# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 # start Validation Reply Form _vrf_PUBL024_GLOBAL ; PROBLEM: The number of authors is greater than 5. RESPONSE: The authors from Leiden Institute of Chemistry are resposible for chemistry, from the University of Helsinki and Radboud University Nijmegen responsible for crystallography and from Leiden Institute of Physics for the physical measurements. ; # end Validation Reply Form # 1. SUBMISSION DETAILS _publ_contact_author ; 'Reedijk, Jan' ; _publ_contact_author_phone +31715274450 _publ_contact_author_fax ? _publ_contact_author_email reedijk@chem.leidenuniv.nl _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission as an X-ray deposition file of a compound coded mgm20.cif ; #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Supramolecular interactions stabilizing mononuclear and dinuclear manganese compounds containing phenol-pyrazole ligands ; loop_ _publ_author_name _publ_author_address M.Viciano-Chumillas ; Leiden Institute of Chemistry, Leiden University, P.O. Box 9502, 2300 RA, Leiden The Netherlands Current address: Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay, CNRD, Universi\'e Paris-Sud, 91405 Orsay, France ; M.Gimenez-Marques ; Leiden Institute of Chemistry, Leiden University, P.O. Box 9502, 2300 RA, Leiden The Netherlands ; S.Tanase ; Leiden Institute of Chemistry, Leiden University, P.O. Box 9502, 2300 RA, Leiden The Netherlands Current address: : Van 't Hoff Institute for Molecular Sciences, University of Amsterdam, Science Park 904, 1098 XH Amsterdam, The Netherlands. ; I.Mutikainen ; University of Helsinki Department of Chemistry Laboratory of Inorganic Chemistry FIN-00014 Helsinki Finland ; ; U.Turpeinen ; ; University of Helsinki Department of Chemistry Laboratory of Inorganic Chemistry FIN-00014 Helsinki Finland ; J.M.M.Smits ; Solid State Chemistry, Institute for Molecules and Materials, Radboud University Nijmegen, Heijendaalseweg 135, 6525 AJ Nijmegen, The Netherlands ; 'R.de Gelder' ; Solid State Chemistry, Institute for Molecules and Materials, Radboud University Nijmegen, Heijendaalseweg 135, 6525 AJ Nijmegen, The Netherlands ; 'L.J.de Jongh' ; Kamerlingh Onnes Laboratory, Leiden Institute of Physics, Leiden University, PO Box 9504, 2300 RA Leiden, The Netherlands. ; J.Reedijk ; Leiden Institute of Chemistry, Leiden University, P.O. Box 9502, 2300 RA, Leiden, The Netherlands Alternate address: Department of Chemistry, College of Science, King Saud University, P.O. Box 2455 Riyadh 11451, Kingdom of Saudi Arabia. ; #============================================================================= # 4. TEXT _publ_section_abstract ; New manganese compounds [Mn(HphpzMe)2(H2phpzMe)(HCO2)] (1), [Mn~2~(phpzMe)~2~(HphpzMe)~2~(OCH~3~)]\.2CH~3~OH (2), Na{[Mn(HphpzPh)(phpzPh)(MeOH)~2~]~2~}(HCO~2~) (3), [Mn(HphpzPh)~2~(EtOH)~2~]ClO~4~\.2EtOH (4) and [Mn(HphpzPh)~2~N~3~] (5) were synthesized and characterized. 1, 4 and 5 are mononuclear manganese(III) compounds, 2 is a mixed-valence dinuclear manganese(III/IV) compound, and 3 is a trinuclear compound containing by two manganese(III) ions and a sodium(I) ion. A remarkable feature is the spontaneous formation of formate as a result of the methanol or methoxide oxidation in compounds 1 and 3. Using ethanol precludes the formation of formate and compound 4 is obtained. The molecular structure of all compounds is stabilized by supramolecular interactions, including strong hydrogen bonding and \p - \p interactions. ; _publ_section_comment ; ; _publ_section_experimental ; A crystal was selected for the X--ray measurements and mounted to the glass fiber using the oil drop method (Kottke & Stalke, 1993) and data were collected at 173 K. The intensity data were corrected for Lorentz and polarization effects and for absorption. The nonhydrogen atoms were refined anisotropically. The methanol H1 atom was picked from a difference map. The other H atoms were geometrically fixed and allowed to ride on the attached atoms. ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst 32, 115-119. Duisenberg, A.J.M., J. Appl. Cryst. 25 (1992) 92-96. Nonius (2002). COLLECT. Nonius BV, Delft, The Netherlands. Kottke, T. and Stalke, D. (1993). J. Appl. Crystallogr. 26, 615--619. Sheldrick, G.M. (1990). SHELXTL. University of G\"ottingen, Germany. Sheldrick, G.M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELX97. University of G\"ottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_contact_author_name 'Reedijk, Jan' #============================================================================= data_mvc90 _database_code_depnum_ccdc_archive 'CCDC 858616' #TrackingRef 'mvc90.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H45 Mn2 N8 O7' _chemical_formula_weight 895.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6470(10) _cell_length_b 21.768(4) _cell_length_c 18.897(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.19(3) _cell_angle_gamma 90.00 _cell_volume 4376.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 148 _cell_measurement_theta_min 4.52 _cell_measurement_theta_max 22.40 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8835 _exptl_absorpt_correction_T_max 0.8835 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54196 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9444 _reflns_number_gt 6012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_cell_refinement 'DirAx (Duisenberg 1992)' _computing_data_reduction 'COLLECT/EVAL (Nonius, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXTL (Sheldrick, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+8.1136P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9444 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1475 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.68656(6) 0.10267(3) 0.85019(3) 0.03458(17) Uani 1 1 d . . . Mn2 Mn 0.51827(6) 0.01278(3) 0.74549(3) 0.03497(17) Uani 1 1 d . . . O10 O 0.6775(3) 0.15039(12) 0.93404(14) 0.0397(6) Uani 1 1 d . . . C11 C 0.6085(4) 0.20131(17) 0.9430(2) 0.0364(9) Uani 1 1 d . . . C12 C 0.4864(4) 0.20985(16) 0.9113(2) 0.0352(8) Uani 1 1 d . . . C13 C 0.4171(4) 0.26244(18) 0.9283(2) 0.0444(10) Uani 1 1 d . . . H13A H 0.3345 0.2675 0.9083 0.053 Uiso 1 1 calc R . . C14 C 0.4660(5) 0.3067(2) 0.9734(3) 0.0542(12) Uani 1 1 d . . . H14A H 0.4175 0.3418 0.9844 0.065 Uiso 1 1 calc R . . C15 C 0.5886(5) 0.2997(2) 1.0032(2) 0.0517(11) Uani 1 1 d . . . H15A H 0.6232 0.3303 1.0341 0.062 Uiso 1 1 calc R . . C16 C 0.6591(4) 0.24784(19) 0.9873(2) 0.0437(10) Uani 1 1 d . . . H16A H 0.7424 0.2438 1.0067 0.052 Uiso 1 1 calc R . . N21 N 0.5066(3) 0.12168(14) 0.83112(16) 0.0352(7) Uani 1 1 d . . . C22 C 0.4322(4) 0.16372(17) 0.8612(2) 0.0349(8) Uani 1 1 d . . . C23 C 0.3084(4) 0.15562(19) 0.8343(2) 0.0439(10) Uani 1 1 d . . . H23A H 0.2369 0.1793 0.8455 0.053 Uiso 1 1 calc R . . C24 C 0.3119(4) 0.10612(19) 0.7881(2) 0.0427(9) Uani 1 1 d . . . N25 N 0.4331(3) 0.08577(14) 0.78627(17) 0.0373(7) Uani 1 1 d . . . C26 C 0.2047(4) 0.0790(2) 0.7437(3) 0.0584(12) Uani 1 1 d . . . H26A H 0.2188 0.0863 0.6935 0.088 Uiso 1 1 calc R . . H26B H 0.1256 0.0984 0.7564 0.088 Uiso 1 1 calc R . . H26C H 0.2000 0.0347 0.7524 0.088 Uiso 1 1 calc R . . O30 O 0.3734(3) -0.03508(12) 0.74123(14) 0.0409(6) Uani 1 1 d . . . C31 C 0.3584(4) -0.09168(18) 0.7691(2) 0.0386(9) Uani 1 1 d . . . C32 C 0.4193(4) -0.11024(19) 0.8330(2) 0.0421(9) Uani 1 1 d . . . C33 C 0.3916(5) -0.1691(2) 0.8599(3) 0.0554(12) Uani 1 1 d . . . H33A H 0.4305 -0.1823 0.9034 0.066 Uiso 1 1 calc R . . C34 C 0.3088(6) -0.2076(2) 0.8238(3) 0.0652(14) Uani 1 1 d . . . H34A H 0.2916 -0.2470 0.8426 0.078 Uiso 1 1 calc R . . C35 C 0.2499(5) -0.1894(2) 0.7603(3) 0.0608(13) Uani 1 1 d . . . H35A H 0.1923 -0.2162 0.7361 0.073 Uiso 1 1 calc R . . C36 C 0.2759(4) -0.1316(2) 0.7322(2) 0.0469(10) Uani 1 1 d . . . H36A H 0.2378 -0.1194 0.6882 0.056 Uiso 1 1 calc R . . N41 N 0.5544(3) -0.01891(14) 0.84098(16) 0.0372(7) Uani 1 1 d . . . C42 C 0.5083(4) -0.06990(18) 0.8721(2) 0.0392(9) Uani 1 1 d . . . C43 C 0.5602(4) -0.0722(2) 0.9411(2) 0.0460(10) Uani 1 1 d . . . H43A H 0.5470 -0.1032 0.9755 0.055 Uiso 1 1 calc R . . C44 C 0.6358(4) -0.01959(19) 0.9493(2) 0.0414(9) Uani 1 1 d . . . N45 N 0.6315(3) 0.01251(15) 0.88832(16) 0.0376(7) Uani 1 1 d . . . C46 C 0.7153(4) 0.0018(2) 1.0122(2) 0.0518(11) Uani 1 1 d . . . H46A H 0.7127 0.0468 1.0149 0.078 Uiso 1 1 calc R . . H46B H 0.8022 -0.0117 1.0071 0.078 Uiso 1 1 calc R . . H46C H 0.6825 -0.0157 1.0556 0.078 Uiso 1 1 calc R . . O50 O 0.4799(3) 0.04049(13) 0.65166(14) 0.0464(7) Uani 1 1 d . . . C51 C 0.4294(4) 0.0011(2) 0.6020(2) 0.0450(10) Uani 1 1 d . . . C52 C 0.4789(4) -0.05839(19) 0.5932(2) 0.0430(10) Uani 1 1 d . . . C53 C 0.4244(5) -0.0964(2) 0.5394(2) 0.0539(12) Uani 1 1 d . . . H53A H 0.4567 -0.1365 0.5326 0.065 Uiso 1 1 calc R . . C54 C 0.3241(5) -0.0757(2) 0.4964(2) 0.0602(14) Uani 1 1 d . . . H54A H 0.2879 -0.1020 0.4611 0.072 Uiso 1 1 calc R . . C55 C 0.2776(6) -0.0178(3) 0.5047(2) 0.0648(15) Uani 1 1 d . . . H55A H 0.2102 -0.0038 0.4744 0.078 Uiso 1 1 calc R . . C56 C 0.3288(5) 0.0214(2) 0.5579(2) 0.0593(13) Uani 1 1 d . . . H56A H 0.2953 0.0615 0.5638 0.071 Uiso 1 1 calc R . . N61 N 0.6127(3) -0.05589(15) 0.70220(18) 0.0420(8) Uani 1 1 d . . . C62 C 0.5878(4) -0.07975(19) 0.6365(2) 0.0439(10) Uani 1 1 d . . . C63 C 0.6826(5) -0.1220(2) 0.6223(2) 0.0542(12) Uani 1 1 d . . . H63A H 0.6885 -0.1458 0.5804 0.065 Uiso 1 1 calc R . . C64 C 0.7662(5) -0.1229(2) 0.6802(3) 0.0536(11) Uani 1 1 d . . . N65 N 0.7210(4) -0.08230(16) 0.72776(19) 0.0477(9) Uani 1 1 d . . . H65A H 0.7569 -0.0743 0.7694 0.057 Uiso 1 1 calc R . . C66 C 0.8860(5) -0.1575(3) 0.6944(3) 0.0725(16) Uani 1 1 d . . . H66A H 0.9038 -0.1598 0.7456 0.109 Uiso 1 1 calc R . . H66B H 0.9551 -0.1362 0.6718 0.109 Uiso 1 1 calc R . . H66C H 0.8777 -0.1991 0.6750 0.109 Uiso 1 1 calc R . . O70 O 0.8600(3) 0.08458(12) 0.86915(14) 0.0397(6) Uani 1 1 d . . . C71 C 0.9360(4) 0.12689(18) 0.9015(2) 0.0375(9) Uani 1 1 d . . . C72 C 0.9437(4) 0.18783(19) 0.8757(2) 0.0378(9) Uani 1 1 d . . . C73 C 1.0244(4) 0.2298(2) 0.9112(2) 0.0430(9) Uani 1 1 d . . . H73A H 1.0297 0.2707 0.8941 0.052 Uiso 1 1 calc R . . C74 C 1.0970(4) 0.2123(2) 0.9710(2) 0.0496(11) Uani 1 1 d . . . H74A H 1.1505 0.2411 0.9949 0.060 Uiso 1 1 calc R . . C75 C 1.0897(4) 0.1522(2) 0.9950(2) 0.0536(12) Uani 1 1 d . . . H75A H 1.1390 0.1398 1.0355 0.064 Uiso 1 1 calc R . . C76 C 1.0114(4) 0.1101(2) 0.9607(2) 0.0470(10) Uani 1 1 d . . . H76A H 1.0088 0.0690 0.9775 0.056 Uiso 1 1 calc R . . N81 N 0.7611(3) 0.18028(15) 0.79229(17) 0.0432(8) Uani 1 1 d . . . C82 C 0.8717(4) 0.20737(18) 0.8118(2) 0.0414(9) Uani 1 1 d . . . C83 C 0.9013(5) 0.2520(2) 0.7608(2) 0.0557(12) Uani 1 1 d . . . H83A H 0.9726 0.2783 0.7618 0.067 Uiso 1 1 calc R . . C84 C 0.8055(5) 0.2499(2) 0.7092(3) 0.0625(14) Uani 1 1 d . . . N85 N 0.7234(4) 0.20621(17) 0.73002(19) 0.0526(10) Uani 1 1 d . . . H85A H 0.6542 0.1960 0.7059 0.063 Uiso 1 1 calc R . . C86 C 0.7828(7) 0.2843(3) 0.6408(3) 0.085(2) Uani 1 1 d . . . H86A H 0.6931 0.2938 0.6345 0.128 Uiso 1 1 calc R . . H86B H 0.8092 0.2588 0.6012 0.128 Uiso 1 1 calc R . . H86C H 0.8313 0.3225 0.6421 0.128 Uiso 1 1 calc R . . O1 O 0.6700(3) 0.05867(12) 0.75630(13) 0.0371(6) Uani 1 1 d . . . C1 C 0.7689(5) 0.0587(3) 0.7048(3) 0.0629(13) Uani 1 1 d . . . H1A H 0.7414 0.0346 0.6632 0.094 Uiso 1 1 calc R . . H1B H 0.8454 0.0404 0.7263 0.094 Uiso 1 1 calc R . . H1C H 0.7863 0.1010 0.6905 0.094 Uiso 1 1 calc R . . O2 O 0.5434(3) 0.16109(15) 0.6327(2) 0.0632(9) Uani 1 1 d . . . H2 H 0.5274 0.1234 0.6359 0.095 Uiso 1 1 calc R . . C2 C 0.4332(5) 0.1935(2) 0.6260(4) 0.087(2) Uani 1 1 d . . . H2A H 0.4518 0.2366 0.6157 0.131 Uiso 1 1 calc R . . H2B H 0.3886 0.1909 0.6703 0.131 Uiso 1 1 calc R . . H2C H 0.3806 0.1762 0.5873 0.131 Uiso 1 1 calc R . . O3 O 0.8833(3) -0.04512(15) 0.84467(19) 0.0621(9) Uani 1 1 d . . . H3 H 0.8667 -0.0076 0.8400 0.093 Uiso 1 1 d . . . C3 C 1.0150(5) -0.0540(3) 0.8432(3) 0.0672(14) Uani 1 1 d . . . H3A H 1.0418 -0.0512 0.7943 0.101 Uiso 1 1 calc R . . H3B H 1.0366 -0.0946 0.8625 0.101 Uiso 1 1 calc R . . H3C H 1.0578 -0.0222 0.8719 0.101 Uiso 1 1 calc 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 0.0398(3) 0.0293(3) 0.0343(3) 0.0007(2) -0.0029(2) 0.0015(2) Mn2 0.0445(3) 0.0323(3) 0.0278(3) -0.0012(2) -0.0027(2) -0.0028(2) O10 0.0492(16) 0.0357(14) 0.0335(14) 0.0015(11) -0.0068(12) 0.0040(12) C11 0.049(2) 0.0318(19) 0.0282(18) 0.0070(15) 0.0030(17) -0.0018(17) C12 0.044(2) 0.0290(18) 0.0329(19) 0.0032(15) 0.0038(17) -0.0003(16) C13 0.045(2) 0.034(2) 0.056(3) -0.0014(18) 0.007(2) -0.0021(18) C14 0.068(3) 0.034(2) 0.062(3) -0.008(2) 0.016(2) 0.001(2) C15 0.072(3) 0.039(2) 0.044(2) -0.0136(19) 0.007(2) -0.012(2) C16 0.056(3) 0.043(2) 0.032(2) 0.0031(17) 0.0014(19) -0.0093(19) N21 0.0420(18) 0.0294(16) 0.0336(17) -0.0031(13) -0.0058(14) 0.0018(14) C22 0.040(2) 0.0311(19) 0.0332(19) 0.0059(15) -0.0014(16) -0.0018(16) C23 0.042(2) 0.040(2) 0.049(2) 0.0014(19) -0.0024(19) 0.0016(18) C24 0.045(2) 0.040(2) 0.042(2) 0.0008(18) -0.0045(18) -0.0019(18) N25 0.0391(18) 0.0336(17) 0.0388(18) -0.0011(14) -0.0057(14) 0.0007(14) C26 0.045(3) 0.058(3) 0.071(3) -0.008(2) -0.012(2) -0.003(2) O30 0.0492(17) 0.0362(14) 0.0367(15) 0.0008(12) -0.0050(12) -0.0052(12) C31 0.047(2) 0.036(2) 0.033(2) -0.0018(16) 0.0070(17) -0.0051(17) C32 0.053(3) 0.041(2) 0.032(2) 0.0029(17) 0.0077(18) -0.0027(19) C33 0.077(3) 0.045(2) 0.044(2) 0.007(2) 0.005(2) -0.011(2) C34 0.089(4) 0.048(3) 0.058(3) 0.018(2) 0.002(3) -0.020(3) C35 0.074(3) 0.050(3) 0.059(3) -0.005(2) 0.009(3) -0.024(2) C36 0.053(3) 0.046(2) 0.042(2) 0.0018(19) 0.006(2) -0.009(2) N41 0.0466(19) 0.0355(17) 0.0292(16) -0.0025(13) -0.0015(14) -0.0007(14) C42 0.049(2) 0.038(2) 0.0310(19) 0.0004(16) 0.0035(17) 0.0040(18) C43 0.060(3) 0.049(2) 0.029(2) 0.0060(18) 0.0009(19) 0.009(2) C44 0.043(2) 0.049(2) 0.032(2) -0.0024(17) 0.0011(17) 0.0067(19) N45 0.0451(19) 0.0382(17) 0.0291(16) -0.0050(13) -0.0034(14) 0.0006(15) C46 0.053(3) 0.066(3) 0.035(2) -0.005(2) -0.0104(19) 0.013(2) O50 0.066(2) 0.0372(15) 0.0353(15) 0.0041(12) -0.0104(14) -0.0107(14) C51 0.057(3) 0.048(2) 0.0291(19) 0.0072(17) -0.0062(18) -0.020(2) C52 0.056(3) 0.046(2) 0.0273(19) -0.0020(17) 0.0042(18) -0.015(2) C53 0.073(3) 0.053(3) 0.036(2) -0.0041(19) 0.003(2) -0.024(2) C54 0.081(4) 0.064(3) 0.034(2) -0.003(2) -0.007(2) -0.032(3) C55 0.082(4) 0.072(4) 0.038(2) 0.009(2) -0.021(2) -0.026(3) C56 0.075(3) 0.055(3) 0.046(3) 0.012(2) -0.016(2) -0.018(2) N61 0.048(2) 0.0410(18) 0.0368(18) -0.0079(14) -0.0001(15) -0.0036(15) C62 0.057(3) 0.042(2) 0.033(2) -0.0091(17) 0.0062(19) -0.011(2) C63 0.068(3) 0.052(3) 0.043(2) -0.020(2) 0.010(2) -0.003(2) C64 0.058(3) 0.046(2) 0.057(3) -0.016(2) 0.010(2) 0.002(2) N65 0.053(2) 0.047(2) 0.042(2) -0.0128(16) -0.0054(17) 0.0047(17) C66 0.071(4) 0.067(3) 0.080(4) -0.026(3) 0.007(3) 0.015(3) O70 0.0434(15) 0.0363(14) 0.0388(15) -0.0030(12) -0.0052(12) 0.0048(12) C71 0.035(2) 0.041(2) 0.037(2) -0.0070(17) -0.0007(16) 0.0032(16) C72 0.039(2) 0.047(2) 0.0272(19) -0.0056(16) -0.0012(16) -0.0010(17) C73 0.047(2) 0.045(2) 0.036(2) -0.0037(18) -0.0050(18) -0.0039(19) C74 0.047(2) 0.063(3) 0.039(2) -0.006(2) -0.0108(19) -0.006(2) C75 0.051(3) 0.066(3) 0.043(2) 0.002(2) -0.018(2) 0.008(2) C76 0.046(2) 0.046(2) 0.048(2) 0.0029(19) -0.010(2) 0.0069(19) N81 0.055(2) 0.0400(18) 0.0334(17) 0.0053(14) -0.0151(16) -0.0061(16) C82 0.053(2) 0.038(2) 0.033(2) -0.0034(16) -0.0074(18) -0.0079(18) C83 0.073(3) 0.055(3) 0.039(2) 0.007(2) -0.014(2) -0.022(2) C84 0.088(4) 0.053(3) 0.045(3) 0.014(2) -0.021(3) -0.020(3) N85 0.069(3) 0.050(2) 0.0366(19) 0.0082(16) -0.0266(18) -0.0092(19) C86 0.123(5) 0.082(4) 0.049(3) 0.028(3) -0.034(3) -0.039(4) O1 0.0450(15) 0.0390(14) 0.0271(13) -0.0022(11) 0.0003(11) -0.0069(12) C1 0.068(3) 0.069(3) 0.051(3) -0.003(2) -0.001(2) -0.010(3) O2 0.076(2) 0.0420(17) 0.069(2) 0.0046(16) -0.0301(19) -0.0026(16) C2 0.061(3) 0.041(3) 0.159(7) -0.008(3) -0.002(4) 0.008(3) O3 0.064(2) 0.0508(19) 0.071(2) -0.0173(16) -0.0101(18) 0.0173(16) C3 0.062(3) 0.069(3) 0.071(4) -0.012(3) 0.004(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O10 1.900(3) . ? Mn1 O70 1.908(3) . ? Mn1 N21 1.980(3) . ? Mn1 O1 2.018(3) . ? Mn1 N45 2.179(3) . ? Mn1 N81 2.179(3) . ? Mn2 O30 1.861(3) . ? Mn2 O50 1.903(3) . ? Mn2 O1 1.904(3) . ? Mn2 N41 1.956(3) . ? Mn2 N61 1.994(3) . ? Mn2 N25 1.999(3) . ? O10 C11 1.344(5) . ? C11 C16 1.409(6) . ? C11 C12 1.422(6) . ? C12 C13 1.406(6) . ? C12 C22 1.482(5) . ? C13 C14 1.376(6) . ? C13 H13A 0.9500 . ? C14 C15 1.410(7) . ? C14 H14A 0.9500 . ? C15 C16 1.395(6) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N21 C22 1.350(5) . ? N21 N25 1.375(4) . ? C22 C23 1.405(6) . ? C23 C24 1.388(6) . ? C23 H23A 0.9500 . ? C24 N25 1.366(5) . ? C24 C26 1.511(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O30 C31 1.352(5) . ? C31 C36 1.402(6) . ? C31 C32 1.407(6) . ? C32 C33 1.414(6) . ? C32 C42 1.471(6) . ? C33 C34 1.378(7) . ? C33 H33A 0.9500 . ? C34 C35 1.390(7) . ? C34 H34A 0.9500 . ? C35 C36 1.398(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N41 C42 1.356(5) . ? N41 N45 1.373(4) . ? C42 C43 1.398(6) . ? C43 C44 1.406(6) . ? C43 H43A 0.9500 . ? C44 N45 1.347(5) . ? C44 C46 1.507(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? O50 C51 1.366(5) . ? C51 C56 1.403(6) . ? C51 C52 1.410(6) . ? C52 C53 1.418(6) . ? C52 C62 1.469(6) . ? C53 C54 1.391(7) . ? C53 H53A 0.9500 . ? C54 C55 1.366(8) . ? C54 H54A 0.9500 . ? C55 C56 1.413(7) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? N61 N65 1.360(5) . ? N61 C62 1.362(5) . ? C62 C63 1.398(7) . ? C63 C64 1.384(7) . ? C63 H63A 0.9500 . ? C64 N65 1.361(6) . ? C64 C66 1.498(7) . ? N65 H65A 0.8800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? O70 C71 1.356(5) . ? C71 C76 1.401(6) . ? C71 C72 1.417(6) . ? C72 C73 1.406(5) . ? C72 C82 1.469(5) . ? C73 C74 1.398(6) . ? C73 H73A 0.9500 . ? C74 C75 1.389(7) . ? C74 H74A 0.9500 . ? C75 C76 1.383(6) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? N81 N85 1.352(4) . ? N81 C82 1.355(5) . ? C82 C83 1.412(6) . ? C83 C84 1.384(6) . ? C83 H83A 0.9500 . ? C84 N85 1.360(6) . ? C84 C86 1.505(6) . ? N85 H85A 0.8800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? O1 C1 1.460(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C2 1.370(6) . ? O2 H2 0.8400 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C3 1.417(6) . ? O3 H3 0.8393 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Mn1 O70 92.07(12) . . ? O10 Mn1 N21 87.57(12) . . ? O70 Mn1 N21 179.64(13) . . ? O10 Mn1 O1 170.76(11) . . ? O70 Mn1 O1 96.81(12) . . ? N21 Mn1 O1 83.56(12) . . ? O10 Mn1 N45 101.17(12) . . ? O70 Mn1 N45 91.31(12) . . ? N21 Mn1 N45 88.71(13) . . ? O1 Mn1 N45 81.24(11) . . ? O10 Mn1 N81 91.49(13) . . ? O70 Mn1 N81 83.45(13) . . ? N21 Mn1 N81 96.61(13) . . ? O1 Mn1 N81 87.00(12) . . ? N45 Mn1 N81 166.49(13) . . ? O30 Mn2 O50 89.36(12) . . ? O30 Mn2 O1 175.71(12) . . ? O50 Mn2 O1 94.87(12) . . ? O30 Mn2 N41 88.62(13) . . ? O50 Mn2 N41 177.65(13) . . ? O1 Mn2 N41 87.14(13) . . ? O30 Mn2 N61 89.59(13) . . ? O50 Mn2 N61 87.09(14) . . ? O1 Mn2 N61 89.90(13) . . ? N41 Mn2 N61 91.70(14) . . ? O30 Mn2 N25 94.25(13) . . ? O50 Mn2 N25 91.30(13) . . ? O1 Mn2 N25 86.40(12) . . ? N41 Mn2 N25 90.05(13) . . ? N61 Mn2 N25 175.82(14) . . ? C11 O10 Mn1 126.9(2) . . ? O10 C11 C16 118.0(4) . . ? O10 C11 C12 123.4(3) . . ? C16 C11 C12 118.6(4) . . ? C13 C12 C11 119.3(4) . . ? C13 C12 C22 120.2(4) . . ? C11 C12 C22 120.5(3) . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C11 120.9(4) . . ? C15 C16 H16A 119.5 . . ? C11 C16 H16A 119.5 . . ? C22 N21 N25 108.4(3) . . ? C22 N21 Mn1 130.1(3) . . ? N25 N21 Mn1 121.1(2) . . ? N21 C22 C23 108.6(3) . . ? N21 C22 C12 120.5(3) . . ? C23 C22 C12 130.8(4) . . ? C24 C23 C22 106.1(4) . . ? C24 C23 H23A 126.9 . . ? C22 C23 H23A 126.9 . . ? N25 C24 C23 108.4(4) . . ? N25 C24 C26 123.6(4) . . ? C23 C24 C26 127.9(4) . . ? C24 N25 N21 108.4(3) . . ? C24 N25 Mn2 135.3(3) . . ? N21 N25 Mn2 115.7(2) . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 O30 Mn2 127.1(3) . . ? O30 C31 C36 116.8(4) . . ? O30 C31 C32 122.6(3) . . ? C36 C31 C32 120.5(4) . . ? C31 C32 C33 118.3(4) . . ? C31 C32 C42 121.8(4) . . ? C33 C32 C42 120.0(4) . . ? C34 C33 C32 120.7(4) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C35 121.0(4) . . ? C33 C34 H34A 119.5 . . ? C35 C34 H34A 119.5 . . ? C34 C35 C36 119.6(4) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? C42 N41 N45 110.0(3) . . ? C42 N41 Mn2 128.8(3) . . ? N45 N41 Mn2 121.1(2) . . ? N41 C42 C43 107.3(4) . . ? N41 C42 C32 120.5(3) . . ? C43 C42 C32 132.2(4) . . ? C42 C43 C44 106.1(4) . . ? C42 C43 H43A 127.0 . . ? C44 C43 H43A 127.0 . . ? N45 C44 C43 109.2(3) . . ? N45 C44 C46 121.0(4) . . ? C43 C44 C46 129.8(4) . . ? C44 N45 N41 107.4(3) . . ? C44 N45 Mn1 138.5(3) . . ? N41 N45 Mn1 113.3(2) . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C51 O50 Mn2 120.4(2) . . ? O50 C51 C56 118.7(4) . . ? O50 C51 C52 121.2(4) . . ? C56 C51 C52 120.0(4) . . ? C51 C52 C53 118.4(4) . . ? C51 C52 C62 121.1(4) . . ? C53 C52 C62 120.5(4) . . ? C54 C53 C52 121.0(5) . . ? C54 C53 H53A 119.5 . . ? C52 C53 H53A 119.5 . . ? C55 C54 C53 120.3(4) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C54 C55 C56 120.5(5) . . ? C54 C55 H55A 119.7 . . ? C56 C55 H55A 119.7 . . ? C51 C56 C55 119.8(5) . . ? C51 C56 H56A 120.1 . . ? C55 C56 H56A 120.1 . . ? N65 N61 C62 107.1(3) . . ? N65 N61 Mn2 127.2(3) . . ? C62 N61 Mn2 125.2(3) . . ? N61 C62 C63 108.0(4) . . ? N61 C62 C52 120.6(4) . . ? C63 C62 C52 131.3(4) . . ? C64 C63 C62 107.7(4) . . ? C64 C63 H63A 126.2 . . ? C62 C63 H63A 126.2 . . ? N65 C64 C63 106.3(4) . . ? N65 C64 C66 121.9(4) . . ? C63 C64 C66 131.8(4) . . ? N61 N65 C64 110.8(4) . . ? N61 N65 H65A 124.6 . . ? C64 N65 H65A 124.6 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C71 O70 Mn1 120.1(2) . . ? O70 C71 C76 119.8(4) . . ? O70 C71 C72 121.5(3) . . ? C76 C71 C72 118.7(4) . . ? C73 C72 C71 119.1(4) . . ? C73 C72 C82 119.6(4) . . ? C71 C72 C82 121.2(3) . . ? C74 C73 C72 121.2(4) . . ? C74 C73 H73A 119.4 . . ? C72 C73 H73A 119.4 . . ? C75 C74 C73 119.0(4) . . ? C75 C74 H74A 120.5 . . ? C73 C74 H74A 120.5 . . ? C76 C75 C74 120.8(4) . . ? C76 C75 H75A 119.6 . . ? C74 C75 H75A 119.6 . . ? C75 C76 C71 121.3(4) . . ? C75 C76 H76A 119.4 . . ? C71 C76 H76A 119.4 . . ? N85 N81 C82 106.3(3) . . ? N85 N81 Mn1 131.2(3) . . ? C82 N81 Mn1 122.0(3) . . ? N81 C82 C83 109.2(4) . . ? N81 C82 C72 121.2(4) . . ? C83 C82 C72 129.5(4) . . ? C84 C83 C82 106.2(4) . . ? C84 C83 H83A 126.9 . . ? C82 C83 H83A 126.9 . . ? N85 C84 C83 106.5(4) . . ? N85 C84 C86 120.8(4) . . ? C83 C84 C86 132.7(5) . . ? N81 N85 C84 111.8(3) . . ? N81 N85 H85A 124.1 . . ? C84 N85 H85A 124.1 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C1 O1 Mn2 124.0(3) . . ? C1 O1 Mn1 123.0(3) . . ? Mn2 O1 Mn1 112.86(13) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 O2 H2 109.5 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 O3 H3 109.5 . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.947 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.084 #============================================================================= data_mvc29a _database_code_depnum_ccdc_archive 'CCDC 858617' #TrackingRef 'mvc29_formate.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H60 Mn2 N8 Na O10' _chemical_formula_weight 1246.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.527(6) _cell_length_b 7.828(2) _cell_length_c 23.528(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.71(3) _cell_angle_gamma 90.00 _cell_volume 5777(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 374 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 23.65 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2588 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8208 _exptl_absorpt_correction_T_max 0.8611 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38466 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5561 _reflns_number_gt 4421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_cell_refinement 'COLLECT (Nonius, 2002)' _computing_data_reduction 'COLLECT (Nonius, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXTL (Sheldrick, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+66.0460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5561 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_restrained_S_all 1.238 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.58972(2) 0.07924(11) 0.73825(4) 0.0265(2) Uani 1 1 d . A . O10 O 0.57569(11) 0.1338(5) 0.80558(16) 0.0311(8) Uani 1 1 d . A . C11 C 0.59722(16) 0.2199(7) 0.8591(2) 0.0300(12) Uani 1 1 d . . . C12 C 0.64104(16) 0.2597(7) 0.8821(2) 0.0302(12) Uani 1 1 d . . . C13 C 0.65972(17) 0.3555(8) 0.9372(2) 0.0356(13) Uani 1 1 d . . . H13A H 0.6890 0.3860 0.9523 0.043 Uiso 1 1 calc R . . C14 C 0.6366(2) 0.4067(8) 0.9703(3) 0.0431(14) Uani 1 1 d . . . H14A H 0.6498 0.4730 1.0073 0.052 Uiso 1 1 calc R . . C15 C 0.59421(19) 0.3607(8) 0.9489(3) 0.0391(14) Uani 1 1 d . . . H15A H 0.5785 0.3914 0.9723 0.047 Uiso 1 1 calc R . . C16 C 0.57464(18) 0.2707(7) 0.8941(3) 0.0354(13) Uani 1 1 d . . . H16A H 0.5453 0.2422 0.8795 0.043 Uiso 1 1 calc R . . N21 N 0.64976(12) 0.1401(6) 0.79092(18) 0.0283(10) Uani 1 1 d . . . C22 C 0.66701(16) 0.2047(7) 0.8499(2) 0.0281(11) Uani 1 1 d . . . C23 C 0.71123(15) 0.2021(7) 0.8707(2) 0.0275(11) Uani 1 1 d . . . H23A H 0.7318 0.2380 0.9104 0.033 Uiso 1 1 calc R . . C24 C 0.71922(15) 0.1363(7) 0.8215(2) 0.0259(11) Uani 1 1 d . . . N25 N 0.68203(12) 0.0982(6) 0.77313(18) 0.0268(9) Uani 1 1 d . . . C31 C 0.75978(14) 0.1128(6) 0.8156(2) 0.0238(10) Uani 1 1 d . . . C32 C 0.79783(16) 0.1707(7) 0.8620(2) 0.0312(12) Uani 1 1 d . . . H32A H 0.7979 0.2246 0.8982 0.037 Uiso 1 1 calc R . . C33 C 0.83584(16) 0.1506(8) 0.8557(3) 0.0385(14) Uani 1 1 d . . . H33A H 0.8617 0.1895 0.8882 0.046 Uiso 1 1 calc R . . C34 C 0.83680(17) 0.0751(8) 0.8033(3) 0.0378(13) Uani 1 1 d . . . H34A H 0.8630 0.0629 0.7995 0.045 Uiso 1 1 calc R . . C35 C 0.79879(16) 0.0170(7) 0.7562(2) 0.0317(12) Uani 1 1 d . . . H35A H 0.7989 -0.0342 0.7197 0.038 Uiso 1 1 calc R . . C36 C 0.76085(15) 0.0338(7) 0.7626(2) 0.0278(11) Uani 1 1 d . . . H36A H 0.7352 -0.0087 0.7308 0.033 Uiso 1 1 calc R . . O40 O 0.53120(11) 0.0236(5) 0.69092(17) 0.0337(9) Uani 1 1 d . A . C41 C 0.51252(16) -0.0719(7) 0.6396(2) 0.0304(11) Uani 1 1 d . . . C42 C 0.53029(15) -0.1029(7) 0.5961(2) 0.0293(11) Uani 1 1 d . . . C43 C 0.50791(16) -0.2050(7) 0.5440(2) 0.0336(12) Uani 1 1 d . . . H43A H 0.5198 -0.2257 0.5147 0.040 Uiso 1 1 calc R . . C44 C 0.46899(18) -0.2768(8) 0.5338(3) 0.0392(13) Uani 1 1 d . . . H44A H 0.4548 -0.3485 0.4986 0.047 Uiso 1 1 calc R . . C45 C 0.45071(17) -0.2436(8) 0.5752(3) 0.0398(14) Uani 1 1 d . . . H45A H 0.4236 -0.2896 0.5677 0.048 Uiso 1 1 calc R . . C46 C 0.47235(17) -0.1428(7) 0.6275(3) 0.0362(13) Uani 1 1 d . . . H46A H 0.4598 -0.1210 0.6558 0.043 Uiso 1 1 calc R . . N51 N 0.59915(12) 0.0290(6) 0.66161(19) 0.0292(10) Uani 1 1 d . . . C52 C 0.57158(15) -0.0309(7) 0.6056(2) 0.0268(11) Uani 1 1 d . . . C53 C 0.58995(15) -0.0139(7) 0.5628(2) 0.0277(11) Uani 1 1 d . . . H53A H 0.5776 -0.0456 0.5199 0.033 Uiso 1 1 calc R . . C54 C 0.62949(15) 0.0581(7) 0.5954(2) 0.0275(11) Uani 1 1 d . . . N55 N 0.63425(12) 0.0846(6) 0.65447(19) 0.0312(10) Uani 1 1 d . . . H55A H 0.6568 0.1313 0.6842 0.037 Uiso 1 1 calc R . . C61 C 0.66477(15) 0.0992(7) 0.5777(2) 0.0252(10) Uani 1 1 d . . . C62 C 0.69945(16) 0.1978(7) 0.6172(2) 0.0303(12) Uani 1 1 d . . . H62A H 0.6987 0.2516 0.6529 0.036 Uiso 1 1 calc R . . C63 C 0.73494(17) 0.2172(8) 0.6042(3) 0.0349(13) Uani 1 1 d . . . H63A H 0.7587 0.2819 0.6316 0.042 Uiso 1 1 calc R . . C64 C 0.73564(17) 0.1423(7) 0.5515(3) 0.0365(13) Uani 1 1 d . . . H64A H 0.7604 0.1525 0.5436 0.044 Uiso 1 1 calc R . . C65 C 0.70077(19) 0.0526(8) 0.5102(3) 0.0410(14) Uani 1 1 d . . . H65A H 0.7009 0.0070 0.4728 0.049 Uiso 1 1 calc R . . C66 C 0.66529(17) 0.0294(7) 0.5235(2) 0.0332(12) Uani 1 1 d . . . H66A H 0.6415 -0.0339 0.4955 0.040 Uiso 1 1 calc R . . O1 O 0.57348(12) 0.3628(6) 0.70533(19) 0.0470(11) Uani 1 1 d G . . H1 H 0.5570 0.4008 0.7204 0.071 Uiso 1 1 d G . . C1 C 0.5525(2) 0.4023(9) 0.6405(3) 0.0502(17) Uani 1 1 d . . . H1A H 0.5480 0.5260 0.6352 0.075 Uiso 1 1 calc R . . H1B H 0.5249 0.3437 0.6222 0.075 Uiso 1 1 calc R . . H1C H 0.5702 0.3646 0.6193 0.075 Uiso 1 1 calc R . . O2 O 0.60178(14) -0.1972(6) 0.7691(2) 0.0476(11) Uani 1 1 d G . . H2 H 0.5842 -0.2774 0.7623 0.071 Uiso 1 1 d G . . C2 C 0.6308(3) -0.2564(12) 0.8295(4) 0.082(3) Uani 1 1 d . . . H2A H 0.6297 -0.3814 0.8307 0.123 Uiso 1 1 calc R . . H2B H 0.6227 -0.2085 0.8615 0.123 Uiso 1 1 calc R . . H2C H 0.6598 -0.2200 0.8376 0.123 Uiso 1 1 calc R . . Na1 Na 0.5000 0.1542(4) 0.7500 0.0363(7) Uani 1 2 d S . . O4 O 0.5118(2) 0.4375(11) 0.7490(4) 0.0381(19) Uani 0.50 1 d P A -1 C5 C 0.4901(4) 0.5668(15) 0.7420(8) 0.036(4) Uani 0.50 1 d P A -1 H5A H 0.5009 0.6687 0.7322 0.043 Uiso 1 1 calc R A -1 O6 O 0.4552(3) 0.5793(10) 0.7464(4) 0.0389(18) Uani 0.50 1 d P A -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 0.0195(4) 0.0329(5) 0.0313(4) 0.0030(3) 0.0146(3) 0.0023(3) O10 0.0275(18) 0.035(2) 0.037(2) 0.0042(17) 0.0199(16) 0.0048(16) C11 0.035(3) 0.029(3) 0.030(3) 0.012(2) 0.017(2) 0.014(2) C12 0.032(3) 0.037(3) 0.025(3) 0.009(2) 0.016(2) 0.011(2) C13 0.030(3) 0.044(3) 0.034(3) 0.006(3) 0.015(2) 0.008(2) C14 0.058(4) 0.040(4) 0.038(3) 0.005(3) 0.026(3) 0.014(3) C15 0.049(3) 0.039(3) 0.046(3) 0.008(3) 0.036(3) 0.017(3) C16 0.038(3) 0.034(3) 0.046(3) 0.009(3) 0.028(3) 0.012(2) N21 0.0203(19) 0.041(3) 0.025(2) 0.0067(19) 0.0105(17) 0.0082(19) C22 0.029(3) 0.029(3) 0.030(3) 0.009(2) 0.016(2) 0.007(2) C23 0.024(2) 0.033(3) 0.024(2) 0.002(2) 0.008(2) 0.004(2) C24 0.021(2) 0.030(3) 0.028(2) 0.005(2) 0.012(2) 0.003(2) N25 0.0174(19) 0.037(3) 0.026(2) 0.0025(18) 0.0086(16) 0.0062(18) C31 0.020(2) 0.024(3) 0.028(2) 0.002(2) 0.0105(19) 0.0003(19) C32 0.027(3) 0.033(3) 0.033(3) -0.004(2) 0.012(2) 0.001(2) C33 0.020(2) 0.046(4) 0.047(3) -0.008(3) 0.012(2) -0.009(2) C34 0.025(3) 0.036(3) 0.056(4) 0.001(3) 0.021(3) -0.005(2) C35 0.028(3) 0.035(3) 0.034(3) -0.001(2) 0.015(2) 0.003(2) C36 0.023(2) 0.027(3) 0.032(3) -0.002(2) 0.010(2) 0.002(2) O40 0.0238(18) 0.038(2) 0.045(2) -0.0045(18) 0.0201(16) -0.0011(16) C41 0.027(2) 0.029(3) 0.036(3) 0.007(2) 0.013(2) 0.005(2) C42 0.023(2) 0.029(3) 0.034(3) 0.009(2) 0.010(2) 0.002(2) C43 0.028(3) 0.038(3) 0.035(3) 0.009(2) 0.013(2) 0.000(2) C44 0.036(3) 0.039(3) 0.040(3) 0.002(3) 0.013(3) -0.005(3) C45 0.025(3) 0.033(3) 0.061(4) 0.005(3) 0.018(3) -0.006(2) C46 0.032(3) 0.029(3) 0.054(3) -0.002(3) 0.024(3) -0.003(2) N51 0.0171(19) 0.045(3) 0.027(2) 0.007(2) 0.0108(17) 0.0001(18) C52 0.020(2) 0.031(3) 0.028(2) 0.011(2) 0.0077(19) 0.007(2) C53 0.023(2) 0.032(3) 0.028(2) 0.004(2) 0.011(2) 0.004(2) C54 0.023(2) 0.036(3) 0.025(2) 0.005(2) 0.0112(19) 0.001(2) N55 0.0161(18) 0.051(3) 0.027(2) -0.002(2) 0.0094(16) -0.003(2) C61 0.023(2) 0.030(3) 0.025(2) 0.005(2) 0.0121(19) -0.002(2) C62 0.033(3) 0.032(3) 0.031(3) -0.005(2) 0.019(2) -0.006(2) C63 0.028(3) 0.041(3) 0.041(3) -0.001(3) 0.018(2) -0.004(2) C64 0.034(3) 0.038(3) 0.048(3) 0.007(3) 0.027(3) 0.001(2) C65 0.053(3) 0.046(4) 0.035(3) -0.005(3) 0.029(3) -0.008(3) C66 0.033(3) 0.040(3) 0.027(3) -0.004(2) 0.013(2) -0.008(2) O1 0.026(2) 0.069(3) 0.039(2) 0.022(2) 0.0070(17) 0.000(2) C1 0.047(3) 0.057(4) 0.037(3) 0.019(3) 0.008(3) -0.001(3) O2 0.047(3) 0.044(3) 0.047(2) 0.011(2) 0.014(2) 0.007(2) C2 0.099(7) 0.080(6) 0.061(5) 0.029(5) 0.027(5) 0.041(5) Na1 0.0251(14) 0.0347(18) 0.0551(19) 0.000 0.0227(14) 0.000 O4 0.031(5) 0.032(5) 0.055(5) 0.004(4) 0.021(5) 0.004(3) C5 0.054(14) 0.022(5) 0.019(10) 0.007(5) 0.001(9) 0.003(5) O6 0.041(4) 0.028(4) 0.054(5) 0.006(4) 0.027(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O10 1.889(3) . ? Mn1 O40 1.905(4) . ? Mn1 N21 1.978(4) . ? Mn1 N51 2.001(4) . ? Mn1 O2 2.265(5) . ? Mn1 O1 2.341(5) . ? Mn1 Na1 3.2761(11) . ? O10 C11 1.346(6) . ? O10 Na1 2.389(3) . ? C11 C16 1.407(7) . ? C11 C12 1.412(7) . ? C12 C13 1.400(8) . ? C12 C22 1.459(7) . ? C13 C14 1.387(8) . ? C13 H13A 0.9500 . ? C14 C15 1.381(9) . ? C14 H14A 0.9500 . ? C15 C16 1.375(8) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N21 C22 1.359(7) . ? N21 N25 1.383(5) . ? C22 C23 1.395(7) . ? C23 C24 1.395(7) . ? C23 H23A 0.9500 . ? C24 N25 1.346(6) . ? C24 C31 1.475(6) . ? C31 C32 1.386(7) . ? C31 C36 1.406(7) . ? C32 C33 1.389(7) . ? C32 H32A 0.9500 . ? C33 C34 1.380(8) . ? C33 H33A 0.9500 . ? C34 C35 1.393(7) . ? C34 H34A 0.9500 . ? C35 C36 1.386(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? O40 C41 1.335(6) . ? O40 Na1 2.321(4) . ? C41 C46 1.407(7) . ? C41 C42 1.417(7) . ? C42 C43 1.396(8) . ? C42 C52 1.461(7) . ? C43 C44 1.382(7) . ? C43 H43A 0.9500 . ? C44 C45 1.389(8) . ? C44 H44A 0.9500 . ? C45 C46 1.388(8) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? N51 C52 1.347(6) . ? N51 N55 1.363(5) . ? C52 C53 1.403(7) . ? C53 C54 1.376(7) . ? C53 H53A 0.9500 . ? C54 N55 1.345(6) . ? C54 C61 1.479(6) . ? N55 H55A 0.8800 . ? C61 C66 1.395(7) . ? C61 C62 1.401(7) . ? C62 C63 1.389(7) . ? C62 H62A 0.9500 . ? C63 C64 1.381(8) . ? C63 H63A 0.9500 . ? C64 C65 1.382(8) . ? C64 H64A 0.9500 . ? C65 C66 1.397(7) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? O1 C1 1.423(7) . ? O1 H1 0.8400 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C2 1.431(8) . ? O2 H2 0.8401 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? Na1 O4 2.256(9) . ? Na1 O4 2.256(9) 2_656 ? Na1 O40 2.321(4) 2_656 ? Na1 O10 2.389(3) 2_656 ? Na1 Mn1 3.2761(10) 2_656 ? O4 C5 1.229(14) . ? C5 O6 1.26(2) . ? C5 H5A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Mn1 O40 87.75(15) . . ? O10 Mn1 N21 89.38(16) . . ? O40 Mn1 N21 177.13(16) . . ? O10 Mn1 N51 174.66(16) . . ? O40 Mn1 N51 87.74(16) . . ? N21 Mn1 N51 95.12(16) . . ? O10 Mn1 O2 91.38(16) . . ? O40 Mn1 O2 88.69(17) . . ? N21 Mn1 O2 91.44(17) . . ? N51 Mn1 O2 91.37(18) . . ? O10 Mn1 O1 87.32(16) . . ? O40 Mn1 O1 88.54(15) . . ? N21 Mn1 O1 91.27(17) . . ? N51 Mn1 O1 89.72(17) . . ? O2 Mn1 O1 176.98(15) . . ? O10 Mn1 Na1 46.03(11) . . ? O40 Mn1 Na1 44.04(11) . . ? N21 Mn1 Na1 133.19(13) . . ? N51 Mn1 Na1 128.84(12) . . ? O2 Mn1 Na1 101.39(13) . . ? O1 Mn1 Na1 75.75(11) . . ? C11 O10 Mn1 131.5(3) . . ? C11 O10 Na1 121.9(3) . . ? Mn1 O10 Na1 99.29(15) . . ? O10 C11 C16 117.7(5) . . ? O10 C11 C12 123.6(4) . . ? C16 C11 C12 118.7(5) . . ? C13 C12 C11 118.5(5) . . ? C13 C12 C22 119.6(5) . . ? C11 C12 C22 121.9(5) . . ? C14 C13 C12 121.6(5) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C15 C14 C13 119.4(6) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C16 C15 C14 120.4(5) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C11 121.3(5) . . ? C15 C16 H16A 119.4 . . ? C11 C16 H16A 119.4 . . ? C22 N21 N25 109.5(4) . . ? C22 N21 Mn1 128.8(3) . . ? N25 N21 Mn1 121.3(3) . . ? N21 C22 C23 107.5(4) . . ? N21 C22 C12 122.5(4) . . ? C23 C22 C12 130.0(5) . . ? C24 C23 C22 106.4(4) . . ? C24 C23 H23A 126.8 . . ? C22 C23 H23A 126.8 . . ? N25 C24 C23 109.5(4) . . ? N25 C24 C31 120.0(4) . . ? C23 C24 C31 130.4(5) . . ? C24 N25 N21 107.2(4) . . ? C32 C31 C36 118.3(4) . . ? C32 C31 C24 120.7(4) . . ? C36 C31 C24 121.1(4) . . ? C31 C32 C33 120.4(5) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C34 C33 C32 121.3(5) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C33 C34 C35 118.9(5) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C36 C35 C34 120.1(5) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C31 121.0(5) . . ? C35 C36 H36A 119.5 . . ? C31 C36 H36A 119.5 . . ? C41 O40 Mn1 130.6(3) . . ? C41 O40 Na1 128.2(3) . . ? Mn1 O40 Na1 101.16(16) . . ? O40 C41 C46 117.9(5) . . ? O40 C41 C42 123.9(5) . . ? C46 C41 C42 118.3(5) . . ? C43 C42 C41 119.0(5) . . ? C43 C42 C52 120.1(5) . . ? C41 C42 C52 120.9(5) . . ? C44 C43 C42 121.8(5) . . ? C44 C43 H43A 119.1 . . ? C42 C43 H43A 119.1 . . ? C43 C44 C45 119.7(6) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C46 C45 C44 119.6(5) . . ? C46 C45 H45A 120.2 . . ? C44 C45 H45A 120.2 . . ? C45 C46 C41 121.6(5) . . ? C45 C46 H46A 119.2 . . ? C41 C46 H46A 119.2 . . ? C52 N51 N55 107.0(4) . . ? C52 N51 Mn1 129.5(3) . . ? N55 N51 Mn1 122.4(3) . . ? N51 C52 C53 108.8(4) . . ? N51 C52 C42 121.9(4) . . ? C53 C52 C42 129.2(5) . . ? C54 C53 C52 106.2(4) . . ? C54 C53 H53A 126.9 . . ? C52 C53 H53A 126.9 . . ? N55 C54 C53 107.7(4) . . ? N55 C54 C61 119.9(4) . . ? C53 C54 C61 132.3(5) . . ? C54 N55 N51 110.3(4) . . ? C54 N55 H55A 124.9 . . ? N51 N55 H55A 124.9 . . ? C66 C61 C62 119.2(4) . . ? C66 C61 C54 120.0(5) . . ? C62 C61 C54 120.6(4) . . ? C63 C62 C61 120.2(5) . . ? C63 C62 H62A 119.9 . . ? C61 C62 H62A 119.9 . . ? C64 C63 C62 119.9(5) . . ? C64 C63 H63A 120.1 . . ? C62 C63 H63A 120.1 . . ? C63 C64 C65 120.7(5) . . ? C63 C64 H64A 119.6 . . ? C65 C64 H64A 119.6 . . ? C64 C65 C66 119.7(5) . . ? C64 C65 H65A 120.2 . . ? C66 C65 H65A 120.1 . . ? C61 C66 C65 120.1(5) . . ? C61 C66 H66A 119.9 . . ? C65 C66 H66A 119.9 . . ? C1 O1 Mn1 120.3(4) . . ? C1 O1 H1 104.2 . . ? Mn1 O1 H1 107.9 . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 O2 Mn1 125.9(5) . . ? C2 O2 H2 95.6 . . ? Mn1 O2 H2 129.1 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 Na1 O4 21.3(3) . 2_656 ? O4 Na1 O40 107.2(2) . . ? O4 Na1 O40 124.7(2) 2_656 . ? O4 Na1 O40 124.7(2) . 2_656 ? O4 Na1 O40 107.2(2) 2_656 2_656 ? O40 Na1 O40 127.8(2) . 2_656 ? O4 Na1 O10 102.7(2) . 2_656 ? O4 Na1 O10 84.9(2) 2_656 2_656 ? O40 Na1 O10 108.54(13) . 2_656 ? O40 Na1 O10 67.86(13) 2_656 2_656 ? O4 Na1 O10 84.9(2) . . ? O4 Na1 O10 102.7(2) 2_656 . ? O40 Na1 O10 67.86(13) . . ? O40 Na1 O10 108.54(13) 2_656 . ? O10 Na1 O10 172.3(2) 2_656 . ? O4 Na1 Mn1 89.69(17) . . ? O4 Na1 Mn1 110.94(18) 2_656 . ? O40 Na1 Mn1 34.79(9) . . ? O40 Na1 Mn1 131.57(13) 2_656 . ? O10 Na1 Mn1 142.98(10) 2_656 . ? O10 Na1 Mn1 34.68(8) . . ? O4 Na1 Mn1 110.94(18) . 2_656 ? O4 Na1 Mn1 89.69(17) 2_656 2_656 ? O40 Na1 Mn1 131.57(13) . 2_656 ? O40 Na1 Mn1 34.79(9) 2_656 2_656 ? O10 Na1 Mn1 34.68(8) 2_656 2_656 ? O10 Na1 Mn1 142.98(10) . 2_656 ? Mn1 Na1 Mn1 159.37(11) . 2_656 ? C5 O4 Na1 135.2(9) . . ? O4 C5 O6 127.2(15) . . ? O4 C5 H5A 116.4 . . ? O6 C5 H5A 116.4 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.622 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.094 #============================================================================= data_mgm20 _database_code_depnum_ccdc_archive 'CCDC 858618' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Cl Mn N4 O10' _chemical_formula_weight 809.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.861 _cell_length_b 11.252(2) _cell_length_c 18.074(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.35(3) _cell_angle_gamma 90.00 _cell_volume 3945.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27407 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 26.49 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9131 _exptl_absorpt_correction_T_max 0.9862 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27407 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 26.49 _reflns_number_total 4066 _reflns_number_gt 2545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_cell_refinement 'DirAx (Duisenberg 1992)' _computing_data_reduction 'COLLECT/EVAL (Nonius, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXTL (Sheldrick, 1990)' _refine_special_details ; The U~ij~ of perchlorate oxygens O3 and O4 were restrained to 0.09 and 0.12 by isor during the refinement. The C3-C4 distance of the solvent ethanol was restrained to 1.45(0.01) \%A. The distance of H1 to O1 was restrained to 0.88(0.01) \%A and H1 to C1 1.88(0.01) \%A to keep the geometry of the coordinating ethanol chemically correct. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+13.4134P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4066 _refine_ls_number_parameters 248 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1907 _refine_ls_wR_factor_gt 0.1565 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.2500 0.2500 0.0000 0.0357(3) Uani 1 2 d S . . O10 O 0.27605(15) 0.1996(3) 0.10003(17) 0.0421(7) Uani 1 1 d . . . C11 C 0.2499(2) 0.2224(4) 0.1614(2) 0.0366(10) Uani 1 1 d . . . C12 C 0.1966(2) 0.3061(4) 0.1626(2) 0.0344(9) Uani 1 1 d . . . C13 C 0.1742(2) 0.3233(4) 0.2308(3) 0.0419(11) Uani 1 1 d . . . H13A H 0.1382 0.3784 0.2318 0.050 Uiso 1 1 calc R . . C14 C 0.2030(2) 0.2628(4) 0.2956(3) 0.0491(12) Uani 1 1 d . . . H14A H 0.1878 0.2766 0.3412 0.059 Uiso 1 1 calc R . . C15 C 0.2551(3) 0.1804(5) 0.2936(3) 0.0528(13) Uani 1 1 d . . . H15A H 0.2756 0.1382 0.3383 0.063 Uiso 1 1 calc R . . C16 C 0.2773(2) 0.1596(4) 0.2276(3) 0.0464(11) Uani 1 1 d . . . H16A H 0.3118 0.1013 0.2271 0.056 Uiso 1 1 calc R . . N21 N 0.17704(17) 0.3531(3) 0.02757(19) 0.0359(8) Uani 1 1 d . . . C22 C 0.16485(19) 0.3760(3) 0.0959(2) 0.0315(9) Uani 1 1 d . . . C23 C 0.11966(19) 0.4745(3) 0.0906(2) 0.0317(9) Uani 1 1 d . . . H23A H 0.1023 0.5091 0.1307 0.038 Uiso 1 1 calc R . . C24 C 0.10590(19) 0.5102(3) 0.0161(2) 0.0288(8) Uani 1 1 d . . . N25 N 0.14163(17) 0.4350(3) -0.02077(19) 0.0339(8) Uani 1 1 d . . . H25A H 0.1417 0.4391 -0.0694 0.041 Uiso 1 1 calc R . . C31 C 0.06480(19) 0.6115(3) -0.0206(2) 0.0297(8) Uani 1 1 d . . . C32 C 0.0566(2) 0.6337(4) -0.0972(2) 0.0386(10) Uani 1 1 d . . . H32A H 0.0770 0.5825 -0.1280 0.046 Uiso 1 1 calc R . . C33 C 0.0182(3) 0.7314(4) -0.1289(3) 0.0525(13) Uani 1 1 d . . . H33A H 0.0123 0.7462 -0.1817 0.063 Uiso 1 1 calc R . . C34 C -0.0118(3) 0.8076(5) -0.0849(3) 0.0534(13) Uani 1 1 d . . . H34A H -0.0373 0.8748 -0.1071 0.064 Uiso 1 1 calc R . . C35 C -0.0041(3) 0.7848(4) -0.0089(3) 0.0500(12) Uani 1 1 d . . . H35A H -0.0249 0.8359 0.0216 0.060 Uiso 1 1 calc R . . C36 C 0.0338(2) 0.6875(4) 0.0234(3) 0.0414(10) Uani 1 1 d . . . H36A H 0.0389 0.6722 0.0760 0.050 Uiso 1 1 calc R . . O1 O 0.32502(17) 0.4016(3) 0.02554(19) 0.0538(9) Uani 1 1 d D . . H1 H 0.3343 0.4189 0.0711 0.081 Uiso 1 1 d D . . C1 C 0.3368(3) 0.5008(4) -0.0198(3) 0.0599(14) Uani 1 1 d D . . H1A H 0.3163 0.4835 -0.0735 0.072 Uiso 1 1 calc R . . H1B H 0.3871 0.5109 -0.0149 0.072 Uiso 1 1 calc R . . C2 C 0.3076(3) 0.6130(5) 0.0017(4) 0.0806(19) Uani 1 1 d . . . H2A H 0.3129 0.6754 -0.0345 0.121 Uiso 1 1 calc R . . H2B H 0.3320 0.6364 0.0527 0.121 Uiso 1 1 calc R . . H2C H 0.2586 0.6018 0.0012 0.121 Uiso 1 1 calc R . . O2 O 0.4142(2) 0.4102(3) 0.1581(2) 0.0670(11) Uani 1 1 d . . . H2D H 0.4337 0.3485 0.1784 0.101 Uiso 1 1 calc R . . C3 C 0.3980(7) 0.4827(8) 0.2129(6) 0.154(4) Uani 1 1 d DU . . H3A H 0.3584 0.5322 0.1879 0.184 Uiso 1 1 calc R . . H3B H 0.4375 0.5374 0.2290 0.184 Uiso 1 1 calc R . . C4 C 0.3817(5) 0.4369(9) 0.2795(5) 0.123(3) Uani 1 1 d D . . H4A H 0.3726 0.5026 0.3116 0.184 Uiso 1 1 calc R . . H4B H 0.4204 0.3895 0.3071 0.184 Uiso 1 1 calc R . . H4C H 0.3406 0.3866 0.2661 0.184 Uiso 1 1 calc R . . Cl1 Cl 0.5000 0.11755(14) 0.2500 0.0516(5) Uani 1 2 d S . . O3 O 0.4822(5) 0.1860(7) 0.1851(4) 0.190(3) Uani 1 1 d U . . O4 O 0.5539(2) 0.0447(6) 0.2391(3) 0.1088(19) Uani 1 1 d U . . 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 0.0327(5) 0.0366(5) 0.0388(5) 0.0048(4) 0.0104(4) 0.0113(4) O10 0.0356(16) 0.0491(17) 0.0429(17) 0.0094(14) 0.0115(13) 0.0186(14) C11 0.030(2) 0.041(2) 0.038(2) 0.0034(18) 0.0053(17) 0.0033(17) C12 0.033(2) 0.032(2) 0.038(2) 0.0040(18) 0.0058(17) 0.0024(18) C13 0.040(2) 0.042(3) 0.044(3) 0.007(2) 0.0088(19) 0.009(2) C14 0.052(3) 0.060(3) 0.037(2) 0.011(2) 0.014(2) 0.014(2) C15 0.052(3) 0.060(3) 0.044(3) 0.020(2) 0.006(2) 0.015(2) C16 0.040(3) 0.051(3) 0.047(3) 0.012(2) 0.007(2) 0.016(2) N21 0.0323(18) 0.0385(19) 0.0369(19) 0.0059(16) 0.0072(15) 0.0091(15) C22 0.026(2) 0.032(2) 0.036(2) 0.0027(17) 0.0051(16) 0.0008(17) C23 0.028(2) 0.032(2) 0.035(2) -0.0017(17) 0.0079(16) 0.0014(16) C24 0.0217(18) 0.031(2) 0.034(2) 0.0002(16) 0.0078(15) -0.0012(16) N25 0.0334(18) 0.0382(19) 0.0312(18) 0.0052(15) 0.0090(14) 0.0111(15) C31 0.0242(19) 0.029(2) 0.037(2) 0.0013(17) 0.0075(16) -0.0007(16) C32 0.039(2) 0.041(2) 0.036(2) 0.0028(19) 0.0091(18) 0.0042(19) C33 0.062(3) 0.054(3) 0.039(3) 0.012(2) 0.005(2) 0.013(2) C34 0.051(3) 0.046(3) 0.062(3) 0.016(2) 0.007(2) 0.017(2) C35 0.049(3) 0.043(3) 0.060(3) 0.001(2) 0.017(2) 0.018(2) C36 0.044(3) 0.041(2) 0.040(2) 0.003(2) 0.013(2) 0.011(2) O1 0.053(2) 0.0443(18) 0.062(2) 0.0028(16) 0.0073(16) -0.0052(16) C1 0.072(4) 0.046(3) 0.069(4) -0.005(3) 0.031(3) -0.007(3) C2 0.075(4) 0.055(3) 0.112(5) 0.005(3) 0.019(4) 0.004(3) O2 0.074(3) 0.057(2) 0.063(2) -0.0033(19) -0.0012(19) 0.015(2) C3 0.251(12) 0.104(6) 0.119(7) -0.003(6) 0.070(8) 0.070(7) C4 0.113(7) 0.156(8) 0.111(7) -0.051(6) 0.052(5) -0.042(6) Cl1 0.0793(12) 0.0386(9) 0.0478(10) 0.000 0.0376(9) 0.000 O3 0.319(8) 0.162(5) 0.132(5) 0.094(4) 0.146(5) 0.141(5) O4 0.061(3) 0.193(5) 0.081(3) 0.013(3) 0.034(2) 0.045(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O10 1.860(3) 7 ? Mn1 O10 1.860(3) . ? Mn1 N21 2.001(3) . ? Mn1 N21 2.001(3) 7 ? Mn1 O1 2.247(3) . ? Mn1 O1 2.247(3) 7 ? O10 C11 1.347(5) . ? C11 C16 1.396(6) . ? C11 C12 1.420(6) . ? C12 C13 1.411(6) . ? C12 C22 1.464(5) . ? C13 C14 1.370(6) . ? C13 H13A 0.9500 . ? C14 C15 1.395(7) . ? C14 H14A 0.9500 . ? C15 C16 1.377(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N21 C22 1.334(5) . ? N21 N25 1.358(4) . ? C22 C23 1.417(5) . ? C23 C24 1.376(6) . ? C23 H23A 0.9500 . ? C24 N25 1.366(5) . ? C24 C31 1.475(5) . ? N25 H25A 0.8800 . ? C31 C32 1.381(6) . ? C31 C36 1.398(6) . ? C32 C33 1.390(6) . ? C32 H32A 0.9500 . ? C33 C34 1.388(7) . ? C33 H33A 0.9500 . ? C34 C35 1.374(7) . ? C34 H34A 0.9500 . ? C35 C36 1.386(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? O1 C1 1.433(6) . ? O1 H1 0.8280 . ? C1 C2 1.476(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O2 C3 1.373(9) . ? O2 H2D 0.8400 . ? C3 C4 1.410(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? Cl1 O3 1.385(5) 2_655 ? Cl1 O3 1.385(5) . ? Cl1 O4 1.395(5) 2_655 ? Cl1 O4 1.395(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Mn1 O10 180.00(19) 7 . ? O10 Mn1 N21 89.97(13) 7 . ? O10 Mn1 N21 90.03(13) . . ? O10 Mn1 N21 90.03(13) 7 7 ? O10 Mn1 N21 89.97(13) . 7 ? N21 Mn1 N21 180.0(2) . 7 ? O10 Mn1 O1 90.14(13) 7 . ? O10 Mn1 O1 89.86(13) . . ? N21 Mn1 O1 89.55(13) . . ? N21 Mn1 O1 90.45(13) 7 . ? O10 Mn1 O1 89.86(13) 7 7 ? O10 Mn1 O1 90.14(13) . 7 ? N21 Mn1 O1 90.45(13) . 7 ? N21 Mn1 O1 89.55(13) 7 7 ? O1 Mn1 O1 180.00(14) . 7 ? C11 O10 Mn1 131.8(3) . . ? O10 C11 C16 117.5(4) . . ? O10 C11 C12 124.0(4) . . ? C16 C11 C12 118.6(4) . . ? C13 C12 C11 118.6(4) . . ? C13 C12 C22 119.0(4) . . ? C11 C12 C22 122.4(4) . . ? C14 C13 C12 121.8(4) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C15 119.0(4) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C16 C15 C14 120.8(4) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C11 121.2(4) . . ? C15 C16 H16A 119.4 . . ? C11 C16 H16A 119.4 . . ? C22 N21 N25 107.1(3) . . ? C22 N21 Mn1 128.8(3) . . ? N25 N21 Mn1 122.4(3) . . ? N21 C22 C23 109.0(3) . . ? N21 C22 C12 121.8(4) . . ? C23 C22 C12 129.1(4) . . ? C24 C23 C22 106.6(3) . . ? C24 C23 H23A 126.7 . . ? C22 C23 H23A 126.7 . . ? N25 C24 C23 106.4(3) . . ? N25 C24 C31 123.6(3) . . ? C23 C24 C31 129.9(4) . . ? N21 N25 C24 110.9(3) . . ? N21 N25 H25A 124.5 . . ? C24 N25 H25A 124.5 . . ? C32 C31 C36 119.3(4) . . ? C32 C31 C24 121.8(4) . . ? C36 C31 C24 119.0(4) . . ? C31 C32 C33 119.6(4) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C34 C33 C32 121.1(4) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C35 C34 C33 119.3(4) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C34 C35 C36 120.2(4) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C35 C36 C31 120.6(4) . . ? C35 C36 H36A 119.7 . . ? C31 C36 H36A 119.7 . . ? C1 O1 Mn1 131.0(3) . . ? C1 O1 H1 110.9 . . ? Mn1 O1 H1 112.3 . . ? O1 C1 C2 113.3(5) . . ? O1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 O2 H2D 109.5 . . ? O2 C3 C4 122.0(8) . . ? O2 C3 H3A 106.8 . . ? C4 C3 H3A 106.8 . . ? O2 C3 H3B 106.8 . . ? C4 C3 H3B 106.8 . . ? H3A C3 H3B 106.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 Cl1 O3 112.4(7) 2_655 . ? O3 Cl1 O4 105.7(3) 2_655 2_655 ? O3 Cl1 O4 112.4(5) . 2_655 ? O3 Cl1 O4 112.4(5) 2_655 . ? O3 Cl1 O4 105.7(3) . . ? O4 Cl1 O4 108.1(5) 2_655 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.201 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.077 #============================================================================= data_mvc307 _database_code_depnum_ccdc_archive 'CCDC 858619' #TrackingRef 'mvc307.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Mn N7 O2' _chemical_formula_sum 'C30 H22 Mn N7 O2' _chemical_formula_weight 567.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.6920(10) _cell_length_b 12.8650(10) _cell_length_c 22.539(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.320(10) _cell_angle_gamma 90.00 _cell_volume 2493.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23888 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8840 _exptl_absorpt_correction_T_max 0.9037 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23888 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5697 _reflns_number_gt 4468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_cell_refinement 'DirAx (Duisenberg 1992)' _computing_data_reduction 'COLLECT/EVAL (Nonius, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXTL (Sheldrick, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+1.3946P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5697 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.37813(4) 0.72453(2) 0.458861(14) 0.02026(10) Uani 1 1 d . . . N1 N 0.4922(2) 0.84226(16) 0.41893(10) 0.0332(5) Uani 1 1 d . . . N2 N 0.5064(2) 0.93320(15) 0.42399(9) 0.0264(4) Uani 1 1 d . . . N3 N 0.5187(2) 1.02342(16) 0.42509(11) 0.0402(5) Uani 1 1 d . . . N11 N 0.51814(19) 0.60840(13) 0.44480(8) 0.0207(4) Uani 1 1 d . . . N12 N 0.4983(2) 0.55413(14) 0.39321(8) 0.0223(4) Uani 1 1 d . . . H12A H 0.4208 0.5637 0.3640 0.027 Uiso 1 1 calc R . . C13 C 0.6121(2) 0.48322(16) 0.39194(10) 0.0218(4) Uani 1 1 d . . . C14 C 0.6184(2) 0.41758(17) 0.33946(10) 0.0225(4) Uani 1 1 d . . . C15 C 0.5363(3) 0.44295(19) 0.28385(11) 0.0296(5) Uani 1 1 d . . . H15A H 0.4735 0.5037 0.2798 0.036 Uiso 1 1 calc R . . C16 C 0.5449(3) 0.3807(2) 0.23428(11) 0.0334(5) Uani 1 1 d . . . H16A H 0.4864 0.3980 0.1967 0.040 Uiso 1 1 calc R . . C17 C 0.6385(3) 0.29367(19) 0.23961(12) 0.0335(6) Uani 1 1 d . . . H17A H 0.6457 0.2516 0.2055 0.040 Uiso 1 1 calc R . . C18 C 0.7215(3) 0.26760(19) 0.29439(12) 0.0370(6) Uani 1 1 d . . . H18A H 0.7860 0.2077 0.2979 0.044 Uiso 1 1 calc R . . C19 C 0.7112(3) 0.32855(18) 0.34446(11) 0.0303(5) Uani 1 1 d . . . H19A H 0.7675 0.3096 0.3822 0.036 Uiso 1 1 calc R . . C110 C 0.7107(2) 0.49345(16) 0.44567(10) 0.0232(4) Uani 1 1 d . . . H11A H 0.8022 0.4543 0.4583 0.028 Uiso 1 1 calc R . . C111 C 0.6487(2) 0.57311(16) 0.47786(10) 0.0219(4) Uani 1 1 d . . . C112 C 0.7033(2) 0.61665(16) 0.53674(10) 0.0218(4) Uani 1 1 d . . . C113 C 0.8384(3) 0.57625(18) 0.57112(11) 0.0287(5) Uani 1 1 d . . . H11B H 0.8938 0.5221 0.5548 0.034 Uiso 1 1 calc R . . C114 C 0.8921(3) 0.6129(2) 0.62737(11) 0.0349(6) Uani 1 1 d . . . H11C H 0.9825 0.5838 0.6500 0.042 Uiso 1 1 calc R . . C115 C 0.8129(3) 0.6933(2) 0.65111(11) 0.0351(6) Uani 1 1 d . . . H11D H 0.8512 0.7203 0.6896 0.042 Uiso 1 1 calc R . . C116 C 0.6788(3) 0.73424(18) 0.61904(10) 0.0288(5) Uani 1 1 d . . . H11E H 0.6251 0.7885 0.6360 0.035 Uiso 1 1 calc R . . C117 C 0.6215(2) 0.69634(17) 0.56188(10) 0.0228(4) Uani 1 1 d . . . O118 O 0.48707(18) 0.73715(12) 0.53481(7) 0.0274(3) Uani 1 1 d . . . N21 N 0.1959(2) 0.79512(13) 0.48509(8) 0.0216(4) Uani 1 1 d . . . N22 N 0.2047(2) 0.85389(14) 0.53555(8) 0.0224(4) Uani 1 1 d . . . H22A H 0.2920 0.8714 0.5582 0.027 Uiso 1 1 calc R . . C23 C 0.0611(2) 0.88184(16) 0.54634(10) 0.0215(4) Uani 1 1 d . . . C24 C 0.0348(2) 0.94592(16) 0.59786(9) 0.0214(4) Uani 1 1 d . . . C25 C 0.1552(3) 0.97984(18) 0.64096(10) 0.0280(5) Uani 1 1 d . . . H25A H 0.2595 0.9619 0.6374 0.034 Uiso 1 1 calc R . . C26 C 0.1246(3) 1.03954(18) 0.68912(10) 0.0289(5) Uani 1 1 d . . . H26A H 0.2078 1.0626 0.7182 0.035 Uiso 1 1 calc R . . C27 C -0.0269(3) 1.06569(18) 0.69498(10) 0.0282(5) Uani 1 1 d . . . H27A H -0.0482 1.1062 0.7281 0.034 Uiso 1 1 calc R . . C28 C -0.1464(3) 1.03233(19) 0.65236(11) 0.0308(5) Uani 1 1 d . . . H28A H -0.2505 1.0504 0.6562 0.037 Uiso 1 1 calc R . . C29 C -0.1172(3) 0.97316(18) 0.60418(10) 0.0267(5) Uani 1 1 d . . . H29A H -0.2011 0.9509 0.5752 0.032 Uiso 1 1 calc R . . C210 C -0.0434(2) 0.83839(16) 0.50131(10) 0.0230(4) Uani 1 1 d . . . H21A H -0.1535 0.8434 0.4970 0.028 Uiso 1 1 calc R . . C211 C 0.0432(2) 0.78572(15) 0.46326(10) 0.0205(4) Uani 1 1 d . . . C212 C -0.0101(2) 0.73182(16) 0.40688(10) 0.0208(4) Uani 1 1 d . . . C213 C -0.1687(3) 0.73296(17) 0.38408(10) 0.0256(5) Uani 1 1 d . . . H21B H -0.2397 0.7652 0.4067 0.031 Uiso 1 1 calc R . . C214 C -0.2243(3) 0.68820(18) 0.32941(11) 0.0294(5) Uani 1 1 d . . . H21C H -0.3324 0.6898 0.3147 0.035 Uiso 1 1 calc R . . C215 C -0.1219(3) 0.64108(17) 0.29616(11) 0.0282(5) Uani 1 1 d . . . H21D H -0.1595 0.6104 0.2585 0.034 Uiso 1 1 calc R . . C216 C 0.0352(3) 0.63876(17) 0.31780(10) 0.0256(5) Uani 1 1 d . . . H21E H 0.1047 0.6061 0.2948 0.031 Uiso 1 1 calc R . . C217 C 0.0937(2) 0.68359(16) 0.37293(10) 0.0215(4) Uani 1 1 d . . . O218 O 0.24809(17) 0.67788(13) 0.39088(7) 0.0276(4) Uani 1 1 d . . . 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 0.01770(16) 0.02051(17) 0.02298(18) -0.00113(13) 0.00432(12) 0.00275(13) N1 0.0349(11) 0.0263(11) 0.0418(12) 0.0041(9) 0.0172(9) 0.0023(9) N2 0.0178(9) 0.0332(12) 0.0293(10) -0.0012(8) 0.0071(7) -0.0009(8) N3 0.0307(11) 0.0277(11) 0.0628(16) -0.0057(10) 0.0092(10) -0.0050(9) N11 0.0200(8) 0.0196(9) 0.0230(9) -0.0002(7) 0.0043(7) 0.0017(7) N12 0.0217(9) 0.0231(9) 0.0224(9) -0.0013(7) 0.0039(7) 0.0033(7) C13 0.0200(10) 0.0189(10) 0.0283(12) 0.0031(8) 0.0092(8) 0.0015(8) C14 0.0209(10) 0.0225(10) 0.0261(11) -0.0013(9) 0.0102(8) -0.0010(9) C15 0.0246(11) 0.0313(12) 0.0336(13) -0.0029(10) 0.0064(9) 0.0036(10) C16 0.0264(12) 0.0449(14) 0.0295(13) -0.0052(11) 0.0058(9) -0.0031(11) C17 0.0346(13) 0.0330(13) 0.0362(14) -0.0115(10) 0.0163(11) -0.0054(11) C18 0.0472(15) 0.0246(12) 0.0430(15) -0.0019(11) 0.0192(12) 0.0062(11) C19 0.0359(13) 0.0257(12) 0.0311(13) 0.0027(10) 0.0109(10) 0.0046(10) C110 0.0226(10) 0.0218(10) 0.0258(11) 0.0038(9) 0.0058(8) 0.0044(9) C111 0.0204(10) 0.0189(10) 0.0272(11) 0.0062(8) 0.0065(8) -0.0011(8) C112 0.0218(10) 0.0192(10) 0.0245(11) 0.0036(8) 0.0038(8) -0.0025(8) C113 0.0249(11) 0.0257(11) 0.0348(13) 0.0023(10) 0.0020(9) 0.0027(9) C114 0.0300(12) 0.0356(13) 0.0359(14) 0.0042(11) -0.0061(10) 0.0021(11) C115 0.0378(14) 0.0347(13) 0.0295(13) -0.0017(10) -0.0060(10) -0.0026(11) C116 0.0310(12) 0.0261(11) 0.0287(12) -0.0008(9) 0.0029(9) -0.0008(10) C117 0.0219(10) 0.0214(10) 0.0251(11) 0.0053(8) 0.0029(8) -0.0019(8) O118 0.0257(8) 0.0290(8) 0.0267(8) -0.0044(6) 0.0004(6) 0.0087(7) N21 0.0203(9) 0.0212(9) 0.0238(9) -0.0013(7) 0.0050(7) 0.0020(7) N22 0.0191(9) 0.0243(9) 0.0242(9) -0.0023(7) 0.0043(7) 0.0017(7) C23 0.0203(10) 0.0188(10) 0.0270(11) 0.0044(8) 0.0087(8) 0.0038(8) C24 0.0238(10) 0.0190(10) 0.0228(11) 0.0041(8) 0.0088(8) 0.0018(8) C25 0.0218(11) 0.0313(12) 0.0322(13) 0.0008(10) 0.0079(9) 0.0007(9) C26 0.0276(12) 0.0319(12) 0.0268(12) 0.0000(9) 0.0026(9) -0.0009(10) C27 0.0354(12) 0.0278(12) 0.0229(12) 0.0001(9) 0.0093(9) 0.0056(10) C28 0.0247(11) 0.0395(14) 0.0294(13) -0.0001(10) 0.0084(9) 0.0093(10) C29 0.0226(11) 0.0308(12) 0.0267(12) -0.0021(9) 0.0041(9) 0.0039(9) C210 0.0186(10) 0.0228(10) 0.0289(12) 0.0019(9) 0.0075(8) 0.0009(9) C211 0.0195(10) 0.0163(10) 0.0267(11) 0.0038(8) 0.0066(8) 0.0017(8) C212 0.0209(10) 0.0163(9) 0.0254(11) 0.0032(8) 0.0041(8) 0.0003(8) C213 0.0216(10) 0.0228(11) 0.0333(12) 0.0026(9) 0.0068(9) 0.0003(9) C214 0.0217(11) 0.0273(12) 0.0380(14) 0.0030(10) 0.0001(9) -0.0033(9) C215 0.0302(12) 0.0241(11) 0.0284(12) 0.0006(9) -0.0018(9) -0.0040(9) C216 0.0273(11) 0.0223(11) 0.0278(12) -0.0003(9) 0.0061(9) 0.0009(9) C217 0.0197(10) 0.0181(10) 0.0269(11) 0.0024(8) 0.0040(8) -0.0002(8) O218 0.0188(7) 0.0340(9) 0.0296(9) -0.0076(7) 0.0027(6) 0.0052(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O118 1.8395(16) . ? Mn1 O218 1.8666(15) . ? Mn1 N11 1.9812(17) . ? Mn1 N21 1.9887(18) . ? Mn1 N1 2.085(2) . ? N1 N2 1.180(3) . ? N2 N3 1.165(3) . ? N11 C111 1.343(3) . ? N11 N12 1.346(2) . ? N12 C13 1.349(3) . ? N12 H12A 0.8800 . ? C13 C110 1.385(3) . ? C13 C14 1.461(3) . ? C14 C15 1.388(3) . ? C14 C19 1.396(3) . ? C15 C16 1.385(3) . ? C15 H15A 0.9500 . ? C16 C17 1.379(4) . ? C16 H16A 0.9500 . ? C17 C18 1.378(4) . ? C17 H17A 0.9500 . ? C18 C19 1.388(3) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C110 C111 1.407(3) . ? C110 H11A 0.9500 . ? C111 C112 1.455(3) . ? C112 C113 1.409(3) . ? C112 C117 1.412(3) . ? C113 C114 1.370(3) . ? C113 H11B 0.9500 . ? C114 C115 1.391(4) . ? C114 H11C 0.9500 . ? C115 C116 1.383(3) . ? C115 H11D 0.9500 . ? C116 C117 1.400(3) . ? C116 H11E 0.9500 . ? C117 O118 1.344(3) . ? N21 C211 1.352(3) . ? N21 N22 1.359(2) . ? N22 C23 1.355(3) . ? N22 H22A 0.8800 . ? C23 C210 1.379(3) . ? C23 C24 1.469(3) . ? C24 C25 1.391(3) . ? C24 C29 1.394(3) . ? C25 C26 1.386(3) . ? C25 H25A 0.9500 . ? C26 C27 1.384(3) . ? C26 H26A 0.9500 . ? C27 C28 1.377(3) . ? C27 H27A 0.9500 . ? C28 C29 1.379(3) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C210 C211 1.396(3) . ? C210 H21A 0.9500 . ? C211 C212 1.463(3) . ? C212 C213 1.401(3) . ? C212 C217 1.409(3) . ? C213 C214 1.382(3) . ? C213 H21B 0.9500 . ? C214 C215 1.383(3) . ? C214 H21C 0.9500 . ? C215 C216 1.383(3) . ? C215 H21D 0.9500 . ? C216 C217 1.397(3) . ? C216 H21E 0.9500 . ? C217 O218 1.346(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O118 Mn1 O218 163.99(7) . . ? O118 Mn1 N11 88.28(7) . . ? O218 Mn1 N11 86.52(7) . . ? O118 Mn1 N21 90.46(7) . . ? O218 Mn1 N21 88.68(7) . . ? N11 Mn1 N21 157.83(7) . . ? O118 Mn1 N1 97.16(8) . . ? O218 Mn1 N1 98.55(8) . . ? N11 Mn1 N1 97.89(8) . . ? N21 Mn1 N1 104.22(8) . . ? N2 N1 Mn1 136.72(17) . . ? N3 N2 N1 175.7(3) . . ? C111 N11 N12 107.24(17) . . ? C111 N11 Mn1 130.95(15) . . ? N12 N11 Mn1 121.63(13) . . ? N11 N12 C13 111.49(17) . . ? N11 N12 H12A 124.3 . . ? C13 N12 H12A 124.3 . . ? N12 C13 C110 106.26(18) . . ? N12 C13 C14 121.45(19) . . ? C110 C13 C14 132.22(19) . . ? C15 C14 C19 118.8(2) . . ? C15 C14 C13 121.4(2) . . ? C19 C14 C13 119.9(2) . . ? C16 C15 C14 120.8(2) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 120.1(2) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 120.3(2) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 120.2(2) . . ? C18 C19 H19A 119.9 . . ? C14 C19 H19A 119.9 . . ? C13 C110 C111 106.60(18) . . ? C13 C110 H11A 126.7 . . ? C111 C110 H11A 126.7 . . ? N11 C111 C110 108.41(19) . . ? N11 C111 C112 120.89(19) . . ? C110 C111 C112 130.70(19) . . ? C113 C112 C117 118.4(2) . . ? C113 C112 C111 119.7(2) . . ? C117 C112 C111 121.92(19) . . ? C114 C113 C112 121.8(2) . . ? C114 C113 H11B 119.1 . . ? C112 C113 H11B 119.1 . . ? C113 C114 C115 119.4(2) . . ? C113 C114 H11C 120.3 . . ? C115 C114 H11C 120.3 . . ? C116 C115 C114 120.5(2) . . ? C116 C115 H11D 119.7 . . ? C114 C115 H11D 119.7 . . ? C115 C116 C117 120.6(2) . . ? C115 C116 H11E 119.7 . . ? C117 C116 H11E 119.7 . . ? O118 C117 C116 116.9(2) . . ? O118 C117 C112 123.8(2) . . ? C116 C117 C112 119.3(2) . . ? C117 O118 Mn1 133.21(15) . . ? C211 N21 N22 106.74(17) . . ? C211 N21 Mn1 129.27(15) . . ? N22 N21 Mn1 123.50(13) . . ? C23 N22 N21 110.86(17) . . ? C23 N22 H22A 124.6 . . ? N21 N22 H22A 124.6 . . ? N22 C23 C210 106.64(19) . . ? N22 C23 C24 122.95(19) . . ? C210 C23 C24 130.41(19) . . ? C25 C24 C29 118.6(2) . . ? C25 C24 C23 122.73(19) . . ? C29 C24 C23 118.70(19) . . ? C26 C25 C24 120.7(2) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C27 C26 C25 120.2(2) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C28 C27 C26 119.3(2) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C27 C28 C29 121.0(2) . . ? C27 C28 H28A 119.5 . . ? C29 C28 H28A 119.5 . . ? C28 C29 C24 120.3(2) . . ? C28 C29 H29A 119.9 . . ? C24 C29 H29A 119.9 . . ? C23 C210 C211 107.02(18) . . ? C23 C210 H21A 126.5 . . ? C211 C210 H21A 126.5 . . ? N21 C211 C210 108.74(19) . . ? N21 C211 C212 121.94(19) . . ? C210 C211 C212 129.26(19) . . ? C213 C212 C217 118.6(2) . . ? C213 C212 C211 119.0(2) . . ? C217 C212 C211 122.25(19) . . ? C214 C213 C212 121.4(2) . . ? C214 C213 H21B 119.3 . . ? C212 C213 H21B 119.3 . . ? C215 C214 C213 119.7(2) . . ? C215 C214 H21C 120.1 . . ? C213 C214 H21C 120.1 . . ? C216 C215 C214 119.9(2) . . ? C216 C215 H21D 120.1 . . ? C214 C215 H21D 120.1 . . ? C215 C216 C217 121.3(2) . . ? C215 C216 H21E 119.4 . . ? C217 C216 H21E 119.4 . . ? O218 C217 C216 117.61(19) . . ? O218 C217 C212 123.34(19) . . ? C216 C217 C212 119.05(19) . . ? C217 O218 Mn1 133.47(14) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.310 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.061 data_LEID72 _database_code_depnum_ccdc_archive 'CCDC 861014' _publ_section_abstract ; ; _publ_section_references ; Beurskens, P. T., Beurskens, G., Bosman, W. P., Gelder, R. de, Garc\'ia-Granda, S., Gould, R. O., Isra\"el, R. & Smits, J. M. M. (1996). DIRDIF-96, A computer program system for crystal structure determination by Patterson methods and direct methods applied to difference structure factors. Crystallography Laboratory, University of Nijmegen, The Netherlands. Beurskens, P. T., Beurskens, G., Strumpel, M. & Nordman, C. E. (1987). In Patterson and Pattersons, pp. 356--367. Glusker, J. P., Patterson, B. K. & Rossi, M., Eds. Oxford, England: Clarendon Press. Duisenberg, A.J.M. (1998). Reflections on area detectors, PhD Thesis, Utrecht University, Utrecht, The Netherlands. International Tables for X-ray Crystallography (1974). Vol. IV, Birmingham, England: Kynoch Press. Nonius B.V. (1999). COLLECT, data collection software. Delft, The Netherlands. Sheldrick, G.M. (1996). SADABS. Program for Emperical Absorption Correction. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97, Program for the refinement of crystal structures. University of G\"ottingen, Germany. Spek, A. L. (2003). PLATON. A Multipurpose Crystallographic Tool. Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #============================================================================== _audit_creation_method 'SHELXL, adapted and expanded' _audit_creation_date 2006-07-27 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H29 Mn N6 O5' _chemical_formula_weight 620.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1408(4) _cell_length_b 13.807(4) _cell_length_c 18.780(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.958(13) _cell_angle_gamma 90.00 _cell_volume 2777.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 370 _cell_measurement_theta_min 2.260 _cell_measurement_theta_max 27.510 _exptl_crystal_description 'rather regular rod' _exptl_crystal_colour brown-green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS multiscan (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method 'area detector \f and \w scan' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.000 _diffrn_reflns_number 24761 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5620 _reflns_number_gt 3285 _reflns_number_observed 3285 _reflns_threshold_expression >2sigma(I) _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Nonius "Collect" program suite (Nonius, 1999) ; _computing_cell_refinement ? _computing_data_reduction ; Nonius "EvalCCD" program suite (Duisenberg, 1998) ; _computing_structure_solution ; DIRDIF (Beurskens et al., 1996), PATTY (Beurskens et al., 1987) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLATON (Spek, 2003) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0070P)^2^+7.1454P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5620 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1403 _refine_ls_R_factor_gt 0.0667 _refine_ls_R_factor_obs 0.0667 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_all 0.1115 _refine_ls_wR_factor_gt 0.0920 _refine_ls_wR_factor_obs 0.0920 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_shift/esd_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.19042(5) 0.12847(5) 0.48469(3) 0.02252(16) Uani 1 d . . . O1A O 0.0799(2) 0.1291(2) 0.54236(13) 0.0242(6) Uani 1 d . . . N1A N 0.4524(3) 0.1638(2) 0.57620(17) 0.0251(8) Uani 1 d . . . H1A H 0.4803 0.1602 0.5373 0.030 Uiso 1 calc R . . N2A N 0.3300(3) 0.1617(2) 0.57413(17) 0.0216(8) Uani 1 d . . . C1A C 0.0934(3) 0.1474(3) 0.6142(2) 0.0216(9) Uani 1 d . . . C2A C -0.0144(3) 0.1465(3) 0.6383(2) 0.0265(10) Uani 1 d . . . H2A H -0.0926 0.1364 0.6041 0.032 Uiso 1 calc R . . C3A C -0.0068(4) 0.1602(3) 0.7116(2) 0.0319(11) Uani 1 d . . . H3A H -0.0799 0.1586 0.7273 0.038 Uiso 1 calc R . . C4A C 0.1068(4) 0.1765(3) 0.7628(2) 0.0347(11) Uani 1 d . . . H4A H 0.1114 0.1848 0.8132 0.042 Uiso 1 calc R . . C5A C 0.2126(4) 0.1802(3) 0.7393(2) 0.0307(10) Uani 1 d . . . H5A H 0.2898 0.1920 0.7741 0.037 Uiso 1 calc R . . C6A C 0.2091(3) 0.1669(3) 0.6651(2) 0.0238(9) Uani 1 d . . . C7A C 0.3262(3) 0.1690(3) 0.6450(2) 0.0233(9) Uani 1 d . . . C8A C 0.4478(3) 0.1758(3) 0.6907(2) 0.0293(10) Uani 1 d . . . H8A H 0.4718 0.1819 0.7426 0.035 Uiso 1 calc R . . C9A C 0.5251(3) 0.1720(3) 0.6458(2) 0.0287(10) Uani 1 d . . . C10A C 0.6641(3) 0.1698(4) 0.6653(2) 0.0422(12) Uani 1 d . . . H10A H 0.6923 0.1033 0.6655 0.063 Uiso 1 calc R . . H10B H 0.6980 0.1980 0.7140 0.063 Uiso 1 calc R . . H10C H 0.6924 0.2068 0.6290 0.063 Uiso 1 calc R . . O1B O 0.2984(2) 0.1313(2) 0.42568(13) 0.0273(7) Uani 1 d . . . N1B N -0.0715(3) 0.0881(2) 0.39825(17) 0.0229(8) Uani 1 d . . . H1B H -0.0966 0.0880 0.4382 0.028 Uiso 1 calc R . . N2B N 0.0492(3) 0.0930(2) 0.39796(16) 0.0206(7) Uani 1 d . . . C1B C 0.2806(3) 0.1168(3) 0.3531(2) 0.0231(9) Uani 1 d . . . C2B C 0.3851(3) 0.1219(3) 0.3264(2) 0.0295(10) Uani 1 d . . . H2B H 0.4638 0.1340 0.3595 0.035 Uiso 1 calc R . . C3B C 0.3755(4) 0.1098(3) 0.2526(2) 0.0362(11) Uani 1 d . . . H3B H 0.4471 0.1147 0.2355 0.043 Uiso 1 calc R . . C4B C 0.2610(4) 0.0906(3) 0.2034(2) 0.0367(11) Uani 1 d . . . H4B H 0.2541 0.0814 0.1529 0.044 Uiso 1 calc R . . C5B C 0.1576(4) 0.0849(3) 0.2292(2) 0.0329(11) Uani 1 d . . . H5B H 0.0797 0.0719 0.1955 0.040 Uiso 1 calc R . . C6B C 0.1636(3) 0.0977(3) 0.3036(2) 0.0239(9) Uani 1 d . . . C7B C 0.0488(3) 0.0927(3) 0.3264(2) 0.0217(9) Uani 1 d . . . C8B C -0.0742(3) 0.0869(3) 0.2822(2) 0.0274(10) Uani 1 d . . . H8B H -0.1010 0.0855 0.2302 0.033 Uiso 1 calc R . . C9B C -0.1480(3) 0.0834(3) 0.3295(2) 0.0262(10) Uani 1 d . . . C10B C -0.2861(3) 0.0776(3) 0.3136(2) 0.0349(11) Uani 1 d . . . H10D H -0.3082 0.0224 0.3393 0.052 Uiso 1 calc R . . H10E H -0.3228 0.0702 0.2607 0.052 Uiso 1 calc R . . H10F H -0.3173 0.1365 0.3303 0.052 Uiso 1 calc R . . O1C O -0.2051(3) 0.2713(2) 0.4756(2) 0.0483(9) Uani 1 d . . . H1C H -0.2663 0.2398 0.4798 0.072 Uiso 1 calc R . . N1C N 0.1312(3) 0.2868(2) 0.45498(18) 0.0286(8) Uani 1 d . . . N2C N 0.0175(3) 0.3064(2) 0.46466(18) 0.0294(8) Uani 1 d . . . H2 H -0.0187 0.2698 0.4903 0.035 Uiso 1 calc R . . C1C C -0.2402(4) 0.3637(3) 0.4566(2) 0.0320(10) Uani 1 d . . . C2C C -0.3555(4) 0.3986(3) 0.4589(2) 0.0380(12) Uani 1 d . . . H2C H -0.4120 0.3581 0.4737 0.046 Uiso 1 calc R . . C3C C -0.3867(4) 0.4932(4) 0.4391(2) 0.0398(12) Uani 1 d . . . H3C H -0.4653 0.5170 0.4402 0.048 Uiso 1 calc R . . C4C C -0.3044(4) 0.5532(3) 0.4179(2) 0.0390(12) Uani 1 d . . . H4C H -0.3261 0.6180 0.4052 0.047 Uiso 1 calc R . . C5C C -0.1899(4) 0.5182(3) 0.4151(2) 0.0345(11) Uani 1 d . . . H5C H -0.1344 0.5594 0.4000 0.041 Uiso 1 calc R . . C6C C -0.1552(4) 0.4229(3) 0.4344(2) 0.0296(10) Uani 1 d . . . C7C C -0.0337(4) 0.3881(3) 0.4306(2) 0.0278(10) Uani 1 d . . . C8C C 0.0526(4) 0.4240(3) 0.3970(2) 0.0343(11) Uani 1 d . . . H8C H 0.0454 0.4808 0.3685 0.041 Uiso 1 calc R . . C9C C 0.1527(4) 0.3593(3) 0.4137(2) 0.0309(10) Uani 1 d . . . C10C C 0.2726(4) 0.3631(3) 0.3929(2) 0.0422(12) Uani 1 d . . . H10G H 0.3225 0.3066 0.4124 0.063 Uiso 1 calc R . . H10H H 0.3181 0.4212 0.4133 0.063 Uiso 1 calc R . . H10I H 0.2551 0.3640 0.3394 0.063 Uiso 1 calc R . . O11 O 0.2350(2) -0.03220(19) 0.50822(14) 0.0270(7) Uani 1 d . . . C12 C 0.3370(4) -0.0645(3) 0.5032(2) 0.0297(10) Uani 1 d . . . H12 H 0.3918 -0.0192 0.4916 0.036 Uiso 1 calc R . . O13 O 0.3745(2) -0.1500(2) 0.51162(15) 0.0317(7) Uani 1 d . . . 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 0.0148(3) 0.0292(4) 0.0240(3) -0.0003(3) 0.0059(2) -0.0018(3) O1A 0.0166(13) 0.0352(18) 0.0216(15) -0.0028(13) 0.0065(10) -0.0014(12) N1A 0.0146(17) 0.030(2) 0.032(2) -0.0046(15) 0.0087(14) -0.0022(14) N2A 0.0093(16) 0.025(2) 0.030(2) -0.0003(15) 0.0056(13) -0.0034(13) C1A 0.023(2) 0.019(3) 0.023(2) -0.0011(17) 0.0070(16) 0.0003(17) C2A 0.017(2) 0.033(3) 0.029(2) -0.0022(19) 0.0052(16) -0.0012(18) C3A 0.024(2) 0.043(3) 0.033(3) -0.007(2) 0.0160(18) -0.003(2) C4A 0.033(3) 0.047(3) 0.026(2) -0.005(2) 0.0111(19) -0.004(2) C5A 0.021(2) 0.041(3) 0.029(3) -0.004(2) 0.0063(17) -0.0020(19) C6A 0.019(2) 0.029(3) 0.025(2) 0.0022(18) 0.0074(16) 0.0019(18) C7A 0.023(2) 0.026(3) 0.022(2) -0.0011(17) 0.0071(16) -0.0009(18) C8A 0.021(2) 0.040(3) 0.025(2) -0.0065(19) 0.0028(17) 0.0001(19) C9A 0.019(2) 0.033(3) 0.031(3) -0.0070(19) 0.0019(18) -0.0010(18) C10A 0.019(2) 0.060(4) 0.044(3) -0.013(2) 0.0035(19) -0.004(2) O1B 0.0200(14) 0.0385(19) 0.0251(16) 0.0015(13) 0.0090(11) -0.0041(13) N1B 0.0151(17) 0.032(2) 0.0231(19) 0.0003(15) 0.0079(13) -0.0026(14) N2B 0.0142(17) 0.022(2) 0.027(2) -0.0007(14) 0.0082(13) -0.0018(13) C1B 0.021(2) 0.026(3) 0.025(2) 0.0016(18) 0.0101(16) 0.0011(18) C2B 0.022(2) 0.035(3) 0.034(3) -0.002(2) 0.0125(17) 0.000(2) C3B 0.031(2) 0.048(3) 0.036(3) -0.004(2) 0.020(2) 0.000(2) C4B 0.038(3) 0.050(3) 0.028(3) -0.010(2) 0.018(2) -0.006(2) C5B 0.029(2) 0.038(3) 0.032(3) -0.004(2) 0.0089(19) -0.002(2) C6B 0.019(2) 0.026(3) 0.029(2) -0.0017(18) 0.0104(16) 0.0008(17) C7B 0.021(2) 0.018(2) 0.028(2) 0.0032(17) 0.0105(17) -0.0004(17) C8B 0.020(2) 0.037(3) 0.027(2) 0.0022(19) 0.0075(17) -0.0014(19) C9B 0.015(2) 0.030(3) 0.031(2) 0.0017(19) 0.0018(17) 0.0001(17) C10B 0.020(2) 0.049(3) 0.034(3) 0.006(2) 0.0042(18) 0.000(2) O1C 0.0315(18) 0.031(2) 0.088(3) 0.0170(18) 0.0262(18) 0.0024(15) N1C 0.0190(19) 0.028(2) 0.039(2) 0.0018(17) 0.0084(15) -0.0025(15) N2C 0.0266(19) 0.024(2) 0.039(2) 0.0065(16) 0.0112(15) -0.0006(16) C1C 0.031(2) 0.029(3) 0.033(2) 0.003(2) 0.0034(18) 0.001(2) C2C 0.031(3) 0.041(3) 0.044(3) 0.005(2) 0.013(2) 0.006(2) C3C 0.040(3) 0.048(4) 0.032(3) -0.002(2) 0.010(2) 0.012(2) C4C 0.049(3) 0.034(3) 0.030(3) 0.002(2) 0.005(2) 0.010(2) C5C 0.037(3) 0.032(3) 0.030(3) 0.001(2) 0.0022(19) 0.002(2) C6C 0.027(2) 0.031(3) 0.029(2) -0.0012(19) 0.0026(18) 0.000(2) C7C 0.029(2) 0.021(3) 0.030(2) 0.0016(18) 0.0038(18) -0.0030(19) C8C 0.035(3) 0.032(3) 0.036(3) 0.008(2) 0.009(2) -0.002(2) C9C 0.030(2) 0.030(3) 0.032(2) -0.002(2) 0.0076(18) -0.007(2) C10C 0.040(3) 0.038(3) 0.054(3) 0.004(2) 0.021(2) -0.006(2) O11 0.0192(15) 0.0284(18) 0.0357(17) 0.0027(13) 0.0112(12) 0.0008(12) C12 0.020(2) 0.032(3) 0.039(3) 0.001(2) 0.0091(18) -0.005(2) O13 0.0249(15) 0.027(2) 0.0451(18) 0.0032(14) 0.0131(13) 0.0033(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1B 1.847(2) . Y Mn1 O1A 1.850(2) . Y Mn1 N2B 1.990(3) . Y Mn1 N2A 2.003(3) . Y Mn1 O11 2.289(3) . Y Mn1 N1C 2.308(4) . Y O1A C1A 1.340(4) . Y N1A C9A 1.339(5) . Y N1A N2A 1.354(4) . Y N2A C7A 1.348(5) . Y C1A C2A 1.395(5) . Y C1A C6A 1.404(5) . Y C2A C3A 1.368(5) . Y C3A C4A 1.382(5) . Y C4A C5A 1.369(5) . Y C5A C6A 1.396(5) . Y C6A C7A 1.454(5) . Y C7A C8A 1.393(5) . Y C8A C9A 1.363(5) . Y C9A C10A 1.490(5) . Y O1B C1B 1.337(4) . Y N1B C9B 1.340(4) . Y N1B N2B 1.348(4) . Y N2B C7B 1.342(5) . Y C1B C2B 1.390(5) . Y C1B C6B 1.402(5) . Y C2B C3B 1.369(5) . Y C3B C4B 1.380(5) . Y C4B C5B 1.370(5) . Y C5B C6B 1.391(5) . Y C6B C7B 1.458(5) . Y C7B C8B 1.395(5) . Y C8B C9B 1.366(5) . Y C9B C10B 1.486(5) . Y O1C C1C 1.354(5) . Y N1C C9C 1.327(5) . Y N1C N2C 1.356(4) . Y N2C C7C 1.344(5) . Y C1C C2C 1.384(5) . Y C1C C6C 1.398(6) . Y C2C C3C 1.376(6) . Y C3C C4C 1.375(6) . Y C4C C5C 1.377(6) . Y C5C C6C 1.390(6) . Y C6C C7C 1.458(5) . Y C7C C8C 1.379(5) . Y C8C C9C 1.396(6) . Y C9C C10C 1.492(5) . Y O11 C12 1.249(4) . Y C12 O13 1.248(5) . Y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Mn1 O1A 178.23(13) . . Y O1B Mn1 N2B 90.72(12) . . Y O1A Mn1 N2B 88.67(12) . . Y O1B Mn1 N2A 90.86(12) . . Y O1A Mn1 N2A 89.77(11) . . Y N2B Mn1 N2A 178.13(13) . . Y O1B Mn1 O11 89.64(11) . . Y O1A Mn1 O11 92.03(11) . . Y N2B Mn1 O11 89.99(11) . . Y N2A Mn1 O11 89.03(11) . . Y O1B Mn1 N1C 91.44(12) . . Y O1A Mn1 N1C 86.86(12) . . Y N2B Mn1 N1C 85.78(12) . . Y N2A Mn1 N1C 95.17(12) . . Y O11 Mn1 N1C 175.65(10) . . Y C1A O1A Mn1 133.0(2) . . Y C9A N1A N2A 111.3(3) . . Y C7A N2A N1A 106.0(3) . . Y C7A N2A Mn1 128.2(2) . . Y N1A N2A Mn1 124.9(2) . . Y O1A C1A C2A 117.2(3) . . Y O1A C1A C6A 123.3(3) . . Y C2A C1A C6A 119.5(3) . . Y C3A C2A C1A 120.3(3) . . Y C2A C3A C4A 121.0(4) . . Y C5A C4A C3A 119.1(4) . . Y C4A C5A C6A 121.8(4) . . Y C5A C6A C1A 118.3(3) . . Y C5A C6A C7A 118.4(3) . . Y C1A C6A C7A 123.3(3) . . Y N2A C7A C8A 108.9(3) . . Y N2A C7A C6A 121.9(3) . . Y C8A C7A C6A 129.2(4) . . Y C9A C8A C7A 106.8(4) . . Y N1A C9A C8A 107.0(3) . . Y N1A C9A C10A 123.2(4) . . Y C8A C9A C10A 129.8(4) . . Y C1B O1B Mn1 132.1(2) . . Y C9B N1B N2B 111.7(3) . . Y C7B N2B N1B 106.0(3) . . Y C7B N2B Mn1 127.2(2) . . Y N1B N2B Mn1 125.0(2) . . Y O1B C1B C2B 117.1(3) . . Y O1B C1B C6B 123.6(3) . . Y C2B C1B C6B 119.2(3) . . Y C3B C2B C1B 121.2(4) . . Y C2B C3B C4B 120.1(4) . . Y C5B C4B C3B 119.2(4) . . Y C4B C5B C6B 122.3(4) . . Y C5B C6B C1B 118.0(3) . . Y C5B C6B C7B 119.0(3) . . Y C1B C6B C7B 123.0(3) . . Y N2B C7B C8B 109.2(3) . . Y N2B C7B C6B 122.1(3) . . Y C8B C7B C6B 128.7(3) . . Y C9B C8B C7B 106.5(3) . . Y N1B C9B C8B 106.7(3) . . Y N1B C9B C10B 123.1(3) . . Y C8B C9B C10B 130.2(4) . . Y C9C N1C N2C 104.7(3) . . Y C9C N1C Mn1 140.4(3) . . Y N2C N1C Mn1 111.8(2) . . Y C7C N2C N1C 113.1(3) . . Y O1C C1C C2C 121.6(4) . . Y O1C C1C C6C 117.4(4) . . Y C2C C1C C6C 121.1(4) . . Y C3C C2C C1C 119.3(4) . . Y C4C C3C C2C 120.7(4) . . Y C3C C4C C5C 119.9(4) . . Y C4C C5C C6C 121.1(4) . . Y C5C C6C C1C 117.9(4) . . Y C5C C6C C7C 119.7(4) . . Y C1C C6C C7C 122.4(4) . . Y N2C C7C C8C 105.2(4) . . Y N2C C7C C6C 122.1(4) . . Y C8C C7C C6C 132.6(4) . . Y C7C C8C C9C 106.3(4) . . Y N1C C9C C8C 110.7(4) . . Y N1C C9C C10C 119.9(4) . . Y C8C C9C C10C 129.5(4) . . Y C12 O11 Mn1 119.0(3) . . Y O13 C12 O11 127.5(4) . . Y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A O13 0.87 2.07 2.868(4) 151.4 3_656 N1B H1B O11 0.87 2.20 2.959(4) 145.8 3_556 O1C H1C O13 0.83 1.77 2.583(4) 167.0 3_556 N2C H2 O1C 0.87 2.02 2.590(4) 122.3 . N2C H2 O1A 0.87 2.31 2.837(4) 118.9 . _diffrn_measured_fraction_theta_max 0.845 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 0.438 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.083 _publ_section_experimental ; Crystal colour: brown-green, crystal shape: rather regular rod. Special remarks: CCD mvc83 +oil. Special experimental condition: crystal was completely embedded in glue. and oil during handling and measurements. Special experimental condition: measurements were performed at -65 degrees C. The crystal diffracted rather weakly and no reliable intensity data could be collected above 25\% theta. Least-squares refinement using calculated weights: w=1/[\s^2^(Fo^2^)+(0.0070P)^2^+7.1454P] where P=(Fo^2^+2Fc^2^)/3 ; #===END