# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Ni, Chengbao' 'Fettinger, James' 'Long, Gary' 'Power, Philip' _publ_contact_author_name 'Power, Philip' _publ_contact_author_email pppower@ucdavis.edu _publ_section_title ; Terphenyl Substituted Derivatives of Manganese(II): Distorted Geometries and Resistance to Elimination ; # Attachment 'CIF-Mn-010510.CIF' data_rw21fmi _database_code_depnum_ccdc_archive 'CCDC 794076' #TrackingRef 'CIF-Mn-010510.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H98 Cl3.72 I0.28 Li2 Mn2 O3' _chemical_formula_sum 'C72 H98 Cl3.72 I0.28 Li2 Mn2 O3' _chemical_formula_weight 1302.67 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.9458(6) _cell_length_b 25.4683(11) _cell_length_c 21.7044(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.1940(10) _cell_angle_gamma 90.00 _cell_volume 6994.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9890 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.87 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7754 _exptl_absorpt_correction_T_max 0.9360 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; A colorless block with approximate orthogonal dimensions 0.40 x 0.37 x 0.10mm3 was placed and optically centered on the Bruker SMART1000(1) CCD system at 90(2)K. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide Omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 40 seconds per frame and 606 frames were collected, at varying phi angles (phi=0? 90? 180? 270?, for each series. The crystal to detector distance was 4.28cm, thus providing a complete sphere of data with processing to 2ThetaMax=55.21? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48227 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.25 _reflns_number_total 12661 _reflns_number_gt 8005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Version 5.054) (Bruker, 2002)' _computing_cell_refinement 'SAINT (7.46A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.46A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: Allcrystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. The SHELXTL(4) program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences and intensity statistics indicated the centrosymmetric monoclinic non-standard space group P21/n (no. 14). The structure was determined by direct methods with the successful location of a majority of the molecule within the asymmetric unit. The bridging halide species were refined as a mixture of chloride and iodide. References: 1. Bruker (2007) APEX (Version 2.0.2) and SAINT (Version 7.46A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008/1) Version 2.10, 'Siemens Area Detector Absorption Correction' Universitat G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universitat G ttingen: G ttingen, Germany. PLAT201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 17 The THF molecules bounded to the lithium appear to disorder over two positions and the lithium ions are also disordered. In addition, the very large librational shifts of the THF atoms and the lithium atoms have different directions. Thus, these atoms were not refined anisotropically. PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.61 Ratio This is due to the large librational shifts of the isopropyl groups on the flanking aryl rings. Such large Ueq(max)/Ueq(min) is normally observed for isopropyl carbon atoms in similar complexes. PLAT413_ALERT_2_B Short Inter XH3 .. XHn H30A .. H80B .. 2.09 Ang. This is caused by disorder of the coordinating THF and large librational shifts of some of the carbons. PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C62 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O4 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O6 Compared to the carbons of the THF (THF with O4 and O6), the oxygen is bounded to the lithium and display less librational shift. However, the carbons of the THF shows larger libratinal shifts. Again, the disorder problem may also be possible reasons. The are also responsible for the following alerts: PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ...2.59 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ...3.98 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C16 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Li1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C84 PLAT413_ALERT_2_C Short Inter XH3 .. XHn H60B .. H76A ..2.13 Ang. PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? The non-integer comes from the iodide impurty of the crystals. The bridging halides are a mixture of chloride and iodide and they were employed in the refinement process. Their numbers sum up to 4, which is expected and consistent with the structure of the complex. ; _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^)+(0.0661P)^2^+6.7944P] 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 12661 _refine_ls_number_parameters 761 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.105 _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 0.46239(4) 0.22937(2) 0.80280(2) 0.03037(15) Uani 1 1 d D . . Mn2 Mn 0.61155(5) 0.11325(2) 0.77481(3) 0.03792(16) Uani 1 1 d D . . Cl1 Cl 0.54221(7) 0.15231(4) 0.86334(4) 0.0385(2) Uani 1 1 d D A . Cl2 Cl 0.5706(4) 0.20228(19) 0.72410(19) 0.0398(7) Uani 0.82 1 d PD A 1 I2 I 0.5821(5) 0.2022(2) 0.7086(2) 0.0332(7) Uani 0.18 1 d P A 2 Cl3 Cl 0.2967(3) 0.19174(16) 0.74340(18) 0.0462(5) Uani 0.90 1 d P A 1 I3 I 0.2747(8) 0.1835(5) 0.7359(5) 0.0462(5) Uani 0.10 1 d P A 2 C1 C 0.4615(3) 0.30401(13) 0.84722(15) 0.0271(7) Uani 1 1 d . A . C2 C 0.5098(3) 0.34692(13) 0.82321(15) 0.0289(8) Uani 1 1 d . . . C3 C 0.5242(3) 0.39508(15) 0.85402(18) 0.0391(9) Uani 1 1 d . A . H3 H 0.5577 0.4229 0.8367 0.047 Uiso 1 1 calc R . . C4 C 0.4903(3) 0.40278(16) 0.90933(19) 0.0454(10) Uani 1 1 d . . . H4 H 0.5032 0.4352 0.9312 0.054 Uiso 1 1 calc R A . C5 C 0.4373(3) 0.36290(15) 0.93262(18) 0.0410(9) Uani 1 1 d . A . H5 H 0.4116 0.3685 0.9700 0.049 Uiso 1 1 calc R . . C6 C 0.4210(3) 0.31461(14) 0.90205(16) 0.0317(8) Uani 1 1 d . . . C7 C 0.5431(3) 0.34218(14) 0.76117(16) 0.0335(8) Uani 1 1 d . A . C8 C 0.6502(3) 0.34123(14) 0.75825(17) 0.0367(9) Uani 1 1 d . . . C9 C 0.6768(4) 0.33750(16) 0.69930(19) 0.0479(11) Uani 1 1 d . A . H9 H 0.7491 0.3364 0.6968 0.057 Uiso 1 1 calc R . . C10 C 0.6003(4) 0.33536(19) 0.6448(2) 0.0625(14) Uani 1 1 d . . . H10 H 0.6198 0.3326 0.6051 0.075 Uiso 1 1 calc R A . C11 C 0.4956(4) 0.3372(2) 0.64785(19) 0.0627(14) Uani 1 1 d . A . H11 H 0.4434 0.3362 0.6099 0.075 Uiso 1 1 calc R . . C12 C 0.4639(3) 0.34066(17) 0.70513(17) 0.0462(10) Uani 1 1 d . . . C13 C 0.7352(3) 0.34325(15) 0.81870(18) 0.0401(9) Uani 1 1 d . A . H13 H 0.7097 0.3685 0.8474 0.048 Uiso 1 1 calc R . . C14 C 0.7467(4) 0.29034(18) 0.8521(2) 0.0593(12) Uani 1 1 d . . . H14A H 0.6797 0.2809 0.8634 0.089 Uiso 1 1 calc R A . H14B H 0.8024 0.2925 0.8904 0.089 Uiso 1 1 calc R . . H14C H 0.7654 0.2635 0.8240 0.089 Uiso 1 1 calc R . . C15 C 0.8400(3) 0.36454(19) 0.8084(2) 0.0564(12) Uani 1 1 d . . . H15A H 0.8702 0.3399 0.7823 0.085 Uiso 1 1 calc R A . H15B H 0.8890 0.3688 0.8492 0.085 Uiso 1 1 calc R . . H15C H 0.8285 0.3986 0.7871 0.085 Uiso 1 1 calc R . . C16 C 0.3481(4) 0.3470(2) 0.7060(2) 0.0626(14) Uani 1 1 d . A . H16 H 0.3370 0.3322 0.7468 0.075 Uiso 1 1 calc R . . C17 C 0.2720(4) 0.3192(3) 0.6534(2) 0.099(2) Uani 1 1 d . . . H17A H 0.2821 0.3323 0.6126 0.148 Uiso 1 1 calc R A . H17B H 0.1993 0.3262 0.6574 0.148 Uiso 1 1 calc R . . H17C H 0.2855 0.2814 0.6561 0.148 Uiso 1 1 calc R . . C18 C 0.3218(4) 0.4051(3) 0.7054(3) 0.101(2) Uani 1 1 d . . . H18A H 0.3640 0.4219 0.7430 0.151 Uiso 1 1 calc R A . H18B H 0.2465 0.4095 0.7051 0.151 Uiso 1 1 calc R . . H18C H 0.3379 0.4214 0.6676 0.151 Uiso 1 1 calc R . . C19 C 0.3489(3) 0.27726(15) 0.92599(17) 0.0374(9) Uani 1 1 d . A . C20 C 0.2394(3) 0.28143(18) 0.89908(19) 0.0493(11) Uani 1 1 d . . . C21 C 0.1695(4) 0.2513(2) 0.9247(2) 0.0644(14) Uani 1 1 d . A . H21 H 0.0959 0.2536 0.9073 0.077 Uiso 1 1 calc R . . C22 C 0.2044(4) 0.2187(2) 0.9739(3) 0.0694(15) Uani 1 1 d . . . H22 H 0.1548 0.1988 0.9907 0.083 Uiso 1 1 calc R A . C23 C 0.3106(4) 0.21404(18) 1.0000(2) 0.0602(13) Uani 1 1 d . A . H23 H 0.3334 0.1907 1.0342 0.072 Uiso 1 1 calc R . . C24 C 0.3862(3) 0.24371(16) 0.97623(18) 0.0434(10) Uani 1 1 d . . . C25 C 0.1968(3) 0.3211(2) 0.8472(2) 0.0623(14) Uani 1 1 d . A . H25 H 0.2578 0.3326 0.8288 0.075 Uiso 1 1 calc R . . C26 C 0.1141(4) 0.2980(3) 0.7937(3) 0.095(2) Uani 1 1 d . . . H26A H 0.1432 0.2670 0.7768 0.142 Uiso 1 1 calc R A . H26B H 0.0942 0.3243 0.7603 0.142 Uiso 1 1 calc R . . H26C H 0.0515 0.2880 0.8097 0.142 Uiso 1 1 calc R . . C27 C 0.1536(4) 0.3698(2) 0.8736(2) 0.0716(15) Uani 1 1 d . . . H27A H 0.0957 0.3598 0.8939 0.107 Uiso 1 1 calc R A . H27B H 0.1273 0.3946 0.8393 0.107 Uiso 1 1 calc R . . H27C H 0.2100 0.3865 0.9047 0.107 Uiso 1 1 calc R . . C28 C 0.5020(4) 0.23927(17) 1.00517(19) 0.0503(11) Uani 1 1 d . A . H28 H 0.5415 0.2513 0.9729 0.060 Uiso 1 1 calc R . . C29 C 0.5375(5) 0.18301(19) 1.0233(2) 0.0691(15) Uani 1 1 d . . . H29A H 0.5144 0.1730 1.0618 0.104 Uiso 1 1 calc R A . H29B H 0.6147 0.1809 1.0305 0.104 Uiso 1 1 calc R . . H29C H 0.5060 0.1591 0.9890 0.104 Uiso 1 1 calc R . . C30 C 0.5345(4) 0.27482(19) 1.0627(2) 0.0694(14) Uani 1 1 d . . . H30A H 0.5147 0.3112 1.0508 0.104 Uiso 1 1 calc R A . H30B H 0.6112 0.2727 1.0783 0.104 Uiso 1 1 calc R . . H30C H 0.4985 0.2635 1.0959 0.104 Uiso 1 1 calc R . . C31 C 0.7429(3) 0.06165(14) 0.78015(17) 0.0358(9) Uani 1 1 d . A . C32 C 0.7745(3) 0.02920(14) 0.83394(16) 0.0332(8) Uani 1 1 d . . . C33 C 0.8519(3) -0.00866(15) 0.83850(17) 0.0380(9) Uani 1 1 d . A . H33 H 0.8699 -0.0297 0.8753 0.046 Uiso 1 1 calc R . . C34 C 0.9039(3) -0.01603(16) 0.78896(19) 0.0439(10) Uani 1 1 d . . . H34 H 0.9564 -0.0424 0.7913 0.053 Uiso 1 1 calc R A . C35 C 0.8776(4) 0.01566(16) 0.73672(19) 0.0486(11) Uani 1 1 d . A . H35 H 0.9144 0.0116 0.7035 0.058 Uiso 1 1 calc R . . C36 C 0.7982(3) 0.05380(15) 0.73113(17) 0.0404(10) Uani 1 1 d . . . C37 C 0.7230(3) 0.03763(14) 0.88950(16) 0.0330(8) Uani 1 1 d . A . C38 C 0.7691(3) 0.07316(14) 0.93671(16) 0.0338(8) Uani 1 1 d . . . C39 C 0.7199(3) 0.08153(15) 0.98729(16) 0.0398(9) Uani 1 1 d . A . H39 H 0.7506 0.1053 1.0198 0.048 Uiso 1 1 calc R . . C40 C 0.6284(4) 0.05620(15) 0.99080(17) 0.0452(10) Uani 1 1 d . . . H40 H 0.5953 0.0631 1.0251 0.054 Uiso 1 1 calc R A . C41 C 0.5839(3) 0.02078(16) 0.94502(18) 0.0463(10) Uani 1 1 d . A . H41 H 0.5205 0.0032 0.9482 0.056 Uiso 1 1 calc R . . C42 C 0.6308(3) 0.01033(15) 0.89374(16) 0.0391(9) Uani 1 1 d . . . C43 C 0.8706(3) 0.10241(15) 0.93471(19) 0.0424(10) Uani 1 1 d . A . H43 H 0.8920 0.0931 0.8944 0.051 Uiso 1 1 calc R . . C44 C 0.8553(4) 0.16145(18) 0.9359(3) 0.0659(13) Uani 1 1 d . . . H44A H 0.8020 0.1722 0.8990 0.099 Uiso 1 1 calc R A . H44B H 0.9224 0.1790 0.9353 0.099 Uiso 1 1 calc R . . H44C H 0.8317 0.1713 0.9744 0.099 Uiso 1 1 calc R . . C45 C 0.9588(4) 0.0852(2) 0.9894(2) 0.0644(13) Uani 1 1 d . . . H45A H 0.9370 0.0914 1.0294 0.097 Uiso 1 1 calc R A . H45B H 1.0230 0.1053 0.9886 0.097 Uiso 1 1 calc R . . H45C H 0.9730 0.0477 0.9853 0.097 Uiso 1 1 calc R . . C46 C 0.5849(4) -0.03220(19) 0.84653(19) 0.0535(12) Uani 1 1 d . A . H46 H 0.6081 -0.0247 0.8063 0.064 Uiso 1 1 calc R . . C47 C 0.4644(4) -0.0349(2) 0.8315(2) 0.0711(16) Uani 1 1 d . . . H47A H 0.4399 -0.0475 0.8687 0.107 Uiso 1 1 calc R A . H47B H 0.4406 -0.0591 0.7963 0.107 Uiso 1 1 calc R . . H47C H 0.4352 0.0001 0.8200 0.107 Uiso 1 1 calc R . . C48 C 0.6297(4) -0.08541(19) 0.8703(2) 0.0706(16) Uani 1 1 d . . . H48A H 0.7070 -0.0845 0.8771 0.106 Uiso 1 1 calc R A . H48B H 0.6020 -0.1124 0.8391 0.106 Uiso 1 1 calc R . . H48C H 0.6091 -0.0936 0.9102 0.106 Uiso 1 1 calc R . . C49 C 0.7757(4) 0.08556(16) 0.6718(2) 0.0550(12) Uani 1 1 d . A . C50 C 0.7239(5) 0.06212(19) 0.6145(2) 0.0664(15) Uani 1 1 d . . . C51 C 0.7105(5) 0.0917(2) 0.5593(2) 0.0813(18) Uani 1 1 d . A . H51 H 0.6767 0.0763 0.5204 0.098 Uiso 1 1 calc R . . C52 C 0.7448(6) 0.1423(2) 0.5601(3) 0.089(2) Uani 1 1 d . . . H52 H 0.7345 0.1617 0.5220 0.107 Uiso 1 1 calc R A . C53 C 0.7945(5) 0.1656(2) 0.6159(3) 0.089(2) Uani 1 1 d . A . H53 H 0.8171 0.2010 0.6157 0.106 Uiso 1 1 calc R . . C54 C 0.8120(4) 0.13813(18) 0.6722(3) 0.0694(16) Uani 1 1 d . . . C55 C 0.6834(6) 0.0058(2) 0.6113(2) 0.0768(17) Uani 1 1 d . A . H55 H 0.7056 -0.0100 0.6542 0.092 Uiso 1 1 calc R . . C56 C 0.5624(6) 0.0034(3) 0.5927(3) 0.103(2) Uani 1 1 d . . . H56A H 0.5321 0.0233 0.6232 0.154 Uiso 1 1 calc R A . H56B H 0.5392 -0.0333 0.5923 0.154 Uiso 1 1 calc R . . H56C H 0.5386 0.0186 0.5506 0.154 Uiso 1 1 calc R . . C57 C 0.7324(5) -0.0271(2) 0.5654(2) 0.0848(18) Uani 1 1 d . . . H57A H 0.7074 -0.0140 0.5224 0.127 Uiso 1 1 calc R A . H57B H 0.7117 -0.0639 0.5677 0.127 Uiso 1 1 calc R . . H57C H 0.8096 -0.0242 0.5770 0.127 Uiso 1 1 calc R . . C58 C 0.8718(4) 0.16362(18) 0.7330(3) 0.0782(18) Uani 1 1 d . A . H58 H 0.8383 0.1515 0.7680 0.094 Uiso 1 1 calc R . . C59 C 0.8668(5) 0.2236(2) 0.7315(4) 0.110(3) Uani 1 1 d . . . H59A H 0.8942 0.2374 0.7739 0.165 Uiso 1 1 calc R A . H59B H 0.7934 0.2348 0.7168 0.165 Uiso 1 1 calc R . . H59C H 0.9098 0.2369 0.7027 0.165 Uiso 1 1 calc R . . C60 C 0.9867(5) 0.1466(2) 0.7487(3) 0.096(2) Uani 1 1 d . . . H60A H 1.0227 0.1599 0.7164 0.144 Uiso 1 1 calc R A . H60B H 0.9906 0.1082 0.7499 0.144 Uiso 1 1 calc R . . H60C H 1.0210 0.1608 0.7899 0.144 Uiso 1 1 calc R . . Li1 Li 0.4058(9) 0.1641(4) 0.6743(5) 0.043(2) Uiso 0.62 1 d P A 1 Li2 Li 0.2796(8) 0.1017(4) 0.7534(5) 0.040(2) Uiso 0.62 1 d P A 1 Cl4 Cl 0.4399(4) 0.07974(11) 0.7174(3) 0.0453(8) Uani 0.62 1 d P A 1 O1 O 0.3596(5) 0.1741(3) 0.5869(3) 0.080(2) Uiso 0.62 1 d PD A 1 C61 C 0.3792(10) 0.2208(4) 0.5548(6) 0.105(3) Uiso 0.62 1 d PD A 1 H61A H 0.4091 0.2485 0.5853 0.126 Uiso 0.62 1 calc PR A 1 H61B H 0.3131 0.2340 0.5276 0.126 Uiso 0.62 1 calc PR A 1 C62 C 0.4556(8) 0.2055(3) 0.5164(5) 0.070(3) Uiso 0.62 1 d PD A 1 H62A H 0.5292 0.2095 0.5405 0.084 Uiso 0.62 1 calc PR A 1 H62B H 0.4461 0.2267 0.4774 0.084 Uiso 0.62 1 calc PR A 1 C63 C 0.4297(12) 0.1495(5) 0.5018(6) 0.121(5) Uiso 0.62 1 d PD A 1 H63A H 0.4912 0.1264 0.5173 0.146 Uiso 0.62 1 calc PR A 1 H63B H 0.4039 0.1439 0.4560 0.146 Uiso 0.62 1 calc PR A 1 C64 C 0.3372(12) 0.1403(6) 0.5403(6) 0.152(5) Uiso 0.62 1 d PD A 1 H64A H 0.2668 0.1475 0.5134 0.183 Uiso 0.62 1 calc PR A 1 H64B H 0.3385 0.1039 0.5563 0.183 Uiso 0.62 1 calc PR A 1 O2 O 0.2549(4) 0.08129(17) 0.8318(2) 0.0340(10) Uiso 0.62 1 d P A 1 C65 C 0.1953(6) 0.0363(3) 0.8414(3) 0.0455(16) Uiso 0.62 1 d P A 1 H65A H 0.2391 0.0044 0.8416 0.055 Uiso 0.62 1 calc PR A 1 H65B H 0.1327 0.0331 0.8064 0.055 Uiso 0.62 1 calc PR A 1 C66 C 0.1615(6) 0.0402(3) 0.9003(3) 0.0487(17) Uiso 0.62 1 d P A 1 H66A H 0.1638 0.0055 0.9212 0.058 Uiso 0.62 1 calc PR A 1 H66B H 0.0888 0.0544 0.8939 0.058 Uiso 0.62 1 calc PR A 1 C67 C 0.2422(7) 0.0785(3) 0.9397(3) 0.0507(19) Uiso 0.62 1 d P A 1 H67A H 0.2070 0.1027 0.9646 0.061 Uiso 0.62 1 calc PR A 1 H67B H 0.2987 0.0592 0.9688 0.061 Uiso 0.62 1 calc PR A 1 C68 C 0.2861(6) 0.1080(3) 0.8909(3) 0.0519(17) Uiso 0.62 1 d P A 1 H68A H 0.2587 0.1444 0.8871 0.062 Uiso 0.62 1 calc PR A 1 H68B H 0.3642 0.1095 0.9033 0.062 Uiso 0.62 1 calc PR A 1 O3 O 0.1790(3) 0.06566(16) 0.68727(18) 0.0387(10) Uiso 0.62 1 d PD A 1 C69 C 0.1168(6) 0.0892(3) 0.6333(3) 0.0555(18) Uiso 0.62 1 d PD A 1 H69A H 0.1456 0.1241 0.6259 0.067 Uiso 0.62 1 calc PR A 1 H69B H 0.0432 0.0937 0.6386 0.067 Uiso 0.62 1 calc PR A 1 C70 C 0.1203(6) 0.0518(3) 0.5774(3) 0.0552(18) Uiso 0.62 1 d PD A 1 H70A H 0.0516 0.0339 0.5630 0.066 Uiso 0.62 1 calc PR A 1 H70B H 0.1382 0.0712 0.5416 0.066 Uiso 0.62 1 calc PR A 1 C71 C 0.2039(5) 0.0138(3) 0.6036(3) 0.0443(16) Uiso 0.62 1 d PD A 1 H71A H 0.2741 0.0259 0.5981 0.053 Uiso 0.62 1 calc PR A 1 H71B H 0.1889 -0.0213 0.5840 0.053 Uiso 0.62 1 calc PR A 1 C72 C 0.1970(6) 0.0132(3) 0.6740(3) 0.0452(17) Uiso 0.62 1 d PD A 1 H72A H 0.1381 -0.0094 0.6807 0.054 Uiso 0.62 1 calc PR A 1 H72B H 0.2638 0.0004 0.7008 0.054 Uiso 0.62 1 calc PR A 1 Li3 Li 0.3795(14) 0.1045(7) 0.8070(8) 0.044(4) Uiso 0.38 1 d P A 2 Li4 Li 0.3445(17) 0.1220(9) 0.6625(10) 0.060(5) Uiso 0.38 1 d P A 2 Cl4B Cl 0.4545(8) 0.0628(2) 0.7239(5) 0.0453(8) Uani 0.38 1 d P A 2 O4 O 0.2942(6) 0.0726(3) 0.8525(4) 0.0386(18) Uiso 0.38 1 d P A 2 C73 C 0.3129(12) 0.0730(6) 0.9201(7) 0.077(4) Uiso 0.38 1 d P A 2 H73A H 0.3341 0.1084 0.9367 0.092 Uiso 0.38 1 calc PR A 2 H73B H 0.3696 0.0478 0.9382 0.092 Uiso 0.38 1 calc PR A 2 C74 C 0.2091(14) 0.0569(8) 0.9366(8) 0.080(5) Uiso 0.38 1 d P A 2 H74A H 0.2081 0.0187 0.9449 0.096 Uiso 0.38 1 calc PR A 2 H74B H 0.1978 0.0761 0.9743 0.096 Uiso 0.38 1 calc PR A 2 C75 C 0.1300(15) 0.0706(9) 0.8824(9) 0.107(6) Uiso 0.38 1 d P A 2 H75A H 0.1051 0.1070 0.8863 0.128 Uiso 0.38 1 calc PR A 2 H75B H 0.0687 0.0466 0.8781 0.128 Uiso 0.38 1 calc PR A 2 O5 O 0.2281(8) 0.0768(4) 0.6229(5) 0.088(3) Uiso 0.38 1 d P A 2 C76 C 0.1776(14) 0.0661(8) 0.8281(8) 0.089(5) Uiso 0.38 1 d P A 2 H76A H 0.1502 0.0937 0.7968 0.107 Uiso 0.38 1 calc PR A 2 H76B H 0.1620 0.0314 0.8078 0.107 Uiso 0.38 1 calc PR A 2 C77 C 0.2038(13) 0.0219(7) 0.6423(9) 0.084(5) Uiso 0.38 1 d P A 2 H77A H 0.2485 0.0113 0.6833 0.101 Uiso 0.38 1 calc PR A 2 H77B H 0.2082 -0.0047 0.6097 0.101 Uiso 0.38 1 calc PR A 2 C78 C 0.0880(12) 0.0343(7) 0.6470(7) 0.087(5) Uiso 0.38 1 d P A 2 H78A H 0.0477 0.0017 0.6504 0.104 Uiso 0.38 1 calc PR A 2 H78B H 0.0856 0.0573 0.6833 0.104 Uiso 0.38 1 calc PR A 2 C79 C 0.0473(13) 0.0615(6) 0.5864(7) 0.078(4) Uiso 0.38 1 d P A 2 H79A H -0.0165 0.0825 0.5879 0.094 Uiso 0.38 1 calc PR A 2 H79B H 0.0307 0.0363 0.5509 0.094 Uiso 0.38 1 calc PR A 2 C80 C 0.1402(13) 0.0964(7) 0.5811(8) 0.095(5) Uiso 0.38 1 d P A 2 H80A H 0.1520 0.0957 0.5375 0.114 Uiso 0.38 1 calc PR A 2 H80B H 0.1262 0.1331 0.5920 0.114 Uiso 0.38 1 calc PR A 2 O6 O 0.3893(6) 0.1541(3) 0.5899(3) 0.0361(18) Uiso 0.38 1 d PD A 2 C81 C 0.3937(16) 0.2070(6) 0.5729(10) 0.105(3) Uiso 0.38 1 d PD A 2 H81A H 0.4058 0.2300 0.6105 0.126 Uiso 0.38 1 calc PR A 2 H81B H 0.3278 0.2179 0.5436 0.126 Uiso 0.38 1 calc PR A 2 C82 C 0.4829(15) 0.2084(6) 0.5423(9) 0.100(7) Uiso 0.38 1 d PD A 2 H82A H 0.5506 0.2100 0.5736 0.120 Uiso 0.38 1 calc PR A 2 H82B H 0.4784 0.2389 0.5136 0.120 Uiso 0.38 1 calc PR A 2 C83 C 0.4732(15) 0.1580(5) 0.5064(6) 0.075(5) Uiso 0.38 1 d PD A 2 H83A H 0.5398 0.1478 0.4941 0.089 Uiso 0.38 1 calc PR A 2 H83B H 0.4144 0.1584 0.4690 0.089 Uiso 0.38 1 calc PR A 2 C84 C 0.4489(8) 0.1236(4) 0.5602(4) 0.040(2) Uiso 0.38 1 d PD A 2 H84A H 0.4098 0.0916 0.5432 0.048 Uiso 0.38 1 calc PR A 2 H84B H 0.5151 0.1131 0.5896 0.048 Uiso 0.38 1 calc PR A 2 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 0.0301(3) 0.0321(3) 0.0294(3) 0.0015(2) 0.0075(2) -0.0034(2) Mn2 0.0424(4) 0.0393(3) 0.0352(3) -0.0040(3) 0.0153(3) -0.0100(3) Cl1 0.0414(5) 0.0460(6) 0.0310(4) 0.0025(4) 0.0138(4) 0.0150(4) Cl2 0.0491(12) 0.0406(9) 0.0374(19) -0.0049(12) 0.0267(12) -0.0124(8) I2 0.0370(15) 0.0412(11) 0.0253(18) -0.0037(12) 0.0156(12) -0.0074(9) Cl3 0.0396(17) 0.0629(16) 0.0349(11) -0.0110(8) 0.0054(11) -0.0126(10) I3 0.0396(17) 0.0629(16) 0.0349(11) -0.0110(8) 0.0054(11) -0.0126(10) C1 0.0224(17) 0.0319(19) 0.0257(17) 0.0052(14) 0.0024(14) 0.0065(14) C2 0.0278(19) 0.0301(19) 0.0277(17) 0.0053(15) 0.0037(14) 0.0053(15) C3 0.046(2) 0.029(2) 0.044(2) 0.0069(17) 0.0153(18) 0.0053(17) C4 0.058(3) 0.033(2) 0.048(2) -0.0025(18) 0.019(2) 0.0060(19) C5 0.046(2) 0.040(2) 0.041(2) 0.0000(18) 0.0181(18) 0.0112(19) C6 0.0283(19) 0.038(2) 0.0286(18) 0.0048(16) 0.0047(15) 0.0095(16) C7 0.043(2) 0.0286(19) 0.0304(18) 0.0067(15) 0.0106(16) -0.0026(17) C8 0.046(2) 0.029(2) 0.037(2) 0.0059(16) 0.0133(17) 0.0007(17) C9 0.063(3) 0.042(2) 0.047(2) 0.0009(19) 0.031(2) -0.006(2) C10 0.091(4) 0.070(3) 0.033(2) 0.003(2) 0.028(2) -0.022(3) C11 0.075(3) 0.079(4) 0.033(2) 0.011(2) 0.008(2) -0.028(3) C12 0.053(3) 0.054(3) 0.031(2) 0.0133(18) 0.0044(18) -0.008(2) C13 0.037(2) 0.037(2) 0.048(2) -0.0004(18) 0.0122(18) -0.0001(18) C14 0.044(3) 0.055(3) 0.074(3) 0.015(2) 0.001(2) 0.001(2) C15 0.044(3) 0.059(3) 0.069(3) -0.004(2) 0.019(2) -0.003(2) C16 0.045(3) 0.092(4) 0.045(3) 0.032(3) -0.002(2) -0.005(3) C17 0.066(4) 0.158(6) 0.057(3) 0.046(4) -0.023(3) -0.038(4) C18 0.049(3) 0.113(5) 0.135(6) 0.046(4) 0.011(3) 0.017(3) C19 0.042(2) 0.041(2) 0.034(2) -0.0066(17) 0.0188(17) 0.0005(18) C20 0.041(2) 0.068(3) 0.046(2) -0.012(2) 0.025(2) -0.003(2) C21 0.050(3) 0.095(4) 0.056(3) -0.018(3) 0.027(2) -0.011(3) C22 0.074(4) 0.068(3) 0.082(4) -0.018(3) 0.051(3) -0.023(3) C23 0.092(4) 0.047(3) 0.053(3) 0.004(2) 0.042(3) 0.003(3) C24 0.059(3) 0.040(2) 0.039(2) 0.0003(18) 0.027(2) 0.003(2) C25 0.034(2) 0.109(4) 0.045(2) 0.002(3) 0.011(2) 0.016(3) C26 0.052(3) 0.140(6) 0.080(4) -0.032(4) -0.013(3) 0.034(4) C27 0.059(3) 0.086(4) 0.072(3) 0.003(3) 0.019(3) 0.015(3) C28 0.063(3) 0.048(3) 0.044(2) 0.0146(19) 0.021(2) 0.022(2) C29 0.115(4) 0.058(3) 0.031(2) 0.000(2) 0.009(2) 0.035(3) C30 0.068(3) 0.047(3) 0.088(4) -0.013(3) 0.006(3) 0.015(2) C31 0.043(2) 0.034(2) 0.036(2) -0.0114(16) 0.0194(17) -0.0151(17) C32 0.036(2) 0.034(2) 0.0326(19) -0.0134(16) 0.0141(16) -0.0114(17) C33 0.039(2) 0.041(2) 0.037(2) -0.0115(17) 0.0152(17) -0.0086(18) C34 0.047(2) 0.036(2) 0.056(3) -0.0173(19) 0.027(2) -0.0108(19) C35 0.071(3) 0.036(2) 0.052(2) -0.0142(19) 0.043(2) -0.012(2) C36 0.058(3) 0.030(2) 0.041(2) -0.0115(17) 0.0292(19) -0.0146(19) C37 0.036(2) 0.035(2) 0.0291(18) -0.0028(15) 0.0108(16) -0.0003(17) C38 0.040(2) 0.031(2) 0.0305(18) -0.0036(15) 0.0080(16) 0.0049(17) C39 0.059(3) 0.032(2) 0.0280(19) -0.0041(16) 0.0094(18) 0.0073(19) C40 0.072(3) 0.039(2) 0.034(2) 0.0007(17) 0.030(2) 0.003(2) C41 0.060(3) 0.047(2) 0.041(2) -0.0037(19) 0.029(2) -0.011(2) C42 0.050(2) 0.042(2) 0.0299(19) -0.0040(16) 0.0180(17) -0.0083(19) C43 0.040(2) 0.042(2) 0.046(2) -0.0172(18) 0.0109(18) -0.0044(18) C44 0.058(3) 0.046(3) 0.096(4) -0.007(3) 0.023(3) -0.014(2) C45 0.047(3) 0.087(4) 0.056(3) -0.021(3) 0.003(2) 0.004(3) C46 0.062(3) 0.068(3) 0.039(2) -0.022(2) 0.031(2) -0.032(2) C47 0.065(3) 0.103(4) 0.052(3) -0.021(3) 0.026(2) -0.043(3) C48 0.083(4) 0.058(3) 0.085(4) -0.034(3) 0.051(3) -0.034(3) C49 0.086(3) 0.037(2) 0.059(3) 0.003(2) 0.054(3) -0.002(2) C50 0.116(4) 0.052(3) 0.043(3) 0.002(2) 0.042(3) 0.001(3) C51 0.141(6) 0.064(4) 0.053(3) 0.017(3) 0.053(3) 0.015(3) C52 0.143(6) 0.065(4) 0.086(4) 0.033(3) 0.083(4) 0.032(4) C53 0.131(5) 0.043(3) 0.128(5) 0.016(3) 0.109(5) 0.013(3) C54 0.100(4) 0.040(3) 0.094(4) 0.000(3) 0.079(3) 0.000(3) C55 0.142(6) 0.059(3) 0.029(2) 0.001(2) 0.016(3) -0.012(3) C56 0.152(7) 0.089(5) 0.075(4) -0.028(3) 0.040(4) -0.022(5) C57 0.140(6) 0.059(3) 0.049(3) -0.003(2) 0.007(3) 0.015(3) C58 0.097(4) 0.038(3) 0.127(5) -0.024(3) 0.085(4) -0.023(3) C59 0.092(4) 0.044(3) 0.221(8) -0.026(4) 0.095(5) -0.014(3) C60 0.104(5) 0.048(3) 0.155(6) -0.021(4) 0.072(4) -0.006(3) Cl4 0.0462(16) 0.039(2) 0.0560(14) -0.0259(19) 0.0225(12) -0.0133(17) Cl4B 0.0462(16) 0.039(2) 0.0560(14) -0.0259(19) 0.0225(12) -0.0133(17) _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 C1 2.133(3) . ? Mn1 Cl3 2.452(2) . ? Mn1 Cl1 2.4643(10) . ? Mn1 Cl2 2.524(3) . ? Mn1 I3 2.808(7) . ? Mn1 I2 2.898(4) . ? Mn1 Li3 3.364(18) . ? Mn2 C31 2.132(4) . ? Mn2 Cl4 2.459(6) . ? Mn2 Cl4B 2.461(10) . ? Mn2 Cl1 2.4932(10) . ? Mn2 Cl2 2.527(5) . ? Mn2 I2 2.666(5) . ? Mn2 Li3 3.232(18) . ? Mn2 Li1 3.328(11) . ? Cl1 Li3 2.515(18) . ? Cl2 Li1 2.386(12) . ? Cl3 Li2 2.318(11) . ? Cl3 Li1 2.373(11) . ? I3 Li4 2.53(2) . ? I3 Li3 2.72(2) . ? C1 C2 1.413(5) . ? C1 C6 1.423(5) . ? C2 C3 1.391(5) . ? C2 C7 1.503(5) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.380(6) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 C19 1.500(5) . ? C7 C8 1.401(5) . ? C7 C12 1.416(5) . ? C8 C9 1.397(5) . ? C8 C13 1.525(5) . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 C11 1.371(7) . ? C10 H10 0.9500 . ? C11 C12 1.392(6) . ? C11 H11 0.9500 . ? C12 C16 1.511(6) . ? C13 C15 1.522(6) . ? C13 C14 1.522(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.516(7) . ? C16 C18 1.519(8) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.389(5) . ? C19 C20 1.419(6) . ? C20 C21 1.389(6) . ? C20 C25 1.527(6) . ? C21 C22 1.352(7) . ? C21 H21 0.9500 . ? C22 C23 1.377(7) . ? C22 H22 0.9500 . ? C23 C24 1.417(6) . ? C23 H23 0.9500 . ? C24 C28 1.502(6) . ? C25 C26 1.521(7) . ? C25 C27 1.523(7) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.528(6) . ? C28 C29 1.530(6) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.417(5) . ? C31 C32 1.418(5) . ? C32 C33 1.380(5) . ? C32 C37 1.511(5) . ? C33 C34 1.396(5) . ? C33 H33 0.9500 . ? C34 C35 1.375(6) . ? C34 H34 0.9500 . ? C35 C36 1.401(6) . ? C35 H35 0.9500 . ? C36 C49 1.497(6) . ? C37 C42 1.401(5) . ? C37 C38 1.402(5) . ? C38 C39 1.398(5) . ? C38 C43 1.518(5) . ? C39 C40 1.364(6) . ? C39 H39 0.9500 . ? C40 C41 1.375(6) . ? C40 H40 0.9500 . ? C41 C42 1.402(5) . ? C41 H41 0.9500 . ? C42 C46 1.523(5) . ? C43 C44 1.518(6) . ? C43 C45 1.528(6) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.521(7) . ? C46 C47 1.527(6) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.414(7) . ? C49 C54 1.418(6) . ? C50 C51 1.394(6) . ? C50 C55 1.525(7) . ? C51 C52 1.362(8) . ? C51 H51 0.9500 . ? C52 C53 1.378(9) . ? C52 H52 0.9500 . ? C53 C54 1.384(7) . ? C53 H53 0.9500 . ? C54 C58 1.528(8) . ? C55 C56 1.533(9) . ? C55 C57 1.537(7) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C60 1.517(8) . ? C58 C59 1.528(7) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? Li1 O1 1.883(12) . ? Li1 Cl4 2.348(11) . ? Li2 O2 1.871(11) . ? Li2 O3 1.952(11) . ? Li2 Cl4 2.431(11) . ? O1 C64 1.313(12) . ? O1 C61 1.427(10) . ? C61 C62 1.473(11) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.483(12) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.616(13) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? O2 C65 1.423(8) . ? O2 C68 1.432(8) . ? C65 C66 1.439(9) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.549(11) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.506(11) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? O3 C72 1.397(7) . ? O3 C69 1.407(7) . ? C69 C70 1.552(9) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.473(9) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.549(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? Li3 O4 1.821(19) . ? Li3 Cl4B 2.461(19) . ? Li3 Li4 3.10(3) . ? Li4 O5 1.95(2) . ? Li4 O6 1.97(2) . ? Li4 Cl4B 2.30(2) . ? O4 C73 1.436(15) . ? O4 C76 1.500(19) . ? C73 C74 1.52(2) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.43(2) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.44(2) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? O5 C80 1.389(18) . ? O5 C77 1.515(19) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.56(2) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.48(2) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.52(2) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? O6 C84 1.350(10) . ? O6 C81 1.402(14) . ? C81 C82 1.450(14) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.492(14) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.543(13) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? 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 Mn1 Cl3 119.89(14) . . ? C1 Mn1 Cl1 120.71(9) . . ? Cl3 Mn1 Cl1 101.00(11) . . ? C1 Mn1 Cl2 127.35(15) . . ? Cl3 Mn1 Cl2 94.95(17) . . ? Cl1 Mn1 Cl2 85.00(11) . . ? C1 Mn1 I3 121.2(3) . . ? Cl3 Mn1 I3 1.6(4) . . ? Cl1 Mn1 I3 99.4(3) . . ? Cl2 Mn1 I3 94.6(3) . . ? C1 Mn1 I2 125.93(15) . . ? Cl3 Mn1 I2 94.26(16) . . ? Cl1 Mn1 I2 87.67(11) . . ? Cl2 Mn1 I2 2.7(2) . . ? I3 Mn1 I2 93.9(3) . . ? C1 Mn1 Li3 143.0(3) . . ? Cl3 Mn1 Li3 52.9(3) . . ? Cl1 Mn1 Li3 48.1(3) . . ? Cl2 Mn1 Li3 89.2(3) . . ? I3 Mn1 Li3 51.3(4) . . ? I2 Mn1 Li3 90.8(3) . . ? C31 Mn2 Cl4 116.00(12) . . ? C31 Mn2 Cl4B 106.06(17) . . ? Cl4 Mn2 Cl4B 11.17(19) . . ? C31 Mn2 Cl1 128.08(10) . . ? Cl4 Mn2 Cl1 95.46(12) . . ? Cl4B Mn2 Cl1 99.0(2) . . ? C31 Mn2 Cl2 131.90(13) . . ? Cl4 Mn2 Cl2 90.39(15) . . ? Cl4B Mn2 Cl2 101.3(2) . . ? Cl1 Mn2 Cl2 84.33(7) . . ? C31 Mn2 I2 125.07(14) . . ? Cl4 Mn2 I2 90.61(16) . . ? Cl4B Mn2 I2 101.0(2) . . ? Cl1 Mn2 I2 92.43(9) . . ? Cl2 Mn2 I2 8.16(13) . . ? C31 Mn2 Li3 135.4(3) . . ? Cl4 Mn2 Li3 45.9(3) . . ? Cl4B Mn2 Li3 49.0(4) . . ? Cl1 Mn2 Li3 50.1(3) . . ? Cl2 Mn2 Li3 92.1(3) . . ? I2 Mn2 Li3 98.1(3) . . ? C31 Mn2 Li1 142.6(2) . . ? Cl4 Mn2 Li1 44.8(2) . . ? Cl4B Mn2 Li1 55.8(2) . . ? Cl1 Mn2 Li1 88.92(18) . . ? Cl2 Mn2 Li1 45.6(2) . . ? I2 Mn2 Li1 46.6(2) . . ? Li3 Mn2 Li1 61.1(4) . . ? Mn1 Cl1 Mn2 94.91(3) . . ? Mn1 Cl1 Li3 85.0(4) . . ? Mn2 Cl1 Li3 80.4(4) . . ? Li1 Cl2 Mn1 81.2(3) . . ? Li1 Cl2 Mn2 85.2(3) . . ? Mn1 Cl2 Mn2 92.62(11) . . ? Mn2 I2 Mn1 81.95(10) . . ? Li2 Cl3 Li1 81.2(4) . . ? Li2 Cl3 Mn1 115.3(3) . . ? Li1 Cl3 Mn1 82.9(3) . . ? Li4 I3 Li3 72.4(7) . . ? Li4 I3 Mn1 101.4(6) . . ? Li3 I3 Mn1 75.0(5) . . ? C2 C1 C6 115.6(3) . . ? C2 C1 Mn1 118.5(2) . . ? C6 C1 Mn1 125.8(3) . . ? C3 C2 C1 122.0(3) . . ? C3 C2 C7 117.8(3) . . ? C1 C2 C7 120.1(3) . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 121.4(3) . . ? C5 C6 C19 115.9(3) . . ? C1 C6 C19 122.3(3) . . ? C8 C7 C12 120.3(3) . . ? C8 C7 C2 121.0(3) . . ? C12 C7 C2 118.6(3) . . ? C9 C8 C7 118.7(4) . . ? C9 C8 C13 121.2(4) . . ? C7 C8 C13 120.1(3) . . ? C10 C9 C8 121.3(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 121.7(4) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 118.2(4) . . ? C11 C12 C16 119.9(4) . . ? C7 C12 C16 121.8(3) . . ? C15 C13 C14 112.6(4) . . ? C15 C13 C8 112.9(3) . . ? C14 C13 C8 111.1(3) . . ? C15 C13 H13 106.6 . . ? C14 C13 H13 106.6 . . ? C8 C13 H13 106.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C17 115.4(5) . . ? C12 C16 C18 109.0(4) . . ? C17 C16 C18 109.8(5) . . ? C12 C16 H16 107.4 . . ? C17 C16 H16 107.4 . . ? C18 C16 H16 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 121.3(4) . . ? C24 C19 C6 121.6(4) . . ? C20 C19 C6 116.8(3) . . ? C21 C20 C19 118.2(4) . . ? C21 C20 C25 119.8(4) . . ? C19 C20 C25 121.8(4) . . ? C22 C21 C20 121.2(5) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 121.0(4) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C24 120.7(4) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C19 C24 C23 117.5(4) . . ? C19 C24 C28 121.6(4) . . ? C23 C24 C28 120.8(4) . . ? C26 C25 C27 110.3(4) . . ? C26 C25 C20 113.1(5) . . ? C27 C25 C20 111.4(4) . . ? C26 C25 H25 107.2 . . ? C27 C25 H25 107.2 . . ? C20 C25 H25 107.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C30 112.1(3) . . ? C24 C28 C29 113.4(4) . . ? C30 C28 C29 109.2(4) . . ? C24 C28 H28 107.3 . . ? C30 C28 H28 107.3 . . ? C29 C28 H28 107.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 115.6(4) . . ? C36 C31 Mn2 124.7(3) . . ? C32 C31 Mn2 119.5(2) . . ? C33 C32 C31 123.0(3) . . ? C33 C32 C37 118.6(3) . . ? C31 C32 C37 118.4(3) . . ? C32 C33 C34 120.0(4) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 118.7(4) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 121.8(3) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C35 C36 C31 120.7(4) . . ? C35 C36 C49 117.1(3) . . ? C31 C36 C49 122.2(4) . . ? C42 C37 C38 120.6(3) . . ? C42 C37 C32 120.5(3) . . ? C38 C37 C32 118.9(3) . . ? C39 C38 C37 118.5(3) . . ? C39 C38 C43 119.2(3) . . ? C37 C38 C43 122.2(3) . . ? C40 C39 C38 121.1(4) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C42 120.8(4) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C37 118.4(3) . . ? C41 C42 C46 119.8(3) . . ? C37 C42 C46 121.7(3) . . ? C44 C43 C38 111.7(3) . . ? C44 C43 C45 110.5(4) . . ? C38 C43 C45 110.2(4) . . ? C44 C43 H43 108.1 . . ? C38 C43 H43 108.1 . . ? C45 C43 H43 108.1 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 C48 109.8(4) . . ? C42 C46 C47 114.3(4) . . ? C48 C46 C47 109.3(4) . . ? C42 C46 H46 107.7 . . ? C48 C46 H46 107.7 . . ? C47 C46 H46 107.7 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C54 119.9(4) . . ? C50 C49 C36 119.9(4) . . ? C54 C49 C36 120.1(4) . . ? C51 C50 C49 118.5(5) . . ? C51 C50 C55 119.4(5) . . ? C49 C50 C55 122.1(4) . . ? C52 C51 C50 121.3(6) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 120.5(5) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C52 C53 C54 121.2(5) . . ? C52 C53 H53 119.4 . . ? C54 C53 H53 119.4 . . ? C53 C54 C49 118.6(5) . . ? C53 C54 C58 120.5(5) . . ? C49 C54 C58 120.9(5) . . ? C50 C55 C56 111.8(5) . . ? C50 C55 C57 110.9(5) . . ? C56 C55 C57 110.3(5) . . ? C50 C55 H55 107.9 . . ? C56 C55 H55 107.9 . . ? C57 C55 H55 107.9 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C60 C58 C54 111.5(4) . . ? C60 C58 C59 108.9(4) . . ? C54 C58 C59 113.2(6) . . ? C60 C58 H58 107.7 . . ? C54 C58 H58 107.7 . . ? C59 C58 H58 107.7 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O1 Li1 Cl4 121.2(6) . . ? O1 Li1 Cl3 119.5(6) . . ? Cl4 Li1 Cl3 96.1(4) . . ? O1 Li1 Cl2 117.7(5) . . ? Cl4 Li1 Cl2 96.7(4) . . ? Cl3 Li1 Cl2 100.8(4) . . ? O1 Li1 Mn2 138.9(5) . . ? Cl4 Li1 Mn2 47.6(2) . . ? Cl3 Li1 Mn2 101.7(3) . . ? Cl2 Li1 Mn2 49.2(2) . . ? O2 Li2 O3 108.8(5) . . ? O2 Li2 Cl3 113.5(5) . . ? O3 Li2 Cl3 117.3(5) . . ? O2 Li2 Cl4 123.3(5) . . ? O3 Li2 Cl4 97.9(4) . . ? Cl3 Li2 Cl4 95.3(4) . . ? Li1 Cl4 Li2 79.4(4) . . ? Li1 Cl4 Mn2 87.6(3) . . ? Li2 Cl4 Mn2 119.9(3) . . ? C64 O1 C61 101.7(9) . . ? C64 O1 Li1 131.2(9) . . ? C61 O1 Li1 123.6(8) . . ? O1 C61 C62 105.4(8) . . ? O1 C61 H61A 110.7 . . ? C62 C61 H61A 110.7 . . ? O1 C61 H61B 110.7 . . ? C62 C61 H61B 110.7 . . ? H61A C61 H61B 108.8 . . ? C61 C62 C63 103.1(8) . . ? C61 C62 H62A 111.1 . . ? C63 C62 H62A 111.1 . . ? C61 C62 H62B 111.1 . . ? C63 C62 H62B 111.1 . . ? H62A C62 H62B 109.1 . . ? C62 C63 C64 100.8(8) . . ? C62 C63 H63A 111.6 . . ? C64 C63 H63A 111.6 . . ? C62 C63 H63B 111.6 . . ? C64 C63 H63B 111.6 . . ? H63A C63 H63B 109.4 . . ? O1 C64 C63 103.7(9) . . ? O1 C64 H64A 111.0 . . ? C63 C64 H64A 111.0 . . ? O1 C64 H64B 111.0 . . ? C63 C64 H64B 111.0 . . ? H64A C64 H64B 109.0 . . ? C65 O2 C68 108.1(5) . . ? C65 O2 Li2 124.1(5) . . ? C68 O2 Li2 127.8(5) . . ? O2 C65 C66 110.5(6) . . ? O2 C65 H65A 109.5 . . ? C66 C65 H65A 109.5 . . ? O2 C65 H65B 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 108.1 . . ? C65 C66 C67 103.8(6) . . ? C65 C66 H66A 111.0 . . ? C67 C66 H66A 111.0 . . ? C65 C66 H66B 111.0 . . ? C67 C66 H66B 111.0 . . ? H66A C66 H66B 109.0 . . ? C68 C67 C66 103.6(6) . . ? C68 C67 H67A 111.0 . . ? C66 C67 H67A 111.0 . . ? C68 C67 H67B 111.0 . . ? C66 C67 H67B 111.0 . . ? H67A C67 H67B 109.0 . . ? O2 C68 C67 108.5(6) . . ? O2 C68 H68A 110.0 . . ? C67 C68 H68A 110.0 . . ? O2 C68 H68B 110.0 . . ? C67 C68 H68B 110.0 . . ? H68A C68 H68B 108.4 . . ? C72 O3 C69 109.1(5) . . ? C72 O3 Li2 119.2(5) . . ? C69 O3 Li2 125.9(5) . . ? O3 C69 C70 106.5(5) . . ? O3 C69 H69A 110.4 . . ? C70 C69 H69A 110.4 . . ? O3 C69 H69B 110.4 . . ? C70 C69 H69B 110.4 . . ? H69A C69 H69B 108.6 . . ? C71 C70 C69 104.0(5) . . ? C71 C70 H70A 110.9 . . ? C69 C70 H70A 110.9 . . ? C71 C70 H70B 110.9 . . ? C69 C70 H70B 110.9 . . ? H70A C70 H70B 109.0 . . ? C70 C71 C72 101.3(5) . . ? C70 C71 H71A 111.5 . . ? C72 C71 H71A 111.5 . . ? C70 C71 H71B 111.5 . . ? C72 C71 H71B 111.5 . . ? H71A C71 H71B 109.3 . . ? O3 C72 C71 104.0(5) . . ? O3 C72 H72A 111.0 . . ? C71 C72 H72A 111.0 . . ? O3 C72 H72B 111.0 . . ? C71 C72 H72B 111.0 . . ? H72A C72 H72B 109.0 . . ? O4 Li3 Cl4B 125.7(9) . . ? O4 Li3 Cl1 119.6(8) . . ? Cl4B Li3 Cl1 98.4(7) . . ? O4 Li3 I3 110.5(8) . . ? Cl4B Li3 I3 97.4(6) . . ? Cl1 Li3 I3 100.6(6) . . ? O4 Li3 Li4 129.5(9) . . ? Cl4B Li3 Li4 47.0(5) . . ? Cl1 Li3 Li4 110.5(7) . . ? I3 Li3 Li4 51.0(6) . . ? O4 Li3 Mn2 147.8(9) . . ? Cl4B Li3 Mn2 48.9(4) . . ? Cl1 Li3 Mn2 49.5(3) . . ? I3 Li3 Mn2 101.6(6) . . ? Li4 Li3 Mn2 73.5(5) . . ? O4 Li3 Mn1 132.0(8) . . ? Cl4B Li3 Mn1 102.1(6) . . ? Cl1 Li3 Mn1 46.9(3) . . ? I3 Li3 Mn1 53.7(3) . . ? Li4 Li3 Mn1 79.4(6) . . ? Mn2 Li3 Mn1 67.2(3) . . ? O5 Li4 O6 102.9(10) . . ? O5 Li4 Cl4B 101.4(10) . . ? O6 Li4 Cl4B 119.1(11) . . ? O5 Li4 I3 107.3(10) . . ? O6 Li4 I3 116.8(10) . . ? Cl4B Li4 I3 107.5(9) . . ? O5 Li4 Li3 107.3(9) . . ? O6 Li4 Li3 149.7(11) . . ? Cl4B Li4 Li3 51.6(6) . . ? I3 Li4 Li3 56.6(6) . . ? Li4 Cl4B Li3 81.4(7) . . ? Li4 Cl4B Mn2 105.7(6) . . ? Li3 Cl4B Mn2 82.1(5) . . ? C73 O4 C76 107.6(10) . . ? C73 O4 Li3 124.2(10) . . ? C76 O4 Li3 122.5(10) . . ? O4 C73 C74 105.8(12) . . ? O4 C73 H73A 110.6 . . ? C74 C73 H73A 110.6 . . ? O4 C73 H73B 110.6 . . ? C74 C73 H73B 110.6 . . ? H73A C73 H73B 108.7 . . ? C75 C74 C73 104.8(14) . . ? C75 C74 H74A 110.8 . . ? C73 C74 H74A 110.8 . . ? C75 C74 H74B 110.8 . . ? C73 C74 H74B 110.8 . . ? H74A C74 H74B 108.9 . . ? C74 C75 C76 107.3(16) . . ? C74 C75 H75A 110.3 . . ? C76 C75 H75A 110.3 . . ? C74 C75 H75B 110.3 . . ? C76 C75 H75B 110.3 . . ? H75A C75 H75B 108.5 . . ? C80 O5 C77 108.9(12) . . ? C80 O5 Li4 121.9(12) . . ? C77 O5 Li4 127.5(12) . . ? C75 C76 O4 105.9(13) . . ? C75 C76 H76A 110.6 . . ? O4 C76 H76A 110.6 . . ? C75 C76 H76B 110.6 . . ? O4 C76 H76B 110.6 . . ? H76A C76 H76B 108.7 . . ? O5 C77 C78 95.1(12) . . ? O5 C77 H77A 112.7 . . ? C78 C77 H77A 112.7 . . ? O5 C77 H77B 112.7 . . ? C78 C77 H77B 112.7 . . ? H77A C77 H77B 110.2 . . ? C79 C78 C77 101.8(13) . . ? C79 C78 H78A 111.4 . . ? C77 C78 H78A 111.4 . . ? C79 C78 H78B 111.4 . . ? C77 C78 H78B 111.4 . . ? H78A C78 H78B 109.3 . . ? C78 C79 C80 101.7(13) . . ? C78 C79 H79A 111.4 . . ? C80 C79 H79A 111.4 . . ? C78 C79 H79B 111.4 . . ? C80 C79 H79B 111.4 . . ? H79A C79 H79B 109.3 . . ? O5 C80 C79 107.0(14) . . ? O5 C80 H80A 110.3 . . ? C79 C80 H80A 110.3 . . ? O5 C80 H80B 110.3 . . ? C79 C80 H80B 110.3 . . ? H80A C80 H80B 108.6 . . ? C84 O6 C81 111.6(9) . . ? C84 O6 Li4 115.9(9) . . ? C81 O6 Li4 130.2(11) . . ? O6 C81 C82 103.0(11) . . ? O6 C81 H81A 111.2 . . ? C82 C81 H81A 111.2 . . ? O6 C81 H81B 111.2 . . ? C82 C81 H81B 111.2 . . ? H81A C81 H81B 109.1 . . ? C81 C82 C83 103.3(12) . . ? C81 C82 H82A 111.1 . . ? C83 C82 H82A 111.1 . . ? C81 C82 H82B 111.1 . . ? C83 C82 H82B 111.1 . . ? H82A C82 H82B 109.1 . . ? C82 C83 C84 95.8(10) . . ? C82 C83 H83A 112.6 . . ? C84 C83 H83A 112.6 . . ? C82 C83 H83B 112.6 . . ? C84 C83 H83B 112.6 . . ? H83A C83 H83B 110.1 . . ? O6 C84 C83 105.2(8) . . ? O6 C84 H84A 110.7 . . ? C83 C84 H84A 110.7 . . ? O6 C84 H84B 110.7 . . ? C83 C84 H84B 110.7 . . ? H84A C84 H84B 108.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.774 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.075 #===END data_c2c _database_code_depnum_ccdc_archive 'CCDC 794077' #TrackingRef 'CIF-Mn-010510.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H74 Mn' _chemical_formula_sum 'C60 H74 Mn' _chemical_formula_weight 850.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.5603(17) _cell_length_b 15.8913(19) _cell_length_c 19.946(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.953(2) _cell_angle_gamma 90.00 _cell_volume 4925.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6843 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 0.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9500 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details 'SADABS 2007/3 (Sheldrick, 2007)' _exptl_special_details ; A colorless plate with approximate orthogonal dimensions 0.17 x 0.13 x 0.09mm3 was placed and optically centered on the Bruker SMART1000(1) CCD system at 90(2)K. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide Omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 30 seconds per frame and 606 frames were collected, at varying phi angles (phi=0? 90? 180? 270?, for each series. The crystal to detector distance was 4.28cm, thus providing a complete sphere of data with processing to 2ThetaMax=55.21? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX SMART 1000 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29350 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5685 _reflns_number_gt 4147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 SMART1000' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. References: 1. Bruker (2007) APEX (Version 2.0.2) and SAINT (Version 7.46A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008/1) Version 2.10, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. ; _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^)+(0.0368P)^2^+6.1097P] 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 5685 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.0000 0.25138(2) 0.2500 0.01695(10) Uani 1 2 d S . . C1 C 0.07684(10) 0.22851(10) 0.33856(8) 0.0148(3) Uani 1 1 d . . . C2 C 0.16102(11) 0.26128(10) 0.33487(8) 0.0164(3) Uani 1 1 d . . . C3 C 0.22855(11) 0.23628(11) 0.37923(9) 0.0199(4) Uani 1 1 d . . . H3A H 0.2841 0.2602 0.3757 0.024 Uiso 1 1 calc R . . C4 C 0.21492(11) 0.17698(11) 0.42816(8) 0.0206(4) Uani 1 1 d . . . H4A H 0.2617 0.1566 0.4561 0.025 Uiso 1 1 calc R . . C5 C 0.13236(11) 0.14765(11) 0.43600(8) 0.0190(4) Uani 1 1 d . . . H5A H 0.1223 0.1086 0.4708 0.023 Uiso 1 1 calc R . . C6 C 0.06340(10) 0.17458(10) 0.39354(8) 0.0152(3) Uani 1 1 d . . . C7 C 0.17825(11) 0.32933(11) 0.28497(8) 0.0172(3) Uani 1 1 d . . . C8 C 0.23383(11) 0.31394(11) 0.23259(8) 0.0204(4) Uani 1 1 d . . . C9 C 0.24956(12) 0.37856(12) 0.18749(9) 0.0238(4) Uani 1 1 d . . . H9A H 0.2851 0.3680 0.1511 0.029 Uiso 1 1 calc R . . C10 C 0.21443(12) 0.45753(12) 0.19491(9) 0.0245(4) Uani 1 1 d . . . H10A H 0.2254 0.5007 0.1636 0.029 Uiso 1 1 calc R . . C11 C 0.16303(11) 0.47365(12) 0.24829(9) 0.0216(4) Uani 1 1 d . . . H11A H 0.1407 0.5287 0.2539 0.026 Uiso 1 1 calc R . . C12 C 0.14358(11) 0.41107(11) 0.29371(8) 0.0181(3) Uani 1 1 d . . . C13 C 0.27923(12) 0.22961(11) 0.22528(9) 0.0225(4) Uani 1 1 d . . . H13A H 0.2560 0.1899 0.2588 0.027 Uiso 1 1 calc R . . C14 C 0.26130(13) 0.19205(13) 0.15589(9) 0.0286(4) Uani 1 1 d . . . H14A H 0.1990 0.1895 0.1460 0.043 Uiso 1 1 calc R . . H14B H 0.2854 0.1352 0.1546 0.043 Uiso 1 1 calc R . . H14C H 0.2879 0.2273 0.1223 0.043 Uiso 1 1 calc R . . C15 C 0.37689(12) 0.23796(13) 0.24097(10) 0.0280(4) Uani 1 1 d . . . H15A H 0.4040 0.1825 0.2381 0.042 Uiso 1 1 calc R . . H15B H 0.3873 0.2607 0.2863 0.042 Uiso 1 1 calc R . . H15C H 0.4015 0.2760 0.2084 0.042 Uiso 1 1 calc R . . C16 C 0.09225(11) 0.43154(11) 0.35498(8) 0.0192(4) Uani 1 1 d . . . H16A H 0.0532 0.3828 0.3624 0.023 Uiso 1 1 calc R . . C17 C 0.15259(12) 0.44015(12) 0.41785(9) 0.0259(4) Uani 1 1 d . . . H17A H 0.1184 0.4475 0.4574 0.039 Uiso 1 1 calc R . . H17B H 0.1900 0.4892 0.4131 0.039 Uiso 1 1 calc R . . H17C H 0.1879 0.3893 0.4233 0.039 Uiso 1 1 calc R . . C18 C 0.03636(12) 0.51025(12) 0.34788(10) 0.0267(4) Uani 1 1 d . . . H18A H 0.0000 0.5067 0.3064 0.040 Uiso 1 1 calc R . . H18B H 0.0733 0.5601 0.3463 0.040 Uiso 1 1 calc R . . H18C H -0.0001 0.5145 0.3864 0.040 Uiso 1 1 calc R . . C19 C -0.02403(10) 0.15218(11) 0.41739(8) 0.0163(3) Uani 1 1 d . . . C20 C -0.06362(11) 0.07451(11) 0.40200(8) 0.0176(3) Uani 1 1 d . . . C21 C -0.13610(11) 0.05081(12) 0.43593(9) 0.0224(4) Uani 1 1 d . . . H21A H -0.1619 -0.0025 0.4270 0.027 Uiso 1 1 calc R . . C22 C -0.17083(11) 0.10368(13) 0.48221(9) 0.0249(4) Uani 1 1 d . . . H22A H -0.2197 0.0865 0.5053 0.030 Uiso 1 1 calc R . . C23 C -0.13442(11) 0.18166(12) 0.49490(9) 0.0228(4) Uani 1 1 d . . . H23A H -0.1603 0.2188 0.5253 0.027 Uiso 1 1 calc R . . C24 C -0.06031(11) 0.20670(11) 0.46386(8) 0.0179(3) Uani 1 1 d . . . C25 C -0.02967(11) 0.01573(11) 0.34979(8) 0.0199(4) Uani 1 1 d . . . H25A H 0.0180 0.0451 0.3274 0.024 Uiso 1 1 calc R . . C26 C 0.00654(19) -0.06382(15) 0.38220(12) 0.0498(7) Uani 1 1 d . . . H26A H 0.0537 -0.0492 0.4146 0.075 Uiso 1 1 calc R . . H26B H 0.0283 -0.1008 0.3476 0.075 Uiso 1 1 calc R . . H26C H -0.0389 -0.0929 0.4054 0.075 Uiso 1 1 calc R . . C27 C -0.09982(13) -0.00583(15) 0.29609(10) 0.0362(5) Uani 1 1 d . . . H27A H -0.1216 0.0461 0.2748 0.054 Uiso 1 1 calc R . . H27B H -0.1471 -0.0351 0.3169 0.054 Uiso 1 1 calc R . . H27C H -0.0758 -0.0423 0.2621 0.054 Uiso 1 1 calc R . . C28 C -0.01875(11) 0.29056(11) 0.48314(8) 0.0208(4) Uani 1 1 d . . . H28A H 0.0279 0.3012 0.4516 0.025 Uiso 1 1 calc R . . C29 C 0.02299(13) 0.28738(13) 0.55407(9) 0.0281(4) Uani 1 1 d . . . H29A H 0.0655 0.2418 0.5570 0.042 Uiso 1 1 calc R . . H29B H -0.0213 0.2771 0.5863 0.042 Uiso 1 1 calc R . . H29C H 0.0516 0.3411 0.5644 0.042 Uiso 1 1 calc R . . C30 C -0.08236(14) 0.36387(13) 0.47616(10) 0.0321(5) Uani 1 1 d . . . H30A H -0.1092 0.3644 0.4306 0.048 Uiso 1 1 calc R . . H30B H -0.0517 0.4170 0.4846 0.048 Uiso 1 1 calc R . . H30C H -0.1269 0.3572 0.5087 0.048 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 0.01947(19) 0.01897(19) 0.01218(17) 0.000 -0.00138(13) 0.000 C1 0.0161(8) 0.0161(8) 0.0123(7) -0.0029(6) 0.0009(6) 0.0012(6) C2 0.0192(8) 0.0179(9) 0.0125(7) -0.0035(6) 0.0029(6) -0.0010(7) C3 0.0151(8) 0.0245(10) 0.0202(8) -0.0027(7) 0.0028(7) -0.0018(7) C4 0.0165(8) 0.0268(9) 0.0183(8) 0.0020(7) -0.0012(7) 0.0036(7) C5 0.0201(9) 0.0220(9) 0.0149(8) 0.0023(7) 0.0030(7) 0.0017(7) C6 0.0169(8) 0.0149(8) 0.0139(8) -0.0034(6) 0.0021(6) 0.0003(6) C7 0.0161(8) 0.0204(9) 0.0150(8) -0.0008(7) 0.0000(6) -0.0046(7) C8 0.0210(9) 0.0215(9) 0.0188(8) -0.0016(7) 0.0027(7) -0.0047(7) C9 0.0254(10) 0.0288(10) 0.0177(9) 0.0008(7) 0.0047(7) -0.0051(8) C10 0.0268(10) 0.0259(10) 0.0205(9) 0.0063(7) -0.0007(7) -0.0049(8) C11 0.0210(9) 0.0216(9) 0.0219(9) 0.0011(7) -0.0018(7) -0.0008(7) C12 0.0151(8) 0.0210(9) 0.0177(8) -0.0006(7) -0.0023(7) -0.0021(7) C13 0.0235(9) 0.0243(10) 0.0200(9) -0.0009(7) 0.0050(7) -0.0033(7) C14 0.0324(11) 0.0313(11) 0.0225(9) -0.0051(8) 0.0047(8) -0.0026(8) C15 0.0224(9) 0.0306(11) 0.0307(10) -0.0028(8) -0.0006(8) -0.0007(8) C16 0.0189(9) 0.0196(9) 0.0191(8) -0.0031(7) 0.0012(7) -0.0010(7) C17 0.0283(10) 0.0286(10) 0.0205(9) -0.0053(8) -0.0008(8) 0.0036(8) C18 0.0248(10) 0.0266(10) 0.0286(10) -0.0031(8) 0.0010(8) 0.0040(8) C19 0.0159(8) 0.0206(9) 0.0125(8) 0.0023(6) 0.0006(6) 0.0017(7) C20 0.0155(8) 0.0217(9) 0.0155(8) 0.0022(7) -0.0005(6) 0.0005(7) C21 0.0181(9) 0.0263(9) 0.0227(9) 0.0018(7) 0.0005(7) -0.0041(7) C22 0.0171(9) 0.0379(11) 0.0201(9) 0.0030(8) 0.0036(7) -0.0032(8) C23 0.0181(9) 0.0341(10) 0.0165(8) -0.0023(8) 0.0029(7) 0.0036(8) C24 0.0161(8) 0.0235(9) 0.0140(8) 0.0019(7) -0.0001(6) 0.0014(7) C25 0.0207(9) 0.0196(9) 0.0194(8) -0.0005(7) 0.0021(7) -0.0019(7) C26 0.0811(19) 0.0367(13) 0.0321(12) 0.0026(10) 0.0070(12) 0.0280(13) C27 0.0293(11) 0.0545(14) 0.0252(10) -0.0126(10) 0.0039(8) -0.0083(10) C28 0.0218(9) 0.0235(9) 0.0174(8) -0.0044(7) 0.0046(7) 0.0019(7) C29 0.0309(10) 0.0288(10) 0.0240(10) -0.0047(8) -0.0031(8) -0.0005(8) C30 0.0370(12) 0.0285(11) 0.0308(10) -0.0013(8) 0.0008(9) 0.0078(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 C1 2.1128(16) 2 ? Mn1 C1 2.1129(16) . ? C1 C2 1.415(2) . ? C1 C6 1.416(2) . ? C2 C3 1.396(2) . ? C2 C7 1.503(2) . ? C3 C4 1.381(2) . ? C3 H3A 0.9500 . ? C4 C5 1.383(2) . ? C4 H4A 0.9500 . ? C5 C6 1.399(2) . ? C5 H5A 0.9500 . ? C6 C19 1.507(2) . ? C7 C8 1.412(2) . ? C7 C12 1.421(2) . ? C8 C9 1.395(2) . ? C8 C13 1.525(3) . ? C9 C10 1.380(3) . ? C9 H9A 0.9500 . ? C10 C11 1.388(3) . ? C10 H10A 0.9500 . ? C11 C12 1.389(2) . ? C11 H11A 0.9500 . ? C12 C16 1.529(2) . ? C13 C14 1.520(2) . ? C13 C15 1.541(3) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.526(2) . ? C16 C17 1.533(2) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.406(2) . ? C19 C24 1.408(2) . ? C20 C21 1.397(2) . ? C20 C25 1.514(2) . ? C21 C22 1.379(3) . ? C21 H21A 0.9500 . ? C22 C23 1.381(3) . ? C22 H22A 0.9500 . ? C23 C24 1.395(2) . ? C23 H23A 0.9500 . ? C24 C28 1.522(2) . ? C25 C26 1.515(3) . ? C25 C27 1.528(3) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.527(2) . ? C28 C30 1.530(3) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mn1 C1 160.19(9) 2 . ? C2 C1 C6 115.92(14) . . ? C2 C1 Mn1 112.26(11) . . ? C6 C1 Mn1 130.68(12) . . ? C3 C2 C1 122.06(15) . . ? C3 C2 C7 118.05(15) . . ? C1 C2 C7 119.76(14) . . ? C4 C3 C2 120.28(16) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 119.16(16) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C4 C5 C6 121.08(16) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 120.98(15) . . ? C5 C6 C19 114.42(14) . . ? C1 C6 C19 124.00(14) . . ? C8 C7 C12 120.03(15) . . ? C8 C7 C2 120.16(15) . . ? C12 C7 C2 119.65(15) . . ? C9 C8 C7 118.96(17) . . ? C9 C8 C13 119.18(16) . . ? C7 C8 C13 121.84(15) . . ? C10 C9 C8 121.11(17) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C11 119.82(17) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C10 C11 C12 121.45(17) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C11 C12 C7 118.53(16) . . ? C11 C12 C16 120.62(16) . . ? C7 C12 C16 120.66(15) . . ? C14 C13 C8 111.58(15) . . ? C14 C13 C15 110.58(15) . . ? C8 C13 C15 111.20(15) . . ? C14 C13 H13A 107.8 . . ? C8 C13 H13A 107.8 . . ? C15 C13 H13A 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C12 114.77(15) . . ? C18 C16 C17 108.96(14) . . ? C12 C16 C17 110.46(14) . . ? C18 C16 H16A 107.5 . . ? C12 C16 H16A 107.5 . . ? C17 C16 H16A 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 119.85(15) . . ? C20 C19 C6 122.07(15) . . ? C24 C19 C6 117.49(15) . . ? C21 C20 C19 119.12(16) . . ? C21 C20 C25 119.08(16) . . ? C19 C20 C25 121.80(15) . . ? C22 C21 C20 120.94(17) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C21 C22 C23 119.90(17) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C23 C24 121.03(17) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C23 C24 C19 119.04(16) . . ? C23 C24 C28 119.20(16) . . ? C19 C24 C28 121.71(15) . . ? C20 C25 C26 110.89(15) . . ? C20 C25 C27 111.00(15) . . ? C26 C25 C27 110.39(18) . . ? C20 C25 H25A 108.2 . . ? C26 C25 H25A 108.2 . . ? C27 C25 H25A 108.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 111.11(15) . . ? C24 C28 C30 112.28(15) . . ? C29 C28 C30 110.60(15) . . ? C24 C28 H28A 107.5 . . ? C29 C28 H28A 107.5 . . ? C30 C28 H28A 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.505 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.053 #===END data_cbn94fmi_DMn_CCtBu _database_code_depnum_ccdc_archive 'CCDC 794078' #TrackingRef 'CIF-Mn-010510.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H97 Li3 Mn O3, 0.375(O C4 H8), 0.25(C6 H14)' _chemical_formula_sum 'C69 H103.50 Li3 Mn O3.38' _chemical_formula_weight 1062.78 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.4309(9) _cell_length_b 23.2517(18) _cell_length_c 22.8247(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.9220(10) _cell_angle_gamma 90.00 _cell_volume 6588.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9850 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.42 _exptl_crystal_description Needle _exptl_crystal_colour Pale_Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method ? _exptl_crystal_F_000 2314 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9199 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details 'SADABS 2008/3 (Sheldrick, 2008)' _exptl_special_details ; A dark amber colored block with approximate orthogonal dimensions 0.13 x 0.11 x 0.07mm3 was placed and optically centered on the Bruker APEXII(1) CCD diffractometer at -183\%C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide omega-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 55 seconds per frame and 606, 606, 606, 500 frames collected per series at varying phi angles (phi=0? 90? 180? 270?, respectively. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45972 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.25 _reflns_number_total 11919 _reflns_number_gt 9428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.2-0) (Bruker, 2007)' _computing_cell_refinement 'SAINT (7.46A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.46A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: The crystal to detector distance was 5.23cm, thus providing a complete sphere of data to 2ThetaMax=55.13? A total of 80670 reflections were collected and corrected for Lorentz and polarization effects and absorption using Blessing's method as incorporated into the program SADABS(2,3) with 15533 unique. All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. The SHELXTL(4) program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences and intensity statistics indicated the centrosymmetric monoclinic non-standard space group P21/n (no. 14). The structure was determined by direct methods with the successful location of a majority of the molecule within the asymmetric unit using the program XS(5). The structure was refined with XL(5). The 80670 data collected were merged based upon identical indices yielding 58527 data [R(int)=0.0368] that were truncated to 50.50?and merged during least-squares refinement to 11919 unique data [R(int)=0.0515]. A series of least-squares difference-Fourier cycles were required to locate the remaining non-hydrogen atoms. All full occupancy non-hydrogen atoms were refined anisotropically. Hydrogen atoms were idealized throughout the final convergence stage. Two THF molecules bound to Li atoms were found to be disordered and optimized. A solvent mixture of THF and a single hexane solvent molecule were found to be overlapping on the same extended site wherein the THF could occupy both sites simultaneously while the hexane could not thereby requiring a 2:1 optimization which indicated the THF:hexane to be 0.375:0.25. The final structure was refined to convergence with a series of restraints that included DFIX, SADI, EADP and ISOR commands to aid the disordered regions with the final residuals R(F)=8.83%, wR(F2)=16.62%, GOF=1.135 for all 11919 unique reflections [R(F)=6.87%, wR(F2)=15.96% for those 9428 data with Fo > 4sigma(Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be negative and therefore not applied. References: 1. Bruker (2007) APEX (Version 2.0.2) and SAINT (Version 7.46A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008/1) Version 2.10, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.86 Ratio Atom C52 has a large libration while the other two carbon atoms attached to C51 do not exhibit this libration to such a magnitude. 366_ALERT_2_A Short? C(sp?)-C(sp?) Bond C49 - C50 ... 1.13 Ang. Atoms C49 and C50 exhibit large thermal motion nearly along the bond between them. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C31 - C32 ... 1.22 Ang. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C37 - C38 ... 1.22 Ang. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C43 - C44 ... 1.22 Ang. These are the triple bonds of the alkyne ligands. PLAT413_ALERT_2_B Short Inter XH3 .. XHn H35C .. H72A .. 2.04 Ang. This is due to the disordered solvents. ; _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^+12.3050P] 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 11919 _refine_ls_number_parameters 766 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1596 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.148 _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 -0.02930(4) 0.229930(19) 0.20716(2) 0.02298(13) Uani 1 1 d . A . Li1 Li 0.0438(5) 0.1065(2) 0.2094(3) 0.0346(13) Uani 1 1 d . A . Li2 Li 0.0417(5) 0.1657(2) 0.1013(2) 0.0353(13) Uani 1 1 d . A . Li3 Li 0.2013(4) 0.1916(2) 0.1889(3) 0.0337(12) Uani 1 1 d . . . O1 O 0.0310(2) 0.03138(10) 0.24557(11) 0.0407(6) Uani 1 1 d D . . O2 O 0.0166(2) 0.15819(11) 0.01696(10) 0.0396(6) Uani 1 1 d . . . C1 C -0.1428(2) 0.29143(13) 0.23977(13) 0.0252(7) Uani 1 1 d . . . C2 C -0.1827(2) 0.28757(13) 0.29663(13) 0.0267(7) Uani 1 1 d . B . C3 C -0.2595(3) 0.32561(14) 0.31691(14) 0.0316(7) Uani 1 1 d . . . H3A H -0.2844 0.3212 0.3553 0.038 Uiso 1 1 calc R B . C4 C -0.2996(3) 0.36966(15) 0.28137(15) 0.0352(8) Uani 1 1 d . B . H4A H -0.3523 0.3953 0.2950 0.042 Uiso 1 1 calc R . . C5 C -0.2617(3) 0.37589(14) 0.22562(15) 0.0317(7) Uani 1 1 d . . . H5A H -0.2881 0.4063 0.2010 0.038 Uiso 1 1 calc R B . C6 C -0.1851(3) 0.33789(13) 0.20539(13) 0.0265(7) Uani 1 1 d . B . C7 C -0.1376(3) 0.24451(13) 0.34015(13) 0.0264(7) Uani 1 1 d . . . C8 C -0.1835(3) 0.18966(14) 0.34484(14) 0.0300(7) Uani 1 1 d . B . C9 C -0.1420(3) 0.15156(15) 0.38711(14) 0.0348(8) Uani 1 1 d . . . H9A H -0.1724 0.1142 0.3900 0.042 Uiso 1 1 calc R B . C10 C -0.0567(3) 0.16746(15) 0.42512(14) 0.0345(8) Uani 1 1 d . B . H10A H -0.0291 0.1412 0.4540 0.041 Uiso 1 1 calc R . . C11 C -0.0120(3) 0.22156(15) 0.42095(14) 0.0328(7) Uani 1 1 d . . . H11A H 0.0460 0.2323 0.4474 0.039 Uiso 1 1 calc R B . C12 C -0.0503(3) 0.26066(14) 0.37870(13) 0.0284(7) Uani 1 1 d . B . C13 C -0.2829(3) 0.17254(15) 0.30718(15) 0.0356(8) Uani 1 1 d . . . H13A H -0.2914 0.2006 0.2740 0.043 Uiso 1 1 calc R B . C14 C -0.2763(4) 0.11256(17) 0.28114(18) 0.0503(10) Uani 1 1 d . B . H14A H -0.2127 0.1099 0.2576 0.075 Uiso 1 1 calc R . . H14B H -0.3412 0.1050 0.2561 0.075 Uiso 1 1 calc R . . H14C H -0.2708 0.0841 0.3128 0.075 Uiso 1 1 calc R . . C15 C -0.3830(3) 0.1770(2) 0.34368(17) 0.0550(11) Uani 1 1 d . B . H15A H -0.3875 0.2159 0.3600 0.082 Uiso 1 1 calc R . . H15B H -0.3776 0.1490 0.3757 0.082 Uiso 1 1 calc R . . H15C H -0.4476 0.1692 0.3186 0.082 Uiso 1 1 calc R . . C16 C -0.0002(3) 0.32009(14) 0.37585(15) 0.0325(7) Uani 1 1 d . . . H16A H -0.0308 0.3392 0.3395 0.039 Uiso 1 1 calc R B . C17 C 0.1215(3) 0.31783(17) 0.37165(19) 0.0489(10) Uani 1 1 d . B . H17A H 0.1394 0.2928 0.3390 0.073 Uiso 1 1 calc R . . H17B H 0.1545 0.3025 0.4083 0.073 Uiso 1 1 calc R . . H17C H 0.1490 0.3567 0.3650 0.073 Uiso 1 1 calc R . . C18 C -0.0304(4) 0.35660(18) 0.42771(19) 0.0573(12) Uani 1 1 d . B . H18A H -0.1089 0.3602 0.4277 0.086 Uiso 1 1 calc R . . H18B H 0.0019 0.3949 0.4246 0.086 Uiso 1 1 calc R . . H18C H -0.0035 0.3383 0.4643 0.086 Uiso 1 1 calc R . . C19 C -0.1439(3) 0.35065(13) 0.14578(14) 0.0305(7) Uani 1 1 d . . . C20 C -0.0556(3) 0.38741(14) 0.14168(16) 0.0380(8) Uani 1 1 d . B . C21 C -0.0210(3) 0.40156(17) 0.08600(17) 0.0471(10) Uani 1 1 d . . . H21A H 0.0389 0.4266 0.0828 0.057 Uiso 1 1 calc R B . C22 C -0.0721(4) 0.37987(17) 0.03582(16) 0.0476(10) Uani 1 1 d . B . H22A H -0.0469 0.3894 -0.0016 0.057 Uiso 1 1 calc R . . C23 C -0.1593(3) 0.34457(16) 0.04001(15) 0.0423(9) Uani 1 1 d . . . H23A H -0.1947 0.3300 0.0052 0.051 Uiso 1 1 calc R B . C24 C -0.1976(3) 0.32952(14) 0.09456(14) 0.0338(8) Uani 1 1 d . B . C25 C -0.0019(3) 0.41440(16) 0.19583(17) 0.0447(9) Uani 1 1 d . . . H25A H -0.0247 0.3920 0.2305 0.054 Uiso 1 1 calc R B . C26 C 0.1204(4) 0.4124(2) 0.1964(2) 0.0585(12) Uani 1 1 d . B . H26A H 0.1440 0.3726 0.1912 0.088 Uiso 1 1 calc R . . H26B H 0.1505 0.4271 0.2341 0.088 Uiso 1 1 calc R . . H26C H 0.1456 0.4362 0.1645 0.088 Uiso 1 1 calc R . . C27 C -0.0410(4) 0.47631(19) 0.2030(2) 0.0670(13) Uani 1 1 d . B . H27A H -0.1199 0.4769 0.2020 0.101 Uiso 1 1 calc R . . H27B H -0.0158 0.5000 0.1709 0.101 Uiso 1 1 calc R . . H27C H -0.0124 0.4917 0.2406 0.101 Uiso 1 1 calc R . . C28 C -0.2997(3) 0.29474(15) 0.09658(15) 0.0358(8) Uani 1 1 d . . . H28A H -0.3094 0.2844 0.1385 0.043 Uiso 1 1 calc R B . C29 C -0.2976(3) 0.23902(16) 0.06181(17) 0.0441(9) Uani 1 1 d . B . H29A H -0.2367 0.2154 0.0765 0.066 Uiso 1 1 calc R . . H29B H -0.2897 0.2478 0.0203 0.066 Uiso 1 1 calc R . . H29C H -0.3650 0.2180 0.0663 0.066 Uiso 1 1 calc R . . C30 C -0.3970(3) 0.33119(18) 0.07554(18) 0.0489(10) Uani 1 1 d . B . H30A H -0.4017 0.3652 0.1006 0.073 Uiso 1 1 calc R . . H30B H -0.4630 0.3084 0.0777 0.073 Uiso 1 1 calc R . . H30C H -0.3886 0.3433 0.0349 0.073 Uiso 1 1 calc R . . C31 C 0.0888(3) 0.18518(14) 0.26592(14) 0.0278(7) Uani 1 1 d . A . C32 C 0.1584(3) 0.16191(14) 0.29718(14) 0.0290(7) Uani 1 1 d . A . C33 C 0.2428(3) 0.13573(15) 0.33750(14) 0.0325(7) Uani 1 1 d . . . C34 C 0.3122(3) 0.18265(17) 0.36612(17) 0.0480(10) Uani 1 1 d . B . H34A H 0.3474 0.2045 0.3358 0.072 Uiso 1 1 calc R . . H34B H 0.3670 0.1652 0.3929 0.072 Uiso 1 1 calc R . . H34C H 0.2669 0.2085 0.3881 0.072 Uiso 1 1 calc R . . C35 C 0.1916(4) 0.1016(3) 0.3853(2) 0.0832(19) Uani 1 1 d . B . H35A H 0.1491 0.0700 0.3676 0.125 Uiso 1 1 calc R . . H35B H 0.1445 0.1268 0.4070 0.125 Uiso 1 1 calc R . . H35C H 0.2481 0.0859 0.4122 0.125 Uiso 1 1 calc R . . C36 C 0.3138(4) 0.0964(2) 0.3025(2) 0.0621(13) Uani 1 1 d . B . H36A H 0.3452 0.1184 0.2710 0.093 Uiso 1 1 calc R . . H36B H 0.2702 0.0648 0.2856 0.093 Uiso 1 1 calc R . . H36C H 0.3716 0.0806 0.3286 0.093 Uiso 1 1 calc R . . C37 C 0.0842(3) 0.25300(14) 0.14082(14) 0.0300(7) Uani 1 1 d . A . C38 C 0.1475(3) 0.26341(14) 0.10290(14) 0.0311(7) Uani 1 1 d . A . C39 C 0.2232(3) 0.27907(15) 0.05693(14) 0.0354(8) Uani 1 1 d . . . C40 C 0.2830(3) 0.33423(17) 0.07459(17) 0.0464(10) Uani 1 1 d . B . H40A H 0.2310 0.3655 0.0787 0.070 Uiso 1 1 calc R . . H40B H 0.3329 0.3444 0.0444 0.070 Uiso 1 1 calc R . . H40C H 0.3235 0.3283 0.1121 0.070 Uiso 1 1 calc R . . C41 C 0.3050(3) 0.23057(18) 0.05001(17) 0.0465(9) Uani 1 1 d . B . H41A H 0.3479 0.2256 0.0869 0.070 Uiso 1 1 calc R . . H41B H 0.3527 0.2404 0.0186 0.070 Uiso 1 1 calc R . . H41C H 0.2668 0.1947 0.0401 0.070 Uiso 1 1 calc R . . C42 C 0.1606(3) 0.2884(2) -0.00188(16) 0.0491(10) Uani 1 1 d . B . H42A H 0.1071 0.3189 0.0024 0.074 Uiso 1 1 calc R . . H42B H 0.1241 0.2527 -0.0140 0.074 Uiso 1 1 calc R . . H42C H 0.2107 0.2997 -0.0316 0.074 Uiso 1 1 calc R . . C43 C -0.0981(3) 0.15412(13) 0.16260(14) 0.0279(7) Uani 1 1 d . . . C44 C -0.1378(3) 0.11163(14) 0.13900(15) 0.0323(8) Uani 1 1 d . A . C45 C -0.1906(3) 0.06052(15) 0.11037(16) 0.0389(8) Uani 1 1 d . . . C46 C -0.2929(3) 0.07868(18) 0.07673(19) 0.0539(11) Uani 1 1 d . A . H46A H -0.3421 0.0964 0.1037 0.081 Uiso 1 1 calc R . . H46B H -0.3274 0.0449 0.0583 0.081 Uiso 1 1 calc R . . H46C H -0.2755 0.1065 0.0464 0.081 Uiso 1 1 calc R . . C47 C -0.2151(4) 0.01608(18) 0.1562(2) 0.0656(14) Uani 1 1 d . A . H47A H -0.2694 0.0313 0.1818 0.098 Uiso 1 1 calc R . . H47B H -0.1492 0.0071 0.1798 0.098 Uiso 1 1 calc R . . H47C H -0.2427 -0.0189 0.1369 0.098 Uiso 1 1 calc R . . C48 C -0.1122(4) 0.03382(19) 0.0676(2) 0.0680(14) Uani 1 1 d . A . H48A H -0.0973 0.0618 0.0369 0.102 Uiso 1 1 calc R . . H48B H -0.1447 -0.0007 0.0496 0.102 Uiso 1 1 calc R . . H48C H -0.0447 0.0235 0.0891 0.102 Uiso 1 1 calc R . . C49 C 0.1658(3) 0.10835(17) 0.14244(14) 0.0329(8) Uani 1 1 d . A . C50 C 0.2305(3) 0.07967(14) 0.12575(14) 0.0349(8) Uani 1 1 d . . . C51 C 0.3189(3) 0.04022(19) 0.10421(17) 0.0509(11) Uani 1 1 d . B . C52 C 0.4043(5) 0.0299(4) 0.1523(2) 0.122(3) Uani 1 1 d . . . H52A H 0.4443 0.0656 0.1605 0.183 Uiso 1 1 calc R B . H52B H 0.4540 0.0000 0.1399 0.183 Uiso 1 1 calc R . . H52C H 0.3703 0.0172 0.1879 0.183 Uiso 1 1 calc R . . C53 C 0.3675(4) 0.0640(2) 0.04933(19) 0.0598(12) Uani 1 1 d . . . H53A H 0.4022 0.1010 0.0584 0.090 Uiso 1 1 calc R B . H53B H 0.3105 0.0694 0.0186 0.090 Uiso 1 1 calc R . . H53C H 0.4211 0.0368 0.0357 0.090 Uiso 1 1 calc R . . C54 C 0.2632(5) -0.0180(2) 0.0874(2) 0.0832(18) Uani 1 1 d . . . H54A H 0.2322 -0.0347 0.1221 0.125 Uiso 1 1 calc R B . H54B H 0.3165 -0.0446 0.0724 0.125 Uiso 1 1 calc R . . H54C H 0.2059 -0.0113 0.0570 0.125 Uiso 1 1 calc R . . C55 C -0.0297(17) 0.0090(7) 0.2932(8) 0.043(3) Uani 0.46 1 d PD A 1 H55A H -0.1054 0.0011 0.2803 0.052 Uiso 0.46 1 calc PR A 1 H55B H -0.0280 0.0358 0.3270 0.052 Uiso 0.46 1 calc PR A 1 C56 C 0.0328(8) -0.0471(4) 0.3082(4) 0.0471(15) Uani 0.46 1 d PDU A 1 H56A H 0.0922 -0.0389 0.3375 0.057 Uiso 0.46 1 calc PR A 1 H56B H -0.0162 -0.0753 0.3255 0.057 Uiso 0.46 1 calc PR A 1 C57 C 0.0734(11) -0.0697(5) 0.2594(5) 0.080(2) Uani 0.46 1 d PDU A 1 H57A H 0.0197 -0.0935 0.2370 0.096 Uiso 0.46 1 calc PR A 1 H57B H 0.1391 -0.0928 0.2687 0.096 Uiso 0.46 1 calc PR A 1 C58 C 0.098(3) -0.0151(8) 0.2277(11) 0.055(2) Uani 0.46 1 d PD A 1 H58A H 0.1748 -0.0048 0.2360 0.066 Uiso 0.46 1 calc PR A 1 H58B H 0.0869 -0.0212 0.1849 0.066 Uiso 0.46 1 calc PR A 1 C55A C -0.0243(15) 0.0250(5) 0.3002(6) 0.043(3) Uani 0.54 1 d PD A 2 H55C H -0.1023 0.0183 0.2918 0.052 Uiso 0.54 1 calc PR A 2 H55D H -0.0152 0.0600 0.3246 0.052 Uiso 0.54 1 calc PR A 2 C56A C 0.0273(6) -0.0268(3) 0.3318(4) 0.0471(15) Uani 0.54 1 d PD A 2 H56C H 0.0584 -0.0159 0.3710 0.057 Uiso 0.54 1 calc PR A 2 H56D H -0.0260 -0.0580 0.3363 0.057 Uiso 0.54 1 calc PR A 2 C57A C 0.1131(9) -0.0450(5) 0.2925(4) 0.080(2) Uani 0.54 1 d PD A 2 H57C H 0.1160 -0.0875 0.2905 0.096 Uiso 0.54 1 calc PR A 2 H57D H 0.1840 -0.0308 0.3081 0.096 Uiso 0.54 1 calc PR A 2 C58A C 0.088(2) -0.0204(7) 0.2320(9) 0.055(2) Uani 0.54 1 d PD A 2 H58C H 0.1546 -0.0118 0.2117 0.066 Uiso 0.54 1 calc PR A 2 H58D H 0.0422 -0.0468 0.2076 0.066 Uiso 0.54 1 calc PR A 2 C59 C -0.0711(3) 0.18608(17) -0.01529(18) 0.0461(9) Uani 1 1 d . B . H59A H -0.0721 0.2277 -0.0063 0.055 Uiso 1 1 calc R . . H59B H -0.1409 0.1691 -0.0052 0.055 Uiso 1 1 calc R . . C60 C -0.0514(3) 0.17630(19) -0.07927(18) 0.0524(11) Uani 1 1 d . . . H60A H -0.0056 0.2070 -0.0949 0.063 Uiso 1 1 calc R B . H60B H -0.1199 0.1743 -0.1033 0.063 Uiso 1 1 calc R . . C61 C 0.0061(3) 0.11906(19) -0.07764(16) 0.0493(10) Uani 1 1 d . B . H61A H -0.0456 0.0868 -0.0763 0.059 Uiso 1 1 calc R . . H61B H 0.0505 0.1143 -0.1121 0.059 Uiso 1 1 calc R . . C62 C 0.0748(3) 0.12266(18) -0.02235(15) 0.0442(9) Uani 1 1 d . B . H62A H 0.0871 0.0839 -0.0054 0.053 Uiso 1 1 calc R . . H62B H 0.1454 0.1401 -0.0299 0.053 Uiso 1 1 calc R . . O3 O 0.3384(8) 0.2285(3) 0.2076(5) 0.0315(14) Uani 0.65 1 d P B 1 C63 C 0.3259(5) 0.2819(2) 0.2390(2) 0.0306(12) Uani 0.65 1 d P B 1 H63A H 0.2757 0.2769 0.2709 0.037 Uiso 0.65 1 calc PR B 1 H63B H 0.2976 0.3124 0.2122 0.037 Uiso 0.65 1 calc PR B 1 C64 C 0.4370(4) 0.2971(3) 0.2637(3) 0.0441(14) Uani 0.65 1 d P B 1 H64A H 0.4538 0.2773 0.3014 0.053 Uiso 0.65 1 calc PR B 1 H64B H 0.4449 0.3392 0.2695 0.053 Uiso 0.65 1 calc PR B 1 C65 C 0.5100(17) 0.2748(9) 0.2143(6) 0.044(2) Uani 0.65 1 d P B 1 H65A H 0.5104 0.3016 0.1807 0.052 Uiso 0.65 1 calc PR B 1 H65B H 0.5849 0.2676 0.2294 0.052 Uiso 0.65 1 calc PR B 1 C66 C 0.4516(4) 0.2197(3) 0.1986(2) 0.0376(13) Uani 0.65 1 d P B 1 H66A H 0.4620 0.2096 0.1572 0.045 Uiso 0.65 1 calc PR B 1 H66B H 0.4799 0.1879 0.2238 0.045 Uiso 0.65 1 calc PR B 1 O3A O 0.3526(18) 0.2108(7) 0.2102(10) 0.0315(14) Uani 0.35 1 d P B 2 C63A C 0.3884(12) 0.2677(5) 0.2268(5) 0.047(3) Uani 0.35 1 d P B 2 H63C H 0.3590 0.2962 0.1980 0.056 Uiso 0.35 1 calc PR B 2 H63D H 0.3625 0.2777 0.2658 0.056 Uiso 0.35 1 calc PR B 2 C64A C 0.504(3) 0.269(2) 0.2285(15) 0.044(2) Uani 0.35 1 d P B 2 H64C H 0.5344 0.2601 0.2684 0.052 Uiso 0.35 1 calc PR B 2 H64D H 0.5307 0.3065 0.2158 0.052 Uiso 0.35 1 calc PR B 2 C65A C 0.5319(10) 0.2190(5) 0.1831(6) 0.052(3) Uani 0.35 1 d P B 2 H65C H 0.5255 0.2326 0.1420 0.063 Uiso 0.35 1 calc PR B 2 H65D H 0.6047 0.2029 0.1917 0.063 Uiso 0.35 1 calc PR B 2 C66A C 0.4455(8) 0.1768(5) 0.1960(5) 0.040(2) Uani 0.35 1 d P B 2 H66C H 0.4283 0.1521 0.1614 0.048 Uiso 0.35 1 calc PR B 2 H66D H 0.4687 0.1519 0.2295 0.048 Uiso 0.35 1 calc PR B 2 O71 O 0.8601(7) 0.0032(5) 0.4418(4) 0.075(3) Uiso 0.38 1 d PD C 1 C71 C 0.8527(9) 0.0130(6) 0.5025(4) 0.064(3) Uiso 0.38 1 d PD C 1 H71A H 0.8912 0.0489 0.5138 0.076 Uiso 0.38 1 calc PR C 1 H71B H 0.8869 -0.0192 0.5249 0.076 Uiso 0.38 1 calc PR C 1 C72 C 0.7374(10) 0.0178(8) 0.5166(5) 0.102(5) Uiso 0.38 1 d PD C 1 H72A H 0.7114 -0.0183 0.5339 0.122 Uiso 0.38 1 calc PR C 1 H72B H 0.7265 0.0498 0.5442 0.122 Uiso 0.38 1 calc PR C 1 C73 C 0.6817(7) 0.0291(5) 0.4593(4) 0.048(3) Uiso 0.38 1 d PD C 1 H73A H 0.6809 0.0707 0.4499 0.058 Uiso 0.38 1 calc PR C 1 H73B H 0.6068 0.0145 0.4579 0.058 Uiso 0.38 1 calc PR C 1 C74 C 0.7502(7) -0.0039(5) 0.4188(4) 0.047(3) Uiso 0.38 1 d PD C 1 H74A H 0.7298 -0.0451 0.4182 0.056 Uiso 0.38 1 calc PR C 1 H74B H 0.7416 0.0114 0.3784 0.056 Uiso 0.38 1 calc PR C 1 C81 C 0.7564(12) 0.0210(7) 0.4775(7) 0.044(4) Uiso 0.25 1 d PD D -2 H81A H 0.7259 0.0021 0.5112 0.066 Uiso 0.25 1 calc PR D -2 H81B H 0.7121 0.0121 0.4419 0.066 Uiso 0.25 1 calc PR D -2 H81C H 0.7577 0.0627 0.4838 0.066 Uiso 0.25 1 calc PR D -2 C82 C 0.8764(14) -0.0017(10) 0.4703(11) 0.066(6) Uiso 0.25 1 d PD D -2 H82A H 0.8700 -0.0440 0.4663 0.080 Uiso 0.25 1 calc PR D -2 H82B H 0.8969 0.0126 0.4316 0.080 Uiso 0.25 1 calc PR D -2 C83 C 0.9727(11) 0.0081(11) 0.5108(9) 0.075(3) Uiso 0.25 1 d PD D -2 H83A H 0.9740 0.0499 0.5191 0.090 Uiso 0.25 1 calc PR D -2 H83B H 0.9566 -0.0110 0.5481 0.090 Uiso 0.25 1 calc PR D -2 C84 C 1.0838(12) -0.0075(9) 0.4996(8) 0.057(5) Uiso 0.25 1 d PD D -2 H84A H 1.0970 0.0118 0.4620 0.069 Uiso 0.25 1 calc PR D -2 H84B H 1.0793 -0.0490 0.4902 0.069 Uiso 0.25 1 calc PR D -2 C85 C 1.1878(15) -0.0019(11) 0.5339(9) 0.073(6) Uiso 0.25 1 d PD D -2 H85A H 1.2237 0.0336 0.5210 0.088 Uiso 0.25 1 calc PR D -2 H85B H 1.2342 -0.0347 0.5238 0.088 Uiso 0.25 1 calc PR D -2 C86 C 1.183(2) 0.0003(14) 0.6013(9) 0.114(9) Uiso 0.25 1 d PD D -2 H86A H 1.1656 0.0396 0.6135 0.171 Uiso 0.25 1 calc PR D -2 H86B H 1.2523 -0.0112 0.6196 0.171 Uiso 0.25 1 calc PR D -2 H86C H 1.1265 -0.0260 0.6137 0.171 Uiso 0.25 1 calc PR D -2 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 0.0259(2) 0.0210(2) 0.0223(2) -0.00101(18) 0.00319(18) 0.00052(19) Li1 0.037(3) 0.026(3) 0.041(3) 0.002(2) 0.002(3) 0.001(2) Li2 0.046(3) 0.030(3) 0.031(3) -0.003(2) 0.006(3) 0.005(3) Li3 0.028(3) 0.033(3) 0.039(3) 0.000(2) -0.001(2) -0.004(2) O1 0.0424(14) 0.0305(13) 0.0495(15) 0.0116(11) 0.0053(12) 0.0009(11) O2 0.0476(15) 0.0420(14) 0.0292(13) -0.0055(11) 0.0018(11) 0.0170(12) C1 0.0273(16) 0.0222(15) 0.0260(16) -0.0049(12) 0.0024(13) -0.0027(13) C2 0.0275(17) 0.0252(16) 0.0271(16) -0.0057(13) 0.0005(13) -0.0026(13) C3 0.0362(19) 0.0336(18) 0.0256(16) -0.0080(14) 0.0077(14) -0.0004(15) C4 0.0352(19) 0.0327(18) 0.0381(19) -0.0094(15) 0.0063(15) 0.0057(15) C5 0.0353(19) 0.0246(16) 0.0350(18) -0.0035(14) -0.0014(15) 0.0048(14) C6 0.0287(17) 0.0232(15) 0.0276(16) -0.0048(13) 0.0001(13) -0.0020(13) C7 0.0305(17) 0.0276(16) 0.0216(15) -0.0044(12) 0.0063(13) 0.0010(13) C8 0.0343(18) 0.0326(18) 0.0234(16) -0.0046(13) 0.0054(13) -0.0058(14) C9 0.046(2) 0.0297(18) 0.0295(17) -0.0009(14) 0.0073(15) -0.0056(16) C10 0.041(2) 0.0366(19) 0.0261(17) 0.0049(14) 0.0049(15) 0.0019(16) C11 0.0371(19) 0.0387(19) 0.0228(16) -0.0031(14) 0.0040(14) -0.0022(15) C12 0.0325(17) 0.0306(17) 0.0228(15) -0.0052(13) 0.0079(13) -0.0012(14) C13 0.038(2) 0.0381(19) 0.0301(18) -0.0035(15) 0.0009(15) -0.0096(16) C14 0.062(3) 0.042(2) 0.047(2) -0.0069(18) 0.003(2) -0.013(2) C15 0.041(2) 0.085(3) 0.039(2) -0.011(2) 0.0022(18) -0.011(2) C16 0.0350(19) 0.0329(18) 0.0296(17) -0.0046(14) 0.0012(14) -0.0046(15) C17 0.039(2) 0.041(2) 0.068(3) -0.0134(19) 0.0137(19) -0.0125(18) C18 0.070(3) 0.042(2) 0.062(3) -0.019(2) 0.023(2) -0.013(2) C19 0.0408(19) 0.0222(16) 0.0286(17) 0.0022(13) 0.0040(14) 0.0072(14) C20 0.051(2) 0.0271(18) 0.0360(19) 0.0014(15) 0.0069(16) 0.0005(16) C21 0.058(3) 0.037(2) 0.048(2) 0.0056(17) 0.0129(19) -0.0046(18) C22 0.065(3) 0.046(2) 0.032(2) 0.0100(17) 0.0104(19) 0.006(2) C23 0.059(3) 0.042(2) 0.0258(18) 0.0030(15) 0.0006(17) 0.0103(19) C24 0.042(2) 0.0306(18) 0.0282(17) -0.0005(14) 0.0020(15) 0.0097(15) C25 0.050(2) 0.037(2) 0.047(2) -0.0046(17) 0.0094(18) -0.0135(18) C26 0.059(3) 0.056(3) 0.061(3) -0.015(2) 0.002(2) -0.009(2) C27 0.077(3) 0.047(3) 0.077(3) -0.021(2) 0.003(3) -0.005(2) C28 0.039(2) 0.0397(19) 0.0284(17) -0.0049(15) -0.0037(15) 0.0045(16) C29 0.043(2) 0.045(2) 0.044(2) -0.0096(17) -0.0086(17) 0.0101(18) C30 0.049(2) 0.050(2) 0.048(2) -0.0117(19) -0.0031(19) 0.0182(19) C31 0.0266(17) 0.0290(17) 0.0281(16) 0.0004(13) 0.0044(14) -0.0018(14) C32 0.0270(17) 0.0320(17) 0.0282(17) -0.0010(14) 0.0058(14) -0.0030(14) C33 0.0287(17) 0.0361(19) 0.0325(18) 0.0061(14) 0.0003(14) 0.0027(14) C34 0.053(2) 0.049(2) 0.039(2) -0.0039(18) -0.0174(18) 0.0052(19) C35 0.037(2) 0.117(5) 0.095(4) 0.075(4) -0.003(2) -0.002(3) C36 0.058(3) 0.063(3) 0.062(3) -0.024(2) -0.023(2) 0.031(2) C37 0.0379(19) 0.0250(16) 0.0273(17) 0.0004(13) 0.0042(15) 0.0011(14) C38 0.0371(19) 0.0274(17) 0.0291(17) 0.0022(13) 0.0042(15) 0.0020(14) C39 0.039(2) 0.041(2) 0.0270(17) 0.0045(15) 0.0092(15) -0.0003(16) C40 0.051(2) 0.051(2) 0.038(2) 0.0023(18) 0.0149(18) -0.0127(19) C41 0.047(2) 0.055(2) 0.040(2) 0.0064(18) 0.0188(18) 0.0040(19) C42 0.047(2) 0.071(3) 0.0297(19) 0.0120(18) 0.0077(17) -0.006(2) C43 0.0288(17) 0.0265(17) 0.0283(16) -0.0012(13) -0.0002(13) 0.0048(14) C44 0.0334(18) 0.0259(17) 0.0376(19) -0.0009(14) 0.0007(15) 0.0037(14) C45 0.044(2) 0.0259(17) 0.046(2) -0.0076(15) -0.0072(17) -0.0017(15) C46 0.059(3) 0.041(2) 0.060(3) -0.0086(19) -0.017(2) -0.009(2) C47 0.093(4) 0.036(2) 0.065(3) 0.003(2) -0.023(3) -0.024(2) C48 0.079(3) 0.044(2) 0.082(3) -0.032(2) 0.008(3) -0.001(2) C49 0.0188(16) 0.056(2) 0.0244(17) 0.0115(16) 0.0019(13) -0.0052(16) C50 0.060(2) 0.0212(16) 0.0222(16) -0.0015(13) -0.0114(16) -0.0014(16) C51 0.055(3) 0.062(3) 0.035(2) 0.0022(19) 0.0026(18) 0.029(2) C52 0.086(4) 0.229(9) 0.050(3) -0.005(4) -0.008(3) 0.102(5) C53 0.055(3) 0.072(3) 0.053(3) 0.003(2) 0.017(2) 0.018(2) C54 0.143(5) 0.046(3) 0.064(3) -0.004(2) 0.036(3) 0.030(3) C55 0.036(3) 0.035(7) 0.058(4) 0.019(5) 0.003(3) -0.015(5) C56 0.048(2) 0.045(2) 0.048(2) 0.0143(17) -0.0003(18) -0.0048(17) C57 0.080(3) 0.075(3) 0.083(3) 0.0038(19) -0.0018(19) 0.0059(19) C58 0.058(5) 0.025(3) 0.081(4) 0.004(3) -0.007(3) 0.004(3) C55A 0.036(3) 0.035(7) 0.058(4) 0.019(5) 0.003(3) -0.015(5) C56A 0.048(2) 0.045(2) 0.048(2) 0.0143(17) -0.0003(18) -0.0048(17) C57A 0.080(3) 0.075(3) 0.083(3) 0.0038(19) -0.0018(19) 0.0059(19) C58A 0.058(5) 0.025(3) 0.081(4) 0.004(3) -0.007(3) 0.004(3) C59 0.036(2) 0.041(2) 0.061(3) 0.0046(19) -0.0005(18) 0.0122(17) C60 0.043(2) 0.064(3) 0.048(2) 0.020(2) -0.0137(19) -0.008(2) C61 0.059(3) 0.060(3) 0.0291(19) -0.0050(18) 0.0091(18) -0.009(2) C62 0.048(2) 0.051(2) 0.034(2) -0.0101(17) 0.0043(17) 0.0158(18) O3 0.025(3) 0.033(5) 0.0368(18) -0.008(4) 0.001(2) -0.003(3) C63 0.029(3) 0.034(3) 0.029(3) -0.005(2) 0.004(2) 0.000(2) C64 0.031(3) 0.049(4) 0.051(4) -0.013(3) -0.008(3) -0.007(3) C65 0.034(3) 0.059(6) 0.038(8) 0.002(6) 0.008(6) -0.016(3) C66 0.025(3) 0.056(4) 0.032(3) -0.010(3) 0.001(2) 0.006(3) O3A 0.025(3) 0.033(5) 0.0368(18) -0.008(4) 0.001(2) -0.003(3) C63A 0.072(9) 0.030(6) 0.038(6) 0.001(5) -0.003(7) -0.008(7) C64A 0.034(3) 0.059(6) 0.038(8) 0.002(6) 0.008(6) -0.016(3) C65A 0.035(7) 0.065(8) 0.056(7) 0.004(6) -0.003(6) -0.007(6) C66A 0.031(6) 0.041(7) 0.048(7) -0.007(5) -0.001(5) 0.008(5) _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 C1 2.167(3) . ? Mn1 C43 2.187(3) . ? Mn1 C37 2.189(3) . ? Mn1 C31 2.199(3) . ? Mn1 Li1 3.010(5) . ? Mn1 Li2 3.011(5) . ? Mn1 Li3 3.050(6) . ? Li1 O1 1.941(6) . ? Li1 C49 2.208(7) . ? Li1 C31 2.292(6) . ? Li1 C43 2.299(7) . ? Li1 C44 2.707(7) . ? Li1 C32 2.723(7) . ? Li1 Li2 2.826(8) . ? Li1 Li3 2.839(8) . ? Li2 O2 1.942(6) . ? Li2 C49 2.213(7) . ? Li2 C37 2.272(6) . ? Li2 C43 2.302(7) . ? Li2 C38 2.623(7) . ? Li2 C44 2.739(7) . ? Li2 Li3 2.809(8) . ? Li3 O3 1.937(12) . ? Li3 O3A 1.97(2) . ? Li3 C49 2.240(7) . ? Li3 C37 2.280(7) . ? Li3 C31 2.306(6) . ? Li3 C38 2.638(7) . ? Li3 C32 2.646(7) . ? O1 C58 1.437(9) . ? O1 C58A 1.437(8) . ? O1 C55 1.451(9) . ? O1 C55A 1.462(8) . ? O2 C59 1.438(4) . ? O2 C62 1.441(4) . ? C1 C2 1.415(4) . ? C1 C6 1.420(4) . ? C2 C3 1.398(4) . ? C2 C7 1.499(4) . ? C3 C4 1.383(5) . ? C3 H3A 0.9500 . ? C4 C5 1.387(5) . ? C4 H4A 0.9500 . ? C5 C6 1.395(4) . ? C5 H5A 0.9500 . ? C6 C19 1.508(4) . ? C7 C8 1.403(4) . ? C7 C12 1.412(4) . ? C8 C9 1.390(5) . ? C8 C13 1.522(5) . ? C9 C10 1.385(5) . ? C9 H9A 0.9500 . ? C10 C11 1.381(5) . ? C10 H10A 0.9500 . ? C11 C12 1.391(5) . ? C11 H11A 0.9500 . ? C12 C16 1.518(4) . ? C13 C14 1.520(5) . ? C13 C15 1.535(5) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.519(5) . ? C16 C17 1.522(5) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.398(5) . ? C19 C24 1.405(5) . ? C20 C21 1.402(5) . ? C20 C25 1.511(5) . ? C21 C22 1.377(6) . ? C21 H21A 0.9500 . ? C22 C23 1.367(6) . ? C22 H22A 0.9500 . ? C23 C24 1.400(5) . ? C23 H23A 0.9500 . ? C24 C28 1.508(5) . ? C25 C26 1.521(6) . ? C25 C27 1.531(6) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.520(5) . ? C28 C30 1.534(5) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.220(4) . ? C32 C33 1.490(5) . ? C33 C35 1.515(5) . ? C33 C34 1.518(5) . ? C33 C36 1.525(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.223(5) . ? C38 C39 1.490(4) . ? C39 C40 1.526(5) . ? C39 C41 1.532(5) . ? C39 C42 1.532(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.218(5) . ? C44 C45 1.492(5) . ? C45 C46 1.512(5) . ? C45 C47 1.513(6) . ? C45 C48 1.545(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.126(5) . ? C50 C51 1.531(5) . ? C51 C52 1.508(6) . ? C51 C53 1.522(6) . ? C51 C54 1.560(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.548(16) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.352(12) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.502(18) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C55A C56A 1.528(14) . ? C55A H55C 0.9900 . ? C55A H55D 0.9900 . ? C56A C57A 1.489(11) . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? C57A C58A 1.513(18) . ? C57A H57C 0.9900 . ? C57A H57D 0.9900 . ? C58A H58C 0.9900 . ? C58A H58D 0.9900 . ? C59 C60 1.510(6) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.510(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.490(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? O3 C66 1.446(11) . ? O3 C63 1.446(9) . ? C63 C64 1.507(7) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.572(19) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.51(2) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? O3A C63A 1.44(2) . ? O3A C66A 1.45(2) . ? C63A C64A 1.43(4) . ? C63A H63C 0.9900 . ? C63A H63D 0.9900 . ? C64A C65A 1.60(5) . ? C64A H64C 0.9900 . ? C64A H64D 0.9900 . ? C65A C66A 1.495(16) . ? C65A H65C 0.9900 . ? C65A H65D 0.9900 . ? C66A H66C 0.9900 . ? C66A H66D 0.9900 . ? O71 C71 1.412(9) . ? O71 C74 1.448(8) . ? C71 C72 1.490(9) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.472(9) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.500(8) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C81 C82 1.598(19) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.49(2) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.462(18) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.48(2) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.54(2) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mn1 C43 116.45(12) . . ? C1 Mn1 C37 122.01(12) . . ? C43 Mn1 C37 97.26(12) . . ? C1 Mn1 C31 121.93(12) . . ? C43 Mn1 C31 97.77(12) . . ? C37 Mn1 C31 95.97(12) . . ? C1 Mn1 Li1 145.53(14) . . ? C43 Mn1 Li1 49.46(14) . . ? C37 Mn1 Li1 92.34(14) . . ? C31 Mn1 Li1 49.22(14) . . ? C1 Mn1 Li2 145.62(14) . . ? C43 Mn1 Li2 49.53(14) . . ? C37 Mn1 Li2 48.72(14) . . ? C31 Mn1 Li2 92.36(14) . . ? Li1 Mn1 Li2 55.99(16) . . ? C1 Mn1 Li3 150.76(13) . . ? C43 Mn1 Li3 92.79(13) . . ? C37 Mn1 Li3 48.21(14) . . ? C31 Mn1 Li3 48.88(13) . . ? Li1 Mn1 Li3 55.86(15) . . ? Li2 Mn1 Li3 55.22(16) . . ? O1 Li1 C49 112.7(3) . . ? O1 Li1 C31 120.1(3) . . ? C49 Li1 C31 102.6(3) . . ? O1 Li1 C43 123.6(3) . . ? C49 Li1 C43 101.9(3) . . ? C31 Li1 C43 92.1(2) . . ? O1 Li1 C44 102.0(3) . . ? C49 Li1 C44 99.8(2) . . ? C31 Li1 C44 118.1(2) . . ? C43 Li1 C44 26.60(12) . . ? O1 Li1 C32 99.4(3) . . ? C49 Li1 C32 98.5(2) . . ? C31 Li1 C32 26.42(12) . . ? C43 Li1 C32 118.3(2) . . ? C44 Li1 C32 143.7(2) . . ? O1 Li1 Li2 144.4(3) . . ? C49 Li1 Li2 50.33(19) . . ? C31 Li1 Li2 95.3(2) . . ? C43 Li1 Li2 52.15(19) . . ? C44 Li1 Li2 59.30(19) . . ? C32 Li1 Li2 113.1(2) . . ? O1 Li1 Li3 140.3(3) . . ? C49 Li1 Li3 50.83(19) . . ? C31 Li1 Li3 52.09(18) . . ? C43 Li1 Li3 96.1(2) . . ? C44 Li1 Li3 115.6(2) . . ? C32 Li1 Li3 56.76(17) . . ? Li2 Li1 Li3 59.5(2) . . ? O1 Li1 Mn1 146.5(3) . . ? C49 Li1 Mn1 100.8(2) . . ? C31 Li1 Mn1 46.60(13) . . ? C43 Li1 Mn1 46.29(13) . . ? C44 Li1 Mn1 72.89(15) . . ? C32 Li1 Mn1 72.99(15) . . ? Li2 Li1 Mn1 62.02(16) . . ? Li3 Li1 Mn1 62.78(16) . . ? O2 Li2 C49 116.1(3) . . ? O2 Li2 C37 119.8(3) . . ? C49 Li2 C37 103.1(3) . . ? O2 Li2 C43 120.2(3) . . ? C49 Li2 C43 101.7(2) . . ? C37 Li2 C43 91.8(2) . . ? O2 Li2 C38 98.5(2) . . ? C49 Li2 C38 100.3(3) . . ? C37 Li2 C38 27.75(13) . . ? C43 Li2 C38 119.1(2) . . ? O2 Li2 C44 100.2(3) . . ? C49 Li2 C44 98.7(2) . . ? C37 Li2 C44 117.5(2) . . ? C43 Li2 C44 26.17(12) . . ? C38 Li2 C44 144.0(2) . . ? O2 Li2 Li3 142.9(3) . . ? C49 Li2 Li3 51.3(2) . . ? C37 Li2 Li3 52.01(19) . . ? C43 Li2 Li3 96.9(2) . . ? C38 Li2 Li3 57.97(18) . . ? C44 Li2 Li3 115.5(2) . . ? O2 Li2 Li1 144.6(3) . . ? C49 Li2 Li1 50.19(18) . . ? C37 Li2 Li1 95.5(2) . . ? C43 Li2 Li1 52.06(18) . . ? C38 Li2 Li1 115.3(2) . . ? C44 Li2 Li1 58.17(18) . . ? Li3 Li2 Li1 60.5(2) . . ? O2 Li2 Mn1 143.3(3) . . ? C49 Li2 Mn1 100.6(2) . . ? C37 Li2 Mn1 46.39(13) . . ? C43 Li2 Mn1 46.28(13) . . ? C38 Li2 Mn1 74.14(15) . . ? C44 Li2 Mn1 72.44(15) . . ? Li3 Li2 Mn1 63.10(16) . . ? Li1 Li2 Mn1 62.00(16) . . ? O3 Li3 O3A 13.2(5) . . ? O3 Li3 C49 129.6(4) . . ? O3A Li3 C49 118.4(5) . . ? O3 Li3 C37 111.2(3) . . ? O3A Li3 C37 123.7(5) . . ? C49 Li3 C37 102.0(2) . . ? O3 Li3 C31 115.0(4) . . ? O3A Li3 C31 115.8(7) . . ? C49 Li3 C31 101.1(2) . . ? C37 Li3 C31 90.6(2) . . ? O3 Li3 C38 94.0(3) . . ? O3A Li3 C38 104.0(6) . . ? C49 Li3 C38 99.1(2) . . ? C37 Li3 C38 27.58(13) . . ? C31 Li3 C38 117.9(3) . . ? O3 Li3 C32 97.3(4) . . ? O3A Li3 C32 93.7(7) . . ? C49 Li3 C32 100.0(2) . . ? C37 Li3 C32 117.3(3) . . ? C31 Li3 C32 27.45(12) . . ? C38 Li3 C32 143.6(3) . . ? O3 Li3 Li2 146.4(4) . . ? O3A Li3 Li2 148.7(7) . . ? C49 Li3 Li2 50.45(18) . . ? C37 Li3 Li2 51.76(18) . . ? C31 Li3 Li2 95.5(2) . . ? C38 Li3 Li2 57.47(18) . . ? C32 Li3 Li2 116.2(2) . . ? O3 Li3 Li1 151.6(4) . . ? O3A Li3 Li1 140.8(6) . . ? C49 Li3 Li1 49.85(18) . . ? C37 Li3 Li1 95.0(2) . . ? C31 Li3 Li1 51.64(18) . . ? C38 Li3 Li1 114.4(2) . . ? C32 Li3 Li1 59.41(18) . . ? Li2 Li3 Li1 60.0(2) . . ? O3 Li3 Mn1 131.5(3) . . ? O3A Li3 Mn1 142.4(6) . . ? C49 Li3 Mn1 98.8(2) . . ? C37 Li3 Mn1 45.71(13) . . ? C31 Li3 Mn1 45.91(13) . . ? C38 Li3 Mn1 73.27(16) . . ? C32 Li3 Mn1 73.36(16) . . ? Li2 Li3 Mn1 61.68(16) . . ? Li1 Li3 Mn1 61.36(16) . . ? C58 O1 C55 105.9(11) . . ? C58A O1 C55 98.2(10) . . ? C58 O1 C55A 118.1(10) . . ? C58A O1 C55A 110.9(9) . . ? C58 O1 Li1 119.6(9) . . ? C58A O1 Li1 127.6(8) . . ? C55 O1 Li1 134.2(7) . . ? C55A O1 Li1 120.4(5) . . ? C59 O2 C62 109.4(3) . . ? C59 O2 Li2 123.1(3) . . ? C62 O2 Li2 127.5(3) . . ? C2 C1 C6 114.7(3) . . ? C2 C1 Mn1 122.5(2) . . ? C6 C1 Mn1 122.8(2) . . ? C3 C2 C1 122.7(3) . . ? C3 C2 C7 116.2(3) . . ? C1 C2 C7 120.9(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 122.6(3) . . ? C5 C6 C19 116.3(3) . . ? C1 C6 C19 121.0(3) . . ? C8 C7 C12 119.8(3) . . ? C8 C7 C2 121.2(3) . . ? C12 C7 C2 119.0(3) . . ? C9 C8 C7 119.6(3) . . ? C9 C8 C13 119.2(3) . . ? C7 C8 C13 121.1(3) . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C11 C10 C9 119.9(3) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C11 C12 C7 118.9(3) . . ? C11 C12 C16 119.8(3) . . ? C7 C12 C16 121.3(3) . . ? C14 C13 C8 113.7(3) . . ? C14 C13 C15 109.7(3) . . ? C8 C13 C15 109.4(3) . . ? C14 C13 H13A 108.0 . . ? C8 C13 H13A 108.0 . . ? C15 C13 H13A 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C18 110.9(3) . . ? C12 C16 C17 112.5(3) . . ? C18 C16 C17 110.7(3) . . ? C12 C16 H16A 107.5 . . ? C18 C16 H16A 107.5 . . ? C17 C16 H16A 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 120.0(3) . . ? C20 C19 C6 119.0(3) . . ? C24 C19 C6 120.9(3) . . ? C19 C20 C21 118.9(3) . . ? C19 C20 C25 121.0(3) . . ? C21 C20 C25 120.0(3) . . ? C22 C21 C20 121.2(4) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 121.3(4) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C23 C24 C19 119.0(3) . . ? C23 C24 C28 119.1(3) . . ? C19 C24 C28 121.8(3) . . ? C20 C25 C26 113.3(3) . . ? C20 C25 C27 110.4(4) . . ? C26 C25 C27 110.5(3) . . ? C20 C25 H25A 107.5 . . ? C26 C25 H25A 107.5 . . ? C27 C25 H25A 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 113.8(3) . . ? C24 C28 C30 110.2(3) . . ? C29 C28 C30 110.0(3) . . ? C24 C28 H28A 107.5 . . ? C29 C28 H28A 107.5 . . ? C30 C28 H28A 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 Mn1 176.7(3) . . ? C32 C31 Li1 96.9(3) . . ? Mn1 C31 Li1 84.18(18) . . ? C32 C31 Li3 92.0(3) . . ? Mn1 C31 Li3 85.21(18) . . ? Li1 C31 Li3 76.3(2) . . ? C31 C32 C33 177.2(3) . . ? C31 C32 Li3 60.6(2) . . ? C33 C32 Li3 121.0(2) . . ? C31 C32 Li1 56.7(2) . . ? C33 C32 Li1 125.9(2) . . ? Li3 C32 Li1 63.83(18) . . ? C32 C33 C35 110.5(3) . . ? C32 C33 C34 109.8(3) . . ? C35 C33 C34 108.5(4) . . ? C32 C33 C36 109.3(3) . . ? C35 C33 C36 109.7(4) . . ? C34 C33 C36 109.0(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 Mn1 177.2(3) . . ? C38 C37 Li2 92.3(3) . . ? Mn1 C37 Li2 84.89(18) . . ? C38 C37 Li3 92.7(3) . . ? Mn1 C37 Li3 86.07(18) . . ? Li2 C37 Li3 76.2(2) . . ? C37 C38 C39 177.3(3) . . ? C37 C38 Li2 59.9(2) . . ? C39 C38 Li2 122.4(3) . . ? C37 C38 Li3 59.7(2) . . ? C39 C38 Li3 122.2(3) . . ? Li2 C38 Li3 64.55(19) . . ? C38 C39 C40 109.6(3) . . ? C38 C39 C41 109.8(3) . . ? C40 C39 C41 109.2(3) . . ? C38 C39 C42 109.9(3) . . ? C40 C39 C42 109.3(3) . . ? C41 C39 C42 108.9(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 Mn1 178.4(3) . . ? C44 C43 Li1 95.7(3) . . ? Mn1 C43 Li1 84.25(18) . . ? C44 C43 Li2 97.4(3) . . ? Mn1 C43 Li2 84.20(18) . . ? Li1 C43 Li2 75.8(2) . . ? C43 C44 C45 177.9(4) . . ? C43 C44 Li1 57.7(2) . . ? C45 C44 Li1 124.0(3) . . ? C43 C44 Li2 56.5(2) . . ? C45 C44 Li2 125.1(3) . . ? Li1 C44 Li2 62.53(19) . . ? C44 C45 C46 109.9(3) . . ? C44 C45 C47 109.9(3) . . ? C46 C45 C47 110.4(4) . . ? C44 C45 C48 108.6(3) . . ? C46 C45 C48 109.4(4) . . ? C47 C45 C48 108.6(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 Li1 138.6(3) . . ? C50 C49 Li2 135.1(3) . . ? Li1 C49 Li2 79.5(2) . . ? C50 C49 Li3 123.0(3) . . ? Li1 C49 Li3 79.3(2) . . ? Li2 C49 Li3 78.2(2) . . ? C49 C50 C51 178.9(4) . . ? C52 C51 C53 111.3(4) . . ? C52 C51 C50 110.6(3) . . ? C53 C51 C50 111.6(3) . . ? C52 C51 C54 109.2(5) . . ? C53 C51 C54 107.6(4) . . ? C50 C51 C54 106.4(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O1 C55 C56 101.2(9) . . ? O1 C55 H55A 111.5 . . ? C56 C55 H55A 111.5 . . ? O1 C55 H55B 111.5 . . ? C56 C55 H55B 111.5 . . ? H55A C55 H55B 109.3 . . ? C57 C56 C55 110.5(9) . . ? C57 C56 H56A 109.6 . . ? C55 C56 H56A 109.6 . . ? C57 C56 H56B 109.6 . . ? C55 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? C56 C57 C58 99.3(11) . . ? C56 C57 H57A 111.9 . . ? C58 C57 H57A 111.9 . . ? C56 C57 H57B 111.9 . . ? C58 C57 H57B 111.9 . . ? H57A C57 H57B 109.6 . . ? O1 C58 C57 111.3(14) . . ? O1 C58 H58A 109.4 . . ? C57 C58 H58A 109.4 . . ? O1 C58 H58B 109.4 . . ? C57 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? O1 C55A C56A 106.1(9) . . ? O1 C55A H55C 110.5 . . ? C56A C55A H55C 110.5 . . ? O1 C55A H55D 110.5 . . ? C56A C55A H55D 110.5 . . ? H55C C55A H55D 108.7 . . ? C57A C56A C55A 103.7(7) . . ? C57A C56A H56C 111.0 . . ? C55A C56A H56C 111.0 . . ? C57A C56A H56D 111.0 . . ? C55A C56A H56D 111.0 . . ? H56C C56A H56D 109.0 . . ? C56A C57A C58A 108.7(9) . . ? C56A C57A H57C 109.9 . . ? C58A C57A H57C 109.9 . . ? C56A C57A H57D 109.9 . . ? C58A C57A H57D 109.9 . . ? H57C C57A H57D 108.3 . . ? O1 C58A C57A 101.6(11) . . ? O1 C58A H58C 111.4 . . ? C57A C58A H58C 111.4 . . ? O1 C58A H58D 111.4 . . ? C57A C58A H58D 111.4 . . ? H58C C58A H58D 109.3 . . ? O2 C59 C60 105.7(3) . . ? O2 C59 H59A 110.6 . . ? C60 C59 H59A 110.6 . . ? O2 C59 H59B 110.6 . . ? C60 C59 H59B 110.6 . . ? H59A C59 H59B 108.7 . . ? C59 C60 C61 102.1(3) . . ? C59 C60 H60A 111.4 . . ? C61 C60 H60A 111.4 . . ? C59 C60 H60B 111.4 . . ? C61 C60 H60B 111.4 . . ? H60A C60 H60B 109.2 . . ? C62 C61 C60 102.8(3) . . ? C62 C61 H61A 111.2 . . ? C60 C61 H61A 111.2 . . ? C62 C61 H61B 111.2 . . ? C60 C61 H61B 111.2 . . ? H61A C61 H61B 109.1 . . ? O2 C62 C61 106.0(3) . . ? O2 C62 H62A 110.5 . . ? C61 C62 H62A 110.5 . . ? O2 C62 H62B 110.5 . . ? C61 C62 H62B 110.5 . . ? H62A C62 H62B 108.7 . . ? C66 O3 C63 108.8(8) . . ? C66 O3 Li3 139.3(6) . . ? C63 O3 Li3 111.9(6) . . ? O3 C63 C64 105.5(6) . . ? O3 C63 H63A 110.6 . . ? C64 C63 H63A 110.6 . . ? O3 C63 H63B 110.6 . . ? C64 C63 H63B 110.6 . . ? H63A C63 H63B 108.8 . . ? C63 C64 C65 101.9(9) . . ? C63 C64 H64A 111.4 . . ? C65 C64 H64A 111.4 . . ? C63 C64 H64B 111.4 . . ? C65 C64 H64B 111.4 . . ? H64A C64 H64B 109.3 . . ? C66 C65 C64 99.3(10) . . ? C66 C65 H65A 111.9 . . ? C64 C65 H65A 111.9 . . ? C66 C65 H65B 111.9 . . ? C64 C65 H65B 111.9 . . ? H65A C65 H65B 109.6 . . ? O3 C66 C65 107.9(10) . . ? O3 C66 H66A 110.1 . . ? C65 C66 H66A 110.1 . . ? O3 C66 H66B 110.1 . . ? C65 C66 H66B 110.1 . . ? H66A C66 H66B 108.4 . . ? C63A O3A C66A 108.7(17) . . ? C63A O3A Li3 123.5(11) . . ? C66A O3A Li3 125.7(14) . . ? C64A C63A O3A 109(2) . . ? C64A C63A H63C 110.0 . . ? O3A C63A H63C 110.0 . . ? C64A C63A H63D 110.0 . . ? O3A C63A H63D 110.0 . . ? H63C C63A H63D 108.4 . . ? C63A C64A C65A 103(3) . . ? C63A C64A H64C 111.2 . . ? C65A C64A H64C 111.2 . . ? C63A C64A H64D 111.2 . . ? C65A C64A H64D 111.2 . . ? H64C C64A H64D 109.1 . . ? C66A C65A C64A 99.4(16) . . ? C66A C65A H65C 111.9 . . ? C64A C65A H65C 111.9 . . ? C66A C65A H65D 111.9 . . ? C64A C65A H65D 111.9 . . ? H65C C65A H65D 109.6 . . ? O3A C66A C65A 105.9(13) . . ? O3A C66A H66C 110.6 . . ? C65A C66A H66C 110.6 . . ? O3A C66A H66D 110.6 . . ? C65A C66A H66D 110.6 . . ? H66C C66A H66D 108.7 . . ? C71 O71 C74 105.5(7) . . ? O71 C71 C72 109.6(8) . . ? O71 C71 H71A 109.8 . . ? C72 C71 H71A 109.8 . . ? O71 C71 H71B 109.8 . . ? C72 C71 H71B 109.8 . . ? H71A C71 H71B 108.2 . . ? C73 C72 C71 103.6(8) . . ? C73 C72 H72A 111.0 . . ? C71 C72 H72A 111.0 . . ? C73 C72 H72B 111.0 . . ? C71 C72 H72B 111.0 . . ? H72A C72 H72B 109.0 . . ? C72 C73 C74 101.5(7) . . ? C72 C73 H73A 111.5 . . ? C74 C73 H73A 111.5 . . ? C72 C73 H73B 111.5 . . ? C74 C73 H73B 111.5 . . ? H73A C73 H73B 109.3 . . ? O71 C74 C73 105.8(7) . . ? O71 C74 H74A 110.6 . . ? C73 C74 H74A 110.6 . . ? O71 C74 H74B 110.6 . . ? C73 C74 H74B 110.6 . . ? H74A C74 H74B 108.7 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C81 127.5(17) . . ? C83 C82 H82A 105.4 . . ? C81 C82 H82A 105.4 . . ? C83 C82 H82B 105.4 . . ? C81 C82 H82B 105.4 . . ? H82A C82 H82B 106.0 . . ? C84 C83 C82 126.1(15) . . ? C84 C83 H83A 105.8 . . ? C82 C83 H83A 105.8 . . ? C84 C83 H83B 105.8 . . ? C82 C83 H83B 105.8 . . ? H83A C83 H83B 106.2 . . ? C83 C84 C85 133.8(16) . . ? C83 C84 H84A 103.8 . . ? C85 C84 H84A 103.8 . . ? C83 C84 H84B 103.8 . . ? C85 C84 H84B 103.8 . . ? H84A C84 H84B 105.4 . . ? C84 C85 C86 116.6(16) . . ? C84 C85 H85A 108.1 . . ? C86 C85 H85A 108.1 . . ? C84 C85 H85B 108.1 . . ? C86 C85 H85B 108.1 . . ? H85A C85 H85B 107.3 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.070 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.060 #===END data_cbn91fmi _database_code_depnum_ccdc_archive 'CCDC 794079' #TrackingRef 'CIF-Mn-010510.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H80 I Li3 Mn O3, C66 H78 I Li3 Mn O3' _chemical_formula_sum 'C132 H158 I2 Li6 Mn2 O6' _chemical_formula_weight 2245.90 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 61.658(9) _cell_length_b 13.1427(19) _cell_length_c 14.888(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12064(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9959 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.47 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4688 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8422 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details 'SADABS 2008/1 (Sheldrick, 2008)' _exptl_special_details ; A colorless needle with approximate orthogonal dimensions 0.23x0.09x0.07mm3 was placed and optically centered on the Bruker SMART APEXII(1) CCD system at -183\%C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide omega-scans, 10 seconds per frame, and 20 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 60 seconds per frame and 606 frames collected per series at varying phi angles (phi=0? 90? 180? 270?. The crystal to detector distance was 5.23cm, thus providing a complete sphere of data to 2ThetaMax=51.16? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 81535 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -74 _diffrn_reflns_limit_h_max 74 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.25 _reflns_number_total 21794 _reflns_number_gt 20084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.2-0) (Bruker, 2007)' _computing_cell_refinement 'SAINT (7.46A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.46A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. A total of 115871 reflections were collected and corrected for Lorentz and polarization effects and absorption using Blessing's method as incorporated into the program SADABS(2,3) with 23686 unique. The SHELXTL(4) program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences, and intensity statistics indicated the non-centrosymmetric orthorhombic space group Pna21 (no. 33). The structure was determined by direct methods with the successful location of a majority of the two different molecules of interest within the asymmetric unit using the program XS(5). A series of difference-Fourier maps were now implemented to locate the remaining non-hydrogen atoms. The main difference between the two molecules is that one possesses two THF molecules and one ether while the other has two ether molecules and one THF. The structure was refined with XL(5). The data collected were merged based upon identical indices yielding 86027 data [R(int)=0.0248] that were truncated to 2thetaMax=50.50?resulting in 81535 data that were further merged during least-squares refinement to 21794 unique data [R(int)=0.0365]. Hydrogen atoms were placed in idealized positions throughout. The final structure was refined to convergence with R(F)=4.05%, wR(F2)=8.34%, GOF=1.096 for all 21794 unique reflections [R(F)=3.53%, wR(F2)=8.17% for those 20084 data with Fo > 4 (Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be 1.5sigma and therefore not applied. The absolute structure parameter, Flack(x)(6), was refined and found to be -0.008(10) indicating that the correct enantiomorph has been chosen. References: 1. Bruker (2004) SMART APEX (Version 2.0.2) and SAINT (Version 7.46A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008) Version 2008/1, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. 6. On Enantiomorph-Polarity Estimation, Flack, H.D. (1983). Acta Cryst., A39, 876-881. PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.82 Ratio PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.66 Ratio PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.19 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.67 Ratio These are due to carbons of the coordinating diethyl ether or THF displaying large librational shifts, which may be also responsiable for some type C alert. Check High Ueq as Compared to Neighbors for C57 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C58 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C83 The large librational shifts of C57 and the direction is different from its neighboring carbons. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C31 - C32 ... 1.21 Ang. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C39 - C40 ... 1.21 Ang. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C47 - C48 ... 1.20 Ang. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C101 - C102 ... 1.21 Ang. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C109 - C110 ... 1.21 Ang. PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C117 - C118 ... 1.21 Ang. These are the C-C triple bonds of the phenyl acetylide ligands. PLAT412_ALERT_2_B Short Intra XH3 .. XHn H59A .. H62C .. 1.76 Ang. The hydrogen atoms are placed at the calulated positions. The short distance is due to the librational shift of the cooridination diethyl ether carbon atoms. ; _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^)+(0.0324P)^2^+13.4718P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(10) _refine_ls_number_reflns 21794 _refine_ls_number_parameters 1354 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.006 _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 0.691137(8) 0.13176(4) 0.21611(4) 0.02206(12) Uani 1 1 d . . . I1 I 0.646530(4) 0.110110(19) -0.030254(18) 0.02966(6) Uani 1 1 d . . . Li1 Li 0.66567(11) -0.0174(5) 0.0963(5) 0.0339(15) Uani 1 1 d . . . Li2 Li 0.64933(12) 0.2102(6) 0.1391(5) 0.0376(16) Uani 1 1 d . . . Li3 Li 0.69034(12) 0.1687(5) 0.0108(5) 0.0350(16) Uani 1 1 d . . . O1 O 0.65836(5) -0.1544(2) 0.0806(2) 0.0421(8) Uani 1 1 d . . . O2 O 0.62380(5) 0.2887(3) 0.1478(3) 0.0639(11) Uani 1 1 d . . . O3 O 0.70515(5) 0.2197(2) -0.09318(19) 0.0376(7) Uani 1 1 d . . . C1 C 0.70832(5) 0.1430(3) 0.3412(3) 0.0220(8) Uani 1 1 d . . . C2 C 0.72143(6) 0.0636(3) 0.3747(2) 0.0220(8) Uani 1 1 d . . . C3 C 0.73180(6) 0.0714(3) 0.4580(3) 0.0272(8) Uani 1 1 d . . . H3 H 0.7405 0.0165 0.4789 0.033 Uiso 1 1 calc R . . C4 C 0.72967(6) 0.1571(3) 0.5101(3) 0.0300(9) Uani 1 1 d . . . H4 H 0.7368 0.1618 0.5665 0.036 Uiso 1 1 calc R . . C5 C 0.71704(6) 0.2363(3) 0.4794(3) 0.0282(8) Uani 1 1 d . . . H5 H 0.7156 0.2961 0.5148 0.034 Uiso 1 1 calc R . . C6 C 0.70617(6) 0.2297(3) 0.3964(2) 0.0229(8) Uani 1 1 d . . . C7 C 0.72398(5) -0.0347(3) 0.3240(2) 0.0215(8) Uani 1 1 d . . . C8 C 0.71080(6) -0.1191(3) 0.3457(3) 0.0294(8) Uani 1 1 d . . . C9 C 0.71403(6) -0.2108(3) 0.3014(3) 0.0325(9) Uani 1 1 d . . . H9 H 0.7055 -0.2682 0.3170 0.039 Uiso 1 1 calc R . . C10 C 0.72953(6) -0.2196(3) 0.2350(3) 0.0328(9) Uani 1 1 d . . . H10 H 0.7314 -0.2825 0.2046 0.039 Uiso 1 1 calc R . . C11 C 0.74220(6) -0.1374(3) 0.2128(3) 0.0284(8) Uani 1 1 d . . . H11 H 0.7528 -0.1443 0.1668 0.034 Uiso 1 1 calc R . . C12 C 0.73992(5) -0.0448(3) 0.2561(2) 0.0212(8) Uani 1 1 d . . . C13 C 0.69354(7) -0.1130(3) 0.4189(3) 0.0372(10) Uani 1 1 d . . . H13 H 0.6908 -0.0394 0.4316 0.045 Uiso 1 1 calc R . . C14 C 0.70130(8) -0.1623(4) 0.5063(3) 0.0520(13) Uani 1 1 d . . . H14A H 0.7048 -0.2340 0.4952 0.078 Uiso 1 1 calc R . . H14B H 0.6898 -0.1577 0.5516 0.078 Uiso 1 1 calc R . . H14C H 0.7143 -0.1269 0.5279 0.078 Uiso 1 1 calc R . . C15 C 0.67207(7) -0.1600(4) 0.3888(4) 0.0485(13) Uani 1 1 d . . . H15A H 0.6742 -0.2323 0.3754 0.073 Uiso 1 1 calc R . . H15B H 0.6669 -0.1249 0.3348 0.073 Uiso 1 1 calc R . . H15C H 0.6613 -0.1528 0.4368 0.073 Uiso 1 1 calc R . . C16 C 0.75542(6) 0.0416(3) 0.2343(3) 0.0267(8) Uani 1 1 d . . . H16 H 0.7483 0.1068 0.2523 0.032 Uiso 1 1 calc R . . C17 C 0.76099(7) 0.0490(4) 0.1358(3) 0.0416(11) Uani 1 1 d . . . H17A H 0.7704 -0.0080 0.1190 0.062 Uiso 1 1 calc R . . H17B H 0.7685 0.1133 0.1243 0.062 Uiso 1 1 calc R . . H17C H 0.7476 0.0465 0.1001 0.062 Uiso 1 1 calc R . . C18 C 0.77613(7) 0.0306(3) 0.2899(3) 0.0373(10) Uani 1 1 d . . . H18A H 0.7724 0.0260 0.3537 0.056 Uiso 1 1 calc R . . H18B H 0.7855 0.0899 0.2799 0.056 Uiso 1 1 calc R . . H18C H 0.7838 -0.0313 0.2716 0.056 Uiso 1 1 calc R . . C19 C 0.69239(6) 0.3181(3) 0.3681(2) 0.0259(8) Uani 1 1 d . . . C20 C 0.70185(6) 0.4033(3) 0.3260(3) 0.0291(9) Uani 1 1 d . . . C21 C 0.68817(7) 0.4840(3) 0.3004(3) 0.0379(10) Uani 1 1 d . . . H21 H 0.6943 0.5420 0.2722 0.046 Uiso 1 1 calc R . . C22 C 0.66654(8) 0.4814(4) 0.3149(3) 0.0409(11) Uani 1 1 d . . . H22 H 0.6577 0.5369 0.2964 0.049 Uiso 1 1 calc R . . C23 C 0.65716(7) 0.3979(3) 0.3568(3) 0.0376(10) Uani 1 1 d . . . H23 H 0.6419 0.3969 0.3668 0.045 Uiso 1 1 calc R . . C24 C 0.66970(7) 0.3158(3) 0.3844(3) 0.0298(9) Uani 1 1 d . . . C25 C 0.72586(7) 0.4116(3) 0.3107(3) 0.0330(9) Uani 1 1 d . . . H25 H 0.7325 0.3448 0.3271 0.040 Uiso 1 1 calc R . . C26 C 0.73171(8) 0.4339(4) 0.2124(3) 0.0488(12) Uani 1 1 d . . . H26A H 0.7246 0.3839 0.1733 0.073 Uiso 1 1 calc R . . H26B H 0.7475 0.4295 0.2047 0.073 Uiso 1 1 calc R . . H26C H 0.7268 0.5024 0.1964 0.073 Uiso 1 1 calc R . . C27 C 0.73601(8) 0.4937(3) 0.3715(3) 0.0466(12) Uani 1 1 d . . . H27A H 0.7298 0.5603 0.3565 0.070 Uiso 1 1 calc R . . H27B H 0.7517 0.4953 0.3622 0.070 Uiso 1 1 calc R . . H27C H 0.7329 0.4778 0.4345 0.070 Uiso 1 1 calc R . . C28 C 0.65960(6) 0.2310(3) 0.4386(3) 0.0334(10) Uani 1 1 d . . . H28 H 0.6680 0.1673 0.4271 0.040 Uiso 1 1 calc R . . C29 C 0.63574(7) 0.2101(4) 0.4162(3) 0.0460(12) Uani 1 1 d . . . H29A H 0.6269 0.2684 0.4347 0.069 Uiso 1 1 calc R . . H29B H 0.6309 0.1491 0.4483 0.069 Uiso 1 1 calc R . . H29C H 0.6342 0.1995 0.3514 0.069 Uiso 1 1 calc R . . C30 C 0.66128(8) 0.2563(4) 0.5390(3) 0.0428(11) Uani 1 1 d . . . H30A H 0.6766 0.2632 0.5557 0.064 Uiso 1 1 calc R . . H30B H 0.6547 0.2015 0.5741 0.064 Uiso 1 1 calc R . . H30C H 0.6537 0.3203 0.5511 0.064 Uiso 1 1 calc R . . C31 C 0.70058(6) 0.0379(3) 0.1019(3) 0.0261(8) Uani 1 1 d . . . C32 C 0.70389(6) -0.0135(3) 0.0361(3) 0.0261(9) Uani 1 1 d . . . C33 C 0.70873(6) -0.0770(3) -0.0417(3) 0.0283(8) Uani 1 1 d . . . C34 C 0.72240(6) -0.1608(3) -0.0346(3) 0.0294(8) Uani 1 1 d . . . H34 H 0.7285 -0.1781 0.0219 0.035 Uiso 1 1 calc R . . C35 C 0.72711(7) -0.2187(3) -0.1092(3) 0.0340(9) Uani 1 1 d . . . H35 H 0.7364 -0.2759 -0.1036 0.041 Uiso 1 1 calc R . . C36 C 0.71845(7) -0.1947(3) -0.1914(3) 0.0403(11) Uani 1 1 d . . . H36 H 0.7218 -0.2352 -0.2425 0.048 Uiso 1 1 calc R . . C37 C 0.70504(8) -0.1123(4) -0.1997(3) 0.0538(14) Uani 1 1 d . . . H37 H 0.6991 -0.0958 -0.2567 0.065 Uiso 1 1 calc R . . C38 C 0.70009(8) -0.0527(4) -0.1257(3) 0.0489(13) Uani 1 1 d . . . H38 H 0.6908 0.0046 -0.1321 0.059 Uiso 1 1 calc R . . C39 C 0.65840(6) 0.0711(3) 0.2250(3) 0.0282(8) Uani 1 1 d . . . C40 C 0.64083(6) 0.0307(3) 0.2263(3) 0.0288(8) Uani 1 1 d . . . C41 C 0.61951(6) -0.0155(3) 0.2359(3) 0.0287(9) Uani 1 1 d . . . C42 C 0.60522(8) -0.0262(4) 0.1659(3) 0.0524(13) Uani 1 1 d . . . H42 H 0.6094 -0.0050 0.1074 0.063 Uiso 1 1 calc R . . C43 C 0.58476(8) -0.0674(4) 0.1791(4) 0.0584(15) Uani 1 1 d . . . H43 H 0.5748 -0.0710 0.1306 0.070 Uiso 1 1 calc R . . C44 C 0.57896(7) -0.1030(4) 0.2621(3) 0.0461(12) Uani 1 1 d . . . H44 H 0.5651 -0.1327 0.2711 0.055 Uiso 1 1 calc R . . C45 C 0.59319(8) -0.0956(4) 0.3319(3) 0.0528(13) Uani 1 1 d . . . H45 H 0.5893 -0.1207 0.3895 0.063 Uiso 1 1 calc R . . C46 C 0.61338(7) -0.0512(4) 0.3186(3) 0.0438(11) Uani 1 1 d . . . H46 H 0.6231 -0.0454 0.3677 0.053 Uiso 1 1 calc R . . C47 C 0.68382(6) 0.2667(3) 0.1351(3) 0.0260(8) Uani 1 1 d . . . C48 C 0.68047(6) 0.3347(3) 0.0836(3) 0.0281(9) Uani 1 1 d . . . C49 C 0.67718(7) 0.4200(3) 0.0221(3) 0.0326(9) Uani 1 1 d . . . C50 C 0.68978(9) 0.5062(4) 0.0288(3) 0.0478(12) Uani 1 1 d . . . H50 H 0.7004 0.5119 0.0748 0.057 Uiso 1 1 calc R . . C51 C 0.68684(9) 0.5850(4) -0.0324(4) 0.0602(14) Uani 1 1 d . . . H51 H 0.6957 0.6440 -0.0282 0.072 Uiso 1 1 calc R . . C52 C 0.67169(10) 0.5796(4) -0.0979(4) 0.0597(15) Uani 1 1 d . . . H52 H 0.6698 0.6343 -0.1388 0.072 Uiso 1 1 calc R . . C53 C 0.65948(10) 0.4958(5) -0.1039(4) 0.0730(19) Uani 1 1 d . . . H53 H 0.6488 0.4918 -0.1498 0.088 Uiso 1 1 calc R . . C54 C 0.66188(8) 0.4155(4) -0.0461(4) 0.0611(15) Uani 1 1 d . . . H54 H 0.6531 0.3566 -0.0527 0.073 Uiso 1 1 calc R . . C55 C 0.66785(13) -0.2260(4) 0.1364(5) 0.086(2) Uani 1 1 d . . . H55A H 0.6729 -0.1943 0.1929 0.104 Uiso 1 1 calc R . . H55B H 0.6803 -0.2594 0.1064 0.104 Uiso 1 1 calc R . . C56 C 0.64998(19) -0.3006(8) 0.1541(7) 0.143(4) Uani 1 1 d U . . H56A H 0.6442 -0.2918 0.2157 0.171 Uiso 1 1 calc R . . H56B H 0.6553 -0.3712 0.1475 0.171 Uiso 1 1 calc R . . C57 C 0.6311(2) -0.2759(9) 0.0788(6) 0.165(5) Uani 1 1 d U . . H57A H 0.6272 -0.3374 0.0438 0.198 Uiso 1 1 calc R . . H57B H 0.6179 -0.2474 0.1069 0.198 Uiso 1 1 calc R . . C58 C 0.64268(10) -0.1973(4) 0.0207(4) 0.0570(15) Uani 1 1 d . . . H58A H 0.6498 -0.2298 -0.0315 0.068 Uiso 1 1 calc R . . H58B H 0.6324 -0.1447 -0.0011 0.068 Uiso 1 1 calc R . . C59 C 0.60282(10) 0.2431(6) 0.1328(7) 0.101(3) Uani 1 1 d U . . H59A H 0.5958 0.2786 0.0819 0.121 Uiso 1 1 calc R . . H59B H 0.6050 0.1714 0.1145 0.121 Uiso 1 1 calc R . . C60 C 0.58861(15) 0.2446(7) 0.2056(6) 0.120(3) Uani 1 1 d U . . H60A H 0.5967 0.2314 0.2611 0.179 Uiso 1 1 calc R . . H60B H 0.5775 0.1921 0.1975 0.179 Uiso 1 1 calc R . . H60C H 0.5816 0.3115 0.2094 0.179 Uiso 1 1 calc R . . C61 C 0.62336(9) 0.3975(4) 0.1533(4) 0.0536(13) Uani 1 1 d . . . H61A H 0.6384 0.4237 0.1524 0.064 Uiso 1 1 calc R . . H61B H 0.6167 0.4179 0.2111 0.064 Uiso 1 1 calc R . . C62 C 0.61113(14) 0.4435(6) 0.0792(4) 0.103(3) Uani 1 1 d . . . H62A H 0.6189 0.4320 0.0225 0.155 Uiso 1 1 calc R . . H62B H 0.6097 0.5168 0.0896 0.155 Uiso 1 1 calc R . . H62C H 0.5967 0.4126 0.0758 0.155 Uiso 1 1 calc R . . C63 C 0.73696(7) 0.2432(4) -0.0062(3) 0.0519(13) Uani 1 1 d . . . H63A H 0.7285 0.2459 0.0495 0.078 Uiso 1 1 calc R . . H63B H 0.7501 0.2844 0.0006 0.078 Uiso 1 1 calc R . . H63C H 0.7410 0.1726 -0.0190 0.078 Uiso 1 1 calc R . . C64 C 0.72396(8) 0.2833(4) -0.0801(3) 0.0501(12) Uani 1 1 d . . . H64A H 0.7193 0.3537 -0.0662 0.060 Uiso 1 1 calc R . . H64B H 0.7327 0.2848 -0.1357 0.060 Uiso 1 1 calc R . . C65 C 0.69426(9) 0.2415(6) -0.1770(4) 0.0721(19) Uani 1 1 d . . . H65A H 0.6928 0.3161 -0.1834 0.087 Uiso 1 1 calc R . . H65B H 0.6795 0.2123 -0.1747 0.087 Uiso 1 1 calc R . . C66 C 0.70541(14) 0.2014(7) -0.2563(4) 0.120(4) Uani 1 1 d U . . H66A H 0.7194 0.2359 -0.2633 0.180 Uiso 1 1 calc R . . H66B H 0.6965 0.2134 -0.3097 0.180 Uiso 1 1 calc R . . H66C H 0.7078 0.1282 -0.2489 0.180 Uiso 1 1 calc R . . Mn71 Mn 0.557696(8) 0.69283(4) 0.60339(4) 0.02190(12) Uani 1 1 d . . . I71 I 0.603105(4) 0.662043(18) 0.852279(18) 0.03044(6) Uani 1 1 d . . . Li71 Li 0.56371(12) 0.5793(6) 0.7799(5) 0.0366(16) Uani 1 1 d . . . Li72 Li 0.60492(10) 0.6438(5) 0.6600(5) 0.0344(16) Uani 1 1 d . . . Li73 Li 0.57792(10) 0.8080(5) 0.7653(5) 0.0324(15) Uani 1 1 d . . . O71 O 0.55104(5) 0.4749(3) 0.8517(3) 0.0537(8) Uani 1 1 d . . . O72 O 0.63409(4) 0.6137(2) 0.6267(2) 0.0389(7) Uani 1 1 d . . . O73 O 0.58083(4) 0.9308(2) 0.82821(17) 0.0315(6) Uani 1 1 d . . . C71 C 0.53907(5) 0.7200(3) 0.4845(3) 0.0228(8) Uani 1 1 d . . . C72 C 0.53988(6) 0.6531(3) 0.4099(3) 0.0256(8) Uani 1 1 d . . . C73 C 0.52952(7) 0.6733(3) 0.3294(3) 0.0310(9) Uani 1 1 d . . . H73 H 0.5311 0.6275 0.2805 0.037 Uiso 1 1 calc R . . C74 C 0.51686(6) 0.7601(3) 0.3195(3) 0.0291(9) Uani 1 1 d . . . H74 H 0.5095 0.7736 0.2647 0.035 Uiso 1 1 calc R . . C75 C 0.51520(6) 0.8268(3) 0.3916(3) 0.0274(8) Uani 1 1 d . . . H75 H 0.5065 0.8860 0.3862 0.033 Uiso 1 1 calc R . . C76 C 0.52612(5) 0.8082(2) 0.4718(3) 0.0219(7) Uani 1 1 d . . . C77 C 0.55217(8) 0.5526(3) 0.4163(3) 0.0366(10) Uani 1 1 d . . . C78 C 0.54071(9) 0.4667(3) 0.4459(3) 0.0459(13) Uani 1 1 d . . . C79 C 0.55154(12) 0.3726(4) 0.4476(3) 0.0590(16) Uani 1 1 d . . . H79 H 0.5441 0.3135 0.4677 0.071 Uiso 1 1 calc R . . C80 C 0.57287(14) 0.3658(4) 0.4201(4) 0.075(2) Uani 1 1 d . . . H80 H 0.5800 0.3016 0.4205 0.090 Uiso 1 1 calc R . . C81 C 0.58384(11) 0.4501(4) 0.3922(3) 0.0644(17) Uani 1 1 d . . . H81 H 0.5986 0.4442 0.3744 0.077 Uiso 1 1 calc R . . C82 C 0.57371(9) 0.5451(4) 0.3895(3) 0.0492(13) Uani 1 1 d . . . C83 C 0.51748(9) 0.4715(3) 0.4738(3) 0.0500(12) Uani 1 1 d . . . H83 H 0.5123 0.5426 0.4629 0.060 Uiso 1 1 calc R . . C84 C 0.51452(13) 0.4488(7) 0.5742(4) 0.103(3) Uani 1 1 d . . . H84A H 0.5196 0.3797 0.5871 0.154 Uiso 1 1 calc R . . H84B H 0.4991 0.4545 0.5899 0.154 Uiso 1 1 calc R . . H84C H 0.5229 0.4978 0.6096 0.154 Uiso 1 1 calc R . . C85 C 0.50336(13) 0.4006(5) 0.4174(6) 0.101(3) Uani 1 1 d . . . H85A H 0.5038 0.4224 0.3545 0.151 Uiso 1 1 calc R . . H85B H 0.4884 0.4031 0.4394 0.151 Uiso 1 1 calc R . . H85C H 0.5089 0.3309 0.4222 0.151 Uiso 1 1 calc R . . C86 C 0.58596(8) 0.6369(4) 0.3548(4) 0.0574(14) Uani 1 1 d . . . H86 H 0.5774 0.6989 0.3710 0.069 Uiso 1 1 calc R . . C87 C 0.58733(13) 0.6322(5) 0.2517(4) 0.087(2) Uani 1 1 d . . . H87A H 0.5971 0.5770 0.2339 0.130 Uiso 1 1 calc R . . H87B H 0.5929 0.6970 0.2286 0.130 Uiso 1 1 calc R . . H87C H 0.5729 0.6196 0.2268 0.130 Uiso 1 1 calc R . . C88 C 0.60879(9) 0.6493(6) 0.3953(5) 0.088(2) Uani 1 1 d . . . H88A H 0.6077 0.6561 0.4606 0.132 Uiso 1 1 calc R . . H88B H 0.6157 0.7102 0.3703 0.132 Uiso 1 1 calc R . . H88C H 0.6176 0.5894 0.3806 0.132 Uiso 1 1 calc R . . C89 C 0.52296(6) 0.8833(3) 0.5472(3) 0.0242(8) Uani 1 1 d . . . C90 C 0.53559(6) 0.9727(3) 0.5517(3) 0.0248(8) Uani 1 1 d . . . C91 C 0.53194(7) 1.0407(3) 0.6210(3) 0.0351(10) Uani 1 1 d . . . H91 H 0.5403 1.1013 0.6240 0.042 Uiso 1 1 calc R . . C92 C 0.51649(7) 1.0226(3) 0.6854(3) 0.0380(11) Uani 1 1 d . . . H92 H 0.5146 1.0693 0.7334 0.046 Uiso 1 1 calc R . . C93 C 0.50368(7) 0.9363(3) 0.6805(3) 0.0329(9) Uani 1 1 d . . . H93 H 0.4928 0.9250 0.7246 0.039 Uiso 1 1 calc R . . C94 C 0.50658(6) 0.8661(3) 0.6117(3) 0.0270(8) Uani 1 1 d . . . C95 C 0.55210(6) 0.9976(3) 0.4792(3) 0.0309(9) Uani 1 1 d . . . H95 H 0.5565 0.9320 0.4506 0.037 Uiso 1 1 calc R . . C96 C 0.54216(8) 1.0645(3) 0.4056(3) 0.0415(11) Uani 1 1 d . . . H96A H 0.5302 1.0280 0.3768 0.062 Uiso 1 1 calc R . . H96B H 0.5533 1.0806 0.3606 0.062 Uiso 1 1 calc R . . H96C H 0.5367 1.1277 0.4323 0.062 Uiso 1 1 calc R . . C97 C 0.57266(7) 1.0485(3) 0.5152(3) 0.0416(11) Uani 1 1 d . . . H97A H 0.5689 1.1131 0.5440 0.062 Uiso 1 1 calc R . . H97B H 0.5827 1.0614 0.4654 0.062 Uiso 1 1 calc R . . H97C H 0.5796 1.0037 0.5592 0.062 Uiso 1 1 calc R . . C98 C 0.49106(6) 0.7770(3) 0.6041(3) 0.0326(9) Uani 1 1 d . . . H98 H 0.4978 0.7253 0.5633 0.039 Uiso 1 1 calc R . . C99 C 0.46990(7) 0.8136(4) 0.5605(4) 0.0494(12) Uani 1 1 d . . . H99A H 0.4596 0.7570 0.5576 0.074 Uiso 1 1 calc R . . H99B H 0.4729 0.8382 0.4996 0.074 Uiso 1 1 calc R . . H99C H 0.4637 0.8689 0.5964 0.074 Uiso 1 1 calc R . . C100 C 0.48630(7) 0.7256(4) 0.6934(3) 0.0468(12) Uani 1 1 d . . . H10A H 0.4791 0.7740 0.7336 0.070 Uiso 1 1 calc R . . H10B H 0.4999 0.7029 0.7207 0.070 Uiso 1 1 calc R . . H10C H 0.4768 0.6668 0.6834 0.070 Uiso 1 1 calc R . . C101 C 0.54577(6) 0.7214(3) 0.7396(3) 0.0275(9) Uani 1 1 d . . . C102 C 0.54243(6) 0.7480(3) 0.8158(3) 0.0238(8) Uani 1 1 d . . . C103 C 0.53781(6) 0.7847(3) 0.9055(3) 0.0241(8) Uani 1 1 d . . . C104 C 0.52220(6) 0.8604(3) 0.9185(3) 0.0275(9) Uani 1 1 d . . . H104 H 0.5146 0.8876 0.8686 0.033 Uiso 1 1 calc R . . C105 C 0.51788(7) 0.8957(3) 1.0043(3) 0.0337(10) Uani 1 1 d . . . H105 H 0.5075 0.9483 1.0126 0.040 Uiso 1 1 calc R . . C106 C 0.52851(6) 0.8553(3) 1.0780(3) 0.0319(9) Uani 1 1 d . . . H106 H 0.5253 0.8795 1.1367 0.038 Uiso 1 1 calc R . . C107 C 0.54368(7) 0.7803(3) 1.0660(3) 0.0319(9) Uani 1 1 d . . . H107 H 0.5509 0.7520 1.1165 0.038 Uiso 1 1 calc R . . C108 C 0.54858(6) 0.7456(3) 0.9799(3) 0.0293(9) Uani 1 1 d . . . H108 H 0.5594 0.6947 0.9720 0.035 Uiso 1 1 calc R . . C109 C 0.58627(6) 0.7871(3) 0.6175(3) 0.0298(9) Uani 1 1 d . . . C110 C 0.60224(6) 0.8374(3) 0.6324(3) 0.0261(8) Uani 1 1 d . . . C111 C 0.62197(6) 0.8975(3) 0.6434(3) 0.0264(8) Uani 1 1 d . . . C112 C 0.63129(7) 0.9142(4) 0.7279(3) 0.0414(11) Uani 1 1 d . . . H112 H 0.6244 0.8894 0.7806 0.050 Uiso 1 1 calc R . . C113 C 0.65081(7) 0.9676(4) 0.7340(4) 0.0540(15) Uani 1 1 d . . . H113 H 0.6573 0.9779 0.7911 0.065 Uiso 1 1 calc R . . C114 C 0.66065(7) 1.0051(4) 0.6592(4) 0.0502(14) Uani 1 1 d . . . H114 H 0.6739 1.0414 0.6643 0.060 Uiso 1 1 calc R . . C115 C 0.65132(8) 0.9902(4) 0.5759(4) 0.0491(12) Uani 1 1 d . . . H115 H 0.6581 1.0164 0.5236 0.059 Uiso 1 1 calc R . . C116 C 0.63203(7) 0.9371(3) 0.5688(3) 0.0376(10) Uani 1 1 d . . . H116 H 0.6256 0.9278 0.5113 0.045 Uiso 1 1 calc R . . C117 C 0.57428(7) 0.5500(3) 0.6357(3) 0.0304(9) Uani 1 1 d . . . C118 C 0.58451(7) 0.4760(3) 0.6599(3) 0.0326(9) Uani 1 1 d . . . C119 C 0.59615(6) 0.3848(3) 0.6883(3) 0.0311(9) Uani 1 1 d . . . C120 C 0.59752(6) 0.3020(3) 0.6309(3) 0.0329(9) Uani 1 1 d . . . H120 H 0.5911 0.3048 0.5728 0.039 Uiso 1 1 calc R . . C121 C 0.60841(7) 0.2142(3) 0.6593(3) 0.0393(10) Uani 1 1 d . . . H121 H 0.6092 0.1568 0.6206 0.047 Uiso 1 1 calc R . . C122 C 0.61796(8) 0.2101(3) 0.7422(3) 0.0458(12) Uani 1 1 d . . . H122 H 0.6258 0.1512 0.7599 0.055 Uiso 1 1 calc R . . C123 C 0.61618(9) 0.2908(4) 0.7993(4) 0.0584(15) Uani 1 1 d . . . H123 H 0.6225 0.2873 0.8574 0.070 Uiso 1 1 calc R . . C124 C 0.60525(9) 0.3776(4) 0.7734(4) 0.0568(15) Uani 1 1 d . . . H124 H 0.6039 0.4329 0.8142 0.068 Uiso 1 1 calc R . . C125 C 0.58813(8) 0.9510(4) 0.9186(3) 0.0423(11) Uani 1 1 d . . . H12A H 0.6036 0.9707 0.9186 0.051 Uiso 1 1 calc R . . H12B H 0.5864 0.8898 0.9566 0.051 Uiso 1 1 calc R . . C126 C 0.57487(10) 1.0339(5) 0.9526(4) 0.0663(17) Uani 1 1 d . . . H12C H 0.5833 1.0778 0.9938 0.080 Uiso 1 1 calc R . . H12D H 0.5620 1.0075 0.9849 0.080 Uiso 1 1 calc R . . C127 C 0.56817(10) 1.0924(4) 0.8683(5) 0.0723(19) Uani 1 1 d . . . H12E H 0.5528 1.1142 0.8724 0.087 Uiso 1 1 calc R . . H12F H 0.5774 1.1534 0.8602 0.087 Uiso 1 1 calc R . . C128 C 0.57120(11) 1.0206(4) 0.7929(4) 0.0660(17) Uani 1 1 d . . . H12G H 0.5570 1.0044 0.7649 0.079 Uiso 1 1 calc R . . H12H H 0.5807 1.0511 0.7466 0.079 Uiso 1 1 calc R . . C129 C 0.56010(10) 0.4370(5) 0.9346(4) 0.0720(18) Uani 1 1 d . . . H12I H 0.5746 0.4678 0.9434 0.086 Uiso 1 1 calc R . . H12J H 0.5621 0.3625 0.9293 0.086 Uiso 1 1 calc R . . C130 C 0.54623(13) 0.4590(6) 1.0171(5) 0.091(2) Uani 1 1 d . . . H13A H 0.5445 0.5327 1.0240 0.136 Uiso 1 1 calc R . . H13B H 0.5533 0.4310 1.0706 0.136 Uiso 1 1 calc R . . H13C H 0.5319 0.4275 1.0097 0.136 Uiso 1 1 calc R . . C131 C 0.53348(9) 0.4149(5) 0.8155(4) 0.0667(16) Uani 1 1 d . . . H13D H 0.5246 0.4586 0.7758 0.080 Uiso 1 1 calc R . . H13E H 0.5241 0.3919 0.8656 0.080 Uiso 1 1 calc R . . C132 C 0.54070(11) 0.3252(5) 0.7642(6) 0.091(2) Uani 1 1 d . . . H13F H 0.5516 0.3460 0.7198 0.137 Uiso 1 1 calc R . . H13G H 0.5283 0.2948 0.7334 0.137 Uiso 1 1 calc R . . H13H H 0.5471 0.2753 0.8053 0.137 Uiso 1 1 calc R . . C133 C 0.64183(8) 0.5229(5) 0.5869(5) 0.0732(19) Uani 1 1 d . . . H13I H 0.6335 0.5061 0.5320 0.088 Uiso 1 1 calc R . . H13J H 0.6409 0.4651 0.6294 0.088 Uiso 1 1 calc R . . C134 C 0.66568(9) 0.5485(6) 0.5642(5) 0.090(2) Uani 1 1 d . . . H13K H 0.6746 0.4861 0.5604 0.109 Uiso 1 1 calc R . . H13L H 0.6668 0.5863 0.5068 0.109 Uiso 1 1 calc R . . C135 C 0.67215(8) 0.6112(4) 0.6393(4) 0.0623(15) Uani 1 1 d . . . H13M H 0.6849 0.6534 0.6240 0.075 Uiso 1 1 calc R . . H13N H 0.6756 0.5692 0.6926 0.075 Uiso 1 1 calc R . . C136 C 0.65269(9) 0.6757(4) 0.6555(5) 0.0621(15) Uani 1 1 d . . . H13O H 0.6515 0.6934 0.7199 0.075 Uiso 1 1 calc R . . H13P H 0.6535 0.7393 0.6201 0.075 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 0.0193(3) 0.0243(3) 0.0226(3) -0.0023(2) -0.0019(2) 0.0006(2) I1 0.02347(11) 0.03725(13) 0.02827(12) 0.00339(12) -0.00610(11) -0.00257(10) Li1 0.030(3) 0.045(4) 0.026(3) -0.005(3) -0.011(3) -0.003(3) Li2 0.032(4) 0.034(4) 0.046(4) 0.001(3) 0.001(3) 0.005(3) Li3 0.039(4) 0.037(4) 0.029(4) 0.003(3) 0.003(3) -0.007(3) O1 0.0508(19) 0.0308(15) 0.0446(19) -0.0060(14) -0.0207(15) 0.0020(14) O2 0.0315(18) 0.045(2) 0.115(3) -0.001(2) 0.0096(19) 0.0137(16) O3 0.0338(16) 0.0532(19) 0.0258(16) 0.0005(14) 0.0010(13) -0.0147(14) C1 0.0156(16) 0.0279(19) 0.022(2) -0.0002(16) 0.0032(15) -0.0010(13) C2 0.0193(17) 0.0254(18) 0.021(2) 0.0024(14) 0.0021(14) 0.0005(14) C3 0.0237(18) 0.0306(19) 0.027(2) 0.0029(17) -0.0027(16) 0.0037(15) C4 0.026(2) 0.038(2) 0.026(2) -0.0012(18) -0.0075(16) 0.0016(17) C5 0.0288(19) 0.0309(19) 0.025(2) -0.0096(18) 0.0002(17) 0.0031(16) C6 0.0153(17) 0.030(2) 0.0234(19) -0.0002(16) 0.0002(15) 0.0012(15) C7 0.0136(16) 0.0244(18) 0.026(2) 0.0002(15) -0.0058(14) 0.0052(14) C8 0.0243(18) 0.0271(18) 0.037(2) 0.0036(19) -0.0001(18) 0.0021(15) C9 0.0194(19) 0.026(2) 0.053(3) 0.0031(19) 0.0010(18) 0.0000(16) C10 0.025(2) 0.027(2) 0.047(3) -0.0055(18) -0.0093(18) 0.0050(16) C11 0.0206(18) 0.032(2) 0.033(2) -0.0031(17) -0.0031(17) 0.0076(16) C12 0.0130(16) 0.0232(19) 0.027(2) -0.0014(15) -0.0021(14) 0.0031(14) C13 0.026(2) 0.035(2) 0.050(3) 0.009(2) 0.0076(19) 0.0010(18) C14 0.048(3) 0.054(3) 0.053(3) 0.018(2) 0.016(2) 0.005(2) C15 0.031(2) 0.045(3) 0.069(3) 0.009(2) 0.010(2) -0.002(2) C16 0.0260(19) 0.0267(19) 0.027(2) -0.0003(16) 0.0049(16) 0.0018(16) C17 0.031(2) 0.055(3) 0.038(3) 0.006(2) 0.0011(19) -0.004(2) C18 0.029(2) 0.034(2) 0.049(3) -0.003(2) -0.0041(19) -0.0026(18) C19 0.034(2) 0.0237(18) 0.020(2) -0.0058(15) -0.0049(16) 0.0059(15) C20 0.032(2) 0.030(2) 0.026(2) -0.0073(16) -0.0062(16) 0.0043(17) C21 0.050(3) 0.029(2) 0.035(2) -0.0052(18) -0.005(2) 0.006(2) C22 0.047(3) 0.040(3) 0.036(2) -0.002(2) -0.010(2) 0.022(2) C23 0.033(2) 0.046(2) 0.034(2) -0.009(2) -0.005(2) 0.0142(18) C24 0.032(2) 0.029(2) 0.029(2) -0.0092(16) -0.0041(16) 0.0066(17) C25 0.034(2) 0.027(2) 0.038(2) -0.0003(18) -0.0045(18) -0.0040(17) C26 0.045(3) 0.058(3) 0.044(3) -0.002(2) 0.001(2) -0.013(2) C27 0.050(3) 0.038(2) 0.052(3) -0.006(2) -0.018(2) -0.005(2) C28 0.023(2) 0.034(2) 0.044(3) -0.0077(19) 0.0021(17) 0.0054(17) C29 0.027(2) 0.057(3) 0.054(3) -0.019(2) 0.005(2) 0.001(2) C30 0.039(3) 0.051(3) 0.038(3) -0.001(2) -0.002(2) 0.000(2) C31 0.0205(18) 0.0284(19) 0.029(2) -0.0012(17) -0.0022(16) 0.0012(15) C32 0.0168(18) 0.032(2) 0.029(2) -0.0012(17) -0.0065(16) -0.0001(16) C33 0.0184(17) 0.036(2) 0.030(2) -0.0071(18) 0.0003(16) 0.0024(15) C34 0.0247(18) 0.0300(19) 0.034(2) -0.003(2) -0.0019(18) -0.0026(15) C35 0.027(2) 0.033(2) 0.041(2) -0.0067(19) 0.0000(18) 0.0040(18) C36 0.036(2) 0.044(3) 0.040(3) -0.019(2) -0.001(2) 0.011(2) C37 0.053(3) 0.076(4) 0.033(3) -0.021(2) -0.013(2) 0.025(3) C38 0.049(3) 0.060(3) 0.037(3) -0.019(2) -0.014(2) 0.030(2) C39 0.027(2) 0.032(2) 0.026(2) -0.0056(17) -0.0058(16) 0.0024(17) C40 0.028(2) 0.0278(19) 0.031(2) -0.0054(17) 0.0103(17) -0.0010(16) C41 0.0214(18) 0.033(2) 0.032(2) -0.0062(17) 0.0031(16) -0.0040(16) C42 0.043(3) 0.072(4) 0.042(3) 0.015(3) -0.001(2) -0.026(3) C43 0.041(3) 0.078(4) 0.056(3) 0.011(3) -0.015(2) -0.028(3) C44 0.029(2) 0.058(3) 0.051(3) -0.006(2) 0.009(2) -0.017(2) C45 0.047(3) 0.074(4) 0.037(3) 0.002(2) 0.015(2) -0.022(3) C46 0.029(2) 0.068(3) 0.034(2) -0.003(2) 0.0061(18) -0.014(2) C47 0.0225(19) 0.028(2) 0.027(2) -0.0049(17) -0.0020(16) -0.0019(16) C48 0.0210(19) 0.026(2) 0.037(2) -0.0023(18) -0.0007(16) -0.0015(16) C49 0.035(2) 0.032(2) 0.031(2) 0.0088(18) 0.0063(18) 0.0041(18) C50 0.059(3) 0.040(3) 0.044(3) 0.009(2) -0.002(2) -0.005(2) C51 0.074(3) 0.039(3) 0.067(3) 0.019(3) 0.010(4) -0.007(2) C52 0.071(4) 0.058(3) 0.050(3) 0.026(3) 0.013(3) 0.017(3) C53 0.055(3) 0.080(4) 0.084(4) 0.041(4) -0.022(3) 0.004(3) C54 0.048(3) 0.061(3) 0.074(4) 0.030(3) -0.022(3) -0.007(2) C55 0.115(6) 0.045(3) 0.099(5) -0.008(3) -0.056(5) 0.017(4) C56 0.221(12) 0.105(7) 0.102(7) 0.046(6) 0.016(7) 0.015(8) C57 0.245(12) 0.165(9) 0.084(6) 0.042(6) -0.063(7) -0.116(9) C58 0.075(4) 0.040(3) 0.056(3) 0.004(2) -0.038(3) -0.016(3) C59 0.054(4) 0.084(5) 0.165(9) 0.010(5) 0.015(5) 0.009(4) C60 0.120(7) 0.135(7) 0.104(6) -0.046(6) 0.036(6) 0.003(6) C61 0.063(3) 0.046(3) 0.051(3) -0.015(2) -0.010(3) 0.011(3) C62 0.131(7) 0.119(6) 0.059(4) 0.004(4) -0.019(4) 0.063(5) C63 0.032(2) 0.073(3) 0.051(3) -0.005(3) 0.002(2) -0.007(2) C64 0.037(3) 0.064(3) 0.049(3) 0.005(3) 0.005(2) -0.013(2) C65 0.050(3) 0.115(5) 0.051(4) 0.033(3) -0.005(3) -0.030(3) C66 0.133(7) 0.198(9) 0.028(3) -0.008(4) 0.007(4) -0.108(7) Mn71 0.0172(3) 0.0223(3) 0.0262(3) -0.0008(2) -0.0021(2) 0.0020(2) I71 0.02625(12) 0.03376(12) 0.03129(13) -0.00143(12) -0.00612(12) 0.00500(10) Li71 0.037(4) 0.037(4) 0.036(4) 0.002(3) -0.008(3) 0.002(3) Li72 0.020(3) 0.041(4) 0.042(4) -0.007(3) 0.000(3) 0.004(3) Li73 0.024(3) 0.040(4) 0.034(4) 0.001(3) -0.003(3) -0.001(3) O71 0.0396(17) 0.065(2) 0.056(2) 0.026(2) -0.0046(18) -0.0069(15) O72 0.0257(15) 0.0460(18) 0.0448(18) -0.0076(15) -0.0021(13) 0.0096(13) O73 0.0318(14) 0.0346(15) 0.0280(16) -0.0015(12) -0.0027(11) 0.0007(12) C71 0.0167(17) 0.0236(18) 0.028(2) -0.0018(16) 0.0027(15) -0.0013(14) C72 0.0268(19) 0.026(2) 0.024(2) 0.0004(16) 0.0031(16) 0.0010(16) C73 0.043(2) 0.028(2) 0.022(2) -0.0013(16) 0.0013(17) 0.0005(18) C74 0.030(2) 0.032(2) 0.025(2) 0.0040(16) -0.0038(16) -0.0009(17) C75 0.0205(18) 0.029(2) 0.033(2) 0.0044(17) -0.0035(16) 0.0028(16) C76 0.0188(16) 0.0214(16) 0.0255(18) 0.0028(17) 0.0009(16) -0.0032(13) C77 0.062(3) 0.032(2) 0.016(2) -0.0042(17) -0.0041(19) 0.012(2) C78 0.087(4) 0.026(2) 0.024(2) -0.0039(17) -0.014(2) 0.003(2) C79 0.112(5) 0.029(2) 0.037(3) -0.002(2) -0.012(3) 0.009(3) C80 0.148(7) 0.045(3) 0.031(3) -0.006(2) -0.006(4) 0.044(4) C81 0.097(5) 0.066(4) 0.030(3) -0.002(3) 0.002(3) 0.050(3) C82 0.069(3) 0.057(3) 0.021(2) 0.001(2) 0.008(2) 0.030(3) C83 0.082(4) 0.029(2) 0.039(3) 0.001(2) -0.011(3) -0.020(2) C84 0.091(5) 0.156(8) 0.060(4) 0.032(5) 0.000(4) -0.032(5) C85 0.116(6) 0.065(4) 0.122(6) -0.038(4) -0.048(5) -0.013(4) C86 0.051(3) 0.068(3) 0.053(3) 0.015(3) 0.020(3) 0.029(2) C87 0.133(6) 0.076(4) 0.052(4) 0.024(3) 0.045(4) 0.054(4) C88 0.044(3) 0.134(6) 0.086(5) 0.042(4) 0.023(3) 0.034(4) C89 0.0191(18) 0.0252(19) 0.028(2) 0.0004(16) -0.0019(15) 0.0067(15) C90 0.0215(18) 0.0206(18) 0.032(2) -0.0030(16) -0.0095(16) 0.0069(15) C91 0.036(2) 0.024(2) 0.045(3) -0.0072(18) -0.016(2) 0.0093(17) C92 0.045(3) 0.041(2) 0.028(2) -0.0096(18) -0.0101(19) 0.026(2) C93 0.030(2) 0.041(2) 0.028(2) 0.0013(18) -0.0017(17) 0.0131(19) C94 0.0214(18) 0.030(2) 0.029(2) 0.0039(17) -0.0034(16) 0.0077(15) C95 0.0202(18) 0.0244(18) 0.048(3) -0.0007(19) -0.0018(19) -0.0010(14) C96 0.042(3) 0.036(2) 0.046(3) 0.007(2) -0.004(2) -0.005(2) C97 0.027(2) 0.034(2) 0.064(3) 0.005(2) -0.008(2) -0.0035(19) C98 0.0214(19) 0.045(2) 0.031(2) -0.002(2) -0.0003(17) 0.0026(17) C99 0.027(2) 0.059(3) 0.062(3) 0.010(3) -0.011(2) -0.001(2) C100 0.027(2) 0.067(3) 0.046(3) 0.018(2) -0.005(2) -0.008(2) C101 0.0175(18) 0.034(2) 0.031(2) 0.0039(18) -0.0035(16) 0.0020(16) C102 0.0123(17) 0.032(2) 0.027(2) 0.0046(16) -0.0018(15) 0.0040(15) C103 0.0190(18) 0.024(2) 0.029(2) 0.0006(16) 0.0023(16) -0.0028(16) C104 0.025(2) 0.030(2) 0.027(2) 0.0048(17) 0.0013(16) 0.0036(17) C105 0.029(2) 0.036(2) 0.036(2) 0.0030(18) 0.0037(17) 0.0097(18) C106 0.033(2) 0.037(2) 0.026(2) 0.0005(17) 0.0051(17) -0.0005(18) C107 0.033(2) 0.038(2) 0.025(2) 0.0023(18) -0.0047(17) 0.0039(18) C108 0.0243(19) 0.032(2) 0.031(2) 0.0013(18) 0.0026(18) 0.0066(15) C109 0.033(2) 0.027(2) 0.029(2) -0.0013(17) -0.0029(17) 0.0035(17) C110 0.0231(19) 0.029(2) 0.027(2) 0.0008(16) 0.0025(16) 0.0078(17) C111 0.0195(18) 0.027(2) 0.032(2) -0.0077(17) -0.0023(16) 0.0017(15) C112 0.025(2) 0.063(3) 0.037(2) -0.014(2) -0.0002(18) 0.002(2) C113 0.024(2) 0.078(4) 0.061(3) -0.038(3) -0.009(2) 0.003(2) C114 0.017(2) 0.043(3) 0.091(4) -0.019(3) -0.004(2) -0.0027(19) C115 0.045(3) 0.046(3) 0.057(3) 0.010(2) 0.005(2) -0.003(2) C116 0.034(2) 0.039(2) 0.040(3) 0.000(2) -0.0034(19) -0.0004(19) C117 0.032(2) 0.026(2) 0.034(2) -0.0035(17) -0.0033(17) 0.0041(17) C118 0.034(2) 0.026(2) 0.038(2) -0.0064(18) -0.0079(19) -0.0007(18) C119 0.027(2) 0.027(2) 0.040(2) 0.0016(18) -0.0056(17) 0.0033(16) C120 0.031(2) 0.029(2) 0.039(2) 0.0010(18) -0.0029(18) 0.0040(17) C121 0.040(2) 0.028(2) 0.050(3) -0.002(2) 0.000(2) 0.0116(19) C122 0.042(3) 0.034(2) 0.062(3) 0.004(2) -0.013(2) 0.011(2) C123 0.068(4) 0.036(3) 0.071(4) -0.005(3) -0.036(3) 0.016(3) C124 0.072(4) 0.037(3) 0.061(3) -0.009(2) -0.030(3) 0.017(3) C125 0.055(3) 0.039(3) 0.034(2) -0.007(2) -0.010(2) 0.000(2) C126 0.062(3) 0.074(4) 0.063(4) -0.033(3) -0.022(3) 0.023(3) C127 0.071(4) 0.040(3) 0.105(5) 0.008(3) 0.027(4) 0.021(3) C128 0.093(4) 0.042(3) 0.062(4) 0.006(3) -0.027(3) 0.017(3) C129 0.067(4) 0.089(5) 0.060(4) 0.044(3) -0.015(3) -0.018(3) C130 0.119(6) 0.088(5) 0.065(4) 0.031(4) -0.004(4) -0.030(5) C131 0.048(3) 0.075(4) 0.078(4) 0.018(3) -0.001(3) -0.017(3) C132 0.060(4) 0.058(4) 0.155(7) 0.022(4) -0.027(4) -0.007(3) C133 0.034(3) 0.076(4) 0.109(5) -0.048(4) 0.001(3) 0.003(3) C134 0.044(3) 0.124(6) 0.103(6) -0.050(5) 0.009(3) 0.015(4) C135 0.036(3) 0.069(4) 0.083(4) -0.009(3) -0.001(3) 0.002(3) C136 0.051(3) 0.049(3) 0.087(4) 0.003(3) 0.005(3) 0.006(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 C1 2.147(4) . ? Mn1 C39 2.174(4) . ? Mn1 C31 2.180(4) . ? Mn1 C47 2.191(4) . ? Mn1 Li2 3.004(7) . ? Mn1 Li1 3.080(7) . ? Mn1 Li3 3.095(7) . ? I1 Li1 2.784(7) . ? I1 Li2 2.850(8) . ? I1 Li3 2.875(7) . ? Li1 O1 1.872(8) . ? Li1 C31 2.274(7) . ? Li1 C39 2.284(8) . ? Li1 C32 2.522(8) . ? Li1 C40 2.547(8) . ? Li1 Li3 3.149(10) . ? Li1 Li2 3.220(10) . ? Li2 O2 1.886(8) . ? Li2 C47 2.254(8) . ? Li2 C39 2.300(8) . ? Li2 C48 2.655(8) . ? Li2 C40 2.743(8) . ? Li2 Li3 3.216(10) . ? Li3 O3 1.918(7) . ? Li3 C31 2.279(8) . ? Li3 C47 2.290(8) . ? Li3 C48 2.511(8) . ? Li3 C32 2.564(8) . ? O1 C55 1.384(6) . ? O1 C58 1.431(5) . ? O2 C61 1.432(6) . ? O2 C59 1.444(8) . ? O3 C64 1.442(5) . ? O3 C65 1.446(6) . ? C1 C2 1.411(5) . ? C1 C6 1.412(5) . ? C2 C3 1.399(5) . ? C2 C7 1.505(5) . ? C3 C4 1.375(6) . ? C3 H3 0.9500 . ? C4 C5 1.377(5) . ? C4 H4 0.9500 . ? C5 C6 1.409(5) . ? C5 H5 0.9500 . ? C6 C19 1.500(5) . ? C7 C8 1.412(5) . ? C7 C12 1.417(5) . ? C8 C9 1.388(6) . ? C8 C13 1.525(6) . ? C9 C10 1.380(6) . ? C9 H9 0.9500 . ? C10 C11 1.373(6) . ? C10 H10 0.9500 . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C12 C16 1.519(5) . ? C13 C15 1.528(6) . ? C13 C14 1.530(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.510(6) . ? C16 C18 1.528(6) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.409(5) . ? C19 C24 1.421(6) . ? C20 C21 1.407(6) . ? C20 C25 1.502(6) . ? C21 C22 1.351(6) . ? C21 H21 0.9500 . ? C22 C23 1.389(7) . ? C22 H22 0.9500 . ? C23 C24 1.390(6) . ? C23 H23 0.9500 . ? C24 C28 1.510(6) . ? C25 C26 1.536(6) . ? C25 C27 1.541(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.533(6) . ? C28 C30 1.534(6) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.208(5) . ? C32 C33 1.458(5) . ? C33 C34 1.390(5) . ? C33 C38 1.396(6) . ? C34 C35 1.377(6) . ? C34 H34 0.9500 . ? C35 C36 1.373(6) . ? C35 H35 0.9500 . ? C36 C37 1.368(7) . ? C36 H36 0.9500 . ? C37 C38 1.386(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.207(5) . ? C40 C41 1.455(5) . ? C41 C46 1.370(6) . ? C41 C42 1.372(6) . ? C42 C43 1.387(6) . ? C42 H42 0.9500 . ? C43 C44 1.369(7) . ? C43 H43 0.9500 . ? C44 C45 1.363(7) . ? C44 H44 0.9500 . ? C45 C46 1.389(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.196(5) . ? C48 C49 1.462(6) . ? C49 C50 1.377(6) . ? C49 C54 1.388(7) . ? C50 C51 1.391(7) . ? C50 H50 0.9500 . ? C51 C52 1.352(8) . ? C51 H51 0.9500 . ? C52 C53 1.337(8) . ? C52 H52 0.9500 . ? C53 C54 1.370(7) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.498(12) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.649(13) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.525(10) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.394(10) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.468(8) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.459(7) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.464(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? Mn71 C71 2.140(4) . ? Mn71 C109 2.165(4) . ? Mn71 C101 2.189(4) . ? Mn71 C117 2.192(4) . ? Mn71 Li71 3.044(7) . ? Mn71 Li72 3.099(7) . ? Mn71 Li73 3.107(7) . ? I71 Li73 2.787(7) . ? I71 Li71 2.871(7) . ? I71 Li72 2.875(7) . ? Li71 O71 1.907(8) . ? Li71 C101 2.252(8) . ? Li71 C117 2.276(9) . ? Li71 C118 2.584(9) . ? Li71 C102 2.631(8) . ? Li71 Li73 3.138(10) . ? Li71 Li72 3.219(10) . ? Li72 O72 1.907(7) . ? Li72 C117 2.285(8) . ? Li72 C109 2.297(8) . ? Li72 C118 2.538(8) . ? Li72 C110 2.583(8) . ? Li72 Li73 3.145(10) . ? Li73 O73 1.875(8) . ? Li73 C109 2.277(8) . ? Li73 C101 2.318(8) . ? Li73 C102 2.444(7) . ? Li73 C110 2.512(8) . ? O71 C129 1.443(6) . ? O71 C131 1.443(6) . ? O72 C133 1.415(6) . ? O72 C136 1.470(6) . ? O73 C128 1.422(6) . ? O73 C125 1.444(5) . ? C71 C72 1.417(5) . ? C71 C76 1.421(5) . ? C72 C73 1.383(5) . ? C72 C77 1.526(5) . ? C73 C74 1.390(6) . ? C73 H73 0.9500 . ? C74 C75 1.389(6) . ? C74 H74 0.9500 . ? C75 C76 1.392(5) . ? C75 H75 0.9500 . ? C76 C89 1.507(5) . ? C77 C82 1.390(7) . ? C77 C78 1.403(7) . ? C78 C79 1.405(7) . ? C78 C83 1.492(8) . ? C79 C80 1.380(10) . ? C79 H79 0.9500 . ? C80 C81 1.364(9) . ? C80 H80 0.9500 . ? C81 C82 1.397(7) . ? C81 H81 0.9500 . ? C82 C86 1.515(7) . ? C83 C85 1.526(7) . ? C83 C84 1.536(8) . ? C83 H83 1.0000 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 C87 1.538(8) . ? C86 C88 1.540(8) . ? C86 H86 1.0000 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 C90 1.411(5) . ? C89 C94 1.413(5) . ? C90 C91 1.383(5) . ? C90 C95 1.519(6) . ? C91 C92 1.372(6) . ? C91 H91 0.9500 . ? C92 C93 1.383(6) . ? C92 H92 0.9500 . ? C93 C94 1.391(6) . ? C93 H93 0.9500 . ? C94 C98 1.517(6) . ? C95 C97 1.530(5) . ? C95 C96 1.533(6) . ? C95 H95 1.0000 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 C100 1.520(6) . ? C98 C99 1.534(6) . ? C98 H98 1.0000 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 C102 1.205(5) . ? C102 C103 1.450(5) . ? C103 C108 1.390(6) . ? C103 C104 1.398(5) . ? C104 C105 1.384(6) . ? C104 H104 0.9500 . ? C105 C106 1.384(6) . ? C105 H105 0.9500 . ? C106 C107 1.371(6) . ? C106 H106 0.9500 . ? C107 C108 1.394(6) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C110 1.206(5) . ? C110 C111 1.459(5) . ? C111 C116 1.375(6) . ? C111 C112 1.400(6) . ? C112 C113 1.396(6) . ? C112 H112 0.9500 . ? C113 C114 1.360(8) . ? C113 H113 0.9500 . ? C114 C115 1.381(7) . ? C114 H114 0.9500 . ? C115 C116 1.383(6) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C117 C118 1.213(6) . ? C118 C119 1.461(6) . ? C119 C120 1.387(6) . ? C119 C124 1.389(7) . ? C120 C121 1.400(6) . ? C120 H120 0.9500 . ? C121 C122 1.369(7) . ? C121 H121 0.9500 . ? C122 C123 1.364(7) . ? C122 H122 0.9500 . ? C123 C124 1.379(7) . ? C123 H123 0.9500 . ? C124 H124 0.9500 . ? C125 C126 1.452(7) . ? C125 H12A 0.9900 . ? C125 H12B 0.9900 . ? C126 C127 1.530(8) . ? C126 H12C 0.9900 . ? C126 H12D 0.9900 . ? C127 C128 1.478(8) . ? C127 H12E 0.9900 . ? C127 H12F 0.9900 . ? C128 H12G 0.9900 . ? C128 H12H 0.9900 . ? C129 C130 1.524(9) . ? C129 H12I 0.9900 . ? C129 H12J 0.9900 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? C131 C132 1.473(9) . ? C131 H13D 0.9900 . ? C131 H13E 0.9900 . ? C132 H13F 0.9800 . ? C132 H13G 0.9800 . ? C132 H13H 0.9800 . ? C133 C134 1.545(8) . ? C133 H13I 0.9900 . ? C133 H13J 0.9900 . ? C134 C135 1.446(8) . ? C134 H13K 0.9900 . ? C134 H13L 0.9900 . ? C135 C136 1.488(7) . ? C135 H13M 0.9900 . ? C135 H13N 0.9900 . ? C136 H13O 0.9900 . ? C136 H13P 0.9900 . ? 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 Mn1 C39 115.52(14) . . ? C1 Mn1 C31 125.67(13) . . ? C39 Mn1 C31 95.02(14) . . ? C1 Mn1 C47 121.54(13) . . ? C39 Mn1 C47 98.00(14) . . ? C31 Mn1 C47 94.82(14) . . ? C1 Mn1 Li2 136.96(17) . . ? C39 Mn1 Li2 49.63(17) . . ? C31 Mn1 Li2 97.24(18) . . ? C47 Mn1 Li2 48.38(17) . . ? C1 Mn1 Li1 142.87(17) . . ? C39 Mn1 Li1 47.80(17) . . ? C31 Mn1 Li1 47.51(16) . . ? C47 Mn1 Li1 95.25(17) . . ? Li2 Mn1 Li1 63.89(19) . . ? C1 Mn1 Li3 148.56(16) . . ? C39 Mn1 Li3 95.89(17) . . ? C31 Mn1 Li3 47.39(17) . . ? C47 Mn1 Li3 47.66(17) . . ? Li2 Mn1 Li3 63.6(2) . . ? Li1 Mn1 Li3 61.32(19) . . ? Li1 I1 Li2 69.7(2) . . ? Li1 I1 Li3 67.6(2) . . ? Li2 I1 Li3 68.4(2) . . ? O1 Li1 C31 122.7(4) . . ? O1 Li1 C39 123.2(4) . . ? C31 Li1 C39 89.6(3) . . ? O1 Li1 C32 101.5(3) . . ? C31 Li1 C32 28.59(15) . . ? C39 Li1 C32 118.1(3) . . ? O1 Li1 C40 100.9(3) . . ? C31 Li1 C40 117.5(3) . . ? C39 Li1 C40 28.26(15) . . ? C32 Li1 C40 145.8(3) . . ? O1 Li1 I1 113.1(3) . . ? C31 Li1 I1 103.5(3) . . ? C39 Li1 I1 100.3(3) . . ? C32 Li1 I1 98.2(3) . . ? C40 Li1 I1 96.3(2) . . ? O1 Li1 Mn1 143.9(3) . . ? C31 Li1 Mn1 44.98(15) . . ? C39 Li1 Mn1 44.84(15) . . ? C32 Li1 Mn1 73.55(18) . . ? C40 Li1 Mn1 73.07(19) . . ? I1 Li1 Mn1 103.0(2) . . ? O1 Li1 Li3 144.4(4) . . ? C31 Li1 Li3 46.3(2) . . ? C39 Li1 Li3 92.2(3) . . ? C32 Li1 Li3 52.4(2) . . ? C40 Li1 Li3 113.9(3) . . ? I1 Li1 Li3 57.57(19) . . ? Mn1 Li1 Li3 59.58(18) . . ? O1 Li1 Li2 147.5(4) . . ? C31 Li1 Li2 89.6(3) . . ? C39 Li1 Li2 45.6(2) . . ? C32 Li1 Li2 110.1(3) . . ? C40 Li1 Li2 55.3(2) . . ? I1 Li1 Li2 56.11(19) . . ? Mn1 Li1 Li2 56.90(18) . . ? Li3 Li1 Li2 60.6(2) . . ? O2 Li2 C47 127.5(4) . . ? O2 Li2 C39 126.9(4) . . ? C47 Li2 C39 92.7(3) . . ? O2 Li2 C48 106.7(3) . . ? C47 Li2 C48 26.62(15) . . ? C39 Li2 C48 119.1(3) . . ? O2 Li2 C40 106.2(3) . . ? C47 Li2 C40 118.4(3) . . ? C39 Li2 C40 25.82(15) . . ? C48 Li2 C40 144.6(3) . . ? O2 Li2 I1 105.2(3) . . ? C47 Li2 I1 100.7(3) . . ? C39 Li2 I1 98.0(3) . . ? C48 Li2 I1 93.0(2) . . ? C40 Li2 I1 90.6(2) . . ? O2 Li2 Mn1 151.4(4) . . ? C47 Li2 Mn1 46.62(17) . . ? C39 Li2 Mn1 46.08(16) . . ? C48 Li2 Mn1 73.11(19) . . ? C40 Li2 Mn1 71.83(19) . . ? I1 Li2 Mn1 103.4(2) . . ? O2 Li2 Li3 142.1(4) . . ? C47 Li2 Li3 45.4(2) . . ? C39 Li2 Li3 90.2(3) . . ? C48 Li2 Li3 49.52(19) . . ? C40 Li2 Li3 106.6(3) . . ? I1 Li2 Li3 56.19(19) . . ? Mn1 Li2 Li3 59.57(18) . . ? O2 Li2 Li1 141.5(4) . . ? C47 Li2 Li1 90.3(3) . . ? C39 Li2 Li1 45.2(2) . . ? C48 Li2 Li1 106.5(3) . . ? C40 Li2 Li1 49.80(19) . . ? I1 Li2 Li1 54.19(18) . . ? Mn1 Li2 Li1 59.22(17) . . ? Li3 Li2 Li1 58.6(2) . . ? O3 Li3 C31 127.8(4) . . ? O3 Li3 C47 122.6(4) . . ? C31 Li3 C47 89.5(3) . . ? O3 Li3 C48 99.2(3) . . ? C31 Li3 C48 117.7(3) . . ? C47 Li3 C48 28.36(16) . . ? O3 Li3 C32 106.8(3) . . ? C31 Li3 C32 28.11(16) . . ? C47 Li3 C32 117.6(3) . . ? C48 Li3 C32 145.8(3) . . ? O3 Li3 I1 111.7(3) . . ? C31 Li3 I1 100.6(3) . . ? C47 Li3 I1 99.1(3) . . ? C48 Li3 I1 95.6(2) . . ? C32 Li3 I1 95.0(2) . . ? O3 Li3 Mn1 147.6(3) . . ? C31 Li3 Mn1 44.72(16) . . ? C47 Li3 Mn1 45.01(16) . . ? C48 Li3 Mn1 73.4(2) . . ? C32 Li3 Mn1 72.75(19) . . ? I1 Li3 Mn1 100.5(2) . . ? O3 Li3 Li1 145.9(4) . . ? C31 Li3 Li1 46.16(19) . . ? C47 Li3 Li1 91.4(3) . . ? C48 Li3 Li1 112.5(3) . . ? C32 Li3 Li1 51.2(2) . . ? I1 Li3 Li1 54.82(17) . . ? Mn1 Li3 Li1 59.11(17) . . ? O3 Li3 Li2 142.6(4) . . ? C31 Li3 Li2 89.5(3) . . ? C47 Li3 Li2 44.5(2) . . ? C48 Li3 Li2 53.5(2) . . ? C32 Li3 Li2 109.1(3) . . ? I1 Li3 Li2 55.45(19) . . ? Mn1 Li3 Li2 56.80(18) . . ? Li1 Li3 Li2 60.8(2) . . ? C55 O1 C58 113.1(4) . . ? C55 O1 Li1 118.5(4) . . ? C58 O1 Li1 128.3(3) . . ? C61 O2 C59 114.0(4) . . ? C61 O2 Li2 124.5(4) . . ? C59 O2 Li2 120.7(4) . . ? C64 O3 C65 112.1(4) . . ? C64 O3 Li3 118.4(3) . . ? C65 O3 Li3 123.0(3) . . ? C2 C1 C6 116.4(3) . . ? C2 C1 Mn1 122.6(3) . . ? C6 C1 Mn1 120.9(3) . . ? C3 C2 C1 121.5(3) . . ? C3 C2 C7 117.3(3) . . ? C1 C2 C7 121.1(3) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 121.1(3) . . ? C5 C6 C19 117.9(3) . . ? C1 C6 C19 121.0(3) . . ? C8 C7 C12 119.3(3) . . ? C8 C7 C2 120.0(3) . . ? C12 C7 C2 120.7(3) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 C13 119.0(3) . . ? C7 C8 C13 121.6(3) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 121.5(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 119.0(3) . . ? C11 C12 C16 119.6(3) . . ? C7 C12 C16 121.3(3) . . ? C8 C13 C15 111.9(4) . . ? C8 C13 C14 111.5(3) . . ? C15 C13 C14 110.4(4) . . ? C8 C13 H13 107.6 . . ? C15 C13 H13 107.6 . . ? C14 C13 H13 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C12 113.5(3) . . ? C17 C16 C18 110.0(3) . . ? C12 C16 C18 109.8(3) . . ? C17 C16 H16 107.8 . . ? C12 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 120.1(3) . . ? C20 C19 C6 120.4(3) . . ? C24 C19 C6 119.5(3) . . ? C21 C20 C19 118.1(4) . . ? C21 C20 C25 119.7(4) . . ? C19 C20 C25 122.2(3) . . ? C22 C21 C20 122.0(4) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 120.2(4) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 121.0(4) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 118.7(4) . . ? C23 C24 C28 120.1(4) . . ? C19 C24 C28 120.9(3) . . ? C20 C25 C26 112.9(4) . . ? C20 C25 C27 111.3(4) . . ? C26 C25 C27 109.3(4) . . ? C20 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 114.3(4) . . ? C24 C28 C30 109.5(4) . . ? C29 C28 C30 108.4(4) . . ? C24 C28 H28 108.2 . . ? C29 C28 H28 108.2 . . ? C30 C28 H28 108.2 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 Mn1 174.1(3) . . ? C32 C31 Li1 87.2(3) . . ? Mn1 C31 Li1 87.5(2) . . ? C32 C31 Li3 89.2(3) . . ? Mn1 C31 Li3 87.9(2) . . ? Li1 C31 Li3 87.5(3) . . ? C31 C32 C33 177.6(4) . . ? C31 C32 Li1 64.2(3) . . ? C33 C32 Li1 117.5(3) . . ? C31 C32 Li3 62.7(3) . . ? C33 C32 Li3 119.0(3) . . ? Li1 C32 Li3 76.5(3) . . ? C34 C33 C38 118.7(4) . . ? C34 C33 C32 121.1(4) . . ? C38 C33 C32 120.1(4) . . ? C35 C34 C33 120.3(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C36 C35 C34 120.6(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 119.9(4) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 120.6(4) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C33 119.9(4) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? C40 C39 Mn1 174.8(3) . . ? C40 C39 Li1 88.1(3) . . ? Mn1 C39 Li1 87.4(2) . . ? C40 C39 Li2 98.1(3) . . ? Mn1 C39 Li2 84.3(2) . . ? Li1 C39 Li2 89.2(3) . . ? C39 C40 C41 175.1(4) . . ? C39 C40 Li1 63.7(3) . . ? C41 C40 Li1 121.0(3) . . ? C39 C40 Li2 56.1(3) . . ? C41 C40 Li2 125.3(3) . . ? Li1 C40 Li2 74.9(2) . . ? C46 C41 C42 118.0(4) . . ? C46 C41 C40 118.7(4) . . ? C42 C41 C40 123.2(4) . . ? C41 C42 C43 121.1(5) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C44 C43 C42 119.9(5) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 119.7(4) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 119.9(4) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 121.3(4) . . ? C41 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C48 C47 Mn1 173.4(3) . . ? C48 C47 Li2 95.8(3) . . ? Mn1 C47 Li2 85.0(2) . . ? C48 C47 Li3 86.1(3) . . ? Mn1 C47 Li3 87.3(2) . . ? Li2 C47 Li3 90.1(3) . . ? C47 C48 C49 177.6(4) . . ? C47 C48 Li3 65.5(3) . . ? C49 C48 Li3 115.4(3) . . ? C47 C48 Li2 57.6(3) . . ? C49 C48 Li2 124.6(3) . . ? Li3 C48 Li2 76.9(2) . . ? C50 C49 C54 118.2(4) . . ? C50 C49 C48 120.5(4) . . ? C54 C49 C48 121.3(4) . . ? C49 C50 C51 119.4(5) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C52 C51 C50 121.6(5) . . ? C52 C51 H51 119.2 . . ? C50 C51 H51 119.2 . . ? C53 C52 C51 118.7(5) . . ? C53 C52 H52 120.6 . . ? C51 C52 H52 120.6 . . ? C52 C53 C54 122.1(6) . . ? C52 C53 H53 118.9 . . ? C54 C53 H53 118.9 . . ? C53 C54 C49 120.0(5) . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? O1 C55 C56 103.9(6) . . ? O1 C55 H55A 111.0 . . ? C56 C55 H55A 111.0 . . ? O1 C55 H55B 111.0 . . ? C56 C55 H55B 111.0 . . ? H55A C55 H55B 109.0 . . ? C55 C56 C57 105.7(6) . . ? C55 C56 H56A 110.6 . . ? C57 C56 H56A 110.6 . . ? C55 C56 H56B 110.6 . . ? C57 C56 H56B 110.6 . . ? H56A C56 H56B 108.7 . . ? C58 C57 C56 100.9(7) . . ? C58 C57 H57A 111.6 . . ? C56 C57 H57A 111.6 . . ? C58 C57 H57B 111.6 . . ? C56 C57 H57B 111.6 . . ? H57A C57 H57B 109.4 . . ? O1 C58 C57 103.3(5) . . ? O1 C58 H58A 111.1 . . ? C57 C58 H58A 111.1 . . ? O1 C58 H58B 111.1 . . ? C57 C58 H58B 111.1 . . ? H58A C58 H58B 109.1 . . ? C60 C59 O2 115.9(8) . . ? C60 C59 H59A 108.3 . . ? O2 C59 H59A 108.3 . . ? C60 C59 H59B 108.3 . . ? O2 C59 H59B 108.3 . . ? H59A C59 H59B 107.4 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O2 C61 C62 112.2(5) . . ? O2 C61 H61A 109.2 . . ? C62 C61 H61A 109.2 . . ? O2 C61 H61B 109.2 . . ? C62 C61 H61B 109.2 . . ? H61A C61 H61B 107.9 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O3 C64 C63 109.6(4) . . ? O3 C64 H64A 109.8 . . ? C63 C64 H64A 109.8 . . ? O3 C64 H64B 109.8 . . ? C63 C64 H64B 109.8 . . ? H64A C64 H64B 108.2 . . ? O3 C65 C66 114.0(6) . . ? O3 C65 H65A 108.8 . . ? C66 C65 H65A 108.8 . . ? O3 C65 H65B 108.8 . . ? C66 C65 H65B 108.8 . . ? H65A C65 H65B 107.6 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C71 Mn71 C109 114.92(14) . . ? C71 Mn71 C101 123.87(13) . . ? C109 Mn71 C101 94.92(15) . . ? C71 Mn71 C117 125.07(14) . . ? C109 Mn71 C117 95.14(15) . . ? C101 Mn71 C117 95.77(15) . . ? C71 Mn71 Li71 149.43(17) . . ? C109 Mn71 Li71 95.63(17) . . ? C101 Mn71 Li71 47.60(17) . . ? C117 Mn71 Li71 48.23(18) . . ? C71 Mn71 Li72 139.79(17) . . ? C109 Mn71 Li72 47.78(17) . . ? C101 Mn71 Li72 95.71(17) . . ? C117 Mn71 Li72 47.44(17) . . ? Li71 Mn71 Li72 63.2(2) . . ? C71 Mn71 Li73 140.89(16) . . ? C109 Mn71 Li73 47.11(16) . . ? C101 Mn71 Li73 48.16(16) . . ? C117 Mn71 Li73 93.43(17) . . ? Li71 Mn71 Li73 61.34(19) . . ? Li72 Mn71 Li73 60.88(18) . . ? Li73 I71 Li71 67.4(2) . . ? Li73 I71 Li72 67.5(2) . . ? Li71 I71 Li72 68.1(2) . . ? O71 Li71 C101 123.0(4) . . ? O71 Li71 C117 121.6(4) . . ? C101 Li71 C117 91.7(3) . . ? O71 Li71 C118 102.3(3) . . ? C101 Li71 C118 119.7(3) . . ? C117 Li71 C118 28.00(16) . . ? O71 Li71 C102 106.7(3) . . ? C101 Li71 C102 27.17(16) . . ? C117 Li71 C102 118.5(3) . . ? C118 Li71 C102 146.1(3) . . ? O71 Li71 I71 114.1(3) . . ? C101 Li71 I71 101.6(3) . . ? C117 Li71 I71 100.1(3) . . ? C118 Li71 I71 92.2(2) . . ? C102 Li71 I71 91.5(2) . . ? O71 Li71 Mn71 141.9(3) . . ? C101 Li71 Mn71 45.86(17) . . ? C117 Li71 Mn71 45.89(16) . . ? C118 Li71 Mn71 73.8(2) . . ? C102 Li71 Mn71 72.62(19) . . ? I71 Li71 Mn71 104.0(2) . . ? O71 Li71 Li73 147.4(4) . . ? C101 Li71 Li73 47.5(2) . . ? C117 Li71 Li73 91.0(3) . . ? C118 Li71 Li73 108.5(3) . . ? C102 Li71 Li73 49.16(19) . . ? I71 Li71 Li73 55.04(18) . . ? Mn71 Li71 Li73 60.32(19) . . ? O71 Li71 Li72 145.5(4) . . ? C101 Li71 Li72 91.2(3) . . ? C117 Li71 Li72 45.2(2) . . ? C118 Li71 Li72 50.4(2) . . ? C102 Li71 Li72 106.5(3) . . ? I71 Li71 Li72 55.99(18) . . ? Mn71 Li71 Li72 59.24(19) . . ? Li73 Li71 Li72 59.3(2) . . ? O72 Li72 C117 128.8(4) . . ? O72 Li72 C109 124.8(4) . . ? C117 Li72 C109 89.1(3) . . ? O72 Li72 C118 106.7(3) . . ? C117 Li72 C118 28.51(16) . . ? C109 Li72 C118 117.7(3) . . ? O72 Li72 C110 102.9(3) . . ? C117 Li72 C110 117.0(3) . . ? C109 Li72 C110 27.84(15) . . ? C118 Li72 C110 145.5(3) . . ? O72 Li72 I71 108.2(3) . . ? C117 Li72 I71 99.8(3) . . ? C109 Li72 I71 100.7(3) . . ? C118 Li72 I71 93.1(3) . . ? C110 Li72 I71 94.2(2) . . ? O72 Li72 Mn71 149.2(4) . . ? C117 Li72 Mn71 44.95(15) . . ? C109 Li72 Mn71 44.27(15) . . ? C118 Li72 Mn71 73.42(19) . . ? C110 Li72 Mn71 72.04(19) . . ? I71 Li72 Mn71 102.5(2) . . ? O72 Li72 Li73 140.4(4) . . ? C117 Li72 Li73 90.7(3) . . ? C109 Li72 Li73 46.3(2) . . ? C118 Li72 Li73 109.5(3) . . ? C110 Li72 Li73 50.88(19) . . ? I71 Li72 Li73 54.93(18) . . ? Mn71 Li72 Li73 59.69(17) . . ? O72 Li72 Li71 146.5(4) . . ? C117 Li72 Li71 45.0(2) . . ? C109 Li72 Li71 88.5(3) . . ? C118 Li72 Li71 51.7(2) . . ? C110 Li72 Li71 107.3(3) . . ? I71 Li72 Li71 55.88(18) . . ? Mn71 Li72 Li71 57.58(17) . . ? Li73 Li72 Li71 59.1(2) . . ? O73 Li73 C109 124.4(4) . . ? O73 Li73 C101 126.0(4) . . ? C109 Li73 C101 88.5(3) . . ? O73 Li73 C102 102.1(3) . . ? C109 Li73 C102 117.4(3) . . ? C101 Li73 C102 29.16(15) . . ? O73 Li73 C110 101.7(3) . . ? C109 Li73 C110 28.64(16) . . ? C101 Li73 C110 117.1(3) . . ? C102 Li73 C110 145.7(3) . . ? O73 Li73 I71 107.9(3) . . ? C109 Li73 I71 103.9(3) . . ? C101 Li73 I71 102.4(3) . . ? C102 Li73 I71 97.7(2) . . ? C110 Li73 I71 98.0(2) . . ? O73 Li73 Mn71 147.7(3) . . ? C109 Li73 Mn71 44.14(16) . . ? C101 Li73 Mn71 44.71(16) . . ? C102 Li73 Mn71 73.9(2) . . ? C110 Li73 Mn71 72.8(2) . . ? I71 Li73 Mn71 104.4(2) . . ? O73 Li73 Li71 144.8(4) . . ? C109 Li73 Li71 90.8(3) . . ? C101 Li73 Li71 45.8(2) . . ? C102 Li73 Li71 54.5(2) . . ? C110 Li73 Li71 111.6(3) . . ? I71 Li73 Li71 57.61(18) . . ? Mn71 Li73 Li71 58.34(18) . . ? O73 Li73 Li72 142.1(3) . . ? C109 Li73 Li72 46.8(2) . . ? C101 Li73 Li72 91.9(3) . . ? C102 Li73 Li72 113.9(3) . . ? C110 Li73 Li72 52.9(2) . . ? I71 Li73 Li72 57.61(19) . . ? Mn71 Li73 Li72 59.43(18) . . ? Li71 Li73 Li72 61.6(2) . . ? C129 O71 C131 114.9(4) . . ? C129 O71 Li71 124.7(4) . . ? C131 O71 Li71 119.4(4) . . ? C133 O72 C136 109.0(3) . . ? C133 O72 Li72 127.0(4) . . ? C136 O72 Li72 123.1(4) . . ? C128 O73 C125 108.8(3) . . ? C128 O73 Li73 119.3(3) . . ? C125 O73 Li73 130.9(3) . . ? C72 C71 C76 115.0(3) . . ? C72 C71 Mn71 121.7(3) . . ? C76 C71 Mn71 123.2(3) . . ? C73 C72 C71 122.9(3) . . ? C73 C72 C77 116.8(3) . . ? C71 C72 C77 120.4(3) . . ? C72 C73 C74 120.6(4) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C75 C74 C73 118.4(4) . . ? C75 C74 H74 120.8 . . ? C73 C74 H74 120.8 . . ? C74 C75 C76 121.1(3) . . ? C74 C75 H75 119.4 . . ? C76 C75 H75 119.4 . . ? C75 C76 C71 121.9(4) . . ? C75 C76 C89 117.5(3) . . ? C71 C76 C89 120.6(3) . . ? C82 C77 C78 121.0(4) . . ? C82 C77 C72 121.2(4) . . ? C78 C77 C72 117.8(4) . . ? C77 C78 C79 118.3(5) . . ? C77 C78 C83 122.5(4) . . ? C79 C78 C83 119.2(5) . . ? C80 C79 C78 120.3(5) . . ? C80 C79 H79 119.8 . . ? C78 C79 H79 119.8 . . ? C81 C80 C79 120.7(5) . . ? C81 C80 H80 119.7 . . ? C79 C80 H80 119.7 . . ? C80 C81 C82 120.9(6) . . ? C80 C81 H81 119.6 . . ? C82 C81 H81 119.6 . . ? C77 C82 C81 118.8(5) . . ? C77 C82 C86 121.2(4) . . ? C81 C82 C86 119.9(5) . . ? C78 C83 C85 111.7(5) . . ? C78 C83 C84 112.1(5) . . ? C85 C83 C84 110.4(6) . . ? C78 C83 H83 107.5 . . ? C85 C83 H83 107.5 . . ? C84 C83 H83 107.5 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C83 C85 H85A 109.5 . . ? C83 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C83 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C82 C86 C87 109.6(5) . . ? C82 C86 C88 114.0(5) . . ? C87 C86 C88 110.2(5) . . ? C82 C86 H86 107.6 . . ? C87 C86 H86 107.6 . . ? C88 C86 H86 107.6 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C90 C89 C94 119.7(3) . . ? C90 C89 C76 120.6(3) . . ? C94 C89 C76 119.6(3) . . ? C91 C90 C89 118.9(4) . . ? C91 C90 C95 119.9(4) . . ? C89 C90 C95 121.1(3) . . ? C92 C91 C90 121.4(4) . . ? C92 C91 H91 119.3 . . ? C90 C91 H91 119.3 . . ? C91 C92 C93 120.2(4) . . ? C91 C92 H92 119.9 . . ? C93 C92 H92 119.9 . . ? C92 C93 C94 120.6(4) . . ? C92 C93 H93 119.7 . . ? C94 C93 H93 119.7 . . ? C93 C94 C89 119.1(4) . . ? C93 C94 C98 119.2(4) . . ? C89 C94 C98 121.6(4) . . ? C90 C95 C97 113.7(4) . . ? C90 C95 C96 111.3(3) . . ? C97 C95 C96 109.3(3) . . ? C90 C95 H95 107.4 . . ? C97 C95 H95 107.4 . . ? C96 C95 H95 107.4 . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C95 C97 H97A 109.5 . . ? C95 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C95 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C94 C98 C100 113.5(4) . . ? C94 C98 C99 109.1(4) . . ? C100 C98 C99 110.2(4) . . ? C94 C98 H98 108.0 . . ? C100 C98 H98 108.0 . . ? C99 C98 H98 108.0 . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C98 C100 H10A 109.5 . . ? C98 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C98 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C102 C101 Mn71 168.3(3) . . ? C102 C101 Li71 94.2(3) . . ? Mn71 C101 Li71 86.5(2) . . ? C102 C101 Li73 81.2(3) . . ? Mn71 C101 Li73 87.1(2) . . ? Li71 C101 Li73 86.7(3) . . ? C101 C102 C103 176.9(4) . . ? C101 C102 Li73 69.6(3) . . ? C103 C102 Li73 110.6(3) . . ? C101 C102 Li71 58.6(3) . . ? C103 C102 Li71 124.5(3) . . ? Li73 C102 Li71 76.3(3) . . ? C108 C103 C104 118.9(4) . . ? C108 C103 C102 121.1(3) . . ? C104 C103 C102 120.0(3) . . ? C105 C104 C103 119.9(4) . . ? C105 C104 H104 120.0 . . ? C103 C104 H104 120.0 . . ? C106 C105 C104 120.8(4) . . ? C106 C105 H105 119.6 . . ? C104 C105 H105 119.6 . . ? C107 C106 C105 119.7(4) . . ? C107 C106 H106 120.2 . . ? C105 C106 H106 120.2 . . ? C106 C107 C108 120.3(4) . . ? C106 C107 H107 119.9 . . ? C108 C107 H107 119.9 . . ? C103 C108 C107 120.5(4) . . ? C103 C108 H108 119.8 . . ? C107 C108 H108 119.8 . . ? C110 C109 Mn71 174.7(4) . . ? C110 C109 Li73 86.6(3) . . ? Mn71 C109 Li73 88.7(2) . . ? C110 C109 Li72 89.4(3) . . ? Mn71 C109 Li72 88.0(2) . . ? Li73 C109 Li72 86.9(3) . . ? C109 C110 C111 175.7(4) . . ? C109 C110 Li73 64.8(3) . . ? C111 C110 Li73 119.5(3) . . ? C109 C110 Li72 62.8(3) . . ? C111 C110 Li72 117.5(3) . . ? Li73 C110 Li72 76.2(2) . . ? C116 C111 C112 118.8(4) . . ? C116 C111 C110 119.4(4) . . ? C112 C111 C110 121.9(4) . . ? C113 C112 C111 119.4(4) . . ? C113 C112 H112 120.3 . . ? C111 C112 H112 120.3 . . ? C114 C113 C112 120.9(5) . . ? C114 C113 H113 119.5 . . ? C112 C113 H113 119.5 . . ? C113 C114 C115 119.8(4) . . ? C113 C114 H114 120.1 . . ? C115 C114 H114 120.1 . . ? C114 C115 C116 119.9(5) . . ? C114 C115 H115 120.1 . . ? C116 C115 H115 120.1 . . ? C111 C116 C115 121.1(4) . . ? C111 C116 H116 119.4 . . ? C115 C116 H116 119.4 . . ? C118 C117 Mn71 173.7(3) . . ? C118 C117 Li71 90.2(4) . . ? Mn71 C117 Li71 85.9(2) . . ? C118 C117 Li72 87.4(3) . . ? Mn71 C117 Li72 87.6(2) . . ? Li71 C117 Li72 89.8(3) . . ? C117 C118 C119 177.9(4) . . ? C117 C118 Li72 64.1(3) . . ? C119 C118 Li72 118.0(3) . . ? C117 C118 Li71 61.8(3) . . ? C119 C118 Li71 118.3(3) . . ? Li72 C118 Li71 77.9(3) . . ? C120 C119 C124 119.0(4) . . ? C120 C119 C118 119.7(4) . . ? C124 C119 C118 121.2(4) . . ? C119 C120 C121 119.3(4) . . ? C119 C120 H120 120.3 . . ? C121 C120 H120 120.3 . . ? C122 C121 C120 120.7(4) . . ? C122 C121 H121 119.6 . . ? C120 C121 H121 119.6 . . ? C123 C122 C121 119.8(4) . . ? C123 C122 H122 120.1 . . ? C121 C122 H122 120.1 . . ? C122 C123 C124 120.6(5) . . ? C122 C123 H123 119.7 . . ? C124 C123 H123 119.7 . . ? C123 C124 C119 120.5(5) . . ? C123 C124 H124 119.7 . . ? C119 C124 H124 119.7 . . ? O73 C125 C126 106.7(4) . . ? O73 C125 H12A 110.4 . . ? C126 C125 H12A 110.4 . . ? O73 C125 H12B 110.4 . . ? C126 C125 H12B 110.4 . . ? H12A C125 H12B 108.6 . . ? C125 C126 C127 104.1(4) . . ? C125 C126 H12C 110.9 . . ? C127 C126 H12C 110.9 . . ? C125 C126 H12D 110.9 . . ? C127 C126 H12D 110.9 . . ? H12C C126 H12D 109.0 . . ? C128 C127 C126 105.6(4) . . ? C128 C127 H12E 110.6 . . ? C126 C127 H12E 110.6 . . ? C128 C127 H12F 110.6 . . ? C126 C127 H12F 110.6 . . ? H12E C127 H12F 108.8 . . ? O73 C128 C127 107.6(4) . . ? O73 C128 H12G 110.2 . . ? C127 C128 H12G 110.2 . . ? O73 C128 H12H 110.2 . . ? C127 C128 H12H 110.2 . . ? H12G C128 H12H 108.5 . . ? O71 C129 C130 114.0(5) . . ? O71 C129 H12I 108.8 . . ? C130 C129 H12I 108.8 . . ? O71 C129 H12J 108.8 . . ? C130 C129 H12J 108.8 . . ? H12I C129 H12J 107.7 . . ? C129 C130 H13A 109.5 . . ? C129 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? C129 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? O71 C131 C132 113.8(5) . . ? O71 C131 H13D 108.8 . . ? C132 C131 H13D 108.8 . . ? O71 C131 H13E 108.8 . . ? C132 C131 H13E 108.8 . . ? H13D C131 H13E 107.7 . . ? C131 C132 H13F 109.5 . . ? C131 C132 H13G 109.5 . . ? H13F C132 H13G 109.5 . . ? C131 C132 H13H 109.5 . . ? H13F C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? O72 C133 C134 103.2(5) . . ? O72 C133 H13I 111.1 . . ? C134 C133 H13I 111.1 . . ? O72 C133 H13J 111.1 . . ? C134 C133 H13J 111.1 . . ? H13I C133 H13J 109.1 . . ? C135 C134 C133 102.6(5) . . ? C135 C134 H13K 111.3 . . ? C133 C134 H13K 111.3 . . ? C135 C134 H13L 111.3 . . ? C133 C134 H13L 111.3 . . ? H13K C134 H13L 109.2 . . ? C134 C135 C136 103.1(5) . . ? C134 C135 H13M 111.1 . . ? C136 C135 H13M 111.1 . . ? C134 C135 H13N 111.1 . . ? C136 C135 H13N 111.1 . . ? H13M C135 H13N 109.1 . . ? O72 C136 C135 105.5(4) . . ? O72 C136 H13O 110.7 . . ? C135 C136 H13O 110.7 . . ? O72 C136 H13P 110.7 . . ? C135 C136 H13P 110.7 . . ? H13O C136 H13P 108.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.794 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.062 #===END data_p21c_DMn_TripLiI _database_code_depnum_ccdc_archive 'CCDC 794080' #TrackingRef 'CIF-Mn-010510.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H68 I Li Mn O, 0.5(C6 H14) ' _chemical_formula_sum ' C52 H75 I Li Mn O ' _chemical_formula_weight 904.90 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1) /c' _symmetry_Hall_group_name_H-m '-P 2ybc' 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 9.4800(10) _cell_length_b 20.122(2) _cell_length_c 25.994(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.2130(10) _cell_angle_gamma 90.00 _cell_volume 4945.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8642 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.52 _exptl_crystal_description Rod _exptl_crystal_colour Pink _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8155 _exptl_absorpt_correction_T_max 0.8971 _exptl_absorpt_process_details 'SADABS 2007/3 (Sheldrick, 2007)' _exptl_special_details ; A pale pink rod crystals with approximate orthogonal dimensions 0.23 x 0.14 x 0.12 mm3 was placed and optically centered on the Bruker SMART1000(1) CCD system at 90(2)K. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide Omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 30 seconds per frame and 606 frames were collected, at varying phi angles (phi=0? 90? 180? 270?, for each series. The crystal to detector distance was 4.28cm, thus providing a complete sphere of data with processing to 2ThetaMax=55.21? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54155 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11334 _reflns_number_gt 10260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. References: 1. Bruker (2004) SMART APEX (Version 2.0.2) and SAINT (Version 7.46A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008) Version 2008/1, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.30 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.40 Ratio PLAT432_ALERT_2_C Short Inter X...Y Contact C50 .. C50 ..3.15 Ang. PLAT223_ALERT_4_C Large Solvent/Anion H Ueq(max)/Ueq(min) ...3.72 Ratio PLAT234_ALERT_4_C Large Hirshfeld Difference C50 -- C51 ..0.19 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference C51 -- C52 ..0.16 Ang. These are due to the disorder and librational shifts of the solvent molecule. PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbours of C51 it may be due to the different direction of thermal motion of C51 compared to its neighbors. ; _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^)+(0.0274P)^2^+2.9546P] 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 11334 _refine_ls_number_parameters 547 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _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 0.26260(2) 0.613156(11) 0.307459(8) 0.01574(5) Uani 1 1 d . . . Li1 Li 0.1626(3) 0.68709(14) 0.19129(11) 0.0276(6) Uani 1 1 d . . . I1 I 0.428499(11) 0.691488(5) 0.247025(4) 0.02467(4) Uani 1 1 d . . . O1 O 0.19953(12) 0.73605(6) 0.13162(4) 0.0247(2) Uani 1 1 d . . . C1 C 0.37944(14) 0.58751(7) 0.37643(5) 0.0137(2) Uani 1 1 d . . . C2 C 0.46229(14) 0.52905(7) 0.37916(5) 0.0142(3) Uani 1 1 d . . . C3 C 0.55885(15) 0.51569(7) 0.42117(5) 0.0170(3) Uani 1 1 d . . . H3A H 0.6147 0.4765 0.4214 0.020 Uiso 1 1 calc R . . C4 C 0.57347(15) 0.55937(7) 0.46254(5) 0.0185(3) Uani 1 1 d . . . H4A H 0.6405 0.5508 0.4907 0.022 Uiso 1 1 calc R . . C5 C 0.48917(15) 0.61566(7) 0.46228(5) 0.0172(3) Uani 1 1 d . . . H5A H 0.4961 0.6448 0.4911 0.021 Uiso 1 1 calc R . . C6 C 0.39386(14) 0.62998(7) 0.42002(5) 0.0146(3) Uani 1 1 d . . . C7 C 0.43868(14) 0.47595(7) 0.33854(5) 0.0144(3) Uani 1 1 d . . . C8 C 0.52368(15) 0.47170(7) 0.29620(5) 0.0168(3) Uani 1 1 d . . . C9 C 0.50104(16) 0.41917(8) 0.26144(6) 0.0216(3) Uani 1 1 d . . . H9A H 0.5587 0.4154 0.2332 0.026 Uiso 1 1 calc R . . C10 C 0.39632(17) 0.37249(8) 0.26735(6) 0.0233(3) Uani 1 1 d . . . H10A H 0.3823 0.3372 0.2432 0.028 Uiso 1 1 calc R . . C11 C 0.31213(16) 0.37726(7) 0.30845(6) 0.0207(3) Uani 1 1 d . . . H11A H 0.2393 0.3455 0.3120 0.025 Uiso 1 1 calc R . . C12 C 0.33270(15) 0.42815(7) 0.34485(5) 0.0166(3) Uani 1 1 d . . . C13 C 0.64195(16) 0.52118(8) 0.28954(6) 0.0203(3) Uani 1 1 d . . . H13A H 0.6167 0.5637 0.3065 0.024 Uiso 1 1 calc R . . C14 C 0.78077(17) 0.49600(9) 0.31629(7) 0.0300(4) Uani 1 1 d . . . H14A H 0.7695 0.4901 0.3532 0.045 Uiso 1 1 calc R . . H14B H 0.8560 0.5284 0.3117 0.045 Uiso 1 1 calc R . . H14C H 0.8058 0.4534 0.3011 0.045 Uiso 1 1 calc R . . C15 C 0.66431(18) 0.53624(9) 0.23300(6) 0.0276(3) Uani 1 1 d . . . H15A H 0.5734 0.5476 0.2147 0.041 Uiso 1 1 calc R . . H15B H 0.7042 0.4971 0.2170 0.041 Uiso 1 1 calc R . . H15C H 0.7297 0.5737 0.2311 0.041 Uiso 1 1 calc R . . C16 C 0.23849(15) 0.43043(7) 0.38983(5) 0.0184(3) Uani 1 1 d . . . H16A H 0.2760 0.4657 0.4143 0.022 Uiso 1 1 calc R . . C17 C 0.23869(18) 0.36451(8) 0.41937(6) 0.0262(3) Uani 1 1 d . . . H17A H 0.3364 0.3516 0.4297 0.039 Uiso 1 1 calc R . . H17B H 0.1939 0.3300 0.3971 0.039 Uiso 1 1 calc R . . H17C H 0.1859 0.3698 0.4502 0.039 Uiso 1 1 calc R . . C18 C 0.08803(17) 0.44960(9) 0.37070(6) 0.0268(3) Uani 1 1 d . . . H18A H 0.0891 0.4929 0.3534 0.040 Uiso 1 1 calc R . . H18B H 0.0291 0.4523 0.4001 0.040 Uiso 1 1 calc R . . H18C H 0.0493 0.4160 0.3463 0.040 Uiso 1 1 calc R . . C19 C 0.30027(15) 0.68988(7) 0.42431(5) 0.0158(3) Uani 1 1 d . . . C20 C 0.16016(16) 0.68081(7) 0.43831(5) 0.0178(3) Uani 1 1 d . . . C21 C 0.07750(17) 0.73662(8) 0.44697(6) 0.0238(3) Uani 1 1 d . . . H21A H -0.0164 0.7309 0.4567 0.029 Uiso 1 1 calc R . . C22 C 0.13074(19) 0.80014(8) 0.44159(7) 0.0284(3) Uani 1 1 d . . . H22A H 0.0739 0.8377 0.4480 0.034 Uiso 1 1 calc R . . C23 C 0.26656(19) 0.80889(8) 0.42685(7) 0.0263(3) Uani 1 1 d . . . H23A H 0.3017 0.8527 0.4228 0.032 Uiso 1 1 calc R . . C24 C 0.35344(16) 0.75457(7) 0.41777(5) 0.0187(3) Uani 1 1 d . . . C25 C 0.10132(16) 0.61153(7) 0.44716(6) 0.0208(3) Uani 1 1 d . . . H25A H 0.1523 0.5798 0.4254 0.025 Uiso 1 1 calc R . . C26 C 0.1330(2) 0.59113(10) 0.50359(7) 0.0353(4) Uani 1 1 d . . . H26A H 0.2352 0.5932 0.5124 0.053 Uiso 1 1 calc R . . H26B H 0.0995 0.5457 0.5085 0.053 Uiso 1 1 calc R . . H26C H 0.0845 0.6215 0.5259 0.053 Uiso 1 1 calc R . . C27 C -0.05645(17) 0.60476(9) 0.43187(7) 0.0285(3) Uani 1 1 d . . . H27A H -0.0757 0.6186 0.3959 0.043 Uiso 1 1 calc R . . H27B H -0.1099 0.6330 0.4542 0.043 Uiso 1 1 calc R . . H27C H -0.0852 0.5583 0.4357 0.043 Uiso 1 1 calc R . . C28 C 0.50349(16) 0.76644(7) 0.40228(6) 0.0210(3) Uani 1 1 d . . . H28A H 0.5360 0.7248 0.3858 0.025 Uiso 1 1 calc R . . C29 C 0.60554(18) 0.78081(9) 0.44936(6) 0.0293(3) Uani 1 1 d . . . H29A H 0.6074 0.7427 0.4729 0.044 Uiso 1 1 calc R . . H29B H 0.5738 0.8204 0.4672 0.044 Uiso 1 1 calc R . . H29C H 0.7007 0.7885 0.4381 0.044 Uiso 1 1 calc R . . C30 C 0.5109(2) 0.82309(8) 0.36299(6) 0.0284(3) Uani 1 1 d . . . H30A H 0.4430 0.8147 0.3335 0.043 Uiso 1 1 calc R . . H30B H 0.6066 0.8254 0.3512 0.043 Uiso 1 1 calc R . . H30C H 0.4880 0.8653 0.3793 0.043 Uiso 1 1 calc R . . C31 C 0.08061(15) 0.61753(7) 0.25383(5) 0.0167(3) Uani 1 1 d . . . C32 C 0.07407(15) 0.57846(7) 0.20822(5) 0.0170(3) Uani 1 1 d . . . C33 C -0.01466(16) 0.59609(7) 0.16478(5) 0.0196(3) Uani 1 1 d . . . H33A H -0.0052 0.5719 0.1316 0.024 Uiso 1 1 calc R . . C34 C -0.10102(15) 0.65239(7) 0.16477(6) 0.0195(3) Uani 1 1 d . . . C35 C -0.09835(16) 0.69002(7) 0.20967(6) 0.0202(3) Uani 1 1 d . . . H35A H -0.1485 0.7338 0.2088 0.024 Uiso 1 1 calc R . . C36 C -0.00975(16) 0.67334(7) 0.25362(5) 0.0185(3) Uani 1 1 d . . . C37 C 0.16489(16) 0.51629(7) 0.20566(6) 0.0210(3) Uani 1 1 d . . . H37A H 0.2249 0.5134 0.2389 0.025 Uiso 1 1 calc R . . C38 C 0.26458(19) 0.51900(9) 0.16199(7) 0.0321(4) Uani 1 1 d . . . H38A H 0.3241 0.5588 0.1659 0.048 Uiso 1 1 calc R . . H38B H 0.2089 0.5207 0.1287 0.048 Uiso 1 1 calc R . . H38C H 0.3246 0.4793 0.1633 0.048 Uiso 1 1 calc R . . C39 C 0.0731(2) 0.45397(8) 0.20147(8) 0.0352(4) Uani 1 1 d . . . H39A H 0.0132 0.4523 0.2306 0.053 Uiso 1 1 calc R . . H39B H 0.1338 0.4145 0.2020 0.053 Uiso 1 1 calc R . . H39C H 0.0133 0.4551 0.1691 0.053 Uiso 1 1 calc R . . C40 C -0.19881(17) 0.67131(8) 0.11786(6) 0.0242(3) Uani 1 1 d . . . H40A H -0.2415 0.7154 0.1254 0.029 Uiso 1 1 calc R . . C41 C -0.32025(19) 0.62177(10) 0.10955(7) 0.0357(4) Uani 1 1 d . . . H41A H -0.3832 0.6357 0.0799 0.054 Uiso 1 1 calc R . . H41B H -0.3735 0.6202 0.1405 0.054 Uiso 1 1 calc R . . H41C H -0.2821 0.5776 0.1029 0.054 Uiso 1 1 calc R . . C42 C -0.1205(2) 0.67964(11) 0.06920(7) 0.0380(4) Uani 1 1 d . . . H42A H -0.0436 0.7118 0.0756 0.057 Uiso 1 1 calc R . . H42B H -0.1863 0.6957 0.0411 0.057 Uiso 1 1 calc R . . H42C H -0.0811 0.6367 0.0596 0.057 Uiso 1 1 calc R . . C43 C -0.01018(18) 0.71813(9) 0.30084(6) 0.0271(3) Uani 1 1 d . . . H43A H 0.0505 0.6964 0.3291 0.032 Uiso 1 1 calc R . . C44 C -0.1589(2) 0.72520(12) 0.31974(7) 0.0452(5) Uani 1 1 d . . . H44A H -0.1982 0.6810 0.3255 0.068 Uiso 1 1 calc R . . H44B H -0.2198 0.7488 0.2937 0.068 Uiso 1 1 calc R . . H44C H -0.1536 0.7503 0.3521 0.068 Uiso 1 1 calc R . . C45 C 0.0550(2) 0.78602(9) 0.29084(8) 0.0428(5) Uani 1 1 d . . . H45A H 0.1513 0.7800 0.2802 0.064 Uiso 1 1 calc R . . H45B H 0.0581 0.8126 0.3225 0.064 Uiso 1 1 calc R . . H45C H -0.0025 0.8089 0.2634 0.064 Uiso 1 1 calc R . . C46 C 0.2833(2) 0.70423(9) 0.09421(7) 0.0310(4) Uani 1 1 d . . . H46A H 0.2215 0.6799 0.0683 0.037 Uiso 1 1 calc R . . H46B H 0.3508 0.6724 0.1115 0.037 Uiso 1 1 calc R . . C47 C 0.3614(2) 0.75879(10) 0.06891(7) 0.0372(4) Uani 1 1 d . . . H47A H 0.3060 0.7761 0.0380 0.045 Uiso 1 1 calc R . . H47B H 0.4547 0.7433 0.0589 0.045 Uiso 1 1 calc R . . C48 C 0.3774(2) 0.81078(10) 0.11097(8) 0.0406(5) Uani 1 1 d . . . H48A H 0.4595 0.8010 0.1355 0.049 Uiso 1 1 calc R . . H48B H 0.3889 0.8557 0.0963 0.049 Uiso 1 1 calc R . . C49 C 0.2412(2) 0.80536(8) 0.13664(7) 0.0347(4) Uani 1 1 d . . . H49A H 0.2551 0.8182 0.1734 0.042 Uiso 1 1 calc R . . H49B H 0.1681 0.8346 0.1194 0.042 Uiso 1 1 calc R . . C50 C 0.1633(16) 0.9845(7) 0.5072(5) 0.144(6) Uani 0.63 1 d PU A 1 H50A H 0.0926 1.0092 0.5252 0.216 Uiso 0.63 1 calc PR A 1 H50B H 0.1670 0.9384 0.5195 0.216 Uiso 0.63 1 calc PR A 1 H50C H 0.1374 0.9851 0.4700 0.216 Uiso 0.63 1 calc PR A 1 C51 C 0.3101(6) 1.0173(2) 0.51822(17) 0.0755(14) Uani 0.63 1 d P A 1 H51A H 0.3032 1.0642 0.5067 0.091 Uiso 0.63 1 calc PR A 1 H51B H 0.3326 1.0177 0.5560 0.091 Uiso 0.63 1 calc PR A 1 C52 C 0.4225(7) 0.9881(4) 0.4954(3) 0.0677(17) Uani 0.63 1 d P . 1 H52A H 0.3990 0.9900 0.4577 0.081 Uiso 0.63 1 calc PR . 1 H52B H 0.4219 0.9405 0.5051 0.081 Uiso 0.63 1 calc PR . 1 C50A C 0.2037(16) 0.9669(8) 0.5104(5) 0.067(3) Uani 0.37 1 d PDU B 2 H50D H 0.1367 0.9391 0.5278 0.100 Uiso 0.37 1 calc PR B 2 H50E H 0.1787 0.9664 0.4732 0.100 Uiso 0.37 1 calc PR B 2 H50F H 0.1996 1.0125 0.5233 0.100 Uiso 0.37 1 calc PR B 2 C51A C 0.3567(7) 0.9389(4) 0.5215(2) 0.0591(19) Uani 0.37 1 d PD B 2 H51C H 0.3530 0.8904 0.5149 0.071 Uiso 0.37 1 calc PR B 2 H51D H 0.3831 0.9449 0.5588 0.071 Uiso 0.37 1 calc PR B 2 C52A C 0.4793(10) 0.9681(4) 0.4913(4) 0.048(2) Uani 0.37 1 d PD . 2 H52C H 0.5618 0.9379 0.4953 0.058 Uiso 0.37 1 calc PR . 2 H52D H 0.4481 0.9704 0.4542 0.058 Uiso 0.37 1 calc PR . 2 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 0.01652(11) 0.01726(10) 0.01307(10) 0.00184(7) -0.00142(7) 0.00168(8) Li1 0.0311(15) 0.0281(14) 0.0238(13) 0.0082(11) 0.0043(11) -0.0045(11) I1 0.02313(6) 0.02672(6) 0.02369(6) 0.00729(4) -0.00148(4) -0.00612(4) O1 0.0263(6) 0.0259(6) 0.0221(5) 0.0048(4) 0.0029(4) -0.0057(5) C1 0.0129(6) 0.0154(6) 0.0130(6) 0.0013(5) 0.0020(5) -0.0011(5) C2 0.0135(6) 0.0152(6) 0.0139(6) 0.0004(5) 0.0024(5) -0.0018(5) C3 0.0166(7) 0.0163(6) 0.0178(6) 0.0014(5) -0.0005(5) 0.0024(5) C4 0.0173(7) 0.0224(7) 0.0151(6) 0.0016(5) -0.0031(5) -0.0003(5) C5 0.0197(7) 0.0193(7) 0.0124(6) -0.0017(5) -0.0002(5) -0.0015(5) C6 0.0149(6) 0.0149(6) 0.0143(6) 0.0018(5) 0.0025(5) -0.0012(5) C7 0.0145(6) 0.0142(6) 0.0140(6) 0.0002(5) -0.0013(5) 0.0028(5) C8 0.0156(7) 0.0184(7) 0.0163(6) 0.0000(5) 0.0008(5) 0.0031(5) C9 0.0234(8) 0.0241(7) 0.0178(7) -0.0030(6) 0.0049(6) 0.0033(6) C10 0.0279(8) 0.0212(7) 0.0204(7) -0.0069(6) 0.0000(6) 0.0005(6) C11 0.0220(7) 0.0177(7) 0.0221(7) -0.0019(5) 0.0001(6) -0.0024(6) C12 0.0170(7) 0.0166(6) 0.0160(6) 0.0004(5) 0.0000(5) 0.0015(5) C13 0.0185(7) 0.0225(7) 0.0203(7) -0.0001(5) 0.0049(5) -0.0009(6) C14 0.0195(8) 0.0399(10) 0.0304(8) 0.0034(7) 0.0009(6) -0.0028(7) C15 0.0263(8) 0.0336(9) 0.0237(8) 0.0038(6) 0.0075(6) -0.0020(7) C16 0.0184(7) 0.0180(7) 0.0193(7) -0.0007(5) 0.0039(5) -0.0026(5) C17 0.0315(9) 0.0246(8) 0.0231(7) 0.0036(6) 0.0062(6) 0.0010(6) C18 0.0202(8) 0.0304(8) 0.0304(8) 0.0034(7) 0.0053(6) 0.0021(6) C19 0.0195(7) 0.0165(6) 0.0111(6) -0.0017(5) 0.0000(5) 0.0012(5) C20 0.0197(7) 0.0193(7) 0.0143(6) -0.0009(5) 0.0003(5) 0.0002(5) C21 0.0203(7) 0.0261(8) 0.0255(8) -0.0024(6) 0.0043(6) 0.0038(6) C22 0.0306(9) 0.0209(8) 0.0340(9) -0.0033(6) 0.0047(7) 0.0081(6) C23 0.0325(9) 0.0159(7) 0.0309(8) -0.0005(6) 0.0037(7) 0.0011(6) C24 0.0228(7) 0.0176(7) 0.0155(6) -0.0006(5) 0.0011(5) -0.0003(6) C25 0.0188(7) 0.0209(7) 0.0231(7) 0.0000(6) 0.0050(6) -0.0008(6) C26 0.0319(9) 0.0400(10) 0.0333(9) 0.0159(8) -0.0025(7) -0.0103(8) C27 0.0231(8) 0.0299(8) 0.0322(9) -0.0005(7) 0.0008(6) -0.0044(7) C28 0.0250(8) 0.0183(7) 0.0201(7) -0.0006(5) 0.0042(6) -0.0035(6) C29 0.0255(8) 0.0354(9) 0.0266(8) 0.0019(7) 0.0007(6) -0.0081(7) C30 0.0367(9) 0.0235(8) 0.0257(8) 0.0029(6) 0.0070(7) -0.0058(7) C31 0.0157(7) 0.0189(7) 0.0156(6) 0.0045(5) 0.0010(5) -0.0007(5) C32 0.0150(7) 0.0174(7) 0.0186(6) 0.0030(5) 0.0004(5) -0.0020(5) C33 0.0210(7) 0.0210(7) 0.0166(6) 0.0017(5) -0.0011(5) -0.0027(6) C34 0.0169(7) 0.0224(7) 0.0188(7) 0.0056(5) -0.0023(5) -0.0026(6) C35 0.0176(7) 0.0204(7) 0.0219(7) 0.0037(5) -0.0019(5) 0.0028(6) C36 0.0177(7) 0.0212(7) 0.0165(6) 0.0022(5) 0.0005(5) 0.0011(5) C37 0.0221(7) 0.0191(7) 0.0212(7) 0.0000(5) -0.0028(6) 0.0022(6) C38 0.0321(9) 0.0343(9) 0.0305(9) 0.0016(7) 0.0068(7) 0.0106(7) C39 0.0334(10) 0.0178(8) 0.0537(11) 0.0018(7) -0.0022(8) -0.0008(7) C40 0.0242(8) 0.0267(8) 0.0207(7) 0.0046(6) -0.0056(6) 0.0013(6) C41 0.0268(9) 0.0467(11) 0.0316(9) 0.0096(8) -0.0105(7) -0.0073(8) C42 0.0303(9) 0.0602(13) 0.0227(8) 0.0152(8) -0.0037(7) -0.0006(9) C43 0.0288(9) 0.0321(8) 0.0194(7) -0.0043(6) -0.0040(6) 0.0140(7) C44 0.0354(10) 0.0752(15) 0.0246(9) -0.0063(9) 0.0002(7) 0.0287(10) C45 0.0596(14) 0.0269(9) 0.0399(11) -0.0123(8) -0.0103(9) 0.0095(9) C46 0.0393(10) 0.0282(8) 0.0261(8) -0.0001(7) 0.0068(7) -0.0041(7) C47 0.0388(10) 0.0385(10) 0.0357(10) 0.0080(8) 0.0121(8) -0.0017(8) C48 0.0466(12) 0.0369(10) 0.0380(10) 0.0058(8) 0.0014(8) -0.0202(9) C49 0.0525(12) 0.0219(8) 0.0304(9) 0.0044(7) 0.0084(8) -0.0002(8) C50 0.197(14) 0.125(10) 0.107(7) 0.042(6) -0.011(8) -0.059(9) C51 0.122(5) 0.057(3) 0.048(2) 0.0104(19) 0.007(3) -0.012(3) C52 0.085(5) 0.073(4) 0.044(3) 0.004(3) -0.001(3) -0.003(3) C50A 0.096(7) 0.067(7) 0.035(4) 0.000(4) -0.017(4) -0.027(5) C51A 0.069(5) 0.078(5) 0.030(3) 0.009(3) 0.003(3) -0.032(4) C52A 0.066(6) 0.044(5) 0.035(3) -0.002(3) 0.006(4) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C1 2.1014(13) . ? Mn1 C31 2.1387(14) . ? Mn1 I1 2.7908(3) . ? Li1 O1 1.892(3) . ? Li1 C31 2.322(3) . ? Li1 C32 2.394(3) . ? Li1 C36 2.400(3) . ? Li1 C33 2.546(3) . ? Li1 C35 2.555(3) . ? Li1 C34 2.637(3) . ? Li1 I1 2.815(3) . ? O1 C46 1.449(2) . ? O1 C49 1.453(2) . ? C1 C2 1.4133(19) . ? C1 C6 1.4177(18) . ? C2 C3 1.3986(19) . ? C2 C7 1.5072(18) . ? C3 C4 1.388(2) . ? C3 H3A 0.9500 . ? C4 C5 1.386(2) . ? C4 H4A 0.9500 . ? C5 C6 1.4002(19) . ? C5 H5A 0.9500 . ? C6 C19 1.5055(19) . ? C7 C12 1.4091(19) . ? C7 C8 1.4137(19) . ? C8 C9 1.397(2) . ? C8 C13 1.519(2) . ? C9 C10 1.383(2) . ? C9 H9A 0.9500 . ? C10 C11 1.383(2) . ? C10 H10A 0.9500 . ? C11 C12 1.398(2) . ? C11 H11A 0.9500 . ? C12 C16 1.5233(19) . ? C13 C14 1.529(2) . ? C13 C15 1.530(2) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.525(2) . ? C16 C17 1.533(2) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.411(2) . ? C19 C20 1.415(2) . ? C20 C21 1.397(2) . ? C20 C25 1.525(2) . ? C21 C22 1.385(2) . ? C21 H21A 0.9500 . ? C22 C23 1.381(2) . ? C22 H22A 0.9500 . ? C23 C24 1.399(2) . ? C23 H23A 0.9500 . ? C24 C28 1.525(2) . ? C25 C27 1.525(2) . ? C25 C26 1.532(2) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.531(2) . ? C28 C30 1.536(2) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.412(2) . ? C31 C32 1.420(2) . ? C32 C33 1.4030(19) . ? C32 C37 1.523(2) . ? C33 C34 1.398(2) . ? C33 H33A 1.0000 . ? C34 C35 1.390(2) . ? C34 C40 1.525(2) . ? C35 C36 1.408(2) . ? C35 H35A 1.0000 . ? C36 C43 1.523(2) . ? C37 C39 1.526(2) . ? C37 C38 1.530(2) . ? C37 H37A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.522(2) . ? C40 C41 1.526(2) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C45 1.530(3) . ? C43 C44 1.533(2) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.502(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.513(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.500(3) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.548(15) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.387(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C52 1.547(14) 3_676 ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C50A C51A 1.564(15) . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? C51A C52A 1.564(10) . ? C51A H51C 0.9900 . ? C51A H51D 0.9900 . ? C52A C52A 1.406(18) 3_676 ? C52A H52C 0.9900 . ? C52A H52D 0.9900 . ? 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 Mn1 C31 156.29(5) . . ? C1 Mn1 I1 109.60(4) . . ? C31 Mn1 I1 94.06(4) . . ? O1 Li1 C31 168.40(17) . . ? O1 Li1 C32 135.63(16) . . ? C31 Li1 C32 35.01(6) . . ? O1 Li1 C36 142.15(16) . . ? C31 Li1 C36 34.75(6) . . ? C32 Li1 C36 60.35(8) . . ? O1 Li1 C33 108.12(13) . . ? C31 Li1 C33 60.50(8) . . ? C32 Li1 C33 32.82(6) . . ? C36 Li1 C33 68.36(9) . . ? O1 Li1 C35 112.42(14) . . ? C31 Li1 C35 60.28(8) . . ? C32 Li1 C35 68.23(9) . . ? C36 Li1 C35 32.83(6) . . ? C33 Li1 C35 55.82(8) . . ? O1 Li1 C34 98.77(13) . . ? C31 Li1 C34 70.36(9) . . ? C32 Li1 C34 57.86(8) . . ? C36 Li1 C34 57.78(8) . . ? C33 Li1 C34 31.23(6) . . ? C35 Li1 C34 31.00(6) . . ? O1 Li1 I1 101.13(12) . . ? C31 Li1 I1 89.53(10) . . ? C32 Li1 I1 104.29(10) . . ? C36 Li1 I1 106.53(11) . . ? C33 Li1 I1 135.25(12) . . ? C35 Li1 I1 138.23(12) . . ? C34 Li1 I1 159.78(11) . . ? Mn1 I1 Li1 75.62(5) . . ? C46 O1 C49 109.02(12) . . ? C46 O1 Li1 117.62(13) . . ? C49 O1 Li1 119.46(13) . . ? C2 C1 C6 116.17(12) . . ? C2 C1 Mn1 120.22(9) . . ? C6 C1 Mn1 123.20(10) . . ? C3 C2 C1 121.91(12) . . ? C3 C2 C7 117.75(12) . . ? C1 C2 C7 120.10(12) . . ? C4 C3 C2 120.37(13) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 119.28(13) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 120.70(13) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 121.45(13) . . ? C5 C6 C19 117.16(12) . . ? C1 C6 C19 121.27(12) . . ? C12 C7 C8 120.08(12) . . ? C12 C7 C2 118.23(12) . . ? C8 C7 C2 121.64(12) . . ? C9 C8 C7 118.69(13) . . ? C9 C8 C13 120.13(13) . . ? C7 C8 C13 121.12(12) . . ? C10 C9 C8 121.30(13) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C11 C10 C9 119.87(14) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 120.92(14) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C11 C12 C7 119.11(13) . . ? C11 C12 C16 118.75(13) . . ? C7 C12 C16 122.13(12) . . ? C8 C13 C14 110.42(13) . . ? C8 C13 C15 113.25(13) . . ? C14 C13 C15 109.08(13) . . ? C8 C13 H13A 108.0 . . ? C14 C13 H13A 108.0 . . ? C15 C13 H13A 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C18 110.14(12) . . ? C12 C16 C17 112.29(12) . . ? C18 C16 C17 110.42(13) . . ? C12 C16 H16A 107.9 . . ? C18 C16 H16A 107.9 . . ? C17 C16 H16A 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 120.03(13) . . ? C24 C19 C6 120.80(13) . . ? C20 C19 C6 119.04(12) . . ? C21 C20 C19 119.09(13) . . ? C21 C20 C25 119.66(13) . . ? C19 C20 C25 121.16(13) . . ? C22 C21 C20 120.85(15) . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C23 C22 C21 119.98(15) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 121.30(15) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C23 C24 C19 118.73(14) . . ? C23 C24 C28 119.62(13) . . ? C19 C24 C28 121.64(13) . . ? C27 C25 C20 113.88(13) . . ? C27 C25 C26 110.18(13) . . ? C20 C25 C26 109.95(13) . . ? C27 C25 H25A 107.5 . . ? C20 C25 H25A 107.5 . . ? C26 C25 H25A 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 111.44(12) . . ? C24 C28 C30 112.40(13) . . ? C29 C28 C30 109.53(13) . . ? C24 C28 H28A 107.8 . . ? C29 C28 H28A 107.8 . . ? C30 C28 H28A 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 116.59(13) . . ? C36 C31 Mn1 119.69(10) . . ? C32 C31 Mn1 120.33(10) . . ? C36 C31 Li1 75.64(11) . . ? C32 C31 Li1 75.25(11) . . ? Mn1 C31 Li1 100.70(9) . . ? C33 C32 C31 121.25(13) . . ? C33 C32 C37 118.68(13) . . ? C31 C32 C37 120.07(12) . . ? C33 C32 Li1 79.56(11) . . ? C31 C32 Li1 69.74(10) . . ? C37 C32 Li1 122.35(12) . . ? C34 C33 C32 121.44(13) . . ? C34 C33 Li1 78.00(11) . . ? C32 C33 Li1 67.62(10) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? Li1 C33 H33A 119.0 . . ? C35 C34 C33 117.82(13) . . ? C35 C34 C40 120.54(14) . . ? C33 C34 C40 121.62(14) . . ? C35 C34 Li1 71.21(11) . . ? C33 C34 Li1 70.78(10) . . ? C40 C34 Li1 130.67(11) . . ? C34 C35 C36 121.64(14) . . ? C34 C35 Li1 77.79(11) . . ? C36 C35 Li1 67.55(10) . . ? C34 C35 H35A 118.8 . . ? C36 C35 H35A 118.8 . . ? Li1 C35 H35A 118.8 . . ? C35 C36 C31 121.22(13) . . ? C35 C36 C43 118.43(13) . . ? C31 C36 C43 120.33(13) . . ? C35 C36 Li1 79.63(11) . . ? C31 C36 Li1 69.61(10) . . ? C43 C36 Li1 121.20(13) . . ? C32 C37 C39 110.91(13) . . ? C32 C37 C38 112.65(13) . . ? C39 C37 C38 110.88(14) . . ? C32 C37 H37A 107.4 . . ? C39 C37 H37A 107.4 . . ? C38 C37 H37A 107.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C34 112.76(14) . . ? C42 C40 C41 111.30(15) . . ? C34 C40 C41 110.98(13) . . ? C42 C40 H40A 107.2 . . ? C34 C40 H40A 107.2 . . ? C41 C40 H40A 107.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C36 C43 C45 111.51(14) . . ? C36 C43 C44 111.73(15) . . ? C45 C43 C44 111.36(16) . . ? C36 C43 H43A 107.3 . . ? C45 C43 H43A 107.3 . . ? C44 C43 H43A 107.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O1 C46 C47 106.43(14) . . ? O1 C46 H46A 110.4 . . ? C47 C46 H46A 110.4 . . ? O1 C46 H46B 110.4 . . ? C47 C46 H46B 110.4 . . ? H46A C46 H46B 108.6 . . ? C46 C47 C48 102.43(15) . . ? C46 C47 H47A 111.3 . . ? C48 C47 H47A 111.3 . . ? C46 C47 H47B 111.3 . . ? C48 C47 H47B 111.3 . . ? H47A C47 H47B 109.2 . . ? C49 C48 C47 103.15(15) . . ? C49 C48 H48A 111.1 . . ? C47 C48 H48A 111.1 . . ? C49 C48 H48B 111.1 . . ? C47 C48 H48B 111.1 . . ? H48A C48 H48B 109.1 . . ? O1 C49 C48 105.48(14) . . ? O1 C49 H49A 110.6 . . ? C48 C49 H49A 110.6 . . ? O1 C49 H49B 110.6 . . ? C48 C49 H49B 110.6 . . ? H49A C49 H49B 108.8 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C50 116.6(7) . . ? C52 C51 H51A 108.1 . . ? C50 C51 H51A 108.1 . . ? C52 C51 H51B 108.1 . . ? C50 C51 H51B 108.1 . . ? H51A C51 H51B 107.3 . . ? C51 C52 C52 123.6(7) . 3_676 ? C51 C52 H52A 106.4 . . ? C52 C52 H52A 106.4 3_676 . ? C51 C52 H52B 106.4 . . ? C52 C52 H52B 106.4 3_676 . ? H52A C52 H52B 106.5 . . ? C51A C50A H50D 109.5 . . ? C51A C50A H50E 109.5 . . ? H50D C50A H50E 109.5 . . ? C51A C50A H50F 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? C50A C51A C52A 119.0(9) . . ? C50A C51A H51C 107.6 . . ? C52A C51A H51C 107.6 . . ? C50A C51A H51D 107.6 . . ? C52A C51A H51D 107.6 . . ? H51C C51A H51D 107.0 . . ? C52A C52A C51A 112.5(9) 3_676 . ? C52A C52A H52C 109.1 3_676 . ? C51A C52A H52C 109.1 . . ? C52A C52A H52D 109.1 3_676 . ? C51A C52A H52D 109.1 . . ? H52C C52A H52D 107.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.651 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.053 #===END data_cbn78fmi_tripMn2 _database_code_depnum_ccdc_archive 'CCDC 794081' #TrackingRef 'CIF-Mn-010510.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H92 Mn2, C6 H6' _chemical_formula_sum 'C66 H98 Mn2' _chemical_formula_weight 1001.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.548(2) _cell_length_b 12.8902(12) _cell_length_c 38.609(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.5250(10) _cell_angle_gamma 90.00 _cell_volume 12055.6(19) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9108 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.52 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4352 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8680 _exptl_absorpt_correction_T_max 0.9432 _exptl_absorpt_process_details 'SADABS 2007/3 (Sheldrick, 2007)' _exptl_special_details ; A pale green bolck with approximate orthogonal dimensions 0.32 x 0.21 x 0.13mm3 was placed and optically centered on the Bruker SMART1000(1) CCD system at 90(2)K. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide Omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 30 seconds per frame and 606 frames were collected, at varying phi angles (phi=0? 90? 180? 270?, for each series. The crystal to detector distance was 4.28cm, thus providing a complete sphere of data with processing to 2ThetaMax=55.21? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II Smart 1000CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49428 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13853 _reflns_number_gt 11384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX SMART 1000' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. References: 1. Bruker (2007) APEX (Version 2.0.2) and SAINT (Version 7.46A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008/1) Version 2.10, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.33 Ratio PLAT213_ALERT_2_C Atom C33 has ADP max/min Ratio ............. 4.00 prola PLAT213_ALERT_2_C Atom C35 has ADP max/min Ratio ............. 3.40 prola PLAT213_ALERT_2_C Atom C39 has ADP max/min Ratio ............. 3.10 prola These are due to bridging triisopropyl phenyl ring, which shows large librational shifts. It is likely the large librational shifts is as a result of the briding nature of the ligand, which can possible adapt two positions as a bridging ligand. PLAT410_ALERT_2_B Short Intra H...H Contact H35 .. H40A .. 1.89 Ang PLAT410_ALERT_2_C Short Intra H...H Contact H33 .. H40 .. 1.97 Ang. It is caused by the large librational shifts of C40, thus the hydrogen atoms on C40. PLAT213_ALERT_2_B Atom C34 has ADP max/min Ratio ............. 4.60 prola PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C34 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C40 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C40A These are cause by the potential disorder of the bridging group. While the phenyl ring is not treated as disorder, thus the atoms all have large thermal parameters and large ADP ratio. However, the isopropyl group (C40) was treated as disordered over two positions, thus is normal. ; _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^)+(0.0358P)^2^+25.0064P] 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 13853 _refine_ls_number_parameters 645 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.061 _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 0.348616(12) 0.56587(2) 0.110007(8) 0.02016(7) Uani 1 1 d . . . Mn2 Mn 0.287902(11) 0.40621(2) 0.127006(8) 0.02097(7) Uani 1 1 d . . . C1 C 0.39250(8) 0.68725(14) 0.09534(5) 0.0215(4) Uani 1 1 d . . . C2 C 0.43356(8) 0.66826(14) 0.07870(5) 0.0234(4) Uani 1 1 d . . . C3 C 0.45967(9) 0.74976(15) 0.06681(5) 0.0279(4) Uani 1 1 d . . . H3 H 0.4873 0.7346 0.0559 0.033 Uiso 1 1 calc R . . C4 C 0.44599(9) 0.85294(15) 0.07067(5) 0.0267(4) Uani 1 1 d . . . C5 C 0.40604(9) 0.87231(15) 0.08724(5) 0.0261(4) Uani 1 1 d . . . H5 H 0.3961 0.9421 0.0901 0.031 Uiso 1 1 calc R . . C6 C 0.38003(8) 0.79231(14) 0.09976(5) 0.0229(4) Uani 1 1 d . . . C7 C 0.45109(9) 0.55727(15) 0.07425(6) 0.0267(4) Uani 1 1 d . . . H7 H 0.4234 0.5103 0.0796 0.032 Uiso 1 1 calc R . . C8 C 0.45136(15) 0.53206(19) 0.03568(7) 0.0568(8) Uani 1 1 d . . . H8A H 0.4150 0.5474 0.0182 0.085 Uiso 1 1 calc R . . H8B H 0.4598 0.4584 0.0342 0.085 Uiso 1 1 calc R . . H8C H 0.4794 0.5743 0.0299 0.085 Uiso 1 1 calc R . . C9 C 0.50717(10) 0.53273(19) 0.10231(7) 0.0424(6) Uani 1 1 d . . . H9A H 0.5354 0.5779 0.0981 0.064 Uiso 1 1 calc R . . H9B H 0.5167 0.4601 0.0998 0.064 Uiso 1 1 calc R . . H9C H 0.5053 0.5445 0.1270 0.064 Uiso 1 1 calc R . . C10 C 0.47492(10) 0.94128(16) 0.05784(6) 0.0317(5) Uani 1 1 d . . . H10 H 0.5014 0.9100 0.0465 0.038 Uiso 1 1 calc R . . C11 C 0.43475(11) 1.00947(17) 0.02917(7) 0.0390(5) Uani 1 1 d . . . H11A H 0.4134 0.9663 0.0086 0.059 Uiso 1 1 calc R . . H11B H 0.4554 1.0616 0.0204 0.059 Uiso 1 1 calc R . . H11C H 0.4096 1.0442 0.0401 0.059 Uiso 1 1 calc R . . C12 C 0.50823(11) 1.00786(18) 0.09040(7) 0.0416(6) Uani 1 1 d . . . H12A H 0.5280 1.0622 0.0818 0.062 Uiso 1 1 calc R . . H12B H 0.5349 0.9640 0.1083 0.062 Uiso 1 1 calc R . . H12C H 0.4831 1.0399 0.1019 0.062 Uiso 1 1 calc R . . C13 C 0.33820(8) 0.82108(15) 0.11875(5) 0.0251(4) Uani 1 1 d . . . H13 H 0.3248 0.7549 0.1265 0.030 Uiso 1 1 calc R . . C14 C 0.28784(9) 0.87695(18) 0.09336(6) 0.0343(5) Uani 1 1 d . . . H14A H 0.2996 0.9415 0.0846 0.051 Uiso 1 1 calc R . . H14B H 0.2620 0.8929 0.1067 0.051 Uiso 1 1 calc R . . H14C H 0.2697 0.8322 0.0725 0.051 Uiso 1 1 calc R . . C15 C 0.36418(9) 0.88525(17) 0.15334(6) 0.0312(5) Uani 1 1 d . . . H15A H 0.3956 0.8474 0.1697 0.047 Uiso 1 1 calc R . . H15B H 0.3367 0.8976 0.1657 0.047 Uiso 1 1 calc R . . H15C H 0.3769 0.9518 0.1467 0.047 Uiso 1 1 calc R . . C16 C 0.24575(7) 0.27930(14) 0.14012(5) 0.0209(4) Uani 1 1 d . . . C17 C 0.19661(8) 0.24062(16) 0.11486(5) 0.0246(4) Uani 1 1 d . . . C18 C 0.16988(8) 0.15427(17) 0.12322(5) 0.0259(4) Uani 1 1 d . . . H18 H 0.1369 0.1301 0.1057 0.031 Uiso 1 1 calc R . . C19 C 0.19019(8) 0.10283(15) 0.15640(5) 0.0234(4) Uani 1 1 d . . . C20 C 0.23880(8) 0.13963(15) 0.18133(5) 0.0239(4) Uani 1 1 d . . . H20 H 0.2537 0.1052 0.2041 0.029 Uiso 1 1 calc R . . C21 C 0.26615(7) 0.22598(14) 0.17368(5) 0.0216(4) Uani 1 1 d . . . C22 C 0.17142(9) 0.2948(2) 0.07844(6) 0.0349(5) Uani 1 1 d . . . H22 H 0.2012 0.3379 0.0740 0.042 Uiso 1 1 calc R . . C23 C 0.15132(14) 0.2207(3) 0.04649(7) 0.0622(8) Uani 1 1 d . . . H23A H 0.1193 0.1821 0.0484 0.093 Uiso 1 1 calc R . . H23B H 0.1809 0.1720 0.0468 0.093 Uiso 1 1 calc R . . H23C H 0.1407 0.2601 0.0236 0.093 Uiso 1 1 calc R . . C24 C 0.12547(12) 0.3684(2) 0.07921(8) 0.0529(7) Uani 1 1 d . . . H24A H 0.0947 0.3287 0.0826 0.079 Uiso 1 1 calc R . . H24B H 0.1127 0.4067 0.0561 0.079 Uiso 1 1 calc R . . H24C H 0.1394 0.4175 0.0995 0.079 Uiso 1 1 calc R . . C25 C 0.16038(8) 0.00897(16) 0.16488(6) 0.0265(4) Uani 1 1 d . . . H25 H 0.1298 -0.0091 0.1421 0.032 Uiso 1 1 calc R . . C26 C 0.19844(9) -0.08509(16) 0.17532(7) 0.0354(5) Uani 1 1 d . . . H26A H 0.2143 -0.0997 0.1558 0.053 Uiso 1 1 calc R . . H26B H 0.1773 -0.1454 0.1788 0.053 Uiso 1 1 calc R . . H26C H 0.2282 -0.0706 0.1981 0.053 Uiso 1 1 calc R . . C27 C 0.13446(9) 0.03233(17) 0.19458(6) 0.0312(5) Uani 1 1 d . . . H27A H 0.1635 0.0496 0.2174 0.047 Uiso 1 1 calc R . . H27B H 0.1141 -0.0287 0.1984 0.047 Uiso 1 1 calc R . . H27C H 0.1091 0.0911 0.1870 0.047 Uiso 1 1 calc R . . C28 C 0.31942(8) 0.26073(16) 0.20241(6) 0.0270(4) Uani 1 1 d . . . H28 H 0.3316 0.3258 0.1931 0.032 Uiso 1 1 calc R . . C29 C 0.36558(9) 0.1815(2) 0.20766(6) 0.0384(5) Uani 1 1 d . . . H29A H 0.3999 0.2093 0.2246 0.058 Uiso 1 1 calc R . . H29B H 0.3708 0.1669 0.1841 0.058 Uiso 1 1 calc R . . H29C H 0.3557 0.1172 0.2177 0.058 Uiso 1 1 calc R . . C30 C 0.31079(10) 0.2873(2) 0.23866(6) 0.0390(5) Uani 1 1 d . . . H30A H 0.2999 0.2247 0.2490 0.059 Uiso 1 1 calc R . . H30B H 0.2817 0.3398 0.2346 0.059 Uiso 1 1 calc R . . H30C H 0.3452 0.3146 0.2556 0.059 Uiso 1 1 calc R . . C31 C 0.25751(8) 0.55696(15) 0.10023(6) 0.0295(5) Uani 1 1 d . A . C32 C 0.23714(10) 0.57935(16) 0.06212(7) 0.0432(7) Uani 1 1 d . . . C33 C 0.19176(13) 0.64590(19) 0.04837(10) 0.0765(13) Uani 1 1 d . A . H33 H 0.1786 0.6602 0.0229 0.092 Uiso 1 1 calc R . . C34 C 0.16583(12) 0.6910(2) 0.07090(12) 0.0913(16) Uani 1 1 d D . . C35 C 0.18514(10) 0.6697(2) 0.10785(11) 0.0679(11) Uani 1 1 d . A . H35 H 0.1673 0.7005 0.1235 0.081 Uiso 1 1 calc R . . C36 C 0.23049(9) 0.60368(17) 0.12302(8) 0.0403(6) Uani 1 1 d . . . C37 C 0.26383(12) 0.53283(19) 0.03586(6) 0.0465(7) Uani 1 1 d . . . H37 H 0.2978 0.4958 0.0510 0.056 Uiso 1 1 calc R . . C38 C 0.22729(14) 0.4517(2) 0.01027(7) 0.0578(8) Uani 1 1 d . . . H38A H 0.2177 0.3970 0.0248 0.087 Uiso 1 1 calc R . . H38B H 0.2474 0.4213 -0.0051 0.087 Uiso 1 1 calc R . . H38C H 0.1935 0.4850 -0.0053 0.087 Uiso 1 1 calc R . . C39 C 0.28271(15) 0.6138(2) 0.01293(8) 0.0768(12) Uani 1 1 d . . . H39A H 0.2505 0.6510 -0.0028 0.115 Uiso 1 1 calc R . . H39B H 0.3017 0.5787 -0.0022 0.115 Uiso 1 1 calc R . . H39C H 0.3080 0.6632 0.0292 0.115 Uiso 1 1 calc R . . C40 C 0.12278(13) 0.7707(3) 0.04637(9) 0.0242(6) Uani 0.565(4) 1 d PD A 1 H40 H 0.1267 0.7740 0.0214 0.029 Uiso 0.565(4) 1 calc PR A 1 C41 C 0.0683(4) 0.7260(11) 0.0442(3) 0.0647(4) Uani 0.565(4) 1 d PD A 1 H41A H 0.0675 0.7104 0.0689 0.097 Uiso 0.565(4) 1 calc PR A 1 H41B H 0.0622 0.6621 0.0298 0.097 Uiso 0.565(4) 1 calc PR A 1 H41C H 0.0391 0.7760 0.0326 0.097 Uiso 0.565(4) 1 calc PR A 1 C42 C 0.1321(7) 0.8765(6) 0.0637(3) 0.0290(18) Uani 0.565(4) 1 d PD A 1 H42A H 0.0980 0.9172 0.0550 0.043 Uiso 0.565(4) 1 calc PR A 1 H42B H 0.1616 0.9119 0.0572 0.043 Uiso 0.565(4) 1 calc PR A 1 H42C H 0.1428 0.8693 0.0904 0.043 Uiso 0.565(4) 1 calc PR A 1 C40A C 0.10969(17) 0.7562(3) 0.06846(12) 0.0242(6) Uani 0.435(4) 1 d PD A 2 H40A H 0.0983 0.7413 0.0905 0.029 Uiso 0.435(4) 1 calc PR A 2 C41A C 0.0658(4) 0.7240(13) 0.0353(3) 0.047(2) Uani 0.435(4) 1 d PD A 2 H41D H 0.0325 0.7651 0.0327 0.071 Uiso 0.435(4) 1 calc PR A 2 H41E H 0.0577 0.6503 0.0371 0.071 Uiso 0.435(4) 1 calc PR A 2 H41F H 0.0781 0.7352 0.0139 0.071 Uiso 0.435(4) 1 calc PR A 2 C42A C 0.1261(10) 0.8682(7) 0.0685(4) 0.0290(18) Uani 0.435(4) 1 d PD A 2 H42D H 0.1506 0.8765 0.0536 0.043 Uiso 0.435(4) 1 calc PR A 2 H42E H 0.1454 0.8904 0.0936 0.043 Uiso 0.435(4) 1 calc PR A 2 H42F H 0.0930 0.9108 0.0582 0.043 Uiso 0.435(4) 1 calc PR A 2 C43 C 0.24976(10) 0.58192(18) 0.16383(8) 0.0419(6) Uani 1 1 d . A . H43 H 0.2801 0.5297 0.1684 0.050 Uiso 1 1 calc R . . C44 C 0.20454(14) 0.5323(2) 0.17685(12) 0.0765(12) Uani 1 1 d . . . H44A H 0.1737 0.5810 0.1730 0.115 Uiso 1 1 calc R A . H44B H 0.2197 0.5157 0.2029 0.115 Uiso 1 1 calc R . . H44C H 0.1913 0.4686 0.1630 0.115 Uiso 1 1 calc R . . C45 C 0.27454(12) 0.67743(19) 0.18739(8) 0.0476(6) Uani 1 1 d . . . H45A H 0.3050 0.7051 0.1799 0.071 Uiso 1 1 calc R A . H45B H 0.2883 0.6571 0.2132 0.071 Uiso 1 1 calc R . . H45C H 0.2460 0.7307 0.1841 0.071 Uiso 1 1 calc R . . C46 C 0.37888(7) 0.41600(13) 0.13744(5) 0.0171(3) Uani 1 1 d . . . C47 C 0.41916(7) 0.44981(13) 0.17013(5) 0.0173(3) Uani 1 1 d . . . C48 C 0.46779(8) 0.39388(15) 0.18520(5) 0.0225(4) Uani 1 1 d . . . H48 H 0.4939 0.4175 0.2073 0.027 Uiso 1 1 calc R . . C49 C 0.47904(8) 0.30436(15) 0.16874(6) 0.0248(4) Uani 1 1 d . . . C50 C 0.43998(8) 0.27083(14) 0.13655(5) 0.0223(4) Uani 1 1 d . . . H50 H 0.4471 0.2100 0.1249 0.027 Uiso 1 1 calc R . . C51 C 0.39085(8) 0.32403(14) 0.12105(5) 0.0185(3) Uani 1 1 d . . . C52 C 0.41043(7) 0.54801(14) 0.18976(5) 0.0190(4) Uani 1 1 d . . . H52 H 0.3759 0.5818 0.1738 0.023 Uiso 1 1 calc R . . C53 C 0.40133(9) 0.52341(16) 0.22615(5) 0.0274(4) Uani 1 1 d . . . H53A H 0.3682 0.4804 0.2218 0.041 Uiso 1 1 calc R . . H53B H 0.3965 0.5882 0.2381 0.041 Uiso 1 1 calc R . . H53C H 0.4334 0.4859 0.2420 0.041 Uiso 1 1 calc R . . C54 C 0.45732(8) 0.62640(15) 0.19514(5) 0.0253(4) Uani 1 1 d . . . H54A H 0.4919 0.5962 0.2109 0.038 Uiso 1 1 calc R . . H54B H 0.4488 0.6894 0.2065 0.038 Uiso 1 1 calc R . . H54C H 0.4613 0.6438 0.1714 0.038 Uiso 1 1 calc R . . C55 C 0.53256(9) 0.24550(17) 0.18563(7) 0.0373(5) Uani 1 1 d . . . H55 H 0.5543 0.2834 0.2082 0.045 Uiso 1 1 calc R . . C56 C 0.52180(11) 0.13575(19) 0.19685(8) 0.0464(6) Uani 1 1 d . . . H56A H 0.4994 0.1394 0.2132 0.070 Uiso 1 1 calc R . . H56B H 0.5571 0.1019 0.2095 0.070 Uiso 1 1 calc R . . H56C H 0.5020 0.0957 0.1750 0.070 Uiso 1 1 calc R . . C57 C 0.56707(10) 0.2428(2) 0.15995(9) 0.0514(7) Uani 1 1 d . . . H57A H 0.5473 0.2037 0.1379 0.077 Uiso 1 1 calc R . . H57B H 0.6025 0.2092 0.1722 0.077 Uiso 1 1 calc R . . H57C H 0.5735 0.3139 0.1532 0.077 Uiso 1 1 calc R . . C58 C 0.34955(8) 0.28040(14) 0.08634(5) 0.0241(4) Uani 1 1 d . . . H58 H 0.3153 0.3235 0.0808 0.029 Uiso 1 1 calc R . . C59 C 0.33316(9) 0.16845(15) 0.09118(6) 0.0276(4) Uani 1 1 d . . . H59A H 0.3655 0.1233 0.0957 0.041 Uiso 1 1 calc R . . H59B H 0.3044 0.1457 0.0690 0.041 Uiso 1 1 calc R . . H59C H 0.3191 0.1646 0.1120 0.041 Uiso 1 1 calc R . . C60 C 0.37036(12) 0.28865(18) 0.05346(6) 0.0404(6) Uani 1 1 d . . . H60A H 0.3772 0.3616 0.0492 0.061 Uiso 1 1 calc R . . H60B H 0.3425 0.2604 0.0318 0.061 Uiso 1 1 calc R . . H60C H 0.4048 0.2493 0.0583 0.061 Uiso 1 1 calc R . . C61 C 0.08248(12) 0.30872(19) 0.17030(8) 0.0448(6) Uani 1 1 d . . . H61 H 0.0812 0.2858 0.1466 0.054 Uiso 1 1 calc R . . C62 C 0.03467(10) 0.33413(18) 0.17703(6) 0.0365(5) Uani 1 1 d . . . H62 H 0.0003 0.3286 0.1581 0.044 Uiso 1 1 calc R . . C63 C 0.03624(10) 0.3676(2) 0.21106(7) 0.0397(5) Uani 1 1 d . . . H63 H 0.0029 0.3852 0.2156 0.048 Uiso 1 1 calc R . . C64 C 0.08571(12) 0.3759(2) 0.23874(7) 0.0491(7) Uani 1 1 d . . . H64 H 0.0866 0.3992 0.2623 0.059 Uiso 1 1 calc R . . C65 C 0.13437(12) 0.3499(2) 0.23207(9) 0.0581(8) Uani 1 1 d . . . H65 H 0.1688 0.3552 0.2510 0.070 Uiso 1 1 calc R . . C66 C 0.13244(12) 0.3161(2) 0.19755(10) 0.0550(8) Uani 1 1 d . . . H66 H 0.1655 0.2981 0.1928 0.066 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 0.02355(14) 0.01228(13) 0.02164(14) 0.00194(10) 0.00294(11) 0.00136(10) Mn2 0.01843(13) 0.01408(13) 0.02821(15) 0.00182(11) 0.00431(11) 0.00136(10) C1 0.0281(10) 0.0178(9) 0.0158(8) 0.0013(7) 0.0032(7) 0.0019(7) C2 0.0332(10) 0.0163(9) 0.0202(9) 0.0007(7) 0.0077(8) 0.0026(8) C3 0.0406(12) 0.0198(9) 0.0270(10) 0.0015(8) 0.0161(9) 0.0026(8) C4 0.0404(11) 0.0179(9) 0.0240(10) 0.0022(7) 0.0132(9) -0.0004(8) C5 0.0399(11) 0.0137(8) 0.0253(10) 0.0004(7) 0.0112(8) 0.0025(8) C6 0.0306(10) 0.0176(9) 0.0191(9) 0.0008(7) 0.0060(8) 0.0016(7) C7 0.0371(11) 0.0162(9) 0.0308(10) 0.0022(8) 0.0166(9) 0.0026(8) C8 0.116(3) 0.0228(12) 0.0390(14) -0.0001(10) 0.0360(16) 0.0143(14) C9 0.0372(13) 0.0321(12) 0.0584(16) 0.0026(11) 0.0159(12) 0.0119(10) C10 0.0478(13) 0.0188(9) 0.0338(11) 0.0034(8) 0.0206(10) 0.0000(9) C11 0.0581(15) 0.0236(11) 0.0400(13) 0.0093(9) 0.0223(11) 0.0009(10) C12 0.0603(16) 0.0279(12) 0.0413(13) -0.0005(10) 0.0227(12) -0.0109(11) C13 0.0327(10) 0.0163(9) 0.0272(10) -0.0008(7) 0.0108(8) 0.0004(8) C14 0.0314(11) 0.0328(12) 0.0354(12) -0.0033(9) 0.0062(9) 0.0026(9) C15 0.0351(11) 0.0324(11) 0.0264(10) -0.0044(8) 0.0104(9) 0.0023(9) C16 0.0190(9) 0.0192(9) 0.0255(9) -0.0027(7) 0.0084(7) 0.0013(7) C17 0.0190(9) 0.0325(11) 0.0241(9) -0.0028(8) 0.0093(7) -0.0018(8) C18 0.0190(9) 0.0360(11) 0.0238(9) -0.0084(8) 0.0082(7) -0.0082(8) C19 0.0228(9) 0.0223(9) 0.0291(10) -0.0061(8) 0.0141(8) -0.0039(7) C20 0.0237(9) 0.0212(9) 0.0269(10) -0.0009(7) 0.0082(8) -0.0008(7) C21 0.0185(9) 0.0183(9) 0.0277(10) -0.0027(7) 0.0069(7) 0.0005(7) C22 0.0256(10) 0.0519(14) 0.0264(10) 0.0043(10) 0.0073(8) -0.0131(10) C23 0.069(2) 0.083(2) 0.0263(13) -0.0054(13) 0.0030(13) -0.0024(17) C24 0.0567(17) 0.0546(17) 0.0456(15) 0.0232(13) 0.0137(13) 0.0132(14) C25 0.0247(10) 0.0255(10) 0.0324(10) -0.0069(8) 0.0133(8) -0.0074(8) C26 0.0332(11) 0.0230(10) 0.0572(14) -0.0071(10) 0.0246(11) -0.0063(9) C27 0.0347(11) 0.0254(10) 0.0408(12) -0.0022(9) 0.0222(10) -0.0044(9) C28 0.0234(9) 0.0235(10) 0.0296(10) 0.0034(8) 0.0022(8) -0.0065(8) C29 0.0230(10) 0.0550(15) 0.0335(12) 0.0011(10) 0.0040(9) 0.0031(10) C30 0.0329(12) 0.0427(13) 0.0379(12) -0.0145(10) 0.0061(10) -0.0077(10) C31 0.0222(9) 0.0147(9) 0.0437(12) 0.0039(8) -0.0005(8) 0.0014(7) C32 0.0420(13) 0.0147(10) 0.0482(14) 0.0064(9) -0.0204(11) -0.0052(9) C33 0.068(2) 0.0138(11) 0.092(2) 0.0010(13) -0.0544(18) 0.0036(12) C34 0.0426(16) 0.0212(13) 0.148(3) -0.0269(17) -0.057(2) 0.0161(12) C35 0.0232(12) 0.0255(13) 0.135(3) -0.0317(16) -0.0029(15) 0.0071(10) C36 0.0216(10) 0.0182(10) 0.0752(18) -0.0077(10) 0.0072(11) 0.0014(8) C37 0.0648(17) 0.0304(12) 0.0251(11) 0.0113(9) -0.0128(11) -0.0171(11) C38 0.085(2) 0.0449(15) 0.0297(12) 0.0020(11) -0.0015(13) -0.0335(15) C39 0.098(3) 0.0560(18) 0.0418(15) 0.0283(14) -0.0260(16) -0.0460(18) C40 0.0225(13) 0.0244(14) 0.0250(13) 0.0070(11) 0.0066(11) 0.0075(11) C41 0.0223(7) 0.0347(6) 0.1275(3) 0.010(3) 0.0103(14) 0.006(2) C42 0.028(3) 0.0233(14) 0.034(2) 0.0059(16) 0.008(2) 0.0089(13) C40A 0.0225(13) 0.0244(14) 0.0250(13) 0.0070(11) 0.0066(11) 0.0075(11) C41A 0.022(3) 0.029(3) 0.080(6) -0.003(4) -0.001(3) 0.004(3) C42A 0.028(3) 0.0233(14) 0.034(2) 0.0059(16) 0.008(2) 0.0089(13) C43 0.0376(12) 0.0238(11) 0.0756(18) -0.0103(11) 0.0339(13) 0.0026(9) C44 0.067(2) 0.0430(17) 0.152(4) -0.019(2) 0.081(2) -0.0052(15) C45 0.0581(16) 0.0273(12) 0.0683(18) -0.0116(12) 0.0355(14) 0.0035(11) C46 0.0199(8) 0.0136(8) 0.0174(8) 0.0015(6) 0.0054(7) 0.0015(6) C47 0.0203(8) 0.0139(8) 0.0188(8) 0.0009(6) 0.0076(7) 0.0002(6) C48 0.0198(9) 0.0212(9) 0.0225(9) -0.0029(7) 0.0012(7) 0.0000(7) C49 0.0185(9) 0.0200(9) 0.0337(10) -0.0012(8) 0.0053(8) 0.0033(7) C50 0.0245(9) 0.0170(9) 0.0269(10) -0.0034(7) 0.0104(8) 0.0030(7) C51 0.0238(9) 0.0148(8) 0.0173(8) 0.0003(6) 0.0070(7) -0.0006(7) C52 0.0217(9) 0.0154(8) 0.0187(8) -0.0018(6) 0.0047(7) 0.0019(7) C53 0.0376(11) 0.0239(10) 0.0227(9) -0.0049(8) 0.0124(8) -0.0037(8) C54 0.0289(10) 0.0178(9) 0.0276(10) -0.0026(7) 0.0068(8) -0.0021(8) C55 0.0214(10) 0.0274(11) 0.0531(14) -0.0101(10) -0.0024(9) 0.0078(8) C56 0.0404(13) 0.0314(12) 0.0539(15) 0.0038(11) -0.0039(11) 0.0137(10) C57 0.0237(11) 0.0385(14) 0.091(2) -0.0166(14) 0.0173(13) 0.0037(10) C58 0.0319(10) 0.0168(9) 0.0196(9) -0.0024(7) 0.0025(8) 0.0021(8) C59 0.0324(11) 0.0196(9) 0.0268(10) -0.0039(8) 0.0036(8) -0.0012(8) C60 0.0697(17) 0.0288(11) 0.0230(10) -0.0063(9) 0.0150(11) -0.0100(11) C61 0.0588(16) 0.0307(12) 0.0562(16) -0.0018(11) 0.0341(14) -0.0038(11) C62 0.0385(12) 0.0327(12) 0.0373(12) 0.0071(9) 0.0107(10) -0.0037(10) C63 0.0384(12) 0.0428(14) 0.0439(13) 0.0024(11) 0.0215(11) -0.0047(10) C64 0.0606(17) 0.0502(16) 0.0354(13) 0.0022(11) 0.0136(12) -0.0152(13) C65 0.0377(14) 0.0420(15) 0.078(2) 0.0144(14) -0.0056(14) -0.0094(12) C66 0.0406(15) 0.0330(14) 0.099(2) 0.0012(14) 0.0335(16) 0.0021(11) _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 C1 2.1046(19) . ? Mn1 C46 2.2205(17) . ? Mn1 C31 2.239(2) . ? Mn1 Mn2 2.7783(4) . ? Mn2 C16 2.1068(19) . ? Mn2 C31 2.2221(19) . ? Mn2 C46 2.2328(18) . ? C1 C6 1.414(3) . ? C1 C2 1.415(3) . ? C2 C3 1.398(3) . ? C2 C7 1.525(3) . ? C3 C4 1.395(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 C10 1.523(3) . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C6 C13 1.521(3) . ? C7 C8 1.526(3) . ? C7 C9 1.530(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.526(3) . ? C10 C12 1.537(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.528(3) . ? C13 C15 1.531(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.412(3) . ? C16 C17 1.414(3) . ? C17 C18 1.396(3) . ? C17 C22 1.518(3) . ? C18 C19 1.388(3) . ? C18 H18 0.9500 . ? C19 C20 1.391(3) . ? C19 C25 1.520(3) . ? C20 C21 1.395(3) . ? C20 H20 0.9500 . ? C21 C28 1.525(3) . ? C22 C23 1.515(4) . ? C22 C24 1.517(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.525(3) . ? C25 C26 1.526(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.523(3) . ? C28 C29 1.524(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.414(3) . ? C31 C32 1.426(3) . ? C32 C33 1.404(3) . ? C32 C37 1.514(4) . ? C33 C34 1.378(6) . ? C33 H33 0.9500 . ? C34 C35 1.381(6) . ? C34 C40 1.582(4) . ? C34 C40A 1.639(5) . ? C35 C36 1.407(3) . ? C35 H35 0.9500 . ? C36 C43 1.520(4) . ? C37 C38 1.535(3) . ? C37 C39 1.542(3) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.486(7) . ? C40 C42 1.505(6) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40A C41A 1.468(6) . ? C40A C42A 1.504(7) . ? C40A H40A 1.0000 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43 C44 1.538(4) . ? C43 C45 1.542(3) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.420(2) . ? C46 C51 1.422(2) . ? C47 C48 1.394(2) . ? C47 C52 1.528(2) . ? C48 C49 1.391(3) . ? C48 H48 0.9500 . ? C49 C50 1.392(3) . ? C49 C55 1.518(3) . ? C50 C51 1.388(3) . ? C50 H50 0.9500 . ? C51 C58 1.526(2) . ? C52 C53 1.529(3) . ? C52 C54 1.530(3) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C57 1.522(4) . ? C55 C56 1.530(3) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C60 1.528(3) . ? C58 C59 1.531(3) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.367(3) . ? C61 C66 1.375(4) . ? C61 H61 0.9500 . ? C62 C63 1.371(3) . ? C62 H62 0.9500 . ? C63 C64 1.376(4) . ? C63 H63 0.9500 . ? C64 C65 1.388(4) . ? C64 H64 0.9500 . ? C65 C66 1.388(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mn1 C46 129.84(7) . . ? C1 Mn1 C31 127.36(7) . . ? C46 Mn1 C31 102.80(7) . . ? C1 Mn1 Mn2 178.01(5) . . ? C46 Mn1 Mn2 51.60(5) . . ? C31 Mn1 Mn2 51.21(5) . . ? C16 Mn2 C31 131.39(7) . . ? C16 Mn2 C46 125.65(7) . . ? C31 Mn2 C46 102.96(7) . . ? C16 Mn2 Mn1 176.66(5) . . ? C31 Mn2 Mn1 51.77(5) . . ? C46 Mn2 Mn1 51.20(4) . . ? C6 C1 C2 116.66(17) . . ? C6 C1 Mn1 121.32(14) . . ? C2 C1 Mn1 121.92(13) . . ? C3 C2 C1 121.28(18) . . ? C3 C2 C7 118.69(18) . . ? C1 C2 C7 120.02(17) . . ? C4 C3 C2 121.30(19) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 117.80(18) . . ? C5 C4 C10 121.26(18) . . ? C3 C4 C10 120.93(19) . . ? C4 C5 C6 121.87(18) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 121.07(18) . . ? C5 C6 C13 118.17(17) . . ? C1 C6 C13 120.76(17) . . ? C2 C7 C8 113.72(17) . . ? C2 C7 C9 110.89(18) . . ? C8 C7 C9 110.7(2) . . ? C2 C7 H7 107.1 . . ? C8 C7 H7 107.1 . . ? C9 C7 H7 107.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 C11 112.48(19) . . ? C4 C10 C12 110.56(18) . . ? C11 C10 C12 109.98(19) . . ? C4 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 C14 112.52(17) . . ? C6 C13 C15 112.07(17) . . ? C14 C13 C15 110.38(17) . . ? C6 C13 H13 107.2 . . ? C14 C13 H13 107.2 . . ? C15 C13 H13 107.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 116.70(17) . . ? C21 C16 Mn2 122.06(13) . . ? C17 C16 Mn2 121.18(14) . . ? C18 C17 C16 120.95(18) . . ? C18 C17 C22 119.09(17) . . ? C16 C17 C22 119.95(18) . . ? C19 C18 C17 121.80(18) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 117.75(18) . . ? C18 C19 C25 120.86(17) . . ? C20 C19 C25 121.38(18) . . ? C19 C20 C21 121.51(18) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C20 C21 C16 121.29(17) . . ? C20 C21 C28 118.14(17) . . ? C16 C21 C28 120.57(17) . . ? C23 C22 C24 110.3(2) . . ? C23 C22 C17 113.5(2) . . ? C24 C22 C17 111.87(19) . . ? C23 C22 H22 106.9 . . ? C24 C22 H22 106.9 . . ? C17 C22 H22 106.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 C27 111.83(16) . . ? C19 C25 C26 111.62(16) . . ? C27 C25 C26 110.52(18) . . ? C19 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 111.13(18) . . ? C30 C28 C21 112.23(17) . . ? C29 C28 C21 111.94(17) . . ? C30 C28 H28 107.1 . . ? C29 C28 H28 107.1 . . ? C21 C28 H28 107.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.8(2) . . ? C36 C31 Mn2 104.50(16) . . ? C32 C31 Mn2 128.04(16) . . ? C36 C31 Mn1 124.05(15) . . ? C32 C31 Mn1 100.52(16) . . ? Mn2 C31 Mn1 77.03(6) . . ? C33 C32 C31 120.1(3) . . ? C33 C32 C37 118.8(3) . . ? C31 C32 C37 121.1(2) . . ? C34 C33 C32 121.6(3) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 118.9(2) . . ? C33 C34 C40 106.2(3) . . ? C35 C34 C40 134.4(3) . . ? C33 C34 C40A 140.1(3) . . ? C35 C34 C40A 100.4(3) . . ? C34 C35 C36 121.8(3) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C35 C36 C31 119.9(3) . . ? C35 C36 C43 119.7(3) . . ? C31 C36 C43 120.35(19) . . ? C32 C37 C38 112.9(2) . . ? C32 C37 C39 114.0(2) . . ? C38 C37 C39 109.2(2) . . ? C32 C37 H37 106.8 . . ? C38 C37 H37 106.8 . . ? C39 C37 H37 106.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C42 112.9(6) . . ? C41 C40 C34 104.0(6) . . ? C42 C40 C34 109.9(7) . . ? C41 C40 H40 109.9 . . ? C42 C40 H40 109.9 . . ? C34 C40 H40 109.9 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41A C40A C42A 114.0(6) . . ? C41A C40A C34 108.5(7) . . ? C42A C40A C34 104.7(10) . . ? C41A C40A H40A 109.8 . . ? C42A C40A H40A 109.8 . . ? C34 C40A H40A 109.8 . . ? C40A C41A H41D 109.5 . . ? C40A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40A C42A H42D 109.5 . . ? C40A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C36 C43 C44 112.7(3) . . ? C36 C43 C45 113.6(2) . . ? C44 C43 C45 110.5(2) . . ? C36 C43 H43 106.5 . . ? C44 C43 H43 106.5 . . ? C45 C43 H43 106.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 116.98(16) . . ? C47 C46 Mn1 101.60(11) . . ? C51 C46 Mn1 127.20(12) . . ? C47 C46 Mn2 126.61(13) . . ? C51 C46 Mn2 103.37(12) . . ? Mn1 C46 Mn2 77.20(6) . . ? C48 C47 C46 120.69(16) . . ? C48 C47 C52 118.22(16) . . ? C46 C47 C52 121.09(15) . . ? C49 C48 C47 121.66(17) . . ? C49 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C48 C49 C50 118.15(17) . . ? C48 C49 C55 120.48(18) . . ? C50 C49 C55 121.37(18) . . ? C51 C50 C49 121.66(17) . . ? C51 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C50 C51 C46 120.85(16) . . ? C50 C51 C58 118.36(16) . . ? C46 C51 C58 120.78(16) . . ? C47 C52 C53 111.89(15) . . ? C47 C52 C54 112.54(15) . . ? C53 C52 C54 110.69(15) . . ? C47 C52 H52 107.1 . . ? C53 C52 H52 107.1 . . ? C54 C52 H52 107.1 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C49 C55 C57 111.1(2) . . ? C49 C55 C56 111.44(19) . . ? C57 C55 C56 110.9(2) . . ? C49 C55 H55 107.7 . . ? C57 C55 H55 107.7 . . ? C56 C55 H55 107.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C51 C58 C60 112.21(18) . . ? C51 C58 C59 112.33(15) . . ? C60 C58 C59 110.37(16) . . ? C51 C58 H58 107.2 . . ? C60 C58 H58 107.2 . . ? C59 C58 H58 107.2 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C66 120.4(3) . . ? C62 C61 H61 119.8 . . ? C66 C61 H61 119.8 . . ? C61 C62 C63 120.1(2) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C62 C63 C64 120.6(2) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C65 119.5(3) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C66 C65 C64 119.6(3) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C61 C66 C65 119.8(3) . . ? C61 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.884 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.055 #===END data_p21n_BMntBu _database_code_depnum_ccdc_archive 'CCDC 794082' #TrackingRef 'CIF-Mn-010510.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H58 Mn' _chemical_formula_sum 'C40 H58 Mn' _chemical_formula_weight 593.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Hall_group_name_H-M '-P 2yn' 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 8.8403(10) _cell_length_b 16.8782(19) _cell_length_c 24.175(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.716(2) _cell_angle_gamma 90.00 _cell_volume 3599.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9092 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.34 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9018 _exptl_absorpt_correction_T_max 0.9365 _exptl_absorpt_process_details 'SADABS 2007/3 (Sheldrick, 2007)' _exptl_special_details ; A colorless block with approximate orthogonal dimensions 0.27 x 0.20 x 0.19mm3 was placed and optically centered on the Bruker SMART1000(1) CCD system at 90(2)K. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide Omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 30 seconds per frame and 606 frames were collected, at varying phi angles (phi=0? 90? 180? 270?, for each series. The crystal to detector distance was 4.28cm, thus providing a complete sphere of data with processing to 2ThetaMax=55.21? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38670 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8321 _reflns_number_gt 5918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. References: 1. Bruker (2007) APEX (Version 2.0.2) and SAINT (Version 7.46A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008/1) Version 2.10, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.80 Ratio This is due to the large librational shift or disorder over two very close positions of the isopropyl group at the para position of phenyl ring of the complex. This large shift happens a lot in similar complexes. The following alerts are also due to this large librational shift of C33. PLAT213_ALERT_2_C Atom C33 has ADP max/min Ratio ............. 3.10 prola PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.62 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C31 ; _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^)+(0.0686P)^2^+2.6452P] 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 8321 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.43589(4) 0.84946(2) 0.154352(16) 0.02921(12) Uani 1 1 d . . . C1 C 0.2797(2) 0.76787(11) 0.18073(7) 0.0133(4) Uani 1 1 d . . . C2 C 0.2174(2) 0.72544(11) 0.13479(7) 0.0138(4) Uani 1 1 d . . . C3 C 0.1041(2) 0.66897(12) 0.13995(8) 0.0186(4) Uani 1 1 d . . . H3A H 0.0624 0.6415 0.1082 0.022 Uiso 1 1 calc R . . C4 C 0.0529(2) 0.65330(13) 0.19204(8) 0.0209(4) Uani 1 1 d . . . H4A H -0.0238 0.6147 0.1960 0.025 Uiso 1 1 calc R . . C5 C 0.1137(2) 0.69411(12) 0.23833(8) 0.0181(4) Uani 1 1 d . . . H5A H 0.0787 0.6829 0.2738 0.022 Uiso 1 1 calc R . . C6 C 0.2259(2) 0.75149(11) 0.23308(7) 0.0137(4) Uani 1 1 d . . . C7 C 0.2815(2) 0.74363(11) 0.07983(7) 0.0146(4) Uani 1 1 d . . . C8 C 0.4039(2) 0.69888(12) 0.06213(8) 0.0181(4) Uani 1 1 d . . . C9 C 0.4639(2) 0.71724(13) 0.01158(8) 0.0209(4) Uani 1 1 d . . . H9A H 0.5461 0.6868 -0.0003 0.025 Uiso 1 1 calc R . . C10 C 0.4067(2) 0.77880(12) -0.02189(8) 0.0186(4) Uani 1 1 d . . . C11 C 0.2898(2) 0.82394(12) -0.00288(8) 0.0183(4) Uani 1 1 d . . . H11A H 0.2516 0.8671 -0.0248 0.022 Uiso 1 1 calc R . . C12 C 0.2259(2) 0.80803(12) 0.04747(8) 0.0158(4) Uani 1 1 d . . . C13 C 0.4728(2) 0.63047(13) 0.09618(8) 0.0217(4) Uani 1 1 d . . . H13A H 0.4157 0.6253 0.1304 0.026 Uiso 1 1 calc R . . C14 C 0.4566(3) 0.55263(13) 0.06425(9) 0.0287(5) Uani 1 1 d . . . H14A H 0.3492 0.5426 0.0541 0.043 Uiso 1 1 calc R . . H14B H 0.4979 0.5092 0.0876 0.043 Uiso 1 1 calc R . . H14C H 0.5123 0.5561 0.0306 0.043 Uiso 1 1 calc R . . C15 C 0.6393(3) 0.64646(15) 0.11422(10) 0.0313(5) Uani 1 1 d . . . H15A H 0.6784 0.6034 0.1383 0.047 Uiso 1 1 calc R . . H15B H 0.6475 0.6967 0.1345 0.047 Uiso 1 1 calc R . . H15C H 0.6986 0.6495 0.0814 0.047 Uiso 1 1 calc R . . C16 C 0.4688(2) 0.79584(13) -0.07802(8) 0.0209(4) Uani 1 1 d . . . H16A H 0.4069 0.8396 -0.0959 0.025 Uiso 1 1 calc R . . C17 C 0.6334(3) 0.82353(16) -0.07245(10) 0.0312(5) Uani 1 1 d . . . H17A H 0.6417 0.8702 -0.0483 0.047 Uiso 1 1 calc R . . H17B H 0.6668 0.8372 -0.1091 0.047 Uiso 1 1 calc R . . H17C H 0.6974 0.7810 -0.0563 0.047 Uiso 1 1 calc R . . C18 C 0.4525(3) 0.72359(15) -0.11573(9) 0.0308(5) Uani 1 1 d . . . H18A H 0.3465 0.7063 -0.1186 0.046 Uiso 1 1 calc R . . H18B H 0.5166 0.6806 -0.1002 0.046 Uiso 1 1 calc R . . H18C H 0.4841 0.7374 -0.1526 0.046 Uiso 1 1 calc R . . C19 C 0.0942(2) 0.85891(12) 0.06418(8) 0.0188(4) Uani 1 1 d . . . H19A H 0.0733 0.8449 0.1031 0.023 Uiso 1 1 calc R . . C20 C -0.0479(3) 0.84068(16) 0.02724(10) 0.0316(5) Uani 1 1 d . . . H20A H -0.0770 0.7852 0.0322 0.047 Uiso 1 1 calc R . . H20B H -0.0274 0.8498 -0.0116 0.047 Uiso 1 1 calc R . . H20C H -0.1307 0.8753 0.0374 0.047 Uiso 1 1 calc R . . C21 C 0.1305(3) 0.94746(13) 0.06251(10) 0.0301(5) Uani 1 1 d . . . H21A H 0.2224 0.9582 0.0862 0.045 Uiso 1 1 calc R . . H21B H 0.0456 0.9777 0.0760 0.045 Uiso 1 1 calc R . . H21C H 0.1466 0.9632 0.0243 0.045 Uiso 1 1 calc R . . C22 C 0.2902(2) 0.79682(11) 0.28291(7) 0.0137(4) Uani 1 1 d . . . C23 C 0.2349(2) 0.87281(11) 0.29426(8) 0.0159(4) Uani 1 1 d . . . C24 C 0.2983(2) 0.91444(12) 0.33993(8) 0.0180(4) Uani 1 1 d . . . H24A H 0.2612 0.9659 0.3473 0.022 Uiso 1 1 calc R . . C25 C 0.4134(2) 0.88325(12) 0.37478(8) 0.0166(4) Uani 1 1 d . . . C26 C 0.4670(2) 0.80792(12) 0.36294(8) 0.0172(4) Uani 1 1 d . . . H26A H 0.5459 0.7856 0.3865 0.021 Uiso 1 1 calc R . . C27 C 0.4085(2) 0.76431(11) 0.31761(8) 0.0152(4) Uani 1 1 d . . . C28 C 0.1129(2) 0.91265(12) 0.25650(8) 0.0209(4) Uani 1 1 d . . . H28A H 0.0659 0.8714 0.2311 0.025 Uiso 1 1 calc R . . C29 C 0.1855(3) 0.97551(15) 0.22100(10) 0.0341(6) Uani 1 1 d . . . H29A H 0.2662 0.9512 0.2009 0.051 Uiso 1 1 calc R . . H29B H 0.2282 1.0178 0.2450 0.051 Uiso 1 1 calc R . . H29C H 0.1084 0.9978 0.1945 0.051 Uiso 1 1 calc R . . C30 C -0.0133(3) 0.95082(16) 0.28793(10) 0.0322(5) Uani 1 1 d . . . H30A H -0.0594 0.9107 0.3109 0.048 Uiso 1 1 calc R . . H30B H -0.0906 0.9728 0.2614 0.048 Uiso 1 1 calc R . . H30C H 0.0295 0.9934 0.3117 0.048 Uiso 1 1 calc R . . C31 C 0.4810(3) 0.92984(12) 0.42396(8) 0.0210(4) Uani 1 1 d . . . H31A H 0.4177 0.9785 0.4275 0.025 Uiso 1 1 calc R . . C32 C 0.6412(3) 0.95683(19) 0.41425(13) 0.0497(8) Uani 1 1 d . . . H32A H 0.6416 0.9840 0.3784 0.075 Uiso 1 1 calc R . . H32B H 0.7085 0.9107 0.4142 0.075 Uiso 1 1 calc R . . H32C H 0.6768 0.9932 0.4439 0.075 Uiso 1 1 calc R . . C33 C 0.4775(4) 0.88429(16) 0.47780(10) 0.0504(8) Uani 1 1 d . . . H33A H 0.3730 0.8686 0.4836 0.076 Uiso 1 1 calc R . . H33B H 0.5162 0.9179 0.5086 0.076 Uiso 1 1 calc R . . H33C H 0.5410 0.8369 0.4760 0.076 Uiso 1 1 calc R . . C34 C 0.4784(2) 0.68446(12) 0.30470(8) 0.0202(4) Uani 1 1 d . . . H34A H 0.4000 0.6527 0.2828 0.024 Uiso 1 1 calc R . . C35 C 0.6129(3) 0.69628(16) 0.26877(10) 0.0377(6) Uani 1 1 d . . . H35A H 0.6548 0.6446 0.2594 0.057 Uiso 1 1 calc R . . H35B H 0.6912 0.7277 0.2892 0.057 Uiso 1 1 calc R . . H35C H 0.5790 0.7242 0.2346 0.057 Uiso 1 1 calc R . . C36 C 0.5281(3) 0.63718(12) 0.35642(9) 0.0223(4) Uani 1 1 d . . . H36A H 0.4428 0.6320 0.3801 0.033 Uiso 1 1 calc R . . H36B H 0.6118 0.6647 0.3768 0.033 Uiso 1 1 calc R . . H36C H 0.5618 0.5844 0.3456 0.033 Uiso 1 1 calc R . . C37 C 0.6076(3) 0.93246(14) 0.14281(10) 0.0289(5) Uani 1 1 d . . . C38 C 0.7585(3) 0.88995(16) 0.15725(11) 0.0337(5) Uani 1 1 d . . . H38A H 0.8425 0.9273 0.1541 0.051 Uiso 1 1 calc R . . H38B H 0.7696 0.8457 0.1316 0.051 Uiso 1 1 calc R . . H38C H 0.7599 0.8698 0.1953 0.051 Uiso 1 1 calc R . . C39 C 0.5958(3) 1.00335(17) 0.18182(13) 0.0441(7) Uani 1 1 d . . . H39A H 0.6812 1.0393 0.1774 0.066 Uiso 1 1 calc R . . H39B H 0.5984 0.9846 0.2202 0.066 Uiso 1 1 calc R . . H39C H 0.5004 1.0315 0.1728 0.066 Uiso 1 1 calc R . . C40 C 0.6064(3) 0.96290(16) 0.08310(11) 0.0369(6) Uani 1 1 d . . . H40A H 0.6950 0.9968 0.0791 0.055 Uiso 1 1 calc R . . H40B H 0.5137 0.9935 0.0744 0.055 Uiso 1 1 calc R . . H40C H 0.6098 0.9179 0.0576 0.055 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 0.0272(2) 0.02772(19) 0.0333(2) 0.00055(15) 0.00643(15) -0.00922(15) C1 0.0146(9) 0.0144(9) 0.0110(9) 0.0001(7) 0.0021(7) 0.0013(7) C2 0.0162(9) 0.0160(9) 0.0092(8) -0.0004(7) 0.0006(7) 0.0035(7) C3 0.0220(10) 0.0209(10) 0.0127(9) -0.0046(8) 0.0002(8) -0.0035(8) C4 0.0234(10) 0.0224(10) 0.0170(10) -0.0019(8) 0.0034(8) -0.0079(9) C5 0.0227(10) 0.0213(10) 0.0108(9) 0.0013(8) 0.0051(8) -0.0009(8) C6 0.0184(9) 0.0141(9) 0.0086(8) -0.0005(7) 0.0003(7) 0.0034(7) C7 0.0184(10) 0.0170(9) 0.0084(8) -0.0030(7) 0.0002(7) -0.0010(8) C8 0.0223(10) 0.0211(10) 0.0109(9) 0.0007(8) 0.0016(8) 0.0030(8) C9 0.0217(10) 0.0280(11) 0.0136(9) -0.0002(8) 0.0059(8) 0.0076(9) C10 0.0196(10) 0.0248(10) 0.0116(9) 0.0009(8) 0.0030(8) -0.0007(8) C11 0.0213(10) 0.0209(10) 0.0129(9) 0.0025(8) 0.0013(8) 0.0028(8) C12 0.0172(9) 0.0180(9) 0.0123(9) -0.0015(7) 0.0010(7) 0.0010(8) C13 0.0273(11) 0.0250(11) 0.0132(9) 0.0019(8) 0.0049(8) 0.0115(9) C14 0.0400(14) 0.0234(11) 0.0228(11) 0.0020(9) 0.0026(10) 0.0051(10) C15 0.0350(13) 0.0338(13) 0.0242(12) -0.0003(10) -0.0059(10) 0.0117(11) C16 0.0211(10) 0.0299(11) 0.0121(9) 0.0037(8) 0.0049(8) 0.0022(9) C17 0.0252(12) 0.0472(15) 0.0216(11) 0.0044(10) 0.0044(9) -0.0050(11) C18 0.0399(14) 0.0402(13) 0.0134(10) -0.0003(10) 0.0095(9) -0.0041(11) C19 0.0207(10) 0.0242(10) 0.0117(9) 0.0003(8) 0.0032(8) 0.0058(8) C20 0.0217(11) 0.0467(15) 0.0261(12) -0.0086(11) -0.0001(9) 0.0094(10) C21 0.0383(13) 0.0239(11) 0.0290(12) -0.0007(9) 0.0096(10) 0.0090(10) C22 0.0177(9) 0.0165(9) 0.0070(8) 0.0002(7) 0.0022(7) -0.0015(7) C23 0.0191(10) 0.0166(9) 0.0119(9) 0.0006(7) 0.0018(7) 0.0019(8) C24 0.0255(11) 0.0138(9) 0.0147(9) -0.0029(7) 0.0021(8) 0.0017(8) C25 0.0221(10) 0.0161(9) 0.0116(9) -0.0024(7) 0.0010(8) -0.0021(8) C26 0.0212(10) 0.0161(9) 0.0137(9) -0.0016(7) -0.0030(8) 0.0017(8) C27 0.0200(10) 0.0140(9) 0.0118(9) -0.0005(7) 0.0024(7) 0.0004(8) C28 0.0271(11) 0.0195(10) 0.0155(10) -0.0031(8) -0.0030(8) 0.0071(9) C29 0.0427(15) 0.0316(13) 0.0279(12) 0.0095(10) 0.0015(11) 0.0110(11) C30 0.0310(13) 0.0398(14) 0.0256(12) -0.0024(10) -0.0006(10) 0.0150(11) C31 0.0297(11) 0.0165(9) 0.0163(10) -0.0058(8) -0.0032(8) -0.0006(8) C32 0.0386(16) 0.0544(18) 0.0560(18) -0.0318(15) 0.0031(14) -0.0187(13) C33 0.105(3) 0.0315(13) 0.0142(11) -0.0064(10) -0.0030(14) -0.0171(16) C34 0.0257(11) 0.0171(10) 0.0167(10) -0.0054(8) -0.0069(8) 0.0058(8) C35 0.0509(16) 0.0406(14) 0.0232(12) 0.0033(10) 0.0135(11) 0.0252(13) C36 0.0255(11) 0.0176(10) 0.0234(11) 0.0004(8) -0.0018(9) 0.0038(8) C37 0.0262(12) 0.0270(11) 0.0343(13) -0.0028(10) 0.0078(10) -0.0071(10) C38 0.0307(13) 0.0377(13) 0.0332(13) 0.0018(11) 0.0045(10) -0.0041(11) C39 0.0391(15) 0.0373(14) 0.0575(18) -0.0165(13) 0.0149(13) -0.0115(12) C40 0.0325(13) 0.0371(14) 0.0417(15) 0.0083(12) 0.0073(11) 0.0000(11) _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 C1 2.0794(19) . ? Mn1 C37 2.097(2) . ? C1 C2 1.404(3) . ? C1 C6 1.408(3) . ? C2 C3 1.394(3) . ? C2 C7 1.509(3) . ? C3 C4 1.391(3) . ? C3 H3A 0.9500 . ? C4 C5 1.392(3) . ? C4 H4A 0.9500 . ? C5 C6 1.398(3) . ? C5 H5A 0.9500 . ? C6 C22 1.507(3) . ? C7 C8 1.409(3) . ? C7 C12 1.409(3) . ? C8 C9 1.398(3) . ? C8 C13 1.522(3) . ? C9 C10 1.392(3) . ? C9 H9A 0.9500 . ? C10 C11 1.387(3) . ? C10 C16 1.524(3) . ? C11 C12 1.400(3) . ? C11 H11A 0.9500 . ? C12 C19 1.522(3) . ? C13 C14 1.526(3) . ? C13 C15 1.532(3) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.524(3) . ? C16 C17 1.526(3) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.525(3) . ? C19 C21 1.530(3) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.406(3) . ? C22 C27 1.409(3) . ? C23 C24 1.395(3) . ? C23 C28 1.524(3) . ? C24 C25 1.382(3) . ? C24 H24A 0.9500 . ? C25 C26 1.393(3) . ? C25 C31 1.516(3) . ? C26 C27 1.392(3) . ? C26 H26A 0.9500 . ? C27 C34 1.523(3) . ? C28 C29 1.532(3) . ? C28 C30 1.532(3) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.514(3) . ? C31 C32 1.520(3) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.524(3) . ? C34 C35 1.531(3) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.531(3) . ? C37 C40 1.531(4) . ? C37 C38 1.535(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mn1 C37 169.68(9) . . ? C2 C1 C6 118.22(17) . . ? C2 C1 Mn1 109.25(13) . . ? C6 C1 Mn1 132.48(14) . . ? C3 C2 C1 121.71(17) . . ? C3 C2 C7 122.05(17) . . ? C1 C2 C7 116.24(17) . . ? C4 C3 C2 119.27(18) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 120.14(19) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 120.61(18) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 120.04(17) . . ? C5 C6 C22 120.82(16) . . ? C1 C6 C22 119.13(17) . . ? C8 C7 C12 119.46(17) . . ? C8 C7 C2 119.88(17) . . ? C12 C7 C2 120.55(17) . . ? C9 C8 C7 119.28(18) . . ? C9 C8 C13 118.66(18) . . ? C7 C8 C13 122.06(17) . . ? C10 C9 C8 122.00(19) . . ? C10 C9 H9A 119.0 . . ? C8 C9 H9A 119.0 . . ? C11 C10 C9 117.90(18) . . ? C11 C10 C16 120.72(18) . . ? C9 C10 C16 121.38(18) . . ? C10 C11 C12 122.27(18) . . ? C10 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C11 C12 C7 119.01(18) . . ? C11 C12 C19 118.73(17) . . ? C7 C12 C19 122.20(17) . . ? C8 C13 C14 111.00(17) . . ? C8 C13 C15 111.34(19) . . ? C14 C13 C15 110.65(18) . . ? C8 C13 H13A 107.9 . . ? C14 C13 H13A 107.9 . . ? C15 C13 H13A 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 C18 110.88(18) . . ? C10 C16 C17 112.06(17) . . ? C18 C16 C17 110.51(19) . . ? C10 C16 H16A 107.7 . . ? C18 C16 H16A 107.7 . . ? C17 C16 H16A 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C19 C20 110.25(17) . . ? C12 C19 C21 112.27(18) . . ? C20 C19 C21 110.34(19) . . ? C12 C19 H19A 107.9 . . ? C20 C19 H19A 107.9 . . ? C21 C19 H19A 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 119.56(17) . . ? C23 C22 C6 120.07(17) . . ? C27 C22 C6 120.35(16) . . ? C24 C23 C22 119.14(18) . . ? C24 C23 C28 118.97(17) . . ? C22 C23 C28 121.82(17) . . ? C25 C24 C23 122.17(18) . . ? C25 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? C24 C25 C26 117.98(18) . . ? C24 C25 C31 121.18(18) . . ? C26 C25 C31 120.83(18) . . ? C27 C26 C25 122.05(18) . . ? C27 C26 H26A 119.0 . . ? C25 C26 H26A 119.0 . . ? C26 C27 C22 119.10(17) . . ? C26 C27 C34 119.65(17) . . ? C22 C27 C34 121.18(17) . . ? C23 C28 C29 109.58(18) . . ? C23 C28 C30 113.49(17) . . ? C29 C28 C30 109.36(19) . . ? C23 C28 H28A 108.1 . . ? C29 C28 H28A 108.1 . . ? C30 C28 H28A 108.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C25 112.46(18) . . ? C33 C31 C32 110.9(2) . . ? C25 C31 C32 111.00(19) . . ? C33 C31 H31A 107.4 . . ? C25 C31 H31A 107.4 . . ? C32 C31 H31A 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 C36 113.23(16) . . ? C27 C34 C35 109.95(18) . . ? C36 C34 C35 109.89(18) . . ? C27 C34 H34A 107.9 . . ? C36 C34 H34A 107.9 . . ? C35 C34 H34A 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C40 108.8(2) . . ? C39 C37 C38 108.5(2) . . ? C40 C37 C38 108.9(2) . . ? C39 C37 Mn1 111.18(16) . . ? C40 C37 Mn1 112.87(17) . . ? C38 C37 Mn1 106.46(16) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.531 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.062