Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Daniel Rabinovich' _publ_contact_author_address ; Department of Chemistry The University of North Carolina at Charlotte 9201 University City Boulevard Charlotte North Carolina 28223 UNITED STATES OF AMERICA ; _publ_contact_author_email DRABINOV@EMAIL.UNCC.EDU _publ_section_title ; Manganese(I) poly(mercaptoimidazolyl)borate complexes: spectroscopic and structural characterization of Mn...H-B interactions in solution and in the solid state ; loop_ _publ_author_name 'Daniel Rabinovich' 'Alison R. Fout' 'Leigh A. Graham' 'Karl R. Kuehne' 'Fred M. Marks' ; B.Mookherji ; 'Arnold L. Rheingold' 'Jennifer L. White' 'Glenn P. A. Yap' 'Lev N. Zakharov' data_danr007 _database_code_depnum_ccdc_archive 'CCDC 246938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H17 B Mn N4 O3.50 S2' _chemical_formula_weight 415.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2360(15) _cell_length_b 14.786(3) _cell_length_c 17.167(3) _cell_angle_alpha 94.238(2) _cell_angle_beta 91.125(2) _cell_angle_gamma 95.144(2) _cell_volume 1823.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9088 _exptl_absorpt_correction_T_max 0.9088 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (600 frames), and at phi = 180 deg (600 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 15406 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8000 _reflns_number_gt 5809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0665P)^2^+2.8175P] 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 8000 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.69977(7) 0.26240(4) 0.10367(3) 0.02268(15) Uani 1 1 d . . . Mn2 Mn 0.29550(8) 0.23958(4) 0.39333(3) 0.02639(16) Uani 1 1 d . . . B1 B 1.0310(5) 0.2999(3) 0.0312(2) 0.0247(8) Uani 1 1 d . . . H10B H 0.9424 0.2953 0.0743 0.030 Uiso 1 1 calc R . . H10C H 1.1539 0.3240 0.0541 0.030 Uiso 1 1 calc R . . B2 B -0.0278(6) 0.2037(3) 0.4717(3) 0.0295(9) Uani 1 1 d . . . H20D H 0.0571 0.2089 0.4274 0.035 Uiso 1 1 calc R . . H20E H -0.1530 0.1813 0.4503 0.035 Uiso 1 1 calc R . . N1 N 0.7981(4) 0.4401(2) -0.10232(18) 0.0278(7) Uani 1 1 d . . . N2 N 0.9656(4) 0.3658(2) -0.02667(17) 0.0243(6) Uani 1 1 d . . . N3 N 0.9731(4) 0.0703(2) -0.07041(18) 0.0297(7) Uani 1 1 d . . . N4 N 1.0452(4) 0.2045(2) -0.00992(17) 0.0248(6) Uani 1 1 d . . . N5 N 0.2144(4) 0.0607(2) 0.59975(18) 0.0309(7) Uani 1 1 d . . . N6 N 0.0400(4) 0.1351(2) 0.52672(18) 0.0288(7) Uani 1 1 d . . . N7 N 0.0431(5) 0.4331(2) 0.57291(19) 0.0339(7) Uani 1 1 d . . . N8 N -0.0351(4) 0.2980(2) 0.51545(19) 0.0309(7) Uani 1 1 d . . . O1 O 0.6925(4) 0.42447(18) 0.21375(16) 0.0360(6) Uani 1 1 d . . . O2 O 0.8399(5) 0.1477(2) 0.22103(18) 0.0485(8) Uani 1 1 d . . . O3 O 0.3243(4) 0.2036(2) 0.15367(17) 0.0389(7) Uani 1 1 d . . . O4 O 0.2971(4) 0.07281(19) 0.28856(16) 0.0396(7) Uani 1 1 d . . . O5 O 0.1484(5) 0.3474(2) 0.27202(18) 0.0515(8) Uani 1 1 d . . . O6 O 0.6734(4) 0.2912(2) 0.34190(17) 0.0418(7) Uani 1 1 d . . . S1 S 0.59398(12) 0.35263(6) 0.00474(5) 0.0248(2) Uani 1 1 d . . . S2 S 0.68793(12) 0.13320(6) 0.01139(6) 0.0285(2) Uani 1 1 d . . . S3 S 0.41051(12) 0.15711(7) 0.49585(5) 0.0292(2) Uani 1 1 d . . . S4 S 0.30959(14) 0.37426(7) 0.47855(6) 0.0351(2) Uani 1 1 d . . . C1 C 0.7000(5) 0.3617(2) 0.1714(2) 0.0249(7) Uani 1 1 d . . . C2 C 0.7886(5) 0.1928(3) 0.1760(2) 0.0319(8) Uani 1 1 d . . . C3 C 0.4689(5) 0.2271(2) 0.1321(2) 0.0263(7) Uani 1 1 d . . . C4 C 0.7912(5) 0.3852(2) -0.04265(19) 0.0228(7) Uani 1 1 d . . . C5 C 0.6370(6) 0.4761(3) -0.1383(2) 0.0365(9) Uani 1 1 d . . . H5A H 0.5242 0.4551 -0.1117 0.055 Uiso 1 1 calc R . . H5B H 0.6260 0.4544 -0.1937 0.055 Uiso 1 1 calc R . . H5C H 0.6532 0.5428 -0.1335 0.055 Uiso 1 1 calc R . . C6 C 0.9792(6) 0.4560(3) -0.1247(2) 0.0343(9) Uani 1 1 d . . . H6A H 1.0223 0.4918 -0.1656 0.041 Uiso 1 1 calc R . . C7 C 1.0834(5) 0.4108(3) -0.0775(2) 0.0325(8) Uani 1 1 d . . . H7A H 1.2144 0.4098 -0.0786 0.039 Uiso 1 1 calc R . . C8 C 0.9075(5) 0.1376(2) -0.0238(2) 0.0259(7) Uani 1 1 d . . . C9 C 0.8632(6) -0.0126(3) -0.1019(2) 0.0368(9) Uani 1 1 d . . . H9A H 0.7380 -0.0139 -0.0810 0.055 Uiso 1 1 calc R . . H9B H 0.9225 -0.0659 -0.0868 0.055 Uiso 1 1 calc R . . H9C H 0.8555 -0.0134 -0.1590 0.055 Uiso 1 1 calc R . . C10 C 1.1567(5) 0.0959(3) -0.0861(2) 0.0339(9) Uani 1 1 d . . . H10A H 1.2361 0.0617 -0.1176 0.041 Uiso 1 1 calc R . . C11 C 1.2013(5) 0.1781(3) -0.0486(2) 0.0321(8) Uani 1 1 d . . . H11A H 1.3189 0.2123 -0.0484 0.038 Uiso 1 1 calc R . . C12 C 0.2916(5) 0.1368(3) 0.3291(2) 0.0296(8) Uani 1 1 d . . . C13 C 0.2038(6) 0.3046(3) 0.3185(2) 0.0360(9) Uani 1 1 d . . . C14 C 0.5280(6) 0.2711(3) 0.3636(2) 0.0309(8) Uani 1 1 d . . . C15 C 0.2157(5) 0.1177(2) 0.5417(2) 0.0268(8) Uani 1 1 d . . . C16 C 0.3774(6) 0.0249(3) 0.6326(3) 0.0419(10) Uani 1 1 d . . . H16A H 0.3399 -0.0144 0.6741 0.063 Uiso 1 1 calc R . . H16B H 0.4645 0.0755 0.6542 0.063 Uiso 1 1 calc R . . H16C H 0.4377 -0.0105 0.5915 0.063 Uiso 1 1 calc R . . C17 C 0.0326(6) 0.0408(3) 0.6209(3) 0.0396(10) Uani 1 1 d . . . H17A H -0.0089 0.0020 0.6600 0.048 Uiso 1 1 calc R . . C18 C -0.0743(6) 0.0868(3) 0.5757(2) 0.0374(9) Uani 1 1 d . . . H18A H -0.2056 0.0862 0.5772 0.045 Uiso 1 1 calc R . . C19 C 0.1003(5) 0.3668(2) 0.5232(2) 0.0288(8) Uani 1 1 d . . . C20 C 0.1517(6) 0.5180(3) 0.5987(3) 0.0420(10) Uani 1 1 d . . . H20A H 0.2700 0.5215 0.5718 0.063 Uiso 1 1 calc R . . H20B H 0.1755 0.5201 0.6552 0.063 Uiso 1 1 calc R . . H20C H 0.0827 0.5695 0.5864 0.063 Uiso 1 1 calc R . . C21 C -0.1321(6) 0.4052(3) 0.5975(3) 0.0428(10) Uani 1 1 d . . . H21A H -0.2043 0.4385 0.6331 0.051 Uiso 1 1 calc R . . C22 C -0.1817(6) 0.3224(3) 0.5619(3) 0.0395(10) Uani 1 1 d . . . H22A H -0.2960 0.2867 0.5674 0.047 Uiso 1 1 calc R . . O7 O 0.5381(5) 0.2561(2) -0.25531(18) 0.0534(9) Uani 1 1 d . . . C23 C 0.3481(8) 0.2566(4) -0.2489(3) 0.0629(15) Uani 1 1 d . . . H23A H 0.3193 0.2772 -0.1946 0.076 Uiso 1 1 calc R . . H23B H 0.2887 0.1939 -0.2601 0.076 Uiso 1 1 calc R . . C24 C 0.2724(9) 0.3159(4) -0.3022(3) 0.0725(17) Uani 1 1 d . . . H24A H 0.1376 0.3141 -0.2965 0.109 Uiso 1 1 calc R . . H24B H 0.2999 0.2954 -0.3559 0.109 Uiso 1 1 calc R . . H24C H 0.3283 0.3784 -0.2902 0.109 Uiso 1 1 calc R . . C25 C 0.6280(8) 0.2044(4) -0.2038(3) 0.0610(14) Uani 1 1 d . . . H25A H 0.5779 0.1398 -0.2121 0.073 Uiso 1 1 calc R . . H25B H 0.6038 0.2260 -0.1493 0.073 Uiso 1 1 calc R . . C26 C 0.8264(8) 0.2117(4) -0.2158(3) 0.0635(15) Uani 1 1 d . . . H26A H 0.8858 0.1730 -0.1806 0.095 Uiso 1 1 calc R . . H26B H 0.8771 0.2752 -0.2046 0.095 Uiso 1 1 calc R . . H26C H 0.8502 0.1918 -0.2701 0.095 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 0.0238(3) 0.0231(3) 0.0211(3) 0.0004(2) 0.0001(2) 0.0033(2) Mn2 0.0317(3) 0.0241(3) 0.0229(3) 0.0007(2) -0.0003(2) 0.0012(2) B1 0.0203(18) 0.028(2) 0.025(2) -0.0027(16) 0.0013(15) 0.0022(15) B2 0.026(2) 0.029(2) 0.033(2) -0.0020(18) -0.0021(17) 0.0014(17) N1 0.0328(16) 0.0236(15) 0.0271(16) 0.0022(13) 0.0028(13) 0.0023(13) N2 0.0203(14) 0.0248(15) 0.0274(15) -0.0010(12) 0.0022(12) 0.0013(11) N3 0.0322(16) 0.0263(16) 0.0304(16) -0.0045(13) -0.0021(13) 0.0087(13) N4 0.0192(14) 0.0256(15) 0.0294(16) -0.0011(12) -0.0019(12) 0.0048(12) N5 0.0372(18) 0.0248(16) 0.0301(17) 0.0006(13) 0.0028(14) 0.0009(13) N6 0.0317(16) 0.0235(16) 0.0294(16) -0.0039(13) 0.0028(13) -0.0021(13) N7 0.0376(18) 0.0296(17) 0.0339(18) -0.0059(14) -0.0097(14) 0.0087(14) N8 0.0290(16) 0.0314(17) 0.0327(17) -0.0007(14) -0.0018(13) 0.0073(13) O1 0.0466(17) 0.0295(15) 0.0305(14) -0.0037(12) -0.0014(12) 0.0015(12) O2 0.061(2) 0.0500(19) 0.0397(17) 0.0126(15) 0.0037(15) 0.0229(16) O3 0.0319(15) 0.0466(18) 0.0381(16) 0.0073(13) 0.0076(12) -0.0008(13) O4 0.0543(18) 0.0327(16) 0.0304(15) -0.0056(12) 0.0002(13) 0.0034(13) O5 0.066(2) 0.0503(19) 0.0415(18) 0.0119(15) -0.0047(16) 0.0205(17) O6 0.0451(17) 0.0446(18) 0.0353(16) 0.0080(13) 0.0069(13) -0.0038(14) S1 0.0206(4) 0.0289(5) 0.0254(4) 0.0034(4) 0.0008(3) 0.0033(3) S2 0.0244(4) 0.0258(5) 0.0338(5) -0.0054(4) 0.0008(4) 0.0005(3) S3 0.0267(5) 0.0341(5) 0.0269(5) 0.0063(4) 0.0004(4) 0.0006(4) S4 0.0360(5) 0.0278(5) 0.0395(6) -0.0061(4) 0.0017(4) -0.0020(4) C1 0.0265(17) 0.0253(18) 0.0229(17) 0.0023(15) -0.0003(14) 0.0022(14) C2 0.034(2) 0.033(2) 0.030(2) 0.0024(16) 0.0011(16) 0.0091(16) C3 0.0313(19) 0.0267(19) 0.0208(17) 0.0003(14) -0.0014(15) 0.0041(15) C4 0.0248(17) 0.0204(17) 0.0221(17) -0.0048(13) 0.0005(13) 0.0016(13) C5 0.042(2) 0.037(2) 0.032(2) 0.0100(17) -0.0022(18) 0.0082(18) C6 0.039(2) 0.030(2) 0.033(2) 0.0039(17) 0.0107(17) -0.0037(17) C7 0.0291(19) 0.030(2) 0.037(2) -0.0005(17) 0.0084(16) -0.0041(15) C8 0.0240(17) 0.0284(19) 0.0249(18) -0.0024(15) -0.0052(14) 0.0060(14) C9 0.043(2) 0.028(2) 0.039(2) -0.0068(17) -0.0074(18) 0.0092(17) C10 0.0293(19) 0.038(2) 0.035(2) -0.0001(17) 0.0009(16) 0.0119(16) C11 0.0251(18) 0.035(2) 0.036(2) -0.0030(17) 0.0020(16) 0.0060(16) C12 0.035(2) 0.029(2) 0.0240(18) 0.0053(16) -0.0035(15) 0.0012(16) C13 0.044(2) 0.032(2) 0.033(2) 0.0009(17) 0.0028(18) 0.0068(18) C14 0.041(2) 0.0260(19) 0.0257(19) 0.0049(15) 0.0024(17) 0.0019(16) C15 0.0321(19) 0.0218(17) 0.0256(18) -0.0008(14) 0.0003(15) 0.0002(14) C16 0.051(3) 0.040(2) 0.038(2) 0.0109(19) 0.006(2) 0.012(2) C17 0.046(2) 0.033(2) 0.040(2) 0.0064(18) 0.0139(19) -0.0024(18) C18 0.035(2) 0.033(2) 0.043(2) -0.0027(18) 0.0107(18) -0.0016(17) C19 0.035(2) 0.0245(18) 0.0264(18) -0.0036(15) -0.0071(16) 0.0079(15) C20 0.051(3) 0.030(2) 0.044(2) -0.0118(18) -0.013(2) 0.0099(19) C21 0.037(2) 0.046(3) 0.045(3) -0.008(2) -0.0008(19) 0.0159(19) C22 0.032(2) 0.041(2) 0.046(2) -0.004(2) 0.0017(18) 0.0106(18) O7 0.063(2) 0.059(2) 0.0427(19) 0.0143(16) -0.0039(17) 0.0187(18) C23 0.080(4) 0.056(3) 0.053(3) -0.002(3) -0.004(3) 0.015(3) C24 0.088(4) 0.083(4) 0.050(3) -0.001(3) -0.012(3) 0.033(4) C25 0.077(4) 0.056(3) 0.050(3) 0.001(3) -0.014(3) 0.014(3) C26 0.074(4) 0.067(4) 0.050(3) -0.007(3) -0.015(3) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C3 1.793(4) . ? Mn1 C1 1.804(4) . ? Mn1 C2 1.814(4) . ? Mn1 S2 2.3842(11) . ? Mn1 S1 2.3911(11) . ? Mn1 B1 2.753(4) . ? Mn2 C14 1.799(4) . ? Mn2 C12 1.809(4) . ? Mn2 C13 1.810(4) . ? Mn2 S4 2.3756(12) . ? Mn2 S3 2.3915(11) . ? Mn2 B2 2.751(4) . ? B1 N2 1.540(5) . ? B1 N4 1.543(5) . ? B2 N8 1.540(5) . ? B2 N6 1.541(5) . ? N1 C4 1.352(4) . ? N1 C6 1.378(5) . ? N1 C5 1.467(5) . ? N2 C4 1.346(4) . ? N2 C7 1.394(5) . ? N3 C8 1.356(4) . ? N3 C10 1.385(5) . ? N3 C9 1.462(5) . ? N4 C8 1.344(4) . ? N4 C11 1.393(4) . ? N5 C15 1.351(5) . ? N5 C17 1.384(5) . ? N5 C16 1.456(5) . ? N6 C15 1.343(5) . ? N6 C18 1.383(5) . ? N7 C19 1.350(5) . ? N7 C21 1.382(5) . ? N7 C20 1.454(5) . ? N8 C19 1.346(5) . ? N8 C22 1.397(5) . ? O1 C1 1.142(4) . ? O2 C2 1.135(5) . ? O3 C3 1.150(4) . ? O4 C12 1.136(4) . ? O5 C13 1.143(5) . ? O6 C14 1.144(5) . ? S1 C4 1.706(3) . ? S2 C8 1.708(4) . ? S3 C15 1.706(4) . ? S4 C19 1.709(4) . ? C6 C7 1.349(6) . ? C10 C11 1.343(5) . ? C17 C18 1.346(6) . ? C21 C22 1.343(6) . ? O7 C23 1.382(6) . ? O7 C25 1.398(6) . ? C23 C24 1.446(7) . ? C25 C26 1.449(7) . ? 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 C3 Mn1 C1 89.16(16) . . ? C3 Mn1 C2 88.85(17) . . ? C1 Mn1 C2 93.73(17) . . ? C3 Mn1 S2 89.53(11) . . ? C1 Mn1 S2 177.50(12) . . ? C2 Mn1 S2 88.37(13) . . ? C3 Mn1 S1 93.26(11) . . ? C1 Mn1 S1 87.71(11) . . ? C2 Mn1 S1 177.46(12) . . ? S2 Mn1 S1 90.24(4) . . ? C3 Mn1 B1 168.47(14) . . ? C1 Mn1 B1 100.58(14) . . ? C2 Mn1 B1 96.59(15) . . ? S2 Mn1 B1 80.50(9) . . ? S1 Mn1 B1 81.08(9) . . ? C14 Mn2 C12 89.08(17) . . ? C14 Mn2 C13 90.24(18) . . ? C12 Mn2 C13 93.41(17) . . ? C14 Mn2 S4 89.63(12) . . ? C12 Mn2 S4 178.39(13) . . ? C13 Mn2 S4 87.56(13) . . ? C14 Mn2 S3 90.98(12) . . ? C12 Mn2 S3 88.44(12) . . ? C13 Mn2 S3 177.80(13) . . ? S4 Mn2 S3 90.61(4) . . ? C14 Mn2 B2 167.15(15) . . ? C12 Mn2 B2 100.08(15) . . ? C13 Mn2 B2 98.13(16) . . ? S4 Mn2 B2 81.04(9) . . ? S3 Mn2 B2 80.37(9) . . ? N2 B1 N4 110.9(3) . . ? N2 B1 Mn1 98.4(2) . . ? N4 B1 Mn1 97.8(2) . . ? N8 B2 N6 110.8(3) . . ? N8 B2 Mn2 98.3(2) . . ? N6 B2 Mn2 98.7(2) . . ? C4 N1 C6 109.4(3) . . ? C4 N1 C5 125.2(3) . . ? C6 N1 C5 125.4(3) . . ? C4 N2 C7 107.9(3) . . ? C4 N2 B1 128.4(3) . . ? C7 N2 B1 123.5(3) . . ? C8 N3 C10 108.6(3) . . ? C8 N3 C9 125.0(3) . . ? C10 N3 C9 126.3(3) . . ? C8 N4 C11 108.0(3) . . ? C8 N4 B1 127.2(3) . . ? C11 N4 B1 124.2(3) . . ? C15 N5 C17 108.5(3) . . ? C15 N5 C16 125.3(3) . . ? C17 N5 C16 126.2(3) . . ? C15 N6 C18 108.1(3) . . ? C15 N6 B2 127.7(3) . . ? C18 N6 B2 123.9(3) . . ? C19 N7 C21 108.7(3) . . ? C19 N7 C20 125.4(4) . . ? C21 N7 C20 125.8(4) . . ? C19 N8 C22 107.9(3) . . ? C19 N8 B2 127.7(3) . . ? C22 N8 B2 124.1(3) . . ? C4 S1 Mn1 103.76(12) . . ? C8 S2 Mn1 103.33(13) . . ? C15 S3 Mn2 104.11(13) . . ? C19 S4 Mn2 103.70(13) . . ? O1 C1 Mn1 177.2(3) . . ? O2 C2 Mn1 178.2(4) . . ? O3 C3 Mn1 176.7(3) . . ? N2 C4 N1 107.8(3) . . ? N2 C4 S1 127.8(3) . . ? N1 C4 S1 124.4(3) . . ? C7 C6 N1 106.7(3) . . ? C6 C7 N2 108.1(3) . . ? N4 C8 N3 108.1(3) . . ? N4 C8 S2 127.7(3) . . ? N3 C8 S2 124.2(3) . . ? C11 C10 N3 107.2(3) . . ? C10 C11 N4 108.1(3) . . ? O4 C12 Mn2 177.1(4) . . ? O5 C13 Mn2 178.4(4) . . ? O6 C14 Mn2 177.4(3) . . ? N6 C15 N5 108.2(3) . . ? N6 C15 S3 127.4(3) . . ? N5 C15 S3 124.4(3) . . ? C18 C17 N5 107.0(4) . . ? C17 C18 N6 108.2(4) . . ? N8 C19 N7 108.2(3) . . ? N8 C19 S4 127.9(3) . . ? N7 C19 S4 123.9(3) . . ? C22 C21 N7 107.5(4) . . ? C21 C22 N8 107.7(4) . . ? C23 O7 C25 116.7(4) . . ? O7 C23 C24 111.6(5) . . ? O7 C25 C26 110.9(5) . . ? 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 C3 Mn1 B1 N2 66.7(8) . . . . ? C1 Mn1 B1 N2 -80.4(2) . . . . ? C2 Mn1 B1 N2 -175.5(2) . . . . ? S2 Mn1 B1 N2 97.3(2) . . . . ? S1 Mn1 B1 N2 5.52(19) . . . . ? C3 Mn1 B1 N4 -45.9(8) . . . . ? C1 Mn1 B1 N4 166.9(2) . . . . ? C2 Mn1 B1 N4 71.9(2) . . . . ? S2 Mn1 B1 N4 -15.35(19) . . . . ? S1 Mn1 B1 N4 -107.1(2) . . . . ? C14 Mn2 B2 N8 53.7(7) . . . . ? C12 Mn2 B2 N8 -171.4(2) . . . . ? C13 Mn2 B2 N8 -76.4(3) . . . . ? S4 Mn2 B2 N8 9.8(2) . . . . ? S3 Mn2 B2 N8 102.0(2) . . . . ? C14 Mn2 B2 N6 -58.9(7) . . . . ? C12 Mn2 B2 N6 76.0(2) . . . . ? C13 Mn2 B2 N6 170.9(2) . . . . ? S4 Mn2 B2 N6 -102.9(2) . . . . ? S3 Mn2 B2 N6 -10.71(19) . . . . ? N4 B1 N2 C4 92.7(4) . . . . ? Mn1 B1 N2 C4 -9.0(4) . . . . ? N4 B1 N2 C7 -81.5(4) . . . . ? Mn1 B1 N2 C7 176.8(3) . . . . ? N2 B1 N4 C8 -84.1(4) . . . . ? Mn1 B1 N4 C8 18.0(4) . . . . ? N2 B1 N4 C11 86.7(4) . . . . ? Mn1 B1 N4 C11 -171.1(3) . . . . ? N8 B2 N6 C15 -89.1(4) . . . . ? Mn2 B2 N6 C15 13.3(4) . . . . ? N8 B2 N6 C18 84.1(4) . . . . ? Mn2 B2 N6 C18 -173.5(3) . . . . ? N6 B2 N8 C19 90.4(4) . . . . ? Mn2 B2 N8 C19 -12.2(4) . . . . ? N6 B2 N8 C22 -82.0(4) . . . . ? Mn2 B2 N8 C22 175.4(3) . . . . ? C3 Mn1 S1 C4 -172.54(16) . . . . ? C1 Mn1 S1 C4 98.44(16) . . . . ? C2 Mn1 S1 C4 -26(3) . . . . ? S2 Mn1 S1 C4 -82.99(12) . . . . ? B1 Mn1 S1 C4 -2.64(14) . . . . ? C3 Mn1 S2 C8 -174.21(17) . . . . ? C1 Mn1 S2 C8 127(3) . . . . ? C2 Mn1 S2 C8 -85.35(18) . . . . ? S1 Mn1 S2 C8 92.53(13) . . . . ? B1 Mn1 S2 C8 11.61(15) . . . . ? C14 Mn2 S3 C15 178.19(17) . . . . ? C12 Mn2 S3 C15 -92.75(18) . . . . ? C13 Mn2 S3 C15 55(4) . . . . ? S4 Mn2 S3 C15 88.55(13) . . . . ? B2 Mn2 S3 C15 7.75(15) . . . . ? C14 Mn2 S4 C19 -178.09(17) . . . . ? C12 Mn2 S4 C19 -141(4) . . . . ? C13 Mn2 S4 C19 91.66(19) . . . . ? S3 Mn2 S4 C19 -87.12(13) . . . . ? B2 Mn2 S4 C19 -6.97(16) . . . . ? C3 Mn1 C1 O1 -30(7) . . . . ? C2 Mn1 C1 O1 -119(7) . . . . ? S2 Mn1 C1 O1 29(9) . . . . ? S1 Mn1 C1 O1 64(7) . . . . ? B1 Mn1 C1 O1 144(7) . . . . ? C3 Mn1 C2 O2 28(12) . . . . ? C1 Mn1 C2 O2 118(12) . . . . ? S2 Mn1 C2 O2 -61(12) . . . . ? S1 Mn1 C2 O2 -118(11) . . . . ? B1 Mn1 C2 O2 -141(12) . . . . ? C1 Mn1 C3 O3 -70(6) . . . . ? C2 Mn1 C3 O3 24(6) . . . . ? S2 Mn1 C3 O3 112(6) . . . . ? S1 Mn1 C3 O3 -158(6) . . . . ? B1 Mn1 C3 O3 142(6) . . . . ? C7 N2 C4 N1 0.6(4) . . . . ? B1 N2 C4 N1 -174.3(3) . . . . ? C7 N2 C4 S1 -176.6(3) . . . . ? B1 N2 C4 S1 8.4(5) . . . . ? C6 N1 C4 N2 0.0(4) . . . . ? C5 N1 C4 N2 179.2(3) . . . . ? C6 N1 C4 S1 177.4(3) . . . . ? C5 N1 C4 S1 -3.5(5) . . . . ? Mn1 S1 C4 N2 -1.2(3) . . . . ? Mn1 S1 C4 N1 -178.0(3) . . . . ? C4 N1 C6 C7 -0.6(4) . . . . ? C5 N1 C6 C7 -179.8(3) . . . . ? N1 C6 C7 N2 1.0(4) . . . . ? C4 N2 C7 C6 -1.0(4) . . . . ? B1 N2 C7 C6 174.2(3) . . . . ? C11 N4 C8 N3 -0.4(4) . . . . ? B1 N4 C8 N3 171.7(3) . . . . ? C11 N4 C8 S2 178.3(3) . . . . ? B1 N4 C8 S2 -9.7(5) . . . . ? C10 N3 C8 N4 0.0(4) . . . . ? C9 N3 C8 N4 -176.8(3) . . . . ? C10 N3 C8 S2 -178.7(3) . . . . ? C9 N3 C8 S2 4.5(5) . . . . ? Mn1 S2 C8 N4 -7.7(4) . . . . ? Mn1 S2 C8 N3 170.7(3) . . . . ? C8 N3 C10 C11 0.4(4) . . . . ? C9 N3 C10 C11 177.1(4) . . . . ? N3 C10 C11 N4 -0.6(4) . . . . ? C8 N4 C11 C10 0.6(4) . . . . ? B1 N4 C11 C10 -171.7(3) . . . . ? C14 Mn2 C12 O4 15(7) . . . . ? C13 Mn2 C12 O4 105(7) . . . . ? S4 Mn2 C12 O4 -22(10) . . . . ? S3 Mn2 C12 O4 -76(7) . . . . ? B2 Mn2 C12 O4 -156(7) . . . . ? C14 Mn2 C13 O5 -58(14) . . . . ? C12 Mn2 C13 O5 -147(14) . . . . ? S4 Mn2 C13 O5 32(14) . . . . ? S3 Mn2 C13 O5 66(16) . . . . ? B2 Mn2 C13 O5 112(14) . . . . ? C12 Mn2 C14 O6 61(8) . . . . ? C13 Mn2 C14 O6 -33(8) . . . . ? S4 Mn2 C14 O6 -120(8) . . . . ? S3 Mn2 C14 O6 149(8) . . . . ? B2 Mn2 C14 O6 -164(7) . . . . ? C18 N6 C15 N5 -0.9(4) . . . . ? B2 N6 C15 N5 173.1(3) . . . . ? C18 N6 C15 S3 177.9(3) . . . . ? B2 N6 C15 S3 -8.0(5) . . . . ? C17 N5 C15 N6 0.9(4) . . . . ? C16 N5 C15 N6 179.5(3) . . . . ? C17 N5 C15 S3 -178.0(3) . . . . ? C16 N5 C15 S3 0.5(5) . . . . ? Mn2 S3 C15 N6 -4.4(4) . . . . ? Mn2 S3 C15 N5 174.3(3) . . . . ? C15 N5 C17 C18 -0.6(4) . . . . ? C16 N5 C17 C18 -179.1(4) . . . . ? N5 C17 C18 N6 0.0(5) . . . . ? C15 N6 C18 C17 0.6(4) . . . . ? B2 N6 C18 C17 -173.7(3) . . . . ? C22 N8 C19 N7 0.0(4) . . . . ? B2 N8 C19 N7 -173.4(3) . . . . ? C22 N8 C19 S4 -179.0(3) . . . . ? B2 N8 C19 S4 7.6(6) . . . . ? C21 N7 C19 N8 0.4(4) . . . . ? C20 N7 C19 N8 178.0(3) . . . . ? C21 N7 C19 S4 179.5(3) . . . . ? C20 N7 C19 S4 -3.0(5) . . . . ? Mn2 S4 C19 N8 3.8(4) . . . . ? Mn2 S4 C19 N7 -175.0(3) . . . . ? C19 N7 C21 C22 -0.7(5) . . . . ? C20 N7 C21 C22 -178.3(4) . . . . ? N7 C21 C22 N8 0.7(5) . . . . ? C19 N8 C22 C21 -0.5(5) . . . . ? B2 N8 C22 C21 173.3(4) . . . . ? C25 O7 C23 C24 177.0(4) . . . . ? C23 O7 C25 C26 -178.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.700 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.089 data_drab58 _database_code_depnum_ccdc_archive 'CCDC 246939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H24 B Mn N4 O3 S2' _chemical_formula_weight 462.27 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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 17.7829(11) _cell_length_b 7.2140(4) _cell_length_c 18.8722(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.2630(10) _cell_angle_gamma 90.00 _cell_volume 2152.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5284 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.15 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15025 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.15 _reflns_number_total 5043 _reflns_number_gt 4563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0489P)^2^+1.8617P] 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 5043 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 -0.038908(19) 0.47222(4) 0.190936(18) 0.03074(10) Uani 1 1 d . . . S1 S -0.05576(5) 0.39275(7) 0.30520(4) 0.04539(16) Uani 1 1 d . . . S2 S 0.10350(4) 0.37968(9) 0.25293(4) 0.04973(18) Uani 1 1 d . . . B1 B 0.02659(15) 0.7713(3) 0.28624(14) 0.0312(4) Uani 1 1 d . . . N1 N -0.02533(11) 0.7572(2) 0.33274(11) 0.0312(4) Uani 1 1 d . . . N2 N -0.10129(11) 0.6514(2) 0.38791(11) 0.0334(4) Uani 1 1 d . . . N3 N 0.11822(10) 0.7012(2) 0.33339(10) 0.0287(3) Uani 1 1 d . . . N4 N 0.24011(10) 0.5612(2) 0.36959(10) 0.0293(3) Uani 1 1 d . . . O1 O -0.02840(19) 0.6007(3) 0.04789(14) 0.0798(7) Uani 1 1 d . . . O2 O -0.21844(13) 0.5720(3) 0.11106(18) 0.0860(8) Uani 1 1 d . . . O3 O -0.08826(12) 0.0976(3) 0.12410(11) 0.0532(5) Uani 1 1 d . . . C1 C -0.06199(13) 0.6043(3) 0.34343(12) 0.0308(4) Uani 1 1 d . . . C2 C -0.04226(15) 0.9036(3) 0.37039(15) 0.0383(5) Uani 1 1 d . . . C3 C -0.08839(15) 0.8396(3) 0.40431(15) 0.0406(5) Uani 1 1 d . . . C4 C -0.15879(14) 0.5317(3) 0.40727(14) 0.0383(5) Uani 1 1 d . . . C5 C -0.1791(2) 0.6323(5) 0.4675(2) 0.0584(8) Uani 1 1 d . . . C6 C -0.23922(18) 0.4991(5) 0.3301(2) 0.0574(7) Uani 1 1 d . . . C7 C -0.11384(17) 0.3517(4) 0.44582(17) 0.0432(5) Uani 1 1 d . . . C8 C 0.15536(12) 0.5506(3) 0.32099(12) 0.0295(4) Uani 1 1 d . . . C9 C 0.18079(14) 0.8076(3) 0.39105(13) 0.0364(5) Uani 1 1 d . . . C10 C 0.25513(14) 0.7232(3) 0.41338(13) 0.0365(5) Uani 1 1 d . . . C11 C 0.30734(12) 0.4279(3) 0.37414(12) 0.0316(4) Uani 1 1 d . . . C12 C 0.29294(16) 0.2412(3) 0.40339(16) 0.0421(5) Uani 1 1 d . . . C13 C 0.30552(16) 0.4129(4) 0.29282(15) 0.0393(5) Uani 1 1 d . . . C14 C 0.39365(15) 0.5039(4) 0.43301(17) 0.0474(6) Uani 1 1 d . . . C15 C -0.02994(17) 0.5473(4) 0.10438(16) 0.0479(6) Uani 1 1 d . . . C16 C -0.14787(15) 0.5380(3) 0.14349(17) 0.0470(6) Uani 1 1 d . . . C17 C -0.06849(13) 0.2417(3) 0.15134(12) 0.0362(4) Uani 1 1 d . . . H1 H -0.0091(14) 0.696(3) 0.2258(14) 0.031(6) Uiso 1 1 d . . . H1A H 0.0292(14) 0.915(3) 0.2729(14) 0.030(6) Uiso 1 1 d . . . H2 H -0.0246(16) 1.021(4) 0.3673(15) 0.036(6) Uiso 1 1 d . . . H3 H -0.1094(19) 0.899(4) 0.4328(18) 0.056(8) Uiso 1 1 d . . . H5A H -0.132(2) 0.668(5) 0.510(2) 0.069(11) Uiso 1 1 d . . . H5B H -0.211(2) 0.550(5) 0.479(2) 0.069(10) Uiso 1 1 d . . . H5C H -0.2116(19) 0.740(5) 0.4452(18) 0.059(9) Uiso 1 1 d . . . H6A H -0.277(2) 0.434(5) 0.340(2) 0.072(10) Uiso 1 1 d . . . H6B H -0.262(2) 0.617(5) 0.307(2) 0.070(10) Uiso 1 1 d . . . H6C H -0.228(2) 0.436(5) 0.293(2) 0.063(10) Uiso 1 1 d . . . H7A H -0.061(2) 0.375(4) 0.4886(19) 0.059(9) Uiso 1 1 d . . . H7B H -0.1023(19) 0.280(5) 0.4109(19) 0.062(9) Uiso 1 1 d . . . H7C H -0.1501(18) 0.282(4) 0.4630(17) 0.053(8) Uiso 1 1 d . . . H9 H 0.1674(17) 0.919(4) 0.4086(16) 0.043(7) Uiso 1 1 d . . . H10 H 0.3082(17) 0.756(4) 0.4491(16) 0.045(7) Uiso 1 1 d . . . H12A H 0.2990(17) 0.251(4) 0.4566(18) 0.051(8) Uiso 1 1 d . . . H12B H 0.3355(18) 0.157(4) 0.4066(17) 0.050(8) Uiso 1 1 d . . . H12C H 0.2406(18) 0.187(4) 0.3690(17) 0.048(7) Uiso 1 1 d . . . H13A H 0.3459(19) 0.331(4) 0.2970(18) 0.056(8) Uiso 1 1 d . . . H13B H 0.2546(19) 0.368(4) 0.2557(17) 0.045(7) Uiso 1 1 d . . . H13C H 0.3177(16) 0.531(4) 0.2805(16) 0.040(7) Uiso 1 1 d . . . H14A H 0.435(2) 0.417(5) 0.4352(19) 0.063(9) Uiso 1 1 d . . . H14B H 0.3960(18) 0.519(4) 0.4852(18) 0.047(7) Uiso 1 1 d . . . H14C H 0.4039(17) 0.621(4) 0.4159(16) 0.045(7) Uiso 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 0.02567(16) 0.03521(17) 0.02812(17) -0.00153(12) 0.00955(13) 0.00145(12) S1 0.0774(4) 0.0247(2) 0.0467(3) -0.0003(2) 0.0393(3) 0.0000(3) S2 0.0268(3) 0.0441(3) 0.0611(4) -0.0249(3) 0.0053(3) 0.0034(2) B1 0.0346(11) 0.0273(10) 0.0349(11) 0.0016(9) 0.0188(10) 0.0021(9) N1 0.0329(8) 0.0255(7) 0.0388(9) 0.0018(7) 0.0196(7) 0.0043(7) N2 0.0346(9) 0.0302(8) 0.0400(9) 0.0037(7) 0.0211(8) 0.0044(7) N3 0.0311(8) 0.0273(8) 0.0308(8) -0.0020(6) 0.0169(7) -0.0027(6) N4 0.0268(8) 0.0323(8) 0.0286(8) -0.0031(7) 0.0124(7) -0.0024(6) O1 0.121(2) 0.0763(15) 0.0629(14) 0.0024(12) 0.0602(15) -0.0091(14) O2 0.0349(10) 0.0620(13) 0.126(2) -0.0046(14) 0.0072(12) 0.0126(9) O3 0.0557(11) 0.0457(10) 0.0459(10) -0.0110(8) 0.0128(9) -0.0048(8) C1 0.0337(10) 0.0269(9) 0.0321(10) 0.0025(7) 0.0155(8) 0.0035(8) C2 0.0425(12) 0.0258(9) 0.0533(13) -0.0017(9) 0.0276(11) 0.0041(9) C3 0.0462(13) 0.0317(10) 0.0536(14) -0.0006(10) 0.0312(11) 0.0075(9) C4 0.0345(11) 0.0401(11) 0.0454(12) 0.0084(9) 0.0227(10) 0.0023(9) C5 0.070(2) 0.0542(16) 0.078(2) 0.0052(16) 0.0570(19) 0.0040(15) C6 0.0374(13) 0.0697(19) 0.0566(17) 0.0168(15) 0.0143(12) -0.0037(13) C7 0.0413(13) 0.0428(12) 0.0480(14) 0.0133(11) 0.0228(12) 0.0032(10) C8 0.0275(9) 0.0300(9) 0.0305(10) -0.0028(8) 0.0129(8) -0.0022(7) C9 0.0397(11) 0.0338(10) 0.0405(11) -0.0108(9) 0.0225(10) -0.0082(9) C10 0.0323(11) 0.0410(11) 0.0363(11) -0.0113(9) 0.0159(9) -0.0099(9) C11 0.0238(9) 0.0379(10) 0.0314(10) -0.0004(8) 0.0112(8) 0.0009(8) C12 0.0402(13) 0.0416(12) 0.0445(13) 0.0089(10) 0.0194(11) 0.0058(10) C13 0.0382(12) 0.0464(13) 0.0384(12) -0.0017(10) 0.0220(10) 0.0005(10) C14 0.0270(11) 0.0574(15) 0.0499(15) -0.0104(12) 0.0107(10) -0.0013(11) C15 0.0544(15) 0.0505(14) 0.0419(13) -0.0058(11) 0.0246(12) -0.0072(11) C16 0.0332(12) 0.0367(11) 0.0596(15) -0.0004(11) 0.0114(11) 0.0032(9) C17 0.0299(10) 0.0436(11) 0.0289(10) -0.0010(9) 0.0080(8) 0.0034(9) _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 C16 1.787(2) . ? Mn1 C15 1.796(3) . ? Mn1 C17 1.800(2) . ? Mn1 S2 2.3480(6) . ? Mn1 S1 2.3792(7) . ? Mn1 H1 1.73(2) . ? S1 C1 1.713(2) . ? S2 C8 1.713(2) . ? B1 N3 1.541(3) . ? B1 N1 1.541(3) . ? B1 H1 1.16(2) . ? B1 H1A 1.07(2) . ? N1 C1 1.343(3) . ? N1 C2 1.381(3) . ? N2 C1 1.358(3) . ? N2 C3 1.388(3) . ? N2 C4 1.506(3) . ? N3 C8 1.346(3) . ? N3 C9 1.379(3) . ? N4 C8 1.361(2) . ? N4 C10 1.385(3) . ? N4 C11 1.506(3) . ? O1 C15 1.146(3) . ? O2 C16 1.143(3) . ? O3 C17 1.141(3) . ? C2 C3 1.333(3) . ? C2 H2 0.91(3) . ? C3 H3 0.89(3) . ? C4 C6 1.521(4) . ? C4 C7 1.524(3) . ? C4 C5 1.525(4) . ? C5 H5A 0.90(4) . ? C5 H5B 0.92(4) . ? C5 H5C 0.94(3) . ? C6 H6A 0.91(4) . ? C6 H6B 0.96(4) . ? C6 H6C 0.93(3) . ? C7 H7A 0.93(3) . ? C7 H7B 0.93(3) . ? C7 H7C 0.98(3) . ? C9 C10 1.336(3) . ? C9 H9 0.94(3) . ? C10 H10 0.91(3) . ? C11 C12 1.521(3) . ? C11 C13 1.524(3) . ? C11 C14 1.526(3) . ? C12 H12A 0.96(3) . ? C12 H12B 0.95(3) . ? C12 H12C 0.94(3) . ? C13 H13A 0.90(3) . ? C13 H13B 0.91(3) . ? C13 H13C 0.93(3) . ? C14 H14A 0.96(3) . ? C14 H14B 0.97(3) . ? C14 H14C 0.95(3) . ? 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 C16 Mn1 C15 89.54(13) . . ? C16 Mn1 C17 89.63(10) . . ? C15 Mn1 C17 91.82(11) . . ? C16 Mn1 S2 178.87(8) . . ? C15 Mn1 S2 90.80(9) . . ? C17 Mn1 S2 89.29(7) . . ? C16 Mn1 S1 87.72(10) . . ? C15 Mn1 S1 175.97(9) . . ? C17 Mn1 S1 91.11(7) . . ? S2 Mn1 S1 91.99(3) . . ? C16 Mn1 H1 90.9(7) . . ? C15 Mn1 H1 85.7(7) . . ? C17 Mn1 H1 177.5(7) . . ? S2 Mn1 H1 90.2(7) . . ? S1 Mn1 H1 91.4(7) . . ? C1 S1 Mn1 103.08(7) . . ? C8 S2 Mn1 104.85(7) . . ? N3 B1 N1 113.60(17) . . ? N3 B1 H1 111.9(11) . . ? N1 B1 H1 109.2(11) . . ? N3 B1 H1A 107.7(12) . . ? N1 B1 H1A 107.4(12) . . ? H1 B1 H1A 106.6(17) . . ? C1 N1 C2 108.40(17) . . ? C1 N1 B1 126.77(17) . . ? C2 N1 B1 124.82(17) . . ? C1 N2 C3 107.64(18) . . ? C1 N2 C4 127.26(18) . . ? C3 N2 C4 124.61(18) . . ? C8 N3 C9 107.67(17) . . ? C8 N3 B1 129.60(17) . . ? C9 N3 B1 122.05(17) . . ? C8 N4 C10 107.51(17) . . ? C8 N4 C11 127.42(17) . . ? C10 N4 C11 125.03(17) . . ? N1 C1 N2 108.08(17) . . ? N1 C1 S1 122.60(15) . . ? N2 C1 S1 129.32(16) . . ? C3 C2 N1 108.01(19) . . ? C3 C2 H2 131.0(16) . . ? N1 C2 H2 120.9(16) . . ? C2 C3 N2 107.9(2) . . ? C2 C3 H3 130(2) . . ? N2 C3 H3 122(2) . . ? N2 C4 C6 107.5(2) . . ? N2 C4 C7 109.79(18) . . ? C6 C4 C7 112.5(2) . . ? N2 C4 C5 109.1(2) . . ? C6 C4 C5 110.3(3) . . ? C7 C4 C5 107.6(2) . . ? C4 C5 H5A 112(2) . . ? C4 C5 H5B 105(2) . . ? H5A C5 H5B 114(3) . . ? C4 C5 H5C 111.5(19) . . ? H5A C5 H5C 107(3) . . ? H5B C5 H5C 108(3) . . ? C4 C6 H6A 110(2) . . ? C4 C6 H6B 109(2) . . ? H6A C6 H6B 110(3) . . ? C4 C6 H6C 112(2) . . ? H6A C6 H6C 110(3) . . ? H6B C6 H6C 107(3) . . ? C4 C7 H7A 111(2) . . ? C4 C7 H7B 112(2) . . ? H7A C7 H7B 104(3) . . ? C4 C7 H7C 108.1(17) . . ? H7A C7 H7C 111(2) . . ? H7B C7 H7C 110(3) . . ? N3 C8 N4 108.52(17) . . ? N3 C8 S2 124.92(15) . . ? N4 C8 S2 126.53(15) . . ? C10 C9 N3 108.62(19) . . ? C10 C9 H9 130.7(17) . . ? N3 C9 H9 120.7(17) . . ? C9 C10 N4 107.69(19) . . ? C9 C10 H10 131.2(17) . . ? N4 C10 H10 121.1(17) . . ? N4 C11 C12 108.97(17) . . ? N4 C11 C13 109.74(17) . . ? C12 C11 C13 111.9(2) . . ? N4 C11 C14 108.61(18) . . ? C12 C11 C14 109.5(2) . . ? C13 C11 C14 108.00(19) . . ? C11 C12 H12A 110.8(18) . . ? C11 C12 H12B 109.2(17) . . ? H12A C12 H12B 106(2) . . ? C11 C12 H12C 113.2(17) . . ? H12A C12 H12C 111(2) . . ? H12B C12 H12C 107(2) . . ? C11 C13 H13A 108.1(19) . . ? C11 C13 H13B 110.7(17) . . ? H13A C13 H13B 108(3) . . ? C11 C13 H13C 106.5(16) . . ? H13A C13 H13C 110(2) . . ? H13B C13 H13C 113(2) . . ? C11 C14 H14A 107.3(19) . . ? C11 C14 H14B 109.8(17) . . ? H14A C14 H14B 111(3) . . ? C11 C14 H14C 110.9(17) . . ? H14A C14 H14C 109(2) . . ? H14B C14 H14C 109(2) . . ? O1 C15 Mn1 176.1(3) . . ? O2 C16 Mn1 176.6(3) . . ? O3 C17 Mn1 178.1(2) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.415 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.064 data_danr003 _database_code_depnum_ccdc_archive 'CCDC 246940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H32 B Mn N4 O3 S2' _chemical_formula_weight 686.52 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7388(14) _cell_length_b 12.9984(18) _cell_length_c 14.648(2) _cell_angle_alpha 69.777(2) _cell_angle_beta 82.398(2) _cell_angle_gamma 78.822(2) _cell_volume 1702.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8978 _exptl_absorpt_correction_T_max 0.9470 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (600 frames), and at phi = 180 deg (600 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 443(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 10669 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.36 _reflns_number_total 4926 _reflns_number_gt 4293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0600P)^2^] 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 4926 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 Mn 0.22371(3) 0.88430(2) 0.62553(2) 0.02283(12) Uani 1 1 d . . . B B 0.5067(2) 0.86940(19) 0.63727(18) 0.0254(6) Uani 1 1 d . . . H10D H 0.5720 0.9152 0.5940 0.030 Uiso 1 1 calc R . . H10E H 0.4146 0.8976 0.6121 0.030 Uiso 1 1 calc R . . S1 S 0.22166(5) 0.87272(5) 0.79163(4) 0.02968(16) Uani 1 1 d . . . S2 S 0.29226(5) 0.68910(4) 0.66568(4) 0.03027(16) Uani 1 1 d . . . N1 N 0.43597(17) 0.88959(15) 0.88530(13) 0.0292(4) Uani 1 1 d . . . N2 N 0.50152(17) 0.87876(14) 0.73956(12) 0.0239(4) Uani 1 1 d . . . N3 N 0.55716(17) 0.57419(14) 0.65435(13) 0.0259(4) Uani 1 1 d . . . N4 N 0.55217(17) 0.74858(14) 0.63768(12) 0.0241(4) Uani 1 1 d . . . O1 O 0.12412(17) 1.12558(13) 0.56938(12) 0.0406(4) Uani 1 1 d . . . O2 O -0.06853(17) 0.84480(15) 0.65694(13) 0.0458(5) Uani 1 1 d . . . O3 O 0.23106(18) 0.90329(15) 0.41864(13) 0.0473(5) Uani 1 1 d . . . C1 C 0.3905(2) 0.88059(16) 0.80456(15) 0.0243(5) Uani 1 1 d . . . C2 C 0.5790(2) 0.8929(2) 0.86976(18) 0.0390(6) Uani 1 1 d . . . H2A H 0.6364 0.8986 0.9131 0.047 Uiso 1 1 calc R . . C3 C 0.6185(2) 0.8863(2) 0.78103(18) 0.0367(6) Uani 1 1 d . . . H3A H 0.7092 0.8867 0.7516 0.044 Uiso 1 1 calc R . . C4 C 0.2393(2) 0.97483(18) 0.97178(16) 0.0318(5) Uani 1 1 d . . . H4A H 0.2178 1.0316 0.9137 0.038 Uiso 1 1 calc R . . C5 C 0.1585(2) 0.97293(19) 1.05689(17) 0.0341(6) Uani 1 1 d . . . H5A H 0.0821 1.0287 1.0556 0.041 Uiso 1 1 calc R . . C6 C 0.1891(2) 0.8892(2) 1.14465(17) 0.0339(5) Uani 1 1 d . . . C7 C 0.3054(2) 0.8089(2) 1.14485(17) 0.0376(6) Uani 1 1 d . . . H7A H 0.3294 0.7536 1.2032 0.045 Uiso 1 1 calc R . . C8 C 0.3864(2) 0.8091(2) 1.06016(16) 0.0357(6) Uani 1 1 d . . . H8A H 0.4635 0.7539 1.0615 0.043 Uiso 1 1 calc R . . C9 C 0.3527(2) 0.89166(19) 0.97337(16) 0.0284(5) Uani 1 1 d . . . C10 C 0.0950(3) 0.8844(3) 1.23617(18) 0.0521(7) Uani 1 1 d . . . H10A H 0.1309 0.8210 1.2892 0.078 Uiso 1 1 calc R . . H10B H 0.0020 0.8783 1.2259 0.078 Uiso 1 1 calc R . . H10C H 0.0923 0.9508 1.2516 0.078 Uiso 1 1 calc R . . C11 C 0.4714(2) 0.67073(16) 0.65353(14) 0.0233(5) Uani 1 1 d . . . C12 C 0.6954(2) 0.59429(19) 0.63657(17) 0.0326(5) Uani 1 1 d . . . H12A H 0.7753 0.5432 0.6323 0.039 Uiso 1 1 calc R . . C13 C 0.6913(2) 0.70062(19) 0.62690(17) 0.0323(5) Uani 1 1 d . . . H13A H 0.7687 0.7368 0.6149 0.039 Uiso 1 1 calc R . . C14 C 0.4173(2) 0.42657(17) 0.73769(16) 0.0290(5) Uani 1 1 d . . . H14A H 0.3806 0.4619 0.7830 0.035 Uiso 1 1 calc R . . C15 C 0.3751(2) 0.32887(18) 0.74348(18) 0.0345(6) Uani 1 1 d . . . H15A H 0.3082 0.2997 0.7923 0.041 Uiso 1 1 calc R . . C16 C 0.4306(2) 0.27320(18) 0.67769(18) 0.0367(6) Uani 1 1 d . . . C17 C 0.5295(3) 0.31889(18) 0.60567(17) 0.0364(6) Uani 1 1 d . . . H17A H 0.5685 0.2824 0.5615 0.044 Uiso 1 1 calc R . . C18 C 0.5720(2) 0.41715(18) 0.59752(16) 0.0319(5) Uani 1 1 d . . . H18A H 0.6382 0.4467 0.5483 0.038 Uiso 1 1 calc R . . C19 C 0.5146(2) 0.47134(17) 0.66389(15) 0.0256(5) Uani 1 1 d . . . C20 C 0.3872(3) 0.1656(2) 0.6858(2) 0.0597(8) Uani 1 1 d . . . H20A H 0.4362 0.1395 0.6347 0.090 Uiso 1 1 calc R . . H20B H 0.2879 0.1770 0.6799 0.090 Uiso 1 1 calc R . . H20C H 0.4096 0.1116 0.7480 0.090 Uiso 1 1 calc R . . C23 C 0.1657(2) 1.03259(19) 0.59295(15) 0.0278(5) Uani 1 1 d . . . C24 C 0.0455(2) 0.86048(17) 0.64506(16) 0.0292(5) Uani 1 1 d . . . C25 C 0.2292(2) 0.89462(18) 0.49909(19) 0.0300(5) Uani 1 1 d . . . C26 C 0.0282(4) 0.4639(3) 0.8324(3) 0.0697(9) Uani 1 1 d . . . H26A H 0.0106 0.5233 0.7754 0.084 Uiso 1 1 calc R . . C27 C -0.0338(3) 0.3717(3) 0.8527(2) 0.0666(9) Uani 1 1 d . . . H27A H -0.0919 0.3682 0.8087 0.080 Uiso 1 1 calc R . . C28 C -0.0108(3) 0.2851(3) 0.9369(3) 0.0682(9) Uani 1 1 d . . . H28A H -0.0549 0.2234 0.9512 0.082 Uiso 1 1 calc R . . C29 C 0.0777(3) 0.2893(3) 1.0008(3) 0.0728(10) Uani 1 1 d . . . H29A H 0.0944 0.2301 1.0582 0.087 Uiso 1 1 calc R . . C30 C 0.1415(3) 0.3813(3) 0.9796(3) 0.0704(9) Uani 1 1 d . . . H30A H 0.2022 0.3838 1.0225 0.084 Uiso 1 1 calc R . . C31 C 0.1161(4) 0.4687(3) 0.8961(3) 0.0694(10) Uani 1 1 d . . . H31A H 0.1582 0.5312 0.8824 0.083 Uiso 1 1 calc R . . C32 C 0.4004(4) 0.4936(3) 1.0745(2) 0.0682(9) Uani 1 1 d . . . H32A H 0.3321 0.4891 1.1259 0.082 Uiso 1 1 calc R . . C33 C 0.3819(3) 0.5778(3) 0.9881(3) 0.0666(9) Uani 1 1 d . . . H33A H 0.3011 0.6307 0.9802 0.080 Uiso 1 1 calc R . . C34 C 0.4824(4) 0.5835(2) 0.9141(2) 0.0674(10) Uani 1 1 d . . . H34A H 0.4707 0.6409 0.8550 0.081 Uiso 1 1 calc R . . C35 C 0.0898(2) 0.5031(2) 0.56408(19) 0.0443(6) Uani 1 1 d . . . H35A H 0.1502 0.5051 0.6074 0.053 Uiso 1 1 calc R . . C36 C 0.0386(3) 0.5989(2) 0.4929(2) 0.0460(7) Uani 1 1 d . . . H36A H 0.0647 0.6659 0.4879 0.055 Uiso 1 1 calc R . . C37 C -0.0513(3) 0.5961(2) 0.42887(19) 0.0478(7) Uani 1 1 d . . . H37A H -0.0860 0.6611 0.3809 0.057 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 Mn 0.02003(19) 0.02245(19) 0.0261(2) -0.00783(14) -0.00275(14) -0.00307(13) B 0.0195(12) 0.0248(13) 0.0300(14) -0.0049(11) 0.0001(10) -0.0083(10) S1 0.0211(3) 0.0430(4) 0.0263(3) -0.0113(3) -0.0003(2) -0.0094(2) S2 0.0196(3) 0.0223(3) 0.0469(4) -0.0089(3) -0.0004(2) -0.0047(2) N1 0.0240(10) 0.0385(11) 0.0279(10) -0.0139(9) -0.0029(8) -0.0055(8) N2 0.0200(9) 0.0256(10) 0.0284(10) -0.0108(8) -0.0010(8) -0.0057(7) N3 0.0213(9) 0.0231(9) 0.0333(10) -0.0104(8) 0.0021(8) -0.0040(7) N4 0.0203(9) 0.0253(10) 0.0276(10) -0.0098(8) 0.0027(7) -0.0070(7) O1 0.0472(10) 0.0241(10) 0.0467(10) -0.0102(8) -0.0018(8) -0.0007(8) O2 0.0204(9) 0.0585(12) 0.0654(12) -0.0273(10) 0.0003(8) -0.0116(8) O3 0.0573(12) 0.0585(12) 0.0311(11) -0.0221(9) -0.0065(8) -0.0054(9) C1 0.0248(12) 0.0201(11) 0.0268(12) -0.0056(9) -0.0041(9) -0.0036(9) C2 0.0247(12) 0.0620(17) 0.0393(15) -0.0252(13) -0.0047(11) -0.0101(11) C3 0.0202(12) 0.0530(16) 0.0424(15) -0.0209(12) -0.0019(10) -0.0093(11) C4 0.0354(13) 0.0318(13) 0.0295(13) -0.0101(10) -0.0079(10) -0.0042(10) C5 0.0297(12) 0.0380(13) 0.0405(15) -0.0217(12) -0.0081(11) 0.0008(10) C6 0.0290(12) 0.0499(15) 0.0312(13) -0.0219(12) -0.0057(10) -0.0074(11) C7 0.0374(14) 0.0465(15) 0.0266(13) -0.0087(11) -0.0093(10) -0.0029(11) C8 0.0277(12) 0.0450(15) 0.0340(14) -0.0153(12) -0.0070(10) 0.0025(11) C9 0.0246(11) 0.0384(13) 0.0283(12) -0.0161(10) -0.0039(9) -0.0079(10) C10 0.0432(15) 0.079(2) 0.0378(15) -0.0273(15) -0.0013(12) -0.0033(14) C11 0.0246(12) 0.0228(11) 0.0214(11) -0.0063(9) -0.0008(9) -0.0037(9) C12 0.0192(11) 0.0340(13) 0.0460(15) -0.0177(11) 0.0022(10) -0.0019(10) C13 0.0191(11) 0.0357(14) 0.0451(14) -0.0180(11) 0.0047(10) -0.0072(10) C14 0.0250(12) 0.0244(12) 0.0353(13) -0.0099(10) -0.0007(10) 0.0001(9) C15 0.0274(12) 0.0277(13) 0.0423(14) -0.0043(11) -0.0037(10) -0.0030(10) C16 0.0367(13) 0.0248(12) 0.0499(15) -0.0106(11) -0.0183(12) -0.0008(10) C17 0.0443(14) 0.0278(13) 0.0400(14) -0.0170(11) -0.0104(12) 0.0037(11) C18 0.0321(13) 0.0291(12) 0.0321(13) -0.0095(10) -0.0023(10) -0.0003(10) C19 0.0234(11) 0.0209(11) 0.0307(12) -0.0068(9) -0.0050(9) -0.0006(9) C20 0.0635(19) 0.0338(15) 0.089(2) -0.0225(15) -0.0169(17) -0.0113(13) C23 0.0252(11) 0.0352(15) 0.0243(12) -0.0109(10) -0.0012(9) -0.0061(10) C24 0.0331(14) 0.0250(12) 0.0301(13) -0.0112(10) -0.0064(10) 0.0005(10) C25 0.0242(12) 0.0249(12) 0.0426(16) -0.0135(11) -0.0045(10) -0.0019(9) C26 0.073(2) 0.069(2) 0.065(2) -0.0262(18) 0.0194(18) -0.0137(18) C27 0.060(2) 0.073(2) 0.075(2) -0.033(2) -0.0092(17) -0.0102(17) C28 0.060(2) 0.056(2) 0.096(3) -0.0253(19) -0.0208(18) -0.0145(16) C29 0.071(2) 0.056(2) 0.097(3) -0.0251(18) -0.0276(19) -0.0069(17) C30 0.0528(19) 0.079(2) 0.102(3) -0.056(2) -0.0095(18) -0.0114(17) C31 0.063(2) 0.069(2) 0.093(3) -0.050(2) 0.0308(19) -0.0283(18) C32 0.082(2) 0.073(2) 0.062(2) -0.0341(19) 0.0162(18) -0.033(2) C33 0.067(2) 0.057(2) 0.087(3) -0.0404(19) -0.036(2) 0.0139(16) C34 0.130(3) 0.0338(16) 0.0391(18) -0.0036(14) -0.028(2) -0.0155(19) C35 0.0308(13) 0.0611(18) 0.0436(16) -0.0216(14) -0.0014(11) -0.0056(12) C36 0.0392(15) 0.0377(15) 0.0607(18) -0.0189(13) 0.0086(13) -0.0086(12) C37 0.0409(15) 0.0414(16) 0.0457(16) -0.0012(13) 0.0002(13) 0.0024(12) _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 Mn C24 1.791(2) . ? Mn C25 1.804(3) . ? Mn C23 1.810(2) . ? Mn S2 2.3759(7) . ? Mn S1 2.3829(7) . ? B N2 1.538(3) . ? B N4 1.545(3) . ? S1 C1 1.706(2) . ? S2 C11 1.708(2) . ? N1 C1 1.365(3) . ? N1 C2 1.387(3) . ? N1 C9 1.436(3) . ? N2 C1 1.345(3) . ? N2 C3 1.394(3) . ? N3 C11 1.363(3) . ? N3 C12 1.395(3) . ? N3 C19 1.432(3) . ? N4 C11 1.340(3) . ? N4 C13 1.390(3) . ? O1 C23 1.141(3) . ? O2 C24 1.148(3) . ? O3 C25 1.142(3) . ? C2 C3 1.333(3) . ? C4 C5 1.379(3) . ? C4 C9 1.384(3) . ? C5 C6 1.391(3) . ? C6 C7 1.383(3) . ? C6 C10 1.510(3) . ? C7 C8 1.378(3) . ? C8 C9 1.380(3) . ? C12 C13 1.333(3) . ? C14 C15 1.381(3) . ? C14 C19 1.383(3) . ? C15 C16 1.392(3) . ? C16 C17 1.383(3) . ? C16 C20 1.500(3) . ? C17 C18 1.380(3) . ? C18 C19 1.389(3) . ? C26 C27 1.369(4) . ? C26 C31 1.371(5) . ? C27 C28 1.361(4) . ? C28 C29 1.375(4) . ? C29 C30 1.375(4) . ? C30 C31 1.363(5) . ? C32 C34 1.352(5) 2_667 ? C32 C33 1.363(5) . ? C33 C34 1.353(5) . ? C34 C32 1.352(5) 2_667 ? C35 C36 1.373(4) . ? C35 C37 1.377(4) 2_566 ? C36 C37 1.380(4) . ? C37 C35 1.377(4) 2_566 ? 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 C24 Mn C25 91.30(10) . . ? C24 Mn C23 90.66(9) . . ? C25 Mn C23 90.06(9) . . ? C24 Mn S2 87.51(7) . . ? C25 Mn S2 88.81(7) . . ? C23 Mn S2 177.82(7) . . ? C24 Mn S1 90.08(7) . . ? C25 Mn S1 178.58(7) . . ? C23 Mn S1 89.54(7) . . ? S2 Mn S1 91.63(2) . . ? N2 B N4 112.36(17) . . ? C1 S1 Mn 103.79(7) . . ? C11 S2 Mn 104.33(7) . . ? C1 N1 C2 108.48(18) . . ? C1 N1 C9 126.49(17) . . ? C2 N1 C9 125.00(18) . . ? C1 N2 C3 107.78(18) . . ? C1 N2 B 128.56(17) . . ? C3 N2 B 123.66(18) . . ? C11 N3 C12 108.27(17) . . ? C11 N3 C19 126.68(17) . . ? C12 N3 C19 124.89(17) . . ? C11 N4 C13 108.11(17) . . ? C11 N4 B 128.19(17) . . ? C13 N4 B 123.59(17) . . ? N2 C1 N1 107.83(17) . . ? N2 C1 S1 127.40(16) . . ? N1 C1 S1 124.77(16) . . ? C3 C2 N1 107.2(2) . . ? C2 C3 N2 108.8(2) . . ? C5 C4 C9 119.5(2) . . ? C4 C5 C6 121.3(2) . . ? C7 C6 C5 118.1(2) . . ? C7 C6 C10 121.1(2) . . ? C5 C6 C10 120.7(2) . . ? C8 C7 C6 121.3(2) . . ? C7 C8 C9 119.8(2) . . ? C8 C9 C4 120.0(2) . . ? C8 C9 N1 119.24(19) . . ? C4 C9 N1 120.7(2) . . ? N4 C11 N3 107.94(17) . . ? N4 C11 S2 126.55(15) . . ? N3 C11 S2 125.47(16) . . ? C13 C12 N3 106.93(18) . . ? C12 C13 N4 108.74(19) . . ? C15 C14 C19 119.4(2) . . ? C14 C15 C16 121.3(2) . . ? C17 C16 C15 117.9(2) . . ? C17 C16 C20 120.9(2) . . ? C15 C16 C20 121.2(2) . . ? C18 C17 C16 121.8(2) . . ? C17 C18 C19 119.1(2) . . ? C14 C19 C18 120.3(2) . . ? C14 C19 N3 120.66(19) . . ? C18 C19 N3 119.00(19) . . ? O1 C23 Mn 176.36(19) . . ? O2 C24 Mn 179.4(2) . . ? O3 C25 Mn 178.6(2) . . ? C27 C26 C31 120.1(3) . . ? C28 C27 C26 120.4(3) . . ? C27 C28 C29 119.7(3) . . ? C28 C29 C30 119.8(3) . . ? C31 C30 C29 120.3(3) . . ? C30 C31 C26 119.7(3) . . ? C34 C32 C33 120.3(3) 2_667 . ? C34 C33 C32 119.2(3) . . ? C32 C34 C33 120.4(3) 2_667 . ? C36 C35 C37 119.8(2) . 2_566 ? C35 C36 C37 120.1(2) . . ? C35 C37 C36 120.1(2) 2_566 . ? 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 C24 Mn S1 C1 174.87(10) . . . . ? C25 Mn S1 C1 -21(3) . . . . ? C23 Mn S1 C1 -94.47(10) . . . . ? S2 Mn S1 C1 87.37(7) . . . . ? C24 Mn S2 C11 178.79(10) . . . . ? C25 Mn S2 C11 87.44(10) . . . . ? C23 Mn S2 C11 146.3(18) . . . . ? S1 Mn S2 C11 -91.21(7) . . . . ? N4 B N2 C1 -95.7(2) . . . . ? N4 B N2 C3 83.9(2) . . . . ? N2 B N4 C11 87.4(2) . . . . ? N2 B N4 C13 -88.3(2) . . . . ? C3 N2 C1 N1 0.3(2) . . . . ? B N2 C1 N1 179.86(18) . . . . ? C3 N2 C1 S1 -179.49(16) . . . . ? B N2 C1 S1 0.1(3) . . . . ? C2 N1 C1 N2 -0.3(2) . . . . ? C9 N1 C1 N2 -178.34(18) . . . . ? C2 N1 C1 S1 179.47(17) . . . . ? C9 N1 C1 S1 1.4(3) . . . . ? Mn S1 C1 N2 -7.9(2) . . . . ? Mn S1 C1 N1 172.42(16) . . . . ? C1 N1 C2 C3 0.2(3) . . . . ? C9 N1 C2 C3 178.3(2) . . . . ? N1 C2 C3 N2 0.0(3) . . . . ? C1 N2 C3 C2 -0.1(3) . . . . ? B N2 C3 C2 -179.8(2) . . . . ? C9 C4 C5 C6 0.3(3) . . . . ? C4 C5 C6 C7 1.6(3) . . . . ? C4 C5 C6 C10 -176.5(2) . . . . ? C5 C6 C7 C8 -2.2(4) . . . . ? C10 C6 C7 C8 175.9(2) . . . . ? C6 C7 C8 C9 0.9(4) . . . . ? C7 C8 C9 C4 1.1(3) . . . . ? C7 C8 C9 N1 -178.6(2) . . . . ? C5 C4 C9 C8 -1.7(3) . . . . ? C5 C4 C9 N1 178.01(19) . . . . ? C1 N1 C9 C8 118.5(2) . . . . ? C2 N1 C9 C8 -59.3(3) . . . . ? C1 N1 C9 C4 -61.2(3) . . . . ? C2 N1 C9 C4 121.1(2) . . . . ? C13 N4 C11 N3 0.9(2) . . . . ? B N4 C11 N3 -175.39(18) . . . . ? C13 N4 C11 S2 -176.66(16) . . . . ? B N4 C11 S2 7.1(3) . . . . ? C12 N3 C11 N4 -1.1(2) . . . . ? C19 N3 C11 N4 -176.53(18) . . . . ? C12 N3 C11 S2 176.46(16) . . . . ? C19 N3 C11 S2 1.0(3) . . . . ? Mn S2 C11 N4 7.9(2) . . . . ? Mn S2 C11 N3 -169.20(16) . . . . ? C11 N3 C12 C13 0.9(2) . . . . ? C19 N3 C12 C13 176.43(19) . . . . ? N3 C12 C13 N4 -0.4(3) . . . . ? C11 N4 C13 C12 -0.3(3) . . . . ? B N4 C13 C12 176.16(19) . . . . ? C19 C14 C15 C16 1.3(3) . . . . ? C14 C15 C16 C17 -0.2(3) . . . . ? C14 C15 C16 C20 178.4(2) . . . . ? C15 C16 C17 C18 -0.7(3) . . . . ? C20 C16 C17 C18 -179.3(2) . . . . ? C16 C17 C18 C19 0.5(3) . . . . ? C15 C14 C19 C18 -1.6(3) . . . . ? C15 C14 C19 N3 178.15(18) . . . . ? C17 C18 C19 C14 0.7(3) . . . . ? C17 C18 C19 N3 -179.03(18) . . . . ? C11 N3 C19 C14 -49.8(3) . . . . ? C12 N3 C19 C14 135.5(2) . . . . ? C11 N3 C19 C18 129.9(2) . . . . ? C12 N3 C19 C18 -44.8(3) . . . . ? C24 Mn C23 O1 -46(3) . . . . ? C25 Mn C23 O1 46(3) . . . . ? S2 Mn C23 O1 -13(5) . . . . ? S1 Mn C23 O1 -136(3) . . . . ? C25 Mn C24 O2 29(26) . . . . ? C23 Mn C24 O2 119(26) . . . . ? S2 Mn C24 O2 -60(26) . . . . ? S1 Mn C24 O2 -151(26) . . . . ? C24 Mn C25 O3 77(9) . . . . ? C23 Mn C25 O3 -14(9) . . . . ? S2 Mn C25 O3 164(9) . . . . ? S1 Mn C25 O3 -88(9) . . . . ? C31 C26 C27 C28 1.2(5) . . . . ? C26 C27 C28 C29 -1.5(5) . . . . ? C27 C28 C29 C30 0.5(5) . . . . ? C28 C29 C30 C31 0.7(5) . . . . ? C29 C30 C31 C26 -1.0(5) . . . . ? C27 C26 C31 C30 0.0(5) . . . . ? C34 C32 C33 C34 -0.2(5) 2_667 . . . ? C32 C33 C34 C32 0.2(5) . . . 2_667 ? C37 C35 C36 C37 0.2(4) 2_566 . . . ? C35 C36 C37 C35 -0.2(4) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.36 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.317 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.053 data_danr015 _database_code_depnum_ccdc_archive 'CCDC 246941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 B Mn N6 O3 S3' _chemical_formula_weight 683.52 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' _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 9.720(4) _cell_length_b 18.476(8) _cell_length_c 17.894(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.915(7) _cell_angle_gamma 90.00 _cell_volume 3212(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 633 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 19.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8814 _exptl_absorpt_correction_T_max 0.9381 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 17720 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6847 _reflns_number_gt 4396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0420P)^2^] 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 6847 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Mn Mn 0.43099(6) 0.20710(3) 0.19744(3) 0.02281(16) Uani 1 1 d . . . B B 0.2353(4) 0.0240(2) 0.1068(2) 0.0192(9) Uani 1 1 d . . . N1 N 0.0244(3) 0.14984(15) 0.21796(16) 0.0250(7) Uani 1 1 d . . . N2 N 0.1296(3) 0.07284(14) 0.14785(15) 0.0172(6) Uani 1 1 d . . . N3 N 0.3571(3) 0.15783(14) -0.03255(15) 0.0203(7) Uani 1 1 d . . . N4 N 0.2855(3) 0.07038(14) 0.03857(15) 0.0182(7) Uani 1 1 d . . . N5 N 0.5439(3) -0.00267(15) 0.23356(16) 0.0229(7) Uani 1 1 d . . . N6 N 0.3590(3) 0.00301(14) 0.16170(14) 0.0174(7) Uani 1 1 d . . . O1 O 0.6161(4) 0.30137(15) 0.11563(19) 0.0616(10) Uani 1 1 d . . . O2 O 0.6390(3) 0.20330(16) 0.32135(17) 0.0486(8) Uani 1 1 d . . . O3 O 0.2841(3) 0.32832(13) 0.26552(14) 0.0351(7) Uani 1 1 d . . . S1 S 0.28565(10) 0.12628(5) 0.26890(5) 0.0219(2) Uani 1 1 d . . . S2 S 0.26421(10) 0.21166(5) 0.09530(5) 0.0237(2) Uani 1 1 d . . . S3 S 0.55189(10) 0.11003(5) 0.13743(5) 0.0221(2) Uani 1 1 d . . . C1 C 0.5408(4) 0.2648(2) 0.1472(2) 0.0354(10) Uani 1 1 d . . . C2 C 0.5557(4) 0.2035(2) 0.2729(2) 0.0308(10) Uani 1 1 d . . . C3 C 0.3412(4) 0.28096(19) 0.2383(2) 0.0256(9) Uani 1 1 d . . . C4 C 0.1442(4) 0.11364(18) 0.21032(19) 0.0210(8) Uani 1 1 d . . . C5 C -0.0045(4) 0.2012(2) 0.2770(2) 0.0366(10) Uani 1 1 d . . . H5A H 0.0737 0.2029 0.3129 0.055 Uiso 1 1 calc R . . H5B H -0.0873 0.1859 0.3025 0.055 Uiso 1 1 calc R . . H5C H -0.0195 0.2493 0.2552 0.055 Uiso 1 1 calc R . . C6 C -0.0641(4) 0.13452(19) 0.1583(2) 0.0261(9) Uani 1 1 d . . . H6A H -0.1541 0.1534 0.1496 0.031 Uiso 1 1 calc R . . C7 C 0.0021(4) 0.08759(18) 0.11489(19) 0.0218(8) Uani 1 1 d . . . H7A H -0.0330 0.0678 0.0691 0.026 Uiso 1 1 calc R . . C8 C 0.3033(4) 0.14333(17) 0.03413(18) 0.0186(8) Uani 1 1 d . . . C9 C 0.3952(4) 0.22943(18) -0.0592(2) 0.0335(10) Uani 1 1 d . . . H9A H 0.3768 0.2655 -0.0207 0.050 Uiso 1 1 calc R . . H9B H 0.3409 0.2409 -0.1049 0.050 Uiso 1 1 calc R . . H9C H 0.4933 0.2300 -0.0700 0.050 Uiso 1 1 calc R . . C10 C 0.3721(4) 0.09497(19) -0.07168(19) 0.0254(9) Uani 1 1 d . . . H10A H 0.4068 0.0902 -0.1204 0.031 Uiso 1 1 calc R . . C11 C 0.3283(4) 0.04124(18) -0.02794(18) 0.0214(8) Uani 1 1 d . . . H11A H 0.3269 -0.0087 -0.0406 0.026 Uiso 1 1 calc R . . C12 C 0.4821(4) 0.03453(18) 0.17746(19) 0.0196(8) Uani 1 1 d . . . C13 C 0.6802(4) 0.0127(2) 0.2684(2) 0.0363(10) Uani 1 1 d . . . H13A H 0.7217 0.0540 0.2431 0.054 Uiso 1 1 calc R . . H13B H 0.7396 -0.0298 0.2638 0.054 Uiso 1 1 calc R . . H13C H 0.6701 0.0243 0.3213 0.054 Uiso 1 1 calc R . . C14 C 0.4590(4) -0.05743(18) 0.25565(19) 0.0262(9) Uani 1 1 d . . . H14A H 0.4768 -0.0909 0.2951 0.031 Uiso 1 1 calc R . . C15 C 0.3461(4) -0.05448(18) 0.21093(19) 0.0233(9) Uani 1 1 d . . . H15A H 0.2698 -0.0865 0.2126 0.028 Uiso 1 1 calc R . . C16 C 0.2477(4) -0.10604(18) 0.04713(19) 0.0247(9) Uani 1 1 d . . . H16A H 0.3387 -0.0938 0.0341 0.030 Uiso 1 1 calc R . . C17 C 0.1992(4) -0.17503(19) 0.0314(2) 0.0295(10) Uani 1 1 d . . . H17A H 0.2558 -0.2087 0.0066 0.035 Uiso 1 1 calc R . . C18 C 0.0687(4) -0.19493(19) 0.0516(2) 0.0332(10) Uani 1 1 d . . . H18A H 0.0345 -0.2420 0.0404 0.040 Uiso 1 1 calc R . . C19 C -0.0113(4) -0.14558(19) 0.0882(2) 0.0292(9) Uani 1 1 d . . . H19A H -0.1002 -0.1592 0.1036 0.035 Uiso 1 1 calc R . . C20 C 0.0370(4) -0.07631(19) 0.10273(19) 0.0262(9) Uani 1 1 d . . . H20A H -0.0204 -0.0433 0.1279 0.031 Uiso 1 1 calc R . . C21 C 0.1668(4) -0.05339(18) 0.08177(18) 0.0195(8) Uani 1 1 d . . . C22 C 0.1088(7) 0.3954(4) 0.0730(3) 0.081(2) Uani 1 1 d . . . H22A H 0.1710 0.3704 0.0423 0.097 Uiso 1 1 calc R . . C23 C 0.1072(6) 0.4697(4) 0.0731(3) 0.083(2) Uani 1 1 d . . . H23A H 0.1671 0.4962 0.0424 0.099 Uiso 1 1 calc R . . C24 C 0.0161(6) 0.5057(3) 0.1191(3) 0.0648(15) Uani 1 1 d . . . H24A H 0.0125 0.5571 0.1201 0.078 Uiso 1 1 calc R . . C25 C -0.0664(6) 0.4662(3) 0.1621(3) 0.0706(17) Uani 1 1 d . . . H25A H -0.1293 0.4897 0.1935 0.085 Uiso 1 1 calc R . . C26 C -0.0603(7) 0.3934(3) 0.1608(4) 0.099(2) Uani 1 1 d . . . H26A H -0.1172 0.3664 0.1927 0.118 Uiso 1 1 calc R . . C27 C 0.0243(7) 0.3579(4) 0.1155(4) 0.096(2) Uani 1 1 d . . . H27A H 0.0238 0.3065 0.1137 0.115 Uiso 1 1 calc R . . C28 C 0.4340(12) 0.4695(7) -0.0586(4) 0.125(4) Uani 1 1 d . . . H28A H 0.3876 0.4478 -0.1005 0.151 Uiso 1 1 calc R . . C29 C 0.3988(9) 0.5360(7) -0.0368(6) 0.120(3) Uani 1 1 d . . . H29A H 0.3267 0.5611 -0.0629 0.143 Uiso 1 1 calc R . . C30 C 0.4639(13) 0.5672(4) 0.0210(6) 0.118(3) Uani 1 1 d . . . H30A H 0.4395 0.6147 0.0361 0.141 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 Mn 0.0222(4) 0.0213(3) 0.0252(3) -0.0055(2) 0.0044(3) -0.0031(3) B 0.016(3) 0.023(2) 0.0184(19) -0.0014(16) 0.0024(18) -0.0003(18) N1 0.019(2) 0.0264(17) 0.0305(17) -0.0041(13) 0.0066(15) 0.0003(14) N2 0.0118(18) 0.0204(15) 0.0197(14) 0.0012(12) 0.0035(13) -0.0001(13) N3 0.0214(19) 0.0196(15) 0.0202(15) 0.0026(12) 0.0049(13) 0.0014(13) N4 0.0164(19) 0.0193(15) 0.0190(15) -0.0027(12) 0.0013(13) 0.0018(13) N5 0.017(2) 0.0274(17) 0.0242(16) -0.0028(13) -0.0039(14) 0.0016(14) N6 0.0137(19) 0.0219(15) 0.0168(14) 0.0014(11) 0.0012(13) 0.0006(13) O1 0.071(3) 0.0385(18) 0.078(2) -0.0063(17) 0.042(2) -0.0216(17) O2 0.031(2) 0.067(2) 0.0470(19) -0.0207(16) -0.0066(16) 0.0021(16) O3 0.0354(19) 0.0295(15) 0.0406(16) -0.0106(13) 0.0056(14) 0.0044(14) S1 0.0204(6) 0.0252(5) 0.0202(4) -0.0016(4) 0.0016(4) -0.0013(4) S2 0.0285(6) 0.0192(4) 0.0236(5) -0.0019(4) 0.0041(4) 0.0028(4) S3 0.0172(6) 0.0217(4) 0.0275(5) -0.0021(4) 0.0043(4) -0.0015(4) C1 0.038(3) 0.025(2) 0.044(2) -0.0100(18) 0.011(2) -0.002(2) C2 0.021(3) 0.034(2) 0.038(2) -0.0111(19) 0.009(2) -0.0007(18) C3 0.022(2) 0.028(2) 0.027(2) -0.0026(16) 0.0009(17) -0.0095(18) C4 0.017(2) 0.0209(18) 0.0256(19) 0.0048(15) 0.0058(16) -0.0002(16) C5 0.031(3) 0.040(2) 0.040(2) -0.0103(19) 0.011(2) 0.005(2) C6 0.007(2) 0.034(2) 0.037(2) -0.0017(17) -0.0020(17) 0.0042(17) C7 0.012(2) 0.0277(19) 0.0253(19) -0.0011(15) -0.0040(16) -0.0027(16) C8 0.011(2) 0.0230(18) 0.0212(18) -0.0001(14) -0.0014(15) 0.0027(15) C9 0.044(3) 0.027(2) 0.030(2) 0.0052(17) 0.011(2) -0.0067(19) C10 0.026(3) 0.031(2) 0.0196(18) -0.0024(16) 0.0052(17) 0.0049(18) C11 0.019(2) 0.0229(18) 0.0227(18) -0.0032(15) 0.0013(16) 0.0045(16) C12 0.016(2) 0.0199(18) 0.0236(18) -0.0027(14) 0.0023(16) 0.0044(16) C13 0.028(3) 0.035(2) 0.044(2) -0.0009(19) -0.013(2) 0.000(2) C14 0.033(3) 0.0218(19) 0.0238(19) 0.0047(15) 0.0004(18) -0.0003(18) C15 0.022(2) 0.0241(19) 0.0242(19) 0.0012(15) 0.0018(17) -0.0006(17) C16 0.024(3) 0.0226(19) 0.0271(19) 0.0005(16) 0.0010(17) -0.0012(17) C17 0.037(3) 0.0201(19) 0.031(2) -0.0018(16) -0.0003(19) -0.0001(18) C18 0.039(3) 0.021(2) 0.039(2) 0.0010(17) -0.008(2) -0.0123(19) C19 0.023(3) 0.030(2) 0.035(2) 0.0058(17) -0.0023(19) -0.0075(18) C20 0.022(3) 0.030(2) 0.027(2) 0.0004(16) 0.0015(17) -0.0014(17) C21 0.015(2) 0.0203(18) 0.0225(18) 0.0001(14) -0.0038(16) 0.0000(15) C22 0.070(5) 0.110(5) 0.063(4) -0.008(4) 0.009(3) 0.047(4) C23 0.059(5) 0.143(6) 0.046(3) 0.007(4) 0.005(3) -0.011(4) C24 0.060(4) 0.073(4) 0.060(3) -0.014(3) -0.007(3) -0.004(3) C25 0.074(5) 0.060(4) 0.079(4) -0.017(3) 0.028(3) 0.016(3) C26 0.118(6) 0.064(4) 0.118(5) -0.011(4) 0.057(5) 0.030(4) C27 0.119(6) 0.081(5) 0.090(5) -0.002(4) 0.033(5) 0.045(4) C28 0.179(10) 0.160(9) 0.036(4) 0.001(5) -0.011(5) -0.121(8) C29 0.115(7) 0.143(9) 0.100(7) 0.051(6) -0.005(6) -0.065(7) C30 0.182(10) 0.079(5) 0.095(6) 0.002(5) 0.049(6) -0.061(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn C1 1.775(4) . ? Mn C2 1.786(4) . ? Mn C3 1.789(4) . ? Mn S2 2.4037(14) . ? Mn S3 2.4156(12) . ? Mn S1 2.4455(12) . ? B N2 1.568(5) . ? B N6 1.576(5) . ? B N4 1.581(5) . ? B C21 1.634(5) . ? N1 C4 1.354(4) . ? N1 C6 1.378(4) . ? N1 C5 1.454(4) . ? N2 C4 1.352(4) . ? N2 C7 1.382(4) . ? N3 C8 1.346(4) . ? N3 C10 1.366(4) . ? N3 C9 1.458(4) . ? N4 C8 1.362(4) . ? N4 C11 1.383(4) . ? N5 C12 1.342(4) . ? N5 C14 1.373(4) . ? N5 C13 1.473(4) . ? N6 C12 1.352(4) . ? N6 C15 1.388(4) . ? O1 C1 1.156(4) . ? O2 C2 1.166(4) . ? O3 C3 1.153(4) . ? S1 C4 1.716(4) . ? S2 C8 1.722(3) . ? S3 C12 1.718(4) . ? C6 C7 1.342(5) . ? C10 C11 1.342(5) . ? C14 C15 1.337(5) . ? C16 C17 1.385(5) . ? C16 C21 1.408(5) . ? C17 C18 1.380(5) . ? C18 C19 1.378(5) . ? C19 C20 1.385(5) . ? C20 C21 1.394(5) . ? C22 C27 1.331(8) . ? C22 C23 1.373(8) . ? C23 C24 1.398(7) . ? C24 C25 1.345(7) . ? C25 C26 1.347(7) . ? C26 C27 1.344(7) . ? C28 C29 1.337(11) . ? C28 C30 1.362(11) 3_665 ? C29 C30 1.326(9) . ? C30 C28 1.362(11) 3_665 ? 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 C1 Mn C2 90.07(19) . . ? C1 Mn C3 93.34(17) . . ? C2 Mn C3 92.74(17) . . ? C1 Mn S2 89.74(14) . . ? C2 Mn S2 179.63(13) . . ? C3 Mn S2 87.59(12) . . ? C1 Mn S3 84.90(13) . . ? C2 Mn S3 88.88(12) . . ? C3 Mn S3 177.62(12) . . ? S2 Mn S3 90.79(4) . . ? C1 Mn S1 178.29(15) . . ? C2 Mn S1 88.34(13) . . ? C3 Mn S1 87.37(12) . . ? S2 Mn S1 91.85(5) . . ? S3 Mn S1 94.43(5) . . ? N2 B N6 110.4(3) . . ? N2 B N4 105.9(3) . . ? N6 B N4 111.5(3) . . ? N2 B C21 111.4(3) . . ? N6 B C21 104.5(3) . . ? N4 B C21 113.3(3) . . ? C4 N1 C6 109.7(3) . . ? C4 N1 C5 125.7(3) . . ? C6 N1 C5 124.5(3) . . ? C4 N2 C7 108.1(3) . . ? C4 N2 B 131.0(3) . . ? C7 N2 B 120.4(3) . . ? C8 N3 C10 109.7(3) . . ? C8 N3 C9 125.5(3) . . ? C10 N3 C9 124.8(3) . . ? C8 N4 C11 107.0(3) . . ? C8 N4 B 128.6(3) . . ? C11 N4 B 124.3(3) . . ? C12 N5 C14 109.5(3) . . ? C12 N5 C13 126.3(3) . . ? C14 N5 C13 124.2(3) . . ? C12 N6 C15 107.2(3) . . ? C12 N6 B 132.5(3) . . ? C15 N6 B 120.1(3) . . ? C4 S1 Mn 103.21(12) . . ? C8 S2 Mn 107.47(12) . . ? C12 S3 Mn 102.28(12) . . ? O1 C1 Mn 177.7(4) . . ? O2 C2 Mn 177.7(4) . . ? O3 C3 Mn 179.1(3) . . ? N2 C4 N1 107.0(3) . . ? N2 C4 S1 129.9(3) . . ? N1 C4 S1 123.0(3) . . ? C7 C6 N1 106.4(3) . . ? C6 C7 N2 108.7(3) . . ? N3 C8 N4 107.6(3) . . ? N3 C8 S2 121.2(3) . . ? N4 C8 S2 131.1(3) . . ? C11 C10 N3 106.8(3) . . ? C10 C11 N4 108.9(3) . . ? N5 C12 N6 107.9(3) . . ? N5 C12 S3 123.7(3) . . ? N6 C12 S3 128.4(3) . . ? C15 C14 N5 106.7(3) . . ? C14 C15 N6 108.8(3) . . ? C17 C16 C21 122.3(4) . . ? C18 C17 C16 120.1(4) . . ? C19 C18 C17 119.1(3) . . ? C18 C19 C20 120.5(4) . . ? C19 C20 C21 122.3(4) . . ? C20 C21 C16 115.6(3) . . ? C20 C21 B 123.8(3) . . ? C16 C21 B 119.8(3) . . ? C27 C22 C23 120.9(6) . . ? C22 C23 C24 118.9(6) . . ? C25 C24 C23 118.7(6) . . ? C26 C25 C24 120.3(5) . . ? C25 C26 C27 121.8(7) . . ? C22 C27 C26 119.4(7) . . ? C29 C28 C30 120.1(7) . 3_665 ? C30 C29 C28 120.5(9) . . ? C29 C30 C28 119.4(8) . 3_665 ? 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 N6 B N2 C4 20.5(5) . . . . ? N4 B N2 C4 -100.3(4) . . . . ? C21 B N2 C4 136.1(3) . . . . ? N6 B N2 C7 -168.9(3) . . . . ? N4 B N2 C7 70.3(4) . . . . ? C21 B N2 C7 -53.3(4) . . . . ? N2 B N4 C8 33.5(5) . . . . ? N6 B N4 C8 -86.5(4) . . . . ? C21 B N4 C8 155.9(3) . . . . ? N2 B N4 C11 -150.7(3) . . . . ? N6 B N4 C11 89.2(4) . . . . ? C21 B N4 C11 -28.4(5) . . . . ? N2 B N6 C12 -90.7(4) . . . . ? N4 B N6 C12 26.7(5) . . . . ? C21 B N6 C12 149.4(3) . . . . ? N2 B N6 C15 82.5(4) . . . . ? N4 B N6 C15 -160.1(3) . . . . ? C21 B N6 C15 -37.3(4) . . . . ? C1 Mn S1 C4 -157(4) . . . . ? C2 Mn S1 C4 -178.83(17) . . . . ? C3 Mn S1 C4 88.35(17) . . . . ? S2 Mn S1 C4 0.85(13) . . . . ? S3 Mn S1 C4 -90.08(13) . . . . ? C1 Mn S2 C8 88.23(17) . . . . ? C2 Mn S2 C8 29(22) . . . . ? C3 Mn S2 C8 -178.42(17) . . . . ? S3 Mn S2 C8 3.33(13) . . . . ? S1 Mn S2 C8 -91.13(13) . . . . ? C1 Mn S3 C12 175.82(19) . . . . ? C2 Mn S3 C12 85.65(18) . . . . ? C3 Mn S3 C12 -142(3) . . . . ? S2 Mn S3 C12 -94.52(13) . . . . ? S1 Mn S3 C12 -2.60(13) . . . . ? C2 Mn C1 O1 29(9) . . . . ? C3 Mn C1 O1 122(9) . . . . ? S2 Mn C1 O1 -151(9) . . . . ? S3 Mn C1 O1 -60(9) . . . . ? S1 Mn C1 O1 7(13) . . . . ? C1 Mn C2 O2 23(9) . . . . ? C3 Mn C2 O2 -71(9) . . . . ? S2 Mn C2 O2 82(25) . . . . ? S3 Mn C2 O2 107(9) . . . . ? S1 Mn C2 O2 -158(9) . . . . ? C1 Mn C3 O3 -114(22) . . . . ? C2 Mn C3 O3 -23(22) . . . . ? S2 Mn C3 O3 157(22) . . . . ? S3 Mn C3 O3 -156(20) . . . . ? S1 Mn C3 O3 65(22) . . . . ? C7 N2 C4 N1 3.4(4) . . . . ? B N2 C4 N1 174.9(3) . . . . ? C7 N2 C4 S1 -172.3(3) . . . . ? B N2 C4 S1 -0.8(5) . . . . ? C6 N1 C4 N2 -2.8(4) . . . . ? C5 N1 C4 N2 -178.8(3) . . . . ? C6 N1 C4 S1 173.2(3) . . . . ? C5 N1 C4 S1 -2.7(5) . . . . ? Mn S1 C4 N2 75.1(3) . . . . ? Mn S1 C4 N1 -99.9(3) . . . . ? C4 N1 C6 C7 1.1(4) . . . . ? C5 N1 C6 C7 177.1(3) . . . . ? N1 C6 C7 N2 1.0(4) . . . . ? C4 N2 C7 C6 -2.8(4) . . . . ? B N2 C7 C6 -175.3(3) . . . . ? C10 N3 C8 N4 1.0(4) . . . . ? C9 N3 C8 N4 -178.5(3) . . . . ? C10 N3 C8 S2 -177.0(3) . . . . ? C9 N3 C8 S2 3.5(5) . . . . ? C11 N4 C8 N3 -0.9(4) . . . . ? B N4 C8 N3 175.4(3) . . . . ? C11 N4 C8 S2 176.8(3) . . . . ? B N4 C8 S2 -6.9(6) . . . . ? Mn S2 C8 N3 -108.1(3) . . . . ? Mn S2 C8 N4 74.5(3) . . . . ? C8 N3 C10 C11 -0.7(4) . . . . ? C9 N3 C10 C11 178.8(3) . . . . ? N3 C10 C11 N4 0.2(4) . . . . ? C8 N4 C11 C10 0.4(4) . . . . ? B N4 C11 C10 -176.1(3) . . . . ? C14 N5 C12 N6 -1.6(4) . . . . ? C13 N5 C12 N6 179.8(3) . . . . ? C14 N5 C12 S3 176.7(3) . . . . ? C13 N5 C12 S3 -1.9(5) . . . . ? C15 N6 C12 N5 0.9(4) . . . . ? B N6 C12 N5 174.7(3) . . . . ? C15 N6 C12 S3 -177.4(3) . . . . ? B N6 C12 S3 -3.5(5) . . . . ? Mn S3 C12 N5 -100.1(3) . . . . ? Mn S3 C12 N6 77.9(3) . . . . ? C12 N5 C14 C15 1.7(4) . . . . ? C13 N5 C14 C15 -179.6(3) . . . . ? N5 C14 C15 N6 -1.2(4) . . . . ? C12 N6 C15 C14 0.2(4) . . . . ? B N6 C15 C14 -174.5(3) . . . . ? C21 C16 C17 C18 -1.8(5) . . . . ? C16 C17 C18 C19 -0.7(6) . . . . ? C17 C18 C19 C20 1.8(6) . . . . ? C18 C19 C20 C21 -0.3(6) . . . . ? C19 C20 C21 C16 -2.1(5) . . . . ? C19 C20 C21 B -172.1(3) . . . . ? C17 C16 C21 C20 3.2(5) . . . . ? C17 C16 C21 B 173.6(3) . . . . ? N2 B C21 C20 -7.5(5) . . . . ? N6 B C21 C20 111.6(4) . . . . ? N4 B C21 C20 -126.8(4) . . . . ? N2 B C21 C16 -177.1(3) . . . . ? N6 B C21 C16 -57.9(4) . . . . ? N4 B C21 C16 63.6(4) . . . . ? C27 C22 C23 C24 0.6(10) . . . . ? C22 C23 C24 C25 0.4(8) . . . . ? C23 C24 C25 C26 0.3(9) . . . . ? C24 C25 C26 C27 -2.0(11) . . . . ? C23 C22 C27 C26 -2.3(11) . . . . ? C25 C26 C27 C22 3.0(11) . . . . ? C30 C28 C29 C30 0.8(13) 3_665 . . . ? C28 C29 C30 C28 -0.8(13) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.857 _refine_diff_density_max 0.432 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.083 data_danr020 _database_code_depnum_ccdc_archive 'CCDC 246942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 B Mn N6 O3 S2' _chemical_formula_weight 444.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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 8.189(2) _cell_length_b 15.692(2) _cell_length_c 14.659(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.65(2) _cell_angle_gamma 90.00 _cell_volume 1813.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8270 _exptl_absorpt_correction_T_max 0.9077 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (600 frames), and at phi = 180 deg (600 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 10199 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.15 _reflns_number_total 3994 _reflns_number_gt 3519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0536P)^2^+1.0806P] 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 3994 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Mn Mn 0.90408(4) 0.08266(2) 0.31897(2) 0.01714(11) Uani 1 1 d . . . S1 S 0.81690(7) 0.22972(3) 0.30949(3) 0.01917(13) Uani 1 1 d . . . S2 S 0.69067(7) 0.03883(4) 0.18090(4) 0.02245(14) Uani 1 1 d . . . B B 0.9056(3) 0.18602(16) 0.09241(16) 0.0180(5) Uani 1 1 d . . . H1 H 0.947(3) 0.2216(16) 0.0374(17) 0.022 Uiso 1 1 d . . . N1 N 1.0839(2) 0.11834(12) 0.25027(12) 0.0198(4) Uani 1 1 d . . . N2 N 1.0639(2) 0.17359(11) 0.17603(12) 0.0180(4) Uani 1 1 d . . . N3 N 0.5962(2) 0.31879(12) 0.17197(12) 0.0212(4) Uani 1 1 d . . . N4 N 0.7605(2) 0.23849(11) 0.11416(12) 0.0179(4) Uani 1 1 d . . . N5 N 0.7234(2) -0.02659(11) 0.01600(13) 0.0211(4) Uani 1 1 d . . . N6 N 0.8376(2) 0.09956(11) 0.04605(12) 0.0182(4) Uani 1 1 d . . . O1 O 1.0288(3) -0.09445(13) 0.32995(16) 0.0497(6) Uani 1 1 d . . . O2 O 1.1365(2) 0.12522(12) 0.50425(12) 0.0344(4) Uani 1 1 d . . . O3 O 0.6454(2) 0.03755(11) 0.41628(12) 0.0320(4) Uani 1 1 d . . . C1 C 1.2504(3) 0.11409(15) 0.29172(15) 0.0228(5) Uani 1 1 d . . . H1A H 1.3006 0.0798 0.3453 0.027 Uiso 1 1 calc R . . C2 C 1.3403(3) 0.16639(15) 0.24625(16) 0.0260(5) Uani 1 1 d . . . H2A H 1.4594 0.1750 0.2618 0.031 Uiso 1 1 calc R . . C3 C 1.2184(3) 0.20282(15) 0.17381(16) 0.0232(5) Uani 1 1 d . . . H3A H 1.2390 0.2423 0.1291 0.028 Uiso 1 1 calc R . . C4 C 0.7244(3) 0.26116(13) 0.19493(14) 0.0176(4) Uani 1 1 d . . . C5 C 0.5261(3) 0.36616(16) 0.23838(17) 0.0278(5) Uani 1 1 d . . . H5A H 0.5754 0.3448 0.3027 0.042 Uiso 1 1 calc R . . H5B H 0.4027 0.3587 0.2213 0.042 Uiso 1 1 calc R . . H5C H 0.5531 0.4268 0.2356 0.042 Uiso 1 1 calc R . . C6 C 0.5529(3) 0.33297(15) 0.07595(16) 0.0256(5) Uani 1 1 d . . . H6A H 0.4679 0.3708 0.0415 0.031 Uiso 1 1 calc R . . C7 C 0.6533(3) 0.28325(14) 0.04029(15) 0.0237(5) Uani 1 1 d . . . H7A H 0.6515 0.2793 -0.0246 0.028 Uiso 1 1 calc R . . C8 C 0.7591(3) 0.03694(14) 0.08064(14) 0.0190(4) Uani 1 1 d . . . C9 C 0.6485(3) -0.10876(16) 0.02792(18) 0.0302(5) Uani 1 1 d . . . H9A H 0.6236 -0.1104 0.0896 0.045 Uiso 1 1 calc R . . H9B H 0.7284 -0.1544 0.0247 0.045 Uiso 1 1 calc R . . H9C H 0.5433 -0.1166 -0.0225 0.045 Uiso 1 1 calc R . . C10 C 0.7771(3) -0.00261(15) -0.06214(15) 0.0242(5) Uani 1 1 d . . . H10A H 0.7660 -0.0347 -0.1184 0.029 Uiso 1 1 calc R . . C11 C 0.8482(3) 0.07510(14) -0.04286(15) 0.0217(5) Uani 1 1 d . . . H11A H 0.8972 0.1075 -0.0834 0.026 Uiso 1 1 calc R . . C12 C 0.9806(3) -0.02630(16) 0.32663(17) 0.0276(5) Uani 1 1 d . . . C13 C 1.0469(3) 0.10983(15) 0.43138(15) 0.0227(5) Uani 1 1 d . . . C14 C 0.7467(3) 0.05557(14) 0.37857(15) 0.0224(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.01744(18) 0.01620(18) 0.01831(17) 0.00172(11) 0.00574(13) 0.00162(12) S1 0.0225(3) 0.0168(3) 0.0175(2) -0.00010(18) 0.0043(2) 0.0030(2) S2 0.0214(3) 0.0257(3) 0.0217(3) -0.0034(2) 0.0085(2) -0.0069(2) B 0.0187(11) 0.0178(11) 0.0177(10) 0.0002(9) 0.0052(9) -0.0002(10) N1 0.0184(9) 0.0202(9) 0.0213(8) 0.0011(7) 0.0063(7) 0.0015(7) N2 0.0168(8) 0.0173(9) 0.0207(8) -0.0001(7) 0.0062(7) -0.0012(7) N3 0.0189(9) 0.0177(9) 0.0262(9) 0.0008(7) 0.0047(7) 0.0031(7) N4 0.0189(9) 0.0147(8) 0.0191(8) 0.0012(7) 0.0035(7) -0.0004(7) N5 0.0223(9) 0.0162(9) 0.0231(9) -0.0033(7) 0.0034(7) -0.0013(8) N6 0.0175(9) 0.0184(9) 0.0186(8) -0.0007(7) 0.0045(7) 0.0007(7) O1 0.0626(14) 0.0283(11) 0.0652(14) 0.0085(9) 0.0295(12) 0.0194(10) O2 0.0294(9) 0.0457(11) 0.0237(8) -0.0031(8) -0.0004(7) 0.0042(8) O3 0.0349(10) 0.0310(10) 0.0370(9) 0.0001(7) 0.0217(8) -0.0033(8) C1 0.0174(10) 0.0271(12) 0.0224(10) -0.0010(9) 0.0026(8) 0.0037(9) C2 0.0163(10) 0.0316(13) 0.0302(11) -0.0039(10) 0.0065(9) -0.0021(10) C3 0.0195(11) 0.0217(11) 0.0295(11) -0.0025(9) 0.0087(9) -0.0049(9) C4 0.0170(10) 0.0131(10) 0.0220(9) -0.0003(8) 0.0043(8) -0.0023(8) C5 0.0271(12) 0.0256(12) 0.0311(12) -0.0046(9) 0.0084(10) 0.0069(10) C6 0.0241(11) 0.0249(12) 0.0245(11) 0.0035(9) 0.0009(9) 0.0058(10) C7 0.0251(11) 0.0229(11) 0.0208(10) 0.0026(8) 0.0020(9) 0.0003(9) C8 0.0174(10) 0.0183(10) 0.0207(10) -0.0017(8) 0.0039(8) 0.0006(8) C9 0.0351(13) 0.0213(12) 0.0341(12) -0.0045(10) 0.0091(11) -0.0082(11) C10 0.0262(11) 0.0258(12) 0.0203(10) -0.0020(9) 0.0055(9) 0.0035(10) C11 0.0226(11) 0.0243(11) 0.0172(9) 0.0004(8) 0.0036(8) 0.0047(9) C12 0.0305(12) 0.0244(12) 0.0310(12) 0.0047(9) 0.0136(10) 0.0064(10) C13 0.0215(11) 0.0220(11) 0.0253(11) 0.0035(9) 0.0074(9) 0.0044(9) C14 0.0262(11) 0.0177(10) 0.0229(10) 0.0000(8) 0.0060(9) 0.0022(9) _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 Mn C14 1.792(2) . ? Mn C13 1.796(2) . ? Mn C12 1.814(2) . ? Mn N1 2.0725(18) . ? Mn S2 2.3906(9) . ? Mn S1 2.4085(7) . ? S1 C4 1.718(2) . ? S2 C8 1.709(2) . ? B N2 1.538(3) . ? B N4 1.548(3) . ? B N6 1.552(3) . ? N1 C1 1.336(3) . ? N1 N2 1.366(2) . ? N2 C3 1.354(3) . ? N3 C4 1.357(3) . ? N3 C6 1.374(3) . ? N3 C5 1.460(3) . ? N4 C4 1.344(3) . ? N4 C7 1.387(3) . ? N5 C8 1.352(3) . ? N5 C10 1.385(3) . ? N5 C9 1.458(3) . ? N6 C8 1.346(3) . ? N6 C11 1.384(3) . ? O1 C12 1.136(3) . ? O2 C13 1.147(3) . ? O3 C14 1.150(3) . ? C1 C2 1.387(3) . ? C2 C3 1.370(3) . ? C6 C7 1.338(3) . ? C10 C11 1.348(3) . ? 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 C14 Mn C13 89.15(10) . . ? C14 Mn C12 91.60(10) . . ? C13 Mn C12 92.20(11) . . ? C14 Mn N1 178.04(9) . . ? C13 Mn N1 90.54(9) . . ? C12 Mn N1 90.34(9) . . ? C14 Mn S2 83.51(8) . . ? C13 Mn S2 172.54(7) . . ? C12 Mn S2 86.71(8) . . ? N1 Mn S2 96.84(6) . . ? C14 Mn S1 90.83(7) . . ? C13 Mn S1 86.28(7) . . ? C12 Mn S1 177.11(8) . . ? N1 Mn S1 87.22(5) . . ? S2 Mn S1 95.12(2) . . ? C4 S1 Mn 112.17(7) . . ? C8 S2 Mn 113.51(8) . . ? N2 B N4 115.61(17) . . ? N2 B N6 111.35(18) . . ? N4 B N6 110.52(17) . . ? C1 N1 N2 106.37(17) . . ? C1 N1 Mn 122.48(14) . . ? N2 N1 Mn 127.64(14) . . ? C3 N2 N1 108.81(17) . . ? C3 N2 B 122.02(18) . . ? N1 N2 B 127.54(17) . . ? C4 N3 C6 109.31(18) . . ? C4 N3 C5 126.22(18) . . ? C6 N3 C5 124.15(19) . . ? C4 N4 C7 108.10(18) . . ? C4 N4 B 133.33(17) . . ? C7 N4 B 117.89(17) . . ? C8 N5 C10 108.80(18) . . ? C8 N5 C9 125.91(19) . . ? C10 N5 C9 125.22(19) . . ? C8 N6 C11 108.06(18) . . ? C8 N6 B 128.67(17) . . ? C11 N6 B 123.27(17) . . ? N1 C1 C2 111.1(2) . . ? C3 C2 C1 104.4(2) . . ? N2 C3 C2 109.3(2) . . ? N4 C4 N3 107.29(18) . . ? N4 C4 S1 129.92(16) . . ? N3 C4 S1 122.77(15) . . ? C7 C6 N3 106.85(19) . . ? C6 C7 N4 108.45(19) . . ? N6 C8 N5 108.03(18) . . ? N6 C8 S2 127.74(16) . . ? N5 C8 S2 123.82(16) . . ? C11 C10 N5 106.73(19) . . ? C10 C11 N6 108.36(19) . . ? O1 C12 Mn 178.9(2) . . ? O2 C13 Mn 178.1(2) . . ? O3 C14 Mn 179.4(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 C14 Mn S1 C4 -112.46(11) . . . . ? C13 Mn S1 C4 158.45(10) . . . . ? C12 Mn S1 C4 100.2(15) . . . . ? N1 Mn S1 C4 67.72(9) . . . . ? S2 Mn S1 C4 -28.91(8) . . . . ? C14 Mn S2 C8 -173.95(11) . . . . ? C13 Mn S2 C8 -163.7(6) . . . . ? C12 Mn S2 C8 -81.96(11) . . . . ? N1 Mn S2 C8 8.00(10) . . . . ? S1 Mn S2 C8 95.80(8) . . . . ? C14 Mn N1 C1 109(3) . . . . ? C13 Mn N1 C1 28.32(19) . . . . ? C12 Mn N1 C1 -63.88(19) . . . . ? S2 Mn N1 C1 -150.61(17) . . . . ? S1 Mn N1 C1 114.57(17) . . . . ? C14 Mn N1 N2 -47(3) . . . . ? C13 Mn N1 N2 -127.55(18) . . . . ? C12 Mn N1 N2 140.25(18) . . . . ? S2 Mn N1 N2 53.52(17) . . . . ? S1 Mn N1 N2 -41.30(17) . . . . ? C1 N1 N2 C3 -0.5(2) . . . . ? Mn N1 N2 C3 158.39(15) . . . . ? C1 N1 N2 B 164.93(19) . . . . ? Mn N1 N2 B -36.1(3) . . . . ? N4 B N2 C3 -118.9(2) . . . . ? N6 B N2 C3 113.9(2) . . . . ? N4 B N2 N1 77.4(3) . . . . ? N6 B N2 N1 -49.9(3) . . . . ? N2 B N4 C4 -17.1(3) . . . . ? N6 B N4 C4 110.5(2) . . . . ? N2 B N4 C7 152.10(19) . . . . ? N6 B N4 C7 -80.3(2) . . . . ? N2 B N6 C8 71.2(3) . . . . ? N4 B N6 C8 -58.8(3) . . . . ? N2 B N6 C11 -109.7(2) . . . . ? N4 B N6 C11 120.4(2) . . . . ? N2 N1 C1 C2 0.5(2) . . . . ? Mn N1 C1 C2 -159.77(15) . . . . ? N1 C1 C2 C3 -0.3(3) . . . . ? N1 N2 C3 C2 0.4(2) . . . . ? B N2 C3 C2 -166.05(19) . . . . ? C1 C2 C3 N2 -0.1(3) . . . . ? C7 N4 C4 N3 0.3(2) . . . . ? B N4 C4 N3 170.3(2) . . . . ? C7 N4 C4 S1 -178.21(17) . . . . ? B N4 C4 S1 -8.2(3) . . . . ? C6 N3 C4 N4 -0.6(2) . . . . ? C5 N3 C4 N4 -174.3(2) . . . . ? C6 N3 C4 S1 178.03(16) . . . . ? C5 N3 C4 S1 4.3(3) . . . . ? Mn S1 C4 N4 -35.6(2) . . . . ? Mn S1 C4 N3 146.04(16) . . . . ? C4 N3 C6 C7 0.7(3) . . . . ? C5 N3 C6 C7 174.6(2) . . . . ? N3 C6 C7 N4 -0.5(3) . . . . ? C4 N4 C7 C6 0.1(3) . . . . ? B N4 C7 C6 -171.66(19) . . . . ? C11 N6 C8 N5 1.1(2) . . . . ? B N6 C8 N5 -179.66(19) . . . . ? C11 N6 C8 S2 -171.62(17) . . . . ? B N6 C8 S2 7.6(3) . . . . ? C10 N5 C8 N6 -1.4(2) . . . . ? C9 N5 C8 N6 175.7(2) . . . . ? C10 N5 C8 S2 171.66(16) . . . . ? C9 N5 C8 S2 -11.2(3) . . . . ? Mn S2 C8 N6 -51.7(2) . . . . ? Mn S2 C8 N5 136.66(17) . . . . ? C8 N5 C10 C11 1.2(2) . . . . ? C9 N5 C10 C11 -176.0(2) . . . . ? N5 C10 C11 N6 -0.5(2) . . . . ? C8 N6 C11 C10 -0.4(2) . . . . ? B N6 C11 C10 -179.66(19) . . . . ? C14 Mn C12 O1 139(13) . . . . ? C13 Mn C12 O1 -132(13) . . . . ? N1 Mn C12 O1 -41(13) . . . . ? S2 Mn C12 O1 56(13) . . . . ? S1 Mn C12 O1 -74(14) . . . . ? C14 Mn C13 O2 40(6) . . . . ? C12 Mn C13 O2 -51(6) . . . . ? N1 Mn C13 O2 -142(6) . . . . ? S2 Mn C13 O2 30(7) . . . . ? S1 Mn C13 O2 131(6) . . . . ? C13 Mn C14 O3 -138(23) . . . . ? C12 Mn C14 O3 -46(23) . . . . ? N1 Mn C14 O3 141(22) . . . . ? S2 Mn C14 O3 40(23) . . . . ? S1 Mn C14 O3 136(23) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.565 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.076