Electronic Supplementary Material for Chemical Communications This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #============================================================================== # 0. AUDIT DETAILS _audit_creation_date ' 2006' _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 Chemical Communications: Carbonyl-metal fragment insertion into eight-vertex [closo-1-CB~7~H~8~]^-^. Facile synthesis of ten-vertex metalladicarbollide complexes [2,2,2-(CO)~3~- 1-OH-closo-2,1,10-MC~2~B~7~H~8~]^n-^ {M= Fe, Ru (n = 0), Mn, Re (n = 1)} Date of submission: 31 May 2006 With thanks, Prof. F. Gordon A. Stone ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Carbonyl-metal fragment insertion into eight-vertex [closo-1-CB~7~H~8~]^-^. Facile synthesis of ten-vertex metalladicarbollide complexes [2,2,2-(CO)~3~- 1-OH-closo-2,1,10-MC~2~B~7~H~8~]^n-^ {M= Fe, Ru (n = 0), Mn, Re (n = 1)} ; loop_ _publ_author_name _publ_author_address A.Franken ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; P.Lei ; 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 ; X-ray intensity 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, 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. All structures were solved using conventional direct methods (Bruker, 2003) and refined by full-matrix least-squares on all F^2^ data using SHELXL-97 (Bruker, 2001). 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. All non-hydrogen atoms were assigned anisotropic displacement parameters. All B-H and C-H hydrogen atoms were included in calculated positions and allowed to ride on their parent atoms, apart from those in the anions of 5 and 6 which were allowed positional refinement. The OH hydrogens in 3b, 4 and 6 were refined using a "rotating model" (AFIX 147 in SHELXL (Bruker, 2001), but that in 5 was successfully allowed positional refinement. All hydrogen atoms had fixed isotropic thermal parameters, calculated as U~iso~(H) = 1.2 x U~iso~(parent). Note that the two crystallographically independent molecules of 3b form hydrogen bonded pairs, whilst the three independent molecules of 4 form hydrogen bonded helices that extend along the crystallographic a axis ; _publ_section_references ; 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. 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_3b _database_code_depnum_ccdc_archive 'CCDC 609673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 B7 Fe O3 P' _chemical_formula_weight 354.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 19.121(11) _cell_length_b 9.018(5) _cell_length_c 20.973(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.516(18) _cell_angle_gamma 90.00 _cell_volume 3516(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4854 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.938 _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 X8 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 46927 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.66 _reflns_number_total 8146 _reflns_number_gt 5898 _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^)+(0.0539P)^2^+0.4891P] 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 8146 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.0973 _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 Fe1 Fe 0.55880(2) 0.19221(4) 0.180955(17) 0.01559(10) Uani 1 1 d . . . C1 C 0.50381(14) 0.2428(3) 0.09215(12) 0.0175(6) Uani 1 1 d . . . O1 O 0.43170(10) 0.2062(2) 0.06863(10) 0.0225(4) Uani 1 1 d . . . H1 H 0.4076 0.2839 0.0577 0.027 Uiso 1 1 calc R . . B3 B 0.53568(17) 0.3999(3) 0.12518(15) 0.0197(7) Uani 1 1 d . . . H3 H 0.4996 0.4871 0.1381 0.024 Uiso 1 1 calc R . . B4 B 0.54415(18) 0.3295(3) 0.04344(15) 0.0204(7) Uani 1 1 d . . . H4 H 0.5148 0.3604 -0.0075 0.024 Uiso 1 1 calc R . . B5 B 0.57109(17) 0.1449(4) 0.08105(14) 0.0182(6) Uani 1 1 d . . . H5 H 0.5631 0.0311 0.0592 0.022 Uiso 1 1 calc R . . B6 B 0.62675(17) 0.3822(4) 0.17389(15) 0.0207(7) Uani 1 1 d . . . H6 H 0.6445 0.4446 0.2211 0.025 Uiso 1 1 calc R . . B7 B 0.61109(18) 0.4512(4) 0.08911(15) 0.0211(7) Uani 1 1 d . . . H7 H 0.6165 0.5664 0.0709 0.025 Uiso 1 1 calc R . . B8 B 0.63632(18) 0.2741(4) 0.05944(16) 0.0224(7) Uani 1 1 d . . . H8 H 0.6620 0.2495 0.0178 0.027 Uiso 1 1 calc R . . B9 B 0.65398(17) 0.1901(4) 0.14055(15) 0.0197(7) Uani 1 1 d . . . H9 H 0.6933 0.1006 0.1614 0.024 Uiso 1 1 calc R . . C10 C 0.67885(15) 0.3538(3) 0.12493(14) 0.0225(6) Uani 1 1 d . . . H10 H 0.7365 0.3900 0.1364 0.027 Uiso 1 1 calc R . . C21 C 0.48786(16) 0.2436(3) 0.21897(13) 0.0224(6) Uani 1 1 d . . . O21 O 0.44349(12) 0.2822(2) 0.24366(11) 0.0360(6) Uani 1 1 d . . . C22 C 0.62358(16) 0.1759(3) 0.25607(14) 0.0265(7) Uani 1 1 d . . . O22 O 0.66620(13) 0.1710(3) 0.30460(10) 0.0417(6) Uani 1 1 d . . . P1 P 0.53158(4) -0.04867(8) 0.18733(3) 0.01477(15) Uani 1 1 d . . . C23 C 0.51642(15) -0.1011(3) 0.26758(13) 0.0221(6) Uani 1 1 d . . . H23A H 0.5597 -0.0742 0.3018 0.027 Uiso 1 1 calc R . . H23B H 0.4757 -0.0421 0.2757 0.027 Uiso 1 1 calc R . . C24 C 0.50022(17) -0.2658(3) 0.27500(14) 0.0288(7) Uani 1 1 d . . . H24A H 0.4927 -0.2837 0.3190 0.043 Uiso 1 1 calc R . . H24B H 0.5408 -0.3255 0.2686 0.043 Uiso 1 1 calc R . . H24C H 0.4567 -0.2934 0.2421 0.043 Uiso 1 1 calc R . . C25 C 0.45043(14) -0.1135(3) 0.12888(12) 0.0184(6) Uani 1 1 d . . . H25A H 0.4511 -0.0757 0.0847 0.022 Uiso 1 1 calc R . . H25B H 0.4515 -0.2232 0.1271 0.022 Uiso 1 1 calc R . . C26 C 0.38039(15) -0.0649(3) 0.14579(14) 0.0233(6) Uani 1 1 d . . . H26A H 0.3394 -0.1033 0.1127 0.035 Uiso 1 1 calc R . . H26B H 0.3782 0.0437 0.1464 0.035 Uiso 1 1 calc R . . H26C H 0.3787 -0.1037 0.1890 0.035 Uiso 1 1 calc R . . C27 C 0.59964(15) -0.1801(3) 0.17469(14) 0.0228(6) Uani 1 1 d . . . H27A H 0.5783 -0.2807 0.1709 0.027 Uiso 1 1 calc R . . H27B H 0.6114 -0.1569 0.1323 0.027 Uiso 1 1 calc R . . C28 C 0.66974(16) -0.1841(4) 0.22753(17) 0.0369(8) Uani 1 1 d . . . H28A H 0.7022 -0.2579 0.2158 0.055 Uiso 1 1 calc R . . H28B H 0.6594 -0.2108 0.2697 0.055 Uiso 1 1 calc R . . H28C H 0.6926 -0.0862 0.2310 0.055 Uiso 1 1 calc R . . Fe1A Fe 0.17056(2) 0.40488(4) 0.055963(17) 0.01478(10) Uani 1 1 d . . . C1A C 0.27298(14) 0.4619(3) 0.07693(12) 0.0150(5) Uani 1 1 d . . . O1A O 0.32054(10) 0.4303(2) 0.03640(9) 0.0198(4) Uani 1 1 d . . . H1A H 0.3329 0.5098 0.0213 0.024 Uiso 1 1 calc R . . B3A B 0.22903(17) 0.6149(3) 0.07883(15) 0.0191(7) Uani 1 1 d . . . H3A H 0.2263 0.7029 0.0406 0.023 Uiso 1 1 calc R . . B4A B 0.30654(18) 0.5495(3) 0.14399(15) 0.0193(7) Uani 1 1 d . . . H4A H 0.3643 0.5849 0.1570 0.023 Uiso 1 1 calc R . . B5A B 0.26471(16) 0.3615(4) 0.13779(14) 0.0164(6) Uani 1 1 d . . . H5A H 0.2900 0.2490 0.1465 0.020 Uiso 1 1 calc R . . B6A B 0.15391(18) 0.5905(4) 0.11700(16) 0.0210(7) Uani 1 1 d . . . H6A H 0.1017 0.6495 0.0978 0.025 Uiso 1 1 calc R . . B7A B 0.23978(18) 0.6652(4) 0.16531(15) 0.0220(7) Uani 1 1 d . . . H7A H 0.2535 0.7812 0.1829 0.026 Uiso 1 1 calc R . . B8A B 0.26444(19) 0.4886(4) 0.20681(15) 0.0225(7) Uani 1 1 d . . . H8A H 0.2976 0.4654 0.2573 0.027 Uiso 1 1 calc R . . B9A B 0.18125(17) 0.3980(4) 0.16193(15) 0.0203(7) Uani 1 1 d . . . H9A H 0.1507 0.3049 0.1781 0.024 Uiso 1 1 calc R . . C10A C 0.18637(16) 0.5617(3) 0.19396(13) 0.0225(6) Uani 1 1 d . . . H10A H 0.1572 0.5937 0.2324 0.027 Uiso 1 1 calc R . . C21A C 0.07776(15) 0.3820(3) 0.05493(13) 0.0219(6) Uani 1 1 d . . . O21A O 0.01782(11) 0.3720(2) 0.05452(11) 0.0317(5) Uani 1 1 d . . . C22A C 0.15485(15) 0.4642(3) -0.02701(13) 0.0227(6) Uani 1 1 d . . . O22A O 0.14602(13) 0.5123(3) -0.07897(10) 0.0368(6) Uani 1 1 d . . . P1A P 0.17670(4) 0.16629(8) 0.02670(3) 0.01587(15) Uani 1 1 d . . . C23A C 0.10504(16) 0.1137(4) -0.04446(15) 0.0300(7) Uani 1 1 d . . . H23C H 0.0580 0.1356 -0.0344 0.036 Uiso 1 1 calc R . . H23D H 0.1091 0.1765 -0.0821 0.036 Uiso 1 1 calc R . . C24A C 0.10563(19) -0.0491(4) -0.06496(17) 0.0412(9) Uani 1 1 d . . . H24D H 0.0659 -0.0672 -0.1031 0.062 Uiso 1 1 calc R . . H24E H 0.1000 -0.1127 -0.0286 0.062 Uiso 1 1 calc R . . H24F H 0.1514 -0.0717 -0.0763 0.062 Uiso 1 1 calc R . . C25A C 0.16996(15) 0.0306(3) 0.09001(14) 0.0210(6) Uani 1 1 d . . . H25C H 0.1831 -0.0681 0.0758 0.025 Uiso 1 1 calc R . . H25D H 0.2057 0.0566 0.1308 0.025 Uiso 1 1 calc R . . C26A C 0.09605(16) 0.0191(3) 0.10571(16) 0.0287(7) Uani 1 1 d . . . H26D H 0.0976 -0.0555 0.1400 0.043 Uiso 1 1 calc R . . H26E H 0.0603 -0.0098 0.0661 0.043 Uiso 1 1 calc R . . H26F H 0.0829 0.1155 0.1211 0.043 Uiso 1 1 calc R . . C27A C 0.25873(15) 0.1074(3) 0.00332(13) 0.0193(6) Uani 1 1 d . . . H27C H 0.3006 0.1397 0.0378 0.023 Uiso 1 1 calc R . . H27D H 0.2595 -0.0024 0.0020 0.023 Uiso 1 1 calc R . . C28A C 0.26778(17) 0.1662(3) -0.06276(13) 0.0272(7) Uani 1 1 d . . . H28D H 0.3131 0.1294 -0.0710 0.041 Uiso 1 1 calc R . . H28E H 0.2685 0.2749 -0.0619 0.041 Uiso 1 1 calc R . . H28F H 0.2275 0.1321 -0.0977 0.041 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 Fe1 0.0172(2) 0.0171(2) 0.01413(18) -0.00050(15) 0.00719(15) -0.00296(16) C1 0.0207(14) 0.0134(13) 0.0187(13) 0.0017(11) 0.0054(11) 0.0000(11) O1 0.0171(10) 0.0182(10) 0.0302(11) 0.0057(9) 0.0016(8) -0.0002(8) B3 0.0237(17) 0.0122(15) 0.0251(16) -0.0005(13) 0.0097(13) -0.0013(13) B4 0.0275(18) 0.0146(16) 0.0202(15) 0.0027(13) 0.0078(13) 0.0003(13) B5 0.0243(17) 0.0153(15) 0.0169(14) 0.0017(12) 0.0087(13) -0.0007(13) B6 0.0209(17) 0.0205(17) 0.0223(15) -0.0015(13) 0.0084(13) -0.0039(13) B7 0.0248(17) 0.0200(17) 0.0212(15) 0.0002(13) 0.0109(13) -0.0040(14) B8 0.0252(17) 0.0206(18) 0.0255(16) 0.0034(14) 0.0138(14) 0.0012(14) B9 0.0210(16) 0.0191(17) 0.0220(15) 0.0033(13) 0.0110(13) -0.0028(13) C10 0.0215(15) 0.0221(15) 0.0265(14) 0.0018(12) 0.0105(12) -0.0057(12) C21 0.0314(16) 0.0179(15) 0.0203(13) -0.0026(12) 0.0110(12) -0.0045(13) O21 0.0410(14) 0.0354(13) 0.0412(13) -0.0066(11) 0.0290(11) 0.0009(11) C22 0.0280(16) 0.0316(18) 0.0209(14) 0.0009(13) 0.0078(13) -0.0125(13) O22 0.0400(14) 0.0565(16) 0.0229(11) 0.0065(11) -0.0038(10) -0.0226(12) P1 0.0143(3) 0.0171(4) 0.0141(3) 0.0018(3) 0.0057(3) -0.0007(3) C23 0.0237(15) 0.0279(16) 0.0160(12) 0.0037(12) 0.0073(11) -0.0021(13) C24 0.0295(17) 0.0327(18) 0.0263(15) 0.0126(14) 0.0107(13) -0.0010(14) C25 0.0210(14) 0.0161(14) 0.0176(13) 0.0013(11) 0.0033(11) -0.0045(11) C26 0.0187(15) 0.0211(16) 0.0285(15) 0.0050(12) 0.0022(12) -0.0022(12) C27 0.0204(15) 0.0193(15) 0.0327(15) 0.0077(13) 0.0146(12) 0.0035(12) C28 0.0226(17) 0.0310(19) 0.058(2) 0.0140(16) 0.0106(15) 0.0052(14) Fe1A 0.0175(2) 0.0142(2) 0.01398(18) -0.00028(15) 0.00641(14) 0.00116(16) C1A 0.0183(14) 0.0158(14) 0.0139(12) 0.0028(10) 0.0099(10) 0.0010(11) O1A 0.0240(11) 0.0177(10) 0.0227(10) 0.0011(8) 0.0158(8) 0.0012(8) B3A 0.0244(17) 0.0146(16) 0.0216(15) -0.0004(13) 0.0118(13) -0.0018(13) B4A 0.0265(18) 0.0142(16) 0.0184(14) -0.0013(13) 0.0079(13) -0.0029(13) B5A 0.0191(16) 0.0161(15) 0.0144(13) 0.0003(12) 0.0045(12) -0.0063(12) B6A 0.0229(17) 0.0172(17) 0.0262(16) -0.0023(13) 0.0124(13) 0.0015(13) B7A 0.0298(18) 0.0179(17) 0.0226(15) -0.0025(13) 0.0149(14) -0.0019(14) B8A 0.0321(19) 0.0209(17) 0.0163(15) -0.0040(13) 0.0096(13) -0.0084(14) B9A 0.0241(17) 0.0206(17) 0.0181(14) 0.0004(13) 0.0090(13) -0.0026(14) C10A 0.0302(16) 0.0215(15) 0.0206(13) -0.0045(12) 0.0153(12) -0.0044(12) C21A 0.0237(16) 0.0194(15) 0.0237(14) -0.0003(12) 0.0076(12) 0.0019(12) O21A 0.0199(12) 0.0340(13) 0.0425(13) 0.0017(10) 0.0100(10) 0.0021(10) C22A 0.0237(15) 0.0214(15) 0.0230(14) -0.0040(12) 0.0054(12) 0.0033(12) O22A 0.0514(15) 0.0411(14) 0.0173(10) 0.0098(10) 0.0067(10) 0.0114(12) P1A 0.0159(3) 0.0164(4) 0.0161(3) -0.0029(3) 0.0053(3) -0.0005(3) C23A 0.0207(16) 0.0370(19) 0.0292(15) -0.0106(14) -0.0005(13) -0.0015(14) C24A 0.0346(19) 0.041(2) 0.046(2) -0.0284(17) 0.0054(16) -0.0090(16) C25A 0.0257(15) 0.0138(14) 0.0264(14) -0.0013(12) 0.0118(12) -0.0020(12) C26A 0.0306(17) 0.0232(16) 0.0384(17) -0.0027(14) 0.0203(14) -0.0069(13) C27A 0.0212(14) 0.0179(15) 0.0212(13) -0.0025(11) 0.0098(11) 0.0010(12) C28A 0.0344(17) 0.0301(17) 0.0214(14) -0.0040(13) 0.0150(13) 0.0016(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 Fe1 C22 1.768(3) . ? Fe1 C21 1.788(3) . ? Fe1 C1 1.966(3) . ? Fe1 B6 2.176(3) . ? Fe1 B9 2.180(3) . ? Fe1 B3 2.198(3) . ? Fe1 B5 2.204(3) . ? Fe1 P1 2.2450(14) . ? C1 O1 1.391(3) . ? C1 B4 1.618(4) . ? C1 B5 1.621(4) . ? C1 B3 1.631(4) . ? B3 B6 1.808(5) . ? B3 B7 1.837(5) . ? B3 B4 1.870(4) . ? B4 B7 1.786(5) . ? B4 B8 1.787(5) . ? B4 B5 1.862(4) . ? B5 B9 1.819(4) . ? B5 B8 1.839(5) . ? B6 C10 1.609(4) . ? B6 B7 1.841(4) . ? B6 B9 1.983(5) . ? B7 C10 1.600(4) . ? B7 B8 1.820(5) . ? B8 C10 1.594(4) . ? B8 B9 1.820(4) . ? B9 C10 1.608(4) . ? C21 O21 1.146(3) . ? C22 O22 1.146(3) . ? P1 C27 1.825(3) . ? P1 C25 1.834(3) . ? P1 C23 1.835(3) . ? C23 C24 1.533(4) . ? C25 C26 1.528(4) . ? C27 C28 1.527(4) . ? Fe1A C22A 1.778(3) . ? Fe1A C21A 1.781(3) . ? Fe1A C1A 1.972(3) . ? Fe1A B6A 2.176(3) . ? Fe1A B9A 2.185(3) . ? Fe1A B3A 2.194(3) . ? Fe1A B5A 2.213(3) . ? Fe1A P1A 2.2479(13) . ? C1A O1A 1.411(3) . ? C1A B5A 1.603(4) . ? C1A B4A 1.610(4) . ? C1A B3A 1.621(4) . ? B3A B6A 1.814(4) . ? B3A B7A 1.834(4) . ? B3A B4A 1.861(5) . ? B4A B8A 1.784(4) . ? B4A B7A 1.785(5) . ? B4A B5A 1.866(4) . ? B5A B9A 1.814(5) . ? B5A B8A 1.847(4) . ? B6A C10A 1.609(4) . ? B6A B7A 1.843(5) . ? B6A B9A 1.986(5) . ? B7A C10A 1.601(4) . ? B7A B8A 1.823(5) . ? B8A C10A 1.596(5) . ? B8A B9A 1.840(5) . ? B9A C10A 1.616(4) . ? C21A O21A 1.148(3) . ? C22A O22A 1.148(3) . ? P1A C27A 1.828(3) . ? P1A C25A 1.832(3) . ? P1A C23A 1.837(3) . ? C23A C24A 1.531(4) . ? C25A C26A 1.528(4) . ? C27A C28A 1.531(4) . ? 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 Fe1 C21 94.06(14) . . ? C22 Fe1 C1 166.28(12) . . ? C21 Fe1 C1 93.94(13) . . ? C22 Fe1 B6 79.70(13) . . ? C21 Fe1 B6 110.72(13) . . ? C1 Fe1 B6 87.06(12) . . ? C22 Fe1 B9 82.59(13) . . ? C21 Fe1 B9 164.84(13) . . ? C1 Fe1 B9 86.80(12) . . ? B6 Fe1 B9 54.16(12) . . ? C22 Fe1 B3 123.86(13) . . ? C21 Fe1 B3 86.41(13) . . ? C1 Fe1 B3 45.71(11) . . ? B6 Fe1 B3 48.84(12) . . ? B9 Fe1 B3 83.28(12) . . ? C22 Fe1 B5 128.53(13) . . ? C21 Fe1 B5 137.29(12) . . ? C1 Fe1 B5 45.30(11) . . ? B6 Fe1 B5 83.66(12) . . ? B9 Fe1 B5 49.04(12) . . ? B3 Fe1 B5 73.24(12) . . ? C22 Fe1 P1 89.45(10) . . ? C21 Fe1 P1 90.77(10) . . ? C1 Fe1 P1 101.57(8) . . ? B6 Fe1 P1 156.40(9) . . ? B9 Fe1 P1 103.94(9) . . ? B3 Fe1 P1 146.68(9) . . ? B5 Fe1 P1 86.97(9) . . ? O1 C1 B4 118.0(2) . . ? O1 C1 B5 125.1(2) . . ? B4 C1 B5 70.18(19) . . ? O1 C1 B3 126.7(2) . . ? B4 C1 B3 70.27(19) . . ? B5 C1 B3 107.7(2) . . ? O1 C1 Fe1 123.19(18) . . ? B4 C1 Fe1 118.79(19) . . ? B5 C1 Fe1 75.12(15) . . ? B3 C1 Fe1 74.64(15) . . ? C1 B3 B6 112.2(2) . . ? C1 B3 B7 107.2(2) . . ? B6 B3 B7 60.66(18) . . ? C1 B3 B4 54.54(16) . . ? B6 B3 B4 102.1(2) . . ? B7 B3 B4 57.57(17) . . ? C1 B3 Fe1 59.64(14) . . ? B6 B3 Fe1 64.97(14) . . ? B7 B3 Fe1 110.75(19) . . ? B4 B3 Fe1 98.57(17) . . ? C1 B4 B7 110.3(2) . . ? C1 B4 B8 110.0(2) . . ? B7 B4 B8 61.26(19) . . ? C1 B4 B5 54.98(16) . . ? B7 B4 B5 103.3(2) . . ? B8 B4 B5 60.50(17) . . ? C1 B4 B3 55.19(16) . . ? B7 B4 B3 60.29(17) . . ? B8 B4 B3 102.5(2) . . ? B5 B4 B3 89.41(19) . . ? C1 B5 B9 111.9(2) . . ? C1 B5 B8 107.3(2) . . ? B9 B5 B8 59.67(18) . . ? C1 B5 B4 54.84(17) . . ? B9 B5 B4 101.6(2) . . ? B8 B5 B4 57.72(17) . . ? C1 B5 Fe1 59.58(13) . . ? B9 B5 Fe1 64.79(14) . . ? B8 B5 Fe1 109.93(18) . . ? B4 B5 Fe1 98.59(17) . . ? C10 B6 B3 108.1(2) . . ? C10 B6 B7 54.75(18) . . ? B3 B6 B7 60.45(18) . . ? C10 B6 B9 51.93(16) . . ? B3 B6 B9 100.1(2) . . ? B7 B6 B9 87.23(19) . . ? C10 B6 Fe1 112.7(2) . . ? B3 B6 Fe1 66.19(14) . . ? B7 B6 Fe1 111.53(18) . . ? B9 B6 Fe1 63.01(13) . . ? C10 B7 B4 108.3(2) . . ? C10 B7 B8 55.13(18) . . ? B4 B7 B8 59.40(18) . . ? C10 B7 B3 107.2(2) . . ? B4 B7 B3 62.14(18) . . ? B8 B7 B3 102.5(2) . . ? C10 B7 B6 55.24(17) . . ? B4 B7 B6 104.2(2) . . ? B8 B7 B6 92.1(2) . . ? B3 B7 B6 58.89(17) . . ? C10 B8 B4 108.5(2) . . ? C10 B8 B7 55.41(18) . . ? B4 B8 B7 59.35(18) . . ? C10 B8 B9 55.72(18) . . ? B4 B8 B9 104.6(2) . . ? B7 B8 B9 93.0(2) . . ? C10 B8 B5 108.2(2) . . ? B4 B8 B5 61.79(18) . . ? B7 B8 B5 102.8(2) . . ? B9 B8 B5 59.62(17) . . ? C10 B9 B5 108.5(2) . . ? C10 B9 B8 55.01(17) . . ? B5 B9 B8 60.70(18) . . ? C10 B9 B6 51.98(17) . . ? B5 B9 B6 100.3(2) . . ? B8 B9 B6 87.7(2) . . ? C10 B9 Fe1 112.6(2) . . ? B5 B9 Fe1 66.17(14) . . ? B8 B9 Fe1 111.73(19) . . ? B6 B9 Fe1 62.83(13) . . ? B8 C10 B7 69.5(2) . . ? B8 C10 B9 69.3(2) . . ? B7 C10 B9 110.8(2) . . ? B8 C10 B6 110.8(2) . . ? B7 C10 B6 70.0(2) . . ? B9 C10 B6 76.1(2) . . ? O21 C21 Fe1 177.2(3) . . ? O22 C22 Fe1 177.4(3) . . ? C27 P1 C25 102.50(14) . . ? C27 P1 C23 103.69(13) . . ? C25 P1 C23 103.92(13) . . ? C27 P1 Fe1 115.90(10) . . ? C25 P1 Fe1 116.13(9) . . ? C23 P1 Fe1 113.10(10) . . ? C24 C23 P1 114.9(2) . . ? C26 C25 P1 113.83(19) . . ? C28 C27 P1 116.4(2) . . ? C22A Fe1A C21A 94.76(13) . . ? C22A Fe1A C1A 94.10(12) . . ? C21A Fe1A C1A 165.27(12) . . ? C22A Fe1A B6A 109.26(13) . . ? C21A Fe1A B6A 79.29(13) . . ? C1A Fe1A B6A 86.70(12) . . ? C22A Fe1A B9A 163.46(13) . . ? C21A Fe1A B9A 82.25(12) . . ? C1A Fe1A B9A 85.91(11) . . ? B6A Fe1A B9A 54.21(12) . . ? C22A Fe1A B3A 85.13(13) . . ? C21A Fe1A B3A 123.91(12) . . ? C1A Fe1A B3A 45.39(11) . . ? B6A Fe1A B3A 49.04(12) . . ? B9A Fe1A B3A 83.14(12) . . ? C22A Fe1A B5A 137.15(13) . . ? C21A Fe1A B5A 128.06(12) . . ? C1A Fe1A B5A 44.58(10) . . ? B6A Fe1A B5A 83.35(12) . . ? B9A Fe1A B5A 48.71(12) . . ? B3A Fe1A B5A 72.69(12) . . ? C22A Fe1A P1A 91.64(10) . . ? C21A Fe1A P1A 90.07(9) . . ? C1A Fe1A P1A 101.41(8) . . ? B6A Fe1A P1A 157.12(9) . . ? B9A Fe1A P1A 104.59(9) . . ? B3A Fe1A P1A 146.01(9) . . ? B5A Fe1A P1A 87.56(9) . . ? O1A C1A B5A 124.3(2) . . ? O1A C1A B4A 116.3(2) . . ? B5A C1A B4A 71.03(19) . . ? O1A C1A B3A 126.7(2) . . ? B5A C1A B3A 108.3(2) . . ? B4A C1A B3A 70.36(19) . . ? O1A C1A Fe1A 123.99(18) . . ? B5A C1A Fe1A 75.68(15) . . ? B4A C1A Fe1A 119.66(18) . . ? B3A C1A Fe1A 74.57(15) . . ? C1A B3A B6A 112.1(2) . . ? C1A B3A B7A 107.2(2) . . ? B6A B3A B7A 60.71(18) . . ? C1A B3A B4A 54.55(16) . . ? B6A B3A B4A 102.4(2) . . ? B7A B3A B4A 57.75(17) . . ? C1A B3A Fe1A 60.05(14) . . ? B6A B3A Fe1A 64.94(14) . . ? B7A B3A Fe1A 111.30(18) . . ? B4A B3A Fe1A 99.48(17) . . ? C1A B4A B8A 109.7(2) . . ? C1A B4A B7A 110.1(2) . . ? B8A B4A B7A 61.46(19) . . ? C1A B4A B3A 55.08(16) . . ? B8A B4A B3A 102.7(2) . . ? B7A B4A B3A 60.36(18) . . ? C1A B4A B5A 54.30(16) . . ? B8A B4A B5A 60.77(17) . . ? B7A B4A B5A 103.2(2) . . ? B3A B4A B5A 88.96(19) . . ? C1A B5A B9A 112.1(2) . . ? C1A B5A B8A 107.0(2) . . ? B9A B5A B8A 60.32(18) . . ? C1A B5A B4A 54.67(16) . . ? B9A B5A B4A 101.9(2) . . ? B8A B5A B4A 57.41(16) . . ? C1A B5A Fe1A 59.74(14) . . ? B9A B5A Fe1A 64.84(14) . . ? B8A B5A Fe1A 110.32(19) . . ? B4A B5A Fe1A 98.69(17) . . ? C10A B6A B3A 107.6(2) . . ? C10A B6A B7A 54.73(17) . . ? B3A B6A B7A 60.19(18) . . ? C10A B6A B9A 52.12(16) . . ? B3A B6A B9A 99.6(2) . . ? B7A B6A B9A 87.5(2) . . ? C10A B6A Fe1A 113.0(2) . . ? B3A B6A Fe1A 66.02(14) . . ? B7A B6A Fe1A 111.75(19) . . ? B9A B6A Fe1A 63.13(13) . . ? C10A B7A B4A 108.0(2) . . ? C10A B7A B8A 55.10(18) . . ? B4A B7A B8A 59.24(18) . . ? C10A B7A B3A 107.0(2) . . ? B4A B7A B3A 61.90(17) . . ? B8A B7A B3A 102.3(2) . . ? C10A B7A B6A 55.17(18) . . ? B4A B7A B6A 104.2(2) . . ? B8A B7A B6A 92.3(2) . . ? B3A B7A B6A 59.10(17) . . ? C10A B8A B4A 108.3(2) . . ? C10A B8A B7A 55.34(18) . . ? B4A B8A B7A 59.29(18) . . ? C10A B8A B9A 55.56(18) . . ? B4A B8A B9A 104.1(2) . . ? B7A B8A B9A 92.7(2) . . ? C10A B8A B5A 107.3(2) . . ? B4A B8A B5A 61.83(17) . . ? B7A B8A B5A 102.5(2) . . ? B9A B8A B5A 58.93(17) . . ? C10A B9A B5A 108.1(2) . . ? C10A B9A B8A 54.56(18) . . ? B5A B9A B8A 60.75(17) . . ? C10A B9A B6A 51.83(17) . . ? B5A B9A B6A 100.2(2) . . ? B8A B9A B6A 87.4(2) . . ? C10A B9A Fe1A 112.28(19) . . ? B5A B9A Fe1A 66.45(13) . . ? B8A B9A Fe1A 111.84(18) . . ? B6A B9A Fe1A 62.67(13) . . ? B8A C10A B7A 69.6(2) . . ? B8A C10A B6A 111.2(2) . . ? B7A C10A B6A 70.1(2) . . ? B8A C10A B9A 69.9(2) . . ? B7A C10A B9A 111.0(2) . . ? B6A C10A B9A 76.0(2) . . ? O21A C21A Fe1A 177.8(3) . . ? O22A C22A Fe1A 175.2(3) . . ? C27A P1A C25A 102.14(13) . . ? C27A P1A C23A 103.35(14) . . ? C25A P1A C23A 104.53(15) . . ? C27A P1A Fe1A 117.02(9) . . ? C25A P1A Fe1A 115.11(10) . . ? C23A P1A Fe1A 113.09(11) . . ? C24A C23A P1A 115.0(2) . . ? C26A C25A P1A 115.3(2) . . ? C28A C27A P1A 115.3(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O1A 0.84 2.09 2.896(3) 160.6 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.797 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.089 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 609674' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 B7 O4 Ru' _chemical_formula_weight 309.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6548(7) _cell_length_b 11.6193(12) _cell_length_c 19.6123(19) _cell_angle_alpha 93.716(5) _cell_angle_beta 98.033(5) _cell_angle_gamma 90.739(5) _cell_volume 1723.2(3) _cell_formula_units_Z 6 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6606 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.01 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.882 _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 X8 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 27098 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.08 _reflns_number_total 8204 _reflns_number_gt 6644 _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^)+(0.0245P)^2^+0.9169P] 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 8204 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru2 Ru 0.70061(3) 0.252539(19) 0.103146(12) 0.01224(6) Uani 1 1 d . . . C1 C 0.5129(4) 0.1880(2) 0.15877(15) 0.0136(6) Uani 1 1 d . . . O1 O 0.5638(3) 0.12955(18) 0.21842(11) 0.0182(5) Uani 1 1 d . . . H1 H 0.4760 0.1203 0.2390 0.027 Uiso 1 1 calc R . . B3 B 0.4553(5) 0.1330(3) 0.07859(18) 0.0172(7) Uani 1 1 d . . . H3 H 0.4691 0.0390 0.0643 0.021 Uiso 1 1 calc R . . B4 B 0.3100(5) 0.2073(3) 0.13438(18) 0.0158(7) Uani 1 1 d . . . H4 H 0.2098 0.1709 0.1641 0.019 Uiso 1 1 calc R . . B5 B 0.4749(4) 0.3274(3) 0.15774(18) 0.0140(7) Uani 1 1 d . . . H5 H 0.5047 0.3861 0.2057 0.017 Uiso 1 1 calc R . . B6 B 0.4735(4) 0.2377(3) 0.01412(18) 0.0175(7) Uani 1 1 d . . . H6 H 0.5188 0.2109 -0.0363 0.021 Uiso 1 1 calc R . . B7 B 0.2617(5) 0.2104(3) 0.04275(18) 0.0172(7) Uani 1 1 d . . . H7 H 0.1432 0.1623 0.0141 0.021 Uiso 1 1 calc R . . B8 B 0.2750(5) 0.3444(3) 0.09781(18) 0.0176(7) Uani 1 1 d . . . H8 H 0.1674 0.4014 0.1124 0.021 Uiso 1 1 calc R . . B9 B 0.4874(4) 0.3862(3) 0.07574(18) 0.0164(7) Uani 1 1 d . . . H9 H 0.5437 0.4751 0.0735 0.020 Uiso 1 1 calc R . . C10 C 0.3252(4) 0.3324(3) 0.02147(16) 0.0182(7) Uani 1 1 d . . . H10 H 0.2672 0.3775 -0.0216 0.022 Uiso 1 1 calc R . . C21 C 0.8363(4) 0.1164(3) 0.08569(16) 0.0179(7) Uani 1 1 d . . . O21 O 0.9057(3) 0.03480(19) 0.07301(12) 0.0264(5) Uani 1 1 d . . . C22 C 0.8666(4) 0.3103(3) 0.18364(16) 0.0180(7) Uani 1 1 d . . . O22 O 0.9531(3) 0.3433(2) 0.23238(12) 0.0302(6) Uani 1 1 d . . . C23 C 0.8118(4) 0.3363(3) 0.03698(16) 0.0178(7) Uani 1 1 d . . . O23 O 0.8647(3) 0.3856(2) -0.00355(12) 0.0280(6) Uani 1 1 d . . . Ru12 Ru 0.47051(3) 0.24777(2) 0.432752(12) 0.01284(6) Uani 1 1 d . . . C101 C 0.2430(4) 0.1955(3) 0.36690(15) 0.0151(6) Uani 1 1 d . . . O101 O 0.2526(3) 0.14298(18) 0.30161(10) 0.0193(5) Uani 1 1 d . . . H101 H 0.1561 0.1092 0.2863 0.029 Uiso 1 1 calc R . . B103 B 0.2173(4) 0.3346(3) 0.38705(18) 0.0168(7) Uani 1 1 d . . . H103 H 0.2225 0.4007 0.3482 0.020 Uiso 1 1 calc R . . B104 B 0.0544(4) 0.2164(3) 0.39065(18) 0.0157(7) Uani 1 1 d . . . H104 H -0.0677 0.1897 0.3544 0.019 Uiso 1 1 calc R . . B105 B 0.2285(4) 0.1283(3) 0.43802(18) 0.0163(7) Uani 1 1 d . . . H105 H 0.2433 0.0327 0.4394 0.020 Uiso 1 1 calc R . . B106 B 0.2874(5) 0.3751(3) 0.47861(18) 0.0164(7) Uani 1 1 d . . . H106 H 0.3555 0.4601 0.4957 0.020 Uiso 1 1 calc R . . B107 B 0.0555(5) 0.3449(3) 0.44677(19) 0.0183(7) Uani 1 1 d . . . H107 H -0.0550 0.4071 0.4392 0.022 Uiso 1 1 calc R . . B108 B 0.0620(5) 0.2015(3) 0.48147(18) 0.0166(7) Uani 1 1 d . . . H108 H -0.0440 0.1508 0.5009 0.020 Uiso 1 1 calc R . . B109 B 0.2939(5) 0.2185(3) 0.51642(18) 0.0176(7) Uani 1 1 d . . . H109 H 0.3673 0.1809 0.5630 0.021 Uiso 1 1 calc R . . C110 C 0.1500(4) 0.3162(3) 0.52160(16) 0.0174(6) Uani 1 1 d . . . H110 H 0.1209 0.3535 0.5700 0.021 Uiso 1 1 calc R . . C121 C 0.5868(4) 0.3482(3) 0.37696(16) 0.0197(7) Uani 1 1 d . . . O121 O 0.6428(3) 0.4100(2) 0.34343(12) 0.0324(6) Uani 1 1 d . . . C122 C 0.6031(4) 0.1138(3) 0.40671(16) 0.0193(7) Uani 1 1 d . . . O122 O 0.6730(3) 0.0346(2) 0.38915(13) 0.0309(6) Uani 1 1 d . . . C123 C 0.6368(4) 0.2926(3) 0.51570(17) 0.0184(7) Uani 1 1 d . . . O123 O 0.7223(3) 0.3191(2) 0.56580(11) 0.0248(5) Uani 1 1 d . . . Ru22 Ru 1.07750(3) 0.77405(2) 0.231567(12) 0.01201(6) Uani 1 1 d . . . C201 C 0.8738(4) 0.8892(2) 0.23722(15) 0.0128(6) Uani 1 1 d . . . O201 O 0.9038(3) 1.00760(16) 0.23955(11) 0.0168(5) Uani 1 1 d . . . H201 H 0.8074 1.0415 0.2386 0.025 Uiso 1 1 calc R . . B203 B 0.8709(4) 0.8085(3) 0.30426(17) 0.0134(7) Uani 1 1 d . . . H203 H 0.9118 0.8452 0.3585 0.016 Uiso 1 1 calc R . . B204 B 0.6797(4) 0.8406(3) 0.23937(18) 0.0144(7) Uani 1 1 d . . . H204 H 0.5704 0.9029 0.2427 0.017 Uiso 1 1 calc R . . B205 B 0.8079(4) 0.8022(3) 0.16743(18) 0.0143(7) Uani 1 1 d . . . H205 H 0.7992 0.8339 0.1144 0.017 Uiso 1 1 calc R . . B206 B 0.9024(4) 0.6561(3) 0.28399(17) 0.0147(7) Uani 1 1 d . . . H206 H 0.9800 0.6028 0.3226 0.018 Uiso 1 1 calc R . . B207 B 0.6822(4) 0.7100(3) 0.28353(18) 0.0153(7) Uani 1 1 d . . . H207 H 0.5895 0.6981 0.3220 0.018 Uiso 1 1 calc R . . B208 B 0.6381(5) 0.7051(3) 0.18905(18) 0.0164(7) Uani 1 1 d . . . H208 H 0.5111 0.6894 0.1535 0.020 Uiso 1 1 calc R . . B209 B 0.8553(5) 0.6507(3) 0.17925(18) 0.0167(7) Uani 1 1 d . . . H209 H 0.8964 0.5935 0.1364 0.020 Uiso 1 1 calc R . . C210 C 0.7327(4) 0.6068(2) 0.23257(15) 0.0157(6) Uani 1 1 d . . . H210 H 0.6891 0.5187 0.2310 0.019 Uiso 1 1 calc R . . C221 C 1.2514(4) 0.8485(3) 0.30351(16) 0.0167(6) Uani 1 1 d . . . O221 O 1.3465(3) 0.88953(19) 0.34763(12) 0.0242(5) Uani 1 1 d . . . C222 C 1.1792(4) 0.8380(3) 0.15634(17) 0.0220(7) Uani 1 1 d . . . O222 O 1.2256(3) 0.8757(2) 0.10985(13) 0.0342(6) Uani 1 1 d . . . C223 C 1.2142(4) 0.6340(3) 0.23154(16) 0.0178(7) Uani 1 1 d . . . O223 O 1.2831(3) 0.54928(19) 0.23455(13) 0.0277(6) 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 Ru2 0.01065(12) 0.01305(12) 0.01312(12) 0.00140(9) 0.00188(9) -0.00027(9) C1 0.0140(15) 0.0118(14) 0.0152(15) 0.0010(11) 0.0025(12) 0.0006(11) O1 0.0174(11) 0.0213(11) 0.0175(11) 0.0082(9) 0.0040(9) 0.0038(9) B3 0.0174(18) 0.0142(16) 0.0203(19) -0.0030(14) 0.0063(15) -0.0050(14) B4 0.0152(17) 0.0159(17) 0.0161(17) -0.0023(13) 0.0031(14) -0.0010(14) B5 0.0121(17) 0.0151(16) 0.0153(17) 0.0015(13) 0.0033(13) -0.0016(13) B6 0.0119(17) 0.0245(19) 0.0150(18) -0.0007(14) -0.0010(14) -0.0052(14) B7 0.0130(17) 0.0238(18) 0.0143(18) -0.0024(14) 0.0022(14) -0.0037(14) B8 0.0129(17) 0.0189(17) 0.0203(19) 0.0009(14) 0.0003(14) 0.0025(14) B9 0.0125(17) 0.0187(17) 0.0180(18) 0.0033(14) 0.0008(14) 0.0015(14) C10 0.0148(16) 0.0245(17) 0.0156(16) 0.0042(13) 0.0014(12) 0.0006(13) C21 0.0156(16) 0.0211(16) 0.0181(16) 0.0029(13) 0.0057(13) -0.0036(13) O21 0.0268(13) 0.0182(12) 0.0370(14) -0.0001(10) 0.0152(11) 0.0028(10) C22 0.0154(16) 0.0185(15) 0.0209(17) 0.0012(13) 0.0055(13) 0.0021(13) O22 0.0219(13) 0.0392(15) 0.0255(13) -0.0052(11) -0.0075(11) 0.0006(11) C23 0.0110(15) 0.0206(16) 0.0212(17) 0.0013(13) 0.0001(13) -0.0003(12) O23 0.0218(13) 0.0357(14) 0.0289(14) 0.0137(11) 0.0064(11) -0.0018(11) Ru12 0.01108(12) 0.01490(12) 0.01275(13) 0.00155(9) 0.00222(9) -0.00036(9) C101 0.0140(15) 0.0168(15) 0.0139(15) -0.0001(12) -0.0001(12) -0.0017(12) O101 0.0198(12) 0.0244(12) 0.0133(11) -0.0033(9) 0.0034(9) -0.0032(10) B103 0.0138(17) 0.0218(18) 0.0145(17) 0.0048(14) -0.0005(14) -0.0009(14) B104 0.0125(17) 0.0175(17) 0.0169(18) 0.0003(14) 0.0017(14) -0.0013(14) B105 0.0124(17) 0.0199(17) 0.0169(18) -0.0007(14) 0.0044(14) -0.0011(14) B106 0.0166(18) 0.0138(16) 0.0183(18) -0.0014(13) 0.0019(14) 0.0012(14) B107 0.0152(18) 0.0153(17) 0.025(2) 0.0013(14) 0.0033(15) 0.0009(14) B108 0.0130(17) 0.0209(18) 0.0169(18) 0.0012(14) 0.0061(14) -0.0001(14) B109 0.0142(18) 0.0211(18) 0.0183(18) 0.0021(14) 0.0044(14) -0.0008(14) C110 0.0135(15) 0.0215(16) 0.0168(16) -0.0019(12) 0.0026(12) -0.0020(12) C121 0.0122(15) 0.0288(18) 0.0171(16) 0.0011(14) -0.0010(13) -0.0024(13) O121 0.0266(14) 0.0446(16) 0.0261(14) 0.0149(12) -0.0005(11) -0.0124(12) C122 0.0138(16) 0.0216(17) 0.0227(17) 0.0006(13) 0.0043(13) -0.0060(13) O122 0.0218(13) 0.0192(12) 0.0519(17) -0.0074(11) 0.0107(12) -0.0014(10) C123 0.0158(16) 0.0185(16) 0.0223(17) 0.0038(13) 0.0066(13) 0.0011(13) O123 0.0206(12) 0.0321(13) 0.0200(12) 0.0016(10) -0.0021(10) -0.0040(10) Ru22 0.00999(12) 0.01275(12) 0.01352(13) -0.00036(9) 0.00303(9) 0.00021(9) C201 0.0130(15) 0.0101(13) 0.0148(15) 0.0000(11) 0.0012(12) -0.0014(11) O201 0.0153(11) 0.0117(10) 0.0235(12) 0.0004(9) 0.0037(9) -0.0003(8) B203 0.0119(17) 0.0138(16) 0.0151(17) 0.0004(13) 0.0039(13) 0.0022(13) B204 0.0134(17) 0.0116(15) 0.0187(18) 0.0011(13) 0.0041(14) -0.0003(13) B205 0.0125(17) 0.0160(16) 0.0150(17) 0.0000(13) 0.0045(13) -0.0011(13) B206 0.0128(17) 0.0184(17) 0.0136(17) 0.0008(13) 0.0039(13) 0.0019(14) B207 0.0109(17) 0.0191(17) 0.0159(17) 0.0010(14) 0.0021(13) -0.0006(14) B208 0.0133(17) 0.0179(17) 0.0183(18) 0.0002(14) 0.0035(14) -0.0041(14) B209 0.0160(18) 0.0167(17) 0.0170(18) 0.0012(14) 0.0015(14) -0.0007(14) C210 0.0151(15) 0.0143(14) 0.0182(16) -0.0002(12) 0.0055(12) -0.0017(12) C221 0.0126(15) 0.0145(15) 0.0238(17) 0.0007(13) 0.0050(13) 0.0012(12) O221 0.0181(12) 0.0243(12) 0.0280(13) -0.0067(10) -0.0013(10) 0.0007(10) C222 0.0149(16) 0.0248(17) 0.0266(19) 0.0040(14) 0.0031(14) 0.0026(13) O222 0.0280(14) 0.0437(16) 0.0368(15) 0.0186(12) 0.0168(12) 0.0072(12) C223 0.0147(16) 0.0201(16) 0.0192(16) -0.0026(13) 0.0060(13) -0.0022(13) O223 0.0243(13) 0.0174(12) 0.0426(15) -0.0012(11) 0.0095(11) 0.0038(10) _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 Ru2 C21 1.942(3) . ? Ru2 C23 1.951(3) . ? Ru2 C22 1.959(3) . ? Ru2 C1 2.082(3) . ? Ru2 B6 2.282(3) . ? Ru2 B3 2.298(3) . ? Ru2 B9 2.300(3) . ? Ru2 B5 2.307(3) . ? C1 O1 1.401(3) . ? C1 B4 1.583(4) . ? C1 B5 1.651(4) . ? C1 B3 1.656(4) . ? B3 B7 1.823(5) . ? B3 B6 1.828(5) . ? B3 B4 1.850(5) . ? B4 B7 1.786(5) . ? B4 B8 1.798(5) . ? B4 B5 1.861(4) . ? B5 B9 1.801(5) . ? B5 B8 1.816(5) . ? B6 C10 1.605(5) . ? B6 B7 1.819(5) . ? B6 B9 2.034(5) . ? B7 C10 1.592(4) . ? B7 B8 1.830(5) . ? B8 C10 1.595(5) . ? B8 B9 1.808(5) . ? B9 C10 1.609(4) . ? C21 O21 1.124(4) . ? C22 O22 1.126(4) . ? C23 O23 1.126(4) . ? Ru12 C121 1.940(3) . ? Ru12 C122 1.948(3) . ? Ru12 C123 1.958(3) . ? Ru12 C101 2.077(3) . ? Ru12 B106 2.280(4) . ? Ru12 B103 2.294(3) . ? Ru12 B109 2.306(3) . ? Ru12 B105 2.318(3) . ? C101 O101 1.394(3) . ? C101 B104 1.595(4) . ? C101 B105 1.658(4) . ? C101 B103 1.660(5) . ? B103 B107 1.819(5) . ? B103 B106 1.830(5) . ? B103 B104 1.854(5) . ? B104 B108 1.794(5) . ? B104 B107 1.795(5) . ? B104 B105 1.871(5) . ? B105 B109 1.810(5) . ? B105 B108 1.820(5) . ? B106 C110 1.609(4) . ? B106 B107 1.819(5) . ? B106 B109 2.007(5) . ? B107 C110 1.600(5) . ? B107 B108 1.839(5) . ? B108 C110 1.595(4) . ? B108 B109 1.815(5) . ? B109 C110 1.601(5) . ? C121 O121 1.124(4) . ? C122 O122 1.130(4) . ? C123 O123 1.124(4) . ? Ru22 C222 1.945(3) . ? Ru22 C223 1.946(3) . ? Ru22 C221 1.949(3) . ? Ru22 C201 2.078(3) . ? Ru22 B206 2.292(3) . ? Ru22 B209 2.293(3) . ? Ru22 B203 2.295(3) . ? Ru22 B205 2.301(3) . ? C201 O201 1.389(3) . ? C201 B204 1.589(4) . ? C201 B205 1.662(4) . ? C201 B203 1.665(4) . ? B203 B207 1.815(4) . ? B203 B206 1.817(5) . ? B203 B204 1.859(5) . ? B204 B207 1.794(5) . ? B204 B208 1.804(5) . ? B204 B205 1.862(5) . ? B205 B208 1.823(4) . ? B205 B209 1.825(5) . ? B206 C210 1.604(4) . ? B206 B207 1.805(5) . ? B206 B209 2.032(5) . ? B207 C210 1.597(4) . ? B207 B208 1.833(5) . ? B208 C210 1.591(5) . ? B208 B209 1.817(5) . ? B209 C210 1.602(4) . ? C221 O221 1.126(3) . ? C222 O222 1.135(4) . ? C223 O223 1.124(4) . ? 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 Ru2 C23 91.36(13) . . ? C21 Ru2 C22 93.89(13) . . ? C23 Ru2 C22 95.06(12) . . ? C21 Ru2 C1 101.85(12) . . ? C23 Ru2 C1 162.07(12) . . ? C22 Ru2 C1 96.06(12) . . ? C21 Ru2 B6 102.78(13) . . ? C23 Ru2 B6 81.87(12) . . ? C22 Ru2 B6 163.09(13) . . ? C1 Ru2 B6 83.41(12) . . ? C21 Ru2 B3 86.24(12) . . ? C23 Ru2 B3 126.33(12) . . ? C22 Ru2 B3 138.61(12) . . ? C1 Ru2 B3 44.10(12) . . ? B6 Ru2 B3 47.05(12) . . ? C21 Ru2 B9 154.82(13) . . ? C23 Ru2 B9 80.30(12) . . ? C22 Ru2 B9 110.40(13) . . ? C1 Ru2 B9 82.66(12) . . ? B6 Ru2 B9 52.72(13) . . ? B3 Ru2 B9 79.93(12) . . ? C21 Ru2 B5 145.53(12) . . ? C23 Ru2 B5 122.75(12) . . ? C22 Ru2 B5 88.29(12) . . ? C1 Ru2 B5 43.81(11) . . ? B6 Ru2 B5 79.62(13) . . ? B3 Ru2 B5 70.17(12) . . ? B9 Ru2 B5 46.02(12) . . ? O1 C1 B4 119.4(2) . . ? O1 C1 B5 124.9(2) . . ? B4 C1 B5 70.2(2) . . ? O1 C1 B3 128.4(2) . . ? B4 C1 B3 69.6(2) . . ? B5 C1 B3 106.3(2) . . ? O1 C1 Ru2 120.9(2) . . ? B4 C1 Ru2 119.7(2) . . ? B5 C1 Ru2 75.37(16) . . ? B3 C1 Ru2 74.91(16) . . ? C1 B3 B7 106.8(2) . . ? C1 B3 B6 113.0(2) . . ? B7 B3 B6 59.75(19) . . ? C1 B3 B4 53.34(18) . . ? B7 B3 B4 58.19(19) . . ? B6 B3 B4 102.1(2) . . ? C1 B3 Ru2 61.00(14) . . ? B7 B3 Ru2 111.68(19) . . ? B6 B3 Ru2 66.00(14) . . ? B4 B3 Ru2 99.50(18) . . ? C1 B4 B7 111.9(3) . . ? C1 B4 B8 111.3(2) . . ? B7 B4 B8 61.4(2) . . ? C1 B4 B3 57.07(19) . . ? B7 B4 B3 60.17(19) . . ? B8 B4 B3 103.4(2) . . ? C1 B4 B5 56.59(18) . . ? B7 B4 B5 102.7(2) . . ? B8 B4 B5 59.47(18) . . ? B3 B4 B5 91.0(2) . . ? C1 B5 B9 114.1(2) . . ? C1 B5 B8 107.3(2) . . ? B9 B5 B8 59.98(19) . . ? C1 B5 B4 53.18(17) . . ? B9 B5 B4 102.5(2) . . ? B8 B5 B4 58.53(18) . . ? C1 B5 Ru2 60.82(15) . . ? B9 B5 Ru2 66.78(15) . . ? B8 B5 Ru2 112.1(2) . . ? B4 B5 Ru2 98.83(18) . . ? C10 B6 B7 54.99(19) . . ? C10 B6 B3 107.6(2) . . ? B7 B6 B3 59.99(19) . . ? C10 B6 B9 50.83(17) . . ? B7 B6 B9 86.6(2) . . ? B3 B6 B9 99.6(2) . . ? C10 B6 Ru2 113.1(2) . . ? B7 B6 Ru2 112.6(2) . . ? B3 B6 Ru2 66.95(15) . . ? B9 B6 Ru2 64.11(13) . . ? C10 B7 B4 108.3(2) . . ? C10 B7 B6 55.66(19) . . ? B4 B7 B6 104.9(2) . . ? C10 B7 B3 108.4(2) . . ? B4 B7 B3 61.64(19) . . ? B6 B7 B3 60.25(19) . . ? C10 B7 B8 55.02(19) . . ? B4 B7 B8 59.61(19) . . ? B6 B7 B8 93.1(2) . . ? B3 B7 B8 103.2(2) . . ? C10 B8 B4 107.7(3) . . ? C10 B8 B9 56.02(19) . . ? B4 B8 B9 104.8(2) . . ? C10 B8 B5 107.9(3) . . ? B4 B8 B5 62.00(18) . . ? B9 B8 B5 59.61(18) . . ? C10 B8 B7 54.88(19) . . ? B4 B8 B7 58.98(19) . . ? B9 B8 B7 93.3(2) . . ? B5 B8 B7 102.8(2) . . ? C10 B9 B5 108.0(2) . . ? C10 B9 B8 55.27(18) . . ? B5 B9 B8 60.40(19) . . ? C10 B9 B6 50.65(17) . . ? B5 B9 B6 99.8(2) . . ? B8 B9 B6 87.0(2) . . ? C10 B9 Ru2 112.0(2) . . ? B5 B9 Ru2 67.20(15) . . ? B8 B9 Ru2 112.7(2) . . ? B6 B9 Ru2 63.18(14) . . ? B7 C10 B8 70.1(2) . . ? B7 C10 B6 69.3(2) . . ? B8 C10 B6 111.8(3) . . ? B7 C10 B9 111.5(3) . . ? B8 C10 B9 68.7(2) . . ? B6 C10 B9 78.5(2) . . ? O21 C21 Ru2 175.7(3) . . ? O22 C22 Ru2 175.5(3) . . ? O23 C23 Ru2 175.3(3) . . ? C121 Ru12 C122 93.10(13) . . ? C121 Ru12 C123 92.39(12) . . ? C122 Ru12 C123 94.34(13) . . ? C121 Ru12 C101 102.39(12) . . ? C122 Ru12 C101 93.97(12) . . ? C123 Ru12 C101 162.61(12) . . ? C121 Ru12 B106 100.30(13) . . ? C122 Ru12 B106 166.60(12) . . ? C123 Ru12 B106 84.78(13) . . ? C101 Ru12 B106 83.60(12) . . ? C121 Ru12 B103 84.78(13) . . ? C122 Ru12 B103 135.74(13) . . ? C123 Ru12 B103 129.91(13) . . ? C101 Ru12 B103 44.30(12) . . ? B106 Ru12 B103 47.17(12) . . ? C121 Ru12 B109 151.50(13) . . ? C122 Ru12 B109 114.72(13) . . ? C123 Ru12 B109 80.02(12) . . ? C101 Ru12 B109 82.63(12) . . ? B106 Ru12 B109 51.93(12) . . ? B103 Ru12 B109 79.50(13) . . ? C121 Ru12 B105 146.28(12) . . ? C122 Ru12 B105 89.67(12) . . ? C123 Ru12 B105 120.92(12) . . ? C101 Ru12 B105 43.90(12) . . ? B106 Ru12 B105 79.42(12) . . ? B103 Ru12 B105 70.27(12) . . ? B109 Ru12 B105 46.09(12) . . ? O101 C101 B104 119.3(2) . . ? O101 C101 B105 126.1(2) . . ? B104 C101 B105 70.2(2) . . ? O101 C101 B103 127.2(2) . . ? B104 C101 B103 69.4(2) . . ? B105 C101 B103 106.2(2) . . ? O101 C101 Ru12 120.8(2) . . ? B104 C101 Ru12 119.9(2) . . ? B105 C101 Ru12 75.82(16) . . ? B103 C101 Ru12 74.81(16) . . ? C101 B103 B107 107.4(2) . . ? C101 B103 B106 112.7(2) . . ? B107 B103 B106 59.79(19) . . ? C101 B103 B104 53.64(18) . . ? B107 B103 B104 58.51(18) . . ? B106 B103 B104 102.0(2) . . ? C101 B103 Ru12 60.89(15) . . ? B107 B103 Ru12 112.3(2) . . ? B106 B103 Ru12 66.01(15) . . ? B104 B103 Ru12 99.87(19) . . ? C101 B104 B108 111.1(2) . . ? C101 B104 B107 111.5(2) . . ? B108 B104 B107 61.6(2) . . ? C101 B104 B103 56.96(18) . . ? B108 B104 B103 103.2(2) . . ? B107 B104 B103 59.78(19) . . ? C101 B104 B105 56.48(18) . . ? B108 B104 B105 59.49(19) . . ? B107 B104 B105 102.8(2) . . ? B103 B104 B105 90.9(2) . . ? C101 B105 B109 113.3(2) . . ? C101 B105 B108 107.0(2) . . ? B109 B105 B108 60.00(19) . . ? C101 B105 B104 53.31(18) . . ? B109 B105 B104 101.9(2) . . ? B108 B105 B104 58.14(19) . . ? C101 B105 Ru12 60.28(14) . . ? B109 B105 Ru12 66.59(15) . . ? B108 B105 Ru12 111.9(2) . . ? B104 B105 Ru12 98.49(18) . . ? C110 B106 B107 55.24(19) . . ? C110 B106 B103 107.7(2) . . ? B107 B106 B103 59.81(19) . . ? C110 B106 B109 51.11(18) . . ? B107 B106 B109 87.2(2) . . ? B103 B106 B109 100.0(2) . . ? C110 B106 Ru12 113.9(2) . . ? B107 B106 Ru12 112.9(2) . . ? B103 B106 Ru12 66.82(16) . . ? B109 B106 Ru12 64.70(14) . . ? C110 B107 B104 107.8(3) . . ? C110 B107 B106 55.71(19) . . ? B104 B107 B106 104.8(2) . . ? C110 B107 B103 108.6(3) . . ? B104 B107 B103 61.71(19) . . ? B106 B107 B103 60.40(19) . . ? C110 B107 B108 54.72(18) . . ? B104 B107 B108 59.14(19) . . ? B106 B107 B108 92.7(2) . . ? B103 B107 B108 102.8(2) . . ? C110 B108 B104 108.1(2) . . ? C110 B108 B109 55.56(19) . . ? B104 B108 B109 104.8(2) . . ? C110 B108 B105 108.2(2) . . ? B104 B108 B105 62.4(2) . . ? B109 B108 B105 59.73(19) . . ? C110 B108 B107 54.99(19) . . ? B104 B108 B107 59.22(19) . . ? B109 B108 B107 92.7(2) . . ? B105 B108 B107 103.1(2) . . ? C110 B109 B105 108.4(3) . . ? C110 B109 B108 55.24(19) . . ? B105 B109 B108 60.27(19) . . ? C110 B109 B106 51.47(18) . . ? B105 B109 B106 100.5(2) . . ? B108 B109 B106 87.5(2) . . ? C110 B109 Ru12 112.9(2) . . ? B105 B109 Ru12 67.32(15) . . ? B108 B109 Ru12 112.7(2) . . ? B106 B109 Ru12 63.37(14) . . ? B108 C110 B107 70.3(2) . . ? B108 C110 B109 69.2(2) . . ? B107 C110 B109 111.3(3) . . ? B108 C110 B106 111.3(3) . . ? B107 C110 B106 69.0(2) . . ? B109 C110 B106 77.4(2) . . ? O121 C121 Ru12 175.0(3) . . ? O122 C122 Ru12 176.5(3) . . ? O123 C123 Ru12 175.1(3) . . ? C222 Ru22 C223 94.97(13) . . ? C222 Ru22 C221 94.36(13) . . ? C223 Ru22 C221 90.85(13) . . ? C222 Ru22 C201 98.44(12) . . ? C223 Ru22 C201 162.88(11) . . ? C221 Ru22 C201 98.66(12) . . ? C222 Ru22 B206 157.60(13) . . ? C223 Ru22 B206 79.98(12) . . ? C221 Ru22 B206 107.45(12) . . ? C201 Ru22 B206 83.59(12) . . ? C222 Ru22 B209 105.24(13) . . ? C223 Ru22 B209 82.55(13) . . ? C221 Ru22 B209 159.75(12) . . ? C201 Ru22 B209 83.68(12) . . ? B206 Ru22 B209 52.62(12) . . ? C222 Ru22 B203 142.41(13) . . ? C223 Ru22 B203 122.58(12) . . ? C221 Ru22 B203 87.51(12) . . ? C201 Ru22 B203 44.43(11) . . ? B206 Ru22 B203 46.67(12) . . ? B209 Ru22 B203 80.12(12) . . ? C222 Ru22 B205 86.00(12) . . ? C223 Ru22 B205 126.90(12) . . ? C221 Ru22 B205 142.13(12) . . ? C201 Ru22 B205 44.25(11) . . ? B206 Ru22 B205 79.95(12) . . ? B209 Ru22 B205 46.83(12) . . ? B203 Ru22 B205 70.59(12) . . ? O201 C201 B204 119.4(2) . . ? O201 C201 B205 126.8(2) . . ? B204 C201 B205 69.9(2) . . ? O201 C201 B203 126.9(2) . . ? B204 C201 B203 69.6(2) . . ? B205 C201 B203 105.9(2) . . ? O201 C201 Ru22 121.38(19) . . ? B204 C201 Ru22 119.25(19) . . ? B205 C201 Ru22 75.02(16) . . ? B203 C201 Ru22 74.72(16) . . ? C201 B203 B207 107.1(2) . . ? C201 B203 B206 113.7(2) . . ? B207 B203 B206 59.60(18) . . ? C201 B203 B204 53.26(17) . . ? B207 B203 B204 58.46(17) . . ? B206 B203 B204 102.3(2) . . ? C201 B203 Ru22 60.85(15) . . ? B207 B203 Ru22 111.75(19) . . ? B206 B203 Ru22 66.57(15) . . ? B204 B203 Ru22 99.08(18) . . ? C201 B204 B207 111.6(2) . . ? C201 B204 B208 111.6(2) . . ? B207 B204 B208 61.27(18) . . ? C201 B204 B203 57.13(18) . . ? B207 B204 B203 59.56(18) . . ? B208 B204 B203 102.8(2) . . ? C201 B204 B205 56.92(18) . . ? B207 B204 B205 102.7(2) . . ? B208 B204 B205 59.61(18) . . ? B203 B204 B205 91.1(2) . . ? C201 B205 B208 107.3(2) . . ? C201 B205 B209 113.6(2) . . ? B208 B205 B209 59.74(19) . . ? C201 B205 B204 53.23(17) . . ? B208 B205 B204 58.60(18) . . ? B209 B205 B204 102.3(2) . . ? C201 B205 Ru22 60.73(15) . . ? B208 B205 Ru22 111.65(19) . . ? B209 B205 Ru22 66.37(15) . . ? B204 B205 Ru22 98.76(18) . . ? C210 B206 B207 55.49(18) . . ? C210 B206 B203 108.1(2) . . ? B207 B206 B203 60.16(18) . . ? C210 B206 B209 50.62(17) . . ? B207 B206 B209 87.1(2) . . ? B203 B206 B209 100.1(2) . . ? C210 B206 Ru22 112.4(2) . . ? B207 B206 Ru22 112.3(2) . . ? B203 B206 Ru22 66.76(15) . . ? B209 B206 Ru22 63.73(13) . . ? C210 B207 B204 108.2(2) . . ? C210 B207 B206 55.87(19) . . ? B204 B207 B206 105.3(2) . . ? C210 B207 B203 108.5(2) . . ? B204 B207 B203 61.98(18) . . ? B206 B207 B203 60.25(18) . . ? C210 B207 B208 54.75(19) . . ? B204 B207 B208 59.61(18) . . ? B206 B207 B208 93.3(2) . . ? B203 B207 B208 103.4(2) . . ? C210 B208 B204 108.0(2) . . ? C210 B208 B209 55.59(19) . . ? B204 B208 B209 105.0(2) . . ? C210 B208 B205 108.2(2) . . ? B204 B208 B205 61.80(18) . . ? B209 B208 B205 60.20(18) . . ? C210 B208 B207 55.04(19) . . ? B204 B208 B207 59.11(18) . . ? B209 B208 B207 93.0(2) . . ? B205 B208 B207 102.8(2) . . ? C210 B209 B208 55.04(19) . . ? C210 B209 B205 107.6(3) . . ? B208 B209 B205 60.05(18) . . ? C210 B209 B206 50.72(17) . . ? B208 B209 B206 86.7(2) . . ? B205 B209 B206 99.7(2) . . ? C210 B209 Ru22 112.5(2) . . ? B208 B209 Ru22 112.2(2) . . ? B205 B209 Ru22 66.81(14) . . ? B206 B209 Ru22 63.65(13) . . ? B208 C210 B207 70.2(2) . . ? B208 C210 B209 69.4(2) . . ? B207 C210 B209 111.7(2) . . ? B208 C210 B206 111.8(2) . . ? B207 C210 B206 68.6(2) . . ? B209 C210 B206 78.7(2) . . ? O221 C221 Ru22 176.3(3) . . ? O222 C222 Ru22 174.7(3) . . ? O223 C223 Ru22 174.2(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O101 0.84 2.25 3.069(3) 165.6 . O101 H101 O201 0.84 2.30 3.134(3) 175.7 1_445 O201 H201 O1 0.84 2.14 2.971(3) 170.6 1_565 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.765 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.116 #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 609675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H39 B7 Mn N O4 P2' _chemical_formula_weight 802.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.972(2) _cell_length_b 15.004(3) _cell_length_c 17.410(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.022(6) _cell_angle_gamma 90.00 _cell_volume 3895.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5539 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.16 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 0.945 _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 X8 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 45746 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 29.67 _reflns_number_total 10928 _reflns_number_gt 8438 _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^)+(0.0478P)^2^+2.7361P] 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 10928 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.29601(13) 0.68344(13) 0.21604(11) 0.0205(4) Uani 1 1 d . . . O1 O 0.37556(10) 0.70200(11) 0.26153(9) 0.0299(3) Uani 1 1 d . . . H1 H 0.3751(17) 0.7605(19) 0.2641(14) 0.036 Uiso 1 1 d . . . Mn2 Mn 0.236225(19) 0.564766(19) 0.217891(15) 0.01634(8) Uani 1 1 d . . . B3 B 0.28931(15) 0.65075(15) 0.12720(12) 0.0200(4) Uani 1 1 d . . . H3 H 0.3497(15) 0.6413(15) 0.1008(13) 0.024 Uiso 1 1 d . . . B4 B 0.25429(16) 0.76145(15) 0.16068(13) 0.0221(4) Uani 1 1 d . . . H4 H 0.2906(15) 0.8278(15) 0.1598(13) 0.027 Uiso 1 1 d . . . B5 B 0.19551(16) 0.70632(15) 0.23745(12) 0.0214(4) Uani 1 1 d . . . H5 H 0.1915(15) 0.7377(15) 0.2947(13) 0.026 Uiso 1 1 d . . . B6 B 0.18273(15) 0.59895(15) 0.09953(12) 0.0205(4) Uani 1 1 d . . . H6 H 0.1733(15) 0.5485(15) 0.0588(13) 0.025 Uiso 1 1 d . . . B7 B 0.20043(16) 0.71544(15) 0.07489(13) 0.0214(4) Uani 1 1 d . . . H7 H 0.2069(15) 0.7446(15) 0.0199(13) 0.026 Uiso 1 1 d . . . B8 B 0.13487(16) 0.75452(16) 0.15228(13) 0.0235(5) Uani 1 1 d . . . H8 H 0.0924(16) 0.8110(16) 0.1548(13) 0.028 Uiso 1 1 d . . . B9 B 0.11276(15) 0.64049(16) 0.18241(13) 0.0213(4) Uani 1 1 d . . . H9 H 0.0529(15) 0.6173(15) 0.2017(13) 0.026 Uiso 1 1 d . . . C10 C 0.10730(14) 0.67538(14) 0.09469(11) 0.0229(4) Uani 1 1 d . . . H10 H 0.0506(16) 0.6744(15) 0.0566(13) 0.027 Uiso 1 1 d . . . C21 C 0.33288(13) 0.49584(13) 0.21007(11) 0.0210(4) Uani 1 1 d . . . O21 O 0.39391(10) 0.45126(10) 0.20211(9) 0.0290(3) Uani 1 1 d . . . C22 C 0.23772(13) 0.54869(13) 0.31990(11) 0.0211(4) Uani 1 1 d . . . O22 O 0.23547(11) 0.53920(11) 0.38526(8) 0.0322(4) Uani 1 1 d . . . C23 C 0.16640(13) 0.46973(14) 0.20012(11) 0.0206(4) Uani 1 1 d . . . O23 O 0.12136(10) 0.40806(10) 0.18766(9) 0.0305(3) Uani 1 1 d . . . P1 P 0.85438(3) 0.86656(3) 0.32929(2) 0.01232(10) Uani 1 1 d . . . N1 N 0.87894(10) 0.86873(10) 0.24270(8) 0.0147(3) Uani 1 1 d . . . C111 C 0.88106(11) 0.96990(12) 0.37775(10) 0.0146(3) Uani 1 1 d . . . C112 C 0.87005(13) 0.97886(14) 0.45622(11) 0.0213(4) Uani 1 1 d . . . H112 H 0.8481 0.9303 0.4841 0.026 Uiso 1 1 calc R . . C113 C 0.89133(14) 1.05881(14) 0.49328(11) 0.0255(4) Uani 1 1 d . . . H113 H 0.8831 1.0656 0.5465 0.031 Uiso 1 1 calc R . . C114 C 0.92467(14) 1.12884(14) 0.45255(12) 0.0263(4) Uani 1 1 d . . . H114 H 0.9392 1.1836 0.4780 0.032 Uiso 1 1 calc R . . C115 C 0.93693(14) 1.11977(13) 0.37527(12) 0.0251(4) Uani 1 1 d . . . H115 H 0.9606 1.1679 0.3480 0.030 Uiso 1 1 calc R . . C116 C 0.91466(13) 1.04031(12) 0.33746(11) 0.0189(4) Uani 1 1 d . . . H116 H 0.9224 1.0342 0.2841 0.023 Uiso 1 1 calc R . . C121 C 0.91852(12) 0.77952(12) 0.37923(10) 0.0139(3) Uani 1 1 d . . . C122 C 1.00180(12) 0.75491(12) 0.35584(10) 0.0162(3) Uani 1 1 d . . . H122 H 1.0250 0.7837 0.3133 0.019 Uiso 1 1 calc R . . C123 C 1.05028(13) 0.68797(13) 0.39533(11) 0.0199(4) Uani 1 1 d . . . H123 H 1.1071 0.6710 0.3797 0.024 Uiso 1 1 calc R . . C124 C 1.01650(13) 0.64552(13) 0.45746(11) 0.0209(4) Uani 1 1 d . . . H124 H 1.0500 0.5993 0.4838 0.025 Uiso 1 1 calc R . . C125 C 0.93451(14) 0.67010(14) 0.48106(11) 0.0223(4) Uani 1 1 d . . . H125 H 0.9117 0.6412 0.5238 0.027 Uiso 1 1 calc R . . C126 C 0.88546(13) 0.73706(13) 0.44226(10) 0.0196(4) Uani 1 1 d . . . H126 H 0.8290 0.7542 0.4586 0.023 Uiso 1 1 calc R . . C131 C 0.73942(12) 0.84034(12) 0.34151(9) 0.0139(3) Uani 1 1 d . . . C132 C 0.70840(13) 0.75549(12) 0.31960(11) 0.0186(4) Uani 1 1 d . . . H132 H 0.7477 0.7140 0.2988 0.022 Uiso 1 1 calc R . . C133 C 0.62089(13) 0.73174(13) 0.32808(11) 0.0210(4) Uani 1 1 d . . . H133 H 0.6002 0.6738 0.3136 0.025 Uiso 1 1 calc R . . C134 C 0.56298(13) 0.79228(14) 0.35778(11) 0.0216(4) Uani 1 1 d . . . H134 H 0.5029 0.7755 0.3642 0.026 Uiso 1 1 calc R . . C135 C 0.59258(13) 0.87677(14) 0.37802(11) 0.0220(4) Uani 1 1 d . . . H135 H 0.5525 0.9185 0.3974 0.026 Uiso 1 1 calc R . . C136 C 0.68090(12) 0.90110(13) 0.37016(10) 0.0175(4) Uani 1 1 d . . . H136 H 0.7012 0.9593 0.3844 0.021 Uiso 1 1 calc R . . P2 P 0.82858(3) 0.89083(3) 0.16127(2) 0.01226(10) Uani 1 1 d . . . C211 C 0.82985(12) 0.79448(12) 0.10026(10) 0.0155(3) Uani 1 1 d . . . C212 C 0.87016(13) 0.71678(13) 0.12863(12) 0.0211(4) Uani 1 1 d . . . H212 H 0.8951 0.7138 0.1807 0.025 Uiso 1 1 calc R . . C213 C 0.87406(15) 0.64324(14) 0.08072(14) 0.0291(5) Uani 1 1 d . . . H213 H 0.9009 0.5896 0.1003 0.035 Uiso 1 1 calc R . . C214 C 0.83934(16) 0.64758(15) 0.00520(14) 0.0330(5) Uani 1 1 d . . . H214 H 0.8424 0.5970 -0.0273 0.040 Uiso 1 1 calc R . . C215 C 0.80002(17) 0.72517(16) -0.02382(13) 0.0338(5) Uani 1 1 d . . . H215 H 0.7765 0.7281 -0.0762 0.041 Uiso 1 1 calc R . . C216 C 0.79496(15) 0.79848(14) 0.02352(11) 0.0246(4) Uani 1 1 d . . . H216 H 0.7676 0.8518 0.0037 0.030 Uiso 1 1 calc R . . C221 C 0.88458(12) 0.97837(12) 0.11445(10) 0.0147(3) Uani 1 1 d . . . C222 C 0.84189(13) 1.02197(13) 0.05058(10) 0.0192(4) Uani 1 1 d . . . H222 H 0.7811 1.0090 0.0343 0.023 Uiso 1 1 calc R . . C223 C 0.88846(15) 1.08404(13) 0.01114(11) 0.0237(4) Uani 1 1 d . . . H223 H 0.8601 1.1124 -0.0333 0.028 Uiso 1 1 calc R . . C224 C 0.97593(15) 1.10502(13) 0.03600(12) 0.0249(4) Uani 1 1 d . . . H224 H 1.0072 1.1484 0.0090 0.030 Uiso 1 1 calc R . . C225 C 1.01814(14) 1.06344(13) 0.09961(12) 0.0237(4) Uani 1 1 d . . . H225 H 1.0780 1.0791 0.1171 0.028 Uiso 1 1 calc R . . C226 C 0.97334(12) 0.99849(12) 0.13843(11) 0.0178(4) Uani 1 1 d . . . H226 H 1.0032 0.9680 0.1811 0.021 Uiso 1 1 calc R . . C231 C 0.71395(12) 0.92465(12) 0.16435(9) 0.0140(3) Uani 1 1 d . . . C232 C 0.64437(12) 0.86340(13) 0.15440(10) 0.0178(4) Uani 1 1 d . . . H232 H 0.6561 0.8038 0.1397 0.021 Uiso 1 1 calc R . . C233 C 0.55769(13) 0.88947(14) 0.16595(11) 0.0218(4) Uani 1 1 d . . . H233 H 0.5103 0.8473 0.1601 0.026 Uiso 1 1 calc R . . C234 C 0.53993(13) 0.97621(14) 0.18586(11) 0.0229(4) Uani 1 1 d . . . H234 H 0.4803 0.9938 0.1930 0.027 Uiso 1 1 calc R . . C235 C 0.60886(14) 1.03767(14) 0.19542(12) 0.0234(4) Uani 1 1 d . . . H235 H 0.5966 1.0975 0.2091 0.028 Uiso 1 1 calc R . . C236 C 0.69588(13) 1.01197(13) 0.18507(11) 0.0194(4) Uani 1 1 d . . . H236 H 0.7433 1.0540 0.1921 0.023 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 C1 0.0214(9) 0.0207(10) 0.0192(9) -0.0018(7) 0.0015(7) -0.0005(8) O1 0.0298(8) 0.0269(8) 0.0313(8) -0.0008(7) -0.0078(6) -0.0075(7) Mn2 0.01732(14) 0.01701(15) 0.01467(13) 0.00057(10) 0.00125(10) 0.00154(11) B3 0.0209(10) 0.0220(11) 0.0176(10) -0.0012(8) 0.0048(8) 0.0026(8) B4 0.0286(11) 0.0181(11) 0.0204(10) 0.0014(8) 0.0065(9) 0.0003(9) B5 0.0286(11) 0.0192(11) 0.0175(10) 0.0004(8) 0.0073(8) 0.0035(9) B6 0.0241(11) 0.0204(11) 0.0169(10) 0.0010(8) 0.0007(8) 0.0011(9) B7 0.0255(11) 0.0224(11) 0.0173(10) 0.0030(8) 0.0066(8) 0.0050(9) B8 0.0268(11) 0.0237(11) 0.0211(10) 0.0057(9) 0.0095(9) 0.0071(9) B9 0.0186(10) 0.0245(11) 0.0213(10) 0.0044(9) 0.0045(8) 0.0034(9) C10 0.0223(10) 0.0263(11) 0.0202(9) 0.0056(8) 0.0020(8) 0.0038(8) C21 0.0222(9) 0.0232(10) 0.0172(9) 0.0005(7) -0.0005(7) -0.0001(8) O21 0.0265(8) 0.0309(8) 0.0293(8) -0.0013(6) 0.0014(6) 0.0097(7) C22 0.0213(9) 0.0205(10) 0.0212(9) -0.0006(7) 0.0008(7) 0.0021(8) O22 0.0391(9) 0.0392(9) 0.0182(7) 0.0036(6) 0.0016(6) 0.0087(7) C23 0.0207(9) 0.0230(10) 0.0178(9) 0.0017(7) 0.0008(7) 0.0018(8) O23 0.0296(8) 0.0271(8) 0.0338(8) -0.0004(7) -0.0024(6) -0.0052(7) P1 0.0139(2) 0.0125(2) 0.01073(19) 0.00024(16) 0.00199(15) 0.00064(16) N1 0.0150(7) 0.0177(8) 0.0115(7) 0.0018(6) 0.0019(5) 0.0023(6) C111 0.0136(8) 0.0157(8) 0.0144(8) -0.0021(7) 0.0005(6) 0.0017(7) C112 0.0243(10) 0.0234(10) 0.0164(9) -0.0002(7) 0.0031(7) -0.0022(8) C113 0.0292(11) 0.0303(11) 0.0168(9) -0.0083(8) 0.0010(8) -0.0001(9) C114 0.0284(11) 0.0196(10) 0.0299(11) -0.0104(8) -0.0021(8) -0.0007(8) C115 0.0291(11) 0.0164(9) 0.0299(11) -0.0012(8) 0.0035(8) -0.0042(8) C116 0.0226(9) 0.0164(9) 0.0180(9) -0.0014(7) 0.0039(7) 0.0002(7) C121 0.0170(8) 0.0129(8) 0.0114(7) 0.0000(6) -0.0006(6) 0.0010(7) C122 0.0193(9) 0.0149(8) 0.0147(8) -0.0006(7) 0.0027(7) -0.0010(7) C123 0.0190(9) 0.0192(9) 0.0211(9) -0.0013(7) 0.0002(7) 0.0036(7) C124 0.0261(10) 0.0170(9) 0.0185(9) 0.0018(7) -0.0037(7) 0.0019(8) C125 0.0272(10) 0.0238(10) 0.0157(8) 0.0057(7) 0.0012(7) 0.0006(8) C126 0.0197(9) 0.0232(10) 0.0162(8) 0.0034(7) 0.0042(7) 0.0024(7) C131 0.0155(8) 0.0148(8) 0.0115(7) 0.0028(6) 0.0007(6) -0.0004(7) C132 0.0229(9) 0.0146(9) 0.0185(8) -0.0002(7) 0.0027(7) 0.0004(7) C133 0.0245(10) 0.0164(9) 0.0219(9) 0.0036(7) 0.0011(7) -0.0061(7) C134 0.0162(9) 0.0259(10) 0.0223(9) 0.0066(8) 0.0003(7) -0.0024(8) C135 0.0173(9) 0.0235(10) 0.0255(10) -0.0001(8) 0.0034(7) 0.0033(8) C136 0.0175(9) 0.0163(9) 0.0188(8) -0.0012(7) 0.0017(7) -0.0003(7) P2 0.0147(2) 0.0115(2) 0.01070(19) 0.00011(16) 0.00153(15) 0.00103(16) C211 0.0179(8) 0.0129(8) 0.0160(8) -0.0013(7) 0.0038(7) 0.0000(7) C212 0.0216(9) 0.0168(9) 0.0250(10) -0.0009(7) 0.0020(8) 0.0000(7) C213 0.0282(11) 0.0151(10) 0.0440(13) -0.0049(9) 0.0031(9) 0.0016(8) C214 0.0345(12) 0.0233(11) 0.0419(13) -0.0192(10) 0.0067(10) -0.0016(9) C215 0.0443(14) 0.0335(12) 0.0230(10) -0.0125(9) -0.0006(9) -0.0034(10) C216 0.0349(11) 0.0203(10) 0.0178(9) -0.0033(8) -0.0019(8) 0.0018(8) C221 0.0199(9) 0.0114(8) 0.0134(8) -0.0015(6) 0.0056(6) 0.0003(7) C222 0.0264(10) 0.0175(9) 0.0139(8) 0.0000(7) 0.0029(7) 0.0031(7) C223 0.0379(12) 0.0163(9) 0.0181(9) 0.0039(7) 0.0094(8) 0.0046(8) C224 0.0369(12) 0.0147(9) 0.0260(10) -0.0019(8) 0.0195(9) -0.0023(8) C225 0.0210(9) 0.0212(10) 0.0306(10) -0.0074(8) 0.0121(8) -0.0036(8) C226 0.0197(9) 0.0164(9) 0.0180(8) -0.0032(7) 0.0050(7) 0.0014(7) C231 0.0150(8) 0.0159(8) 0.0109(7) 0.0023(6) 0.0007(6) 0.0029(7) C232 0.0208(9) 0.0167(9) 0.0157(8) -0.0001(7) 0.0007(7) 0.0002(7) C233 0.0176(9) 0.0269(10) 0.0204(9) 0.0014(8) -0.0001(7) -0.0029(8) C234 0.0177(9) 0.0315(11) 0.0198(9) 0.0055(8) 0.0045(7) 0.0077(8) C235 0.0250(10) 0.0191(10) 0.0267(10) 0.0030(8) 0.0063(8) 0.0084(8) C236 0.0206(9) 0.0154(9) 0.0225(9) 0.0009(7) 0.0031(7) 0.0018(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 C1 O1 1.399(2) . ? C1 B4 1.607(3) . ? C1 B3 1.617(3) . ? C1 B5 1.618(3) . ? C1 Mn2 1.994(2) . ? O1 H1 0.88(3) . ? Mn2 C23 1.779(2) . ? Mn2 C22 1.790(2) . ? Mn2 C21 1.793(2) . ? Mn2 B6 2.205(2) . ? Mn2 B9 2.211(2) . ? Mn2 B3 2.238(2) . ? Mn2 B5 2.244(2) . ? B3 B6 1.802(3) . ? B3 B7 1.825(3) . ? B3 B4 1.851(3) . ? B4 B7 1.774(3) . ? B4 B8 1.784(3) . ? B4 B5 1.858(3) . ? B5 B9 1.795(3) . ? B5 B8 1.819(3) . ? B6 C10 1.607(3) . ? B6 B7 1.825(3) . ? B6 B9 1.958(3) . ? B7 C10 1.584(3) . ? B7 B8 1.832(3) . ? B8 C10 1.585(3) . ? B8 B9 1.828(3) . ? B9 C10 1.610(3) . ? C21 O21 1.151(2) . ? C22 O22 1.150(2) . ? C23 O23 1.154(2) . ? P1 N1 1.5830(15) . ? P1 C111 1.7935(18) . ? P1 C131 1.7963(18) . ? P1 C121 1.7993(18) . ? N1 P2 1.5815(15) . ? C111 C116 1.387(3) . ? C111 C112 1.397(2) . ? C112 C113 1.386(3) . ? C113 C114 1.385(3) . ? C114 C115 1.381(3) . ? C115 C116 1.388(3) . ? C121 C122 1.395(3) . ? C121 C126 1.396(2) . ? C122 C123 1.386(3) . ? C123 C124 1.388(3) . ? C124 C125 1.378(3) . ? C125 C126 1.385(3) . ? C131 C136 1.387(3) . ? C131 C132 1.397(3) . ? C132 C133 1.378(3) . ? C133 C134 1.387(3) . ? C134 C135 1.378(3) . ? C135 C136 1.390(3) . ? P2 C221 1.7922(18) . ? P2 C211 1.7949(18) . ? P2 C231 1.7950(18) . ? C211 C212 1.384(3) . ? C211 C216 1.393(3) . ? C212 C213 1.387(3) . ? C213 C214 1.372(3) . ? C214 C215 1.380(3) . ? C215 C216 1.380(3) . ? C221 C226 1.391(3) . ? C221 C222 1.396(2) . ? C222 C223 1.382(3) . ? C223 C224 1.379(3) . ? C224 C225 1.376(3) . ? C225 C226 1.391(3) . ? C231 C232 1.389(3) . ? C231 C236 1.392(3) . ? C232 C233 1.387(3) . ? C233 C234 1.379(3) . ? C234 C235 1.383(3) . ? C235 C236 1.386(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 B4 117.47(17) . . ? O1 C1 B3 125.45(17) . . ? B4 C1 B3 70.07(14) . . ? O1 C1 B5 126.15(17) . . ? B4 C1 B5 70.33(14) . . ? B3 C1 B5 107.67(16) . . ? O1 C1 Mn2 121.97(14) . . ? B4 C1 Mn2 120.56(14) . . ? B3 C1 Mn2 75.78(11) . . ? B5 C1 Mn2 75.99(11) . . ? H1 O1 C1 102.6(17) . . ? C23 Mn2 C22 91.18(9) . . ? C23 Mn2 C21 89.45(9) . . ? C22 Mn2 C21 93.30(9) . . ? C23 Mn2 C1 166.04(8) . . ? C22 Mn2 C1 99.77(8) . . ? C21 Mn2 C1 98.47(9) . . ? C23 Mn2 B6 82.19(9) . . ? C22 Mn2 B6 158.48(9) . . ? C21 Mn2 B6 107.02(9) . . ? C1 Mn2 B6 84.50(8) . . ? C23 Mn2 B9 84.21(9) . . ? C22 Mn2 B9 106.49(9) . . ? C21 Mn2 B9 159.29(8) . . ? C1 Mn2 B9 84.39(8) . . ? B6 Mn2 B9 52.63(8) . . ? C23 Mn2 B3 125.37(8) . . ? C22 Mn2 B3 143.43(9) . . ? C21 Mn2 B3 86.56(9) . . ? C1 Mn2 B3 44.47(8) . . ? B6 Mn2 B3 47.85(8) . . ? B9 Mn2 B3 81.18(8) . . ? C23 Mn2 B5 128.44(9) . . ? C22 Mn2 B5 87.53(8) . . ? C21 Mn2 B5 142.10(9) . . ? C1 Mn2 B5 44.42(8) . . ? B6 Mn2 B5 80.82(8) . . ? B9 Mn2 B5 47.51(9) . . ? B3 Mn2 B5 71.31(8) . . ? C1 B3 B6 111.45(16) . . ? C1 B3 B7 107.30(15) . . ? B6 B3 B7 60.40(13) . . ? C1 B3 B4 54.71(12) . . ? B6 B3 B4 101.69(15) . . ? B7 B3 B4 57.70(12) . . ? C1 B3 Mn2 59.75(10) . . ? B6 B3 Mn2 65.11(10) . . ? B7 B3 Mn2 111.73(13) . . ? B4 B3 Mn2 99.62(12) . . ? C1 B4 B7 110.22(16) . . ? C1 B4 B8 109.93(16) . . ? B7 B4 B8 61.96(13) . . ? C1 B4 B3 55.22(12) . . ? B7 B4 B3 60.41(12) . . ? B8 B4 B3 103.38(16) . . ? C1 B4 B5 55.12(12) . . ? B7 B4 B5 102.91(16) . . ? B8 B4 B5 59.90(13) . . ? B3 B4 B5 89.55(14) . . ? C1 B5 B9 111.88(16) . . ? C1 B5 B8 107.71(15) . . ? B9 B5 B8 60.77(13) . . ? C1 B5 B4 54.55(12) . . ? B9 B5 B4 102.08(15) . . ? B8 B5 B4 58.04(12) . . ? C1 B5 Mn2 59.59(10) . . ? B9 B5 Mn2 65.30(10) . . ? B8 B5 Mn2 112.05(13) . . ? B4 B5 Mn2 99.21(12) . . ? C10 B6 B3 107.95(17) . . ? C10 B6 B7 54.53(12) . . ? B3 B6 B7 60.42(13) . . ? C10 B6 B9 52.58(12) . . ? B3 B6 B9 100.62(14) . . ? B7 B6 B9 88.08(14) . . ? C10 B6 Mn2 114.28(14) . . ? B3 B6 Mn2 67.04(10) . . ? B7 B6 Mn2 113.22(13) . . ? B9 B6 Mn2 63.85(9) . . ? C10 B7 B4 107.96(16) . . ? C10 B7 B6 55.70(13) . . ? B4 B7 B6 103.85(15) . . ? C10 B7 B3 107.87(16) . . ? B4 B7 B3 61.89(13) . . ? B6 B7 B3 59.18(12) . . ? C10 B7 B8 54.73(13) . . ? B4 B7 B8 59.30(13) . . ? B6 B7 B8 92.03(14) . . ? B3 B7 B8 102.56(15) . . ? C10 B8 B4 107.40(16) . . ? C10 B8 B5 107.54(16) . . ? B4 B8 B5 62.06(13) . . ? C10 B8 B9 55.72(13) . . ? B4 B8 B9 103.67(15) . . ? B5 B8 B9 58.95(12) . . ? C10 B8 B7 54.66(13) . . ? B4 B8 B7 58.75(13) . . ? B5 B8 B7 102.18(15) . . ? B9 B8 B7 91.93(15) . . ? C10 B9 B5 107.64(16) . . ? C10 B9 B8 54.47(13) . . ? B5 B9 B8 60.28(13) . . ? C10 B9 B6 52.44(12) . . ? B5 B9 B6 100.36(14) . . ? B8 B9 B6 87.97(13) . . ? C10 B9 Mn2 113.83(14) . . ? B5 B9 Mn2 67.20(10) . . ? B8 B9 Mn2 113.14(13) . . ? B6 B9 Mn2 63.52(9) . . ? B7 C10 B8 70.61(15) . . ? B7 C10 B6 69.76(14) . . ? B8 C10 B6 111.01(17) . . ? B7 C10 B9 110.94(17) . . ? B8 C10 B9 69.81(14) . . ? B6 C10 B9 74.99(14) . . ? O21 C21 Mn2 177.39(17) . . ? O22 C22 Mn2 177.54(18) . . ? O23 C23 Mn2 179.15(18) . . ? N1 P1 C111 111.69(8) . . ? N1 P1 C131 114.97(8) . . ? C111 P1 C131 108.05(8) . . ? N1 P1 C121 108.45(8) . . ? C111 P1 C121 108.22(8) . . ? C131 P1 C121 105.08(8) . . ? P2 N1 P1 136.53(10) . . ? C116 C111 C112 120.04(17) . . ? C116 C111 P1 119.76(13) . . ? C112 C111 P1 120.19(14) . . ? C113 C112 C111 119.77(18) . . ? C114 C113 C112 119.79(18) . . ? C115 C114 C113 120.59(18) . . ? C114 C115 C116 119.98(19) . . ? C111 C116 C115 119.81(18) . . ? C122 C121 C126 119.74(16) . . ? C122 C121 P1 120.27(13) . . ? C126 C121 P1 119.99(14) . . ? C123 C122 C121 119.33(17) . . ? C122 C123 C124 120.54(18) . . ? C125 C124 C123 120.28(18) . . ? C124 C125 C126 119.78(18) . . ? C125 C126 C121 120.32(17) . . ? C136 C131 C132 119.46(17) . . ? C136 C131 P1 122.73(14) . . ? C132 C131 P1 117.80(14) . . ? C133 C132 C131 120.19(18) . . ? C132 C133 C134 120.13(18) . . ? C135 C134 C133 120.01(18) . . ? C134 C135 C136 120.24(18) . . ? C131 C136 C135 119.94(18) . . ? N1 P2 C221 110.86(8) . . ? N1 P2 C211 109.43(8) . . ? C221 P2 C211 106.94(8) . . ? N1 P2 C231 114.50(8) . . ? C221 P2 C231 107.04(8) . . ? C211 P2 C231 107.76(8) . . ? C212 C211 C216 119.59(17) . . ? C212 C211 P2 119.61(14) . . ? C216 C211 P2 120.70(14) . . ? C211 C212 C213 119.70(19) . . ? C214 C213 C212 120.4(2) . . ? C213 C214 C215 120.29(19) . . ? C214 C215 C216 119.8(2) . . ? C215 C216 C211 120.19(19) . . ? C226 C221 C222 119.75(17) . . ? C226 C221 P2 119.69(14) . . ? C222 C221 P2 120.40(14) . . ? C223 C222 C221 119.74(19) . . ? C224 C223 C222 120.30(19) . . ? C225 C224 C223 120.38(18) . . ? C224 C225 C226 120.11(19) . . ? C221 C226 C225 119.66(18) . . ? C232 C231 C236 119.64(17) . . ? C232 C231 P2 121.20(14) . . ? C236 C231 P2 118.81(14) . . ? C233 C232 C231 119.77(18) . . ? C234 C233 C232 120.41(19) . . ? C233 C234 C235 120.09(18) . . ? C234 C235 C236 119.93(19) . . ? C235 C236 C231 120.14(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.519 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.073 #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 609676' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H39 B7 N O4 P2 Re' _chemical_formula_weight 933.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 15.098(3) _cell_length_b 15.289(3) _cell_length_c 17.297(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.085(9) _cell_angle_gamma 90.00 _cell_volume 3953.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9749 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.20 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 3.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.798 _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 X8 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 44201 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 29.69 _reflns_number_total 10667 _reflns_number_gt 7985 _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^)+(0.0166P)^2^+2.0053P] 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 10667 _refine_ls_number_parameters 530 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1054(2) 0.4266(2) 0.11391(19) 0.0172(8) Uani 1 1 d . . . O1 O 0.03656(16) 0.48287(17) 0.08134(14) 0.0258(6) Uani 1 1 d . . . H1 H 0.0000 0.4549 0.0495 0.031 Uiso 1 1 calc R . . Re1 Re 0.205616(9) 0.473460(10) 0.201721(7) 0.01680(5) Uani 1 1 d . . . B3 B 0.1946(3) 0.4064(3) 0.0755(2) 0.0219(10) Uani 1 1 d . . . H3 H 0.205(2) 0.439(2) 0.028(2) 0.026 Uiso 1 1 d . . . B4 B 0.1025(3) 0.3290(3) 0.0807(2) 0.0221(10) Uani 1 1 d . . . H4 H 0.049(2) 0.315(2) 0.037(2) 0.026 Uiso 1 1 d . . . B5 B 0.1000(3) 0.3565(3) 0.1839(2) 0.0194(9) Uani 1 1 d . . . H5 H 0.043(2) 0.352(2) 0.212(2) 0.023 Uiso 1 1 d . . . B6 B 0.2822(3) 0.3598(3) 0.1487(3) 0.0288(11) Uani 1 1 d . . . H6 H 0.353(3) 0.368(2) 0.147(2) 0.035 Uiso 1 1 d . . . B7 B 0.2128(3) 0.2898(3) 0.0785(3) 0.0301(11) Uani 1 1 d . . . H7 H 0.232(2) 0.250(3) 0.030(2) 0.036 Uiso 1 1 d . . . B8 B 0.1466(3) 0.2548(3) 0.1543(3) 0.0288(11) Uani 1 1 d . . . H8 H 0.114(2) 0.193(3) 0.163(2) 0.035 Uiso 1 1 d . . . B9 B 0.2142(3) 0.3230(3) 0.2266(3) 0.0271(11) Uani 1 1 d . . . H9 H 0.226(2) 0.304(2) 0.290(2) 0.033 Uiso 1 1 d . . . C10 C 0.2521(3) 0.2622(3) 0.1646(3) 0.0334(11) Uani 1 1 d . . . H10 H 0.300(3) 0.215(3) 0.172(2) 0.040 Uiso 1 1 d . . . C21 C 0.1478(2) 0.5859(3) 0.1942(2) 0.0274(10) Uani 1 1 d . . . O21 O 0.11388(18) 0.6530(2) 0.18879(19) 0.0418(9) Uani 1 1 d . . . C22 C 0.3181(2) 0.5308(3) 0.2028(2) 0.0254(9) Uani 1 1 d . . . O22 O 0.38620(17) 0.5636(2) 0.19851(16) 0.0350(7) Uani 1 1 d . . . C23 C 0.2165(2) 0.4815(3) 0.3132(2) 0.0279(10) Uani 1 1 d . . . O23 O 0.2189(2) 0.4813(2) 0.37991(16) 0.0443(9) Uani 1 1 d . . . P1 P 0.63680(5) 0.63861(6) 0.17311(5) 0.01315(19) Uani 1 1 d . . . N1 N 0.61532(17) 0.63120(19) 0.25938(15) 0.0140(6) Uani 1 1 d . . . C111 C 0.6139(2) 0.5383(2) 0.12093(19) 0.0153(8) Uani 1 1 d . . . C112 C 0.6245(2) 0.5323(3) 0.0423(2) 0.0204(8) Uani 1 1 d . . . H112 H 0.6420 0.5821 0.0154 0.024 Uiso 1 1 calc R . . C113 C 0.6094(2) 0.4539(3) 0.0040(2) 0.0258(10) Uani 1 1 d . . . H113 H 0.6172 0.4495 -0.0495 0.031 Uiso 1 1 calc R . . C114 C 0.5833(2) 0.3820(3) 0.0421(2) 0.0278(10) Uani 1 1 d . . . H114 H 0.5731 0.3280 0.0151 0.033 Uiso 1 1 calc R . . C115 C 0.5718(2) 0.3876(3) 0.1194(2) 0.0273(9) Uani 1 1 d . . . H115 H 0.5536 0.3375 0.1456 0.033 Uiso 1 1 calc R . . C116 C 0.5866(2) 0.4657(2) 0.1589(2) 0.0217(8) Uani 1 1 d . . . H116 H 0.5781 0.4696 0.2122 0.026 Uiso 1 1 calc R . . C121 C 0.7493(2) 0.6706(2) 0.16475(18) 0.0139(7) Uani 1 1 d . . . C122 C 0.8112(2) 0.6133(2) 0.14199(18) 0.0162(8) Uani 1 1 d . . . H122 H 0.7945 0.5544 0.1296 0.019 Uiso 1 1 calc R . . C123 C 0.8970(2) 0.6409(3) 0.1372(2) 0.0214(9) Uani 1 1 d . . . H123 H 0.9394 0.6012 0.1213 0.026 Uiso 1 1 calc R . . C124 C 0.9215(2) 0.7260(3) 0.1554(2) 0.0225(9) Uani 1 1 d . . . H124 H 0.9806 0.7452 0.1515 0.027 Uiso 1 1 calc R . . C125 C 0.8603(2) 0.7832(2) 0.1794(2) 0.0211(8) Uani 1 1 d . . . H125 H 0.8774 0.8418 0.1924 0.025 Uiso 1 1 calc R . . C126 C 0.7748(2) 0.7560(2) 0.1847(2) 0.0179(8) Uani 1 1 d . . . H126 H 0.7330 0.7955 0.2018 0.021 Uiso 1 1 calc R . . C131 C 0.5679(2) 0.7230(2) 0.12365(18) 0.0145(8) Uani 1 1 d . . . C132 C 0.5942(2) 0.7656(2) 0.05989(19) 0.0201(8) Uani 1 1 d . . . H132 H 0.6487 0.7499 0.0419 0.024 Uiso 1 1 calc R . . C133 C 0.5412(2) 0.8311(3) 0.0223(2) 0.0243(9) Uani 1 1 d . . . H133 H 0.5596 0.8609 -0.0210 0.029 Uiso 1 1 calc R . . C134 C 0.4620(2) 0.8529(3) 0.0477(2) 0.0238(9) Uani 1 1 d . . . H134 H 0.4254 0.8975 0.0218 0.029 Uiso 1 1 calc R . . C135 C 0.4354(2) 0.8102(2) 0.1105(2) 0.0206(8) Uani 1 1 d . . . H135 H 0.3803 0.8255 0.1276 0.025 Uiso 1 1 calc R . . C136 C 0.4878(2) 0.7456(2) 0.14901(19) 0.0166(8) Uani 1 1 d . . . H136 H 0.4692 0.7168 0.1926 0.020 Uiso 1 1 calc R . . P2 P 0.66876(6) 0.60971(6) 0.34231(5) 0.01323(19) Uani 1 1 d . . . C211 C 0.7825(2) 0.5763(2) 0.33948(18) 0.0147(8) Uani 1 1 d . . . C212 C 0.7998(2) 0.4909(3) 0.3198(2) 0.0214(9) Uani 1 1 d . . . H212 H 0.7529 0.4489 0.3145 0.026 Uiso 1 1 calc R . . C213 C 0.8848(2) 0.4666(3) 0.3079(2) 0.0258(9) Uani 1 1 d . . . H213 H 0.8965 0.4076 0.2952 0.031 Uiso 1 1 calc R . . C214 C 0.9526(2) 0.5270(3) 0.3143(2) 0.0246(9) Uani 1 1 d . . . H214 H 1.0108 0.5104 0.3051 0.030 Uiso 1 1 calc R . . C215 C 0.9355(2) 0.6122(3) 0.3343(2) 0.0217(9) Uani 1 1 d . . . H215 H 0.9823 0.6542 0.3386 0.026 Uiso 1 1 calc R . . C216 C 0.8513(2) 0.6368(2) 0.34787(19) 0.0168(8) Uani 1 1 d . . . H216 H 0.8405 0.6951 0.3630 0.020 Uiso 1 1 calc R . . C221 C 0.6135(2) 0.5245(2) 0.38710(19) 0.0158(7) Uani 1 1 d . . . C222 C 0.5241(2) 0.5067(2) 0.3598(2) 0.0193(8) Uani 1 1 d . . . H222 H 0.4938 0.5388 0.3171 0.023 Uiso 1 1 calc R . . C223 C 0.4796(3) 0.4423(3) 0.3950(2) 0.0267(9) Uani 1 1 d . . . H223 H 0.4190 0.4292 0.3755 0.032 Uiso 1 1 calc R . . C224 C 0.5226(3) 0.3974(3) 0.4579(2) 0.0291(9) Uani 1 1 d . . . H224 H 0.4916 0.3534 0.4823 0.035 Uiso 1 1 calc R . . C225 C 0.6107(3) 0.4158(3) 0.4858(2) 0.0281(9) Uani 1 1 d . . . H225 H 0.6397 0.3850 0.5300 0.034 Uiso 1 1 calc R . . C226 C 0.6567(2) 0.4778(2) 0.4508(2) 0.0205(8) Uani 1 1 d . . . H226 H 0.7178 0.4890 0.4697 0.025 Uiso 1 1 calc R . . C231 C 0.6724(2) 0.7050(2) 0.4034(2) 0.0162(8) Uani 1 1 d . . . C232 C 0.6450(2) 0.7843(2) 0.3704(2) 0.0191(8) Uani 1 1 d . . . H232 H 0.6236 0.7878 0.3162 0.023 Uiso 1 1 calc R . . C233 C 0.6487(2) 0.8580(3) 0.4159(2) 0.0263(9) Uani 1 1 d . . . H233 H 0.6306 0.9127 0.3929 0.032 Uiso 1 1 calc R . . C234 C 0.6783(2) 0.8531(3) 0.4946(2) 0.0279(10) Uani 1 1 d . . . H234 H 0.6803 0.9042 0.5260 0.033 Uiso 1 1 calc R . . C235 C 0.7049(3) 0.7744(3) 0.5274(2) 0.0305(10) Uani 1 1 d . . . H235 H 0.7255 0.7711 0.5818 0.037 Uiso 1 1 calc R . . C236 C 0.7022(2) 0.7000(3) 0.4828(2) 0.0249(9) Uani 1 1 d . . . H236 H 0.7206 0.6455 0.5061 0.030 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 C1 0.0184(17) 0.019(2) 0.0136(16) 0.0002(15) -0.0003(13) -0.0002(15) O1 0.0268(13) 0.0255(17) 0.0217(13) -0.0004(12) -0.0087(11) 0.0015(12) Re1 0.01480(7) 0.02300(10) 0.01202(7) 0.00076(6) -0.00010(5) -0.00128(6) B3 0.031(2) 0.023(3) 0.0119(19) 0.0047(18) 0.0060(17) -0.008(2) B4 0.028(2) 0.025(3) 0.016(2) -0.0038(18) 0.0121(17) -0.0076(19) B5 0.024(2) 0.019(3) 0.0169(19) 0.0006(17) 0.0056(17) -0.0029(18) B6 0.024(2) 0.032(3) 0.032(2) 0.003(2) 0.009(2) 0.005(2) B7 0.035(3) 0.023(3) 0.036(3) -0.001(2) 0.020(2) -0.003(2) B8 0.041(3) 0.019(3) 0.030(2) -0.001(2) 0.016(2) 0.003(2) B9 0.029(2) 0.025(3) 0.028(2) 0.010(2) 0.0062(19) 0.008(2) C10 0.032(2) 0.025(3) 0.045(3) 0.006(2) 0.012(2) 0.0137(19) C21 0.0154(18) 0.039(3) 0.026(2) -0.008(2) -0.0018(15) -0.0065(19) O21 0.0279(15) 0.0274(19) 0.066(2) -0.0128(16) -0.0075(15) 0.0072(14) C22 0.0242(19) 0.033(3) 0.0178(18) -0.0024(18) -0.0010(15) 0.0034(19) O22 0.0238(14) 0.049(2) 0.0324(15) -0.0030(14) 0.0032(12) -0.0136(14) C23 0.0256(19) 0.037(3) 0.0195(19) -0.0020(18) -0.0020(16) -0.0103(18) O23 0.0519(19) 0.064(2) 0.0158(14) -0.0031(15) 0.0006(13) -0.0235(17) P1 0.0147(4) 0.0134(5) 0.0112(4) -0.0003(4) 0.0013(3) 0.0015(4) N1 0.0132(13) 0.0172(18) 0.0120(13) 0.0003(12) 0.0029(11) 0.0017(12) C111 0.0128(15) 0.015(2) 0.0176(17) -0.0032(15) 0.0022(13) 0.0035(14) C112 0.0185(17) 0.024(2) 0.0183(17) -0.0029(17) 0.0026(14) -0.0022(16) C113 0.0237(19) 0.034(3) 0.0189(18) -0.0072(18) -0.0001(15) 0.0004(17) C114 0.025(2) 0.022(2) 0.034(2) -0.0162(19) -0.0032(17) 0.0012(17) C115 0.032(2) 0.017(2) 0.033(2) 0.0004(18) 0.0046(18) -0.0050(17) C116 0.0260(19) 0.018(2) 0.0218(18) -0.0039(16) 0.0050(15) -0.0006(16) C121 0.0145(16) 0.013(2) 0.0139(16) 0.0049(14) 0.0020(13) -0.0009(14) C122 0.0173(16) 0.016(2) 0.0149(16) 0.0002(14) 0.0027(13) 0.0016(15) C123 0.0173(17) 0.029(3) 0.0197(18) 0.0035(16) 0.0077(14) 0.0051(16) C124 0.0157(17) 0.027(3) 0.0244(19) 0.0094(17) 0.0017(15) 0.0013(16) C125 0.0230(18) 0.012(2) 0.028(2) 0.0030(16) 0.0017(16) -0.0018(16) C126 0.0152(17) 0.016(2) 0.0226(18) 0.0010(16) 0.0032(14) 0.0044(15) C131 0.0166(16) 0.014(2) 0.0124(16) -0.0028(14) 0.0009(13) 0.0002(14) C132 0.0178(17) 0.026(2) 0.0168(17) 0.0027(16) 0.0043(14) 0.0018(16) C133 0.033(2) 0.024(2) 0.0134(17) 0.0058(16) -0.0025(16) -0.0018(18) C134 0.0238(19) 0.023(2) 0.0216(19) -0.0004(17) -0.0057(16) 0.0060(17) C135 0.0188(17) 0.023(2) 0.0190(18) -0.0064(16) -0.0002(14) 0.0021(16) C136 0.0165(17) 0.019(2) 0.0141(16) -0.0044(15) 0.0007(13) -0.0014(15) P2 0.0152(4) 0.0130(5) 0.0115(4) -0.0011(4) 0.0016(3) 0.0012(4) C211 0.0168(16) 0.017(2) 0.0097(15) 0.0016(14) 0.0001(13) 0.0023(15) C212 0.0219(18) 0.018(2) 0.0248(19) 0.0020(16) 0.0051(15) -0.0019(15) C213 0.0257(19) 0.020(2) 0.032(2) 0.0030(18) 0.0065(16) 0.0102(17) C214 0.0177(17) 0.031(3) 0.0251(19) 0.0058(19) 0.0031(15) 0.0075(18) C215 0.0176(17) 0.029(3) 0.0179(18) 0.0014(16) 0.0010(14) -0.0065(16) C216 0.0204(17) 0.014(2) 0.0144(16) -0.0012(14) -0.0017(14) -0.0004(15) C221 0.0204(16) 0.014(2) 0.0140(15) -0.0028(15) 0.0041(13) 0.0022(15) C222 0.0217(18) 0.019(2) 0.0185(17) -0.0002(15) 0.0090(14) 0.0017(15) C223 0.0253(19) 0.019(2) 0.039(2) -0.0072(19) 0.0158(17) -0.0012(17) C224 0.039(2) 0.018(2) 0.036(2) 0.0017(18) 0.0253(19) 0.0005(18) C225 0.048(2) 0.018(2) 0.0216(19) 0.0046(17) 0.0142(18) 0.0092(19) C226 0.0281(19) 0.016(2) 0.0180(17) 0.0004(16) 0.0042(15) 0.0003(17) C231 0.0154(16) 0.013(2) 0.0199(17) -0.0040(15) 0.0018(14) 0.0011(14) C232 0.0219(18) 0.015(2) 0.0211(18) 0.0007(16) 0.0069(15) 0.0009(15) C233 0.029(2) 0.016(2) 0.035(2) -0.0005(18) 0.0080(17) 0.0007(17) C234 0.027(2) 0.020(2) 0.037(2) -0.0161(19) 0.0060(18) -0.0026(17) C235 0.037(2) 0.031(3) 0.0211(19) -0.0102(18) -0.0049(17) 0.0066(19) C236 0.034(2) 0.017(2) 0.0214(19) -0.0040(17) -0.0031(16) 0.0068(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.405(4) . ? C1 B4 1.597(6) . ? C1 B3 1.613(6) . ? C1 B5 1.627(5) . ? C1 Re1 2.112(3) . ? Re1 C22 1.908(4) . ? Re1 C23 1.915(4) . ? Re1 C21 1.924(5) . ? Re1 B9 2.340(5) . ? Re1 B6 2.345(5) . ? Re1 B5 2.387(4) . ? Re1 B3 2.397(4) . ? B3 B7 1.803(7) . ? B3 B4 1.837(6) . ? B3 B6 1.841(6) . ? B4 B8 1.763(6) . ? B4 B7 1.775(7) . ? B4 B5 1.839(6) . ? B5 B8 1.810(7) . ? B5 B9 1.850(6) . ? B6 C10 1.594(7) . ? B6 B7 1.832(7) . ? B6 B9 1.891(7) . ? B7 C10 1.582(6) . ? B7 B8 1.836(7) . ? B8 C10 1.582(6) . ? B8 B9 1.826(7) . ? B9 C10 1.585(7) . ? C21 O21 1.144(5) . ? C22 O22 1.156(4) . ? C23 O23 1.150(5) . ? P1 N1 1.575(3) . ? P1 C111 1.788(3) . ? P1 C121 1.793(3) . ? P1 C131 1.796(3) . ? N1 P2 1.578(3) . ? C111 C116 1.382(5) . ? C111 C112 1.395(5) . ? C112 C113 1.373(5) . ? C113 C114 1.368(6) . ? C114 C115 1.375(6) . ? C115 C116 1.379(5) . ? C121 C122 1.379(5) . ? C121 C126 1.391(5) . ? C122 C123 1.377(5) . ? C123 C124 1.377(5) . ? C124 C125 1.379(5) . ? C125 C126 1.371(5) . ? C131 C132 1.386(5) . ? C131 C136 1.388(5) . ? C132 C133 1.386(5) . ? C133 C134 1.371(5) . ? C134 C135 1.375(5) . ? C135 C136 1.377(5) . ? P2 C221 1.782(4) . ? P2 C231 1.795(4) . ? P2 C211 1.799(3) . ? C211 C216 1.382(5) . ? C211 C212 1.384(5) . ? C212 C213 1.380(5) . ? C213 C214 1.371(5) . ? C214 C215 1.381(5) . ? C215 C216 1.378(5) . ? C221 C222 1.393(4) . ? C221 C226 1.396(5) . ? C222 C223 1.380(5) . ? C223 C224 1.372(5) . ? C224 C225 1.379(5) . ? C225 C226 1.366(5) . ? C231 C232 1.379(5) . ? C231 C236 1.386(5) . ? C232 C233 1.372(5) . ? C233 C234 1.373(5) . ? C234 C235 1.367(5) . ? C235 C236 1.372(5) . ? 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 O1 C1 B4 116.5(3) . . ? O1 C1 B3 124.4(3) . . ? B4 C1 B3 69.8(3) . . ? O1 C1 B5 126.1(3) . . ? B4 C1 B5 69.5(3) . . ? B3 C1 B5 108.2(3) . . ? O1 C1 Re1 119.7(2) . . ? B4 C1 Re1 123.8(2) . . ? B3 C1 Re1 78.86(19) . . ? B5 C1 Re1 78.14(18) . . ? C22 Re1 C23 90.59(15) . . ? C22 Re1 C21 89.14(16) . . ? C23 Re1 C21 89.11(17) . . ? C22 Re1 C1 135.16(14) . . ? C23 Re1 C1 134.16(15) . . ? C21 Re1 C1 88.96(14) . . ? C22 Re1 B9 115.07(16) . . ? C23 Re1 B9 83.31(17) . . ? C21 Re1 B9 154.58(16) . . ? C1 Re1 B9 79.30(14) . . ? C22 Re1 B6 81.83(17) . . ? C23 Re1 B6 117.67(17) . . ? C21 Re1 B6 151.63(17) . . ? C1 Re1 B6 79.03(15) . . ? B9 Re1 B6 47.60(17) . . ? C22 Re1 B5 157.33(16) . . ? C23 Re1 B5 98.00(15) . . ? C21 Re1 B5 111.82(15) . . ? C1 Re1 B5 41.85(13) . . ? B9 Re1 B5 46.07(15) . . ? B6 Re1 B5 75.60(16) . . ? C22 Re1 B3 98.83(15) . . ? C23 Re1 B3 158.35(17) . . ? C21 Re1 B3 110.35(15) . . ? C1 Re1 B3 41.31(14) . . ? B9 Re1 B3 75.05(16) . . ? B6 Re1 B3 45.67(15) . . ? B5 Re1 B3 66.56(15) . . ? C1 B3 B7 108.1(3) . . ? C1 B3 B4 54.7(2) . . ? B7 B3 B4 58.3(3) . . ? C1 B3 B6 110.5(3) . . ? B7 B3 B6 60.4(3) . . ? B4 B3 B6 101.0(3) . . ? C1 B3 Re1 59.83(18) . . ? B7 B3 Re1 113.9(2) . . ? B4 B3 Re1 100.7(2) . . ? B6 B3 Re1 65.66(19) . . ? C1 B4 B8 110.7(3) . . ? C1 B4 B7 110.2(3) . . ? B8 B4 B7 62.5(3) . . ? C1 B4 B3 55.5(2) . . ? B8 B4 B3 103.8(3) . . ? B7 B4 B3 59.9(3) . . ? C1 B4 B5 56.0(2) . . ? B8 B4 B5 60.3(2) . . ? B7 B4 B5 104.3(3) . . ? B3 B4 B5 91.1(3) . . ? C1 B5 B8 107.0(3) . . ? C1 B5 B4 54.5(2) . . ? B8 B5 B4 57.8(2) . . ? C1 B5 B9 109.7(3) . . ? B8 B5 B9 59.8(3) . . ? B4 B5 B9 100.3(3) . . ? C1 B5 Re1 60.01(18) . . ? B8 B5 Re1 113.6(3) . . ? B4 B5 Re1 101.1(2) . . ? B9 B5 Re1 65.6(2) . . ? C10 B6 B7 54.4(3) . . ? C10 B6 B3 106.7(3) . . ? B7 B6 B3 58.8(2) . . ? C10 B6 B9 53.3(3) . . ? B7 B6 B9 89.0(3) . . ? B3 B6 B9 101.3(3) . . ? C10 B6 Re1 117.2(3) . . ? B7 B6 Re1 115.1(3) . . ? B3 B6 Re1 68.7(2) . . ? B9 B6 Re1 66.1(2) . . ? C10 B7 B4 107.4(4) . . ? C10 B7 B3 109.1(3) . . ? B4 B7 B3 61.8(3) . . ? C10 B7 B6 55.1(3) . . ? B4 B7 B6 103.8(3) . . ? B3 B7 B6 60.8(2) . . ? C10 B7 B8 54.5(3) . . ? B4 B7 B8 58.4(3) . . ? B3 B7 B8 102.3(3) . . ? B6 B7 B8 90.9(3) . . ? C10 B8 B4 107.9(4) . . ? C10 B8 B5 109.4(4) . . ? B4 B8 B5 61.9(2) . . ? C10 B8 B9 54.9(3) . . ? B4 B8 B9 104.1(3) . . ? B5 B8 B9 61.2(2) . . ? C10 B8 B7 54.5(3) . . ? B4 B8 B7 59.0(3) . . ? B5 B8 B7 102.9(3) . . ? B9 B8 B7 90.8(3) . . ? C10 B9 B8 54.7(3) . . ? C10 B9 B5 107.3(3) . . ? B8 B9 B5 59.0(2) . . ? C10 B9 B6 53.7(3) . . ? B8 B9 B6 89.3(3) . . ? B5 B9 B6 101.7(3) . . ? C10 B9 Re1 117.9(3) . . ? B8 B9 Re1 115.1(2) . . ? B5 B9 Re1 68.3(2) . . ? B6 B9 Re1 66.3(2) . . ? B7 C10 B8 71.0(3) . . ? B7 C10 B9 110.9(3) . . ? B8 C10 B9 70.4(3) . . ? B7 C10 B6 70.5(3) . . ? B8 C10 B6 110.7(3) . . ? B9 C10 B6 73.0(3) . . ? O21 C21 Re1 179.0(4) . . ? O22 C22 Re1 175.5(3) . . ? O23 C23 Re1 175.1(4) . . ? N1 P1 C111 111.44(16) . . ? N1 P1 C121 114.81(14) . . ? C111 P1 C121 108.15(16) . . ? N1 P1 C131 108.69(16) . . ? C111 P1 C131 108.52(15) . . ? C121 P1 C131 104.88(16) . . ? P1 N1 P2 136.81(18) . . ? C116 C111 C112 119.6(3) . . ? C116 C111 P1 119.9(3) . . ? C112 C111 P1 120.6(3) . . ? C113 C112 C111 119.6(4) . . ? C114 C113 C112 120.5(4) . . ? C113 C114 C115 120.2(4) . . ? C114 C115 C116 120.2(4) . . ? C115 C116 C111 119.9(4) . . ? C122 C121 C126 119.5(3) . . ? C122 C121 P1 122.5(3) . . ? C126 C121 P1 118.0(3) . . ? C123 C122 C121 120.2(3) . . ? C124 C123 C122 120.1(4) . . ? C123 C124 C125 119.9(3) . . ? C126 C125 C124 120.3(4) . . ? C125 C126 C121 119.9(3) . . ? C132 C131 C136 119.6(3) . . ? C132 C131 P1 120.4(3) . . ? C136 C131 P1 120.0(3) . . ? C133 C132 C131 120.2(3) . . ? C134 C133 C132 119.8(4) . . ? C133 C134 C135 120.2(3) . . ? C134 C135 C136 120.7(4) . . ? C135 C136 C131 119.5(3) . . ? N1 P2 C221 109.67(15) . . ? N1 P2 C231 109.61(16) . . ? C221 P2 C231 108.36(17) . . ? N1 P2 C211 113.73(15) . . ? C221 P2 C211 108.12(16) . . ? C231 P2 C211 107.20(15) . . ? C216 C211 C212 119.5(3) . . ? C216 C211 P2 120.8(3) . . ? C212 C211 P2 119.2(3) . . ? C213 C212 C211 120.1(3) . . ? C214 C213 C212 120.4(4) . . ? C213 C214 C215 119.5(4) . . ? C216 C215 C214 120.6(3) . . ? C215 C216 C211 119.8(3) . . ? C222 C221 C226 119.4(3) . . ? C222 C221 P2 119.1(3) . . ? C226 C221 P2 121.5(3) . . ? C223 C222 C221 120.0(3) . . ? C224 C223 C222 120.1(4) . . ? C223 C224 C225 120.1(4) . . ? C226 C225 C224 120.8(3) . . ? C225 C226 C221 119.7(3) . . ? C232 C231 C236 119.7(3) . . ? C232 C231 P2 119.1(3) . . ? C236 C231 P2 121.2(3) . . ? C233 C232 C231 120.0(3) . . ? C232 C233 C234 120.3(4) . . ? C235 C234 C233 119.7(4) . . ? C234 C235 C236 120.8(4) . . ? C235 C236 C231 119.5(4) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.942 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.153 #===END