# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. W Geiger' _publ_contact_author_email william.geiger@uvm.edu _publ_section_title ; Anodic Electrochemical Behavior of New Mn and Re Tricarbonyl Complexes of Tris(oxazolinyl)phenyl borate Ligands: Comparison to Analogous Tris(pyrazolyl) borate Complexes ; loop_ _publ_author_name Geiger A.Sadow K.Wu D.Mukherjee A.Ellern #===end data_ToMRe(CO)3_sad27 _database_code_depnum_ccdc_archive 'CCDC 817558' #TrackingRef '- Tom_Re_combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H29 B Mn N3 O6), 0.5 (C7 H8)' _chemical_formula_sum 'C27.50 H33 B Mn N3 O6' _chemical_formula_weight 567.32 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.766(4) _cell_length_b 9.139(4) _cell_length_c 17.493(8) _cell_angle_alpha 88.637(8) _cell_angle_beta 82.993(7) _cell_angle_gamma 87.624(7) _cell_volume 1389.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 930 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.42 _exptl_crystal_description colorless _exptl_crystal_colour prism _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; The best but very small and weakly diffracted weak crystal was selected under ambient conditions and covered with PARATONE oil. The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on SMART 1000 CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 40 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 40 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11991 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.52 _reflns_number_total 6274 _reflns_number_gt 4497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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. The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. All hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. One of main cluster rings shows the signs of small disorder. The highest residual densitypeaks were found in this disordered area, however, splitting model lead to unstable refinement, therefore SIMU and DELU similarity restrains were used for this moiety. PART -1 instruction was used to model disordered by symmetry toluene solvent Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _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^)+(0.1559P)^2^+4.6298P] 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 6274 _refine_ls_number_parameters 367 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2832 _refine_ls_wR_factor_gt 0.2461 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.088 _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 1.07013(8) -0.05012(8) 0.78198(4) 0.0190(2) Uani 1 1 d . . . B1 B 0.8902(6) 0.1226(5) 0.6508(3) 0.0158(9) Uani 1 1 d . . . C1 C 1.0749(5) 0.1423(5) 0.6423(3) 0.0174(9) Uani 1 1 d . . . C2 C 1.3107(6) 0.1991(6) 0.5882(3) 0.0301(11) Uani 1 1 d . . . H2A H 1.3658 0.2906 0.5756 0.036 Uiso 1 1 calc R . . H2B H 1.3556 0.1218 0.5526 0.036 Uiso 1 1 calc R . . C3 C 1.3192(5) 0.1516(5) 0.6723(3) 0.0232(10) Uani 1 1 d . . . C4 C 1.3271(6) 0.2854(6) 0.7226(4) 0.0344(13) Uani 1 1 d . . . H4A H 1.2377 0.3515 0.7180 0.052 Uiso 1 1 calc R . . H4B H 1.4216 0.3368 0.7056 0.052 Uiso 1 1 calc R . . H4C H 1.3272 0.2534 0.7765 0.052 Uiso 1 1 calc R . . C5 C 1.4535(6) 0.0426(6) 0.6810(4) 0.0306(12) Uani 1 1 d . . . H5A H 1.4549 0.0163 0.7355 0.046 Uiso 1 1 calc R . . H5B H 1.5504 0.0874 0.6610 0.046 Uiso 1 1 calc R . . H5C H 1.4413 -0.0456 0.6519 0.046 Uiso 1 1 calc R . . C6 C 0.8345(5) 0.1687(5) 0.7399(3) 0.0184(9) Uani 1 1 d . . . C7 C 0.6930(11) 0.2775(10) 0.8405(4) 0.0628(13) Uani 1 1 d U . . H7A H 0.5884 0.2456 0.8596 0.075 Uiso 1 1 calc R . . H7B H 0.7031 0.3788 0.8576 0.075 Uiso 1 1 calc R . . C8 C 0.8101(11) 0.1783(10) 0.8704(4) 0.0657(12) Uani 1 1 d U . . C9 C 0.9316(11) 0.2959(10) 0.8952(5) 0.0675(13) Uani 1 1 d U . . H9A H 1.0185 0.2426 0.9148 0.101 Uiso 1 1 calc R . . H9B H 0.8793 0.3594 0.9354 0.101 Uiso 1 1 calc R . . H9C H 0.9693 0.3556 0.8501 0.101 Uiso 1 1 calc R . . C10 C 0.7667(11) 0.0818(10) 0.9329(4) 0.0679(13) Uani 1 1 d U . . H10A H 0.6962 0.0108 0.9174 0.102 Uiso 1 1 calc R . . H10B H 0.7154 0.1380 0.9764 0.102 Uiso 1 1 calc R . . H10C H 0.8585 0.0299 0.9483 0.102 Uiso 1 1 calc R . . C11 C 0.8742(5) -0.0544(5) 0.6557(3) 0.0190(9) Uani 1 1 d . . . C12 C 0.8146(7) -0.2787(6) 0.6214(3) 0.0317(12) Uani 1 1 d . . . H12A H 0.8944 -0.3200 0.5820 0.038 Uiso 1 1 calc R . . H12B H 0.7185 -0.3315 0.6205 0.038 Uiso 1 1 calc R . . C13 C 0.8683(6) -0.2888(5) 0.7017(3) 0.0245(10) Uani 1 1 d . . . C14 C 0.7299(6) -0.3012(6) 0.7639(4) 0.0349(13) Uani 1 1 d . . . H14A H 0.7657 -0.3066 0.8148 0.052 Uiso 1 1 calc R . . H14B H 0.6751 -0.3899 0.7558 0.052 Uiso 1 1 calc R . . H14C H 0.6603 -0.2151 0.7607 0.052 Uiso 1 1 calc R . . C15 C 0.9868(7) -0.4136(5) 0.7094(4) 0.0325(12) Uani 1 1 d . . . H15A H 1.0194 -0.4133 0.7610 0.049 Uiso 1 1 calc R . . H15B H 1.0762 -0.4004 0.6707 0.049 Uiso 1 1 calc R . . H15C H 0.9410 -0.5072 0.7015 0.049 Uiso 1 1 calc R . . C16 C 0.8111(5) 0.2057(5) 0.5817(3) 0.0165(9) Uani 1 1 d . . . C17 C 0.8218(6) 0.1426(5) 0.5088(3) 0.0238(10) Uani 1 1 d . . . H17A H 0.8723 0.0492 0.5015 0.029 Uiso 1 1 calc R . . C18 C 0.7613(6) 0.2118(6) 0.4469(3) 0.0276(11) Uani 1 1 d . . . H18A H 0.7708 0.1649 0.3985 0.033 Uiso 1 1 calc R . . C19 C 0.6877(6) 0.3481(5) 0.4550(3) 0.0253(10) Uani 1 1 d . . . H19A H 0.6458 0.3953 0.4128 0.030 Uiso 1 1 calc R . . C20 C 0.6760(7) 0.4149(5) 0.5261(3) 0.0282(11) Uani 1 1 d . . . H20A H 0.6261 0.5088 0.5325 0.034 Uiso 1 1 calc R . . C21 C 0.7370(6) 0.3451(5) 0.5883(3) 0.0229(10) Uani 1 1 d . . . H21A H 0.7282 0.3932 0.6363 0.027 Uiso 1 1 calc R . . C22 C 0.9976(6) -0.1687(6) 0.8604(3) 0.0276(11) Uani 1 1 d . . . C23 C 1.1890(6) 0.0236(6) 0.8486(3) 0.0293(11) Uani 1 1 d . . . C24 C 1.2222(6) -0.1884(6) 0.7600(3) 0.0257(10) Uani 1 1 d . . . N1 N 1.1622(4) 0.0863(4) 0.6916(2) 0.0181(8) Uani 1 1 d . . . N2 N 0.8930(5) 0.1106(4) 0.7980(2) 0.0210(8) Uani 1 1 d . . . N3 N 0.9330(4) -0.1391(4) 0.7056(2) 0.0169(8) Uani 1 1 d . . . O1 O 1.1455(4) 0.2222(4) 0.5837(2) 0.0248(8) Uani 1 1 d . . . O2 O 0.7187(4) 0.2717(4) 0.75765(19) 0.0237(7) Uani 1 1 d . . . O3 O 0.7890(4) -0.1220(4) 0.6083(2) 0.0253(8) Uani 1 1 d . . . O4 O 0.9638(6) -0.2487(5) 0.9117(3) 0.0477(12) Uani 1 1 d . . . O5 O 1.2678(6) 0.0580(6) 0.8924(3) 0.0510(12) Uani 1 1 d . . . O6 O 1.3181(5) -0.2797(4) 0.7510(3) 0.0374(10) Uani 1 1 d . . . C25 C 0.706(3) 0.512(3) 0.0759(15) 0.075(7) Uani 0.50 1 d P A -1 H25A H 0.7022 0.4263 0.1109 0.112 Uiso 0.50 1 calc PR A -1 H25B H 0.6929 0.6015 0.1061 0.112 Uiso 0.50 1 calc PR A -1 H25C H 0.8063 0.5112 0.0439 0.112 Uiso 0.50 1 calc PR A -1 C26 C 0.5855(13) 0.5068(13) 0.0273(6) 0.044(3) Uani 0.50 1 d PG A -1 C27 C 0.4892(18) 0.3889(10) 0.0345(8) 0.050(6) Uani 0.50 1 d PG A -1 H27A H 0.5051 0.3116 0.0704 0.060 Uiso 0.50 1 calc PR A -1 C28 C 0.3697(15) 0.3840(17) -0.0107(11) 0.085(8) Uani 0.50 1 d PG A -1 H28A H 0.3039 0.3034 -0.0057 0.102 Uiso 0.50 1 calc PR A -1 C29 C 0.3465(12) 0.497(2) -0.0631(10) 0.091(12) Uani 0.50 1 d PG A -1 H29A H 0.2648 0.4937 -0.0940 0.110 Uiso 0.50 1 calc PR A -1 C30 C 0.4428(16) 0.6149(18) -0.0703(7) 0.062(5) Uani 0.50 1 d PG A -1 H30A H 0.4269 0.6921 -0.1062 0.074 Uiso 0.50 1 calc PR A -1 C31 C 0.5623(13) 0.6198(10) -0.0251(7) 0.040(5) Uani 0.50 1 d PG A -1 H31A H 0.6281 0.7003 -0.0301 0.048 Uiso 0.50 1 calc PR A -1 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 0.0179(4) 0.0221(4) 0.0172(4) 0.0046(3) -0.0044(3) 0.0024(3) B1 0.015(2) 0.017(2) 0.015(2) 0.0028(17) -0.0022(18) 0.0006(18) C1 0.018(2) 0.014(2) 0.020(2) -0.0010(16) -0.0006(17) -0.0009(16) C2 0.020(2) 0.035(3) 0.035(3) 0.010(2) -0.002(2) -0.004(2) C3 0.014(2) 0.022(2) 0.034(3) 0.004(2) -0.0044(19) 0.0009(18) C4 0.025(3) 0.029(3) 0.051(4) -0.002(2) -0.009(2) -0.002(2) C5 0.014(2) 0.031(3) 0.047(3) 0.005(2) -0.007(2) 0.001(2) C6 0.016(2) 0.014(2) 0.025(2) -0.0007(17) -0.0019(18) 0.0007(16) C7 0.079(3) 0.072(3) 0.031(2) -0.005(2) 0.006(2) 0.031(3) C8 0.080(3) 0.074(3) 0.037(2) -0.0026(19) 0.004(2) 0.030(2) C9 0.081(3) 0.076(3) 0.039(2) -0.004(2) 0.003(2) 0.029(2) C10 0.083(3) 0.076(3) 0.039(2) -0.0004(19) 0.006(2) 0.031(2) C11 0.017(2) 0.020(2) 0.021(2) -0.0001(17) -0.0026(17) 0.0017(17) C12 0.039(3) 0.020(2) 0.038(3) 0.000(2) -0.013(2) -0.002(2) C13 0.023(2) 0.017(2) 0.033(3) 0.0054(19) -0.007(2) -0.0010(18) C14 0.027(3) 0.032(3) 0.046(3) 0.008(2) -0.001(2) -0.007(2) C15 0.032(3) 0.015(2) 0.050(3) 0.006(2) -0.006(2) 0.002(2) C16 0.016(2) 0.018(2) 0.016(2) 0.0043(16) -0.0056(16) 0.0015(16) C17 0.030(3) 0.022(2) 0.019(2) -0.0003(18) -0.0037(19) 0.007(2) C18 0.039(3) 0.029(3) 0.015(2) 0.0007(19) -0.005(2) 0.004(2) C19 0.029(3) 0.026(2) 0.021(2) 0.0046(19) -0.007(2) 0.006(2) C20 0.038(3) 0.020(2) 0.028(3) 0.0005(19) -0.009(2) 0.007(2) C21 0.028(2) 0.020(2) 0.021(2) -0.0029(18) -0.0084(19) 0.0010(19) C22 0.029(3) 0.032(3) 0.021(2) 0.009(2) -0.003(2) 0.002(2) C23 0.031(3) 0.037(3) 0.020(2) 0.002(2) -0.007(2) 0.002(2) C24 0.025(2) 0.031(3) 0.021(2) 0.0071(19) -0.0046(19) -0.001(2) N1 0.0137(17) 0.0212(19) 0.0190(19) 0.0007(15) -0.0013(15) -0.0002(15) N2 0.0203(19) 0.025(2) 0.0170(19) -0.0002(15) -0.0013(15) -0.0014(16) N3 0.0168(18) 0.0151(17) 0.0183(18) 0.0030(14) -0.0012(14) 0.0016(14) O1 0.0222(17) 0.0271(18) 0.0240(18) 0.0095(14) 0.0003(14) -0.0006(14) O2 0.0261(18) 0.0245(17) 0.0193(16) -0.0003(13) -0.0018(14) 0.0098(14) O3 0.0311(19) 0.0170(16) 0.0306(19) -0.0011(14) -0.0136(15) -0.0028(14) O4 0.055(3) 0.053(3) 0.033(2) 0.021(2) 0.001(2) 0.004(2) O5 0.046(3) 0.073(3) 0.039(3) -0.004(2) -0.023(2) -0.003(2) O6 0.028(2) 0.033(2) 0.051(3) 0.0072(18) -0.0093(18) 0.0089(17) C25 0.093(19) 0.084(15) 0.046(10) -0.022(10) -0.007(13) 0.030(12) C26 0.055(9) 0.045(8) 0.029(7) -0.012(6) 0.006(6) 0.012(7) C27 0.065(16) 0.033(8) 0.046(11) -0.009(7) 0.017(11) -0.012(8) C28 0.056(13) 0.074(14) 0.11(2) -0.044(14) 0.048(13) -0.027(11) C29 0.041(13) 0.15(3) 0.08(2) -0.054(19) -0.008(13) 0.003(15) C30 0.053(10) 0.090(14) 0.040(9) -0.011(9) -0.009(7) 0.031(10) C31 0.028(9) 0.059(11) 0.031(8) 0.009(7) 0.004(6) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C22 1.798(5) . ? Mn1 C24 1.811(5) . ? Mn1 C23 1.814(5) . ? Mn1 N2 2.091(4) . ? Mn1 N1 2.094(4) . ? Mn1 N3 2.101(4) . ? B1 C16 1.623(6) . ? B1 C1 1.625(7) . ? B1 C11 1.629(7) . ? B1 C6 1.636(7) . ? C1 N1 1.303(6) . ? C1 O1 1.346(5) . ? C2 O1 1.466(6) . ? C2 C3 1.533(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.520(6) . ? C3 C5 1.530(7) . ? C3 C4 1.532(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N2 1.287(6) . ? C6 O2 1.368(5) . ? C7 O2 1.441(7) . ? C7 C8 1.477(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.413(12) . ? C8 N2 1.513(8) . ? C8 C9 1.645(14) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.293(6) . ? C11 O3 1.357(6) . ? C12 O3 1.457(6) . ? C12 C13 1.533(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N3 1.508(6) . ? C13 C15 1.526(7) . ? C13 C14 1.534(8) . ? 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 1.403(6) . ? C16 C21 1.407(6) . ? C17 C18 1.391(7) . ? C17 H17A 0.9500 . ? C18 C19 1.382(7) . ? C18 H18A 0.9500 . ? C19 C20 1.388(7) . ? C19 H19A 0.9500 . ? C20 C21 1.400(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 O4 1.162(6) . ? C23 O5 1.149(7) . ? C24 O6 1.159(6) . ? C25 C26 1.44(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 H31A 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 C22 Mn1 C24 86.6(2) . . ? C22 Mn1 C23 86.2(2) . . ? C24 Mn1 C23 87.0(2) . . ? C22 Mn1 N2 96.6(2) . . ? C24 Mn1 N2 175.47(19) . . ? C23 Mn1 N2 96.4(2) . . ? C22 Mn1 N1 178.0(2) . . ? C24 Mn1 N1 91.88(19) . . ? C23 Mn1 N1 92.5(2) . . ? N2 Mn1 N1 84.98(16) . . ? C22 Mn1 N3 93.0(2) . . ? C24 Mn1 N3 92.3(2) . . ? C23 Mn1 N3 179.0(2) . . ? N2 Mn1 N3 84.31(15) . . ? N1 Mn1 N3 88.29(15) . . ? C16 B1 C1 112.2(4) . . ? C16 B1 C11 115.3(4) . . ? C1 B1 C11 103.4(4) . . ? C16 B1 C6 119.2(4) . . ? C1 B1 C6 103.1(4) . . ? C11 B1 C6 101.7(3) . . ? N1 C1 O1 116.3(4) . . ? N1 C1 B1 122.9(4) . . ? O1 C1 B1 120.8(4) . . ? O1 C2 C3 103.9(4) . . ? O1 C2 H2A 111.0 . . ? C3 C2 H2A 111.0 . . ? O1 C2 H2B 111.0 . . ? C3 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N1 C3 C5 113.7(4) . . ? N1 C3 C4 108.7(4) . . ? C5 C3 C4 110.8(4) . . ? N1 C3 C2 100.1(4) . . ? C5 C3 C2 112.4(4) . . ? C4 C3 C2 110.6(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 O2 115.3(4) . . ? N2 C6 B1 123.4(4) . . ? O2 C6 B1 121.4(4) . . ? O2 C7 C8 107.1(6) . . ? O2 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O2 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C10 C8 C7 119.7(8) . . ? C10 C8 N2 116.9(7) . . ? C7 C8 N2 102.9(6) . . ? C10 C8 C9 110.0(7) . . ? C7 C8 C9 101.3(7) . . ? N2 C8 C9 103.9(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 O3 115.2(4) . . ? N3 C11 B1 124.1(4) . . ? O3 C11 B1 120.6(4) . . ? O3 C12 C13 103.8(4) . . ? O3 C12 H12A 111.0 . . ? C13 C12 H12A 111.0 . . ? O3 C12 H12B 111.0 . . ? C13 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? N3 C13 C15 113.2(4) . . ? N3 C13 C12 100.2(4) . . ? C15 C13 C12 112.8(5) . . ? N3 C13 C14 108.7(4) . . ? C15 C13 C14 111.1(4) . . ? C12 C13 C14 110.3(5) . . ? 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 C21 115.8(4) . . ? C17 C16 B1 120.2(4) . . ? C21 C16 B1 123.9(4) . . ? C18 C17 C16 122.5(4) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19A 120.6 . . ? C20 C19 H19A 120.6 . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C16 121.7(4) . . ? C20 C21 H21A 119.1 . . ? C16 C21 H21A 119.1 . . ? O4 C22 Mn1 174.1(5) . . ? O5 C23 Mn1 174.0(5) . . ? O6 C24 Mn1 175.6(5) . . ? C1 N1 C3 106.9(4) . . ? C1 N1 Mn1 120.4(3) . . ? C3 N1 Mn1 132.5(3) . . ? C6 N2 C8 108.0(5) . . ? C6 N2 Mn1 120.6(3) . . ? C8 N2 Mn1 131.4(4) . . ? C11 N3 C13 108.0(4) . . ? C11 N3 Mn1 119.5(3) . . ? C13 N3 Mn1 132.0(3) . . ? C1 O1 C2 105.6(4) . . ? C6 O2 C7 106.6(4) . . ? C11 O3 C12 106.1(4) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 120.0 . . ? C27 C26 C25 119.3(17) . . ? C31 C26 C25 120.7(17) . . ? C28 C27 C26 120.0 . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31A 120.0 . . ? C26 C31 H31A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.735 _refine_diff_density_min -1.746 _refine_diff_density_rms 0.149 # Attachment '- Tom_Re_combined.cif' data_sad27 _database_code_depnum_ccdc_archive 'CCDC 817559' #TrackingRef '- Tom_Re_combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H29 B N3 O6 Re), 0.5(C7 H8)' _chemical_formula_sum 'C27.50 H33 B N3 O6 Re' _chemical_formula_weight 698.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.786(6) _cell_length_b 9.096(7) _cell_length_c 17.428(11) _cell_angle_alpha 89.121(6) _cell_angle_beta 83.015(6) _cell_angle_gamma 87.254(6) _cell_volume 1380.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.27 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 4.446 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; A X-ray quality crystal was selected under ambient conditions and covered with PARATONE oil The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on SMART 1000 CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 30 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 30 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11846 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6220 _reflns_number_gt 5031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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. The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. All hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. One of main cluster rings shows the signs of small disorder, however, splitting model lead to unstable refinement, therefore SIMU and DELU similarity restrains were used for this moiety and for C-atoms of disordered by symmetry element toluene solvent. EADP constrains were used for C atoms of CO ligands. PART -1 instruction was used to model disordered by symmetry toluene solvent All significant residual density was found nearby Re atom. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _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^)+(0.0429P)^2^+23.4582P] 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 6220 _refine_ls_number_parameters 355 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.117 _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 Re1 Re 1.08081(4) -0.05590(4) 0.78445(2) 0.01927(13) Uani 1 1 d . . . B1 B 0.8918(12) 0.1240(11) 0.6514(6) 0.018(2) Uani 1 1 d . . . C1 C 1.0733(11) 0.1403(11) 0.6415(5) 0.023(2) Uani 1 1 d . . . C2 C 1.3049(11) 0.2042(13) 0.5855(6) 0.030(2) Uani 1 1 d . . . H2A H 1.3566 0.2975 0.5731 0.035 Uiso 1 1 calc R . . H2B H 1.3509 0.1277 0.5488 0.035 Uiso 1 1 calc R . . C3 C 1.3177(11) 0.1566(11) 0.6682(6) 0.025(2) Uani 1 1 d . . . C4 C 1.3276(13) 0.2886(13) 0.7183(7) 0.035(3) Uani 1 1 d . . . H4A H 1.2387 0.3563 0.7144 0.052 Uiso 1 1 calc R . . H4B H 1.4221 0.3389 0.7009 0.052 Uiso 1 1 calc R . . H4C H 1.3287 0.2564 0.7722 0.052 Uiso 1 1 calc R . . C5 C 1.4536(11) 0.0464(12) 0.6718(7) 0.030(2) Uani 1 1 d . . . H5A H 1.4598 0.0166 0.7257 0.045 Uiso 1 1 calc R . . H5B H 1.5487 0.0924 0.6508 0.045 Uiso 1 1 calc R . . H5C H 1.4395 -0.0403 0.6412 0.045 Uiso 1 1 calc R . . C6 C 0.8355(10) 0.1704(10) 0.7402(5) 0.0164(18) Uani 1 1 d . . . C7 C 0.6889(16) 0.2757(15) 0.8414(7) 0.045(2) Uani 1 1 d U . . H7A H 0.5891 0.2332 0.8595 0.054 Uiso 1 1 calc R . . H7B H 0.6866 0.3784 0.8598 0.054 Uiso 1 1 calc R . . C8 C 0.8192(17) 0.1852(17) 0.8714(8) 0.052(2) Uani 1 1 d U . . C9 C 0.9322(18) 0.3038(17) 0.8940(8) 0.057(2) Uani 1 1 d U . . H9A H 1.0206 0.2537 0.9140 0.085 Uiso 1 1 calc R . . H9B H 0.8782 0.3688 0.9337 0.085 Uiso 1 1 calc R . . H9C H 0.9678 0.3622 0.8481 0.085 Uiso 1 1 calc R . . C10 C 0.7787(18) 0.0898(18) 0.9356(8) 0.058(2) Uani 1 1 d U . . H10A H 0.7080 0.0176 0.9213 0.087 Uiso 1 1 calc R . . H10B H 0.7288 0.1479 0.9793 0.087 Uiso 1 1 calc R . . H10C H 0.8715 0.0384 0.9504 0.087 Uiso 1 1 calc R . . C11 C 0.8757(10) -0.0533(10) 0.6552(5) 0.0190(18) Uani 1 1 d . . . C12 C 0.8094(13) -0.2791(11) 0.6209(6) 0.030(2) Uani 1 1 d . . . H12A H 0.8859 -0.3235 0.5804 0.036 Uiso 1 1 calc R . . H12B H 0.7116 -0.3291 0.6215 0.036 Uiso 1 1 calc R . . C13 C 0.8678(12) -0.2889(10) 0.7003(6) 0.026(2) Uani 1 1 d . . . C14 C 0.7334(13) -0.3023(13) 0.7638(7) 0.037(3) Uani 1 1 d . . . H14A H 0.7718 -0.3075 0.8143 0.055 Uiso 1 1 calc R . . H14B H 0.6796 -0.3917 0.7559 0.055 Uiso 1 1 calc R . . H14C H 0.6624 -0.2162 0.7618 0.055 Uiso 1 1 calc R . . C15 C 0.9870(13) -0.4162(12) 0.7038(7) 0.034(3) Uani 1 1 d . . . H15A H 1.0227 -0.4196 0.7549 0.051 Uiso 1 1 calc R . . H15B H 1.0742 -0.4013 0.6641 0.051 Uiso 1 1 calc R . . H15C H 0.9406 -0.5091 0.6944 0.051 Uiso 1 1 calc R . . C16 C 0.8114(10) 0.2053(9) 0.5832(5) 0.0151(17) Uani 1 1 d . . . C17 C 0.8244(11) 0.1432(11) 0.5095(6) 0.024(2) Uani 1 1 d . . . H17A H 0.8769 0.0499 0.5018 0.029 Uiso 1 1 calc R . . C18 C 0.7638(12) 0.2122(12) 0.4463(6) 0.028(2) Uani 1 1 d . . . H18A H 0.7755 0.1664 0.3971 0.033 Uiso 1 1 calc R . . C19 C 0.6859(12) 0.3495(12) 0.4572(5) 0.026(2) Uani 1 1 d . . . H19A H 0.6433 0.3977 0.4154 0.032 Uiso 1 1 calc R . . C20 C 0.6714(12) 0.4141(11) 0.5281(6) 0.026(2) Uani 1 1 d . . . H20A H 0.6185 0.5074 0.5354 0.031 Uiso 1 1 calc R . . C21 C 0.7336(12) 0.3446(11) 0.5903(6) 0.025(2) Uani 1 1 d . . . H21A H 0.7229 0.3928 0.6387 0.029 Uiso 1 1 calc R . . C22 C 1.0027(13) -0.1807(13) 0.8689(6) 0.0319(17) Uani 1 1 d . . . C23 C 1.2105(13) 0.0211(13) 0.8521(6) 0.0319(17) Uani 1 1 d . . . C24 C 1.2390(12) -0.2040(11) 0.7609(6) 0.027(2) Uani 1 1 d . . . N1 N 1.1649(9) 0.0901(9) 0.6892(4) 0.0186(11) Uani 1 1 d . . . N2 N 0.8948(9) 0.1137(9) 0.7985(4) 0.0186(11) Uani 1 1 d . . . N3 N 0.9333(9) -0.1389(8) 0.7040(4) 0.0200(16) Uani 1 1 d . . . O1 O 1.1400(8) 0.2238(8) 0.5827(4) 0.0240(15) Uani 1 1 d . . . O2 O 0.7184(8) 0.2715(8) 0.7577(4) 0.0247(15) Uani 1 1 d . . . O3 O 0.7874(8) -0.1210(7) 0.6083(4) 0.0264(16) Uani 1 1 d . . . O4 O 0.9656(11) -0.2591(10) 0.9189(5) 0.049(2) Uani 1 1 d . . . O5 O 1.2887(11) 0.0641(11) 0.8954(5) 0.048(2) Uani 1 1 d . . . O6 O 1.3359(9) -0.2954(9) 0.7470(5) 0.0374(19) Uani 1 1 d . . . C25 C 0.712(3) 0.515(3) 0.0789(16) 0.049(3) Uani 0.50 1 d PU A -1 H25A H 0.7129 0.4321 0.1152 0.074 Uiso 0.50 1 calc PR A -1 H25B H 0.6969 0.6075 0.1078 0.074 Uiso 0.50 1 calc PR A -1 H25C H 0.8095 0.5151 0.0452 0.074 Uiso 0.50 1 calc PR A -1 C26 C 0.5820(19) 0.502(2) 0.0304(11) 0.049(3) Uani 0.50 1 d PGU A -1 C27 C 0.481(2) 0.3886(18) 0.0322(10) 0.050(3) Uani 0.50 1 d PGU A -1 H27A H 0.4903 0.3073 0.0664 0.060 Uiso 0.50 1 calc PR A -1 C28 C 0.3657(18) 0.3944(18) -0.0160(11) 0.050(3) Uani 0.50 1 d PGU A -1 H28A H 0.2965 0.3170 -0.0148 0.060 Uiso 0.50 1 calc PR A -1 C29 C 0.3517(17) 0.513(2) -0.0661(9) 0.050(3) Uani 0.50 1 d PGU A -1 H29A H 0.2731 0.5173 -0.0990 0.060 Uiso 0.50 1 calc PR A -1 C30 C 0.453(2) 0.6266(18) -0.0679(9) 0.049(3) Uani 0.50 1 d PGU A -1 H30A H 0.4434 0.7080 -0.1021 0.059 Uiso 0.50 1 calc PR A -1 C31 C 0.5680(18) 0.6209(19) -0.0197(11) 0.049(3) Uani 0.50 1 d PGU A -1 H31A H 0.6372 0.6982 -0.0210 0.059 Uiso 0.50 1 calc PR A -1 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 Re1 0.01825(19) 0.0230(2) 0.0168(2) 0.00404(13) -0.00448(13) 0.00155(14) B1 0.016(5) 0.012(5) 0.024(5) 0.004(4) 0.003(4) 0.002(4) C1 0.022(5) 0.029(5) 0.014(4) -0.005(4) 0.011(4) -0.007(4) C2 0.018(5) 0.034(6) 0.037(6) 0.008(5) -0.004(4) -0.006(4) C3 0.021(5) 0.021(5) 0.036(6) 0.006(4) -0.009(4) -0.002(4) C4 0.031(6) 0.035(6) 0.041(7) -0.003(5) -0.007(5) -0.011(5) C5 0.018(5) 0.031(6) 0.041(6) 0.001(5) -0.006(4) 0.000(4) C6 0.023(5) 0.019(4) 0.009(4) 0.001(3) -0.010(3) 0.001(4) C7 0.052(5) 0.056(6) 0.022(5) -0.003(4) 0.013(4) 0.018(5) C8 0.057(5) 0.064(5) 0.030(4) -0.002(4) 0.006(4) 0.020(4) C9 0.062(5) 0.067(6) 0.038(5) -0.006(4) 0.000(4) 0.017(4) C10 0.064(6) 0.069(6) 0.035(5) 0.004(4) 0.010(4) 0.022(5) C11 0.014(4) 0.021(5) 0.021(5) 0.001(4) 0.000(4) 0.000(4) C12 0.038(6) 0.018(5) 0.033(6) 0.001(4) -0.005(5) -0.001(4) C13 0.028(5) 0.009(4) 0.042(6) 0.004(4) -0.007(4) 0.004(4) C14 0.027(6) 0.030(6) 0.053(8) 0.010(5) -0.002(5) -0.010(5) C15 0.037(6) 0.029(6) 0.039(6) 0.007(5) -0.017(5) -0.001(5) C16 0.012(4) 0.015(4) 0.018(4) 0.001(3) 0.002(3) -0.006(3) C17 0.026(5) 0.017(5) 0.027(5) -0.004(4) 0.002(4) 0.002(4) C18 0.032(6) 0.038(6) 0.014(5) -0.007(4) 0.000(4) -0.002(5) C19 0.034(6) 0.033(6) 0.015(5) 0.004(4) -0.019(4) 0.005(4) C20 0.032(5) 0.023(5) 0.024(5) -0.002(4) -0.014(4) 0.013(4) C21 0.030(5) 0.022(5) 0.019(5) 0.000(4) 0.002(4) 0.001(4) C22 0.029(4) 0.046(5) 0.020(4) 0.007(3) 0.000(3) 0.001(3) C23 0.029(4) 0.046(5) 0.020(4) 0.007(3) 0.000(3) 0.001(3) C24 0.031(6) 0.019(5) 0.036(6) 0.008(4) -0.020(5) -0.010(4) N1 0.017(3) 0.027(3) 0.012(3) -0.002(2) 0.000(2) -0.001(2) N2 0.017(3) 0.027(3) 0.012(3) -0.002(2) 0.000(2) -0.001(2) N3 0.026(4) 0.015(4) 0.019(4) 0.005(3) -0.008(3) 0.006(3) O1 0.022(3) 0.026(4) 0.023(4) 0.009(3) -0.001(3) 0.004(3) O2 0.028(4) 0.029(4) 0.016(3) 0.002(3) 0.002(3) 0.002(3) O3 0.031(4) 0.022(4) 0.030(4) -0.001(3) -0.017(3) -0.004(3) O4 0.049(5) 0.051(6) 0.046(5) 0.025(4) -0.004(4) -0.003(4) O5 0.052(5) 0.062(6) 0.036(5) -0.001(4) -0.030(4) -0.009(5) O6 0.032(4) 0.031(4) 0.049(5) 0.005(4) -0.012(4) 0.014(3) C25 0.047(7) 0.063(6) 0.038(6) -0.010(5) -0.012(5) 0.023(6) C26 0.047(7) 0.063(6) 0.038(6) -0.011(5) -0.012(5) 0.023(5) C27 0.047(7) 0.063(6) 0.038(6) -0.011(5) -0.011(5) 0.022(5) C28 0.047(7) 0.064(6) 0.039(6) -0.012(5) -0.011(5) 0.022(6) C29 0.046(7) 0.064(6) 0.039(6) -0.012(5) -0.012(5) 0.023(6) C30 0.046(7) 0.063(6) 0.038(6) -0.011(5) -0.012(5) 0.023(6) C31 0.046(7) 0.063(6) 0.038(6) -0.010(5) -0.012(5) 0.023(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 Re1 C23 1.899(12) . ? Re1 C24 1.901(11) . ? Re1 C22 1.924(11) . ? Re1 N2 2.187(8) . ? Re1 N3 2.187(8) . ? Re1 N1 2.189(8) . ? B1 C1 1.596(14) . ? B1 C16 1.608(13) . ? B1 C6 1.621(14) . ? B1 C11 1.626(14) . ? C1 N1 1.290(12) . ? C1 O1 1.357(11) . ? C2 O1 1.458(11) . ? C2 C3 1.515(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.501(12) . ? C3 C4 1.507(15) . ? C3 C5 1.528(13) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N2 1.287(11) . ? C6 O2 1.357(11) . ? C7 O2 1.451(13) . ? C7 C8 1.517(18) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.427(19) . ? C8 N2 1.502(14) . ? C8 C9 1.59(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.278(11) . ? C11 O3 1.365(11) . ? C12 O3 1.459(12) . ? C12 C13 1.535(15) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N3 1.511(13) . ? C13 C14 1.524(16) . ? C13 C15 1.529(14) . ? 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 1.402(13) . ? C16 C21 1.410(13) . ? C17 C18 1.407(14) . ? C17 H17A 0.9500 . ? C18 C19 1.399(15) . ? C18 H18A 0.9500 . ? C19 C20 1.367(14) . ? C19 H19A 0.9500 . ? C20 C21 1.400(13) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 O4 1.144(13) . ? C23 O5 1.163(14) . ? C24 O6 1.168(13) . ? C25 C26 1.51(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 H31A 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 C23 Re1 C24 86.1(5) . . ? C23 Re1 C22 87.3(5) . . ? C24 Re1 C22 86.8(5) . . ? C23 Re1 N2 98.8(4) . . ? C24 Re1 N2 173.9(4) . . ? C22 Re1 N2 97.0(4) . . ? C23 Re1 N3 178.2(4) . . ? C24 Re1 N3 94.4(4) . . ? C22 Re1 N3 94.5(4) . . ? N2 Re1 N3 80.6(3) . . ? C23 Re1 N1 92.9(4) . . ? C24 Re1 N1 94.6(4) . . ? C22 Re1 N1 178.6(4) . . ? N2 Re1 N1 81.6(3) . . ? N3 Re1 N1 85.4(3) . . ? C1 B1 C16 112.4(8) . . ? C1 B1 C6 104.6(8) . . ? C16 B1 C6 118.9(7) . . ? C1 B1 C11 102.9(7) . . ? C16 B1 C11 114.3(8) . . ? C6 B1 C11 101.9(7) . . ? N1 C1 O1 114.8(8) . . ? N1 C1 B1 125.3(8) . . ? O1 C1 B1 119.6(8) . . ? O1 C2 C3 103.9(8) . . ? O1 C2 H2A 111.0 . . ? C3 C2 H2A 111.0 . . ? O1 C2 H2B 111.0 . . ? C3 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N1 C3 C4 109.2(9) . . ? N1 C3 C2 100.6(7) . . ? C4 C3 C2 110.5(9) . . ? N1 C3 C5 113.3(8) . . ? C4 C3 C5 112.1(9) . . ? C2 C3 C5 110.6(9) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 O2 115.3(8) . . ? N2 C6 B1 123.5(8) . . ? O2 C6 B1 121.2(7) . . ? O2 C7 C8 106.2(9) . . ? O2 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? O2 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? C10 C8 N2 116.6(12) . . ? C10 C8 C7 116.6(12) . . ? N2 C8 C7 101.3(10) . . ? C10 C8 C9 110.0(13) . . ? N2 C8 C9 106.7(11) . . ? C7 C8 C9 104.3(12) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 O3 114.5(8) . . ? N3 C11 B1 124.4(9) . . ? O3 C11 B1 120.9(8) . . ? O3 C12 C13 103.2(8) . . ? O3 C12 H12A 111.1 . . ? C13 C12 H12A 111.1 . . ? O3 C12 H12B 111.1 . . ? C13 C12 H12B 111.1 . . ? H12A C12 H12B 109.1 . . ? N3 C13 C14 109.4(8) . . ? N3 C13 C15 113.6(8) . . ? C14 C13 C15 111.6(9) . . ? N3 C13 C12 100.5(7) . . ? C14 C13 C12 110.1(9) . . ? C15 C13 C12 111.1(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 . . ? C17 C16 C21 115.3(8) . . ? C17 C16 B1 120.4(8) . . ? C21 C16 B1 124.2(8) . . ? C16 C17 C18 123.3(9) . . ? C16 C17 H17A 118.3 . . ? C18 C17 H17A 118.3 . . ? C19 C18 C17 118.7(9) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? C20 C19 C18 119.8(8) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 120.8(9) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C16 122.1(9) . . ? C20 C21 H21A 118.9 . . ? C16 C21 H21A 118.9 . . ? O4 C22 Re1 175.6(10) . . ? O5 C23 Re1 177.6(10) . . ? O6 C24 Re1 179.5(10) . . ? C1 N1 C3 108.2(8) . . ? C1 N1 Re1 120.1(6) . . ? C3 N1 Re1 131.6(6) . . ? C6 N2 C8 109.3(8) . . ? C6 N2 Re1 121.8(6) . . ? C8 N2 Re1 128.9(7) . . ? C11 N3 C13 108.9(8) . . ? C11 N3 Re1 121.1(7) . . ? C13 N3 Re1 129.7(6) . . ? C1 O1 C2 105.8(7) . . ? C6 O2 C7 106.6(7) . . ? C11 O3 C12 106.9(7) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 120.0 . . ? C27 C26 C25 127.4(18) . . ? C31 C26 C25 112.6(18) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31A 120.0 . . ? C26 C31 H31A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.707 _refine_diff_density_min -2.137 _refine_diff_density_rms 0.315 #===end data_ToPMnCO3_Sad179 _database_code_depnum_ccdc_archive 'CCDC 817560' #TrackingRef '- Tom_Re_combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Sad179 _chemical_melting_point ? _chemical_formula_moiety 'C27 H35 B Mn N3 O6, 2(C6 H6)' _chemical_formula_sum 'C39 H47 B Mn N3 O6' _chemical_formula_weight 719.55 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.1721(6) _cell_length_b 10.7282(6) _cell_length_c 17.8200(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.9580(10) _cell_angle_gamma 90.00 _cell_volume 1895.15(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8481 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8971 _exptl_absorpt_correction_T_max 0.9577 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; The high quality crystal was selected under ambient conditions and covered with PARATONE oil. The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on SMART 1000 CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 10 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 10 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19555 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9296 _reflns_number_gt 8477 _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. The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. All hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(9) _refine_ls_number_reflns 9296 _refine_ls_number_parameters 457 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.38553(2) 0.24346(2) 0.107127(12) 0.02089(6) Uani 1 1 d . . . B1 B 0.25302(18) 0.08468(17) 0.22876(10) 0.0215(3) Uani 1 1 d . . . C1 C 0.2424(2) 0.5080(2) 0.24869(13) 0.0431(5) Uani 1 1 d . . . H1A H 0.1986 0.4430 0.2131 0.065 Uiso 1 1 calc R . . H1B H 0.2014 0.5889 0.2320 0.065 Uiso 1 1 calc R . . H1C H 0.2307 0.4895 0.3006 0.065 Uiso 1 1 calc R . . C2 C 0.39213(19) 0.51211(17) 0.24924(10) 0.0296(4) Uani 1 1 d . . . H2 H 0.4009 0.5335 0.1960 0.036 Uiso 1 1 calc R . . C3 C 0.4656(2) 0.61391(18) 0.30381(12) 0.0398(5) Uani 1 1 d . . . H3A H 0.4566 0.5966 0.3564 0.060 Uiso 1 1 calc R . . H3B H 0.4256 0.6953 0.2874 0.060 Uiso 1 1 calc R . . H3C H 0.5613 0.6147 0.3024 0.060 Uiso 1 1 calc R . . C4 C 0.46173(16) 0.38610(16) 0.27063(9) 0.0234(3) Uani 1 1 d . . . H4 H 0.5575 0.3913 0.2656 0.028 Uiso 1 1 calc R . . C5 C 0.45786(18) 0.33960(17) 0.35139(10) 0.0293(4) Uani 1 1 d . . . H5A H 0.5487 0.3133 0.3798 0.035 Uiso 1 1 calc R . . H5B H 0.4245 0.4057 0.3812 0.035 Uiso 1 1 calc R . . C6 C 0.34029(15) 0.20722(14) 0.26254(9) 0.0211(3) Uani 1 1 d . . . C7 C 0.6724(2) 0.0053(3) 0.27086(12) 0.0475(5) Uani 1 1 d . . . H7A H 0.6494 -0.0784 0.2859 0.071 Uiso 1 1 calc R . . H7B H 0.6055 0.0651 0.2808 0.071 Uiso 1 1 calc R . . H7C H 0.7620 0.0284 0.3009 0.071 Uiso 1 1 calc R . . C8 C 0.67267(17) 0.00629(17) 0.18500(11) 0.0290(4) Uani 1 1 d . . . H8 H 0.6961 0.0928 0.1716 0.035 Uiso 1 1 calc R . . C9 C 0.78108(19) -0.08075(19) 0.16790(13) 0.0388(5) Uani 1 1 d . . . H9A H 0.8698 -0.0539 0.1974 0.058 Uiso 1 1 calc R . . H9B H 0.7796 -0.0781 0.1128 0.058 Uiso 1 1 calc R . . H9C H 0.7634 -0.1661 0.1826 0.058 Uiso 1 1 calc R . . C10 C 0.53386(16) -0.02547(16) 0.13347(10) 0.0251(3) Uani 1 1 d . . . H10 H 0.5387 -0.0237 0.0780 0.030 Uiso 1 1 calc R . . C11 C 0.47564(18) -0.14932(17) 0.15237(12) 0.0321(4) Uani 1 1 d . . . H11A H 0.4255 -0.1912 0.1051 0.039 Uiso 1 1 calc R . . H11B H 0.5477 -0.2056 0.1798 0.039 Uiso 1 1 calc R . . C12 C 0.35941(15) 0.00910(16) 0.18974(9) 0.0224(3) Uani 1 1 d . . . C13 C 0.0635(3) 0.0823(2) -0.05519(14) 0.0508(6) Uani 1 1 d . . . H13A H 0.1388 0.0443 -0.0182 0.076 Uiso 1 1 calc R . . H13B H 0.0768 0.0705 -0.1075 0.076 Uiso 1 1 calc R . . H13C H -0.0212 0.0427 -0.0507 0.076 Uiso 1 1 calc R . . C14 C 0.05758(18) 0.22084(17) -0.03843(10) 0.0321(4) Uani 1 1 d . . . H14 H 0.1389 0.2601 -0.0514 0.039 Uiso 1 1 calc R . . C15 C -0.0661(2) 0.2809(2) -0.09026(13) 0.0519(6) Uani 1 1 d . . . H15A H -0.1480 0.2406 -0.0817 0.078 Uiso 1 1 calc R . . H15B H -0.0616 0.2708 -0.1443 0.078 Uiso 1 1 calc R . . H15C H -0.0683 0.3699 -0.0781 0.078 Uiso 1 1 calc R . . C16 C 0.06304(15) 0.2491(2) 0.04569(9) 0.0268(3) Uani 1 1 d . . . H16 H 0.0618 0.3417 0.0522 0.032 Uiso 1 1 calc R . . C17 C -0.05232(19) 0.1932(2) 0.07734(12) 0.0439(5) Uani 1 1 d . . . H17A H -0.1152 0.2591 0.0863 0.053 Uiso 1 1 calc R . . H17B H -0.1033 0.1312 0.0410 0.053 Uiso 1 1 calc R . . C18 C 0.14772(15) 0.14101(15) 0.15468(9) 0.0218(3) Uani 1 1 d . . . C19 C 0.18283(16) 0.01412(16) 0.28901(9) 0.0227(3) Uani 1 1 d . . . C20 C 0.11331(18) 0.08380(18) 0.33406(11) 0.0331(4) Uani 1 1 d . . . H20 H 0.1120 0.1720 0.3295 0.040 Uiso 1 1 calc R . . C21 C 0.0459(2) 0.0285(2) 0.38539(11) 0.0397(5) Uani 1 1 d . . . H21 H 0.0003 0.0788 0.4153 0.048 Uiso 1 1 calc R . . C22 C 0.0456(2) -0.0992(2) 0.39274(12) 0.0395(5) Uani 1 1 d . . . H22 H -0.0007 -0.1375 0.4274 0.047 Uiso 1 1 calc R . . C23 C 0.1128(2) -0.1706(2) 0.34957(12) 0.0380(4) Uani 1 1 d . . . H23 H 0.1135 -0.2587 0.3547 0.046 Uiso 1 1 calc R . . C24 C 0.18012(18) -0.11464(17) 0.29822(10) 0.0285(4) Uani 1 1 d . . . H24 H 0.2254 -0.1660 0.2686 0.034 Uiso 1 1 calc R . . C25 C 0.33631(17) 0.39715(17) 0.07003(10) 0.0261(3) Uani 1 1 d . . . C26 C 0.38788(18) 0.19014(17) 0.01127(10) 0.0281(4) Uani 1 1 d . . . C27 C 0.55760(18) 0.29371(17) 0.11528(11) 0.0293(4) Uani 1 1 d . . . C28 C 0.8214(3) 0.4814(6) 0.40418(19) 0.1057(18) Uani 1 1 d . . . H28 H 0.7982 0.4977 0.4520 0.127 Uiso 1 1 calc R . . C29 C 0.8314(3) 0.3557(5) 0.3783(3) 0.1001(15) Uani 1 1 d . . . H29 H 0.8155 0.2866 0.4084 0.120 Uiso 1 1 calc R . . C30 C 0.8644(3) 0.3389(3) 0.3089(2) 0.0773(9) Uani 1 1 d . . . H30 H 0.8716 0.2569 0.2901 0.093 Uiso 1 1 calc R . . C31 C 0.8867(3) 0.4361(4) 0.26707(19) 0.0726(8) Uani 1 1 d . . . H31 H 0.9099 0.4216 0.2190 0.087 Uiso 1 1 calc R . . C32 C 0.8774(3) 0.5549(3) 0.2908(2) 0.0740(8) Uani 1 1 d . . . H32 H 0.8930 0.6226 0.2596 0.089 Uiso 1 1 calc R . . C33 C 0.8461(3) 0.5765(4) 0.3588(2) 0.0818(10) Uani 1 1 d . . . H33 H 0.8409 0.6600 0.3757 0.098 Uiso 1 1 calc R . . C34 C 0.5397(3) 0.8899(3) 0.44386(14) 0.0651(8) Uani 1 1 d . . . H34 H 0.4584 0.8538 0.4156 0.078 Uiso 1 1 calc R . . C35 C 0.6474(3) 0.8166(3) 0.47194(15) 0.0597(7) Uani 1 1 d . . . H35 H 0.6412 0.7291 0.4639 0.072 Uiso 1 1 calc R . . C36 C 0.7652(3) 0.8680(3) 0.51187(15) 0.0632(8) Uani 1 1 d . . . H36 H 0.8408 0.8161 0.5315 0.076 Uiso 1 1 calc R . . C37 C 0.7747(3) 0.9934(3) 0.52360(15) 0.0680(9) Uani 1 1 d . . . H37 H 0.8574 1.0291 0.5505 0.082 Uiso 1 1 calc R . . C38 C 0.6653(4) 1.0680(3) 0.49658(18) 0.0736(9) Uani 1 1 d . . . H38 H 0.6707 1.1552 0.5058 0.088 Uiso 1 1 calc R . . C39 C 0.5470(3) 1.0155(4) 0.45585(16) 0.0732(9) Uani 1 1 d . . . H39 H 0.4707 1.0666 0.4362 0.088 Uiso 1 1 calc R . . N1 N 0.39175(13) 0.28311(13) 0.22107(8) 0.0214(3) Uani 1 1 d . . . N2 N 0.42892(13) 0.06360(13) 0.14701(8) 0.0220(3) Uani 1 1 d . . . N3 N 0.18428(13) 0.19896(13) 0.09975(8) 0.0228(3) Uani 1 1 d . . . O1 O 0.36575(11) 0.23439(13) 0.33850(6) 0.0260(2) Uani 1 1 d . . . O2 O 0.38542(12) -0.11329(11) 0.20177(8) 0.0297(3) Uani 1 1 d . . . O3 O 0.01348(11) 0.13418(13) 0.14945(7) 0.0307(3) Uani 1 1 d . . . O4 O 0.30788(14) 0.49372(12) 0.04354(8) 0.0367(3) Uani 1 1 d . . . O5 O 0.39706(15) 0.15670(16) -0.04885(8) 0.0443(4) Uani 1 1 d . . . O6 O 0.66190(14) 0.33321(15) 0.11414(10) 0.0466(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01988(10) 0.02345(11) 0.02025(10) 0.00305(10) 0.00643(8) 0.00130(10) B1 0.0210(8) 0.0214(8) 0.0229(9) 0.0005(7) 0.0070(7) 0.0008(7) C1 0.0377(10) 0.0394(11) 0.0482(12) -0.0052(9) 0.0010(9) 0.0154(9) C2 0.0404(10) 0.0224(8) 0.0239(8) 0.0010(7) 0.0026(7) 0.0040(7) C3 0.0573(13) 0.0226(9) 0.0366(10) -0.0019(8) 0.0043(9) -0.0024(8) C4 0.0220(7) 0.0233(8) 0.0242(8) 0.0007(6) 0.0033(6) -0.0001(6) C5 0.0323(9) 0.0284(9) 0.0239(8) 0.0011(7) -0.0005(7) -0.0040(7) C6 0.0181(7) 0.0240(8) 0.0212(7) 0.0014(6) 0.0042(6) 0.0049(5) C7 0.0341(10) 0.0731(16) 0.0326(10) -0.0060(11) 0.0015(8) 0.0104(11) C8 0.0236(8) 0.0284(9) 0.0352(9) 0.0001(7) 0.0069(7) 0.0041(7) C9 0.0265(9) 0.0375(11) 0.0547(13) 0.0021(9) 0.0135(8) 0.0078(8) C10 0.0248(8) 0.0253(8) 0.0268(8) 0.0000(6) 0.0089(6) 0.0057(6) C11 0.0299(9) 0.0269(9) 0.0441(10) -0.0047(8) 0.0180(8) 0.0026(7) C12 0.0208(7) 0.0222(8) 0.0235(8) -0.0008(6) 0.0034(6) 0.0006(6) C13 0.0597(14) 0.0450(13) 0.0447(13) -0.0157(10) 0.0052(11) -0.0069(11) C14 0.0325(8) 0.0361(11) 0.0248(8) 0.0051(7) 0.0001(7) -0.0078(7) C15 0.0470(12) 0.0614(16) 0.0371(11) 0.0157(10) -0.0123(9) -0.0087(10) C16 0.0218(7) 0.0283(8) 0.0275(7) 0.0003(8) -0.0002(6) 0.0028(8) C17 0.0224(9) 0.0748(15) 0.0329(10) 0.0124(10) 0.0026(7) 0.0054(9) C18 0.0191(7) 0.0231(8) 0.0241(8) -0.0032(6) 0.0066(6) 0.0009(6) C19 0.0193(7) 0.0277(8) 0.0205(7) 0.0025(6) 0.0034(6) -0.0008(6) C20 0.0338(9) 0.0328(10) 0.0366(10) -0.0003(8) 0.0161(8) -0.0006(8) C21 0.0397(11) 0.0515(12) 0.0339(10) -0.0031(9) 0.0212(9) -0.0032(9) C22 0.0391(11) 0.0514(12) 0.0318(10) 0.0081(9) 0.0160(8) -0.0090(9) C23 0.0430(11) 0.0348(10) 0.0386(11) 0.0100(8) 0.0141(9) -0.0070(8) C24 0.0297(8) 0.0280(9) 0.0293(8) 0.0030(7) 0.0096(7) -0.0017(7) C25 0.0236(8) 0.0324(9) 0.0227(8) 0.0021(7) 0.0057(6) -0.0002(7) C26 0.0295(9) 0.0287(8) 0.0282(9) 0.0057(7) 0.0110(7) 0.0011(7) C27 0.0272(9) 0.0296(8) 0.0324(9) 0.0060(7) 0.0097(7) 0.0041(7) C28 0.0367(15) 0.229(6) 0.0474(17) -0.003(3) 0.0016(12) 0.006(3) C29 0.0362(15) 0.142(4) 0.112(3) 0.078(3) -0.0060(17) -0.0007(19) C30 0.0434(15) 0.0662(19) 0.115(3) 0.0075(19) 0.0023(16) 0.0005(13) C31 0.0571(16) 0.093(2) 0.0674(18) -0.0070(18) 0.0131(14) -0.0112(16) C32 0.0620(18) 0.079(2) 0.078(2) 0.0051(17) 0.0087(15) -0.0122(15) C33 0.0504(16) 0.092(2) 0.097(3) -0.029(2) 0.0037(16) -0.0056(16) C34 0.0618(17) 0.097(2) 0.0358(13) -0.0092(14) 0.0086(11) -0.0107(16) C35 0.081(2) 0.0546(15) 0.0512(15) -0.0114(12) 0.0317(15) -0.0044(14) C36 0.0586(16) 0.091(2) 0.0472(14) 0.0152(14) 0.0276(12) 0.0273(15) C37 0.0681(18) 0.096(2) 0.0454(14) -0.0130(15) 0.0250(13) -0.0339(17) C38 0.125(3) 0.0454(15) 0.0648(18) 0.0041(13) 0.051(2) -0.0069(17) C39 0.084(2) 0.095(2) 0.0441(14) 0.0325(16) 0.0224(14) 0.0391(19) N1 0.0203(6) 0.0210(6) 0.0229(7) -0.0002(5) 0.0048(5) 0.0008(5) N2 0.0205(6) 0.0236(7) 0.0232(7) -0.0004(5) 0.0077(5) 0.0040(5) N3 0.0199(6) 0.0275(7) 0.0206(6) 0.0007(5) 0.0037(5) 0.0016(5) O1 0.0299(5) 0.0272(6) 0.0204(5) 0.0030(6) 0.0047(4) -0.0018(6) O2 0.0309(6) 0.0214(6) 0.0419(7) 0.0030(5) 0.0189(5) 0.0031(5) O3 0.0184(6) 0.0429(7) 0.0310(6) 0.0053(5) 0.0060(5) 0.0001(5) O4 0.0424(8) 0.0308(7) 0.0347(7) 0.0095(6) 0.0039(6) 0.0057(6) O5 0.0542(9) 0.0541(9) 0.0292(7) 0.0007(6) 0.0189(7) 0.0062(7) O6 0.0261(7) 0.0470(9) 0.0698(11) 0.0089(8) 0.0172(7) -0.0041(6) _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 C25 1.8050(18) . ? Mn1 C27 1.8058(18) . ? Mn1 C26 1.8066(18) . ? Mn1 N1 2.0615(14) . ? Mn1 N2 2.0694(14) . ? Mn1 N3 2.0774(14) . ? B1 C19 1.606(2) . ? B1 C18 1.619(2) . ? B1 C6 1.624(2) . ? B1 C12 1.628(2) . ? C1 C2 1.522(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.534(2) . ? C2 C3 1.540(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.492(2) . ? C4 C5 1.532(2) . ? C4 H4 1.0000 . ? C5 O1 1.452(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.287(2) . ? C6 O1 1.3516(19) . ? C7 C8 1.531(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.527(2) . ? C8 C10 1.540(2) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.492(2) . ? C10 C11 1.523(3) . ? C10 H10 1.0000 . ? C11 O2 1.459(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N2 1.290(2) . ? C12 O2 1.347(2) . ? C13 C14 1.520(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.518(2) . ? C14 C15 1.527(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N3 1.4852(19) . ? C16 C17 1.534(3) . ? C16 H16 1.0000 . ? C17 O3 1.454(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N3 1.283(2) . ? C18 O3 1.3497(19) . ? C19 C24 1.392(2) . ? C19 C20 1.399(2) . ? C20 C21 1.393(3) . ? C20 H20 0.9500 . ? C21 C22 1.376(3) . ? C21 H21 0.9500 . ? C22 C23 1.372(3) . ? C22 H22 0.9500 . ? C23 C24 1.396(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 O4 1.148(2) . ? C26 O5 1.153(2) . ? C27 O6 1.147(2) . ? C28 C33 1.359(6) . ? C28 C29 1.436(7) . ? C28 H28 0.9500 . ? C29 C30 1.365(6) . ? C29 H29 0.9500 . ? C30 C31 1.329(5) . ? C30 H30 0.9500 . ? C31 C32 1.354(5) . ? C31 H31 0.9500 . ? C32 C33 1.340(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.350(4) . ? C34 C39 1.363(5) . ? C34 H34 0.9500 . ? C35 C36 1.365(4) . ? C35 H35 0.9500 . ? C36 C37 1.361(4) . ? C36 H36 0.9500 . ? C37 C38 1.368(5) . ? C37 H37 0.9500 . ? C38 C39 1.378(5) . ? C38 H38 0.9500 . ? C39 H39 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 C25 Mn1 C27 86.62(8) . . ? C25 Mn1 C26 90.25(8) . . ? C27 Mn1 C26 87.28(8) . . ? C25 Mn1 N1 96.71(7) . . ? C27 Mn1 N1 92.53(7) . . ? C26 Mn1 N1 173.01(7) . . ? C25 Mn1 N2 176.22(7) . . ? C27 Mn1 N2 97.04(7) . . ? C26 Mn1 N2 89.00(7) . . ? N1 Mn1 N2 84.09(5) . . ? C25 Mn1 N3 89.90(7) . . ? C27 Mn1 N3 175.79(7) . . ? C26 Mn1 N3 95.12(7) . . ? N1 Mn1 N3 85.52(5) . . ? N2 Mn1 N3 86.49(5) . . ? C19 B1 C18 114.14(13) . . ? C19 B1 C6 114.93(14) . . ? C18 B1 C6 101.93(13) . . ? C19 B1 C12 119.25(14) . . ? C18 B1 C12 102.67(13) . . ? C6 B1 C12 101.60(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C4 112.44(16) . . ? C1 C2 C3 111.57(16) . . ? C4 C2 C3 109.67(15) . . ? C1 C2 H2 107.6 . . ? C4 C2 H2 107.6 . . ? C3 C2 H2 107.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 101.86(13) . . ? N1 C4 C2 111.91(13) . . ? C5 C4 C2 114.38(14) . . ? N1 C4 H4 109.5 . . ? C5 C4 H4 109.5 . . ? C2 C4 H4 109.5 . . ? O1 C5 C4 104.84(13) . . ? O1 C5 H5A 110.8 . . ? C4 C5 H5A 110.8 . . ? O1 C5 H5B 110.8 . . ? C4 C5 H5B 110.8 . . ? H5A C5 H5B 108.9 . . ? N1 C6 O1 115.30(14) . . ? N1 C6 B1 123.91(14) . . ? O1 C6 B1 120.78(14) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C7 111.00(16) . . ? C9 C8 C10 110.63(15) . . ? C7 C8 C10 112.80(15) . . ? C9 C8 H8 107.4 . . ? C7 C8 H8 107.4 . . ? C10 C8 H8 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 101.26(13) . . ? N2 C10 C8 110.81(14) . . ? C11 C10 C8 114.28(15) . . ? N2 C10 H10 110.1 . . ? C11 C10 H10 110.1 . . ? C8 C10 H10 110.1 . . ? O2 C11 C10 103.34(13) . . ? O2 C11 H11A 111.1 . . ? C10 C11 H11A 111.1 . . ? O2 C11 H11B 111.1 . . ? C10 C11 H11B 111.1 . . ? H11A C11 H11B 109.1 . . ? N2 C12 O2 114.95(14) . . ? N2 C12 B1 122.10(14) . . ? O2 C12 B1 122.91(14) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C13 113.29(17) . . ? C16 C14 C15 110.83(17) . . ? C13 C14 C15 110.96(17) . . ? C16 C14 H14 107.1 . . ? C13 C14 H14 107.1 . . ? C15 C14 H14 107.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C14 114.15(14) . . ? N3 C16 C17 102.25(14) . . ? C14 C16 C17 115.05(15) . . ? N3 C16 H16 108.3 . . ? C14 C16 H16 108.3 . . ? C17 C16 H16 108.3 . . ? O3 C17 C16 104.89(13) . . ? O3 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? O3 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.8 . . ? N3 C18 O3 115.81(14) . . ? N3 C18 B1 123.44(14) . . ? O3 C18 B1 120.68(14) . . ? C24 C19 C20 115.88(16) . . ? C24 C19 B1 124.75(15) . . ? C20 C19 B1 119.30(15) . . ? C21 C20 C19 122.37(18) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C22 C21 C20 119.93(19) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.36(18) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 120.47(18) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 121.98(18) . . ? C19 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? O4 C25 Mn1 176.70(16) . . ? O5 C26 Mn1 176.20(17) . . ? O6 C27 Mn1 173.06(17) . . ? C33 C28 C29 118.6(3) . . ? C33 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C30 C29 C28 117.6(3) . . ? C30 C29 H29 121.2 . . ? C28 C29 H29 121.2 . . ? C31 C30 C29 120.8(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 122.0(3) . . ? C30 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C33 C32 C31 119.5(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C28 121.4(4) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? C35 C34 C39 120.4(3) . . ? C35 C34 H34 119.8 . . ? C39 C34 H34 119.8 . . ? C34 C35 C36 120.2(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 120.2(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.0(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C39 119.5(3) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C34 C39 C38 119.7(3) . . ? C34 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C6 N1 C4 109.27(13) . . ? C6 N1 Mn1 120.56(11) . . ? C4 N1 Mn1 129.87(10) . . ? C12 N2 C10 108.18(13) . . ? C12 N2 Mn1 121.51(11) . . ? C10 N2 Mn1 130.30(10) . . ? C18 N3 C16 109.27(13) . . ? C18 N3 Mn1 120.87(11) . . ? C16 N3 Mn1 128.38(11) . . ? C6 O1 C5 107.34(12) . . ? C12 O2 C11 106.85(13) . . ? C18 O3 C17 107.18(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.371 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.118 #===end data_ToPMnCO3_Sad179a _database_code_depnum_ccdc_archive 'CCDC 817561' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Sad174 _chemical_melting_point ? _chemical_formula_moiety 'C27 H35 B N3 O6 Re, 2(C7 H8)' _chemical_formula_sum 'C41 H51 B N3 O6 Re' _chemical_formula_weight 878.86 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.2280(17) _cell_length_b 10.8316(18) _cell_length_c 18.363(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.083(2) _cell_angle_gamma 90.00 _cell_volume 2003.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.16 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 3.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4484 _exptl_absorpt_correction_T_max 0.7280 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; The high quality crystal was selected under ambient conditions and covered with PARATONE oil. The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on APEX II CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 10 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 10 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20977 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.68 _reflns_number_total 10039 _reflns_number_gt 9220 _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. The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. All hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _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^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(6) _refine_ls_number_reflns 10039 _refine_ls_number_parameters 477 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.385938(10) 0.24996(3) 0.103561(6) 0.02231(4) Uani 1 1 d . . . B1 B 0.2398(4) 0.0852(4) 0.2242(2) 0.0235(8) Uani 1 1 d . . . C1 C 0.6666(5) 0.0142(7) 0.2558(3) 0.0646(18) Uani 1 1 d . . . H1A H 0.6460 -0.0672 0.2740 0.097 Uiso 1 1 calc R . . H1B H 0.6011 0.0744 0.2667 0.097 Uiso 1 1 calc R . . H1C H 0.7555 0.0395 0.2803 0.097 Uiso 1 1 calc R . . C2 C 0.6625(4) 0.0080(4) 0.1719(3) 0.0340(9) Uani 1 1 d . . . H2 H 0.6842 0.0921 0.1549 0.041 Uiso 1 1 calc R . . C3 C 0.7670(4) -0.0811(4) 0.1532(3) 0.0416(11) Uani 1 1 d . . . H3A H 0.7520 -0.1632 0.1725 0.062 Uiso 1 1 calc R . . H3B H 0.8555 -0.0518 0.1756 0.062 Uiso 1 1 calc R . . H3C H 0.7606 -0.0856 0.0994 0.062 Uiso 1 1 calc R . . C4 C 0.5239(4) -0.0275(3) 0.1295(2) 0.0254(8) Uani 1 1 d . . . H4 H 0.5252 -0.0305 0.0752 0.030 Uiso 1 1 calc R . . C5 C 0.4697(4) -0.1486(4) 0.1543(3) 0.0345(9) Uani 1 1 d . . . H5A H 0.4235 -0.1962 0.1114 0.041 Uiso 1 1 calc R . . H5B H 0.5419 -0.1999 0.1819 0.041 Uiso 1 1 calc R . . C6 C 0.3497(4) 0.0099(3) 0.1878(2) 0.0241(7) Uani 1 1 d . . . C7 C 0.0704(7) 0.0643(5) -0.0380(3) 0.0620(16) Uani 1 1 d . . . H7A H 0.1479 0.0337 -0.0037 0.093 Uiso 1 1 calc R . . H7B H 0.0782 0.0416 -0.0887 0.093 Uiso 1 1 calc R . . H7C H -0.0105 0.0277 -0.0255 0.093 Uiso 1 1 calc R . . C8 C 0.0633(5) 0.2039(4) -0.0319(2) 0.0360(10) Uani 1 1 d . . . H8 H 0.1448 0.2389 -0.0472 0.043 Uiso 1 1 calc R . . C9 C -0.0568(4) 0.2540(9) -0.0847(2) 0.0548(12) Uani 1 1 d . . . H9A H -0.0472 0.2361 -0.1358 0.082 Uiso 1 1 calc R . . H9B H -0.0628 0.3434 -0.0781 0.082 Uiso 1 1 calc R . . H9C H -0.1377 0.2145 -0.0741 0.082 Uiso 1 1 calc R . . C10 C 0.0618(3) 0.2453(7) 0.04701(18) 0.0287(7) Uani 1 1 d . . . H10 H 0.0605 0.3376 0.0483 0.034 Uiso 1 1 calc R . . C11 C -0.0534(4) 0.1966(5) 0.0815(3) 0.0465(12) Uani 1 1 d . . . H11A H -0.1095 0.2655 0.0935 0.056 Uiso 1 1 calc R . . H11B H -0.1091 0.1394 0.0472 0.056 Uiso 1 1 calc R . . C12 C 0.1402(3) 0.1414(3) 0.1533(2) 0.0228(7) Uani 1 1 d . . . C13 C 0.4395(6) 0.6103(4) 0.2988(3) 0.0466(12) Uani 1 1 d . . . H13A H 0.4301 0.5905 0.3497 0.070 Uiso 1 1 calc R . . H13B H 0.3964 0.6896 0.2844 0.070 Uiso 1 1 calc R . . H13C H 0.5339 0.6156 0.2955 0.070 Uiso 1 1 calc R . . C14 C 0.3741(5) 0.5093(4) 0.2470(2) 0.0343(9) Uani 1 1 d . . . H14 H 0.3883 0.5303 0.1959 0.041 Uiso 1 1 calc R . . C15 C 0.2235(5) 0.5028(5) 0.2454(3) 0.0470(12) Uani 1 1 d . . . H15A H 0.1850 0.4380 0.2110 0.071 Uiso 1 1 calc R . . H15B H 0.1831 0.5824 0.2292 0.071 Uiso 1 1 calc R . . H15C H 0.2065 0.4838 0.2951 0.071 Uiso 1 1 calc R . . C16 C 0.4413(4) 0.3849(3) 0.2679(2) 0.0274(8) Uani 1 1 d . . . H16 H 0.5373 0.3905 0.2638 0.033 Uiso 1 1 calc R . . C17 C 0.4287(4) 0.3372(4) 0.3452(2) 0.0336(9) Uani 1 1 d . . . H17A H 0.5165 0.3125 0.3732 0.040 Uiso 1 1 calc R . . H17B H 0.3904 0.4014 0.3736 0.040 Uiso 1 1 calc R . . C18 C 0.3228(4) 0.2066(3) 0.2583(2) 0.0250(8) Uani 1 1 d . . . C19 C 0.1609(4) 0.0128(4) 0.2803(2) 0.0241(7) Uani 1 1 d . . . C20 C 0.1482(4) -0.1154(4) 0.2809(2) 0.0294(8) Uani 1 1 d . . . H20 H 0.1900 -0.1633 0.2482 0.035 Uiso 1 1 calc R . . C21 C 0.0755(4) -0.1755(4) 0.3284(2) 0.0367(10) Uani 1 1 d . . . H21 H 0.0681 -0.2629 0.3273 0.044 Uiso 1 1 calc R . . C22 C 0.0152(4) -0.1087(5) 0.3761(2) 0.0392(10) Uani 1 1 d . . . H22 H -0.0325 -0.1493 0.4091 0.047 Uiso 1 1 calc R . . C23 C 0.0241(4) 0.0184(5) 0.3760(3) 0.0391(10) Uani 1 1 d . . . H23 H -0.0192 0.0656 0.4083 0.047 Uiso 1 1 calc R . . C24 C 0.0958(4) 0.0774(4) 0.3290(2) 0.0330(9) Uani 1 1 d . . . H24 H 0.1008 0.1650 0.3300 0.040 Uiso 1 1 calc R . . C25 C 0.3362(4) 0.4124(4) 0.0671(2) 0.0280(8) Uani 1 1 d . . . C26 C 0.3968(4) 0.1967(4) 0.0047(2) 0.0302(9) Uani 1 1 d . . . C27 C 0.5663(4) 0.3033(4) 0.1133(2) 0.0315(9) Uani 1 1 d . . . C28 C 0.5495(6) 0.4275(8) 0.5884(3) 0.077(2) Uani 1 1 d . . . H28A H 0.5403 0.4057 0.6390 0.116 Uiso 1 1 calc R . . H28B H 0.5974 0.5059 0.5887 0.116 Uiso 1 1 calc R . . H28C H 0.5991 0.3626 0.5679 0.116 Uiso 1 1 calc R . . C29 C 0.4174(5) 0.4400(5) 0.5426(3) 0.0507(12) Uani 1 1 d . . . C30 C 0.3377(6) 0.3370(6) 0.5259(3) 0.0569(15) Uani 1 1 d . . . H30 H 0.3700 0.2592 0.5452 0.068 Uiso 1 1 calc R . . C31 C 0.2164(7) 0.3422(7) 0.4835(4) 0.0706(18) Uani 1 1 d . . . H31 H 0.1665 0.2688 0.4718 0.085 Uiso 1 1 calc R . . C32 C 0.1638(7) 0.4563(9) 0.4565(4) 0.082(2) Uani 1 1 d . . . H32 H 0.0772 0.4621 0.4279 0.098 Uiso 1 1 calc R . . C33 C 0.2401(9) 0.5573(8) 0.4726(4) 0.080(2) Uani 1 1 d . . . H33 H 0.2059 0.6348 0.4539 0.096 Uiso 1 1 calc R . . C34 C 0.3656(7) 0.5536(6) 0.5148(3) 0.0639(17) Uani 1 1 d . . . H34 H 0.4163 0.6271 0.5248 0.077 Uiso 1 1 calc R . . C35 C 0.8399(8) 0.5627(10) 0.2383(4) 0.103(3) Uani 1 1 d . . . H35A H 0.7519 0.5780 0.2088 0.154 Uiso 1 1 calc R . . H35B H 0.8917 0.5108 0.2101 0.154 Uiso 1 1 calc R . . H35C H 0.8858 0.6415 0.2501 0.154 Uiso 1 1 calc R . . C36 C 0.8254(6) 0.5001(6) 0.3065(3) 0.0597(15) Uani 1 1 d . . . C37 C 0.8058(5) 0.5634(6) 0.3680(4) 0.0592(15) Uani 1 1 d . . . H37 H 0.8037 0.6511 0.3664 0.071 Uiso 1 1 calc R . . C38 C 0.7888(6) 0.5046(7) 0.4320(4) 0.0682(17) Uani 1 1 d . . . H38 H 0.7757 0.5518 0.4738 0.082 Uiso 1 1 calc R . . C39 C 0.7905(7) 0.3815(7) 0.4359(4) 0.0720(19) Uani 1 1 d . . . H39 H 0.7775 0.3411 0.4800 0.086 Uiso 1 1 calc R . . C40 C 0.8112(6) 0.3136(6) 0.3758(4) 0.0642(16) Uani 1 1 d . . . H40 H 0.8138 0.2261 0.3792 0.077 Uiso 1 1 calc R . . C41 C 0.8280(6) 0.3682(6) 0.3118(4) 0.0676(18) Uani 1 1 d . . . H41 H 0.8414 0.3194 0.2707 0.081 Uiso 1 1 calc R . . N1 N 0.4210(3) 0.0620(3) 0.14465(18) 0.0236(6) Uani 1 1 d . . . N2 N 0.1789(3) 0.2007(3) 0.10058(17) 0.0234(6) Uani 1 1 d . . . N3 N 0.3781(3) 0.2834(3) 0.22010(17) 0.0225(7) Uani 1 1 d . . . O1 O 0.3769(3) -0.1099(3) 0.20214(17) 0.0315(6) Uani 1 1 d . . . O2 O 0.0079(3) 0.1321(3) 0.14869(16) 0.0328(6) Uani 1 1 d . . . O3 O 0.3407(3) 0.2314(3) 0.33155(13) 0.0285(7) Uani 1 1 d . . . O4 O 0.3070(3) 0.5088(3) 0.04344(17) 0.0399(7) Uani 1 1 d . . . O5 O 0.4066(3) 0.1631(3) -0.05328(17) 0.0435(8) Uani 1 1 d . . . O6 O 0.6726(3) 0.3424(3) 0.1166(2) 0.0499(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02017(6) 0.02384(6) 0.02397(6) 0.00323(11) 0.00676(4) 0.00158(10) B1 0.0209(19) 0.027(2) 0.024(2) 0.0018(17) 0.0059(16) 0.0032(16) C1 0.037(3) 0.096(5) 0.054(3) -0.026(3) -0.010(2) 0.022(3) C2 0.0237(19) 0.030(2) 0.048(3) -0.0017(19) 0.0051(18) 0.0029(16) C3 0.028(2) 0.035(2) 0.064(3) 0.002(2) 0.013(2) 0.0070(18) C4 0.0235(18) 0.0264(19) 0.0276(19) 0.0006(15) 0.0086(15) 0.0049(15) C5 0.033(2) 0.028(2) 0.048(3) -0.0030(18) 0.0218(19) 0.0046(17) C6 0.0237(18) 0.0234(17) 0.0257(19) -0.0004(15) 0.0052(14) 0.0015(15) C7 0.079(4) 0.046(3) 0.058(4) -0.020(3) 0.006(3) -0.009(3) C8 0.038(2) 0.039(2) 0.030(2) 0.0046(16) 0.0020(18) -0.0117(17) C9 0.049(2) 0.073(3) 0.035(2) 0.011(4) -0.0123(18) -0.014(5) C10 0.0226(14) 0.0302(18) 0.0311(16) 0.001(3) -0.0016(12) -0.002(3) C11 0.025(2) 0.079(4) 0.035(2) 0.014(2) 0.0023(18) 0.007(2) C12 0.0181(16) 0.0254(18) 0.0255(19) -0.0035(15) 0.0054(14) 0.0018(14) C13 0.067(3) 0.028(2) 0.043(3) -0.0022(19) 0.004(2) -0.002(2) C14 0.047(3) 0.028(2) 0.027(2) 0.0014(16) 0.0032(18) 0.0048(18) C15 0.038(3) 0.049(3) 0.050(3) -0.008(2) -0.003(2) 0.021(2) C16 0.0233(18) 0.0252(19) 0.033(2) -0.0034(16) 0.0036(16) 0.0000(15) C17 0.035(2) 0.033(2) 0.030(2) -0.0020(17) -0.0019(17) -0.0039(18) C18 0.0220(17) 0.0271(17) 0.0262(19) 0.0006(14) 0.0053(15) 0.0049(13) C19 0.0204(17) 0.030(2) 0.0219(18) 0.0019(15) 0.0049(15) -0.0006(15) C20 0.030(2) 0.031(2) 0.029(2) -0.0012(16) 0.0095(17) -0.0027(16) C21 0.038(2) 0.034(2) 0.039(2) 0.0062(19) 0.0115(19) -0.0053(19) C22 0.036(2) 0.053(3) 0.031(2) 0.007(2) 0.0127(18) -0.009(2) C23 0.035(2) 0.050(3) 0.036(2) -0.003(2) 0.0178(19) 0.000(2) C24 0.032(2) 0.031(2) 0.039(2) -0.0024(18) 0.0151(18) 0.0005(17) C25 0.0247(18) 0.031(2) 0.029(2) 0.0019(16) 0.0068(16) -0.0002(16) C26 0.029(2) 0.0298(19) 0.034(2) 0.0071(17) 0.0093(17) 0.0050(15) C27 0.030(2) 0.0296(19) 0.036(2) 0.0066(17) 0.0108(18) 0.0064(16) C28 0.066(4) 0.116(6) 0.047(4) -0.001(4) 0.003(3) 0.003(4) C29 0.056(3) 0.061(3) 0.035(3) -0.004(2) 0.007(2) -0.003(3) C30 0.069(4) 0.061(3) 0.046(3) -0.009(3) 0.024(3) -0.024(3) C31 0.070(4) 0.092(5) 0.054(4) -0.002(3) 0.022(3) -0.017(4) C32 0.049(4) 0.148(8) 0.051(4) -0.013(4) 0.011(3) 0.007(4) C33 0.109(6) 0.083(5) 0.051(4) -0.006(4) 0.021(4) 0.028(5) C34 0.097(5) 0.050(3) 0.045(3) -0.003(3) 0.013(3) 0.014(3) C35 0.080(5) 0.147(9) 0.076(5) 0.009(5) -0.002(4) -0.043(5) C36 0.047(3) 0.070(4) 0.057(4) 0.002(3) -0.006(3) -0.006(3) C37 0.045(3) 0.053(3) 0.074(4) -0.002(3) -0.004(3) 0.003(2) C38 0.067(4) 0.071(4) 0.065(4) -0.011(3) 0.005(3) 0.007(3) C39 0.071(4) 0.070(4) 0.069(4) 0.010(3) -0.006(3) -0.010(3) C40 0.068(4) 0.052(3) 0.067(4) 0.001(3) -0.005(3) 0.005(3) C41 0.046(3) 0.071(4) 0.079(5) -0.024(4) -0.007(3) 0.004(3) N1 0.0210(15) 0.0215(15) 0.0296(17) 0.0013(13) 0.0077(13) 0.0025(12) N2 0.0196(14) 0.0276(14) 0.0231(15) 0.0024(12) 0.0042(12) 0.0027(11) N3 0.0203(14) 0.0207(17) 0.0265(15) -0.0004(11) 0.0038(12) 0.0016(10) O1 0.0307(15) 0.0245(14) 0.0436(17) 0.0044(12) 0.0181(13) 0.0040(11) O2 0.0188(13) 0.0472(18) 0.0326(15) 0.0067(13) 0.0052(11) -0.0004(12) O3 0.0331(12) 0.031(2) 0.0216(11) 0.0003(12) 0.0042(9) -0.0030(13) O4 0.0473(18) 0.0328(16) 0.0388(17) 0.0095(14) 0.0048(14) 0.0068(14) O5 0.053(2) 0.051(2) 0.0304(17) 0.0005(14) 0.0193(15) 0.0088(16) O6 0.0245(16) 0.045(2) 0.082(3) 0.0088(18) 0.0158(16) -0.0033(14) _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 Re1 C27 1.911(4) . ? Re1 C25 1.919(4) . ? Re1 C26 1.927(4) . ? Re1 N2 2.175(3) . ? Re1 N1 2.179(3) . ? Re1 N3 2.186(3) . ? B1 C19 1.619(6) . ? B1 C6 1.624(5) . ? B1 C12 1.624(5) . ? B1 C18 1.630(6) . ? C1 C2 1.536(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.523(6) . ? C2 C4 1.542(6) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.492(4) . ? C4 C5 1.524(6) . ? C4 H4 1.0000 . ? C5 O1 1.463(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.296(5) . ? C6 O1 1.344(4) . ? C7 C8 1.518(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.519(6) . ? C8 C9 1.526(7) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.491(5) . ? C10 C11 1.526(6) . ? C10 H10 1.0000 . ? C11 O2 1.460(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N2 1.280(5) . ? C12 O2 1.345(4) . ? C13 C14 1.524(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.531(6) . ? C14 C15 1.537(7) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N3 1.483(5) . ? C16 C17 1.537(6) . ? C16 H16 1.0000 . ? C17 O3 1.452(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N3 1.281(5) . ? C18 O3 1.353(5) . ? C19 C24 1.394(6) . ? C19 C20 1.395(5) . ? C20 C21 1.402(6) . ? C20 H20 0.9500 . ? C21 C22 1.364(6) . ? C21 H21 0.9500 . ? C22 C23 1.379(7) . ? C22 H22 0.9500 . ? C23 C24 1.382(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 O4 1.150(5) . ? C26 O5 1.146(5) . ? C27 O6 1.159(5) . ? C28 C29 1.467(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.385(8) . ? C29 C34 1.401(8) . ? C30 C31 1.345(9) . ? C30 H30 0.9500 . ? C31 C32 1.403(11) . ? C31 H31 0.9500 . ? C32 C33 1.346(11) . ? C32 H32 0.9500 . ? C33 C34 1.379(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.455(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.365(9) . ? C36 C41 1.432(9) . ? C37 C38 1.375(9) . ? C37 H37 0.9500 . ? C38 C39 1.335(9) . ? C38 H38 0.9500 . ? C39 C40 1.374(10) . ? C39 H39 0.9500 . ? C40 C41 1.352(9) . ? C40 H40 0.9500 . ? C41 H41 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 C27 Re1 C25 87.01(17) . . ? C27 Re1 C26 87.99(18) . . ? C25 Re1 C26 90.05(17) . . ? C27 Re1 N2 174.81(15) . . ? C25 Re1 N2 91.09(14) . . ? C26 Re1 N2 96.85(15) . . ? C27 Re1 N1 98.76(14) . . ? C25 Re1 N1 174.20(14) . . ? C26 Re1 N1 90.76(14) . . ? N2 Re1 N1 83.11(11) . . ? C27 Re1 N3 93.35(15) . . ? C25 Re1 N3 97.89(14) . . ? C26 Re1 N3 172.00(13) . . ? N2 Re1 N3 82.12(11) . . ? N1 Re1 N3 81.24(11) . . ? C19 B1 C6 118.5(3) . . ? C19 B1 C12 112.3(3) . . ? C6 B1 C12 103.9(3) . . ? C19 B1 C18 115.5(3) . . ? C6 B1 C18 102.2(3) . . ? C12 B1 C18 102.5(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 110.9(4) . . ? C3 C2 C4 110.3(4) . . ? C1 C2 C4 112.2(4) . . ? C3 C2 H2 107.7 . . ? C1 C2 H2 107.7 . . ? C4 C2 H2 107.7 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 101.5(3) . . ? N1 C4 C2 111.1(3) . . ? C5 C4 C2 114.5(3) . . ? N1 C4 H4 109.8 . . ? C5 C4 H4 109.8 . . ? C2 C4 H4 109.8 . . ? O1 C5 C4 103.9(3) . . ? O1 C5 H5A 111.0 . . ? C4 C5 H5A 111.0 . . ? O1 C5 H5B 111.0 . . ? C4 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? N1 C6 O1 114.9(3) . . ? N1 C6 B1 122.5(3) . . ? O1 C6 B1 122.6(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 C10 111.9(5) . . ? C7 C8 C9 110.5(5) . . ? C10 C8 C9 111.1(4) . . ? C7 C8 H8 107.7 . . ? C10 C8 H8 107.7 . . ? C9 C8 H8 107.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C8 113.1(4) . . ? N2 C10 C11 101.7(3) . . ? C8 C10 C11 115.6(4) . . ? N2 C10 H10 108.7 . . ? C8 C10 H10 108.7 . . ? C11 C10 H10 108.7 . . ? O2 C11 C10 105.5(3) . . ? O2 C11 H11A 110.6 . . ? C10 C11 H11A 110.6 . . ? O2 C11 H11B 110.6 . . ? C10 C11 H11B 110.6 . . ? H11A C11 H11B 108.8 . . ? N2 C12 O2 115.5(3) . . ? N2 C12 B1 124.1(3) . . ? O2 C12 B1 120.3(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C13 C14 C16 110.2(4) . . ? C13 C14 C15 111.9(4) . . ? C16 C14 C15 111.6(4) . . ? C13 C14 H14 107.6 . . ? C16 C14 H14 107.6 . . ? C15 C14 H14 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C14 112.0(3) . . ? N3 C16 C17 101.5(3) . . ? C14 C16 C17 114.9(3) . . ? N3 C16 H16 109.4 . . ? C14 C16 H16 109.4 . . ? C17 C16 H16 109.4 . . ? O3 C17 C16 104.8(3) . . ? O3 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? O3 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? N3 C18 O3 114.8(3) . . ? N3 C18 B1 124.3(3) . . ? O3 C18 B1 120.8(3) . . ? C24 C19 C20 116.1(4) . . ? C24 C19 B1 120.9(4) . . ? C20 C19 B1 123.0(3) . . ? C19 C20 C21 121.8(4) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 120.2(4) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 119.4(4) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 120.3(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 122.2(4) . . ? C23 C24 H24 118.9 . . ? C19 C24 H24 118.9 . . ? O4 C25 Re1 178.3(4) . . ? O5 C26 Re1 178.0(4) . . ? O6 C27 Re1 175.6(4) . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 117.2(6) . . ? C30 C29 C28 120.0(6) . . ? C34 C29 C28 122.8(6) . . ? C31 C30 C29 122.8(7) . . ? C31 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C30 C31 C32 120.0(7) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 117.8(7) . . ? C33 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? C32 C33 C34 123.1(7) . . ? C32 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C33 C34 C29 119.1(7) . . ? C33 C34 H34 120.5 . . ? C29 C34 H34 120.5 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C41 116.7(6) . . ? C37 C36 C35 122.0(7) . . ? C41 C36 C35 121.3(7) . . ? C36 C37 C38 122.2(6) . . ? C36 C37 H37 118.9 . . ? C38 C37 H37 118.9 . . ? C39 C38 C37 120.4(7) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 119.6(7) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 121.6(6) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C36 119.4(6) . . ? C40 C41 H41 120.3 . . ? C36 C41 H41 120.3 . . ? C6 N1 C4 108.7(3) . . ? C6 N1 Re1 122.8(2) . . ? C4 N1 Re1 128.4(2) . . ? C12 N2 C10 110.1(3) . . ? C12 N2 Re1 122.2(2) . . ? C10 N2 Re1 127.1(3) . . ? C18 N3 C16 110.2(3) . . ? C18 N3 Re1 121.6(2) . . ? C16 N3 Re1 128.0(2) . . ? C6 O1 C5 107.0(3) . . ? C12 O2 C11 107.2(3) . . ? C18 O3 C17 107.5(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.980 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.211