# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_General _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'NChem_All.cif' _audit_creation_date 2011-02-10 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Masaaki Kojima' _publ_contact_author_email kojima@cc.okayama-u.ac.jp _publ_contact_author_fax +81-86-255-3712 _publ_contact_author_phone +81-86-255-3712 _publ_contact_letter ; Please consider this CIF submission for publication in Nature Chemistry. ; _publ_requested_category 'FI ' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; A single tripodal ligand stabilizing three different oxidation states (II, III, and IV) of manganese ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_address Y.Sunatsuki ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Kita-ku, Okayama 700-8530, Japan ; Y.Kishima ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Kita-ku, Okayama 700-8530, Japan ; T.Kobayashi ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Kita-ku, Okayama 700-8530, Japan ; T.Yamaguchi ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Kita-ku, Okayama 700-8530, Japan ; T.Suzuki ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Kita-ku, Okayama 700-8530, Japan ; ; M.Kojima ; ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Kita-ku, Okayama 700-8530, Japan ; J.Krzystek ; National High Magnetic Field Laboratory, Florida State University, Tallahassee, Florida 32310, USA ; M.R.Sundberg ; Department of Chemistry, Laboratory of Inorganic Chemistry, University of Helsinki, POB 55, FIN-0014, Finland ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_references ; ENTER OTHER REFERENCES Rigaku Americas and Rigaku Corporation. (2007). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku Americas, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. M.C. Burla, R. Caliandro, M. Camalli, B. Carrozzini, G.L. Cascarano, L. De Caro, C. Giacovazzo, G. Polidori, R. Spagna (2005) SIR2004 Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; #============================================================================== data__100110k _database_code_depnum_ccdc_archive 'CCDC 812372' #TrackingRef 'NChem_All.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C31 H42 Mn N4 O8 ' _chemical_formula_moiety 'C29 H30 Mn N3 O6, 2(C H4 O), H4 N ' _chemical_formula_weight 653.63 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,+Z 3 +X,1/2-Y,1/2+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,-Z 7 -X,1/2+Y,1/2-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 10.8867(10) _cell_length_b 25.958(2) _cell_length_c 22.332(2) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 6310.8(9) _cell_formula_units_Z 8 _cell_measurement_reflns_used 57244 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.0 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760.00 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.867 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 193.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 90736 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7231 _reflns_number_gt 5976 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1756 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7231 _refine_ls_number_parameters 398 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0935P)^2^+7.8323P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.75 _refine_diff_density_min -0.43 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Mn(1) Mn 0.83428(4) 0.117208(15) 0.112646(17) 0.02852(13) Uani 1.00 1 d . . . O(1) O 0.80367(18) 0.14418(7) 0.02290(8) 0.0332(4) Uani 1.00 1 d . . . O(2) O 0.69025(18) 0.16537(8) 0.14307(9) 0.0381(4) Uani 1.00 1 d . . . O(3) O 0.70518(19) 0.05794(8) 0.09751(9) 0.0395(4) Uani 1.00 1 d . . . O(4) O 0.67022(19) 0.16510(8) -0.07151(9) 0.0407(4) Uani 1.00 1 d . . . O(5) O 0.48089(18) 0.21278(8) 0.13574(11) 0.0449(5) Uani 1.00 1 d . . . O(6) O 0.4877(2) 0.01963(8) 0.07435(10) 0.0453(5) Uani 1.00 1 d . . . O(7) O 0.9101(3) 0.24031(10) 0.02108(14) 0.0694(7) Uani 1.00 1 d . . . O(8) O 0.3212(2) 0.16310(11) -0.00281(13) 0.0624(6) Uani 1.00 1 d . . . N(1) N 1.0135(2) 0.09295(9) 0.07017(10) 0.0344(4) Uani 1.00 1 d . . . N(2) N 0.9490(2) 0.17416(9) 0.16338(10) 0.0341(4) Uani 1.00 1 d . . . N(3) N 0.9070(2) 0.06157(9) 0.18220(10) 0.0348(4) Uani 1.00 1 d . . . N(4) N 0.5476(2) 0.13077(9) 0.04892(11) 0.0393(5) Uani 1.00 1 d . . . C(1) C 1.2409(2) 0.10068(14) 0.19919(14) 0.0473(7) Uani 1.00 1 d . . . C(2) C 1.1115(2) 0.10482(12) 0.17152(12) 0.0374(5) Uani 1.00 1 d . . . C(3) C 1.1181(2) 0.08016(13) 0.10930(12) 0.0396(6) Uani 1.00 1 d . . . C(4) C 1.0233(2) 0.07789(11) 0.01610(12) 0.0362(5) Uani 1.00 1 d . . . C(5) C 0.9388(2) 0.08872(11) -0.03304(12) 0.0341(5) Uani 1.00 1 d . . . C(6) C 0.9692(2) 0.06722(12) -0.08919(13) 0.0412(6) Uani 1.00 1 d . . . C(7) C 0.9013(3) 0.07824(13) -0.13924(13) 0.0440(6) Uani 1.00 1 d . . . C(8) C 0.8008(2) 0.11153(11) -0.13503(13) 0.0387(6) Uani 1.00 1 d . . . C(9) C 0.7684(2) 0.13254(10) -0.08075(12) 0.0324(5) Uani 1.00 1 d . . . C(10) C 0.8368(2) 0.12167(10) -0.02740(12) 0.0310(5) Uani 1.00 1 d . . . C(11) C 0.6022(3) 0.18174(12) -0.12240(14) 0.0430(6) Uani 1.00 1 d . . . C(12) C 1.0812(2) 0.16294(12) 0.16798(14) 0.0402(6) Uani 1.00 1 d . . . C(13) C 0.9138(2) 0.21585(11) 0.18854(12) 0.0348(5) Uani 1.00 1 d . . . C(14) C 0.7912(2) 0.23800(11) 0.18740(11) 0.0347(5) Uani 1.00 1 d . . . C(15) C 0.7788(3) 0.28896(12) 0.20977(13) 0.0427(6) Uani 1.00 1 d . . . C(16) C 0.6683(3) 0.31446(12) 0.20690(14) 0.0451(7) Uani 1.00 1 d . . . C(17) C 0.5662(2) 0.29013(11) 0.18173(13) 0.0405(6) Uani 1.00 1 d . . . C(18) C 0.5752(2) 0.24044(11) 0.16112(12) 0.0359(5) Uani 1.00 1 d . . . C(19) C 0.6888(2) 0.21215(10) 0.16318(11) 0.0326(5) Uani 1.00 1 d . . . C(20) C 0.3651(2) 0.23787(14) 0.13076(17) 0.0486(7) Uani 1.00 1 d . . . C(21) C 1.0222(2) 0.07570(12) 0.21247(12) 0.0397(6) Uani 1.00 1 d . . . C(22) C 0.8590(2) 0.01827(11) 0.19683(12) 0.0355(5) Uani 1.00 1 d . . . C(23) C 0.7430(2) -0.00250(10) 0.17697(12) 0.0350(5) Uani 1.00 1 d . . . C(24) C 0.6982(3) -0.04676(12) 0.20759(14) 0.0447(7) Uani 1.00 1 d . . . C(25) C 0.5857(3) -0.06747(12) 0.19540(15) 0.0495(7) Uani 1.00 1 d . . . C(26) C 0.5127(3) -0.04613(11) 0.15095(15) 0.0450(7) Uani 1.00 1 d . . . C(27) C 0.5539(2) -0.00400(11) 0.11879(13) 0.0376(6) Uani 1.00 1 d . . . C(28) C 0.6711(2) 0.01933(10) 0.13000(13) 0.0337(5) Uani 1.00 1 d . . . C(29) C 0.3778(3) -0.00456(14) 0.05507(17) 0.0515(7) Uani 1.00 1 d . . . C(30) C 1.0306(3) 0.22675(14) 0.00348(18) 0.0581(8) Uani 1.00 1 d . . . C(31) C 0.2844(4) 0.14234(19) -0.0588(2) 0.0713(11) Uani 1.00 1 d . . . H(1) H 1.3026 0.1014 0.1673 0.057 Uiso 1.00 1 c R . . H(2) H 1.2477 0.0683 0.2215 0.057 Uiso 1.00 1 c R . . H(3) H 1.2545 0.1297 0.2264 0.057 Uiso 1.00 1 c R . . H(4) H 1.1949 0.0914 0.0895 0.047 Uiso 1.00 1 c R . . H(5) H 1.1221 0.0423 0.1140 0.047 Uiso 1.00 1 c R . . H(6) H 1.0931 0.0574 0.0068 0.043 Uiso 1.00 1 c R . . H(7) H 1.0378 0.0448 -0.0923 0.049 Uiso 1.00 1 c R . . H(8) H 0.9224 0.0633 -0.1767 0.053 Uiso 1.00 1 c R . . H(9) H 0.7547 0.1197 -0.1699 0.046 Uiso 1.00 1 c R . . H(10) H 0.6379 0.2137 -0.1379 0.052 Uiso 1.00 1 c R . . H(11) H 0.5166 0.1878 -0.1108 0.052 Uiso 1.00 1 c R . . H(12) H 0.6053 0.1551 -0.1535 0.052 Uiso 1.00 1 c R . . H(13) H 1.1141 0.1802 0.2041 0.048 Uiso 1.00 1 c R . . H(14) H 1.1234 0.1778 0.1327 0.048 Uiso 1.00 1 c R . . H(15) H 0.9743 0.2344 0.2104 0.042 Uiso 1.00 1 c R . . H(16) H 0.8479 0.3057 0.2270 0.051 Uiso 1.00 1 c R . . H(17) H 0.6614 0.3486 0.2220 0.054 Uiso 1.00 1 c R . . H(18) H 0.4902 0.3080 0.1789 0.049 Uiso 1.00 1 c R . . H(19) H 0.3166 0.2313 0.1669 0.058 Uiso 1.00 1 c R . . H(20) H 0.3212 0.2246 0.0957 0.058 Uiso 1.00 1 c R . . H(21) H 0.3778 0.2750 0.1262 0.058 Uiso 1.00 1 c R . . H(22) H 1.0627 0.0440 0.2272 0.048 Uiso 1.00 1 c R . . H(23) H 1.0029 0.0975 0.2476 0.048 Uiso 1.00 1 c R . . H(24) H 0.9050 -0.0025 0.2238 0.043 Uiso 1.00 1 c R . . H(25) H 0.7481 -0.0624 0.2374 0.054 Uiso 1.00 1 c R . . H(26) H 0.5575 -0.0965 0.2173 0.059 Uiso 1.00 1 c R . . H(27) H 0.4343 -0.0605 0.1426 0.054 Uiso 1.00 1 c R . . H(28) H 0.3962 -0.0282 0.0221 0.062 Uiso 1.00 1 c R . . H(29) H 0.3195 0.0217 0.0414 0.062 Uiso 1.00 1 c R . . H(30) H 0.3418 -0.0239 0.0884 0.062 Uiso 1.00 1 c R . . H(31) H 0.5515 0.1495 0.0859 0.047 Uiso 1.00 1 c R . . H(32) H 0.6043 0.1453 0.0207 0.047 Uiso 1.00 1 c R . . H(33) H 0.5693 0.0953 0.0562 0.047 Uiso 1.00 1 c R . . H(34) H 0.4658 0.1323 0.0330 0.047 Uiso 1.00 1 c R . . H(35) H 0.8594 0.2103 0.0234 0.083 Uiso 1.00 1 c R . . H(36) H 1.0765 0.2144 0.0384 0.070 Uiso 1.00 1 c R . . H(37) H 1.0720 0.2570 -0.0133 0.070 Uiso 1.00 1 c R . . H(38) H 1.0269 0.1995 -0.0268 0.070 Uiso 1.00 1 c R . . H(39) H 0.3425 0.2003 -0.0106 0.075 Uiso 1.00 1 c R . . H(40) H 0.3434 0.1160 -0.0714 0.086 Uiso 1.00 1 c R . . H(41) H 0.2818 0.1699 -0.0888 0.086 Uiso 1.00 1 c R . . H(42) H 0.2027 0.1269 -0.0549 0.086 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0273(2) 0.0321(2) 0.0262(2) 0.00189(14) -0.00044(14) 0.00258(14) O(1) 0.0362(9) 0.0371(9) 0.0262(8) 0.0050(7) 0.0009(7) 0.0022(7) O(2) 0.0329(9) 0.0380(10) 0.0434(10) 0.0040(8) -0.0020(8) -0.0077(8) O(3) 0.0414(10) 0.0357(10) 0.0414(10) -0.0070(8) -0.0055(8) 0.0098(8) O(4) 0.0427(11) 0.0471(11) 0.0324(9) 0.0083(8) -0.0065(8) 0.0055(8) O(5) 0.0308(10) 0.0444(11) 0.0595(13) 0.0074(8) -0.0015(9) -0.0084(9) O(6) 0.0409(11) 0.0394(10) 0.0557(12) -0.0078(8) -0.0074(9) 0.0037(9) O(7) 0.088(2) 0.0454(13) 0.0746(18) -0.0060(13) 0.0140(15) 0.0000(12) O(8) 0.0546(14) 0.0681(16) 0.0647(16) 0.0016(12) -0.0150(12) 0.0110(13) N(1) 0.0299(11) 0.0429(12) 0.0304(10) 0.0055(9) -0.0003(8) 0.0036(9) N(2) 0.0291(10) 0.0393(11) 0.0338(11) 0.0001(9) -0.0057(8) 0.0028(9) N(3) 0.0332(11) 0.0422(12) 0.0291(10) 0.0058(9) 0.0007(8) 0.0045(9) N(4) 0.0400(12) 0.0379(12) 0.0401(12) 0.0036(10) -0.0007(10) 0.0041(9) C(1) 0.0334(14) 0.067(2) 0.0414(15) 0.0065(14) -0.0107(12) 0.0079(14) C(2) 0.0289(12) 0.0506(15) 0.0326(13) 0.0046(11) -0.0045(10) 0.0050(11) C(3) 0.0290(13) 0.0544(17) 0.0353(13) 0.0098(12) -0.0016(10) 0.0050(12) C(4) 0.0322(13) 0.0407(14) 0.0357(13) 0.0055(10) 0.0016(10) -0.0005(11) C(5) 0.0356(13) 0.0364(13) 0.0302(12) 0.0001(11) 0.0006(10) -0.0018(10) C(6) 0.0415(15) 0.0461(15) 0.0361(14) 0.0031(12) 0.0011(12) -0.0086(12) C(7) 0.0489(17) 0.0519(17) 0.0310(13) -0.0008(13) 0.0003(12) -0.0107(12) C(8) 0.0448(15) 0.0428(15) 0.0284(12) -0.0075(12) -0.0045(11) -0.0012(11) C(9) 0.0343(13) 0.0334(12) 0.0297(12) -0.0046(10) -0.0012(10) 0.0025(9) C(10) 0.0333(13) 0.0326(12) 0.0270(11) -0.0046(10) 0.0013(9) 0.0023(9) C(11) 0.0454(16) 0.0448(15) 0.0387(14) -0.0004(13) -0.0120(12) 0.0049(12) C(12) 0.0280(13) 0.0495(16) 0.0432(15) -0.0012(11) -0.0050(11) -0.0002(12) C(13) 0.0354(13) 0.0410(14) 0.0281(12) -0.0044(11) -0.0052(10) -0.0006(10) C(14) 0.0411(14) 0.0371(13) 0.0258(11) -0.0006(11) -0.0015(10) -0.0005(10) C(15) 0.0514(17) 0.0400(15) 0.0366(14) -0.0040(13) -0.0036(12) -0.0061(11) C(16) 0.0571(19) 0.0354(14) 0.0427(15) 0.0013(13) 0.0043(13) -0.0065(12) C(17) 0.0440(15) 0.0386(14) 0.0387(14) 0.0074(12) 0.0059(12) 0.0001(11) C(18) 0.0355(13) 0.0388(14) 0.0334(13) 0.0016(11) 0.0020(10) -0.0015(10) C(19) 0.0355(13) 0.0343(12) 0.0279(11) 0.0025(10) 0.0007(10) -0.0012(10) C(20) 0.0317(14) 0.0564(18) 0.0578(19) 0.0095(13) 0.0008(13) -0.0036(15) C(21) 0.0355(14) 0.0517(16) 0.0318(13) 0.0049(12) -0.0048(11) 0.0075(11) C(22) 0.0428(14) 0.0362(13) 0.0274(11) 0.0112(11) 0.0051(10) 0.0046(10) C(23) 0.0460(15) 0.0290(12) 0.0300(12) 0.0055(10) 0.0080(11) 0.0010(9) C(24) 0.0629(19) 0.0347(14) 0.0365(14) 0.0024(13) 0.0050(13) 0.0047(11) C(25) 0.071(2) 0.0339(14) 0.0432(16) -0.0095(14) 0.0083(15) 0.0021(12) C(26) 0.0529(17) 0.0349(14) 0.0471(16) -0.0084(12) 0.0084(14) -0.0031(12) C(27) 0.0415(15) 0.0309(12) 0.0403(14) 0.0005(11) 0.0045(11) -0.0022(10) C(28) 0.0390(14) 0.0279(12) 0.0343(12) 0.0017(10) 0.0055(10) -0.0006(10) C(29) 0.0389(16) 0.0540(18) 0.062(2) -0.0077(14) 0.0004(14) -0.0029(15) C(30) 0.070(2) 0.0483(18) 0.056(2) -0.0037(17) -0.0015(17) 0.0024(15) C(31) 0.060(2) 0.092(3) 0.062(2) -0.013(2) -0.0024(19) -0.002(2) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mn(1) O(1) 2.1490(18) yes . . Mn(1) O(2) 2.117(2) yes . . Mn(1) O(3) 2.111(2) yes . . Mn(1) N(1) 2.259(2) yes . . Mn(1) N(2) 2.243(2) yes . . Mn(1) N(3) 2.264(2) yes . . O(1) C(10) 1.317(3) yes . . O(2) C(19) 1.295(3) yes . . O(3) C(28) 1.292(3) yes . . O(4) C(9) 1.378(3) yes . . O(4) C(11) 1.424(3) yes . . O(5) C(18) 1.375(3) yes . . O(5) C(20) 1.423(3) yes . . O(6) C(27) 1.372(3) yes . . O(6) C(29) 1.418(4) yes . . O(7) C(30) 1.414(5) yes . . O(8) C(31) 1.420(5) yes . . N(1) C(3) 1.473(3) yes . . N(1) C(4) 1.274(3) yes . . N(2) C(12) 1.472(3) yes . . N(2) C(13) 1.278(3) yes . . N(3) C(21) 1.471(3) yes . . N(3) C(22) 1.282(3) yes . . C(1) C(2) 1.541(4) yes . . C(2) C(3) 1.531(3) yes . . C(2) C(12) 1.546(4) yes . . C(2) C(21) 1.534(4) yes . . C(4) C(5) 1.459(3) yes . . C(5) C(6) 1.412(4) yes . . C(5) C(10) 1.408(3) yes . . C(6) C(7) 1.370(4) yes . . C(7) C(8) 1.397(4) yes . . C(8) C(9) 1.375(3) yes . . C(9) C(10) 1.433(3) yes . . C(13) C(14) 1.453(4) yes . . C(14) C(15) 1.420(4) yes . . C(14) C(19) 1.409(3) yes . . C(15) C(16) 1.375(4) yes . . C(16) C(17) 1.397(4) yes . . C(17) C(18) 1.373(4) yes . . C(18) C(19) 1.439(3) yes . . C(22) C(23) 1.444(4) yes . . C(23) C(24) 1.423(4) yes . . C(23) C(28) 1.426(3) yes . . C(24) C(25) 1.364(5) yes . . C(25) C(26) 1.387(4) yes . . C(26) C(27) 1.383(4) yes . . C(27) C(28) 1.434(4) yes . . O(7) H(35) 0.956 no . . O(8) H(39) 1.008 no . . N(4) H(31) 0.958 no . . N(4) H(32) 0.959 no . . N(4) H(33) 0.965 no . . N(4) H(34) 0.960 no . . C(1) H(1) 0.980 no . . C(1) H(2) 0.980 no . . C(1) H(3) 0.980 no . . C(3) H(4) 0.990 no . . C(3) H(5) 0.990 no . . C(4) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(11) H(10) 0.980 no . . C(11) H(11) 0.980 no . . C(11) H(12) 0.980 no . . C(12) H(13) 0.990 no . . C(12) H(14) 0.990 no . . C(13) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(17) H(18) 0.950 no . . C(20) H(19) 0.980 no . . C(20) H(20) 0.980 no . . C(20) H(21) 0.980 no . . C(21) H(22) 0.990 no . . C(21) H(23) 0.990 no . . C(22) H(24) 0.950 no . . C(24) H(25) 0.950 no . . C(25) H(26) 0.950 no . . C(26) H(27) 0.950 no . . C(29) H(28) 0.980 no . . C(29) H(29) 0.980 no . . C(29) H(30) 0.980 no . . C(30) H(36) 0.980 no . . C(30) H(37) 0.980 no . . C(30) H(38) 0.980 no . . C(31) H(40) 0.980 no . . C(31) H(41) 0.980 no . . C(31) H(42) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Mn(1) O(2) 89.55(7) yes . . . O(1) Mn(1) O(3) 89.13(7) yes . . . O(1) Mn(1) N(1) 80.39(7) yes . . . O(1) Mn(1) N(2) 110.05(7) yes . . . O(1) Mn(1) N(3) 154.42(7) yes . . . O(2) Mn(1) O(3) 89.35(8) yes . . . O(2) Mn(1) N(1) 159.88(8) yes . . . O(2) Mn(1) N(2) 82.02(8) yes . . . O(2) Mn(1) N(3) 114.55(8) yes . . . O(3) Mn(1) N(1) 107.73(8) yes . . . O(3) Mn(1) N(2) 158.77(8) yes . . . O(3) Mn(1) N(3) 82.98(8) yes . . . N(1) Mn(1) N(2) 85.12(8) yes . . . N(1) Mn(1) N(3) 78.94(8) yes . . . N(2) Mn(1) N(3) 83.06(8) yes . . . Mn(1) O(1) C(10) 127.49(16) yes . . . Mn(1) O(2) C(19) 132.37(17) yes . . . Mn(1) O(3) C(28) 131.81(18) yes . . . C(9) O(4) C(11) 118.0(2) yes . . . C(18) O(5) C(20) 117.0(2) yes . . . C(27) O(6) C(29) 117.7(2) yes . . . Mn(1) N(1) C(3) 118.77(16) yes . . . Mn(1) N(1) C(4) 123.81(18) yes . . . C(3) N(1) C(4) 115.3(2) yes . . . Mn(1) N(2) C(12) 116.70(17) yes . . . Mn(1) N(2) C(13) 127.81(19) yes . . . C(12) N(2) C(13) 115.5(2) yes . . . Mn(1) N(3) C(21) 117.02(17) yes . . . Mn(1) N(3) C(22) 126.29(19) yes . . . C(21) N(3) C(22) 116.7(2) yes . . . C(1) C(2) C(3) 107.0(2) yes . . . C(1) C(2) C(12) 106.5(2) yes . . . C(1) C(2) C(21) 107.8(2) yes . . . C(3) C(2) C(12) 111.8(2) yes . . . C(3) C(2) C(21) 111.4(2) yes . . . C(12) C(2) C(21) 112.1(2) yes . . . N(1) C(3) C(2) 114.1(2) yes . . . N(1) C(4) C(5) 126.9(2) yes . . . C(4) C(5) C(6) 116.4(2) yes . . . C(4) C(5) C(10) 123.2(2) yes . . . C(6) C(5) C(10) 120.3(2) yes . . . C(5) C(6) C(7) 121.0(2) yes . . . C(6) C(7) C(8) 119.8(2) yes . . . C(7) C(8) C(9) 120.4(2) yes . . . O(4) C(9) C(8) 125.0(2) yes . . . O(4) C(9) C(10) 113.5(2) yes . . . C(8) C(9) C(10) 121.4(2) yes . . . O(1) C(10) C(5) 124.2(2) yes . . . O(1) C(10) C(9) 118.7(2) yes . . . C(5) C(10) C(9) 117.1(2) yes . . . N(2) C(12) C(2) 113.9(2) yes . . . N(2) C(13) C(14) 127.1(2) yes . . . C(13) C(14) C(15) 116.7(2) yes . . . C(13) C(14) C(19) 123.0(2) yes . . . C(15) C(14) C(19) 120.2(2) yes . . . C(14) C(15) C(16) 121.0(2) yes . . . C(15) C(16) C(17) 119.8(2) yes . . . C(16) C(17) C(18) 120.2(2) yes . . . O(5) C(18) C(17) 125.1(2) yes . . . O(5) C(18) C(19) 112.9(2) yes . . . C(17) C(18) C(19) 122.0(2) yes . . . O(2) C(19) C(14) 124.8(2) yes . . . O(2) C(19) C(18) 118.5(2) yes . . . C(14) C(19) C(18) 116.7(2) yes . . . N(3) C(21) C(2) 112.9(2) yes . . . N(3) C(22) C(23) 127.3(2) yes . . . C(22) C(23) C(24) 117.0(2) yes . . . C(22) C(23) C(28) 123.9(2) yes . . . C(24) C(23) C(28) 119.1(2) yes . . . C(23) C(24) C(25) 122.0(2) yes . . . C(24) C(25) C(26) 120.0(2) yes . . . C(25) C(26) C(27) 120.1(3) yes . . . O(6) C(27) C(26) 124.0(2) yes . . . O(6) C(27) C(28) 113.9(2) yes . . . C(26) C(27) C(28) 122.1(2) yes . . . O(3) C(28) C(23) 124.3(2) yes . . . O(3) C(28) C(27) 119.0(2) yes . . . C(23) C(28) C(27) 116.6(2) yes . . . C(30) O(7) H(35) 110.3 no . . . C(31) O(8) H(39) 106.0 no . . . H(31) N(4) H(32) 109.7 no . . . H(31) N(4) H(33) 109.2 no . . . H(31) N(4) H(34) 109.8 no . . . H(32) N(4) H(33) 109.2 no . . . H(32) N(4) H(34) 109.7 no . . . H(33) N(4) H(34) 109.2 no . . . C(2) C(1) H(1) 109.5 no . . . C(2) C(1) H(2) 109.5 no . . . C(2) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . N(1) C(3) H(4) 108.7 no . . . N(1) C(3) H(5) 108.7 no . . . C(2) C(3) H(4) 108.7 no . . . C(2) C(3) H(5) 108.7 no . . . H(4) C(3) H(5) 107.6 no . . . N(1) C(4) H(6) 116.5 no . . . C(5) C(4) H(6) 116.5 no . . . C(5) C(6) H(7) 119.5 no . . . C(7) C(6) H(7) 119.5 no . . . C(6) C(7) H(8) 120.1 no . . . C(8) C(7) H(8) 120.1 no . . . C(7) C(8) H(9) 119.8 no . . . C(9) C(8) H(9) 119.8 no . . . O(4) C(11) H(10) 109.5 no . . . O(4) C(11) H(11) 109.5 no . . . O(4) C(11) H(12) 109.5 no . . . H(10) C(11) H(11) 109.5 no . . . H(10) C(11) H(12) 109.5 no . . . H(11) C(11) H(12) 109.5 no . . . N(2) C(12) H(13) 108.8 no . . . N(2) C(12) H(14) 108.8 no . . . C(2) C(12) H(13) 108.8 no . . . C(2) C(12) H(14) 108.8 no . . . H(13) C(12) H(14) 107.7 no . . . N(2) C(13) H(15) 116.5 no . . . C(14) C(13) H(15) 116.5 no . . . C(14) C(15) H(16) 119.5 no . . . C(16) C(15) H(16) 119.5 no . . . C(15) C(16) H(17) 120.1 no . . . C(17) C(16) H(17) 120.1 no . . . C(16) C(17) H(18) 119.9 no . . . C(18) C(17) H(18) 119.9 no . . . O(5) C(20) H(19) 109.5 no . . . O(5) C(20) H(20) 109.5 no . . . O(5) C(20) H(21) 109.5 no . . . H(19) C(20) H(20) 109.5 no . . . H(19) C(20) H(21) 109.5 no . . . H(20) C(20) H(21) 109.5 no . . . N(3) C(21) H(22) 109.0 no . . . N(3) C(21) H(23) 109.0 no . . . C(2) C(21) H(22) 109.0 no . . . C(2) C(21) H(23) 109.0 no . . . H(22) C(21) H(23) 107.8 no . . . N(3) C(22) H(24) 116.4 no . . . C(23) C(22) H(24) 116.3 no . . . C(23) C(24) H(25) 119.0 no . . . C(25) C(24) H(25) 119.0 no . . . C(24) C(25) H(26) 120.0 no . . . C(26) C(25) H(26) 120.0 no . . . C(25) C(26) H(27) 120.0 no . . . C(27) C(26) H(27) 120.0 no . . . O(6) C(29) H(28) 109.5 no . . . O(6) C(29) H(29) 109.5 no . . . O(6) C(29) H(30) 109.5 no . . . H(28) C(29) H(29) 109.5 no . . . H(28) C(29) H(30) 109.5 no . . . H(29) C(29) H(30) 109.5 no . . . O(7) C(30) H(36) 109.5 no . . . O(7) C(30) H(37) 109.5 no . . . O(7) C(30) H(38) 109.5 no . . . H(36) C(30) H(37) 109.5 no . . . H(36) C(30) H(38) 109.5 no . . . H(37) C(30) H(38) 109.5 no . . . O(8) C(31) H(40) 109.5 no . . . O(8) C(31) H(41) 109.5 no . . . O(8) C(31) H(42) 109.5 no . . . H(40) C(31) H(41) 109.5 no . . . H(40) C(31) H(42) 109.5 no . . . H(41) C(31) H(42) 109.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Mn(1) N(4) 3.448(2) ? . . O(1) O(7) 2.751(3) ? . . O(1) N(4) 2.869(3) ? . . O(1) C(30) 3.299(4) ? . . O(2) N(4) 2.764(3) ? . . O(3) N(4) 2.774(3) ? . . O(4) N(4) 3.132(3) ? . . O(4) C(20) 3.549(4) ? . 6_555 O(4) C(30) 3.535(4) ? . 6_455 O(5) N(4) 2.970(3) ? . . O(5) C(30) 3.525(4) ? . 6_455 O(6) O(6) 3.484(3) ? . 5_655 O(6) N(4) 3.012(3) ? . . O(6) C(29) 3.264(4) ? . 5_655 O(7) O(1) 2.751(3) ? . . O(7) O(8) 2.718(3) ? . 6_555 O(7) C(10) 3.360(3) ? . . O(7) C(20) 3.473(4) ? . 6_555 O(7) C(31) 3.444(5) ? . 6_555 O(8) O(7) 2.718(3) ? . 6_455 O(8) N(4) 2.848(3) ? . . O(8) C(20) 3.591(4) ? . . O(8) C(30) 3.572(4) ? . 1_455 N(3) C(1) 3.364(3) ? . 8_455 N(4) Mn(1) 3.448(2) ? . . N(4) O(1) 2.869(3) ? . . N(4) O(2) 2.764(3) ? . . N(4) O(3) 2.774(3) ? . . N(4) O(4) 3.132(3) ? . . N(4) O(5) 2.970(3) ? . . N(4) O(6) 3.012(3) ? . . N(4) O(8) 2.848(3) ? . . N(4) C(10) 3.588(3) ? . . C(1) N(3) 3.364(3) ? . 8_555 C(1) C(22) 3.409(4) ? . 8_555 C(10) O(7) 3.360(3) ? . . C(10) N(4) 3.588(3) ? . . C(10) C(30) 3.517(4) ? . . C(11) C(20) 3.547(4) ? . 6_555 C(20) O(4) 3.549(4) ? . 6_455 C(20) O(7) 3.473(4) ? . 6_455 C(20) O(8) 3.591(4) ? . . C(20) C(11) 3.547(4) ? . 6_455 C(22) C(1) 3.409(4) ? . 8_455 C(29) O(6) 3.264(4) ? . 5_655 C(30) O(1) 3.299(4) ? . . C(30) O(4) 3.535(4) ? . 6_555 C(30) O(5) 3.525(4) ? . 6_555 C(30) O(8) 3.572(4) ? . 1_655 C(30) C(10) 3.517(4) ? . . C(31) O(7) 3.444(5) ? . 6_455 Mn(1) H(31) 3.247 ? . . Mn(1) H(32) 3.319 ? . . Mn(1) H(33) 3.199 ? . . Mn(1) H(35) 3.144 ? . . O(1) H(31) 3.088 ? . . O(1) H(32) 2.172 ? . . O(1) H(33) 2.945 ? . . O(1) H(35) 1.820 ? . . O(1) H(36) 3.501 ? . . O(1) H(38) 3.033 ? . . O(2) H(3) 3.137 ? . 8_455 O(2) H(13) 3.533 ? . 8_455 O(2) H(31) 2.021 ? . . O(2) H(32) 2.935 ? . . O(2) H(33) 2.968 ? . . O(2) H(34) 3.571 ? . . O(2) H(35) 3.449 ? . . O(3) H(28) 2.990 ? . 5_655 O(3) H(31) 2.918 ? . . O(3) H(32) 3.048 ? . . O(3) H(33) 1.995 ? . . O(3) H(34) 3.549 ? . . O(4) H(20) 3.346 ? . 6_555 O(4) H(21) 3.003 ? . 6_555 O(4) H(27) 3.345 ? . 5_655 O(4) H(32) 2.241 ? . . O(4) H(33) 3.553 ? . . O(4) H(34) 3.336 ? . . O(4) H(35) 3.180 ? . . O(4) H(36) 3.373 ? . 6_455 O(4) H(37) 2.970 ? . 6_455 O(5) H(1) 3.553 ? . 1_455 O(5) H(15) 3.483 ? . 8_455 O(5) H(31) 2.129 ? . . O(5) H(32) 3.387 ? . . O(5) H(34) 3.107 ? . . O(5) H(37) 3.012 ? . 6_455 O(5) H(38) 3.369 ? . 6_455 O(6) H(1) 3.587 ? . 1_455 O(6) H(28) 2.507 ? . 5_655 O(6) H(29) 3.499 ? . 5_655 O(6) H(31) 3.451 ? . . O(6) H(33) 2.193 ? . . O(6) H(34) 3.076 ? . . O(7) H(11) 2.973 ? . 6_555 O(7) H(20) 2.928 ? . 6_555 O(7) H(21) 3.332 ? . 6_555 O(7) H(34) 3.573 ? . 6_555 O(7) H(39) 1.724 ? . 6_555 O(7) H(41) 3.110 ? . 6_555 O(8) H(4) 3.099 ? . 1_455 O(8) H(11) 3.280 ? . . O(8) H(20) 2.718 ? . . O(8) H(31) 3.214 ? . . O(8) H(32) 3.160 ? . . O(8) H(33) 3.483 ? . . O(8) H(34) 1.938 ? . . O(8) H(35) 3.344 ? . 6_455 O(8) H(36) 3.117 ? . 1_455 O(8) H(37) 3.447 ? . 6_455 O(8) H(38) 3.383 ? . 1_455 N(1) H(36) 3.302 ? . . N(1) H(38) 3.516 ? . . N(1) H(42) 3.581 ? . 1_655 N(2) H(3) 3.445 ? . 8_455 N(2) H(35) 3.406 ? . . N(2) H(36) 3.287 ? . . N(3) H(2) 2.768 ? . 8_455 N(3) H(3) 3.170 ? . 8_455 N(3) H(7) 3.465 ? . 5_755 N(4) H(28) 3.158 ? . 5_655 N(4) H(37) 3.031 ? . 6_455 N(4) H(39) 3.164 ? . . N(4) H(40) 3.509 ? . . C(1) H(19) 3.562 ? . 1_655 C(1) H(23) 3.091 ? . 8_555 C(3) H(29) 3.068 ? . 1_655 C(4) H(29) 3.584 ? . 1_655 C(4) H(38) 3.299 ? . . C(4) H(42) 2.819 ? . 1_655 C(5) H(35) 3.507 ? . . C(5) H(38) 3.034 ? . . C(5) H(42) 3.078 ? . 1_655 C(6) H(5) 3.061 ? . 5_755 C(6) H(30) 3.567 ? . 5_655 C(6) H(42) 3.073 ? . 1_655 C(7) H(5) 3.189 ? . 5_755 C(7) H(18) 3.231 ? . 6_555 C(7) H(24) 3.446 ? . 5_755 C(7) H(25) 3.225 ? . 4_654 C(7) H(26) 3.269 ? . 4_654 C(7) H(30) 3.206 ? . 5_655 C(8) H(18) 3.094 ? . 6_555 C(8) H(21) 3.068 ? . 6_555 C(8) H(25) 3.167 ? . 4_654 C(8) H(27) 2.887 ? . 5_655 C(8) H(30) 2.944 ? . 5_655 C(9) H(21) 2.864 ? . 6_555 C(9) H(27) 3.206 ? . 5_655 C(9) H(28) 3.502 ? . 5_655 C(9) H(30) 3.070 ? . 5_655 C(9) H(32) 2.905 ? . . C(9) H(35) 3.235 ? . . C(9) H(38) 3.520 ? . . C(10) H(21) 3.501 ? . 6_555 C(10) H(28) 3.512 ? . 5_655 C(10) H(30) 3.475 ? . 5_655 C(10) H(32) 2.818 ? . . C(10) H(33) 3.526 ? . . C(10) H(35) 2.577 ? . . C(10) H(38) 2.892 ? . . C(11) H(15) 3.246 ? . 6_455 C(11) H(19) 3.396 ? . 6_555 C(11) H(20) 3.457 ? . 6_555 C(11) H(21) 3.205 ? . 6_555 C(11) H(26) 3.523 ? . 5_655 C(11) H(27) 3.205 ? . 5_655 C(11) H(32) 3.333 ? . . C(11) H(36) 3.297 ? . 6_455 C(11) H(37) 3.438 ? . 6_455 C(11) H(40) 3.486 ? . . C(11) H(41) 3.581 ? . . C(12) H(10) 3.329 ? . 6_555 C(12) H(19) 3.117 ? . 1_655 C(12) H(20) 3.463 ? . 1_655 C(12) H(36) 3.187 ? . . C(13) H(3) 3.408 ? . 8_455 C(13) H(10) 3.251 ? . 6_555 C(13) H(11) 3.243 ? . 6_555 C(13) H(19) 3.421 ? . 8_555 C(14) H(3) 3.430 ? . 8_455 C(14) H(11) 3.557 ? . 6_555 C(14) H(13) 3.441 ? . 8_455 C(14) H(19) 3.270 ? . 8_555 C(14) H(41) 3.252 ? . 6_555 C(15) H(9) 3.594 ? . 3_555 C(15) H(11) 3.457 ? . 6_555 C(15) H(18) 3.425 ? . 8_555 C(15) H(19) 3.162 ? . 8_555 C(15) H(26) 3.471 ? . 2_655 C(15) H(41) 2.905 ? . 6_555 C(16) H(9) 3.373 ? . 3_555 C(16) H(10) 3.557 ? . 3_555 C(16) H(12) 3.289 ? . 3_555 C(16) H(15) 3.492 ? . 8_455 C(16) H(25) 3.394 ? . 2_655 C(16) H(41) 2.941 ? . 6_555 C(17) H(15) 2.984 ? . 8_455 C(17) H(16) 3.157 ? . 8_455 C(17) H(38) 3.496 ? . 6_455 C(17) H(41) 3.301 ? . 6_555 C(18) H(13) 3.418 ? . 8_455 C(18) H(15) 3.077 ? . 8_455 C(18) H(31) 2.910 ? . . C(18) H(37) 3.302 ? . 6_455 C(18) H(38) 3.421 ? . 6_455 C(19) H(3) 3.342 ? . 8_455 C(19) H(13) 3.183 ? . 8_455 C(19) H(31) 2.805 ? . . C(20) H(10) 2.779 ? . 6_455 C(20) H(13) 3.520 ? . 1_455 C(20) H(14) 3.059 ? . 1_455 C(20) H(31) 3.223 ? . . C(20) H(37) 3.460 ? . 6_455 C(20) H(38) 3.337 ? . 6_455 C(20) H(39) 3.313 ? . . C(21) H(2) 3.338 ? . 8_455 C(21) H(3) 3.510 ? . 8_455 C(22) H(2) 2.546 ? . 8_455 C(22) H(3) 3.550 ? . 8_455 C(22) H(7) 3.063 ? . 5_755 C(22) H(8) 3.216 ? . 5_755 C(23) H(2) 2.919 ? . 8_455 C(23) H(7) 3.236 ? . 5_755 C(23) H(22) 3.144 ? . 8_455 C(24) H(2) 3.423 ? . 8_455 C(24) H(8) 2.930 ? . 4_655 C(24) H(9) 3.367 ? . 4_655 C(24) H(17) 3.134 ? . 2_645 C(24) H(22) 3.138 ? . 8_455 C(24) H(40) 3.561 ? . 5_655 C(25) H(8) 2.860 ? . 4_655 C(25) H(12) 3.222 ? . 5_655 C(25) H(16) 3.444 ? . 2_645 C(25) H(17) 3.561 ? . 2_645 C(25) H(22) 3.379 ? . 8_455 C(25) H(24) 3.158 ? . 8_455 C(25) H(40) 3.138 ? . 5_655 C(26) H(9) 3.507 ? . 5_655 C(26) H(12) 3.108 ? . 5_655 C(26) H(24) 3.238 ? . 8_455 C(26) H(40) 2.982 ? . 5_655 C(27) H(28) 3.299 ? . 5_655 C(27) H(33) 2.936 ? . . C(27) H(40) 3.288 ? . 5_655 C(28) H(22) 3.459 ? . 8_455 C(28) H(28) 3.481 ? . 5_655 C(28) H(33) 2.798 ? . . C(29) H(4) 3.281 ? . 1_455 C(29) H(5) 3.310 ? . 1_455 C(29) H(28) 3.122 ? . 5_655 C(29) H(33) 3.326 ? . . C(29) H(33) 3.471 ? . 5_655 C(30) H(10) 3.573 ? . 6_555 C(30) H(11) 3.269 ? . 6_555 C(30) H(14) 3.312 ? . . C(30) H(20) 3.421 ? . 6_555 C(30) H(21) 3.340 ? . 6_555 C(30) H(32) 3.459 ? . 6_555 C(30) H(39) 3.478 ? . 1_655 C(30) H(39) 2.794 ? . 6_555 C(30) H(42) 3.455 ? . 1_655 C(31) H(6) 3.368 ? . 1_455 C(31) H(11) 3.022 ? . . C(31) H(34) 2.859 ? . . C(31) H(38) 3.251 ? . 1_455 H(1) O(5) 3.553 ? . 1_655 H(1) O(6) 3.587 ? . 1_655 H(1) H(19) 3.375 ? . 1_655 H(1) H(20) 3.580 ? . 1_655 H(1) H(23) 2.895 ? . 8_555 H(1) H(29) 3.495 ? . 1_655 H(1) H(31) 3.493 ? . 1_655 H(1) H(34) 3.576 ? . 1_655 H(2) N(3) 2.768 ? . 8_555 H(2) C(21) 3.338 ? . 8_555 H(2) C(22) 2.546 ? . 8_555 H(2) C(23) 2.919 ? . 8_555 H(2) C(24) 3.423 ? . 8_555 H(2) H(23) 2.961 ? . 8_555 H(2) H(24) 2.793 ? . 8_555 H(2) H(25) 3.513 ? . 8_555 H(3) O(2) 3.137 ? . 8_555 H(3) N(2) 3.445 ? . 8_555 H(3) N(3) 3.170 ? . 8_555 H(3) C(13) 3.408 ? . 8_555 H(3) C(14) 3.430 ? . 8_555 H(3) C(19) 3.342 ? . 8_555 H(3) C(21) 3.510 ? . 8_555 H(3) C(22) 3.550 ? . 8_555 H(3) H(19) 3.029 ? . 1_655 H(3) H(23) 2.889 ? . 8_555 H(4) O(8) 3.099 ? . 1_655 H(4) C(29) 3.281 ? . 1_655 H(4) H(29) 2.504 ? . 1_655 H(4) H(30) 3.394 ? . 1_655 H(4) H(34) 3.379 ? . 1_655 H(4) H(42) 3.355 ? . 1_655 H(5) C(6) 3.061 ? . 5_755 H(5) C(7) 3.189 ? . 5_755 H(5) C(29) 3.310 ? . 1_655 H(5) H(7) 2.893 ? . 5_755 H(5) H(8) 3.115 ? . 5_755 H(5) H(29) 2.744 ? . 1_655 H(5) H(30) 2.999 ? . 1_655 H(6) C(31) 3.368 ? . 1_655 H(6) H(7) 3.566 ? . 5_755 H(6) H(29) 2.744 ? . 1_655 H(6) H(40) 3.575 ? . 1_655 H(6) H(42) 2.563 ? . 1_655 H(7) N(3) 3.465 ? . 5_755 H(7) C(22) 3.063 ? . 5_755 H(7) C(23) 3.236 ? . 5_755 H(7) H(5) 2.893 ? . 5_755 H(7) H(6) 3.566 ? . 5_755 H(7) H(24) 3.195 ? . 5_755 H(7) H(42) 2.909 ? . 1_655 H(8) C(22) 3.216 ? . 5_755 H(8) C(24) 2.930 ? . 4_654 H(8) C(25) 2.860 ? . 4_654 H(8) H(5) 3.115 ? . 5_755 H(8) H(18) 3.422 ? . 6_555 H(8) H(22) 3.010 ? . 5_755 H(8) H(24) 2.669 ? . 5_755 H(8) H(25) 2.669 ? . 4_654 H(8) H(26) 2.528 ? . 4_654 H(9) C(15) 3.594 ? . 3_554 H(9) C(16) 3.373 ? . 3_554 H(9) C(24) 3.367 ? . 4_654 H(9) C(26) 3.507 ? . 5_655 H(9) H(16) 3.176 ? . 3_554 H(9) H(17) 2.747 ? . 3_554 H(9) H(18) 3.184 ? . 6_555 H(9) H(21) 3.196 ? . 6_555 H(9) H(25) 2.550 ? . 4_654 H(9) H(26) 3.300 ? . 4_654 H(9) H(27) 2.639 ? . 5_655 H(9) H(30) 3.255 ? . 5_655 H(10) C(12) 3.329 ? . 6_455 H(10) C(13) 3.251 ? . 6_455 H(10) C(16) 3.557 ? . 3_554 H(10) C(20) 2.779 ? . 6_555 H(10) C(30) 3.573 ? . 6_455 H(10) H(13) 3.136 ? . 6_455 H(10) H(14) 2.822 ? . 6_455 H(10) H(15) 2.757 ? . 6_455 H(10) H(17) 3.531 ? . 3_554 H(10) H(19) 2.498 ? . 6_555 H(10) H(20) 2.727 ? . 6_555 H(10) H(21) 2.642 ? . 6_555 H(10) H(36) 2.978 ? . 6_455 H(10) H(37) 3.535 ? . 6_455 H(11) O(7) 2.973 ? . 6_455 H(11) O(8) 3.280 ? . . H(11) C(13) 3.243 ? . 6_455 H(11) C(14) 3.557 ? . 6_455 H(11) C(15) 3.457 ? . 6_455 H(11) C(30) 3.269 ? . 6_455 H(11) C(31) 3.022 ? . . H(11) H(15) 3.038 ? . 6_455 H(11) H(16) 3.183 ? . 6_455 H(11) H(26) 3.454 ? . 5_655 H(11) H(27) 3.424 ? . 5_655 H(11) H(32) 3.280 ? . . H(11) H(34) 3.564 ? . . H(11) H(36) 3.080 ? . 6_455 H(11) H(37) 3.178 ? . 6_455 H(11) H(39) 2.951 ? . . H(11) H(40) 2.795 ? . . H(11) H(41) 2.644 ? . . H(12) C(16) 3.289 ? . 3_554 H(12) C(25) 3.222 ? . 5_655 H(12) C(26) 3.108 ? . 5_655 H(12) H(15) 3.446 ? . 6_455 H(12) H(16) 3.404 ? . 6_455 H(12) H(17) 2.849 ? . 3_554 H(12) H(21) 3.530 ? . 6_555 H(12) H(26) 2.737 ? . 5_655 H(12) H(27) 2.506 ? . 5_655 H(12) H(40) 3.539 ? . . H(13) O(2) 3.533 ? . 8_555 H(13) C(14) 3.441 ? . 8_555 H(13) C(18) 3.418 ? . 8_555 H(13) C(19) 3.183 ? . 8_555 H(13) C(20) 3.520 ? . 1_655 H(13) H(10) 3.136 ? . 6_555 H(13) H(19) 2.703 ? . 1_655 H(13) H(20) 3.503 ? . 1_655 H(14) C(20) 3.059 ? . 1_655 H(14) C(30) 3.312 ? . . H(14) H(10) 2.822 ? . 6_555 H(14) H(19) 2.632 ? . 1_655 H(14) H(20) 2.606 ? . 1_655 H(14) H(36) 2.367 ? . . H(15) O(5) 3.483 ? . 8_555 H(15) C(11) 3.246 ? . 6_555 H(15) C(16) 3.492 ? . 8_555 H(15) C(17) 2.984 ? . 8_555 H(15) C(18) 3.077 ? . 8_555 H(15) H(10) 2.757 ? . 6_555 H(15) H(11) 3.038 ? . 6_555 H(15) H(12) 3.446 ? . 6_555 H(15) H(18) 3.131 ? . 8_555 H(15) H(19) 3.236 ? . 8_555 H(16) C(17) 3.157 ? . 8_555 H(16) C(25) 3.444 ? . 2_655 H(16) H(9) 3.176 ? . 3_555 H(16) H(11) 3.183 ? . 6_555 H(16) H(12) 3.404 ? . 6_555 H(16) H(18) 2.612 ? . 8_555 H(16) H(19) 3.076 ? . 8_555 H(16) H(21) 3.389 ? . 8_555 H(16) H(25) 3.589 ? . 2_655 H(16) H(26) 2.749 ? . 2_655 H(16) H(41) 3.231 ? . 6_555 H(17) C(24) 3.134 ? . 2_655 H(17) C(25) 3.561 ? . 2_655 H(17) H(9) 2.747 ? . 3_555 H(17) H(10) 3.531 ? . 3_555 H(17) H(12) 2.849 ? . 3_555 H(17) H(25) 2.537 ? . 2_655 H(17) H(26) 3.378 ? . 2_655 H(17) H(26) 3.090 ? . 7_655 H(17) H(41) 3.285 ? . 6_555 H(18) C(7) 3.231 ? . 6_455 H(18) C(8) 3.094 ? . 6_455 H(18) C(15) 3.425 ? . 8_455 H(18) H(8) 3.422 ? . 6_455 H(18) H(9) 3.184 ? . 6_455 H(18) H(15) 3.131 ? . 8_455 H(18) H(16) 2.612 ? . 8_455 H(18) H(26) 3.433 ? . 7_655 H(18) H(38) 3.425 ? . 6_455 H(19) C(1) 3.562 ? . 1_455 H(19) C(11) 3.396 ? . 6_455 H(19) C(12) 3.117 ? . 1_455 H(19) C(13) 3.421 ? . 8_455 H(19) C(14) 3.270 ? . 8_455 H(19) C(15) 3.162 ? . 8_455 H(19) H(1) 3.375 ? . 1_455 H(19) H(3) 3.029 ? . 1_455 H(19) H(10) 2.498 ? . 6_455 H(19) H(13) 2.703 ? . 1_455 H(19) H(14) 2.632 ? . 1_455 H(19) H(15) 3.236 ? . 8_455 H(19) H(16) 3.076 ? . 8_455 H(20) O(4) 3.346 ? . 6_455 H(20) O(7) 2.928 ? . 6_455 H(20) O(8) 2.718 ? . . H(20) C(11) 3.457 ? . 6_455 H(20) C(12) 3.463 ? . 1_455 H(20) C(30) 3.421 ? . 6_455 H(20) H(1) 3.580 ? . 1_455 H(20) H(10) 2.727 ? . 6_455 H(20) H(13) 3.503 ? . 1_455 H(20) H(14) 2.606 ? . 1_455 H(20) H(31) 3.183 ? . . H(20) H(34) 3.190 ? . . H(20) H(35) 3.179 ? . 6_455 H(20) H(36) 2.967 ? . 1_455 H(20) H(37) 3.327 ? . 6_455 H(20) H(38) 3.357 ? . 6_455 H(20) H(39) 2.467 ? . . H(21) O(4) 3.003 ? . 6_455 H(21) O(7) 3.332 ? . 6_455 H(21) C(8) 3.068 ? . 6_455 H(21) C(9) 2.864 ? . 6_455 H(21) C(10) 3.501 ? . 6_455 H(21) C(11) 3.205 ? . 6_455 H(21) C(30) 3.340 ? . 6_455 H(21) H(9) 3.196 ? . 6_455 H(21) H(10) 2.642 ? . 6_455 H(21) H(12) 3.530 ? . 6_455 H(21) H(16) 3.389 ? . 8_455 H(21) H(35) 3.369 ? . 6_455 H(21) H(37) 3.394 ? . 6_455 H(21) H(38) 2.828 ? . 6_455 H(22) C(23) 3.144 ? . 8_555 H(22) C(24) 3.138 ? . 8_555 H(22) C(25) 3.379 ? . 8_555 H(22) C(28) 3.459 ? . 8_555 H(22) H(8) 3.010 ? . 5_755 H(22) H(25) 3.510 ? . 8_555 H(23) C(1) 3.091 ? . 8_455 H(23) H(1) 2.895 ? . 8_455 H(23) H(2) 2.961 ? . 8_455 H(23) H(3) 2.889 ? . 8_455 H(24) C(7) 3.446 ? . 5_755 H(24) C(25) 3.158 ? . 8_555 H(24) C(26) 3.238 ? . 8_555 H(24) H(2) 2.793 ? . 8_455 H(24) H(7) 3.195 ? . 5_755 H(24) H(8) 2.669 ? . 5_755 H(24) H(26) 3.231 ? . 8_555 H(24) H(27) 3.358 ? . 8_555 H(25) C(7) 3.225 ? . 4_655 H(25) C(8) 3.167 ? . 4_655 H(25) C(16) 3.394 ? . 2_645 H(25) H(2) 3.513 ? . 8_455 H(25) H(8) 2.669 ? . 4_655 H(25) H(9) 2.550 ? . 4_655 H(25) H(16) 3.589 ? . 2_645 H(25) H(17) 2.537 ? . 2_645 H(25) H(22) 3.510 ? . 8_455 H(25) H(27) 3.360 ? . 8_555 H(26) C(7) 3.269 ? . 4_655 H(26) C(11) 3.523 ? . 5_655 H(26) C(15) 3.471 ? . 2_645 H(26) H(8) 2.528 ? . 4_655 H(26) H(9) 3.300 ? . 4_655 H(26) H(11) 3.454 ? . 5_655 H(26) H(12) 2.737 ? . 5_655 H(26) H(16) 2.749 ? . 2_645 H(26) H(17) 3.378 ? . 2_645 H(26) H(17) 3.090 ? . 7_645 H(26) H(18) 3.433 ? . 7_645 H(26) H(24) 3.231 ? . 8_455 H(26) H(40) 3.470 ? . 5_655 H(27) O(4) 3.345 ? . 5_655 H(27) C(8) 2.887 ? . 5_655 H(27) C(9) 3.206 ? . 5_655 H(27) C(11) 3.205 ? . 5_655 H(27) H(9) 2.639 ? . 5_655 H(27) H(11) 3.424 ? . 5_655 H(27) H(12) 2.506 ? . 5_655 H(27) H(24) 3.358 ? . 8_455 H(27) H(25) 3.360 ? . 8_455 H(27) H(40) 3.234 ? . 5_655 H(28) O(3) 2.990 ? . 5_655 H(28) O(6) 2.507 ? . 5_655 H(28) N(4) 3.158 ? . 5_655 H(28) C(9) 3.502 ? . 5_655 H(28) C(10) 3.512 ? . 5_655 H(28) C(27) 3.299 ? . 5_655 H(28) C(28) 3.481 ? . 5_655 H(28) C(29) 3.122 ? . 5_655 H(28) H(28) 2.868 ? . 5_655 H(28) H(29) 3.409 ? . 5_655 H(28) H(32) 3.186 ? . 5_655 H(28) H(33) 2.494 ? . 5_655 H(28) H(34) 3.327 ? . 5_655 H(29) O(6) 3.499 ? . 5_655 H(29) C(3) 3.068 ? . 1_455 H(29) C(4) 3.584 ? . 1_455 H(29) H(1) 3.495 ? . 1_455 H(29) H(4) 2.504 ? . 1_455 H(29) H(5) 2.744 ? . 1_455 H(29) H(6) 2.744 ? . 1_455 H(29) H(28) 3.409 ? . 5_655 H(29) H(33) 3.340 ? . . H(29) H(34) 3.289 ? . . H(29) H(40) 3.522 ? . . H(30) C(6) 3.567 ? . 5_655 H(30) C(7) 3.206 ? . 5_655 H(30) C(8) 2.944 ? . 5_655 H(30) C(9) 3.070 ? . 5_655 H(30) C(10) 3.475 ? . 5_655 H(30) H(4) 3.394 ? . 1_455 H(30) H(5) 2.999 ? . 1_455 H(30) H(9) 3.255 ? . 5_655 H(31) Mn(1) 3.247 ? . . H(31) O(1) 3.088 ? . . H(31) O(2) 2.021 ? . . H(31) O(3) 2.918 ? . . H(31) O(5) 2.129 ? . . H(31) O(6) 3.451 ? . . H(31) O(8) 3.214 ? . . H(31) C(18) 2.910 ? . . H(31) C(19) 2.805 ? . . H(31) C(20) 3.223 ? . . H(31) H(1) 3.493 ? . 1_455 H(31) H(20) 3.183 ? . . H(31) H(37) 2.927 ? . 6_455 H(31) H(39) 3.399 ? . . H(32) Mn(1) 3.319 ? . . H(32) O(1) 2.172 ? . . H(32) O(2) 2.935 ? . . H(32) O(3) 3.048 ? . . H(32) O(4) 2.241 ? . . H(32) O(5) 3.387 ? . . H(32) O(8) 3.160 ? . . H(32) C(9) 2.905 ? . . H(32) C(10) 2.818 ? . . H(32) C(11) 3.333 ? . . H(32) C(30) 3.459 ? . 6_455 H(32) H(11) 3.280 ? . . H(32) H(28) 3.186 ? . 5_655 H(32) H(35) 3.250 ? . . H(32) H(37) 2.565 ? . 6_455 H(32) H(39) 3.263 ? . . H(32) H(40) 3.589 ? . . H(33) Mn(1) 3.199 ? . . H(33) O(1) 2.945 ? . . H(33) O(2) 2.968 ? . . H(33) O(3) 1.995 ? . . H(33) O(4) 3.553 ? . . H(33) O(6) 2.193 ? . . H(33) O(8) 3.483 ? . . H(33) C(10) 3.526 ? . . H(33) C(27) 2.936 ? . . H(33) C(28) 2.798 ? . . H(33) C(29) 3.326 ? . . H(33) C(29) 3.471 ? . 5_655 H(33) H(28) 2.494 ? . 5_655 H(33) H(29) 3.340 ? . . H(34) O(2) 3.571 ? . . H(34) O(3) 3.549 ? . . H(34) O(4) 3.336 ? . . H(34) O(5) 3.107 ? . . H(34) O(6) 3.076 ? . . H(34) O(7) 3.573 ? . 6_455 H(34) O(8) 1.938 ? . . H(34) C(31) 2.859 ? . . H(34) H(1) 3.576 ? . 1_455 H(34) H(4) 3.379 ? . 1_455 H(34) H(11) 3.564 ? . . H(34) H(20) 3.190 ? . . H(34) H(28) 3.327 ? . 5_655 H(34) H(29) 3.289 ? . . H(34) H(37) 3.128 ? . 6_455 H(34) H(39) 2.422 ? . . H(34) H(40) 2.719 ? . . H(34) H(41) 3.516 ? . . H(34) H(42) 3.476 ? . . H(35) Mn(1) 3.144 ? . . H(35) O(1) 1.820 ? . . H(35) O(2) 3.449 ? . . H(35) O(4) 3.180 ? . . H(35) O(8) 3.344 ? . 6_555 H(35) N(2) 3.406 ? . . H(35) C(5) 3.507 ? . . H(35) C(9) 3.235 ? . . H(35) C(10) 2.577 ? . . H(35) H(20) 3.179 ? . 6_555 H(35) H(21) 3.369 ? . 6_555 H(35) H(32) 3.250 ? . . H(35) H(37) 3.250 ? . 6_455 H(35) H(39) 2.345 ? . 6_555 H(35) H(41) 3.538 ? . 6_555 H(36) O(1) 3.501 ? . . H(36) O(4) 3.373 ? . 6_555 H(36) O(8) 3.117 ? . 1_655 H(36) N(1) 3.302 ? . . H(36) N(2) 3.287 ? . . H(36) C(11) 3.297 ? . 6_555 H(36) C(12) 3.187 ? . . H(36) H(10) 2.978 ? . 6_555 H(36) H(11) 3.080 ? . 6_555 H(36) H(14) 2.367 ? . . H(36) H(20) 2.967 ? . 1_655 H(36) H(39) 3.117 ? . 1_655 H(36) H(39) 3.432 ? . 6_555 H(36) H(42) 3.375 ? . 1_655 H(37) O(4) 2.970 ? . 6_555 H(37) O(5) 3.012 ? . 6_555 H(37) O(8) 3.447 ? . 6_555 H(37) N(4) 3.031 ? . 6_555 H(37) C(11) 3.438 ? . 6_555 H(37) C(18) 3.302 ? . 6_555 H(37) C(20) 3.460 ? . 6_555 H(37) H(10) 3.535 ? . 6_555 H(37) H(11) 3.178 ? . 6_555 H(37) H(20) 3.327 ? . 6_555 H(37) H(21) 3.394 ? . 6_555 H(37) H(31) 2.927 ? . 6_555 H(37) H(32) 2.565 ? . 6_555 H(37) H(34) 3.128 ? . 6_555 H(37) H(35) 3.250 ? . 6_555 H(37) H(39) 3.293 ? . 1_655 H(37) H(39) 2.785 ? . 6_555 H(38) O(1) 3.033 ? . . H(38) O(5) 3.369 ? . 6_555 H(38) O(8) 3.383 ? . 1_655 H(38) N(1) 3.516 ? . . H(38) C(4) 3.299 ? . . H(38) C(5) 3.034 ? . . H(38) C(9) 3.520 ? . . H(38) C(10) 2.892 ? . . H(38) C(17) 3.496 ? . 6_555 H(38) C(18) 3.421 ? . 6_555 H(38) C(20) 3.337 ? . 6_555 H(38) C(31) 3.251 ? . 1_655 H(38) H(18) 3.425 ? . 6_555 H(38) H(20) 3.357 ? . 6_555 H(38) H(21) 2.828 ? . 6_555 H(38) H(39) 3.455 ? . 1_655 H(38) H(39) 3.390 ? . 6_555 H(38) H(41) 3.195 ? . 1_655 H(38) H(42) 2.759 ? . 1_655 H(39) O(7) 1.724 ? . 6_455 H(39) N(4) 3.164 ? . . H(39) C(20) 3.313 ? . . H(39) C(30) 3.478 ? . 1_455 H(39) C(30) 2.794 ? . 6_455 H(39) H(11) 2.951 ? . . H(39) H(20) 2.467 ? . . H(39) H(31) 3.399 ? . . H(39) H(32) 3.263 ? . . H(39) H(34) 2.422 ? . . H(39) H(35) 2.345 ? . 6_455 H(39) H(36) 3.117 ? . 1_455 H(39) H(36) 3.432 ? . 6_455 H(39) H(37) 3.293 ? . 1_455 H(39) H(37) 2.785 ? . 6_455 H(39) H(38) 3.455 ? . 1_455 H(39) H(38) 3.390 ? . 6_455 H(40) N(4) 3.509 ? . . H(40) C(11) 3.486 ? . . H(40) C(24) 3.561 ? . 5_655 H(40) C(25) 3.138 ? . 5_655 H(40) C(26) 2.982 ? . 5_655 H(40) C(27) 3.288 ? . 5_655 H(40) H(6) 3.575 ? . 1_455 H(40) H(11) 2.795 ? . . H(40) H(12) 3.539 ? . . H(40) H(26) 3.470 ? . 5_655 H(40) H(27) 3.234 ? . 5_655 H(40) H(29) 3.522 ? . . H(40) H(32) 3.589 ? . . H(40) H(34) 2.719 ? . . H(41) O(7) 3.110 ? . 6_455 H(41) C(11) 3.581 ? . . H(41) C(14) 3.252 ? . 6_455 H(41) C(15) 2.905 ? . 6_455 H(41) C(16) 2.941 ? . 6_455 H(41) C(17) 3.301 ? . 6_455 H(41) H(11) 2.644 ? . . H(41) H(16) 3.231 ? . 6_455 H(41) H(17) 3.285 ? . 6_455 H(41) H(34) 3.516 ? . . H(41) H(35) 3.538 ? . 6_455 H(41) H(38) 3.195 ? . 1_455 H(42) N(1) 3.581 ? . 1_455 H(42) C(4) 2.819 ? . 1_455 H(42) C(5) 3.078 ? . 1_455 H(42) C(6) 3.073 ? . 1_455 H(42) C(30) 3.455 ? . 1_455 H(42) H(4) 3.355 ? . 1_455 H(42) H(6) 2.563 ? . 1_455 H(42) H(7) 2.909 ? . 1_455 H(42) H(34) 3.476 ? . . H(42) H(36) 3.375 ? . 1_455 H(42) H(38) 2.759 ? . 1_455 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(7) H(35) O(1) . . . 2.751(3) 0.956 1.820 163.8 no O(8) H(39) O(7) . . 6_455 2.718(3) 1.008 1.724 167.9 no N(4) H(31) O(2) . . . 2.764(3) 0.958 2.021 132.9 no N(4) H(31) O(5) . . . 2.970(3) 0.958 2.129 145.7 no N(4) H(32) O(1) . . . 2.869(3) 0.959 2.172 128.6 no N(4) H(32) O(4) . . . 3.132(3) 0.959 2.241 154.1 no N(4) H(33) O(3) . . . 2.774(3) 0.965 1.995 136.3 no N(4) H(33) O(6) . . . 3.012(3) 0.965 2.193 141.9 no N(4) H(34) O(8) . . . 2.848(3) 0.960 1.938 157.4 no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data__080604k _database_code_depnum_ccdc_archive 'CCDC 812373' #TrackingRef 'NChem_All.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C29 H30 Mn N3 O6 ' _chemical_formula_moiety 'C29 H30 Mn N3 O6 ' _chemical_formula_weight 571.51 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 10.6650(8) _cell_length_b 15.9645(11) _cell_length_c 15.6061(9) _cell_angle_alpha 90.0000 _cell_angle_beta 92.637(2) _cell_angle_gamma 90.0000 _cell_volume 2654.3(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16153 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192.00 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 0.973 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 193.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 25633 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6046 _reflns_number_gt 4646 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0914 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6046 _refine_ls_number_parameters 353 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0368P)^2^+1.3357P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.32 _refine_diff_density_min -0.45 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Mn(1) Mn 0.43998(3) 0.231941(17) 0.625884(17) 0.01973(7) Uani 1.00 1 d . . . O(1) O 0.29718(12) 0.31709(8) 0.63949(8) 0.0257(2) Uani 1.00 1 d . . . O(2) O 0.32931(12) 0.13701(8) 0.62917(8) 0.0249(2) Uani 1.00 1 d . . . O(3) O 0.42271(12) 0.23576(8) 0.50539(8) 0.0231(2) Uani 1.00 1 d . . . O(4) O 0.06451(14) 0.38831(10) 0.59807(11) 0.0417(3) Uani 1.00 1 d . . . O(5) O 0.13371(15) 0.02519(9) 0.59807(10) 0.0392(3) Uani 1.00 1 d . . . O(6) O 0.24758(13) 0.20402(9) 0.38872(8) 0.0293(3) Uani 1.00 1 d . . . N(1) N 0.55811(15) 0.33666(10) 0.63569(10) 0.0251(3) Uani 1.00 1 d . . . N(2) N 0.48355(14) 0.21565(9) 0.75180(10) 0.0222(3) Uani 1.00 1 d . . . N(3) N 0.61527(15) 0.16340(10) 0.60680(10) 0.0259(3) Uani 1.00 1 d . . . C(1) C 0.8324(2) 0.26162(16) 0.77545(15) 0.0410(5) Uani 1.00 1 d . . . C(2) C 0.70776(18) 0.24962(13) 0.72395(13) 0.0284(4) Uani 1.00 1 d . . . C(3) C 0.69161(19) 0.32214(14) 0.65987(14) 0.0317(4) Uani 1.00 1 d . . . C(4) C 0.5249(2) 0.41310(13) 0.62209(12) 0.0284(4) Uani 1.00 1 d . . . C(5) C 0.40046(19) 0.44371(12) 0.60161(12) 0.0264(4) Uani 1.00 1 d . . . C(6) C 0.3889(2) 0.52810(13) 0.57655(13) 0.0332(4) Uani 1.00 1 d . . . C(7) C 0.2747(2) 0.56338(13) 0.55836(14) 0.0361(5) Uani 1.00 1 d . . . C(8) C 0.1672(2) 0.51438(14) 0.56466(14) 0.0358(5) Uani 1.00 1 d . . . C(9) C 0.1746(2) 0.43211(13) 0.58948(12) 0.0302(4) Uani 1.00 1 d . . . C(10) C 0.29246(19) 0.39319(12) 0.61085(11) 0.0245(4) Uani 1.00 1 d . . . C(11) C 0.0528(2) 0.31401(16) 0.5487(2) 0.0551(7) Uani 1.00 1 d . . . C(12) C 0.60128(19) 0.25209(13) 0.78766(12) 0.0283(4) Uani 1.00 1 d . . . C(13) C 0.41430(18) 0.17562(11) 0.80352(12) 0.0240(4) Uani 1.00 1 d . . . C(14) C 0.30443(18) 0.12720(12) 0.78118(12) 0.0248(4) Uani 1.00 1 d . . . C(15) C 0.2399(2) 0.09081(13) 0.84897(13) 0.0324(4) Uani 1.00 1 d . . . C(16) C 0.1424(2) 0.03684(14) 0.83235(15) 0.0387(5) Uani 1.00 1 d . . . C(17) C 0.1061(2) 0.01790(14) 0.74756(15) 0.0373(5) Uani 1.00 1 d . . . C(18) C 0.1678(2) 0.05186(13) 0.67984(13) 0.0298(4) Uani 1.00 1 d . . . C(19) C 0.26930(18) 0.10828(12) 0.69461(12) 0.0245(4) Uani 1.00 1 d . . . C(20) C 0.0910(2) 0.08942(16) 0.54010(16) 0.0480(6) Uani 1.00 1 d . . . C(21) C 0.71160(19) 0.16566(13) 0.67648(13) 0.0310(4) Uani 1.00 1 d . . . C(22) C 0.63300(19) 0.12105(13) 0.53897(12) 0.0280(4) Uani 1.00 1 d . . . C(23) C 0.54188(19) 0.11367(12) 0.46762(12) 0.0257(4) Uani 1.00 1 d . . . C(24) C 0.5583(2) 0.04862(13) 0.40834(13) 0.0323(4) Uani 1.00 1 d . . . C(25) C 0.4714(2) 0.03570(13) 0.34258(13) 0.0341(4) Uani 1.00 1 d . . . C(26) C 0.3648(2) 0.08551(13) 0.33419(12) 0.0314(4) Uani 1.00 1 d . . . C(27) C 0.34732(18) 0.15054(12) 0.39120(12) 0.0252(4) Uani 1.00 1 d . . . C(28) C 0.43803(18) 0.16788(11) 0.45790(11) 0.0222(3) Uani 1.00 1 d . . . C(29) C 0.1497(2) 0.18938(16) 0.32565(14) 0.0395(5) Uani 1.00 1 d . . . H(1) H 0.8264 0.3105 0.8130 0.049 Uiso 1.00 1 c R . . H(2) H 0.9000 0.2703 0.7359 0.049 Uiso 1.00 1 c R . . H(3) H 0.8505 0.2117 0.8104 0.049 Uiso 1.00 1 c R . . H(4) H 0.7282 0.3738 0.6858 0.038 Uiso 1.00 1 c R . . H(5) H 0.7376 0.3091 0.6078 0.038 Uiso 1.00 1 c R . . H(6) H 0.5899 0.4538 0.6260 0.034 Uiso 1.00 1 c R . . H(7) H 0.4624 0.5612 0.5723 0.040 Uiso 1.00 1 c R . . H(8) H 0.2682 0.6205 0.5416 0.043 Uiso 1.00 1 c R . . H(9) H 0.0872 0.5385 0.5515 0.043 Uiso 1.00 1 c R . . H(10) H 0.0131 0.3270 0.4924 0.066 Uiso 1.00 1 c R . . H(11) H 0.0010 0.2735 0.5784 0.066 Uiso 1.00 1 c R . . H(12) H 0.1362 0.2901 0.5412 0.066 Uiso 1.00 1 c R . . H(13) H 0.6282 0.2210 0.8402 0.034 Uiso 1.00 1 c R . . H(14) H 0.5860 0.3110 0.8042 0.034 Uiso 1.00 1 c R . . H(15) H 0.4386 0.1785 0.8628 0.029 Uiso 1.00 1 c R . . H(16) H 0.2645 0.1040 0.9067 0.039 Uiso 1.00 1 c R . . H(17) H 0.0997 0.0124 0.8782 0.046 Uiso 1.00 1 c R . . H(18) H 0.0375 -0.0191 0.7362 0.045 Uiso 1.00 1 c R . . H(19) H 0.1607 0.1273 0.5290 0.058 Uiso 1.00 1 c R . . H(20) H 0.0232 0.1210 0.5654 0.058 Uiso 1.00 1 c R . . H(21) H 0.0599 0.0640 0.4860 0.058 Uiso 1.00 1 c R . . H(22) H 0.7954 0.1578 0.6528 0.037 Uiso 1.00 1 c R . . H(23) H 0.6974 0.1194 0.7171 0.037 Uiso 1.00 1 c R . . H(24) H 0.7108 0.0926 0.5351 0.034 Uiso 1.00 1 c R . . H(25) H 0.6302 0.0135 0.4140 0.039 Uiso 1.00 1 c R . . H(26) H 0.4840 -0.0077 0.3023 0.041 Uiso 1.00 1 c R . . H(27) H 0.3037 0.0750 0.2893 0.038 Uiso 1.00 1 c R . . H(28) H 0.0828 0.2307 0.3321 0.047 Uiso 1.00 1 c R . . H(29) H 0.1159 0.1329 0.3330 0.047 Uiso 1.00 1 c R . . H(30) H 0.1830 0.1945 0.2684 0.047 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.01887(14) 0.02120(15) 0.01893(14) -0.00097(11) -0.00126(10) -0.00006(11) O(1) 0.0277(7) 0.0236(6) 0.0259(6) 0.0020(5) 0.0030(5) 0.0010(5) O(2) 0.0272(7) 0.0251(6) 0.0226(6) -0.0032(5) 0.0016(5) -0.0001(5) O(3) 0.0245(6) 0.0242(6) 0.0204(6) 0.0034(5) -0.0016(4) -0.0012(5) O(4) 0.0279(8) 0.0395(8) 0.0584(10) 0.0047(7) 0.0091(7) 0.0009(7) O(5) 0.0441(9) 0.0328(8) 0.0399(8) -0.0102(7) -0.0072(6) -0.0034(6) O(6) 0.0246(7) 0.0379(8) 0.0250(7) 0.0009(6) -0.0047(5) -0.0021(6) N(1) 0.0229(8) 0.0285(8) 0.0236(8) -0.0012(6) -0.0013(6) 0.0011(6) N(2) 0.0225(8) 0.0222(8) 0.0216(7) 0.0000(6) -0.0014(5) -0.0001(6) N(3) 0.0234(8) 0.0288(8) 0.0253(8) 0.0039(6) -0.0019(6) 0.0012(6) C(1) 0.0256(11) 0.0549(14) 0.0412(12) -0.0037(10) -0.0116(9) 0.0026(11) C(2) 0.0204(9) 0.0360(11) 0.0284(10) -0.0018(8) -0.0046(7) 0.0024(8) C(3) 0.0224(10) 0.0361(11) 0.0363(11) -0.0055(8) -0.0030(8) 0.0036(9) C(4) 0.0319(10) 0.0283(10) 0.0248(9) -0.0065(8) -0.0003(7) -0.0008(8) C(5) 0.0313(10) 0.0254(9) 0.0224(9) -0.0007(8) -0.0003(7) -0.0002(7) C(6) 0.0437(13) 0.0248(10) 0.0310(10) -0.0037(9) -0.0006(9) 0.0004(8) C(7) 0.0493(14) 0.0226(10) 0.0364(11) 0.0057(9) 0.0004(9) 0.0025(8) C(8) 0.0388(12) 0.0346(11) 0.0340(11) 0.0124(9) 0.0016(9) 0.0006(9) C(9) 0.0322(11) 0.0316(10) 0.0269(10) 0.0049(8) 0.0047(8) -0.0022(8) C(10) 0.0318(10) 0.0242(9) 0.0177(8) 0.0031(8) 0.0030(7) -0.0031(7) C(11) 0.0350(14) 0.0411(14) 0.089(2) -0.0047(11) -0.0020(13) -0.0095(14) C(12) 0.0277(10) 0.0332(11) 0.0233(9) -0.0036(8) -0.0060(7) -0.0009(8) C(13) 0.0298(10) 0.0215(9) 0.0206(9) 0.0059(7) -0.0004(7) -0.0003(7) C(14) 0.0252(10) 0.0222(9) 0.0271(9) 0.0024(7) 0.0040(7) 0.0004(7) C(15) 0.0340(11) 0.0343(11) 0.0295(10) 0.0020(9) 0.0075(8) 0.0034(8) C(16) 0.0350(12) 0.0392(12) 0.0429(12) -0.0034(10) 0.0147(9) 0.0061(10) C(17) 0.0291(11) 0.0330(11) 0.0501(13) -0.0073(9) 0.0063(9) 0.0015(10) C(18) 0.0290(10) 0.0251(10) 0.0351(11) -0.0023(8) -0.0008(8) -0.0003(8) C(19) 0.0235(9) 0.0198(9) 0.0303(10) 0.0020(7) 0.0035(7) -0.0004(7) C(20) 0.0504(15) 0.0460(14) 0.0462(14) -0.0140(12) -0.0124(11) 0.0048(11) C(21) 0.0213(10) 0.0394(12) 0.0317(10) 0.0056(8) -0.0052(7) 0.0020(9) C(22) 0.0257(10) 0.0294(10) 0.0291(10) 0.0071(8) 0.0032(7) 0.0035(8) C(23) 0.0305(10) 0.0265(9) 0.0205(9) 0.0021(8) 0.0047(7) 0.0035(7) C(24) 0.0428(12) 0.0278(10) 0.0267(10) 0.0085(9) 0.0079(8) 0.0029(8) C(25) 0.0531(14) 0.0261(10) 0.0233(10) 0.0029(9) 0.0055(9) -0.0024(8) C(26) 0.0411(12) 0.0310(10) 0.0220(9) -0.0067(9) 0.0002(8) -0.0003(8) C(27) 0.0279(10) 0.0267(9) 0.0213(9) -0.0024(8) 0.0021(7) 0.0029(7) C(28) 0.0265(9) 0.0234(9) 0.0168(8) -0.0002(7) 0.0025(7) 0.0007(7) C(29) 0.0268(11) 0.0592(15) 0.0315(11) -0.0027(10) -0.0089(8) -0.0034(10) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mn(1) O(1) 2.0596(13) yes . . Mn(1) O(2) 1.9230(13) yes . . Mn(1) O(3) 1.8820(12) yes . . Mn(1) N(1) 2.0947(16) yes . . Mn(1) N(2) 2.0152(15) yes . . Mn(1) N(3) 2.1982(16) yes . . O(1) C(10) 1.295(2) yes . . O(2) C(19) 1.313(2) yes . . O(3) C(28) 1.327(2) yes . . O(4) C(9) 1.378(2) yes . . O(4) C(11) 1.417(3) yes . . O(5) C(18) 1.378(2) yes . . O(5) C(20) 1.428(2) yes . . O(6) C(27) 1.363(2) yes . . O(6) C(29) 1.420(2) yes . . N(1) C(3) 1.474(2) yes . . N(1) C(4) 1.286(2) yes . . N(2) C(12) 1.471(2) yes . . N(2) C(13) 1.288(2) yes . . N(3) C(21) 1.462(2) yes . . N(3) C(22) 1.277(2) yes . . C(1) C(2) 1.533(2) yes . . C(2) C(3) 1.534(3) yes . . C(2) C(12) 1.544(2) yes . . C(2) C(21) 1.533(2) yes . . C(4) C(5) 1.437(2) yes . . C(5) C(6) 1.407(2) yes . . C(5) C(10) 1.419(2) yes . . C(6) C(7) 1.360(3) yes . . C(7) C(8) 1.395(3) yes . . C(8) C(9) 1.371(3) yes . . C(9) C(10) 1.428(2) yes . . C(13) C(14) 1.433(2) yes . . C(14) C(15) 1.413(2) yes . . C(14) C(19) 1.418(2) yes . . C(15) C(16) 1.366(3) yes . . C(16) C(17) 1.395(3) yes . . C(17) C(18) 1.381(3) yes . . C(18) C(19) 1.419(2) yes . . C(22) C(23) 1.449(2) yes . . C(23) C(24) 1.407(2) yes . . C(23) C(28) 1.408(2) yes . . C(24) C(25) 1.367(2) yes . . C(25) C(26) 1.389(3) yes . . C(26) C(27) 1.385(2) yes . . C(27) C(28) 1.415(2) yes . . C(1) H(1) 0.980 no . . C(1) H(2) 0.980 no . . C(1) H(3) 0.980 no . . C(3) H(4) 0.990 no . . C(3) H(5) 0.990 no . . C(4) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(11) H(10) 0.980 no . . C(11) H(11) 0.980 no . . C(11) H(12) 0.980 no . . C(12) H(13) 0.990 no . . C(12) H(14) 0.990 no . . C(13) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(17) H(18) 0.950 no . . C(20) H(19) 0.980 no . . C(20) H(20) 0.980 no . . C(20) H(21) 0.980 no . . C(21) H(22) 0.990 no . . C(21) H(23) 0.990 no . . C(22) H(24) 0.950 no . . C(24) H(25) 0.950 no . . C(25) H(26) 0.950 no . . C(26) H(27) 0.950 no . . C(29) H(28) 0.980 no . . C(29) H(29) 0.980 no . . C(29) H(30) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Mn(1) O(2) 93.42(5) yes . . . O(1) Mn(1) O(3) 92.45(5) yes . . . O(1) Mn(1) N(1) 84.88(5) yes . . . O(1) Mn(1) N(2) 97.07(5) yes . . . O(1) Mn(1) N(3) 168.52(5) yes . . . O(2) Mn(1) O(3) 91.16(5) yes . . . O(2) Mn(1) N(1) 174.18(5) yes . . . O(2) Mn(1) N(2) 89.23(5) yes . . . O(2) Mn(1) N(3) 97.94(5) yes . . . O(3) Mn(1) N(1) 94.48(5) yes . . . O(3) Mn(1) N(2) 170.43(6) yes . . . O(3) Mn(1) N(3) 85.73(5) yes . . . N(1) Mn(1) N(2) 85.46(6) yes . . . N(1) Mn(1) N(3) 83.96(6) yes . . . N(2) Mn(1) N(3) 84.75(5) yes . . . Mn(1) O(1) C(10) 126.94(12) yes . . . Mn(1) O(2) C(19) 128.16(11) yes . . . Mn(1) O(3) C(28) 121.51(11) yes . . . C(9) O(4) C(11) 115.23(17) yes . . . C(18) O(5) C(20) 115.31(16) yes . . . C(27) O(6) C(29) 117.65(15) yes . . . Mn(1) N(1) C(3) 117.63(12) yes . . . Mn(1) N(1) C(4) 125.84(13) yes . . . C(3) N(1) C(4) 116.54(17) yes . . . Mn(1) N(2) C(12) 118.33(11) yes . . . Mn(1) N(2) C(13) 124.18(12) yes . . . C(12) N(2) C(13) 117.50(15) yes . . . Mn(1) N(3) C(21) 117.38(12) yes . . . Mn(1) N(3) C(22) 122.34(13) yes . . . C(21) N(3) C(22) 120.25(16) yes . . . C(1) C(2) C(3) 108.42(17) yes . . . C(1) C(2) C(12) 107.75(16) yes . . . C(1) C(2) C(21) 108.71(16) yes . . . C(3) C(2) C(12) 109.67(16) yes . . . C(3) C(2) C(21) 110.46(16) yes . . . C(12) C(2) C(21) 111.74(16) yes . . . N(1) C(3) C(2) 111.32(16) yes . . . N(1) C(4) C(5) 127.17(19) yes . . . C(4) C(5) C(6) 117.12(18) yes . . . C(4) C(5) C(10) 122.01(17) yes . . . C(6) C(5) C(10) 120.76(18) yes . . . C(5) C(6) C(7) 121.4(2) yes . . . C(6) C(7) C(8) 118.95(19) yes . . . C(7) C(8) C(9) 121.4(2) yes . . . O(4) C(9) C(8) 118.39(19) yes . . . O(4) C(9) C(10) 120.08(17) yes . . . C(8) C(9) C(10) 121.44(19) yes . . . O(1) C(10) C(5) 123.34(17) yes . . . O(1) C(10) C(9) 120.58(17) yes . . . C(5) C(10) C(9) 116.04(17) yes . . . N(2) C(12) C(2) 112.65(15) yes . . . N(2) C(13) C(14) 126.93(17) yes . . . C(13) C(14) C(15) 117.42(16) yes . . . C(13) C(14) C(19) 121.59(17) yes . . . C(15) C(14) C(19) 120.61(17) yes . . . C(14) C(15) C(16) 120.65(19) yes . . . C(15) C(16) C(17) 119.5(2) yes . . . C(16) C(17) C(18) 121.3(2) yes . . . O(5) C(18) C(17) 118.22(18) yes . . . O(5) C(18) C(19) 120.87(18) yes . . . C(17) C(18) C(19) 120.77(18) yes . . . O(2) C(19) C(14) 123.37(17) yes . . . O(2) C(19) C(18) 119.41(16) yes . . . C(14) C(19) C(18) 117.14(17) yes . . . N(3) C(21) C(2) 110.34(16) yes . . . N(3) C(22) C(23) 124.08(18) yes . . . C(22) C(23) C(24) 117.77(18) yes . . . C(22) C(23) C(28) 121.96(17) yes . . . C(24) C(23) C(28) 120.26(17) yes . . . C(23) C(24) C(25) 120.28(19) yes . . . C(24) C(25) C(26) 120.57(19) yes . . . C(25) C(26) C(27) 120.16(18) yes . . . O(6) C(27) C(26) 125.38(17) yes . . . O(6) C(27) C(28) 113.86(16) yes . . . C(26) C(27) C(28) 120.75(17) yes . . . O(3) C(28) C(23) 123.92(16) yes . . . O(3) C(28) C(27) 118.22(16) yes . . . C(23) C(28) C(27) 117.81(16) yes . . . C(2) C(1) H(1) 109.5 no . . . C(2) C(1) H(2) 109.5 no . . . C(2) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . N(1) C(3) H(4) 109.4 no . . . N(1) C(3) H(5) 109.4 no . . . C(2) C(3) H(4) 109.4 no . . . C(2) C(3) H(5) 109.4 no . . . H(4) C(3) H(5) 108.0 no . . . N(1) C(4) H(6) 116.4 no . . . C(5) C(4) H(6) 116.4 no . . . C(5) C(6) H(7) 119.3 no . . . C(7) C(6) H(7) 119.3 no . . . C(6) C(7) H(8) 120.5 no . . . C(8) C(7) H(8) 120.5 no . . . C(7) C(8) H(9) 119.3 no . . . C(9) C(8) H(9) 119.3 no . . . O(4) C(11) H(10) 109.5 no . . . O(4) C(11) H(11) 109.5 no . . . O(4) C(11) H(12) 109.5 no . . . H(10) C(11) H(11) 109.5 no . . . H(10) C(11) H(12) 109.5 no . . . H(11) C(11) H(12) 109.5 no . . . N(2) C(12) H(13) 109.1 no . . . N(2) C(12) H(14) 109.1 no . . . C(2) C(12) H(13) 109.1 no . . . C(2) C(12) H(14) 109.1 no . . . H(13) C(12) H(14) 107.8 no . . . N(2) C(13) H(15) 116.5 no . . . C(14) C(13) H(15) 116.5 no . . . C(14) C(15) H(16) 119.7 no . . . C(16) C(15) H(16) 119.7 no . . . C(15) C(16) H(17) 120.2 no . . . C(17) C(16) H(17) 120.2 no . . . C(16) C(17) H(18) 119.4 no . . . C(18) C(17) H(18) 119.4 no . . . O(5) C(20) H(19) 109.5 no . . . O(5) C(20) H(20) 109.5 no . . . O(5) C(20) H(21) 109.5 no . . . H(19) C(20) H(20) 109.5 no . . . H(19) C(20) H(21) 109.5 no . . . H(20) C(20) H(21) 109.5 no . . . N(3) C(21) H(22) 109.6 no . . . N(3) C(21) H(23) 109.6 no . . . C(2) C(21) H(22) 109.6 no . . . C(2) C(21) H(23) 109.6 no . . . H(22) C(21) H(23) 108.1 no . . . N(3) C(22) H(24) 118.0 no . . . C(23) C(22) H(24) 118.0 no . . . C(23) C(24) H(25) 119.9 no . . . C(25) C(24) H(25) 119.9 no . . . C(24) C(25) H(26) 119.7 no . . . C(26) C(25) H(26) 119.7 no . . . C(25) C(26) H(27) 119.9 no . . . C(27) C(26) H(27) 119.9 no . . . O(6) C(29) H(28) 109.5 no . . . O(6) C(29) H(29) 109.5 no . . . O(6) C(29) H(30) 109.5 no . . . H(28) C(29) H(29) 109.5 no . . . H(28) C(29) H(30) 109.5 no . . . H(29) C(29) H(30) 109.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(26) 3.460(2) ? . 4_555 O(1) C(29) 3.368(2) ? . 4_555 O(2) C(24) 3.260(2) ? . 3_656 O(2) C(25) 3.497(2) ? . 3_656 O(3) C(13) 3.451(2) ? . 4_554 O(4) C(16) 3.449(2) ? . 2_556 O(5) C(24) 3.495(2) ? . 3_656 O(6) C(13) 2.973(2) ? . 4_554 O(6) C(14) 3.246(2) ? . 4_554 O(6) C(15) 3.334(2) ? . 4_554 N(2) C(27) 3.420(2) ? . 4_555 N(3) C(25) 3.413(2) ? . 3_656 C(1) C(29) 3.526(3) ? . 4_655 C(4) C(6) 3.406(2) ? . 3_666 C(6) C(4) 3.406(2) ? . 3_666 C(6) C(6) 3.557(3) ? . 3_666 C(10) C(26) 3.551(2) ? . 4_555 C(12) C(27) 3.573(2) ? . 4_555 C(12) C(28) 3.485(2) ? . 4_555 C(13) O(3) 3.451(2) ? . 4_555 C(13) O(6) 2.973(2) ? . 4_555 C(13) C(27) 3.190(2) ? . 4_555 C(13) C(28) 3.472(2) ? . 4_555 C(13) C(29) 3.580(2) ? . 4_555 C(14) O(6) 3.246(2) ? . 4_555 C(14) C(29) 3.447(3) ? . 4_555 C(15) O(6) 3.334(2) ? . 4_555 C(16) O(4) 3.449(2) ? . 2_546 C(19) C(24) 3.536(2) ? . 3_656 C(22) C(24) 3.512(2) ? . 3_656 C(22) C(25) 3.333(2) ? . 3_656 C(23) C(24) 3.434(2) ? . 3_656 C(24) O(2) 3.260(2) ? . 3_656 C(24) O(5) 3.495(2) ? . 3_656 C(24) C(19) 3.536(2) ? . 3_656 C(24) C(22) 3.512(2) ? . 3_656 C(24) C(23) 3.434(2) ? . 3_656 C(24) C(24) 3.531(2) ? . 3_656 C(25) O(2) 3.497(2) ? . 3_656 C(25) N(3) 3.413(2) ? . 3_656 C(25) C(22) 3.333(2) ? . 3_656 C(26) O(1) 3.460(2) ? . 4_554 C(26) C(10) 3.551(2) ? . 4_554 C(27) N(2) 3.420(2) ? . 4_554 C(27) C(12) 3.573(2) ? . 4_554 C(27) C(13) 3.190(2) ? . 4_554 C(28) C(12) 3.485(2) ? . 4_554 C(28) C(13) 3.472(2) ? . 4_554 C(29) O(1) 3.368(2) ? . 4_554 C(29) C(1) 3.526(3) ? . 4_454 C(29) C(13) 3.580(2) ? . 4_554 C(29) C(14) 3.447(3) ? . 4_554 O(1) H(27) 2.902 ? . 4_555 O(1) H(30) 2.406 ? . 4_555 O(2) H(25) 2.539 ? . 3_656 O(2) H(26) 3.029 ? . 3_656 O(3) H(13) 3.528 ? . 4_554 O(3) H(15) 2.625 ? . 4_554 O(3) H(16) 3.395 ? . 4_554 O(4) H(2) 3.406 ? . 1_455 O(4) H(9) 3.014 ? . 3_566 O(4) H(17) 2.681 ? . 2_556 O(4) H(18) 3.213 ? . 2_556 O(4) H(30) 3.178 ? . 4_555 O(5) H(21) 2.787 ? . 3_556 O(5) H(24) 3.305 ? . 3_656 O(5) H(25) 2.608 ? . 3_656 O(6) H(15) 2.812 ? . 4_554 O(6) H(16) 3.082 ? . 4_554 N(1) H(8) 3.468 ? . 3_666 N(2) H(26) 3.446 ? . 3_656 N(2) H(30) 3.532 ? . 4_555 N(3) H(26) 3.074 ? . 3_656 C(1) H(28) 2.777 ? . 4_655 C(1) H(29) 3.541 ? . 4_655 C(3) H(8) 3.322 ? . 3_666 C(4) H(7) 3.070 ? . 3_666 C(4) H(8) 3.493 ? . 3_666 C(4) H(26) 3.239 ? . 4_555 C(5) H(7) 3.142 ? . 3_666 C(5) H(16) 3.396 ? . 4_554 C(5) H(26) 3.374 ? . 4_555 C(5) H(27) 3.163 ? . 4_555 C(6) H(6) 3.193 ? . 3_666 C(6) H(7) 3.206 ? . 3_666 C(6) H(13) 3.350 ? . 2_656 C(6) H(15) 3.144 ? . 2_656 C(6) H(16) 3.594 ? . 4_554 C(7) H(3) 3.440 ? . 2_656 C(7) H(5) 3.294 ? . 3_666 C(7) H(6) 3.290 ? . 3_666 C(7) H(10) 3.589 ? . 3_566 C(7) H(13) 3.124 ? . 2_656 C(7) H(16) 3.569 ? . 4_554 C(7) H(17) 3.517 ? . 4_554 C(8) H(9) 3.303 ? . 3_566 C(8) H(10) 3.277 ? . 3_566 C(8) H(16) 3.311 ? . 4_554 C(8) H(17) 3.022 ? . 2_556 C(8) H(17) 2.996 ? . 4_554 C(9) H(9) 3.506 ? . 3_566 C(9) H(16) 3.106 ? . 4_554 C(9) H(17) 3.254 ? . 2_556 C(9) H(17) 3.472 ? . 4_554 C(9) H(27) 3.352 ? . 4_555 C(9) H(30) 3.444 ? . 4_555 C(10) H(16) 3.187 ? . 4_554 C(10) H(27) 2.827 ? . 4_555 C(10) H(30) 3.103 ? . 4_555 C(11) H(2) 3.481 ? . 1_455 C(11) H(5) 3.527 ? . 1_455 C(11) H(9) 3.162 ? . 3_566 C(11) H(16) 3.491 ? . 4_554 C(13) H(7) 2.931 ? . 2_646 C(13) H(26) 3.354 ? . 3_656 C(13) H(30) 3.250 ? . 4_555 C(14) H(6) 3.298 ? . 2_646 C(14) H(7) 3.465 ? . 2_646 C(14) H(26) 3.270 ? . 3_656 C(14) H(28) 3.397 ? . 4_555 C(14) H(30) 3.130 ? . 4_555 C(15) H(4) 3.526 ? . 2_646 C(15) H(6) 2.858 ? . 2_646 C(15) H(7) 3.385 ? . 2_646 C(15) H(28) 3.310 ? . 4_555 C(16) H(4) 2.966 ? . 2_646 C(16) H(6) 3.187 ? . 2_646 C(16) H(9) 3.113 ? . 2_546 C(17) H(1) 3.526 ? . 2_646 C(17) H(4) 3.055 ? . 2_646 C(17) H(29) 3.564 ? . 3_556 C(18) H(25) 2.859 ? . 3_656 C(19) H(25) 2.824 ? . 3_656 C(19) H(26) 3.081 ? . 3_656 C(19) H(30) 3.491 ? . 4_555 C(20) H(21) 2.949 ? . 3_556 C(20) H(25) 3.444 ? . 3_656 C(21) H(26) 3.299 ? . 3_656 C(22) H(26) 3.355 ? . 3_656 C(23) H(13) 3.455 ? . 4_554 C(23) H(14) 2.879 ? . 4_554 C(23) H(25) 3.349 ? . 3_656 C(24) H(14) 2.793 ? . 4_554 C(25) H(14) 2.813 ? . 4_554 C(25) H(23) 3.175 ? . 3_656 C(25) H(24) 3.458 ? . 3_656 C(26) H(14) 2.936 ? . 4_554 C(26) H(23) 3.425 ? . 3_656 C(27) H(14) 3.003 ? . 4_554 C(27) H(15) 2.938 ? . 4_554 C(28) H(13) 3.314 ? . 4_554 C(28) H(14) 2.951 ? . 4_554 C(28) H(15) 2.867 ? . 4_554 C(29) H(1) 3.445 ? . 4_454 C(29) H(2) 3.020 ? . 4_454 C(29) H(3) 3.559 ? . 4_454 C(29) H(18) 3.483 ? . 3_556 H(1) C(17) 3.526 ? . 2_656 H(1) C(29) 3.445 ? . 4_655 H(1) H(18) 3.193 ? . 2_656 H(1) H(28) 2.816 ? . 4_655 H(1) H(29) 3.219 ? . 4_655 H(2) O(4) 3.406 ? . 1_655 H(2) C(11) 3.481 ? . 1_655 H(2) C(29) 3.020 ? . 4_655 H(2) H(11) 2.730 ? . 1_655 H(2) H(18) 3.451 ? . 2_656 H(2) H(28) 2.405 ? . 4_655 H(2) H(29) 3.108 ? . 4_655 H(2) H(30) 3.088 ? . 4_655 H(3) C(7) 3.440 ? . 2_646 H(3) C(29) 3.559 ? . 4_655 H(3) H(8) 3.054 ? . 2_646 H(3) H(9) 3.549 ? . 2_646 H(3) H(10) 3.318 ? . 4_655 H(3) H(28) 2.651 ? . 4_655 H(4) C(15) 3.526 ? . 2_656 H(4) C(16) 2.966 ? . 2_656 H(4) C(17) 3.055 ? . 2_656 H(4) H(8) 3.552 ? . 3_666 H(4) H(17) 3.071 ? . 2_656 H(4) H(18) 3.221 ? . 2_656 H(5) C(7) 3.294 ? . 3_666 H(5) C(11) 3.527 ? . 1_655 H(5) H(8) 2.587 ? . 3_666 H(5) H(10) 3.527 ? . 1_655 H(5) H(11) 2.923 ? . 1_655 H(6) C(6) 3.193 ? . 3_666 H(6) C(7) 3.290 ? . 3_666 H(6) C(14) 3.298 ? . 2_656 H(6) C(15) 2.858 ? . 2_656 H(6) C(16) 3.187 ? . 2_656 H(6) H(7) 3.128 ? . 3_666 H(6) H(8) 3.303 ? . 3_666 H(6) H(16) 2.914 ? . 2_656 H(6) H(17) 3.444 ? . 2_656 H(6) H(26) 3.141 ? . 4_555 H(7) C(4) 3.070 ? . 3_666 H(7) C(5) 3.142 ? . 3_666 H(7) C(6) 3.206 ? . 3_666 H(7) C(13) 2.931 ? . 2_656 H(7) C(14) 3.465 ? . 2_656 H(7) C(15) 3.385 ? . 2_656 H(7) H(6) 3.128 ? . 3_666 H(7) H(7) 3.115 ? . 3_666 H(7) H(13) 3.071 ? . 2_656 H(7) H(15) 2.356 ? . 2_656 H(7) H(16) 2.995 ? . 2_656 H(8) N(1) 3.468 ? . 3_666 H(8) C(3) 3.322 ? . 3_666 H(8) C(4) 3.493 ? . 3_666 H(8) H(3) 3.054 ? . 2_656 H(8) H(4) 3.552 ? . 3_666 H(8) H(5) 2.587 ? . 3_666 H(8) H(6) 3.303 ? . 3_666 H(8) H(10) 3.136 ? . 3_566 H(8) H(13) 2.647 ? . 2_656 H(8) H(15) 3.526 ? . 2_656 H(9) O(4) 3.014 ? . 3_566 H(9) C(8) 3.303 ? . 3_566 H(9) C(9) 3.506 ? . 3_566 H(9) C(11) 3.162 ? . 3_566 H(9) C(16) 3.113 ? . 2_556 H(9) H(3) 3.549 ? . 2_656 H(9) H(9) 2.698 ? . 3_566 H(9) H(10) 2.480 ? . 3_566 H(9) H(17) 2.356 ? . 2_556 H(9) H(17) 2.833 ? . 4_554 H(10) C(7) 3.589 ? . 3_566 H(10) C(8) 3.277 ? . 3_566 H(10) H(3) 3.318 ? . 4_454 H(10) H(5) 3.527 ? . 1_455 H(10) H(8) 3.136 ? . 3_566 H(10) H(9) 2.480 ? . 3_566 H(10) H(16) 3.244 ? . 4_554 H(10) H(17) 3.279 ? . 4_554 H(11) H(2) 2.730 ? . 1_455 H(11) H(5) 2.923 ? . 1_455 H(11) H(22) 3.131 ? . 1_455 H(11) H(30) 3.506 ? . 4_555 H(12) H(16) 3.067 ? . 4_554 H(12) H(30) 3.565 ? . 4_555 H(13) O(3) 3.528 ? . 4_555 H(13) C(6) 3.350 ? . 2_646 H(13) C(7) 3.124 ? . 2_646 H(13) C(23) 3.455 ? . 4_555 H(13) C(28) 3.314 ? . 4_555 H(13) H(7) 3.071 ? . 2_646 H(13) H(8) 2.647 ? . 2_646 H(14) C(23) 2.879 ? . 4_555 H(14) C(24) 2.793 ? . 4_555 H(14) C(25) 2.813 ? . 4_555 H(14) C(26) 2.936 ? . 4_555 H(14) C(27) 3.003 ? . 4_555 H(14) C(28) 2.951 ? . 4_555 H(14) H(25) 3.307 ? . 4_555 H(14) H(26) 3.324 ? . 4_555 H(14) H(27) 3.517 ? . 4_555 H(15) O(3) 2.625 ? . 4_555 H(15) O(6) 2.812 ? . 4_555 H(15) C(6) 3.144 ? . 2_646 H(15) C(27) 2.938 ? . 4_555 H(15) C(28) 2.867 ? . 4_555 H(15) H(7) 2.356 ? . 2_646 H(15) H(8) 3.526 ? . 2_646 H(16) O(3) 3.395 ? . 4_555 H(16) O(6) 3.082 ? . 4_555 H(16) C(5) 3.396 ? . 4_555 H(16) C(6) 3.594 ? . 4_555 H(16) C(7) 3.569 ? . 4_555 H(16) C(8) 3.311 ? . 4_555 H(16) C(9) 3.106 ? . 4_555 H(16) C(10) 3.187 ? . 4_555 H(16) C(11) 3.491 ? . 4_555 H(16) H(6) 2.914 ? . 2_646 H(16) H(7) 2.995 ? . 2_646 H(16) H(10) 3.244 ? . 4_555 H(16) H(12) 3.067 ? . 4_555 H(16) H(28) 3.445 ? . 4_555 H(17) O(4) 2.681 ? . 2_546 H(17) C(7) 3.517 ? . 4_555 H(17) C(8) 3.022 ? . 2_546 H(17) C(8) 2.996 ? . 4_555 H(17) C(9) 3.254 ? . 2_546 H(17) C(9) 3.472 ? . 4_555 H(17) H(4) 3.071 ? . 2_646 H(17) H(6) 3.444 ? . 2_646 H(17) H(9) 2.356 ? . 2_546 H(17) H(9) 2.833 ? . 4_555 H(17) H(10) 3.279 ? . 4_555 H(18) O(4) 3.213 ? . 2_546 H(18) C(29) 3.483 ? . 3_556 H(18) H(1) 3.193 ? . 2_646 H(18) H(2) 3.451 ? . 2_646 H(18) H(4) 3.221 ? . 2_646 H(18) H(29) 2.642 ? . 3_556 H(19) H(25) 3.262 ? . 3_656 H(20) H(21) 3.176 ? . 3_556 H(20) H(22) 2.901 ? . 1_455 H(20) H(24) 3.374 ? . 1_455 H(21) O(5) 2.787 ? . 3_556 H(21) C(20) 2.949 ? . 3_556 H(21) H(20) 3.176 ? . 3_556 H(21) H(21) 2.460 ? . 3_556 H(21) H(24) 3.523 ? . 3_656 H(22) H(11) 3.131 ? . 1_655 H(22) H(20) 2.901 ? . 1_655 H(23) C(25) 3.175 ? . 3_656 H(23) C(26) 3.425 ? . 3_656 H(23) H(26) 2.638 ? . 3_656 H(23) H(27) 3.104 ? . 3_656 H(24) O(5) 3.305 ? . 3_656 H(24) C(25) 3.458 ? . 3_656 H(24) H(20) 3.374 ? . 1_655 H(24) H(21) 3.523 ? . 3_656 H(25) O(2) 2.539 ? . 3_656 H(25) O(5) 2.608 ? . 3_656 H(25) C(18) 2.859 ? . 3_656 H(25) C(19) 2.824 ? . 3_656 H(25) C(20) 3.444 ? . 3_656 H(25) C(23) 3.349 ? . 3_656 H(25) H(14) 3.307 ? . 4_554 H(25) H(19) 3.262 ? . 3_656 H(26) O(2) 3.029 ? . 3_656 H(26) N(2) 3.446 ? . 3_656 H(26) N(3) 3.074 ? . 3_656 H(26) C(4) 3.239 ? . 4_554 H(26) C(5) 3.374 ? . 4_554 H(26) C(13) 3.354 ? . 3_656 H(26) C(14) 3.270 ? . 3_656 H(26) C(19) 3.081 ? . 3_656 H(26) C(21) 3.299 ? . 3_656 H(26) C(22) 3.355 ? . 3_656 H(26) H(6) 3.141 ? . 4_554 H(26) H(14) 3.324 ? . 4_554 H(26) H(23) 2.638 ? . 3_656 H(27) O(1) 2.902 ? . 4_554 H(27) C(5) 3.163 ? . 4_554 H(27) C(9) 3.352 ? . 4_554 H(27) C(10) 2.827 ? . 4_554 H(27) H(14) 3.517 ? . 4_554 H(27) H(23) 3.104 ? . 3_656 H(28) C(1) 2.777 ? . 4_454 H(28) C(14) 3.397 ? . 4_554 H(28) C(15) 3.310 ? . 4_554 H(28) H(1) 2.816 ? . 4_454 H(28) H(2) 2.405 ? . 4_454 H(28) H(3) 2.651 ? . 4_454 H(28) H(16) 3.445 ? . 4_554 H(29) C(1) 3.541 ? . 4_454 H(29) C(17) 3.564 ? . 3_556 H(29) H(1) 3.219 ? . 4_454 H(29) H(2) 3.108 ? . 4_454 H(29) H(18) 2.642 ? . 3_556 H(30) O(1) 2.406 ? . 4_554 H(30) O(4) 3.178 ? . 4_554 H(30) N(2) 3.532 ? . 4_554 H(30) C(9) 3.444 ? . 4_554 H(30) C(10) 3.103 ? . 4_554 H(30) C(13) 3.250 ? . 4_554 H(30) C(14) 3.130 ? . 4_554 H(30) C(19) 3.491 ? . 4_554 H(30) H(2) 3.088 ? . 4_454 H(30) H(11) 3.506 ? . 4_554 H(30) H(12) 3.565 ? . 4_554 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__080512 _database_code_depnum_ccdc_archive 'CCDC 812374' #TrackingRef 'NChem_All.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C29 H30 Cl Mn N3 O10 ' _chemical_formula_moiety 'C29 H30 Mn N3 O6, Cl O4 ' _chemical_formula_weight 670.96 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 13.8339(8) _cell_length_b 15.3790(13) _cell_length_c 14.4240(10) _cell_angle_alpha 90.0000 _cell_angle_beta 109.2237(19) _cell_angle_gamma 90.0000 _cell_volume 2897.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20823 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388.00 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 0.941 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 200.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 28037 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6604 _reflns_number_gt 5584 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0878 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6604 _refine_ls_number_parameters 398 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0419P)^2^+1.4247P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.35 _refine_diff_density_min -0.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Mn(1) Mn 0.833993(18) 0.273236(15) 0.499611(17) 0.01866(6) Uani 1.00 1 d . . . Cl(1) Cl 0.73162(4) 0.34270(3) 0.05986(4) 0.03577(12) Uani 1.00 1 d . . . O(1) O 0.79077(8) 0.38824(7) 0.47968(8) 0.0231(2) Uani 1.00 1 d . . . O(2) O 0.72391(9) 0.24761(8) 0.54056(9) 0.0228(2) Uani 1.00 1 d . . . O(3) O 0.91765(9) 0.29243(7) 0.62868(8) 0.0234(2) Uani 1.00 1 d . . . O(4) O 0.72596(10) 0.53722(8) 0.52734(10) 0.0329(2) Uani 1.00 1 d . . . O(5) O 0.60454(10) 0.27238(9) 0.65654(11) 0.0347(3) Uani 1.00 1 d . . . O(6) O 0.95426(11) 0.35077(9) 0.80669(9) 0.0376(3) Uani 1.00 1 d . . . O(7) O 0.83855(13) 0.33220(14) 0.10913(16) 0.0705(5) Uani 1.00 1 d . . . O(8) O 0.67894(14) 0.26957(11) 0.08042(13) 0.0589(4) Uani 1.00 1 d . . . O(9) O 0.70644(18) 0.34780(15) -0.04411(13) 0.0772(6) Uani 1.00 1 d . . . O(10) O 0.69685(15) 0.41962(12) 0.09436(15) 0.0732(6) Uani 1.00 1 d . . . N(1) N 0.75310(11) 0.24870(9) 0.35983(10) 0.0228(2) Uani 1.00 1 d . . . N(2) N 0.87056(10) 0.14735(9) 0.50605(10) 0.0215(2) Uani 1.00 1 d . . . N(3) N 0.95183(10) 0.30119(9) 0.45555(10) 0.0223(2) Uani 1.00 1 d . . . C(1) C 0.94235(17) 0.11879(14) 0.27788(16) 0.0395(4) Uani 1.00 1 d . . . C(2) C 0.90586(14) 0.17070(11) 0.35030(13) 0.0277(3) Uani 1.00 1 d . . . C(3) C 0.78960(14) 0.18096(12) 0.30698(13) 0.0297(3) Uani 1.00 1 d . . . C(4) C 0.66766(13) 0.28709(11) 0.31662(12) 0.0253(3) Uani 1.00 1 d . . . C(5) C 0.62779(13) 0.35849(11) 0.35666(12) 0.0243(3) Uani 1.00 1 d . . . C(6) C 0.52447(13) 0.38224(12) 0.31220(14) 0.0306(4) Uani 1.00 1 d . . . C(7) C 0.48843(13) 0.45489(13) 0.34390(14) 0.0326(4) Uani 1.00 1 d . . . C(8) C 0.55377(13) 0.50875(12) 0.41544(13) 0.0290(3) Uani 1.00 1 d . . . C(9) C 0.65582(13) 0.48783(11) 0.45896(12) 0.0245(3) Uani 1.00 1 d . . . C(10) C 0.69355(12) 0.40895(11) 0.43367(12) 0.0215(3) Uani 1.00 1 d . . . C(11) C 0.69727(16) 0.62470(12) 0.53882(16) 0.0370(4) Uani 1.00 1 d . . . C(12) C 0.93454(14) 0.12018(11) 0.44773(13) 0.0276(3) Uani 1.00 1 d . . . C(13) C 0.83377(12) 0.08851(11) 0.54821(12) 0.0241(3) Uani 1.00 1 d . . . C(14) C 0.76489(12) 0.10297(11) 0.60211(12) 0.0229(3) Uani 1.00 1 d . . . C(15) C 0.74144(14) 0.03333(12) 0.65359(14) 0.0306(3) Uani 1.00 1 d . . . C(16) C 0.67532(15) 0.04445(13) 0.70548(15) 0.0367(4) Uani 1.00 1 d . . . C(17) C 0.63047(15) 0.12536(13) 0.70587(14) 0.0344(4) Uani 1.00 1 d . . . C(18) C 0.65123(13) 0.19475(12) 0.65546(13) 0.0261(3) Uani 1.00 1 d . . . C(19) C 0.71658(12) 0.18399(11) 0.59888(12) 0.0208(3) Uani 1.00 1 d . . . C(20) C 0.67398(16) 0.34326(13) 0.69180(17) 0.0410(4) Uani 1.00 1 d . . . C(21) C 0.95853(14) 0.25926(12) 0.36614(13) 0.0283(3) Uani 1.00 1 d . . . C(22) C 1.01970(12) 0.35734(11) 0.50077(13) 0.0256(3) Uani 1.00 1 d . . . C(23) C 1.02944(13) 0.39661(11) 0.59358(13) 0.0262(3) Uani 1.00 1 d . . . C(24) C 1.09723(14) 0.46720(12) 0.62666(15) 0.0343(4) Uani 1.00 1 d . . . C(25) C 1.11390(15) 0.50038(13) 0.71898(16) 0.0409(5) Uani 1.00 1 d . . . C(26) C 1.06798(15) 0.46310(13) 0.78177(15) 0.0383(4) Uani 1.00 1 d . . . C(27) C 1.00252(14) 0.39296(12) 0.75179(13) 0.0298(3) Uani 1.00 1 d . . . C(28) C 0.98018(12) 0.35987(11) 0.65504(12) 0.0240(3) Uani 1.00 1 d . . . C(29) C 0.9866(2) 0.36831(18) 0.91020(15) 0.0546(6) Uani 1.00 1 d . . . H(1) H 0.9355 0.1544 0.2197 0.047 Uiso 1.00 1 c R . . H(2) H 0.9007 0.0662 0.2583 0.047 Uiso 1.00 1 c R . . H(3) H 1.0143 0.1025 0.3091 0.047 Uiso 1.00 1 c R . . H(4) H 0.7705 0.1968 0.2367 0.036 Uiso 1.00 1 c R . . H(5) H 0.7562 0.1249 0.3116 0.036 Uiso 1.00 1 c R . . H(6) H 0.6279 0.2666 0.2534 0.030 Uiso 1.00 1 c R . . H(7) H 0.4804 0.3480 0.2607 0.037 Uiso 1.00 1 c R . . H(8) H 0.4179 0.4691 0.3170 0.039 Uiso 1.00 1 c R . . H(9) H 0.5276 0.5605 0.4344 0.035 Uiso 1.00 1 c R . . H(10) H 0.6740 0.6535 0.4746 0.044 Uiso 1.00 1 c R . . H(11) H 0.7564 0.6560 0.5828 0.044 Uiso 1.00 1 c R . . H(12) H 0.6417 0.6247 0.5669 0.044 Uiso 1.00 1 c R . . H(13) H 0.9254 0.0571 0.4339 0.033 Uiso 1.00 1 c R . . H(14) H 1.0075 0.1306 0.4858 0.033 Uiso 1.00 1 c R . . H(15) H 0.8541 0.0302 0.5432 0.029 Uiso 1.00 1 c R . . H(16) H 0.7716 -0.0220 0.6525 0.037 Uiso 1.00 1 c R . . H(17) H 0.6602 -0.0027 0.7409 0.044 Uiso 1.00 1 c R . . H(18) H 0.5845 0.1328 0.7418 0.041 Uiso 1.00 1 c R . . H(19) H 0.7427 0.3205 0.7262 0.049 Uiso 1.00 1 c R . . H(20) H 0.6511 0.3786 0.7371 0.049 Uiso 1.00 1 c R . . H(21) H 0.6758 0.3792 0.6363 0.049 Uiso 1.00 1 c R . . H(22) H 1.0314 0.2519 0.3719 0.034 Uiso 1.00 1 c R . . H(23) H 0.9258 0.2969 0.3087 0.034 Uiso 1.00 1 c R . . H(24) H 1.0678 0.3744 0.4700 0.031 Uiso 1.00 1 c R . . H(25) H 1.1312 0.4916 0.5853 0.041 Uiso 1.00 1 c R . . H(26) H 1.1574 0.5494 0.7402 0.049 Uiso 1.00 1 c R . . H(27) H 1.0817 0.4860 0.8460 0.046 Uiso 1.00 1 c R . . H(28) H 0.9445 0.3347 0.9402 0.066 Uiso 1.00 1 c R . . H(29) H 0.9789 0.4305 0.9208 0.066 Uiso 1.00 1 c R . . H(30) H 1.0586 0.3517 0.9402 0.066 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.02117(13) 0.01576(12) 0.01911(13) -0.00022(9) 0.00672(9) -0.00092(9) Cl(1) 0.0381(2) 0.0275(2) 0.0344(2) -0.00383(18) 0.00214(19) 0.00146(18) O(1) 0.0235(5) 0.0181(5) 0.0254(6) 0.0010(4) 0.0049(4) 0.0004(4) O(2) 0.0239(5) 0.0208(5) 0.0254(5) 0.0015(4) 0.0103(4) 0.0019(4) O(3) 0.0270(6) 0.0198(5) 0.0210(5) -0.0011(4) 0.0047(4) -0.0004(4) O(4) 0.0382(7) 0.0238(6) 0.0330(7) 0.0054(5) 0.0069(5) -0.0051(5) O(5) 0.0306(6) 0.0328(7) 0.0455(8) 0.0016(5) 0.0190(5) -0.0068(6) O(6) 0.0438(8) 0.0432(8) 0.0224(6) 0.0035(6) 0.0061(5) -0.0052(5) O(7) 0.0372(9) 0.0731(13) 0.0866(14) 0.0011(8) 0.0005(9) -0.0185(10) O(8) 0.0695(11) 0.0489(10) 0.0532(10) -0.0206(8) 0.0133(8) 0.0102(7) O(9) 0.1054(16) 0.0833(15) 0.0384(9) -0.0239(12) 0.0175(9) 0.0106(9) O(10) 0.0697(11) 0.0440(10) 0.0804(13) 0.0184(8) -0.0098(10) -0.0186(9) N(1) 0.0268(7) 0.0210(6) 0.0205(6) -0.0029(5) 0.0075(5) -0.0024(5) N(2) 0.0244(6) 0.0171(6) 0.0243(7) 0.0002(5) 0.0096(5) -0.0022(5) N(3) 0.0236(6) 0.0205(6) 0.0239(7) 0.0013(5) 0.0093(5) 0.0023(5) C(1) 0.0488(11) 0.0393(11) 0.0382(11) 0.0008(8) 0.0249(9) -0.0097(8) C(2) 0.0344(9) 0.0256(8) 0.0280(8) -0.0004(7) 0.0170(7) -0.0050(7) C(3) 0.0353(9) 0.0286(9) 0.0262(8) -0.0019(7) 0.0117(7) -0.0089(7) C(4) 0.0279(8) 0.0249(8) 0.0206(8) -0.0059(6) 0.0046(6) -0.0006(6) C(5) 0.0257(8) 0.0219(8) 0.0246(8) -0.0006(6) 0.0072(6) 0.0035(6) C(6) 0.0252(8) 0.0296(9) 0.0326(9) -0.0021(7) 0.0035(7) 0.0052(7) C(7) 0.0231(8) 0.0345(10) 0.0396(10) 0.0041(7) 0.0094(7) 0.0118(8) C(8) 0.0318(9) 0.0276(9) 0.0321(9) 0.0073(7) 0.0168(7) 0.0081(7) C(9) 0.0309(8) 0.0217(8) 0.0225(8) 0.0010(6) 0.0110(6) 0.0038(6) C(10) 0.0232(8) 0.0205(7) 0.0210(7) 0.0008(6) 0.0076(6) 0.0057(6) C(11) 0.0459(11) 0.0235(9) 0.0441(11) 0.0013(8) 0.0182(9) -0.0038(8) C(12) 0.0318(9) 0.0216(8) 0.0348(9) 0.0031(6) 0.0183(7) -0.0019(7) C(13) 0.0269(8) 0.0175(7) 0.0267(8) 0.0006(6) 0.0070(6) -0.0005(6) C(14) 0.0259(8) 0.0201(8) 0.0225(8) -0.0034(6) 0.0077(6) -0.0019(6) C(15) 0.0369(9) 0.0227(8) 0.0328(9) -0.0035(7) 0.0125(7) 0.0009(7) C(16) 0.0444(11) 0.0327(10) 0.0380(10) -0.0101(8) 0.0205(8) 0.0039(8) C(17) 0.0361(10) 0.0397(10) 0.0338(10) -0.0085(8) 0.0203(8) -0.0039(8) C(18) 0.0244(8) 0.0286(8) 0.0259(8) -0.0039(6) 0.0091(6) -0.0043(7) C(19) 0.0208(7) 0.0214(7) 0.0187(7) -0.0048(6) 0.0045(6) -0.0027(6) C(20) 0.0456(11) 0.0293(10) 0.0520(12) 0.0013(8) 0.0216(9) -0.0120(9) C(21) 0.0325(9) 0.0290(9) 0.0280(8) -0.0013(7) 0.0163(7) -0.0008(7) C(22) 0.0223(8) 0.0215(8) 0.0329(9) 0.0004(6) 0.0090(6) 0.0065(6) C(23) 0.0239(8) 0.0186(8) 0.0309(9) 0.0009(6) 0.0019(6) 0.0013(6) C(24) 0.0266(9) 0.0215(8) 0.0477(11) -0.0013(6) 0.0025(8) 0.0011(8) C(25) 0.0318(10) 0.0236(9) 0.0548(13) -0.0016(7) -0.0026(9) -0.0089(8) C(26) 0.0335(10) 0.0317(10) 0.0383(10) 0.0063(8) -0.0037(8) -0.0142(8) C(27) 0.0270(8) 0.0274(9) 0.0285(9) 0.0087(7) 0.0004(7) -0.0043(7) C(28) 0.0211(8) 0.0186(7) 0.0270(8) 0.0050(6) 0.0007(6) -0.0016(6) C(29) 0.0652(15) 0.0674(16) 0.0222(10) 0.0113(12) 0.0020(9) -0.0049(10) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mn(1) O(1) 1.8588(10) yes . . Mn(1) O(2) 1.8482(14) yes . . Mn(1) O(3) 1.8638(10) yes . . Mn(1) N(1) 1.9935(12) yes . . Mn(1) N(2) 1.9954(14) yes . . Mn(1) N(3) 1.9820(15) yes . . Cl(1) O(7) 1.4237(17) yes . . Cl(1) O(8) 1.4235(19) yes . . Cl(1) O(9) 1.4257(19) yes . . Cl(1) O(10) 1.427(2) yes . . O(1) C(10) 1.3278(17) yes . . O(2) C(19) 1.316(2) yes . . O(3) C(28) 1.3236(19) yes . . O(4) C(9) 1.3642(19) yes . . O(4) C(11) 1.428(2) yes . . O(5) C(18) 1.360(2) yes . . O(5) C(20) 1.431(2) yes . . O(6) C(27) 1.357(2) yes . . O(6) C(29) 1.436(2) yes . . N(1) C(3) 1.475(2) yes . . N(1) C(4) 1.284(2) yes . . N(2) C(12) 1.468(2) yes . . N(2) C(13) 1.285(2) yes . . N(3) C(21) 1.472(2) yes . . N(3) C(22) 1.284(2) yes . . C(1) C(2) 1.527(3) yes . . C(2) C(3) 1.530(2) yes . . C(2) C(12) 1.539(2) yes . . C(2) C(21) 1.526(2) yes . . C(4) C(5) 1.433(2) yes . . C(5) C(6) 1.409(2) yes . . C(5) C(10) 1.414(2) yes . . C(6) C(7) 1.362(2) yes . . C(7) C(8) 1.398(2) yes . . C(8) C(9) 1.381(2) yes . . C(9) C(10) 1.415(2) yes . . C(13) C(14) 1.432(2) yes . . C(14) C(15) 1.401(2) yes . . C(14) C(19) 1.407(2) yes . . C(15) C(16) 1.370(3) yes . . C(16) C(17) 1.391(2) yes . . C(17) C(18) 1.374(2) yes . . C(18) C(19) 1.413(2) yes . . C(22) C(23) 1.434(2) yes . . C(23) C(24) 1.411(2) yes . . C(23) C(28) 1.403(2) yes . . C(24) C(25) 1.373(3) yes . . C(25) C(26) 1.390(3) yes . . C(26) C(27) 1.383(2) yes . . C(27) C(28) 1.421(2) yes . . C(1) H(1) 0.980 no . . C(1) H(2) 0.980 no . . C(1) H(3) 0.980 no . . C(3) H(4) 0.990 no . . C(3) H(5) 0.990 no . . C(4) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(11) H(10) 0.980 no . . C(11) H(11) 0.980 no . . C(11) H(12) 0.980 no . . C(12) H(13) 0.990 no . . C(12) H(14) 0.990 no . . C(13) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(17) H(18) 0.950 no . . C(20) H(19) 0.980 no . . C(20) H(20) 0.980 no . . C(20) H(21) 0.980 no . . C(21) H(22) 0.990 no . . C(21) H(23) 0.990 no . . C(22) H(24) 0.950 no . . C(24) H(25) 0.950 no . . C(25) H(26) 0.950 no . . C(26) H(27) 0.950 no . . C(29) H(28) 0.980 no . . C(29) H(29) 0.980 no . . C(29) H(30) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Mn(1) O(2) 89.73(5) yes . . . O(1) Mn(1) O(3) 93.79(4) yes . . . O(1) Mn(1) N(1) 88.79(5) yes . . . O(1) Mn(1) N(2) 173.76(4) yes . . . O(1) Mn(1) N(3) 90.04(5) yes . . . O(2) Mn(1) O(3) 91.18(5) yes . . . O(2) Mn(1) N(1) 92.04(6) yes . . . O(2) Mn(1) N(2) 90.07(5) yes . . . O(2) Mn(1) N(3) 179.77(5) yes . . . O(3) Mn(1) N(1) 175.89(6) yes . . . O(3) Mn(1) N(2) 92.44(4) yes . . . O(3) Mn(1) N(3) 88.86(5) yes . . . N(1) Mn(1) N(2) 84.99(5) yes . . . N(1) Mn(1) N(3) 87.93(6) yes . . . N(2) Mn(1) N(3) 90.15(6) yes . . . O(7) Cl(1) O(8) 108.99(11) yes . . . O(7) Cl(1) O(9) 112.65(14) yes . . . O(7) Cl(1) O(10) 109.52(11) yes . . . O(8) Cl(1) O(9) 107.34(12) yes . . . O(8) Cl(1) O(10) 109.14(12) yes . . . O(9) Cl(1) O(10) 109.12(12) yes . . . Mn(1) O(1) C(10) 121.79(9) yes . . . Mn(1) O(2) C(19) 127.44(10) yes . . . Mn(1) O(3) C(28) 122.90(10) yes . . . C(9) O(4) C(11) 116.73(13) yes . . . C(18) O(5) C(20) 114.02(14) yes . . . C(27) O(6) C(29) 118.16(16) yes . . . Mn(1) N(1) C(3) 118.87(9) yes . . . Mn(1) N(1) C(4) 121.62(12) yes . . . C(3) N(1) C(4) 119.41(13) yes . . . Mn(1) N(2) C(12) 116.16(11) yes . . . Mn(1) N(2) C(13) 124.85(13) yes . . . C(12) N(2) C(13) 118.56(14) yes . . . Mn(1) N(3) C(21) 118.79(10) yes . . . Mn(1) N(3) C(22) 121.60(13) yes . . . C(21) N(3) C(22) 119.55(16) yes . . . C(1) C(2) C(3) 108.33(14) yes . . . C(1) C(2) C(12) 108.47(14) yes . . . C(1) C(2) C(21) 108.66(17) yes . . . C(3) C(2) C(12) 110.20(16) yes . . . C(3) C(2) C(21) 110.80(14) yes . . . C(12) C(2) C(21) 110.31(13) yes . . . N(1) C(3) C(2) 110.77(13) yes . . . N(1) C(4) C(5) 124.86(14) yes . . . C(4) C(5) C(6) 118.87(14) yes . . . C(4) C(5) C(10) 120.26(14) yes . . . C(6) C(5) C(10) 120.63(16) yes . . . C(5) C(6) C(7) 119.24(15) yes . . . C(6) C(7) C(8) 120.97(15) yes . . . C(7) C(8) C(9) 120.89(17) yes . . . O(4) C(9) C(8) 125.19(16) yes . . . O(4) C(9) C(10) 115.39(14) yes . . . C(8) C(9) C(10) 119.42(14) yes . . . O(1) C(10) C(5) 123.02(15) yes . . . O(1) C(10) C(9) 118.40(13) yes . . . C(5) C(10) C(9) 118.46(13) yes . . . N(2) C(12) C(2) 110.90(14) yes . . . N(2) C(13) C(14) 125.85(16) yes . . . C(13) C(14) C(15) 118.74(16) yes . . . C(13) C(14) C(19) 120.88(16) yes . . . C(15) C(14) C(19) 120.27(17) yes . . . C(14) C(15) C(16) 120.46(17) yes . . . C(15) C(16) C(17) 119.52(19) yes . . . C(16) C(17) C(18) 121.4(2) yes . . . O(5) C(18) C(17) 119.54(19) yes . . . O(5) C(18) C(19) 120.40(17) yes . . . C(17) C(18) C(19) 119.98(17) yes . . . O(2) C(19) C(14) 122.94(17) yes . . . O(2) C(19) C(18) 118.74(15) yes . . . C(14) C(19) C(18) 118.14(16) yes . . . N(3) C(21) C(2) 110.95(16) yes . . . N(3) C(22) C(23) 125.84(18) yes . . . C(22) C(23) C(24) 119.17(18) yes . . . C(22) C(23) C(28) 120.30(15) yes . . . C(24) C(23) C(28) 120.22(17) yes . . . C(23) C(24) C(25) 119.6(2) yes . . . C(24) C(25) C(26) 120.79(18) yes . . . C(25) C(26) C(27) 120.71(19) yes . . . O(6) C(27) C(26) 125.99(17) yes . . . O(6) C(27) C(28) 114.34(15) yes . . . C(26) C(27) C(28) 119.66(19) yes . . . O(3) C(28) C(23) 122.80(15) yes . . . O(3) C(28) C(27) 118.24(16) yes . . . C(23) C(28) C(27) 118.87(15) yes . . . C(2) C(1) H(1) 109.5 no . . . C(2) C(1) H(2) 109.5 no . . . C(2) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . N(1) C(3) H(4) 109.5 no . . . N(1) C(3) H(5) 109.5 no . . . C(2) C(3) H(4) 109.5 no . . . C(2) C(3) H(5) 109.5 no . . . H(4) C(3) H(5) 108.1 no . . . N(1) C(4) H(6) 117.6 no . . . C(5) C(4) H(6) 117.6 no . . . C(5) C(6) H(7) 120.4 no . . . C(7) C(6) H(7) 120.4 no . . . C(6) C(7) H(8) 119.5 no . . . C(8) C(7) H(8) 119.5 no . . . C(7) C(8) H(9) 119.6 no . . . C(9) C(8) H(9) 119.6 no . . . O(4) C(11) H(10) 109.5 no . . . O(4) C(11) H(11) 109.5 no . . . O(4) C(11) H(12) 109.5 no . . . H(10) C(11) H(11) 109.5 no . . . H(10) C(11) H(12) 109.5 no . . . H(11) C(11) H(12) 109.5 no . . . N(2) C(12) H(13) 109.5 no . . . N(2) C(12) H(14) 109.5 no . . . C(2) C(12) H(13) 109.5 no . . . C(2) C(12) H(14) 109.5 no . . . H(13) C(12) H(14) 108.1 no . . . N(2) C(13) H(15) 117.1 no . . . C(14) C(13) H(15) 117.1 no . . . C(14) C(15) H(16) 119.8 no . . . C(16) C(15) H(16) 119.8 no . . . C(15) C(16) H(17) 120.2 no . . . C(17) C(16) H(17) 120.2 no . . . C(16) C(17) H(18) 119.3 no . . . C(18) C(17) H(18) 119.3 no . . . O(5) C(20) H(19) 109.5 no . . . O(5) C(20) H(20) 109.5 no . . . O(5) C(20) H(21) 109.5 no . . . H(19) C(20) H(20) 109.5 no . . . H(19) C(20) H(21) 109.5 no . . . H(20) C(20) H(21) 109.5 no . . . N(3) C(21) H(22) 109.5 no . . . N(3) C(21) H(23) 109.4 no . . . C(2) C(21) H(22) 109.5 no . . . C(2) C(21) H(23) 109.4 no . . . H(22) C(21) H(23) 108.0 no . . . N(3) C(22) H(24) 117.1 no . . . C(23) C(22) H(24) 117.1 no . . . C(23) C(24) H(25) 120.2 no . . . C(25) C(24) H(25) 120.2 no . . . C(24) C(25) H(26) 119.6 no . . . C(26) C(25) H(26) 119.6 no . . . C(25) C(26) H(27) 119.6 no . . . C(27) C(26) H(27) 119.6 no . . . O(6) C(29) H(28) 109.5 no . . . O(6) C(29) H(29) 109.5 no . . . O(6) C(29) H(30) 109.5 no . . . H(28) C(29) H(29) 109.5 no . . . H(28) C(29) H(30) 109.5 no . . . H(29) C(29) H(30) 109.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(24) 3.356(2) ? . 3_766 O(6) C(4) 3.599(2) ? . 4_555 O(6) C(16) 3.451(2) ? . 2_656 O(7) C(25) 3.484(3) ? . 3_766 O(7) C(26) 3.566(2) ? . 3_766 O(8) N(3) 3.252(2) ? . 4_454 O(8) C(3) 3.404(2) ? . . O(8) C(4) 3.472(2) ? . . O(8) C(11) 3.577(3) ? . 2_645 O(8) C(21) 3.583(2) ? . 4_454 O(8) C(22) 2.884(2) ? . 4_454 O(8) C(23) 3.332(2) ? . 4_454 O(9) C(15) 3.450(3) ? . 2_655 O(10) C(12) 3.530(2) ? . 2_655 O(10) C(13) 3.253(2) ? . 2_655 O(10) C(25) 3.313(2) ? . 3_766 N(3) O(8) 3.252(2) ? . 4_555 C(1) C(7) 3.386(3) ? . 2_645 C(1) C(8) 3.277(3) ? . 2_645 C(3) O(8) 3.404(2) ? . . C(4) O(6) 3.599(2) ? . 4_454 C(4) O(8) 3.472(2) ? . . C(4) C(27) 3.515(2) ? . 4_454 C(7) C(1) 3.386(3) ? . 2_655 C(8) C(1) 3.277(3) ? . 2_655 C(8) C(8) 3.260(2) ? . 3_666 C(11) O(8) 3.577(3) ? . 2_655 C(12) O(10) 3.530(2) ? . 2_645 C(13) O(10) 3.253(2) ? . 2_645 C(15) O(9) 3.450(3) ? . 2_645 C(16) O(6) 3.451(2) ? . 2_646 C(16) C(27) 3.586(2) ? . 2_646 C(16) C(29) 3.561(3) ? . 2_646 C(19) C(29) 3.532(2) ? . 4_454 C(21) O(8) 3.583(2) ? . 4_555 C(22) O(8) 2.884(2) ? . 4_555 C(22) C(24) 3.364(2) ? . 3_766 C(23) O(8) 3.332(2) ? . 4_555 C(24) O(1) 3.356(2) ? . 3_766 C(24) C(22) 3.364(2) ? . 3_766 C(25) O(7) 3.484(3) ? . 3_766 C(25) O(10) 3.313(2) ? . 3_766 C(26) O(7) 3.566(2) ? . 3_766 C(27) C(4) 3.515(2) ? . 4_555 C(27) C(16) 3.586(2) ? . 2_656 C(29) C(16) 3.561(3) ? . 2_656 C(29) C(19) 3.532(2) ? . 4_555 Cl(1) H(4) 3.306 ? . . Cl(1) H(10) 3.293 ? . 2_645 Cl(1) H(11) 3.568 ? . 2_645 Cl(1) H(14) 2.957 ? . 4_454 Cl(1) H(15) 3.281 ? . 2_655 Cl(1) H(22) 3.492 ? . 4_454 Cl(1) H(26) 3.242 ? . 3_766 O(1) H(25) 2.474 ? . 3_766 O(2) H(30) 2.734 ? . 4_454 O(3) H(6) 3.013 ? . 4_555 O(3) H(7) 2.820 ? . 4_555 O(4) H(8) 3.457 ? . 3_666 O(4) H(17) 3.250 ? . 2_656 O(4) H(24) 3.150 ? . 3_766 O(4) H(25) 2.976 ? . 3_766 O(5) H(1) 2.995 ? . 4_455 O(5) H(3) 3.452 ? . 4_455 O(5) H(9) 3.177 ? . 3_666 O(5) H(22) 3.589 ? . 4_455 O(5) H(28) 3.578 ? . 4_454 O(5) H(30) 3.532 ? . 4_454 O(6) H(6) 3.292 ? . 4_555 O(6) H(7) 3.174 ? . 4_555 O(6) H(17) 2.709 ? . 2_656 O(7) H(1) 3.227 ? . . O(7) H(4) 3.122 ? . . O(7) H(10) 2.984 ? . 2_645 O(7) H(18) 3.353 ? . 4_554 O(7) H(23) 2.784 ? . . O(7) H(26) 2.821 ? . 3_766 O(7) H(27) 2.997 ? . 3_766 O(7) H(28) 3.230 ? . 1_554 O(8) H(4) 2.461 ? . . O(8) H(6) 2.808 ? . . O(8) H(10) 3.003 ? . 2_645 O(8) H(11) 3.283 ? . 2_645 O(8) H(14) 2.778 ? . 4_454 O(8) H(22) 3.047 ? . 4_454 O(8) H(24) 2.862 ? . 4_454 O(9) H(3) 2.903 ? . 4_454 O(9) H(10) 3.402 ? . 2_645 O(9) H(11) 3.077 ? . 2_645 O(9) H(14) 2.942 ? . 4_454 O(9) H(15) 2.929 ? . 2_655 O(9) H(16) 2.619 ? . 2_655 O(9) H(19) 3.536 ? . 1_554 O(9) H(20) 3.029 ? . 1_554 O(9) H(22) 2.784 ? . 4_454 O(9) H(28) 3.380 ? . 1_554 O(10) H(5) 3.413 ? . 2_655 O(10) H(13) 2.654 ? . 2_655 O(10) H(14) 2.686 ? . 4_454 O(10) H(15) 2.530 ? . 2_655 O(10) H(26) 2.612 ? . 3_766 O(10) H(27) 3.239 ? . 3_766 N(2) H(7) 3.483 ? . 4_555 N(3) H(25) 3.372 ? . 3_766 N(3) H(26) 3.567 ? . 3_766 C(1) H(8) 3.557 ? . 2_645 C(1) H(9) 3.345 ? . 2_645 C(1) H(10) 3.505 ? . 2_645 C(1) H(20) 3.131 ? . 4_554 C(4) H(30) 3.432 ? . 4_454 C(5) H(2) 3.560 ? . 2_655 C(6) H(2) 3.286 ? . 2_655 C(6) H(12) 3.313 ? . 3_666 C(7) H(1) 3.464 ? . 2_655 C(7) H(2) 2.991 ? . 2_655 C(7) H(3) 3.158 ? . 2_655 C(7) H(9) 3.287 ? . 3_666 C(7) H(12) 2.814 ? . 3_666 C(7) H(16) 3.497 ? . 4_454 C(7) H(20) 3.187 ? . 3_666 C(7) H(21) 3.490 ? . 3_666 C(8) H(1) 3.005 ? . 2_655 C(8) H(2) 2.915 ? . 2_655 C(8) H(3) 3.384 ? . 2_655 C(8) H(9) 2.950 ? . 3_666 C(8) H(12) 3.470 ? . 3_666 C(8) H(20) 3.430 ? . 3_666 C(8) H(21) 3.471 ? . 3_666 C(9) H(1) 3.558 ? . 2_655 C(9) H(2) 3.205 ? . 2_655 C(9) H(9) 3.454 ? . 3_666 C(9) H(25) 3.229 ? . 3_766 C(10) H(2) 3.582 ? . 2_655 C(10) H(25) 2.954 ? . 3_766 C(11) H(8) 3.335 ? . 3_666 C(11) H(18) 3.585 ? . 2_656 C(11) H(24) 3.295 ? . 3_766 C(12) H(13) 3.453 ? . 3_756 C(13) H(7) 3.220 ? . 4_555 C(14) H(7) 3.194 ? . 4_555 C(14) H(8) 3.316 ? . 4_555 C(14) H(30) 3.114 ? . 4_454 C(15) H(8) 2.779 ? . 4_555 C(15) H(20) 2.968 ? . 2_646 C(15) H(29) 3.285 ? . 2_646 C(16) H(8) 3.215 ? . 4_555 C(16) H(11) 3.356 ? . 2_646 C(16) H(20) 3.413 ? . 2_646 C(16) H(21) 3.580 ? . 2_646 C(16) H(27) 3.502 ? . 2_646 C(16) H(29) 2.895 ? . 2_646 C(17) H(11) 2.971 ? . 2_646 C(17) H(27) 3.510 ? . 2_646 C(17) H(29) 3.576 ? . 2_646 C(18) H(28) 3.490 ? . 4_454 C(18) H(30) 3.029 ? . 4_454 C(19) H(30) 2.650 ? . 4_454 C(20) H(1) 3.452 ? . 4_455 C(20) H(3) 3.302 ? . 4_455 C(20) H(8) 3.138 ? . 3_666 C(20) H(9) 3.153 ? . 3_666 C(20) H(16) 2.965 ? . 2_656 C(20) H(17) 3.217 ? . 2_656 C(21) H(18) 3.327 ? . 4_554 C(21) H(26) 3.459 ? . 3_766 C(22) H(25) 3.096 ? . 3_766 C(23) H(4) 3.594 ? . 4_555 C(23) H(6) 3.377 ? . 4_555 C(23) H(25) 3.282 ? . 3_766 C(24) H(4) 3.482 ? . 4_555 C(24) H(5) 3.177 ? . 4_555 C(24) H(24) 3.316 ? . 3_766 C(25) H(5) 2.765 ? . 4_555 C(25) H(23) 3.167 ? . 3_766 C(25) H(24) 3.598 ? . 3_766 C(26) H(5) 2.839 ? . 4_555 C(26) H(17) 3.109 ? . 2_656 C(26) H(18) 3.302 ? . 2_656 C(27) H(5) 3.338 ? . 4_555 C(27) H(6) 3.001 ? . 4_555 C(27) H(17) 2.794 ? . 2_656 C(28) H(6) 2.840 ? . 4_555 C(28) H(7) 3.541 ? . 4_555 C(28) H(17) 3.522 ? . 2_656 C(29) H(17) 3.146 ? . 2_656 H(1) O(5) 2.995 ? . 4_554 H(1) O(7) 3.227 ? . . H(1) C(7) 3.464 ? . 2_645 H(1) C(8) 3.005 ? . 2_645 H(1) C(9) 3.558 ? . 2_645 H(1) C(20) 3.452 ? . 4_554 H(1) H(9) 2.834 ? . 2_645 H(1) H(10) 2.713 ? . 2_645 H(1) H(20) 2.953 ? . 4_554 H(2) C(5) 3.560 ? . 2_645 H(2) C(6) 3.286 ? . 2_645 H(2) C(7) 2.991 ? . 2_645 H(2) C(8) 2.915 ? . 2_645 H(2) C(9) 3.205 ? . 2_645 H(2) C(10) 3.582 ? . 2_645 H(2) H(8) 3.392 ? . 2_645 H(2) H(9) 3.245 ? . 2_645 H(2) H(10) 3.446 ? . 2_645 H(3) O(5) 3.452 ? . 4_554 H(3) O(9) 2.903 ? . 4_555 H(3) C(7) 3.158 ? . 2_645 H(3) C(8) 3.384 ? . 2_645 H(3) C(20) 3.302 ? . 4_554 H(3) H(8) 3.086 ? . 2_645 H(3) H(9) 3.428 ? . 2_645 H(3) H(15) 3.076 ? . 3_756 H(3) H(16) 3.088 ? . 3_756 H(3) H(20) 2.457 ? . 4_554 H(4) Cl(1) 3.306 ? . . H(4) O(7) 3.122 ? . . H(4) O(8) 2.461 ? . . H(4) C(23) 3.594 ? . 4_454 H(4) C(24) 3.482 ? . 4_454 H(4) H(10) 3.445 ? . 2_645 H(5) O(10) 3.413 ? . 2_645 H(5) C(24) 3.177 ? . 4_454 H(5) C(25) 2.765 ? . 4_454 H(5) C(26) 2.839 ? . 4_454 H(5) C(27) 3.338 ? . 4_454 H(5) H(26) 3.032 ? . 4_454 H(5) H(27) 3.127 ? . 4_454 H(6) O(3) 3.013 ? . 4_454 H(6) O(6) 3.292 ? . 4_454 H(6) O(8) 2.808 ? . . H(6) C(23) 3.377 ? . 4_454 H(6) C(27) 3.001 ? . 4_454 H(6) C(28) 2.840 ? . 4_454 H(7) O(3) 2.820 ? . 4_454 H(7) O(6) 3.174 ? . 4_454 H(7) N(2) 3.483 ? . 4_454 H(7) C(13) 3.220 ? . 4_454 H(7) C(14) 3.194 ? . 4_454 H(7) C(28) 3.541 ? . 4_454 H(7) H(12) 3.461 ? . 3_666 H(7) H(15) 3.578 ? . 4_454 H(8) O(4) 3.457 ? . 3_666 H(8) C(1) 3.557 ? . 2_655 H(8) C(11) 3.335 ? . 3_666 H(8) C(14) 3.316 ? . 4_454 H(8) C(15) 2.779 ? . 4_454 H(8) C(16) 3.215 ? . 4_454 H(8) C(20) 3.138 ? . 3_666 H(8) H(2) 3.392 ? . 2_655 H(8) H(3) 3.086 ? . 2_655 H(8) H(9) 3.443 ? . 3_666 H(8) H(12) 2.544 ? . 3_666 H(8) H(16) 2.687 ? . 4_454 H(8) H(17) 3.406 ? . 4_454 H(8) H(20) 2.551 ? . 3_666 H(8) H(21) 2.855 ? . 3_666 H(9) O(5) 3.177 ? . 3_666 H(9) C(1) 3.345 ? . 2_655 H(9) C(7) 3.287 ? . 3_666 H(9) C(8) 2.950 ? . 3_666 H(9) C(9) 3.454 ? . 3_666 H(9) C(20) 3.153 ? . 3_666 H(9) H(1) 2.834 ? . 2_655 H(9) H(2) 3.245 ? . 2_655 H(9) H(3) 3.428 ? . 2_655 H(9) H(8) 3.443 ? . 3_666 H(9) H(9) 2.929 ? . 3_666 H(9) H(20) 3.013 ? . 3_666 H(9) H(21) 2.816 ? . 3_666 H(10) Cl(1) 3.293 ? . 2_655 H(10) O(7) 2.984 ? . 2_655 H(10) O(8) 3.003 ? . 2_655 H(10) O(9) 3.402 ? . 2_655 H(10) C(1) 3.505 ? . 2_655 H(10) H(1) 2.713 ? . 2_655 H(10) H(2) 3.446 ? . 2_655 H(10) H(4) 3.445 ? . 2_655 H(10) H(24) 3.421 ? . 3_766 H(11) Cl(1) 3.568 ? . 2_655 H(11) O(8) 3.283 ? . 2_655 H(11) O(9) 3.077 ? . 2_655 H(11) C(16) 3.356 ? . 2_656 H(11) C(17) 2.971 ? . 2_656 H(11) H(17) 3.439 ? . 2_656 H(11) H(18) 2.777 ? . 2_656 H(11) H(22) 3.129 ? . 3_766 H(11) H(24) 2.817 ? . 3_766 H(12) C(6) 3.313 ? . 3_666 H(12) C(7) 2.814 ? . 3_666 H(12) C(8) 3.470 ? . 3_666 H(12) H(7) 3.461 ? . 3_666 H(12) H(8) 2.544 ? . 3_666 H(12) H(28) 3.433 ? . 2_656 H(13) O(10) 2.654 ? . 2_645 H(13) C(12) 3.453 ? . 3_756 H(13) H(13) 2.897 ? . 3_756 H(13) H(14) 3.136 ? . 3_756 H(13) H(15) 3.248 ? . 3_756 H(14) Cl(1) 2.957 ? . 4_555 H(14) O(8) 2.778 ? . 4_555 H(14) O(9) 2.942 ? . 4_555 H(14) O(10) 2.686 ? . 4_555 H(14) H(13) 3.136 ? . 3_756 H(14) H(15) 3.238 ? . 3_756 H(15) Cl(1) 3.281 ? . 2_645 H(15) O(9) 2.929 ? . 2_645 H(15) O(10) 2.530 ? . 2_645 H(15) H(3) 3.076 ? . 3_756 H(15) H(7) 3.578 ? . 4_555 H(15) H(13) 3.248 ? . 3_756 H(15) H(14) 3.238 ? . 3_756 H(16) O(9) 2.619 ? . 2_645 H(16) C(7) 3.497 ? . 4_555 H(16) C(20) 2.965 ? . 2_646 H(16) H(3) 3.088 ? . 3_756 H(16) H(8) 2.687 ? . 4_555 H(16) H(19) 3.032 ? . 2_646 H(16) H(20) 2.212 ? . 2_646 H(16) H(21) 3.265 ? . 2_646 H(16) H(28) 3.598 ? . 2_646 H(16) H(29) 3.353 ? . 2_646 H(17) O(4) 3.250 ? . 2_646 H(17) O(6) 2.709 ? . 2_646 H(17) C(20) 3.217 ? . 2_646 H(17) C(26) 3.109 ? . 2_646 H(17) C(27) 2.794 ? . 2_646 H(17) C(28) 3.522 ? . 2_646 H(17) C(29) 3.146 ? . 2_646 H(17) H(8) 3.406 ? . 4_555 H(17) H(11) 3.439 ? . 2_646 H(17) H(19) 3.000 ? . 2_646 H(17) H(20) 3.114 ? . 2_646 H(17) H(21) 2.990 ? . 2_646 H(17) H(27) 3.168 ? . 2_646 H(17) H(28) 3.561 ? . 2_646 H(17) H(29) 2.692 ? . 2_646 H(18) O(7) 3.353 ? . 4_455 H(18) C(11) 3.585 ? . 2_646 H(18) C(21) 3.327 ? . 4_455 H(18) C(26) 3.302 ? . 2_646 H(18) H(11) 2.777 ? . 2_646 H(18) H(22) 2.849 ? . 4_455 H(18) H(23) 2.884 ? . 4_455 H(18) H(24) 3.377 ? . 4_455 H(18) H(27) 3.173 ? . 2_646 H(19) O(9) 3.536 ? . 1_556 H(19) H(16) 3.032 ? . 2_656 H(19) H(17) 3.000 ? . 2_656 H(20) O(9) 3.029 ? . 1_556 H(20) C(1) 3.131 ? . 4_455 H(20) C(7) 3.187 ? . 3_666 H(20) C(8) 3.430 ? . 3_666 H(20) C(15) 2.968 ? . 2_656 H(20) C(16) 3.413 ? . 2_656 H(20) H(1) 2.953 ? . 4_455 H(20) H(3) 2.457 ? . 4_455 H(20) H(8) 2.551 ? . 3_666 H(20) H(9) 3.013 ? . 3_666 H(20) H(16) 2.212 ? . 2_656 H(20) H(17) 3.114 ? . 2_656 H(20) H(22) 3.559 ? . 4_455 H(21) C(7) 3.490 ? . 3_666 H(21) C(8) 3.471 ? . 3_666 H(21) C(16) 3.580 ? . 2_656 H(21) H(8) 2.855 ? . 3_666 H(21) H(9) 2.816 ? . 3_666 H(21) H(16) 3.265 ? . 2_656 H(21) H(17) 2.990 ? . 2_656 H(22) Cl(1) 3.492 ? . 4_555 H(22) O(5) 3.589 ? . 4_554 H(22) O(8) 3.047 ? . 4_555 H(22) O(9) 2.784 ? . 4_555 H(22) H(11) 3.129 ? . 3_766 H(22) H(18) 2.849 ? . 4_554 H(22) H(20) 3.559 ? . 4_554 H(23) O(7) 2.784 ? . . H(23) C(25) 3.167 ? . 3_766 H(23) H(18) 2.884 ? . 4_554 H(23) H(26) 2.621 ? . 3_766 H(24) O(4) 3.150 ? . 3_766 H(24) O(8) 2.862 ? . 4_555 H(24) C(11) 3.295 ? . 3_766 H(24) C(24) 3.316 ? . 3_766 H(24) C(25) 3.598 ? . 3_766 H(24) H(10) 3.421 ? . 3_766 H(24) H(11) 2.817 ? . 3_766 H(24) H(18) 3.377 ? . 4_554 H(24) H(25) 3.318 ? . 3_766 H(25) O(1) 2.474 ? . 3_766 H(25) O(4) 2.976 ? . 3_766 H(25) N(3) 3.372 ? . 3_766 H(25) C(9) 3.229 ? . 3_766 H(25) C(10) 2.954 ? . 3_766 H(25) C(22) 3.096 ? . 3_766 H(25) C(23) 3.282 ? . 3_766 H(25) H(24) 3.318 ? . 3_766 H(26) Cl(1) 3.242 ? . 3_766 H(26) O(7) 2.821 ? . 3_766 H(26) O(10) 2.612 ? . 3_766 H(26) N(3) 3.567 ? . 3_766 H(26) C(21) 3.459 ? . 3_766 H(26) H(5) 3.032 ? . 4_555 H(26) H(23) 2.621 ? . 3_766 H(27) O(7) 2.997 ? . 3_766 H(27) O(10) 3.239 ? . 3_766 H(27) C(16) 3.502 ? . 2_656 H(27) C(17) 3.510 ? . 2_656 H(27) H(5) 3.127 ? . 4_555 H(27) H(17) 3.168 ? . 2_656 H(27) H(18) 3.173 ? . 2_656 H(28) O(5) 3.578 ? . 4_555 H(28) O(7) 3.230 ? . 1_556 H(28) O(9) 3.380 ? . 1_556 H(28) C(18) 3.490 ? . 4_555 H(28) H(12) 3.433 ? . 2_646 H(28) H(16) 3.598 ? . 2_656 H(28) H(17) 3.561 ? . 2_656 H(29) C(15) 3.285 ? . 2_656 H(29) C(16) 2.895 ? . 2_656 H(29) C(17) 3.576 ? . 2_656 H(29) H(16) 3.353 ? . 2_656 H(29) H(17) 2.692 ? . 2_656 H(29) H(29) 3.041 ? . 3_767 H(30) O(2) 2.734 ? . 4_555 H(30) O(5) 3.532 ? . 4_555 H(30) C(4) 3.432 ? . 4_555 H(30) C(14) 3.114 ? . 4_555 H(30) C(18) 3.029 ? . 4_555 H(30) C(19) 2.650 ? . 4_555 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data__080821 _database_code_depnum_ccdc_archive 'CCDC 812375' #TrackingRef 'NChem_All.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C29 H30 F6 Mn N3 O6 P ' _chemical_formula_moiety 'C29 H30 Mn N3 O6, F6 P ' _chemical_formula_weight 716.47 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 13.7229(10) _cell_length_b 15.9755(11) _cell_length_c 14.5327(10) _cell_angle_alpha 90.0000 _cell_angle_beta 108.966(2) _cell_angle_gamma 90.0000 _cell_volume 3013.0(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 32730 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468.00 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.944 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 193.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 47216 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6871 _reflns_number_gt 5560 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1323 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6871 _refine_ls_number_parameters 416 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0697P)^2^+3.1599P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.72 _refine_diff_density_min -0.49 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Mn(1) Mn 0.17082(3) 0.77023(2) 0.50478(2) 0.01915(11) Uani 1.00 1 d . . . P(1) P 0.24785(6) 0.85294(4) 0.94974(5) 0.03553(17) Uani 1.00 1 d . . . F(1) F 0.3051(2) 0.91420(18) 0.8977(2) 0.0903(8) Uani 1.00 1 d . . . F(2) F 0.33175(16) 0.87953(14) 1.05081(14) 0.0624(5) Uani 1.00 1 d . . . F(3) F 0.31940(18) 0.77667(13) 0.94100(17) 0.0648(6) Uani 1.00 1 d . . . F(4) F 0.1680(2) 0.83054(18) 0.8482(2) 0.1032(11) Uani 1.00 1 d . . . F(5) F 0.17688(15) 0.92892(12) 0.95994(14) 0.0564(5) Uani 1.00 1 d . . . F(6) F 0.1933(2) 0.79594(15) 1.0060(2) 0.0948(9) Uani 1.00 1 d . . . O(1) O 0.28165(13) 0.75002(10) 0.46116(12) 0.0236(3) Uani 1.00 1 d . . . O(2) O 0.21206(12) 0.88145(10) 0.52678(12) 0.0234(3) Uani 1.00 1 d . . . O(3) O 0.08422(13) 0.79127(10) 0.37830(11) 0.0235(3) Uani 1.00 1 d . . . O(4) O 0.39826(15) 0.78136(12) 0.34214(15) 0.0374(4) Uani 1.00 1 d . . . O(5) O 0.27693(15) 1.02352(11) 0.47424(13) 0.0322(4) Uani 1.00 1 d . . . O(6) O 0.04528(15) 0.85513(13) 0.20379(13) 0.0378(4) Uani 1.00 1 d . . . N(1) N 0.13807(15) 0.64774(12) 0.49613(14) 0.0226(3) Uani 1.00 1 d . . . N(2) N 0.25346(16) 0.74526(13) 0.64318(14) 0.0244(4) Uani 1.00 1 d . . . N(3) N 0.05167(15) 0.79279(12) 0.55095(14) 0.0222(3) Uani 1.00 1 d . . . C(1) C 0.0672(2) 0.61187(19) 0.7239(2) 0.0394(6) Uani 1.00 1 d . . . C(2) C 0.1019(2) 0.66441(16) 0.65194(18) 0.0283(5) Uani 1.00 1 d . . . C(3) C 0.0750(2) 0.61766(15) 0.55451(19) 0.0294(5) Uani 1.00 1 d . . . C(4) C 0.17602(18) 0.59333(14) 0.45168(17) 0.0244(4) Uani 1.00 1 d . . . C(5) C 0.24420(18) 0.61060(15) 0.39704(17) 0.0241(4) Uani 1.00 1 d . . . C(6) C 0.2686(2) 0.54557(16) 0.34313(19) 0.0311(5) Uani 1.00 1 d . . . C(7) C 0.3346(2) 0.55968(18) 0.2909(2) 0.0370(6) Uani 1.00 1 d . . . C(8) C 0.3767(2) 0.63919(19) 0.2915(2) 0.0365(6) Uani 1.00 1 d . . . C(9) C 0.35435(19) 0.70429(16) 0.34348(19) 0.0291(5) Uani 1.00 1 d . . . C(10) C 0.29017(17) 0.69014(15) 0.40133(16) 0.0224(4) Uani 1.00 1 d . . . C(11) C 0.3253(2) 0.84778(19) 0.3084(2) 0.0450(7) Uani 1.00 1 d . . . C(12) C 0.2188(2) 0.67799(17) 0.69494(18) 0.0309(5) Uani 1.00 1 d . . . C(13) C 0.3376(2) 0.78418(16) 0.68693(18) 0.0286(5) Uani 1.00 1 d . . . C(14) C 0.37641(19) 0.85456(15) 0.64847(17) 0.0266(4) Uani 1.00 1 d . . . C(15) C 0.4796(2) 0.87962(17) 0.6933(2) 0.0336(5) Uani 1.00 1 d . . . C(16) C 0.5151(2) 0.95094(18) 0.6624(2) 0.0354(5) Uani 1.00 1 d . . . C(17) C 0.4491(2) 1.00075(16) 0.58967(19) 0.0305(5) Uani 1.00 1 d . . . C(18) C 0.34706(19) 0.97814(15) 0.54519(17) 0.0254(4) Uani 1.00 1 d . . . C(19) C 0.30978(18) 0.90237(14) 0.57141(16) 0.0228(4) Uani 1.00 1 d . . . C(20) C 0.3017(2) 1.10945(16) 0.4658(2) 0.0374(6) Uani 1.00 1 d . . . C(21) C 0.0452(2) 0.74892(16) 0.63838(17) 0.0265(4) Uani 1.00 1 d . . . C(22) C -0.01659(18) 0.84800(15) 0.51007(17) 0.0251(4) Uani 1.00 1 d . . . C(23) C -0.02676(18) 0.89006(14) 0.42025(17) 0.0249(4) Uani 1.00 1 d . . . C(24) C -0.09367(19) 0.95949(16) 0.3926(2) 0.0309(5) Uani 1.00 1 d . . . C(25) C -0.1096(2) 0.99632(17) 0.3035(2) 0.0366(6) Uani 1.00 1 d . . . C(26) C -0.0639(2) 0.96328(17) 0.2385(2) 0.0357(6) Uani 1.00 1 d . . . C(27) C -0.00034(18) 0.89364(16) 0.26238(18) 0.0284(5) Uani 1.00 1 d . . . C(28) C 0.02231(17) 0.85716(14) 0.35640(16) 0.0225(4) Uani 1.00 1 d . . . C(29) C 0.0081(2) 0.8756(2) 0.1020(2) 0.0494(8) Uani 1.00 1 d . . . H(1) H 0.0702 0.5523 0.7088 0.047 Uiso 1.00 1 c R . . H(2) H -0.0036 0.6269 0.7188 0.047 Uiso 1.00 1 c R . . H(3) H 0.1129 0.6228 0.7903 0.047 Uiso 1.00 1 c R . . H(4) H 0.0868 0.5570 0.5669 0.035 Uiso 1.00 1 c R . . H(5) H 0.0011 0.6260 0.5175 0.035 Uiso 1.00 1 c R . . H(6) H 0.1572 0.5365 0.4554 0.029 Uiso 1.00 1 c R . . H(7) H 0.2394 0.4916 0.3428 0.037 Uiso 1.00 1 c R . . H(8) H 0.3513 0.5156 0.2547 0.044 Uiso 1.00 1 c R . . H(9) H 0.4220 0.6487 0.2551 0.044 Uiso 1.00 1 c R . . H(10) H 0.3074 0.8532 0.2377 0.054 Uiso 1.00 1 c R . . H(11) H 0.3554 0.9003 0.3396 0.054 Uiso 1.00 1 c R . . H(12) H 0.2630 0.8352 0.3248 0.054 Uiso 1.00 1 c R . . H(13) H 0.2369 0.6928 0.7646 0.037 Uiso 1.00 1 c R . . H(14) H 0.2549 0.6253 0.6902 0.037 Uiso 1.00 1 c R . . H(15) H 0.3773 0.7648 0.7497 0.034 Uiso 1.00 1 c R . . H(16) H 0.5242 0.8473 0.7447 0.040 Uiso 1.00 1 c R . . H(17) H 0.5853 0.9666 0.6907 0.042 Uiso 1.00 1 c R . . H(18) H 0.4744 1.0508 0.5704 0.037 Uiso 1.00 1 c R . . H(19) H 0.2749 1.1436 0.5083 0.045 Uiso 1.00 1 c R . . H(20) H 0.2704 1.1277 0.3982 0.045 Uiso 1.00 1 c R . . H(21) H 0.3766 1.1159 0.4853 0.045 Uiso 1.00 1 c R . . H(22) H -0.0281 0.7394 0.6319 0.032 Uiso 1.00 1 c R . . H(23) H 0.0761 0.7843 0.6965 0.032 Uiso 1.00 1 c R . . H(24) H -0.0646 0.8623 0.5421 0.030 Uiso 1.00 1 c R . . H(25) H -0.1275 0.9806 0.4353 0.037 Uiso 1.00 1 c R . . H(26) H -0.1520 1.0446 0.2860 0.044 Uiso 1.00 1 c R . . H(27) H -0.0766 0.9890 0.1767 0.043 Uiso 1.00 1 c R . . H(28) H -0.0478 0.8373 0.0681 0.059 Uiso 1.00 1 c R . . H(29) H 0.0644 0.8701 0.0747 0.059 Uiso 1.00 1 c R . . H(30) H -0.0176 0.9332 0.0937 0.059 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.02186(18) 0.01633(17) 0.01934(18) 0.00110(12) 0.00682(13) 0.00109(12) P(1) 0.0396(3) 0.0271(3) 0.0332(3) 0.0052(2) 0.0025(3) -0.0010(2) F(1) 0.115(2) 0.0838(18) 0.0883(18) -0.0075(16) 0.0555(17) 0.0237(14) F(2) 0.0548(11) 0.0672(13) 0.0474(10) 0.0188(10) -0.0078(9) -0.0130(9) F(3) 0.0675(13) 0.0538(12) 0.0679(13) 0.0251(10) 0.0151(11) -0.0135(10) F(4) 0.0918(19) 0.099(2) 0.0745(16) 0.0282(15) -0.0338(14) -0.0539(15) F(5) 0.0587(11) 0.0415(10) 0.0564(11) 0.0224(8) 0.0016(9) -0.0028(8) F(6) 0.108(2) 0.0451(12) 0.161(2) 0.0023(13) 0.084(2) 0.0233(15) O(1) 0.0248(8) 0.0221(7) 0.0257(8) -0.0002(6) 0.0106(6) -0.0009(6) O(2) 0.0235(7) 0.0178(7) 0.0258(8) 0.0004(6) 0.0037(6) 0.0001(6) O(3) 0.0267(8) 0.0209(7) 0.0210(7) 0.0006(6) 0.0053(6) 0.0002(6) O(4) 0.0325(9) 0.0375(10) 0.0469(11) -0.0031(8) 0.0192(8) 0.0078(8) O(5) 0.0391(10) 0.0221(8) 0.0323(9) -0.0032(7) 0.0075(8) 0.0032(7) O(6) 0.0393(10) 0.0516(12) 0.0218(8) 0.0019(8) 0.0090(7) 0.0074(8) N(1) 0.0261(9) 0.0190(9) 0.0246(9) -0.0005(7) 0.0109(8) 0.0027(7) N(2) 0.0254(9) 0.0246(9) 0.0227(9) 0.0038(7) 0.0070(8) 0.0042(7) N(3) 0.0241(9) 0.0219(9) 0.0214(9) 0.0006(7) 0.0086(7) -0.0016(7) C(1) 0.0434(15) 0.0430(15) 0.0368(14) 0.0027(12) 0.0201(12) 0.0151(12) C(2) 0.0330(12) 0.0277(12) 0.0281(11) 0.0026(9) 0.0153(10) 0.0078(9) C(3) 0.0359(13) 0.0220(11) 0.0370(13) -0.0027(9) 0.0210(11) 0.0037(10) C(4) 0.0297(11) 0.0169(10) 0.0261(11) 0.0001(8) 0.0085(9) 0.0025(8) C(5) 0.0261(11) 0.0230(11) 0.0225(10) 0.0045(9) 0.0070(9) 0.0039(8) C(6) 0.0366(13) 0.0255(12) 0.0311(12) 0.0049(10) 0.0110(10) -0.0005(10) C(7) 0.0450(15) 0.0374(14) 0.0331(13) 0.0116(12) 0.0190(12) -0.0038(11) C(8) 0.0370(14) 0.0441(15) 0.0350(13) 0.0072(11) 0.0210(12) 0.0030(11) C(9) 0.0277(12) 0.0313(12) 0.0302(12) 0.0015(9) 0.0119(10) 0.0054(10) C(10) 0.0220(10) 0.0232(10) 0.0210(10) 0.0048(8) 0.0057(8) 0.0031(8) C(11) 0.0510(18) 0.0319(14) 0.0565(18) -0.0030(12) 0.0235(15) 0.0124(13) C(12) 0.0331(13) 0.0324(13) 0.0280(12) 0.0050(10) 0.0108(10) 0.0119(10) C(13) 0.0294(12) 0.0279(12) 0.0248(11) 0.0072(9) 0.0037(9) 0.0006(9) C(14) 0.0271(12) 0.0249(11) 0.0251(11) 0.0014(9) 0.0049(9) -0.0038(9) C(15) 0.0274(12) 0.0335(13) 0.0336(13) 0.0027(10) 0.0012(10) -0.0046(10) C(16) 0.0244(12) 0.0361(14) 0.0428(14) -0.0020(10) 0.0070(11) -0.0102(11) C(17) 0.0314(12) 0.0266(12) 0.0361(13) -0.0054(10) 0.0146(11) -0.0087(10) C(18) 0.0299(12) 0.0241(11) 0.0229(10) 0.0002(9) 0.0093(9) -0.0051(9) C(19) 0.0232(10) 0.0216(10) 0.0228(10) 0.0000(8) 0.0063(8) -0.0060(8) C(20) 0.0466(15) 0.0224(12) 0.0428(15) -0.0028(11) 0.0138(12) 0.0018(11) C(21) 0.0299(12) 0.0308(12) 0.0207(10) 0.0022(9) 0.0108(9) 0.0010(9) C(22) 0.0252(11) 0.0228(11) 0.0269(11) 0.0013(8) 0.0081(9) -0.0051(9) C(23) 0.0218(10) 0.0207(10) 0.0283(11) -0.0006(8) 0.0027(9) -0.0017(9) C(24) 0.0275(12) 0.0233(11) 0.0372(13) 0.0019(9) 0.0040(10) -0.0024(10) C(25) 0.0305(13) 0.0237(12) 0.0460(15) 0.0022(10) -0.0008(11) 0.0076(11) C(26) 0.0313(13) 0.0329(13) 0.0346(13) -0.0047(10) -0.0007(11) 0.0147(11) C(27) 0.0238(11) 0.0304(12) 0.0262(11) -0.0059(9) 0.0014(9) 0.0046(9) C(28) 0.0218(10) 0.0187(10) 0.0229(10) -0.0034(8) 0.0014(8) -0.0004(8) C(29) 0.0540(19) 0.067(2) 0.0222(12) -0.0080(16) 0.0051(12) 0.0070(13) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mn(1) O(1) 1.856(2) yes . . Mn(1) O(2) 1.8606(16) yes . . Mn(1) O(3) 1.8665(14) yes . . Mn(1) N(1) 2.0026(19) yes . . Mn(1) N(2) 2.0020(18) yes . . Mn(1) N(3) 1.992(2) yes . . P(1) F(1) 1.592(3) yes . . P(1) F(2) 1.6013(18) yes . . P(1) F(3) 1.596(2) yes . . P(1) F(4) 1.567(2) yes . . P(1) F(5) 1.593(2) yes . . P(1) F(6) 1.567(3) yes . . O(1) C(10) 1.323(3) yes . . O(2) C(19) 1.329(2) yes . . O(3) C(28) 1.325(2) yes . . O(4) C(9) 1.374(3) yes . . O(4) C(11) 1.432(3) yes . . O(5) C(18) 1.367(2) yes . . O(5) C(20) 1.429(3) yes . . O(6) C(27) 1.357(3) yes . . O(6) C(29) 1.437(3) yes . . N(1) C(3) 1.476(3) yes . . N(1) C(4) 1.289(3) yes . . N(2) C(12) 1.476(3) yes . . N(2) C(13) 1.284(3) yes . . N(3) C(21) 1.479(3) yes . . N(3) C(22) 1.283(2) yes . . C(1) C(2) 1.533(4) yes . . C(2) C(3) 1.536(3) yes . . C(2) C(12) 1.536(3) yes . . C(2) C(21) 1.539(3) yes . . C(4) C(5) 1.437(3) yes . . C(5) C(6) 1.406(3) yes . . C(5) C(10) 1.411(3) yes . . C(6) C(7) 1.377(4) yes . . C(7) C(8) 1.394(4) yes . . C(8) C(9) 1.377(4) yes . . C(9) C(10) 1.419(4) yes . . C(13) C(14) 1.433(3) yes . . C(14) C(15) 1.411(3) yes . . C(14) C(19) 1.417(2) yes . . C(15) C(16) 1.371(4) yes . . C(16) C(17) 1.396(3) yes . . C(17) C(18) 1.386(3) yes . . C(18) C(19) 1.414(3) yes . . C(22) C(23) 1.434(3) yes . . C(23) C(24) 1.413(3) yes . . C(23) C(28) 1.413(3) yes . . C(24) C(25) 1.373(4) yes . . C(25) C(26) 1.396(4) yes . . C(26) C(27) 1.387(3) yes . . C(27) C(28) 1.424(3) yes . . C(1) H(1) 0.980 no . . C(1) H(2) 0.980 no . . C(1) H(3) 0.980 no . . C(3) H(4) 0.990 no . . C(3) H(5) 0.990 no . . C(4) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(11) H(10) 0.980 no . . C(11) H(11) 0.980 no . . C(11) H(12) 0.980 no . . C(12) H(13) 0.990 no . . C(12) H(14) 0.990 no . . C(13) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(17) H(18) 0.950 no . . C(20) H(19) 0.980 no . . C(20) H(20) 0.980 no . . C(20) H(21) 0.980 no . . C(21) H(22) 0.990 no . . C(21) H(23) 0.990 no . . C(22) H(24) 0.950 no . . C(24) H(25) 0.950 no . . C(25) H(26) 0.950 no . . C(26) H(27) 0.950 no . . C(29) H(28) 0.980 no . . C(29) H(29) 0.980 no . . C(29) H(30) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Mn(1) O(2) 89.29(7) yes . . . O(1) Mn(1) O(3) 91.44(7) yes . . . O(1) Mn(1) N(1) 90.04(8) yes . . . O(1) Mn(1) N(2) 92.81(8) yes . . . O(1) Mn(1) N(3) 179.53(7) yes . . . O(2) Mn(1) O(3) 93.33(6) yes . . . O(2) Mn(1) N(1) 173.44(6) yes . . . O(2) Mn(1) N(2) 88.64(7) yes . . . O(2) Mn(1) N(3) 90.37(8) yes . . . O(3) Mn(1) N(1) 93.21(7) yes . . . O(3) Mn(1) N(2) 175.34(9) yes . . . O(3) Mn(1) N(3) 88.25(7) yes . . . N(1) Mn(1) N(2) 84.87(7) yes . . . N(1) Mn(1) N(3) 90.34(8) yes . . . N(2) Mn(1) N(3) 87.51(8) yes . . . F(1) P(1) F(2) 87.35(13) yes . . . F(1) P(1) F(3) 91.15(15) yes . . . F(1) P(1) F(4) 89.73(15) yes . . . F(1) P(1) F(5) 89.25(14) yes . . . F(1) P(1) F(6) 176.80(15) yes . . . F(2) P(1) F(3) 89.88(11) yes . . . F(2) P(1) F(4) 177.05(15) yes . . . F(2) P(1) F(5) 89.52(10) yes . . . F(2) P(1) F(6) 89.89(14) yes . . . F(3) P(1) F(4) 90.62(13) yes . . . F(3) P(1) F(5) 179.26(12) yes . . . F(3) P(1) F(6) 90.48(14) yes . . . F(4) P(1) F(5) 90.00(13) yes . . . F(4) P(1) F(6) 93.01(16) yes . . . F(5) P(1) F(6) 89.09(14) yes . . . Mn(1) O(1) C(10) 127.40(15) yes . . . Mn(1) O(2) C(19) 121.77(14) yes . . . Mn(1) O(3) C(28) 122.21(14) yes . . . C(9) O(4) C(11) 114.1(2) yes . . . C(18) O(5) C(20) 116.44(18) yes . . . C(27) O(6) C(29) 117.5(2) yes . . . Mn(1) N(1) C(3) 116.34(15) yes . . . Mn(1) N(1) C(4) 124.83(18) yes . . . C(3) N(1) C(4) 118.5(2) yes . . . Mn(1) N(2) C(12) 119.07(14) yes . . . Mn(1) N(2) C(13) 121.72(18) yes . . . C(12) N(2) C(13) 119.16(19) yes . . . Mn(1) N(3) C(21) 119.27(15) yes . . . Mn(1) N(3) C(22) 121.61(18) yes . . . C(21) N(3) C(22) 119.0(2) yes . . . C(1) C(2) C(3) 109.2(2) yes . . . C(1) C(2) C(12) 108.32(19) yes . . . C(1) C(2) C(21) 108.2(2) yes . . . C(3) C(2) C(12) 110.5(2) yes . . . C(3) C(2) C(21) 110.40(18) yes . . . C(12) C(2) C(21) 110.3(2) yes . . . N(1) C(3) C(2) 111.2(2) yes . . . N(1) C(4) C(5) 126.1(2) yes . . . C(4) C(5) C(6) 118.8(2) yes . . . C(4) C(5) C(10) 120.7(2) yes . . . C(6) C(5) C(10) 120.4(2) yes . . . C(5) C(6) C(7) 120.3(2) yes . . . C(6) C(7) C(8) 119.4(2) yes . . . C(7) C(8) C(9) 121.7(3) yes . . . O(4) C(9) C(8) 119.5(2) yes . . . O(4) C(9) C(10) 120.7(2) yes . . . C(8) C(9) C(10) 119.7(2) yes . . . O(1) C(10) C(5) 123.1(2) yes . . . O(1) C(10) C(9) 118.6(2) yes . . . C(5) C(10) C(9) 118.2(2) yes . . . N(2) C(12) C(2) 111.24(19) yes . . . N(2) C(13) C(14) 125.1(2) yes . . . C(13) C(14) C(15) 119.1(2) yes . . . C(13) C(14) C(19) 120.3(2) yes . . . C(15) C(14) C(19) 120.3(2) yes . . . C(14) C(15) C(16) 119.6(2) yes . . . C(15) C(16) C(17) 120.6(2) yes . . . C(16) C(17) C(18) 120.9(2) yes . . . O(5) C(18) C(17) 124.8(2) yes . . . O(5) C(18) C(19) 115.4(2) yes . . . C(17) C(18) C(19) 119.8(2) yes . . . O(2) C(19) C(14) 122.7(2) yes . . . O(2) C(19) C(18) 118.69(18) yes . . . C(14) C(19) C(18) 118.5(2) yes . . . N(3) C(21) C(2) 110.9(2) yes . . . N(3) C(22) C(23) 125.7(2) yes . . . C(22) C(23) C(24) 119.3(2) yes . . . C(22) C(23) C(28) 119.8(2) yes . . . C(24) C(23) C(28) 120.6(2) yes . . . C(23) C(24) C(25) 119.7(2) yes . . . C(24) C(25) C(26) 120.5(2) yes . . . C(25) C(26) C(27) 121.2(2) yes . . . O(6) C(27) C(26) 126.0(2) yes . . . O(6) C(27) C(28) 114.5(2) yes . . . C(26) C(27) C(28) 119.5(2) yes . . . O(3) C(28) C(23) 122.9(2) yes . . . O(3) C(28) C(27) 118.6(2) yes . . . C(23) C(28) C(27) 118.4(2) yes . . . C(2) C(1) H(1) 109.5 no . . . C(2) C(1) H(2) 109.5 no . . . C(2) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . N(1) C(3) H(4) 109.4 no . . . N(1) C(3) H(5) 109.4 no . . . C(2) C(3) H(4) 109.4 no . . . C(2) C(3) H(5) 109.4 no . . . H(4) C(3) H(5) 108.0 no . . . N(1) C(4) H(6) 117.0 no . . . C(5) C(4) H(6) 117.0 no . . . C(5) C(6) H(7) 119.8 no . . . C(7) C(6) H(7) 119.8 no . . . C(6) C(7) H(8) 120.3 no . . . C(8) C(7) H(8) 120.3 no . . . C(7) C(8) H(9) 119.1 no . . . C(9) C(8) H(9) 119.1 no . . . O(4) C(11) H(10) 109.5 no . . . O(4) C(11) H(11) 109.5 no . . . O(4) C(11) H(12) 109.5 no . . . H(10) C(11) H(11) 109.5 no . . . H(10) C(11) H(12) 109.5 no . . . H(11) C(11) H(12) 109.5 no . . . N(2) C(12) H(13) 109.4 no . . . N(2) C(12) H(14) 109.4 no . . . C(2) C(12) H(13) 109.4 no . . . C(2) C(12) H(14) 109.4 no . . . H(13) C(12) H(14) 108.0 no . . . N(2) C(13) H(15) 117.4 no . . . C(14) C(13) H(15) 117.4 no . . . C(14) C(15) H(16) 120.2 no . . . C(16) C(15) H(16) 120.2 no . . . C(15) C(16) H(17) 119.7 no . . . C(17) C(16) H(17) 119.7 no . . . C(16) C(17) H(18) 119.6 no . . . C(18) C(17) H(18) 119.6 no . . . O(5) C(20) H(19) 109.5 no . . . O(5) C(20) H(20) 109.5 no . . . O(5) C(20) H(21) 109.5 no . . . H(19) C(20) H(20) 109.5 no . . . H(19) C(20) H(21) 109.5 no . . . H(20) C(20) H(21) 109.5 no . . . N(3) C(21) H(22) 109.5 no . . . N(3) C(21) H(23) 109.5 no . . . C(2) C(21) H(22) 109.5 no . . . C(2) C(21) H(23) 109.5 no . . . H(22) C(21) H(23) 108.0 no . . . N(3) C(22) H(24) 117.1 no . . . C(23) C(22) H(24) 117.1 no . . . C(23) C(24) H(25) 120.2 no . . . C(25) C(24) H(25) 120.2 no . . . C(24) C(25) H(26) 119.8 no . . . C(26) C(25) H(26) 119.8 no . . . C(25) C(26) H(27) 119.4 no . . . C(27) C(26) H(27) 119.4 no . . . O(6) C(29) H(28) 109.5 no . . . O(6) C(29) H(29) 109.5 no . . . O(6) C(29) H(30) 109.5 no . . . H(28) C(29) H(29) 109.5 no . . . H(28) C(29) H(30) 109.5 no . . . H(29) C(29) H(30) 109.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F(1) C(4) 3.561(3) ? . 2_556 F(1) C(25) 3.563(3) ? . 3_576 F(2) C(1) 3.392(3) ? . 4_565 F(2) C(2) 3.585(3) ? . 4_565 F(2) C(3) 3.321(3) ? . 4_565 F(2) C(4) 3.417(3) ? . 2_556 F(2) C(6) 3.562(3) ? . 2_556 F(2) C(21) 3.462(3) ? . 4_565 F(3) N(3) 3.261(2) ? . 4_565 F(3) C(21) 3.495(2) ? . 4_565 F(3) C(22) 2.928(3) ? . 4_565 F(3) C(23) 3.472(3) ? . 4_565 F(4) C(12) 3.521(4) ? . . F(4) C(21) 3.240(3) ? . . F(4) C(25) 3.465(3) ? . 3_576 F(5) C(4) 3.307(2) ? . 2_556 F(5) C(5) 3.529(2) ? . 2_556 F(5) C(6) 3.291(3) ? . 2_556 F(5) C(26) 3.283(3) ? . 3_576 F(6) C(20) 3.005(3) ? . 2_546 F(6) C(29) 3.511(5) ? . 1_556 O(2) C(24) 3.422(3) ? . 3_576 O(6) C(13) 3.561(3) ? . 4_464 N(3) F(3) 3.261(2) ? . 4_464 C(1) F(2) 3.392(3) ? . 4_464 C(1) C(16) 3.439(4) ? . 2_546 C(1) C(17) 3.306(4) ? . 2_546 C(2) F(2) 3.585(3) ? . 4_464 C(3) F(2) 3.321(3) ? . 4_464 C(4) F(1) 3.561(3) ? . 2_546 C(4) F(2) 3.417(3) ? . 2_546 C(4) F(5) 3.307(2) ? . 2_546 C(5) F(5) 3.529(2) ? . 2_546 C(6) F(2) 3.562(3) ? . 2_546 C(6) F(5) 3.291(3) ? . 2_546 C(10) C(29) 3.589(3) ? . 4_565 C(12) F(4) 3.521(4) ? . . C(13) O(6) 3.561(3) ? . 4_565 C(13) C(27) 3.554(3) ? . 4_565 C(16) C(1) 3.439(4) ? . 2_556 C(17) C(1) 3.306(4) ? . 2_556 C(17) C(17) 3.334(4) ? . 3_676 C(20) F(6) 3.005(3) ? . 2_556 C(21) F(2) 3.462(3) ? . 4_464 C(21) F(3) 3.495(2) ? . 4_464 C(21) F(4) 3.240(3) ? . . C(22) F(3) 2.928(3) ? . 4_464 C(22) C(24) 3.515(3) ? . 3_576 C(23) F(3) 3.472(3) ? . 4_464 C(24) O(2) 3.422(3) ? . 3_576 C(24) C(22) 3.515(3) ? . 3_576 C(24) C(24) 3.580(3) ? . 3_576 C(25) F(1) 3.563(3) ? . 3_576 C(25) F(4) 3.465(3) ? . 3_576 C(26) F(5) 3.283(3) ? . 3_576 C(27) C(13) 3.554(3) ? . 4_464 C(29) F(6) 3.511(5) ? . 1_554 C(29) C(10) 3.589(3) ? . 4_464 P(1) H(5) 3.307 ? . 4_565 P(1) H(6) 3.322 ? . 2_556 P(1) H(19) 3.432 ? . 2_546 P(1) H(27) 3.531 ? . 3_576 P(1) H(29) 3.562 ? . 1_556 F(1) H(1) 3.452 ? . 2_556 F(1) H(4) 2.678 ? . 2_556 F(1) H(5) 2.763 ? . 4_565 F(1) H(6) 2.815 ? . 2_556 F(1) H(15) 3.562 ? . . F(1) H(26) 2.886 ? . 3_576 F(1) H(27) 3.345 ? . 3_576 F(2) H(1) 3.504 ? . 4_565 F(2) H(2) 2.737 ? . 4_565 F(2) H(4) 3.578 ? . 4_565 F(2) H(5) 2.525 ? . 4_565 F(2) H(6) 2.516 ? . 2_556 F(2) H(7) 2.745 ? . 2_556 F(2) H(10) 2.872 ? . 1_556 F(2) H(22) 2.688 ? . 4_565 F(3) H(5) 2.841 ? . 4_565 F(3) H(13) 2.786 ? . . F(3) H(15) 3.135 ? . . F(3) H(19) 2.712 ? . 2_546 F(3) H(22) 2.893 ? . 4_565 F(3) H(24) 2.846 ? . 4_565 F(4) H(3) 3.447 ? . . F(4) H(9) 3.220 ? . 4_465 F(4) H(13) 2.821 ? . . F(4) H(19) 3.581 ? . 2_546 F(4) H(23) 2.278 ? . . F(4) H(26) 2.748 ? . 3_576 F(4) H(27) 3.118 ? . 3_576 F(5) H(6) 2.799 ? . 2_556 F(5) H(7) 2.899 ? . 2_556 F(5) H(26) 3.504 ? . 3_576 F(5) H(27) 2.404 ? . 3_576 F(5) H(29) 2.779 ? . 1_556 F(5) H(30) 3.021 ? . 3_576 F(6) H(10) 3.346 ? . 1_556 F(6) H(19) 2.493 ? . 2_546 F(6) H(20) 2.992 ? . 2_546 F(6) H(21) 3.047 ? . 2_546 F(6) H(29) 2.585 ? . 1_556 O(1) H(28) 2.733 ? . 4_565 O(2) H(25) 2.631 ? . 3_576 O(2) H(26) 3.307 ? . 3_576 O(3) H(15) 2.984 ? . 4_464 O(3) H(16) 2.882 ? . 4_464 O(4) H(2) 2.957 ? . 4_564 O(4) H(18) 3.227 ? . 3_676 O(4) H(22) 3.533 ? . 4_564 O(5) H(8) 3.221 ? . 2_555 O(5) H(17) 3.506 ? . 3_676 O(5) H(24) 3.380 ? . 3_576 O(5) H(25) 2.773 ? . 3_576 O(6) H(8) 2.897 ? . 2_555 O(6) H(15) 3.229 ? . 4_464 O(6) H(16) 3.317 ? . 4_464 N(1) H(16) 3.477 ? . 4_464 N(2) H(28) 3.507 ? . 4_565 N(3) H(26) 3.484 ? . 3_576 C(1) H(18) 3.364 ? . 2_546 C(4) H(16) 3.196 ? . 4_464 C(5) H(16) 3.182 ? . 4_464 C(5) H(17) 3.319 ? . 4_464 C(5) H(28) 3.226 ? . 4_565 C(6) H(10) 3.334 ? . 2_545 C(6) H(11) 3.520 ? . 2_545 C(6) H(17) 2.766 ? . 4_464 C(6) H(29) 3.571 ? . 2_545 C(7) H(17) 3.281 ? . 4_464 C(7) H(20) 2.870 ? . 2_545 C(7) H(27) 3.393 ? . 2_545 C(7) H(30) 3.234 ? . 2_545 C(8) H(20) 2.845 ? . 2_545 C(8) H(22) 3.581 ? . 4_564 C(8) H(27) 3.560 ? . 2_545 C(9) H(20) 3.586 ? . 2_545 C(9) H(28) 3.170 ? . 4_565 C(10) H(28) 2.740 ? . 4_565 C(11) H(2) 3.060 ? . 4_564 C(11) H(7) 3.102 ? . 2_555 C(11) H(8) 3.530 ? . 2_555 C(11) H(17) 3.208 ? . 3_676 C(11) H(18) 3.183 ? . 3_676 C(13) H(28) 3.313 ? . 4_565 C(14) H(28) 3.553 ? . 4_565 C(15) H(1) 3.276 ? . 2_556 C(16) H(1) 2.987 ? . 2_556 C(16) H(2) 3.330 ? . 2_556 C(16) H(3) 3.447 ? . 2_556 C(16) H(7) 3.456 ? . 4_565 C(16) H(11) 2.973 ? . 3_676 C(16) H(18) 3.433 ? . 3_676 C(16) H(20) 3.564 ? . 3_676 C(16) H(21) 3.166 ? . 3_676 C(17) H(1) 3.135 ? . 2_556 C(17) H(2) 3.319 ? . 2_556 C(17) H(3) 2.921 ? . 2_556 C(17) H(11) 2.993 ? . 3_676 C(17) H(18) 2.963 ? . 3_676 C(17) H(21) 3.475 ? . 3_676 C(18) H(1) 3.583 ? . 2_556 C(18) H(3) 3.241 ? . 2_556 C(18) H(18) 3.423 ? . 3_676 C(18) H(25) 3.186 ? . 3_576 C(19) H(25) 3.099 ? . 3_576 C(19) H(26) 3.552 ? . 3_576 C(20) H(3) 3.358 ? . 2_556 C(20) H(8) 3.543 ? . 2_555 C(20) H(17) 3.369 ? . 3_676 C(20) H(24) 3.249 ? . 3_576 C(20) H(25) 3.475 ? . 3_576 C(21) H(9) 3.205 ? . 4_465 C(22) H(19) 3.469 ? . 3_576 C(22) H(25) 3.319 ? . 3_576 C(22) H(26) 3.553 ? . 3_576 C(23) H(13) 3.552 ? . 4_464 C(23) H(15) 3.446 ? . 4_464 C(23) H(25) 3.204 ? . 3_576 C(24) H(13) 3.460 ? . 4_464 C(24) H(14) 3.291 ? . 4_464 C(24) H(24) 3.520 ? . 3_576 C(24) H(25) 3.384 ? . 3_576 C(25) H(14) 2.820 ? . 4_464 C(25) H(23) 3.534 ? . 3_576 C(25) H(24) 3.517 ? . 3_576 C(26) H(8) 3.005 ? . 2_555 C(26) H(9) 3.530 ? . 2_555 C(26) H(14) 2.747 ? . 4_464 C(27) H(8) 2.893 ? . 2_555 C(27) H(14) 3.191 ? . 4_464 C(27) H(15) 3.010 ? . 4_464 C(28) H(15) 2.855 ? . 4_464 C(29) H(8) 3.233 ? . 2_555 H(1) F(1) 3.452 ? . 2_546 H(1) F(2) 3.504 ? . 4_464 H(1) C(15) 3.276 ? . 2_546 H(1) C(16) 2.987 ? . 2_546 H(1) C(17) 3.135 ? . 2_546 H(1) C(18) 3.583 ? . 2_546 H(1) H(6) 3.550 ? . 3_566 H(1) H(17) 3.254 ? . 2_546 H(1) H(18) 3.456 ? . 2_546 H(2) F(2) 2.737 ? . 4_464 H(2) O(4) 2.957 ? . 4_465 H(2) C(11) 3.060 ? . 4_465 H(2) C(16) 3.330 ? . 2_546 H(2) C(17) 3.319 ? . 2_546 H(2) H(10) 2.714 ? . 4_465 H(2) H(11) 3.038 ? . 4_465 H(2) H(17) 3.241 ? . 2_546 H(2) H(18) 3.198 ? . 2_546 H(3) F(4) 3.447 ? . . H(3) C(16) 3.447 ? . 2_546 H(3) C(17) 2.921 ? . 2_546 H(3) C(18) 3.241 ? . 2_546 H(3) C(20) 3.358 ? . 2_546 H(3) H(18) 2.904 ? . 2_546 H(3) H(19) 2.850 ? . 2_546 H(3) H(21) 3.219 ? . 2_546 H(4) F(1) 2.678 ? . 2_546 H(4) F(2) 3.578 ? . 4_464 H(4) H(4) 3.124 ? . 3_566 H(4) H(5) 3.247 ? . 3_566 H(4) H(6) 3.583 ? . 3_566 H(5) P(1) 3.307 ? . 4_464 H(5) F(1) 2.763 ? . 4_464 H(5) F(2) 2.525 ? . 4_464 H(5) F(3) 2.841 ? . 4_464 H(5) H(4) 3.247 ? . 3_566 H(5) H(6) 3.489 ? . 3_566 H(6) P(1) 3.322 ? . 2_546 H(6) F(1) 2.815 ? . 2_546 H(6) F(2) 2.516 ? . 2_546 H(6) F(5) 2.799 ? . 2_546 H(6) H(1) 3.550 ? . 3_566 H(6) H(4) 3.583 ? . 3_566 H(6) H(5) 3.489 ? . 3_566 H(6) H(16) 3.539 ? . 4_464 H(7) F(2) 2.745 ? . 2_546 H(7) F(5) 2.899 ? . 2_546 H(7) C(11) 3.102 ? . 2_545 H(7) C(16) 3.456 ? . 4_464 H(7) H(10) 2.486 ? . 2_545 H(7) H(11) 2.933 ? . 2_545 H(7) H(12) 3.482 ? . 2_545 H(7) H(17) 2.601 ? . 4_464 H(7) H(29) 3.218 ? . 2_545 H(8) O(5) 3.221 ? . 2_545 H(8) O(6) 2.897 ? . 2_545 H(8) C(11) 3.530 ? . 2_545 H(8) C(20) 3.543 ? . 2_545 H(8) C(26) 3.005 ? . 2_545 H(8) C(27) 2.893 ? . 2_545 H(8) C(29) 3.233 ? . 2_545 H(8) H(10) 3.413 ? . 2_545 H(8) H(11) 3.285 ? . 2_545 H(8) H(12) 3.305 ? . 2_545 H(8) H(17) 3.474 ? . 4_464 H(8) H(20) 2.920 ? . 2_545 H(8) H(27) 2.955 ? . 2_545 H(8) H(29) 3.320 ? . 2_545 H(8) H(30) 2.920 ? . 2_545 H(9) F(4) 3.220 ? . 4_564 H(9) C(21) 3.205 ? . 4_564 H(9) C(26) 3.530 ? . 2_545 H(9) H(20) 2.869 ? . 2_545 H(9) H(22) 2.770 ? . 4_564 H(9) H(23) 2.741 ? . 4_564 H(9) H(24) 3.165 ? . 4_564 H(9) H(27) 3.260 ? . 2_545 H(10) F(2) 2.872 ? . 1_554 H(10) F(6) 3.346 ? . 1_554 H(10) C(6) 3.334 ? . 2_555 H(10) H(2) 2.714 ? . 4_564 H(10) H(7) 2.486 ? . 2_555 H(10) H(8) 3.413 ? . 2_555 H(10) H(17) 3.246 ? . 3_676 H(10) H(22) 3.451 ? . 4_564 H(11) C(6) 3.520 ? . 2_555 H(11) C(16) 2.973 ? . 3_676 H(11) C(17) 2.993 ? . 3_676 H(11) H(2) 3.038 ? . 4_564 H(11) H(7) 2.933 ? . 2_555 H(11) H(8) 3.285 ? . 2_555 H(11) H(17) 2.368 ? . 3_676 H(11) H(18) 2.405 ? . 3_676 H(12) H(7) 3.482 ? . 2_555 H(12) H(8) 3.305 ? . 2_555 H(13) F(3) 2.786 ? . . H(13) F(4) 2.821 ? . . H(13) C(23) 3.552 ? . 4_565 H(13) C(24) 3.460 ? . 4_565 H(13) H(19) 3.447 ? . 2_546 H(14) C(24) 3.291 ? . 4_565 H(14) C(25) 2.820 ? . 4_565 H(14) C(26) 2.747 ? . 4_565 H(14) C(27) 3.191 ? . 4_565 H(14) H(26) 3.128 ? . 4_565 H(14) H(27) 3.002 ? . 4_565 H(15) F(1) 3.562 ? . . H(15) F(3) 3.135 ? . . H(15) O(3) 2.984 ? . 4_565 H(15) O(6) 3.229 ? . 4_565 H(15) C(23) 3.446 ? . 4_565 H(15) C(27) 3.010 ? . 4_565 H(15) C(28) 2.855 ? . 4_565 H(15) H(28) 3.527 ? . 4_565 H(16) O(3) 2.882 ? . 4_565 H(16) O(6) 3.317 ? . 4_565 H(16) N(1) 3.477 ? . 4_565 H(16) C(4) 3.196 ? . 4_565 H(16) C(5) 3.182 ? . 4_565 H(16) H(6) 3.539 ? . 4_565 H(17) O(5) 3.506 ? . 3_676 H(17) C(5) 3.319 ? . 4_565 H(17) C(6) 2.766 ? . 4_565 H(17) C(7) 3.281 ? . 4_565 H(17) C(11) 3.208 ? . 3_676 H(17) C(20) 3.369 ? . 3_676 H(17) H(1) 3.254 ? . 2_556 H(17) H(2) 3.241 ? . 2_556 H(17) H(7) 2.601 ? . 4_565 H(17) H(8) 3.474 ? . 4_565 H(17) H(10) 3.246 ? . 3_676 H(17) H(11) 2.368 ? . 3_676 H(17) H(20) 3.086 ? . 3_676 H(17) H(21) 3.069 ? . 3_676 H(18) O(4) 3.227 ? . 3_676 H(18) C(1) 3.364 ? . 2_556 H(18) C(11) 3.183 ? . 3_676 H(18) C(16) 3.433 ? . 3_676 H(18) C(17) 2.963 ? . 3_676 H(18) C(18) 3.423 ? . 3_676 H(18) H(1) 3.456 ? . 2_556 H(18) H(2) 3.198 ? . 2_556 H(18) H(3) 2.904 ? . 2_556 H(18) H(11) 2.405 ? . 3_676 H(18) H(18) 2.873 ? . 3_676 H(19) P(1) 3.432 ? . 2_556 H(19) F(3) 2.712 ? . 2_556 H(19) F(4) 3.581 ? . 2_556 H(19) F(6) 2.493 ? . 2_556 H(19) C(22) 3.469 ? . 3_576 H(19) H(3) 2.850 ? . 2_556 H(19) H(13) 3.447 ? . 2_556 H(19) H(24) 2.738 ? . 3_576 H(19) H(25) 3.127 ? . 3_576 H(20) F(6) 2.992 ? . 2_556 H(20) C(7) 2.870 ? . 2_555 H(20) C(8) 2.845 ? . 2_555 H(20) C(9) 3.586 ? . 2_555 H(20) C(16) 3.564 ? . 3_676 H(20) H(8) 2.920 ? . 2_555 H(20) H(9) 2.869 ? . 2_555 H(20) H(17) 3.086 ? . 3_676 H(20) H(24) 3.217 ? . 3_576 H(21) F(6) 3.047 ? . 2_556 H(21) C(16) 3.166 ? . 3_676 H(21) C(17) 3.475 ? . 3_676 H(21) H(3) 3.219 ? . 2_556 H(21) H(17) 3.069 ? . 3_676 H(22) F(2) 2.688 ? . 4_464 H(22) F(3) 2.893 ? . 4_464 H(22) O(4) 3.533 ? . 4_465 H(22) C(8) 3.581 ? . 4_465 H(22) H(9) 2.770 ? . 4_465 H(22) H(10) 3.451 ? . 4_465 H(23) F(4) 2.278 ? . . H(23) C(25) 3.534 ? . 3_576 H(23) H(9) 2.741 ? . 4_465 H(23) H(26) 2.906 ? . 3_576 H(24) F(3) 2.846 ? . 4_464 H(24) O(5) 3.380 ? . 3_576 H(24) C(20) 3.249 ? . 3_576 H(24) C(24) 3.520 ? . 3_576 H(24) C(25) 3.517 ? . 3_576 H(24) H(9) 3.165 ? . 4_465 H(24) H(19) 2.738 ? . 3_576 H(24) H(20) 3.217 ? . 3_576 H(24) H(25) 3.577 ? . 3_576 H(24) H(26) 3.530 ? . 3_576 H(25) O(2) 2.631 ? . 3_576 H(25) O(5) 2.773 ? . 3_576 H(25) C(18) 3.186 ? . 3_576 H(25) C(19) 3.099 ? . 3_576 H(25) C(20) 3.475 ? . 3_576 H(25) C(22) 3.319 ? . 3_576 H(25) C(23) 3.204 ? . 3_576 H(25) C(24) 3.384 ? . 3_576 H(25) H(19) 3.127 ? . 3_576 H(25) H(24) 3.577 ? . 3_576 H(25) H(25) 3.448 ? . 3_576 H(26) F(1) 2.886 ? . 3_576 H(26) F(4) 2.748 ? . 3_576 H(26) F(5) 3.504 ? . 3_576 H(26) O(2) 3.307 ? . 3_576 H(26) N(3) 3.484 ? . 3_576 H(26) C(19) 3.552 ? . 3_576 H(26) C(22) 3.553 ? . 3_576 H(26) H(14) 3.128 ? . 4_464 H(26) H(23) 2.906 ? . 3_576 H(26) H(24) 3.530 ? . 3_576 H(27) P(1) 3.531 ? . 3_576 H(27) F(1) 3.345 ? . 3_576 H(27) F(4) 3.118 ? . 3_576 H(27) F(5) 2.404 ? . 3_576 H(27) C(7) 3.393 ? . 2_555 H(27) C(8) 3.560 ? . 2_555 H(27) H(8) 2.955 ? . 2_555 H(27) H(9) 3.260 ? . 2_555 H(27) H(14) 3.002 ? . 4_464 H(28) O(1) 2.733 ? . 4_464 H(28) N(2) 3.507 ? . 4_464 H(28) C(5) 3.226 ? . 4_464 H(28) C(9) 3.170 ? . 4_464 H(28) C(10) 2.740 ? . 4_464 H(28) C(13) 3.313 ? . 4_464 H(28) C(14) 3.553 ? . 4_464 H(28) H(15) 3.527 ? . 4_464 H(29) P(1) 3.562 ? . 1_554 H(29) F(5) 2.779 ? . 1_554 H(29) F(6) 2.585 ? . 1_554 H(29) C(6) 3.571 ? . 2_555 H(29) H(7) 3.218 ? . 2_555 H(29) H(8) 3.320 ? . 2_555 H(30) F(5) 3.021 ? . 3_576 H(30) C(7) 3.234 ? . 2_555 H(30) H(8) 2.920 ? . 2_555 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data__080709b _database_code_depnum_ccdc_archive 'CCDC 812376' #TrackingRef 'NChem_All.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C29 H30 F6 K Mn N3 O6 P ' _chemical_formula_moiety 'C29 H30 Mn N3 O6, F6 P, K ' _chemical_formula_weight 755.57 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 13.0303(11) _cell_length_b 15.8880(12) _cell_length_c 15.6809(12) _cell_angle_alpha 90.0000 _cell_angle_beta 92.234(3) _cell_angle_gamma 90.0000 _cell_volume 3243.9(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16926 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544.00 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.647 _exptl_absorpt_correction_T_max 0.967 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 193.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 29502 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7358 _reflns_number_gt 4877 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1808 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7358 _refine_ls_number_parameters 425 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0841P)^2^+4.6209P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.12 _refine_diff_density_min -0.60 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; K K 0.200 0.250 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Mn(1) Mn 0.04309(4) 0.23236(3) 0.12056(3) 0.02383(15) Uani 1.00 1 d . . . K(1) K 0.29795(7) 0.21842(6) 0.05235(6) 0.0357(2) Uani 1.00 1 d . . . P(1) P 0.55124(12) 0.22256(15) -0.02519(12) 0.0836(6) Uani 1.00 1 d . . . F(1) F 0.4575(2) 0.2855(2) -0.0342(2) 0.0737(9) Uani 1.00 1 d . . . F(2) F 0.4683(2) 0.1446(2) -0.0301(2) 0.0897(11) Uani 1.00 1 d . . . F(3) F 0.5315(4) 0.2205(3) 0.0755(2) 0.1245(17) Uani 1.00 1 d . . . F(4) F 0.6396(3) 0.1561(5) -0.0111(4) 0.193(3) Uani 1.00 1 d . . . F(5) F 0.6261(4) 0.2956(5) -0.0138(6) 0.229(4) Uani 1.00 1 d . . . F(6) F 0.5567(4) 0.2104(4) -0.1228(3) 0.157(2) Uani 1.00 1 d . . . O(1) O 0.14800(19) 0.14350(16) 0.14574(15) 0.0277(5) Uani 1.00 1 d . . . O(2) O 0.1594(2) 0.31603(16) 0.13284(17) 0.0317(6) Uani 1.00 1 d . . . O(3) O 0.07242(19) 0.22180(15) 0.00376(16) 0.0271(5) Uani 1.00 1 d . . . O(4) O 0.3202(2) 0.0606(2) 0.1396(2) 0.0546(9) Uani 1.00 1 d . . . O(5) O 0.3435(2) 0.3784(2) 0.1252(2) 0.0479(7) Uani 1.00 1 d . . . O(6) O 0.2107(2) 0.17789(18) -0.10473(16) 0.0340(6) Uani 1.00 1 d . . . N(1) N 0.0051(2) 0.22693(19) 0.24406(19) 0.0262(6) Uani 1.00 1 d . . . N(2) N -0.0538(2) 0.3428(2) 0.1161(2) 0.0311(7) Uani 1.00 1 d . . . N(3) N -0.0943(2) 0.1656(2) 0.09495(19) 0.0281(6) Uani 1.00 1 d . . . C(1) C -0.2803(3) 0.2726(3) 0.2392(3) 0.0479(11) Uani 1.00 1 d . . . C(2) C -0.1772(3) 0.2601(2) 0.1975(2) 0.0336(8) Uani 1.00 1 d . . . C(3) C -0.0921(3) 0.2674(2) 0.2679(2) 0.0328(8) Uani 1.00 1 d . . . C(4) C 0.0583(3) 0.1905(2) 0.3049(2) 0.0296(8) Uani 1.00 1 d . . . C(5) C 0.1511(3) 0.1429(2) 0.2986(2) 0.0298(8) Uani 1.00 1 d . . . C(6) C 0.2004(3) 0.1151(2) 0.3757(2) 0.0392(9) Uani 1.00 1 d . . . C(7) C 0.2879(3) 0.0685(3) 0.3737(3) 0.0541(12) Uani 1.00 1 d . . . C(8) C 0.3302(3) 0.0483(3) 0.2947(3) 0.0551(13) Uani 1.00 1 d . . . C(9) C 0.2838(3) 0.0752(2) 0.2193(2) 0.0404(9) Uani 1.00 1 d . . . C(10) C 0.1911(2) 0.1226(2) 0.2191(2) 0.0298(8) Uani 1.00 1 d . . . C(11) C 0.4142(4) 0.0137(4) 0.1352(4) 0.083(2) Uani 1.00 1 d . . . C(12) C -0.1637(3) 0.3282(2) 0.1298(2) 0.0370(9) Uani 1.00 1 d . . . C(13) C -0.0251(3) 0.4198(2) 0.1103(2) 0.0319(8) Uani 1.00 1 d . . . C(14) C 0.0790(3) 0.4494(2) 0.1045(2) 0.0318(8) Uani 1.00 1 d . . . C(15) C 0.0938(3) 0.5368(2) 0.0905(2) 0.0416(10) Uani 1.00 1 d . . . C(16) C 0.1894(4) 0.5710(2) 0.0884(2) 0.0483(11) Uani 1.00 1 d . . . C(17) C 0.2755(3) 0.5202(2) 0.1007(2) 0.0458(11) Uani 1.00 1 d . . . C(18) C 0.2641(3) 0.4343(2) 0.1140(2) 0.0370(9) Uani 1.00 1 d . . . C(19) C 0.1649(3) 0.3968(2) 0.1171(2) 0.0285(7) Uani 1.00 1 d . . . C(20) C 0.4441(3) 0.4129(4) 0.1362(4) 0.0763(18) Uani 1.00 1 d . . . C(21) C -0.1765(2) 0.1724(2) 0.1568(2) 0.0334(8) Uani 1.00 1 d . . . C(22) C -0.1120(2) 0.1213(2) 0.0270(2) 0.0281(7) Uani 1.00 1 d . . . C(23) C -0.0390(2) 0.1072(2) -0.0390(2) 0.0265(7) Uani 1.00 1 d . . . C(24) C -0.0617(3) 0.0422(2) -0.0983(2) 0.0319(8) Uani 1.00 1 d . . . C(25) C 0.0069(3) 0.0237(2) -0.1603(2) 0.0345(8) Uani 1.00 1 d . . . C(26) C 0.0995(3) 0.0679(2) -0.1643(2) 0.0321(8) Uani 1.00 1 d . . . C(27) C 0.1226(2) 0.1315(2) -0.1068(2) 0.0278(7) Uani 1.00 1 d . . . C(28) C 0.0512(2) 0.1544(2) -0.0441(2) 0.0248(7) Uani 1.00 1 d . . . C(29) C 0.2805(3) 0.1657(3) -0.1720(2) 0.0418(10) Uani 1.00 1 d . . . H(1) H -0.2710 0.3099 0.2887 0.058 Uiso 1.00 1 c R . . H(2) H -0.3065 0.2181 0.2577 0.058 Uiso 1.00 1 c R . . H(3) H -0.3295 0.2979 0.1979 0.058 Uiso 1.00 1 c R . . H(4) H -0.0791 0.3277 0.2802 0.039 Uiso 1.00 1 c R . . H(5) H -0.1161 0.2409 0.3207 0.039 Uiso 1.00 1 c R . . H(6) H 0.0327 0.1960 0.3605 0.036 Uiso 1.00 1 c R . . H(7) H 0.1724 0.1291 0.4289 0.047 Uiso 1.00 1 c R . . H(8) H 0.3206 0.0496 0.4254 0.065 Uiso 1.00 1 c R . . H(9) H 0.3913 0.0158 0.2936 0.066 Uiso 1.00 1 c R . . H(10) H 0.4095 -0.0246 0.0862 0.100 Uiso 1.00 1 c R . . H(11) H 0.4254 -0.0189 0.1878 0.100 Uiso 1.00 1 c R . . H(12) H 0.4716 0.0526 0.1286 0.100 Uiso 1.00 1 c R . . H(13) H -0.1985 0.3104 0.0755 0.044 Uiso 1.00 1 c R . . H(14) H -0.1960 0.3812 0.1484 0.044 Uiso 1.00 1 c R . . H(15) H -0.0776 0.4613 0.1099 0.038 Uiso 1.00 1 c R . . H(16) H 0.0355 0.5722 0.0825 0.050 Uiso 1.00 1 c R . . H(17) H 0.1973 0.6296 0.0785 0.058 Uiso 1.00 1 c R . . H(18) H 0.3422 0.5443 0.1000 0.055 Uiso 1.00 1 c R . . H(19) H 0.4740 0.3957 0.1918 0.092 Uiso 1.00 1 c R . . H(20) H 0.4402 0.4744 0.1337 0.092 Uiso 1.00 1 c R . . H(21) H 0.4871 0.3923 0.0908 0.092 Uiso 1.00 1 c R . . H(22) H -0.1658 0.1293 0.2019 0.040 Uiso 1.00 1 c R . . H(23) H -0.2438 0.1615 0.1274 0.040 Uiso 1.00 1 c R . . H(24) H -0.1779 0.0961 0.0196 0.034 Uiso 1.00 1 c R . . H(25) H -0.1239 0.0114 -0.0954 0.038 Uiso 1.00 1 c R . . H(26) H -0.0089 -0.0194 -0.2007 0.041 Uiso 1.00 1 c R . . H(27) H 0.1466 0.0540 -0.2068 0.039 Uiso 1.00 1 c R . . H(28) H 0.2924 0.2196 -0.2005 0.050 Uiso 1.00 1 c R . . H(29) H 0.2510 0.1254 -0.2135 0.050 Uiso 1.00 1 c R . . H(30) H 0.3458 0.1438 -0.1482 0.050 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0232(2) 0.0259(2) 0.0225(2) -0.0009(2) 0.0020(2) -0.0011(2) K(1) 0.0266(4) 0.0436(5) 0.0373(4) -0.0024(3) 0.0055(3) -0.0030(3) P(1) 0.0358(7) 0.1428(18) 0.0718(10) 0.0044(9) -0.0040(7) -0.0164(11) F(1) 0.059(2) 0.085(2) 0.078(2) -0.0091(17) 0.0122(16) 0.0120(18) F(2) 0.069(2) 0.099(2) 0.102(2) 0.014(2) 0.006(2) -0.021(2) F(3) 0.169(4) 0.127(3) 0.074(2) 0.019(3) -0.040(2) -0.011(2) F(4) 0.070(3) 0.296(8) 0.208(6) 0.085(4) -0.057(3) -0.078(6) F(5) 0.072(3) 0.197(6) 0.415(12) -0.071(4) -0.024(5) 0.018(7) F(6) 0.115(4) 0.273(7) 0.088(3) 0.025(4) 0.056(3) 0.002(4) O(1) 0.0301(13) 0.0286(12) 0.0244(12) 0.0009(10) -0.0000(10) -0.0010(10) O(2) 0.0335(14) 0.0278(13) 0.0338(14) 0.0023(11) -0.0002(11) -0.0033(11) O(3) 0.0286(13) 0.0283(13) 0.0244(12) -0.0042(10) 0.0012(10) -0.0016(10) O(4) 0.052(2) 0.064(2) 0.0486(18) 0.0272(17) 0.0143(15) 0.0082(16) O(5) 0.0321(15) 0.0537(19) 0.0579(19) -0.0070(14) -0.0007(14) -0.0081(15) O(6) 0.0282(13) 0.0468(16) 0.0274(13) -0.0021(12) 0.0046(10) -0.0040(12) N(1) 0.0281(15) 0.0259(15) 0.0250(15) -0.0011(12) 0.0050(12) -0.0040(12) N(2) 0.0314(17) 0.0345(17) 0.0276(16) 0.0007(14) 0.0022(13) -0.0007(13) N(3) 0.0266(15) 0.0318(16) 0.0260(15) 0.0013(13) 0.0034(12) -0.0018(13) C(1) 0.035(2) 0.059(2) 0.050(2) 0.004(2) 0.013(2) -0.007(2) C(2) 0.0279(19) 0.038(2) 0.035(2) 0.0019(16) 0.0060(16) -0.0023(17) C(3) 0.035(2) 0.036(2) 0.0284(19) 0.0042(17) 0.0070(16) -0.0032(16) C(4) 0.036(2) 0.0282(18) 0.0249(18) -0.0086(16) 0.0036(15) -0.0004(15) C(5) 0.0319(19) 0.0273(18) 0.0299(19) -0.0033(15) -0.0024(15) 0.0029(15) C(6) 0.043(2) 0.044(2) 0.030(2) -0.0045(19) -0.0037(17) 0.0059(18) C(7) 0.047(2) 0.069(3) 0.045(2) 0.009(2) -0.012(2) 0.019(2) C(8) 0.043(2) 0.067(3) 0.055(2) 0.017(2) -0.001(2) 0.016(2) C(9) 0.040(2) 0.042(2) 0.039(2) 0.0053(19) 0.0031(18) 0.0058(19) C(10) 0.0315(19) 0.0276(18) 0.0300(19) -0.0025(15) -0.0018(15) 0.0014(15) C(11) 0.076(4) 0.103(4) 0.074(3) 0.056(3) 0.033(3) 0.024(3) C(12) 0.028(2) 0.038(2) 0.045(2) 0.0096(17) 0.0035(17) 0.0022(18) C(13) 0.038(2) 0.0299(19) 0.0273(19) 0.0070(17) -0.0017(16) 0.0024(16) C(14) 0.043(2) 0.0283(18) 0.0243(18) -0.0042(17) 0.0042(16) -0.0009(15) C(15) 0.061(2) 0.030(2) 0.035(2) 0.001(2) 0.006(2) -0.0010(17) C(16) 0.072(3) 0.031(2) 0.043(2) -0.009(2) 0.010(2) -0.0008(19) C(17) 0.054(2) 0.044(2) 0.041(2) -0.022(2) 0.009(2) -0.007(2) C(18) 0.039(2) 0.040(2) 0.032(2) -0.0072(18) 0.0042(17) -0.0116(17) C(19) 0.041(2) 0.0272(18) 0.0176(16) -0.0005(16) 0.0011(14) -0.0033(14) C(20) 0.038(2) 0.084(4) 0.106(5) -0.023(2) -0.004(3) -0.026(3) C(21) 0.0251(18) 0.043(2) 0.033(2) -0.0038(16) 0.0069(15) -0.0030(17) C(22) 0.0271(18) 0.0271(18) 0.0298(19) -0.0024(15) -0.0034(15) 0.0029(15) C(23) 0.0336(19) 0.0241(17) 0.0216(17) 0.0002(15) -0.0016(14) 0.0015(14) C(24) 0.039(2) 0.0263(18) 0.0298(19) -0.0045(16) -0.0030(16) 0.0017(15) C(25) 0.048(2) 0.0253(18) 0.030(2) 0.0007(17) -0.0022(17) -0.0022(15) C(26) 0.041(2) 0.0312(19) 0.0247(18) 0.0033(17) 0.0031(16) -0.0004(15) C(27) 0.0297(18) 0.0282(17) 0.0253(17) 0.0008(15) -0.0014(14) 0.0032(15) C(28) 0.0306(18) 0.0247(17) 0.0188(15) 0.0020(14) -0.0027(13) 0.0039(13) C(29) 0.033(2) 0.062(2) 0.031(2) 0.001(2) 0.0045(17) -0.003(2) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mn(1) K(1) 3.5353(10) yes . . Mn(1) O(1) 1.994(2) yes . . Mn(1) O(2) 2.019(2) yes . . Mn(1) O(3) 1.893(2) yes . . Mn(1) N(1) 2.019(3) yes . . Mn(1) N(2) 2.162(3) yes . . Mn(1) N(3) 2.106(3) yes . . K(1) P(1) 3.5621(18) yes . . K(1) F(1) 2.742(3) yes . . K(1) F(2) 2.864(4) yes . . K(1) F(3) 3.050(6) yes . . K(1) O(1) 2.757(2) yes . . K(1) O(2) 2.727(2) yes . . K(1) O(3) 3.007(2) yes . . K(1) O(4) 2.866(3) yes . . K(1) O(5) 2.840(3) yes . . K(1) O(6) 2.749(2) yes . . P(1) F(1) 1.581(3) yes . . P(1) F(2) 1.643(4) yes . . P(1) F(3) 1.609(4) yes . . P(1) F(4) 1.572(7) yes . . P(1) F(5) 1.521(7) yes . . P(1) F(6) 1.548(5) yes . . O(1) C(10) 1.304(4) yes . . O(2) C(19) 1.310(4) yes . . O(3) C(28) 1.330(4) yes . . O(4) C(9) 1.373(5) yes . . O(4) C(11) 1.437(7) yes . . O(5) C(18) 1.369(5) yes . . O(5) C(20) 1.425(6) yes . . O(6) C(27) 1.363(4) yes . . O(6) C(29) 1.433(5) yes . . N(1) C(3) 1.482(5) yes . . N(1) C(4) 1.294(4) yes . . N(2) C(12) 1.475(5) yes . . N(2) C(13) 1.283(5) yes . . N(3) C(21) 1.477(5) yes . . N(3) C(22) 1.290(4) yes . . C(1) C(2) 1.530(6) yes . . C(2) C(3) 1.538(5) yes . . C(2) C(12) 1.531(5) yes . . C(2) C(21) 1.533(5) yes . . C(4) C(5) 1.433(5) yes . . C(5) C(6) 1.418(5) yes . . C(5) C(10) 1.406(5) yes . . C(6) C(7) 1.361(6) yes . . C(7) C(8) 1.412(7) yes . . C(8) C(9) 1.375(6) yes . . C(9) C(10) 1.423(5) yes . . C(13) C(14) 1.443(5) yes . . C(14) C(15) 1.419(5) yes . . C(14) C(19) 1.404(5) yes . . C(15) C(16) 1.362(7) yes . . C(16) C(17) 1.389(6) yes . . C(17) C(18) 1.390(6) yes . . C(18) C(19) 1.426(5) yes . . C(22) C(23) 1.449(5) yes . . C(23) C(24) 1.413(5) yes . . C(23) C(28) 1.400(5) yes . . C(24) C(25) 1.378(5) yes . . C(25) C(26) 1.400(5) yes . . C(26) C(27) 1.380(5) yes . . C(27) C(28) 1.427(5) yes . . C(1) H(1) 0.980 no . . C(1) H(2) 0.980 no . . C(1) H(3) 0.980 no . . C(3) H(4) 0.990 no . . C(3) H(5) 0.990 no . . C(4) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(11) H(10) 0.980 no . . C(11) H(11) 0.980 no . . C(11) H(12) 0.980 no . . C(12) H(13) 0.990 no . . C(12) H(14) 0.990 no . . C(13) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(17) H(18) 0.950 no . . C(20) H(19) 0.980 no . . C(20) H(20) 0.980 no . . C(20) H(21) 0.980 no . . C(21) H(22) 0.990 no . . C(21) H(23) 0.990 no . . C(22) H(24) 0.950 no . . C(24) H(25) 0.950 no . . C(25) H(26) 0.950 no . . C(26) H(27) 0.950 no . . C(29) H(28) 0.980 no . . C(29) H(29) 0.980 no . . C(29) H(30) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 K(1) Mn(1) O(1) 51.00(7) yes . . . K(1) Mn(1) O(2) 50.19(7) yes . . . K(1) Mn(1) O(3) 58.28(7) yes . . . K(1) Mn(1) N(1) 123.76(8) yes . . . K(1) Mn(1) N(2) 126.54(9) yes . . . K(1) Mn(1) N(3) 135.41(8) yes . . . O(1) Mn(1) O(2) 86.62(10) yes . . . O(1) Mn(1) O(3) 88.06(10) yes . . . O(1) Mn(1) N(1) 88.38(11) yes . . . O(1) Mn(1) N(2) 167.52(11) yes . . . O(1) Mn(1) N(3) 104.59(11) yes . . . O(2) Mn(1) O(3) 88.37(10) yes . . . O(2) Mn(1) N(1) 98.50(11) yes . . . O(2) Mn(1) N(2) 84.48(11) yes . . . O(2) Mn(1) N(3) 168.23(11) yes . . . O(3) Mn(1) N(1) 172.06(11) yes . . . O(3) Mn(1) N(2) 100.39(11) yes . . . O(3) Mn(1) N(3) 88.45(11) yes . . . N(1) Mn(1) N(2) 84.32(12) yes . . . N(1) Mn(1) N(3) 85.59(11) yes . . . N(2) Mn(1) N(3) 84.95(12) yes . . . Mn(1) K(1) P(1) 174.81(4) yes . . . Mn(1) K(1) F(1) 149.83(8) yes . . . Mn(1) K(1) F(2) 156.38(8) yes . . . Mn(1) K(1) F(3) 155.20(8) yes . . . Mn(1) K(1) O(1) 34.20(5) yes . . . Mn(1) K(1) O(2) 34.68(5) yes . . . Mn(1) K(1) O(3) 32.37(4) yes . . . Mn(1) K(1) O(4) 89.39(7) yes . . . Mn(1) K(1) O(5) 90.36(6) yes . . . Mn(1) K(1) O(6) 85.71(5) yes . . . P(1) K(1) F(1) 24.98(8) yes . . . P(1) K(1) F(2) 26.93(9) yes . . . P(1) K(1) F(3) 26.77(8) yes . . . P(1) K(1) O(1) 150.98(7) yes . . . P(1) K(1) O(2) 141.86(7) yes . . . P(1) K(1) O(3) 145.33(6) yes . . . P(1) K(1) O(4) 95.80(8) yes . . . P(1) K(1) O(5) 86.50(7) yes . . . P(1) K(1) O(6) 93.14(6) yes . . . F(1) K(1) F(2) 47.13(11) yes . . . F(1) K(1) F(3) 44.17(11) yes . . . F(1) K(1) O(1) 175.76(9) yes . . . F(1) K(1) O(2) 122.44(9) yes . . . F(1) K(1) O(3) 128.30(9) yes . . . F(1) K(1) O(4) 120.78(10) yes . . . F(1) K(1) O(5) 72.58(10) yes . . . F(1) K(1) O(6) 86.71(9) yes . . . F(2) K(1) F(3) 43.18(11) yes . . . F(2) K(1) O(1) 129.87(10) yes . . . F(2) K(1) O(2) 168.79(10) yes . . . F(2) K(1) O(3) 131.30(9) yes . . . F(2) K(1) O(4) 77.96(11) yes . . . F(2) K(1) O(5) 113.25(10) yes . . . F(2) K(1) O(6) 78.47(9) yes . . . F(3) K(1) O(1) 131.75(10) yes . . . F(3) K(1) O(2) 127.90(11) yes . . . F(3) K(1) O(3) 171.98(10) yes . . . F(3) K(1) O(4) 82.57(11) yes . . . F(3) K(1) O(5) 75.56(11) yes . . . F(3) K(1) O(6) 119.00(10) yes . . . O(1) K(1) O(2) 60.26(7) yes . . . O(1) K(1) O(3) 55.71(7) yes . . . O(1) K(1) O(4) 55.21(8) yes . . . O(1) K(1) O(5) 108.30(8) yes . . . O(1) K(1) O(6) 95.62(7) yes . . . O(2) K(1) O(3) 56.57(7) yes . . . O(2) K(1) O(4) 109.47(9) yes . . . O(2) K(1) O(5) 55.70(8) yes . . . O(2) K(1) O(6) 106.85(8) yes . . . O(3) K(1) O(4) 102.50(8) yes . . . O(3) K(1) O(5) 105.83(8) yes . . . O(3) K(1) O(6) 53.93(7) yes . . . O(4) K(1) O(5) 125.12(10) yes . . . O(4) K(1) O(6) 104.69(9) yes . . . O(5) K(1) O(6) 130.00(9) yes . . . K(1) P(1) F(1) 47.09(13) yes . . . K(1) P(1) F(2) 52.12(14) yes . . . K(1) P(1) F(3) 58.6(2) yes . . . K(1) P(1) F(4) 128.5(2) yes . . . K(1) P(1) F(5) 124.9(3) yes . . . K(1) P(1) F(6) 114.5(2) yes . . . F(1) P(1) F(2) 88.2(2) yes . . . F(1) P(1) F(3) 87.0(2) yes . . . F(1) P(1) F(4) 175.6(3) yes . . . F(1) P(1) F(5) 91.0(3) yes . . . F(1) P(1) F(6) 93.2(2) yes . . . F(2) P(1) F(3) 84.3(2) yes . . . F(2) P(1) F(4) 88.7(3) yes . . . F(2) P(1) F(5) 175.8(4) yes . . . F(2) P(1) F(6) 85.1(3) yes . . . F(3) P(1) F(4) 89.6(3) yes . . . F(3) P(1) F(5) 91.6(4) yes . . . F(3) P(1) F(6) 169.4(3) yes . . . F(4) P(1) F(5) 91.9(3) yes . . . F(4) P(1) F(6) 89.7(3) yes . . . F(5) P(1) F(6) 99.0(4) yes . . . K(1) F(1) P(1) 107.94(18) yes . . . K(1) F(2) P(1) 100.95(19) yes . . . K(1) F(3) P(1) 94.6(2) yes . . . Mn(1) O(1) K(1) 94.80(9) yes . . . Mn(1) O(1) C(10) 128.6(2) yes . . . K(1) O(1) C(10) 106.8(2) yes . . . Mn(1) O(2) K(1) 95.13(9) yes . . . Mn(1) O(2) C(19) 132.3(2) yes . . . K(1) O(2) C(19) 115.3(2) yes . . . Mn(1) O(3) K(1) 89.35(9) yes . . . Mn(1) O(3) C(28) 124.9(2) yes . . . K(1) O(3) C(28) 108.0(2) yes . . . K(1) O(4) C(9) 104.8(2) yes . . . K(1) O(4) C(11) 120.1(3) yes . . . C(9) O(4) C(11) 117.2(3) yes . . . K(1) O(5) C(18) 112.5(2) yes . . . K(1) O(5) C(20) 124.7(3) yes . . . C(18) O(5) C(20) 117.0(3) yes . . . K(1) O(6) C(27) 117.8(2) yes . . . K(1) O(6) C(29) 116.1(2) yes . . . C(27) O(6) C(29) 117.9(3) yes . . . Mn(1) N(1) C(3) 117.9(2) yes . . . Mn(1) N(1) C(4) 125.6(2) yes . . . C(3) N(1) C(4) 116.5(3) yes . . . Mn(1) N(2) C(12) 115.9(2) yes . . . Mn(1) N(2) C(13) 127.2(2) yes . . . C(12) N(2) C(13) 116.6(3) yes . . . Mn(1) N(3) C(21) 118.1(2) yes . . . Mn(1) N(3) C(22) 123.8(2) yes . . . C(21) N(3) C(22) 118.1(3) yes . . . C(1) C(2) C(3) 107.7(3) yes . . . C(1) C(2) C(12) 109.3(3) yes . . . C(1) C(2) C(21) 108.4(3) yes . . . C(3) C(2) C(12) 110.2(3) yes . . . C(3) C(2) C(21) 110.6(3) yes . . . C(12) C(2) C(21) 110.5(3) yes . . . N(1) C(3) C(2) 112.7(3) yes . . . N(1) C(4) C(5) 127.9(3) yes . . . C(4) C(5) C(6) 117.5(3) yes . . . C(4) C(5) C(10) 121.7(3) yes . . . C(6) C(5) C(10) 120.8(3) yes . . . C(5) C(6) C(7) 120.1(4) yes . . . C(6) C(7) C(8) 120.0(4) yes . . . C(7) C(8) C(9) 120.7(4) yes . . . O(4) C(9) C(8) 125.0(4) yes . . . O(4) C(9) C(10) 114.3(3) yes . . . C(8) C(9) C(10) 120.7(4) yes . . . O(1) C(10) C(5) 124.2(3) yes . . . O(1) C(10) C(9) 118.2(3) yes . . . C(5) C(10) C(9) 117.7(3) yes . . . N(2) C(12) C(2) 110.5(3) yes . . . N(2) C(13) C(14) 126.3(3) yes . . . C(13) C(14) C(15) 117.5(3) yes . . . C(13) C(14) C(19) 122.9(3) yes . . . C(15) C(14) C(19) 119.5(3) yes . . . C(14) C(15) C(16) 121.6(4) yes . . . C(15) C(16) C(17) 120.0(4) yes . . . C(16) C(17) C(18) 120.1(4) yes . . . O(5) C(18) C(17) 124.9(4) yes . . . O(5) C(18) C(19) 114.0(3) yes . . . C(17) C(18) C(19) 121.1(3) yes . . . O(2) C(19) C(14) 124.1(3) yes . . . O(2) C(19) C(18) 118.1(3) yes . . . C(14) C(19) C(18) 117.7(3) yes . . . N(3) C(21) C(2) 110.9(3) yes . . . N(3) C(22) C(23) 124.9(3) yes . . . C(22) C(23) C(24) 117.2(3) yes . . . C(22) C(23) C(28) 122.2(3) yes . . . C(24) C(23) C(28) 120.6(3) yes . . . C(23) C(24) C(25) 119.7(3) yes . . . C(24) C(25) C(26) 120.5(3) yes . . . C(25) C(26) C(27) 120.3(3) yes . . . O(6) C(27) C(26) 125.0(3) yes . . . O(6) C(27) C(28) 114.6(3) yes . . . C(26) C(27) C(28) 120.4(3) yes . . . O(3) C(28) C(23) 123.8(3) yes . . . O(3) C(28) C(27) 117.8(3) yes . . . C(23) C(28) C(27) 118.3(3) yes . . . C(2) C(1) H(1) 109.5 no . . . C(2) C(1) H(2) 109.5 no . . . C(2) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . N(1) C(3) H(4) 109.1 no . . . N(1) C(3) H(5) 109.1 no . . . C(2) C(3) H(4) 109.1 no . . . C(2) C(3) H(5) 109.1 no . . . H(4) C(3) H(5) 107.8 no . . . N(1) C(4) H(6) 116.0 no . . . C(5) C(4) H(6) 116.1 no . . . C(5) C(6) H(7) 119.9 no . . . C(7) C(6) H(7) 119.9 no . . . C(6) C(7) H(8) 120.0 no . . . C(8) C(7) H(8) 120.0 no . . . C(7) C(8) H(9) 119.7 no . . . C(9) C(8) H(9) 119.7 no . . . O(4) C(11) H(10) 109.5 no . . . O(4) C(11) H(11) 109.5 no . . . O(4) C(11) H(12) 109.5 no . . . H(10) C(11) H(11) 109.5 no . . . H(10) C(11) H(12) 109.5 no . . . H(11) C(11) H(12) 109.5 no . . . N(2) C(12) H(13) 109.5 no . . . N(2) C(12) H(14) 109.5 no . . . C(2) C(12) H(13) 109.5 no . . . C(2) C(12) H(14) 109.5 no . . . H(13) C(12) H(14) 108.1 no . . . N(2) C(13) H(15) 116.8 no . . . C(14) C(13) H(15) 116.8 no . . . C(14) C(15) H(16) 119.2 no . . . C(16) C(15) H(16) 119.2 no . . . C(15) C(16) H(17) 120.0 no . . . C(17) C(16) H(17) 120.0 no . . . C(16) C(17) H(18) 119.9 no . . . C(18) C(17) H(18) 120.0 no . . . O(5) C(20) H(19) 109.5 no . . . O(5) C(20) H(20) 109.5 no . . . O(5) C(20) H(21) 109.5 no . . . H(19) C(20) H(20) 109.5 no . . . H(19) C(20) H(21) 109.5 no . . . H(20) C(20) H(21) 109.5 no . . . N(3) C(21) H(22) 109.5 no . . . N(3) C(21) H(23) 109.5 no . . . C(2) C(21) H(22) 109.5 no . . . C(2) C(21) H(23) 109.5 no . . . H(22) C(21) H(23) 108.0 no . . . N(3) C(22) H(24) 117.5 no . . . C(23) C(22) H(24) 117.5 no . . . C(23) C(24) H(25) 120.1 no . . . C(25) C(24) H(25) 120.1 no . . . C(24) C(25) H(26) 119.7 no . . . C(26) C(25) H(26) 119.7 no . . . C(25) C(26) H(27) 119.8 no . . . C(27) C(26) H(27) 119.8 no . . . O(6) C(29) H(28) 109.5 no . . . O(6) C(29) H(29) 109.5 no . . . O(6) C(29) H(30) 109.5 no . . . H(28) C(29) H(29) 109.5 no . . . H(28) C(29) H(30) 109.5 no . . . H(29) C(29) H(30) 109.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F(1) C(7) 3.478(6) ? . 4_554 F(2) C(11) 3.403(7) ? . 3_655 F(3) C(1) 3.578(6) ? . 1_655 F(4) C(11) 3.385(10) ? . 3_655 F(4) C(21) 3.499(7) ? . 1_655 F(4) C(22) 3.314(6) ? . 1_655 F(5) C(12) 3.516(8) ? . 1_655 F(5) C(16) 3.444(8) ? . 3_665 F(5) C(17) 3.493(9) ? . 3_665 F(6) C(1) 3.102(7) ? . 4_654 F(6) C(11) 3.587(10) ? . 3_655 O(1) C(24) 3.234(4) ? . 3_555 O(1) C(25) 3.349(4) ? . 3_555 O(2) C(29) 3.400(4) ? . 4_555 O(3) C(4) 3.414(4) ? . 4_554 O(5) C(29) 3.388(5) ? . 4_555 O(6) C(4) 3.179(4) ? . 4_554 O(6) C(5) 3.305(4) ? . 4_554 O(6) C(6) 3.305(5) ? . 4_554 N(1) C(27) 3.548(4) ? . 4_555 N(3) C(25) 3.361(4) ? . 3_555 C(1) F(3) 3.578(6) ? . 1_455 C(1) F(6) 3.102(7) ? . 4_455 C(4) O(3) 3.414(4) ? . 4_555 C(4) O(6) 3.179(4) ? . 4_555 C(4) C(15) 3.583(5) ? . 2_545 C(4) C(27) 3.244(5) ? . 4_555 C(4) C(28) 3.421(5) ? . 4_555 C(5) O(6) 3.305(4) ? . 4_555 C(5) C(29) 3.499(6) ? . 4_555 C(6) O(6) 3.305(5) ? . 4_555 C(7) F(1) 3.478(6) ? . 4_555 C(10) C(25) 3.566(5) ? . 3_555 C(11) F(2) 3.403(7) ? . 3_655 C(11) F(4) 3.385(10) ? . 3_655 C(11) F(6) 3.587(10) ? . 3_655 C(12) F(5) 3.516(8) ? . 1_455 C(13) C(15) 3.313(5) ? . 3_565 C(15) C(4) 3.583(5) ? . 2_555 C(15) C(13) 3.313(5) ? . 3_565 C(16) F(5) 3.444(8) ? . 3_665 C(17) F(5) 3.493(9) ? . 3_665 C(21) F(4) 3.499(7) ? . 1_455 C(22) F(4) 3.314(6) ? . 1_455 C(22) C(24) 3.596(5) ? . 3_555 C(22) C(25) 3.367(5) ? . 3_555 C(23) C(24) 3.431(5) ? . 3_555 C(24) O(1) 3.234(4) ? . 3_555 C(24) C(22) 3.596(5) ? . 3_555 C(24) C(23) 3.431(5) ? . 3_555 C(25) O(1) 3.349(4) ? . 3_555 C(25) N(3) 3.361(4) ? . 3_555 C(25) C(10) 3.566(5) ? . 3_555 C(25) C(22) 3.367(5) ? . 3_555 C(27) N(1) 3.548(4) ? . 4_554 C(27) C(4) 3.244(5) ? . 4_554 C(28) C(4) 3.421(5) ? . 4_554 C(29) O(2) 3.400(4) ? . 4_554 C(29) O(5) 3.388(5) ? . 4_554 C(29) C(5) 3.499(6) ? . 4_554 K(1) H(7) 3.471 ? . 4_554 P(1) H(10) 3.333 ? . 3_655 F(1) H(8) 3.219 ? . 4_554 F(2) H(10) 2.655 ? . 3_655 F(2) H(11) 3.505 ? . 3_655 F(2) H(12) 3.593 ? . 3_655 F(3) H(2) 3.487 ? . 1_655 F(3) H(3) 2.865 ? . 1_655 F(3) H(23) 3.151 ? . 1_655 F(4) H(1) 3.434 ? . 4_654 F(4) H(10) 2.471 ? . 3_655 F(4) H(13) 3.475 ? . 1_655 F(4) H(23) 2.602 ? . 1_655 F(4) H(24) 2.589 ? . 1_655 F(5) H(3) 3.348 ? . 1_655 F(5) H(13) 2.645 ? . 1_655 F(5) H(17) 2.815 ? . 3_665 F(5) H(18) 2.918 ? . 3_665 F(5) H(23) 3.467 ? . 1_655 F(6) H(1) 2.704 ? . 4_654 F(6) H(2) 2.870 ? . 4_654 F(6) H(3) 3.233 ? . 4_654 F(6) H(10) 3.036 ? . 3_655 F(6) H(11) 3.220 ? . 3_655 F(6) H(19) 3.493 ? . 4_554 O(1) H(25) 2.600 ? . 3_555 O(1) H(26) 2.835 ? . 3_555 O(2) H(7) 3.326 ? . 4_554 O(2) H(27) 3.262 ? . 4_555 O(2) H(28) 3.130 ? . 4_555 O(2) H(29) 2.806 ? . 4_555 O(3) H(6) 2.632 ? . 4_554 O(3) H(7) 2.968 ? . 4_554 O(4) H(25) 2.862 ? . 3_555 O(5) H(8) 3.338 ? . 4_554 O(5) H(28) 3.237 ? . 4_555 O(5) H(29) 2.845 ? . 4_555 O(5) H(30) 3.570 ? . 4_555 O(6) H(6) 3.097 ? . 4_554 O(6) H(7) 3.155 ? . 4_554 N(1) H(26) 3.367 ? . 3_555 N(2) H(16) 3.411 ? . 3_565 N(2) H(17) 3.544 ? . 3_565 N(3) H(26) 3.126 ? . 3_555 C(3) H(17) 3.567 ? . 2_545 C(4) H(16) 2.883 ? . 2_545 C(4) H(26) 3.223 ? . 3_555 C(4) H(28) 3.372 ? . 4_555 C(5) H(15) 3.377 ? . 2_545 C(5) H(16) 3.317 ? . 2_545 C(5) H(26) 3.068 ? . 3_555 C(5) H(28) 2.857 ? . 4_555 C(6) H(15) 2.934 ? . 2_545 C(6) H(16) 3.240 ? . 2_545 C(6) H(28) 3.142 ? . 4_555 C(7) H(14) 3.222 ? . 2_545 C(7) H(15) 3.245 ? . 2_545 C(7) H(28) 3.563 ? . 4_555 C(8) H(14) 3.321 ? . 2_545 C(8) H(19) 3.520 ? . 2_645 C(8) H(20) 3.366 ? . 2_645 C(9) H(25) 3.112 ? . 3_555 C(9) H(28) 3.496 ? . 4_555 C(10) H(25) 2.988 ? . 3_555 C(10) H(26) 2.890 ? . 3_555 C(10) H(28) 3.081 ? . 4_555 C(11) H(19) 3.562 ? . 2_645 C(12) H(17) 3.347 ? . 3_565 C(13) H(16) 3.024 ? . 3_565 C(13) H(26) 3.358 ? . 4_555 C(13) H(27) 3.592 ? . 4_555 C(14) H(7) 3.298 ? . 4_554 C(14) H(16) 3.255 ? . 3_565 C(14) H(26) 3.486 ? . 4_555 C(14) H(27) 3.055 ? . 4_555 C(15) H(5) 3.537 ? . 2_555 C(15) H(6) 3.131 ? . 2_555 C(15) H(15) 3.142 ? . 3_565 C(15) H(16) 3.583 ? . 3_565 C(15) H(26) 3.594 ? . 4_555 C(15) H(27) 3.533 ? . 4_555 C(16) H(5) 3.215 ? . 2_555 C(16) H(13) 3.192 ? . 3_565 C(16) H(15) 3.421 ? . 3_565 C(16) H(22) 3.441 ? . 2_555 C(17) H(8) 3.043 ? . 4_554 C(18) H(7) 3.255 ? . 4_554 C(18) H(8) 3.086 ? . 4_554 C(18) H(27) 3.257 ? . 4_555 C(18) H(29) 2.878 ? . 4_555 C(19) H(7) 2.985 ? . 4_554 C(19) H(27) 2.888 ? . 4_555 C(19) H(29) 2.865 ? . 4_555 C(20) H(3) 3.571 ? . 1_655 C(20) H(9) 2.881 ? . 2_655 C(20) H(11) 3.364 ? . 2_655 C(20) H(29) 3.566 ? . 4_555 C(21) H(26) 3.476 ? . 3_555 C(22) H(26) 3.492 ? . 3_555 C(23) H(4) 3.044 ? . 4_554 C(23) H(5) 3.391 ? . 4_554 C(23) H(25) 3.486 ? . 3_555 C(24) H(4) 2.814 ? . 4_554 C(25) H(4) 2.760 ? . 4_554 C(25) H(22) 3.276 ? . 3_555 C(26) H(4) 2.960 ? . 4_554 C(26) H(22) 3.310 ? . 3_555 C(26) H(24) 3.579 ? . 3_555 C(27) H(4) 3.178 ? . 4_554 C(27) H(6) 3.015 ? . 4_554 C(28) H(4) 3.192 ? . 4_554 C(28) H(5) 3.413 ? . 4_554 C(28) H(6) 2.813 ? . 4_554 C(28) H(25) 3.530 ? . 3_555 C(29) H(19) 3.506 ? . 4_554 H(1) F(4) 3.434 ? . 4_455 H(1) F(6) 2.704 ? . 4_455 H(1) H(11) 3.411 ? . 2_555 H(2) F(3) 3.487 ? . 1_455 H(2) F(6) 2.870 ? . 4_455 H(2) H(17) 3.210 ? . 2_545 H(2) H(18) 3.592 ? . 2_545 H(3) F(3) 2.865 ? . 1_455 H(3) F(5) 3.348 ? . 1_455 H(3) F(6) 3.233 ? . 4_455 H(3) C(20) 3.571 ? . 1_455 H(3) H(9) 3.557 ? . 2_555 H(3) H(19) 2.993 ? . 1_455 H(3) H(21) 3.235 ? . 1_455 H(4) C(23) 3.044 ? . 4_555 H(4) C(24) 2.814 ? . 4_555 H(4) C(25) 2.760 ? . 4_555 H(4) C(26) 2.960 ? . 4_555 H(4) C(27) 3.178 ? . 4_555 H(4) C(28) 3.192 ? . 4_555 H(4) H(25) 3.282 ? . 4_555 H(4) H(26) 3.191 ? . 4_555 H(4) H(27) 3.489 ? . 4_555 H(5) C(15) 3.537 ? . 2_545 H(5) C(16) 3.215 ? . 2_545 H(5) C(23) 3.391 ? . 4_555 H(5) C(28) 3.413 ? . 4_555 H(5) H(16) 3.235 ? . 2_545 H(5) H(17) 2.622 ? . 2_545 H(6) O(3) 2.632 ? . 4_555 H(6) O(6) 3.097 ? . 4_555 H(6) C(15) 3.131 ? . 2_545 H(6) C(27) 3.015 ? . 4_555 H(6) C(28) 2.813 ? . 4_555 H(6) H(16) 2.349 ? . 2_545 H(6) H(17) 3.352 ? . 2_545 H(7) K(1) 3.471 ? . 4_555 H(7) O(2) 3.326 ? . 4_555 H(7) O(3) 2.968 ? . 4_555 H(7) O(6) 3.155 ? . 4_555 H(7) C(14) 3.298 ? . 4_555 H(7) C(18) 3.255 ? . 4_555 H(7) C(19) 2.985 ? . 4_555 H(7) H(15) 2.990 ? . 2_545 H(7) H(16) 2.854 ? . 2_545 H(7) H(28) 3.548 ? . 4_555 H(8) F(1) 3.219 ? . 4_555 H(8) O(5) 3.338 ? . 4_555 H(8) C(17) 3.043 ? . 4_555 H(8) C(18) 3.086 ? . 4_555 H(8) H(14) 3.315 ? . 2_545 H(8) H(15) 3.487 ? . 2_545 H(8) H(18) 3.120 ? . 4_555 H(8) H(20) 3.496 ? . 2_645 H(8) H(20) 3.584 ? . 4_555 H(8) H(21) 3.555 ? . 2_645 H(8) H(21) 3.443 ? . 4_555 H(9) C(20) 2.881 ? . 2_645 H(9) H(3) 3.557 ? . 2_545 H(9) H(14) 3.473 ? . 2_545 H(9) H(19) 2.597 ? . 2_645 H(9) H(20) 2.521 ? . 2_645 H(9) H(21) 3.069 ? . 2_645 H(10) P(1) 3.333 ? . 3_655 H(10) F(2) 2.655 ? . 3_655 H(10) F(4) 2.471 ? . 3_655 H(10) F(6) 3.036 ? . 3_655 H(10) H(24) 3.573 ? . 3_555 H(11) F(2) 3.505 ? . 3_655 H(11) F(6) 3.220 ? . 3_655 H(11) C(20) 3.364 ? . 2_645 H(11) H(1) 3.411 ? . 2_545 H(11) H(19) 2.633 ? . 2_645 H(11) H(20) 3.246 ? . 2_645 H(12) F(2) 3.593 ? . 3_655 H(13) F(4) 3.475 ? . 1_455 H(13) F(5) 2.645 ? . 1_455 H(13) C(16) 3.192 ? . 3_565 H(13) H(17) 2.597 ? . 3_565 H(14) C(7) 3.222 ? . 2_555 H(14) C(8) 3.321 ? . 2_555 H(14) H(8) 3.315 ? . 2_555 H(14) H(9) 3.473 ? . 2_555 H(14) H(17) 3.562 ? . 3_565 H(15) C(5) 3.377 ? . 2_555 H(15) C(6) 2.934 ? . 2_555 H(15) C(7) 3.245 ? . 2_555 H(15) C(15) 3.142 ? . 3_565 H(15) C(16) 3.421 ? . 3_565 H(15) H(7) 2.990 ? . 2_555 H(15) H(8) 3.487 ? . 2_555 H(15) H(16) 3.133 ? . 3_565 H(15) H(17) 3.591 ? . 3_565 H(15) H(26) 3.204 ? . 4_555 H(16) N(2) 3.411 ? . 3_565 H(16) C(4) 2.883 ? . 2_555 H(16) C(5) 3.317 ? . 2_555 H(16) C(6) 3.240 ? . 2_555 H(16) C(13) 3.024 ? . 3_565 H(16) C(14) 3.255 ? . 3_565 H(16) C(15) 3.583 ? . 3_565 H(16) H(5) 3.235 ? . 2_555 H(16) H(6) 2.349 ? . 2_555 H(16) H(7) 2.854 ? . 2_555 H(16) H(15) 3.133 ? . 3_565 H(16) H(16) 3.553 ? . 3_565 H(16) H(26) 3.570 ? . 4_555 H(17) F(5) 2.815 ? . 3_665 H(17) N(2) 3.544 ? . 3_565 H(17) C(3) 3.567 ? . 2_555 H(17) C(12) 3.347 ? . 3_565 H(17) H(2) 3.210 ? . 2_555 H(17) H(5) 2.622 ? . 2_555 H(17) H(6) 3.352 ? . 2_555 H(17) H(13) 2.597 ? . 3_565 H(17) H(14) 3.562 ? . 3_565 H(17) H(15) 3.591 ? . 3_565 H(17) H(22) 3.482 ? . 2_555 H(18) F(5) 2.918 ? . 3_665 H(18) H(2) 3.592 ? . 2_555 H(18) H(8) 3.120 ? . 4_554 H(19) F(6) 3.493 ? . 4_555 H(19) C(8) 3.520 ? . 2_655 H(19) C(11) 3.562 ? . 2_655 H(19) C(29) 3.506 ? . 4_555 H(19) H(3) 2.993 ? . 1_655 H(19) H(9) 2.597 ? . 2_655 H(19) H(11) 2.633 ? . 2_655 H(19) H(28) 3.481 ? . 4_555 H(19) H(29) 3.332 ? . 4_555 H(19) H(30) 3.132 ? . 4_555 H(20) C(8) 3.366 ? . 2_655 H(20) H(8) 3.496 ? . 2_655 H(20) H(8) 3.584 ? . 4_554 H(20) H(9) 2.521 ? . 2_655 H(20) H(11) 3.246 ? . 2_655 H(21) H(3) 3.235 ? . 1_655 H(21) H(8) 3.555 ? . 2_655 H(21) H(8) 3.443 ? . 4_554 H(21) H(9) 3.069 ? . 2_655 H(22) C(16) 3.441 ? . 2_545 H(22) C(25) 3.276 ? . 3_555 H(22) C(26) 3.310 ? . 3_555 H(22) H(17) 3.482 ? . 2_545 H(22) H(26) 2.870 ? . 3_555 H(22) H(27) 2.925 ? . 3_555 H(23) F(3) 3.151 ? . 1_455 H(23) F(4) 2.602 ? . 1_455 H(23) F(5) 3.467 ? . 1_455 H(24) F(4) 2.589 ? . 1_455 H(24) C(26) 3.579 ? . 3_555 H(24) H(10) 3.573 ? . 3_555 H(25) O(1) 2.600 ? . 3_555 H(25) O(4) 2.862 ? . 3_555 H(25) C(9) 3.112 ? . 3_555 H(25) C(10) 2.988 ? . 3_555 H(25) C(23) 3.486 ? . 3_555 H(25) C(28) 3.530 ? . 3_555 H(25) H(4) 3.282 ? . 4_554 H(26) O(1) 2.835 ? . 3_555 H(26) N(1) 3.367 ? . 3_555 H(26) N(3) 3.126 ? . 3_555 H(26) C(4) 3.223 ? . 3_555 H(26) C(5) 3.068 ? . 3_555 H(26) C(10) 2.890 ? . 3_555 H(26) C(13) 3.358 ? . 4_554 H(26) C(14) 3.486 ? . 4_554 H(26) C(15) 3.594 ? . 4_554 H(26) C(21) 3.476 ? . 3_555 H(26) C(22) 3.492 ? . 3_555 H(26) H(4) 3.191 ? . 4_554 H(26) H(15) 3.204 ? . 4_554 H(26) H(16) 3.570 ? . 4_554 H(26) H(22) 2.870 ? . 3_555 H(27) O(2) 3.262 ? . 4_554 H(27) C(13) 3.592 ? . 4_554 H(27) C(14) 3.055 ? . 4_554 H(27) C(15) 3.533 ? . 4_554 H(27) C(18) 3.257 ? . 4_554 H(27) C(19) 2.888 ? . 4_554 H(27) H(4) 3.489 ? . 4_554 H(27) H(22) 2.925 ? . 3_555 H(28) O(2) 3.130 ? . 4_554 H(28) O(5) 3.237 ? . 4_554 H(28) C(4) 3.372 ? . 4_554 H(28) C(5) 2.857 ? . 4_554 H(28) C(6) 3.142 ? . 4_554 H(28) C(7) 3.563 ? . 4_554 H(28) C(9) 3.496 ? . 4_554 H(28) C(10) 3.081 ? . 4_554 H(28) H(7) 3.548 ? . 4_554 H(28) H(19) 3.481 ? . 4_554 H(29) O(2) 2.806 ? . 4_554 H(29) O(5) 2.845 ? . 4_554 H(29) C(18) 2.878 ? . 4_554 H(29) C(19) 2.865 ? . 4_554 H(29) C(20) 3.566 ? . 4_554 H(29) H(19) 3.332 ? . 4_554 H(30) O(5) 3.570 ? . 4_554 H(30) H(19) 3.132 ? . 4_554 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data__090823 _database_code_depnum_ccdc_archive 'CCDC 812377' #TrackingRef 'NChem_All.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C29 H30 K Mn N4 O9 ' _chemical_formula_moiety 'C29 H30 Mn N3 O6, N O3, K ' _chemical_formula_weight 672.61 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.4584(3) _cell_length_b 15.9260(8) _cell_length_c 16.0765(4) _cell_angle_alpha 90.0000 _cell_angle_beta 94.5337(8) _cell_angle_gamma 90.0000 _cell_volume 2924.56(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 21188 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.0 _cell_measurement_temperature 180.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392.00 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_T_max 0.937 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 180.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 28111 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6704 _reflns_number_gt 5515 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1069 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6704 _refine_ls_number_parameters 398 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0505P)^2^+1.3501P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.47 _refine_diff_density_min -0.47 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; K K 0.200 0.250 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Mn(1) Mn 0.95799(3) 0.224575(19) 0.115923(18) 0.01780(8) Uani 1.00 1 d . . . K(1) K 0.66773(4) 0.20206(3) 0.03429(3) 0.02642(12) Uani 1.00 1 d . . . O(1) O 0.90746(12) 0.21151(9) 0.00128(9) 0.0217(3) Uani 1.00 1 d . . . O(2) O 0.83159(12) 0.30421(9) 0.12474(9) 0.0221(3) Uani 1.00 1 d . . . O(3) O 0.83896(12) 0.13347(9) 0.14292(9) 0.0219(3) Uani 1.00 1 d . . . O(4) O 0.74929(13) 0.17196(11) -0.11973(9) 0.0294(3) Uani 1.00 1 d . . . O(5) O 0.62005(13) 0.36051(10) 0.10197(10) 0.0296(3) Uani 1.00 1 d . . . O(6) O 0.63991(15) 0.05257(12) 0.13352(11) 0.0387(4) Uani 1.00 1 d . . . O(7) O 0.47252(17) 0.25439(17) -0.06489(13) 0.0594(6) Uani 1.00 1 d . . . O(8) O 0.42895(16) 0.16699(14) 0.03065(15) 0.0559(5) Uani 1.00 1 d . . . O(9) O 0.29211(15) 0.23069(13) -0.04483(12) 0.0436(4) Uani 1.00 1 d . . . N(1) N 1.10431(15) 0.15847(11) 0.09774(11) 0.0220(3) Uani 1.00 1 d . . . N(2) N 1.07156(16) 0.33733(12) 0.11593(11) 0.0251(3) Uani 1.00 1 d . . . N(3) N 1.01093(15) 0.22275(11) 0.24118(11) 0.0205(3) Uani 1.00 1 d . . . N(4) N 0.39708(17) 0.21695(13) -0.02727(12) 0.0310(4) Uani 1.00 1 d . . . C(1) C 1.3369(2) 0.25949(18) 0.24639(17) 0.0387(6) Uani 1.00 1 d . . . C(2) C 1.21332(19) 0.25191(15) 0.20257(14) 0.0263(4) Uani 1.00 1 d . . . C(3) C 1.20271(19) 0.16462(15) 0.16284(14) 0.0272(4) Uani 1.00 1 d . . . C(4) C 1.12223(18) 0.11714(13) 0.03102(13) 0.0221(4) Uani 1.00 1 d . . . C(5) C 1.03881(18) 0.10419(13) -0.03980(13) 0.0216(4) Uani 1.00 1 d . . . C(6) C 1.0661(2) 0.04477(14) -0.10075(14) 0.0261(4) Uani 1.00 1 d . . . C(7) C 0.9884(2) 0.02890(14) -0.16840(14) 0.0284(4) Uani 1.00 1 d . . . C(8) C 0.8809(2) 0.07070(14) -0.17706(13) 0.0269(4) Uani 1.00 1 d . . . C(9) C 0.85327(18) 0.12919(13) -0.11821(13) 0.0220(4) Uani 1.00 1 d . . . C(10) C 0.93341(18) 0.14940(13) -0.04890(12) 0.0203(4) Uani 1.00 1 d . . . C(11) C 0.6753(2) 0.16966(17) -0.19615(14) 0.0330(5) Uani 1.00 1 d . . . C(12) C 1.19652(19) 0.32108(15) 0.13539(15) 0.0301(5) Uani 1.00 1 d . . . C(13) C 1.0370(2) 0.41357(14) 0.11205(13) 0.0275(4) Uani 1.00 1 d . . . C(14) C 0.9157(2) 0.44057(14) 0.10155(13) 0.0262(4) Uani 1.00 1 d . . . C(15) C 0.8944(2) 0.52733(15) 0.08891(15) 0.0353(5) Uani 1.00 1 d . . . C(16) C 0.7830(2) 0.55892(16) 0.08397(16) 0.0416(6) Uani 1.00 1 d . . . C(17) C 0.6888(2) 0.50478(16) 0.08974(15) 0.0344(5) Uani 1.00 1 d . . . C(18) C 0.7068(2) 0.41975(14) 0.09925(13) 0.0263(4) Uani 1.00 1 d . . . C(19) C 0.82149(18) 0.38504(13) 0.10821(12) 0.0218(4) Uani 1.00 1 d . . . C(20) C 0.5030(2) 0.38918(19) 0.09079(18) 0.0427(6) Uani 1.00 1 d . . . C(21) C 1.12454(19) 0.26267(15) 0.26815(14) 0.0271(4) Uani 1.00 1 d . . . C(22) C 0.95200(18) 0.19341(13) 0.29999(13) 0.0220(4) Uani 1.00 1 d . . . C(23) C 0.84261(19) 0.14865(13) 0.29188(13) 0.0233(4) Uani 1.00 1 d . . . C(24) C 0.7874(2) 0.13170(16) 0.36545(15) 0.0324(5) Uani 1.00 1 d . . . C(25) C 0.6821(2) 0.09130(19) 0.36255(17) 0.0428(6) Uani 1.00 1 d . . . C(26) C 0.6293(2) 0.06467(18) 0.28469(17) 0.0408(6) Uani 1.00 1 d . . . C(27) C 0.6831(2) 0.07773(15) 0.21236(15) 0.0301(5) Uani 1.00 1 d . . . C(28) C 0.79237(18) 0.12153(13) 0.21322(13) 0.0224(4) Uani 1.00 1 d . . . C(29) C 0.5394(2) -0.0003(2) 0.1286(2) 0.0544(8) Uani 1.00 1 d . . . H(1) H 1.3946 0.2602 0.2045 0.046 Uiso 1.00 1 c R . . H(2) H 1.3522 0.2115 0.2838 0.046 Uiso 1.00 1 c R . . H(3) H 1.3429 0.3116 0.2788 0.046 Uiso 1.00 1 c R . . H(4) H 1.2766 0.1510 0.1378 0.033 Uiso 1.00 1 c R . . H(5) H 1.1915 0.1226 0.2069 0.033 Uiso 1.00 1 c R . . H(6) H 1.1976 0.0929 0.0282 0.027 Uiso 1.00 1 c R . . H(7) H 1.1386 0.0157 -0.0948 0.031 Uiso 1.00 1 c R . . H(8) H 1.0078 -0.0106 -0.2094 0.034 Uiso 1.00 1 c R . . H(9) H 0.8268 0.0589 -0.2234 0.032 Uiso 1.00 1 c R . . H(10) H 0.7187 0.1908 -0.2420 0.040 Uiso 1.00 1 c R . . H(11) H 0.6062 0.2049 -0.1906 0.040 Uiso 1.00 1 c R . . H(12) H 0.6504 0.1117 -0.2080 0.040 Uiso 1.00 1 c R . . H(13) H 1.2360 0.3732 0.1559 0.036 Uiso 1.00 1 c R . . H(14) H 1.2324 0.3030 0.0843 0.036 Uiso 1.00 1 c R . . H(15) H 1.0953 0.4561 0.1164 0.033 Uiso 1.00 1 c R . . H(16) H 0.9585 0.5643 0.0838 0.042 Uiso 1.00 1 c R . . H(17) H 0.7702 0.6175 0.0766 0.050 Uiso 1.00 1 c R . . H(18) H 0.6115 0.5266 0.0871 0.041 Uiso 1.00 1 c R . . H(19) H 0.4852 0.4233 0.1389 0.051 Uiso 1.00 1 c R . . H(20) H 0.4499 0.3409 0.0858 0.051 Uiso 1.00 1 c R . . H(21) H 0.4928 0.4232 0.0399 0.051 Uiso 1.00 1 c R . . H(22) H 1.1563 0.2372 0.3214 0.033 Uiso 1.00 1 c R . . H(23) H 1.1121 0.3233 0.2780 0.033 Uiso 1.00 1 c R . . H(24) H 0.9849 0.2025 0.3554 0.026 Uiso 1.00 1 c R . . H(25) H 0.8240 0.1487 0.4178 0.039 Uiso 1.00 1 c R . . H(26) H 0.6448 0.0812 0.4123 0.051 Uiso 1.00 1 c R . . H(27) H 0.5555 0.0373 0.2823 0.049 Uiso 1.00 1 c R . . H(28) H 0.5541 -0.0490 0.1653 0.065 Uiso 1.00 1 c R . . H(29) H 0.5228 -0.0196 0.0709 0.065 Uiso 1.00 1 c R . . H(30) H 0.4720 0.0311 0.1461 0.065 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.01735(15) 0.02002(16) 0.01579(15) 0.00150(12) -0.00012(11) -0.00134(12) K(1) 0.0207(2) 0.0345(2) 0.0238(2) -0.00010(19) 0.00002(18) -0.00030(19) O(1) 0.0239(7) 0.0246(7) 0.0167(6) 0.0038(5) 0.0017(5) -0.0014(5) O(2) 0.0226(7) 0.0192(7) 0.0247(7) 0.0027(5) 0.0038(6) -0.0002(5) O(3) 0.0249(7) 0.0216(7) 0.0190(7) -0.0000(5) 0.0020(5) -0.0005(5) O(4) 0.0272(7) 0.0417(9) 0.0188(7) 0.0040(7) -0.0019(6) -0.0021(6) O(5) 0.0236(7) 0.0327(8) 0.0322(8) 0.0073(6) -0.0002(6) -0.0000(7) O(6) 0.0388(9) 0.0428(10) 0.0330(9) -0.0185(8) -0.0062(7) 0.0082(7) O(7) 0.0314(9) 0.1073(18) 0.0385(11) -0.0169(11) -0.0021(8) 0.0235(11) O(8) 0.0316(9) 0.0644(14) 0.0710(14) 0.0024(9) -0.0007(9) 0.0319(11) O(9) 0.0245(8) 0.0581(12) 0.0478(11) 0.0050(8) 0.0014(7) 0.0114(9) N(1) 0.0212(8) 0.0231(9) 0.0213(8) 0.0006(6) -0.0012(7) 0.0012(7) N(2) 0.0240(8) 0.0281(9) 0.0229(9) -0.0037(7) 0.0007(7) 0.0001(7) N(3) 0.0202(8) 0.0200(8) 0.0210(8) 0.0021(6) -0.0003(6) -0.0022(6) N(4) 0.0245(9) 0.0404(11) 0.0277(10) -0.0006(8) -0.0006(8) -0.0016(8) C(1) 0.0257(11) 0.0540(16) 0.0347(13) -0.0050(11) -0.0072(10) -0.0002(12) C(2) 0.0206(10) 0.0331(11) 0.0244(10) -0.0025(8) -0.0034(8) -0.0003(9) C(3) 0.0202(9) 0.0342(12) 0.0265(11) 0.0054(8) -0.0035(8) -0.0007(9) C(4) 0.0230(9) 0.0211(10) 0.0228(10) 0.0024(8) 0.0058(8) 0.0038(8) C(5) 0.0262(10) 0.0195(9) 0.0196(9) -0.0011(8) 0.0040(8) 0.0013(7) C(6) 0.0344(11) 0.0196(10) 0.0249(11) 0.0027(8) 0.0069(9) 0.0005(8) C(7) 0.0431(12) 0.0216(10) 0.0211(10) 0.0022(9) 0.0066(9) -0.0039(8) C(8) 0.0373(12) 0.0243(11) 0.0189(10) -0.0033(9) 0.0010(9) -0.0004(8) C(9) 0.0250(10) 0.0226(10) 0.0186(9) -0.0029(8) 0.0027(8) 0.0039(8) C(10) 0.0276(10) 0.0194(9) 0.0146(9) -0.0017(8) 0.0054(8) 0.0019(7) C(11) 0.0289(11) 0.0463(14) 0.0224(11) -0.0045(10) -0.0064(9) -0.0008(10) C(12) 0.0219(10) 0.0337(12) 0.0342(12) -0.0074(9) -0.0005(9) -0.0008(10) C(13) 0.0335(11) 0.0251(11) 0.0233(10) -0.0098(9) -0.0004(9) 0.0014(8) C(14) 0.0367(11) 0.0209(10) 0.0200(10) -0.0008(9) -0.0030(9) -0.0006(8) C(15) 0.0513(14) 0.0219(11) 0.0313(12) -0.0049(10) -0.0045(11) 0.0023(9) C(16) 0.0614(17) 0.0211(11) 0.0402(14) 0.0085(11) -0.0095(13) 0.0016(10) C(17) 0.0421(13) 0.0308(12) 0.0290(12) 0.0144(10) -0.0060(10) -0.0010(9) C(18) 0.0330(11) 0.0282(11) 0.0172(9) 0.0082(9) -0.0011(8) -0.0018(8) C(19) 0.0285(10) 0.0214(10) 0.0151(9) 0.0040(8) -0.0001(8) -0.0016(7) C(20) 0.0278(12) 0.0519(16) 0.0483(15) 0.0162(11) 0.0031(11) -0.0004(13) C(21) 0.0265(10) 0.0295(11) 0.0245(10) -0.0031(9) -0.0038(9) -0.0038(9) C(22) 0.0284(10) 0.0199(9) 0.0174(9) 0.0062(8) -0.0001(8) -0.0024(7) C(23) 0.0274(10) 0.0202(10) 0.0226(10) 0.0041(8) 0.0041(8) 0.0027(8) C(24) 0.0395(12) 0.0350(13) 0.0234(11) 0.0032(10) 0.0065(9) 0.0022(9) C(25) 0.0443(14) 0.0534(17) 0.0328(13) -0.0086(12) 0.0165(11) 0.0111(12) C(26) 0.0343(13) 0.0491(15) 0.0400(14) -0.0112(11) 0.0085(11) 0.0122(12) C(27) 0.0298(11) 0.0290(12) 0.0309(12) -0.0024(9) -0.0014(9) 0.0073(9) C(28) 0.0261(10) 0.0169(9) 0.0242(10) 0.0033(8) 0.0017(8) 0.0037(8) C(29) 0.0471(16) 0.0593(18) 0.0544(18) -0.0309(15) -0.0104(14) 0.0131(15) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mn(1) K(1) 3.4961(5) yes . . Mn(1) O(1) 1.8991(14) yes . . Mn(1) O(2) 1.9387(14) yes . . Mn(1) O(3) 2.0609(14) yes . . Mn(1) N(1) 2.0205(17) yes . . Mn(1) N(2) 2.2177(19) yes . . Mn(1) N(3) 2.0569(17) yes . . K(1) O(1) 2.8426(14) yes . . K(1) O(2) 2.8026(14) yes . . K(1) O(3) 2.7479(14) yes . . K(1) O(4) 2.7568(15) yes . . K(1) O(5) 2.8186(16) yes . . K(1) O(6) 2.8974(19) yes . . K(1) O(7) 2.771(2) yes . . K(1) O(8) 2.7885(19) yes . . K(1) N(4) 3.1887(19) yes . . O(1) C(10) 1.325(2) yes . . O(2) C(19) 1.318(2) yes . . O(3) C(28) 1.301(2) yes . . O(4) C(9) 1.371(2) yes . . O(4) C(11) 1.437(2) yes . . O(5) C(18) 1.374(2) yes . . O(5) C(20) 1.415(2) yes . . O(6) C(27) 1.383(2) yes . . O(6) C(29) 1.425(3) yes . . O(7) N(4) 1.245(3) yes . . O(8) N(4) 1.257(3) yes . . O(9) N(4) 1.233(2) yes . . N(1) C(3) 1.480(2) yes . . N(1) C(4) 1.289(2) yes . . N(2) C(12) 1.464(2) yes . . N(2) C(13) 1.277(2) yes . . N(3) C(21) 1.482(2) yes . . N(3) C(22) 1.292(2) yes . . C(1) C(2) 1.536(3) yes . . C(2) C(3) 1.531(3) yes . . C(2) C(12) 1.544(3) yes . . C(2) C(21) 1.531(3) yes . . C(4) C(5) 1.442(2) yes . . C(5) C(6) 1.415(3) yes . . C(5) C(10) 1.404(2) yes . . C(6) C(7) 1.373(3) yes . . C(7) C(8) 1.397(3) yes . . C(8) C(9) 1.382(3) yes . . C(9) C(10) 1.424(2) yes . . C(13) C(14) 1.452(3) yes . . C(14) C(15) 1.415(3) yes . . C(14) C(19) 1.406(3) yes . . C(15) C(16) 1.368(3) yes . . C(16) C(17) 1.390(3) yes . . C(17) C(18) 1.376(3) yes . . C(18) C(19) 1.422(3) yes . . C(22) C(23) 1.439(2) yes . . C(23) C(24) 1.411(3) yes . . C(23) C(28) 1.415(2) yes . . C(24) C(25) 1.365(3) yes . . C(25) C(26) 1.412(3) yes . . C(26) C(27) 1.374(3) yes . . C(27) C(28) 1.432(3) yes . . C(1) H(1) 0.980 no . . C(1) H(2) 0.980 no . . C(1) H(3) 0.980 no . . C(3) H(4) 0.990 no . . C(3) H(5) 0.990 no . . C(4) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(11) H(10) 0.980 no . . C(11) H(11) 0.980 no . . C(11) H(12) 0.980 no . . C(12) H(13) 0.990 no . . C(12) H(14) 0.990 no . . C(13) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(17) H(18) 0.950 no . . C(20) H(19) 0.980 no . . C(20) H(20) 0.980 no . . C(20) H(21) 0.980 no . . C(21) H(22) 0.990 no . . C(21) H(23) 0.990 no . . C(22) H(24) 0.950 no . . C(24) H(25) 0.950 no . . C(25) H(26) 0.950 no . . C(26) H(27) 0.950 no . . C(29) H(28) 0.980 no . . C(29) H(29) 0.980 no . . C(29) H(30) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 K(1) Mn(1) O(1) 54.30(4) yes . . . K(1) Mn(1) O(2) 53.17(4) yes . . . K(1) Mn(1) O(3) 51.76(3) yes . . . K(1) Mn(1) N(1) 131.91(5) yes . . . K(1) Mn(1) N(2) 128.60(4) yes . . . K(1) Mn(1) N(3) 124.35(5) yes . . . O(1) Mn(1) O(2) 88.30(6) yes . . . O(1) Mn(1) O(3) 88.35(5) yes . . . O(1) Mn(1) N(1) 89.73(6) yes . . . O(1) Mn(1) N(2) 102.86(6) yes . . . O(1) Mn(1) N(3) 172.87(6) yes . . . O(2) Mn(1) O(3) 86.24(5) yes . . . O(2) Mn(1) N(1) 169.96(6) yes . . . O(2) Mn(1) N(2) 84.95(6) yes . . . O(2) Mn(1) N(3) 95.85(6) yes . . . O(3) Mn(1) N(1) 103.54(6) yes . . . O(3) Mn(1) N(2) 165.50(6) yes . . . O(3) Mn(1) N(3) 86.14(6) yes . . . N(1) Mn(1) N(2) 85.89(7) yes . . . N(1) Mn(1) N(3) 87.16(7) yes . . . N(2) Mn(1) N(3) 83.32(6) yes . . . Mn(1) K(1) O(1) 32.86(2) yes . . . Mn(1) K(1) O(2) 33.62(2) yes . . . Mn(1) K(1) O(3) 36.09(3) yes . . . Mn(1) K(1) O(4) 88.57(3) yes . . . Mn(1) K(1) O(5) 88.33(3) yes . . . Mn(1) K(1) O(6) 91.17(3) yes . . . Mn(1) K(1) O(7) 152.37(5) yes . . . Mn(1) K(1) O(8) 158.61(5) yes . . . Mn(1) K(1) N(4) 169.08(4) yes . . . O(1) K(1) O(2) 56.53(4) yes . . . O(1) K(1) O(3) 59.18(4) yes . . . O(1) K(1) O(4) 55.97(4) yes . . . O(1) K(1) O(5) 104.14(4) yes . . . O(1) K(1) O(6) 107.23(4) yes . . . O(1) K(1) O(7) 128.66(5) yes . . . O(1) K(1) O(8) 165.40(5) yes . . . O(1) K(1) N(4) 150.30(4) yes . . . O(2) K(1) O(3) 59.04(4) yes . . . O(2) K(1) O(4) 107.83(4) yes . . . O(2) K(1) O(5) 54.72(4) yes . . . O(2) K(1) O(6) 106.84(4) yes . . . O(2) K(1) O(7) 126.96(6) yes . . . O(2) K(1) O(8) 138.00(5) yes . . . O(2) K(1) N(4) 135.49(4) yes . . . O(3) K(1) O(4) 103.06(4) yes . . . O(3) K(1) O(5) 105.13(4) yes . . . O(3) K(1) O(6) 55.08(4) yes . . . O(3) K(1) O(7) 171.39(6) yes . . . O(3) K(1) O(8) 125.72(5) yes . . . O(3) K(1) N(4) 148.74(5) yes . . . O(4) K(1) O(5) 126.31(5) yes . . . O(4) K(1) O(6) 114.30(5) yes . . . O(4) K(1) O(7) 81.43(5) yes . . . O(4) K(1) O(8) 110.37(6) yes . . . O(4) K(1) N(4) 97.16(4) yes . . . O(5) K(1) O(6) 119.34(5) yes . . . O(5) K(1) O(7) 77.32(6) yes . . . O(5) K(1) O(8) 88.14(5) yes . . . O(5) K(1) N(4) 80.78(4) yes . . . O(6) K(1) O(7) 116.43(6) yes . . . O(6) K(1) O(8) 72.33(5) yes . . . O(6) K(1) N(4) 94.90(5) yes . . . O(7) K(1) O(8) 45.73(6) yes . . . O(7) K(1) N(4) 22.76(5) yes . . . O(8) K(1) N(4) 23.05(5) yes . . . Mn(1) O(1) K(1) 92.84(5) yes . . . Mn(1) O(1) C(10) 127.36(12) yes . . . K(1) O(1) C(10) 109.93(11) yes . . . Mn(1) O(2) K(1) 93.21(5) yes . . . Mn(1) O(2) C(19) 132.73(13) yes . . . K(1) O(2) C(19) 114.70(11) yes . . . Mn(1) O(3) K(1) 92.15(5) yes . . . Mn(1) O(3) C(28) 127.55(12) yes . . . K(1) O(3) C(28) 106.78(11) yes . . . K(1) O(4) C(9) 115.23(11) yes . . . K(1) O(4) C(11) 123.59(12) yes . . . C(9) O(4) C(11) 117.12(17) yes . . . K(1) O(5) C(18) 116.08(12) yes . . . K(1) O(5) C(20) 116.78(14) yes . . . C(18) O(5) C(20) 117.11(18) yes . . . K(1) O(6) C(27) 102.68(13) yes . . . K(1) O(6) C(29) 125.38(15) yes . . . C(27) O(6) C(29) 116.9(2) yes . . . K(1) O(7) N(4) 97.83(14) yes . . . K(1) O(8) N(4) 96.65(14) yes . . . Mn(1) N(1) C(3) 117.24(13) yes . . . Mn(1) N(1) C(4) 125.11(14) yes . . . C(3) N(1) C(4) 117.38(17) yes . . . Mn(1) N(2) C(12) 114.88(14) yes . . . Mn(1) N(2) C(13) 126.14(15) yes . . . C(12) N(2) C(13) 118.23(19) yes . . . Mn(1) N(3) C(21) 117.68(13) yes . . . Mn(1) N(3) C(22) 126.21(14) yes . . . C(21) N(3) C(22) 116.02(17) yes . . . K(1) N(4) O(7) 59.40(12) yes . . . K(1) N(4) O(8) 60.30(11) yes . . . K(1) N(4) O(9) 172.46(15) yes . . . O(7) N(4) O(8) 119.38(19) yes . . . O(7) N(4) O(9) 120.4(2) yes . . . O(8) N(4) O(9) 120.2(2) yes . . . C(1) C(2) C(3) 107.62(19) yes . . . C(1) C(2) C(12) 108.92(19) yes . . . C(1) C(2) C(21) 108.30(18) yes . . . C(3) C(2) C(12) 110.77(18) yes . . . C(3) C(2) C(21) 110.71(18) yes . . . C(12) C(2) C(21) 110.42(18) yes . . . N(1) C(3) C(2) 112.72(17) yes . . . N(1) C(4) C(5) 126.21(19) yes . . . C(4) C(5) C(6) 118.26(18) yes . . . C(4) C(5) C(10) 121.33(18) yes . . . C(6) C(5) C(10) 120.41(18) yes . . . C(5) C(6) C(7) 120.5(2) yes . . . C(6) C(7) C(8) 120.1(2) yes . . . C(7) C(8) C(9) 120.06(19) yes . . . O(4) C(9) C(8) 124.65(18) yes . . . O(4) C(9) C(10) 114.05(17) yes . . . C(8) C(9) C(10) 121.30(19) yes . . . O(1) C(10) C(5) 123.51(17) yes . . . O(1) C(10) C(9) 118.91(17) yes . . . C(5) C(10) C(9) 117.52(18) yes . . . N(2) C(12) C(2) 109.95(18) yes . . . N(2) C(13) C(14) 125.3(2) yes . . . C(13) C(14) C(15) 117.3(2) yes . . . C(13) C(14) C(19) 122.57(19) yes . . . C(15) C(14) C(19) 120.0(2) yes . . . C(14) C(15) C(16) 121.1(2) yes . . . C(15) C(16) C(17) 119.6(2) yes . . . C(16) C(17) C(18) 120.5(2) yes . . . O(5) C(18) C(17) 125.2(2) yes . . . O(5) C(18) C(19) 113.27(18) yes . . . C(17) C(18) C(19) 121.5(2) yes . . . O(2) C(19) C(14) 125.04(18) yes . . . O(2) C(19) C(18) 117.77(18) yes . . . C(14) C(19) C(18) 117.15(19) yes . . . N(3) C(21) C(2) 111.49(17) yes . . . N(3) C(22) C(23) 127.94(18) yes . . . C(22) C(23) C(24) 117.65(19) yes . . . C(22) C(23) C(28) 121.48(19) yes . . . C(24) C(23) C(28) 120.9(2) yes . . . C(23) C(24) C(25) 121.0(2) yes . . . C(24) C(25) C(26) 119.2(2) yes . . . C(25) C(26) C(27) 121.0(2) yes . . . O(6) C(27) C(26) 125.4(2) yes . . . O(6) C(27) C(28) 113.5(2) yes . . . C(26) C(27) C(28) 121.0(2) yes . . . O(3) C(28) C(23) 124.45(18) yes . . . O(3) C(28) C(27) 118.75(18) yes . . . C(23) C(28) C(27) 116.80(19) yes . . . C(2) C(1) H(1) 109.5 no . . . C(2) C(1) H(2) 109.5 no . . . C(2) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . N(1) C(3) H(4) 109.0 no . . . N(1) C(3) H(5) 109.1 no . . . C(2) C(3) H(4) 109.0 no . . . C(2) C(3) H(5) 109.0 no . . . H(4) C(3) H(5) 107.8 no . . . N(1) C(4) H(6) 116.9 no . . . C(5) C(4) H(6) 116.9 no . . . C(5) C(6) H(7) 119.8 no . . . C(7) C(6) H(7) 119.8 no . . . C(6) C(7) H(8) 119.9 no . . . C(8) C(7) H(8) 119.9 no . . . C(7) C(8) H(9) 120.0 no . . . C(9) C(8) H(9) 120.0 no . . . O(4) C(11) H(10) 109.5 no . . . O(4) C(11) H(11) 109.5 no . . . O(4) C(11) H(12) 109.5 no . . . H(10) C(11) H(11) 109.5 no . . . H(10) C(11) H(12) 109.5 no . . . H(11) C(11) H(12) 109.5 no . . . N(2) C(12) H(13) 109.7 no . . . N(2) C(12) H(14) 109.7 no . . . C(2) C(12) H(13) 109.7 no . . . C(2) C(12) H(14) 109.7 no . . . H(13) C(12) H(14) 108.2 no . . . N(2) C(13) H(15) 117.4 no . . . C(14) C(13) H(15) 117.3 no . . . C(14) C(15) H(16) 119.4 no . . . C(16) C(15) H(16) 119.4 no . . . C(15) C(16) H(17) 120.2 no . . . C(17) C(16) H(17) 120.2 no . . . C(16) C(17) H(18) 119.8 no . . . C(18) C(17) H(18) 119.8 no . . . O(5) C(20) H(19) 109.5 no . . . O(5) C(20) H(20) 109.5 no . . . O(5) C(20) H(21) 109.5 no . . . H(19) C(20) H(20) 109.5 no . . . H(19) C(20) H(21) 109.5 no . . . H(20) C(20) H(21) 109.5 no . . . N(3) C(21) H(22) 109.3 no . . . N(3) C(21) H(23) 109.3 no . . . C(2) C(21) H(22) 109.3 no . . . C(2) C(21) H(23) 109.3 no . . . H(22) C(21) H(23) 108.0 no . . . N(3) C(22) H(24) 116.0 no . . . C(23) C(22) H(24) 116.0 no . . . C(23) C(24) H(25) 119.5 no . . . C(25) C(24) H(25) 119.5 no . . . C(24) C(25) H(26) 120.4 no . . . C(26) C(25) H(26) 120.4 no . . . C(25) C(26) H(27) 119.5 no . . . C(27) C(26) H(27) 119.5 no . . . O(6) C(29) H(28) 109.5 no . . . O(6) C(29) H(29) 109.5 no . . . O(6) C(29) H(30) 109.5 no . . . H(28) C(29) H(29) 109.5 no . . . H(28) C(29) H(30) 109.5 no . . . H(29) C(29) H(30) 109.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(24) 3.524(2) ? . 4_554 O(2) C(11) 3.534(2) ? . 4_555 O(3) C(6) 3.133(2) ? . 3_755 O(3) C(7) 3.262(2) ? . 3_755 O(4) C(22) 3.483(2) ? . 4_554 O(4) C(23) 3.401(2) ? . 4_554 O(4) C(24) 3.169(3) ? . 4_554 O(5) C(11) 3.292(2) ? . 4_555 O(7) C(1) 3.305(3) ? . 4_454 O(8) C(3) 3.480(3) ? . 1_455 O(9) N(1) 3.462(2) ? . 1_455 O(9) C(1) 3.439(3) ? . 4_454 O(9) C(4) 2.987(2) ? . 1_455 O(9) C(5) 3.539(2) ? . 1_455 O(9) C(12) 3.488(3) ? . 1_455 O(9) C(16) 3.504(3) ? . 3_665 O(9) C(21) 3.439(2) ? . 4_454 N(1) O(9) 3.462(2) ? . 1_655 N(1) C(7) 3.393(2) ? . 3_755 C(1) O(7) 3.305(3) ? . 4_655 C(1) O(9) 3.439(3) ? . 4_655 C(3) O(8) 3.480(3) ? . 1_655 C(4) O(9) 2.987(2) ? . 1_655 C(4) C(6) 3.598(3) ? . 3_755 C(4) C(7) 3.512(3) ? . 3_755 C(5) O(9) 3.539(2) ? . 1_655 C(5) C(6) 3.551(3) ? . 3_755 C(6) O(3) 3.133(2) ? . 3_755 C(6) C(4) 3.598(3) ? . 3_755 C(6) C(5) 3.551(3) ? . 3_755 C(7) O(3) 3.262(2) ? . 3_755 C(7) N(1) 3.393(2) ? . 3_755 C(7) C(4) 3.512(3) ? . 3_755 C(7) C(28) 3.585(3) ? . 3_755 C(8) C(19) 3.536(2) ? . 4_554 C(9) C(22) 3.351(2) ? . 4_554 C(10) C(22) 3.507(2) ? . 4_554 C(11) O(2) 3.534(2) ? . 4_554 C(11) O(5) 3.292(2) ? . 4_554 C(11) C(23) 3.485(3) ? . 4_554 C(11) C(24) 3.527(3) ? . 4_554 C(12) O(9) 3.488(3) ? . 1_655 C(13) C(15) 3.514(3) ? . 3_765 C(15) C(13) 3.514(3) ? . 3_765 C(15) C(22) 3.576(3) ? . 2_755 C(16) O(9) 3.504(3) ? . 3_665 C(19) C(8) 3.536(2) ? . 4_555 C(21) O(9) 3.439(2) ? . 4_655 C(22) O(4) 3.483(2) ? . 4_555 C(22) C(9) 3.351(2) ? . 4_555 C(22) C(10) 3.507(2) ? . 4_555 C(22) C(15) 3.576(3) ? . 2_745 C(23) O(4) 3.401(2) ? . 4_555 C(23) C(11) 3.485(3) ? . 4_555 C(24) O(1) 3.524(2) ? . 4_555 C(24) O(4) 3.169(3) ? . 4_555 C(24) C(11) 3.527(3) ? . 4_555 C(28) C(7) 3.585(3) ? . 3_755 K(1) H(25) 3.591 ? . 4_554 O(1) H(24) 2.915 ? . 4_554 O(1) H(25) 2.733 ? . 4_554 O(2) H(9) 3.276 ? . 4_555 O(2) H(10) 2.591 ? . 4_555 O(2) H(25) 3.405 ? . 4_554 O(3) H(7) 2.517 ? . 3_755 O(3) H(8) 2.785 ? . 3_755 O(4) H(24) 3.409 ? . 4_554 O(4) H(25) 3.029 ? . 4_554 O(5) H(1) 3.552 ? . 1_455 O(5) H(10) 2.791 ? . 4_555 O(5) H(11) 3.510 ? . 4_555 O(5) H(12) 3.079 ? . 4_555 O(5) H(26) 3.221 ? . 4_554 O(6) H(7) 2.874 ? . 3_755 O(7) H(2) 2.754 ? . 4_454 O(7) H(3) 3.006 ? . 4_454 O(7) H(17) 3.442 ? . 3_665 O(7) H(26) 3.316 ? . 4_554 O(8) H(1) 3.216 ? . 1_455 O(8) H(4) 2.560 ? . 1_455 O(8) H(6) 2.900 ? . 1_455 O(8) H(14) 3.289 ? . 1_455 O(8) H(29) 2.937 ? . 3_655 O(9) H(2) 3.036 ? . 4_454 O(9) H(3) 3.015 ? . 4_454 O(9) H(4) 3.216 ? . 1_455 O(9) H(6) 2.751 ? . 1_455 O(9) H(14) 2.516 ? . 1_455 O(9) H(17) 2.561 ? . 3_665 O(9) H(22) 2.604 ? . 4_454 O(9) H(23) 3.489 ? . 4_454 N(1) H(8) 3.284 ? . 3_755 N(2) H(16) 3.565 ? . 3_765 N(3) H(8) 3.422 ? . 3_755 N(4) H(2) 3.247 ? . 4_454 N(4) H(3) 3.163 ? . 4_454 N(4) H(4) 3.260 ? . 1_455 N(4) H(6) 3.201 ? . 1_455 N(4) H(14) 3.032 ? . 1_455 N(4) H(17) 3.319 ? . 3_665 N(4) H(28) 3.548 ? . 3_655 N(4) H(29) 3.364 ? . 3_655 C(1) H(11) 3.221 ? . 4_655 C(1) H(20) 3.249 ? . 1_655 C(1) H(28) 3.550 ? . 2_755 C(3) H(8) 3.561 ? . 3_755 C(5) H(23) 3.318 ? . 4_554 C(5) H(24) 3.541 ? . 4_554 C(6) H(23) 2.942 ? . 4_554 C(7) H(5) 3.202 ? . 3_755 C(7) H(23) 2.913 ? . 4_554 C(8) H(5) 3.214 ? . 3_755 C(8) H(23) 3.270 ? . 4_554 C(9) H(23) 3.597 ? . 4_554 C(9) H(24) 3.121 ? . 4_554 C(10) H(24) 2.903 ? . 4_554 C(10) H(25) 3.478 ? . 4_554 C(11) H(28) 3.325 ? . 3_655 C(12) H(17) 3.596 ? . 3_765 C(12) H(20) 3.087 ? . 1_655 C(13) H(8) 3.300 ? . 4_555 C(13) H(16) 3.172 ? . 3_765 C(14) H(8) 3.330 ? . 4_555 C(14) H(9) 3.067 ? . 4_555 C(14) H(16) 3.412 ? . 3_765 C(14) H(25) 3.370 ? . 4_554 C(15) H(8) 3.407 ? . 4_555 C(15) H(9) 3.458 ? . 4_555 C(15) H(15) 3.322 ? . 3_765 C(15) H(24) 3.210 ? . 2_755 C(16) H(5) 3.502 ? . 2_755 C(16) H(14) 3.479 ? . 3_765 C(16) H(22) 3.270 ? . 2_755 C(16) H(24) 3.583 ? . 2_755 C(17) H(9) 3.435 ? . 4_555 C(17) H(21) 3.051 ? . 3_665 C(17) H(26) 3.169 ? . 4_554 C(18) H(9) 3.084 ? . 4_555 C(18) H(10) 3.095 ? . 4_555 C(18) H(12) 3.253 ? . 4_555 C(18) H(25) 3.481 ? . 4_554 C(18) H(26) 3.033 ? . 4_554 C(19) H(9) 2.846 ? . 4_555 C(19) H(10) 3.016 ? . 4_555 C(19) H(25) 3.110 ? . 4_554 C(20) H(1) 3.076 ? . 1_455 C(20) H(12) 3.529 ? . 4_555 C(20) H(13) 3.321 ? . 1_455 C(20) H(14) 3.385 ? . 1_455 C(20) H(18) 3.332 ? . 3_665 C(20) H(26) 3.495 ? . 2_655 C(20) H(26) 3.440 ? . 4_554 C(20) H(27) 3.224 ? . 2_655 C(21) H(17) 3.543 ? . 2_745 C(22) H(8) 3.304 ? . 3_755 C(22) H(10) 3.274 ? . 4_555 C(22) H(16) 2.910 ? . 2_745 C(23) H(8) 3.145 ? . 3_755 C(23) H(10) 2.955 ? . 4_555 C(23) H(15) 3.453 ? . 2_745 C(23) H(16) 3.206 ? . 2_745 C(24) H(10) 3.373 ? . 4_555 C(24) H(11) 3.405 ? . 4_555 C(24) H(15) 3.107 ? . 2_745 C(24) H(16) 3.150 ? . 2_745 C(25) H(11) 3.450 ? . 4_555 C(25) H(15) 3.335 ? . 2_745 C(25) H(19) 3.290 ? . 2_645 C(26) H(13) 3.515 ? . 2_745 C(26) H(19) 2.925 ? . 2_645 C(27) H(7) 3.250 ? . 3_755 C(28) H(7) 3.043 ? . 3_755 C(28) H(8) 2.897 ? . 3_755 C(28) H(10) 3.204 ? . 4_555 C(29) H(3) 3.562 ? . 2_745 C(29) H(12) 3.154 ? . 3_655 C(29) H(29) 3.246 ? . 3_655 H(1) O(5) 3.552 ? . 1_655 H(1) O(8) 3.216 ? . 1_655 H(1) C(20) 3.076 ? . 1_655 H(1) H(11) 2.896 ? . 4_655 H(1) H(19) 3.018 ? . 1_655 H(1) H(20) 2.426 ? . 1_655 H(2) O(7) 2.754 ? . 4_655 H(2) O(9) 3.036 ? . 4_655 H(2) N(4) 3.247 ? . 4_655 H(2) H(11) 3.198 ? . 4_655 H(2) H(17) 3.120 ? . 2_745 H(3) O(7) 3.006 ? . 4_655 H(3) O(9) 3.015 ? . 4_655 H(3) N(4) 3.163 ? . 4_655 H(3) C(29) 3.562 ? . 2_755 H(3) H(11) 3.030 ? . 4_655 H(3) H(19) 3.385 ? . 1_655 H(3) H(20) 3.458 ? . 1_655 H(3) H(28) 2.639 ? . 2_755 H(4) O(8) 2.560 ? . 1_655 H(4) O(9) 3.216 ? . 1_655 H(4) N(4) 3.260 ? . 1_655 H(4) H(30) 2.937 ? . 1_655 H(5) C(7) 3.202 ? . 3_755 H(5) C(8) 3.214 ? . 3_755 H(5) C(16) 3.502 ? . 2_745 H(5) H(8) 2.901 ? . 3_755 H(5) H(9) 2.912 ? . 3_755 H(5) H(17) 3.474 ? . 2_745 H(6) O(8) 2.900 ? . 1_655 H(6) O(9) 2.751 ? . 1_655 H(6) N(4) 3.201 ? . 1_655 H(7) O(3) 2.517 ? . 3_755 H(7) O(6) 2.874 ? . 3_755 H(7) C(27) 3.250 ? . 3_755 H(7) C(28) 3.043 ? . 3_755 H(7) H(23) 3.279 ? . 4_554 H(8) O(3) 2.785 ? . 3_755 H(8) N(1) 3.284 ? . 3_755 H(8) N(3) 3.422 ? . 3_755 H(8) C(3) 3.561 ? . 3_755 H(8) C(13) 3.300 ? . 4_554 H(8) C(14) 3.330 ? . 4_554 H(8) C(15) 3.407 ? . 4_554 H(8) C(22) 3.304 ? . 3_755 H(8) C(23) 3.145 ? . 3_755 H(8) C(28) 2.897 ? . 3_755 H(8) H(5) 2.901 ? . 3_755 H(8) H(15) 3.170 ? . 4_554 H(8) H(16) 3.437 ? . 4_554 H(8) H(23) 3.226 ? . 4_554 H(9) O(2) 3.276 ? . 4_554 H(9) C(14) 3.067 ? . 4_554 H(9) C(15) 3.458 ? . 4_554 H(9) C(17) 3.435 ? . 4_554 H(9) C(18) 3.084 ? . 4_554 H(9) C(19) 2.846 ? . 4_554 H(9) H(5) 2.912 ? . 3_755 H(10) O(2) 2.591 ? . 4_554 H(10) O(5) 2.791 ? . 4_554 H(10) C(18) 3.095 ? . 4_554 H(10) C(19) 3.016 ? . 4_554 H(10) C(22) 3.274 ? . 4_554 H(10) C(23) 2.955 ? . 4_554 H(10) C(24) 3.373 ? . 4_554 H(10) C(28) 3.204 ? . 4_554 H(11) O(5) 3.510 ? . 4_554 H(11) C(1) 3.221 ? . 4_454 H(11) C(24) 3.405 ? . 4_554 H(11) C(25) 3.450 ? . 4_554 H(11) H(1) 2.896 ? . 4_454 H(11) H(2) 3.198 ? . 4_454 H(11) H(3) 3.030 ? . 4_454 H(11) H(28) 3.135 ? . 3_655 H(12) O(5) 3.079 ? . 4_554 H(12) C(18) 3.253 ? . 4_554 H(12) C(20) 3.529 ? . 4_554 H(12) C(29) 3.154 ? . 3_655 H(12) H(19) 3.036 ? . 4_554 H(12) H(27) 3.490 ? . 3_655 H(12) H(28) 2.687 ? . 3_655 H(12) H(29) 3.412 ? . 3_655 H(12) H(30) 2.891 ? . 3_655 H(13) C(20) 3.321 ? . 1_655 H(13) C(26) 3.515 ? . 2_755 H(13) H(19) 2.997 ? . 1_655 H(13) H(20) 2.825 ? . 1_655 H(14) O(8) 3.289 ? . 1_655 H(14) O(9) 2.516 ? . 1_655 H(14) N(4) 3.032 ? . 1_655 H(14) C(16) 3.479 ? . 3_765 H(14) C(20) 3.385 ? . 1_655 H(14) H(17) 2.878 ? . 3_765 H(14) H(19) 3.525 ? . 1_655 H(14) H(20) 2.563 ? . 1_655 H(15) C(15) 3.322 ? . 3_765 H(15) C(23) 3.453 ? . 2_755 H(15) C(24) 3.107 ? . 2_755 H(15) C(25) 3.335 ? . 2_755 H(15) H(8) 3.170 ? . 4_555 H(15) H(16) 3.244 ? . 3_765 H(15) H(25) 3.263 ? . 2_755 H(16) N(2) 3.565 ? . 3_765 H(16) C(13) 3.172 ? . 3_765 H(16) C(14) 3.412 ? . 3_765 H(16) C(22) 2.910 ? . 2_755 H(16) C(23) 3.206 ? . 2_755 H(16) C(24) 3.150 ? . 2_755 H(16) H(8) 3.437 ? . 4_555 H(16) H(15) 3.244 ? . 3_765 H(16) H(16) 3.572 ? . 3_765 H(16) H(22) 3.457 ? . 2_755 H(16) H(24) 2.474 ? . 2_755 H(16) H(25) 2.833 ? . 2_755 H(17) O(7) 3.442 ? . 3_665 H(17) O(9) 2.561 ? . 3_665 H(17) N(4) 3.319 ? . 3_665 H(17) C(12) 3.596 ? . 3_765 H(17) C(21) 3.543 ? . 2_755 H(17) H(2) 3.120 ? . 2_755 H(17) H(5) 3.474 ? . 2_755 H(17) H(14) 2.878 ? . 3_765 H(17) H(20) 3.546 ? . 3_665 H(17) H(21) 3.482 ? . 3_665 H(17) H(22) 2.610 ? . 2_755 H(17) H(24) 3.228 ? . 2_755 H(18) C(20) 3.332 ? . 3_665 H(18) H(20) 3.516 ? . 3_665 H(18) H(21) 2.419 ? . 3_665 H(18) H(26) 3.063 ? . 2_655 H(18) H(26) 3.341 ? . 4_554 H(18) H(27) 2.956 ? . 2_655 H(19) C(25) 3.290 ? . 2_655 H(19) C(26) 2.925 ? . 2_655 H(19) H(1) 3.018 ? . 1_455 H(19) H(3) 3.385 ? . 1_455 H(19) H(12) 3.036 ? . 4_555 H(19) H(13) 2.997 ? . 1_455 H(19) H(14) 3.525 ? . 1_455 H(19) H(26) 3.005 ? . 2_655 H(19) H(27) 2.283 ? . 2_655 H(19) H(28) 3.245 ? . 2_655 H(20) C(1) 3.249 ? . 1_455 H(20) C(12) 3.087 ? . 1_455 H(20) H(1) 2.426 ? . 1_455 H(20) H(3) 3.458 ? . 1_455 H(20) H(13) 2.825 ? . 1_455 H(20) H(14) 2.563 ? . 1_455 H(20) H(17) 3.546 ? . 3_665 H(20) H(18) 3.516 ? . 3_665 H(21) C(17) 3.051 ? . 3_665 H(21) H(17) 3.482 ? . 3_665 H(21) H(18) 2.419 ? . 3_665 H(21) H(21) 2.773 ? . 3_665 H(21) H(26) 3.098 ? . 2_655 H(21) H(26) 2.795 ? . 4_554 H(21) H(27) 3.468 ? . 2_655 H(22) O(9) 2.604 ? . 4_655 H(22) C(16) 3.270 ? . 2_745 H(22) H(16) 3.457 ? . 2_745 H(22) H(17) 2.610 ? . 2_745 H(23) O(9) 3.489 ? . 4_655 H(23) C(5) 3.318 ? . 4_555 H(23) C(6) 2.942 ? . 4_555 H(23) C(7) 2.913 ? . 4_555 H(23) C(8) 3.270 ? . 4_555 H(23) C(9) 3.597 ? . 4_555 H(23) H(7) 3.279 ? . 4_555 H(23) H(8) 3.226 ? . 4_555 H(24) O(1) 2.915 ? . 4_555 H(24) O(4) 3.409 ? . 4_555 H(24) C(5) 3.541 ? . 4_555 H(24) C(9) 3.121 ? . 4_555 H(24) C(10) 2.903 ? . 4_555 H(24) C(15) 3.210 ? . 2_745 H(24) C(16) 3.583 ? . 2_745 H(24) H(16) 2.474 ? . 2_745 H(24) H(17) 3.228 ? . 2_745 H(25) K(1) 3.591 ? . 4_555 H(25) O(1) 2.733 ? . 4_555 H(25) O(2) 3.405 ? . 4_555 H(25) O(4) 3.029 ? . 4_555 H(25) C(10) 3.478 ? . 4_555 H(25) C(14) 3.370 ? . 4_555 H(25) C(18) 3.481 ? . 4_555 H(25) C(19) 3.110 ? . 4_555 H(25) H(15) 3.263 ? . 2_745 H(25) H(16) 2.833 ? . 2_745 H(26) O(5) 3.221 ? . 4_555 H(26) O(7) 3.316 ? . 4_555 H(26) C(17) 3.169 ? . 4_555 H(26) C(18) 3.033 ? . 4_555 H(26) C(20) 3.495 ? . 2_645 H(26) C(20) 3.440 ? . 4_555 H(26) H(18) 3.063 ? . 2_645 H(26) H(18) 3.341 ? . 4_555 H(26) H(19) 3.005 ? . 2_645 H(26) H(21) 3.098 ? . 2_645 H(26) H(21) 2.795 ? . 4_555 H(27) C(20) 3.224 ? . 2_645 H(27) H(12) 3.490 ? . 3_655 H(27) H(18) 2.956 ? . 2_645 H(27) H(19) 2.283 ? . 2_645 H(27) H(21) 3.468 ? . 2_645 H(28) N(4) 3.548 ? . 3_655 H(28) C(1) 3.550 ? . 2_745 H(28) C(11) 3.325 ? . 3_655 H(28) H(3) 2.639 ? . 2_745 H(28) H(11) 3.135 ? . 3_655 H(28) H(12) 2.687 ? . 3_655 H(28) H(19) 3.245 ? . 2_645 H(29) O(8) 2.937 ? . 3_655 H(29) N(4) 3.364 ? . 3_655 H(29) C(29) 3.246 ? . 3_655 H(29) H(12) 3.412 ? . 3_655 H(29) H(29) 2.383 ? . 3_655 H(29) H(30) 3.499 ? . 3_655 H(30) H(4) 2.937 ? . 1_455 H(30) H(12) 2.891 ? . 3_655 H(30) H(29) 3.499 ? . 3_655 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================