# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ana Fernandes' _publ_contact_author_email ANACRIS@ITQB.UNL.PT _publ_section_title ; Activation of B-H bonds by an oxo-rhenium complex ; loop_ _publ_author_name 'Ana Fernandes' 'Jose A Fernandes' 'Filipe Paz' 'Carlos C Romao' # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 680868' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '23 September 2008' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H35 B I O4 P2 Re, 2(C7 H8)' _chemical_formula_sum 'C56 H51 B I O4 P2 Re' _chemical_formula_weight 1173.82 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' 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.2359(8) _cell_length_b 18.2151(7) _cell_length_c 26.5497(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9302.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9413 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 29.38 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4656 _exptl_absorpt_coefficient_mu 3.394 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3830 _exptl_absorpt_correction_T_max 0.7278 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 X8 Kappa CCD APEX II' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 298065 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 29.13 _reflns_number_total 12505 _reflns_number_gt 10697 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare at al. 1994)' _computing_structure_refinement 'SHELXTL (Bruker 2001)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material '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^)+(0.0351P)^2^+98.1056P] 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 12505 _refine_ls_number_parameters 476 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.658421(12) 0.262673(15) 0.105578(8) 0.03261(8) Uani 1 1 d D . . H1 H 0.5736(12) 0.236(4) 0.102(3) 0.04(2) Uiso 1 1 d D . . O1 O 0.6645(3) 0.3485(3) 0.07778(17) 0.0501(13) Uani 1 1 d . . . O2 O 0.6411(3) 0.1673(3) 0.13494(17) 0.0419(11) Uani 1 1 d . . . I1 I 0.80041(2) 0.24606(3) 0.126890(17) 0.04328(12) Uani 1 1 d . . . P1 P 0.63107(8) 0.30631(9) 0.19167(5) 0.0259(3) Uani 1 1 d . . . P2 P 0.66967(8) 0.20067(9) 0.02260(5) 0.0264(3) Uani 1 1 d . . . B1 B 0.5948(5) 0.1128(5) 0.1391(3) 0.0416(17) Uani 1 1 d . . . O3 O 0.5261(4) 0.1144(4) 0.1199(2) 0.0693(18) Uani 1 1 d . . . O4 O 0.6089(4) 0.0474(4) 0.1622(3) 0.0689(17) Uani 1 1 d . . . C1 C 0.4997(6) 0.0428(5) 0.1320(4) 0.067(3) Uani 1 1 d . . . C2 C 0.5513(5) 0.0041(5) 0.1564(3) 0.060(2) Uani 1 1 d . . . C3 C 0.5460(8) -0.0691(6) 0.1685(5) 0.094(4) Uani 1 1 d . . . H3 H 0.5815 -0.0963 0.1850 0.113 Uiso 1 1 calc R . . C4 C 0.4801(10) -0.0995(7) 0.1533(5) 0.111(6) Uani 1 1 d . . . H4 H 0.4705 -0.1496 0.1604 0.133 Uiso 1 1 calc R . . C5 C 0.4315(10) -0.0585(9) 0.1290(5) 0.126(7) Uani 1 1 d . . . H5 H 0.3891 -0.0814 0.1195 0.151 Uiso 1 1 calc R . . C6 C 0.4406(8) 0.0126(9) 0.1179(5) 0.116(6) Uani 1 1 d . . . H6 H 0.4060 0.0400 0.1007 0.139 Uiso 1 1 calc R . . C7 C 0.5418(3) 0.2854(4) 0.2099(2) 0.0299(12) Uani 1 1 d . . . C8 C 0.4875(3) 0.3144(4) 0.1816(2) 0.0398(15) Uani 1 1 d . . . H8 H 0.4972 0.3422 0.1522 0.048 Uiso 1 1 calc R . . C9 C 0.4192(4) 0.3029(5) 0.1962(3) 0.0478(18) Uani 1 1 d . . . H9 H 0.3824 0.3241 0.1773 0.057 Uiso 1 1 calc R . . C10 C 0.4043(4) 0.2605(5) 0.2381(3) 0.051(2) Uani 1 1 d . . . H10 H 0.3575 0.2526 0.2480 0.061 Uiso 1 1 calc R . . C11 C 0.4577(4) 0.2298(5) 0.2651(3) 0.055(2) Uani 1 1 d . . . H11 H 0.4474 0.1998 0.2934 0.067 Uiso 1 1 calc R . . C12 C 0.5265(4) 0.2420(4) 0.2517(3) 0.0418(15) Uani 1 1 d . . . H12 H 0.5630 0.2209 0.2710 0.050 Uiso 1 1 calc R . . C13 C 0.6816(3) 0.2709(3) 0.2440(2) 0.0286(12) Uani 1 1 d . . . C14 C 0.7011(4) 0.1972(4) 0.2458(3) 0.0390(14) Uani 1 1 d . . . H14 H 0.6919 0.1661 0.2179 0.047 Uiso 1 1 calc R . . C15 C 0.7338(4) 0.1696(5) 0.2880(3) 0.0474(17) Uani 1 1 d . . . H15 H 0.7464 0.1192 0.2891 0.057 Uiso 1 1 calc R . . C16 C 0.7481(4) 0.2140(5) 0.3284(2) 0.0466(18) Uani 1 1 d . . . H16 H 0.7695 0.1940 0.3576 0.056 Uiso 1 1 calc R . . C17 C 0.7318(4) 0.2867(5) 0.3267(2) 0.0462(18) Uani 1 1 d . . . H17 H 0.7435 0.3178 0.3541 0.055 Uiso 1 1 calc R . . C18 C 0.6980(3) 0.3156(4) 0.2849(2) 0.0372(14) Uani 1 1 d . . . H18 H 0.6859 0.3662 0.2843 0.045 Uiso 1 1 calc R . . C19 C 0.6389(3) 0.4051(3) 0.1974(2) 0.0309(12) Uani 1 1 d . . . C20 C 0.5894(4) 0.4475(4) 0.2226(3) 0.0436(16) Uani 1 1 d . . . H20 H 0.5490 0.4251 0.2362 0.052 Uiso 1 1 calc R . . C21 C 0.5995(5) 0.5226(4) 0.2278(3) 0.055(2) Uani 1 1 d . . . H21 H 0.5660 0.5514 0.2452 0.066 Uiso 1 1 calc R . . C22 C 0.6574(5) 0.5555(4) 0.2079(3) 0.055(2) Uani 1 1 d . . . H22 H 0.6630 0.6071 0.2107 0.066 Uiso 1 1 calc R . . C23 C 0.7068(4) 0.5147(4) 0.1842(3) 0.053(2) Uani 1 1 d . . . H23 H 0.7472 0.5379 0.1712 0.063 Uiso 1 1 calc R . . C24 C 0.6987(4) 0.4394(4) 0.1790(3) 0.0416(15) Uani 1 1 d . . . H24 H 0.7338 0.4111 0.1629 0.050 Uiso 1 1 calc R . . C25 C 0.6029(3) 0.2288(4) -0.0222(2) 0.0320(13) Uani 1 1 d . . . C26 C 0.5331(3) 0.2249(4) -0.0090(2) 0.0352(13) Uani 1 1 d . . . H26 H 0.5203 0.2090 0.0238 0.042 Uiso 1 1 calc R . . C27 C 0.4820(4) 0.2443(5) -0.0436(3) 0.0486(18) Uani 1 1 d . . . H27 H 0.4343 0.2376 -0.0355 0.058 Uiso 1 1 calc R . . C28 C 0.5007(4) 0.2737(5) -0.0901(3) 0.0508(19) Uani 1 1 d . . . H28 H 0.4659 0.2899 -0.1129 0.061 Uiso 1 1 calc R . . C29 C 0.5693(4) 0.2792(5) -0.1030(3) 0.0492(18) Uani 1 1 d . . . H29 H 0.5819 0.2976 -0.1352 0.059 Uiso 1 1 calc R . . C30 C 0.6207(4) 0.2578(4) -0.0692(2) 0.0414(15) Uani 1 1 d . . . H30 H 0.6683 0.2630 -0.0781 0.050 Uiso 1 1 calc R . . C31 C 0.6627(3) 0.1018(3) 0.0288(2) 0.0314(12) Uani 1 1 d . . . C32 C 0.6065(4) 0.0621(4) 0.0105(3) 0.0462(17) Uani 1 1 d . . . H32 H 0.5717 0.0863 -0.0086 0.055 Uiso 1 1 calc R . . C33 C 0.6006(4) -0.0123(5) 0.0199(4) 0.057(2) Uani 1 1 d . . . H33 H 0.5612 -0.0384 0.0080 0.068 Uiso 1 1 calc R . . C34 C 0.6516(5) -0.0488(4) 0.0464(3) 0.054(2) Uani 1 1 d . . . H34 H 0.6470 -0.0997 0.0533 0.065 Uiso 1 1 calc R . . C35 C 0.7095(5) -0.0109(5) 0.0628(3) 0.056(2) Uani 1 1 d . . . H35 H 0.7459 -0.0365 0.0794 0.067 Uiso 1 1 calc R . . C36 C 0.7150(4) 0.0642(4) 0.0553(3) 0.0455(17) Uani 1 1 d . . . H36 H 0.7540 0.0902 0.0680 0.055 Uiso 1 1 calc R . . C37 C 0.7510(3) 0.2164(4) -0.0110(2) 0.0300(12) Uani 1 1 d . . . C38 C 0.7858(3) 0.1606(4) -0.0363(2) 0.0369(14) Uani 1 1 d . . . H38 H 0.7684 0.1118 -0.0350 0.044 Uiso 1 1 calc R . . C39 C 0.8461(4) 0.1759(4) -0.0635(2) 0.0426(16) Uani 1 1 d . . . H39 H 0.8700 0.1373 -0.0803 0.051 Uiso 1 1 calc R . . C40 C 0.8710(3) 0.2461(4) -0.0663(2) 0.0416(16) Uani 1 1 d . . . H40 H 0.9117 0.2563 -0.0853 0.050 Uiso 1 1 calc R . . C41 C 0.8366(4) 0.3024(4) -0.0412(2) 0.0421(16) Uani 1 1 d . . . H41 H 0.8538 0.3513 -0.0432 0.051 Uiso 1 1 calc R . . C42 C 0.7772(3) 0.2874(4) -0.0132(2) 0.0360(13) Uani 1 1 d . . . H42 H 0.7545 0.3258 0.0045 0.043 Uiso 1 1 calc R . . C1T C 0.5666(6) 0.0187(9) 0.3182(5) 0.134(2) Uiso 1 1 d D . . H1T1 H 0.5295 -0.0123 0.3319 0.201 Uiso 1 1 calc R . . H1T2 H 0.5784 0.0020 0.2841 0.201 Uiso 1 1 calc R . . H1T3 H 0.5507 0.0698 0.3168 0.201 Uiso 1 1 calc R . . C2T C 0.6289(5) 0.0135(6) 0.3509(4) 0.134(2) Uiso 1 1 d GD . . C3T C 0.6267(5) 0.0376(6) 0.4005(4) 0.134(2) Uiso 1 1 d GD . . H3T H 0.5840 0.0535 0.4148 0.161 Uiso 1 1 calc R . . C4T C 0.6871(6) 0.0385(6) 0.4293(3) 0.134(2) Uiso 1 1 d G . . H4T H 0.6857 0.0550 0.4632 0.161 Uiso 1 1 calc R . . C5T C 0.7496(5) 0.0153(6) 0.4084(4) 0.134(2) Uiso 1 1 d G . . H5T H 0.7909 0.0159 0.4280 0.161 Uiso 1 1 calc R . . C6T C 0.7517(5) -0.0088(6) 0.3587(4) 0.134(2) Uiso 1 1 d G . . H6T H 0.7945 -0.0247 0.3445 0.161 Uiso 1 1 calc R . . C7T C 0.6914(5) -0.0097(6) 0.3300(3) 0.134(2) Uiso 1 1 d GD . . H7T H 0.6928 -0.0262 0.2960 0.161 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02429(11) 0.05294(16) 0.02060(11) -0.00688(9) -0.00216(8) 0.00496(10) O1 0.070(4) 0.052(3) 0.028(2) -0.003(2) 0.001(2) 0.011(3) O2 0.048(3) 0.047(3) 0.031(2) -0.004(2) 0.003(2) -0.022(2) I1 0.02602(19) 0.0694(3) 0.0344(2) -0.0019(2) -0.00143(15) -0.00321(19) P1 0.0244(7) 0.0340(8) 0.0193(6) -0.0019(5) 0.0009(5) -0.0039(6) P2 0.0256(7) 0.0336(8) 0.0200(6) -0.0005(5) -0.0005(5) 0.0004(6) B1 0.047(4) 0.043(4) 0.035(4) -0.002(3) -0.001(3) -0.006(4) O3 0.073(4) 0.066(4) 0.068(4) 0.014(3) -0.011(3) -0.015(3) O4 0.071(4) 0.059(4) 0.076(4) 0.016(3) -0.004(4) -0.003(3) C1 0.076(6) 0.054(5) 0.072(6) -0.001(4) -0.021(5) -0.019(5) C2 0.072(6) 0.049(5) 0.059(5) 0.004(4) 0.005(4) -0.016(4) C3 0.130(11) 0.058(6) 0.095(8) 0.024(6) 0.044(8) -0.002(7) C4 0.184(16) 0.066(7) 0.082(8) -0.010(6) 0.047(10) -0.064(9) C5 0.175(17) 0.114(12) 0.089(10) 0.025(9) -0.013(10) -0.083(12) C6 0.109(11) 0.130(12) 0.107(10) 0.039(9) -0.033(8) -0.067(9) C7 0.027(3) 0.038(3) 0.025(3) -0.006(2) 0.000(2) -0.008(2) C8 0.030(3) 0.062(4) 0.027(3) 0.001(3) 0.001(2) -0.004(3) C9 0.033(3) 0.074(5) 0.036(3) 0.000(3) 0.001(3) -0.003(3) C10 0.030(3) 0.088(6) 0.036(3) -0.007(4) 0.006(3) -0.019(4) C11 0.045(4) 0.085(6) 0.036(4) 0.010(4) 0.004(3) -0.028(4) C12 0.038(3) 0.057(4) 0.030(3) 0.006(3) 0.000(3) -0.014(3) C13 0.026(3) 0.039(3) 0.021(2) 0.000(2) 0.000(2) -0.011(2) C14 0.042(4) 0.043(4) 0.032(3) 0.005(3) -0.009(3) -0.003(3) C15 0.049(4) 0.056(5) 0.038(3) 0.014(3) -0.003(3) -0.003(3) C16 0.038(3) 0.078(5) 0.024(3) 0.012(3) -0.003(3) 0.002(4) C17 0.041(4) 0.073(5) 0.024(3) -0.004(3) -0.005(3) -0.007(4) C18 0.032(3) 0.053(4) 0.026(3) -0.006(3) -0.002(2) -0.006(3) C19 0.037(3) 0.033(3) 0.023(3) -0.002(2) 0.002(2) -0.004(2) C20 0.043(4) 0.041(4) 0.047(4) -0.006(3) 0.012(3) -0.004(3) C21 0.060(5) 0.037(4) 0.068(5) -0.013(4) 0.015(4) -0.001(4) C22 0.064(5) 0.040(4) 0.061(5) -0.008(3) 0.005(4) -0.010(4) C23 0.056(5) 0.045(4) 0.058(5) -0.002(4) 0.014(4) -0.022(4) C24 0.042(4) 0.044(4) 0.040(3) -0.002(3) 0.012(3) -0.011(3) C25 0.029(3) 0.045(4) 0.023(3) -0.003(2) -0.001(2) 0.002(2) C26 0.031(3) 0.046(4) 0.028(3) 0.000(3) -0.002(2) 0.004(3) C27 0.027(3) 0.082(6) 0.037(3) 0.007(3) -0.005(3) -0.002(3) C28 0.040(4) 0.074(6) 0.038(4) 0.003(4) -0.010(3) 0.002(4) C29 0.053(4) 0.062(5) 0.033(3) 0.013(3) -0.007(3) -0.003(4) C30 0.036(3) 0.061(5) 0.027(3) 0.003(3) 0.001(3) -0.002(3) C31 0.036(3) 0.032(3) 0.026(3) -0.002(2) 0.003(2) 0.000(2) C32 0.039(4) 0.041(4) 0.059(4) -0.004(3) 0.000(3) 0.000(3) C33 0.047(4) 0.044(4) 0.080(6) -0.007(4) 0.003(4) -0.008(3) C34 0.080(6) 0.036(4) 0.047(4) -0.004(3) 0.012(4) -0.004(4) C35 0.078(6) 0.050(5) 0.039(4) 0.002(3) -0.010(4) 0.017(4) C36 0.053(4) 0.047(4) 0.036(3) -0.001(3) -0.011(3) 0.003(3) C37 0.028(3) 0.042(3) 0.021(2) 0.000(2) -0.001(2) 0.000(2) C38 0.038(3) 0.043(4) 0.030(3) -0.003(3) 0.001(3) 0.004(3) C39 0.037(3) 0.059(4) 0.032(3) -0.007(3) 0.006(3) 0.009(3) C40 0.029(3) 0.068(5) 0.027(3) -0.005(3) 0.002(2) 0.002(3) C41 0.036(3) 0.060(5) 0.031(3) -0.003(3) 0.000(3) -0.012(3) C42 0.037(3) 0.046(4) 0.026(3) -0.007(3) 0.001(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 1.732(5) . ? Re1 O2 1.933(5) . ? Re1 P1 2.4766(14) . ? Re1 P2 2.4851(14) . ? Re1 I1 2.8057(5) . ? Re1 H1 1.703(10) . ? O2 B1 1.337(9) . ? P1 C19 1.813(6) . ? P1 C13 1.815(6) . ? P1 C7 1.823(6) . ? P2 C31 1.813(6) . ? P2 C37 1.824(6) . ? P2 C25 1.824(6) . ? B1 O4 1.367(10) . ? B1 O3 1.417(11) . ? O3 C1 1.436(11) . ? O4 C2 1.370(11) . ? C1 C6 1.316(14) . ? C1 C2 1.381(14) . ? C2 C3 1.374(13) . ? C3 C4 1.44(2) . ? C3 H3 0.9500 . ? C4 C5 1.36(2) . ? C4 H4 0.9500 . ? C5 C6 1.341(19) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.392(9) . ? C7 C12 1.395(9) . ? C8 C9 1.385(9) . ? C8 H8 0.9500 . ? C9 C10 1.384(11) . ? C9 H9 0.9500 . ? C10 C11 1.371(12) . ? C10 H10 0.9500 . ? C11 C12 1.389(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.393(8) . ? C13 C14 1.394(9) . ? C14 C15 1.381(9) . ? C14 H14 0.9500 . ? C15 C16 1.372(11) . ? C15 H15 0.9500 . ? C16 C17 1.363(12) . ? C16 H16 0.9500 . ? C17 C18 1.387(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.396(9) . ? C19 C24 1.397(9) . ? C20 C21 1.388(10) . ? C20 H20 0.9500 . ? C21 C22 1.370(11) . ? C21 H21 0.9500 . ? C22 C23 1.361(12) . ? C22 H22 0.9500 . ? C23 C24 1.388(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.389(8) . ? C25 C30 1.397(9) . ? C26 C27 1.392(9) . ? C26 H26 0.9500 . ? C27 C28 1.394(10) . ? C27 H27 0.9500 . ? C28 C29 1.365(11) . ? C28 H28 0.9500 . ? C29 C30 1.392(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.389(9) . ? C31 C36 1.404(9) . ? C32 C33 1.382(11) . ? C32 H32 0.9500 . ? C33 C34 1.379(12) . ? C33 H33 0.9500 . ? C34 C35 1.380(12) . ? C34 H34 0.9500 . ? C35 C36 1.387(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.389(9) . ? C37 C38 1.390(9) . ? C38 C39 1.395(9) . ? C38 H38 0.9500 . ? C39 C40 1.367(11) . ? C39 H39 0.9500 . ? C40 C41 1.392(10) . ? C40 H40 0.9500 . ? C41 C42 1.389(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C1T C2T 1.482(6) . ? C1T H1T1 0.9800 . ? C1T H1T2 0.9800 . ? C1T H1T3 0.9800 . ? C2T C3T 1.3900 . ? C2T C7T 1.3900 . ? C3T C4T 1.3900 . ? C3T H3T 0.9500 . ? C4T C5T 1.3900 . ? C4T H4T 0.9500 . ? C5T C6T 1.3900 . ? C5T H5T 0.9500 . ? C6T C7T 1.3900 . ? C6T H6T 0.9500 . ? C7T H7T 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 O2 173.8(2) . . ? O1 Re1 P1 96.77(16) . . ? O2 Re1 P1 83.08(14) . . ? O1 Re1 P2 91.52(16) . . ? O2 Re1 P2 87.95(14) . . ? P1 Re1 P2 169.28(5) . . ? O1 Re1 I1 96.76(19) . . ? O2 Re1 I1 89.41(15) . . ? P1 Re1 I1 93.17(4) . . ? P2 Re1 I1 92.58(4) . . ? O1 Re1 H1 107(2) . . ? O2 Re1 H1 67(2) . . ? P1 Re1 H1 86(3) . . ? P2 Re1 H1 85(3) . . ? I1 Re1 H1 156(2) . . ? B1 O2 Re1 144.6(5) . . ? C19 P1 C13 104.1(3) . . ? C19 P1 C7 105.3(3) . . ? C13 P1 C7 103.1(3) . . ? C19 P1 Re1 112.27(19) . . ? C13 P1 Re1 118.6(2) . . ? C7 P1 Re1 112.18(18) . . ? C31 P2 C37 105.3(3) . . ? C31 P2 C25 106.6(3) . . ? C37 P2 C25 103.9(3) . . ? C31 P2 Re1 111.38(19) . . ? C37 P2 Re1 115.9(2) . . ? C25 P2 Re1 112.9(2) . . ? O2 B1 O4 123.5(8) . . ? O2 B1 O3 125.2(7) . . ? O4 B1 O3 111.3(7) . . ? B1 O3 C1 103.4(7) . . ? B1 O4 C2 107.0(7) . . ? C6 C1 C2 122.7(11) . . ? C6 C1 O3 128.5(11) . . ? C2 C1 O3 108.3(8) . . ? O4 C2 C3 126.4(11) . . ? O4 C2 C1 109.8(8) . . ? C3 C2 C1 123.6(10) . . ? C2 C3 C4 111.9(13) . . ? C2 C3 H3 124.0 . . ? C4 C3 H3 124.0 . . ? C5 C4 C3 121.8(12) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 123.0(15) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C1 C6 C5 117.1(15) . . ? C1 C6 H6 121.5 . . ? C5 C6 H6 121.5 . . ? C8 C7 C12 119.0(6) . . ? C8 C7 P1 119.0(5) . . ? C12 C7 P1 121.9(5) . . ? C9 C8 C7 120.3(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 120.3(7) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 119.6(6) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.9(7) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 119.7(7) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C18 C13 C14 118.4(6) . . ? C18 C13 P1 120.7(5) . . ? C14 C13 P1 120.7(4) . . ? C15 C14 C13 120.0(7) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.8(8) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 120.0(6) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.3(7) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.4(7) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C20 C19 C24 118.8(6) . . ? C20 C19 P1 122.2(5) . . ? C24 C19 P1 118.8(5) . . ? C21 C20 C19 119.8(7) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.4(8) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.5(7) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.5(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 119.9(7) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 118.8(6) . . ? C26 C25 P2 120.1(5) . . ? C30 C25 P2 121.0(5) . . ? C25 C26 C27 120.2(6) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 119.9(6) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0(7) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.4(7) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 120.4(6) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C32 C31 C36 118.6(6) . . ? C32 C31 P2 122.9(5) . . ? C36 C31 P2 118.5(5) . . ? C33 C32 C31 120.8(7) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 120.4(8) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.6(7) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.6(8) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 119.9(7) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C42 C37 C38 119.1(6) . . ? C42 C37 P2 118.6(5) . . ? C38 C37 P2 122.3(5) . . ? C37 C38 C39 120.3(7) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 120.4(6) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 119.8(6) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C42 C41 C40 120.1(7) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C37 C42 C41 120.3(6) . . ? C37 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C2T C1T H1T1 109.5 . . ? C2T C1T H1T2 109.5 . . ? H1T1 C1T H1T2 109.5 . . ? C2T C1T H1T3 109.5 . . ? H1T1 C1T H1T3 109.5 . . ? H1T2 C1T H1T3 109.5 . . ? C3T C2T C7T 120.0 . . ? C3T C2T C1T 120.8(5) . . ? C7T C2T C1T 118.9(5) . . ? C4T C3T C2T 120.0 . . ? C4T C3T H3T 120.0 . . ? C2T C3T H3T 120.0 . . ? C3T C4T C5T 120.0 . . ? C3T C4T H4T 120.0 . . ? C5T C4T H4T 120.0 . . ? C6T C5T C4T 120.0 . . ? C6T C5T H5T 120.0 . . ? C4T C5T H5T 120.0 . . ? C7T C6T C5T 120.0 . . ? C7T C6T H6T 120.0 . . ? C5T C6T H6T 120.0 . . ? C6T C7T C2T 120.0 . . ? C6T C7T H7T 120.0 . . ? C2T C7T H7T 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Re1 O2 B1 13(2) . . . . ? P1 Re1 O2 B1 102.0(8) . . . . ? P2 Re1 O2 B1 -72.2(8) . . . . ? I1 Re1 O2 B1 -164.8(8) . . . . ? O1 Re1 P1 C19 -7.9(3) . . . . ? O2 Re1 P1 C19 178.3(3) . . . . ? P2 Re1 P1 C19 -148.4(3) . . . . ? I1 Re1 P1 C19 89.3(2) . . . . ? O1 Re1 P1 C13 -129.5(3) . . . . ? O2 Re1 P1 C13 56.7(3) . . . . ? P2 Re1 P1 C13 90.1(3) . . . . ? I1 Re1 P1 C13 -32.3(2) . . . . ? O1 Re1 P1 C7 110.4(3) . . . . ? O2 Re1 P1 C7 -63.4(3) . . . . ? P2 Re1 P1 C7 -30.0(4) . . . . ? I1 Re1 P1 C7 -152.4(2) . . . . ? O1 Re1 P2 C31 -177.5(3) . . . . ? O2 Re1 P2 C31 -3.6(3) . . . . ? P1 Re1 P2 C31 -36.7(4) . . . . ? I1 Re1 P2 C31 85.7(2) . . . . ? O1 Re1 P2 C37 62.2(3) . . . . ? O2 Re1 P2 C37 -124.0(3) . . . . ? P1 Re1 P2 C37 -157.1(3) . . . . ? I1 Re1 P2 C37 -34.7(2) . . . . ? O1 Re1 P2 C25 -57.5(3) . . . . ? O2 Re1 P2 C25 116.3(3) . . . . ? P1 Re1 P2 C25 83.2(4) . . . . ? I1 Re1 P2 C25 -154.4(2) . . . . ? Re1 O2 B1 O4 173.4(6) . . . . ? Re1 O2 B1 O3 -5.7(14) . . . . ? O2 B1 O3 C1 177.5(8) . . . . ? O4 B1 O3 C1 -1.7(9) . . . . ? O2 B1 O4 C2 -176.3(8) . . . . ? O3 B1 O4 C2 2.9(10) . . . . ? B1 O3 C1 C6 -172.1(14) . . . . ? B1 O3 C1 C2 -0.1(10) . . . . ? B1 O4 C2 C3 171.6(10) . . . . ? B1 O4 C2 C1 -2.9(11) . . . . ? C6 C1 C2 O4 174.5(12) . . . . ? O3 C1 C2 O4 1.9(12) . . . . ? C6 C1 C2 C3 -0.3(19) . . . . ? O3 C1 C2 C3 -172.9(9) . . . . ? O4 C2 C3 C4 -174.6(10) . . . . ? C1 C2 C3 C4 -0.8(16) . . . . ? C2 C3 C4 C5 1.2(19) . . . . ? C3 C4 C5 C6 -1(3) . . . . ? C2 C1 C6 C5 1(2) . . . . ? O3 C1 C6 C5 171.9(13) . . . . ? C4 C5 C6 C1 -1(3) . . . . ? C19 P1 C7 C8 61.9(6) . . . . ? C13 P1 C7 C8 170.8(5) . . . . ? Re1 P1 C7 C8 -60.5(6) . . . . ? C19 P1 C7 C12 -117.1(6) . . . . ? C13 P1 C7 C12 -8.3(6) . . . . ? Re1 P1 C7 C12 120.5(5) . . . . ? C12 C7 C8 C9 2.7(10) . . . . ? P1 C7 C8 C9 -176.3(6) . . . . ? C7 C8 C9 C10 -2.0(12) . . . . ? C8 C9 C10 C11 -0.1(13) . . . . ? C9 C10 C11 C12 1.4(13) . . . . ? C10 C11 C12 C7 -0.7(13) . . . . ? C8 C7 C12 C11 -1.4(11) . . . . ? P1 C7 C12 C11 177.7(6) . . . . ? C19 P1 C13 C18 18.9(6) . . . . ? C7 P1 C13 C18 -90.9(5) . . . . ? Re1 P1 C13 C18 144.5(4) . . . . ? C19 P1 C13 C14 -165.3(5) . . . . ? C7 P1 C13 C14 85.0(5) . . . . ? Re1 P1 C13 C14 -39.7(6) . . . . ? C18 C13 C14 C15 2.1(10) . . . . ? P1 C13 C14 C15 -173.9(5) . . . . ? C13 C14 C15 C16 -0.7(11) . . . . ? C14 C15 C16 C17 -1.7(11) . . . . ? C15 C16 C17 C18 2.7(11) . . . . ? C16 C17 C18 C13 -1.2(10) . . . . ? C14 C13 C18 C17 -1.2(9) . . . . ? P1 C13 C18 C17 174.8(5) . . . . ? C13 P1 C19 C20 -94.6(6) . . . . ? C7 P1 C19 C20 13.6(6) . . . . ? Re1 P1 C19 C20 135.9(5) . . . . ? C13 P1 C19 C24 81.1(6) . . . . ? C7 P1 C19 C24 -170.8(5) . . . . ? Re1 P1 C19 C24 -48.5(6) . . . . ? C24 C19 C20 C21 1.6(11) . . . . ? P1 C19 C20 C21 177.2(6) . . . . ? C19 C20 C21 C22 0.6(13) . . . . ? C20 C21 C22 C23 -2.1(14) . . . . ? C21 C22 C23 C24 1.3(14) . . . . ? C22 C23 C24 C19 1.0(13) . . . . ? C20 C19 C24 C23 -2.4(11) . . . . ? P1 C19 C24 C23 -178.2(6) . . . . ? C31 P2 C25 C26 69.7(6) . . . . ? C37 P2 C25 C26 -179.3(5) . . . . ? Re1 P2 C25 C26 -52.9(6) . . . . ? C31 P2 C25 C30 -113.5(6) . . . . ? C37 P2 C25 C30 -2.5(6) . . . . ? Re1 P2 C25 C30 123.9(5) . . . . ? C30 C25 C26 C27 5.0(11) . . . . ? P2 C25 C26 C27 -178.2(6) . . . . ? C25 C26 C27 C28 -5.5(12) . . . . ? C26 C27 C28 C29 4.1(13) . . . . ? C27 C28 C29 C30 -2.2(13) . . . . ? C28 C29 C30 C25 1.7(13) . . . . ? C26 C25 C30 C29 -3.0(11) . . . . ? P2 C25 C30 C29 -179.9(6) . . . . ? C37 P2 C31 C32 -122.6(6) . . . . ? C25 P2 C31 C32 -12.6(6) . . . . ? Re1 P2 C31 C32 111.0(5) . . . . ? C37 P2 C31 C36 60.5(6) . . . . ? C25 P2 C31 C36 170.5(5) . . . . ? Re1 P2 C31 C36 -65.9(5) . . . . ? C36 C31 C32 C33 2.5(11) . . . . ? P2 C31 C32 C33 -174.4(6) . . . . ? C31 C32 C33 C34 -1.8(13) . . . . ? C32 C33 C34 C35 -1.2(13) . . . . ? C33 C34 C35 C36 3.6(13) . . . . ? C34 C35 C36 C31 -2.8(12) . . . . ? C32 C31 C36 C35 -0.2(11) . . . . ? P2 C31 C36 C35 176.9(6) . . . . ? C31 P2 C37 C42 -168.1(5) . . . . ? C25 P2 C37 C42 80.0(5) . . . . ? Re1 P2 C37 C42 -44.5(5) . . . . ? C31 P2 C37 C38 14.9(6) . . . . ? C25 P2 C37 C38 -97.0(5) . . . . ? Re1 P2 C37 C38 138.4(4) . . . . ? C42 C37 C38 C39 -0.1(9) . . . . ? P2 C37 C38 C39 176.9(5) . . . . ? C37 C38 C39 C40 -1.0(10) . . . . ? C38 C39 C40 C41 0.9(10) . . . . ? C39 C40 C41 C42 0.2(10) . . . . ? C38 C37 C42 C41 1.3(9) . . . . ? P2 C37 C42 C41 -175.8(5) . . . . ? C40 C41 C42 C37 -1.3(10) . . . . ? C7T C2T C3T C4T 0.0 . . . . ? C1T C2T C3T C4T -174.2(12) . . . . ? C2T C3T C4T C5T 0.0 . . . . ? C3T C4T C5T C6T 0.0 . . . . ? C4T C5T C6T C7T 0.0 . . . . ? C5T C6T C7T C2T 0.0 . . . . ? C3T C2T C7T C6T 0.0 . . . . ? C1T C2T C7T C6T 174.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.445 _refine_diff_density_min -5.076 _refine_diff_density_rms 0.152 # ===== END ===== # # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 680869' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '04 March 2008' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H43 B I O4 P2 Re, 1.5(C7 H8)' _chemical_formula_sum 'C52.50 H55 B I O4 P2 Re' _chemical_formula_weight 1135.82 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' 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.173(3) _cell_length_b 18.349(3) _cell_length_c 27.388(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9635(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9391 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.70 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4520 _exptl_absorpt_coefficient_mu 3.273 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4609 _exptl_absorpt_correction_T_max 0.7797 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 X8 Kappa CCD APEX II' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 147899 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 29.13 _reflns_number_total 12941 _reflns_number_gt 8361 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare at al. 1994)' _computing_structure_refinement 'SHELXTL (Bruker 2001)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material '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^)+(0.0367P)^2^+132.8221P] 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 12941 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Re1 Re 0.846312(14) 0.259597(15) 0.894819(10) 0.02460(8) Uani 1 1 d . . . I1 I 0.70112(3) 0.24675(3) 0.874170(19) 0.03446(13) Uani 1 1 d . . . H1 H 0.933(4) 0.239(4) 0.900(2) 0.015(17) Uiso 1 1 d . . . O1 O 0.8433(3) 0.3431(3) 0.9245(2) 0.0404(15) Uani 1 1 d . . . O2 O 0.8636(3) 0.1652(3) 0.86370(19) 0.0312(12) Uani 1 1 d . . . P1 P 0.87058(10) 0.31003(11) 0.81257(7) 0.0251(4) Uani 1 1 d . . . P2 P 0.83332(10) 0.19177(10) 0.97291(7) 0.0250(4) Uani 1 1 d . . . B1 B 0.9149(5) 0.1165(5) 0.8543(3) 0.0297(19) Uani 1 1 d . . . O3 O 0.9107(3) 0.0686(3) 0.8165(2) 0.0412(15) Uani 1 1 d . . . O4 O 0.9742(4) 0.1098(4) 0.8809(3) 0.060(2) Uani 1 1 d . . . C1 C 0.9666(5) 0.0168(5) 0.8222(4) 0.043(2) Uani 1 1 d . . . C2 C 1.0196(5) 0.0583(5) 0.8549(4) 0.046(2) Uani 1 1 d . . . C3 C 0.9343(7) -0.0503(6) 0.8460(5) 0.075(4) Uani 1 1 d . . . H3A H 0.9148 -0.0368 0.8778 0.113 Uiso 1 1 calc R . . H3B H 0.9703 -0.0876 0.8505 0.113 Uiso 1 1 calc R . . H3C H 0.8972 -0.0694 0.8251 0.113 Uiso 1 1 calc R . . C4 C 0.9938(7) -0.0069(7) 0.7737(4) 0.073(4) Uani 1 1 d . . . H4A H 0.9569 -0.0322 0.7557 0.110 Uiso 1 1 calc R . . H4B H 1.0333 -0.0400 0.7785 0.110 Uiso 1 1 calc R . . H4C H 1.0091 0.0358 0.7552 0.110 Uiso 1 1 calc R . . C5 C 1.0544(7) 0.0098(7) 0.8922(5) 0.085(4) Uani 1 1 d . . . H5A H 1.0824 0.0396 0.9144 0.127 Uiso 1 1 calc R . . H5B H 1.0847 -0.0253 0.8755 0.127 Uiso 1 1 calc R . . H5C H 1.0187 -0.0165 0.9108 0.127 Uiso 1 1 calc R . . C6 C 1.0726(7) 0.1017(7) 0.8286(6) 0.079(4) Uani 1 1 d . . . H6A H 1.0495 0.1329 0.8045 0.119 Uiso 1 1 calc R . . H6B H 1.1051 0.0688 0.8120 0.119 Uiso 1 1 calc R . . H6C H 1.0982 0.1320 0.8519 0.119 Uiso 1 1 calc R . . C7 C 0.8235(4) 0.2742(4) 0.7596(3) 0.0258(15) Uani 1 1 d . . . C8 C 0.8009(5) 0.2012(5) 0.7598(3) 0.0373(19) Uani 1 1 d . . . H8 H 0.8082 0.1713 0.7876 0.045 Uiso 1 1 calc R . . C9 C 0.7679(5) 0.1736(5) 0.7189(3) 0.045(2) Uani 1 1 d . . . H9 H 0.7525 0.1244 0.7189 0.054 Uiso 1 1 calc R . . C10 C 0.7569(5) 0.2161(6) 0.6782(3) 0.050(3) Uani 1 1 d . . . H10 H 0.7332 0.1966 0.6507 0.060 Uiso 1 1 calc R . . C11 C 0.7803(5) 0.2867(6) 0.6774(3) 0.042(2) Uani 1 1 d . . . H11 H 0.7741 0.3155 0.6489 0.050 Uiso 1 1 calc R . . C12 C 0.8129(4) 0.3164(5) 0.7182(3) 0.0335(18) Uani 1 1 d . . . H12 H 0.8280 0.3657 0.7177 0.040 Uiso 1 1 calc R . . C13 C 0.8476(4) 0.4067(4) 0.8122(3) 0.0286(15) Uani 1 1 d . . . C14 C 0.7778(5) 0.4254(5) 0.8063(3) 0.042(2) Uani 1 1 d . . . H14 H 0.7439 0.3883 0.8016 0.050 Uiso 1 1 calc R . . C15 C 0.7574(6) 0.4979(5) 0.8073(4) 0.050(3) Uani 1 1 d . . . H15 H 0.7098 0.5105 0.8027 0.061 Uiso 1 1 calc R . . C16 C 0.8060(6) 0.5513(5) 0.8148(4) 0.051(3) Uani 1 1 d . . . H16 H 0.7920 0.6010 0.8149 0.061 Uiso 1 1 calc R . . C17 C 0.8748(6) 0.5337(5) 0.8222(4) 0.055(3) Uani 1 1 d . . . H17 H 0.9083 0.5708 0.8283 0.066 Uiso 1 1 calc R . . C18 C 0.8950(5) 0.4607(5) 0.8205(4) 0.044(2) Uani 1 1 d . . . H18 H 0.9426 0.4484 0.8253 0.053 Uiso 1 1 calc R . . C19 C 0.9619(4) 0.3035(4) 0.7936(3) 0.0301(17) Uani 1 1 d . . . C20 C 1.0155(4) 0.3241(5) 0.8259(3) 0.0354(19) Uani 1 1 d . . . H20 H 1.0043 0.3401 0.8579 0.043 Uiso 1 1 calc R . . C21 C 1.0851(4) 0.3211(6) 0.8109(4) 0.046(2) Uani 1 1 d . . . H21 H 1.1211 0.3365 0.8323 0.055 Uiso 1 1 calc R . . C22 C 1.1008(4) 0.2959(6) 0.7657(4) 0.054(3) Uani 1 1 d . . . H22 H 1.1483 0.2950 0.7558 0.065 Uiso 1 1 calc R . . C23 C 1.0510(5) 0.2720(6) 0.7340(3) 0.054(3) Uani 1 1 d . . . H23 H 1.0636 0.2529 0.7030 0.064 Uiso 1 1 calc R . . C24 C 0.9813(4) 0.2762(5) 0.7481(3) 0.038(2) Uani 1 1 d . . . H24 H 0.9461 0.2600 0.7262 0.045 Uiso 1 1 calc R . . C25 C 0.7551(4) 0.2153(4) 1.0080(3) 0.0268(15) Uani 1 1 d . . . C26 C 0.7420(5) 0.2874(5) 1.0184(3) 0.039(2) Uani 1 1 d . . . H26 H 0.7716 0.3243 1.0057 0.047 Uiso 1 1 calc R . . C27 C 0.6857(5) 0.3064(5) 1.0476(3) 0.042(2) Uani 1 1 d . . . H27 H 0.6768 0.3563 1.0545 0.051 Uiso 1 1 calc R . . C28 C 0.6420(4) 0.2530(6) 1.0667(3) 0.041(2) Uani 1 1 d . . . H28 H 0.6042 0.2660 1.0874 0.050 Uiso 1 1 calc R . . C29 C 0.6540(5) 0.1824(6) 1.0556(4) 0.050(2) Uani 1 1 d . . . H29 H 0.6236 0.1459 1.0680 0.060 Uiso 1 1 calc R . . C30 C 0.7105(5) 0.1621(5) 1.0262(3) 0.043(2) Uani 1 1 d . . . H30 H 0.7183 0.1122 1.0187 0.051 Uiso 1 1 calc R . . C31 C 0.8295(4) 0.0938(4) 0.9649(3) 0.0294(17) Uani 1 1 d . . . C32 C 0.7766(5) 0.0635(5) 0.9366(3) 0.041(2) Uani 1 1 d . . . H32 H 0.7435 0.0944 0.9213 0.049 Uiso 1 1 calc R . . C33 C 0.7717(6) -0.0108(5) 0.9307(3) 0.051(3) Uani 1 1 d . . . H33 H 0.7344 -0.0305 0.9121 0.062 Uiso 1 1 calc R . . C34 C 0.8197(7) -0.0568(5) 0.9512(4) 0.057(3) Uani 1 1 d . . . H34 H 0.8167 -0.1079 0.9462 0.068 Uiso 1 1 calc R . . C35 C 0.8726(7) -0.0275(5) 0.9792(4) 0.059(3) Uani 1 1 d . . . H35 H 0.9057 -0.0592 0.9938 0.071 Uiso 1 1 calc R . . C36 C 0.8786(5) 0.0471(5) 0.9864(3) 0.043(2) Uani 1 1 d . . . H36 H 0.9154 0.0663 1.0057 0.051 Uiso 1 1 calc R . . C37 C 0.9032(4) 0.2053(4) 1.0167(3) 0.0279(16) Uani 1 1 d . . . C38 C 0.8886(5) 0.2092(7) 1.0659(3) 0.053(3) Uani 1 1 d . . . H38 H 0.8414 0.2078 1.0765 0.064 Uiso 1 1 calc R . . C39 C 0.9415(5) 0.2152(8) 1.1002(4) 0.075(4) Uani 1 1 d . . . H39 H 0.9307 0.2175 1.1340 0.090 Uiso 1 1 calc R . . C40 C 1.0114(5) 0.2179(6) 1.0844(4) 0.054(3) Uani 1 1 d . . . H40 H 1.0481 0.2219 1.1075 0.065 Uiso 1 1 calc R . . C41 C 1.0257(5) 0.2148(6) 1.0361(3) 0.047(2) Uani 1 1 d . . . H41 H 1.0727 0.2178 1.0254 0.056 Uiso 1 1 calc R . . C42 C 0.9733(4) 0.2073(5) 1.0022(3) 0.0337(18) Uani 1 1 d . . . H42 H 0.9847 0.2035 0.9686 0.040 Uiso 1 1 calc R . . C1T C 0.9339(11) 0.0942(14) 0.6559(9) 0.175(10) Uani 1 1 d . . . H1T1 H 0.9673 0.1019 0.6292 0.263 Uiso 1 1 calc R . . H1T2 H 0.9558 0.0648 0.6815 0.263 Uiso 1 1 calc R . . H1T3 H 0.9200 0.1415 0.6695 0.263 Uiso 1 1 calc R . . C2T C 0.8698(7) 0.0547(9) 0.6364(6) 0.086(4) Uani 1 1 d . . . C3T C 0.8521(9) 0.0579(8) 0.5883(6) 0.091(4) Uani 1 1 d . . . H3T H 0.8819 0.0833 0.5664 0.110 Uiso 1 1 calc R . . C4T C 0.7943(12) 0.0264(9) 0.5707(7) 0.107(6) Uani 1 1 d . . . H4T H 0.7818 0.0297 0.5372 0.128 Uiso 1 1 calc R . . C5T C 0.7534(10) -0.0115(11) 0.6046(12) 0.134(9) Uani 1 1 d . . . H5T H 0.7116 -0.0342 0.5938 0.161 Uiso 1 1 calc R . . C6T C 0.7723(13) -0.0169(9) 0.6534(10) 0.128(9) Uani 1 1 d . . . H6T H 0.7443 -0.0433 0.6759 0.153 Uiso 1 1 calc R . . C7T C 0.8288(11) 0.0148(9) 0.6672(6) 0.098(5) Uani 1 1 d . . . H7T H 0.8427 0.0102 0.7003 0.118 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02231(14) 0.02818(14) 0.02331(14) 0.00237(12) 0.00063(11) 0.00017(12) I1 0.0232(2) 0.0444(3) 0.0358(3) 0.0023(2) 0.00127(19) 0.0038(2) O1 0.059(4) 0.036(3) 0.027(3) 0.012(2) 0.019(3) 0.016(3) O2 0.036(3) 0.026(3) 0.032(3) 0.006(2) 0.002(2) 0.008(2) P1 0.0190(9) 0.0307(10) 0.0255(9) 0.0021(8) 0.0017(7) 0.0021(7) P2 0.0253(10) 0.0243(9) 0.0254(9) 0.0030(7) 0.0002(7) -0.0012(7) B1 0.032(5) 0.025(4) 0.033(5) 0.001(3) 0.001(4) 0.007(4) O3 0.034(3) 0.037(3) 0.053(4) -0.010(3) -0.009(3) 0.009(3) O4 0.050(4) 0.072(5) 0.058(5) -0.026(4) -0.023(3) 0.028(4) C1 0.034(5) 0.048(5) 0.049(6) -0.010(4) -0.003(4) 0.011(4) C2 0.034(5) 0.044(5) 0.059(6) -0.013(4) -0.013(4) 0.014(4) C3 0.061(8) 0.042(6) 0.122(12) 0.004(7) 0.005(7) 0.006(6) C4 0.077(9) 0.076(8) 0.067(8) -0.025(6) 0.005(6) 0.031(7) C5 0.081(9) 0.093(10) 0.079(9) -0.005(8) -0.034(7) 0.037(8) C6 0.059(8) 0.061(8) 0.118(12) -0.020(7) 0.007(8) -0.005(6) C7 0.022(3) 0.032(4) 0.024(4) -0.002(3) 0.000(3) 0.003(3) C8 0.038(5) 0.046(5) 0.029(4) 0.004(4) -0.002(4) 0.005(4) C9 0.051(6) 0.047(5) 0.038(5) -0.004(4) -0.002(4) -0.002(4) C10 0.047(6) 0.075(7) 0.029(5) -0.011(5) -0.011(4) 0.006(5) C11 0.038(5) 0.063(6) 0.025(4) 0.003(4) -0.001(4) 0.009(4) C12 0.032(4) 0.042(5) 0.026(4) 0.002(3) 0.003(3) 0.008(4) C13 0.030(4) 0.027(4) 0.029(4) 0.008(3) 0.001(3) -0.001(3) C14 0.033(5) 0.040(5) 0.052(6) 0.002(4) 0.004(4) 0.007(4) C15 0.052(6) 0.050(6) 0.049(6) 0.010(5) 0.010(5) 0.023(5) C16 0.067(7) 0.036(5) 0.050(6) -0.003(4) 0.007(5) 0.015(5) C17 0.058(7) 0.032(5) 0.076(8) -0.005(5) 0.007(6) -0.005(4) C18 0.034(5) 0.042(5) 0.055(6) 0.004(4) 0.005(4) -0.008(4) C19 0.025(4) 0.035(4) 0.031(4) 0.008(3) 0.010(3) 0.002(3) C20 0.022(4) 0.047(5) 0.037(5) 0.008(4) 0.003(3) 0.000(3) C21 0.020(4) 0.066(6) 0.053(6) 0.022(5) 0.000(4) -0.001(4) C22 0.015(4) 0.090(8) 0.058(6) 0.027(6) 0.007(4) 0.007(4) C23 0.036(5) 0.091(8) 0.034(5) 0.012(5) 0.012(4) 0.018(5) C24 0.027(4) 0.055(5) 0.031(4) 0.005(4) 0.003(3) 0.008(4) C25 0.021(4) 0.040(4) 0.019(3) -0.001(3) -0.001(3) 0.000(3) C26 0.047(5) 0.039(5) 0.032(4) 0.001(4) 0.009(4) 0.010(4) C27 0.045(5) 0.049(5) 0.034(5) 0.006(4) 0.011(4) 0.015(4) C28 0.030(4) 0.069(6) 0.025(4) -0.003(4) 0.002(3) 0.006(4) C29 0.031(5) 0.067(7) 0.050(6) -0.007(5) 0.010(4) -0.019(5) C30 0.040(5) 0.043(5) 0.045(5) -0.002(4) 0.010(4) -0.010(4) C31 0.040(5) 0.022(4) 0.027(4) 0.004(3) 0.007(3) -0.001(3) C32 0.050(6) 0.038(5) 0.034(5) 0.000(4) 0.004(4) -0.011(4) C33 0.077(8) 0.038(5) 0.039(5) 0.002(4) 0.007(5) -0.026(5) C34 0.101(9) 0.024(4) 0.045(6) -0.003(4) 0.009(6) -0.014(5) C35 0.089(8) 0.031(5) 0.057(7) 0.011(4) 0.005(6) 0.021(5) C36 0.049(6) 0.038(5) 0.041(5) 0.006(4) 0.000(4) 0.003(4) C37 0.026(4) 0.025(4) 0.033(4) 0.003(3) -0.004(3) 0.000(3) C38 0.028(5) 0.102(8) 0.030(5) -0.004(5) 0.001(4) -0.009(5) C39 0.034(5) 0.165(13) 0.026(5) 0.000(6) -0.002(4) 0.019(7) C40 0.029(5) 0.089(8) 0.044(5) -0.005(5) -0.017(4) -0.003(5) C41 0.024(4) 0.069(6) 0.047(6) 0.011(5) 0.002(4) -0.002(4) C42 0.025(4) 0.046(5) 0.031(4) 0.009(3) -0.005(3) -0.001(4) C1T 0.107(17) 0.23(3) 0.19(2) 0.01(2) -0.055(16) -0.012(18) C2T 0.051(8) 0.112(12) 0.095(11) 0.030(9) -0.005(7) 0.011(8) C3T 0.104(13) 0.080(10) 0.090(11) 0.014(8) 0.017(10) 0.000(9) C4T 0.130(16) 0.065(10) 0.125(15) -0.021(10) -0.036(13) 0.027(10) C5T 0.067(10) 0.104(15) 0.23(3) -0.085(18) 0.009(16) -0.011(10) C6T 0.127(18) 0.059(10) 0.20(2) -0.030(13) 0.095(17) -0.011(10) C7T 0.129(15) 0.070(10) 0.095(12) 0.020(9) 0.026(11) 0.032(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 Re1 O1 1.735(6) . ? Re1 O2 1.958(5) . ? Re1 P1 2.479(2) . ? Re1 P2 2.4870(19) . ? Re1 I1 2.8504(7) . ? Re1 H1 1.71(7) . ? O2 B1 1.354(10) . ? P1 C13 1.827(8) . ? P1 C19 1.831(8) . ? P1 C7 1.831(8) . ? P2 C31 1.813(8) . ? P2 C37 1.816(8) . ? P2 C25 1.832(8) . ? B1 O4 1.355(11) . ? B1 O3 1.360(11) . ? O3 C1 1.440(10) . ? O4 C2 1.469(11) . ? C1 C4 1.490(14) . ? C1 C3 1.524(15) . ? C1 C2 1.555(13) . ? C2 C6 1.478(16) . ? C2 C5 1.509(14) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.388(11) . ? C7 C8 1.408(11) . ? C8 C9 1.381(12) . ? C8 H8 0.9500 . ? C9 C10 1.378(13) . ? C9 H9 0.9500 . ? C10 C11 1.370(14) . ? C10 H10 0.9500 . ? C11 C12 1.392(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.363(11) . ? C13 C14 1.391(11) . ? C14 C15 1.388(12) . ? C14 H14 0.9500 . ? C15 C16 1.367(15) . ? C15 H15 0.9500 . ? C16 C17 1.374(15) . ? C16 H16 0.9500 . ? C17 C18 1.395(13) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.392(11) . ? C19 C20 1.407(11) . ? C20 C21 1.396(11) . ? C20 H20 0.9500 . ? C21 C22 1.355(14) . ? C21 H21 0.9500 . ? C22 C23 1.364(14) . ? C22 H22 0.9500 . ? C23 C24 1.395(12) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.378(11) . ? C25 C30 1.389(11) . ? C26 C27 1.387(12) . ? C26 H26 0.9500 . ? C27 C28 1.393(13) . ? C27 H27 0.9500 . ? C28 C29 1.350(14) . ? C28 H28 0.9500 . ? C29 C30 1.401(13) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.392(12) . ? C31 C36 1.401(12) . ? C32 C33 1.376(12) . ? C32 H32 0.9500 . ? C33 C34 1.369(15) . ? C33 H33 0.9500 . ? C34 C35 1.379(16) . ? C34 H34 0.9500 . ? C35 C36 1.389(13) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.377(12) . ? C37 C42 1.402(11) . ? C38 C39 1.386(13) . ? C38 H38 0.9500 . ? C39 C40 1.409(14) . ? C39 H39 0.9500 . ? C40 C41 1.353(13) . ? C40 H40 0.9500 . ? C41 C42 1.373(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C1T C2T 1.52(2) . ? C1T H1T1 0.9800 . ? C1T H1T2 0.9800 . ? C1T H1T3 0.9800 . ? C2T C3T 1.36(2) . ? C2T C7T 1.37(2) . ? C3T C4T 1.34(2) . ? C3T H3T 0.9500 . ? C4T C5T 1.40(3) . ? C4T H4T 0.9500 . ? C5T C6T 1.39(3) . ? C5T H5T 0.9500 . ? C6T C7T 1.29(3) . ? C6T H6T 0.9500 . ? C7T H7T 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 O2 172.0(3) . . ? O1 Re1 P1 95.83(17) . . ? O2 Re1 P1 84.43(16) . . ? O1 Re1 P2 92.08(17) . . ? O2 Re1 P2 87.06(16) . . ? P1 Re1 P2 170.72(6) . . ? O1 Re1 I1 97.7(2) . . ? O2 Re1 I1 90.32(17) . . ? P1 Re1 I1 91.94(5) . . ? P2 Re1 I1 91.80(5) . . ? O1 Re1 H1 101(2) . . ? O2 Re1 H1 71(2) . . ? P1 Re1 H1 89(2) . . ? P2 Re1 H1 85(2) . . ? I1 Re1 H1 161(2) . . ? B1 O2 Re1 142.1(6) . . ? C13 P1 C19 107.0(4) . . ? C13 P1 C7 103.0(3) . . ? C19 P1 C7 102.9(4) . . ? C13 P1 Re1 108.8(3) . . ? C19 P1 Re1 114.4(3) . . ? C7 P1 Re1 119.6(3) . . ? C31 P2 C37 104.2(4) . . ? C31 P2 C25 105.3(4) . . ? C37 P2 C25 103.0(3) . . ? C31 P2 Re1 113.3(3) . . ? C37 P2 Re1 115.2(3) . . ? C25 P2 Re1 114.5(3) . . ? O2 B1 O4 124.6(8) . . ? O2 B1 O3 121.9(8) . . ? O4 B1 O3 113.5(7) . . ? B1 O3 C1 107.6(7) . . ? B1 O4 C2 107.2(7) . . ? O3 C1 C4 111.0(8) . . ? O3 C1 C3 106.1(8) . . ? C4 C1 C3 106.8(10) . . ? O3 C1 C2 102.9(7) . . ? C4 C1 C2 115.3(9) . . ? C3 C1 C2 114.4(9) . . ? O4 C2 C6 107.2(9) . . ? O4 C2 C5 108.3(9) . . ? C6 C2 C5 110.1(10) . . ? O4 C2 C1 102.0(7) . . ? C6 C2 C1 115.6(10) . . ? C5 C2 C1 113.0(9) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 119.2(7) . . ? C12 C7 P1 121.3(6) . . ? C8 C7 P1 119.4(6) . . ? C9 C8 C7 119.2(8) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 121.2(9) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 119.9(9) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.3(8) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.2(8) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C18 C13 C14 118.7(8) . . ? C18 C13 P1 123.0(7) . . ? C14 C13 P1 118.2(6) . . ? C15 C14 C13 120.4(9) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 119.9(10) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.5(9) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 119.1(9) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C13 C18 C17 121.3(9) . . ? C13 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C24 C19 C20 117.6(7) . . ? C24 C19 P1 122.1(6) . . ? C20 C19 P1 120.2(6) . . ? C21 C20 C19 120.1(8) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 119.7(9) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 122.4(8) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C22 C23 C24 118.5(9) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C19 C24 C23 121.5(9) . . ? C19 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C26 C25 C30 119.1(8) . . ? C26 C25 P2 119.0(6) . . ? C30 C25 P2 121.8(7) . . ? C25 C26 C27 120.2(9) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 120.6(9) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C29 C28 C27 119.2(8) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 121.1(9) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C25 C30 C29 119.8(9) . . ? C25 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C36 118.6(8) . . ? C32 C31 P2 119.5(6) . . ? C36 C31 P2 121.9(7) . . ? C33 C32 C31 120.7(9) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 121.1(10) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 118.8(9) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C34 C35 C36 121.6(10) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 119.1(9) . . ? C35 C36 H36 120.4 . . ? C31 C36 H36 120.4 . . ? C38 C37 C42 118.1(7) . . ? C38 C37 P2 120.2(6) . . ? C42 C37 P2 121.6(6) . . ? C37 C38 C39 121.1(9) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C38 C39 C40 119.4(9) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 119.4(8) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C40 C41 C42 121.1(8) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C41 C42 C37 120.8(8) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C2T C1T H1T1 109.5 . . ? C2T C1T H1T2 109.5 . . ? H1T1 C1T H1T2 109.5 . . ? C2T C1T H1T3 109.5 . . ? H1T1 C1T H1T3 109.5 . . ? H1T2 C1T H1T3 109.5 . . ? C3T C2T C7T 118.5(16) . . ? C3T C2T C1T 121.3(17) . . ? C7T C2T C1T 120.2(18) . . ? C4T C3T C2T 122.4(16) . . ? C4T C3T H3T 118.8 . . ? C2T C3T H3T 118.8 . . ? C3T C4T C5T 116.1(19) . . ? C3T C4T H4T 121.9 . . ? C5T C4T H4T 121.9 . . ? C6T C5T C4T 121.8(19) . . ? C6T C5T H5T 119.1 . . ? C4T C5T H5T 119.1 . . ? C7T C6T C5T 118.0(19) . . ? C7T C6T H6T 121.0 . . ? C5T C6T H6T 121.0 . . ? C6T C7T C2T 123(2) . . ? C6T C7T H7T 118.4 . . ? C2T C7T H7T 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Re1 O2 B1 91.4(8) . . . . ? P2 Re1 O2 B1 -84.9(8) . . . . ? I1 Re1 O2 B1 -176.7(8) . . . . ? O1 Re1 P1 C13 -18.1(4) . . . . ? O2 Re1 P1 C13 170.0(3) . . . . ? I1 Re1 P1 C13 79.8(3) . . . . ? O1 Re1 P1 C19 101.5(4) . . . . ? O2 Re1 P1 C19 -70.5(3) . . . . ? I1 Re1 P1 C19 -160.6(3) . . . . ? O1 Re1 P1 C7 -135.9(3) . . . . ? O2 Re1 P1 C7 52.1(3) . . . . ? I1 Re1 P1 C7 -38.0(3) . . . . ? O1 Re1 P2 C31 177.9(4) . . . . ? O2 Re1 P2 C31 -10.1(3) . . . . ? I1 Re1 P2 C31 80.1(3) . . . . ? O1 Re1 P2 C37 -62.2(4) . . . . ? O2 Re1 P2 C37 109.8(3) . . . . ? I1 Re1 P2 C37 -160.0(3) . . . . ? O1 Re1 P2 C25 57.0(3) . . . . ? O2 Re1 P2 C25 -131.0(3) . . . . ? I1 Re1 P2 C25 -40.7(3) . . . . ? Re1 O2 B1 O4 24.6(15) . . . . ? Re1 O2 B1 O3 -155.9(6) . . . . ? O2 B1 O3 C1 -169.7(8) . . . . ? O4 B1 O3 C1 9.9(11) . . . . ? O2 B1 O4 C2 -172.5(9) . . . . ? O3 B1 O4 C2 7.9(11) . . . . ? B1 O3 C1 C4 -145.9(9) . . . . ? B1 O3 C1 C3 98.5(9) . . . . ? B1 O3 C1 C2 -22.0(9) . . . . ? B1 O4 C2 C6 101.3(10) . . . . ? B1 O4 C2 C5 -139.9(10) . . . . ? B1 O4 C2 C1 -20.6(10) . . . . ? O3 C1 C2 O4 25.5(9) . . . . ? C4 C1 C2 O4 146.5(9) . . . . ? C3 C1 C2 O4 -89.1(9) . . . . ? O3 C1 C2 C6 -90.4(10) . . . . ? C4 C1 C2 C6 30.6(13) . . . . ? C3 C1 C2 C6 155.0(9) . . . . ? O3 C1 C2 C5 141.5(9) . . . . ? C4 C1 C2 C5 -97.5(12) . . . . ? C3 C1 C2 C5 26.9(12) . . . . ? C13 P1 C7 C12 33.0(7) . . . . ? C19 P1 C7 C12 -78.1(7) . . . . ? Re1 P1 C7 C12 153.8(5) . . . . ? C13 P1 C7 C8 -150.4(6) . . . . ? C19 P1 C7 C8 98.4(7) . . . . ? Re1 P1 C7 C8 -29.7(7) . . . . ? C12 C7 C8 C9 -0.8(12) . . . . ? P1 C7 C8 C9 -177.4(7) . . . . ? C7 C8 C9 C10 0.0(14) . . . . ? C8 C9 C10 C11 1.5(15) . . . . ? C9 C10 C11 C12 -2.2(14) . . . . ? C8 C7 C12 C11 0.0(12) . . . . ? P1 C7 C12 C11 176.6(6) . . . . ? C10 C11 C12 C7 1.4(13) . . . . ? C19 P1 C13 C18 -29.1(8) . . . . ? C7 P1 C13 C18 -137.1(7) . . . . ? Re1 P1 C13 C18 95.0(7) . . . . ? C19 P1 C13 C14 155.3(7) . . . . ? C7 P1 C13 C14 47.2(7) . . . . ? Re1 P1 C13 C14 -80.7(7) . . . . ? C18 C13 C14 C15 2.2(13) . . . . ? P1 C13 C14 C15 178.0(7) . . . . ? C13 C14 C15 C16 -1.0(15) . . . . ? C14 C15 C16 C17 -1.0(16) . . . . ? C15 C16 C17 C18 1.8(16) . . . . ? C14 C13 C18 C17 -1.4(14) . . . . ? P1 C13 C18 C17 -177.0(8) . . . . ? C16 C17 C18 C13 -0.6(16) . . . . ? C13 P1 C19 C24 -108.2(7) . . . . ? C7 P1 C19 C24 -0.1(8) . . . . ? Re1 P1 C19 C24 131.2(6) . . . . ? C13 P1 C19 C20 74.0(7) . . . . ? C7 P1 C19 C20 -177.9(6) . . . . ? Re1 P1 C19 C20 -46.6(7) . . . . ? C24 C19 C20 C21 3.9(12) . . . . ? P1 C19 C20 C21 -178.2(7) . . . . ? C19 C20 C21 C22 -2.1(14) . . . . ? C20 C21 C22 C23 -1.1(16) . . . . ? C21 C22 C23 C24 2.4(16) . . . . ? C20 C19 C24 C23 -2.6(13) . . . . ? P1 C19 C24 C23 179.5(7) . . . . ? C22 C23 C24 C19 -0.4(15) . . . . ? C31 P2 C25 C26 -177.7(7) . . . . ? C37 P2 C25 C26 73.4(7) . . . . ? Re1 P2 C25 C26 -52.5(7) . . . . ? C31 P2 C25 C30 5.4(8) . . . . ? C37 P2 C25 C30 -103.6(7) . . . . ? Re1 P2 C25 C30 130.6(6) . . . . ? C30 C25 C26 C27 1.2(13) . . . . ? P2 C25 C26 C27 -175.8(7) . . . . ? C25 C26 C27 C28 0.3(14) . . . . ? C26 C27 C28 C29 -1.7(14) . . . . ? C27 C28 C29 C30 1.5(15) . . . . ? C26 C25 C30 C29 -1.4(13) . . . . ? P2 C25 C30 C29 175.5(7) . . . . ? C28 C29 C30 C25 0.0(15) . . . . ? C37 P2 C31 C32 174.1(6) . . . . ? C25 P2 C31 C32 66.0(7) . . . . ? Re1 P2 C31 C32 -59.9(7) . . . . ? C37 P2 C31 C36 -6.0(8) . . . . ? C25 P2 C31 C36 -114.1(7) . . . . ? Re1 P2 C31 C36 120.1(6) . . . . ? C36 C31 C32 C33 1.3(13) . . . . ? P2 C31 C32 C33 -178.7(7) . . . . ? C31 C32 C33 C34 -1.9(14) . . . . ? C32 C33 C34 C35 1.7(16) . . . . ? C33 C34 C35 C36 -0.9(17) . . . . ? C34 C35 C36 C31 0.3(16) . . . . ? C32 C31 C36 C35 -0.5(13) . . . . ? P2 C31 C36 C35 179.6(7) . . . . ? C31 P2 C37 C38 -92.6(8) . . . . ? C25 P2 C37 C38 17.2(9) . . . . ? Re1 P2 C37 C38 142.6(7) . . . . ? C31 P2 C37 C42 83.2(7) . . . . ? C25 P2 C37 C42 -167.1(7) . . . . ? Re1 P2 C37 C42 -41.7(7) . . . . ? C42 C37 C38 C39 0.2(16) . . . . ? P2 C37 C38 C39 176.1(10) . . . . ? C37 C38 C39 C40 0(2) . . . . ? C38 C39 C40 C41 0(2) . . . . ? C39 C40 C41 C42 -1.5(18) . . . . ? C40 C41 C42 C37 2.3(15) . . . . ? C38 C37 C42 C41 -1.6(13) . . . . ? P2 C37 C42 C41 -177.4(7) . . . . ? C7T C2T C3T C4T 3(2) . . . . ? C1T C2T C3T C4T -176.8(17) . . . . ? C2T C3T C4T C5T -1(2) . . . . ? C3T C4T C5T C6T -1(3) . . . . ? C4T C5T C6T C7T 1(3) . . . . ? C5T C6T C7T C2T 2(3) . . . . ? C3T C2T C7T C6T -4(3) . . . . ? C1T C2T C7T C6T 176.6(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.532 _refine_diff_density_min -2.245 _refine_diff_density_rms 0.181 # ===== END ===== #