# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. #============================================================================== # 0. AUDIT DETAILS _audit_creation_date ' 2003' _audit_creation_method SHELX-97 _audit_update_record ; ? ; _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry and Biochemistry Baylor University PO Box 97348 Waco TX, 76798-7348 USA ; _publ_contact_author_email 'Gordon Stone@baylor.edu' _publ_contact_author_fax '+1 254 710 2403' _publ_contact_author_phone '+1 254 710 4427' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; This CIF is submitted as supplementary data for the following Article, Ref. B304101H, in Chemical Communications: The seventeen- and eighteen-electron metallacarbaboranes [1,1,1-(CO)~3~-2-Ph-closo-1,2-MnCB~9~H~9~]^n-^ (n = 1, 2): a structurally characterized, redox-related pair PLEASE NOTE that the data herein should entirely replace that originally submitted. Date of (re-)submission: 6 June 2003 With thanks, Prof. F. G. A. Stone ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The seventeen- and eighteen-electron metallacarbaboranes [1,1,1-(CO)~3~-2-Ph-closo-1,2-MnCB~9~H~9~]^n-^ (n = 1, 2): a structurally characterized, redox-related pair ; loop_ _publ_author_name _publ_author_address S.Du ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; R.D.Farley ; EPSRC National ENDOR Service Cardiff University Cardiff CF10 3TB UK ; J.N.Harvey ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; J.C.Jeffrey ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; J.A.Kautz ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; J.P.Maher ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; ; T.D.McGrath ; ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; D.M.Murphy ; EPSRC National ENDOR Service Cardiff University Cardiff CF10 3TB UK ; T.Riis-Johannessen ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; F.G.A.Stone ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #============================================================================== _publ_section_exptl_refinement ; Diffracted intensities were collected on an Enraf-Nonius CAD-4 using graphite-monochromated Mo-K\a X-radiation. The final unit cell dimensions were determined from the setting angle values of 25 accurately centered reflections. The stability of the crystal during the period of the data collection was monitored by measuring the intensities of three standard reflections every two hours. Data were collected at a constant scan speed of 5.17\% min^-1^ in \w, with a scan range of 1.15 + 0.34tan\q. The data were corrected for Lorentz, polarization and X-ray absorption effects. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times U~iso~ value of the parent atom, except for methyl hydrogens where U~iso~ = 1.5 U~iso~. Data were processed by the SHELXTL program (Siemens, 1995). ; _publ_section_references ; Bruker (2001a). SAINT integration software. Bruker Analytical X-ray Instruments Inc., Madison, WI, 2001. Bruker (2001b). SHELXTL Version 5. Bruker Analytical X-ray Instruments Inc., Madison, WI, 2001. Bruker (2001c). SMART diffractometer control software. Bruker Analytical X-ray Instruments Inc., Madison, WI, 2001. Enraf-Nonius (1989). CAD-4 Software. Version 5. Enraf-Nonius, Delft, The Netherlands. Harms, K. (1993). XCAD4 A Program to extract intensities from a CAD-4 file. University of Marburg, Germany. Sheldrick, G.M. (1996). SADABS. Program for absorption correction with the Siemens SMART system. University of Gottingen, Germany. Sheldrick, G.M. (1997a). SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997b). SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Siemens (1995). SHELXTL-PC. Version 5.03. Bruker Analytical X-ray Instruments Inc. (1995), Madison, Wisconsin, USA. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== data_2a _database_code_CSD 208486 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H64 B9 Mn N2 O3 P2' _chemical_formula_weight 1003.24 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' P P 0.1023 0.0942 '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 13.4979(9) _cell_length_b 26.154(2) _cell_length_c 15.1792(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.521(7) _cell_angle_gamma 90.00 _cell_volume 5356.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.1 _cell_measurement_theta_max 15.6 _exptl_crystal_description prisms _exptl_crystal_colour orange _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.798 _exptl_absorpt_correction_T_max 0.817 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 8.67 _diffrn_reflns_number 8652 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.1361 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.16 _reflns_number_total 8303 _reflns_number_gt 4211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 (Enraf-Nonius, 1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'XP in SHELXTL-PC (Siemens, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _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 w=1/[\s^2^(Fo^2^)+(0.1203P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated positions, riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8303 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1815 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.2466 _refine_ls_wR_factor_gt 0.1884 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.02245(8) 0.20173(4) 0.17046(7) 0.0304(3) Uani 1 d . . . C1 C 0.0414(6) 0.1822(3) 0.3058(4) 0.039(2) Uani 1 d . . . B2 B 0.0841(7) 0.1314(3) 0.2603(6) 0.0428(18) Uani 1 d . . . H2 H 0.1632 0.1223 0.2697 0.051 Uiso 1 calc R . . B3 B 0.0249(7) 0.1118(3) 0.1544(6) 0.041(2) Uani 1 d . . . H3 H 0.0740 0.0918 0.1091 0.049 Uiso 1 calc R . . B4 B -0.0675(7) 0.1460(3) 0.1062(5) 0.039(2) Uani 1 d . . . H4 H -0.0850 0.1508 0.0355 0.047 Uiso 1 calc R . . B5 B -0.1345(6) 0.1655(3) 0.1927(5) 0.035(2) Uani 1 d . . . H5 H -0.2048 0.1852 0.1770 0.043 Uiso 1 calc R . . B6 B -0.0661(7) 0.1856(3) 0.3040(6) 0.0428(18) Uani 1 d . . . H6 H -0.0984 0.2157 0.3449 0.051 Uiso 1 calc R . . B7 B -0.0106(6) 0.1281(3) 0.3438(6) 0.035(2) Uani 1 d . . . H7 H -0.0061 0.1135 0.4117 0.042 Uiso 1 calc R . . B8 B -0.0097(6) 0.0851(3) 0.2565(5) 0.036(2) Uani 1 d . . . H8 H 0.0075 0.0449 0.2718 0.043 Uiso 1 calc R . . B9 B -0.1021(7) 0.0989(3) 0.1765(5) 0.038(2) Uani 1 d . . . H9 H -0.1494 0.0677 0.1513 0.045 Uiso 1 calc R . . B10 B -0.1199(6) 0.1220(3) 0.2837(5) 0.034(2) Uani 1 d . . . H10 H -0.1863 0.1095 0.3182 0.041 Uiso 1 calc R . . C2 C 0.0234(6) 0.2141(3) 0.0571(5) 0.047(2) Uani 1 d . . . O2 O 0.0268(5) 0.2265(3) -0.0175(4) 0.081(2) Uani 1 d . . . C3 C -0.0284(6) 0.2643(3) 0.1817(5) 0.041(2) Uani 1 d . . . O3 O -0.0658(4) 0.3042(2) 0.1826(4) 0.0636(17) Uani 1 d . . . C4 C 0.1509(6) 0.2185(3) 0.1757(5) 0.0355(19) Uani 1 d . . . O4 O 0.2353(4) 0.2275(2) 0.1770(4) 0.0640(18) Uani 1 d . . . C5 C 0.1050(5) 0.2145(3) 0.3670(5) 0.0352(19) Uani 1 d . . . C6 C 0.0824(6) 0.2659(3) 0.3800(5) 0.048(2) Uani 1 d . . . H6A H 0.0291 0.2807 0.3495 0.058 Uiso 1 calc R . . C7 C 0.1396(8) 0.2952(4) 0.4388(5) 0.064(3) Uani 1 d . . . H7A H 0.1227 0.3293 0.4475 0.077 Uiso 1 calc R . . C8 C 0.2217(8) 0.2752(5) 0.4853(6) 0.074(3) Uani 1 d . . . H8A H 0.2591 0.2953 0.5243 0.089 Uiso 1 calc R . . C9 C 0.2449(8) 0.2255(5) 0.4714(6) 0.081(3) Uani 1 d . . . H9A H 0.3003 0.2114 0.4998 0.097 Uiso 1 calc R . . C10 C 0.1851(6) 0.1946(4) 0.4137(5) 0.059(2) Uani 1 d . . . H10A H 0.2004 0.1601 0.4075 0.071 Uiso 1 calc R . . N1 N -0.4921(4) 0.3227(2) 0.2297(4) 0.0435(17) Uani 1 d . . . C21 C -0.4682(7) 0.3765(4) 0.2601(6) 0.068(3) Uani 1 d . . . H21A H -0.4131 0.3894 0.2269 0.082 Uiso 1 calc R . . H21B H -0.5249 0.3983 0.2475 0.082 Uiso 1 calc R . . C22 C -0.4418(8) 0.3797(4) 0.3575(7) 0.086(3) Uani 1 d . . . H22A H -0.4276 0.4146 0.3731 0.129 Uiso 1 calc R . . H22B H -0.3847 0.3589 0.3703 0.129 Uiso 1 calc R . . H22C H -0.4966 0.3677 0.3909 0.129 Uiso 1 calc R . . C23 C -0.5811(6) 0.3015(3) 0.2765(6) 0.052(2) Uani 1 d . . . H23A H -0.5965 0.2681 0.2520 0.062 Uiso 1 calc R . . H23B H -0.5626 0.2966 0.3382 0.062 Uiso 1 calc R . . C24 C -0.6724(7) 0.3331(4) 0.2716(7) 0.080(3) Uani 1 d . . . H24A H -0.7237 0.3166 0.3037 0.120 Uiso 1 calc R . . H24B H -0.6936 0.3370 0.2111 0.120 Uiso 1 calc R . . H24C H -0.6589 0.3661 0.2968 0.120 Uiso 1 calc R . . C25 C -0.5135(8) 0.3276(4) 0.1306(6) 0.070(3) Uani 1 d . . . H25A H -0.5672 0.3519 0.1218 0.084 Uiso 1 calc R . . H25B H -0.4553 0.3420 0.1038 0.084 Uiso 1 calc R . . C26 C -0.5410(8) 0.2784(4) 0.0819(6) 0.084(3) Uani 1 d . . . H26A H -0.5527 0.2857 0.0206 0.126 Uiso 1 calc R . . H26B H -0.5998 0.2641 0.1063 0.126 Uiso 1 calc R . . H26C H -0.4876 0.2543 0.0883 0.126 Uiso 1 calc R . . C27 C -0.4082(6) 0.2873(4) 0.2465(7) 0.069(3) Uani 1 d . . . H27A H -0.4265 0.2542 0.2220 0.083 Uiso 1 calc R . . H27B H -0.4004 0.2830 0.3097 0.083 Uiso 1 calc R . . C28 C -0.3084(7) 0.3017(5) 0.2112(8) 0.112(5) Uani 1 d . . . H28A H -0.2610 0.2755 0.2263 0.167 Uiso 1 calc R . . H28B H -0.2872 0.3336 0.2366 0.167 Uiso 1 calc R . . H28C H -0.3136 0.3050 0.1483 0.167 Uiso 1 calc R . . N2 N 1.0068(4) 0.4401(2) 0.2497(3) 0.0286(14) Uani 1 d . . . P1 P 0.90351(13) 0.46239(7) 0.27867(11) 0.0262(5) Uani 1 d . . . C31 C 0.8570(5) 0.4242(3) 0.3673(4) 0.0284(17) Uani 1 d . . . C32 C 0.7971(6) 0.4459(3) 0.4307(5) 0.044(2) Uani 1 d . . . H32A H 0.7819 0.4806 0.4291 0.053 Uiso 1 calc R . . C33 C 0.7607(7) 0.4147(4) 0.4962(5) 0.056(2) Uani 1 d . . . H33A H 0.7216 0.4288 0.5395 0.067 Uiso 1 calc R . . C34 C 0.7812(7) 0.3636(4) 0.4983(6) 0.058(3) Uani 1 d . . . H34A H 0.7554 0.3432 0.5422 0.069 Uiso 1 calc R . . C35 C 0.8397(6) 0.3424(3) 0.4358(5) 0.051(2) Uani 1 d . . . H35A H 0.8529 0.3075 0.4372 0.061 Uiso 1 calc R . . C36 C 0.8792(5) 0.3725(3) 0.3705(5) 0.0394(19) Uani 1 d . . . H36A H 0.9204 0.3582 0.3291 0.047 Uiso 1 calc R . . C41 C 0.8124(5) 0.4570(3) 0.1897(4) 0.0275(16) Uani 1 d . . . C42 C 0.7186(5) 0.4799(3) 0.1957(5) 0.0361(18) Uani 1 d . . . H42A H 0.7033 0.4990 0.2452 0.043 Uiso 1 calc R . . C43 C 0.6490(6) 0.4739(3) 0.1278(5) 0.045(2) Uani 1 d . . . H43A H 0.5870 0.4892 0.1310 0.054 Uiso 1 calc R . . C44 C 0.6729(7) 0.4449(3) 0.0551(6) 0.052(2) Uani 1 d . . . H44A H 0.6263 0.4405 0.0095 0.063 Uiso 1 calc R . . C45 C 0.7639(6) 0.4228(3) 0.0495(5) 0.049(2) Uani 1 d . . . H45A H 0.7790 0.4035 0.0002 0.059 Uiso 1 calc R . . C46 C 0.8331(6) 0.4288(3) 0.1160(5) 0.0378(19) Uani 1 d . . . H46A H 0.8950 0.4136 0.1114 0.045 Uiso 1 calc R . . C51 C 0.9110(5) 0.5272(3) 0.3164(4) 0.0260(16) Uani 1 d . . . C52 C 0.8705(5) 0.5679(3) 0.2693(5) 0.0371(19) Uani 1 d . . . H52A H 0.8334 0.5620 0.2177 0.045 Uiso 1 calc R . . C53 C 0.8854(6) 0.6173(3) 0.2994(6) 0.046(2) Uani 1 d . . . H53A H 0.8583 0.6447 0.2680 0.055 Uiso 1 calc R . . C54 C 0.9397(6) 0.6261(3) 0.3749(6) 0.051(2) Uani 1 d . . . H54A H 0.9486 0.6593 0.3955 0.061 Uiso 1 calc R . . C55 C 0.9818(6) 0.5854(3) 0.4212(5) 0.048(2) Uani 1 d . . . H55A H 1.0202 0.5914 0.4719 0.058 Uiso 1 calc R . . C56 C 0.9666(5) 0.5367(3) 0.3924(5) 0.0356(18) Uani 1 d . . . H56A H 0.9940 0.5095 0.4241 0.043 Uiso 1 calc R . . P2 P 1.10772(13) 0.46472(7) 0.22108(11) 0.0256(4) Uani 1 d . . . C61 C 1.1555(5) 0.4274(3) 0.1332(4) 0.0278(16) Uani 1 d . . . C62 C 1.1287(5) 0.3764(3) 0.1241(5) 0.0339(18) Uani 1 d . . . H62A H 1.0833 0.3627 0.1627 0.041 Uiso 1 calc R . . C63 C 1.1667(6) 0.3452(3) 0.0600(5) 0.043(2) Uani 1 d . . . H63A H 1.1475 0.3111 0.0552 0.051 Uiso 1 calc R . . C64 C 1.2334(6) 0.3657(3) 0.0035(5) 0.050(2) Uani 1 d . . . H64A H 1.2586 0.3454 -0.0410 0.060 Uiso 1 calc R . . C65 C 1.2636(6) 0.4154(3) 0.0113(5) 0.054(2) Uani 1 d . . . H65A H 1.3110 0.4283 -0.0260 0.065 Uiso 1 calc R . . C66 C 1.2233(6) 0.4464(3) 0.0750(5) 0.044(2) Uani 1 d . . . H66A H 1.2422 0.4806 0.0786 0.052 Uiso 1 calc R . . C71 C 1.0950(5) 0.5294(3) 0.1808(4) 0.0300(17) Uani 1 d . . . C72 C 1.0343(5) 0.5365(3) 0.1070(4) 0.0394(19) Uani 1 d . . . H72A H 1.0077 0.5082 0.0780 0.047 Uiso 1 calc R . . C73 C 1.0124(6) 0.5843(3) 0.0755(5) 0.050(2) Uani 1 d . . . H73A H 0.9710 0.5883 0.0261 0.060 Uiso 1 calc R . . C74 C 1.0526(6) 0.6267(4) 0.1180(6) 0.052(2) Uani 1 d . . . H74A H 1.0385 0.6593 0.0971 0.063 Uiso 1 calc R . . C75 C 1.1132(6) 0.6202(3) 0.1910(6) 0.049(2) Uani 1 d . . . H75A H 1.1405 0.6486 0.2193 0.059 Uiso 1 calc R . . C76 C 1.1341(5) 0.5716(3) 0.2232(5) 0.0359(18) Uani 1 d . . . H76A H 1.1744 0.5676 0.2733 0.043 Uiso 1 calc R . . C81 C 1.2003(5) 0.4633(3) 0.3088(4) 0.0284(16) Uani 1 d . . . C82 C 1.2939(5) 0.4836(3) 0.2980(5) 0.0353(18) Uani 1 d . . . H82A H 1.3089 0.5003 0.2459 0.042 Uiso 1 calc R . . C83 C 1.3651(5) 0.4790(3) 0.3647(5) 0.0394(19) Uani 1 d . . . H83A H 1.4276 0.4930 0.3577 0.047 Uiso 1 calc R . . C84 C 1.3439(6) 0.4536(3) 0.4415(5) 0.0398(19) Uani 1 d . . . H84A H 1.3923 0.4504 0.4859 0.048 Uiso 1 calc R . . C85 C 1.2516(6) 0.4332(3) 0.4526(5) 0.0387(19) Uani 1 d . . . H85A H 1.2373 0.4161 0.5045 0.046 Uiso 1 calc R . . C86 C 1.1801(6) 0.4379(3) 0.3867(5) 0.0341(18) Uani 1 d . . . H86A H 1.1175 0.4240 0.3945 0.041 Uiso 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 0.0361(7) 0.0294(6) 0.0260(6) -0.0024(5) 0.0053(5) -0.0046(5) C1 0.055(5) 0.042(5) 0.018(4) 0.000(3) -0.012(4) -0.021(4) B2 0.056(4) 0.032(4) 0.042(4) 0.007(3) 0.025(3) 0.027(3) B3 0.051(6) 0.036(5) 0.037(5) -0.009(4) 0.019(5) -0.012(5) B4 0.052(6) 0.042(6) 0.023(5) -0.010(4) 0.003(4) -0.018(5) B5 0.028(5) 0.044(6) 0.035(5) -0.001(4) 0.001(4) -0.002(4) B6 0.056(4) 0.032(4) 0.042(4) 0.007(3) 0.025(3) 0.027(3) B7 0.034(5) 0.042(5) 0.029(5) 0.006(4) 0.003(4) 0.004(4) B8 0.047(6) 0.026(5) 0.036(5) 0.007(4) 0.005(4) -0.001(4) B9 0.050(6) 0.031(5) 0.032(5) -0.001(4) 0.013(4) -0.015(4) B10 0.031(5) 0.044(5) 0.026(5) -0.004(4) 0.009(4) 0.002(4) C2 0.065(6) 0.044(5) 0.032(5) -0.002(4) 0.003(4) -0.019(4) O2 0.132(6) 0.081(5) 0.029(3) 0.008(3) 0.002(4) -0.043(4) C3 0.039(5) 0.036(5) 0.049(5) 0.000(4) 0.014(4) -0.002(4) O3 0.068(4) 0.037(4) 0.086(5) 0.007(3) 0.009(4) 0.009(3) C4 0.044(5) 0.027(4) 0.036(4) 0.001(3) 0.006(4) -0.001(4) O4 0.036(4) 0.067(4) 0.089(5) -0.003(4) 0.009(3) -0.020(3) C5 0.039(5) 0.035(5) 0.032(4) -0.004(3) 0.009(4) -0.002(4) C6 0.063(6) 0.046(5) 0.035(5) -0.005(4) 0.001(4) -0.010(4) C7 0.109(9) 0.044(5) 0.039(5) -0.009(5) -0.001(6) -0.022(6) C8 0.071(8) 0.109(10) 0.041(6) -0.024(6) 0.001(5) -0.042(7) C9 0.071(7) 0.121(10) 0.050(6) -0.005(7) -0.024(5) -0.014(7) C10 0.062(6) 0.062(6) 0.052(5) -0.003(5) -0.019(5) 0.011(5) N1 0.035(4) 0.043(4) 0.052(4) 0.003(3) -0.001(3) -0.004(3) C21 0.078(7) 0.052(6) 0.075(7) -0.011(5) 0.016(6) -0.019(5) C22 0.087(8) 0.086(8) 0.083(8) -0.030(7) -0.026(6) 0.007(7) C23 0.048(5) 0.050(5) 0.058(5) 0.008(5) 0.007(4) -0.003(5) C24 0.054(6) 0.106(9) 0.081(7) -0.020(7) 0.015(6) -0.005(6) C25 0.088(8) 0.080(8) 0.044(5) 0.012(5) 0.009(5) -0.011(6) C26 0.092(8) 0.093(9) 0.067(7) -0.034(6) 0.006(6) -0.012(7) C27 0.043(6) 0.082(8) 0.081(7) -0.017(6) 0.004(5) 0.011(5) C28 0.056(7) 0.155(13) 0.124(11) -0.054(9) 0.004(7) 0.006(8) N2 0.027(3) 0.028(3) 0.032(3) -0.003(3) 0.009(3) -0.001(3) P1 0.0267(10) 0.0312(11) 0.0207(9) -0.0012(8) 0.0020(8) -0.0006(8) C31 0.021(4) 0.035(4) 0.030(4) 0.000(3) 0.000(3) -0.004(3) C32 0.040(5) 0.057(6) 0.035(4) -0.001(4) 0.012(4) 0.003(4) C33 0.061(6) 0.071(7) 0.037(5) -0.005(5) 0.014(4) -0.018(5) C34 0.062(6) 0.068(7) 0.044(5) 0.013(5) 0.013(5) -0.021(5) C35 0.062(6) 0.044(5) 0.047(5) 0.002(4) 0.005(5) -0.004(4) C36 0.041(5) 0.046(5) 0.032(4) -0.004(4) 0.007(4) 0.004(4) C41 0.028(4) 0.030(4) 0.024(4) 0.001(3) 0.001(3) -0.002(3) C42 0.042(5) 0.034(4) 0.033(4) -0.003(3) 0.001(4) -0.002(4) C43 0.027(4) 0.048(5) 0.060(6) -0.002(4) -0.009(4) -0.004(4) C44 0.054(6) 0.052(6) 0.050(6) -0.001(4) -0.020(5) -0.012(5) C45 0.059(6) 0.052(6) 0.035(5) -0.017(4) -0.008(4) -0.002(5) C46 0.036(4) 0.047(5) 0.031(4) -0.009(4) 0.000(4) 0.003(4) C51 0.029(4) 0.027(4) 0.022(4) -0.001(3) 0.003(3) -0.009(3) C52 0.036(4) 0.027(4) 0.048(5) -0.010(4) -0.002(4) 0.001(3) C53 0.041(5) 0.039(5) 0.058(6) -0.005(4) 0.009(4) 0.001(4) C54 0.054(6) 0.028(5) 0.072(6) -0.022(5) 0.021(5) -0.008(4) C55 0.058(6) 0.055(6) 0.032(5) -0.012(4) 0.006(4) -0.020(5) C56 0.042(5) 0.034(5) 0.031(4) -0.005(4) -0.002(4) 0.000(4) P2 0.0258(10) 0.0299(10) 0.0213(9) 0.0027(8) 0.0037(8) 0.0017(8) C61 0.034(4) 0.028(4) 0.022(4) 0.000(3) 0.003(3) 0.004(3) C62 0.037(4) 0.034(5) 0.031(4) 0.008(3) 0.007(3) 0.003(4) C63 0.062(6) 0.025(4) 0.041(5) -0.005(4) -0.004(4) 0.002(4) C64 0.062(6) 0.052(6) 0.036(5) 0.003(4) 0.008(4) 0.019(5) C65 0.062(6) 0.055(6) 0.048(5) -0.001(4) 0.031(5) -0.003(5) C66 0.053(5) 0.037(5) 0.042(5) -0.001(4) 0.025(4) 0.003(4) C71 0.028(4) 0.031(4) 0.032(4) 0.001(3) 0.006(3) 0.004(3) C72 0.044(5) 0.050(5) 0.024(4) -0.001(4) -0.005(4) 0.008(4) C73 0.055(6) 0.061(6) 0.034(5) 0.022(4) -0.010(4) 0.022(5) C74 0.049(5) 0.053(6) 0.056(6) 0.016(5) 0.011(5) 0.015(5) C75 0.054(6) 0.034(5) 0.061(6) 0.003(4) 0.004(5) 0.007(4) C76 0.027(4) 0.043(5) 0.037(4) 0.005(4) -0.002(3) 0.000(4) C81 0.027(4) 0.037(4) 0.022(4) 0.004(3) -0.005(3) 0.005(3) C82 0.039(5) 0.029(4) 0.038(4) 0.015(3) 0.002(4) 0.003(4) C83 0.032(4) 0.035(5) 0.050(5) -0.001(4) -0.018(4) 0.000(4) C84 0.046(5) 0.041(5) 0.032(4) 0.006(4) -0.013(4) 0.008(4) C85 0.048(5) 0.041(5) 0.027(4) 0.006(4) 0.004(4) 0.006(4) C86 0.041(5) 0.033(4) 0.029(4) 0.004(3) 0.008(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles: correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn C2 1.751(8) . ? Mn C3 1.784(8) . ? Mn C4 1.788(8) . ? Mn B4 2.118(8) . ? Mn C1 2.125(7) . ? Mn B5 2.354(8) . ? Mn B3 2.365(9) . ? Mn B6 2.417(8) . ? Mn B2 2.424(9) . ? C1 B6 1.453(11) . ? C1 C5 1.506(10) . ? C1 B2 1.612(11) . ? C1 B7 1.688(11) . ? B2 B8 1.752(13) . ? B2 B7 1.825(11) . ? B2 B3 1.849(13) . ? B3 B4 1.686(13) . ? B3 B8 1.775(11) . ? B3 B9 1.788(12) . ? B4 B5 1.693(11) . ? B4 B9 1.703(11) . ? B5 B10 1.796(12) . ? B5 B9 1.814(12) . ? B5 B6 1.974(13) . ? B6 B7 1.779(11) . ? B6 B10 1.837(13) . ? B7 B10 1.721(12) . ? B7 B8 1.738(12) . ? B8 B9 1.756(13) . ? B8 B10 1.830(11) . ? B9 B10 1.758(11) . ? C2 O2 1.181(9) . ? C3 O3 1.161(9) . ? C4 O4 1.163(8) . ? C5 C10 1.379(10) . ? C5 C6 1.394(10) . ? C6 C7 1.394(11) . ? C7 C8 1.399(13) . ? C8 C9 1.355(15) . ? C9 C10 1.426(13) . ? N1 C27 1.480(10) . ? N1 C21 1.514(10) . ? N1 C23 1.517(9) . ? N1 C25 1.529(10) . ? C21 C22 1.513(12) . ? C23 C24 1.485(12) . ? C25 C26 1.527(12) . ? C27 C28 1.510(13) . ? N2 P2 1.578(5) . ? N2 P1 1.584(5) . ? P1 C51 1.791(7) . ? P1 C31 1.801(7) . ? P1 C41 1.808(7) . ? C31 C36 1.386(10) . ? C31 C32 1.393(9) . ? C32 C33 1.386(10) . ? C33 C34 1.364(12) . ? C34 C35 1.367(11) . ? C35 C36 1.384(10) . ? C41 C46 1.375(9) . ? C41 C42 1.405(9) . ? C42 C43 1.385(10) . ? C43 C44 1.384(11) . ? C44 C45 1.363(11) . ? C45 C46 1.366(10) . ? C51 C56 1.381(9) . ? C51 C52 1.386(9) . ? C52 C53 1.385(10) . ? C53 C54 1.364(11) . ? C54 C55 1.389(11) . ? C55 C56 1.360(10) . ? P2 C61 1.787(7) . ? P2 C81 1.803(7) . ? P2 C71 1.804(7) . ? C61 C66 1.382(9) . ? C61 C62 1.390(9) . ? C62 C63 1.380(9) . ? C63 C64 1.368(10) . ? C64 C65 1.367(11) . ? C65 C66 1.384(10) . ? C71 C76 1.376(10) . ? C71 C72 1.384(9) . ? C72 C73 1.367(10) . ? C73 C74 1.385(12) . ? C74 C75 1.370(11) . ? C75 C76 1.388(10) . ? C81 C82 1.385(9) . ? C81 C86 1.389(9) . ? C82 C83 1.382(9) . ? C83 C84 1.378(10) . ? C84 C85 1.370(10) . ? C85 C86 1.377(10) . ? 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 C2 Mn C3 86.4(4) . . ? C2 Mn C4 88.0(4) . . ? C3 Mn C4 98.4(3) . . ? C2 Mn B4 72.1(3) . . ? C3 Mn B4 117.2(4) . . ? C4 Mn B4 137.1(3) . . ? C2 Mn C1 171.9(4) . . ? C3 Mn C1 99.4(3) . . ? C4 Mn C1 85.7(3) . . ? B4 Mn C1 109.4(3) . . ? C2 Mn B5 104.2(3) . . ? C3 Mn B5 90.3(3) . . ? C4 Mn B5 165.5(3) . . ? B4 Mn B5 44.1(3) . . ? C1 Mn B5 81.4(3) . . ? C2 Mn B3 94.7(3) . . ? C3 Mn B3 158.2(3) . . ? C4 Mn B3 103.5(3) . . ? B4 Mn B3 43.7(3) . . ? C1 Mn B3 81.9(3) . . ? B5 Mn B3 68.3(3) . . ? C2 Mn B6 150.8(4) . . ? C3 Mn B6 83.1(3) . . ? C4 Mn B6 120.4(3) . . ? B4 Mn B6 88.6(3) . . ? C1 Mn B6 36.6(3) . . ? B5 Mn B6 48.9(3) . . ? B3 Mn B6 85.5(3) . . ? C2 Mn B2 132.9(3) . . ? C3 Mn B2 140.3(3) . . ? C4 Mn B2 81.0(3) . . ? B4 Mn B2 85.5(4) . . ? C1 Mn B2 40.9(3) . . ? B5 Mn B2 84.9(3) . . ? B3 Mn B2 45.4(3) . . ? B6 Mn B2 64.3(3) . . ? B6 C1 C5 122.0(7) . . ? B6 C1 B2 114.2(7) . . ? C5 C1 B2 121.5(7) . . ? B6 C1 B7 68.5(5) . . ? C5 C1 B7 119.6(6) . . ? B2 C1 B7 67.1(5) . . ? B6 C1 Mn 82.7(5) . . ? C5 C1 Mn 120.9(5) . . ? B2 C1 Mn 79.6(4) . . ? B7 C1 Mn 119.4(5) . . ? C1 B2 B8 108.6(6) . . ? C1 B2 B7 58.4(4) . . ? B8 B2 B7 58.1(5) . . ? C1 B2 B3 116.7(6) . . ? B8 B2 B3 59.0(5) . . ? B7 B2 B3 107.2(6) . . ? C1 B2 Mn 59.6(4) . . ? B8 B2 Mn 105.6(5) . . ? B7 B2 Mn 100.9(4) . . ? B3 B2 Mn 65.6(4) . . ? B4 B3 B8 112.3(6) . . ? B4 B3 B9 58.6(5) . . ? B8 B3 B9 59.1(5) . . ? B4 B3 B2 121.9(6) . . ? B8 B3 B2 57.8(5) . . ? B9 B3 B2 106.5(6) . . ? B4 B3 Mn 60.3(4) . . ? B8 B3 Mn 107.3(5) . . ? B9 B3 Mn 98.8(5) . . ? B2 B3 Mn 69.0(4) . . ? B3 B4 B5 103.2(6) . . ? B3 B4 B9 63.7(5) . . ? B5 B4 B9 64.6(5) . . ? B3 B4 Mn 75.9(5) . . ? B5 B4 Mn 75.4(4) . . ? B9 B4 Mn 111.9(5) . . ? B4 B5 B10 110.8(6) . . ? B4 B5 B9 58.0(5) . . ? B10 B5 B9 58.3(5) . . ? B4 B5 B6 119.7(6) . . ? B10 B5 B6 58.1(4) . . ? B9 B5 B6 105.2(6) . . ? B4 B5 Mn 60.5(4) . . ? B10 B5 Mn 106.5(5) . . ? B9 B5 Mn 98.4(4) . . ? B6 B5 Mn 67.2(4) . . ? C1 B6 B7 62.0(5) . . ? C1 B6 B10 109.8(6) . . ? B7 B6 B10 56.8(5) . . ? C1 B6 B5 116.4(6) . . ? B7 B6 B5 104.4(6) . . ? B10 B6 B5 56.1(5) . . ? C1 B6 Mn 60.7(4) . . ? B7 B6 Mn 102.6(4) . . ? B10 B6 Mn 102.7(5) . . ? B5 B6 Mn 63.9(3) . . ? C1 B7 B10 104.8(6) . . ? C1 B7 B8 105.8(6) . . ? B10 B7 B8 63.9(5) . . ? C1 B7 B6 49.5(5) . . ? B10 B7 B6 63.3(5) . . ? B8 B7 B6 107.5(6) . . ? C1 B7 B2 54.5(4) . . ? B10 B7 B2 104.1(6) . . ? B8 B7 B2 58.8(5) . . ? B6 B7 B2 91.2(5) . . ? B7 B8 B2 63.1(5) . . ? B7 B8 B9 112.0(6) . . ? B2 B8 B9 112.3(6) . . ? B7 B8 B3 114.7(6) . . ? B2 B8 B3 63.2(5) . . ? B9 B8 B3 60.8(5) . . ? B7 B8 B10 57.6(5) . . ? B2 B8 B10 102.6(6) . . ? B9 B8 B10 58.7(5) . . ? B3 B8 B10 102.9(6) . . ? B4 B9 B8 112.4(6) . . ? B4 B9 B10 112.2(6) . . ? B8 B9 B10 62.8(5) . . ? B4 B9 B3 57.7(5) . . ? B8 B9 B3 60.1(5) . . ? B10 B9 B3 105.3(6) . . ? B4 B9 B5 57.5(5) . . ? B8 B9 B5 105.9(6) . . ? B10 B9 B5 60.3(5) . . ? B3 B9 B5 94.6(6) . . ? B7 B10 B9 112.7(6) . . ? B7 B10 B5 115.1(6) . . ? B9 B10 B5 61.4(5) . . ? B7 B10 B8 58.5(5) . . ? B9 B10 B8 58.6(5) . . ? B5 B10 B8 103.6(5) . . ? B7 B10 B6 59.9(5) . . ? B9 B10 B6 113.8(6) . . ? B5 B10 B6 65.8(5) . . ? B8 B10 B6 101.3(6) . . ? O2 C2 Mn 174.3(7) . . ? O3 C3 Mn 174.4(8) . . ? O4 C4 Mn 177.0(7) . . ? C10 C5 C6 117.5(8) . . ? C10 C5 C1 122.1(7) . . ? C6 C5 C1 120.3(7) . . ? C7 C6 C5 120.1(9) . . ? C6 C7 C8 122.4(9) . . ? C9 C8 C7 117.6(9) . . ? C8 C9 C10 120.6(10) . . ? C5 C10 C9 121.7(9) . . ? C27 N1 C21 111.9(7) . . ? C27 N1 C23 107.6(6) . . ? C21 N1 C23 111.2(6) . . ? C27 N1 C25 110.3(7) . . ? C21 N1 C25 104.8(6) . . ? C23 N1 C25 111.2(6) . . ? C22 C21 N1 113.1(8) . . ? C24 C23 N1 116.0(7) . . ? C26 C25 N1 116.2(8) . . ? N1 C27 C28 118.0(9) . . ? P2 N2 P1 134.3(4) . . ? N2 P1 C51 113.2(3) . . ? N2 P1 C31 109.3(3) . . ? C51 P1 C31 107.7(3) . . ? N2 P1 C41 110.5(3) . . ? C51 P1 C41 110.1(3) . . ? C31 P1 C41 105.7(3) . . ? C36 C31 C32 120.1(7) . . ? C36 C31 P1 119.2(5) . . ? C32 C31 P1 120.7(6) . . ? C33 C32 C31 118.7(8) . . ? C34 C33 C32 121.1(8) . . ? C33 C34 C35 120.1(8) . . ? C34 C35 C36 120.4(8) . . ? C35 C36 C31 119.5(7) . . ? C46 C41 C42 118.9(7) . . ? C46 C41 P1 120.0(5) . . ? C42 C41 P1 121.0(5) . . ? C43 C42 C41 119.9(7) . . ? C44 C43 C42 119.1(7) . . ? C45 C44 C43 120.8(8) . . ? C44 C45 C46 120.3(8) . . ? C45 C46 C41 120.9(7) . . ? C56 C51 C52 119.4(7) . . ? C56 C51 P1 117.5(5) . . ? C52 C51 P1 122.9(5) . . ? C53 C52 C51 119.6(7) . . ? C54 C53 C52 120.3(8) . . ? C53 C54 C55 120.0(8) . . ? C56 C55 C54 119.9(8) . . ? C55 C56 C51 120.7(7) . . ? N2 P2 C61 108.3(3) . . ? N2 P2 C81 112.0(3) . . ? C61 P2 C81 106.4(3) . . ? N2 P2 C71 113.6(3) . . ? C61 P2 C71 107.0(3) . . ? C81 P2 C71 109.2(3) . . ? C66 C61 C62 117.2(6) . . ? C66 C61 P2 122.7(6) . . ? C62 C61 P2 120.0(5) . . ? C63 C62 C61 122.5(7) . . ? C64 C63 C62 118.3(7) . . ? C65 C64 C63 121.2(7) . . ? C64 C65 C66 119.8(7) . . ? C61 C66 C65 121.0(7) . . ? C76 C71 C72 118.8(7) . . ? C76 C71 P2 124.2(6) . . ? C72 C71 P2 116.8(6) . . ? C73 C72 C71 121.6(8) . . ? C72 C73 C74 119.4(8) . . ? C75 C74 C73 119.7(8) . . ? C74 C75 C76 120.6(8) . . ? C71 C76 C75 119.9(7) . . ? C82 C81 C86 119.0(6) . . ? C82 C81 P2 121.4(5) . . ? C86 C81 P2 119.4(5) . . ? C83 C82 C81 119.8(7) . . ? C84 C83 C82 120.4(7) . . ? C85 C84 C83 120.1(7) . . ? C84 C85 C86 119.9(7) . . ? C85 C86 C81 120.7(7) . . ? _diffrn_measured_fraction_theta_max 0.845 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.845 _refine_diff_density_max 1.633 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.095 #============================================================================== data_3 _database_code_CSD 208487 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H44 B9 Mn N O3 P2' _chemical_formula_weight 872.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' _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 10.89980(10) _cell_length_b 13.90490(10) _cell_length_c 15.7182(2) _cell_angle_alpha 85.1960(10) _cell_angle_beta 70.3330(10) _cell_angle_gamma 79.9260(10) _cell_volume 2207.91(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11234 _cell_measurement_theta_min 6.458 _cell_measurement_theta_max 140.042 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 3.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.286 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'Bruker Proteum CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17517 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 70.22 _reflns_number_total 7517 _reflns_number_gt 6672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001c)' _computing_cell_refinement 'SAINT (Bruker, 2001a)' _computing_data_reduction 'SAINT (Bruker, 2001a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001b)' _computing_publication_material 'SHELXTL (Bruker, 2001b)' _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^)+(0.0737P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7517 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 0.25642(3) 1.03118(2) 0.329904(19) 0.01986(9) Uani 1 1 d . . . C2 C 0.1206(2) 1.12019(15) 0.39397(13) 0.0279(4) Uani 1 1 d . . . O2 O 0.04437(15) 1.18259(11) 0.43313(10) 0.0380(4) Uani 1 1 d . . . C3 C 0.3491(2) 1.13355(15) 0.31216(13) 0.0295(5) Uani 1 1 d . . . O3 O 0.40309(18) 1.19898(11) 0.30392(11) 0.0464(4) Uani 1 1 d . . . C4 C 0.29967(19) 0.97836(13) 0.43057(13) 0.0242(4) Uani 1 1 d . . . O4 O 0.32449(16) 0.94568(11) 0.49261(10) 0.0349(3) Uani 1 1 d . . . C1 C 0.41120(18) 0.97498(13) 0.22101(12) 0.0201(4) Uani 1 1 d . . . C11 C 0.54794(18) 0.99354(13) 0.20505(12) 0.0211(4) Uani 1 1 d . . . C12 C 0.60896(19) 0.96500(15) 0.27063(13) 0.0275(4) Uani 1 1 d . . . H12 H 0.5649 0.9321 0.3230 0.033 Uiso 1 1 calc R . . C13 C 0.7336(2) 0.98491(16) 0.25871(15) 0.0325(5) Uani 1 1 d . . . H13 H 0.7724 0.9659 0.3032 0.039 Uiso 1 1 calc R . . C14 C 0.8009(2) 1.03297(16) 0.18101(15) 0.0322(5) Uani 1 1 d . . . H14 H 0.8846 1.0467 0.1730 0.039 Uiso 1 1 calc R . . C15 C 0.7426(2) 1.06048(15) 0.11523(14) 0.0294(4) Uani 1 1 d . . . H15 H 0.7878 1.0924 0.0626 0.035 Uiso 1 1 calc R . . C16 C 0.61728(19) 1.04091(13) 0.12683(13) 0.0246(4) Uani 1 1 d . . . H16 H 0.5794 1.0597 0.0819 0.029 Uiso 1 1 calc R . . B2 B 0.3571(2) 0.87849(15) 0.26875(14) 0.0208(4) Uani 1 1 d . . . H2 H 0.4214 0.8238 0.2958 0.025 Uiso 1 1 calc R . . B3 B 0.1803(2) 0.88709(15) 0.32970(14) 0.0226(4) Uani 1 1 d . . . H3 H 0.1560 0.8357 0.3878 0.027 Uiso 1 1 calc R . . B4 B 0.0721(2) 0.99462(16) 0.34018(15) 0.0252(5) Uani 1 1 d . . . H4 H -0.0173 1.0193 0.3968 0.030 Uiso 1 1 calc R . . B5 B 0.1350(2) 1.04813(16) 0.23162(15) 0.0239(4) Uani 1 1 d . . . H5 H 0.0769 1.1166 0.2171 0.029 Uiso 1 1 calc R . . B6 B 0.3107(2) 1.03916(15) 0.17352(14) 0.0213(4) Uani 1 1 d . . . H6 H 0.3415 1.1034 0.1311 0.026 Uiso 1 1 calc R . . B7 B 0.3783(2) 0.91074(15) 0.14915(14) 0.0216(4) Uani 1 1 d . . . H7 H 0.4533 0.8787 0.0878 0.026 Uiso 1 1 calc R . . B8 B 0.2471(2) 0.84910(15) 0.21507(14) 0.0226(4) Uani 1 1 d . . . H8 H 0.2497 0.7733 0.1985 0.027 Uiso 1 1 calc R . . B9 B 0.0935(2) 0.92533(16) 0.24771(15) 0.0241(4) Uani 1 1 d . . . H9 H 0.0062 0.9006 0.2419 0.029 Uiso 1 1 calc R . . B10 B 0.2172(2) 0.95683(15) 0.14865(15) 0.0229(4) Uani 1 1 d . . . H10 H 0.1986 0.9599 0.0838 0.027 Uiso 1 1 calc R . . N1 N 0.64635(14) 0.57982(11) 0.22390(10) 0.0197(3) Uani 1 1 d . . . P1 P 0.58817(4) 0.48040(3) 0.24173(3) 0.01682(11) Uani 1 1 d . . . C21 C 0.60260(19) 0.43011(13) 0.13618(12) 0.0225(4) Uani 1 1 d . . . C22 C 0.66497(19) 0.47653(15) 0.05543(13) 0.0271(4) Uani 1 1 d . . . H22 H 0.7017 0.5320 0.0559 0.033 Uiso 1 1 calc R . . C23 C 0.6725(2) 0.43994(19) -0.02618(14) 0.0383(5) Uani 1 1 d . . . H23 H 0.7139 0.4711 -0.0804 0.046 Uiso 1 1 calc R . . C24 C 0.6186(3) 0.35754(17) -0.02668(15) 0.0427(6) Uani 1 1 d . . . H24 H 0.6246 0.3329 -0.0814 0.051 Uiso 1 1 calc R . . C25 C 0.5560(3) 0.31150(16) 0.05303(17) 0.0455(6) Uani 1 1 d . . . H25 H 0.5194 0.2562 0.0521 0.055 Uiso 1 1 calc R . . C26 C 0.5473(3) 0.34738(15) 0.13510(15) 0.0366(5) Uani 1 1 d . . . H26 H 0.5047 0.3163 0.1890 0.044 Uiso 1 1 calc R . . C31 C 0.65829(17) 0.39112(13) 0.30892(12) 0.0201(4) Uani 1 1 d . . . C32 C 0.7282(2) 0.29981(14) 0.27898(14) 0.0268(4) Uani 1 1 d . . . H32 H 0.7406 0.2809 0.2209 0.032 Uiso 1 1 calc R . . C33 C 0.7793(2) 0.23679(15) 0.33695(15) 0.0335(5) Uani 1 1 d . . . H33 H 0.8260 0.1756 0.3175 0.040 Uiso 1 1 calc R . . C34 C 0.7609(2) 0.26498(16) 0.42318(15) 0.0320(5) Uani 1 1 d . . . H34 H 0.7950 0.2224 0.4614 0.038 Uiso 1 1 calc R . . C35 C 0.69238(19) 0.35567(15) 0.45316(14) 0.0282(4) Uani 1 1 d . . . H35 H 0.6807 0.3742 0.5112 0.034 Uiso 1 1 calc R . . C36 C 0.64114(18) 0.41888(14) 0.39630(12) 0.0225(4) Uani 1 1 d . . . H36 H 0.5951 0.4801 0.4162 0.027 Uiso 1 1 calc R . . C41 C 0.41486(17) 0.50506(13) 0.30696(12) 0.0181(4) Uani 1 1 d . . . C42 C 0.35422(19) 0.43519(13) 0.36776(13) 0.0230(4) Uani 1 1 d . . . H42 H 0.4027 0.3748 0.3747 0.028 Uiso 1 1 calc R . . C43 C 0.22143(19) 0.45567(14) 0.41800(14) 0.0281(4) Uani 1 1 d . . . H43 H 0.1812 0.4095 0.4594 0.034 Uiso 1 1 calc R . . C44 C 0.14879(19) 0.54520(15) 0.40642(14) 0.0274(4) Uani 1 1 d . . . H44 H 0.0597 0.5589 0.4400 0.033 Uiso 1 1 calc R . . C45 C 0.20829(19) 0.61434(14) 0.34501(13) 0.0241(4) Uani 1 1 d . . . H45 H 0.1588 0.6739 0.3369 0.029 Uiso 1 1 calc R . . C46 C 0.34168(18) 0.59494(13) 0.29544(12) 0.0209(4) Uani 1 1 d . . . H46 H 0.3819 0.6417 0.2548 0.025 Uiso 1 1 calc R . . P2 P 0.78137(4) 0.60911(3) 0.22234(3) 0.01750(11) Uani 1 1 d . . . C51 C 0.83819(18) 0.69175(13) 0.12864(12) 0.0215(4) Uani 1 1 d . . . C52 C 0.74619(18) 0.75523(13) 0.09874(12) 0.0225(4) Uani 1 1 d . . . H51 H 0.6570 0.7501 0.1227 0.027 Uiso 1 1 calc R . . C53 C 0.7888(2) 0.82619(14) 0.03283(13) 0.0285(4) Uani 1 1 d . . . H52 H 0.7280 0.8686 0.0124 0.034 Uiso 1 1 calc R . . C54 C 0.9214(2) 0.83399(16) -0.00262(15) 0.0374(5) Uani 1 1 d . . . H53 H 0.9492 0.8820 -0.0464 0.045 Uiso 1 1 calc R . . C55 C 1.0128(2) 0.77077(17) 0.02675(17) 0.0407(6) Uani 1 1 d . . . H54 H 1.1019 0.7760 0.0023 0.049 Uiso 1 1 calc R . . C56 C 0.9718(2) 0.69966(15) 0.09247(15) 0.0316(5) Uani 1 1 d . . . H55 H 1.0332 0.6573 0.1124 0.038 Uiso 1 1 calc R . . C61 C 0.91308(17) 0.50808(13) 0.21256(13) 0.0212(4) Uani 1 1 d . . . C62 C 0.95400(19) 0.47129(14) 0.28553(13) 0.0256(4) Uani 1 1 d . . . H62 H 0.9177 0.5021 0.3408 0.031 Uiso 1 1 calc R . . C63 C 1.0492(2) 0.38858(16) 0.27549(16) 0.0345(5) Uani 1 1 d . . . H63 H 1.0753 0.3633 0.3245 0.041 Uiso 1 1 calc R . . C64 C 1.1054(2) 0.34350(15) 0.19331(16) 0.0349(5) Uani 1 1 d . . . H64 H 1.1701 0.2887 0.1869 0.042 Uiso 1 1 calc R . . C65 C 1.0656(2) 0.37985(16) 0.12030(15) 0.0351(5) Uani 1 1 d . . . H65 H 1.1035 0.3495 0.0649 0.042 Uiso 1 1 calc R . . C66 C 0.9692(2) 0.46167(14) 0.13007(13) 0.0279(4) Uani 1 1 d . . . H66 H 0.9419 0.4857 0.0813 0.033 Uiso 1 1 calc R . . C71 C 0.75745(18) 0.67641(12) 0.32106(12) 0.0200(4) Uani 1 1 d . . . C72 C 0.63141(18) 0.69688(13) 0.38442(12) 0.0215(4) Uani 1 1 d . . . H72 H 0.5616 0.6711 0.3785 0.026 Uiso 1 1 calc R . . C73 C 0.6111(2) 0.75617(14) 0.45638(13) 0.0267(4) Uani 1 1 d . . . H73 H 0.5275 0.7704 0.4988 0.032 Uiso 1 1 calc R . . C74 C 0.7155(2) 0.79391(14) 0.46467(14) 0.0309(5) Uani 1 1 d . . . H74 H 0.7015 0.8336 0.5129 0.037 Uiso 1 1 calc R . . C75 C 0.8412(2) 0.77337(15) 0.40191(14) 0.0310(4) Uani 1 1 d . . . H75 H 0.9109 0.7989 0.4083 0.037 Uiso 1 1 calc R . . C76 C 0.86195(19) 0.71502(14) 0.33006(13) 0.0264(4) Uani 1 1 d . . . H76 H 0.9457 0.7014 0.2876 0.032 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 0.02124(16) 0.01571(15) 0.02053(17) 0.00170(10) -0.00538(12) -0.00137(12) C2 0.0295(10) 0.0280(10) 0.0277(10) -0.0011(8) -0.0133(8) 0.0000(9) O2 0.0343(8) 0.0366(8) 0.0406(9) -0.0131(7) -0.0145(7) 0.0114(7) C3 0.0370(11) 0.0226(10) 0.0226(10) -0.0011(7) -0.0016(8) -0.0040(9) O3 0.0635(11) 0.0272(8) 0.0394(9) -0.0042(6) 0.0037(8) -0.0234(8) C4 0.0267(9) 0.0174(8) 0.0265(10) 0.0005(7) -0.0059(8) -0.0041(8) O4 0.0462(9) 0.0307(8) 0.0289(8) 0.0055(6) -0.0164(7) -0.0038(7) C1 0.0208(8) 0.0175(8) 0.0194(9) 0.0021(6) -0.0053(7) 0.0003(7) C11 0.0197(8) 0.0169(8) 0.0258(10) 0.0016(7) -0.0074(7) -0.0021(8) C12 0.0244(9) 0.0303(10) 0.0259(10) 0.0084(8) -0.0080(8) -0.0045(9) C13 0.0274(10) 0.0397(12) 0.0337(12) 0.0085(9) -0.0157(9) -0.0066(10) C14 0.0241(10) 0.0382(12) 0.0369(12) 0.0036(9) -0.0112(9) -0.0114(9) C15 0.0285(10) 0.0308(10) 0.0280(11) 0.0071(8) -0.0064(8) -0.0120(9) C16 0.0273(9) 0.0217(9) 0.0258(10) 0.0024(7) -0.0107(8) -0.0043(8) B2 0.0207(10) 0.0177(9) 0.0228(10) 0.0010(7) -0.0073(8) -0.0002(9) B3 0.0228(10) 0.0218(10) 0.0224(11) 0.0031(8) -0.0065(8) -0.0047(9) B4 0.0198(10) 0.0244(11) 0.0284(11) 0.0010(8) -0.0050(9) -0.0026(9) B5 0.0208(10) 0.0214(10) 0.0276(11) 0.0029(8) -0.0083(9) 0.0005(9) B6 0.0208(10) 0.0192(10) 0.0220(10) 0.0044(7) -0.0067(8) -0.0014(9) B7 0.0230(10) 0.0197(10) 0.0216(10) 0.0020(7) -0.0080(8) -0.0018(9) B8 0.0239(10) 0.0203(10) 0.0243(11) 0.0023(8) -0.0100(9) -0.0027(9) B9 0.0213(10) 0.0250(11) 0.0255(11) 0.0043(8) -0.0079(9) -0.0040(9) B10 0.0227(10) 0.0210(10) 0.0252(11) 0.0039(8) -0.0098(9) -0.0020(9) N1 0.0188(7) 0.0168(7) 0.0227(8) 0.0037(5) -0.0073(6) -0.0018(6) P1 0.0188(2) 0.0144(2) 0.0174(2) 0.00231(15) -0.00692(17) -0.00232(18) C21 0.0272(9) 0.0197(9) 0.0207(9) -0.0011(7) -0.0111(7) 0.0026(8) C22 0.0233(9) 0.0322(10) 0.0249(10) 0.0006(8) -0.0095(8) 0.0009(9) C23 0.0327(11) 0.0539(14) 0.0222(11) -0.0030(9) -0.0091(9) 0.0101(11) C24 0.0565(14) 0.0415(13) 0.0315(12) -0.0158(10) -0.0255(11) 0.0179(12) C25 0.0774(18) 0.0241(10) 0.0477(15) -0.0074(9) -0.0385(14) -0.0017(12) C26 0.0612(15) 0.0238(10) 0.0323(12) 0.0022(8) -0.0242(11) -0.0095(10) C31 0.0184(8) 0.0182(8) 0.0243(9) 0.0058(7) -0.0081(7) -0.0051(7) C32 0.0275(9) 0.0224(9) 0.0295(10) 0.0017(7) -0.0099(8) -0.0016(8) C33 0.0311(11) 0.0220(10) 0.0460(13) 0.0082(8) -0.0157(10) 0.0016(9) C34 0.0263(10) 0.0336(11) 0.0399(12) 0.0192(9) -0.0185(9) -0.0087(9) C35 0.0257(9) 0.0371(11) 0.0261(10) 0.0105(8) -0.0126(8) -0.0132(9) C36 0.0220(9) 0.0233(9) 0.0236(10) 0.0048(7) -0.0088(7) -0.0065(8) C41 0.0189(8) 0.0177(8) 0.0200(9) 0.0000(6) -0.0093(7) -0.0030(7) C42 0.0237(9) 0.0180(9) 0.0288(10) 0.0036(7) -0.0109(8) -0.0047(8) C43 0.0251(9) 0.0237(10) 0.0336(11) 0.0097(8) -0.0067(8) -0.0096(8) C44 0.0182(9) 0.0302(10) 0.0340(11) 0.0023(8) -0.0081(8) -0.0062(8) C45 0.0221(9) 0.0200(9) 0.0317(10) 0.0026(7) -0.0126(8) -0.0014(8) C46 0.0237(9) 0.0185(8) 0.0223(9) 0.0047(6) -0.0101(7) -0.0055(8) P2 0.0162(2) 0.0156(2) 0.0194(2) 0.00374(15) -0.00538(17) -0.00220(18) C51 0.0232(9) 0.0175(8) 0.0220(9) 0.0052(6) -0.0064(7) -0.0034(8) C52 0.0209(9) 0.0198(9) 0.0226(9) 0.0012(7) -0.0042(7) 0.0007(8) C53 0.0323(10) 0.0202(9) 0.0278(10) 0.0053(7) -0.0083(8) 0.0035(9) C54 0.0389(12) 0.0275(11) 0.0374(12) 0.0175(9) -0.0053(10) -0.0064(10) C55 0.0257(10) 0.0392(12) 0.0502(14) 0.0198(10) -0.0057(10) -0.0103(10) C56 0.0223(9) 0.0298(11) 0.0391(12) 0.0151(8) -0.0088(9) -0.0047(9) C61 0.0174(8) 0.0165(8) 0.0276(10) 0.0049(7) -0.0058(7) -0.0029(7) C62 0.0268(9) 0.0218(9) 0.0303(10) 0.0019(7) -0.0134(8) -0.0023(8) C63 0.0351(11) 0.0270(10) 0.0465(13) 0.0057(9) -0.0244(10) 0.0010(10) C64 0.0274(10) 0.0210(10) 0.0519(14) 0.0018(9) -0.0124(10) 0.0050(9) C65 0.0317(11) 0.0290(11) 0.0341(12) -0.0015(8) -0.0012(9) 0.0040(10) C66 0.0271(10) 0.0261(10) 0.0233(10) 0.0052(7) -0.0031(8) 0.0016(9) C71 0.0242(9) 0.0145(8) 0.0215(9) 0.0035(6) -0.0094(7) -0.0016(8) C72 0.0227(9) 0.0173(8) 0.0247(10) 0.0042(7) -0.0083(7) -0.0047(8) C73 0.0305(10) 0.0214(9) 0.0249(10) 0.0027(7) -0.0067(8) -0.0015(8) C74 0.0487(13) 0.0202(9) 0.0275(11) 0.0011(7) -0.0157(9) -0.0094(9) C75 0.0372(11) 0.0281(10) 0.0352(11) 0.0067(8) -0.0175(9) -0.0170(9) C76 0.0241(9) 0.0270(10) 0.0291(10) 0.0044(7) -0.0091(8) -0.0088(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles: correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C2 1.817(2) . ? Mn1 C3 1.836(2) . ? Mn1 C4 1.858(2) . ? Mn1 C1 2.0508(18) . ? Mn1 B4 2.109(2) . ? Mn1 B3 2.299(2) . ? Mn1 B5 2.324(2) . ? Mn1 B6 2.324(2) . ? Mn1 B2 2.335(2) . ? C2 O2 1.146(2) . ? C3 O3 1.143(3) . ? C4 O4 1.136(2) . ? C1 C11 1.491(3) . ? C1 B2 1.588(3) . ? C1 B6 1.628(3) . ? C1 B7 1.660(3) . ? C11 C16 1.389(3) . ? C11 C12 1.401(3) . ? C12 C13 1.382(3) . ? C13 C14 1.381(3) . ? C14 C15 1.382(3) . ? C15 C16 1.388(3) . ? B2 B8 1.796(3) . ? B2 B3 1.828(3) . ? B2 B7 1.842(3) . ? B3 B4 1.717(3) . ? B3 B8 1.788(3) . ? B3 B9 1.835(3) . ? B4 B9 1.739(3) . ? B4 B5 1.765(3) . ? B5 B10 1.791(3) . ? B5 B6 1.810(3) . ? B5 B9 1.818(3) . ? B6 B10 1.804(3) . ? B6 B7 1.828(3) . ? B7 B10 1.763(3) . ? B7 B8 1.771(3) . ? B8 B9 1.755(3) . ? B8 B10 1.799(3) . ? B9 B10 1.764(3) . ? N1 P1 1.5855(15) . ? N1 P2 1.5863(16) . ? P1 C31 1.7980(18) . ? P1 C21 1.8017(18) . ? P1 C41 1.8072(18) . ? C21 C22 1.388(3) . ? C21 C26 1.393(3) . ? C22 C23 1.391(3) . ? C23 C24 1.378(4) . ? C24 C25 1.374(4) . ? C25 C26 1.389(3) . ? C31 C32 1.391(3) . ? C31 C36 1.400(3) . ? C32 C33 1.395(3) . ? C33 C34 1.382(3) . ? C34 C35 1.379(3) . ? C35 C36 1.384(3) . ? C41 C42 1.392(3) . ? C41 C46 1.393(2) . ? C42 C43 1.387(3) . ? C43 C44 1.387(3) . ? C44 C45 1.385(3) . ? C45 C46 1.389(3) . ? P2 C51 1.7958(18) . ? P2 C71 1.7992(18) . ? P2 C61 1.8001(18) . ? C51 C52 1.394(3) . ? C51 C56 1.395(3) . ? C52 C53 1.388(3) . ? C53 C54 1.383(3) . ? C54 C55 1.384(3) . ? C55 C56 1.385(3) . ? C61 C66 1.393(3) . ? C61 C62 1.394(3) . ? C62 C63 1.388(3) . ? C63 C64 1.380(3) . ? C64 C65 1.386(3) . ? C65 C66 1.387(3) . ? C71 C76 1.393(3) . ? C71 C72 1.396(3) . ? C72 C73 1.390(3) . ? C73 C74 1.381(3) . ? C74 C75 1.390(3) . ? C75 C76 1.379(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 C2 Mn1 C3 82.99(9) . . ? C2 Mn1 C4 94.22(8) . . ? C3 Mn1 C4 95.44(9) . . ? C2 Mn1 C1 157.37(8) . . ? C3 Mn1 C1 83.52(8) . . ? C4 Mn1 C1 105.09(8) . . ? C2 Mn1 B4 68.28(9) . . ? C3 Mn1 B4 143.54(9) . . ? C4 Mn1 B4 108.20(9) . . ? C1 Mn1 B4 115.07(8) . . ? C2 Mn1 B3 109.05(9) . . ? C3 Mn1 B3 167.80(8) . . ? C4 Mn1 B3 85.85(8) . . ? C1 Mn1 B3 84.44(7) . . ? B4 Mn1 B3 45.59(8) . . ? C2 Mn1 B5 82.79(8) . . ? C3 Mn1 B5 109.86(9) . . ? C4 Mn1 B5 153.86(8) . . ? C1 Mn1 B5 84.82(7) . . ? B4 Mn1 B5 46.61(8) . . ? B3 Mn1 B5 70.85(8) . . ? C2 Mn1 B6 117.26(8) . . ? C3 Mn1 B6 84.33(8) . . ? C4 Mn1 B6 148.13(8) . . ? C1 Mn1 B6 43.12(7) . . ? B4 Mn1 B6 89.23(8) . . ? B3 Mn1 B6 88.19(8) . . ? B5 Mn1 B6 45.84(7) . . ? C2 Mn1 B2 155.47(9) . . ? C3 Mn1 B2 121.54(8) . . ? C4 Mn1 B2 84.06(8) . . ? C1 Mn1 B2 41.83(7) . . ? B4 Mn1 B2 88.95(8) . . ? B3 Mn1 B2 46.45(7) . . ? B5 Mn1 B2 88.07(7) . . ? B6 Mn1 B2 69.43(7) . . ? O2 C2 Mn1 172.89(19) . . ? O3 C3 Mn1 177.36(18) . . ? O4 C4 Mn1 179.08(18) . . ? C11 C1 B2 123.88(15) . . ? C11 C1 B6 123.74(15) . . ? B2 C1 B6 111.21(15) . . ? C11 C1 B7 120.96(15) . . ? B2 C1 B7 69.03(13) . . ? B6 C1 B7 67.55(12) . . ? C11 C1 Mn1 121.39(13) . . ? B2 C1 Mn1 78.71(10) . . ? B6 C1 Mn1 77.44(10) . . ? B7 C1 Mn1 117.62(12) . . ? C16 C11 C12 118.11(17) . . ? C16 C11 C1 121.74(17) . . ? C12 C11 C1 120.13(17) . . ? C13 C12 C11 121.04(18) . . ? C14 C13 C12 120.21(19) . . ? C13 C14 C15 119.40(19) . . ? C14 C15 C16 120.71(19) . . ? C15 C16 C11 120.53(18) . . ? C1 B2 B8 107.97(15) . . ? C1 B2 B3 117.90(14) . . ? B8 B2 B3 59.12(12) . . ? C1 B2 B7 57.33(11) . . ? B8 B2 B7 58.24(12) . . ? B3 B2 B7 107.78(14) . . ? C1 B2 Mn1 59.46(9) . . ? B8 B2 Mn1 103.64(11) . . ? B3 B2 Mn1 65.75(9) . . ? B7 B2 Mn1 98.53(11) . . ? B4 B3 B8 111.46(15) . . ? B4 B3 B2 123.14(15) . . ? B8 B3 B2 59.57(11) . . ? B4 B3 B9 58.50(12) . . ? B8 B3 B9 57.92(11) . . ? B2 B3 B9 107.58(14) . . ? B4 B3 Mn1 61.33(10) . . ? B8 B3 Mn1 105.33(12) . . ? B2 B3 Mn1 67.81(9) . . ? B9 B3 Mn1 97.56(11) . . ? B3 B4 B9 64.16(13) . . ? B3 B4 B5 100.66(15) . . ? B9 B4 B5 62.52(13) . . ? B3 B4 Mn1 73.08(11) . . ? B9 B4 Mn1 108.25(13) . . ? B5 B4 Mn1 73.12(11) . . ? B4 B5 B10 111.23(15) . . ? B4 B5 B6 121.39(15) . . ? B10 B5 B6 60.13(12) . . ? B4 B5 B9 58.04(12) . . ? B10 B5 B9 58.52(12) . . ? B6 B5 B9 107.99(14) . . ? B4 B5 Mn1 60.27(10) . . ? B10 B5 Mn1 105.54(11) . . ? B6 B5 Mn1 67.10(9) . . ? B9 B5 Mn1 97.21(11) . . ? C1 B6 B10 107.64(14) . . ? C1 B6 B5 118.57(15) . . ? B10 B6 B5 59.41(12) . . ? C1 B6 B7 57.07(11) . . ? B10 B6 B7 58.08(11) . . ? B5 B6 B7 108.23(14) . . ? C1 B6 Mn1 59.45(9) . . ? B10 B6 Mn1 105.06(12) . . ? B5 B6 Mn1 67.06(9) . . ? B7 B6 Mn1 99.31(11) . . ? C1 B7 B10 108.10(15) . . ? C1 B7 B8 105.95(14) . . ? B10 B7 B8 61.20(12) . . ? C1 B7 B6 55.38(11) . . ? B10 B7 B6 60.29(12) . . ? B8 B7 B6 103.05(14) . . ? C1 B7 B2 53.63(11) . . ? B10 B7 B2 104.15(14) . . ? B8 B7 B2 59.60(11) . . ? B6 B7 B2 92.62(13) . . ? B9 B8 B7 113.25(15) . . ? B9 B8 B3 62.38(12) . . ? B7 B8 B3 112.80(15) . . ? B9 B8 B2 112.64(15) . . ? B7 B8 B2 62.15(12) . . ? B3 B8 B2 61.31(12) . . ? B9 B8 B10 59.51(12) . . ? B7 B8 B10 59.19(12) . . ? B3 B8 B10 105.05(14) . . ? B2 B8 B10 104.56(15) . . ? B4 B9 B8 112.02(16) . . ? B4 B9 B10 113.79(16) . . ? B8 B9 B10 61.49(12) . . ? B4 B9 B5 59.44(12) . . ? B8 B9 B5 104.13(15) . . ? B10 B9 B5 59.98(12) . . ? B4 B9 B3 57.35(12) . . ? B8 B9 B3 59.69(11) . . ? B10 B9 B3 104.53(15) . . ? B5 B9 B3 94.37(14) . . ? B7 B10 B9 113.17(15) . . ? B7 B10 B5 112.06(16) . . ? B9 B10 B5 61.50(12) . . ? B7 B10 B8 59.61(12) . . ? B9 B10 B8 59.00(12) . . ? B5 B10 B8 103.44(14) . . ? B7 B10 B6 61.64(12) . . ? B9 B10 B6 110.66(15) . . ? B5 B10 B6 60.46(12) . . ? B8 B10 B6 102.89(14) . . ? P1 N1 P2 134.03(10) . . ? N1 P1 C31 114.35(8) . . ? N1 P1 C21 110.19(9) . . ? C31 P1 C21 110.83(8) . . ? N1 P1 C41 108.78(8) . . ? C31 P1 C41 104.52(8) . . ? C21 P1 C41 107.81(8) . . ? C22 C21 C26 119.80(18) . . ? C22 C21 P1 119.58(15) . . ? C26 C21 P1 120.58(15) . . ? C21 C22 C23 119.9(2) . . ? C24 C23 C22 120.0(2) . . ? C25 C24 C23 120.5(2) . . ? C24 C25 C26 120.2(2) . . ? C25 C26 C21 119.7(2) . . ? C32 C31 C36 119.72(16) . . ? C32 C31 P1 124.39(15) . . ? C36 C31 P1 115.88(13) . . ? C31 C32 C33 119.34(19) . . ? C34 C33 C32 120.27(19) . . ? C35 C34 C33 120.71(17) . . ? C34 C35 C36 119.59(19) . . ? C35 C36 C31 120.37(17) . . ? C42 C41 C46 120.02(16) . . ? C42 C41 P1 120.72(13) . . ? C46 C41 P1 119.26(14) . . ? C43 C42 C41 119.99(17) . . ? C42 C43 C44 119.87(18) . . ? C45 C44 C43 120.31(18) . . ? C44 C45 C46 120.16(17) . . ? C45 C46 C41 119.64(17) . . ? N1 P2 C51 109.88(8) . . ? N1 P2 C71 110.58(8) . . ? C51 P2 C71 105.00(8) . . ? N1 P2 C61 114.73(8) . . ? C51 P2 C61 107.05(8) . . ? C71 P2 C61 109.10(8) . . ? C52 C51 C56 120.12(17) . . ? C52 C51 P2 119.28(14) . . ? C56 C51 P2 120.25(14) . . ? C53 C52 C51 119.44(18) . . ? C54 C53 C52 120.25(18) . . ? C53 C54 C55 120.37(19) . . ? C54 C55 C56 120.1(2) . . ? C55 C56 C51 119.77(19) . . ? C66 C61 C62 119.44(17) . . ? C66 C61 P2 117.94(14) . . ? C62 C61 P2 122.49(15) . . ? C63 C62 C61 119.77(19) . . ? C64 C63 C62 120.51(19) . . ? C63 C64 C65 120.08(19) . . ? C64 C65 C66 119.8(2) . . ? C65 C66 C61 120.39(19) . . ? C76 C71 C72 120.21(17) . . ? C76 C71 P2 119.92(14) . . ? C72 C71 P2 119.64(15) . . ? C73 C72 C71 119.45(18) . . ? C74 C73 C72 119.82(18) . . ? C73 C74 C75 120.86(19) . . ? C76 C75 C74 119.7(2) . . ? C75 C76 C71 119.98(18) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 70.22 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.461 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.058 #==============================================================================