Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #============================================================================== # 0. AUDIT DETAILS _audit_creation_date ' 2005' _audit_creation_method SHELX-97 _audit_update_record ; ? ; #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry and Biochemistry Baylor University One Bear Place # 97348 Waco TX, 76798-7348 USA ; _publ_contact_author_email 'Gordon Stone@baylor.edu' _publ_contact_author_fax '+1 254 710 2403' _publ_contact_author_phone '+1 254 710 4427' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; This CIF is submitted as supplementary data for the following manuscript, submitted to Dalton Transactions: Alkyne coupling at a rhenium-monocarborane substrate: synthesis of Re,B-\h^2^:\s-butadienyl complexes With thanks, Professor F. G. A. Stone July 14th, 2005 ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Alkyne coupling at a rhenium-monocarborane substrate: synthesis of Re,B-\h^2^:\s-butadienyl complexes ; loop_ _publ_author_name _publ_author_address S.Du ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; J.A.Kautz ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; T.D.McGrath ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; F.G.A.Stone ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #============================================================================== _publ_section_exptl_refinement ; Diffracted intensities for 6, 7c, and 8b were collected at 293(2) K on an Enraf-Nonius CAD4 diffractometer using graphite-monochromated Mo K\a X-radiation (\l = 0.71073 \%A). Intensity data were corrected for Lorentz, polarization and X-ray absorption effects, the last using a numerical method based on measurement of the crystal faces. For the crystal of compound 9, data were collected at 110(2) K on a Bruker-Nonius X8 APEX CCD area-detector diffractometer using Mo-K\a X-radiation. Several sets of narrow data 'frames' were collected at different values of \q, for various initial values of \f and\w, and using 0.5\% increments of \f or \w. The data frames were integrated using SAINT (Bruker, 2003); the substantial redundancy in data allowed an empirical absorption correction (SADABS: Bruker, 2003) to be applied, based on multiple measurements of equivalent reflections. The structures were solved using conventional direct methods and refined by full-matrix least-squares on all F2 data using SHELXTL versions 5.03 or 6.12 (Bruker, 1995 and 2001). All non-hydrogen atoms were assigned anisotropic displacement parameters. The locations of the cage carbon atoms were verified by examination of the appropriate internuclear distances and the magnitudes of their isotropic thermal displacement parameters. Hydrogen atoms bonded to nitrogen and the acetylenic hydrogens in 7c and 9 were allowed positional refinement; the remaining hydrogen atoms were included in calculated positions and set riding on their parent atoms. All hydrogen atoms were assigned calculated isotropic thermal parameters [U~iso~(H) = 1.2 x U~iso~(parent), or U~iso~(H) = 1.5 x U~iso~(parent) for methyl hydrogens]. ; _publ_section_references ; Bruker (1995). SHELXTL-PC. Version 5.03. Bruker Analytical X-ray Instruments Inc. (1995), Madison, Wisconsin, USA. Bruker (2001). SHELXTL-PC. Version 6.12. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Bruker (2003). APEX 2. Version 1.0-5. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Enraf-Nonius (1989). CAD-4 Software. Version 5. Enraf-Nonius, Delft, The Netherlands. Harms, K. (1993). XCAD4 A Program to extract intensities from a CAD-4 file. University of Marburg, Germany. Sheldrick, G.M. (1990). SHELXS97. Program for crystal structure solution. University of G\\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 278686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 B10 N O3 Re' _chemical_formula_weight 472.55 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 8.6239(7) _cell_length_b 14.246(2) _cell_length_c 15.6634(10) _cell_angle_alpha 73.562(9) _cell_angle_beta 78.594(7) _cell_angle_gamma 75.626(10) _cell_volume 1771.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 6.864 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.217 _exptl_absorpt_correction_T_max 0.406 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 8.76 _diffrn_reflns_number 8709 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8102 _reflns_number_gt 6253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (Enraf-Nonius, 1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.5254P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00199(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8102 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.05918(3) 0.218101(17) 0.288440(16) 0.03331(8) Uani 1 1 d . . . C1 C 0.2829(7) 0.1502(4) 0.3438(4) 0.0308(12) Uani 1 1 d . . . B3 B 0.3270(9) 0.2065(6) 0.2273(5) 0.0386(16) Uani 1 1 d . . . H3 H 0.3496 0.2819 0.1941 0.046 Uiso 1 1 calc R . . B4 B 0.4695(9) 0.1160(6) 0.2910(5) 0.0431(18) Uani 1 1 d . . . H4 H 0.5780 0.1366 0.3014 0.052 Uiso 1 1 calc R . . B5 B 0.3680(9) 0.0279(6) 0.3778(5) 0.0434(17) Uani 1 1 d . . . H5 H 0.4115 -0.0074 0.4432 0.052 Uiso 1 1 calc R . . B6 B 0.1560(9) 0.0593(5) 0.3697(5) 0.0351(15) Uani 1 1 d . . . H6 H 0.0675 0.0391 0.4292 0.042 Uiso 1 1 calc R . . B7 B 0.2283(9) 0.1468(6) 0.1740(5) 0.0429(17) Uani 1 1 d . . . H7 H 0.1862 0.1822 0.1082 0.051 Uiso 1 1 calc R . . B8 B 0.4409(9) 0.1051(6) 0.1858(6) 0.0457(19) Uani 1 1 d . . . H8 H 0.5344 0.1153 0.1270 0.055 Uiso 1 1 calc R . . B9 B 0.4682(9) -0.0019(6) 0.2753(6) 0.048(2) Uani 1 1 d . . . H9 H 0.5795 -0.0598 0.2741 0.058 Uiso 1 1 calc R . . B10 B 0.2769(10) -0.0344(5) 0.3224(6) 0.0436(17) Uani 1 1 d . . . H10 H 0.2661 -0.1129 0.3507 0.052 Uiso 1 1 calc R . . B11 B 0.1228(9) 0.0554(6) 0.2641(5) 0.0409(17) Uani 1 1 d . . . H11 H 0.0147 0.0342 0.2540 0.049 Uiso 1 1 calc R . . B12 B 0.3186(10) 0.0163(6) 0.2055(6) 0.0487(19) Uani 1 1 d . . . H12 H 0.3315 -0.0298 0.1579 0.058 Uiso 1 1 calc R . . C2 C -0.0911(9) 0.2250(6) 0.2057(5) 0.0548(19) Uani 1 1 d . . . O2 O -0.1774(8) 0.2302(5) 0.1588(5) 0.0830(19) Uani 1 1 d . . . C3 C 0.0408(8) 0.3618(5) 0.2288(5) 0.0477(17) Uani 1 1 d . . . O3 O 0.0429(7) 0.4427(4) 0.1906(4) 0.0728(17) Uani 1 1 d . . . C4 C -0.1365(8) 0.2132(6) 0.3794(5) 0.0505(18) Uani 1 1 d . . . O4 O -0.2451(6) 0.2032(5) 0.4320(4) 0.0803(19) Uani 1 1 d . . . N1 N 0.2132(6) 0.2322(4) 0.3825(3) 0.0322(11) Uani 1 1 d . . . H1 H 0.257(8) 0.283(5) 0.356(4) 0.039 Uiso 1 1 d . . . C5 C 0.1871(8) 0.2345(5) 0.4812(4) 0.0432(15) Uani 1 1 d . . . C6 C 0.3539(9) 0.2288(6) 0.5026(5) 0.0541(18) Uani 1 1 d . . . H6A H 0.4206 0.1647 0.4996 0.081 Uiso 1 1 calc R . . H6B H 0.3448 0.2379 0.5620 0.081 Uiso 1 1 calc R . . H6C H 0.4019 0.2804 0.4598 0.081 Uiso 1 1 calc R . . C7 C 0.0813(10) 0.3367(6) 0.4857(5) 0.060(2) Uani 1 1 d . . . H7A H -0.0242 0.3404 0.4721 0.091 Uiso 1 1 calc R . . H7B H 0.1294 0.3881 0.4428 0.091 Uiso 1 1 calc R . . H7C H 0.0720 0.3460 0.5450 0.091 Uiso 1 1 calc R . . C8 C 0.1123(11) 0.1500(6) 0.5443(5) 0.061(2) Uani 1 1 d . . . H8A H 0.0068 0.1551 0.5300 0.091 Uiso 1 1 calc R . . H8B H 0.1035 0.1543 0.6052 0.091 Uiso 1 1 calc R . . H8C H 0.1794 0.0870 0.5376 0.091 Uiso 1 1 calc R . . Re10 Re -0.46591(3) 0.678731(17) 0.111978(15) 0.02988(8) Uani 1 1 d . . . C101 C -0.6560(8) 0.6713(5) 0.2238(4) 0.0369(14) Uani 1 1 d . . . B103 B -0.6136(9) 0.5575(5) 0.1869(5) 0.0380(16) Uani 1 1 d . . . H103 H -0.6692 0.5372 0.1390 0.046 Uiso 1 1 calc R . . B104 B -0.7229(11) 0.5723(6) 0.2933(5) 0.050(2) Uani 1 1 d . . . H104 H -0.8510 0.5671 0.3095 0.060 Uiso 1 1 calc R . . B105 B -0.6467(11) 0.6552(6) 0.3342(5) 0.049(2) Uani 1 1 d . . . H105 H -0.7267 0.7025 0.3765 0.059 Uiso 1 1 calc R . . B106 B -0.4880(9) 0.7005(6) 0.2546(5) 0.0407(16) Uani 1 1 d . . . H106 H -0.4624 0.7739 0.2496 0.049 Uiso 1 1 calc R . . B107 B -0.4055(10) 0.5111(6) 0.1975(5) 0.0418(17) Uani 1 1 d . . . H107 H -0.3261 0.4627 0.1561 0.050 Uiso 1 1 calc R . . B108 B -0.5609(12) 0.4689(6) 0.2832(5) 0.051(2) Uani 1 1 d . . . H108 H -0.5828 0.3930 0.2959 0.061 Uiso 1 1 calc R . . B109 B -0.5817(13) 0.5253(6) 0.3732(6) 0.058(2) Uani 1 1 d . . . H109 H -0.6177 0.4859 0.4429 0.070 Uiso 1 1 calc R . . B110 B -0.4437(12) 0.6030(7) 0.3483(5) 0.055(2) Uani 1 1 d . . . H110 H -0.3908 0.6137 0.4025 0.067 Uiso 1 1 calc R . . B111 B -0.3276(10) 0.5996(5) 0.2397(6) 0.0451(18) Uani 1 1 d . . . H111 H -0.2003 0.6065 0.2243 0.054 Uiso 1 1 calc R . . B112 B -0.3878(12) 0.4908(6) 0.3143(6) 0.055(2) Uani 1 1 d . . . H112 H -0.2952 0.4289 0.3452 0.066 Uiso 1 1 calc R . . C12 C -0.3947(7) 0.8076(5) 0.0712(4) 0.0400(15) Uani 1 1 d . . . O12 O -0.3500(6) 0.8803(4) 0.0550(4) 0.0609(14) Uani 1 1 d . . . C13 C -0.5260(8) 0.6603(5) 0.0036(4) 0.0399(14) Uani 1 1 d . . . O13 O -0.5550(7) 0.6390(5) -0.0546(4) 0.0660(16) Uani 1 1 d . . . C14 C -0.2495(8) 0.6233(5) 0.0556(5) 0.0450(16) Uani 1 1 d . . . O14 O -0.1275(6) 0.5935(5) 0.0205(4) 0.0680(16) Uani 1 1 d . . . N11 N -0.7132(6) 0.7585(4) 0.1587(3) 0.0327(11) Uani 1 1 d . . . H11A H -0.691(7) 0.810(5) 0.167(4) 0.039 Uiso 1 1 d . . . C15 C -0.8755(7) 0.7904(6) 0.1222(5) 0.0489(17) Uani 1 1 d . . . C16 C -0.9217(8) 0.7088(6) 0.0948(6) 0.061(2) Uani 1 1 d . . . H16A H -0.9317 0.6535 0.1461 0.092 Uiso 1 1 calc R . . H16B H -0.8398 0.6869 0.0493 0.092 Uiso 1 1 calc R . . H16C H -1.0230 0.7340 0.0715 0.092 Uiso 1 1 calc R . . C17 C -0.8569(9) 0.8777(6) 0.0447(6) 0.066(2) Uani 1 1 d . . . H17A H -0.8280 0.9282 0.0645 0.099 Uiso 1 1 calc R . . H17B H -0.9571 0.9044 0.0203 0.099 Uiso 1 1 calc R . . H17C H -0.7737 0.8569 -0.0008 0.099 Uiso 1 1 calc R . . C18 C -0.9998(9) 0.8194(8) 0.2005(7) 0.080(3) Uani 1 1 d . . . H18A H -1.0074 0.7609 0.2489 0.119 Uiso 1 1 calc R . . H18B H -1.1035 0.8478 0.1804 0.119 Uiso 1 1 calc R . . H18C H -0.9660 0.8675 0.2212 0.119 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 Re1 0.03242(14) 0.03115(14) 0.03487(15) -0.00699(11) -0.00429(10) -0.00539(10) C1 0.035(3) 0.032(3) 0.025(3) -0.005(2) -0.004(2) -0.010(2) B3 0.039(4) 0.043(4) 0.032(4) -0.008(3) 0.003(3) -0.014(3) B4 0.032(4) 0.055(5) 0.045(4) -0.018(4) 0.001(3) -0.013(3) B5 0.046(4) 0.042(4) 0.038(4) -0.006(3) -0.007(3) -0.004(3) B6 0.040(4) 0.026(3) 0.037(4) -0.003(3) 0.001(3) -0.013(3) B7 0.047(4) 0.046(4) 0.037(4) -0.011(3) -0.012(3) -0.007(3) B8 0.039(4) 0.052(5) 0.045(4) -0.025(4) 0.013(3) -0.008(3) B9 0.038(4) 0.043(4) 0.059(5) -0.021(4) 0.001(4) 0.005(3) B10 0.051(4) 0.026(4) 0.051(5) -0.007(3) -0.008(4) -0.006(3) B11 0.040(4) 0.038(4) 0.047(4) -0.015(3) -0.003(3) -0.010(3) B12 0.057(5) 0.045(4) 0.049(5) -0.021(4) -0.004(4) -0.009(4) C2 0.053(4) 0.061(5) 0.053(5) -0.011(4) -0.016(4) -0.013(4) O2 0.075(4) 0.099(5) 0.083(5) -0.015(4) -0.047(4) -0.013(4) C3 0.045(4) 0.037(4) 0.060(5) -0.009(3) -0.015(3) -0.003(3) O3 0.072(4) 0.039(3) 0.094(5) 0.010(3) -0.025(3) -0.005(3) C4 0.033(3) 0.050(4) 0.064(5) -0.009(4) -0.007(3) -0.005(3) O4 0.042(3) 0.097(5) 0.086(5) -0.013(4) 0.014(3) -0.014(3) N1 0.036(3) 0.028(3) 0.033(3) -0.011(2) 0.000(2) -0.008(2) C5 0.057(4) 0.043(4) 0.036(4) -0.019(3) -0.001(3) -0.013(3) C6 0.074(5) 0.053(4) 0.040(4) -0.008(3) -0.022(4) -0.013(4) C7 0.070(5) 0.054(5) 0.055(5) -0.028(4) 0.011(4) -0.008(4) C8 0.092(6) 0.064(5) 0.030(4) -0.014(4) 0.004(4) -0.032(5) Re10 0.03201(13) 0.02923(13) 0.02902(14) -0.00778(10) -0.00609(9) -0.00518(10) C101 0.044(3) 0.034(3) 0.035(3) -0.013(3) 0.000(3) -0.010(3) B103 0.055(4) 0.032(4) 0.031(4) -0.013(3) -0.009(3) -0.007(3) B104 0.067(5) 0.048(5) 0.037(4) -0.006(4) 0.004(4) -0.031(4) B105 0.076(6) 0.041(4) 0.032(4) -0.007(3) 0.006(4) -0.027(4) B106 0.053(4) 0.036(4) 0.038(4) -0.012(3) -0.011(3) -0.011(3) B107 0.051(4) 0.034(4) 0.044(4) -0.012(3) -0.019(3) -0.003(3) B108 0.087(6) 0.030(4) 0.041(4) -0.001(3) -0.019(4) -0.024(4) B109 0.105(8) 0.041(5) 0.037(4) -0.005(4) -0.015(5) -0.029(5) B110 0.097(7) 0.044(5) 0.033(4) -0.004(3) -0.026(4) -0.020(5) B111 0.060(5) 0.030(4) 0.052(5) -0.010(3) -0.029(4) -0.005(3) B112 0.081(6) 0.036(4) 0.048(5) -0.001(4) -0.027(4) -0.007(4) C12 0.034(3) 0.040(4) 0.041(4) -0.006(3) 0.003(3) -0.012(3) O12 0.063(3) 0.055(3) 0.065(4) -0.017(3) 0.011(3) -0.024(3) C13 0.041(3) 0.049(4) 0.032(3) -0.012(3) -0.007(3) -0.010(3) O13 0.072(4) 0.092(4) 0.048(3) -0.032(3) -0.016(3) -0.019(3) C14 0.042(4) 0.047(4) 0.046(4) -0.018(3) -0.005(3) -0.003(3) O14 0.044(3) 0.075(4) 0.085(4) -0.041(3) 0.001(3) 0.005(3) N11 0.035(3) 0.029(3) 0.036(3) -0.012(2) -0.003(2) -0.006(2) C15 0.028(3) 0.051(4) 0.070(5) -0.024(4) -0.006(3) -0.002(3) C16 0.033(4) 0.069(5) 0.090(6) -0.032(5) -0.021(4) -0.001(3) C17 0.054(5) 0.050(5) 0.090(7) -0.003(4) -0.041(4) 0.003(4) C18 0.043(4) 0.101(8) 0.102(8) -0.059(6) 0.003(4) 0.000(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 C2 1.974(8) . ? Re1 C3 1.975(7) . ? Re1 C4 1.983(7) . ? Re1 C1 2.161(6) . ? Re1 N1 2.247(5) . ? Re1 B6 2.299(7) . ? Re1 B3 2.303(7) . ? Re1 B11 2.368(7) . ? Re1 B7 2.374(8) . ? C1 N1 1.415(7) . ? C1 B4 1.680(9) . ? C1 B5 1.689(10) . ? C1 B3 1.780(9) . ? C1 B6 1.807(8) . ? B3 B8 1.745(10) . ? B3 B4 1.772(11) . ? B3 B7 1.785(10) . ? B4 B8 1.768(11) . ? B4 B9 1.769(11) . ? B4 B5 1.817(11) . ? B5 B9 1.778(11) . ? B5 B10 1.791(11) . ? B5 B6 1.792(10) . ? B6 B10 1.726(10) . ? B6 B11 1.752(11) . ? B7 B12 1.795(12) . ? B7 B8 1.812(11) . ? B7 B11 1.886(11) . ? B8 B9 1.757(12) . ? B8 B12 1.767(11) . ? B9 B12 1.776(12) . ? B9 B10 1.784(11) . ? B10 B12 1.767(12) . ? B10 B11 1.792(11) . ? B11 B12 1.792(11) . ? C2 O2 1.121(9) . ? C3 O3 1.141(8) . ? C4 O4 1.128(8) . ? N1 H1 0.86(7) . ? N1 C5 1.526(8) . ? C5 C8 1.518(9) . ? C5 C6 1.519(10) . ? C5 C7 1.527(10) . ? Re10 C13 1.971(6) . ? Re10 C14 1.974(7) . ? Re10 C12 1.974(6) . ? Re10 C101 2.147(6) . ? Re10 N11 2.242(5) . ? Re10 B106 2.306(7) . ? Re10 B103 2.310(7) . ? Re10 B107 2.370(8) . ? Re10 B111 2.386(8) . ? C101 N11 1.415(8) . ? C101 B104 1.671(10) . ? C101 B105 1.695(10) . ? C101 B106 1.787(10) . ? C101 B103 1.802(9) . ? B103 B108 1.728(11) . ? B103 B107 1.775(11) . ? B103 B104 1.786(10) . ? B104 B108 1.780(13) . ? B104 B105 1.793(11) . ? B104 B109 1.794(13) . ? B105 B110 1.755(14) . ? B105 B109 1.758(12) . ? B105 B106 1.776(11) . ? B106 B110 1.742(11) . ? B106 B111 1.764(11) . ? B107 B108 1.786(12) . ? B107 B112 1.801(11) . ? B107 B111 1.882(10) . ? B108 B109 1.770(11) . ? B108 B112 1.780(12) . ? B109 B110 1.738(12) . ? B109 B112 1.768(14) . ? B110 B112 1.752(12) . ? B110 B111 1.803(12) . ? B111 B112 1.781(12) . ? C12 O12 1.138(8) . ? C13 O13 1.128(7) . ? C14 O14 1.127(8) . ? N11 H11A 0.86(6) . ? N11 C15 1.532(8) . ? C15 C17 1.488(11) . ? C15 C16 1.508(10) . ? C15 C18 1.541(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 83.3(3) . . ? C2 Re1 C4 83.4(3) . . ? C3 Re1 C4 104.0(3) . . ? C2 Re1 C1 150.1(3) . . ? C3 Re1 C1 113.5(3) . . ? C4 Re1 C1 113.9(3) . . ? C2 Re1 N1 172.1(3) . . ? C3 Re1 N1 90.0(2) . . ? C4 Re1 N1 94.3(2) . . ? C1 Re1 N1 37.38(19) . . ? C2 Re1 B6 114.5(3) . . ? C3 Re1 B6 161.1(3) . . ? C4 Re1 B6 85.4(3) . . ? C1 Re1 B6 47.7(2) . . ? N1 Re1 B6 72.7(2) . . ? C2 Re1 B3 115.7(3) . . ? C3 Re1 B3 84.2(3) . . ? C4 Re1 B3 160.3(3) . . ? C1 Re1 B3 46.9(2) . . ? N1 Re1 B3 67.5(2) . . ? B6 Re1 B3 82.1(3) . . ? C2 Re1 B11 76.2(3) . . ? C3 Re1 B11 144.4(3) . . ? C4 Re1 B11 102.2(3) . . ? C1 Re1 B11 76.3(2) . . ? N1 Re1 B11 111.7(2) . . ? B6 Re1 B11 44.1(3) . . ? B3 Re1 B11 79.1(3) . . ? C2 Re1 B7 76.3(3) . . ? C3 Re1 B7 100.3(3) . . ? C4 Re1 B7 146.1(3) . . ? C1 Re1 B7 76.3(2) . . ? N1 Re1 B7 109.1(2) . . ? B6 Re1 B7 78.8(3) . . ? B3 Re1 B7 44.8(3) . . ? B11 Re1 B7 46.9(3) . . ? N1 C1 B4 131.1(5) . . ? N1 C1 B5 138.1(5) . . ? B4 C1 B5 65.3(4) . . ? N1 C1 B3 104.0(5) . . ? B4 C1 B3 61.5(4) . . ? B5 C1 B3 115.9(5) . . ? N1 C1 B6 113.0(4) . . ? B4 C1 B6 115.3(5) . . ? B5 C1 B6 61.6(4) . . ? B3 C1 B6 114.8(4) . . ? N1 C1 Re1 74.6(3) . . ? B4 C1 Re1 129.5(4) . . ? B5 C1 Re1 129.2(4) . . ? B3 C1 Re1 70.8(3) . . ? B6 C1 Re1 70.2(3) . . ? B8 B3 B4 60.3(5) . . ? B8 B3 C1 102.2(5) . . ? B4 B3 C1 56.5(4) . . ? B8 B3 B7 61.8(4) . . ? B4 B3 B7 110.0(6) . . ? C1 B3 B7 103.9(5) . . ? B8 B3 Re1 123.2(5) . . ? B4 B3 Re1 116.7(4) . . ? C1 B3 Re1 62.4(3) . . ? B7 B3 Re1 69.7(3) . . ? C1 B4 B8 105.3(5) . . ? C1 B4 B9 103.3(5) . . ? B8 B4 B9 59.6(5) . . ? C1 B4 B3 62.0(4) . . ? B8 B4 B3 59.1(4) . . ? B9 B4 B3 107.6(6) . . ? C1 B4 B5 57.6(4) . . ? B8 B4 B5 107.6(5) . . ? B9 B4 B5 59.4(4) . . ? B3 B4 B5 110.0(5) . . ? C1 B5 B9 102.5(5) . . ? C1 B5 B10 104.7(5) . . ? B9 B5 B10 60.0(4) . . ? C1 B5 B6 62.5(4) . . ? B9 B5 B6 106.5(6) . . ? B10 B5 B6 57.6(4) . . ? C1 B5 B4 57.1(4) . . ? B9 B5 B4 59.0(4) . . ? B10 B5 B4 107.3(5) . . ? B6 B5 B4 109.5(5) . . ? B10 B6 B11 62.0(4) . . ? B10 B6 B5 61.1(4) . . ? B11 B6 B5 110.5(5) . . ? B10 B6 C1 102.5(5) . . ? B11 B6 C1 103.8(5) . . ? B5 B6 C1 56.0(4) . . ? B10 B6 Re1 124.0(5) . . ? B11 B6 Re1 70.0(3) . . ? B5 B6 Re1 116.2(4) . . ? C1 B6 Re1 62.1(3) . . ? B3 B7 B12 105.2(5) . . ? B3 B7 B8 58.0(4) . . ? B12 B7 B8 58.7(4) . . ? B3 B7 B11 108.2(5) . . ? B12 B7 B11 58.2(4) . . ? B8 B7 B11 105.6(5) . . ? B3 B7 Re1 65.5(3) . . ? B12 B7 Re1 117.0(5) . . ? B8 B7 Re1 116.5(4) . . ? B11 B7 Re1 66.4(3) . . ? B3 B8 B9 109.4(5) . . ? B3 B8 B12 108.2(5) . . ? B9 B8 B12 60.5(5) . . ? B3 B8 B4 60.6(4) . . ? B9 B8 B4 60.3(5) . . ? B12 B8 B4 108.1(6) . . ? B3 B8 B7 60.2(4) . . ? B9 B8 B7 109.6(5) . . ? B12 B8 B7 60.2(5) . . ? B4 B8 B7 108.9(5) . . ? B8 B9 B4 60.2(5) . . ? B8 B9 B12 60.0(5) . . ? B4 B9 B12 107.7(6) . . ? B8 B9 B5 109.9(5) . . ? B4 B9 B5 61.6(4) . . ? B12 B9 B5 107.7(5) . . ? B8 B9 B10 109.1(6) . . ? B4 B9 B10 109.7(5) . . ? B12 B9 B10 59.5(5) . . ? B5 B9 B10 60.3(4) . . ? B6 B10 B12 108.0(5) . . ? B6 B10 B9 109.2(5) . . ? B12 B10 B9 60.0(5) . . ? B6 B10 B5 61.2(4) . . ? B12 B10 B5 107.5(5) . . ? B9 B10 B5 59.7(4) . . ? B6 B10 B11 59.7(4) . . ? B12 B10 B11 60.4(4) . . ? B9 B10 B11 109.1(5) . . ? B5 B10 B11 108.7(5) . . ? B6 B11 B12 105.8(5) . . ? B6 B11 B10 58.3(4) . . ? B12 B11 B10 59.1(5) . . ? B6 B11 B7 109.3(5) . . ? B12 B11 B7 58.4(4) . . ? B10 B11 B7 106.6(5) . . ? B6 B11 Re1 65.9(3) . . ? B12 B11 Re1 117.4(4) . . ? B10 B11 Re1 117.3(4) . . ? B7 B11 Re1 66.7(3) . . ? B10 B12 B8 109.4(6) . . ? B10 B12 B9 60.5(5) . . ? B8 B12 B9 59.4(5) . . ? B10 B12 B11 60.5(5) . . ? B8 B12 B11 111.7(5) . . ? B9 B12 B11 109.4(6) . . ? B10 B12 B7 111.8(5) . . ? B8 B12 B7 61.1(5) . . ? B9 B12 B7 109.5(6) . . ? B11 B12 B7 63.4(4) . . ? O2 C2 Re1 179.0(8) . . ? O3 C3 Re1 174.2(7) . . ? O4 C4 Re1 175.0(7) . . ? H1 N1 C1 111(4) . . ? H1 N1 C5 103(4) . . ? C1 N1 C5 128.6(5) . . ? H1 N1 Re1 107(4) . . ? C1 N1 Re1 68.0(3) . . ? C5 N1 Re1 135.0(4) . . ? C8 C5 C6 110.7(7) . . ? C8 C5 N1 113.8(5) . . ? C6 C5 N1 105.0(5) . . ? C8 C5 C7 111.8(6) . . ? C6 C5 C7 109.5(6) . . ? N1 C5 C7 105.7(6) . . ? C13 Re10 C14 80.7(3) . . ? C13 Re10 C12 104.4(3) . . ? C14 Re10 C12 85.1(3) . . ? C13 Re10 C101 113.4(2) . . ? C14 Re10 C101 150.3(3) . . ? C12 Re10 C101 114.2(2) . . ? C13 Re10 N11 95.2(2) . . ? C14 Re10 N11 172.1(2) . . ? C12 Re10 N11 89.4(2) . . ? C101 Re10 N11 37.5(2) . . ? C13 Re10 B106 160.4(3) . . ? C14 Re10 B106 117.6(3) . . ? C12 Re10 B106 85.1(3) . . ? C101 Re10 B106 47.2(2) . . ? N11 Re10 B106 67.4(2) . . ? C13 Re10 B103 84.0(3) . . ? C14 Re10 B103 112.9(3) . . ? C12 Re10 B103 161.4(3) . . ? C101 Re10 B103 47.5(2) . . ? N11 Re10 B103 73.1(2) . . ? B106 Re10 B103 82.3(3) . . ? C13 Re10 B107 101.2(3) . . ? C14 Re10 B107 75.6(3) . . ? C12 Re10 B107 144.8(3) . . ? C101 Re10 B107 76.0(3) . . ? N11 Re10 B107 111.9(2) . . ? B106 Re10 B107 78.5(3) . . ? B103 Re10 B107 44.6(3) . . ? C13 Re10 B111 145.2(3) . . ? C14 Re10 B111 78.3(3) . . ? C12 Re10 B111 101.1(3) . . ? C101 Re10 B111 76.0(3) . . ? N11 Re10 B111 108.4(3) . . ? B106 Re10 B111 44.1(3) . . ? B103 Re10 B111 79.1(3) . . ? B107 Re10 B111 46.6(2) . . ? N11 C101 B104 138.9(6) . . ? N11 C101 B105 130.1(5) . . ? B104 C101 B105 64.4(4) . . ? N11 C101 B106 103.3(5) . . ? B104 C101 B106 115.2(6) . . ? B105 C101 B106 61.2(4) . . ? N11 C101 B103 114.2(5) . . ? B104 C101 B103 61.8(4) . . ? B105 C101 B103 115.0(5) . . ? B106 C101 B103 115.6(5) . . ? N11 C101 Re10 74.9(3) . . ? B104 C101 Re10 130.0(5) . . ? B105 C101 Re10 129.5(5) . . ? B106 C101 Re10 71.1(3) . . ? B103 C101 Re10 71.0(3) . . ? B108 B103 B107 61.3(5) . . ? B108 B103 B104 60.8(5) . . ? B107 B103 B104 109.2(6) . . ? B108 B103 C101 101.4(5) . . ? B107 B103 C101 102.4(5) . . ? B104 B103 C101 55.5(4) . . ? B108 B103 Re10 122.5(5) . . ? B107 B103 Re10 69.5(3) . . ? B104 B103 Re10 115.0(4) . . ? C101 B103 Re10 61.5(3) . . ? C101 B104 B108 104.6(6) . . ? C101 B104 B103 62.7(4) . . ? B108 B104 B103 57.9(4) . . ? C101 B104 B105 58.5(4) . . ? B108 B104 B105 106.7(6) . . ? B103 B104 B105 111.0(5) . . ? C101 B104 B109 103.3(6) . . ? B108 B104 B109 59.4(5) . . ? B103 B104 B109 107.1(6) . . ? B105 B104 B109 58.7(5) . . ? C101 B105 B110 105.7(6) . . ? C101 B105 B109 103.8(5) . . ? B110 B105 B109 59.3(5) . . ? C101 B105 B106 61.9(4) . . ? B110 B105 B106 59.1(5) . . ? B109 B105 B106 107.4(6) . . ? C101 B105 B104 57.2(4) . . ? B110 B105 B104 108.5(6) . . ? B109 B105 B104 60.7(5) . . ? B106 B105 B104 109.8(5) . . ? B110 B106 B111 61.9(5) . . ? B110 B106 B105 59.8(5) . . ? B111 B106 B105 109.6(6) . . ? B110 B106 C101 102.3(5) . . ? B111 B106 C101 103.9(5) . . ? B105 B106 C101 56.8(4) . . ? B110 B106 Re10 123.8(5) . . ? B111 B106 Re10 70.4(3) . . ? B105 B106 Re10 116.4(4) . . ? C101 B106 Re10 61.7(3) . . ? B103 B107 B108 58.0(4) . . ? B103 B107 B112 106.6(6) . . ? B108 B107 B112 59.5(5) . . ? B103 B107 B111 109.7(5) . . ? B108 B107 B111 105.9(5) . . ? B112 B107 B111 57.8(4) . . ? B103 B107 Re10 65.9(3) . . ? B108 B107 Re10 116.7(5) . . ? B112 B107 Re10 117.6(4) . . ? B111 B107 Re10 67.2(3) . . ? B103 B108 B109 110.9(6) . . ? B103 B108 B104 61.2(5) . . ? B109 B108 B104 60.7(5) . . ? B103 B108 B112 109.7(6) . . ? B109 B108 B112 59.8(5) . . ? B104 B108 B112 108.1(6) . . ? B103 B108 B107 60.7(4) . . ? B109 B108 B107 109.5(6) . . ? B104 B108 B107 109.0(5) . . ? B112 B108 B107 60.7(5) . . ? B110 B109 B105 60.3(5) . . ? B110 B109 B112 60.0(5) . . ? B105 B109 B112 107.7(6) . . ? B110 B109 B108 109.2(6) . . ? B105 B109 B108 108.7(6) . . ? B112 B109 B108 60.4(5) . . ? B110 B109 B104 109.2(6) . . ? B105 B109 B104 60.6(5) . . ? B112 B109 B104 108.0(6) . . ? B108 B109 B104 59.9(5) . . ? B109 B110 B106 109.9(6) . . ? B109 B110 B112 60.9(5) . . ? B106 B110 B112 108.1(6) . . ? B109 B110 B105 60.4(5) . . ? B106 B110 B105 61.0(5) . . ? B112 B110 B105 108.6(6) . . ? B109 B110 B111 109.7(6) . . ? B106 B110 B111 59.6(4) . . ? B112 B110 B111 60.1(5) . . ? B105 B110 B111 108.7(6) . . ? B106 B111 B112 105.9(6) . . ? B106 B111 B110 58.5(5) . . ? B112 B111 B110 58.5(5) . . ? B106 B111 B107 108.4(5) . . ? B112 B111 B107 58.8(4) . . ? B110 B111 B107 105.7(6) . . ? B106 B111 Re10 65.5(3) . . ? B112 B111 Re10 117.7(5) . . ? B110 B111 Re10 116.8(5) . . ? B107 B111 Re10 66.2(3) . . ? B110 B112 B109 59.2(5) . . ? B110 B112 B108 108.1(7) . . ? B109 B112 B108 59.8(5) . . ? B110 B112 B111 61.3(5) . . ? B109 B112 B111 109.3(6) . . ? B108 B112 B111 110.6(6) . . ? B110 B112 B107 111.5(6) . . ? B109 B112 B107 108.8(6) . . ? B108 B112 B107 59.8(5) . . ? B111 B112 B107 63.4(4) . . ? O12 C12 Re10 174.0(6) . . ? O13 C13 Re10 172.5(7) . . ? O14 C14 Re10 177.6(7) . . ? H11A N11 C101 111(4) . . ? H11A N11 C15 108(4) . . ? C101 N11 C15 128.8(5) . . ? H11A N11 Re10 101(4) . . ? C101 N11 Re10 67.6(3) . . ? C15 N11 Re10 134.2(4) . . ? C17 C15 C16 111.7(7) . . ? C17 C15 N11 104.8(5) . . ? C16 C15 N11 113.8(6) . . ? C17 C15 C18 112.5(7) . . ? C16 C15 C18 109.4(6) . . ? N11 C15 C18 104.6(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.472 _refine_diff_density_min -1.845 _refine_diff_density_rms 0.154 #============================================================================== data_7c _database_code_depnum_ccdc_archive 'CCDC 278687' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H30 B10 N O2 Re' _chemical_formula_weight 526.68 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7063(6) _cell_length_b 14.1589(13) _cell_length_c 20.4558(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.992(6) _cell_angle_gamma 90.00 _cell_volume 2215.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.23 _cell_measurement_theta_max 19.55 _exptl_crystal_description orange _exptl_crystal_colour plate _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 5.492 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.26877 _exptl_absorpt_correction_T_max 0.70804 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5383 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.40 _reflns_number_total 5014 _reflns_number_gt 3896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (Enraf-Nonius, 1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+1.7233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5014 _refine_ls_number_parameters 250 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Re Re 0.95320(3) 0.199925(16) 0.065445(10) 0.03026(8) Uani 1 1 d . . . C1 C 0.9780(7) 0.2116(4) 0.1714(3) 0.0321(12) Uani 1 1 d . . . B3 B 1.0371(9) 0.0968(5) 0.1532(3) 0.0372(14) Uani 1 1 d . . . H3 H 1.1682 0.0688 0.1485 0.045 Uiso 1 1 calc R . . B4 B 0.9808(11) 0.1278(6) 0.2318(4) 0.0463(18) Uani 1 1 d . . . H4 H 1.0774 0.1232 0.2759 0.056 Uiso 1 1 calc R . . B5 B 0.8205(11) 0.2210(6) 0.2224(4) 0.051(2) Uani 1 1 d . . . H5 H 0.8173 0.2756 0.2605 0.061 Uiso 1 1 calc R . . B6 B 0.7661(9) 0.2488(6) 0.1378(4) 0.0446(17) Uani 1 1 d . . . H6 H 0.7187 0.3201 0.1236 0.054 Uiso 1 1 calc R . . B7 B 0.8480(10) 0.0522(5) 0.1036(4) 0.0430(16) Uani 1 1 d . . . H7 H 0.8551 -0.0035 0.0665 0.052 Uiso 1 1 calc R . . B8 B 0.8896(10) 0.0262(6) 0.1900(4) 0.0500(19) Uani 1 1 d . . . H8 H 0.9246 -0.0454 0.2080 0.060 Uiso 1 1 calc R . . B9 B 0.7552(11) 0.1022(7) 0.2319(4) 0.057(2) Uani 1 1 d . . . H9 H 0.7026 0.0796 0.2770 0.069 Uiso 1 1 calc R . . B10 B 0.6307(11) 0.1736(6) 0.1745(4) 0.052(2) Uani 1 1 d . . . H10 H 0.4985 0.1962 0.1827 0.062 Uiso 1 1 calc R . . B11 B 0.6802(9) 0.1462(6) 0.0933(4) 0.0461(18) Uani 1 1 d . . . H11 H 0.5807 0.1494 0.0500 0.055 Uiso 1 1 calc R . . B12 B 0.6758(11) 0.0546(6) 0.1530(4) 0.054(2) Uani 1 1 d . . . H12 H 0.5732 0.0002 0.1464 0.064 Uiso 1 1 calc R . . C2 C 0.8432(8) 0.1303(5) -0.0120(3) 0.0430(15) Uani 1 1 d . . . O2 O 0.7837(7) 0.0908(4) -0.0581(2) 0.0638(14) Uani 1 1 d . . . C3 C 0.8510(8) 0.3137(5) 0.0215(3) 0.0422(15) Uani 1 1 d . . . O3 O 0.7806(8) 0.3770(4) -0.0028(3) 0.0726(17) Uani 1 1 d . . . C4 C 1.1984(7) 0.1534(5) 0.0366(3) 0.0363(13) Uani 1 1 d . . . H4A H 1.272(8) 0.105(5) 0.050(3) 0.044 Uiso 1 1 d . . . C5 C 1.1592(8) 0.2216(5) -0.0016(3) 0.0391(14) Uani 1 1 d . . . C6 C 1.1975(10) 0.2779(5) -0.0602(3) 0.0500(17) Uani 1 1 d . . . C7 C 1.0496(11) 0.2658(7) -0.1167(3) 0.064(2) Uani 1 1 d . . . H7A H 0.9442 0.2930 -0.1044 0.096 Uiso 1 1 calc R . . H7B H 1.0314 0.1998 -0.1258 0.096 Uiso 1 1 calc R . . H7C H 1.0805 0.2970 -0.1553 0.096 Uiso 1 1 calc R . . C8 C 1.2289(12) 0.3823(6) -0.0435(4) 0.071(2) Uani 1 1 d . . . H8A H 1.1241 0.4094 -0.0305 0.106 Uiso 1 1 calc R . . H8B H 1.2601 0.4149 -0.0815 0.106 Uiso 1 1 calc R . . H8C H 1.3220 0.3880 -0.0080 0.106 Uiso 1 1 calc R . . C9 C 1.3664(11) 0.2360(7) -0.0811(4) 0.071(2) Uani 1 1 d . . . H9A H 1.4605 0.2447 -0.0463 0.106 Uiso 1 1 calc R . . H9B H 1.3940 0.2675 -0.1201 0.106 Uiso 1 1 calc R . . H9C H 1.3502 0.1698 -0.0899 0.106 Uiso 1 1 calc R . . N N 1.1137(6) 0.2710(4) 0.1542(2) 0.0337(11) Uani 1 1 d D . . H H 1.217(5) 0.243(4) 0.159(3) 0.040 Uiso 1 1 d D . . C10 C 1.1584(9) 0.3710(4) 0.1796(3) 0.0447(15) Uani 1 1 d . . . C11 C 1.2103(13) 0.3589(7) 0.2542(4) 0.082(3) Uani 1 1 d . . . H11A H 1.2390 0.4195 0.2738 0.124 Uiso 1 1 calc R . . H11B H 1.3099 0.3179 0.2618 0.124 Uiso 1 1 calc R . . H11C H 1.1143 0.3320 0.2736 0.124 Uiso 1 1 calc R . . C12 C 1.3159(10) 0.4001(6) 0.1475(4) 0.063(2) Uani 1 1 d . . . H12A H 1.3503 0.4629 0.1614 0.094 Uiso 1 1 calc R . . H12B H 1.2873 0.3990 0.1005 0.094 Uiso 1 1 calc R . . H12C H 1.4103 0.3571 0.1602 0.094 Uiso 1 1 calc R . . C13 C 1.0107(13) 0.4391(6) 0.1640(6) 0.101(4) Uani 1 1 d . . . H13A H 1.0452 0.5002 0.1812 0.152 Uiso 1 1 calc R . . H13B H 0.9109 0.4175 0.1836 0.152 Uiso 1 1 calc R . . H13C H 0.9813 0.4431 0.1171 0.152 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 Re 0.02744(12) 0.03034(12) 0.03264(12) -0.00014(11) 0.00224(8) 0.00212(11) C1 0.026(3) 0.032(3) 0.040(3) -0.001(2) 0.008(2) 0.001(2) B3 0.042(4) 0.034(4) 0.035(3) 0.003(3) 0.004(3) 0.000(3) B4 0.054(5) 0.045(4) 0.041(4) 0.007(3) 0.013(3) 0.004(4) B5 0.054(5) 0.050(5) 0.053(5) -0.001(4) 0.023(4) 0.000(4) B6 0.034(4) 0.043(4) 0.059(5) 0.003(4) 0.015(3) 0.008(3) B7 0.044(4) 0.035(4) 0.050(4) -0.001(3) 0.005(3) -0.004(3) B8 0.046(4) 0.041(4) 0.066(5) 0.009(4) 0.020(4) -0.002(3) B9 0.062(5) 0.058(5) 0.059(5) 0.009(4) 0.032(4) -0.001(4) B10 0.042(4) 0.052(5) 0.066(5) 0.001(4) 0.027(4) 0.003(4) B11 0.030(4) 0.046(4) 0.062(5) 0.003(4) 0.005(3) -0.001(3) B12 0.044(4) 0.053(5) 0.067(5) 0.003(4) 0.021(4) -0.005(4) C2 0.033(3) 0.046(4) 0.048(4) -0.007(3) -0.005(3) 0.003(3) O2 0.060(3) 0.073(4) 0.056(3) -0.013(3) -0.002(2) -0.012(3) C3 0.042(3) 0.046(4) 0.038(3) 0.000(3) 0.002(3) 0.007(3) O3 0.082(4) 0.058(4) 0.076(4) 0.021(3) 0.001(3) 0.025(3) C4 0.026(3) 0.046(4) 0.038(3) -0.003(3) 0.007(2) 0.002(3) C5 0.037(3) 0.042(4) 0.040(3) -0.004(3) 0.009(3) -0.005(3) C6 0.066(5) 0.047(4) 0.039(3) 0.004(3) 0.010(3) -0.003(3) C7 0.068(5) 0.085(6) 0.037(4) 0.012(4) 0.002(3) -0.006(5) C8 0.103(7) 0.058(5) 0.055(5) 0.011(4) 0.024(4) -0.016(5) C9 0.070(5) 0.098(7) 0.049(4) 0.013(4) 0.027(4) -0.005(5) N 0.032(3) 0.030(2) 0.039(3) -0.004(2) 0.003(2) 0.003(2) C10 0.050(4) 0.032(3) 0.052(4) -0.014(3) 0.006(3) -0.007(3) C11 0.102(7) 0.092(7) 0.054(5) -0.027(5) 0.012(5) -0.049(6) C12 0.074(5) 0.044(4) 0.072(5) -0.011(4) 0.015(4) -0.014(4) C13 0.090(7) 0.042(5) 0.162(11) -0.044(6) -0.022(7) 0.011(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 Re C3 1.962(6) . ? Re C2 1.967(6) . ? Re C4 2.150(6) . ? Re C1 2.158(6) . ? Re C5 2.242(6) . ? Re B6 2.295(7) . ? Re N 2.300(5) . ? Re B3 2.344(7) . ? Re B11 2.371(7) . ? Re B7 2.407(7) . ? C1 N 1.419(7) . ? C1 B5 1.701(10) . ? C1 B4 1.712(9) . ? C1 B3 1.740(9) . ? C1 B6 1.773(9) . ? B3 B8 1.751(10) . ? B3 B4 1.770(10) . ? B3 B7 1.787(10) . ? B4 B8 1.775(12) . ? B4 B9 1.776(12) . ? B4 B5 1.801(12) . ? B5 B9 1.772(12) . ? B5 B6 1.776(12) . ? B5 B10 1.789(13) . ? B6 B10 1.725(11) . ? B6 B11 1.797(12) . ? B7 B12 1.764(11) . ? B7 B8 1.796(11) . ? B7 B11 1.850(11) . ? B8 B12 1.774(12) . ? B8 B9 1.785(12) . ? B9 B10 1.745(13) . ? B9 B12 1.787(13) . ? B10 B12 1.786(12) . ? B10 B11 1.791(12) . ? B11 B12 1.784(12) . ? C2 O2 1.144(7) . ? C3 O3 1.131(8) . ? C4 H4A 0.91(7) . ? C4 C5 1.256(9) . ? C5 C6 1.497(9) . ? C6 C8 1.530(10) . ? C6 C7 1.531(10) . ? C6 C9 1.537(11) . ? N H 0.88(2) . ? N C10 1.532(8) . ? C10 C13 1.497(11) . ? C10 C12 1.505(10) . ? C10 C11 1.540(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Re C2 86.2(3) . . ? C3 Re C4 116.3(3) . . ? C2 Re C4 86.1(2) . . ? C3 Re C1 112.2(2) . . ? C2 Re C1 145.4(3) . . ? C4 Re C1 109.0(2) . . ? C3 Re C5 83.2(3) . . ? C2 Re C5 81.0(3) . . ? C4 Re C5 33.1(2) . . ? C1 Re C5 128.4(2) . . ? C3 Re B6 78.4(3) . . ? C2 Re B6 115.3(3) . . ? C4 Re B6 155.7(3) . . ? C1 Re B6 46.8(2) . . ? C5 Re B6 154.2(3) . . ? C3 Re N 98.6(2) . . ? C2 Re N 172.7(2) . . ? C4 Re N 86.8(2) . . ? C1 Re N 36.95(19) . . ? C5 Re N 94.0(2) . . ? B6 Re N 71.3(2) . . ? C3 Re B3 157.0(3) . . ? C2 Re B3 110.9(3) . . ? C4 Re B3 81.4(2) . . ? C1 Re B3 45.3(2) . . ? C5 Re B3 113.8(2) . . ? B6 Re B3 80.2(3) . . ? N Re B3 66.2(2) . . ? C3 Re B11 93.1(3) . . ? C2 Re B11 74.0(3) . . ? C4 Re B11 143.4(3) . . ? C1 Re B11 75.9(3) . . ? C5 Re B11 155.0(3) . . ? B6 Re B11 45.3(3) . . ? N Re B11 111.0(2) . . ? B3 Re B11 77.6(3) . . ? C3 Re B7 136.8(3) . . ? C2 Re B7 72.3(3) . . ? C4 Re B7 99.5(3) . . ? C1 Re B7 74.6(2) . . ? C5 Re B7 127.5(3) . . ? B6 Re B7 77.9(3) . . ? N Re B7 107.1(2) . . ? B3 Re B7 44.2(2) . . ? B11 Re B7 45.5(3) . . ? N C1 B5 135.1(5) . . ? N C1 B4 130.2(5) . . ? B5 C1 B4 63.7(4) . . ? N C1 B3 106.3(4) . . ? B5 C1 B3 115.4(5) . . ? B4 C1 B3 61.7(4) . . ? N C1 B6 113.6(5) . . ? B5 C1 B6 61.4(4) . . ? B4 C1 B6 114.5(5) . . ? B3 C1 B6 116.6(5) . . ? N C1 Re 77.0(3) . . ? B5 C1 Re 129.8(4) . . ? B4 C1 Re 131.6(4) . . ? B3 C1 Re 73.0(3) . . ? B6 C1 Re 70.7(3) . . ? C1 B3 B8 104.0(5) . . ? C1 B3 B4 58.4(4) . . ? B8 B3 B4 60.5(4) . . ? C1 B3 B7 103.6(5) . . ? B8 B3 B7 61.0(4) . . ? B4 B3 B7 109.3(5) . . ? C1 B3 Re 61.7(3) . . ? B8 B3 Re 123.5(5) . . ? B4 B3 Re 117.8(4) . . ? B7 B3 Re 69.8(3) . . ? C1 B4 B3 60.0(4) . . ? C1 B4 B8 104.2(5) . . ? B3 B4 B8 59.2(4) . . ? C1 B4 B9 102.5(5) . . ? B3 B4 B9 107.4(6) . . ? B8 B4 B9 60.3(5) . . ? C1 B4 B5 57.8(4) . . ? B3 B4 B5 109.1(5) . . ? B8 B4 B5 108.5(6) . . ? B9 B4 B5 59.4(5) . . ? C1 B5 B9 103.1(5) . . ? C1 B5 B6 61.3(4) . . ? B9 B5 B6 106.3(6) . . ? C1 B5 B10 103.4(6) . . ? B9 B5 B10 58.7(5) . . ? B6 B5 B10 57.9(5) . . ? C1 B5 B4 58.4(4) . . ? B9 B5 B4 59.6(5) . . ? B6 B5 B4 110.1(6) . . ? B10 B5 B4 106.7(6) . . ? B10 B6 C1 103.0(6) . . ? B10 B6 B5 61.4(5) . . ? C1 B6 B5 57.3(4) . . ? B10 B6 B11 61.1(5) . . ? C1 B6 B11 102.8(5) . . ? B5 B6 B11 110.0(6) . . ? B10 B6 Re 123.7(5) . . ? C1 B6 Re 62.5(3) . . ? B5 B6 Re 118.0(5) . . ? B11 B6 Re 69.6(4) . . ? B12 B7 B3 106.6(6) . . ? B12 B7 B8 59.7(5) . . ? B3 B7 B8 58.5(4) . . ? B12 B7 B11 59.1(5) . . ? B3 B7 B11 108.7(5) . . ? B8 B7 B11 107.3(6) . . ? B12 B7 Re 118.4(5) . . ? B3 B7 Re 66.0(3) . . ? B8 B7 Re 118.1(4) . . ? B11 B7 Re 66.2(3) . . ? B3 B8 B12 107.8(6) . . ? B3 B8 B4 60.3(4) . . ? B12 B8 B4 108.3(6) . . ? B3 B8 B9 107.9(6) . . ? B12 B8 B9 60.3(5) . . ? B4 B8 B9 59.9(5) . . ? B3 B8 B7 60.5(4) . . ? B12 B8 B7 59.2(4) . . ? B4 B8 B7 108.7(5) . . ? B9 B8 B7 107.7(6) . . ? B10 B9 B5 61.1(5) . . ? B10 B9 B4 109.8(6) . . ? B5 B9 B4 61.0(5) . . ? B10 B9 B8 109.3(6) . . ? B5 B9 B8 109.3(5) . . ? B4 B9 B8 59.8(4) . . ? B10 B9 B12 60.7(5) . . ? B5 B9 B12 109.3(6) . . ? B4 B9 B12 107.6(5) . . ? B8 B9 B12 59.6(5) . . ? B6 B10 B9 109.8(6) . . ? B6 B10 B12 109.2(5) . . ? B9 B10 B12 60.8(5) . . ? B6 B10 B5 60.7(5) . . ? B9 B10 B5 60.2(5) . . ? B12 B10 B5 108.5(6) . . ? B6 B10 B11 61.4(5) . . ? B9 B10 B11 109.7(6) . . ? B12 B10 B11 59.8(5) . . ? B5 B10 B11 109.7(5) . . ? B12 B11 B10 59.9(5) . . ? B12 B11 B6 106.1(6) . . ? B10 B11 B6 57.5(4) . . ? B12 B11 B7 58.1(4) . . ? B10 B11 B7 106.0(6) . . ? B6 B11 B7 108.4(5) . . ? B12 B11 Re 119.3(5) . . ? B10 B11 Re 116.7(5) . . ? B6 B11 Re 65.1(3) . . ? B7 B11 Re 68.2(3) . . ? B7 B12 B8 61.0(4) . . ? B7 B12 B11 62.8(4) . . ? B8 B12 B11 111.3(6) . . ? B7 B12 B10 110.0(6) . . ? B8 B12 B10 107.9(6) . . ? B11 B12 B10 60.2(5) . . ? B7 B12 B9 109.0(6) . . ? B8 B12 B9 60.2(5) . . ? B11 B12 B9 108.1(6) . . ? B10 B12 B9 58.5(5) . . ? O2 C2 Re 177.7(6) . . ? O3 C3 Re 175.0(6) . . ? H4A C4 C5 150(4) . . ? H4A C4 Re 133(4) . . ? C5 C4 Re 77.5(4) . . ? C4 C5 C6 148.4(6) . . ? C4 C5 Re 69.4(4) . . ? C6 C5 Re 141.7(5) . . ? C5 C6 C8 112.2(6) . . ? C5 C6 C7 110.1(6) . . ? C8 C6 C7 111.0(7) . . ? C5 C6 C9 105.9(6) . . ? C8 C6 C9 108.6(7) . . ? C7 C6 C9 108.9(6) . . ? H N C1 113(4) . . ? H N C10 103(4) . . ? C1 N C10 127.2(5) . . ? H N Re 106(4) . . ? C1 N Re 66.1(3) . . ? C10 N Re 138.5(4) . . ? C13 C10 C12 111.3(7) . . ? C13 C10 N 112.9(6) . . ? C12 C10 N 105.4(5) . . ? C13 C10 C11 112.5(7) . . ? C12 C10 C11 109.7(6) . . ? N C10 C11 104.8(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.459 _refine_diff_density_min -1.148 _refine_diff_density_rms 0.151 #============================================================================== data_8b _database_code_depnum_ccdc_archive 'CCDC 278688' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H36 B10 N O2 Re' _chemical_formula_weight 628.81 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0404(7) _cell_length_b 14.2838(14) _cell_length_c 17.573(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.507(7) _cell_angle_gamma 90.00 _cell_volume 2724.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.24 _cell_measurement_theta_max 23.43 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method ? _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 4.480 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.46 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-4\q/3 _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11065 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.55 _reflns_number_total 6284 _reflns_number_observed 4072 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (Enraf-Nonius, 1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6284 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_obs 0.0437 _refine_ls_wR_factor_all 0.0686 _refine_ls_wR_factor_obs 0.0574 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.018 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.56207(2) -0.05482(2) -0.190554(13) 0.03230(7) Uani 1 d . . C1 C 0.5044(5) -0.0373(4) -0.3131(3) 0.0355(14) Uani 1 d . . B3 B 0.6465(6) -0.1102(4) -0.2952(4) 0.036(2) Uani 1 d . . B7 B 0.5967(7) -0.2054(4) -0.2404(4) 0.040(2) Uani 1 d . . H3 H 0.6616(7) -0.2466(4) -0.1985(4) 0.048 Uiso 1 calc R . B11 B 0.4358(6) -0.1852(5) -0.2255(4) 0.046(2) Uani 1 d . . H4 H 0.4020(6) -0.2140(5) -0.1751(4) 0.055 Uiso 1 calc R . B6 B 0.3773(6) -0.0792(5) -0.2707(4) 0.046(2) Uani 1 d . . H5 H 0.3037(6) -0.0409(5) -0.2494(4) 0.055 Uiso 1 calc R . B4 B 0.5429(7) -0.1014(5) -0.3854(4) 0.045(2) Uani 1 d . . H6 H 0.5768(7) -0.0711(5) -0.4352(4) 0.055 Uiso 1 calc R . B8 B 0.5936(7) -0.2126(5) -0.3448(4) 0.050(2) Uani 1 d . . H7 H 0.6574(7) -0.2574(5) -0.3698(4) 0.060 Uiso 1 calc R . B12 B 0.4726(7) -0.2590(5) -0.3030(4) 0.050(2) Uani 1 d . . H8 H 0.4610(7) -0.3353(5) -0.2999(4) 0.060 Uiso 1 calc R . B10 B 0.3429(7) -0.1834(5) -0.3226(4) 0.056(2) Uani 1 d . . H9 H 0.2483(7) -0.2109(5) -0.3341(4) 0.067 Uiso 1 calc R . B5 B 0.3849(6) -0.0837(5) -0.3718(4) 0.048(2) Uani 1 d . . H10 H 0.3186(6) -0.0430(5) -0.4132(4) 0.058 Uiso 1 calc R . B9 B 0.4386(7) -0.1973(5) -0.3921(4) 0.054(2) Uani 1 d . . H11 H 0.4043(7) -0.2320(5) -0.4477(4) 0.065 Uiso 1 calc R . C2 C 0.5929(6) -0.1364(4) -0.0983(4) 0.045(2) Uani 1 d . . O2 O 0.6115(5) -0.1835(3) -0.0459(3) 0.073(2) Uani 1 d . . C3 C 0.4725(5) 0.0237(4) -0.1278(4) 0.052(2) Uani 1 d . . O3 O 0.4195(4) 0.0656(3) -0.0907(3) 0.079(2) Uani 1 d . . N N 0.5460(4) 0.0521(4) -0.2859(3) 0.0352(11) Uani 1 d . . H H 0.6067(43) 0.0636(40) -0.2949(30) 0.031(17) Uiso 1 d . . C4 C 0.4800(5) 0.1459(4) -0.3049(4) 0.043(2) Uani 1 d . . C5 C 0.4955(6) 0.1684(5) -0.3876(4) 0.069(2) Uani 1 d . . H5A H 0.5815(6) 0.1692(5) -0.3903(4) 0.103 Uiso 1 calc R . H5B H 0.4601(6) 0.2285(5) -0.4023(4) 0.103 Uiso 1 calc R . H5C H 0.4546(6) 0.1214(5) -0.4221(4) 0.103 Uiso 1 calc R . C6 C 0.3467(5) 0.1438(5) -0.2974(4) 0.060(2) Uani 1 d . . H6A H 0.3034(5) 0.0994(5) -0.3334(4) 0.090 Uiso 1 calc R . H6B H 0.3113(5) 0.2048(5) -0.3082(4) 0.090 Uiso 1 calc R . H6C H 0.3401(5) 0.1258(5) -0.2456(4) 0.090 Uiso 1 calc R . C7 C 0.5507(6) 0.2154(4) -0.2489(4) 0.061(2) Uani 1 d . . H7A H 0.6355(6) 0.2157(4) -0.2546(4) 0.092 Uiso 1 calc R . H7B H 0.5452(6) 0.1978(4) -0.1969(4) 0.092 Uiso 1 calc R . H7C H 0.5163(6) 0.2767(4) -0.2596(4) 0.092 Uiso 1 calc R . C8 C 0.7705(4) -0.0502(4) -0.1795(3) 0.0354(12) Uani 1 d . . H8A H 0.8153(4) -0.1008(4) -0.1487(3) 0.042 Uiso 1 calc R . C9 C 0.7463(4) 0.0279(4) -0.1377(3) 0.0345(14) Uani 1 d . . H9A H 0.7550(4) 0.0868(4) -0.1648(3) 0.041 Uiso 1 calc R . C10 C 0.7774(5) 0.0376(4) -0.0521(3) 0.0368(14) Uani 1 d . . C11 C 0.8480(6) -0.0259(5) -0.0047(4) 0.061(2) Uani 1 d . . H11A H 0.8775(6) -0.0789(5) -0.0261(4) 0.073 Uiso 1 calc R . C12 C 0.8760(7) -0.0121(7) 0.0746(4) 0.082(3) Uani 1 d . . H12A H 0.9243(7) -0.0556(7) 0.1059(4) 0.098 Uiso 1 calc R . C13 C 0.8331(8) 0.0649(7) 0.1067(4) 0.090(3) Uani 1 d . . H13A H 0.8513(8) 0.0737(7) 0.1600(4) 0.108 Uiso 1 calc R . C14 C 0.7629(8) 0.1295(6) 0.0606(5) 0.080(3) Uani 1 d . . H14A H 0.7338(8) 0.1822(6) 0.0826(5) 0.096 Uiso 1 calc R . C15 C 0.7357(6) 0.1163(5) -0.0182(4) 0.053(2) Uani 1 d . . H15A H 0.6888(6) 0.1607(5) -0.0493(4) 0.063 Uiso 1 calc R . C16 C 0.7697(4) -0.0556(4) -0.2659(3) 0.0353(12) Uani 1 d . . C17 C 0.8614(5) -0.0148(4) -0.2943(3) 0.0419(15) Uani 1 d . . H17A H 0.9160(5) 0.0186(4) -0.2576(3) 0.050 Uiso 1 calc R . C18 C 0.8936(5) -0.0127(5) -0.3746(3) 0.045(2) Uani 1 d . . C19 C 1.0315(6) 0.0016(7) -0.3651(4) 0.096(3) Uani 1 d . . H19A H 1.0542(6) 0.0582(7) -0.3366(4) 0.144 Uiso 1 calc R . H19B H 1.0543(6) 0.0061(7) -0.4151(4) 0.144 Uiso 1 calc R . H19C H 1.0734(6) -0.0505(7) -0.3374(4) 0.144 Uiso 1 calc R . C20 C 0.8576(6) -0.1021(5) -0.4195(4) 0.066(2) Uani 1 d . . H20A H 0.7702(6) -0.1111(5) -0.4256(4) 0.098 Uiso 1 calc R . H20B H 0.8994(6) -0.1542(5) -0.3919(4) 0.098 Uiso 1 calc R . H20C H 0.8803(6) -0.0976(5) -0.4696(4) 0.098 Uiso 1 calc R . C21 C 0.8280(7) 0.0708(4) -0.4184(4) 0.070(2) Uani 1 d . . H21A H 0.7405(7) 0.0623(4) -0.4247(4) 0.105 Uiso 1 calc R . H21B H 0.8510(7) 0.0754(4) -0.4684(4) 0.105 Uiso 1 calc R . H21C H 0.8512(7) 0.1272(4) -0.3897(4) 0.105 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.03250(11) 0.03705(11) 0.02900(12) -0.00618(15) 0.01001(8) -0.00327(15) C1 0.032(3) 0.036(4) 0.038(3) 0.000(3) 0.005(3) 0.001(3) B3 0.044(4) 0.037(4) 0.028(4) -0.011(3) 0.005(3) 0.007(3) B7 0.056(4) 0.035(4) 0.032(4) 0.001(3) 0.016(3) -0.002(3) B11 0.049(4) 0.045(4) 0.047(5) -0.005(4) 0.017(4) -0.014(4) B6 0.035(4) 0.054(5) 0.050(5) -0.016(4) 0.011(3) -0.011(3) B4 0.055(5) 0.050(4) 0.031(4) -0.010(4) 0.008(4) 0.004(4) B8 0.065(5) 0.047(4) 0.039(4) -0.014(4) 0.016(4) 0.002(4) B12 0.063(6) 0.036(4) 0.052(5) -0.016(4) 0.015(5) -0.009(4) B10 0.050(5) 0.068(5) 0.051(5) -0.017(4) 0.010(4) -0.016(4) B5 0.040(4) 0.063(5) 0.038(4) -0.010(4) -0.005(3) -0.009(4) B9 0.071(5) 0.061(5) 0.029(4) -0.017(4) 0.007(4) -0.011(5) C2 0.058(4) 0.046(4) 0.036(4) -0.006(3) 0.019(3) -0.008(3) O2 0.116(4) 0.068(3) 0.038(3) 0.004(3) 0.016(3) -0.014(3) C3 0.039(3) 0.056(4) 0.063(5) -0.015(4) 0.015(3) -0.006(3) O3 0.073(3) 0.086(4) 0.088(4) -0.040(3) 0.044(3) -0.001(3) N 0.029(2) 0.042(3) 0.035(3) -0.003(3) 0.006(2) 0.002(3) C4 0.036(3) 0.040(4) 0.051(4) 0.004(3) 0.006(3) 0.013(3) C5 0.083(5) 0.075(5) 0.050(5) 0.024(4) 0.015(4) 0.035(5) C6 0.043(4) 0.058(5) 0.078(5) 0.001(4) 0.008(4) 0.019(3) C7 0.062(4) 0.037(4) 0.081(5) -0.006(4) 0.006(4) 0.005(3) C8 0.029(3) 0.052(3) 0.024(3) 0.003(3) 0.001(2) -0.001(3) C9 0.033(3) 0.044(4) 0.029(3) 0.002(3) 0.013(2) -0.012(3) C10 0.038(3) 0.043(4) 0.029(3) 0.000(3) 0.008(3) -0.012(3) C11 0.065(4) 0.073(5) 0.039(4) 0.000(4) -0.004(4) -0.011(4) C12 0.087(6) 0.109(7) 0.043(5) 0.011(5) -0.007(5) -0.030(5) C13 0.097(7) 0.138(9) 0.035(5) -0.009(6) 0.010(5) -0.061(7) C14 0.090(6) 0.096(7) 0.064(6) -0.034(5) 0.039(5) -0.044(5) C15 0.060(4) 0.062(4) 0.038(4) -0.009(3) 0.015(3) -0.024(4) C16 0.030(3) 0.043(3) 0.034(3) 0.000(3) 0.008(2) 0.009(3) C17 0.036(3) 0.055(4) 0.034(4) -0.003(3) 0.005(3) 0.001(3) C18 0.041(3) 0.059(4) 0.037(4) 0.007(3) 0.015(3) 0.001(3) C19 0.048(4) 0.191(9) 0.056(5) -0.010(6) 0.030(4) -0.010(5) C20 0.089(6) 0.064(4) 0.053(5) -0.005(4) 0.038(4) 0.001(4) C21 0.109(6) 0.063(5) 0.042(4) 0.001(4) 0.024(4) 0.006(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 Re C3 1.962(6) . y Re C2 1.975(7) . y Re C1 2.147(6) . y Re N 2.250(5) . y Re C8 2.275(5) . y Re B6 2.285(7) . ? Re B11 2.341(6) . ? Re B3 2.346(6) . ? Re B7 2.379(6) . ? Re C9 2.389(5) . y C1 N 1.411(7) . y C1 B5 1.657(8) . ? C1 B4 1.682(8) . ? C1 B6 1.806(8) . ? C1 B3 1.862(8) . ? B3 C16 1.571(8) . y B3 B8 1.748(9) . ? B3 B4 1.782(9) . ? B3 B7 1.809(9) . ? B7 B12 1.768(10) . ? B7 B8 1.832(9) . ? B7 B11 1.865(9) . ? B11 B6 1.777(10) . ? B11 B10 1.824(10) . ? B11 B12 1.825(10) . ? B6 B10 1.750(10) . ? B6 B5 1.794(10) . ? B4 B9 1.780(10) . ? B4 B8 1.789(10) . ? B4 B5 1.822(10) . ? B8 B12 1.767(10) . ? B8 B9 1.775(10) . ? B12 B9 1.776(10) . ? B12 B10 1.776(11) . ? B10 B9 1.765(10) . ? B10 B5 1.770(10) . ? B5 B9 1.785(10) . ? C2 O2 1.128(7) . ? C3 O3 1.125(6) . ? N C4 1.533(7) . ? C4 C6 1.502(8) . ? C4 C7 1.510(8) . ? C4 C5 1.529(8) . ? C8 C9 1.389(7) . y C8 C16 1.519(7) . ? C9 C10 1.487(7) . ? C10 C11 1.374(8) . ? C10 C15 1.389(8) . ? C11 C12 1.384(9) . ? C12 C13 1.361(11) . ? C13 C14 1.371(11) . ? C14 C15 1.375(9) . ? C16 C17 1.340(7) . ? C17 C18 1.518(8) . ? C18 C19 1.515(8) . ? C18 C20 1.516(8) . ? C18 C21 1.528(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Re C2 84.5(3) . . ? C3 Re C1 114.2(2) . . ? C2 Re C1 150.2(2) . . ? C3 Re N 93.0(2) . . ? C2 Re N 171.9(2) . . ? C1 Re N 37.3(2) . . ? C3 Re C8 122.8(2) . . ? C2 Re C8 85.8(2) . . ? C1 Re C8 101.1(2) . . ? N Re C8 89.1(2) . . ? C3 Re B6 87.1(3) . . ? C2 Re B6 114.6(2) . . ? C1 Re B6 48.0(2) . . ? N Re B6 72.8(2) . . ? C8 Re B6 146.4(2) . . ? C3 Re B11 105.4(2) . . ? C2 Re B11 75.6(2) . . ? C1 Re B11 77.1(2) . . ? N Re B11 112.5(2) . . ? C8 Re B11 126.2(2) . . ? B6 Re B11 45.2(2) . . ? C3 Re B3 161.2(3) . . ? C2 Re B3 114.3(2) . . ? C1 Re B3 48.7(2) . . ? N Re B3 68.5(2) . . ? C8 Re B3 62.3(2) . . ? B6 Re B3 84.4(2) . . ? B11 Re B3 80.2(2) . . ? C3 Re B7 148.7(2) . . ? C2 Re B7 75.7(2) . . ? C1 Re B7 77.0(2) . . ? N Re B7 109.6(2) . . ? C8 Re B7 80.2(2) . . ? B6 Re B7 79.7(2) . . ? B11 Re B7 46.6(2) . . ? B3 Re B7 45.0(2) . . ? C3 Re C9 88.8(2) . . ? C2 Re C9 88.0(2) . . ? C1 Re C9 114.1(2) . . ? N Re C9 84.2(2) . . ? C8 Re C9 34.5(2) . . ? B6 Re C9 156.4(2) . . ? B11 Re C9 156.9(2) . . ? B3 Re C9 92.3(2) . . ? B7 Re C9 114.0(2) . . ? N C1 B5 138.3(5) . . ? N C1 B4 129.6(5) . . ? B5 C1 B4 66.1(4) . . ? N C1 B6 112.9(5) . . ? B5 C1 B6 62.2(4) . . ? B4 C1 B6 117.0(5) . . ? N C1 B3 103.6(4) . . ? B5 C1 B3 115.6(4) . . ? B4 C1 B3 60.1(3) . . ? B6 C1 B3 116.1(4) . . ? N C1 Re 75.3(3) . . ? B5 C1 Re 129.4(4) . . ? B4 C1 Re 128.7(4) . . ? B6 C1 Re 70.0(3) . . ? B3 C1 Re 71.2(3) . . ? C16 B3 B8 140.3(5) . . ? C16 B3 B4 129.3(5) . . ? B8 B3 B4 60.9(4) . . ? C16 B3 B7 121.9(5) . . ? B8 B3 B7 62.0(4) . . ? B4 B3 B7 108.6(5) . . ? C16 B3 C1 115.5(4) . . ? B8 B3 C1 100.9(4) . . ? B4 B3 C1 54.9(3) . . ? B7 B3 C1 100.5(4) . . ? C16 B3 Re 91.2(3) . . y B8 B3 Re 121.9(4) . . ? B4 B3 Re 113.0(4) . . ? B7 B3 Re 68.5(3) . . ? C1 B3 Re 60.1(2) . . ? B12 B7 B3 105.7(5) . . ? B12 B7 B8 58.8(4) . . ? B3 B7 B8 57.4(4) . . ? B12 B7 B11 60.2(4) . . ? B3 B7 B11 110.4(5) . . ? B8 B7 B11 107.8(5) . . ? B12 B7 Re 117.5(4) . . ? B3 B7 Re 66.5(3) . . ? B8 B7 Re 116.4(4) . . ? B11 B7 Re 65.7(3) . . ? B6 B11 B10 58.1(4) . . ? B6 B11 B12 105.6(5) . . ? B10 B11 B12 58.2(4) . . ? B6 B11 B7 110.3(5) . . ? B10 B11 B7 105.0(5) . . ? B12 B11 B7 57.2(4) . . ? B6 B11 Re 65.8(3) . . ? B10 B11 Re 116.1(4) . . ? B12 B11 Re 116.9(4) . . ? B7 B11 Re 67.8(3) . . ? B10 B6 B11 62.3(4) . . ? B10 B6 B5 59.9(4) . . ? B11 B6 B5 109.5(5) . . ? B10 B6 C1 100.2(5) . . ? B11 B6 C1 102.8(4) . . ? B5 B6 C1 54.8(3) . . ? B10 B6 Re 122.4(4) . . ? B11 B6 Re 69.1(3) . . ? B5 B6 Re 114.7(4) . . ? C1 B6 Re 62.0(3) . . ? C1 B4 B9 102.6(5) . . ? C1 B4 B3 64.9(4) . . ? B9 B4 B3 107.9(5) . . ? C1 B4 B8 106.6(5) . . ? B9 B4 B8 59.6(4) . . ? B3 B4 B8 58.6(4) . . ? C1 B4 B5 56.3(3) . . ? B9 B4 B5 59.4(4) . . ? B3 B4 B5 111.6(5) . . ? B8 B4 B5 107.9(5) . . ? B3 B8 B12 108.4(5) . . ? B3 B8 B9 109.7(5) . . ? B12 B8 B9 60.2(4) . . ? B3 B8 B4 60.5(4) . . ? B12 B8 B4 107.1(5) . . ? B9 B8 B4 59.9(4) . . ? B3 B8 B7 60.7(4) . . ? B12 B8 B7 58.8(4) . . ? B9 B8 B7 107.6(5) . . ? B4 B8 B7 107.3(5) . . ? B8 B12 B7 62.4(4) . . ? B8 B12 B9 60.1(4) . . ? B7 B12 B9 110.4(5) . . ? B8 B12 B10 109.6(5) . . ? B7 B12 B10 111.3(5) . . ? B9 B12 B10 59.6(4) . . ? B8 B12 B11 112.5(5) . . ? B7 B12 B11 62.5(4) . . ? B9 B12 B11 109.4(5) . . ? B10 B12 B11 60.9(4) . . ? B6 B10 B9 110.9(5) . . ? B6 B10 B5 61.3(4) . . ? B9 B10 B5 60.7(4) . . ? B6 B10 B12 109.0(5) . . ? B9 B10 B12 60.2(4) . . ? B5 B10 B12 108.1(5) . . ? B6 B10 B11 59.6(4) . . ? B9 B10 B11 109.9(5) . . ? B5 B10 B11 108.4(5) . . ? B12 B10 B11 60.9(4) . . ? C1 B5 B10 105.5(5) . . ? C1 B5 B9 103.4(5) . . ? B10 B5 B9 59.5(4) . . ? C1 B5 B6 63.0(4) . . ? B10 B5 B6 58.8(4) . . ? B9 B5 B6 107.9(5) . . ? C1 B5 B4 57.6(3) . . ? B10 B5 B4 107.2(5) . . ? B9 B5 B4 59.1(4) . . ? B6 B5 B4 110.7(5) . . ? B10 B9 B8 109.7(5) . . ? B10 B9 B12 60.2(4) . . ? B8 B9 B12 59.7(4) . . ? B10 B9 B4 109.2(5) . . ? B8 B9 B4 60.4(4) . . ? B12 B9 B4 107.1(5) . . ? B10 B9 B5 59.8(4) . . ? B8 B9 B5 110.2(5) . . ? B12 B9 B5 107.4(5) . . ? B4 B9 B5 61.5(4) . . ? O2 C2 Re 179.2(6) . . ? O3 C3 Re 177.4(6) . . ? C1 N C4 127.2(4) . . ? C1 N Re 67.4(3) . . y C4 N Re 136.5(4) . . ? C6 C4 C7 110.7(6) . . ? C6 C4 C5 111.7(5) . . ? C7 C4 C5 110.3(6) . . ? C6 C4 N 113.4(5) . . ? C7 C4 N 105.3(5) . . ? C5 C4 N 105.0(5) . . ? C9 C8 C16 127.1(5) . . ? C9 C8 Re 77.2(3) . . ? C16 C8 Re 95.3(3) . . y C8 C9 C10 125.4(5) . . ? C8 C9 Re 68.2(3) . . ? C10 C9 Re 117.5(3) . . ? C11 C10 C15 118.0(6) . . ? C11 C10 C9 123.6(6) . . ? C15 C10 C9 118.4(5) . . ? C10 C11 C12 120.9(7) . . ? C13 C12 C11 120.1(8) . . ? C12 C13 C14 120.0(8) . . ? C13 C14 C15 120.0(8) . . ? C14 C15 C10 120.9(7) . . ? C17 C16 C8 118.8(5) . . ? C17 C16 B3 139.6(5) . . ? C8 C16 B3 101.5(4) . . y C16 C17 C18 132.5(5) . . ? C19 C18 C20 109.5(6) . . ? C19 C18 C17 107.5(5) . . ? C20 C18 C17 112.6(5) . . ? C19 C18 C21 109.0(6) . . ? C20 C18 C21 109.9(5) . . ? C17 C18 C21 108.3(5) . . ? _refine_diff_density_max .798 _refine_diff_density_min -.581 _refine_diff_density_rms .136 #============================================================================== data_9 _database_code_depnum_ccdc_archive 'CCDC 278689' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H39 B10 N2 O Re' _chemical_formula_weight 629.84 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 Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.6011(9) _cell_length_b 11.5856(10) _cell_length_c 22.6485(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2781.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6853 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 32.71 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 4.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4594 _exptl_absorpt_correction_T_max 0.6487 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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-Nonius X-8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27494 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 32.84 _reflns_number_total 9889 _reflns_number_gt 9177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.042(11) _refine_ls_number_reflns 9889 _refine_ls_number_parameters 322 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Re Re 0.690877(15) 0.524465(14) 0.048009(7) 0.01364(5) Uani 1 1 d . . . C1 C 0.7504(4) 0.5460(4) -0.0437(2) 0.0170(8) Uani 1 1 d . . . B3 B 0.6756(5) 0.6745(4) -0.0210(2) 0.0167(9) Uani 1 1 d . . . H3 H 0.7188 0.7542 -0.0017 0.020 Uiso 1 1 calc R . . B4 B 0.6995(6) 0.6394(5) -0.0968(2) 0.0199(9) Uani 1 1 d . . . H4 H 0.7630 0.6937 -0.1249 0.024 Uiso 1 1 calc R . . B5 B 0.6915(6) 0.4852(5) -0.1063(2) 0.0185(9) Uani 1 1 d . . . H5 H 0.7498 0.4397 -0.1403 0.022 Uiso 1 1 calc R . . B6 B 0.6582(5) 0.4179(5) -0.0363(2) 0.0175(9) Uani 1 1 d . . . H6 H 0.6897 0.3273 -0.0274 0.021 Uiso 1 1 calc R . . B7 B 0.5231(5) 0.6287(5) 0.0009(2) 0.0182(9) Uani 1 1 d . . . H7 H 0.4664 0.6767 0.0347 0.022 Uiso 1 1 calc R . . B8 B 0.5501(5) 0.6876(5) -0.0718(3) 0.0203(10) Uani 1 1 d . . . H8 H 0.5116 0.7739 -0.0849 0.024 Uiso 1 1 calc R . . B9 B 0.5590(5) 0.5752(5) -0.1239(2) 0.0208(10) Uani 1 1 d . . . H9 H 0.5277 0.5879 -0.1706 0.025 Uiso 1 1 calc R . . B10 B 0.5339(6) 0.4411(5) -0.0864(3) 0.0203(11) Uani 1 1 d . . . H10 H 0.4856 0.3673 -0.1090 0.024 Uiso 1 1 calc R . . B11 B 0.5111(5) 0.4696(6) -0.0086(2) 0.0189(9) Uani 1 1 d . . . H11 H 0.4458 0.4157 0.0188 0.023 Uiso 1 1 calc R . . B12 B 0.4503(5) 0.5667(5) -0.0630(2) 0.0195(10) Uani 1 1 d . . . H12 H 0.3458 0.5741 -0.0693 0.023 Uiso 1 1 calc R . . N1 N 0.8670(4) 0.5438(3) -0.01103(18) 0.0163(7) Uani 1 1 d D . . H100 H 0.904(5) 0.614(3) -0.008(3) 0.020 Uiso 1 1 d D . . C11 C 0.9828(4) 0.4739(5) -0.0288(2) 0.0197(8) Uani 1 1 d . . . C12 C 1.0784(5) 0.4893(5) 0.0209(2) 0.0266(10) Uani 1 1 d . . . H12A H 1.0968 0.5715 0.0260 0.040 Uiso 1 1 calc R . . H12B H 1.1563 0.4481 0.0109 0.040 Uiso 1 1 calc R . . H12C H 1.0436 0.4580 0.0576 0.040 Uiso 1 1 calc R . . C13 C 1.0338(5) 0.5288(7) -0.0860(3) 0.0334(13) Uani 1 1 d . . . H13A H 0.9716 0.5194 -0.1177 0.050 Uiso 1 1 calc R . . H13B H 1.1127 0.4906 -0.0973 0.050 Uiso 1 1 calc R . . H13C H 1.0495 0.6111 -0.0794 0.050 Uiso 1 1 calc R . . C14 C 0.9547(5) 0.3464(5) -0.0370(3) 0.0296(12) Uani 1 1 d . . . H14A H 0.8935 0.3366 -0.0691 0.044 Uiso 1 1 calc R . . H14B H 0.9197 0.3148 -0.0004 0.044 Uiso 1 1 calc R . . H14C H 1.0328 0.3055 -0.0470 0.044 Uiso 1 1 calc R . . C21 C 0.7233(5) 0.3669(4) 0.0755(2) 0.0196(9) Uani 1 1 d . . . O21 O 0.7363(4) 0.2727(4) 0.08940(19) 0.0298(9) Uani 1 1 d . . . C31 C 0.7655(5) 0.6593(5) 0.1013(2) 0.0202(9) Uani 1 1 d . . . H31 H 0.750(6) 0.742(6) 0.110(3) 0.024 Uiso 1 1 d . . . C32 C 0.7948(5) 0.5699(5) 0.1303(2) 0.0207(9) Uani 1 1 d . . . C33 C 0.8472(5) 0.5171(6) 0.1868(2) 0.0234(9) Uani 1 1 d . . . C34 C 0.9493(6) 0.4280(7) 0.1751(3) 0.0346(13) Uani 1 1 d . . . H34A H 0.9798 0.3968 0.2127 0.052 Uiso 1 1 calc R . . H34B H 1.0195 0.4644 0.1540 0.052 Uiso 1 1 calc R . . H34C H 0.9146 0.3652 0.1511 0.052 Uiso 1 1 calc R . . C35 C 0.9027(6) 0.6189(6) 0.2225(3) 0.0323(13) Uani 1 1 d . . . H35A H 0.8362 0.6756 0.2304 0.048 Uiso 1 1 calc R . . H35B H 0.9703 0.6555 0.1996 0.048 Uiso 1 1 calc R . . H35C H 0.9368 0.5902 0.2599 0.048 Uiso 1 1 calc R . . C36 C 0.7389(6) 0.4631(6) 0.2219(2) 0.0272(11) Uani 1 1 d . . . H36A H 0.6738 0.5215 0.2291 0.041 Uiso 1 1 calc R . . H36B H 0.7709 0.4342 0.2597 0.041 Uiso 1 1 calc R . . H36C H 0.7026 0.3991 0.1993 0.041 Uiso 1 1 calc R . . C41 C 0.5479(4) 0.5283(5) 0.1064(2) 0.0190(8) Uani 1 1 d . . . N41 N 0.4708(4) 0.5296(5) 0.14335(19) 0.0234(8) Uani 1 1 d . . . C42 C 0.3910(4) 0.5352(5) 0.1928(2) 0.0204(9) Uani 1 1 d . . . C43 C 0.4007(5) 0.6334(5) 0.2287(2) 0.0216(9) Uani 1 1 d . . . C44 C 0.4880(6) 0.7316(5) 0.2135(3) 0.0298(12) Uani 1 1 d . . . H44A H 0.4816 0.7917 0.2438 0.045 Uiso 1 1 calc R . . H44B H 0.4642 0.7639 0.1750 0.045 Uiso 1 1 calc R . . H44C H 0.5750 0.7032 0.2117 0.045 Uiso 1 1 calc R . . C45 C 0.3249(6) 0.6346(5) 0.2795(2) 0.0264(10) Uani 1 1 d . . . H45 H 0.3284 0.6990 0.3054 0.032 Uiso 1 1 calc R . . C46 C 0.2451(5) 0.5434(5) 0.2924(2) 0.0257(11) Uani 1 1 d . . . H46 H 0.1947 0.5460 0.3271 0.031 Uiso 1 1 calc R . . C47 C 0.2379(5) 0.4483(5) 0.2555(2) 0.0239(10) Uani 1 1 d . . . H47 H 0.1830 0.3864 0.2652 0.029 Uiso 1 1 calc R . . C48 C 0.3111(5) 0.4425(5) 0.2037(2) 0.0223(9) Uani 1 1 d . . . C49 C 0.3034(6) 0.3422(5) 0.1620(3) 0.0327(12) Uani 1 1 d . . . H49A H 0.2422 0.2860 0.1769 0.049 Uiso 1 1 calc R . . H49B H 0.3865 0.3057 0.1587 0.049 Uiso 1 1 calc R . . H49C H 0.2765 0.3696 0.1230 0.049 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 Re 0.01504(7) 0.01359(7) 0.01227(7) -0.00067(6) 0.00083(6) -0.00031(6) C1 0.0151(18) 0.019(2) 0.0163(18) -0.0005(16) -0.0005(15) 0.0003(14) B3 0.018(2) 0.0129(19) 0.019(2) 0.0005(17) -0.0004(18) 0.0003(18) B4 0.023(2) 0.020(2) 0.016(2) 0.0037(17) -0.002(2) 0.001(2) B5 0.026(2) 0.016(2) 0.0138(18) -0.0052(17) 0.0014(18) 0.000(2) B6 0.021(2) 0.014(2) 0.018(2) -0.0022(17) -0.0002(16) 0.0021(18) B7 0.017(2) 0.016(2) 0.022(2) -0.0006(19) 0.0001(18) 0.0009(19) B8 0.021(2) 0.018(2) 0.022(2) 0.001(2) -0.0029(19) 0.002(2) B9 0.023(2) 0.023(2) 0.017(2) 0.001(2) -0.0032(18) 0.002(2) B10 0.022(2) 0.018(2) 0.021(2) -0.003(2) -0.0030(19) -0.002(2) B11 0.020(2) 0.018(2) 0.019(2) -0.001(2) -0.0003(17) 0.000(2) B12 0.019(2) 0.020(2) 0.020(2) -0.0002(19) -0.0008(17) 0.001(2) N1 0.0178(17) 0.0140(18) 0.0171(16) -0.0019(13) 0.0009(13) -0.0008(14) C11 0.0167(18) 0.022(2) 0.0203(19) -0.001(2) 0.0032(15) 0.007(2) C12 0.022(2) 0.030(3) 0.028(2) -0.006(2) -0.0055(19) 0.004(2) C13 0.026(2) 0.047(4) 0.027(2) 0.006(3) 0.010(2) 0.002(3) C14 0.023(2) 0.022(2) 0.044(3) -0.012(2) 0.004(2) 0.005(2) C21 0.028(2) 0.0123(18) 0.019(2) 0.0013(16) -0.0007(16) -0.0019(17) O21 0.038(2) 0.0237(19) 0.028(2) 0.0055(16) -0.0067(16) -0.0044(17) C31 0.022(2) 0.019(2) 0.020(2) -0.0040(17) 0.0020(17) -0.0039(18) C32 0.020(2) 0.023(2) 0.0191(19) -0.0049(17) -0.0028(16) -0.0034(19) C33 0.025(2) 0.029(2) 0.0163(19) -0.002(2) -0.0005(16) -0.001(2) C34 0.032(3) 0.046(4) 0.026(3) -0.004(3) -0.007(2) 0.009(3) C35 0.041(3) 0.030(3) 0.026(3) -0.006(2) -0.008(2) -0.009(3) C36 0.033(3) 0.029(3) 0.019(2) 0.007(2) -0.0003(18) -0.002(2) C41 0.0186(19) 0.020(2) 0.0181(18) -0.0028(19) -0.0020(15) 0.0025(19) N41 0.0185(16) 0.033(2) 0.0183(17) -0.003(2) 0.0011(14) -0.0005(19) C42 0.0178(19) 0.028(3) 0.0149(18) -0.0031(18) 0.0021(14) 0.0020(19) C43 0.024(2) 0.022(2) 0.019(2) -0.0007(18) 0.0000(17) 0.0036(19) C44 0.033(3) 0.027(3) 0.029(3) 0.001(2) 0.003(2) -0.003(2) C45 0.033(3) 0.028(2) 0.018(2) -0.0012(19) 0.0042(19) 0.005(2) C46 0.023(2) 0.033(3) 0.021(2) 0.004(2) 0.0058(18) 0.006(2) C47 0.019(2) 0.029(3) 0.023(2) 0.0032(19) 0.0033(17) -0.0007(18) C48 0.021(2) 0.025(2) 0.0204(19) -0.0014(17) 0.0005(19) -0.001(2) C49 0.035(3) 0.032(3) 0.031(3) -0.009(2) 0.006(2) -0.007(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 Re C21 1.959(5) . ? Re C41 2.012(5) . ? Re C31 2.126(5) . ? Re C1 2.185(5) . ? Re C32 2.228(5) . ? Re B6 2.300(5) . ? Re N1 2.307(4) . ? Re B3 2.343(5) . ? Re B11 2.384(5) . ? Re B7 2.400(5) . ? C1 N1 1.440(6) . ? C1 B5 1.701(7) . ? C1 B4 1.705(7) . ? C1 B3 1.763(7) . ? C1 B6 1.785(7) . ? B3 B8 1.766(8) . ? B3 B7 1.773(7) . ? B3 B4 1.782(7) . ? B4 B8 1.772(8) . ? B4 B9 1.774(8) . ? B4 B5 1.801(7) . ? B5 B9 1.793(8) . ? B5 B6 1.801(7) . ? B5 B10 1.804(8) . ? B6 B10 1.761(8) . ? B6 B11 1.784(7) . ? B7 B12 1.792(8) . ? B7 B8 1.806(8) . ? B7 B11 1.860(9) . ? B8 B9 1.760(8) . ? B8 B12 1.767(8) . ? B9 B10 1.790(9) . ? B9 B12 1.799(8) . ? B10 B12 1.784(8) . ? B10 B11 1.809(8) . ? B11 B12 1.788(8) . ? N1 H100 0.90(2) . ? N1 C11 1.525(6) . ? C11 C14 1.518(8) . ? C11 C12 1.524(7) . ? C11 C13 1.541(8) . ? C21 O21 1.144(6) . ? C31 H31 1.00(7) . ? C31 C32 1.266(7) . ? C32 C33 1.524(7) . ? C33 C34 1.520(9) . ? C33 C36 1.530(8) . ? C33 C35 1.545(8) . ? C41 N41 1.171(6) . ? N41 C42 1.405(6) . ? C42 C48 1.390(8) . ? C42 C43 1.401(7) . ? C43 C45 1.404(7) . ? C43 C44 1.507(8) . ? C45 C46 1.386(8) . ? C46 C47 1.384(8) . ? C47 C48 1.409(7) . ? C48 C49 1.500(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Re C41 86.8(2) . . ? C21 Re C31 116.0(2) . . ? C41 Re C31 83.8(2) . . ? C21 Re C1 110.97(19) . . ? C41 Re C1 147.11(17) . . ? C31 Re C1 110.36(18) . . ? C21 Re C32 82.4(2) . . ? C41 Re C32 79.49(18) . . ? C31 Re C32 33.7(2) . . ? C1 Re C32 128.72(18) . . ? C21 Re B6 77.9(2) . . ? C41 Re B6 116.36(19) . . ? C31 Re B6 157.13(19) . . ? C1 Re B6 46.81(19) . . ? C32 Re B6 153.59(19) . . ? C21 Re N1 97.65(18) . . ? C41 Re N1 171.23(18) . . ? C31 Re N1 87.49(17) . . ? C1 Re N1 37.28(15) . . ? C32 Re N1 93.54(16) . . ? B6 Re N1 72.12(16) . . ? C21 Re B3 156.27(19) . . ? C41 Re B3 111.7(2) . . ? C31 Re B3 81.9(2) . . ? C1 Re B3 45.68(18) . . ? C32 Re B3 114.64(19) . . ? B6 Re B3 80.46(19) . . ? N1 Re B3 66.24(16) . . ? C21 Re B11 93.6(2) . . ? C41 Re B11 75.94(18) . . ? C31 Re B11 143.0(2) . . ? C1 Re B11 75.51(17) . . ? C32 Re B11 155.30(18) . . ? B6 Re B11 44.74(19) . . ? N1 Re B11 111.16(17) . . ? B3 Re B11 77.5(2) . . ? C21 Re B7 137.7(2) . . ? C41 Re B7 73.87(19) . . ? C31 Re B7 99.1(2) . . ? C1 Re B7 74.60(17) . . ? C32 Re B7 128.28(19) . . ? B6 Re B7 77.86(19) . . ? N1 Re B7 107.06(17) . . ? B3 Re B7 43.89(19) . . ? B11 Re B7 45.8(2) . . ? N1 C1 B5 137.4(4) . . ? N1 C1 B4 130.1(4) . . ? B5 C1 B4 63.8(3) . . ? N1 C1 B3 104.5(4) . . ? B5 C1 B3 115.3(4) . . ? B4 C1 B3 61.8(3) . . ? N1 C1 B6 114.1(4) . . ? B5 C1 B6 62.2(3) . . ? B4 C1 B6 114.9(4) . . ? B3 C1 B6 115.4(3) . . ? N1 C1 Re 76.0(2) . . ? B5 C1 Re 129.7(3) . . ? B4 C1 Re 130.6(3) . . ? B3 C1 Re 71.9(2) . . ? B6 C1 Re 70.0(2) . . ? C1 B3 B8 102.8(4) . . ? C1 B3 B7 103.8(4) . . ? B8 B3 B7 61.4(3) . . ? C1 B3 B4 57.5(3) . . ? B8 B3 B4 59.9(3) . . ? B7 B3 B4 109.3(4) . . ? C1 B3 Re 62.4(2) . . ? B8 B3 Re 123.4(3) . . ? B7 B3 Re 69.8(2) . . ? B4 B3 Re 117.6(3) . . ? C1 B4 B8 105.0(4) . . ? C1 B4 B9 104.1(4) . . ? B8 B4 B9 59.5(3) . . ? C1 B4 B3 60.7(3) . . ? B8 B4 B3 59.6(3) . . ? B9 B4 B3 108.1(4) . . ? C1 B4 B5 58.0(3) . . ? B8 B4 B5 108.0(4) . . ? B9 B4 B5 60.2(3) . . ? B3 B4 B5 109.5(4) . . ? C1 B5 B9 103.4(3) . . ? C1 B5 B6 61.2(3) . . ? B9 B5 B6 107.1(4) . . ? C1 B5 B4 58.2(3) . . ? B9 B5 B4 59.1(3) . . ? B6 B5 B4 109.5(3) . . ? C1 B5 B10 104.5(4) . . ? B9 B5 B10 59.7(3) . . ? B6 B5 B10 58.5(3) . . ? B4 B5 B10 107.2(4) . . ? B10 B6 B11 61.4(3) . . ? B10 B6 C1 102.9(4) . . ? B11 B6 C1 103.4(4) . . ? B10 B6 B5 60.8(3) . . ? B11 B6 B5 109.5(4) . . ? C1 B6 B5 56.7(3) . . ? B10 B6 Re 124.5(3) . . ? B11 B6 Re 70.1(2) . . ? C1 B6 Re 63.2(2) . . ? B5 B6 Re 117.9(3) . . ? B3 B7 B12 106.6(4) . . ? B3 B7 B8 59.1(3) . . ? B12 B7 B8 58.8(3) . . ? B3 B7 B11 109.0(4) . . ? B12 B7 B11 58.6(3) . . ? B8 B7 B11 106.2(4) . . ? B3 B7 Re 66.3(2) . . ? B12 B7 Re 118.5(3) . . ? B8 B7 Re 118.5(3) . . ? B11 B7 Re 66.7(2) . . ? B9 B8 B3 109.4(4) . . ? B9 B8 B12 61.3(3) . . ? B3 B8 B12 108.0(4) . . ? B9 B8 B4 60.3(3) . . ? B3 B8 B4 60.5(3) . . ? B12 B8 B4 108.7(4) . . ? B9 B8 B7 109.9(4) . . ? B3 B8 B7 59.5(3) . . ? B12 B8 B7 60.2(3) . . ? B4 B8 B7 108.3(4) . . ? B8 B9 B4 60.2(3) . . ? B8 B9 B10 108.5(4) . . ? B4 B9 B10 109.0(4) . . ? B8 B9 B5 108.9(4) . . ? B4 B9 B5 60.6(3) . . ? B10 B9 B5 60.4(3) . . ? B8 B9 B12 59.5(3) . . ? B4 B9 B12 107.2(4) . . ? B10 B9 B12 59.6(3) . . ? B5 B9 B12 107.4(4) . . ? B6 B10 B12 107.7(4) . . ? B6 B10 B9 109.1(4) . . ? B12 B10 B9 60.5(3) . . ? B6 B10 B5 60.7(3) . . ? B12 B10 B5 107.6(4) . . ? B9 B10 B5 59.9(3) . . ? B6 B10 B11 60.0(3) . . ? B12 B10 B11 59.7(3) . . ? B9 B10 B11 108.8(4) . . ? B5 B10 B11 108.3(4) . . ? B6 B11 B12 106.5(4) . . ? B6 B11 B10 58.7(3) . . ? B12 B11 B10 59.5(3) . . ? B6 B11 B7 108.3(4) . . ? B12 B11 B7 58.8(3) . . ? B10 B11 B7 106.6(4) . . ? B6 B11 Re 65.1(2) . . ? B12 B11 Re 119.4(4) . . ? B10 B11 Re 117.8(3) . . ? B7 B11 Re 67.6(2) . . ? B8 B12 B10 108.4(4) . . ? B8 B12 B11 111.1(4) . . ? B10 B12 B11 60.8(3) . . ? B8 B12 B7 61.0(3) . . ? B10 B12 B7 110.7(4) . . ? B11 B12 B7 62.6(3) . . ? B8 B12 B9 59.1(3) . . ? B10 B12 B9 59.9(3) . . ? B11 B12 B9 109.4(4) . . ? B7 B12 B9 108.8(4) . . ? H100 N1 C1 114(4) . . ? H100 N1 C11 99(4) . . ? C1 N1 C11 124.4(4) . . ? H100 N1 Re 113(4) . . ? C1 N1 Re 66.7(2) . . ? C11 N1 Re 138.8(3) . . ? C14 C11 C12 109.5(5) . . ? C14 C11 N1 113.1(4) . . ? C12 C11 N1 106.2(4) . . ? C14 C11 C13 111.5(5) . . ? C12 C11 C13 109.8(4) . . ? N1 C11 C13 106.6(4) . . ? O21 C21 Re 175.8(5) . . ? H31 C31 C32 137(4) . . ? H31 C31 Re 139(4) . . ? C32 C31 Re 77.6(3) . . ? C31 C32 C33 148.7(5) . . ? C31 C32 Re 68.7(3) . . ? C33 C32 Re 142.1(4) . . ? C34 C33 C32 112.7(4) . . ? C34 C33 C36 110.4(6) . . ? C32 C33 C36 109.0(4) . . ? C34 C33 C35 109.8(5) . . ? C32 C33 C35 105.8(5) . . ? C36 C33 C35 109.1(5) . . ? N41 C41 Re 175.3(4) . . ? C41 N41 C42 172.5(5) . . ? C48 C42 C43 124.7(4) . . ? C48 C42 N41 118.2(5) . . ? C43 C42 N41 117.1(5) . . ? C42 C43 C45 116.2(5) . . ? C42 C43 C44 121.7(5) . . ? C45 C43 C44 122.1(5) . . ? C46 C45 C43 121.0(5) . . ? C47 C46 C45 120.8(5) . . ? C46 C47 C48 120.7(5) . . ? C42 C48 C47 116.5(5) . . ? C42 C48 C49 121.3(5) . . ? C47 C48 C49 122.2(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.658 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.155 #===END