1.0000 Uani . . . . . . . O1 O 0.4945(3) 0.7219(3) 0.2803(2) 0.0175 1.0000 Uani . . . . . . . O2 O 0.1759(3) 0.8283(3) 0.2823(2) 0.0213 1.0000 Uani . . . . . . . O3 O 0.4497(3) 0.5460(3) 0.2986(2) 0.0191 1.0000 Uani . . . . . . . O4 O 0.7006(3) 0.4150(3) 0.2678(2) 0.0209 1.0000 Uani . . . . . . . O5 O 0.7036(3) 0.6988(3) 0.2907(3) 0.0214 1.0000 Uani . . . . . . . O6 O 0.6082(3) 0.9260(3) 0.2796(2) 0.0200 1.0000 Uani . . . . . . . O7 O 0.3045(3) 0.9313(3) 0.2952(3) 0.0200 1.0000 Uani . . . . . . . O8 O 0.6676(3) 0.7583(3) 0.1068(3) 0.0232 1.0000 Uani . . . . . . . O9 O 0.4488(3) 0.7628(3) 0.1098(3) 0.0243 1.0000 Uani . . . . . . . O10 O 0.6556(3) 0.5559(3) 0.1063(3) 0.0226 1.0000 Uani . . . . . . . O11 O 0.6843(4) 0.6646(3) -0.0595(3) 0.0266 1.0000 Uani . . . . . . . O12 O 0.2515(3) 0.7927(3) 0.4524(2) 0.0220 1.0000 Uani . . . . . . . O13 O 0.5433(3) 0.5766(3) 0.4343(2) 0.0218 1.0000 Uani . . . . . . . O14 O 0.4338(4) 0.8630(3) 0.4437(3) 0.0266 1.0000 Uani . . . . . . . O15 O 0.7111(3) 0.4158(3) 0.5029(3) 0.0260 1.0000 Uani . . . . . . . O16 O 0.5678(6) 0.3119(4) 0.3878(3) 0.0810 1.0000 Uani D U . . . . . O17 O 0.3333(4) 0.0429(3) 0.5744(4) 0.0495 1.0000 Uani . . . . . . . Re1 Re 0.613474(19) 0.685542(16) 0.066682(14) 0.0165 1.0000 Uani . . . . . . . Mn2 Mn 0.59199(7) 0.56784(6) 0.27955(5) 0.0151 1.0000 Uani . . . . . . . Mn3 Mn 0.55525(7) 0.81996(6) 0.28555(5) 0.0166 1.0000 Uani . . . . . . . N2 N 0.7377(4) 0.5947(3) 0.2501(3) 0.0183 1.0000 Uani . . . . . . . N3 N 0.4160(4) 0.9360(3) 0.2544(3) 0.0188 1.0000 Uani . . . . . . . Mn1 Mn 0.33127(7) 0.78190(6) 0.28410(5) 0.0166 1.0000 Uani . . . . . . . N1 N 0.3701(4) 0.6242(3) 0.2605(3) 0.0173 1.0000 Uani . . . . . . . H172 H 0.9090 0.6488 0.1792 0.0311 1.0000 Uiso R . . . . . . H171 H 1.0250 0.5323 0.1178 0.0310 1.0000 Uiso R . . . . . . H183 H 1.0475 0.5829 0.2510 0.0669 1.0000 Uiso R . . . . . . H182 H 0.9205 0.5849 0.3244 0.0668 1.0000 Uiso R . . . . . . H181 H 1.0397 0.4725 0.2620 0.0669 1.0000 Uiso R . . . . . . H111 H 0.8243 0.2128 0.2002 0.0256 1.0000 Uiso R . . . . . . H121 H 1.0345 0.1050 0.0876 0.0311 1.0000 Uiso R . . . . . . H131 H 1.1629 0.1877 0.0182 0.0310 1.0000 Uiso R . . . . . . H141 H 1.0841 0.3731 0.0682 0.0340 1.0000 Uiso R . . . . . . H201 H 0.7850 0.9713 0.1925 0.0279 1.0000 Uiso R . . . . . . H211 H 0.8227 1.0668 0.0603 0.0301 1.0000 Uiso R . . . . . . H221 H 0.6873 1.1294 -0.0153 0.0300 1.0000 Uiso R . . . . . . H231 H 0.5119 1.1050 0.0478 0.0320 1.0000 Uiso R . . . . . . H51 H 0.2752 0.5483 0.0779 0.0279 1.0000 Uiso R . . . . . . H41 H 0.1418 0.6656 0.0116 0.0328 1.0000 Uiso R . . . . . . H31 H 0.0179 0.8553 0.0750 0.0309 1.0000 Uiso R . . . . . . H21 H 0.0377 0.9266 0.1964 0.0283 1.0000 Uiso R . . . . . . H81 H 0.3749 0.4355 0.2605 0.0311 1.0000 Uiso R . . . . . . H82 H 0.3085 0.4529 0.1909 0.0309 1.0000 Uiso R . . . . . . H91 H 0.5274 0.3214 0.1079 0.0439 1.0000 Uiso R . . . . . . H92 H 0.5636 0.4096 0.1251 0.0439 1.0000 Uiso R . . . . . . H93 H 0.5001 0.4257 0.0545 0.0439 1.0000 Uiso R . . . . . . H281 H 0.1131 0.9479 0.4904 0.0330 1.0000 Uiso R . . . . . . H282 H 0.0658 0.8605 0.4923 0.0330 1.0000 Uiso R . . . . . . H291 H -0.0076 0.9419 0.6514 0.0579 1.0000 Uiso R . . . . . . H292 H 0.1330 0.8983 0.6341 0.0581 1.0000 Uiso R . . . . . . H293 H 0.0830 0.8140 0.6379 0.0580 1.0000 Uiso R . . . . . . H262 H 0.3397 1.1082 0.1150 0.0359 1.0000 Uiso R . . . . . . H261 H 0.2653 1.0474 0.1805 0.0355 1.0000 Uiso R . . . . . . H271 H 0.1465 1.2403 0.2432 0.0650 1.0000 Uiso R . . . . . . H273 H 0.2617 1.2327 0.2558 0.0649 1.0000 Uiso R . . . . . . H272 H 0.1876 1.1729 0.3207 0.0649 1.0000 Uiso R . . . . . . H302 H 0.7712 0.5261 0.4642 0.0461 1.0000 Uiso R . . . . . . H301 H 0.8648 0.4088 0.3939 0.0462 1.0000 Uiso R . . . . . . H311 H 0.9537 0.4366 0.4837 0.1058 1.0000 Uiso R . . . . . . H313 H 0.8372 0.4482 0.5819 0.1060 1.0000 Uiso R . . . . . . H312 H 0.9310 0.3336 0.5110 0.1061 1.0000 Uiso R . . . . . . H341 H 0.1614 0.1279 0.6698 0.0772 1.0000 Uiso R . . . . . . H342 H 0.2226 0.2005 0.6106 0.0773 1.0000 Uiso R . . . . . . H352 H 0.0725 0.2184 0.5721 0.1420 1.0000 Uiso R . . . . . . H351 H 0.1368 0.0883 0.5453 0.1420 1.0000 Uiso R . . . . . . H353 H 0.2059 0.1530 0.4801 0.1420 1.0000 Uiso R . . . . . . H355 H 0.2602 0.7332 0.4718 0.0314 1.0000 Uiso R . . . . . . H354 H 0.3662 0.0456 0.6090 0.0708 1.0000 Uiso R . . . . . . H151 H 0.6673 0.4443 0.5609 0.0370 1.0000 Uiso R . . . . . . H356 H 0.5044 0.6250 0.4825 0.0310 1.0000 Uiso R . . . . . . H357 H 0.3725 0.8540 0.4578 0.0430 1.0000 Uiso R . . . . . . H132 H 0.5879 0.5236 0.4529 0.0313 1.0000 Uiso R . . . . . . H142 H 0.4298 0.9081 0.4791 0.0435 1.0000 Uiso R . . . . . . H322 H 0.6280 0.1598 0.3336 0.0560 1.0000 Uiso R . . . . . . H321 H 0.5759 0.2493 0.2711 0.0560 1.0000 Uiso R . . . . . . H333 H 0.4339 0.1819 0.3551 0.0760 1.0000 Uiso R . . . . . . H331 H 0.4241 0.2180 0.4557 0.0758 1.0000 Uiso R . . . . . . H332 H 0.3699 0.3086 0.3960 0.0761 1.0000 Uiso R . . . . . . H161 H 0.6170 0.3323 0.3487 0.1109 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 C1 0.017(2) 0.022(2) 0.024(2) 0.006(2) -0.011(2) -0.012(2) C2 0.015(2) 0.020(2) 0.028(3) 0.001(2) -0.008(2) -0.006(2) C3 0.022(3) 0.028(3) 0.024(3) 0.010(2) -0.014(2) -0.010(2) C4 0.027(3) 0.032(3) 0.024(3) 0.007(2) -0.016(2) -0.017(2) C5 0.023(3) 0.025(3) 0.022(2) 0.003(2) -0.009(2) -0.014(2) C6 0.016(2) 0.019(2) 0.021(2) 0.0073(19) -0.009(2) -0.0082(19) C7 0.016(2) 0.018(2) 0.020(2) 0.0024(18) -0.007(2) -0.0086(19) C8 0.029(3) 0.018(2) 0.029(3) 0.009(2) -0.016(2) -0.012(2) C9 0.026(3) 0.019(3) 0.042(3) -0.006(2) -0.014(3) -0.006(2) C10 0.015(2) 0.018(2) 0.020(2) 0.0017(18) -0.009(2) -0.0033(19) C11 0.020(3) 0.021(2) 0.024(2) 0.007(2) -0.011(2) -0.010(2) C12 0.031(3) 0.017(2) 0.028(3) -0.001(2) -0.016(2) -0.002(2) C13 0.020(3) 0.026(3) 0.029(3) -0.004(2) -0.009(2) 0.000(2) C14 0.019(3) 0.031(3) 0.036(3) 0.004(2) -0.011(2) -0.010(2) C15 0.023(3) 0.022(2) 0.021(2) 0.005(2) -0.012(2) -0.008(2) C16 0.017(2) 0.020(2) 0.020(2) 0.0071(19) -0.009(2) -0.010(2) C17 0.020(3) 0.024(3) 0.033(3) 0.006(2) -0.011(2) -0.011(2) C18 0.036(3) 0.047(4) 0.047(4) 0.015(3) -0.027(3) -0.030(3) C19 0.021(2) 0.013(2) 0.023(2) -0.0015(18) -0.008(2) -0.0056(19) C20 0.024(3) 0.019(2) 0.027(3) 0.000(2) -0.011(2) -0.010(2) C21 0.029(3) 0.016(2) 0.029(3) 0.001(2) -0.007(2) -0.009(2) C22 0.030(3) 0.018(2) 0.023(3) 0.002(2) -0.006(2) -0.011(2) C23 0.031(3) 0.020(3) 0.026(3) 0.006(2) -0.014(2) -0.008(2) C24 0.021(2) 0.013(2) 0.022(2) 0.0015(18) -0.010(2) -0.0058(19) C25 0.029(3) 0.013(2) 0.025(3) 0.0025(19) -0.016(2) -0.008(2) C26 0.030(3) 0.023(3) 0.034(3) 0.011(2) -0.021(3) -0.013(2) C27 0.039(4) 0.033(3) 0.054(4) 0.000(3) -0.028(3) 0.007(3) C28 0.026(3) 0.027(3) 0.028(3) 0.000(2) -0.010(2) -0.006(2) C29 0.042(4) 0.045(4) 0.028(3) -0.003(3) -0.009(3) -0.005(3) C30 0.029(3) 0.043(4) 0.043(4) 0.011(3) -0.012(3) -0.020(3) C31 0.043(4) 0.079(6) 0.081(6) 0.026(5) -0.035(4) -0.030(4) C32 0.079(4) 0.025(3) 0.031(3) 0.002(2) -0.018(3) -0.025(3) C33 0.060(4) 0.051(4) 0.042(4) 0.005(3) -0.026(3) -0.010(4) C34 0.044(5) 0.082(6) 0.067(5) -0.018(5) -0.033(4) -0.002(4) C35 0.083(7) 0.086(7) 0.122(9) -0.004(6) -0.080(7) -0.010(6) O1 0.0171(17) 0.0133(15) 0.0232(17) 0.0031(13) -0.0107(15) -0.0067(13) O2 0.0174(17) 0.0204(17) 0.0244(18) -0.0005(14) -0.0118(15) -0.0050(14) O3 0.0180(17) 0.0147(16) 0.0254(18) 0.0074(13) -0.0133(15) -0.0057(14) O4 0.0190(18) 0.0143(16) 0.0237(18) 0.0045(13) -0.0080(15) -0.0052(14) O5 0.0224(18) 0.0150(16) 0.0310(19) 0.0020(14) -0.0166(16) -0.0076(14) O6 0.0244(18) 0.0182(16) 0.0237(17) 0.0059(14) -0.0145(16) -0.0119(15) O7 0.0177(17) 0.0141(16) 0.0287(18) 0.0031(14) -0.0117(15) -0.0067(14) O8 0.0251(19) 0.0185(17) 0.0270(18) 0.0034(14) -0.0119(16) -0.0108(15) O9 0.0255(19) 0.0202(17) 0.0297(19) 0.0062(15) -0.0165(17) -0.0093(15) O10 0.0247(19) 0.0182(17) 0.0245(18) -0.0008(14) -0.0110(16) -0.0094(15) O11 0.031(2) 0.0255(19) 0.0256(19) 0.0036(15) -0.0134(17) -0.0144(17) O12 0.0196(18) 0.0183(17) 0.0252(18) 0.0067(14) -0.0113(16) -0.0062(14) O13 0.0253(19) 0.0182(17) 0.0172(16) 0.0026(13) -0.0115(15) -0.0052(15) O14 0.028(2) 0.0283(19) 0.0262(19) -0.0007(15) -0.0131(17) -0.0138(17) O15 0.0236(19) 0.0254(19) 0.0240(18) 0.0072(15) -0.0085(16) -0.0103(16) O16 0.143(5) 0.063(3) 0.024(2) -0.010(2) 0.010(3) -0.079(3) O17 0.050(3) 0.035(2) 0.063(3) -0.014(2) -0.044(3) 0.000(2) Re1 0.01857(10) 0.01542(10) 0.01670(10) 0.00342(7) -0.00890(8) -0.00823(8) Mn2 0.0146(3) 0.0118(3) 0.0189(3) 0.0033(3) -0.0089(3) -0.0052(3) Mn3 0.0189(4) 0.0129(3) 0.0211(4) 0.0040(3) -0.0122(3) -0.0072(3) N2 0.022(2) 0.0153(19) 0.021(2) 0.0053(16) -0.0121(18) -0.0097(17) N3 0.020(2) 0.0163(19) 0.024(2) 0.0036(16) -0.0134(18) -0.0090(17) Mn1 0.0155(4) 0.0131(3) 0.0215(4) 0.0022(3) -0.0104(3) -0.0051(3) N1 0.015(2) 0.0142(19) 0.0192(19) 0.0019(15) -0.0070(17) -0.0044(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.096296(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 C1 . C2 . 1.397(7) yes C1 . C6 . 1.419(7) yes C1 . O2 . 1.334(6) yes C2 . C3 . 1.380(7) yes C2 . H21 . 0.930 no C3 . C4 . 1.391(7) yes C3 . H31 . 0.927 no C4 . C5 . 1.383(7) yes C4 . H41 . 0.932 no C5 . C6 . 1.394(7) yes C5 . H51 . 0.926 no C6 . C7 . 1.482(6) yes C7 . C8 . 1.495(6) yes C7 . N1 . 1.291(6) yes C8 . C9 . 1.528(7) yes C8 . H81 . 0.964 no C8 . H82 . 0.974 no C9 . H91 . 0.958 no C9 . H92 . 0.957 no C9 . H93 . 0.955 no C10 . C11 . 1.393(7) yes C10 . C15 . 1.415(7) yes C10 . O4 . 1.342(6) yes C11 . C12 . 1.381(7) yes C11 . H111 . 0.933 no C12 . C13 . 1.385(8) yes C12 . H121 . 0.929 no C13 . C14 . 1.381(7) yes C13 . H131 . 0.927 no C14 . C15 . 1.420(7) yes C14 . H141 . 0.932 no C15 . C16 . 1.467(7) yes C16 . C17 . 1.505(7) yes C16 . N2 . 1.305(6) yes C17 . C18 . 1.508(7) yes C17 . H172 . 0.964 no C17 . H171 . 0.967 no C18 . H183 . 0.956 no C18 . H182 . 0.959 no C18 . H181 . 0.954 no C19 . C20 . 1.388(7) yes C19 . C24 . 1.419(7) yes C19 . O6 . 1.349(6) yes C20 . C21 . 1.384(7) yes C20 . H201 . 0.925 no C21 . C22 . 1.395(8) yes C21 . H211 . 0.934 no C22 . C23 . 1.371(8) yes C22 . H221 . 0.926 no C23 . C24 . 1.402(7) yes C23 . H231 . 0.922 no C24 . C25 . 1.463(7) yes C25 . C26 . 1.500(7) yes C25 . N3 . 1.301(6) yes C26 . C27 . 1.524(8) yes C26 . H262 . 0.967 no C26 . H261 . 0.969 no C27 . H271 . 0.958 no C27 . H273 . 0.959 no C27 . H272 . 0.953 no C28 . C29 . 1.494(8) yes C28 . O12 . 1.443(6) yes C28 . H281 . 0.970 no C28 . H282 . 0.964 no C29 . H291 . 0.958 no C29 . H292 . 0.961 no C29 . H293 . 0.958 no C30 . C31 . 1.467(9) yes C30 . O15 . 1.432(7) yes C30 . H302 . 0.969 no C30 . H301 . 0.970 no C31 . H311 . 0.963 no C31 . H313 . 0.956 no C31 . H312 . 0.958 no C32 . C33 . 1.484(10) yes C32 . O16 . 1.417(7) yes C32 . H322 . 0.965 no C32 . H321 . 0.961 no C33 . H333 . 0.961 no C33 . H331 . 0.958 no C33 . H332 . 0.959 no C34 . C35 . 1.405(10) yes C34 . O17 . 1.372(8) yes C34 . H341 . 0.960 no C34 . H342 . 0.965 no C35 . H352 . 0.960 no C35 . H351 . 0.959 no C35 . H353 . 0.960 no O1 . Mn2 . 1.888(3) yes O1 . Mn3 . 1.881(3) yes O1 . Mn1 . 1.892(3) yes O2 . Mn1 . 1.857(3) yes O3 . Mn2 . 1.942(4) yes O3 . N1 . 1.398(5) yes O4 . Mn2 . 1.872(3) yes O5 . Mn3 . 1.916(3) yes O5 . N2 . 1.381(5) yes O6 . Mn3 . 1.869(3) yes O7 . N3 . 1.369(5) yes O7 . Mn1 . 1.915(3) yes O8 . Re1 . 1.731(4) yes O8 . Mn3 . 2.443(4) yes O9 . Re1 . 1.741(4) yes O9 . Mn1 . 2.382(4) yes O10 . Re1 . 1.740(3) yes O10 . Mn2 . 2.377(3) yes O11 . Re1 . 1.705(4) yes O12 . Mn1 . 2.288(3) yes O12 . H355 . 0.818 no O13 . Mn2 . 2.142(3) yes O13 . H356 . 0.818 no O13 . H132 . 0.815 no O14 . Mn3 . 2.170(4) yes O14 . H357 . 0.814 no O14 . H142 . 0.815 no O15 . H151 . 0.815 no O16 . H161 . 0.821 no O17 . H354 . 0.821 no Re1 . Mn2 . 3.4532(7) yes Re1 . Mn1 . 3.4805(8) yes Mn2 . N2 . 1.991(4) yes Mn2 . Mn1 . 3.2957(10) yes Mn3 . N3 . 2.006(4) yes Mn3 . Mn1 . 3.2490(11) yes Mn1 . N1 . 1.995(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . C6 . 118.4(5) yes C2 . C1 . O2 . 118.1(4) yes C6 . C1 . O2 . 123.4(4) yes C1 . C2 . C3 . 121.7(5) yes C1 . C2 . H21 . 119.3 no C3 . C2 . H21 . 119.1 no C2 . C3 . C4 . 119.8(5) yes C2 . C3 . H31 . 120.3 no C4 . C3 . H31 . 119.8 no C3 . C4 . C5 . 119.5(5) yes C3 . C4 . H41 . 120.5 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 121.6(5) yes C4 . C5 . H51 . 119.3 no C6 . C5 . H51 . 119.1 no C1 . C6 . C5 . 118.9(4) yes C1 . C6 . C7 . 121.7(4) yes C5 . C6 . C7 . 119.3(4) yes C6 . C7 . C8 . 120.1(4) yes C6 . C7 . N1 . 118.6(4) yes C8 . C7 . N1 . 121.3(4) yes C7 . C8 . C9 . 111.6(4) yes C7 . C8 . H81 . 107.6 no C9 . C8 . H81 . 108.5 no C7 . C8 . H82 . 109.8 no C9 . C8 . H82 . 110.4 no H81 . C8 . H82 . 108.8 no C8 . C9 . H91 . 109.3 no C8 . C9 . H92 . 110.0 no H91 . C9 . H92 . 109.6 no C8 . C9 . H93 . 109.6 no H91 . C9 . H93 . 108.8 no H92 . C9 . H93 . 109.4 no C11 . C10 . C15 . 119.4(4) yes C11 . C10 . O4 . 117.4(5) yes C15 . C10 . O4 . 123.2(4) yes C10 . C11 . C12 . 122.1(5) yes C10 . C11 . H111 . 118.3 no C12 . C11 . H111 . 119.6 no C11 . C12 . C13 . 119.5(5) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 120.4 no C12 . C13 . C14 . 119.5(5) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 122.3(5) yes C13 . C14 . H141 . 118.5 no C15 . C14 . H141 . 119.1 no C14 . C15 . C10 . 117.1(5) yes C14 . C15 . C16 . 119.3(5) yes C10 . C15 . C16 . 123.5(5) yes C15 . C16 . C17 . 122.4(4) yes C15 . C16 . N2 . 119.1(5) yes C17 . C16 . N2 . 118.4(4) yes C16 . C17 . C18 . 111.6(4) yes C16 . C17 . H172 . 108.3 no C18 . C17 . H172 . 108.8 no C16 . C17 . H171 . 109.5 no C18 . C17 . H171 . 109.3 no H172 . C17 . H171 . 109.3 no C17 . C18 . H183 . 109.9 no C17 . C18 . H182 . 109.5 no H183 . C18 . H182 . 109.3 no C17 . C18 . H181 . 109.9 no H183 . C18 . H181 . 109.2 no H182 . C18 . H181 . 109.0 no C20 . C19 . C24 . 120.1(5) yes C20 . C19 . O6 . 117.5(5) yes C24 . C19 . O6 . 122.3(5) yes C19 . C20 . C21 . 121.2(5) yes C19 . C20 . H201 . 119.3 no C21 . C20 . H201 . 119.5 no C20 . C21 . C22 . 119.8(5) yes C20 . C21 . H211 . 120.4 no C22 . C21 . H211 . 119.8 no C21 . C22 . C23 . 118.8(5) yes C21 . C22 . H221 . 120.0 no C23 . C22 . H221 . 121.2 no C22 . C23 . C24 . 123.5(5) yes C22 . C23 . H231 . 118.1 no C24 . C23 . H231 . 118.4 no C19 . C24 . C23 . 116.5(5) yes C19 . C24 . C25 . 122.3(4) yes C23 . C24 . C25 . 121.2(5) yes C24 . C25 . C26 . 122.2(4) yes C24 . C25 . N3 . 118.7(5) yes C26 . C25 . N3 . 119.1(5) yes C25 . C26 . C27 . 111.7(5) yes C25 . C26 . H262 . 108.5 no C27 . C26 . H262 . 109.3 no C25 . C26 . H261 . 108.9 no C27 . C26 . H261 . 109.8 no H262 . C26 . H261 . 108.5 no C26 . C27 . H271 . 110.3 no C26 . C27 . H273 . 109.2 no H271 . C27 . H273 . 109.9 no C26 . C27 . H272 . 109.1 no H271 . C27 . H272 . 109.4 no H273 . C27 . H272 . 108.9 no C29 . C28 . O12 . 112.4(5) yes C29 . C28 . H281 . 108.2 no O12 . C28 . H281 . 107.2 no C29 . C28 . H282 . 109.2 no O12 . C28 . H282 . 109.8 no H281 . C28 . H282 . 110.0 no C28 . C29 . H291 . 109.3 no C28 . C29 . H292 . 109.7 no H291 . C29 . H292 . 109.6 no C28 . C29 . H293 . 110.1 no H291 . C29 . H293 . 108.8 no H292 . C29 . H293 . 109.4 no C31 . C30 . O15 . 113.8(5) yes C31 . C30 . H302 . 108.6 no O15 . C30 . H302 . 108.3 no C31 . C30 . H301 . 108.0 no O15 . C30 . H301 . 108.3 no H302 . C30 . H301 . 109.8 no C30 . C31 . H311 . 109.5 no C30 . C31 . H313 . 108.8 no H311 . C31 . H313 . 110.1 no C30 . C31 . H312 . 109.2 no H311 . C31 . H312 . 109.5 no H313 . C31 . H312 . 109.7 no C33 . C32 . O16 . 111.2(6) yes C33 . C32 . H322 . 108.4 no O16 . C32 . H322 . 108.2 no C33 . C32 . H321 . 110.9 no O16 . C32 . H321 . 109.1 no H322 . C32 . H321 . 109.0 no C32 . C33 . H333 . 110.4 no C32 . C33 . H331 . 110.4 no H333 . C33 . H331 . 109.3 no C32 . C33 . H332 . 109.2 no H333 . C33 . H332 . 109.2 no H331 . C33 . H332 . 108.4 no C35 . C34 . O17 . 116.3(7) yes C35 . C34 . H341 . 106.9 no O17 . C34 . H341 . 107.5 no C35 . C34 . H342 . 108.6 no O17 . C34 . H342 . 108.2 no H341 . C34 . H342 . 109.0 no C34 . C35 . H352 . 109.6 no C34 . C35 . H351 . 109.3 no H352 . C35 . H351 . 109.6 no C34 . C35 . H353 . 108.5 no H352 . C35 . H353 . 110.0 no H351 . C35 . H353 . 109.8 no Mn2 . O1 . Mn3 . 119.69(17) yes Mn2 . O1 . Mn1 . 121.33(17) yes Mn3 . O1 . Mn1 . 118.86(16) yes C1 . O2 . Mn1 . 120.4(3) yes Mn2 . O3 . N1 . 113.1(3) yes C10 . O4 . Mn2 . 124.8(3) yes Mn3 . O5 . N2 . 115.0(3) yes C19 . O6 . Mn3 . 120.1(3) yes N3 . O7 . Mn1 . 112.8(3) yes Re1 . O8 . Mn3 . 113.27(17) yes Re1 . O9 . Mn1 . 114.26(17) yes Re1 . O10 . Mn2 . 113.12(16) yes C28 . O12 . Mn1 . 115.9(3) yes C28 . O12 . H355 . 107.9 no Mn1 . O12 . H355 . 113.9 no Mn2 . O13 . H356 . 137.6 no Mn2 . O13 . H132 . 118.3 no H356 . O13 . H132 . 101.0 no Mn3 . O14 . H357 . 111.0 no Mn3 . O14 . H142 . 122.9 no H357 . O14 . H142 . 120.3 no C30 . O15 . H151 . 108.4 no C32 . O16 . H161 . 110.2 no C34 . O17 . H354 . 109.3 no O9 . Re1 . O10 . 110.33(17) yes O9 . Re1 . O8 . 110.15(16) yes O10 . Re1 . O8 . 110.52(16) yes O9 . Re1 . O11 . 109.19(17) yes O10 . Re1 . O11 . 108.50(16) yes O8 . Re1 . O11 . 108.08(17) yes O9 . Re1 . Mn2 . 93.41(12) yes O10 . Re1 . Mn2 . 39.27(11) yes O8 . Re1 . Mn2 . 84.99(11) yes O11 . Re1 . Mn2 . 147.00(12) yes O9 . Re1 . Mn1 . 38.60(12) yes O10 . Re1 . Mn1 . 85.71(11) yes O8 . Re1 . Mn1 . 93.18(12) yes O11 . Re1 . Mn1 . 147.31(13) yes Mn2 . Re1 . Mn1 . 56.757(17) yes O13 . Mn2 . O10 . 177.39(13) yes O13 . Mn2 . O3 . 92.06(14) yes O10 . Mn2 . O3 . 90.36(13) yes O13 . Mn2 . O1 . 97.40(13) yes O10 . Mn2 . O1 . 83.57(13) yes O3 . Mn2 . O1 . 90.05(14) yes O13 . Mn2 . O4 . 86.65(14) yes O10 . Mn2 . O4 . 92.23(13) yes O3 . Mn2 . O4 . 93.30(15) yes O1 . Mn2 . O4 . 174.65(15) yes O13 . Mn2 . Re1 . 152.72(9) yes O10 . Mn2 . Re1 . 27.60(8) yes O3 . Mn2 . Re1 . 96.10(10) yes O1 . Mn2 . Re1 . 56.73(10) yes O4 . Mn2 . Re1 . 118.68(11) yes O13 . Mn2 . N2 . 92.14(15) yes O10 . Mn2 . N2 . 85.48(14) yes O3 . Mn2 . N2 . 175.45(15) yes O1 . Mn2 . N2 . 87.66(15) yes O4 . Mn2 . N2 . 88.71(16) yes O13 . Mn2 . Mn1 . 100.39(9) yes O10 . Mn2 . Mn1 . 81.65(9) yes O3 . Mn2 . Mn1 . 60.85(9) yes O1 . Mn2 . Mn1 . 29.37(10) yes O4 . Mn2 . Mn1 . 153.18(12) yes Re1 . Mn2 . N2 . 79.36(11) yes Re1 . Mn2 . Mn1 . 62.039(18) yes N2 . Mn2 . Mn1 . 116.56(11) yes O14 . Mn3 . O8 . 169.64(14) yes O14 . Mn3 . O5 . 97.09(14) yes O8 . Mn3 . O5 . 86.21(13) yes O14 . Mn3 . O1 . 88.53(14) yes O8 . Mn3 . O1 . 81.59(13) yes O5 . Mn3 . O1 . 90.82(14) yes O14 . Mn3 . O6 . 95.22(14) yes O8 . Mn3 . O6 . 94.29(13) yes O5 . Mn3 . O6 . 94.63(15) yes O1 . Mn3 . O6 . 172.95(14) yes O14 . Mn3 . N3 . 92.83(15) yes O8 . Mn3 . N3 . 83.59(14) yes O5 . Mn3 . N3 . 169.78(16) yes O1 . Mn3 . N3 . 86.98(15) yes O6 . Mn3 . N3 . 86.87(16) yes O14 . Mn3 . Mn1 . 82.58(10) yes O8 . Mn3 . Mn1 . 87.31(9) yes O5 . Mn3 . Mn1 . 121.36(11) yes O1 . Mn3 . Mn1 . 30.67(10) yes O6 . Mn3 . Mn1 . 143.98(11) yes N3 . Mn3 . Mn1 . 57.50(12) yes O5 . N2 . Mn2 . 114.6(3) yes O5 . N2 . C16 . 116.9(4) yes Mn2 . N2 . C16 . 128.5(3) yes O7 . N3 . Mn3 . 115.2(3) yes O7 . N3 . C25 . 117.7(4) yes Mn3 . N3 . C25 . 127.1(4) yes O12 . Mn1 . O9 . 169.81(13) yes O12 . Mn1 . O7 . 90.17(14) yes O9 . Mn1 . O7 . 88.50(13) yes O12 . Mn1 . O1 . 87.35(13) yes O9 . Mn1 . O1 . 82.60(13) yes O7 . Mn1 . O1 . 91.71(14) yes O12 . Mn1 . O2 . 94.58(14) yes O9 . Mn1 . O2 . 95.57(14) yes O7 . Mn1 . O2 . 93.01(15) yes O1 . Mn1 . O2 . 174.89(14) yes O12 . Mn1 . Mn3 . 88.31(9) yes O9 . Mn1 . Mn3 . 82.20(9) yes O7 . Mn1 . Mn3 . 61.25(10) yes O1 . Mn1 . Mn3 . 30.47(10) yes O2 . Mn1 . Mn3 . 154.15(11) yes O12 . Mn1 . Mn2 . 85.17(9) yes O9 . Mn1 . Mn2 . 86.85(9) yes O7 . Mn1 . Mn2 . 120.88(11) yes O1 . Mn1 . Mn2 . 29.30(10) yes O2 . Mn1 . Mn2 . 146.09(11) yes O12 . Mn1 . Re1 . 143.15(9) yes O9 . Mn1 . Re1 . 27.14(8) yes O7 . Mn1 . Re1 . 94.50(10) yes O1 . Mn1 . Re1 . 56.03(10) yes O2 . Mn1 . Re1 . 121.56(11) yes O12 . Mn1 . N1 . 94.42(14) yes O9 . Mn1 . N1 . 86.66(14) yes O7 . Mn1 . N1 . 175.07(15) yes O1 . Mn1 . N1 . 86.72(15) yes O2 . Mn1 . N1 . 88.41(16) yes Mn3 . Mn1 . Mn2 . 59.72(2) yes Mn3 . Mn1 . Re1 . 62.733(19) yes Mn2 . Mn1 . Re1 . 61.203(18) yes Mn3 . Mn1 . N1 . 117.02(12) yes Mn2 . Mn1 . N1 . 57.90(12) yes Re1 . Mn1 . N1 . 80.75(11) yes O3 . N1 . Mn1 . 116.2(3) yes O3 . N1 . C7 . 115.9(4) yes Mn1 . N1 . C7 . 127.9(3) yes # Attachment 'new (2).cif' data_eb7029 _database_code_depnum_ccdc_archive 'CCDC 694669' _audit_creation_date 07-02-28 _audit_creation_method CRYSTALS_ver_12.84 _chemical_formula_moiety 'C30 H39 Cl1 Mn3 N3 O14' _chemical_compound_source 'Costas Milios, CM3009' _exptl_crystal_recrystallization_method 'evaporation of MeOH' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.3784(3) _cell_length_b 13.3784(3) _cell_length_c 34.0617(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5279.7(2) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/3,y+2/3,z+2/3 -x+1/3,-y+2/3,-z+2/3 x+2/3,y+1/3,z+1/3 -x+2/3,-y+1/3,-z+1/3 -y,x-y,z y,-x+y,-z -y+1/3,x-y+2/3,z+2/3 y+1/3,-x+y+2/3,-z+2/3 -y+2/3,x-y+1/3,z+1/3 y+2/3,-x+y+1/3,-z+1/3 -x+y,-x,z x-y,x,-z -x+y+1/3,-x+2/3,z+2/3 x-y+1/3,x+2/3,-z+2/3 -x+y+2/3,-x+1/3,z+1/3 x-y+2/3,x+1/3,-z+1/3 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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' 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' _cell_formula_units_Z 6 # Given Formula = C36 H30 Cl3 Mn3 N3 O6 # Dc = 1.65 Fooo = 2664.00 Mu = 13.39 M = 290.60 # Found Formula = C30 H39 Cl1 Mn3 N3 O14 # Dc = 1.63 FOOO = 2664.00 Mu = 12.07 M = 288.63 _chemical_formula_sum 'C30 H39 Cl1 Mn3 N3 O14' _chemical_formula_weight 865.89 _cell_measurement_reflns_used 9243 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 30.45 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.17 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 1.207 # Sheldrick geometric approximatio 0.69 0.81 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.81 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 63184 _reflns_number_total 3607 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections with Friedels Law is 3607 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3601 _diffrn_reflns_theta_min 1.794 _diffrn_reflns_theta_max 30.569 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.569 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 46 _reflns_limit_h_min -19 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 48 _oxford_diffrn_Wilson_B_factor 1.29 _oxford_diffrn_Wilson_scale 31.46 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.37 _refine_diff_density_max 0.62 _refine_ls_number_reflns 3606 _refine_ls_number_restraints 0 _refine_ls_number_parameters 154 #_refine_ls_R_factor_ref 0.0387 _refine_ls_wR_factor_ref 0.0679 _refine_ls_goodness_of_fit_ref 0.8547 #_reflns_number_all 3606 _refine_ls_R_factor_all 0.0387 _refine_ls_wR_factor_all 0.0679 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2879 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_gt 0.0660 _refine_ls_shift/su_max 0.000893 # 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 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; The structure consists of an Mn~3~ complex and a ClO~4~^-^ counterion. Each Mn has bound a molecule of MeOH solvent, and there are three Et-SnO^-^ ions in the complex. The central O^2-^ ion and the Cl atom are located on the 3-fold axis. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. 701_ALERT_1_B Bond Calc 1.8785(3), Rep 1.8777(3), Dev.. 2.67 Sigma MN1 -O2 1.555 1.555 702_ALERT_1_B Angle Calc 30.45(1), Rep 30.43(1), Dev.. 2.30 Sigma O2 -MN1 -MN1 13.665 1.555 13.665 701_ALERT_1_C Bond Calc 1.8785(3), Rep 1.8790(3), Dev.. 1.67 Sigma MN1 -O2 1.555 7.655 702_ALERT_1_C Angle Calc 30.45(1), Rep 30.47(1), Dev.. 1.70 Sigma O2 -MN1 -MN1 7.655 1.555 13.665 702_ALERT_1_C Angle Calc 119.10(2), Rep 119.06(2), Dev.. 1.90 Sigma MN1 -O2 -MN1 13.665 1.555 7.655 702_ALERT_1_C Angle Calc 119.10(2), Rep 119.13(2), Dev.. 1.30 Sigma MN1 -O2 -MN1 7.655 1.555 1.555 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 0.03 Deg. CL17 -O18 -CL17 13.665 1.555 1.555 Atoms Cl17 and O2 are located on crystallographic special positions, which places restraints on the bond distances and angles. These restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif can be badly in error. #=============================================================================== 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.79 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay, changes in the volume of the crystal illuminated, etc. 152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? No action taken 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 14 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 1240 1240 0 23.01 0.550 1.000 1641 1641 0 25.24 0.600 1.000 2124 2124 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 2705 2705 0 29.84 0.700 0.999 3390 3387 3 30.57 0.716 0.996 3621 3607 14 ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mn1 Mn 0.606667(19) 0.433088(18) 0.550692(6) 0.0146 1.0000 Uani . . . . . . O2 O 0.6666 0.3334 0.54543(5) 0.0150 1.0000 Uani S T . . . . N3 N 0.76469(10) 0.55874(10) 0.56448(4) 0.0164 1.0000 Uani . . . . . . O4 O 0.85280(9) 0.54679(9) 0.54859(3) 0.0185 1.0000 Uani . . . . . . C5 C 0.79422(13) 0.64404(13) 0.58889(4) 0.0188 1.0000 Uani . . . . . . C6 C 0.70622(13) 0.66942(13) 0.60378(4) 0.0189 1.0000 Uani . . . . . . C7 C 0.59366(13) 0.61918(12) 0.58771(4) 0.0176 1.0000 Uani . . . . . . O8 O 0.55578(9) 0.53948(9) 0.55925(3) 0.0192 1.0000 Uani . . . . . . C9 C 0.51809(14) 0.65566(14) 0.60098(5) 0.0218 1.0000 Uani . . . . . . C10 C 0.55034(15) 0.73790(15) 0.62991(5) 0.0255 1.0000 Uani . . . . . . C11 C 0.65875(16) 0.78525(15) 0.64694(5) 0.0280 1.0000 Uani . . . . . . C12 C 0.73528(15) 0.75200(14) 0.63391(5) 0.0254 1.0000 Uani . . . . . . C13 C 0.91929(14) 0.71829(14) 0.59939(5) 0.0281 1.0000 Uani . . . . . . C14 C 0.97776(16) 0.82052(16) 0.57180(7) 0.0432 1.0000 Uani . . . . . . O15 O 0.61451(10) 0.47024(10) 0.48774(3) 0.0226 1.0000 Uani . . . . . . C16 C 0.70979(16) 0.57643(17) 0.47390(5) 0.0337 1.0000 Uani . . . . . . Cl17 Cl 0.6666 0.3334 0.637729(18) 0.0182 1.0000 Uani S T . . . . O18 O 0.60017(9) 0.38459(10) 0.62337(3) 0.0216 1.0000 Uani . . . . . . O19 O 0.6666 0.3334 0.67976(6) 0.0282 1.0000 Uani S T . . . . H91 H 0.4478 0.6242 0.5901 0.0278 1.0000 Uiso R . . . . . H101 H 0.4984 0.7615 0.6383 0.0329 1.0000 Uiso R . . . . . H111 H 0.6784 0.8405 0.6664 0.0322 1.0000 Uiso R . . . . . H121 H 0.8078 0.7849 0.6456 0.0295 1.0000 Uiso R . . . . . H131 H 0.9268 0.7434 0.6270 0.0339 1.0000 Uiso R . . . . . H132 H 0.9568 0.6721 0.5970 0.0319 1.0000 Uiso R . . . . . H141 H 1.0619 0.8659 0.5763 0.0635 1.0000 Uiso R . . . . . H142 H 0.9504 0.8773 0.5759 0.0645 1.0000 Uiso R . . . . . H143 H 0.9653 0.7991 0.5440 0.0615 1.0000 Uiso R . . . . . H10 H 0.7068 0.5799 0.4457 0.0486 1.0000 Uiso R . . . . . H13 H 0.7814 0.5814 0.4812 0.0486 1.0000 Uiso R . . . . . H16 H 0.7049 0.6398 0.4861 0.0503 1.0000 Uiso R . . . . . H1 H 0.5584 0.4584 0.4756 0.0358 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 0.01359(11) 0.01318(11) 0.01765(11) -0.00099(8) -0.00086(8) 0.00707(9) O2 0.0134(5) 0.0134(5) 0.0180(9) 0.0000 0.0000 0.0067(2) N3 0.0150(6) 0.0158(6) 0.0190(6) 0.0008(5) 0.0007(5) 0.0081(5) O4 0.0154(5) 0.0156(5) 0.0255(6) 0.0005(4) 0.0025(4) 0.0085(4) C5 0.0181(7) 0.0164(7) 0.0213(7) -0.0007(6) -0.0023(6) 0.0082(6) C6 0.0207(7) 0.0159(7) 0.0198(7) -0.0013(6) -0.0004(6) 0.0089(6) C7 0.0222(7) 0.0150(7) 0.0165(7) 0.0009(5) 0.0006(6) 0.0099(6) O8 0.0203(5) 0.0188(5) 0.0222(5) -0.0061(4) -0.0049(4) 0.0125(4) C9 0.0231(8) 0.0233(8) 0.0225(8) -0.0009(6) -0.0005(6) 0.0142(7) C10 0.0319(9) 0.0266(8) 0.0240(8) -0.0002(7) 0.0051(7) 0.0190(7) C11 0.0343(9) 0.0251(8) 0.0244(8) -0.0074(7) 0.0010(7) 0.0146(8) C12 0.0253(8) 0.0237(8) 0.0248(8) -0.0060(6) -0.0028(6) 0.0105(7) C13 0.0201(8) 0.0259(8) 0.0366(10) -0.0124(7) -0.0067(7) 0.0103(7) C14 0.0238(9) 0.0229(9) 0.0792(17) 0.0026(10) 0.0061(10) 0.0088(8) O15 0.0235(6) 0.0265(6) 0.0193(5) 0.0019(4) -0.0026(4) 0.0136(5) C16 0.0272(9) 0.0410(11) 0.0282(9) 0.0133(8) 0.0038(7) 0.0137(8) Cl17 0.01934(18) 0.01934(18) 0.0159(3) 0.0000 0.0000 0.00967(9) O18 0.0222(6) 0.0240(6) 0.0228(6) 0.0005(4) 0.0008(4) 0.0148(5) O19 0.0345(7) 0.0345(7) 0.0156(9) 0.0000 0.0000 0.0172(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.17140(6) 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 . O4 7_655 1.9026(10) yes Mn1 . O2 7_655 1.8790(3) yes Mn1 . O2 13_665 1.8788(3) yes Mn1 . Mn1 13_665 3.2388(4) yes Mn1 . O2 . 1.8777(3) yes Mn1 . N3 . 1.9904(12) yes Mn1 . O8 . 1.8823(10) yes Mn1 . O15 . 2.1917(11) yes Mn1 . O18 . 2.5497(11) yes N3 . O4 . 1.3771(15) yes N3 . C5 . 1.3035(19) yes C5 . C6 . 1.469(2) yes C5 . C13 . 1.501(2) yes C6 . C7 . 1.417(2) yes C6 . C12 . 1.413(2) yes C7 . O8 . 1.3393(17) yes C7 . C9 . 1.399(2) yes C9 . C10 . 1.376(2) yes C9 . H91 . 0.896 no C10 . C11 . 1.387(2) yes C10 . H101 . 0.941 no C11 . C12 . 1.378(2) yes C11 . H111 . 0.929 no C12 . H121 . 0.931 no C13 . C14 . 1.515(3) yes C13 . H131 . 0.988 no C13 . H132 . 0.975 no C14 . H141 . 0.988 no C14 . H142 . 1.005 no C14 . H143 . 0.978 no O15 . C16 . 1.433(2) yes O15 . H1 . 0.801 no C16 . H10 . 0.963 no C16 . H13 . 0.959 no C16 . H16 . 0.975 no Cl17 . O18 7_655 1.4533(11) yes Cl17 . O18 13_665 1.4532(11) yes Cl17 . O19 7_655 1.432(2) yes Cl17 . O18 . 1.4521(11) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O4 7_655 Mn1 . O2 7_655 90.84(3) yes O4 7_655 Mn1 . O2 13_665 90.88(3) yes O2 7_655 Mn1 . O2 13_665 0.040 yes O4 7_655 Mn1 . Mn1 13_665 121.05(3) yes O2 7_655 Mn1 . Mn1 13_665 30.467(9) yes O2 13_665 Mn1 . Mn1 13_665 30.427(9) yes O4 7_655 Mn1 . O2 . 90.86(3) yes O2 7_655 Mn1 . O2 . 0.016 yes O2 13_665 Mn1 . O2 . 0.025 yes Mn1 13_665 Mn1 . O2 . 30.453(9) yes O4 7_655 Mn1 . N3 . 168.36(5) yes O2 7_655 Mn1 . N3 . 88.40(4) yes O2 13_665 Mn1 . N3 . 88.36(4) yes Mn1 13_665 Mn1 . N3 . 58.04(4) yes O2 . Mn1 . N3 . 88.39(4) yes O4 7_655 Mn1 . O8 . 92.57(5) yes O2 7_655 Mn1 . O8 . 175.24(5) yes O2 13_665 Mn1 . O8 . 175.21(5) yes Mn1 13_665 Mn1 . O8 . 145.63(3) yes O2 . Mn1 . O8 . 175.23(5) yes O4 7_655 Mn1 . O15 . 94.23(4) yes O2 7_655 Mn1 . O15 . 94.53(6) yes O2 13_665 Mn1 . O15 . 94.52(6) yes Mn1 13_665 Mn1 . O15 . 95.33(3) yes O2 . Mn1 . O15 . 94.52(6) yes O4 7_655 Mn1 . O18 . 85.70(4) yes O2 7_655 Mn1 . O18 . 83.34(6) yes O2 13_665 Mn1 . O18 . 83.35(6) yes Mn1 13_665 Mn1 . O18 . 82.90(2) yes O2 . Mn1 . O18 . 83.35(6) yes N3 . Mn1 . O8 . 87.59(5) yes N3 . Mn1 . O15 . 97.42(5) yes O8 . Mn1 . O15 . 88.53(5) yes N3 . Mn1 . O18 . 82.67(4) yes O8 . Mn1 . O18 . 93.61(4) yes O15 . Mn1 . O18 . 177.86(4) yes Mn1 13_665 O2 . Mn1 7_655 119.062(17) yes Mn1 13_665 O2 . Mn1 . 119.117(17) yes Mn1 7_655 O2 . Mn1 . 119.126(17) yes Mn1 . N3 . O4 . 114.74(9) yes Mn1 . N3 . C5 . 128.23(11) yes O4 . N3 . C5 . 116.75(12) yes N3 . O4 . Mn1 13_665 113.75(8) yes N3 . C5 . C6 . 119.70(13) yes N3 . C5 . C13 . 118.75(14) yes C6 . C5 . C13 . 121.47(13) yes C5 . C6 . C7 . 122.80(13) yes C5 . C6 . C12 . 119.51(14) yes C7 . C6 . C12 . 117.60(14) yes C6 . C7 . O8 . 123.14(13) yes C6 . C7 . C9 . 119.46(14) yes O8 . C7 . C9 . 117.37(14) yes C7 . O8 . Mn1 . 125.32(9) yes C7 . C9 . C10 . 121.19(15) yes C7 . C9 . H91 . 118.4 no C10 . C9 . H91 . 120.4 no C9 . C10 . C11 . 120.21(15) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.9 no C10 . C11 . C12 . 119.60(15) yes C10 . C11 . H111 . 118.6 no C12 . C11 . H111 . 121.8 no C6 . C12 . C11 . 121.88(16) yes C6 . C12 . H121 . 119.6 no C11 . C12 . H121 . 118.5 no C5 . C13 . C14 . 110.56(15) yes C5 . C13 . H131 . 110.0 no C14 . C13 . H131 . 111.4 no C5 . C13 . H132 . 108.5 no C14 . C13 . H132 . 108.9 no H131 . C13 . H132 . 107.3 no C13 . C14 . H141 . 111.9 no C13 . C14 . H142 . 112.2 no H141 . C14 . H142 . 104.4 no C13 . C14 . H143 . 113.6 no H141 . C14 . H143 . 107.8 no H142 . C14 . H143 . 106.4 no Mn1 . O15 . C16 . 117.68(10) yes Mn1 . O15 . H1 . 121.8 no C16 . O15 . H1 . 107.9 no O15 . C16 . H10 . 109.7 no O15 . C16 . H13 . 110.2 no H10 . C16 . H13 . 108.6 no O15 . C16 . H16 . 108.0 no H10 . C16 . H16 . 111.1 no H13 . C16 . H16 . 109.2 no O18 7_655 Cl17 . O18 13_665 109.23(5) yes O18 7_655 Cl17 . O19 7_655 109.62(5) yes O18 13_665 Cl17 . O19 7_655 109.67(5) yes O18 7_655 Cl17 . O18 . 109.29(5) yes O18 13_665 Cl17 . O18 . 109.29(5) yes O19 7_655 Cl17 . O18 . 109.72(5) yes Mn1 . O18 . Cl17 13_665 119.72(6) yes Mn1 . O18 . Cl17 . 119.74(6) yes Cl17 13_665 O18 . Cl17 . 0.028 yes