# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1365 data_reniofenilb _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H37 B2 Cl2 N4 O4 Re' _chemical_formula_weight 844.40 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2740(10) _cell_length_b 13.0070(10) _cell_length_c 13.3500(10) _cell_angle_alpha 100.639(7) _cell_angle_beta 100.376(8) _cell_angle_gamma 108.309(7) _cell_volume 1766.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method ? _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 3.634 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8934 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.97 _reflns_number_total 8504 _reflns_number_observed 7250 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 400 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+1.7336P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8104 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_obs 0.0347 _refine_ls_wR_factor_all 0.0838 _refine_ls_wR_factor_obs 0.0736 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.064 _refine_ls_restrained_S_all 1.114 _refine_ls_restrained_S_obs 1.064 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.22988(2) 0.158741(14) 0.457088(13) 0.03108(6) Uani 1 d . . O1 O 0.1152(3) 0.1961(3) 0.5035(2) 0.0407(7) Uani 1 d . . O2 O 0.3590(3) 0.1263(2) 0.4039(2) 0.0409(7) Uani 1 d . . O3 O 0.3818(3) 0.2869(2) 0.5732(2) 0.0361(6) Uani 1 d . . O4 O 0.2051(3) 0.2413(2) 0.3362(2) 0.0367(7) Uani 1 d . . N1 N 0.2629(4) 0.0801(3) 0.5737(3) 0.0378(8) Uani 1 d . . N2 N 0.0956(4) 0.0295(3) 0.3358(3) 0.0370(8) Uani 1 d . . N11 N 0.3470(4) 0.1449(3) 0.6676(3) 0.0387(8) Uani 1 d . . N21 N 0.0698(4) 0.0524(3) 0.2406(3) 0.0382(8) Uani 1 d . . C2 C 0.4522(8) 0.0964(8) 0.3681(7) 0.107(3) Uani 1 d . . H2A H 0.5086(8) 0.1584(8) 0.3497(7) 0.141(11) Uiso 1 calc R . H2B H 0.4126(8) 0.0338(8) 0.3070(7) 0.141(11) Uiso 1 calc R . H2C H 0.5013(8) 0.0757(8) 0.4222(7) 0.141(11) Uiso 1 calc R . C3 C 0.4648(5) 0.3824(4) 0.5491(4) 0.0596(15) Uani 1 d . . H3A H 0.4324(5) 0.3815(4) 0.4772(4) 0.141(11) Uiso 1 calc R . H3B H 0.5503(5) 0.3802(4) 0.5589(4) 0.141(11) Uiso 1 calc R . H3C H 0.4674(5) 0.4497(4) 0.5950(4) 0.141(11) Uiso 1 calc R . C4 C 0.2025(6) 0.3524(4) 0.3620(4) 0.0606(15) Uani 1 d . . H4A H 0.2415(6) 0.3864(4) 0.4359(4) 0.141(11) Uiso 1 calc R . H4B H 0.1145(6) 0.3488(4) 0.3457(4) 0.141(11) Uiso 1 calc R . H4C H 0.2496(6) 0.3963(4) 0.3218(4) 0.141(11) Uiso 1 calc R . C5 C 0.5736(5) 0.3029(4) 0.7229(4) 0.0447(11) Uani 1 d . . C6 C 0.3618(4) 0.3447(4) 0.7640(3) 0.0400(10) Uani 1 d . . C7 C 0.0473(4) 0.2092(4) 0.1547(3) 0.0406(10) Uani 1 d . . C8 C 0.2632(4) 0.1598(4) 0.1697(3) 0.0418(10) Uani 1 d . . C11 C 0.3557(5) 0.0793(4) 0.7322(4) 0.0522(12) Uani 1 d . . H11 H 0.4060(5) 0.1039(4) 0.8014(4) 0.070(7) Uiso 1 calc R . C12 C 0.2800(5) -0.0291(4) 0.6818(4) 0.0523(12) Uani 1 d . . H12 H 0.2693(5) -0.0917(4) 0.7083(4) 0.070(7) Uiso 1 calc R . C13 C 0.2229(5) -0.0256(4) 0.5834(4) 0.0478(11) Uani 1 d . . H13 H 0.1648(5) -0.0875(4) 0.5308(4) 0.070(7) Uiso 1 calc R . C21 C -0.0256(5) -0.0372(4) 0.1742(4) 0.0495(12) Uani 1 d . . H21 H -0.0618(5) -0.0427(4) 0.1043(4) 0.070(7) Uiso 1 calc R . C22 C -0.0619(5) -0.1200(4) 0.2254(4) 0.0495(12) Uani 1 d . . H22 H -0.1246(5) -0.1913(4) 0.1974(4) 0.070(7) Uiso 1 calc R . C23 C 0.0144(4) -0.0747(4) 0.3268(4) 0.0437(11) Uani 1 d . . H23 H 0.0105(4) -0.1106(4) 0.3809(4) 0.070(7) Uiso 1 calc R . C51 C 0.6591(5) 0.4087(5) 0.7854(4) 0.0594(14) Uani 1 d . . H51 H 0.6261(5) 0.4628(5) 0.8100(4) 0.077(4) Uiso 1 calc R . C52 C 0.7917(6) 0.4343(7) 0.8111(5) 0.084(2) Uani 1 d . . H52 H 0.8467(6) 0.5049(7) 0.8524(5) 0.077(4) Uiso 1 calc R . C53 C 0.8419(7) 0.3544(9) 0.7753(7) 0.095(3) Uani 1 d . . H53 H 0.9308(7) 0.3715(9) 0.7918(7) 0.077(4) Uiso 1 calc R . C54 C 0.7610(7) 0.2506(8) 0.7156(7) 0.095(3) Uani 1 d . . H54 H 0.7945(7) 0.1964(8) 0.6923(7) 0.077(4) Uiso 1 calc R . C55 C 0.6297(6) 0.2264(5) 0.6899(5) 0.066(2) Uani 1 d . . H55 H 0.5762(6) 0.1554(5) 0.6484(5) 0.077(4) Uiso 1 calc R . C61 C 0.2755(5) 0.3942(4) 0.7286(4) 0.0488(11) Uani 1 d . . H61 H 0.2523(5) 0.3900(4) 0.6571(4) 0.077(4) Uiso 1 calc R . C62 C 0.2226(6) 0.4498(5) 0.7969(5) 0.0601(14) Uani 1 d . . H62 H 0.1660(6) 0.4832(5) 0.7712(5) 0.077(4) Uiso 1 calc R . C63 C 0.2542(6) 0.4551(5) 0.9021(5) 0.068(2) Uani 1 d . . H63 H 0.2188(6) 0.4920(5) 0.9480(5) 0.077(4) Uiso 1 calc R . C64 C 0.3371(6) 0.4067(5) 0.9395(4) 0.063(2) Uani 1 d . . H64 H 0.3577(6) 0.4102(5) 1.0110(4) 0.077(4) Uiso 1 calc R . C65 C 0.3913(5) 0.3523(4) 0.8727(4) 0.0530(12) Uani 1 d . . H65 H 0.4485(5) 0.3201(4) 0.9000(4) 0.077(4) Uiso 1 calc R . C71 C 0.0602(5) 0.2388(4) 0.0622(4) 0.0497(12) Uani 1 d . . H71 H 0.1318(5) 0.2368(4) 0.0377(4) 0.077(4) Uiso 1 calc R . C72 C -0.0299(6) 0.2716(5) 0.0045(4) 0.065(2) Uani 1 d . . H72 H -0.0181(6) 0.2905(5) -0.0578(4) 0.077(4) Uiso 1 calc R . C73 C -0.1361(6) 0.2762(5) 0.0385(5) 0.074(2) Uani 1 d . . H73 H -0.1965(6) 0.2982(5) -0.0004(5) 0.077(4) Uiso 1 calc R . C74 C -0.1523(6) 0.2480(6) 0.1307(6) 0.076(2) Uani 1 d . . H74 H -0.2231(6) 0.2522(6) 0.1554(6) 0.077(4) Uiso 1 calc R . C75 C -0.0633(5) 0.2132(5) 0.1865(5) 0.0631(15) Uani 1 d . . H75 H -0.0773(5) 0.1918(5) 0.2474(5) 0.077(4) Uiso 1 calc R . C81 C 0.3729(5) 0.2548(5) 0.1835(5) 0.0595(14) Uani 1 d . . H81 H 0.3803(5) 0.3222(5) 0.2272(5) 0.077(4) Uiso 1 calc R . C82 C 0.4707(6) 0.2522(7) 0.1345(6) 0.077(2) Uani 1 d . . H82 H 0.5428(6) 0.3169(7) 0.1470(6) 0.077(4) Uiso 1 calc R . C83 C 0.4619(7) 0.1556(8) 0.0684(5) 0.087(2) Uani 1 d . . H83 H 0.5269(7) 0.1539(8) 0.0347(5) 0.077(4) Uiso 1 calc R . C84 C 0.3562(7) 0.0611(7) 0.0522(6) 0.092(2) Uani 1 d . . H84 H 0.3493(7) -0.0055(7) 0.0074(6) 0.077(4) Uiso 1 calc R . C85 C 0.2598(6) 0.0639(5) 0.1017(5) 0.067(2) Uani 1 d . . H85 H 0.1889(6) -0.0018(5) 0.0890(5) 0.077(4) Uiso 1 calc R . B1 B 0.4200(5) 0.2753(4) 0.6860(4) 0.0377(11) Uani 1 d . . B2 B 0.1481(5) 0.1677(4) 0.2218(4) 0.0369(10) Uani 1 d . . Cl1 Cl 0.2628(3) 0.6196(3) 0.5996(2) 0.1534(12) Uani 1 d . . Cl2 Cl 0.0588(2) 0.6697(2) 0.4821(2) 0.1190(8) Uani 1 d . . C1S C 0.1731(11) 0.6111(10) 0.4823(8) 0.141(4) Uani 1 d . . H1S1 H 0.1307(11) 0.5325(10) 0.4451(8) 0.169 Uiso 1 calc R . H1S2 H 0.2306(11) 0.6460(10) 0.4424(8) 0.169 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.03276(9) 0.02817(8) 0.03078(8) 0.00848(6) 0.01016(6) 0.00728(6) O1 0.043(2) 0.042(2) 0.039(2) 0.0101(13) 0.0147(14) 0.0148(14) O2 0.040(2) 0.038(2) 0.048(2) 0.0117(14) 0.0185(14) 0.0141(14) O3 0.038(2) 0.0310(14) 0.0326(15) 0.0103(12) 0.0089(12) 0.0028(12) O4 0.046(2) 0.0291(14) 0.0317(15) 0.0082(12) 0.0085(13) 0.0091(13) N1 0.039(2) 0.033(2) 0.039(2) 0.0103(15) 0.010(2) 0.010(2) N2 0.042(2) 0.032(2) 0.033(2) 0.0081(14) 0.011(2) 0.007(2) N11 0.042(2) 0.038(2) 0.034(2) 0.0132(15) 0.008(2) 0.009(2) N21 0.040(2) 0.035(2) 0.031(2) 0.0060(14) 0.007(2) 0.004(2) C2 0.119(7) 0.158(8) 0.111(6) 0.055(6) 0.066(5) 0.108(7) C3 0.052(3) 0.052(3) 0.056(3) 0.028(3) 0.009(2) -0.011(2) C4 0.090(4) 0.035(3) 0.049(3) 0.007(2) 0.002(3) 0.023(3) C5 0.042(3) 0.054(3) 0.039(2) 0.019(2) 0.008(2) 0.016(2) C6 0.039(2) 0.037(2) 0.035(2) 0.007(2) 0.008(2) 0.003(2) C7 0.036(2) 0.041(2) 0.036(2) 0.008(2) 0.005(2) 0.006(2) C8 0.041(2) 0.047(3) 0.033(2) 0.011(2) 0.007(2) 0.012(2) C11 0.055(3) 0.060(3) 0.045(3) 0.027(2) 0.008(2) 0.019(3) C12 0.057(3) 0.042(3) 0.065(3) 0.030(2) 0.022(3) 0.015(2) C13 0.053(3) 0.034(2) 0.054(3) 0.017(2) 0.010(2) 0.012(2) C21 0.046(3) 0.045(3) 0.039(2) 0.004(2) 0.002(2) 0.000(2) C22 0.046(3) 0.035(2) 0.052(3) 0.004(2) 0.012(2) -0.002(2) C23 0.044(3) 0.032(2) 0.050(3) 0.011(2) 0.016(2) 0.005(2) C51 0.049(3) 0.069(4) 0.044(3) 0.016(3) 0.003(2) 0.004(3) C52 0.048(4) 0.111(6) 0.057(4) 0.030(4) -0.005(3) -0.013(4) C53 0.044(4) 0.159(8) 0.096(6) 0.077(6) 0.014(4) 0.032(5) C54 0.066(5) 0.134(7) 0.122(7) 0.063(6) 0.042(5) 0.061(5) C55 0.059(4) 0.068(4) 0.076(4) 0.025(3) 0.017(3) 0.024(3) C61 0.052(3) 0.044(3) 0.043(3) 0.007(2) 0.008(2) 0.013(2) C62 0.058(3) 0.053(3) 0.070(4) 0.010(3) 0.022(3) 0.021(3) C63 0.069(4) 0.063(4) 0.061(4) -0.002(3) 0.033(3) 0.012(3) C64 0.067(4) 0.071(4) 0.042(3) 0.008(3) 0.025(3) 0.010(3) C65 0.053(3) 0.057(3) 0.038(2) 0.009(2) 0.010(2) 0.008(2) C71 0.054(3) 0.057(3) 0.041(2) 0.017(2) 0.009(2) 0.022(2) C72 0.078(4) 0.073(4) 0.048(3) 0.025(3) 0.008(3) 0.034(3) C73 0.066(4) 0.073(4) 0.077(4) 0.019(3) -0.009(3) 0.030(3) C74 0.049(3) 0.095(5) 0.090(5) 0.029(4) 0.019(3) 0.032(3) C75 0.047(3) 0.084(4) 0.066(4) 0.033(3) 0.017(3) 0.024(3) C81 0.051(3) 0.060(3) 0.066(3) 0.017(3) 0.022(3) 0.013(3) C82 0.043(3) 0.100(5) 0.085(5) 0.031(4) 0.027(3) 0.014(3) C83 0.060(4) 0.132(7) 0.072(4) 0.013(4) 0.031(3) 0.037(4) C84 0.076(5) 0.106(6) 0.081(5) -0.018(4) 0.027(4) 0.034(4) C85 0.055(3) 0.064(4) 0.069(4) -0.006(3) 0.021(3) 0.014(3) B1 0.039(3) 0.035(2) 0.033(2) 0.011(2) 0.007(2) 0.005(2) B2 0.041(3) 0.033(2) 0.030(2) 0.008(2) 0.008(2) 0.006(2) Cl1 0.181(3) 0.196(3) 0.125(2) 0.075(2) 0.050(2) 0.098(3) Cl2 0.111(2) 0.0951(15) 0.175(2) 0.043(2) 0.059(2) 0.0513(14) C1S 0.189(11) 0.170(10) 0.129(8) 0.052(8) 0.057(8) 0.138(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 1.693(3) . ? Re1 O2 1.857(3) . ? Re1 N1 2.055(4) . ? Re1 N2 2.062(3) . ? Re1 O3 2.100(3) . ? Re1 O4 2.122(3) . ? O2 C2 1.362(7) . ? O3 C3 1.431(5) . ? O3 B1 1.538(5) . ? O4 C4 1.433(5) . ? O4 B2 1.543(5) . ? N1 C13 1.345(6) . ? N1 N11 1.364(5) . ? N2 C23 1.345(5) . ? N2 N21 1.360(5) . ? N11 C11 1.333(6) . ? N11 B1 1.585(6) . ? N21 C21 1.337(6) . ? N21 B2 1.574(6) . ? C5 C55 1.386(8) . ? C5 C51 1.404(7) . ? C5 B1 1.615(7) . ? C6 C61 1.386(7) . ? C6 C65 1.406(6) . ? C6 B1 1.614(7) . ? C7 C71 1.379(6) . ? C7 C75 1.401(7) . ? C7 B2 1.607(7) . ? C8 C85 1.386(7) . ? C8 C81 1.401(7) . ? C8 B2 1.601(7) . ? C11 C12 1.363(7) . ? C12 C13 1.370(7) . ? C21 C22 1.374(7) . ? C22 C23 1.374(7) . ? C51 C52 1.388(8) . ? C52 C53 1.383(11) . ? C53 C54 1.362(12) . ? C54 C55 1.376(9) . ? C61 C62 1.390(7) . ? C62 C63 1.368(8) . ? C63 C64 1.355(9) . ? C64 C65 1.380(7) . ? C71 C72 1.384(7) . ? C72 C73 1.369(9) . ? C73 C74 1.375(9) . ? C74 C75 1.380(8) . ? C81 C82 1.386(8) . ? C82 C83 1.360(10) . ? C83 C84 1.366(10) . ? C84 C85 1.376(8) . ? Cl1 C1S 1.668(10) . ? Cl2 C1S 1.690(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 O2 176.38(14) . . ? O1 Re1 N1 93.06(15) . . ? O2 Re1 N1 89.85(14) . . ? O1 Re1 N2 93.04(15) . . ? O2 Re1 N2 88.39(14) . . ? N1 Re1 N2 102.87(14) . . ? O1 Re1 O3 93.05(13) . . ? O2 Re1 O3 85.49(13) . . ? N1 Re1 O3 77.55(12) . . ? N2 Re1 O3 173.87(13) . . ? O1 Re1 O4 89.40(13) . . ? O2 Re1 O4 87.64(13) . . ? N1 Re1 O4 177.23(13) . . ? N2 Re1 O4 78.22(12) . . ? O3 Re1 O4 101.08(11) . . ? C2 O2 Re1 175.9(4) . . ? C3 O3 B1 116.3(3) . . ? C3 O3 Re1 122.1(3) . . ? B1 O3 Re1 121.1(2) . . ? C4 O4 B2 120.1(3) . . ? C4 O4 Re1 119.8(3) . . ? B2 O4 Re1 117.3(2) . . ? C13 N1 N11 106.3(4) . . ? C13 N1 Re1 136.2(3) . . ? N11 N1 Re1 117.5(3) . . ? C23 N2 N21 107.5(4) . . ? C23 N2 Re1 135.8(3) . . ? N21 N2 Re1 116.4(3) . . ? C11 N11 N1 108.6(4) . . ? C11 N11 B1 129.7(4) . . ? N1 N11 B1 121.7(3) . . ? C21 N21 N2 108.2(4) . . ? C21 N21 B2 130.3(4) . . ? N2 N21 B2 121.5(3) . . ? C55 C5 C51 116.0(5) . . ? C55 C5 B1 122.2(5) . . ? C51 C5 B1 121.7(5) . . ? C61 C6 C65 116.3(5) . . ? C61 C6 B1 122.9(4) . . ? C65 C6 B1 120.6(4) . . ? C71 C7 C75 115.9(5) . . ? C71 C7 B2 123.4(4) . . ? C75 C7 B2 120.7(4) . . ? C85 C8 C81 114.5(5) . . ? C85 C8 B2 124.2(4) . . ? C81 C8 B2 121.1(4) . . ? N11 C11 C12 109.8(4) . . ? C11 C12 C13 104.9(4) . . ? N1 C13 C12 110.4(4) . . ? N21 C21 C22 109.5(4) . . ? C23 C22 C21 105.1(4) . . ? N2 C23 C22 109.6(4) . . ? C52 C51 C5 121.4(6) . . ? C53 C52 C51 119.8(7) . . ? C54 C53 C52 119.9(7) . . ? C53 C54 C55 119.8(8) . . ? C54 C55 C5 123.0(7) . . ? C6 C61 C62 121.9(5) . . ? C63 C62 C61 119.7(6) . . ? C64 C63 C62 120.1(5) . . ? C63 C64 C65 120.7(5) . . ? C64 C65 C6 121.2(5) . . ? C7 C71 C72 122.2(5) . . ? C73 C72 C71 120.5(5) . . ? C72 C73 C74 119.2(6) . . ? C73 C74 C75 119.9(6) . . ? C74 C75 C7 122.3(5) . . ? C82 C81 C8 122.6(6) . . ? C83 C82 C81 120.3(6) . . ? C82 C83 C84 119.0(6) . . ? C83 C84 C85 120.5(7) . . ? C84 C85 C8 123.1(6) . . ? O3 B1 N11 100.2(3) . . ? O3 B1 C6 110.6(4) . . ? N11 B1 C6 109.9(4) . . ? O3 B1 C5 110.6(4) . . ? N11 B1 C5 108.7(4) . . ? C6 B1 C5 115.8(4) . . ? O4 B2 N21 100.9(3) . . ? O4 B2 C8 109.4(4) . . ? N21 B2 C8 111.9(4) . . ? O4 B2 C7 112.0(4) . . ? N21 B2 C7 107.9(4) . . ? C8 B2 C7 114.0(4) . . ? Cl1 C1S Cl2 116.9(6) . . ? _refine_diff_density_max 0.879 _refine_diff_density_min -0.956 _refine_diff_density_rms 0.108 data_newrehb _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H39 B N4 O P Re' _chemical_formula_weight 699.63 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8554(7) _cell_length_b 11.0350(10) _cell_length_c 14.868(2) _cell_angle_alpha 107.354(7) _cell_angle_beta 91.229(5) _cell_angle_gamma 100.002(5) _cell_volume 1515.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method ? _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 4.091 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6841 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.96 _reflns_number_total 6579 _reflns_number_observed 5316 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 544 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.6832P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6035 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_obs 0.0286 _refine_ls_wR_factor_all 0.0944 _refine_ls_wR_factor_obs 0.0703 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 0.975 _refine_ls_restrained_S_all 1.170 _refine_ls_restrained_S_obs 0.975 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.22476(2) 0.23076(2) 0.256207(11) 0.05255(7) Uani 1 d . . P P 0.33411(10) 0.15053(11) 0.35950(7) 0.0469(2) Uani 1 d . . N1 N 0.1921(4) 0.0702(4) 0.1249(2) 0.0551(8) Uani 1 d . . N2 N 0.1794(5) 0.3383(4) 0.1624(3) 0.0720(11) Uani 1 d . . N11 N 0.2730(4) 0.0937(4) 0.0551(3) 0.0620(9) Uani 1 d . . N21 N 0.2575(5) 0.3241(4) 0.0863(3) 0.0779(13) Uani 1 d . . C1 C 0.5202(4) 0.2170(4) 0.3901(3) 0.0507(9) Uani 1 d . . C2 C 0.2708(4) 0.1757(5) 0.4779(3) 0.0520(10) Uani 1 d . . C3 C 0.3329(4) -0.0244(4) 0.3209(3) 0.0529(10) Uani 1 d . . C11 C 0.2464(6) -0.0118(6) -0.0228(3) 0.0722(13) Uani 1 d . . C12 C 0.1484(6) -0.1010(5) -0.0032(4) 0.0776(15) Uani 1 d . . H12 H 0.1104(6) -0.1825(5) -0.0440(4) 0.101(21) Uiso 1 calc R . C13 C 0.1155(5) -0.0481(5) 0.0888(3) 0.0623(11) Uani 1 d . . C21 C 0.2226(9) 0.3976(6) 0.0347(5) 0.097(2) Uani 1 d . . C22 C 0.1248(9) 0.4591(7) 0.0798(6) 0.114(3) Uani 1 d . . H22 H 0.0827(9) 0.5173(7) 0.0605(6) 0.103(21) Uiso 1 calc R . C23 C 0.0975(7) 0.4211(5) 0.1598(5) 0.092(2) Uani 1 d . . C101 C 0.6215(4) 0.1426(5) 0.3685(3) 0.0562(10) Uani 1 d . . H101 H 0.5968(4) 0.0538(5) 0.3397(3) 0.095(5) Uiso 1 calc R . C102 C 0.7608(5) 0.2005(6) 0.3898(4) 0.0698(13) Uani 1 d . . H102 H 0.8283(5) 0.1499(6) 0.3746(4) 0.095(5) Uiso 1 calc R . C103 C 0.7990(5) 0.3301(6) 0.4325(4) 0.0771(15) Uani 1 d . . H103 H 0.8920(5) 0.3682(6) 0.4455(4) 0.095(5) Uiso 1 calc R . C104 C 0.6998(6) 0.4036(6) 0.4561(5) 0.086(2) Uani 1 d . . H104 H 0.7251(6) 0.4918(6) 0.4871(5) 0.095(5) Uiso 1 calc R . C105 C 0.5619(5) 0.3478(5) 0.4342(4) 0.0740(14) Uani 1 d . . H105 H 0.4956(5) 0.3995(5) 0.4496(4) 0.095(5) Uiso 1 calc R . C111 C 0.3200(8) -0.0145(8) -0.1108(4) 0.106(2) Uani 1 d . . H11A H 0.3835(8) 0.0657(8) -0.1005(4) 0.245(24) Uiso 1 calc R . H11B H 0.2537(8) -0.0264(8) -0.1624(4) 0.245(24) Uiso 1 calc R . H11C H 0.3698(8) -0.0845(8) -0.1256(4) 0.245(24) Uiso 1 calc R . C131 C 0.0174(6) -0.1068(6) 0.1450(4) 0.081(2) Uani 1 d . . H13A H 0.0171(6) -0.0460(6) 0.2066(4) 0.245(24) Uiso 1 calc R . H13B H 0.0451(6) -0.1832(6) 0.1513(4) 0.245(24) Uiso 1 calc R . H13C H -0.0738(6) -0.1291(6) 0.1137(4) 0.245(24) Uiso 1 calc R . C201 C 0.1345(5) 0.1835(7) 0.4917(3) 0.078(2) Uani 1 d . . H201 H 0.0750(5) 0.1791(7) 0.4409(3) 0.095(5) Uiso 1 calc R . C202 C 0.0843(6) 0.1977(8) 0.5800(4) 0.099(2) Uani 1 d . . H202 H -0.0085(6) 0.2011(8) 0.5874(4) 0.095(5) Uiso 1 calc R . C203 C 0.1688(6) 0.2067(7) 0.6555(4) 0.088(2) Uani 1 d . . H203 H 0.1351(6) 0.2179(7) 0.7149(4) 0.095(5) Uiso 1 calc R . C204 C 0.3042(6) 0.1992(7) 0.6434(3) 0.090(2) Uani 1 d . . H204 H 0.3629(6) 0.2037(7) 0.6946(3) 0.095(5) Uiso 1 calc R . C205 C 0.3551(5) 0.1849(6) 0.5556(3) 0.077(2) Uani 1 d . . H205 H 0.4481(5) 0.1814(6) 0.5490(3) 0.095(5) Uiso 1 calc R . C211 C 0.2923(9) 0.4043(8) -0.0527(5) 0.131(3) Uani 1 d . . H21A H 0.3577(9) 0.3473(8) -0.0649(5) 0.273(28) Uiso 1 calc R . H21B H 0.3395(9) 0.4912(8) -0.0439(5) 0.273(28) Uiso 1 calc R . H21C H 0.2243(9) 0.3786(8) -0.1054(5) 0.273(28) Uiso 1 calc R . C231 C 0.0001(9) 0.4605(8) 0.2348(6) 0.122(3) Uani 1 d . . H23A H 0.0069(9) 0.4157(8) 0.2805(6) 0.273(28) Uiso 1 calc R . H23B H -0.0928(9) 0.4390(8) 0.2064(6) 0.273(28) Uiso 1 calc R . H23C H 0.0240(9) 0.5521(8) 0.2655(6) 0.273(28) Uiso 1 calc R . C301 C 0.3647(5) -0.0787(5) 0.2280(3) 0.0639(12) Uani 1 d . . H301 H 0.3864(5) -0.0266(5) 0.1894(3) 0.095(5) Uiso 1 calc R . C302 C 0.3637(6) -0.2092(6) 0.1938(4) 0.079(2) Uani 1 d . . H302 H 0.3862(6) -0.2449(6) 0.1323(4) 0.095(5) Uiso 1 calc R . C303 C 0.3298(6) -0.2871(6) 0.2498(5) 0.086(2) Uani 1 d . . H303 H 0.3289(6) -0.3754(6) 0.2259(5) 0.095(5) Uiso 1 calc R . C304 C 0.2975(5) -0.2354(6) 0.3406(5) 0.0792(15) Uani 1 d . . H304 H 0.2748(5) -0.2884(6) 0.3785(5) 0.095(5) Uiso 1 calc R . C305 C 0.2986(5) -0.1047(5) 0.3759(4) 0.0646(12) Uani 1 d . . H305 H 0.2760(5) -0.0701(5) 0.4375(4) 0.095(5) Uiso 1 calc R . B B 0.3588(7) 0.2293(6) 0.0797(4) 0.074(2) Uani 1 d . . H0 H 0.4305(7) 0.2378(6) 0.0362(4) 0.066(14) Uiso 1 calc R . C1A C 0.5585(11) 0.3294(11) 0.2055(7) 0.063(3) Uani 0.53(2) d P 1 H1A1 H 0.6155(11) 0.3084(11) 0.1527(7) 0.066(15) Uiso 0.53(2) calc PR 1 H1A2 H 0.5983(11) 0.3085(11) 0.2580(7) 0.066(15) Uiso 0.53(2) calc PR 1 C2A C 0.5486(14) 0.4690(14) 0.2334(10) 0.085(4) Uani 0.53(2) d P 1 H2A1 H 0.6395(14) 0.5210(14) 0.2511(10) 0.109(18) Uiso 0.53(2) calc PR 1 H2A2 H 0.4926(14) 0.4882(14) 0.2860(10) 0.109(18) Uiso 0.53(2) calc PR 1 H2A3 H 0.5074(14) 0.4875(14) 0.1811(10) 0.109(18) Uiso 0.53(2) calc PR 1 C1B C 0.5060(13) 0.3920(15) 0.2135(9) 0.063(4) Uani 0.47(2) d P 2 H1B1 H 0.4799(13) 0.4476(15) 0.1790(9) 0.066(15) Uiso 0.47(2) calc PR 2 H1B2 H 0.4985(13) 0.4317(15) 0.2804(9) 0.066(15) Uiso 0.47(2) calc PR 2 C2B C 0.6486(12) 0.3693(14) 0.1953(11) 0.087(5) Uani 0.47(2) d P 2 H2B1 H 0.7122(12) 0.4505(14) 0.2150(11) 0.109(18) Uiso 0.47(2) calc PR 2 H2B2 H 0.6531(12) 0.3282(14) 0.1290(11) 0.109(18) Uiso 0.47(2) calc PR 2 H2B3 H 0.6724(12) 0.3146(14) 0.2303(11) 0.109(18) Uiso 0.47(2) calc PR 2 O O 0.4149(3) 0.2573(3) 0.1783(2) 0.0683(9) Uani 1 d . . H1 H 0.3092 0.3692 0.3303 0.050 Uiso 1 d . . H2 H 0.0562 0.2103 0.2432 0.050 Uiso 1 d . . H3 H 0.1132 0.1272 0.2911 0.050 Uiso 1 d . . H4 H 0.1565 0.3235 0.3456 0.050 Uiso 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 Re 0.04984(10) 0.05871(11) 0.04354(10) 0.01178(7) 0.00029(6) 0.00285(7) P 0.0350(4) 0.0614(6) 0.0382(5) 0.0079(4) 0.0051(4) 0.0053(4) N1 0.055(2) 0.064(2) 0.043(2) 0.016(2) 0.0019(14) 0.002(2) N2 0.085(3) 0.059(2) 0.070(3) 0.024(2) -0.015(2) 0.003(2) N11 0.066(2) 0.072(2) 0.047(2) 0.021(2) 0.009(2) 0.004(2) N21 0.098(3) 0.067(3) 0.064(3) 0.032(2) -0.017(2) -0.015(2) C1 0.037(2) 0.066(3) 0.041(2) 0.008(2) 0.0034(15) 0.004(2) C2 0.040(2) 0.072(3) 0.038(2) 0.009(2) 0.0054(15) 0.010(2) C3 0.037(2) 0.063(3) 0.051(2) 0.006(2) 0.000(2) 0.009(2) C11 0.087(4) 0.077(3) 0.049(3) 0.012(2) 0.008(2) 0.020(3) C12 0.095(4) 0.062(3) 0.062(3) 0.004(2) -0.002(3) 0.005(3) C13 0.060(3) 0.064(3) 0.056(2) 0.014(2) -0.006(2) -0.002(2) C21 0.123(6) 0.070(4) 0.087(4) 0.041(3) -0.045(4) -0.032(4) C22 0.139(7) 0.066(4) 0.131(7) 0.044(4) -0.066(6) -0.011(4) C23 0.108(5) 0.053(3) 0.099(5) 0.013(3) -0.039(4) 0.000(3) C101 0.043(2) 0.071(3) 0.052(2) 0.016(2) 0.003(2) 0.010(2) C102 0.039(2) 0.100(4) 0.069(3) 0.022(3) 0.006(2) 0.015(2) C103 0.041(2) 0.102(4) 0.076(3) 0.019(3) 0.000(2) -0.006(2) C104 0.059(3) 0.081(4) 0.091(4) -0.002(3) -0.006(3) -0.006(3) C105 0.047(2) 0.072(3) 0.081(3) -0.008(3) 0.001(2) 0.008(2) C111 0.134(6) 0.121(6) 0.060(3) 0.017(3) 0.038(4) 0.027(5) C131 0.071(3) 0.078(4) 0.079(3) 0.023(3) -0.001(3) -0.018(3) C201 0.044(2) 0.138(5) 0.054(3) 0.030(3) 0.010(2) 0.021(3) C202 0.054(3) 0.172(7) 0.067(3) 0.029(4) 0.025(3) 0.025(4) C203 0.078(4) 0.133(5) 0.047(3) 0.018(3) 0.027(2) 0.013(3) C204 0.076(3) 0.148(6) 0.040(2) 0.022(3) 0.004(2) 0.019(4) C205 0.051(3) 0.128(5) 0.046(2) 0.016(3) 0.003(2) 0.020(3) C211 0.154(7) 0.140(7) 0.100(5) 0.084(5) -0.041(5) -0.050(5) C231 0.128(6) 0.095(5) 0.138(7) 0.015(5) -0.013(5) 0.047(5) C301 0.055(2) 0.078(3) 0.052(2) 0.006(2) 0.005(2) 0.018(2) C302 0.068(3) 0.082(4) 0.071(3) -0.009(3) -0.002(3) 0.029(3) C303 0.068(3) 0.065(3) 0.109(5) 0.002(3) -0.012(3) 0.016(3) C304 0.061(3) 0.073(3) 0.099(4) 0.026(3) -0.008(3) 0.003(2) C305 0.049(2) 0.072(3) 0.068(3) 0.020(2) 0.001(2) 0.004(2) B 0.075(4) 0.083(4) 0.060(3) 0.034(3) 0.005(3) -0.014(3) C1A 0.056(7) 0.056(6) 0.081(6) 0.029(5) 0.011(5) 0.009(5) C2A 0.079(8) 0.059(8) 0.115(10) 0.033(7) -0.002(6) -0.008(6) C1B 0.054(7) 0.059(9) 0.080(7) 0.038(6) -0.003(5) -0.005(6) C2B 0.043(7) 0.101(10) 0.135(12) 0.075(9) 0.010(6) -0.006(6) O 0.054(2) 0.085(2) 0.061(2) 0.031(2) -0.0019(14) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re N2 2.167(4) . ? Re N1 2.183(4) . ? Re O 2.246(3) . ? Re P 2.3185(11) . ? Re H1 1.6595(2) . ? Re H2 1.6365(2) . ? Re H3 1.6506(2) . ? Re H4 1.6530(2) . ? P C3 1.840(5) . ? P C2 1.839(4) . ? P C1 1.845(4) . ? N1 C13 1.336(6) . ? N1 N11 1.379(5) . ? N2 C23 1.329(8) . ? N2 N21 1.368(7) . ? N11 C11 1.357(6) . ? N11 B 1.520(7) . ? N21 C21 1.349(7) . ? N21 B 1.551(9) . ? C1 C105 1.378(6) . ? C1 C101 1.384(6) . ? C2 C205 1.376(6) . ? C2 C201 1.377(6) . ? C3 C305 1.382(7) . ? C3 C301 1.398(6) . ? C11 C12 1.355(8) . ? C11 C111 1.505(8) . ? C12 C13 1.389(7) . ? C12 H12 0.93 . ? C13 C131 1.480(7) . ? C21 C22 1.350(11) . ? C21 C211 1.498(11) . ? C22 C23 1.391(11) . ? C22 H22 0.93 . ? C23 C231 1.502(11) . ? C101 C102 1.396(6) . ? C101 H101 0.93 . ? C102 C103 1.361(8) . ? C102 H102 0.93 . ? C103 C104 1.363(8) . ? C103 H103 0.93 . ? C104 C105 1.379(7) . ? C104 H104 0.93 . ? C105 H105 0.93 . ? C111 H11A 0.96 . ? C111 H11B 0.96 . ? C111 H11C 0.96 . ? C131 H13A 0.96 . ? C131 H13B 0.96 . ? C131 H13C 0.96 . ? C201 C202 1.387(7) . ? C201 H201 0.93 . ? C202 C203 1.353(8) . ? C202 H202 0.93 . ? C203 C204 1.364(8) . ? C203 H203 0.93 . ? C204 C205 1.382(7) . ? C204 H204 0.93 . ? C205 H205 0.93 . ? C211 H21A 0.96 . ? C211 H21B 0.96 . ? C211 H21C 0.96 . ? C231 H23A 0.96 . ? C231 H23B 0.96 . ? C231 H23C 0.96 . ? C301 C302 1.375(7) . ? C301 H301 0.93 . ? C302 C303 1.372(9) . ? C302 H302 0.93 . ? C303 C304 1.368(9) . ? C303 H303 0.93 . ? C304 C305 1.378(8) . ? C304 H304 0.93 . ? C305 H305 0.93 . ? B O 1.478(6) . ? B H0 0.98 . ? C1A O 1.480(11) . ? C1A C2A 1.49(2) . ? C1A H1A1 0.97 . ? C1A H1A2 0.97 . ? C2A H2A1 0.96 . ? C2A H2A2 0.96 . ? C2A H2A3 0.96 . ? C1B C2B 1.49(2) . ? C1B O 1.530(15) . ? C1B H1B1 0.97 . ? C1B H1B2 0.97 . ? C2B H2B1 0.96 . ? C2B H2B2 0.96 . ? C2B H2B3 0.96 . ? 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 N2 Re N1 82.46(15) . . ? N2 Re O 74.0(2) . . ? N1 Re O 73.87(13) . . ? N2 Re P 163.98(12) . . ? N1 Re P 103.06(10) . . ? O Re P 92.87(9) . . ? N2 Re H1 87.90(11) . . ? N1 Re H1 154.44(9) . . ? O Re H1 80.74(9) . . ? P Re H1 80.78(3) . . ? N2 Re H2 73.73(13) . . ? N1 Re H2 82.21(9) . . ? O Re H2 141.87(8) . . ? P Re H2 121.64(3) . . ? H1 Re H2 117.699(12) . . ? N2 Re H3 126.65(12) . . ? N1 Re H3 81.56(9) . . ? O Re H3 145.53(10) . . ? P Re H3 69.32(3) . . ? H1 Re H3 122.617(13) . . ? H2 Re H3 53.837(7) . . ? N2 Re H4 92.73(13) . . ? N1 Re H4 148.04(9) . . ? O Re H4 135.14(9) . . ? P Re H4 90.20(3) . . ? H1 Re H4 55.649(8) . . ? H2 Re H4 66.200(9) . . ? H3 Re H4 76.127(11) . . ? C3 P C2 101.8(2) . . ? C3 P C1 101.4(2) . . ? C2 P C1 100.8(2) . . ? C3 P Re 116.76(14) . . ? C2 P Re 117.30(14) . . ? C1 P Re 116.12(15) . . ? C13 N1 N11 107.0(4) . . ? C13 N1 Re 139.5(3) . . ? N11 N1 Re 113.5(3) . . ? C23 N2 N21 108.5(5) . . ? C23 N2 Re 137.0(5) . . ? N21 N2 Re 114.4(3) . . ? C11 N11 N1 108.9(4) . . ? C11 N11 B 136.0(4) . . ? N1 N11 B 114.9(4) . . ? C21 N21 N2 109.0(6) . . ? C21 N21 B 136.5(6) . . ? N2 N21 B 114.4(4) . . ? C105 C1 C101 117.7(4) . . ? C105 C1 P 118.9(3) . . ? C101 C1 P 123.3(3) . . ? C205 C2 C201 117.2(4) . . ? C205 C2 P 122.3(3) . . ? C201 C2 P 120.6(3) . . ? C305 C3 C301 118.6(5) . . ? C305 C3 P 124.6(4) . . ? C301 C3 P 116.7(4) . . ? N11 C11 C12 107.8(4) . . ? N11 C11 C111 120.9(5) . . ? C12 C11 C111 131.3(5) . . ? C11 C12 C13 107.3(5) . . ? C11 C12 H12 126.3(3) . . ? C13 C12 H12 126.3(3) . . ? N1 C13 C12 108.9(5) . . ? N1 C13 C131 122.0(4) . . ? C12 C13 C131 129.0(5) . . ? C22 C21 N21 106.8(7) . . ? C22 C21 C211 131.5(7) . . ? N21 C21 C211 121.7(8) . . ? C21 C22 C23 108.8(6) . . ? C21 C22 H22 125.6(4) . . ? C23 C22 H22 125.6(5) . . ? N2 C23 C22 106.9(7) . . ? N2 C23 C231 122.2(6) . . ? C22 C23 C231 131.0(7) . . ? C1 C101 C102 120.2(5) . . ? C1 C101 H101 119.9(3) . . ? C102 C101 H101 119.9(3) . . ? C103 C102 C101 120.7(5) . . ? C103 C102 H102 119.6(3) . . ? C101 C102 H102 119.6(3) . . ? C102 C103 C104 119.5(5) . . ? C102 C103 H103 120.3(3) . . ? C104 C103 H103 120.3(3) . . ? C103 C104 C105 120.3(5) . . ? C103 C104 H104 119.9(3) . . ? C105 C104 H104 119.9(3) . . ? C1 C105 C104 121.6(5) . . ? C1 C105 H105 119.2(2) . . ? C104 C105 H105 119.2(3) . . ? C11 C111 H11A 109.5(4) . . ? C11 C111 H11B 109.5(4) . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5(4) . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C13 C131 H13A 109.5(3) . . ? C13 C131 H13B 109.5(3) . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5(3) . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C2 C201 C202 121.1(5) . . ? C2 C201 H201 119.5(3) . . ? C202 C201 H201 119.5(3) . . ? C203 C202 C201 120.8(5) . . ? C203 C202 H202 119.6(3) . . ? C201 C202 H202 119.6(3) . . ? C202 C203 C204 118.9(5) . . ? C202 C203 H203 120.5(3) . . ? C204 C203 H203 120.5(3) . . ? C203 C204 C205 120.6(5) . . ? C203 C204 H204 119.7(3) . . ? C205 C204 H204 119.7(3) . . ? C2 C205 C204 121.3(5) . . ? C2 C205 H205 119.4(3) . . ? C204 C205 H205 119.4(3) . . ? C21 C211 H21A 109.5(5) . . ? C21 C211 H21B 109.5(4) . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5(4) . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C23 C231 H23A 109.5(4) . . ? C23 C231 H23B 109.5(4) . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5(4) . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C302 C301 C3 119.9(5) . . ? C302 C301 H301 120.0(3) . . ? C3 C301 H301 120.0(3) . . ? C303 C302 C301 120.5(5) . . ? C303 C302 H302 119.8(3) . . ? C301 C302 H302 119.8(3) . . ? C304 C303 C302 120.2(5) . . ? C304 C303 H303 119.9(4) . . ? C302 C303 H303 119.9(3) . . ? C303 C304 C305 119.9(6) . . ? C303 C304 H304 120.1(4) . . ? C305 C304 H304 120.1(4) . . ? C304 C305 C3 120.8(5) . . ? C304 C305 H305 119.6(4) . . ? C3 C305 H305 119.6(3) . . ? O B N11 104.4(4) . . ? O B N21 104.4(5) . . ? N11 B N21 107.6(4) . . ? O B H0 113.2(3) . . ? N11 B H0 113.2(3) . . ? N21 B H0 113.2(3) . . ? O C1A C2A 105.6(10) . . ? O C1A H1A1 110.6(4) . . ? C2A C1A H1A1 110.6(7) . . ? O C1A H1A2 110.6(5) . . ? C2A C1A H1A2 110.6(7) . . ? H1A1 C1A H1A2 108.7 . . ? C1A C2A H2A1 109.5(7) . . ? C1A C2A H2A2 109.5(7) . . ? H2A1 C2A H2A2 109.5 . . ? C1A C2A H2A3 109.5(7) . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C2B C1B O 104.6(12) . . ? C2B C1B H1B1 110.8(7) . . ? O C1B H1B1 110.8(5) . . ? C2B C1B H1B2 110.8(8) . . ? O C1B H1B2 110.8(5) . . ? H1B1 C1B H1B2 108.9 . . ? C1B C2B H2B1 109.5(9) . . ? C1B C2B H2B2 109.5(8) . . ? H2B1 C2B H2B2 109.5 . . ? C1B C2B H2B3 109.5(7) . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C1A O B 118.2(5) . . ? B O C1B 110.7(5) . . ? C1A O Re 134.8(5) . . ? B O Re 103.3(3) . . ? C1B O Re 115.0(6) . . ? _refine_diff_density_max 1.065 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.084 data_rehp2b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H44 B N4 O2 P2 Re' _chemical_formula_weight 919.78 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.625(2) _cell_length_b 12.683(3) _cell_length_c 15.885(4) _cell_angle_alpha 96.65(2) _cell_angle_beta 100.20(2) _cell_angle_gamma 115.54(2) _cell_volume 2030.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method ? _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 3.113 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6692 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.02 _reflns_number_total 6370 _reflns_number_observed 5498 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 315 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1232P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6055 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_obs 0.0618 _refine_ls_wR_factor_all 0.1845 _refine_ls_wR_factor_obs 0.1560 _refine_ls_goodness_of_fit_all 1.123 _refine_ls_goodness_of_fit_obs 1.127 _refine_ls_restrained_S_all 1.234 _refine_ls_restrained_S_obs 1.127 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.01875(3) 0.01956(3) 0.25999(2) 0.0266(2) Uani 1 d . . P1 P -0.1437(2) 0.0808(2) 0.2484(2) 0.0282(5) Uani 1 d . . P2 P 0.2078(2) 0.1950(2) 0.3089(2) 0.0295(5) Uani 1 d . . O1 O -0.0979(6) -0.1373(6) 0.1468(4) 0.0333(15) Uani 1 d . . O2 O -0.1331(9) -0.3491(7) 0.1141(6) 0.057(2) Uani 1 d . . N1 N -0.0789(7) -0.1329(7) 0.3144(5) 0.028(2) Uani 1 d . . N2 N 0.1418(9) -0.0732(8) 0.2456(6) 0.038(2) Uani 1 d . . N11 N -0.1204(9) -0.2425(8) 0.2602(6) 0.041(2) Uani 1 d . . N21 N 0.0737(10) -0.1869(8) 0.1998(6) 0.043(2) Uani 1 d . . C10 C -0.0860(14) -0.1225(12) 0.0598(7) 0.058(3) Uani 1 d . . H10A H -0.1007(14) -0.0563(12) 0.0479(7) 0.181(42) Uiso 1 calc R . H10B H -0.1500(14) -0.1941(12) 0.0180(7) 0.181(42) Uiso 1 calc R . H10C H 0.0009(14) -0.1073(12) 0.0554(7) 0.181(42) Uiso 1 calc R . C11 C -0.1860(13) -0.3302(11) 0.2983(9) 0.057(3) Uani 1 d . . H11 H -0.2232(13) -0.4117(11) 0.2744(9) 0.054(15) Uiso 1 calc R . C12 C -0.1899(13) -0.2796(12) 0.3800(9) 0.060(3) Uani 1 d . . H12 H -0.2293(13) -0.3186(12) 0.4211(9) 0.054(15) Uiso 1 calc R . C13 C -0.1215(11) -0.1576(11) 0.3854(7) 0.045(3) Uani 1 d . . H13 H -0.1070(11) -0.0997(11) 0.4333(7) 0.054(15) Uiso 1 calc R . C20 C -0.2736(17) -0.4030(13) 0.0752(11) 0.085(5) Uani 1 d . . H20A H -0.3012(17) -0.4777(13) 0.0358(11) 0.181(42) Uiso 1 calc R . H20B H -0.2930(17) -0.3501(13) 0.0436(11) 0.181(42) Uiso 1 calc R . H20C H -0.3197(17) -0.4170(13) 0.1206(11) 0.181(42) Uiso 1 calc R . C21 C 0.1566(13) -0.2353(11) 0.1978(8) 0.050(3) Uani 1 d . . H21 H 0.1330(13) -0.3137(11) 0.1718(8) 0.054(15) Uiso 1 calc R . C22 C 0.2791(12) -0.1506(12) 0.2401(8) 0.054(3) Uani 1 d . . H22 H 0.3561(12) -0.1582(12) 0.2481(8) 0.054(15) Uiso 1 calc R . C23 C 0.2671(11) -0.0513(11) 0.2688(7) 0.042(3) Uani 1 d . . H23 H 0.3367(11) 0.0217(11) 0.3002(7) 0.054(15) Uiso 1 calc R . C111 C -0.3079(9) -0.0396(9) 0.1843(7) 0.034(2) Uani 1 d . . C112 C -0.3550(11) -0.1505(10) 0.2046(8) 0.048(3) Uani 1 d . . H112 H -0.3023(11) -0.1630(10) 0.2496(8) 0.055(7) Uiso 1 calc R . C113 C -0.4762(11) -0.2439(11) 0.1616(9) 0.058(3) Uani 1 d . . H113 H -0.5050(11) -0.3184(11) 0.1761(9) 0.055(7) Uiso 1 calc R . C114 C -0.5537(12) -0.2228(13) 0.0958(9) 0.062(4) Uani 1 d . . H114 H -0.6359(12) -0.2845(13) 0.0651(9) 0.055(7) Uiso 1 calc R . C115 C -0.5131(12) -0.1170(14) 0.0761(8) 0.065(4) Uani 1 d . . H115 H -0.5678(12) -0.1047(14) 0.0323(8) 0.055(7) Uiso 1 calc R . C116 C -0.3909(12) -0.0236(12) 0.1189(8) 0.053(3) Uani 1 d . . H116 H -0.3641(12) 0.0504(12) 0.1037(8) 0.055(7) Uiso 1 calc R . C211 C -0.1967(9) 0.1237(8) 0.3452(6) 0.028(2) Uani 1 d . . C212 C -0.1196(9) 0.1530(9) 0.4280(6) 0.032(2) Uani 1 d . . H212 H -0.0390(9) 0.1518(9) 0.4359(6) 0.055(7) Uiso 1 calc R . C213 C -0.1583(11) 0.1851(10) 0.5020(7) 0.045(3) Uani 1 d . . H213 H -0.1051(11) 0.2026(10) 0.5580(7) 0.055(7) Uiso 1 calc R . C214 C -0.2757(11) 0.1901(11) 0.4901(8) 0.048(3) Uani 1 d . . H214 H -0.3026(11) 0.2118(11) 0.5381(8) 0.055(7) Uiso 1 calc R . C215 C -0.3539(11) 0.1626(11) 0.4059(8) 0.049(3) Uani 1 d . . H215 H -0.4329(11) 0.1667(11) 0.3978(8) 0.055(7) Uiso 1 calc R . C216 C -0.3159(10) 0.1291(10) 0.3333(7) 0.041(2) Uani 1 d . . H216 H -0.3695(10) 0.1104(10) 0.2773(7) 0.055(7) Uiso 1 calc R . C311 C -0.1260(9) 0.2022(9) 0.1894(7) 0.034(2) Uani 1 d . . C312 C -0.1318(10) 0.3043(9) 0.2231(7) 0.039(2) Uani 1 d . . H312 H -0.1443(10) 0.3147(9) 0.2791(7) 0.055(7) Uiso 1 calc R . C313 C -0.1193(11) 0.3921(11) 0.1755(9) 0.048(3) Uani 1 d . . H313 H -0.1232(11) 0.4605(11) 0.1997(9) 0.055(7) Uiso 1 calc R . C314 C -0.1012(11) 0.3781(12) 0.0928(10) 0.058(4) Uani 1 d . . H314 H -0.0924(11) 0.4366(12) 0.0605(10) 0.055(7) Uiso 1 calc R . C315 C -0.0964(14) 0.2767(13) 0.0585(8) 0.062(4) Uani 1 d . . H315 H -0.0853(14) 0.2658(13) 0.0021(8) 0.055(7) Uiso 1 calc R . C316 C -0.1077(13) 0.1902(12) 0.1064(8) 0.053(3) Uani 1 d . . H316 H -0.1029(13) 0.1224(12) 0.0820(8) 0.055(7) Uiso 1 calc R . C411 C 0.1993(9) 0.3373(9) 0.3184(7) 0.033(2) Uani 1 d . . C412 C 0.1608(11) 0.3769(10) 0.3877(8) 0.043(3) Uani 1 d . . H412 H 0.1432(11) 0.3337(10) 0.4314(8) 0.055(7) Uiso 1 calc R . C413 C 0.1482(13) 0.4821(12) 0.3922(9) 0.061(4) Uani 1 d . . H413 H 0.1218(13) 0.5079(12) 0.4390(9) 0.055(7) Uiso 1 calc R . C414 C 0.1739(12) 0.5474(11) 0.3296(9) 0.057(3) Uani 1 d . . H414 H 0.1660(12) 0.6176(11) 0.3337(9) 0.055(7) Uiso 1 calc R . C415 C 0.2122(12) 0.5080(11) 0.2592(9) 0.054(3) Uani 1 d . . H415 H 0.2289(12) 0.5512(11) 0.2154(9) 0.055(7) Uiso 1 calc R . C416 C 0.2253(11) 0.4037(10) 0.2547(8) 0.048(3) Uani 1 d . . H416 H 0.2521(11) 0.3782(10) 0.2080(8) 0.055(7) Uiso 1 calc R . C511 C 0.3348(9) 0.2237(9) 0.2449(7) 0.035(2) Uani 1 d . . C512 C 0.4651(11) 0.3010(11) 0.2795(9) 0.054(3) Uani 1 d . . H512 H 0.4935(11) 0.3431(11) 0.3373(9) 0.055(7) Uiso 1 calc R . C513 C 0.5568(13) 0.3180(12) 0.2294(11) 0.066(4) Uani 1 d . . H513 H 0.6457(13) 0.3690(12) 0.2550(11) 0.055(7) Uiso 1 calc R . C514 C 0.5182(14) 0.2613(15) 0.1439(10) 0.071(4) Uani 1 d . . H514 H 0.5792(14) 0.2743(15) 0.1104(10) 0.055(7) Uiso 1 calc R . C515 C 0.3861(14) 0.1839(18) 0.1078(10) 0.092(6) Uani 1 d . . H515 H 0.3564(14) 0.1441(18) 0.0493(10) 0.055(7) Uiso 1 calc R . C516 C 0.2999(12) 0.1666(14) 0.1593(9) 0.066(4) Uani 1 d . . H516 H 0.2118(12) 0.1124(14) 0.1344(9) 0.055(7) Uiso 1 calc R . C611 C 0.3099(9) 0.2183(9) 0.4200(7) 0.033(2) Uani 1 d . . C612 C 0.2946(10) 0.1205(10) 0.4565(7) 0.038(2) Uani 1 d . . H612 H 0.2290(10) 0.0449(10) 0.4263(7) 0.055(7) Uiso 1 calc R . C613 C 0.3729(10) 0.1321(10) 0.5355(7) 0.040(3) Uani 1 d . . H613 H 0.3607(10) 0.0646(10) 0.5579(7) 0.055(7) Uiso 1 calc R . C614 C 0.4689(11) 0.2419(11) 0.5815(7) 0.048(3) Uani 1 d . . H614 H 0.5220(11) 0.2488(11) 0.6352(7) 0.055(7) Uiso 1 calc R . C615 C 0.4880(11) 0.3426(11) 0.5495(8) 0.048(3) Uani 1 d . . H615 H 0.5534(11) 0.4176(11) 0.5809(8) 0.055(7) Uiso 1 calc R . C616 C 0.4071(10) 0.3298(10) 0.4691(8) 0.046(3) Uani 1 d . . H616 H 0.4184(10) 0.3978(10) 0.4474(8) 0.055(7) Uiso 1 calc R . B B -0.0779(12) -0.2376(9) 0.1742(7) 0.034(3) Uani 1 d . . H1 H 0.0475 0.0843 0.1736 0.050 Uiso 1 d . . H2 H 0.0403 0.0725 0.3651 0.050 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0227(2) 0.0373(3) 0.0283(2) 0.0076(2) 0.0027(2) 0.0227(2) P1 0.0253(12) 0.0401(14) 0.0283(12) 0.0075(11) 0.0026(10) 0.0249(12) P2 0.0240(12) 0.0360(14) 0.0329(13) 0.0097(11) 0.0029(10) 0.0190(11) O1 0.032(4) 0.046(4) 0.024(3) 0.005(3) 0.003(3) 0.022(3) O2 0.064(6) 0.047(5) 0.060(5) 0.000(4) 0.005(4) 0.033(4) N1 0.033(4) 0.041(5) 0.029(4) 0.012(4) 0.011(4) 0.030(4) N2 0.040(5) 0.049(6) 0.043(5) 0.014(4) 0.013(4) 0.034(5) N11 0.052(6) 0.035(5) 0.044(5) 0.014(4) 0.014(4) 0.025(4) N21 0.060(6) 0.048(6) 0.041(5) 0.011(4) 0.017(5) 0.041(5) C10 0.085(10) 0.069(8) 0.031(6) 0.020(6) 0.007(6) 0.048(8) C11 0.057(8) 0.043(7) 0.070(9) 0.017(6) 0.019(7) 0.021(6) C12 0.058(8) 0.073(9) 0.058(8) 0.034(7) 0.022(7) 0.032(7) C13 0.045(6) 0.069(8) 0.043(6) 0.026(6) 0.015(5) 0.042(6) C20 0.088(12) 0.060(9) 0.088(12) 0.002(8) -0.011(9) 0.034(9) C21 0.072(9) 0.063(8) 0.050(7) 0.022(6) 0.023(7) 0.057(7) C22 0.045(7) 0.088(9) 0.056(7) 0.017(7) 0.010(6) 0.056(7) C23 0.037(6) 0.063(7) 0.055(7) 0.021(6) 0.010(5) 0.047(6) C111 0.025(5) 0.047(6) 0.035(5) 0.002(5) 0.006(4) 0.024(5) C112 0.035(6) 0.058(7) 0.061(7) 0.018(6) 0.002(5) 0.034(6) C113 0.030(6) 0.049(7) 0.086(10) 0.015(7) 0.006(6) 0.015(6) C114 0.037(7) 0.068(9) 0.052(8) -0.017(7) -0.001(6) 0.011(6) C115 0.043(7) 0.086(10) 0.048(7) 0.005(7) -0.026(6) 0.029(7) C116 0.045(7) 0.068(8) 0.051(7) 0.025(6) 0.000(6) 0.031(6) C211 0.027(5) 0.036(5) 0.026(5) 0.005(4) 0.000(4) 0.022(4) C212 0.027(5) 0.045(6) 0.030(5) 0.006(4) 0.005(4) 0.023(5) C213 0.035(6) 0.055(7) 0.036(6) -0.010(5) -0.003(5) 0.023(5) C214 0.045(7) 0.060(7) 0.048(7) 0.002(6) 0.015(6) 0.032(6) C215 0.043(6) 0.075(8) 0.053(7) 0.013(6) 0.015(6) 0.047(6) C216 0.034(6) 0.058(7) 0.038(6) 0.005(5) 0.005(5) 0.030(5) C311 0.025(5) 0.043(6) 0.041(6) 0.016(5) 0.001(4) 0.024(5) C312 0.035(6) 0.041(6) 0.050(6) 0.010(5) 0.008(5) 0.027(5) C313 0.041(6) 0.049(7) 0.066(8) 0.020(6) 0.012(6) 0.029(6) C314 0.041(7) 0.064(8) 0.088(10) 0.042(8) 0.010(7) 0.037(6) C315 0.086(10) 0.087(10) 0.042(7) 0.037(7) 0.023(7) 0.057(9) C316 0.069(8) 0.076(9) 0.042(6) 0.025(6) 0.020(6) 0.054(7) C411 0.022(5) 0.041(6) 0.041(6) 0.009(5) 0.001(4) 0.020(4) C412 0.040(6) 0.041(6) 0.049(6) 0.013(5) 0.006(5) 0.021(5) C413 0.055(8) 0.064(8) 0.069(8) -0.006(7) -0.001(7) 0.043(7) C414 0.057(8) 0.047(7) 0.067(8) 0.011(6) -0.009(7) 0.034(6) C415 0.051(7) 0.054(7) 0.061(8) 0.025(6) -0.006(6) 0.031(6) C416 0.046(7) 0.050(7) 0.054(7) 0.023(6) 0.010(6) 0.026(6) C511 0.029(5) 0.051(6) 0.040(6) 0.023(5) 0.010(4) 0.029(5) C512 0.036(6) 0.062(8) 0.063(8) 0.011(6) 0.010(6) 0.022(6) C513 0.038(7) 0.066(9) 0.107(12) 0.030(8) 0.038(8) 0.024(7) C514 0.051(8) 0.108(12) 0.066(9) 0.029(9) 0.030(7) 0.040(8) C515 0.047(8) 0.170(18) 0.046(8) 0.005(10) 0.015(7) 0.044(10) C516 0.025(6) 0.111(12) 0.053(8) 0.011(8) 0.013(6) 0.024(7) C611 0.024(5) 0.040(6) 0.042(6) 0.011(5) 0.003(4) 0.023(5) C612 0.030(5) 0.049(6) 0.041(6) 0.008(5) 0.006(5) 0.025(5) C613 0.036(6) 0.052(7) 0.040(6) 0.023(5) 0.004(5) 0.028(6) C614 0.036(6) 0.073(8) 0.042(6) 0.028(6) -0.001(5) 0.031(6) C615 0.037(6) 0.049(7) 0.046(6) 0.006(5) -0.011(5) 0.019(5) C616 0.036(6) 0.042(6) 0.056(7) 0.012(5) -0.005(5) 0.021(5) B 0.048(7) 0.021(5) 0.034(6) -0.005(5) 0.008(5) 0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N1 2.149(8) . ? Re1 N2 2.233(8) . ? Re1 O1 2.239(7) . ? Re1 P2 2.272(3) . ? Re1 P1 2.319(2) . ? Re1 H1 1.6902(5) . ? Re1 H2 1.6583(6) . ? P1 C311 1.849(10) . ? P1 C111 1.857(10) . ? P1 C211 1.863(9) . ? P2 C411 1.840(10) . ? P2 C611 1.857(10) . ? P2 C511 1.872(10) . ? O1 C10 1.439(12) . ? O1 B 1.486(13) . ? O2 B 1.419(13) . ? O2 C20 1.45(2) . ? N1 C13 1.328(13) . ? N1 N11 1.379(12) . ? N2 C23 1.331(13) . ? N2 N21 1.344(13) . ? N11 C11 1.332(14) . ? N11 B 1.532(14) . ? N21 C21 1.350(14) . ? N21 B 1.55(2) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 C12 1.40(2) . ? C11 H11 0.93 . ? C12 C13 1.38(2) . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 C22 1.34(2) . ? C21 H21 0.93 . ? C22 C23 1.36(2) . ? C22 H22 0.93 . ? C23 H23 0.93 . ? C111 C112 1.37(2) . ? C111 C116 1.383(15) . ? C112 C113 1.37(2) . ? C112 H112 0.93 . ? C113 C114 1.38(2) . ? C113 H113 0.93 . ? C114 C115 1.31(2) . ? C114 H114 0.93 . ? C115 C116 1.38(2) . ? C115 H115 0.93 . ? C116 H116 0.93 . ? C211 C212 1.361(13) . ? C211 C216 1.398(13) . ? C212 C213 1.408(14) . ? C212 H212 0.93 . ? C213 C214 1.38(2) . ? C213 H213 0.93 . ? C214 C215 1.39(2) . ? C214 H214 0.93 . ? C215 C216 1.389(15) . ? C215 H215 0.93 . ? C216 H216 0.93 . ? C311 C312 1.378(14) . ? C311 C316 1.374(15) . ? C312 C313 1.388(15) . ? C312 H312 0.93 . ? C313 C314 1.37(2) . ? C313 H313 0.93 . ? C314 C315 1.37(2) . ? C314 H314 0.93 . ? C315 C316 1.38(2) . ? C315 H315 0.93 . ? C316 H316 0.93 . ? C411 C412 1.38(2) . ? C411 C416 1.382(15) . ? C412 C413 1.40(2) . ? C412 H412 0.93 . ? C413 C414 1.36(2) . ? C413 H413 0.93 . ? C414 C415 1.39(2) . ? C414 H414 0.93 . ? C415 C416 1.39(2) . ? C415 H415 0.93 . ? C416 H416 0.93 . ? C511 C512 1.36(2) . ? C511 C516 1.36(2) . ? C512 C513 1.40(2) . ? C512 H512 0.93 . ? C513 C514 1.36(2) . ? C513 H513 0.93 . ? C514 C515 1.38(2) . ? C514 H514 0.93 . ? C515 C516 1.37(2) . ? C515 H515 0.93 . ? C516 H516 0.93 . ? C611 C612 1.384(14) . ? C611 C616 1.393(15) . ? C612 C613 1.365(14) . ? C612 H612 0.93 . ? C613 C614 1.36(2) . ? C613 H613 0.93 . ? C614 C615 1.37(2) . ? C614 H614 0.93 . ? C615 C616 1.39(2) . ? C615 H615 0.93 . ? C616 H616 0.93 . ? 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 N1 Re1 N2 79.5(3) . . ? N1 Re1 O1 73.4(3) . . ? N2 Re1 O1 73.1(3) . . ? N1 Re1 P2 134.7(2) . . ? N2 Re1 P2 88.3(2) . . ? O1 Re1 P2 143.5(2) . . ? N1 Re1 P1 96.7(2) . . ? N2 Re1 P1 166.9(2) . . ? O1 Re1 P1 93.8(2) . . ? P2 Re1 P1 102.95(9) . . ? N1 Re1 H1 151.4(2) . . ? N2 Re1 H1 94.8(2) . . ? O1 Re1 H1 78.1(2) . . ? P2 Re1 H1 72.34(7) . . ? P1 Re1 H1 82.54(6) . . ? N1 Re1 H2 73.7(2) . . ? N2 Re1 H2 110.0(2) . . ? O1 Re1 H2 145.6(2) . . ? P2 Re1 H2 69.98(7) . . ? P1 Re1 H2 80.51(6) . . ? H1 Re1 H2 133.61(3) . . ? C311 P1 C111 100.9(5) . . ? C311 P1 C211 102.4(4) . . ? C111 P1 C211 97.2(4) . . ? C311 P1 Re1 117.4(3) . . ? C111 P1 Re1 112.7(3) . . ? C211 P1 Re1 122.5(3) . . ? C411 P2 C611 100.2(5) . . ? C411 P2 C511 100.5(5) . . ? C611 P2 C511 99.9(4) . . ? C411 P2 Re1 119.4(3) . . ? C611 P2 Re1 116.6(3) . . ? C511 P2 Re1 116.9(4) . . ? C10 O1 B 115.4(8) . . ? C10 O1 Re1 119.5(7) . . ? B O1 Re1 105.7(5) . . ? B O2 C20 115.9(10) . . ? C13 N1 N11 105.5(8) . . ? C13 N1 Re1 139.3(7) . . ? N11 N1 Re1 115.1(6) . . ? C23 N2 N21 106.1(8) . . ? C23 N2 Re1 139.6(8) . . ? N21 N2 Re1 114.3(6) . . ? C11 N11 N1 110.0(9) . . ? C11 N11 B 134.6(10) . . ? N1 N11 B 115.4(8) . . ? N2 N21 C21 109.3(10) . . ? N2 N21 B 115.5(8) . . ? C21 N21 B 134.4(10) . . ? O1 C10 H10A 109.5(6) . . ? O1 C10 H10B 109.5(6) . . ? H10A C10 H10B 109.5 . . ? O1 C10 H10C 109.5(6) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N11 C11 C12 108.7(11) . . ? N11 C11 H11 125.6(7) . . ? C12 C11 H11 125.6(7) . . ? C13 C12 C11 103.7(11) . . ? C13 C12 H12 128.2(7) . . ? C11 C12 H12 128.2(7) . . ? N1 C13 C12 112.2(11) . . ? N1 C13 H13 123.9(6) . . ? C12 C13 H13 123.9(7) . . ? O2 C20 H20A 109.5(7) . . ? O2 C20 H20B 109.5(7) . . ? H20A C20 H20B 109.5 . . ? O2 C20 H20C 109.5(8) . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N21 108.2(11) . . ? C22 C21 H21 125.9(7) . . ? N21 C21 H21 125.9(7) . . ? C21 C22 C23 105.8(10) . . ? C21 C22 H22 127.1(7) . . ? C23 C22 H22 127.1(7) . . ? N2 C23 C22 110.6(11) . . ? N2 C23 H23 124.7(6) . . ? C22 C23 H23 124.7(7) . . ? C112 C111 C116 116.6(10) . . ? C112 C111 P1 119.3(8) . . ? C116 C111 P1 124.0(9) . . ? C113 C112 C111 123.1(11) . . ? C113 C112 H112 118.4(7) . . ? C111 C112 H112 118.4(6) . . ? C112 C113 C114 117.5(12) . . ? C112 C113 H113 121.3(7) . . ? C114 C113 H113 121.3(8) . . ? C115 C114 C113 121.0(12) . . ? C115 C114 H114 119.5(8) . . ? C113 C114 H114 119.5(8) . . ? C114 C115 C116 121.3(11) . . ? C114 C115 H115 119.3(8) . . ? C116 C115 H115 119.3(7) . . ? C115 C116 C111 120.4(11) . . ? C115 C116 H116 119.8(7) . . ? C111 C116 H116 119.8(7) . . ? C212 C211 C216 118.8(9) . . ? C212 C211 P1 121.2(7) . . ? C216 C211 P1 120.0(7) . . ? C211 C212 C213 122.0(9) . . ? C211 C212 H212 119.0(6) . . ? C213 C212 H212 119.0(6) . . ? C214 C213 C212 119.0(10) . . ? C214 C213 H213 120.5(7) . . ? C212 C213 H213 120.5(6) . . ? C213 C214 C215 119.5(10) . . ? C213 C214 H214 120.3(7) . . ? C215 C214 H214 120.3(6) . . ? C216 C215 C214 121.1(10) . . ? C216 C215 H215 119.4(6) . . ? C214 C215 H215 119.4(6) . . ? C215 C216 C211 119.6(10) . . ? C215 C216 H216 120.2(6) . . ? C211 C216 H216 120.2(6) . . ? C312 C311 C316 117.3(10) . . ? C312 C311 P1 124.0(8) . . ? C316 C311 P1 118.7(8) . . ? C311 C312 C313 121.6(11) . . ? C311 C312 H312 119.2(6) . . ? C313 C312 H312 119.2(7) . . ? C314 C313 C312 120.0(11) . . ? C314 C313 H313 120.0(7) . . ? C312 C313 H313 120.0(7) . . ? C315 C314 C313 118.9(11) . . ? C315 C314 H314 120.6(8) . . ? C313 C314 H314 120.6(7) . . ? C314 C315 C316 120.8(12) . . ? C314 C315 H315 119.6(8) . . ? C316 C315 H315 119.6(8) . . ? C311 C316 C315 121.4(12) . . ? C311 C316 H316 119.3(7) . . ? C315 C316 H316 119.3(8) . . ? C412 C411 C416 118.7(10) . . ? C412 C411 P2 120.2(8) . . ? C416 C411 P2 121.0(8) . . ? C411 C412 C413 119.9(11) . . ? C411 C412 H412 120.0(6) . . ? C413 C412 H412 120.0(8) . . ? C414 C413 C412 121.3(13) . . ? C414 C413 H413 119.4(8) . . ? C412 C413 H413 119.4(8) . . ? C413 C414 C415 119.3(11) . . ? C413 C414 H414 120.4(8) . . ? C415 C414 H414 120.4(7) . . ? C416 C415 C414 119.6(11) . . ? C416 C415 H415 120.2(8) . . ? C414 C415 H415 120.2(7) . . ? C411 C416 C415 121.2(12) . . ? C411 C416 H416 119.4(7) . . ? C415 C416 H416 119.4(8) . . ? C512 C511 C516 116.3(10) . . ? C512 C511 P2 123.1(9) . . ? C516 C511 P2 120.6(8) . . ? C511 C512 C513 121.0(13) . . ? C511 C512 H512 119.5(7) . . ? C513 C512 H512 119.5(9) . . ? C514 C513 C512 121.1(13) . . ? C514 C513 H513 119.5(8) . . ? C512 C513 H513 119.5(9) . . ? C513 C514 C515 118.4(13) . . ? C513 C514 H514 120.8(8) . . ? C515 C514 H514 120.8(9) . . ? C516 C515 C514 119.0(14) . . ? C516 C515 H515 120.5(9) . . ? C514 C515 H515 120.5(9) . . ? C511 C516 C515 124.2(12) . . ? C511 C516 H516 117.9(6) . . ? C515 C516 H516 117.9(9) . . ? C612 C611 C616 116.7(9) . . ? C612 C611 P2 119.6(8) . . ? C616 C611 P2 123.6(7) . . ? C613 C612 C611 121.8(10) . . ? C613 C612 H612 119.1(7) . . ? C611 C612 H612 119.1(6) . . ? C614 C613 C612 120.4(10) . . ? C614 C613 H613 119.8(6) . . ? C612 C613 H613 119.8(7) . . ? C613 C614 C615 120.6(10) . . ? C613 C614 H614 119.7(6) . . ? C615 C614 H614 119.7(7) . . ? C614 C615 C616 118.6(11) . . ? C614 C615 H615 120.7(7) . . ? C616 C615 H615 120.7(7) . . ? C611 C616 C615 121.9(10) . . ? C611 C616 H616 119.1(6) . . ? C615 C616 H616 119.1(7) . . ? O2 B O1 119.6(9) . . ? O2 B N11 115.3(9) . . ? O1 B N11 102.2(7) . . ? O2 B N21 108.4(9) . . ? O1 B N21 103.8(8) . . ? N11 B N21 106.2(9) . . ? _refine_diff_density_max 4.669 _refine_diff_density_min -3.152 _refine_diff_density_rms 0.256