# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- ZBHAN110923.cif' #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; 'Han, Zheng-Bo' College of Chemistry liaoning University Shenyang, 110036 P. R. China ; _publ_contact_author_phone 86-24-62207849 _publ_contact_author_fax 86-24-62202380 _publ_contact_author_email ceshzb@lnu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to CrystEngComm. Aug. 30, 2011 ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Ming-Yang Zhang' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Zheng-Bo Han' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; _publ_contact_author_name 'Han, Zheng-Bo' #====================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 842229' #TrackingRef '- ZBHAN110923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Mn3 N8 O22' _chemical_formula_weight 1031.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 9.5565(5) _cell_length_b 12.4706(6) _cell_length_c 22.8429(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.600(2) _cell_angle_gamma 90.00 _cell_volume 2656.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1058 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7518 _exptl_absorpt_correction_T_max 0.8357 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14431 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.11 _reflns_number_total 9587 _reflns_number_gt 8382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(15) _refine_ls_number_reflns 9587 _refine_ls_number_parameters 572 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.36704(6) -0.19349(5) 0.30921(3) 0.02638(14) Uani 1 1 d . . . Mn2 Mn 0.66763(6) 0.64351(5) 0.28271(3) 0.02840(14) Uani 1 1 d . . . Mn3 Mn 0.05658(6) -0.33013(5) 0.27397(3) 0.02974(15) Uani 1 1 d . . . O1 O 0.2020(3) 0.2424(2) 0.24025(14) 0.0390(7) Uani 1 1 d . . . O2 O 0.3909(4) 0.3681(3) 0.08860(15) 0.0488(8) Uani 1 1 d . . . O3 O 0.1099(4) 0.0714(3) 0.06044(15) 0.0450(8) Uani 1 1 d . . . O4 O 0.1390(3) -0.1614(2) 0.26737(13) 0.0295(6) Uani 1 1 d . . . O5 O -0.0683(3) -0.0864(2) 0.22148(15) 0.0414(8) Uani 1 1 d . . . O6 O 0.4814(3) 0.5515(2) 0.28098(15) 0.0360(7) Uani 1 1 d . . . O7 O 0.2831(3) 0.6478(2) 0.27323(13) 0.0318(6) Uani 1 1 d . . . O8 O 0.1077(4) 0.3285(3) -0.13112(14) 0.0423(8) Uani 1 1 d . . . O9 O 0.3011(3) 0.2226(2) -0.10657(13) 0.0367(7) Uani 1 1 d . . . O10 O 0.8382(5) -0.2941(3) 0.56972(18) 0.0665(11) Uani 1 1 d . . . O11 O 0.5777(5) -0.1864(3) 0.70132(18) 0.0622(10) Uani 1 1 d . . . O12 O 0.5749(4) 0.0108(3) 0.53558(15) 0.0518(9) Uani 1 1 d . . . O13 O 0.5938(3) -0.2361(2) 0.34321(12) 0.0320(6) Uani 1 1 d . . . O14 O 0.8113(3) -0.1718(3) 0.38538(15) 0.0503(9) Uani 1 1 d . . . O15 O 0.7493(3) -0.5269(2) 0.73186(15) 0.0413(7) Uani 1 1 d . . . O16 O 0.9854(3) -0.5090(2) 0.76992(14) 0.0380(7) Uani 1 1 d . . . O17 O 0.4322(3) 0.1372(2) 0.73017(13) 0.0356(7) Uani 1 1 d . . . O18 O 0.5657(4) 0.2692(3) 0.70544(14) 0.0429(8) Uani 1 1 d . . . O1W O 0.8570(3) 0.7542(2) 0.28439(14) 0.0337(6) Uani 1 1 d . . . H1WB H 0.8433 0.8058 0.2595 0.040 Uiso 1 1 d R . . H1WA H 0.8763 0.7810 0.3194 0.040 Uiso 1 1 d R . . O19 O 0.4124(4) -0.0301(2) 0.34328(16) 0.0474(8) Uani 1 1 d . . . O20 O -0.0075(4) -0.3255(3) 0.17796(16) 0.0531(9) Uani 1 1 d . . . O2W O 0.7875(5) 0.5765(4) 0.36518(18) 0.0785(13) Uani 1 1 d . . . H2WB H 0.7386 0.5625 0.3912 0.094 Uiso 1 1 d R . . H2WA H 0.8196 0.5165 0.3563 0.094 Uiso 1 1 d R . . N1 N 0.1445(4) 0.1597(2) 0.15003(16) 0.0286(7) Uani 1 1 d . . . N2 N 0.2881(4) 0.3137(3) 0.16469(15) 0.0295(7) Uani 1 1 d . . . N3 N 0.2551(4) 0.2193(3) 0.07380(15) 0.0318(8) Uani 1 1 d . . . N4 N 0.7140(4) -0.1394(3) 0.55295(15) 0.0304(7) Uani 1 1 d . . . N5 N 0.7078(4) -0.2442(3) 0.63659(17) 0.0371(8) Uani 1 1 d . . . N6 N 0.5810(4) -0.0820(3) 0.62143(16) 0.0344(8) Uani 1 1 d . . . N7 N 0.5151(8) 0.1341(4) 0.3613(2) 0.090(2) Uani 1 1 d . . . N8 N -0.0252(12) -0.2259(7) 0.0969(4) 0.129(3) Uani 1 1 d D . . C1 C 0.2114(4) 0.2377(3) 0.18842(18) 0.0284(9) Uani 1 1 d . . . C2 C 0.3160(5) 0.3051(3) 0.10754(18) 0.0325(9) Uani 1 1 d . . . C3 C 0.1648(4) 0.1448(3) 0.09264(19) 0.0307(9) Uani 1 1 d . . . C4 C 0.0549(4) 0.0815(3) 0.1725(2) 0.0336(9) Uani 1 1 d . . . H4A H -0.0110 0.0468 0.1383 0.040 Uiso 1 1 calc R . . H4B H -0.0039 0.1187 0.1970 0.040 Uiso 1 1 calc R . . C5 C 0.1473(4) -0.0041(3) 0.2107(2) 0.0369(10) Uani 1 1 d . . . H5A H 0.2086 -0.0382 0.1862 0.044 Uiso 1 1 calc R . . H5B H 0.2113 0.0317 0.2450 0.044 Uiso 1 1 calc R . . C6 C 0.0659(4) -0.0892(3) 0.23410(19) 0.0306(9) Uani 1 1 d . . . C7 C 0.3667(5) 0.3963(3) 0.2050(2) 0.0359(10) Uani 1 1 d . . . H7A H 0.4403 0.4292 0.1861 0.043 Uiso 1 1 calc R . . H7B H 0.4165 0.3624 0.2430 0.043 Uiso 1 1 calc R . . C8 C 0.2672(4) 0.4828(3) 0.2184(2) 0.0365(10) Uani 1 1 d . . . H8A H 0.1927 0.4502 0.2368 0.044 Uiso 1 1 calc R . . H8B H 0.2188 0.5181 0.1806 0.044 Uiso 1 1 calc R . . C9 C 0.3519(4) 0.5660(3) 0.26114(18) 0.0279(9) Uani 1 1 d . . . C10 C 0.2815(5) 0.2070(4) 0.01247(17) 0.0378(10) Uani 1 1 d . . . H10A H 0.2797 0.1300 0.0018 0.045 Uiso 1 1 calc R . . H10B H 0.3774 0.2358 0.0114 0.045 Uiso 1 1 calc R . . C11 C 0.1688(5) 0.2660(4) -0.0321(2) 0.0423(11) Uani 1 1 d . . . H11A H 0.0754 0.2302 -0.0341 0.051 Uiso 1 1 calc R . . H11B H 0.1612 0.3397 -0.0171 0.051 Uiso 1 1 calc R . . C12 C 0.1946(5) 0.2728(3) -0.09469(19) 0.0335(10) Uani 1 1 d . . . C13 C 0.7593(5) -0.2295(4) 0.5860(2) 0.0411(11) Uani 1 1 d . . . C14 C 0.6197(5) -0.1717(3) 0.65761(19) 0.0342(10) Uani 1 1 d . . . C15 C 0.6221(5) -0.0653(3) 0.56777(19) 0.0344(9) Uani 1 1 d . . . C16 C 0.7528(5) -0.1279(4) 0.49357(19) 0.0409(11) Uani 1 1 d . . . H16A H 0.8483 -0.1601 0.4953 0.049 Uiso 1 1 calc R . . H16B H 0.7579 -0.0509 0.4837 0.049 Uiso 1 1 calc R . . C17 C 0.6410(5) -0.1837(4) 0.4449(2) 0.0383(10) Uani 1 1 d . . . H17A H 0.6202 -0.2552 0.4598 0.046 Uiso 1 1 calc R . . H17B H 0.5511 -0.1415 0.4378 0.046 Uiso 1 1 calc R . . C18 C 0.6852(4) -0.1969(3) 0.38781(19) 0.0328(9) Uani 1 1 d . . . C19 C 0.7259(6) -0.3506(4) 0.6653(3) 0.0506(13) Uani 1 1 d . . . H19A H 0.6462 -0.3623 0.6860 0.061 Uiso 1 1 calc R . . H19B H 0.7177 -0.4058 0.6336 0.061 Uiso 1 1 calc R . . C20 C 0.8620(5) -0.3672(4) 0.7089(2) 0.0438(12) Uani 1 1 d . . . H20A H 0.8745 -0.3100 0.7397 0.053 Uiso 1 1 calc R . . H20B H 0.9425 -0.3623 0.6881 0.053 Uiso 1 1 calc R . . C21 C 0.8658(4) -0.4759(3) 0.7394(2) 0.0328(9) Uani 1 1 d . . . C22 C 0.4936(5) 0.0019(3) 0.6419(2) 0.0372(10) Uani 1 1 d . . . H22A H 0.4121 0.0209 0.6087 0.045 Uiso 1 1 calc R . . H22B H 0.4540 -0.0263 0.6755 0.045 Uiso 1 1 calc R . . C23 C 0.5791(5) 0.0989(4) 0.6619(2) 0.0445(12) Uani 1 1 d . . . H23A H 0.5919 0.1385 0.6259 0.053 Uiso 1 1 calc R . . H23B H 0.6754 0.0760 0.6840 0.053 Uiso 1 1 calc R . . C24 C 0.5189(5) 0.1755(4) 0.7013(2) 0.0363(10) Uani 1 1 d . . . C25 C 0.5776(16) 0.2291(9) 0.3452(5) 0.170(6) Uani 1 1 d . . . H25A H 0.6063 0.2182 0.3070 0.255 Uiso 1 1 calc R . . H25B H 0.6622 0.2472 0.3764 0.255 Uiso 1 1 calc R . . H25C H 0.5079 0.2877 0.3411 0.255 Uiso 1 1 calc R . . C26 C 0.4725(13) 0.1491(6) 0.4161(4) 0.122(4) Uani 1 1 d . . . H26A H 0.3919 0.1014 0.4177 0.183 Uiso 1 1 calc R . . H26B H 0.4430 0.2237 0.4193 0.183 Uiso 1 1 calc R . . H26C H 0.5530 0.1324 0.4495 0.183 Uiso 1 1 calc R . . C27 C 0.4826(7) 0.0455(6) 0.3305(3) 0.0739(19) Uani 1 1 d . . . H27 H 0.5169 0.0390 0.2946 0.089 Uiso 1 1 calc R . . C28 C 0.1329(14) -0.2156(17) 0.0972(6) 0.216(9) Uani 1 1 d . . . H28A H 0.1467 -0.2201 0.0560 0.324 Uiso 1 1 calc R . . H28B H 0.1858 -0.2738 0.1212 0.324 Uiso 1 1 calc R . . H28C H 0.1685 -0.1464 0.1147 0.324 Uiso 1 1 calc R . . C29 C -0.1146(14) -0.1627(10) 0.0574(7) 0.176(6) Uani 1 1 d D . . H29A H -0.2141 -0.1831 0.0563 0.263 Uiso 1 1 calc R . . H29B H -0.0946 -0.1715 0.0174 0.263 Uiso 1 1 calc R . . H29C H -0.0998 -0.0876 0.0699 0.263 Uiso 1 1 calc R . . C30 C -0.0941(11) -0.2948(10) 0.1408(4) 0.130(4) Uani 1 1 d D . . H30 H -0.1937 -0.3083 0.1364 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0227(3) 0.0278(3) 0.0292(3) -0.0022(3) 0.0070(2) -0.0034(2) Mn2 0.0214(3) 0.0263(3) 0.0367(3) -0.0035(3) 0.0046(2) -0.0010(2) Mn3 0.0236(3) 0.0300(3) 0.0365(3) -0.0070(3) 0.0085(3) -0.0049(2) O1 0.051(2) 0.0339(16) 0.0349(18) -0.0018(12) 0.0159(14) 0.0012(13) O2 0.0442(19) 0.058(2) 0.048(2) 0.0032(16) 0.0172(16) -0.0194(16) O3 0.053(2) 0.0410(18) 0.0381(17) -0.0137(14) 0.0031(15) -0.0043(15) O4 0.0234(15) 0.0268(14) 0.0374(17) 0.0028(11) 0.0044(12) -0.0002(11) O5 0.0229(16) 0.0347(17) 0.067(2) 0.0077(15) 0.0095(15) 0.0006(12) O6 0.0265(16) 0.0277(15) 0.0516(18) -0.0028(13) 0.0036(13) -0.0024(12) O7 0.0255(15) 0.0261(14) 0.0449(17) -0.0057(12) 0.0105(13) -0.0046(11) O8 0.052(2) 0.0424(18) 0.0335(17) 0.0015(14) 0.0114(16) 0.0143(15) O9 0.0321(17) 0.0462(18) 0.0336(16) -0.0001(13) 0.0109(13) 0.0053(14) O10 0.077(3) 0.059(2) 0.064(2) -0.0115(19) 0.017(2) 0.031(2) O11 0.075(3) 0.068(3) 0.051(2) 0.0203(19) 0.028(2) 0.003(2) O12 0.068(2) 0.048(2) 0.0404(19) 0.0126(16) 0.0134(17) 0.0158(17) O13 0.0248(15) 0.0401(16) 0.0302(15) -0.0081(12) 0.0041(12) -0.0003(12) O14 0.0331(18) 0.076(2) 0.046(2) -0.0276(17) 0.0181(16) -0.0198(16) O15 0.0299(16) 0.0352(16) 0.058(2) 0.0128(14) 0.0085(14) -0.0067(13) O16 0.0213(15) 0.0381(17) 0.0527(19) 0.0104(14) 0.0042(13) 0.0063(12) O17 0.0307(16) 0.0437(17) 0.0362(16) -0.0061(13) 0.0158(13) -0.0027(13) O18 0.053(2) 0.0367(18) 0.0368(17) -0.0041(14) 0.0044(15) -0.0130(15) O1W 0.0310(15) 0.0363(17) 0.0368(16) -0.0070(12) 0.0138(13) -0.0060(12) O19 0.051(2) 0.0328(17) 0.059(2) -0.0078(15) 0.0124(17) -0.0096(15) O20 0.050(2) 0.072(3) 0.0340(19) 0.0006(17) 0.0031(18) -0.0024(18) O2W 0.090(3) 0.088(3) 0.053(2) 0.007(2) 0.004(2) 0.042(3) N1 0.0252(17) 0.0264(17) 0.0335(18) 0.0004(14) 0.0048(14) 0.0030(13) N2 0.0324(19) 0.0264(17) 0.0311(18) -0.0052(14) 0.0102(15) -0.0014(14) N3 0.0312(19) 0.041(2) 0.0250(17) -0.0049(15) 0.0095(15) 0.0016(15) N4 0.0282(18) 0.0312(18) 0.0318(18) -0.0024(15) 0.0065(14) 0.0015(14) N5 0.0286(19) 0.033(2) 0.046(2) 0.0092(16) -0.0001(16) -0.0022(15) N6 0.0309(19) 0.036(2) 0.0344(19) -0.0018(15) 0.0028(15) 0.0017(15) N7 0.140(6) 0.063(3) 0.051(3) -0.001(3) -0.015(3) -0.049(4) N8 0.171(9) 0.111(6) 0.093(6) -0.007(5) 0.000(6) 0.029(6) C1 0.031(2) 0.023(2) 0.030(2) -0.0011(16) 0.0060(17) 0.0080(16) C2 0.032(2) 0.038(2) 0.028(2) 0.0017(17) 0.0060(18) 0.0031(18) C3 0.026(2) 0.031(2) 0.033(2) 0.0014(17) 0.0006(17) 0.0061(16) C4 0.027(2) 0.027(2) 0.048(3) 0.0024(18) 0.0094(19) -0.0015(16) C5 0.024(2) 0.029(2) 0.055(3) 0.007(2) 0.004(2) -0.0036(17) C6 0.030(2) 0.028(2) 0.033(2) -0.0042(17) 0.0061(18) -0.0017(16) C7 0.028(2) 0.033(2) 0.045(3) -0.0132(19) 0.0059(19) -0.0016(17) C8 0.024(2) 0.033(2) 0.051(3) -0.011(2) 0.0051(19) 0.0006(17) C9 0.023(2) 0.024(2) 0.038(2) 0.0024(16) 0.0098(18) -0.0051(15) C10 0.038(2) 0.056(3) 0.021(2) -0.0030(19) 0.0085(18) 0.014(2) C11 0.043(3) 0.055(3) 0.033(2) 0.005(2) 0.017(2) 0.010(2) C12 0.036(2) 0.037(2) 0.027(2) -0.0049(18) 0.0055(19) -0.0086(19) C13 0.037(3) 0.038(3) 0.048(3) 0.000(2) 0.009(2) 0.004(2) C14 0.034(2) 0.039(2) 0.030(2) 0.0052(18) 0.0084(19) -0.0101(18) C15 0.033(2) 0.037(2) 0.032(2) -0.0006(18) 0.0059(18) 0.0009(18) C16 0.033(2) 0.059(3) 0.031(2) -0.009(2) 0.0084(19) -0.012(2) C17 0.032(2) 0.047(3) 0.038(2) -0.0027(19) 0.0120(19) -0.0013(19) C18 0.026(2) 0.036(2) 0.036(2) -0.0114(18) 0.0059(18) -0.0076(17) C19 0.047(3) 0.037(3) 0.061(3) 0.015(2) -0.004(2) -0.013(2) C20 0.026(2) 0.035(2) 0.071(3) 0.014(2) 0.010(2) -0.0017(18) C21 0.030(2) 0.027(2) 0.043(3) 0.0013(18) 0.0116(19) 0.0014(17) C22 0.029(2) 0.037(2) 0.048(3) -0.0121(19) 0.013(2) -0.0116(18) C23 0.038(3) 0.053(3) 0.050(3) -0.022(2) 0.025(2) -0.012(2) C24 0.029(2) 0.044(3) 0.035(2) -0.0010(19) 0.0037(19) -0.0032(19) C25 0.273(17) 0.149(9) 0.094(7) -0.021(7) 0.052(9) -0.132(11) C26 0.210(12) 0.067(5) 0.082(6) -0.029(4) 0.017(7) -0.014(6) C27 0.081(5) 0.087(5) 0.046(3) 0.003(3) -0.001(3) -0.030(4) C28 0.093(9) 0.43(3) 0.117(10) -0.055(13) 0.002(8) -0.004(12) C29 0.114(9) 0.165(12) 0.219(15) 0.022(11) -0.025(10) 0.011(8) C30 0.111(7) 0.208(11) 0.059(5) -0.037(6) -0.011(5) 0.073(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O17 2.152(3) 2_554 ? Mn1 O9 2.182(3) 2 ? Mn1 O19 2.191(3) . ? Mn1 O13 2.202(3) . ? Mn1 O4 2.217(3) . ? Mn1 O7 2.224(3) 1_545 ? Mn2 O6 2.111(3) . ? Mn2 O15 2.114(3) 2_554 ? Mn2 O18 2.121(3) 2_564 ? Mn2 O2W 2.149(4) . ? Mn2 O13 2.255(3) 1_565 ? Mn2 O1W 2.270(3) . ? Mn3 O16 2.114(3) 2_444 ? Mn3 O8 2.116(3) 2 ? Mn3 O20 2.145(4) . ? Mn3 O7 2.186(3) 1_545 ? Mn3 O1W 2.235(3) 1_445 ? Mn3 O4 2.263(3) . ? O1 C1 1.208(5) . ? O2 C2 1.205(5) . ? O3 C3 1.219(5) . ? O4 C6 1.282(5) . ? O5 C6 1.252(5) . ? O6 C9 1.234(5) . ? O7 C9 1.276(5) . ? O7 Mn3 2.186(3) 1_565 ? O7 Mn1 2.224(3) 1_565 ? O8 C12 1.250(5) . ? O8 Mn3 2.116(3) 2_554 ? O9 C12 1.273(5) . ? O9 Mn1 2.182(3) 2_554 ? O10 C13 1.216(5) . ? O11 C14 1.169(5) . ? O12 C15 1.224(5) . ? O13 C18 1.286(5) . ? O13 Mn2 2.255(3) 1_545 ? O14 C18 1.258(5) . ? O15 C21 1.261(5) . ? O15 Mn2 2.114(3) 2 ? O16 C21 1.271(5) . ? O16 Mn3 2.114(3) 2_645 ? O17 C24 1.260(5) . ? O17 Mn1 2.152(3) 2 ? O18 C24 1.248(5) . ? O18 Mn2 2.121(3) 2_565 ? O1W Mn3 2.235(3) 1_665 ? O1W H1WB 0.8498 . ? O1W H1WA 0.8499 . ? O19 C27 1.229(7) . ? O20 C30 1.116(9) . ? O2W H2WB 0.8495 . ? O2W H2WA 0.8500 . ? N1 C1 1.371(5) . ? N1 C3 1.379(5) . ? N1 C4 1.463(5) . ? N2 C1 1.380(5) . ? N2 C2 1.393(5) . ? N2 C7 1.474(5) . ? N3 C2 1.372(5) . ? N3 C3 1.398(5) . ? N3 C10 1.485(5) . ? N4 C13 1.369(6) . ? N4 C15 1.368(5) . ? N4 C16 1.489(5) . ? N5 C13 1.365(6) . ? N5 C14 1.391(6) . ? N5 C19 1.474(6) . ? N6 C15 1.382(5) . ? N6 C14 1.392(6) . ? N6 C22 1.478(5) . ? N7 C27 1.311(8) . ? N7 C26 1.411(10) . ? N7 C25 1.411(10) . ? N8 C29 1.352(11) . ? N8 C28 1.515(15) . ? N8 C30 1.570(12) . ? C4 C5 1.530(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.484(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C8 1.512(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.530(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.504(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.504(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C16 C17 1.530(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.466(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.470(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.520(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 C23 1.475(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.510(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O17 Mn1 O9 170.51(12) 2_554 2 ? O17 Mn1 O19 85.63(13) 2_554 . ? O9 Mn1 O19 85.08(12) 2 . ? O17 Mn1 O13 86.11(11) 2_554 . ? O9 Mn1 O13 95.76(11) 2 . ? O19 Mn1 O13 89.78(12) . . ? O17 Mn1 O4 90.95(11) 2_554 . ? O9 Mn1 O4 87.94(11) 2 . ? O19 Mn1 O4 94.87(12) . . ? O13 Mn1 O4 174.30(11) . . ? O17 Mn1 O7 97.30(11) 2_554 1_545 ? O9 Mn1 O7 91.58(11) 2 1_545 ? O19 Mn1 O7 170.51(12) . 1_545 ? O13 Mn1 O7 99.41(11) . 1_545 ? O4 Mn1 O7 76.11(10) . 1_545 ? O6 Mn2 O15 91.51(12) . 2_554 ? O6 Mn2 O18 91.77(13) . 2_564 ? O15 Mn2 O18 93.05(13) 2_554 2_564 ? O6 Mn2 O2W 95.22(16) . . ? O15 Mn2 O2W 91.38(15) 2_554 . ? O18 Mn2 O2W 171.62(17) 2_564 . ? O6 Mn2 O13 89.89(11) . 1_565 ? O15 Mn2 O13 175.52(13) 2_554 1_565 ? O18 Mn2 O13 91.16(12) 2_564 1_565 ? O2W Mn2 O13 84.26(14) . 1_565 ? O6 Mn2 O1W 175.48(11) . . ? O15 Mn2 O1W 92.25(11) 2_554 . ? O18 Mn2 O1W 85.52(13) 2_564 . ? O2W Mn2 O1W 87.21(16) . . ? O13 Mn2 O1W 86.55(10) 1_565 . ? O16 Mn3 O8 93.11(12) 2_444 2 ? O16 Mn3 O20 87.92(13) 2_444 . ? O8 Mn3 O20 176.19(15) 2 . ? O16 Mn3 O7 100.96(11) 2_444 1_545 ? O8 Mn3 O7 90.09(12) 2 1_545 ? O20 Mn3 O7 93.31(13) . 1_545 ? O16 Mn3 O1W 100.22(11) 2_444 1_445 ? O8 Mn3 O1W 84.14(13) 2 1_445 ? O20 Mn3 O1W 92.07(13) . 1_445 ? O7 Mn3 O1W 158.31(10) 1_545 1_445 ? O16 Mn3 O4 173.10(12) 2_444 . ? O8 Mn3 O4 93.06(11) 2 . ? O20 Mn3 O4 86.13(13) . . ? O7 Mn3 O4 75.93(10) 1_545 . ? O1W Mn3 O4 83.50(10) 1_445 . ? C6 O4 Mn1 137.7(3) . . ? C6 O4 Mn3 122.7(2) . . ? Mn1 O4 Mn3 97.30(10) . . ? C9 O6 Mn2 134.4(3) . . ? C9 O7 Mn3 131.3(2) . 1_565 ? C9 O7 Mn1 129.0(2) . 1_565 ? Mn3 O7 Mn1 99.40(11) 1_565 1_565 ? C12 O8 Mn3 131.2(3) . 2_554 ? C12 O9 Mn1 131.9(3) . 2_554 ? C18 O13 Mn1 129.3(3) . . ? C18 O13 Mn2 119.3(2) . 1_545 ? Mn1 O13 Mn2 111.10(12) . 1_545 ? C21 O15 Mn2 133.8(3) . 2 ? C21 O16 Mn3 125.1(3) . 2_645 ? C24 O17 Mn1 131.2(3) . 2 ? C24 O18 Mn2 129.5(3) . 2_565 ? Mn3 O1W Mn2 114.05(12) 1_665 . ? Mn3 O1W H1WB 107.2 1_665 . ? Mn2 O1W H1WB 116.3 . . ? Mn3 O1W H1WA 105.7 1_665 . ? Mn2 O1W H1WA 105.3 . . ? H1WB O1W H1WA 107.7 . . ? C27 O19 Mn1 134.8(4) . . ? C30 O20 Mn3 141.8(5) . . ? Mn2 O2W H2WB 115.0 . . ? Mn2 O2W H2WA 106.5 . . ? H2WB O2W H2WA 105.6 . . ? C1 N1 C3 124.1(3) . . ? C1 N1 C4 118.4(3) . . ? C3 N1 C4 117.3(3) . . ? C1 N2 C2 122.8(3) . . ? C1 N2 C7 118.5(3) . . ? C2 N2 C7 117.6(3) . . ? C2 N3 C3 124.1(3) . . ? C2 N3 C10 118.2(4) . . ? C3 N3 C10 117.7(4) . . ? C13 N4 C15 124.1(4) . . ? C13 N4 C16 118.0(4) . . ? C15 N4 C16 117.5(4) . . ? C13 N5 C14 124.2(4) . . ? C13 N5 C19 118.1(4) . . ? C14 N5 C19 116.9(4) . . ? C15 N6 C14 123.9(4) . . ? C15 N6 C22 117.6(4) . . ? C14 N6 C22 118.4(4) . . ? C27 N7 C26 120.5(6) . . ? C27 N7 C25 129.2(7) . . ? C26 N7 C25 110.0(7) . . ? C29 N8 C28 116.0(12) . . ? C29 N8 C30 117.0(11) . . ? C28 N8 C30 126.8(10) . . ? O1 C1 N1 122.5(4) . . ? O1 C1 N2 120.7(4) . . ? N1 C1 N2 116.7(3) . . ? O2 C2 N3 121.3(4) . . ? O2 C2 N2 122.4(4) . . ? N3 C2 N2 116.3(4) . . ? O3 C3 N1 122.9(4) . . ? O3 C3 N3 121.8(4) . . ? N1 C3 N3 115.3(3) . . ? N1 C4 C5 110.8(3) . . ? N1 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 114.9(3) . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? O5 C6 O4 123.7(4) . . ? O5 C6 C5 119.2(4) . . ? O4 C6 C5 117.1(4) . . ? N2 C7 C8 111.6(3) . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 110.1(3) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O6 C9 O7 124.1(4) . . ? O6 C9 C8 118.9(3) . . ? O7 C9 C8 117.0(3) . . ? N3 C10 C11 110.2(3) . . ? N3 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N3 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 115.5(4) . . ? C12 C11 H11A 108.4 . . ? C10 C11 H11A 108.4 . . ? C12 C11 H11B 108.4 . . ? C10 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? O8 C12 O9 125.2(4) . . ? O8 C12 C11 116.2(4) . . ? O9 C12 C11 118.6(4) . . ? O10 C13 N5 122.1(4) . . ? O10 C13 N4 121.2(4) . . ? N5 C13 N4 116.6(4) . . ? O11 C14 N6 122.5(4) . . ? O11 C14 N5 122.6(4) . . ? N6 C14 N5 114.8(3) . . ? O12 C15 N4 123.2(4) . . ? O12 C15 N6 120.7(4) . . ? N4 C15 N6 116.1(4) . . ? N4 C16 C17 110.1(3) . . ? N4 C16 H16A 109.6 . . ? C17 C16 H16A 109.6 . . ? N4 C16 H16B 109.6 . . ? C17 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C18 C17 C16 113.9(4) . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? O14 C18 O13 123.5(4) . . ? O14 C18 C17 118.4(4) . . ? O13 C18 C17 118.0(4) . . ? C20 C19 N5 115.4(4) . . ? C20 C19 H19A 108.4 . . ? N5 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? N5 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C19 C20 C21 111.4(4) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? O15 C21 O16 125.0(4) . . ? O15 C21 C20 117.1(4) . . ? O16 C21 C20 118.0(4) . . ? C23 C22 N6 111.4(3) . . ? C23 C22 H22A 109.3 . . ? N6 C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? N6 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 116.5(4) . . ? C22 C23 H23A 108.2 . . ? C24 C23 H23A 108.2 . . ? C22 C23 H23B 108.2 . . ? C24 C23 H23B 108.2 . . ? H23A C23 H23B 107.3 . . ? O18 C24 O17 125.5(4) . . ? O18 C24 C23 117.4(4) . . ? O17 C24 C23 116.9(4) . . ? N7 C25 H25A 109.5 . . ? N7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N7 C26 H26A 109.5 . . ? N7 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N7 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O19 C27 N7 126.6(6) . . ? O19 C27 H27 116.7 . . ? N7 C27 H27 116.7 . . ? N8 C28 H28A 109.5 . . ? N8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N8 C29 H29A 109.5 . . ? N8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O20 C30 N8 109.2(9) . . ? O20 C30 H30 125.4 . . ? N8 C30 H30 125.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O17 Mn1 O4 C6 -39.6(4) 2_554 . . . ? O9 Mn1 O4 C6 131.0(4) 2 . . . ? O19 Mn1 O4 C6 46.1(4) . . . . ? O13 Mn1 O4 C6 -98.4(11) . . . . ? O7 Mn1 O4 C6 -136.9(4) 1_545 . . . ? O17 Mn1 O4 Mn3 121.99(12) 2_554 . . . ? O9 Mn1 O4 Mn3 -67.43(12) 2 . . . ? O19 Mn1 O4 Mn3 -152.31(12) . . . . ? O13 Mn1 O4 Mn3 63.2(11) . . . . ? O7 Mn1 O4 Mn3 24.71(10) 1_545 . . . ? O16 Mn3 O4 C6 76.3(10) 2_444 . . . ? O8 Mn3 O4 C6 -130.5(3) 2 . . . ? O20 Mn3 O4 C6 45.8(3) . . . . ? O7 Mn3 O4 C6 140.2(3) 1_545 . . . ? O1W Mn3 O4 C6 -46.7(3) 1_445 . . . ? O16 Mn3 O4 Mn1 -89.1(9) 2_444 . . . ? O8 Mn3 O4 Mn1 64.13(13) 2 . . . ? O20 Mn3 O4 Mn1 -119.59(14) . . . . ? O7 Mn3 O4 Mn1 -25.19(11) 1_545 . . . ? O1W Mn3 O4 Mn1 147.88(12) 1_445 . . . ? O15 Mn2 O6 C9 -118.6(4) 2_554 . . . ? O18 Mn2 O6 C9 -25.5(4) 2_564 . . . ? O2W Mn2 O6 C9 149.9(4) . . . . ? O13 Mn2 O6 C9 65.7(4) 1_565 . . . ? O1W Mn2 O6 C9 27.7(18) . . . . ? O17 Mn1 O13 C18 113.9(3) 2_554 . . . ? O9 Mn1 O13 C18 -56.7(4) 2 . . . ? O19 Mn1 O13 C18 28.3(4) . . . . ? O4 Mn1 O13 C18 173.0(10) . . . . ? O7 Mn1 O13 C18 -149.3(3) 1_545 . . . ? O17 Mn1 O13 Mn2 -60.44(14) 2_554 . . 1_545 ? O9 Mn1 O13 Mn2 128.90(13) 2 . . 1_545 ? O19 Mn1 O13 Mn2 -146.07(15) . . . 1_545 ? O4 Mn1 O13 Mn2 -1.4(12) . . . 1_545 ? O7 Mn1 O13 Mn2 36.33(14) 1_545 . . 1_545 ? O6 Mn2 O1W Mn3 -171.7(15) . . . 1_665 ? O15 Mn2 O1W Mn3 -25.46(16) 2_554 . . 1_665 ? O18 Mn2 O1W Mn3 -118.35(15) 2_564 . . 1_665 ? O2W Mn2 O1W Mn3 65.80(17) . . . 1_665 ? O13 Mn2 O1W Mn3 150.21(15) 1_565 . . 1_665 ? O17 Mn1 O19 C27 -18.9(6) 2_554 . . . ? O9 Mn1 O19 C27 163.0(6) 2 . . . ? O13 Mn1 O19 C27 67.2(6) . . . . ? O4 Mn1 O19 C27 -109.5(6) . . . . ? O7 Mn1 O19 C27 -127.3(8) 1_545 . . . ? O16 Mn3 O20 C30 103.3(12) 2_444 . . . ? O8 Mn3 O20 C30 -2(3) 2 . . . ? O7 Mn3 O20 C30 -155.8(12) 1_545 . . . ? O1W Mn3 O20 C30 3.1(12) 1_445 . . . ? O4 Mn3 O20 C30 -80.2(12) . . . . ? C3 N1 C1 O1 -172.8(4) . . . . ? C4 N1 C1 O1 2.0(6) . . . . ? C3 N1 C1 N2 9.0(5) . . . . ? C4 N1 C1 N2 -176.3(3) . . . . ? C2 N2 C1 O1 172.4(4) . . . . ? C7 N2 C1 O1 4.3(6) . . . . ? C2 N2 C1 N1 -9.4(5) . . . . ? C7 N2 C1 N1 -177.5(3) . . . . ? C3 N3 C2 O2 -178.5(4) . . . . ? C10 N3 C2 O2 -1.2(6) . . . . ? C3 N3 C2 N2 2.4(6) . . . . ? C10 N3 C2 N2 179.8(3) . . . . ? C1 N2 C2 O2 -175.0(4) . . . . ? C7 N2 C2 O2 -6.8(6) . . . . ? C1 N2 C2 N3 4.0(6) . . . . ? C7 N2 C2 N3 172.2(4) . . . . ? C1 N1 C3 O3 176.1(4) . . . . ? C4 N1 C3 O3 1.2(6) . . . . ? C1 N1 C3 N3 -3.1(5) . . . . ? C4 N1 C3 N3 -177.9(3) . . . . ? C2 N3 C3 O3 177.9(4) . . . . ? C10 N3 C3 O3 0.6(6) . . . . ? C2 N3 C3 N1 -2.9(6) . . . . ? C10 N3 C3 N1 179.7(3) . . . . ? C1 N1 C4 C5 -78.1(4) . . . . ? C3 N1 C4 C5 97.0(4) . . . . ? N1 C4 C5 C6 -178.2(4) . . . . ? Mn1 O4 C6 O5 -172.6(3) . . . . ? Mn3 O4 C6 O5 29.2(5) . . . . ? Mn1 O4 C6 C5 6.3(6) . . . . ? Mn3 O4 C6 C5 -151.9(3) . . . . ? C4 C5 C6 O5 0.4(6) . . . . ? C4 C5 C6 O4 -178.6(4) . . . . ? C1 N2 C7 C8 -77.6(5) . . . . ? C2 N2 C7 C8 113.7(4) . . . . ? N2 C7 C8 C9 179.0(4) . . . . ? Mn2 O6 C9 O7 -52.6(6) . . . . ? Mn2 O6 C9 C8 126.2(4) . . . . ? Mn3 O7 C9 O6 -154.3(3) 1_565 . . . ? Mn1 O7 C9 O6 18.6(6) 1_565 . . . ? Mn3 O7 C9 C8 26.9(5) 1_565 . . . ? Mn1 O7 C9 C8 -160.2(3) 1_565 . . . ? C7 C8 C9 O6 -3.5(5) . . . . ? C7 C8 C9 O7 175.4(4) . . . . ? C2 N3 C10 C11 -89.3(5) . . . . ? C3 N3 C10 C11 88.2(5) . . . . ? N3 C10 C11 C12 171.9(4) . . . . ? Mn3 O8 C12 O9 20.1(7) 2_554 . . . ? Mn3 O8 C12 C11 -159.9(3) 2_554 . . . ? Mn1 O9 C12 O8 -8.0(6) 2_554 . . . ? Mn1 O9 C12 C11 172.0(3) 2_554 . . . ? C10 C11 C12 O8 -174.7(4) . . . . ? C10 C11 C12 O9 5.2(6) . . . . ? C14 N5 C13 O10 178.7(5) . . . . ? C19 N5 C13 O10 -12.0(7) . . . . ? C14 N5 C13 N4 -3.4(7) . . . . ? C19 N5 C13 N4 165.9(4) . . . . ? C15 N4 C13 O10 178.0(5) . . . . ? C16 N4 C13 O10 5.7(7) . . . . ? C15 N4 C13 N5 0.0(7) . . . . ? C16 N4 C13 N5 -172.3(4) . . . . ? C15 N6 C14 O11 -176.2(5) . . . . ? C22 N6 C14 O11 5.3(7) . . . . ? C15 N6 C14 N5 1.6(6) . . . . ? C22 N6 C14 N5 -176.9(3) . . . . ? C13 N5 C14 O11 -179.7(5) . . . . ? C19 N5 C14 O11 10.9(7) . . . . ? C13 N5 C14 N6 2.6(6) . . . . ? C19 N5 C14 N6 -166.9(4) . . . . ? C13 N4 C15 O12 -174.7(5) . . . . ? C16 N4 C15 O12 -2.4(6) . . . . ? C13 N4 C15 N6 3.7(6) . . . . ? C16 N4 C15 N6 176.0(4) . . . . ? C14 N6 C15 O12 173.9(4) . . . . ? C22 N6 C15 O12 -7.6(6) . . . . ? C14 N6 C15 N4 -4.5(6) . . . . ? C22 N6 C15 N4 174.0(4) . . . . ? C13 N4 C16 C17 86.7(5) . . . . ? C15 N4 C16 C17 -86.1(5) . . . . ? N4 C16 C17 C18 -167.5(4) . . . . ? Mn1 O13 C18 O14 -134.6(4) . . . . ? Mn2 O13 C18 O14 39.3(6) 1_545 . . . ? Mn1 O13 C18 C17 47.2(6) . . . . ? Mn2 O13 C18 C17 -138.8(3) 1_545 . . . ? C16 C17 C18 O14 6.5(6) . . . . ? C16 C17 C18 O13 -175.2(4) . . . . ? C13 N5 C19 C20 87.3(6) . . . . ? C14 N5 C19 C20 -102.6(5) . . . . ? N5 C19 C20 C21 175.8(4) . . . . ? Mn2 O15 C21 O16 27.1(7) 2 . . . ? Mn2 O15 C21 C20 -153.5(3) 2 . . . ? Mn3 O16 C21 O15 37.1(6) 2_645 . . . ? Mn3 O16 C21 C20 -142.3(3) 2_645 . . . ? C19 C20 C21 O15 -11.8(6) . . . . ? C19 C20 C21 O16 167.6(4) . . . . ? C15 N6 C22 C23 -71.3(5) . . . . ? C14 N6 C22 C23 107.3(5) . . . . ? N6 C22 C23 C24 -161.4(4) . . . . ? Mn2 O18 C24 O17 53.3(6) 2_565 . . . ? Mn2 O18 C24 C23 -121.9(4) 2_565 . . . ? Mn1 O17 C24 O18 -16.3(7) 2 . . . ? Mn1 O17 C24 C23 159.0(3) 2 . . . ? C22 C23 C24 O18 -161.0(5) . . . . ? C22 C23 C24 O17 23.3(7) . . . . ? Mn1 O19 C27 N7 -169.6(5) . . . . ? C26 N7 C27 O19 2.0(13) . . . . ? C25 N7 C27 O19 -170.3(11) . . . . ? Mn3 O20 C30 N8 126.0(8) . . . . ? C29 N8 C30 O20 -165.2(10) . . . . ? C28 N8 C30 O20 9.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.958 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.067 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.085 0.312 0.452 447 95 ' ' 2 0.085 -0.312 0.952 447 95 ' ' _platon_squeeze_details ; ; #====================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 842230' #TrackingRef '- ZBHAN110923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H78 Mn3 N12 O24' _chemical_formula_weight 1372.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3147(15) _cell_length_b 12.5692(13) _cell_length_c 17.753(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.401(6) _cell_angle_gamma 90.00 _cell_volume 3184.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1434 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7905 _exptl_absorpt_correction_T_max 0.8471 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26699 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6262 _reflns_number_gt 5374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+3.0458P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6262 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.83309(2) 0.56594(3) 0.145332(19) 0.03183(11) Uani 1 1 d . . . Mn2 Mn 1.0000 0.5000 0.0000 0.02617(12) Uani 1 2 d S . . C1 C 1.06559(16) 0.04381(18) 0.18315(13) 0.0336(5) Uani 1 1 d . . . C2 C 1.14420(17) -0.05856(18) 0.28645(13) 0.0346(5) Uani 1 1 d . . . C3 C 1.17876(16) 0.13073(18) 0.27275(13) 0.0345(5) Uani 1 1 d . . . C4 C 1.09654(17) 0.23411(17) 0.17097(13) 0.0349(5) Uani 1 1 d . . . H4A H 1.0813 0.2218 0.1175 0.042 Uiso 1 1 calc R . . H4B H 1.1517 0.2791 0.1764 0.042 Uiso 1 1 calc R . . C5 C 1.01606(18) 0.28954(19) 0.20402(14) 0.0392(5) Uani 1 1 d . . . H5A H 1.0357 0.3115 0.2552 0.047 Uiso 1 1 calc R . . H5B H 0.9650 0.2393 0.2068 0.047 Uiso 1 1 calc R . . C6 C 0.98026(16) 0.38616(17) 0.15956(12) 0.0314(5) Uani 1 1 d . . . C7 C 1.02413(17) -0.14300(18) 0.19991(14) 0.0384(5) Uani 1 1 d . . . H7A H 0.9606 -0.1204 0.1851 0.046 Uiso 1 1 calc R . . H7B H 1.0218 -0.1914 0.2423 0.046 Uiso 1 1 calc R . . C8 C 1.06305(18) -0.20123(19) 0.13467(15) 0.0414(6) Uani 1 1 d . . . H8A H 1.1276 -0.2209 0.1488 0.050 Uiso 1 1 calc R . . H8B H 1.0629 -0.1536 0.0917 0.050 Uiso 1 1 calc R . . C9 C 1.00796(17) -0.30057(17) 0.11155(14) 0.0352(5) Uani 1 1 d . . . C10 C 1.26214(17) 0.0272(2) 0.37382(13) 0.0379(5) Uani 1 1 d . . . H10A H 1.3150 0.0731 0.3659 0.045 Uiso 1 1 calc R . . H10B H 1.2852 -0.0450 0.3799 0.045 Uiso 1 1 calc R . . C11 C 1.2182(2) 0.0612(2) 0.44472(14) 0.0502(7) Uani 1 1 d . . . H11A H 1.2147 0.1382 0.4454 0.060 Uiso 1 1 calc R . . H11B H 1.1546 0.0341 0.4425 0.060 Uiso 1 1 calc R . . C12 C 1.26903(16) 0.02452(18) 0.51754(13) 0.0342(5) Uani 1 1 d . . . C13 C 0.7150(2) 0.5101(3) 0.3831(2) 0.0619(8) Uani 1 1 d . . . H13A H 0.7328 0.4664 0.3422 0.093 Uiso 1 1 calc R . . H13B H 0.6504 0.4976 0.3912 0.093 Uiso 1 1 calc R . . H13C H 0.7533 0.4928 0.4282 0.093 Uiso 1 1 calc R . . C14 C 0.7041(3) 0.6984(3) 0.42216(17) 0.0680(9) Uani 1 1 d . . . H14A H 0.7143 0.7695 0.4048 0.102 Uiso 1 1 calc R . . H14B H 0.7428 0.6858 0.4679 0.102 Uiso 1 1 calc R . . H14C H 0.6394 0.6900 0.4318 0.102 Uiso 1 1 calc R . . C15 C 0.7846(3) 0.7633(2) 0.28578(19) 0.0647(9) Uani 1 1 d . . . H15A H 0.8119 0.7694 0.2382 0.097 Uiso 1 1 calc R . . H15B H 0.8273 0.7913 0.3253 0.097 Uiso 1 1 calc R . . H15C H 0.7271 0.8028 0.2838 0.097 Uiso 1 1 calc R . . C16 C 0.76518(19) 0.6486(2) 0.30140(15) 0.0455(6) Uani 1 1 d . . . C17 C 0.5332(3) 0.6997(5) -0.0250(3) 0.119(2) Uani 1 1 d . . . H17A H 0.4781 0.7354 -0.0105 0.178 Uiso 1 1 calc R . . H17B H 0.5165 0.6303 -0.0443 0.178 Uiso 1 1 calc R . . H17C H 0.5608 0.7402 -0.0633 0.178 Uiso 1 1 calc R . . C18 C 0.5579(3) 0.6299(5) 0.1125(3) 0.123(2) Uani 1 1 d . . . H18A H 0.6062 0.6247 0.1529 0.185 Uiso 1 1 calc R . . H18B H 0.5366 0.5598 0.0980 0.185 Uiso 1 1 calc R . . H18C H 0.5064 0.6703 0.1290 0.185 Uiso 1 1 calc R . . C19 C 0.7214(4) 0.7663(3) -0.0155(2) 0.1031(16) Uani 1 1 d . . . H19A H 0.7190 0.7182 -0.0576 0.155 Uiso 1 1 calc R . . H19B H 0.7852 0.7869 -0.0025 0.155 Uiso 1 1 calc R . . H19C H 0.6847 0.8284 -0.0289 0.155 Uiso 1 1 calc R . . C20 C 0.6815(4) 0.7106(3) 0.0532(3) 0.0941(15) Uani 1 1 d . . . C21 C 0.5440(3) 0.9725(5) 0.1135(3) 0.1090(17) Uani 1 1 d . . . H21A H 0.5441 0.9221 0.0729 0.164 Uiso 1 1 calc R . . H21B H 0.5797 0.9447 0.1571 0.164 Uiso 1 1 calc R . . H21C H 0.5713 1.0381 0.0985 0.164 Uiso 1 1 calc R . . C22 C 0.4231(3) 1.0716(3) 0.1956(2) 0.0928(13) Uani 1 1 d . . . H22A H 0.3752 1.1236 0.1836 0.139 Uiso 1 1 calc R . . H22B H 0.4830 1.1063 0.2017 0.139 Uiso 1 1 calc R . . H22C H 0.4111 1.0361 0.2418 0.139 Uiso 1 1 calc R . . C23 C 0.2819(3) 0.9594(4) 0.1248(3) 0.0839(12) Uani 1 1 d . . . H23A H 0.2813 1.0142 0.1624 0.126 Uiso 1 1 calc R . . H23B H 0.2594 0.8941 0.1449 0.126 Uiso 1 1 calc R . . H23C H 0.2421 0.9797 0.0812 0.126 Uiso 1 1 calc R . . C24 C 0.3988(8) 0.9408(4) 0.0985(3) 0.177(4) Uani 1 1 d . . . N1 N 1.11673(13) 0.13141(14) 0.20940(11) 0.0318(4) Uani 1 1 d . . . N2 N 1.08078(14) -0.04887(14) 0.22422(11) 0.0336(4) Uani 1 1 d . . . N3 N 1.19378(14) 0.03281(15) 0.30701(10) 0.0337(4) Uani 1 1 d . . . N4 N 0.72810(16) 0.62220(19) 0.36430(13) 0.0492(5) Uani 1 1 d . . . N5 N 0.5996(3) 0.6893(4) 0.0400(3) 0.1146(16) Uani 1 1 d . . . N6 N 0.4234(5) 0.9965(3) 0.1365(2) 0.139(2) Uani 1 1 d . . . O1 O 1.01172(14) 0.04803(15) 0.12773(11) 0.0536(5) Uani 1 1 d . . . O2 O 1.15618(15) -0.14088(14) 0.32046(11) 0.0535(5) Uani 1 1 d . . . O3 O 1.21847(14) 0.20996(14) 0.29606(11) 0.0546(5) Uani 1 1 d . . . O4 O 1.02164(13) 0.41202(14) 0.10352(10) 0.0444(4) Uani 1 1 d . . . O5 O 0.91087(13) 0.43182(14) 0.18395(10) 0.0447(4) Uani 1 1 d . . . O6 O 0.94052(13) -0.32282(15) 0.14992(11) 0.0507(5) Uani 1 1 d . . . O7 O 1.03409(13) -0.35171(14) 0.05703(11) 0.0477(4) Uani 1 1 d . . . O8 O 1.34702(11) -0.02291(13) 0.51685(9) 0.0357(4) Uani 1 1 d . . . O9 O 1.22942(13) 0.03662(15) 0.57691(10) 0.0463(4) Uani 1 1 d . . . O10 O 0.78455(15) 0.57733(15) 0.25546(11) 0.0546(5) Uani 1 1 d . . . O11 O 0.73104(16) 0.69299(18) 0.11187(13) 0.0673(6) Uani 1 1 d . . . O12 O 0.4007(2) 0.8750(3) 0.0504(2) 0.1232(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0353(2) 0.02801(18) 0.03213(19) -0.00320(13) 0.00230(14) 0.00067(13) Mn2 0.0325(2) 0.0221(2) 0.0237(2) 0.00046(17) 0.00122(17) -0.00078(17) C1 0.0354(12) 0.0281(11) 0.0364(12) -0.0022(9) -0.0041(10) 0.0027(9) C2 0.0426(13) 0.0284(11) 0.0321(11) -0.0011(9) -0.0009(10) 0.0019(9) C3 0.0372(12) 0.0293(11) 0.0359(12) -0.0016(9) -0.0038(9) -0.0004(9) C4 0.0413(13) 0.0262(11) 0.0368(12) 0.0065(9) 0.0004(10) 0.0010(9) C5 0.0510(14) 0.0327(12) 0.0346(12) 0.0095(10) 0.0073(10) 0.0077(11) C6 0.0376(12) 0.0259(11) 0.0300(11) 0.0016(9) -0.0022(9) 0.0007(9) C7 0.0410(13) 0.0265(11) 0.0469(14) -0.0057(10) -0.0010(10) -0.0071(10) C8 0.0419(13) 0.0299(12) 0.0521(15) -0.0102(11) 0.0018(11) -0.0054(10) C9 0.0381(13) 0.0240(10) 0.0420(13) -0.0020(9) -0.0069(10) 0.0006(9) C10 0.0394(13) 0.0398(13) 0.0327(12) -0.0009(10) -0.0082(10) 0.0046(10) C11 0.0552(16) 0.0576(17) 0.0363(13) -0.0028(12) -0.0063(12) 0.0225(13) C12 0.0374(12) 0.0299(11) 0.0340(12) -0.0013(9) -0.0044(10) -0.0008(9) C13 0.0585(19) 0.0609(19) 0.068(2) 0.0088(16) 0.0152(15) -0.0009(15) C14 0.089(2) 0.071(2) 0.0462(17) -0.0109(15) 0.0198(16) 0.0126(18) C15 0.089(2) 0.0478(17) 0.0601(19) -0.0042(14) 0.0248(17) 0.0012(16) C16 0.0450(14) 0.0505(15) 0.0409(14) -0.0027(12) 0.0033(11) 0.0091(12) C17 0.088(3) 0.176(5) 0.087(3) -0.039(3) -0.031(2) 0.055(3) C18 0.088(3) 0.174(6) 0.113(4) -0.021(4) 0.045(3) -0.007(3) C19 0.179(5) 0.067(2) 0.065(2) 0.002(2) 0.023(3) -0.006(3) C20 0.107(3) 0.068(2) 0.102(3) -0.037(2) -0.026(3) 0.045(2) C21 0.046(2) 0.169(5) 0.111(4) -0.002(3) 0.003(2) -0.015(3) C22 0.113(3) 0.079(3) 0.083(3) -0.022(2) -0.018(2) 0.012(2) C23 0.058(2) 0.104(3) 0.094(3) 0.007(2) 0.029(2) 0.002(2) C24 0.401(14) 0.078(3) 0.051(3) -0.004(3) 0.004(5) -0.016(5) N1 0.0362(10) 0.0228(9) 0.0354(10) 0.0008(7) -0.0049(8) 0.0009(7) N2 0.0406(11) 0.0225(9) 0.0366(10) -0.0034(8) -0.0039(8) -0.0024(8) N3 0.0400(11) 0.0294(9) 0.0301(10) -0.0010(8) -0.0076(8) 0.0011(8) N4 0.0526(13) 0.0531(14) 0.0429(12) -0.0056(10) 0.0093(10) 0.0071(11) N5 0.082(2) 0.128(3) 0.126(3) -0.049(3) -0.039(2) 0.046(2) N6 0.290(7) 0.070(2) 0.052(2) -0.0097(18) -0.019(3) 0.005(3) O1 0.0597(12) 0.0401(10) 0.0558(12) 0.0019(8) -0.0287(10) -0.0024(9) O2 0.0753(13) 0.0318(9) 0.0510(11) 0.0113(8) -0.0112(10) -0.0021(9) O3 0.0669(13) 0.0333(9) 0.0594(12) -0.0005(8) -0.0223(10) -0.0139(9) O4 0.0483(10) 0.0466(10) 0.0388(9) 0.0188(8) 0.0075(8) 0.0096(8) O5 0.0517(11) 0.0382(9) 0.0450(10) 0.0061(8) 0.0095(8) 0.0132(8) O6 0.0538(11) 0.0416(10) 0.0575(11) -0.0136(9) 0.0093(9) -0.0173(9) O7 0.0543(11) 0.0342(9) 0.0548(11) -0.0158(8) 0.0052(9) -0.0069(8) O8 0.0327(8) 0.0389(9) 0.0347(8) 0.0029(7) -0.0013(7) 0.0031(7) O9 0.0477(10) 0.0540(11) 0.0378(10) 0.0009(8) 0.0061(8) 0.0090(8) O10 0.0753(14) 0.0472(11) 0.0436(10) -0.0037(9) 0.0197(10) 0.0130(10) O11 0.0750(15) 0.0624(13) 0.0611(13) -0.0085(11) -0.0163(11) 0.0291(11) O12 0.099(2) 0.156(3) 0.116(2) -0.083(3) 0.0223(19) -0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O6 2.0754(18) 1_565 ? Mn1 O5 2.1058(17) . ? Mn1 O10 2.1294(19) . ? Mn1 O11 2.214(2) . ? Mn1 O9 2.2500(18) 4_565 ? Mn1 O8 2.3674(16) 4_565 ? Mn1 C12 2.638(2) 4_565 ? Mn2 O4 2.1469(16) . ? Mn2 O4 2.1469(16) 3_765 ? Mn2 O7 2.1590(16) 3_755 ? Mn2 O7 2.1590(16) 1_565 ? Mn2 O8 2.2514(16) 4_565 ? Mn2 O8 2.2514(16) 2_755 ? C1 O1 1.204(3) . ? C1 N2 1.383(3) . ? C1 N1 1.383(3) . ? C2 O2 1.204(3) . ? C2 N2 1.381(3) . ? C2 N3 1.384(3) . ? C3 O3 1.204(3) . ? C3 N1 1.378(3) . ? C3 N3 1.382(3) . ? C4 N1 1.478(3) . ? C4 C5 1.504(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.516(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O4 1.240(3) . ? C6 O5 1.253(3) . ? C7 N2 1.480(3) . ? C7 C8 1.512(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.516(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O7 1.243(3) . ? C9 O6 1.255(3) . ? C10 N3 1.480(3) . ? C10 C11 1.511(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.506(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O9 1.244(3) . ? C12 O8 1.266(3) . ? C12 Mn1 2.638(2) 4_666 ? C13 N4 1.463(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N4 1.465(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.498(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 O10 1.257(3) . ? C16 N4 1.315(3) . ? C17 N5 1.443(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N5 1.640(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.554(7) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N5 1.208(6) . ? C20 O11 1.234(5) . ? C21 N6 1.829(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N6 1.412(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.786(11) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N6 1.016(7) . ? C24 O12 1.191(6) . ? O6 Mn1 2.0754(18) 1_545 ? O7 Mn2 2.1590(16) 1_545 ? O8 Mn2 2.2514(16) 2_745 ? O8 Mn1 2.3674(16) 4_666 ? O9 Mn1 2.2500(18) 4_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mn1 O5 98.91(8) 1_565 . ? O6 Mn1 O10 102.22(8) 1_565 . ? O5 Mn1 O10 87.51(7) . . ? O6 Mn1 O11 89.79(9) 1_565 . ? O5 Mn1 O11 170.42(9) . . ? O10 Mn1 O11 86.72(8) . . ? O6 Mn1 O9 149.67(7) 1_565 4_565 ? O5 Mn1 O9 91.57(7) . 4_565 ? O10 Mn1 O9 106.62(8) . 4_565 ? O11 Mn1 O9 82.77(8) . 4_565 ? O6 Mn1 O8 94.29(7) 1_565 4_565 ? O5 Mn1 O8 92.83(6) . 4_565 ? O10 Mn1 O8 163.24(7) . 4_565 ? O11 Mn1 O8 90.51(7) . 4_565 ? O9 Mn1 O8 56.62(6) 4_565 4_565 ? O6 Mn1 C12 122.11(8) 1_565 4_565 ? O5 Mn1 C12 94.31(7) . 4_565 ? O10 Mn1 C12 134.60(8) . 4_565 ? O11 Mn1 C12 84.35(8) . 4_565 ? O9 Mn1 C12 28.07(7) 4_565 4_565 ? O8 Mn1 C12 28.66(7) 4_565 4_565 ? O4 Mn2 O4 180.00(9) . 3_765 ? O4 Mn2 O7 88.24(7) . 3_755 ? O4 Mn2 O7 91.76(7) 3_765 3_755 ? O4 Mn2 O7 91.76(7) . 1_565 ? O4 Mn2 O7 88.24(7) 3_765 1_565 ? O7 Mn2 O7 180.00(9) 3_755 1_565 ? O4 Mn2 O8 91.72(6) . 4_565 ? O4 Mn2 O8 88.28(6) 3_765 4_565 ? O7 Mn2 O8 89.17(6) 3_755 4_565 ? O7 Mn2 O8 90.83(6) 1_565 4_565 ? O4 Mn2 O8 88.28(6) . 2_755 ? O4 Mn2 O8 91.72(6) 3_765 2_755 ? O7 Mn2 O8 90.83(6) 3_755 2_755 ? O7 Mn2 O8 89.17(6) 1_565 2_755 ? O8 Mn2 O8 180.00(8) 4_565 2_755 ? O1 C1 N2 122.2(2) . . ? O1 C1 N1 122.0(2) . . ? N2 C1 N1 115.80(19) . . ? O2 C2 N2 122.5(2) . . ? O2 C2 N3 122.0(2) . . ? N2 C2 N3 115.48(19) . . ? O3 C3 N1 122.2(2) . . ? O3 C3 N3 122.1(2) . . ? N1 C3 N3 115.67(19) . . ? N1 C4 C5 110.68(19) . . ? N1 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 113.99(19) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? O4 C6 O5 126.7(2) . . ? O4 C6 C5 117.7(2) . . ? O5 C6 C5 115.6(2) . . ? N2 C7 C8 112.6(2) . . ? N2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C9 113.0(2) . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? O7 C9 O6 126.7(2) . . ? O7 C9 C8 117.1(2) . . ? O6 C9 C8 116.2(2) . . ? N3 C10 C11 111.2(2) . . ? N3 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N3 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 115.1(2) . . ? C12 C11 H11A 108.5 . . ? C10 C11 H11A 108.5 . . ? C12 C11 H11B 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O9 C12 O8 121.7(2) . . ? O9 C12 C11 117.9(2) . . ? O8 C12 C11 120.3(2) . . ? O9 C12 Mn1 58.33(12) . 4_666 ? O8 C12 Mn1 63.71(12) . 4_666 ? C11 C12 Mn1 169.41(19) . 4_666 ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O10 C16 N4 119.6(3) . . ? O10 C16 C15 120.8(2) . . ? N4 C16 C15 119.5(2) . . ? N5 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N5 C20 O11 127.6(6) . . ? N5 C20 C19 111.0(5) . . ? O11 C20 C19 121.4(5) . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 H22A 109.5 . . ? N6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 O12 158.2(12) . . ? N6 C24 C23 91.2(7) . . ? O12 C24 C23 110.6(7) . . ? C3 N1 C1 124.13(18) . . ? C3 N1 C4 118.22(18) . . ? C1 N1 C4 117.38(18) . . ? C2 N2 C1 124.30(19) . . ? C2 N2 C7 118.35(19) . . ? C1 N2 C7 117.35(19) . . ? C3 N3 C2 124.29(19) . . ? C3 N3 C10 117.74(19) . . ? C2 N3 C10 117.78(19) . . ? C16 N4 C13 120.2(2) . . ? C16 N4 C14 124.2(3) . . ? C13 N4 C14 115.4(3) . . ? C20 N5 C17 134.8(6) . . ? C20 N5 C18 110.8(4) . . ? C17 N5 C18 114.3(4) . . ? C24 N6 C22 159.0(10) . . ? C24 N6 C21 91.4(7) . . ? C22 N6 C21 109.4(5) . . ? C6 O4 Mn2 140.86(16) . . ? C6 O5 Mn1 131.88(15) . . ? C9 O6 Mn1 136.67(16) . 1_545 ? C9 O7 Mn2 137.80(17) . 1_545 ? C12 O8 Mn2 143.92(15) . 2_745 ? C12 O8 Mn1 87.64(13) . 4_666 ? Mn2 O8 Mn1 108.18(6) 2_745 4_666 ? C12 O9 Mn1 93.60(14) . 4_666 ? C16 O10 Mn1 138.37(19) . . ? C20 O11 Mn1 132.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C4 C5 C6 -170.32(19) . . . . ? C4 C5 C6 O4 -2.6(3) . . . . ? C4 C5 C6 O5 177.4(2) . . . . ? N2 C7 C8 C9 177.48(19) . . . . ? C7 C8 C9 O7 178.3(2) . . . . ? C7 C8 C9 O6 -1.9(3) . . . . ? N3 C10 C11 C12 160.3(2) . . . . ? C10 C11 C12 O9 -169.9(2) . . . . ? C10 C11 C12 O8 5.9(4) . . . . ? C10 C11 C12 Mn1 -103.4(10) . . . 4_666 ? O3 C3 N1 C1 -176.1(2) . . . . ? N3 C3 N1 C1 5.0(3) . . . . ? O3 C3 N1 C4 -2.2(4) . . . . ? N3 C3 N1 C4 179.0(2) . . . . ? O1 C1 N1 C3 179.6(2) . . . . ? N2 C1 N1 C3 -0.9(3) . . . . ? O1 C1 N1 C4 5.6(4) . . . . ? N2 C1 N1 C4 -174.9(2) . . . . ? C5 C4 N1 C3 -88.8(3) . . . . ? C5 C4 N1 C1 85.6(3) . . . . ? O2 C2 N2 C1 -179.3(2) . . . . ? N3 C2 N2 C1 0.3(3) . . . . ? O2 C2 N2 C7 1.5(4) . . . . ? N3 C2 N2 C7 -178.9(2) . . . . ? O1 C1 N2 C2 177.6(2) . . . . ? N1 C1 N2 C2 -2.0(3) . . . . ? O1 C1 N2 C7 -3.2(4) . . . . ? N1 C1 N2 C7 177.3(2) . . . . ? C8 C7 N2 C2 -99.2(3) . . . . ? C8 C7 N2 C1 81.6(3) . . . . ? O3 C3 N3 C2 174.2(2) . . . . ? N1 C3 N3 C2 -6.9(3) . . . . ? O3 C3 N3 C10 -0.8(4) . . . . ? N1 C3 N3 C10 178.1(2) . . . . ? O2 C2 N3 C3 -176.0(2) . . . . ? N2 C2 N3 C3 4.4(3) . . . . ? O2 C2 N3 C10 -0.9(4) . . . . ? N2 C2 N3 C10 179.4(2) . . . . ? C11 C10 N3 C3 82.1(3) . . . . ? C11 C10 N3 C2 -93.3(3) . . . . ? O10 C16 N4 C13 3.9(4) . . . . ? C15 C16 N4 C13 -175.5(3) . . . . ? O10 C16 N4 C14 179.1(3) . . . . ? C15 C16 N4 C14 -0.4(4) . . . . ? O11 C20 N5 C17 -176.9(4) . . . . ? C19 C20 N5 C17 3.1(7) . . . . ? O11 C20 N5 C18 -0.2(6) . . . . ? C19 C20 N5 C18 179.7(3) . . . . ? O12 C24 N6 C22 -174.0(11) . . . . ? C23 C24 N6 C22 5.7(16) . . . . ? O12 C24 N6 C21 -2.6(17) . . . . ? C23 C24 N6 C21 177.1(3) . . . . ? O5 C6 O4 Mn2 -21.8(4) . . . . ? C5 C6 O4 Mn2 158.1(2) . . . . ? O4 Mn2 O4 C6 75(100) 3_765 . . . ? O7 Mn2 O4 C6 -96.3(3) 3_755 . . . ? O7 Mn2 O4 C6 83.7(3) 1_565 . . . ? O8 Mn2 O4 C6 -7.2(3) 4_565 . . . ? O8 Mn2 O4 C6 172.8(3) 2_755 . . . ? O4 C6 O5 Mn1 0.4(4) . . . . ? C5 C6 O5 Mn1 -179.58(16) . . . . ? O6 Mn1 O5 C6 -58.3(2) 1_565 . . . ? O10 Mn1 O5 C6 -160.3(2) . . . . ? O11 Mn1 O5 C6 146.7(4) . . . . ? O9 Mn1 O5 C6 93.1(2) 4_565 . . . ? O8 Mn1 O5 C6 36.4(2) 4_565 . . . ? C12 Mn1 O5 C6 65.1(2) 4_565 . . . ? O7 C9 O6 Mn1 -6.4(4) . . . 1_545 ? C8 C9 O6 Mn1 173.88(18) . . . 1_545 ? O6 C9 O7 Mn2 -5.9(4) . . . 1_545 ? C8 C9 O7 Mn2 173.84(18) . . . 1_545 ? O9 C12 O8 Mn2 -111.5(3) . . . 2_745 ? C11 C12 O8 Mn2 72.9(3) . . . 2_745 ? Mn1 C12 O8 Mn2 -118.3(2) 4_666 . . 2_745 ? O9 C12 O8 Mn1 6.7(2) . . . 4_666 ? C11 C12 O8 Mn1 -168.8(2) . . . 4_666 ? O8 C12 O9 Mn1 -7.1(2) . . . 4_666 ? C11 C12 O9 Mn1 168.6(2) . . . 4_666 ? N4 C16 O10 Mn1 174.1(2) . . . . ? C15 C16 O10 Mn1 -6.5(5) . . . . ? O6 Mn1 O10 C16 44.3(3) 1_565 . . . ? O5 Mn1 O10 C16 142.9(3) . . . . ? O11 Mn1 O10 C16 -44.7(3) . . . . ? O9 Mn1 O10 C16 -126.2(3) 4_565 . . . ? O8 Mn1 O10 C16 -125.6(3) 4_565 . . . ? C12 Mn1 O10 C16 -123.5(3) 4_565 . . . ? N5 C20 O11 Mn1 98.5(5) . . . . ? C19 C20 O11 Mn1 -81.4(5) . . . . ? O6 Mn1 O11 C20 113.4(4) 1_565 . . . ? O5 Mn1 O11 C20 -91.3(6) . . . . ? O10 Mn1 O11 C20 -144.3(4) . . . . ? O9 Mn1 O11 C20 -37.1(4) 4_565 . . . ? O8 Mn1 O11 C20 19.1(4) 4_565 . . . ? C12 Mn1 O11 C20 -8.9(4) 4_565 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.863 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.055 #======================== data_3 _database_code_depnum_ccdc_archive 'CCDC 842231' #TrackingRef '- ZBHAN110923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H19 Mn N4 O10' _chemical_formula_weight 506.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1120(11) _cell_length_b 23.1084(19) _cell_length_c 6.7362(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.9860(10) _cell_angle_gamma 90.00 _cell_volume 2038.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7789 _exptl_absorpt_correction_T_max 0.8315 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10974 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4002 _reflns_number_gt 3013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+5.7359P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4002 _refine_ls_number_parameters 306 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.05737(5) 0.70834(3) 0.22696(10) 0.0194(2) Uani 1 1 d . . . C1 C 0.4697(4) 0.6310(2) 0.8872(7) 0.0291(11) Uani 1 1 d . . . C2 C 0.6500(4) 0.6500(2) 0.9583(7) 0.0294(11) Uani 1 1 d . . . C3 C 0.5637(4) 0.6907(2) 0.6624(7) 0.0229(10) Uani 1 1 d . . . C4 C 0.3865(4) 0.6643(2) 0.5781(7) 0.0253(10) Uani 1 1 d . . . H4A H 0.3539 0.6256 0.5751 0.030 Uiso 1 1 calc R . . H4B H 0.4088 0.6728 0.4429 0.030 Uiso 1 1 calc R . . C5 C 0.3090(4) 0.7092(2) 0.6342(7) 0.0279(11) Uani 1 1 d . . . H5A H 0.3410 0.7480 0.6337 0.033 Uiso 1 1 calc R . . H5B H 0.2879 0.7013 0.7705 0.033 Uiso 1 1 calc R . . C6 C 0.2155(3) 0.7089(2) 0.4920(6) 0.0205(9) Uani 1 1 d . . . C7 C 0.5521(4) 0.6025(2) 1.2083(8) 0.0333(12) Uani 1 1 d . . . H7A H 0.4798 0.5990 1.2422 0.040 Uiso 1 1 calc R . . H7B H 0.5867 0.6289 1.3059 0.040 Uiso 1 1 calc R . . C8 C 0.6026(5) 0.5429(3) 1.2232(8) 0.0415(14) Uani 1 1 d . . . H8A H 0.5570 0.5136 1.1584 0.050 Uiso 1 1 calc R . . H8B H 0.6673 0.5434 1.1536 0.050 Uiso 1 1 calc R . . C9 C 0.6240(5) 0.5272(2) 1.4391(8) 0.0361(13) Uani 1 1 d . . . C10 C 0.7472(4) 0.7068(2) 0.7297(7) 0.0251(10) Uani 1 1 d . . . H10A H 0.7918 0.7119 0.8516 0.030 Uiso 1 1 calc R . . H10B H 0.7334 0.7455 0.6716 0.030 Uiso 1 1 calc R . . C11 C 0.8020(4) 0.6702(2) 0.5828(7) 0.0234(10) Uani 1 1 d . . . H11A H 0.7616 0.6697 0.4546 0.028 Uiso 1 1 calc R . . H11B H 0.8067 0.6300 0.6327 0.028 Uiso 1 1 calc R . . C12 C 0.9082(4) 0.6923(2) 0.5485(7) 0.0222(10) Uani 1 1 d . . . C13 C 0.1021(6) 0.6225(3) -0.1138(10) 0.0578(18) Uani 1 1 d . . . H13A H 0.1630 0.6446 -0.1182 0.069 Uiso 1 1 calc R . . C14 C 0.0873(5) 0.5765(3) -0.2616(9) 0.0498(16) Uani 1 1 d . . . H14A H 0.1367 0.5674 -0.3551 0.060 Uiso 1 1 calc R . . C15 C -0.0002(6) 0.5488(3) -0.2540(12) 0.0583(19) Uani 1 1 d . . . C16 C -0.0674(7) 0.5573(3) -0.1212(10) 0.063(2) Uani 1 1 d . . . H16A H -0.1280 0.5349 -0.1163 0.075 Uiso 1 1 calc R . . C17 C -0.0436(6) 0.6018(3) 0.0130(10) 0.0501(18) Uani 1 1 d . . . H17A H -0.0922 0.6090 0.1098 0.060 Uiso 1 1 calc R . . C18 C -0.0244(6) 0.5029(4) -0.4151(10) 0.062(2) Uani 1 1 d . . . H18A H -0.0780 0.4764 -0.3928 0.074 Uiso 1 1 calc R . . N1 N 0.4768(3) 0.66322(18) 0.7188(6) 0.0230(8) Uani 1 1 d . . . N2 N 0.5568(3) 0.6275(2) 1.0065(6) 0.0293(10) Uani 1 1 d . . . N3 N 0.6507(3) 0.68033(17) 0.7823(6) 0.0217(8) Uani 1 1 d . . . N4 N 0.0403(4) 0.63587(19) 0.0221(6) 0.0298(10) Uani 1 1 d . . . O1 O 0.3900(3) 0.60791(19) 0.9283(6) 0.0414(10) Uani 1 1 d . . . O2 O 0.7252(3) 0.6443(2) 1.0671(6) 0.0431(10) Uani 1 1 d . . . O3 O 0.5650(3) 0.72130(16) 0.5173(5) 0.0321(8) Uani 1 1 d . . . O4 O 0.2052(3) 0.67042(15) 0.3611(5) 0.0271(8) Uani 1 1 d . . . O5 O 0.1495(2) 0.74854(15) 0.5027(5) 0.0237(7) Uani 1 1 d . . . O6 O 0.5890(4) 0.55148(19) 1.5770(6) 0.0500(11) Uani 1 1 d . . . O7 O 0.6866(4) 0.48325(19) 1.4581(6) 0.0470(11) Uani 1 1 d . . . O8 O 0.9391(3) 0.73472(17) 0.6533(5) 0.0341(9) Uani 1 1 d . . . O9 O 0.9588(3) 0.66716(15) 0.4215(5) 0.0261(7) Uani 1 1 d . . . O1W O 0.2610(4) 0.56270(17) 0.2049(7) 0.0420(10) Uani 1 1 d D . . H1WB H 0.318(4) 0.567(3) 0.153(16) 0.15(5) Uiso 1 1 d D . . H1WA H 0.236(5) 0.5948(16) 0.230(10) 0.05(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0161(4) 0.0243(4) 0.0176(3) -0.0006(3) -0.0008(2) 0.0014(3) C1 0.025(3) 0.037(3) 0.026(2) 0.001(2) 0.003(2) -0.002(2) C2 0.020(3) 0.039(3) 0.028(2) 0.002(2) -0.004(2) -0.005(2) C3 0.020(2) 0.024(2) 0.024(2) -0.0033(19) 0.0014(18) 0.003(2) C4 0.016(2) 0.035(3) 0.024(2) -0.002(2) -0.0046(18) 0.004(2) C5 0.017(2) 0.039(3) 0.027(2) -0.008(2) -0.0033(19) 0.005(2) C6 0.015(2) 0.027(2) 0.019(2) 0.0047(19) -0.0008(17) -0.002(2) C7 0.034(3) 0.036(3) 0.030(3) 0.003(2) 0.001(2) 0.003(2) C8 0.054(4) 0.035(3) 0.036(3) 0.000(2) 0.003(3) 0.008(3) C9 0.039(3) 0.033(3) 0.036(3) 0.006(2) 0.001(2) -0.005(3) C10 0.015(2) 0.033(3) 0.027(2) -0.002(2) 0.0027(18) -0.004(2) C11 0.016(2) 0.030(3) 0.024(2) -0.0014(19) -0.0010(18) -0.001(2) C12 0.020(2) 0.025(2) 0.021(2) 0.0031(18) -0.0010(18) 0.000(2) C13 0.060(5) 0.060(4) 0.054(4) -0.003(3) 0.005(3) -0.007(4) C14 0.053(4) 0.065(4) 0.032(3) -0.001(3) 0.008(3) 0.002(4) C15 0.040(4) 0.062(4) 0.073(5) 0.037(4) 0.001(3) 0.004(3) C16 0.083(6) 0.061(4) 0.044(4) -0.004(3) -0.002(4) 0.027(4) C17 0.059(4) 0.041(3) 0.046(3) -0.015(3) -0.027(3) 0.014(3) C18 0.073(5) 0.062(4) 0.051(4) -0.006(4) 0.004(4) -0.006(4) N1 0.015(2) 0.030(2) 0.0238(19) 0.0006(16) -0.0021(15) 0.0030(17) N2 0.023(2) 0.042(2) 0.023(2) 0.0086(19) 0.0005(16) -0.002(2) N3 0.015(2) 0.027(2) 0.0226(19) 0.0001(16) 0.0010(15) -0.0021(16) N4 0.040(3) 0.031(2) 0.0177(19) -0.0043(17) 0.0011(18) 0.012(2) O1 0.025(2) 0.061(3) 0.038(2) 0.0093(19) 0.0011(16) -0.0147(19) O2 0.028(2) 0.062(3) 0.038(2) 0.0119(19) -0.0118(17) -0.006(2) O3 0.032(2) 0.034(2) 0.0304(18) 0.0100(15) 0.0007(15) 0.0009(16) O4 0.0235(18) 0.0315(19) 0.0259(17) -0.0054(15) -0.0044(14) 0.0010(15) O5 0.0175(17) 0.0296(17) 0.0241(16) -0.0006(14) 0.0023(13) 0.0029(14) O6 0.066(3) 0.044(2) 0.041(2) 0.005(2) 0.009(2) 0.016(2) O7 0.055(3) 0.047(3) 0.040(2) 0.0057(19) 0.004(2) 0.012(2) O8 0.027(2) 0.041(2) 0.035(2) -0.0116(17) 0.0060(16) -0.0117(17) O9 0.0239(18) 0.0302(18) 0.0246(16) 0.0005(14) 0.0051(14) -0.0015(15) O1W 0.044(3) 0.033(2) 0.050(2) 0.0104(19) 0.009(2) 0.0071(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O8 2.074(4) 4_475 ? Mn1 O9 2.114(3) 1_455 ? Mn1 N4 2.174(4) . ? Mn1 O5 2.219(3) 4_575 ? Mn1 O4 2.272(3) . ? Mn1 O5 2.354(3) . ? C1 O1 1.218(6) . ? C1 N1 1.364(6) . ? C1 N2 1.365(6) . ? C2 O2 1.205(6) . ? C2 N3 1.378(6) . ? C2 N2 1.382(7) . ? C3 O3 1.207(6) . ? C3 N1 1.375(6) . ? C3 N3 1.384(6) . ? C4 N1 1.477(6) . ? C4 C5 1.514(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.516(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.255(6) . ? C6 O5 1.264(6) . ? C7 N2 1.481(6) . ? C7 C8 1.528(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.511(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O6 1.197(7) . ? C9 O7 1.308(7) . ? C10 N3 1.465(6) . ? C10 C11 1.510(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.511(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O9 1.253(6) . ? C12 O8 1.263(6) . ? C13 N4 1.292(8) . ? C13 C14 1.462(9) . ? C13 H13A 0.9500 . ? C14 C15 1.318(10) . ? C14 H14A 0.9500 . ? C15 C16 1.302(10) . ? C15 C18 1.540(11) . ? C16 C17 1.394(9) . ? C16 H16A 0.9500 . ? C17 N4 1.352(8) . ? C17 H17A 0.9500 . ? C18 C18 1.346(14) 3_564 ? C18 H18A 0.9500 . ? O5 Mn1 2.219(3) 4_576 ? O8 Mn1 2.074(4) 4_676 ? O9 Mn1 2.114(3) 1_655 ? O1W H1WB 0.85(2) . ? O1W H1WA 0.83(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Mn1 O9 87.73(14) 4_475 1_455 ? O8 Mn1 N4 106.61(16) 4_475 . ? O9 Mn1 N4 90.04(15) 1_455 . ? O8 Mn1 O5 88.81(13) 4_475 4_575 ? O9 Mn1 O5 174.96(13) 1_455 4_575 ? N4 Mn1 O5 87.45(15) . 4_575 ? O8 Mn1 O4 162.14(14) 4_475 . ? O9 Mn1 O4 96.67(13) 1_455 . ? N4 Mn1 O4 90.74(14) . . ? O5 Mn1 O4 87.73(12) 4_575 . ? O8 Mn1 O5 106.57(14) 4_475 . ? O9 Mn1 O5 89.64(12) 1_455 . ? N4 Mn1 O5 146.78(14) . . ? O5 Mn1 O5 94.85(10) 4_575 . ? O4 Mn1 O5 56.35(12) . . ? O1 C1 N1 121.6(5) . . ? O1 C1 N2 122.8(5) . . ? N1 C1 N2 115.6(4) . . ? O2 C2 N3 122.5(5) . . ? O2 C2 N2 121.4(5) . . ? N3 C2 N2 116.1(4) . . ? O3 C3 N1 122.7(4) . . ? O3 C3 N3 121.9(4) . . ? N1 C3 N3 115.4(4) . . ? N1 C4 C5 112.2(4) . . ? N1 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N1 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C6 111.8(4) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? O4 C6 O5 120.3(4) . . ? O4 C6 C5 120.0(4) . . ? O5 C6 C5 119.6(4) . . ? N2 C7 C8 111.9(4) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C7 109.8(5) . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O6 C9 O7 123.5(5) . . ? O6 C9 C8 125.1(5) . . ? O7 C9 C8 111.4(5) . . ? N3 C10 C11 111.8(4) . . ? N3 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 112.7(4) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? O9 C12 O8 125.1(4) . . ? O9 C12 C11 118.3(4) . . ? O8 C12 C11 116.6(4) . . ? N4 C13 C14 126.3(7) . . ? N4 C13 H13A 116.9 . . ? C14 C13 H13A 116.9 . . ? C15 C14 C13 114.3(7) . . ? C15 C14 H14A 122.9 . . ? C13 C14 H14A 122.9 . . ? C16 C15 C14 125.2(9) . . ? C16 C15 C18 117.8(7) . . ? C14 C15 C18 117.1(7) . . ? C15 C16 C17 114.8(9) . . ? C15 C16 H16A 122.6 . . ? C17 C16 H16A 122.6 . . ? N4 C17 C16 127.9(7) . . ? N4 C17 H17A 116.1 . . ? C16 C17 H17A 116.1 . . ? C18 C18 C15 125.3(10) 3_564 . ? C18 C18 H18A 117.4 3_564 . ? C15 C18 H18A 117.4 . . ? C1 N1 C3 125.1(4) . . ? C1 N1 C4 117.1(4) . . ? C3 N1 C4 117.5(4) . . ? C1 N2 C2 124.2(4) . . ? C1 N2 C7 119.4(4) . . ? C2 N2 C7 116.3(4) . . ? C2 N3 C3 123.2(4) . . ? C2 N3 C10 117.7(4) . . ? C3 N3 C10 118.9(4) . . ? C13 N4 C17 111.5(5) . . ? C13 N4 Mn1 126.0(5) . . ? C17 N4 Mn1 122.3(4) . . ? C6 O4 Mn1 93.7(3) . . ? C6 O5 Mn1 139.7(3) . 4_576 ? C6 O5 Mn1 89.7(3) . . ? Mn1 O5 Mn1 116.04(14) 4_576 . ? C12 O8 Mn1 147.2(3) . 4_676 ? C12 O9 Mn1 125.3(3) . 1_655 ? H1WB O1W H1WA 111(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C4 C5 C6 -178.6(4) . . . . ? C4 C5 C6 O4 7.1(6) . . . . ? C4 C5 C6 O5 -171.0(4) . . . . ? N2 C7 C8 C9 163.3(5) . . . . ? C7 C8 C9 O6 13.9(9) . . . . ? C7 C8 C9 O7 -165.9(5) . . . . ? N3 C10 C11 C12 -172.0(4) . . . . ? C10 C11 C12 O9 -176.3(4) . . . . ? C10 C11 C12 O8 4.4(6) . . . . ? N4 C13 C14 C15 2.7(11) . . . . ? C13 C14 C15 C16 -4.5(10) . . . . ? C13 C14 C15 C18 175.6(6) . . . . ? C14 C15 C16 C17 3.7(11) . . . . ? C18 C15 C16 C17 -176.4(6) . . . . ? C15 C16 C17 N4 -0.9(10) . . . . ? C16 C15 C18 C18 165.0(10) . . . 3_564 ? C14 C15 C18 C18 -15.1(14) . . . 3_564 ? O1 C1 N1 C3 179.9(5) . . . . ? N2 C1 N1 C3 0.9(7) . . . . ? O1 C1 N1 C4 -5.7(7) . . . . ? N2 C1 N1 C4 175.3(4) . . . . ? O3 C3 N1 C1 -175.9(5) . . . . ? N3 C3 N1 C1 4.9(7) . . . . ? O3 C3 N1 C4 9.8(7) . . . . ? N3 C3 N1 C4 -169.5(4) . . . . ? C5 C4 N1 C1 84.3(6) . . . . ? C5 C4 N1 C3 -100.9(5) . . . . ? O1 C1 N2 C2 175.7(5) . . . . ? N1 C1 N2 C2 -5.4(8) . . . . ? O1 C1 N2 C7 -9.7(8) . . . . ? N1 C1 N2 C7 169.2(4) . . . . ? O2 C2 N2 C1 -178.1(5) . . . . ? N3 C2 N2 C1 3.5(8) . . . . ? O2 C2 N2 C7 7.1(8) . . . . ? N3 C2 N2 C7 -171.2(4) . . . . ? C8 C7 N2 C1 108.5(6) . . . . ? C8 C7 N2 C2 -76.4(6) . . . . ? O2 C2 N3 C3 -175.4(5) . . . . ? N2 C2 N3 C3 3.0(7) . . . . ? O2 C2 N3 C10 -0.6(8) . . . . ? N2 C2 N3 C10 177.7(4) . . . . ? O3 C3 N3 C2 173.9(5) . . . . ? N1 C3 N3 C2 -6.8(7) . . . . ? O3 C3 N3 C10 -0.8(7) . . . . ? N1 C3 N3 C10 178.5(4) . . . . ? C11 C10 N3 C2 99.2(5) . . . . ? C11 C10 N3 C3 -85.8(5) . . . . ? C14 C13 N4 C17 -0.4(9) . . . . ? C14 C13 N4 Mn1 -175.1(5) . . . . ? C16 C17 N4 C13 -0.6(9) . . . . ? C16 C17 N4 Mn1 174.4(5) . . . . ? O8 Mn1 N4 C13 113.0(5) 4_475 . . . ? O9 Mn1 N4 C13 -159.3(5) 1_455 . . . ? O5 Mn1 N4 C13 25.0(5) 4_575 . . . ? O4 Mn1 N4 C13 -62.7(5) . . . . ? O5 Mn1 N4 C13 -69.9(6) . . . . ? O8 Mn1 N4 C17 -61.2(4) 4_475 . . . ? O9 Mn1 N4 C17 26.5(4) 1_455 . . . ? O5 Mn1 N4 C17 -149.2(4) 4_575 . . . ? O4 Mn1 N4 C17 123.1(4) . . . . ? O5 Mn1 N4 C17 115.9(4) . . . . ? O5 C6 O4 Mn1 0.8(4) . . . . ? C5 C6 O4 Mn1 -177.3(4) . . . . ? O8 Mn1 O4 C6 17.9(6) 4_475 . . . ? O9 Mn1 O4 C6 -85.6(3) 1_455 . . . ? N4 Mn1 O4 C6 -175.7(3) . . . . ? O5 Mn1 O4 C6 96.9(3) 4_575 . . . ? O5 Mn1 O4 C6 -0.5(2) . . . . ? O4 C6 O5 Mn1 131.4(4) . . . 4_576 ? C5 C6 O5 Mn1 -50.5(7) . . . 4_576 ? O4 C6 O5 Mn1 -0.8(4) . . . . ? C5 C6 O5 Mn1 177.3(4) . . . . ? O8 Mn1 O5 C6 -173.7(3) 4_475 . . . ? O9 Mn1 O5 C6 98.7(3) 1_455 . . . ? N4 Mn1 O5 C6 9.2(4) . . . . ? O5 Mn1 O5 C6 -83.6(2) 4_575 . . . ? O4 Mn1 O5 C6 0.5(2) . . . . ? O8 Mn1 O5 Mn1 38.50(19) 4_475 . . 4_576 ? O9 Mn1 O5 Mn1 -49.02(16) 1_455 . . 4_576 ? N4 Mn1 O5 Mn1 -138.5(2) . . . 4_576 ? O5 Mn1 O5 Mn1 128.7(2) 4_575 . . 4_576 ? O4 Mn1 O5 Mn1 -147.3(2) . . . 4_576 ? O9 C12 O8 Mn1 -1.3(10) . . . 4_676 ? C11 C12 O8 Mn1 178.0(4) . . . 4_676 ? O8 C12 O9 Mn1 -38.2(6) . . . 1_655 ? C11 C12 O9 Mn1 142.5(3) . . . 1_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB O1 0.85(2) 2.06(7) 2.785(6) 143(9) 1_554 O1W H1WA O4 0.83(2) 2.01(3) 2.814(5) 162(7) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.244 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.103 #End of Crystallographic Information File